Document Ozwd7B9OY4a3Mm1JjzjNYjQ2X

THE SHERWIN-WILLIAMS COMPANY COATINGS DIVISION SPECIFICATION FOR PURCHASED MATERIAL PG: 01 S.W. CODE: 031710 CAS NO: 108-8o-3 WH__MATWRIAL- TOLIMNR SUPPLIER: ASHLAND DISTRIBUTION CO-2250 MATERIAL: TOLUENE CODE: VERSION NO 14 TEST DESCRIPTION & PROCEDURE REVISION DATE: 11/09/1995 Method Code Minimum HTC: 2902.30 ISSUED BY MRW78C Maximum Units PHYSICAL APPEARANCE SEE ADDNL. INFO BELOW ITM 999.001 CERTIFICATE OF ANALYSIS WITH OR aeFORE SHIPMENT: OR BEFORE SHIPMENT: MUST ADD ANTI-STATIC ADDITIVE TO SHIPMENT. STATE "YES' ON COA, DISTILLATION OF AROMATIC HC 1 , DEG C RANGE ASTM DB50 109.6 COLOR, PT-CO SCALE (APHA UNITS) ASTM D1209 SPECIFIC GRAVITY AT 15.6/15.6 DEG C ASTM D891 0.869 WARRANTED QUALITY LIMITS: IR ANALYSIS, QUALITATIVE MATCH STANDARD SPECTRUM ITM 543.000 % H2O IN VOLATILE SOLVENTS FISCHER REAGENT TITRATION ASTM D1364 GC ANALYSIS OF SOLVENT M/XT'S, MATCH STD CURVE ITM 741.200 SPECIFIC GRAVITY AT 25/25 DEG C ASTM D891 0.960 AROMATICS IN HYDROCARBON SOLV BY GC, XYLENE ETHYLBENZENE ASTM D2306 REFRACTIVE INDEX ri 20 DEG C ASTM 0I218 1.494 ACIDITY OF AROMATIC HC'S MG NAOH/100 ML SAMPLE ASTM D847 COPPER CORROSION FOR AROMATIC HYDROCARBONS ASTM DB49 AROMATICS IN HYDROCARBON SOLV BY GC, BENZENE ASTM D2306 AROMATICS IN HYDROCARBON SOLV BY GC, TOLUENE ASTM D2306 99.5 CONDUCTIVITY OF HYDROCARBON FUELS. ASTM D2624 1000 ADDITIONAL INFORMATION: 1)PHYSICAL APPEARANCE 2)ANTI-STATIC ADDITIVE 3)COPPER CORROSION CLEAR, WATER WHITE LIQUID, FREE OF SUSPENDED MATTER. USE DUPONT STADIS 450 TO MEET MINIMUM CONDUCTIVITY. APPROXIMATELY 4 PPM. PASS 111.6 20 0,873 0.02 0.866 0,2 1.497 0.005 0.03 N/A DEG C NONE N/A N/A N/A G/CC VOL % NONE VOL % VOL% PS/M * CONTINUED ON NEXT PAGE THE SHERWIN-WILLIAMS COMPANY COATINGS DIVISION SPECIFICATION FOR PURCHASED MATERIAL PG: 02 S.W. CODE: 031710 CAS NO: loa-BB -a TOLUPNE SUPPLIER: ASHLAND DISTRIBUTION CO-2250 MATERIAL: TOLUENE CODE: VERSION NO: 14 REVISION DATE: 11/09/1995 HTC: 2902.30 ISSUED BY: MRW78C PRACTICAL REQUIREMENTS: THE MATERIAL SHALL REMAIN CONSTANT IN SUCCESSIVE LOTS OR SHIPMENTS WITH RESPECT TO UNSPECIFIED CHARACTERISTICS TO THE EXTENT THAT THE SELLER WARRANTS THAT NO KNOWN CHANGES ARE TO BE MADE IN PHYSICAL OR CHEMICAL PROPERTIES OF THIS MATERIAL WITHOUT THE DUE NOTIFICATION IN WRITING TO THE COATINGS DIVISION PURCHASING DEPARTMENT OF THE SHERWIN-WILLIAMS COMPANY. THE UNDERSIGNED HEREBY CERTIFIES THAT ALL PRODUCT DELIVERED UNDER THIS CODE NUMBER WILL MEET THE FOREGOING SPECIFICATION. BY: COMPANY: TITLE: DATE: ** LAST SPEC PAGE Or * sidid Ashland 11111111.1 "1 Ashland Distribution Company Division of Ashland, Inc. Customer Certificate of Analysis Industrial Chemicals & Solvents Division Ship Date: 11/22/02 Customer. Sherwin Williams Company Product: Toluene 03-17-10 HMIS 2300 Bons Lane South Tank No.: 169 Vessel: TOLUENE Richmond, KY 40475 Ship Quantity: 6721 Ticket: 24792 Fax 9: 614-790-6624 1C&S PO / Lot No.: 4500561750-C3C0 Attn: Deb Nist (WM Columbus) Analysis Test Method Customer PO No.: Specification P80970C2-214 V/P Test Results Appearance Specific Gravity, g/mL gi60F Gravity, pounds/plko Saybok Color Pt / Co Color (APHA) Acid Wash Color Knurl-Butasol Value Sulfur Compounds (MS, SO2) Sulfttr, ppm Acidity Copper Strip Corrosion Saturates, % Benzene, % Toluene, % Xylene, % > Xylene, % Initial Boiling Point, C Dry Point, C Dist Range, C Water Content, ppm visual D491 Cale D-156 1)-1209 D441 D-1133 0-853 D-3961/4045 D447 D-130/849 D-2306 D-2306 13-2306 D-2306 D-2306 0-850 0.850 D-850 Aquatest 0.869 to 0.873 report only report only 10 max. report only report only report only report only report only report only 0.5 max. 0.03 max. 99.5 min. 0.5 max. 0.5 max. 109.6 min. 111.6 max. 1 max. 500 max. Clear liquid, fres of particulates 0.3718 7.260 30 I ON 104 Nes 0.3 Nes 1B 0.03 Not detected 99.97 0.01 0.00 110.4 110.6 0.2 23 Pass Pass Pau Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pam Pam Pass Pass Pass WI 22 2002 And-Star added ANTI-STAY ADDED 360ML A Responsible Care Company Ashland Distribution Company, Division of Ashland Inc., Box 2219, Columbus, Ohio 43216 Shipment c/o Marathon Ashland Petroleum LLC, PO Box 1491, Cstlettsburg, Ky 41119, 606-921-6801 SW-Scearce 01264 agimeib. Ashland 414=11110 Ashland Distribution Company Division of Ashland, Inc. Customer Certificate of Analysis Industrial Chemicals & Solvents Division Ship Date: 11-25-2002 Customer: Sherwin Williams Company Product: Toluene 03.1740 HMIS 2300 Bous Lane South Tank No.: 170 Vessel: TOLUENE Richmond, KY 40475 Ship Quantity: 7083 Ticket: 24832 Fax #: 614-790-6624 Ann: Deb Nht (IC&S Columbus) Analysis Test Method !CIS PO / Lot No.: Customer PO No.: 45005671611-6a4 7pb0970e2 - 21 Specification Test Results Appearance Specific Gravity, WhIL gl60P Gravity, pounds/gallon Saybolt Color Pt / Co Color (APHA) Acid Wash Color Kauri-Butaaol Wu* Sulfur Compouads (1125, S02) Sulker, ppm Acidity Copper Strip Corrosion Saturates, % Bemuse, % Toluene, % Xylenr, % > Xylene, % Initial Boiling Point, C Dry Point, C Dist. Range, C Water Content, ppm visual 13491 Cale D-156 D-1209 . D-848 D-1133 13453 D-396114045 13447 D-1301849 D-2306 D-2306 D-2306 D-2306 D-2306 13450 D-850 12450 Aquatest 0.869 to 0173 report only report only ID mu. report only report only report only report only report only report only 0.5 max. 0.03 max. 99.5 mkt. 0.5 max. 0.5 mu. 109.6 min. 111.6 max. 1 max. 500 max. Clear liquid, free of particulates 0.8718 7.260 30 2 ON 106 Net 0.3 Net 1B 0.06 0.01 99.88 Not detected 0.06 110.5 110.6 0.1 33 Pass Pass Pass Pass .CA.71 Pass Pass /P) Pass Pass Pus omit: Pus Pass Pass Pass Pass Pass Pass Pass Pus Pass Pans Anti-Stet added APPROVED lS09002 A Responsible Care Company Ashland Distribution Company, Division of Ashland Inc., Box 2219. Columbus, Ohio 43216 Shipment do Marathon Ashland Petroleum LIZ. PO Son 1492. Canonsburg. 1Cy 41129. 606-9214802 F14.4-3a234 SW-Scearce 01263 V() Ashland Distribution Company Division of Ashland, Ina Customer Certificate of Analysis Industrial Chemicals & Solvents Division Ship Date: 11-25-02 Customer Sherwin Williams Company Product: Toluene 03-17-10 HMIS 2300 BOUS Lane South Richmond, KY 40475 Tank No.: 170 Ship Quantity: 7066 Vessel: 3225 Ticket: 24024 Fax #: 614-790.6624 IC&S PO / 1,ot No.: 4500561764-e30 Attn: Deb NW (IC&S Columbus) Analysis Test Method Customer PO No.: Specification pb0970e2 gh- 2.11. Test Results Appearance @AiSpecific Gravity, g/inL Gravity, pounda/plion Saybok Color Pt / Co Color (APHA) Acid Wash Color Kauri-Butanel Value Sulfur Compounds (H2S, SO2) Sulfur, ppnt Acidity Copper Strip Corrosion Saturates, % BeliZOIN, % Toluene, % Xylene, % > Xylem*, % Initial BoWng Point, C Dry Point, C Dist. Range, C Water Content, ppm visual D-891 Cale D-156 D-1209 D-8411 D-1133 0-853 D-3961/4045 D-847 0-130/849 D-2306 D-2306 0-2306 D-2306 D-2304 D-1150 0.850 D-850 Aquatest 0.869 to 0.873 report only report only 10 max. report only report only report only report only report only report only 0.5 max. 0.03 max. 99.3 min. 0.5 mu. 0.5 max. 109.6 min. 111.6 max. 1 max. 500 max. Clear liquid, free of particulates 0.8718 7.260 30 2 ON 106 Neg 0.3 Neg lB 0.06 0.01 99.81 Not detected 0.06 110.5 110.6 0.1 33 Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pus Pass Pass Pass Pass Pass Pass Pass Pass Pus An1I-Stal added ANTI-ETAT ADDED REL4216 A Responsible Care Company Ashland Distribution Company, Division of Ashland Inc., Box 2219, Columbus, Ohio 43216 Shipment do Munition Ashland Petroleum LLC, PO Box 1492, Catlettsburg, Ky 41129, 60 6921-6802 SW-Scearce 01262 dirommop itieW 4111111111111PP Aslard Diu:dance Comp eliy Division of Ashland, liss. Customer Certificate of Analysis Cuba= Sherwin Willow Clamor firg Loot *gab NicbgjonolKif 40475 Fax 0: 614-7904624 Industrial Chemicals & Solvents Division Ship Deb: 12/01)02 Product: Tana To* No.; 169 Slip Quality: 15606 TicksI WAS PO La No.: 450036171443C0 01'74 ~OP Apparatus Swills Garrity, 60F Gravity. pounds/sallow SaybsM Cebu Pt / Co Color (AMA) Acid Wash Color Kanar4laitaino1 Vasa Salter Coispeands (H25, 502) Weir, ppm Acidity Copper stiff' Carrosies Sidsratea, % Den:um % Tobias% % Xylem % Xylem, % loilW Soap; Paint. C Dry Pc4nt, C Dist. Range. C Wain. Contest, ppm viand 491 Cale D-156 13.1209 D-141 19- 1 D-153 D-396114045 D-447 D-1301149 D-2306 D-2306 D-2306 D-23041 11-2306 D-156 D-$50 13-850 AqualoaS 010 to 0.173 report only riPat WY 10 mu. ',Poi gat/ saran only report WY sport only report only Mort 011IY 0.5 max. 0.03 au. 99.5 Ina. 0.5 suss. 0.5 ans. 109.6 alit 111.6 Rua. 1 tom. SOO woo. Clear KIM, irso of particulates 0.1711 7.2611 30 I ON 104 Nei 03 Ng 14 0.04 0.01 99.1$ 0.00 0.06 110.5 110.6 0.1 33 Pass Pass Pass Pass Pass Pus Pass Pm Puss Paso Pus Pus Pus Pus Pus Pass Pats Pus Pm Pm Ass1410 added A PArcoorthle Cant CArnspeny 170 &haat Disiribasion Composy. Division of Ashbed is*, Ron 2219. Cokoribus, Ohio 41216 S hipment do Marathon Ashland Patokunk Ii.C. P0 Hot 1492. C111463kary. Ky 41129. 606.9214602 PS:SI TOOL Z 334 6599V;6909: xe3 AIG AN 8b1 300-dUW SW-Scearce 01255 MAP-CC LAB KY DIV Fax:6063216659 On 4 2002 14:1'3 P.04 0 11' Act DiaSAWS= Company Division or Ashland, Inc. Customer Certificate of Analysis Industrial Chemicals & Solvents Division Ship Date: 12-03-02 Customer. Sliorwli Walton Comma/ Prod= Tolosa, 03.17-10 S 2300 Snip Lam &nib Tank No.: 169 Vessel: GATX-53911 Sicbseed. KY 40475 Ship Ousatitc 24705 Tick*: Fax 0: 614790-6424 !GU PO / Lot No.: Ann' Dab NW aCatil Columbus) Analysis Teat Method Customer PO No.: Specification P110070C10131L,234 Tut Results Appearance Sputilk Gravity, Wail. 060F Gravity, poseek/pllos Saybolt Color Pt !Co Color (AMR) Add Wads Color ICaurillatimill Vats* Soifer Compounds (1125, 502) Sailor, pPik Acidity Copper Strip Corral" Sourstio, % Boastau, % Tolosa*, % Kyles*, % ). Xylsuo,% laWol Delliag Polak C Dr, Pawl. C Dist. Ramo, C Water Coulees, pma visual 0-191 Cak D-154 D-1269 DIAS D4133 D-653 13-3961/4045 D-147 D.130/49 D23114 D-2306 0-23116 D-2306 D3306 D-150 0450 0.151 Aquatint 0.1169 to 0.013 report nab rayon only 10 sea. report only report OW rout only report only report =Pt Men oily 0.5 mos. 0.03 usu. 99.5 Reim 0.5 seas. 03 mom. 1094 adm t11.04 ewe. l racc. 500 issa. Char liquid, free of particulates 0.1710 7.260 30 I ON 104 Noy 0.3 Nog ID 0.04 0.01 99.00 0.06 Me 110.5 1153 Si 33 Pus Pau Pars Pus Paso Pass Pau Pass Pus Pass Pau Pass Pus Ps* Paso Plat Pau Peas Pau Pus Arm-Slat Weed oliggi JABS 4 tesponsolie Co. Coreeney Arlikin Manaus common, Dwane of Added Isk, Bas 3219, Columbus, Ohio 43216 Shippent Mwethee Mime Perzelean LAX, POD= 1492, Clambers, Ky 41129. 6%4214302 SW-Scearce 01256 MAP-0C LAB KY DIV Fax :6069216659 Nil 4 71)02 14:19 P. 02 'diamobt Aghisnd. iquolow AMshialamndiDoirstArisbiuthtieoknICnoom. pany Customer Certificate of Analysis Customer: Iborwis WO's* Cowmen Dian Loss Solidi s Ridesond, KY 40475 Fax M: 614-7414624 Ada: 0th NIA AGM Colusatel Analysis Test Method Appanage Speeltle Gravity, WEIL ow Crispy, peardsiplas Saba Color Pt / Co Color (APHA) Asa Wash Color Ksuri-Doteast Volvo Suitor Cosoppeode (11211.1102) 5strur, ppm Acidity Copper Strip Corneas Satoratak 96 Dusaver, % Tobin* % xylem., *Ai > Xylem, % Wald Min Past C Dry roial. C Det. Rapt C Wear Costae, ppm sliest D401 Cue 0.156 13-1110 D-0414 D-1133 1311113 D3901/4040 D-147 D-130/141 04304 D.2306 04304 0-3306 04304 D450 0-050 1)-1151 Aqsatast ? 16" Industrial Chemicals is Solvents Division Shi Dots 1343-02 Product: Tatum 03-17-10 HMIS Tara No.: 169 Vaal: 20311 Shia Owens; 35401 Ttekor 1Ck5 plaadit No.: 4500513152-C3C0 ,..- Custeur PO No.: 1.412;) li i ti`A)ft /IF15r 50 C ." 5q Z g4.,:212,f. Cf i 5pecificatior 0.0114 ia 0.473 report only report ate 10 nu. report rely report only report pair report only mart war report sat/ 0.5 ism 0.03 apt. 90.5 Naha. 0.6 Nem 0.5 sin. 1001.11 axis. 111.11 am. 1 rase SOO taw Test Dash' Clan liquid, tree or ardeolatos 04711 7.260 30 1 ON 104 Nog 0.3 Pia IS 0.04 0.01 94.40 040 0.04 110.5 110.6 0.1 33 Pass Pass Pus Pus Pass Pass Pen Pass Pus Pass Pus Pus Pau Pass Pam Pall Pus Pass Pau Paso topasals Coo Cosupor AniadDisigrbedas Caput Divines ofAshlead lac Doi 2214, Conanue, phis 422I6 Shivers cip Mershon Ae1d W haaleaell..1.C, PO Doi 1492, Celli al% ity 41129, 6044114= SW-Scearce 01257 )C15--QC LAB KY DIV Fax Ashland giumow V=ilsi c11 are" Customer Certificate of Analysis Dec 6 2002 12:51 P.06 op giIndustrial Chemicals St Solvents Division L-- Fax 9; Riebsoad. ICY 44475 .014-7/44424 Analysis Teat MAW Appesrattes Species Gravity, gfral. oar Gravity, paaa40100816 5aybalt Cater icColor (AMA) Avid Wireto Cater Kauvi4kataist Vase Salter Campanile (11211, 902) %afar, ppm Acidity Copper Strip Canalise Saterstee, % Beesarte, % Tetuan % Xylem% % % laid,' Ilelliag Polak C Dry avers, C Diet. Malta, C Wake.Coslat.pp4 visual D-1191 Cala 11.156 13-120, 1144$ 04133 D453 II-394114140 D1147 0431141 D2394 21-2300 11.2.30* 122304 D.2300 0.450 DASO 13-5411 Mauna Tank 14o.: 179 514.9 GearatilY: 20515 Ticket 1C&11 PO t Lot No.: 45001894591X11 o.. SpacifleatIon 0.44. ea 4.073 report ally report Daly le rim revert only rapers only rapport may raper. oily mart only report 'sly 0.5 mat. 0.03 sax. 99.3 wiz. as mai. 0.5 wow 10114 sea. 111.11 ram I main. SOO sum Teat amulet Clear liquid, free ef particulates Plum urns Pala 7.240 Pao 39 Pan 2 Pao ON Pus 194 Pala Nei Pam 0.3 Pale Pim Pan 111 Pen 0.05 Piss 0,03 Pen 99.91 Poe OM Pus 0.09 Peas 111.4 Poe 119.11 9.41 Para Pus 45 Pate Angel added ILIAJufftlife)17 A issooribis Cos Comply Arbleol Dielrelsokre Company, Diriiica or Asthma Ira, Bon 2219, Ccirambes, OW 43216 Shipaula ob tbiredern 44161,01141relstri LLC. PO Si' 1492, Caikarbars, *y 41129. 6064214102 mem SW-Scearce 01258 . MAP-OC LAB KY DIV ribs. Ashland Fax:5069216659 DC 12 2002 3:so P.02 tetkrie Diatribe*, Comeau Direr, CC Ultlaid, Customer Certificate of Analysis Cunomer: 1 t *ifk: SUMO' W91Siae4 Co0100117 Bemis Lee Sautb l*Ipese, KY 44475 GUI/44624 Industrial Chemicals & Solvents Division Strip Dm* t240-03 ProduFk Waage 03-17-10 Haas 2300 Tapir Nei 171 Vessel: AC521-79319 Ship gusalpy: ISM Ticket ICU p0 Lot No.: _45005400111-000 Analysis Test Madre Appanage Spells Gray*, We 5160111 Crarity, pautdaigalku Wet Color Fl! Co Color (APHA) Add W. Caber 1Care-Ialassi Vale Sulfror Cesperesda (H31, 503) Sulfur, pus Melt, Copper Strip Corneae Saturate, % Beaseu Sf. Toles, V. Xylem, % w Vole, % WOW Odle. Pee C Dry Peek C Die Ileum C Water Came pm "bed D491 Cale D-154 0.12119 D440 D1133 D453 04141/4044 D447 0431114, D-3311 D-334 132300 04350 043011 D-1154 n..ser 0.010 Mowed Sesithatke 0.140 le Lin report** newt oily 10 ma. raper, alp ripen ale report NO report Gab remit oely mod olliy 0-4 en. 0.03 mss. 39.5 We. 04 me. 0.5 um 149.3 Wm. 111.4 mu. 1 rims 300 ales. Tut Remelts Om 140111,11w ef particulates Pais Wit Pm 7160 30 3 Pose Pau Pete Os Per 104 Pus Nag Pus 0.3 Pm Nee Pm 11 Pala 0.03 PM 0.03 Pus 9014 Pus Oil Put 0.00 Pau 110.2 Put 111.1 0.11 22 Pau Pile Pass 5.102C? g(-f ''.-1/431.2 011 miti-31.1 Wei JAN 2 9 TfP APPROVED lit51 ancembIsCareCampory Ashlma Dketems Creeper'', Divisies of Ashland 1.i, Bow 2319. Coin** Ohm 43216 Sbipme aio Miretece Jueim Pongees LW, PO Bee 1492. Cadmeers, Ly 41129,6064214403 SW-Scearce 01259 MAP--QC LA9 KY DIV Fax :6(69216659 c_.Dec 26 2002 13:21 P.04 Arra. Ashland Ashland Distribution Cu/W=7 Diva!lea at Ashland, Inc. Customer Certificate of Analysis 111G'OP 3 rsAP rt.& Industrial Chemicals & Solvents Division Ship Date 12-26-42 cIaI'lP0c OA' Customer: Mord' Willi.ats Cesium Sew J. Saudi Product: Telma* link No.: 170 03.1710 2300 Vessel: ACX-79304 Fax M Riclunsisd. ICY 40475 15j4.790-6624 Ship Quantity 26024 [CAS PO I Lot No.: Ticket: -0" A Analysis Test Method Customer PO No.: Specification lailtiadts Appearance Spaces Grayky, Wes14260IP Gravity, panalessilea !Waal Coier Pt / G COW (APHA) Acid Wails Color liCaatri.Batasei Vide SuWar Compounds (MX 307) UMW; ppas Acidity Copper Strip Caws*, 31durslie, % Bouses, % % Bylaw" % % UMW Boiling Point, C Dry row, C Diet. Rana. C Water Combat. pp= ylaaal 0.391 Cale 0456 0-1209 D./140 D.1133 0453 D-3961/4045 0447 0-1301449 0-2306 D-2386 0-2306 0-2306 0-2306 0.440 040 D450 Aquiline 0.869 to 0.573 Mow*** raPort only 10 mu. Mow* 'sly rarigt eni! report say report only report only report only 0.3 ram 0.03 as's. 99.3 ao. %rum. 0.5 was. 109.6 leis. 111.4 max. 1 =as. 500 sum Char tkpild, free 01 perdu:labs 01711 7.260 30 1 ONt 106 Neu 0.6 Nag 10 0.02 0.01 Not detected 0.01 110.3 a 04 0.1 24 Pus Pau Piss Pus Put Pus Par Pau Pus Pus Pees Pee Pus Peas P ass Pus Pus Pass Pus Feu Asa-Sir 41401 APPROVED A Rw94444914C119* erawriair Aehland DbMbOice Company, Woke of Ashland los., Box 2219, Column a. Oleo 43216 pon Morally* A *lam Parninom PO Roo 1492 f7r1149dwno iC1 77q r414.07+,..cool ISOM= SW-Scearce 01260 IL AlJkAri tAdr Ashland. faiwor 0:ittrAi ltickirm Customer Certificate of Analysis "I ziPfr' Ind Chemical, Sc Solvents Division Gust 1241-11 Outliner: On& Willem Capron, Produce Wiese Digo Um Base Usk Yia.: Wasik Pei 6144,14124 Ship WEST MSS new icris PO Mot 45M011 PO Analysis Teat Method Speollicsice Tog Reinke Appearing. Spline Cooley, shal. env ring 1.11111 Groggy, posiderpags Cale Sa buit COMP Wild Pt / Ca Cider (A RA) D42011 Ade Womb alai 1)4411 ICsuri.lessal Vain* 14131 Soffit CsinpanedO 802) D4 MINA ppm 140611/40411 Acidity DSO Copper Ship Camden D.1311440 &stints% % 043Se % 13.23114 Wiese, *AI DOM Wvitss%lowgolb% D-nos 1431111 Inithd Ulm Pelt, C DDS D. POO. C D411 Dist Nang% C 0450 Wider COMMIEtt ppes Aquila* 0.119 Si 021 ntitri mat matt eaty 10 gion. report oily Men WY report sob repast illy mad sal, syWirt ruff LS man. SAS mss. PM ad& 0.11 mg: LS saw 101i ids. Miura. 1 Des. SOS sass Clear Squid, is et policaleles Pass MIS Pass 1_20 Pass 310 Pair .1 Pus Olt Pals 114 Pats Nei Pass Rd Pair Mai Pus 11 Pus 0.S6 Pug OM Pea 99.11 OAS Pus Pas 0.0d Page 111.0 Pass 1 MS Pow 0.1 Pus 29 Piss FEe, 1 41`4"0/-1 Afek,e, Rerpegalie Ora Crag MUM Obribidift Ccepay, Walser Mind 75 Us 2219, Csimift OY. 432111 Wpm. eilo Manage Ambient Petroleum 11.C, PO Dot 1402, CimieN4tisra,k7 41120, $06.00141102 SW-Scearce 01261 11FP-GC LAO KY DIV Fax:6069216659 Jan 9 2003 11:12 P.06 PtIM MIAMI= Queerly Ciit et Juldind.1116 Customer Certificate of Analysis Industrial Chemicals & Solvents Division Ship Dee 01-0443 Customer Shortie Sinew Commies Product Teem 03-17.10 HMIS 2300 1. Lase Seeds Rickets& KY 40471 Ti'* NCL: 14, She OutitItz Lill Vogel: GATX-17040 Tide Fax 43 61.679114634 1C111 70 I Lot No.: 43011501241-011 rINsMINPMENIMINIMMIEW111111321=1111111111.......m11s,1==Mmil. Analysis Tut Method Specificatice Toot Races Appssesete Speeds Gravity, Wes1. 011601, Gnu*, pessdsigailso Ssybelt Csisr Pt / Cs We (APRA) Add Wish Color Kmarlastossi Wise Suitor CAmpsoods (833,1102) Soffit, ppm Addle Coppe Strip Corrodeo Saterstos. % lissossay % Toles& % Kyle& % Ryles, % IRON Mai Perk C Dry Peet, C DM. Reis. C Water Csalsok ppr visual D4111 Cake D-136 0.1200 0.040 D1133 0453 0-31411/4040 13447 0-U0111, 13-230* D-2306 0-2306 0.2390 D-2304 0400 DSSO 0400 Meese 0.069 to 0173 report see report oily 10 .as resort *se Mot NAY report only report *se Mai/ amir Mot 081Y 04 sum 0.03.1:. 90.3 ads. 0.3 nu. IS ms& 109.1 oda n1.6 ease. 1 sae.. 3110 es& ,, Our lied& Ms sii porticokes 0.1711 7.260 30 1 ON NI Nig 0.4 kr Nig 11 0.00 0.02 97,93 0.00 0.00 1113 110.4 0.3 112 Pus Pus Pus Pus Pus Pus Pus Pus Poe Pus Pus Pus Pus Pus Pus Pa Pus PPM Pon Pus Sf92. g she c 1 le Ant43191 milled Wkkk 411-0 APPIOVED A Itespeosili Astitail DisIrkupas Came Divlsios of Mewl Da, llas 2219. Columbus Ohio 43216 Shimmed sh Mindisi Added PossisestiC, 1'0 Ban tut Cstiesborg. sy 41129. 64:144:1-6102 SW-Scearce 01307 1111112ft land - A. ,tribution Company Di+ ; Ashland, Inc. Cu st0 i ler Certificate of Analysis s-qi 7 9 3 fiu.) 04 Industrial Chemicals & Solvents Division Ship Date: 2-24-03 4/* f u #14 Cum . Sherwin Williams Company Bogus 1.n ne South Product Toluene Tank No.: 169 03-17-10 Vessel: IS 2300 504; In.lionond, KY 40475 Ship Quantity: 6686 Ticket 26595 Fax 614-790-6624 IC&S PO / Lot No.: 4500620897-c3co Ann' Deb Niat (TC&S Columbus) Customer PO No.: pb0970e2rra Ai' t S Test Method Specification Test Results A o. cc SI u/mL @NI loune"gittlon 'olor (APHA) Ar " h Color I; iiinol Value Si: . iipounds (H2S, 502) SI' in A k C Corrotion Sot . % BP" 10 11 I 1), D' . ilg Point. C C 'P. C .1 t. Nun, visual D-891 Cale D-156 D-1209 D-848 D-1133 1)-853 D-396114045 1)-847 D-1301849 D-2306 13-2306 D-2306 D-2306 D-2306 D-850 D-850 13-850 Aquatest 0.869 to 0.873 report only report only 10 max. report only report only report only report only report only report only 0.5 max. 0.03 max. 99.5 min. 0.5 max. 0.5 max. 109.6 min. 111.6 max. 1 mix. 500 mut. Clear liquid, free of partkulates 0.8718 7.260 30 1 ON 104 Nes 0.5 Nes 111 0.04 Not detected 99.86 0.10 0.00 110.2 110.6 0.4 84 Pus Pass Pus Pass Pass Pass Pass Pus Pass Pass Pass Pus Pass Pass Pass Pass Pau Pass Pass Pass An ' :tl ant APPROVED 1S09002 A Raw ire Company Ashland Distribution Company, Division of Ashland Inc., Box 2219, Columbus, Ohio 43216 Shipneni cro Marathon Ashland Petroleum MC, PO llox 1492, Cadetlsburg, Ky 41129, 606-921-6502 h1.31234 SW-Scearce 01306 Amigo. Ashland Ashland Distribution Company Division of Ashland, Inc. Customer Certificate of Analysis Industrial Chemicals & Solvents Division Ship Date: 2-25-03 Customer: Sherwin Williams Company Product: Toluene 03-17-10 HMIS 2300 Bow Lane South Tank No.: 169 Vessel: Richmond, KY 40475 Ship Quantity: 6800 Ticket: 26626 Fax #: 614-790-6624 1C&S PO / Lot No.: 45006222511-C303 Attn: Deb Nist (IC&S Columbus) Analysis Test Method Customer PO No.: Specification P110970C2-271 V."Test Results Appearance Specific Gravity, g/mL @601 Gravity, pouads/gallon Saybolt Color Pt / Co Color (APHA) Acid Wash Color Kauri-Butanol Value Suitor Compounds (1125, 502) Sulfur, ppm Acidity Copper Strip Corrosion Saturates, % Benzene, Toluene, % Xylene, % > Xylene, % Initial Boiling Point, C Dry Point, C Dist. Range, C Water Content, ppm visual D-891 Cale D-156 D-1209 0-848 0-1133 0-853 0-3961/4045 0-847 D-130/849 11-2306 D-2306 D-2306 D-2306 0-2306 D-850 0-850 0-850 Aq mama 0.869 to 0.873 report only report only 10 max. report only report only report only report only report only report only 0.5 max. 0.03 max. 99.5 min. 0.5 max. 0.5 max. 109.6 min. 111.6 max. I max. 500 max. Clear liquid, free of particulates 0.8718 7.260 30 1 ON 104 Nei 0.5 Neg 18 0,04 Not detected 99.86 0.10 0.00 110.2 1104 0.4 84 Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Anti-Stu added ANTI-STAT ADDED A Responsible Care Company Ashland Distribution Company, Division of Ashland Inc., Box 2219, Columbus, Ohio 43216 Shipment c/o Marathon Ashland Petroleum 1.1C, PO Bon 1492, Catlettsburg, Ky 41129, 606-921-6802 SW-Scearce 01305 NAP-0C LAB KY DIV Fax Mar 6 2003 10:40 P.02 Mend . ==zgrwir Customer Certificate of Analysis Industrial Chemicals & Solvents Division Ship Der 02-27.03 Cussosavn SbmwhiWtIllans Campos, Product Woos _........__s_t S-1W-1 BOLan_ OotiLineo bath Talc No,: 169 Vaud: Ellig40--03 111464pall ILY 40475 Shia Ounglian 24510 Ticket Fmk* Attg 414-70114634 Mat 69 / lot ND4 4soisososi6c3cs songmN.e..tmensurag Analysis Tad hdeihed Specification Tut Remake Appowases Sped* faraday, VaL Greet% posedolpllse Saybolt Csisr Pt/ Cs Color (AP11A) Add %A Cods, KauraAletard Vats. Soltsr Onspossis ons, 902) Salter, PM AtiAtt/ Copper Strip Corrosion Betaintoo,% leemsp, % Telseue, % X714.4% XYlus. IWW Bei Feint, C Dm Pales. C DINA.11.6ge, C Wow Conte" ppm rheel D-061 Colo D-156 D-1205 D440 13-1133 D-353 D-3911/406$ D-1147 19.130/.. 12-3306 D-2306 D-3200 D-2364 D-23116 13436 D1116 is-356 Aerialist Ole to 0.673 re MO may MPH* 0 itlY 10 maw report oar, re report may mmtely report Nay nport *alp 9.9 woo. 0.03 soot. 994 one. 0.5 nu. 0.5 mu. 100.6 in& 111.6 ens. 1 msg. soirees Char liquid, tree of perdu:nista Pass 04710 Pass 7460 Pus Pus 1 Pus ON 104 Pon Neg IRO 05 Pose Nei Pus 12 Pus ir 10 0.04 Pus 7 Not dotocted MIS 0.06 11.00 110.4 110.6 0.2 16 Pass Pus PPounss Mil rlti)1 Pub ks1 Pms Per Pass Aari-Sessaist APPIIOVID Ragariblis Caw Company Ashland Disuributko Cowes. Divilsa dAalhad lea, Dot 2219. Coalmin. Me 0216 Mime fife Mambas ArliimmiPsteolem 14.C, PO Bat let Csikesbaes 41112t 600921-GM 0 SW-Scearce 01304 MAP-0C LAB KY DIV Fax:6059216E69 Mar 4 2003 11:39 P.02 dasom. larkland miumpr Ashland DIstrilsolias Comport Midas al MINA Customer Certificate of Analysis Cam'` arTIO Welodt Conroy, Rom Lose Soutb Ridumml. IC! 40413 Industrial Chemicals & Solvents Division Skip Dow 03-02-0 Product Token_ 0347.1013 2300 Tink i1q.: 1H Wasik GAIX-43794. Ship 9toodtr; 35134 71ckst: WAS PO / Lot No.: 43004054634300 . Analysis Ted Method Curtomar N Spocillootice Tod Results Amoroso, Spells Omit?, Oa SW Grady, posodiftolloo &wink Color / Co Cider (APDA) Add /Pub Color ICoort-Dolsool Was %War Cis (1123, 302) %M r. ppm Ada!), Copp Strip Corrodes Sotorooss, % Nome. % Tobias', % xyiki" % Mika* % Mad Maim PO* C Der Polak C DIM asyry C Wooer Cooloot, pp, visaed D-01 Cole 11-156 D130 0441 D-1133 D-03 0401/41148 D447 0-1311640 1153011 04304 Dns D4344 D.2304 D-I50 MHO 0450 Aquatint 0.50 to 0.113 repast day mat only IS eleni. :sport only raped Oily moll only r.SOrt oily Mort 4411 Mort 000 OS now 0.03 sal. 99.4 Isla 0.5 ona. IS soa. 1004 soli. 1114 ism 1 insa. aoar tiquid, fres of porde:04d 03710 7.24e 34 1 Os IN MI 0.0 Km 18 0.03 Not slolosioi 90.93 0.45 0.00 110.2 110.4 0.4 311 Pao Pan Pus Pus Paso Paw Pin Pau Pass Pass Pan Pan Paso Pan Pus Pus Pus Paw Pao Pre 4) 41-) 05" 1) '' i' 4.,10i ' )4,1 kIV .1,,, t 1 Wit 1 7 212 1.111 IDs 8-3 iLt): JO / Nit iola.&. APPItOWD 1444p4saii Cara Salami Dirriadea Company, Division of Mini Ina, ion 2219. Cimino, ale 4721 6 snifssi is tiffanies Aisne PeinivaiLLA PO Are 11192, Ky 411" 4106-9214401 SW-Scearce 01303 MAP-QC LAB KY DIV Fax:6069216659 Mar S 2003 13:46 P.02 Immbw AEIbag qmosPv =iillfi tgZEstimrdiar Customer Certificate of Analysis common Pee 10: amp' Immo ainiel Dom Low loads IRIchrest. KY 400 214.7314111141 Industrial Chemicals & Solvents Division Deist 034443 Product plow 0347-10 'swam' Took No.: 170 5bio Ousatitn 35135 Vesesit 1711.11411, . IC..3 PO t tat No.: 4100411 't A Analysis P ' That Modted Spocifistedos Test Roseits Amoroso Specific Growl% shol. sear Groggy, pooadatplio. Saybolt Color Pt / Co Calor (AURA) Acid Wu Color kourtriabool Vole* ilditirCedip000de (BM ) Sollort ppm Middy Col", Strip Corrode, 8slsn.sa.96 llsousos, S Toledo* S Xylem % XOta 911 latdol Mies Petit, C Dry Isla% C DWI. Mom C %tor Coutes% ppo ritual D491 Cols D-1114 0120, D4411 11.1133 PAO 11-3941/4040 01147 01304149 15.23011 12.33116 D3110 D4302 D-3300 D4511 13430 0.440 mortise 0.110 to LIM report poly report only 10 ma. report oily report ost report 0517 report sap r*Poit es), report Gulp 04 sal. 0.03 m MI EY. 0.5 raw 0.5 ow. 1091.4 War 1114 ass, 1 MI. SOO saw Char Noold, free of pordsoloses 11.07111 7.240 34 1 ON 104 Nes 0.3 Nes 13 0.04 Not delipeoid IOU 0.02 112. 1 10.4 INA OA 43 Pao Pia c c8cPus Paso Pus Puts C Pao Pen ? .-2 t e v j Pea 3 Poe Pia Pao Psee Piss Pose Poo Pen Pew Paw Pose Asaftisdie 410 0'173 ,vee6,7-- A itsvirsible Cant Clem AWNS Diirlhollem Camper, Mimi= iArll.a bs, 9sie 2214, Cohrlar. Olkle 43314 arm* nto HWY= Aiding Paltry= L&C. PO Ow 14,2. Codeabburg, Xy 41179. 404-91141103 SW-Scearce 01302 :4FP-CC LAB KY DIV Fax:6068219391 Mar 17 2003 14:27 P.02 ArMind sNemor gilt=fer. Customer Certificate of Analysis Cu.m= 0hsrnlo VAIN* Coosoom 114401my Smelt illokalgoi ICY 40475 Poo 514404134 Industrial Chemicals & Solvents Division 3151, Dow 03-144) IProdvot 'Nom* 0347-10 10415 moo Took 140.3 10 1/410111 VILIC-301171 Shia Omoodivs 257121 Mot 1045 PO / Let /44.1 PPOPIOC14711 Analysis Too 14whod Appommees Nowak Gravity, shol. 4/00, Gravity. pootodoloolos Soyboll Color Pt/ Co Oiler (APIA) Add Wail *kw KoorFilotaiol Woo 5a1tir Cimaysosdo $02) 5.111101 PIN* Miditt Cowl, Strip Commies Moraine % Dawao Tolson% 16 Wu" % rikel 110 laidal bass Pols4 C Dry Poiorp C mit Resift C 70/01,0044046 POm Afoot DIM coat D154 11-12011 0-0410 D-I133 D-1153 D-3911/4845 D447 Ds130110 11-23011 D-330 D-1344 D.23011 D4305 000 DIN D401 Moot* warm more =sr mart only 10 was moot only Merl 4017 Mott 0013` more 0417 mot 0* marl cooly OA mom WO rm. 90.11 odo. 11.1 toss 100A era. 1114 mai. leas sos too Rauh' Claw 04144. Dos of oodloololos 11711 7.21* 30 Os 104 74% Ott Nes 11 LEO Ni. ioloolo4 Poo Poor Poo Pus Paw arr Pa m 4C`rrP Poo roe 9 Poo c.4.41 Pa. m oti 0.03 MOO 1103 1110 0.3 54 pm, pia Pees MAI-Mo salsa 1 Itaigaii1ds Cm Caspar AilludDlOrhalca Comm, Dlyblis of Mimi kg, ler.Z1), Calm* OW *MG 311pri cis 110eilia1Askirsi boils 1.14 PO Ike 1402. eo441311. 4 41124 10114314111 ts SW-Scearce 01301 MAP--QC LAB KY DIV Fax:6069216659 Mar 19 2003 9:5? P.02 Aukiand. s111111111111PP Milked Oho*id= Compote Divides of MAW. 1no. Customer Certificate of Analysis Industrial Chemical's & Solvents Division Ship Dian 03-11143 Cusiowoor. Simproll Vali= Cot000xr___ 10111 Lam sell ?Indio* 'Taboos Took No.: 1011 034740 pesmq Womb AC1747131M Muss& KY 4047$ Sidle Waits: 21091 rob* fix ill 614-7904420 1C.13 PO / Lot 141o.: 19111974C3-171 Analysis I. t _ : Tat Method Spuifitodoo Two Ramie emmoreloo Sposiflo Gravity, VAL VW Grimier, poundaIplow Saybell CoUr Ft co Color (AMA) M1 Ws& Color ICaar1-111alawil Who Soifer Commends (HA 303) Sulfur, pro Acidity Comm $t* Camino Satanism, % Buse*. r Tob0000, % Xyloot. % 41 % Moto C Dry Nato C Ski Anse C Water coeteet, ppm visual D491 Cale D-1 M D-1209 1-14$ D1133 D4153 WM4141 D-147 D4311/1149 12.2304 0.2304 14301 D-2306 D-23011 D4511. D-150 1-1411 Minoan( 4.10 to 0.473 roPort *WY report only 10 moz. mut poly Mort 014 mime war report otly rind mil reput only 04 manc.. 063 mu WS eau. 0.5 mss. 11.5 awl. 101.11 elm 111.4 was. 1 11011S. SOO Slam Cher Ileobl, Du el wash*, 11.11711 7.240 311 1 0r4 104 Ms 0.1 Ns 11 012 0.01 9990 IA 0.40 111.2 1104 0.4 12$ Plos Pau Pus Pus Pus Poo Pus Pus Pus Poo Poo Pug Pau Pao Pus Pao Pus Pau Pots Aidari Nita I0 rti ,= 44Ar6-4 41--- ltaroodob Cm, Campo, Aohliod DIsuBscito Caveat DIAUce OM/4.41u, Ben 2319, Cobs**. Me 43214 swops Imusilm Mob= LW, PO Boa 1492, Cadeobtoo. Kr 41129, 61164214102 P111111141 D3 IO SW-Scearce 01300 IfP-OC LAB KY Did Fax :6069215659 Max 19 2003 9157 P.02 ".% q411111011P Aabhad Umatilla' Company Milks a Akio& IDA Customer Certificate of Analysis Industrial Chemicals & Solvents Division RIthimmILKY 40475 Poo 4: 614-7304624 Analysis , Tom Mcthod Ammon Spoollia Groin%y, grid. 0018 Gravity, poomi/plloo oars* Color Pt11 Co Color (AMA) Add Womb Color 141.041.0mol Woo 541117 Comma& 41111, NM Sotto, ppm Adttly Cooper SD* Commis* Saiondoo, Dieren. ToOmoo. Xylows, s ILO." % Mild MON Pets, C Dry 11.194 C Met. Isms C Wow Coolaolt ppm Asset D-801 Colo 0.130 D.1208 D44$ 011.33 DAD 1341161/4640 0.141 0-130410 04306 02306 04306 04306 134300 0450 Din 0-860 Aquae. TO No.: le Vtus Af7141304 Slav Coaadm 219913 liakat 1C1101 P0! Lark,, PB0s7IC24711 ipoolficalle* 0.069 to 0.473 report 141 report say 10 ma. report sety Mori mill Men WI Import oar report oily Flg0r1 8117 0.5 aim 043 mom 99.5 ode. 0.5 ass. 0.5 max. 1011.6 oda. 111.6 asas. I ma. 500 mu. Tom Smolt Clam Ile" era at particulate 0.$710 7.2611 00 1 ON 104 Nei RI Nes 111 0.02 001 046 0.03 040 1111.2 110.1 11.4 121 s=11sss Pam Pus Ps* Pisa Pus Pus Pow Pia Pon Pam Pam Pao Pus Pon Pa* Pow Pus Plus Pia Aati4ies sided 11 / 1 41ae;1`44-- T4 ItsommitisCmo Camay Ashirmi Dhastrorima Compaq, Mese sf Addes1 Mc, Dew 2310. Colonise Oils 43210 Skips* ole Mentlso Melo/ Perohnli LLC. PO pox IVA Cadeembes, lip 41129 6044114ES UMW ,, SW-Scearce 01299 MAMC LAB KY DIV Fax:60632I6659 Apr 2 2003 13:22 P.06 glIMPIPP gtgr=n.r.17 Customer Certificate of Analysis Cu:scour amnia WILlhasse Cornrow BOOSLorO IN 1114.04. KY 40475 Fos Os 1144304424 Analysis Tani Meshed Appreinsises Speslis Qrselly, WaL SOW Creel% peimilliallso SONO Calor Pt / Co Calor (APRA) ARM Wok Cake Kna141.04041 Wei Whir OWES& OM 304 Slifar, mom Addy C011993019 Corrodes Sebirekto % 141011s114 14 Tolosa% % Vow. % s. Xylem, 14 Mid 11411181Poisk C My Pelle, C 131r1 Ibings,C WNW 1;40491, ppm Ana D4i91 Cele 0-1.13 DMA! 0445 0-1133 0493 0.341111/4045 D04? D.130100 0-1394 1333011 043011 03304 04300 DOSS DOSS 0405 Agiatei0 Industrial Chemicals at Solvents Division Ship Nies 040343 Product Tolima 03.17-1014W) 2300 TOOL 1404 115 WU& UTLII-300111 Ousatim 335413 - Time ICA3 PO Lel No.; 4340143534C301 C0 I.4;____211M14===g;=::=1=== 030 to 0.173 Mort only report ugly le airs evert only Mod 0017 report sedy revere wally Mori war matt suly 4.9 mar. 11.63 nos KS nun. 04 ons.. 04 mu. 103.4 Ws. 1114 1114111. 1 re. 333 way. Test Raisins Moe Hirai, Dee of pertlestitoss 0.1710 7.20 30 3 ON 10i Nei 0.7 Nkfl 1i 0.02 Net deirstei 3940 0.03 OM 110.3 104 0.3 133 Pao Pau Pus Pus Pass Pus Pus Para Pus Pets Pun POI Psis Pus Pen Pus Pare ham PUB Puss Azal.ritra sided gam_/ 0 '7' 1 904i. Psyymibi Caw Qum, Mims Dissibeske Csnapnly. Division efAsidere Ise.. Bon 32I9. Goblet al. 412111 31ipme do Maim A414.4 Privelem 1-1-4 P01300 1492, C41304440, Ky 41129, 609-931-900 SW-Scearce 01298 11P-OC LAB KY DIV Fax :6069'216659 Rpr 3 2003 15:50 P.02 011111111MIPP =r=cammy Customer Certificate of Analysis Galan Pox 01 COmIlkor Omas Latie 8p* IllelmeakKY 49170 _614.7941174 Industrial Chemicals & Solvents Division Dom 144143 Prodtatt Wass 03-174 031411 2300 Tank.: 170 Vass* 9$4.171-91/11 Ship Ossititin 14141 'rid= 1C1010 /1-01144 45048t4r&gal Analysis Ts Unshod Ammonium Sped& amity, OIL GOP Gravity, pooadatpibit 30641 Color Pt / Co Cher (APRA) Add Wadi Color Kaartploaessid Vida. %Swift Compemoda pt 301) *UNA pp. Addlly Capper Ship Cerro*" Satanism, % Ileamow, S Totsens, 44 X76.04 s Xylem, x 151da1 WM. Mat, C Dui Petal. C Pa/s. C Water Comm% ppm visual D41111 Cato 058 04200 D440 04133 04OP 0,38011/400 D407 D430i0 o4104 11301 043* 03301 04808 D.050 D-110 0.151 Aqua spitukuou Uff MIS/3 MINI oal? report nip le im . !VW MY Moe odr report only rum tidy report aaly ropers Gab OJ mom 013 um 00J rimll GA Isia ass ulm 11L4 mos. 1 OM 500 raL Ted Ragas Our lipid, Prod of putoilotso 11711 73* 8 1 ON 101 Nag 0.7 Neu 111 1.07 Net &OWN 90.95 0.03 41.011 110.3 1111.11 03 233 Pao Pass Pus Pus Pus Pam Pim Pa m Pim Pass Poser Pam Paso PPailtao 4,64in Wei itsomplis Cue aids* Dismirdlai Ompoy, Dining orAdamt Ns, Pm 2210, Crim MU 43214 Shirdeml ale Maim MIMI Mohan' U.C. r0 Bag Ha. CeilaiWi Klr 11129. 4/4421-4102 tY) tt SW-Scearce 01297 ==glitarriPm7 Customer Certificate of Analysis Morrow Studds WIDIano Comeau paw Lies State Rldistemd. KY 40475 Fax it 414-790.6624 Analysis Tod Meted Appienuate SP14.0 Grey*. Iredo 060Y rowdy, passeldgeges %yes% Color Pt Ca Celor (OHO Add WWI Color irossrlastaisid Vides Misr Cseseusida nus,son PP61 Asisley Copper Ibip CAriesles Siderdes, % lasmisee. % Taleses, Xylem, % % Wild Bean P91 , C Dry Paid, C Det. Ramp, C WOW Consul ppm vestal 0491 Cala 0-151 D-1209 D440 D- 1133 0-053 D-3961/4045 0-147 D-13040 023110 0-2306 0-2346 11-3306 0-2.300 0-0511 0450 04410 Alvaseess Industrial Chemicals & Solvents Division Daft' 114137/03 Product Tokens 03-17-10 64:13 23014 Tack No.. 179 Vont GAIX.37064 Ship Ousaatr 13453 ?idiot 1C11..3 PO /14 No. 450605Stqa 4;, 1,1110f Spoodursort 0.069 to 0.673 report ratty rood aely 10 mu. report way import tidy rapid s111 report oily mart ady "Port mil 03 uss. 0.03 dm 993 ugh 03 mu. 0.3 des. 109.6 We 111.4 ass. 1 Nu. SOO rani. TestRviults Clear Ovid. Ow sf pordudattes 0,0710 7.260 30 1 ON 106 Nag 0.1 16 0.07 Okl 99.90 0.02 0.00 110.3 11.04 11.3 233 Pass Pus Pass Pass Pau Pau Ppe Pus Pus Peso Pus Pass Pees Pus Pus Pas Pass Pus Piss Pan Aa641444 adds. A 214,604011 Can Company ZO'd Deribiiiiai Camp o% Uhlman or &tiled lia., 8.0 n19, warm*. Ohio 43216 Shipritai CIO MIIMPICO Asliliod MAIN= LLC. PO lox len. Colman. ty 41129 014-921-4s02 80:L1 WM SZ atb 6S99105909: )(el Ala AA SD )111-41:11 SW-Scearce 01296 MAP-0C LAB KY DIV erIs4=1M rm. Amami. wimmr. Fax:6069216659 Apr 341 2003 13 : 24 P.02 Industrial Chemicals & Solvents Division Customer Certificate of Analysis Ship Dag 04-2343 Cuss sr Sourrio NMa1 Comes, Product Tolima. 034 7-J0 11341112300 Bous Loop Oft* Tort No.: le) Vouch ACF76-70114 2140014. KY 40475 Shit ONIONY: 35326 TECIUM Pm Oh 411TM-4624 10105 ro / Lae No.: 45110557355.C301 Analysis Toot Method PO N Specifludou Tat Rude Animus= Spoils Gran% !.I. gar trinity, pousdarpliso SODA Color Pt / Co *du (AMA) Ana Stub Color Kuri-Rnion Vido Senor Ompuon (RIM 302) SWOT, pus Ann* Cow Strip Cunene SidirsOn. % Bmw. % Tcheoc, % X7111414. % % WIWI Beg* Pent, C Dry !Out, C Din Rasp. C Wan Camel. ppm Aron Con D-156 D-12011 D441 D-1133 1)411 D-3011/41145 D447 D-130/040 D-2306 D1304 D4306 11.33116 D-2306 D-1150 0.0114 Is WS report only Mori wir e row 001, report only report sly retort 047 mat poly er 0.5 um 0.03 nos. 30.6 0.5 mu. 11.5 mu. 1011.6 sin 111.6 ons. I mu. 300 mos. Clew insid. Its ot ponicantes Pau 0.0711 Piss 7.240 Pin 30 Pow 1 Poo S. Pus 104 Pus thof Pam 0.1 Pus Nag P.M 11 P.M MI5 Pus 0.00 Put P0.513 Pus 0.01 Pan 0.00 Parr. 110.4 Pon 1166 Pan 0.1 Pie 150 Paso 447? 8 f. Andiandoil I6F14 A Rammoiblo Core Cum" MOW Dioramas Coops Diriota efAolioadlos, Dort 1219, CLAW,* QOM 41210 Slipsom Maradsza Aohlast Tadao LLC, PO Soo 1441. CaImAtri, Kr 41 119, 8064214 03 iv SW-Scearce 01295 -1A11s111=tk 441111111MIPP Ashland Distribution Company Division of Ashland, Inc. Customer Certificate of Analysis Industrial Chemicals & Solvents Division Ship Date: 05-02-1003 Customer. Sherwin Williams Company Boos Lane Saab Product: Toluene Tank No.: 170 03-17-10 HMIS 2300 Vessel: TOLUENE ItichmentkICY 40475 Fax 6: 614-790-6624 Attn: Deb Nist (1C&3 Columbus) Analysis Tem Method Ship Quantity: 6370 Ticket 28095 IC&S PO / Lot No.: 4500670823-c3eo Customer PO No.: pb0910e2-304 Specification Test Results Appearance Specific Gravity, &IL @60F Gravity, pounds/Inflow Saybolt Color Pt / Co Color (APHA) Acid Wasb Color Kann-Butane' Wu* Sulfur Compounds (112S, 502) Sutra'. ppm Acidity Copper Strip Corrosion Saturates, % Benzene, I Toluene, 1 Xylenei % > Xylene, 1 Initial Boiling Point, C Dry Point, C Dist. Range, C Water Content, ppm visual D-891 Cale 11-156 D-1209 D-848 D-1133 D-853 D-3961/4045 D-847 D-130/849 0-2306 D-2306 D-2306 D-2306 13-2306 D-850 D-850 13-850 Aquatest 0.869 to 0.573 report only report only 10 max. report only report only Mon only report only report only report only 0.S max. 0.03 max. 99.3 min. 0.5 max. 0.5 max. 109.6 min. 111.6 max. 1 max. 500 max. Clear liquid, free of pardealatss Pass 0.8718 Pass 7.260 Pass 30 Pass e1 cCAg Pass ON Pass o)106 c.p Pass .4Nag Pass 0.1 4# Pass Nes 4 4 ' 13 1. ats/ ki 0.06 7-^ Pass Pass Pass Not detected Pass 99,93 Pass 0.02 Pass 0.00 Pass I Pass 110.6 Pass 0.5 t, Pass 94 fil Pass Anti-Etas added ariti-sea added 1509002 A Responsible Cate Company Ashland Distribution Company, Division of Ashland Inc., Box 2219, Columbus, Ohio 43216 Shipment do Marathon Ashland Petroleum LLC, PO Box 1492, Cadansburs, Ky 41129, 606921-6802 F M.311234 SW-Scearce 01294 LHO KT ULV dimerb Malawi 1-ax:bU69215659 i1 5 2003 13:17 P.04 4ii 531k-2- emzgzit_opipm, Industrial Chemicals & Solvents Division Customer Certificate of Analysis Wet 434643 sigt--Thesiatmeatelm ssssAMIL401111LIN.111. Plommi. KY 4506 t A47464624 aisimagialligratlePswo Analysis Ten 14dbod Product Tape *1740 iDe4 2300 Tuuk Nv.l 17, 10 Ship Camay: 25137 V 'Mot Icalt 70/ LW N.j 4111114463111-C313 gosera,.f.tINIZE2za___=====zs Tat Issult ApyrITS111111 Veda Gravity, glyiL 404111 1:314PW4P 061mistids WWI Color Pt / Co Cioisr (AIWA) Add NVash Color Kuldaraimisi Vase Maw Castpuesio 014103) When 11610 . AdiNy Cw11)11$11 Sistreoles01 Wm* % % X34180. % IAN Dan Nat C 114yy Petsr. C ViitarCommet MED Pa. D116 D1300 D1144 3M234 21-110 D39111/4444 D044 DOOMS 112306 D23416 D.2306 DOW D2346 awl Doe D464 Alostsst 0.565 t. 4.173 mart tidy Mal sal? Naga Molt nil' mod NI n_ 816Y Mot Ger ropeel Orly Mod 0104 vos, Lai dm MI Mt. OJ 0.4 du. 104.4 oda 111.4 maw / ism S1111 Ism Clew UgiY. bee d psylieurelue 0.4711 Pap 7245 38 ' Poe 1 Pmis O18N4. Nos Pu Pus Pum Pro Nig losal IS Puss 046 NOS Not deteded Pos "3$ Pim 4.113 Pus OA* Pas 114.1 Pot 114.41 Pasa as Prs 44 4 Pau AmPlut edd4 MAY i 9 AXisposhiCau 0-p.., Allard Moniblds. Comps, Divider ardlerl ler nig. CON** Mb 43316 Wpm. Ofeseks Ardor Mulles LLC.PO IIar 1M. Cribrebers, Ky 41 la 1104.9214101 SW-Scearce 01293 MAP-0C LAB KY DIV Fax:6069216659 May 6 2003 15:31 P.02 =rA1sbhigicisw.q"" Customer Certificate of Analysis Cusiontort Duels Weans Common Bun Love Sara RickisolML KY 0175 Pet 61 414-75t4434 al--. - Analysis Test Modrod Appanage Sprains Gravity. pa. fi101 Crate, poonds/pilleo WIWI cu. Pt / Co Cobs (APRA) Add Wine Calor Konel-Dotinsl Vele. Sulfor Compenne 11f20, 301) Soifer, ppm Adair Copper *rip Corrosion % 13s0sono, "As Token% V. Xylem, 74 &flaw % Initial Monks Pent, C Dry Polak C D1sL Faap, C Wear Causer, pp. Nina D4111 Cols D4 36 141211! 044111 1:14233 D441 1114861/4645 01147 11430/80 D2364 D-231111 11-3306 0.334 D-2364 D460 D4911 14450 Apotuir tmlustrial Chemicals & Solvents Division Ship Data 05-0443 Prance Toneas Tank No.: lop 03-1740 HMS nog Vesuk D711,2C-261060 Shin Ousstint 25213 Ticket: 1043 PO / Lot Na: 4130060117310 C PO l't SpasifIcation Test Ranks 0.M N 1.873 mart oily report sett 10 moo. report only report ugly ropers ply mart oily report ony report only 0,03 um 903 ma. 0.5 reel. 0.5 mss. 100.4 wank 1114 am 1 lugs. 500 aux. Clam' 16"16437t1116. .8 PlirdnInis PPal : 7.264 Pass 30 Par 3 Pau 0P1 Pus 106 Pus Nap Pus cCif 0.4 Pon Nap Pus il'''' 1 s Pus 4.67 Pus 0.3nu 31;i41 0.01 Pau *96 Pau 1/4.) 0.01 Pus 0.00 Pus 110.3 1104 03 Pus 4). Pus Put 117 Pus SW-Scoarce 01292 icP-QC 08 KY DIV drimb. Ashland goomor Mtsisjesloan d =Erre F-ax:6069216659 May 7 2003 10:28 P.02 Industrial Chemicals & Solvents Division 13. C, 1Z?(3--' 6 Customer Certificate of Analysis Ship Nt.: 10-04441 Praiser Tole 07470Z:23."0.0."-n'. Sons Loss 50.01 Tian Ns.: 169 %fetish ITILX110341 Dichasati. KY 40470 2149 Nun* 13732 Tialaq Pax* 614-736440 WAS PO / Lei No.: 451411714.5114:30) ' :d.. P Analysis Tau Mebod Apposes... Amid Opseilis Gm*. Vail. VOW 9.301 Gm*, posailaigalkis Cole Saytel1 Color D154 Pt I Cs Caist (APRA) 1)-1200 MM Wssh Color D4411 1Lauri4latassi Was 04131 Swats Compasais (RI% KM D.53 Naha; ppm WM/4044 Acidity 13447 Capper strip CMossiss 1343040 Seamilso, % 134300 Inacessa, % D-2.304 Telers, % D3011 X310,01% V110 % 141111 WIN) Paha. C 1}1306 D.23114 D4511 Dry Pair* C D4311 MA Row. C 134041 Water Omni. ppm Aerestest N Specification 0.044 se 4.1173 matt only repsot snip 10 um ripen! may report only report svAy npeu nip report oily report *sly 0.3 aim 0.03 maii. 19.5 We. 0.3 sus. 0.3 ass 105.14 IOW 1114 am 1 sits. SOO mss. Test Rued% AIMIIMOMMss.ss1,1sss Our Basid, fru of piptisolstre Pus 0.11711 Pus 7.260 30 Pus Pus 2 Pus ON Pus !04 Psis Nog Pan 04 Psis Nei Pr 111 Pas 0.07 Pus 11.01 Puss 9100 Pus 0.01 Piss 440 Pus 110.3 Pus 1104 0.3 si Pus rose Pus /NNW. 0-4- I. , APPROVED A Anima& Cffie Comm, Ashiri DEISibidai Comport, Dividel dMYisilw, aeo 221( COIMIY1 Oh o 4324 Sidman, Os itmathes Ae104114 Parcaniku.c. PO NON tll1. Calkotbers. Ky 41126, 6014214402 SW-Scearce 01291 LAI KY 111V dirmarb Ashland. 44.11111w D Dtestitiso itupsal Fax ;6069216659 1189 2/ 2W3 14:01 P. 02 k.. Industrial Solvecntss Division Customer Certificate of Analysis Ship Dan 08-1843 I p 03. 7- gotaLsao South Webs/ea& KY 40473 Tank No; 10 Shia Outality: 25178 Yodel: 1.1T1440811241 Mast Pas 614.72404 104 P9 tLat 450116112218.C,C0 Analysis Test Method - le Spetitiestioo -itC5935 Applerallie Sped0s Grath gial 401 Gravity. possildgellue Soybelt Color PI /Co War (APIA) Add Wish Color ICsoellIstowsl Van SuUir Corpossels (1124 502) Whir, ppm Adam, Coppr 8114p Caressio4 auras% % Daum, % Tamest % igliso % Xy1eas, ialtial Yossiog Pcdo, C Dry Polito C Hest. 1oow C Wake Cause% pp. visas' 0-1131 Cale 11-126 D.120 D4141 11.1133 1:6431 D-06114448 0447 0.130180 D-130 12.230 0-1306 0.1326 13-23011 Dan 1:.458 WIN Mount 0.80 to 0.173 moans adir mart only 10 mil. repot poly report *sty repot *MY few" mi "P.M ow? WW1 04te 4.11 maw 043 pax. 911.$ me& IS maa. 45 mm. 10.6 mil. 1113 mu. 1 Iwo& 544 mu. Cigar liquiM rem of partkahis 087111 14141 34 2 ON 10 Neg 04 Neg 12 OM Net dental 0116 Oil 0.04 110.4 110.6 NJ 31 Pus Pus Pam Pam Put Pus Pass Pial Pam has Pus Pam Past Pam Pam Pan Pass Pass Pam Pus Aa4.5os midai 77- 1 APROVED A Ramarabie Cam Cammay CD/Mmi. MIAs d'Agliadko. Roux 221., Calmaras. obi. 43314 Shiplamt do Mambo Aildial PQ Boo 1492, Calmaws, ky 41129. 606421.61102 lC SW-Scearce 01290 ammalip Ashland rietZei=ErclY Customer Certificate of Analysis Customer: 9Mruwlearig Ceara*, Bow Lintlostk ItlebotXoodY. 9413 Fab M 614-7110-6124 Analysis Test tubed Ammon 3pseide Gravity, OIL +86011 Gravity, peraiddislion 8sybo11 Calor Pt 1 Co Color (AMA) Ada Weak Cater lEssri-autursi Whoa Stdkr Commie orts. so seem pp Aeldtly Copper Strip Caimans 5slorstes, % Beam" % Tams, % Xybsob % Xylem% % lair/ 11018, Palst. C Dry Pitat. C Dbl./bap, C Water Casket, pp. Ansi D-881 Cs' D-156 0-120* 0-11411 D-1133 D-853 D-396114043 MO D-L18/848 0-2306 D-2306 0-2306 D-2306 0-2306 DAS D-855 11-855 A quatui Industrial Chemicals & Sawmill Division Ship Des: 0513003 Preetsp: Tolson Task lie.: 170 01.-.1..'50 2300 Vomet2!FilFTEM ZaciAMES---Mi Tidast IC*5 PO / Let Neg 43110608342.C3C0- C Spasifiestias 0.863 0.673 Men selY report 017 10 mut. Merl oft report *sly reper1 oahr Mort WI Mae oily MIK 00IY 0.5 asts. 0.03 rem 99.3 aid* 0.3 spas. 0.5 mos. 104 stir. 1113 was 1 113113. 500 mu. Tag Rods Class leisiet, free of perdu alai= Pam 0.1715 Pass 7.250 Pan 30 Pais 1 Parr DPI Pats 106 Pass Nes Pass 0.6 ' Pass Nag Pau 11 Pon 0.07 Pus Not delude. Pas 9931 Peas 0.02 Pass 0.00 Pals 1103 Puss 1104 Pan 0.1 Pass ss Pass A saspaadis Can Crawl 03'd Attest Melaka Camioss% DIvitlat efAitlesi ha, Das2210, oahmrs, nib MIS Surat ise Woman Mini Poreins La. PO Ws lePl. Carstlabri, lip 4312g. 60147.148482 P1031234 LS:ST sO OE 61141 6S9917.6909:xe3 AM AA 8,31 )1-4d4 SW-Scearce 01289 MAP-OC LAB KY DIV Faxt6069216659 Jun 6 wpas 12:35 PAM Arabi Ashland . ignow, At4r40: 2:78" Customer Certificate of Analysis Industrial Chemicals & Solvents Division Sbip Data 044443 11. ,, :I 03. 7-10 11011,sui 300ilt Usk Ns.: 170 Vessel: GATX-5710 lysbesed. ICY 40475 Pm 0; 414.71104424 Ship Ousidilin 23173 Tic100 15,13 110 /Lot No 4500142353-0CS PO No. Analysis Test WOW Ammonia. Spacing Grave% shal. SSW Gravity. pruulikillits lloplooll Caw lit i Co Calor (AIWA) Add Wash Caw 1Caurtaulassi Vast Sonar CSupaseds MA 30%) SoliMppla Aellty C.syper Strip Camila Salurolia, S leasees, % Visas, % Xylem, % > Xylwa, % NMI &slam Mat, C Dry Ptime, C Diu. asap, C Waist Curing, ppm ritual D-001 Cal 13-1511 D.1210 D444 D103 1153 D-3501/4040 D447 D-1301W0 D.2300 D434111 D-23N D-23W D.2306 D450 D450 D4$ Masten Syseillosticti 0.140 as 0.1173 roma emir ..pat stay 10 ross. mum O*1 avinvi WY mut sally mutt nay report tidy report silly 0.5 aim 0.03 was. WS ob. 0-4 mas. 0.5 was. 109.11 Ws 111.4 want. 1 Imai. SOO aisa. Tut Ranh' `1sss.=PI.MMPI.1 aim Ilsold. Au st psrUssialss Pao 04715 Paw 7.240 30 :1016 azY 1 Pus 5. Pus 105 Pus Nog ha 0.1 Par net Pass 13 Pus s Pus Net duseild Puss MD Pais 0.01 Pus 0.00 Pus 110.5 Pus 110.11 LI Pus Pass 47 Pass tlimpsiallaltCwOmpeely "%him DiEriprose Caeca* Dhisioa otAmbhai , 221% Gamow, aft 432i6 Sigma clo Mime= Aohlaal !Woburn UC. 70 8ta 1492. Cade*" Ry 41120. 606421.6502 160511111 SW-Scearce 01288 ,...-41CLAB KY DIV Fax :6069216659 Jun 15 2003 1352 P.02 Ashland Asiteed Iklinran6d1.1EariPani Customer Certificate of Analysis Customer again Wearies Cop ..Y somoklaue South _Biome*. KY 40475 Fax 0: 61t7904624 C Analysis Mu Tcza Method Appearance Sped& Gravity, WEL WOW GenvIty, pensdeliallos Seykell Cobs Pt I C. Cider (AIWA) AMA's* Color irdiceSSetasei Valle Suitor Craspennads (HA 501) Sultkr. pp. Acidity Capp, IltrIp Corydon Soterstok % lohotroo, t4p TOE, 9.0 Xylem.% ,.. Xylem, %I, Inled Mhos Poi*, C Dry Mit, C Dist. Rasp, C wirer ammo, ppot, Aloud 0401 Cek 0-156 0-1203 0440 0.1133 0453 D-4961/4104,1 0447 0.134111410 0-2306 0-2306 04304 0-2306 0-2306 0450 D-030 0-1S0 Aquama industrial Chemicals & Solvents Division Ship nee 64643 Product: Token, Tank Na.: 169 vessel: 11TLX4011006 Ship Quint*. 25044 Ticker Mal PO 1 LAS Nob: 4500613151-C3C0 ClaideUr PO No.: Specification 0.660 to 0.173 "Peet 6617 report lick 10 walk - Mon cet:f report racy report *ay rftrart 0011, Mort oblY report NO OS max. 0.03 mos. 90.3 main. 0.5 nun. 0.5 was. tri4 min. tit Ls maw. 1 Ian. SOO iresx. Tat Remake Clear Itiptia.frea of particulates 0.0711 7.260 30 2 On 104 iging 0.3 Hag Ill CIO Not IMMO 99.011 0.01 0,00 110.3 1 10.6 tki 40 Pan Pas Pao Pus Pau Pus Pass Peer Pass Pau Pau Pao Pau Pus Peas Pass PUS POMO Pas Pus Ami-Stet riP APPROVED A oasposom Carr cco4any Ashland Diakonal Cawley, Drriansi et Astrear be.. Om ntt Colonies, Me 43216 slime* do Metstiowo Aa61re Poevidein U.C. oo nog 1497. cul000us icy 1212o, 601-9214103 SW-Scearce 01287 AP-0C LAB KY DIV Fax:6069216659 As/ 26 2003 12:59 P.02 ..--;-d1M111111. AMINO elmorp ttt=1,,.c.anwri Customer Certificate of Analysis Industrial Chemicals & Salmis Division Sts DONK 0445-03 Cuswour 911wwia Wream Commas ON= Lawn Sao* Riellmald. KY 00475 Fax lk 6144904114 Al= ... +,1 . f Analysis Tort Wood Product Talmo 034740 10.411 230rj_.. 'Fmk Tic: 170 shipqmpsty: 25211 very un.x4silit arrkaa MILS P01 Lot NO.: 4500714111443.10 N 'Specification Teat RaostIa iPperame Speellk thirty, 0/1111+ VOIP Om*, F001/1040601 Saybd1ONar Pt / Co Cohr (AM) Add Womb Cabe Kaarlitiguaal Viler pmSolar Comma* 3021 Suillw Pro AsION? Camper eb1p Canes Salorsom lkmaxa, T010010,11. Xylem. 14 X.0004 % laKlal 'sew C Dr: PrlOt, C lImasa,C Water Casixxl, PON viand 1-1111 Cale 1361511 D..1210 D-I40 0-1133 1-053 0-39411/4045 D-I47 1-1311040 14304 0-1306 1-1300 143114 14300 0-150 0.450 0450 Aquas.* 0.10 OD 0.173 marl only 'VW oar 10 MAL mart only report "sty rapid Nolo report may roPIN1 ply nPart 400 0.5 ism OM lam i0J rik. 0.5 um. OJ aim IMO Wu. 1114 wax. 1 ma. 500 max. Char Tkaald, Rye at pardauloAs* 04715 7.260 30 1 ON 105 Net 0.1 Piwg 11 0.00 93.10 0.01 0.06 1104 1104 0.3 71 Pace Pau Pao Pau Pus Pan Peal Pan Pao Poo Para Poi Pao Per Pau Pow Pam Pam Pus Peam 1 --2" A 1 .3 2.'/' Aaa.lassodal A Rammed' Coo 223 1. 1.0:114.. /16e4._ gie4A A7PMV1D Aahlood Cdowdoka Comm, DiMiaa of Agri 1m, Dos 2715, Cabsima, OW 43216 Salmi M 34mdm .autind Pmeime PO 1493, Cadmium, Ky 41135, 1104.4111-4404 SW-Scoarce 01286 IsIPP-OC LPG KY 1):V Fax:6069216659 arribb. Asiskari . 4411mir Divigkor=bele7P-Y Customer Certificate of Analysis 11, 41 Jul 1 2003 15:19 Indusien cab cl Protium P.04 -- sion Fez Ps IldursuL ILY 00011 04741024 Appoutue* 15041114 Gravity, giaL (1)487 Gravity, psumbOialke 3ay8011 Claw / Cs Color ONLY Mid Womb Gate Kalw4-auus. Yoko 341ter Caroms& 0133, 803) ;Ain mu Audi, Caw Cserulas SiNowilse, % % TARN" 16 Xytuie, N. 344 Wad SIMI NOM C Dry Mit, C %a Raw. C Water Outdo, pp* used 1441 Cale 1.1841 u-not 1411418 D- 1133 D443 1.3441/411111 14147 D430/404 1-2306 11.1304 1/4.141 14346 O-2344 D4S0 D450 D.R. Annsamt Specification 1301. 1.573 Mon 011 Mort 4417 IS on. report may report oily Merl 4417 report only 149404 WY mon auly 0.5 inia OM max. VA* IL& 0.4 mom 44 arm 101.0111. 11L6 fox. 1 Ass SOO Ism Mil' 444 free el putludifto urn 7261 34 I sr WS Nee OA Nog 11 5.00 0.34 99.18 OA woo 1113 11 ill 03 74 Pi.. Pus PUP Pus Pus Pus PUS Pam Pus has Pau Pau Pam Pro Pus rum Pus Pao Pass ran Am04** Divine efAshim4 Us. ass MR, Colima* OW 43314 A1 Can Camay Snipe* eta atssesta mind 11111111111111 ELC. PO See 103, Cadolveurp, 41125, 606421-072 ? W4230 , C,13 "I'Ll4r11.1 SW-Scearce 0i288 MAP-CC LAB KY DIV Fax :6069216669 Jul 23 2003 12:26 P.04 da1111111b Ambient' lqumPP ritiotauak.s betci. .p.,, Industrial Chemicals & Solvents Division Customer Certificate of Analysis Ship Deal 574043 Sem ism kith ---110111111141ELIE.L.--- Fax 1k 614-7104 Product Watt* Took No.: 175 03.17.12 1114111 2300 Vomit max4M4 Shin 00155111 14711 Ticket 1CO3 PO / l al No.: 03007147104301 A Analysis ss11sss=...... ....111 Test Method 1011111ss Appursses vivre' eposifli Getsity, CON D411 Gni*, pssisistsiss isybsil Claw Cale rm.% Pt 1 Cs Case (APRA) D-1200 Ada Wris Calm D-848 ILsorillsosssl Wes 114133 Csopsosils (Ha 002) D-$53 flotsri ppr D-30111/4048 Add* D447 Cops ilslp Corrodes %swam 414. 11.13540 D.23011 Raisste, Wises. % DOW D-2301 Xyliss, D-2306 X/i100, D-2304 Wild Wilms P. C Dry Polak C 01141 DI& losp, C 0450 Cssisst, pp* Aquila Spestasslos OA, is 0,873 Molt NOY report serf 14 ass Merl WV report *sly mow. only Mori 0513 rayon oily 1100,11104 0.5 ass. 0.03 am t0.5 oss. .laws. 103.8 WE. 1MS poss. 1 mu. 3N Tao Rom* Our Ihisid, fres of parelsololoo 0.1711 7.20 30 1 ON 105 Ni LI Nos LOS Pus pus Poo. Pms Pao Pus Per Pao Poo PO= Pro Poo Pon ss 0.05 110.4 MIA 0.2 154 Poo Pars Pim Pus Pan 1FI N1G !' Ano.sisi 27 :3 A RolooliadoeseCempap Maud Dkaikeioo Ompson DIvZu of &Sal bs, box 311,, Columba, Obi. 41310 Slipsiercgo hisfolboo Askhod PokOho00 LLC. 10 Boi NIL Caikiaburi Ky cat womi-esca F11.31814 it SW-Scearce 01284 MAP-OC LAB KY DIV Fax:6069216659 4aM1111111ft Ashisad MOW 4:4114. grairj Customer Certificate of Analysis Ctsvms: Muerte Willkamo Cemiesv Busr UM Sas* Rlehnind. KY 40479 Psi 1k 414-79044241 Jul 30 2003 13:55 P.04 51.044 C10 &I'27 'RC-- Industrial Chemicals & Solvents Division Ship Date 07-311413 Product Ulm* 93-17-10 3 2308 Tank NO.: 171 Vets* GATX41111041 - 316e Oisathr: 2040 MAP 1C413 P01161 Tic J0R71921111-0C1 Analysis Tel Method Appalls** Sysellle GPM% riaL POP Gravity, putidriplise Saybell Color Pt Co Color (AMA) MP Wm& Calor Knurl-Outeist Wdw UMW Cuspinsio (112IL 302) Mew, rpm Maly Cows OPP Csrr.al.er % Benisso, % WWI% % Xyloss, % g7101141t % laftlid Draft hist, C Dry Polak C DIP. Rump C Wear C111604,1, Net 12491 CP. D-156 D-1309 D-0411 D-1133 13.101 D-3961/4048 D447 11436049 D.1306 1.2306 DON D-2316 04304 D450 1451 0450 Aquatint BpsalioNse II.110 OP 0.$73 mot rely Med 4119 tO wed. ruin /My repast oily rout Italy report .sly report oily rigout Ply 6.5 pas. Ole nue. MI TAW 04 ass. 0.5 trall. 109.4 alp 1114 on. 1 sus. SOO mu. Test Repko Our &pie, fres of prIterlitst 7.261 30 t au 106 Nig 2.1 Nei 11 US IA 9917 0.02 LOS 111"03.6 OS 176 ssss Pus Pan Pis Put Pus Pam Pus Piss Pip Pi Pus Pus Past PIN PIN his Past Pap Pip PIM Act-Stet 1411o4904084 Clio cillgaffy s-as-er AG 6 ,;: . Ma 61-- 4342/ Asklarml Dquibudou Compoit, Mirka of hie.. Si. 2219, Collor/bac Mb 43116 30011114100 Mends* MVPS rod= LLC. PO BO 1491. Catlesiburi, Ky 41129. 6064214101 15091102 F 166414 /0 SW-Scearce 01283 MAP--OC LRB KY DIV Fax Alibut 14111111111PP IVIVegar't Customer Certificate of Analysis Aug 8 2003 12:09 P.02 Industrial Chemicals * SWents Division $Y 4047e Ti): )70 Ship9medtr k404 Vex* krrlar31}141, Twit, ' Analysis Test Method Amimsome *aft Gawky, Ws& gme envoy, peurdifisios esylsh Oar . Per Co OW (UNA) 40111Wasb War Na seLasessal Vass dMMlr Coupsumb OM Man 0010 Addite ' Copp, 111r1p Carrssie listoralust % Ilissask% Tabor, % 1441It % Itylw" ]dial Maks. Pout, C Du Polo, C Dit. Wow C WibrCsu12.1, ppm Asia WW1 Cab D191 D- 120 DI411 W133 D053 D-1011140411 Die D.13W1140 0-23111 13430$ 0-00 D30$ D.2384 D-110 0-00 Actuated* Spaced= OAP le OS* Mon solY Mon mil 10 ma. 1Port IN* Merl as* alki roPowt 0011, men me mud ads 0.$ 0122. OAy ass. 99.5 sale. OS nu. 0,5 mu. 104 Wu 1114 Iwo. 11112. NA um ; I Ns I 7. 564# 2 I I' Test itan$0 Chet 1111111d, It.. apsubibus 7.34$ 30 ON 104 N. Nes 1$ 0.00 0.01 0.77 0.03 0.11 110.4 nag 0.2 77 Pros Pup Pia Pus F. Pow Pau Pau Pus Pus Paw Pus Put Pao Pus Pass Pus pow Pus Pus Fle04111 oldie I3 /3 ilfr? APPROvi1D A Ikesposor 4w coma., nitwimfsAsbiled DiaislladasmCeotsm* DMIwioipsasapre1A10li1b11i.1li1r0_11D11a1111M41C01asmbs. MIrib 41110 wiammt igla Minds* Mild Pabgame ILO. Po Dee Mt 001.10ras Ky 411* d01.0114102 SW-Scearce 01282 rrir--wt. I.t W M LILY t ex :auti4a2laas9 Hug i 2ULk5 11:1}y r. 1.14 MAW "411111111111P Customer Certificate of Analysts sImlails111111OPMs11.1. Dargeamellork_ Industria Ship DOE 0443 Solvents Division Fax IR 914.790.0134 A DID # ' Analysis Too Method Appian/an Spoils GoariO, 091. WM Growl% poodolialbe 4a-bell Oder x r C.a Coler (Arno Adt Wok Color 14:aualMormaiVaIre SOW Coormotir mason saran Intim Add* Clow SatipCorrois Olitlirldnit Taboo irs DOWN II, Deli srailtr.0 Dry Mahe MIL 11**E4 C Waft. Cosimi, vinkal D491 Cale D-1.9411 D.1209 0.11411 .H33 D463 D-3961/4045 0447 0430149 114309 D306 D396 13.2309 1123011 30.40 DA* D4 Meals* ICVIP0 Colmar PO N speradooloa , Tor Rooks 10== Mar Urptki, fro elpartivisha 04719 7.110 30 ON 196 Nag 04 Plog 131 0.09 0.01 99.77 IS 1 1194 I1.2 For Pro Pim Pro Paw Pair Pt's Pan Pa pin Pus Paw Paas Poo Pus Pan Pan Pan Pam Pao 1111.1914110dai APalpsoao caw Coampow Airmssuannia Campo% DivivilowurAdsirsii ha, iNs,2210, *holm, age LIM kluillson Fmk= LIZ WINN. 1492. Catletlisto. Ly 11129, 6011.911.6101 Clag.0 301d rr1,-.1. SW-Scearce 01281 MAP-QC 08 KY DIV Fax :6C69216659 Aug 12 2003 12:28 P. 04 miumPP Industrial Chemicals & Solvents Division Customer Certificate of Analysis Ship Dale: IS-1043 Cuegna Nimrod* Whim Conisert_ Pr0411011 Tolima 03-11-10 105 3300 Deatiess fin& Tisk Nat 170 Voile FA1X-254114 Mara KY *ICS Omekv: 23491 Work Na * 6144011404_ IC/AUSU Lai 1.4*: 450413063:143CO .A1964011el 1rgelCameek--- Analysis Tea Who, ipoottlaigion Tea Results Apporamo Swine Gm*. $11` Gravity, pousalgiNse Sybil. Color PI / GC*. (APNA) Acid Wadi Oat Know.418ftemi Value &Efts Composeis Mt& 302) Solar, we Addle, Capp* IN Corr*** Elatinflwoo % VuEUEy lIr Telook X.014 % > xPilsot % WWItsNhig POW, C Or Ptak C 01.1. heir, C V*414,011111, opsa vineel D4101 Calor IMMO 18.144 n4333 D453 D334114010 13.647 0430//0 NOS D43411 D2311 D1341I 04300 WSW Do1110 DM, Mutest 0.II9 le LS73 NW. 01117 nowt NV 10 nu. *Mien will I Mork 001, filor0 NOY evpiel Marl NO 44 rim 4.00 nom 0,5 rift 4.1 mph oi ream. 10.1164* 111.E vim II maw Mau. CIMr 1140* free et per`pdlabe SITIO 7.340 311 1 IN 1011 Ilse Nei IA ISM LSI 0.00 110.5 1104 0.1 Pao Tara Pies Poe Pus Poo Pam rue Pro Pow Pre Pus Pus Pau Pow Pro Pus Pew Pais Pam Asii-Sies WW1 itspor011 Um." 5-6 845' HA a I :" Ja--c i.,72111 1-0742. 1 ge,.? e7"- Ashhoi Diemilmithe Compasy, ABihrsi Ti,., 33110, CNN*" 412111 lisipmei Iftiolita MAW reiviraLC.V011at Coesmerag, 41t* 601-931-50:44 SW-Scearce 01280 MAP-CC 11:19 kY oru Fax:6069216659 Rug 12 20(33 9.20 P.06 Asklasti Nommi ADieveMigiacrys.Y Customer Certificate of Analysis Cusuipsa "eels *Met Crsossis 11111141011 kith Mclean& KY 40473 P. IP 010.704424 Ater Analysis Tut 340104 Appearanse spudlk Gawky, 0t1 0010 ONO% psuolriplai Saybs0 Odor ft / Cs Calor (AMA) Add Wiab Car Kouraressel vamp !War camproode 111=4 '02) Whir. so Adaty Copper 111r1p Consols. 3alw100. % ilinsesa.% Trieseep '14 WAWA ; X71w0. % 101101a104106, C Dry Pik* C Dik Dram C Watt. Cones* ppm visual 1/401 D.156 13.1200 D-1146 D-1133 14453 039614045 D-647 1-10/100 0.2306 13-230 D-2306 11-2396 0-131111 0.066 13-150 D-I50 Agnate* Industrial Chemicals & Solvents Division Ship Dens 110.1043 Putivice Titus. 03.174 0 101211 2300 Tack No. 10 shgl 04446ty 23165 Vault RAT7[20117 Tletrt 1W PO r Lot Ns.: 4300737421-ace C Specification 4.160 to 6.573 mere rely report 44IY 10 num report only Merl isir mind 0111Y mitt arry repeat only report sulky 0.5 u.s. OM otos. 004 gas. kg nu. 0.S Pus. 104 NU. 1111 rm. I AM. 3011 mu. Tut Ranks Mar 1414 liree 0.0716 7.266 30 2 Is 011 N. ea Nes IN 00 6.01 905$ 0.01 0.00 110.4 110.6 02 2113 pulisalaiss Psis Puy Pus Pus Pus Pete Pau Pao Psis Pus . Pus ?Us Pus Pus Parr Pass Pm Parr Pau Pau AUG 2 5 r /03 5517 iLii-77,3 RumettliteCne Drury Dineen of Mimi lust lu2210. celnues, Olds ShipmEleJo 'Moans AskIsal Mao lauxopmetwas am 'An 1501002 P11.101111 SW-Scearco 01279 MAP-QC LAB KY DIV s1101.111. Fax:5069216659 Pug 12 2003 15:39 P.02 0==Z:7cm* Customer Certificate of Analysis ...10/1107 Fes 6: Share's Csuosso Sew Limo llootb Rlaiousd.101 40475 0147104414 Analysis ssss s Ammar* Sonag: (Surd% OIL OW GrprMlr+ puoMMOilso Subs* asks / Cs Color (AMA) Add Ws* Cs sr kod$41otand Value Solror Compounds (101, $02) Sabo. ppm Asollor Copper Ship Corridor Saturoloa, Burro, 114 Tokmx". % Xylem, %. X7101 `04 MY Slav Dry zoslos,C DIN. Lwow C C Wider Comsos, ppm Tut Msdis4 Asia D411 Cols D4 D-1200 D6411 D1133 DSO D-3%1041146 0447 D43100 1:1-2306 1)4314 04366 0-2306 D306 Es40 1:0459 MIX Amman Industrial Chemicals & Solvents Division Ship Dust 06-1343 Prodsch Taus, -.1=1s1s110sNalme 03-0-10 ISM 2300 Took Nis 10 Vaal: ACIM9307 Ship Cuostilm 2411111 Tisk* ICU PO 1.400.4 450171000-C1C0 No.: 0.0011 to 0273 rasa nay mar 10 nat. rotor, witi report oily report nay roPorl esh ruses 'ply relied WY man. OM am. 91M Eds. 0.5 as.. 0.$ issa. 109.6 WA lam stns: 500 sus. (]ear WM& Ove erpanisibiss MIS 7.24$ 30 2 Oa 10$ Keg 0.1 Nag *1 0.13 0.11 9,66 0.00 1.00 1104 110.4 Pam Pao Pao Pus Pao Pam Pus Paw Pas Pus Pow Pug Pus Pus Pass Poo Pam 36 Pses Asinatailal A limperlitam Compaq, Masa Ditribuda Calvary, Maim atAgimiloa. oat 3216. Cohoria4.016. 43216 Slipowe do Mina= Miami Portioantl.C, PO Bat tal, Oriansm, Ky 411" 06421-6102 P*311234 SW-Scearce 01278 MAP-CC LAB KY EV -airsab Ashland Fax:606921665g Pug LB 2003 16:03 P.06 miziauir"" Customer Certificate of Analysis Industrial Chemicals & Solvents Division Ship Ds* 6114643 Customer Boot Lao* 1406 Tohula Tack No.: 160 03117-10 nag 2303 Vomit &mown Ktelrososol. KY 41/475 Ship l 11111x. 13680 Tisk* Pox 414-M424 tad PO ILO No.: 4501/74541430 PO Analysis Test Method Spocifieshes Test Resale "ippon.* Spotlit Gravity, *AL OW GrtwIty, froomWsellest 3679811 Cher Pr ' 7.4 CAW (AFRO An Will Odor Le.A.14106661 V kiss 94.1.1r Common& ta219. $02) I ttl9w, ppm 4ttaity Copp...Kb* Csersslos rt.iataa, % 1g 'AM" 9 Xylem% % itfisas, % Z. al it %Kiss Palo, C Mat, C Kamm(' 4"11 1 Er Cutter, PPn vitae( D-801 Cale D4341 0.1209 0449 04133 12.163 12-3116114045 0.147 D430/949 0-2396 04.3116 D-2306 04306 0-2396 041511 045111 D-050 441169114 0.169 b 9.17.3 impart oily report salty 10 mot. report stay report sub rerai Mimi ONO ripest salt' rePert 011 OS eau. 2.03 sus. 99310. OS tau. mu. 109.610. 1214 mai. i Num 501i ram anr 110.14, frau at portrsahan Pus Dill' PO40 7.260 Pass 3$ Pas, 2 Pot Or Pass 11111 Pow Pits 0.1 Par Ns Pao Pus 0.00 990 Per Pisa 0.09 Pass MAO Psis 1104 Pass Psis 0.1 Tan 400 ha ..zed odd A &3ti, A ittspowihk Con 0Assmstt Ash14441:44wierior Campery, Vying* ag As/dog his., Om 2219, Ceram, age 41210 Shipoot Gio Airmails AsithsdhissicAn114. PO Mx 1402, CalioNerg, Kr 41 IS. 60114214M Pta411134 SW-Scearce 01277 ticP-CIC LAB KY DIV Fax:6069216659 Pug 18 2003 16:03 P.06 Aeqdduionwg, Aikkai Di*ION Canpay Divinut of Ae Customer Certificate of Analysis industrial Chemicals St Solvents Division C M=Mis.m. 5.t11116" 11111. MMus& XY 0479 'Ini Pm 01 614.79114424 :ozianigUiMEN Analysis Tut Monett Appranims Spada Growth 00.. esor Gem*, proollersollota Sgt.* Color Pt I Co Coin (AMA) Acid Wait Color Koartadosin Vain linfor C000pose MA 1102) war, 1144 Aridity Copper Strip Cunene Samna% % souk % Tolman Mr XY1404. % ',. Xylotto, % Lund Millie NW, C 'ft, 'Mai, C Mt 11b1111C Water cubit, PM *oil D411 Cab WM W2I1 D4411 D4131 0455 D-3001/4044 D44? D431/441 D43114 D4341 D-2306 D4304 134306 D4911 DUG D-1131 Aunt* Product T 03.174 0 mm.ow. Mak No4 10 SIdo Ountitic 23614 Vona ACIII-71133 Ticket ICU P011.0 000741111-C3C0 Cuatoto.r PO Na: Spoticalsos rt10970Cb.i'It 1.7 cr"Tat itopidis LOT-34- ken 421. to 4.173 Mon logi Mort only 10 wok report nip report en, report ealy report WV Mont any ryPert gay 0.5 nu. 0.03 mu. 913 min 0.5 mu. OS on. 109.41 War 1114 atm 1 ,.ma. SOO ma. Clear Bunk du of pardoning* 0.1711 7.240 30 2 pa 10S Nag Li Piot to 0.10 0.00 34.11 0.00 0.00 110.5 1104 11.1 400 Pen Pam Pen Pao Pan Poo Pao Pan Pan Pao Pr Pen Pan Pan Pus Parts Pus Poi his Pus Aut1-3021wh4ri A nwporilikCanCompny As144,411)11n441414 041 , Divition at Ashamed 1444 04i 2319, CiArims, Ohio 432114 noire eto Pareadmet AdalsoiPoltoloriLC, PO Sox 1492. Coos n% 1(p 41129, 44*P21-41103 11 1440114 SW-Scearce 01276 airsibb Ashland industrial Chanicals & Solvent' Division Customer Certificate of Analysis Cu.toanar; S, 4140044.1 00.3143 T4ig1404 1.9 This gloat,' 14614 Analysis Tod IOWA Appramssoo Mama Spwitia Cmaotp, Oa WM! 111.091 Gully, p000dolgalla. Cala Saybit Calm 11/ Co Cal* (APRA) Aoki WW1 Color 1Coarlaolomd Yahoo 114311 13.130, D4411 11.1133 SOW Compass* Q131/. 502) MD Baffin ma 04001/440 Add Ma *alp Cumin 13.1311.01611 Solaraill,16 D-3306 mamma% lb 134300 Wash % DOW Vial% 94. . Weft % WW1 Mk. PM* C 0.33011 SON Dift MT Pohl, C Dane D1.1.134404C %POI, COWIN* Pim D4511 Aq. sive* two to us raPfl WV Apart only 10 mom report oalir 751:11.6410Y moss *sly Med o1 r out telY mom 0.03 mam 994 id& Al mas MS mai, 1094 Ws iii4 mos. 1 mom WI IIIM rare Rai* Clear Hold, Ns of poplimololum Polo oirt" Piss TAM Pro 30 Pao 3 Nag ON Pia 100 Pop NAB taw al Pam sii Pan 13 Par 0.07 Pam 0.01 PM MO 0.00 Poo Pam Par Pam 110.1 PIN Pa 101.5" Pam Psis 61, %q Ur Ait1401 Masi al A itairmillo CM clergy" 93 .a *\633d4L \403c( Wpm' eh %WM Mire fterstiumlie. Po Ike 193.Calambwia Xp 11119, 1004ill AO PM-I034 OT WO: daS 08SM5909: wniztus Homan! SW-Scearce 01275 RESEPRO4 ATRIUM Fax:6069212580 Sep 9 2003 15:48 P.02 dromiab AiNand. muinow guazglakx Industrial Chemicals & Solvents Division Customer Certificate of Analysis DapO 09-0840 cartoon Sample WIlltaiss Commit Boas Law Boo* BMus* KY 40471 FIX 0: 114-7944424 Al Ddb Mat OCAS_Columbeal Analysis Test Method Aiisoraiss Sunnis Gravity, shil41110, Grivity, issidllItsikit Ssybsil Color Pt i Co Color (APRA) Add WW1 Color Ka sr4Bitsiel Valor gilftw CoMpsisds RA 102) 5.11W ppm MOW? Copier Strip Corrals* Soul ON% 14 Blasso % Tolson. tlo *i% % 2' X.7000, % Initial Millis tot* C Dry Salsa C Diu& Romp C %tor Onto% pp. visual D-1111 Cali MI6 D-120 D4611 0.1133 WS) 1:63961I4041; 0417 12.130/1411 0-130 D.4311 D4315 04300 0.23011 MN D-Sse 01150 Aquatint Prottiott reins 0747-10111 2300 Task No.: 161 Vito* GA1X430111 Sidi multi: 24141 Tisk, MIS Po/ Lot No.; 4100111.74-C2001 Maine PO No.: 10233.1 Spa:Maio* 0.10 to 0.173 report only report Italy le mu. mon oily mat oily report ally ripest sal, mart city report oaly II mu 0.03 sus. MS ale. 0.5 mita 0.1 EMIL 101.1 NIL 111.4 :gas. I rim 500 was. s. ss Tat Bassi s ssssssss ss.MMPOMMINI Our [lova, Cress of partlestaso Pus 03715 Pus. 7.20 Pus 3* Paso 2 Pim On Pus 1 011 Pass Nag PUS 43 Paso Nut Pus is Pus 047 Pau 0.01 XPass 99.1111 0.12 Pius Pass 0-00 210.1 Paso Pus 1104 mg rasa Pass 43 Pass sNI! Aa03111 added SEP I 8 90414 51'570 /04011 - A Kauai* Can Cowpony Ashird Dotriarsta Carly, Ottisla of Athloo4 Ina. Da 419. Calorabao. Obis 43215 Mums do Wines. kalarl Panama LLC. r0 Su 1402. Cassaatirs Ky 41139, 404.9214101 SW-Scearce 01274 RESO4a34 ATRIUM Fax:6059212580 Sep 15 2003 15:13 P.02 Ashland iminew Of4=2&""7 Customer Certificate of Analysis' Industrial Chemicals & Solvatts II. I 1443 cn selmiosolo Bildrusi lar JALgi____atzadag 17S Vas& tip OUIWOY: ISM reitot ICamp Lot 1194 43147011111471p Analysis Tut Mulled Appeonap 3.0111k Cru445 Wet. OM Grew*, presdsipliss MIAMI 01P PI 'Cs Color onso Mtn Witdi Cofer Illor141s1m1 Wee Iliihreapeado (101,103) Ssihr Ns Adair Cowper le* Corrals* 31111railes % Dunns, 16 Win* % Via, ii , 17!.. 14 101111 *Ass Pei^ C Dry Palst, C 01st PasysC Wsur Cols pm vImed D.1S1 Cale WU D4300 D441 . D.1133 : DIM 13.311111/40111 TOW 314311/1 DOSS u43011 D4314 D4304 043411 0430 MN D416 AVM* SysIlaurios 8.301s 1473 mai oily 1144181100 10 na. mai wily, Mod *MT mat esti tweet only mai air reportall 11.3 mu SA aus 99.3 silk 0.5 row 041 was INA ob. si la sou 1 was 105 ass. mil4p1 Mai OCT - 6_. .3 Tat Issalto Clow 1464 fru of pueiraisiss W1S 7.2110 is 1 IP 1St Nue 4 N1 HI OM PM dsiosisi *33 0.01 Ii. HU 110.11 sa 33 Pus Pus Pan Pus Ama Pao P... low Pas Pus Pus Puss Pus Pass Pia PIN Pus Pi* Pus Pus 69kiikl A slaa ktoyesible Cup Cum, layr,9 7 57 75-- .A.htis1 DurIbrisa cuspot Wass sidod 41 MP, Colosimi, ilo 13214 SWIM des PagtAb ArkilethesialisLLC, FO aim IWA. CUINNIMP K7 4113% 198-7214.071 raptor SW-Scearce 01273 RESEARCH ATRIUM Fax:6069212580 Sep 18 2003 10:54 P.0? %mow Industrial Cheinic tit a Customer Certificate of Analysis Matignon illoontis MistCumin SIM LqUinitila Pan 0: Itkimsni. KY 40476 MINIM ,.ssssss=1ss Dane a.7 neag.,,172. 1L.Siakamt___ Atialltity: 71doss, WAIN / L.oNt o.; 45007.5113C30/ Analysis Tin Method Appearance SPonof Orr*. WM. WW1 Govelto neendo/palo Unbolt Cow Pt/ Cool:sign COW* As Wait Coke Knarlaslinal Woo Nino Cangenek (11:1&104 $vitnr, paw UM" Copper OW Coombs Satinda. W Dosaanst VA taiga% % %AMA 2' Vim* % Inillel Wan row, C Dr/ rib" C 061 C Water Coalanii, visual Ow liquid fret et partiegailis Pan Cat D.106 131200 134111 1:1113I 0.10 as 0.173 report sat/ ropers oaly 10 am. report silly mod Delp 0.17111 7.20 sr 1 IN 1011 Pals Pus Pus Pus PIN Pon 134111 D.3501/40011 "Vol ea* mai wily Nag Pan Par 1/447 Mort My Nag Per 11.130/040 DOS Mot MY 01 MIS is Par D4300 OA no. Not deissail Pus D2315 Dans oto ads Or! s11nt. 90.91 0.01 Pee DUNI Dal D41110 U nay, 100.4 inlin. in.1 msg. 0.00 taut Psis Pat Pow D4100 Anaalen i num no alai 53 Pao Paw 7 -517 4/2 ,, - bi PI &6r 4P2s7 , ,i Ald4no Wei 1Y: A paprriiir Cue Claim, Award Dipeallien Camonry,Dnialm Omaha len, DMZ it. Calwalm, Oho tots Stipment rleltuaere Mimi Maim LIZ, Po 5i WA lty 4112t 5064214102 F111.30414 SW-Scearce 01272 RESEAKH AIRIL14 Fax:5069212590 Sep 25 2003 9:07 P. 04 moat ql11111111P` N=5=arp'sal Customer Certificate of Analysis Industrial Chemicals & Solvents Division rash Nat 10 Sh10 Oaratiiv: 24140 SAS PO / Lot Nas Test Mod Aesparraws Sessile Gerrity, Val. OM Gnirlw 1,0100001601 Say1011 Cols, n^a c (AMA) Add We* Color Kass1480841Vaina Sutter Cassaireis We Mir, no Ades *gigot 080 Ceresete SNw/11A lf Boussot % Wee* %- X:rinse qtr a nimbi % 1.10$ MOM lostst, C Ovr %Imo e DIA Mob C Weer OMEN, pp. visual P-801 Cats WIN 11110 D441 net s 040 13.3100400 D40 D13100 now D-1301 D43111 0130 11430 1/411 twig D40 Agnates)/ Sewillsallapt OAP Os 8.873 Mart oar retort osly ties; nest we report oily MEI mil Mbar* WY rePore fob tspirt only 03 LOS ma. 0.8 0.8 NIL LS MM. iii. 1114 maw 1 ran. tux. Tat imults Close kink fret 0 pardadies 0.8718 7.21 38 I Os Net Cl Net ID 11.0 Not 114401441 99.911 1.02 110.7 *mho 0.3 135 hat Pus Pus Pam Pus Pan Pun Pats Pass Put Pass Psis Piss PUS Pus Pus Pam Pam Pus Pus Aidasi midst \I-jk 51'st -4f AS!PItOVIID A RoponibbCov Coca" Amiss pitmen COMM OMAN of Aphind gra, MN 2219, C414441445 OW 43215 Shiposs shiltalerliho Arbbsta Penis= LLC. PO Bus 14115. Combo% Itv 411* 505.5214555 P WOW SW-Scearce 01271 11,ESEFRO4 PIR1114 Fax :5069212S 0111111111111W Ashland . olompoi VIVAI* TS r Customer Certificate of Analysis Sep 29 2003 15:50 P.02 Industrial Chemicals & Solvents Division Use Loa Scietb Weiirm4,car 40475 shin OuSthot 24857 _Palk 61 44220134 immagimaggagSltiaMe Analysis Test Method NimmimM.11.11r 1Ca5 PO / Lot j40.1 mmes.....a. sigEr0aito Speetfloollos .11ss11...1M.y 450117705001X0 Test items Isi=ouomouramIt oppeorues Spiel*. Mei, shot WIT Georg% pousdotollm Soya* Color Pt/ Co Color (APRA) Ads WWI Oiler georl-lotooll valor Wm) 0-401 Celt D-156 D-1305 0-4411 04133 040 to 0.871 report eolr WPM mar 15 omoo millet ear Men 8111, Ow H4s41. frw at mahatma. 0.11715 7.140 IS I 1)* 104 Per res. Pea Pus PIN NM Pap SolMot Culposo& ODA SOX 9olfor, pp. Aoldlit Copper Solo Cernisla. Soessolook 98 asavos, % Tolosa% % Xrteos, J. ' X19004 % 1,40M MUNI Poise, C Dry Polito C Ma stoop. C Water Cool sit, pp. DMA D49111/404$ 1)447 0.130,141 1113110 043011 D13011 1743214 043011 34611 D464 Oils Mutest report may MOrt clakt noun Golf import wely III mi. tie sum 99.5 all. MI sass. II sus IOU ode. if 11.6 mom 1 mos. 505 otos, riss et Nos 1111 0.04 Not sleteetsi 99.93 0.81 VIII 1101 I MI 0.4 135 Pan . Pus Poo Poo Asp Pees Pew Pm PUB Pus Psis Poo pees ket-stse Weed so .44 so OCT I 6 s],-,),3 Rzeosesibi it Con Compaq Miami Digitalin Ceousy. MIAs 444.10.4 us. leo 11 IP. Coimbra. OW 42310 *met do Mauro Mire haulms 12.C. PO lee lo12. Ceduslor k4.423-4441 SW-Scoarne 01 270 wor% 1A.:.)0 r.ui Asidwat _arvinido aggai.m.p.re. Customer Certificate of Analysis Dposa Los Ise* widesii, ICY 41.7. 047204(21 indusoial Chemicals a Solvents Division Skip Dus i SAM rfinetu_ is; 0347-101DM I V0114, AC17472914 Analysis Tss Melia Apperrease Spoils gis Cavite, psosiessiliss awls* Color Pt Cs CM, (MIA) Asill Wash Colsr Kasaiarimal Vries Sulfur Osmosis (A Ma WIWI, ppm Add* Opp, IN* QM** Sabsesiss, % Dosrsvo, % Taboo, % Xplso4 % >. *Au* % bidet alibi NMI C Div rime. C Dist. Rapt C Wiley *latent. PP= AIDA Cab b1011D42310 Did 131I D-D0 13.3410/4046 D447 DOWNS DON =OS ow* 13.2311 D344 DM. 044111 AIDIOISt *atom odssi Ts* Raul* LSO so 0473 rePerhil* -oak 111 sum Oar *AK This et partlesissus 0.1111 720 30 3 Pkb PIO Pus Psis Pun l oak IV". WY OV Pao /Vert tilbc now ear rvioNt *dr now WY Oi ass. 0.03 sati. NJ alb LS wax 0.1 bib Non Nes LOS Not lisloolst MID vat Par Pink P.. Pas pus Parr Pin Pass ems IDU sib!. Mae mar. l air. 501 mks 1104 1104 06 30 Pas Dam Nil fte^oN P 1.5i " 7 Pas NOV 3 4 Ci 361 /OCZ02- 401"/ 4L4.44astiers..03 30. Pasposials Can Comporf maid Diurimiss Shimoda MindurMlir.i stAblibilsa., Mit Okb 43E0 cu, PO His M91, Catlifebori. Ky 41120, 60114214M 9e/t'0 30Vd ltr1HS.70 he:9906/. T9 6P :60 ECIezito aT SW-Scearce 01268 1o/07/2053 15:25 6147906624 KttitHICA riIKitA Fax ..4.gramb. Atalimmt ASi-LAND 1Cas Ott ? 2003 15:06 PAGE 02/83 P,04 ati lormar Customer Certificate of Analysis Pus ill; 3081P 116011 XY 4M71 cuessisi k, . Altair" Too MAW Appeimes And NINO 0:1Invfty, VAL OW D-814 Gaya* plosed.Iplles colt 1140411 Calor WOO Pt Mir Cher (AMA) 04304 As *Fa Color D4411 Xims1411.14sal Vibe D4111 1liter Cespeomill (11210,802) SID pow D4061/4040 Atilily 134141 Carper Strip Ciao** D41.449 388111114114 asis ns` % D.230$ D43.11 11piesee, 9204m1 Volk W4 D-2301 ). Mum UMW Ward Who MAI C D-1118 Dr7 hemp C D400 Di140. bop, C D4011 %WC's*** pp* Muslin Tank 11441 sm. 0011#01 231511 Vinde rorSlipla 11414 Sp orlon 0.1010 Uri More mit Mori 401ir uary report of* Moot GeV retort mat Mort asir ryperi tidy mai esly smi, SA am Ogia Rik IS am 0.11 max. la& ada. it.4 Meow attar. 500 01106 Tat Rea* Mar Num, free el partials** MIS 7.247 30 Per Pan Paso PIN ON talc Sue 03 14111 1,11 0.01 rag delsoted Mut 050 0.81 1140 r iot. 0.4 PIN Ploo Pop PIN Par Pate Pits Pere Pe* Paw Paw Pus Pan PMa 424414imilloi ir;i 2 d 141113 A llasprollie Coo AthloilDherliidet Cospow. DlykkeforAskim0 Ia. dw znik it Olit. 41214 Skipagat "Marmke 4461441'41,414im LI.C, 11011as 14N. Collishinve. it, 41120, 6201214102 P11141111114 SW-Scearce 01269  RESEARCH ATRIUM Fax:6069212580 Nov 5 2003 14M P.02 41111111M. Maid 1.411111110111. jtryis=1i,,nt",". Customer Corti ate of Analysis industrial Chemicals & Solvents Division Fax Of Rhanank KY 40471 0147904.9 Analysis no Method Appanage Spetalle Olevftp, gent. 001P Gnat , paisitt/plia WW1 Calor Pt / Co Calor (APRA) Mid Wolf Cabe Kareasitat000t Woe CompnanCIM SOS) $1111114 ppm Atter Copper S$rlp Carron. Satarata, 44 Batanta, 'Nam,, X310104 Xlisset 114 Waal Bakes Pea. C Dr/ Poit. C Diet b. C Wake Caatsat, ppm Anal 11.001 Cola 143i D4209 1.1411 1.1133 Das DORM D847 8-120/148 LOOS 043111 14340 0.2311 /459 ease Aqaba AeRilot added Tank No.:, y1 Voids UTLX.280364 .2111993111011LONIEEM s=1.06 IC 01EMP. OrgolScides LW to 1.073 rant alp Min NIP 10 ago. roper! Daly mart oety Mori 4140 non air report opt, Mort debt OA an OA was 09.11 sea sno. 0.5 lam INA Ws. tga.a mow SOD imo. Tog boo* Clear 11414 Ma of parthraken 1. 7.747 30 2 ON tolt Nos 0.3 Nag 11 0.10 0.82 49A6 0.08 OAS 1194 104 0.2 17 NOV I 9 ,_j os-c.( *4.,z0-141::$z,,v;cs fiff il l i ff i ll if i ll if r Ammo cyter....... A Rama* Coe Atelattavagas oink* of Pawl lee. leo 2110. Cehrelee, Okla 43201 52loneo Wilma* Aollblid Pinhole LI.C. PO Bee 102. callsheme. * 41124 606.081-6102 hsoaso SW-Scearce 01267 Mow 04 03 03:54rp LaberatorU 513-341-2114 sMIIsIINNIMMN111.s+ PI Ashland Distribution Company Division of Ashland Inc, Customer Certificate of Analysis 6POT-- Industrial Chemical & Solvents Division DATE: November 3, 2003 Product TOLUENE Tank 4 !memo:1124ns. New Albany, Indiana Ship Date: et.144 f.7 3 . -AN ..) -.....dousrarIP4- 11714,6 Ship Quantity 4/00. Sales Order No: 41` r8/4 't nPe 0 2,ar5:2zCLCpCt2tomer Order No: Zd2c233--1 Lot No: ..-freir-741101PX0721/4131 7, 1" Analysis Analysis Description API Gravity CD 80 Deg F (ID 4052) Specific Gravity 60 Deg F (0.4052) LBSIGALIBO Deg F (C) 4052) Odor (D.1290) Colo( (0 156) Coke Pi/Co (D 1209) Copper Corrosion (0 849) Add Wash Color (0 848) Kafiri Wilmot Value (0 1133) Addlty (0 847) Acidity (0 847) (MOB) Sulfur (0 853) Water Contenl (E 1064) (ppm) ANSI' (G.C) Paraffins (GC.) (ppm) Benzene Content (0 C.) (ppm) Ethylbenzens Content (G.C.) (ppm) Xylem* (G.C.) (ppm) Xylenes & Ethylberasne (G.C.) (ppm) (Mediation (13850) Deg C initial Bolling Point Dry Point Total DIstiSaibn Range Refractive Index. 25 Deg C (0 1218) Appearance (Visual) Limits 0.859-0.873 20 max Pan 2 max 90 min No Free Acid Free 99.5 min 1.0 to include 110.5 NQIL THE ABOVE ANALYSIS WAS PERFORMED BY PITERTEK TESTING SERVICES, CALEB Me THE SAMPLE, AS TESTED. CONFORMS TO ASHLAND CHENCAL SPECIFICATIONS. Test Results 30.8 01718 7.260 Characteristic +30 Less limn 5 Pass 1140.9 No Free Add 0.115 Free 403 99.80 687.5 37.7 332.7 971.3 1304.0 109.7 110.7 1.4939 Clear and free of sediment endior suspended solids Intense 6September) 2003 Lab Ref. DOIMD-Dat -s prn al% .. NW 2 5 ( 0 c UT/ Ashland Distribution Company, Division of Ashland Inc., Box 2219, Columbus, Ohio 43216 SW-Scearce 01265 Nov 04 03 03:54p Laboratory 1sINIM 513-941-2174 Ashland Ashland Distribution Company Division of Ashland Inc. Customer Certificate of Analysis Customer illn d 0d 92. yr) & //We'd 36,0 Analysis Industrial Chemical & Solvents Division DATE: Novornbst 3, 2003 Product: TOLUENE aTank 4 Transmontaigne, New Albany, Indiana Ship Date: Ship Quantity: ' 4 '5 9 9' Sales Order No: le...oiop 157 519A- -- d do Customer Order No: l0 .2. 3 3 -- " Lot No: poi // ,,a, --4 3 Analysis Description Limits Test Results API Gravity C180 Deg F (D 4052) 30.8 Specific Gravity a 60 Deg F (D-4052) 0.869-0.873 0.8718 LBSKIAL.11313 Deg F (D 4052) 7.280 Odor (111298) Characteristic Color (D 158) +30 Color PtICo (D 1209) 20 max Less then 5 Copper Corrosion (D 849) Acid Wash Color (0 11411) Kaurl Bulanol Value (0 1133) Pass 2 max 90 min Pass 1- 100.2 Ad* (D 847) Aciciti(0547) (4017) Sulfur (0 853) Water Content (E 10841 (ppm) No Free Add Free No Free Acid 0.115 Free 403 Assay (GC) (%) 99.5 min 99.80 ParafBna (G.C.) (ppm) 807.5 Benzene Content (G.C.) (ppm) Ethylbenzana Content (G.C.) (ppm) 37.7 332.7 Xylenes (G.C.) (ppm) 971.3 Xylenes 8 Etbylbenzene (G.C.) (pm) 1304.0 Distlitetico (D850) Deg C Initial Bolling Point 102.7 Dry Point Total Distillation Range 1.0 to Include 110.6 110.7 1.0 Refractive Indix(1 25 Deg C (0 1218) 1.4939 Appearance (Visual) Clear and free of sediment andlor suspended solids rigul THE ABOVE ANALYSIS WAS PERFORMED BY INTERTEK TESTING SERVICES, CALEB ens THE SAMPLE, AS TESTED. CONFORMS TO ASHLAND CHEMICAL "SPECIFICATIONS. Ashland Distribution Company. Division of Ashland Inc, Box 2219, Columbus, Ohio 43216 SW-Scearce 01266 ASHLAND. Ashland Distribution Company Division of Ashland, Inc. P.O. Box 2219, Columbus, OH 43216 Customer Certificate of Analysis Customer. Shirwia Williams ComlawY Bone LatmSooth Richmond, KY 40475 Fax It: 614-7904424 Amu Deb Pfist (Ice's couirous) Analysis Test Method Appeanum Specific Gravity, gAnL 43601, Gravity,pounds/ Sayboit Color Pt / Co Color (APRA) Acid Wash Color Knurlautanot Vohs, Sulfur Compounds (MS, SO2) ppm Acidity Colmar Strip Corrodes Saturates, X Batmen% N Toluene, % Xylem, % > Xylane, % Initial Boiling Point, C Dry Point, C Dist. Range, C Water Content, ppm visual 0-091 Cale 0-156 0-1209 0-8411 0-1133 0-833 0-5453 0447 0-130/0491111311 0-2306 0-2306 D-2306 0-3306 0-2306 0450 0450 0450 Agnate. Shi Date: 2-2-04 Product: Toluene Tank Nix: 170 Ship quantity: 6459 ICAtS PO / Lot No.: Customer PO No.: Vessel: TOLUENE Ticked: 24019 Specification 0.069 to 0.073 report only report only 10 max. report only report only report only report only report only report oily 0.5 max. 0.03 imam 993 tali. 03 max. 0.5 max. 109.6 min. 111.6 max. 1 max. 500 max. Test Renato Clear liquid, hoe of particulate 0.171$ 7.260 30 3 On 105 Meg 0.3 Meg 1B 0.04 0.01 99.117 0.04 0.00 110.3 1104 0.4 170 Pass Pass Pass Pus Pau Pass Pass Pass Pass Pus Pass Pass Paso Pass Pass Pus Pass Pm Pass Pm 7.61. Anti-Elm added rel it 204 antis= suds& A Responsible Cue S-6 APPROVED 0ISO 3501:2001 Shipment do hinnithae Ashland Petroleum LLC. PO Sat 1492. Catienshur& Ky 41129, 606-421-6102 1711-91214 SW-Scearce 01352 Ashland Distribution Company Division of Ashland, Inc. P.O. Box 2219, Columbus, OH 43216 Customer Certificate of Analysis Customer: Sherwin Williams Company Bout if South Richmond, KY 40475 Fax al: 614-790-662411502-774-5631 Attn: Deb Nist (IC&S Columbus)/kevin Analysis Test Method Appearance Specific Gravity, g/mL 601? Gravity, pounds/gallon Saybolt Color Pt Co Color (APHA) Acid Wash Color Kauri-Butanol Value Sulibr Compounds (H2S, S02) Sulfur, ppm Acidity Copper Strip Corrosion Situ rotes, % Benzene, I Toluene, % Xylem., % > Xylem, % Initial Boiling Point, C Dry Point, C Dist. Range, C Water Content, ppm visual D491 Cale D-156 D-1209 D-848 D-1133 D-853 D-5453 D-847 D-130/84911838 D-2306 D-2306 D-2306 D-2306 D-2306 D-850 D450 D-850 Aquatest Ship Date: 212/04 Product Toluene 03- 1740 MIS 2300 Tank No.: 170 Vessel: TOLUENE Ship Quantity: 6720 Ticket IC&S PO / Lot No.: 45008579170430 Customer PO No.: 10233-re1204 Specification 0.869 to 0.873 report only report only 10 max. report only report only report only report only report only report only 0.5 max. 0.03 max. 99.5 min. 0.5 max. 0.5 max. 109.6 min. 111.6 max. 1 max. 500 max. Test Results Clear liquid, free of pardeulates 0.8713 7.260 2 On 105 Neg 0.3 Neg 1B 0.04 0.01 99.87 0.08 COO 110.2 110.6 0.4 170 Pass Pass Pass Pass Pass Pass Pass Pass Pus Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Anti-Stat added 360 ml anti out added s* ,01.0 MO AP D ISO 111111:29110 A Responsible Care Company Shipment do Marathon Ashland Petroleum LLC, PO Box 1492, Catlettstnos Ky 41129, 606-92 I -6802 SW-Scearce 01351 Ashland Distribution Company Division of Ashland, Inc. P.O. Box 2219. Columbus, OH 43216 Customer Certificate of Analysis Customer Sherwin Williams Company Botts Lane South Richmond, ICY 40475 Fax d: 614-790-6624 AMU Deb Nist (IC&S Columbus) Analysis Test Method Appearance Specific Gravity, glmL @CIF Gravity, pounds/gallon Saybolt Calor Pt / Co Color (API1A) Add Wash Color Kaurl-Butanol Value Sulfur Compounds (MS, sop Sulfur, ppm Acidity Copper Strip Corrosion Saturates, % Benzene, % Toluene, % Xylene, % > Xylene, % Initial Boiling Point, C Dry Point, C Dist. Range, C Water Content, ppm visual D-1191 Cale D-156 D-1209 0-848 D-1133 0483 0-5453 0-847 D-I301849/1838 D-2306 D-2306 13-2306 0-2306 13-2306 0-850 0-1150 D-850 Aquatest Ship Date: 2-26-4 Product Toluene 03-17-10 HMIS 2300 Tank No.: TK169 Vessel; TOLUENE Ship Quantity: 6623 Ticket 24574 IC&S PO / Lot No.: 4500874973-C3CO Customer PO No.: 10233-1 Specification 0.869 to 0.873 report only report only 10 MIL report only report only report only report only report only report only 0.5 max. 0.03 max. 99.5 rain. 0.5 max. 0.5 max. 109.6 min. 111.6 max. 1 max. 500 max. Test Results Clear liquid, free of particulates 0.8718 7.260 30 2 ON 105 Neg 0.2 Neg 1B 0.04 0.01 99.79 0.17 0.00 110.1 110.3 0.7 Pass Pass Pass Pass Pass Pus Pass Pass Pass Pass Pus Pass Pass Pus Pass Pass Pass Pus Pass Pass Anti-Stet added AN714TAT ADDED Shipment de Marathon Ashland Petroleum LLC, PO Bot 1497, Catlettsburg, Ky 4 1129, 606-921-6502 SW-Scearce 01350 ASHLAND Ashland Distribution Company Division of Ashland, Inc. P.O. Box 22i 9, Columbus, OH 43216 Customer Certificate of Analysis Customer: Sherwin Williams Company Boats Lane South Richmond, KY 40475 Fax N: 614-790-6624 Attn: Deb NIA (IC&S Columbus) Analysis Test Method Appearance Specific Gravity, g/mL Cg6OF Gravity, pounds/gallon SayboIt Color Pt / Co Color (APHA) Acid Wash Color 1Caurantanol Value Sulfur Compounds (H2S, SO2) Sulfur, ppm Acidity Copper Strip Corrosion Saturates, % Benzene, Talueoe. % Xylem', V. % Initial Boiling Point, C Dry Point, C Dist. Ranee. C Witter Content, ppm visual 0-891 Cale D-156 0.1209 13-848 D-1133 13-853 D-5453 D-847 13-130184911838 D-2306 0-2306 D-2306 0-2306 0-2306 D-850 13-850 D-850 Aquattst Ship Date: 2-27-04 Product: Toluene 03-17-10 HMS 2300 Tank No.: 169 Vessel: TOLUENE Ship Quantity: 6679 Ticket: 24590 IC&S PO! Lot No.: 4500874982-c3co Customer PO No.: 10233-2 Specification 0.869 to 0.873 report only report only 10 max. report only report only report only report only report only report only 0.5 max. 0.03 max. 99.5 min. 0.5 max. 0.5 max. 109.6 min. 111.6 max. 1 max. 500 max. Test Results Clear liquid, fres of particulates 0.8718 7.260 30 ON 105 Nee 0.2 Net 0.04 0.01 99.79 0.17 0.00 110.1 110.8 0.7 122 Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass s AntiStat added ANTI STAT ADDED!!!? z-1,516` 5c40 5'1' 59 APPROVED ISO 11081: 21011 A Responsib4e Care Company Shipment rho Marathon Ashland Petroleum LLC, PO Boa 1492, Citlettrhurg, Ky 41129, 606-921-6142 1/1-35234 SW-Scearce 01349 "SHLANICI Ashland Distribution Company Division of Ashland, Inc. P.O. Box 2219, Columbus, OH 43216 --r Customer Certificate of Analysis Ship Date: 3/2/04 Customer Sherwin Williams Company Bons Lane South Product: Toluene Tank No.: 170 03-17-10 HMIS 2300 Vessel: 8072 Richmond, KY 40475 Ship Quantity: 6496 Ticket: 24671 Fax 4: 614-7904624 IC&S PO / Lot No.: 4500878970-C3C0 Attn: Deb Nist (IC&S Columbus) Analysis Test Method Customer PO No.: Specification 10233-1 Test Results Appearance Specific Gravity, g,/ml. 04601r Gravity, pounds/gallon Saybolt Color Pt / Co Color (APHA) Acid Wash Color Kauri.Butanol Value Sulfur Compounds (H28,502) Sulfur, ppm Acidity Copper Strip Corrosion Saturates,'/. Benzene, 'V. ToWens, % Xyleoe, % > Xykne, % Initial Boiling Point, C Dry Point, C Dist. Range, C Water Content, ppm visual D-891 Cale D-156 D-1209 D-848 D.853 D-5453 D-847 11-130/1149/1838 D-2306 D-2306 D-2306 D.2306 D2306 11850 13-850 D-850 Aquatest 0.869 to 0.873 report only report only 10 max. report only report only report only report only report only report only 0.5 max. 0.03 nurx,,,, 9.5 0.5 0.5 1 6 pin, 1114 max. 1 inns. .7 500 max. Clear liquid, free of particulates 0.8117 7.260 30 2 IN 106 Neg 0.3 Nei 1B 0,05 0.01 99.82 0.11 0.00 109.8 110.6 0.8 186 Pass Pass Pass Pass Pass. Pas Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass s=7.111- Anti-Stat added A Responsible Care Company 5-9101 4 at 24 (67 2 Shipment c/o Marathon Ashland Petroleum LLC, PO Box 1492, Catlettsburg, Ky 41129, 506-9214802 TR-30234 SW-Scearce 01348 -A6111-111-ANID, Ashland Distribution Company Division of Ashland, Ina P.O. Box 2219, Columbus, OH 43216 Customer Certificate of Analysis Customer: Sherwin Williams ComPanv Bogs Lass South Richmond, KY 40475 Fax if: 614-790-6624 Attn: Deb Nist (IC&S Columbus) Analysis Test Method Appearance Specific Gravity, g/mL &OP Gravity, pounds/gallop Saybolt Color Pt / Co Color (APHA) Acid Wash Color ICsorl-Butanof Woe Sulfur Compounds (1128, SO2) Suitor, ppm Acidity Copper Strip Corrosion Saturates, % Bums, % Toluene, I Xylene, % > Xylem, % Initial Boiling Point, C Dry Point, C Dist. Rugs, C Water Content, ppm visual 0-891 / D-4052 Cale 0-156 D-1209 0-848 D-1133 D-853 0.5453 0447 D-1301849/1838 0-2306 D-2306 D-2306 D-2306 D-2306 0-850 D-850 0450 Aquatest Ship Date: 3-20.04 Product: Toluene 03-17-IC HMIS 230G-- Tank No.: 170 Vessel: TOLUENE Ship Quantity: 6783 Ticket: 25153 1Cdt.9 PO / Lot No.: 4500892310-e3co Customer PO No.: 10233-1 Specification 0.869 to 0.873 report only report only 10 max. report only report only report only report only report only report only 0.5 max. 0.03 mix. 99.5 min. 0.5 mac 0.5 max. 109.6 min. 111.6 max. 1 mu. 500 mat, Test Results Clear liquid, free of particulates Pass 0.8718 Pass 7.260 Pass 30 Pass 2 Pass ON Pass 108 Pass Net Pass 0.6 Pass Net Pass ID Pass 0.05 Pass 0.01 Pass 99.98 Pass 0.04 Pass 0.00 Pass 109.9 Pass 110.6 Pass 0.7 Pass 134 Pass .. Ami-Stet added ANTI STAT ADDED1111 A Reaponsible Care Company Shipment cJo Marathon Ashland Petroleum LLC, PO Box 1492, Catlettsburg, Ky 41129, 606-921-6802 SW-Scearce 01347 Ashland Distribution Company Division of Ashland, Inc. P.O. Box 2219, Columbus, OH 43216 Customer Certificate of Analysis Ship Date: 3/22/04 Customer: Sherwin Williams Company Product: Toluene 03-1740 HMIS 2300 Bow Lane South Tank No.: 160 Vessel: TOLUENE Richmond, KY 40475 Ship quantity: 6721 Ticket: 25184 Fax n: 614-790.6624 1C&S PO / Lot No.: 4500892306-c3co Attn: Deb Mist (IC&S Columbus) Analysis Test Method Customer PO No,: Specification 10233.1 Test Results Appearance Specific Gravity, g/mL ig60F Gravity, pounda/galion Sayboh Color Pt / Co Color (APHA) Acid Wash Color Kauri-Butanol Value Sulfur Compounds (HU, SO2) Sulfur, ppm Acidity Copper Strip Corrosion Saturates, % Benzene, % Toluene, % Xylene, % > Xylene, Initial Boiling Point, C Dry Point, C Dist. Range, C Wrier Content, ppm visual 0-891 / D-4052 Cale D-156 D-1209 0-843 0-1133 13-853 D-5453 D-847 D130/84911838 0-2306 D2306 0-2306 0-2306 0-2306 0450 0450 0-850 Aquatest 0.869 to 0.873 report only report only 10 mos. repora only report only report only report only report only report only 0.5 mss. 0.03 max. 99.5 min. 0.5 max. 0.5 max. 109.6 min. 111.6 max. 1 max. 500 max. Clear liquid, free of particulates 0.8718 7.260 30 2 ON 107 Neg 0.3 Neg lB 0.05 0.00 99.84 0.10 0.00 110.2 110.6 0.4 59 Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pus Pass Pass Pus Pass Pass Pass Pass . Pass Anti-Slat added APPROVED t4 ISO MI.: COOS it II A Responsible Care Company Shipment c/o Marathon Ashland Petroleum LLC, PO But 1492, Catlettsburg, Ky 41129, 606-921.002 rVI-311234 SW-Scearce 01346 Ft r 19 04 tot 113* L &dor :tar u 513-341-2174 .1 L.1.1.7hland Ashland Distribution Company Division of Ashland Inc. Customer Certificate of Analysis Industrial Chemical & Solvents Division DATE: Aprl 19. 2004 /PM N SNP Dan'1 /9 04 it , / Ship CtuentIty: _adAr Oisr ,--: !110 6 Sala* Order No: ie /9 Customer Order No: /O a 33 -- Lot No: indiana Analysis Description API Gravity 80 Deg F (0 4052) Specific Gravity 41) 80 Deg F (D-4052) LBSiGAU80 Dag F (D 4052) Odor (0.1298) Color (13 158) Color Pt/Co (0 1209) Copper Ccirosion (0 849) Add Wash Color (0 848) Kauai eulanol Value (D 1133) Addy (D1147) AddRY (Co 647) 0100/4) Sulfur (I) in) Water Content (61084) (ppm) Assay (G.C) (%) ParsMns (G.C.) (ppm) Benzene Content (G.C.) (ppm) Ethylbenzene Canasta (G.C.) (ppm) Xylenes (G.C.) (ppm) Xylem L EMylbenxene (G.C.) (ppm) Distillation (MO) Deg C initial Boiling Point Dry Point Total Distiliallon Range Refractive Index* 25 Deg C (D 1218) Appearance (Visual) Limits 0.13894,373 20 mu Pass 2 max 90 min No Free Add Free 99.5 min 1.010 Include 110.8 Test Results 30.9 0.8711 7.255 Characteristic +30 Less that 5 Pass 199.2 No Five Acid 0.023 Frye 220.0 99.78 460.2 40.0 440.4 12722 1712.8 1101 110.9 0.8 1.4941 Clew and free of sediment andke suspended solids MOVE OPULYSIS WAS PEUCRNED BY INTERTEN 'MISTING SUM& CALEB NETT. THE MOLL AS TESTED, CONFORM TO ASHLAND CONICAL SAECIFICA11001. 3"-/?--/ t Phoimmeelail-Carail , Campy. Ashland Distribution Corn , Division of Ashland lna., Son 2119, Columbus, Ohio 43216 SW-Sesame 01345 qa. 1 "" r a. [AgaVend Ashland Distribution Company Division of Ashland Inc. Customer Certificate of Analysis Industrial Chemical & Solvents Division DATE April 19, 2004 Custorner I) rznA 1/4 Product TOLUENE Tank 4 ft Trsnwncnta New MOW, Indiana Ship Date: it90d 41" 0 Ship Quantity: eo dv/Sales Order No: - Ar170-F Customer Order Na: fetz,z 3-4 icitma; .04z -- 4 O -- di Analysis Analysis Description Limits Teat Results API Gravity 0 CO Deg F (1) 4052) 30.9 Specific Gravity 60 Deg F (0.4052) 0.889.0.873 0.8711 LBSIGAU80 Deg F (1) 4052) 7.255 Odor (0.1296) Color (0 156) Characteristic *30 Color Pi/Co (0 1209) 20 max Less than 5 Copper Corrosion (0 849) Pass Pass Acid Wish Color (D 848) 2 rasa 1- Kauri Milano! Valuer (D 4133) 90 min 99.2 Acidity (0 847) No Free Acid No Free Acid AdditY 847) (i2) Sulfur (0 853) Free 0.023 Free Water Content (E 1064) (ppm) AWN (G.C) (%) 99.5 mkt 220.0 99.75 Preens (G.C.) (ppm) 480.2 Benzine Content (D.C.) (ppm) 46.0 Ethylbenzene Content (G.C.) (ppm) 440.4 Xylem (G.C.) (ppm) 1272.2 Xylem & Ethylbertzene (G.C.) (ppm) 17126 Distillation (DUO) Ogg C Initial Boding Point 4K 61455411966 4.44.1 Or/ Point 110.9 Total DIst2allon Range 1.0 to Include 110.8 0.8 Refrecthel index. 25 Deg C (ES 1218) 1,4941 Appearance (Visual) Clear and sediment suspended solids tom: THE ABOVE ANALYSS WAS PERFORMED BY MERTES revue SERVICES, CALEB BRETT. DIE SAMPLE, AS TESTED. CONFORMS TO ASHLAND CHEMICAL SPECIFICATIONS. IA sulk M i. , 9 /0 interMk Case Brett AM 19, 2004 Lab Rat 000147-001 11%s18 (Owl CaP1M Ashland Distribution Compiti on of Ashland Inc., Box 2219, Columbus, Ohio 43216 SW-Scearce 01344 =1. =r 19 04 10; 19a, Labor at oru [Ashl and 913-941-2174 Ashland Distribution Company Division of Ashland Inc. Customer Certificate of Analysis Industrial Chemical & Solvents Division DATE April 19, 2004 Customer dif 111111 ALA 411.1k Product TOLUENE Tank 4 T. a n New Ship Date: 2c0 Ship Quantity: Indiana aiiirSZW-47.026;11ir Customer 1101111,-- Lot No: "/ 'jib /tea Analysis Analysis Description LIMNS Test Results API Gravity 660 Deo F (Di 4052) 30.9 Specific Grisly *SO Deg F (D-4052) 0,869-0.873 0.8711 LBS1GAU60 Deg F (0 4052) 7.255 Odor (0.1296) Color 156) Characteristic +30 Color Pt/Co (0 1209) 20 max Less than 5 Copper Corrosion (0 549) Pass Pass Acid Wes& Color (0 645) 2 max 1- Mud Butenoi VIM (D 1133) Addlty co 847) 90 mkt No Free Acid 99.2 No Fist Add Addily (D 847) (WOO 0.023 Sulfur (D 853) Free Free Water Content (E 1064) (ppm) 220.0 Ant/ (aC) (%) Paraffins (G.C.) (ppm) Biome Content ((3.c) (ppm) 99.5 min 99.78 460.2 46.0 Elhylbanzene Content (GC.) (ppm) 440.4 Xylenee (G.C.) (ppm) 12722 Venom & Ethylbenxerte (G.C.) (ppm) 1712.6 DistMallon (0850) Deg C Initial Boling Point 110.1 Dry Rent 110.9 Total Distillation Range 1.0 to include 110.6 0.8 Refractive index@ 25 Deg C (D 1218) 1.4941 Appearance (Visual) Clear end tree of sediment and/or susconded solids NC= THE MOW ANALYSIS WAS PERFORMED BY INTERTEK TESTING SERVICES, CALEB BRETT. THE SAMPLE. Al TESTED. CONFORMS TO ASHLAND CHEMICAL SPEOFICATIONs. e tel,C. 6, 032- 0 a? l7 lel Caleb Brea LAri R"a't "00t041147-001 Ashland Distribution Company, Division of Ashland inc., Box 2219, Columbus, Ohio 43216 (6 SW-Scearce 01343 Ashland Distribution Company Division of Ashland inc. Customer Certificate of Analysis Customer: Stl cA sv,A.1 Wi LL 0-'3 3 9.5-- 40.19,0.5 1 Avve ..540 nCrh 4/4.14,1 o. rod 1.10 17s- $0,4 o oalremoloods 0 0,,4S"o ems r Iaarnisifir /7 /0 //r t/.0 e......44or 2 .70G Analysis Industrial Chemical & Solvents Division DATE: April 19, 2004 Product TOLUENE Tank 4 a Ilinsmcntalcol, New Mint lams Ship Data: e4/-2J --044 ship Quantity: G 3 ea Solos Order No: 4,/ roe 7/ 6 7 9a 4 Yee) Customer Order No; / a 2 3,7- Lot No: Analysis Description API Gordy 060 Deg F (0 4052) Spedlio Grin* SOO Ows F (D4052) LBSOALNIO Deg F at 4052) Odor (13-1251) Color (D1511) Color PVCo ID 1209) CORM Corrosion (1) 849) Add Wash Color (D lceud Bubmol VOW (D 1133) Addy (0 1147) AddlY(D 647) 0114,0 Sults ID 853) *awl lacyWaist Corded (E 1064) (ppm) (ik) Paraffins (GC.) (one Elanzsee Callan (0.C) (ppm) Ethylbenzene Content (o.C.) (ppm) Xylem (G.C.) (ppm) Xylsnes 1 ebylbsrusne (G.C.) (porn) 01:011otion (ONO) Oos C Inlilal Nang PoIrt Dry Point Total Oldham Rang. Reach* index. 25 Deo C (D 1218) Appearance (Visual) Limits 0.859.0.873 20 mu Pass 2 max 90 min No Free Add Free 99.5 min 1.0 to indido 110.8 Test Results 30,9 0.5711 1.259 Obaractsrlsk +30 Lisa than 5 Pass 199.2 No Fres Acid 0.023 Fres 99.79 4602 48.0 440.4 12722 1712.5 110.1 110.9 0.8 1.4941 Clear and sediment Impended .olds 100111 ANALYSIS WAS POMO= SY 1101MOS TESTING IERVICft ULM OREM MS WPM AS TESTED, CONFORMS TO ASHLAND CIIISICAL SPICIFICATIOSS. 14515 71 Cal 7 (7 " Apo 11 Cabb Omit Lab Rai ocommi, DI amk. 5441c. qr. 44A;0Aftsweigmb.... Asbland Distribution Company, Div*ision ofAiblsod Ina, Box 2219, Columbus, Ohio 43216 SW-Scearce 01342 41LiTwidan "4/7-s 5 rn. 513-941-?1 174 eid.ed I p. 1 Ashland Distribution Company Division of Ashland inc. Customer Certificate of Analysis Customer. _5 1, cow. 9,,r atfr er.5 5 0.evy,, 4", 40 75" /91 ,(01-4.4m-o .3 vo / Rra a.0.140 0 a 17 A7 Merl code0 2 lo Industrial Chemical IL Solvents DWIsion GATE AM 19, 2004 sssss=1.. Produd: TOLUENE Tank 4 II Trinsmonlairms, New AUK Indians SNp Date: co - 2 / -air/ Ship Quantity: Co 773- Ulu Order No: k/3 va 9i 6 7 Pe 3 e o CLoutstomer Order No / a140c 2 3.1 /..s,ssssssss-s......,sss Analysis Analysis Desalpdon Limits Test Results API &oily 0 60 Dag F (D 4052) 30.9 Spode Cirely 50 Dag F (0-4052) 0.559-0.873 0.5711 L13803AU118 F (13 4054 7.251 Odor (0-1290 Color (0 1581 C#3h0aradarisio Color PtCo (0 1209) 20 mu test than 6 Copper Corrosion (0 1149) Paso Pass Acid Mae Color (0 541) 2 man 1- K. al llutand Value (0 1133) 90 mkt 992 Add* / (D 847) No Res Add No Free Add Addtf 54T) (WOO suet (0 663) Weaw Content(8 4064) (ppm) Free 0.025 Free 220.0 Ault (MC) (.4) 99.5 mh 99.76 Psrallins (0.C) (ppm) 460.2 Baran, Content AC.) (ppm) 46.0 Elnytentene ConIM (A.C.) ( ,wn) 440.4 X)498.1(aq (ppm) Xylem & elytibaresne (0-.c.) (ppm) 12T22 1712.6 Oistilislise (D850) a9 C heal &Min Point 110.3 Dry Point 110.9 Total Dislialion Range 1,0 lo Include 110.8 0.11 Refracts, Mane 25 Deg C (0 1215) 1.4941 Appearance (Visual) Clear and sidtinoni andior suspended mMe IALlsOVe "Wan WAS PERFCOMED Wf MVOS TENTING Wm= CALB wry. pit Welt AS /EST CeNFONAS 10 MOUND CHINCAL SPOCW=710N11. Caleb Ome A94 19, 2094 Lab Rat 001147.001 As bland Distribution Company, Division of Aselaod lno., Box 2219, Columbus, Ohio 43216 SW-Scearce 01341 G7 =Ashland Ashland DIselbutIon Company Milan of Ashland Inc. Customer Certificate of Analysis Industrial Chemical 8 Solvents Division DATE AM ilk 2004 ACsutsitro/mI mere, ozca.) p2. r # PA, C.opropfro, Product TOLUBIE Tank 40 Tonsocitibis New 7.r *fr.y..s- Oozes k iafivrivg.19 so eev4- 4 af 7,- SliP 0111N Ottl"..":=-4 Shipauentity: 62 240 S1 cief, eonido 43 / 7 /0 iy. 0 1.r.s .2 ? a 6 Bela Order NoWro 090297.27 cyc c Custcaur Order No: /0,2 37-/. Lot No: Analysis r' Mr/ 1 fro.r /9,444() Analysis Dissolution API Gravay a 10 Deg F (D 4052) Speck Gamily SI 03 Deg F (04054 I-SWAIM 0i F (0 4052) Ode( (04294 Cola (D150) Color PVC* (D 1209) Copper Canada) (0 849) Add Week *kw (D 844 xeurl BuIanel Vitus ID 1133) Acidity (0 847) Acidttf 841) NOV Sulfur (D 853) Water 03nlint (I 1054) (son) Ms Parillfins (MC.) (ppm) amens ConIsni (0.C.) (ppm) Elnylbenzene Contort (OZ.) (ppm) Xylem. (G.c.) (ppr) Xylem' & ElhylbanasnanC.) (ppm) Olaaation (0150) Des C MI Bolling Palos Dry Point Total Oledladon Rave Ready, Index. 25 Dee G (0 1218) Appearance (Wual) UNDO 010-0273 20 num Pass 2 man 90 min No Free Add Free 99.5 rris 1.0 to IneLde 110.8 Test Results 30.9 0,1011 1255 awe:Seeds +30 Use ban 5 Nee 1- n.2 No Free Add 1023 Fro 221.0 MTh 4802 48.0 4404 17722 17121 1111 1101 01 1.4941 Clew end We d subset end& suspended molds THE A904 MAY= WAS PENC01110 OV ORM% MIMI =WU CAMS OREM MI Witt AS 71071D.CONFORMS 70 ASHLAND CHIMIAL IPICIFIrADON0, Caleb Ikell Ape 19, 2004 Lob Itie 000000111 , 11.4c4.01ss11s 111n Ashland Dloribution C.ornpanelvision of Ashland Inc., Sax 2219, Columbus, Ohio 43216 SW-Scearce 01340 Apr 19 l74 101 10s Laboratorw 513-94411174 p. ss1 Ash=and Ashland DIstrAwtbn Company Division of Ashland Inc. Customer Certificate CIJI1 (93-/7-1.0 r Val 23f) Analysis Industrial Chemical & Solvents Division OA Apd119. 2004 Product TOLUENE Tank 4 Ship Oa* die pa 4W "is CIrdw 146: 41149 90741712Y Colony Order Nos 40 12 33 Lot Mx dekel - et, -" 0 Ale trAff Ma Description Limb Teal Results API Gristly b 80 OW (0 4052) Spada Gra* GOO Deg F 034052) 0.869-0.573 30.9 0.8711 L88/0ALI6e Dee 1, (0 4052) 7.255 Odor (0.1296) Chsrecierialis Color (0 156) +30 Color PtiCo (0 1209) 20 max Lim Than 5 Copper Cenosias (0 849) Pao Pus Acid Wash Cake CO 641) 2 mu 1- Kousi Wheel Value (3 1133) 90 min 992 Athiai (0 347) No Free Aoki No Rwonid Addlt1 147) (AWN 0,023 Sulfur 553) Free Fr* Water Canted (E1064) (ppm) 220.6 AIM (G.C) (1) Porallins AC.) (ppm) 99.5 min 9175 4002 Benzene Ccelsni (0.C.) (ppm) 46.0 Eihylbencene Content (G.C.) (Pent) 440.4 XYinnoo(PO xvianes Eihylbersena (0.C.1 (ppm) 12722 17121 Disillalion (OM) Deg C Weal Meg Point 110.1 Dry Pain! 110.9 Total Diellalion Range 1.0 le lackide 110.6 Refractive Index. 25 Deg C (I) 1218) 1.4941 Appearance (Visual) Clear and he of sediment gnaw suspended solids tSUL THE A10%41 ANALYINIVIA9 PERIMIED WV PITMEN intim IlelnrCEI CAD MEM THE WIRE. All TEM COHPORDMI10 AMMO CHUM& OPECIM4110141. 4enti 11 Com. Ashland Dimension *se Awl tie, 2004 Lab net 000647.001 Division of Asians! Ina, Box 2219, Columbus, Ohio 43216 SW-Scearce 01339 Apr 19 04 101 11316 Labor atoibu 513-841-91.74 14". r.1 NIi/,nd AshlandDliklbution CompanY Division d Ashland inc. Customer Certificate of Analysis Oulomen 1.4/. ;1/41914,51. 3 e&F-6 24A49SO gef* AlCiefrks owe, /4. xjaii -7 5- -a.00440 1 / 7 /0 6.e0, 0,;r,s 2. 30 G Industrial Chemical & Solvents Division CAM Aprl 15, 2004 ProductTO--LIrff"-----Now ty. Jane Tank4 MP Otte airs- d de r adre Ship Quietly: 6, 2. 7 ? 3slaa War Ha: 41S a,g2G Y63 y c o Customer Order Na / a 2 3 Lot Not Analysis Analysis Deacripdon Test Results API Gravity a SO Dig F (0 4052) 20.11 Spec& Gm* (1110 Deg F (04062) LELS/GALAIO ass F (D 4052) Odor pine) 0.34194.513 01111 7.2511 Chwadscisk Coke (9 155 Color Pits 33 1205) 20 mu Las then 5 Cop)* CISP*011 ID 044 Pus Pus Acid Weak** (I) 54&) met 1- *ail Island Vika (D 1133) 93 MIA 992 Add*/ (D $47) No Free Add No Frog Add Ada, (3)0laP) O* Sues en) 0.023 Fria Wally Como (E 1054) (ppm) AAssh (G.C) Paraffins (9.C.) (ppm) Symms OWNS (o.c.) (ppm) 9 .5min 220.0 454 9A pnple-ii 00 Elliyibsreans Contra AC.) (ppm) 440.4 Xylanas (G.C.) (ppm) 12722 Vann & glialbsnisns (G.C.) (ppm) 1712.0 Dlatlls0on (0550) Dq C Initlai Boffins Point 110.1 Dry Pon* 1101 To Olsallation Range 1.0 is include 110.5 03 Reiman ladss. 25 Daa C (Dula) 1.4941 AN:smarm (Wu* Clumi and midlevel indict ausimnded Tthealnl;ow AMMO= WAS PERFORMSD INTIM= MONS =VICES, CAWS ISM Die MOLL AS TOMO, CONFORMS 70 AMMO COMM, SPIOMATICRIL aj, r slais Cori Omer. Unhand Ap1111, 2004 Lib Rit 000147.001 Ashland Distribution Company, Diviaioa of Asbland Ina., Son 7219, Columbus, Ohio 43216 SW-Scearce 01338 Rpr- 19 04 lOtISa Laboratory SI3-341-11747- .14T-- rs. Ashland DIsirlbutIon Company Division of Ashland Ina Customer Certificate of Analysis C:usto I. CALAPenfola? 194 -- /0 Industrial Chemical & Solvents 0A11:Porl 19, 2004 Product TOLUENE Tank 4 Ship NE ee Ship OA*: el ,ge) Sates wit Ne44.9166024o1/ Customer Ordst Na /401A a A -- Analysis Description AP1 Grally 80 Ose F (0 4052) Spodtio Gra* a SO Dos F (0-4052) LasioAueo Des F (n 4052) Odor (04294 Color (0 158) Color Ft/Co (0 1209) Copper Carob, (0 849) Add With Color (0 $48) ksud Bulanol Value (0 1133) Acidity (0 847) Matt (0 847) (lkiscirag) Suitor 853) Wats( NNW (E 1064) (ppm) mum (o.c) Paraffins (0.C) (ppm) Germane Content P.C) (ppm) Elhylasozano Content (0.C.) (ppm) xylaoss (G.C.) (ppm) Xylonss & Ethylbonuno (0.C.) (ppm) 015Olailoa (0650) Dos C Mt Doing Pokd Ory Point Total Oistliation Range &drachm, India 25 Deg C (0 1215) Appearance (Visual) MIL THE A30'4 ANALYIPS WAS TSII IAMPLI. AS MITA Umits 0.869.0.873 20 ma Pass 2 max 90 min No Rao Add Free 99.5 mei Test Results 30.9 0.8711 7.258 Chorschstalls 30 lass Than Pass 1- 992 No Fran Acid 0.023 Erse 220.0 95.73 150.2 460 440.4 12712 1712.5 1.0 to Include 110.5 110.1 1101 01 1.1941 Cloy end free of sediment andior stnpendsd sopds CAJIII Inn non, nowdobb for Cwww Ashland Disiiilastion Company, Division of Ashland ins., Boa 2119, Columbus, Ohio 43216 l c M2 SW-Scoa roe 01337 Apr 19 04 1t7: 18s Laboratory 513-941-2174 I Ashland rAshlan nDistrriibbuuttion Company Division of Ashland Inc. Customer Certific of Analysis industrial Chemical & Solvents Division DATE: April 19, 2004 Cu 5HI5 ..-fziwr.aarAcatii Analysis Product: TOLUENE Tank 4 Traromonta Ship Data: k_ 41, New Ship Quantity: Wei Order No: WI Customer Order las7 3 -5 - I Lot No; -atf et, J. PM LP 1:4 WI 'A/WMCR 1.1 Indiana Analysis Description Limits Test Results API Gravity 000 Deg F (D 4052) 30.9 Specific Gravity 80 Deg F (D-4052) 0.8694.873 0.8711 LBEVGAU60 Deg F (0 4052) 7.255 Odor (13-1296) Characieristic Cabo (D 156) Color Pt/Co xi 1209) 20 max +30 Less than 5 Copper Canniest (D 649) Pais Pass Mid Wash Color (13 648) 2 max Knurl &Anal lido (0 1133) 90 min (D 847) No Free Add No Free Acid (0 847) NOW Sulfur (0 853) Free 0.023 Fret Water Contend (E 1064) (ppm) 220.0 Assay (G.C) (%) Paral5ns (G.C.) (ppm) 99.5 min 99.711 460.2 Benzene content (MC.) (ppm) 46.0 Ethytoenzene Content (G.C.) (ppm) 440.4 Xyleries (B.C.) (porn) 1272.2 Xylem, Eitybotione (G.C.) (ppm) 1712.6 Dialliation (D450) Deg C Initial Boiling Point 110.1 Dry Point 110.9 Total Negation Range 1.0 to Include 110.6 0.8 Refractive Index() 23 Deg C (D 1216) 1.4941 Appearance (Visual) Clear end tree sediment suspended 1831g THE ABOVE AMM.Y815 WAS FERO:MEV SY Pef.R1EK TESTING SERVICVL CALEB NETT. THE &AMPLE. AS TESTED, CONFORMS TO ASHLAND CHEMICAL SFECIRCATICtit 5 /vt e 40406 Caleb LIU AM 3, 2004 Lab Rat 000447-001 iftwimmlab Cove. Gown" Ashland Distribution Company, Division of Ashland Inc., Bon 2219, Columbus, Ohio 43216 SW-Scearce 01336 Apr 19 04 los lea Labaratory 51 3-34 1 .-- 04r:-.1.1651- . "--A1-1s111h-11land Ashland Distribution Company Division of Ashland Inc. Customer Certificate of Analysis Industrial Chemical 8 Solvents Division DATE: Awl 19, 2004 Customer Order No /nA s Lot No: .11 --4471M111111M 7177Allreilf, MEOW" .! Analysis Analysis Description Limits Test Remits API Gravity 41 60 Dog F (0 4092) 30.9 Specific Grayly 60 Deg F (0.4052) 0.6694573 0.6711 LBS./GAM Deg F (0 4052) 7.255 Odor (0.1296) Color (0 156) CharsciadaLlo 4.30 Color PVCo (0 1209) 20 mu Uise than Copper Cccroslon t0 649) Add Wash Color (0 641) Pus 2 mu Pus 1- Knurl Butarxi Vain, (0 1133) 90 mln 99.2 Acidly (0 547) No Free Acid No Five Add Patty (D 847) (Montag) 0.02$ Sulfur ID 853) Free Frsa Waist Cogent (E 1054) (ppm) 220.0 Assaf' AC) (%) Paraffins (G.C.) (ppm) Benzine Contort (G.C.) (ppel) Eihylhenzene Contort (0.C.) (ppm) Xylem (0.C.) (ppm) Xylem. I Elhylbormono (Gt.) (ppm) 0111111stlon (DUO) Deg C 99.5 min '1 st? t/1151 99.76 4602 46,0 440.4 12722 1712.0 Initial Bang Point 110.1 Dry Point 110.9 Total gallon Range 1.0 IO include 1101 Refractive Inflow* 25 Deg C (01218) 1.4941 Appearance (Visual) Clear WI's@ of sedlmsnt mutter swindled scads NIL rne Allow won WAS PWcIWED Irr INTERWATIStete stiterott cull 'Krt. nio TI ono. CONFORM 70 /4/41.M0 OCANCAL 1104COICA ss 400 C/1 Ashland Distribution Company, Division of Ashland Ino., Box 2219, Columbus, Ohio 43216 SW-Scearce 01335 --- Ror 19 0 10s 19 Lalsorater 51 3-94 1 '-12.747-411- Ashland Distribution Company Division of Ashland Inc. Customer Certificate of Analysis Dustvw A A.,2/ Ltit--vvidd industrial Chemical & Solvents Division DATE Apel 19, 2004 Produch TOLUENE Tank 4 A ship Ws: 7, 713 I AKIkke2 le I Analysis Customer 0 uN: /(9.2 Lol No: s / Analysis Description API Gravity 80 Oap F (1) 4052) Specific Gravity 0 SO Ova F (0-4052) LBSMAU50 Ogg F (0 4052) Odor (0.1290) Color (D 150) Color PVCo (D1209) Copper Corrosion (0 549) Add With Color (I) 045) Mut Selina Vitus (01133) Acidity (0 $47) Litnits 0.5594.173 20 runt Pus 2 max 90 mkt No No Acid Test Results 30.1 0.1711 Ian Charedeetado 30 Less than 5 Paso 1- 98.2 No Fri Acid AddItY (0 Kr) ()dicing) SAN (0 053) water Content (E 1054) (ppm) Maw (0.0 (%) Paraltins (G.C.) (ppm) Bowe Content (G.C.) (ppm) Eihylberaene Content (D.C.) (ppm) xylenos (G.c.) (ppm) Venn. Ettlybenzeos (G.C.) (porn) oiselatica (DUO) Dee C inaist WIN Point Pry Point Total Oissitstion Range Refractive index* 25 Deg C (0 1218) Appearance (Vises') Free 99.5 min 1.0 to 'Mode 110.5 0.023 Free 220.0 99.71 480.2 45.0 440.4 1272.2 1712.1 110.1 110.9 0,5 1.4941 Clear and flee of sediment indict suspended solids rrNs SA=SCNI AML.TISS WAS PERFCRIAED SY WTERTESIvniNG IIIDEVICSA CAB SNIT. 1141 sAmPtE, Al TESTED, COMMA TO AMMO CHEMICA. ErCIFICATICSIK Caleb BM Apri 10,2004 Lib Rot 000347.001 14 Ashland Distribution Company, Division of Asbiaod Ina, Box 2239, Columbus, Ohio 43215 SW-Scearce 01334 Ba Labareto .rts 513 --1141.-134-47.-1.43-r r1 Ashland Ashland Distribution Company Division of Ashland inc. Customer Certificate of Analysis Industrial Chemical & Solvents Division DATE Aprl 19, 2004 pP Sates Omer Order Ho; ,aef.., A p est C:7 93,e2 s4 / Customer Order No: /0.2 3 3 - Lot No: Analysis Description API Gravity 00 Da; F (0 4052) SPKtlic Gravity 60 Deg F (0-4052) 1.11SiGJILI60 Deg F (0 4052) Wu (01298) Color (0 155) Color PtiCo (0 1209) Copper Corrosion (0 549) Acid Wash Color (054$) Kw' Buiancl Yaks (0 1133) Acidity (0 847) AcktitY 947) PEN/ Sulfur (0 553) Waist Content (E 1044) (poo9 AU,/ (0C) (S) Paraffin. AC.) (ppm) 9ortzene Ccellaat (0.C.) (ppm) Ethyibeitions Content 10.0 (ppm) Xylem (G.C.) (ppm) Xylem* & Ektylbortune (G.C.) (ppm) Otstkation (0950) C Mal Bolling Point Dry Pohl Total olsciation Range Reirsetive Nese 25 Deg C (Cl 1218) Appearance (Viso* Limits 0.559-0.573 20 max Pus 2 ma 90 min No Free Acid Free 93.5 Mn 1.0 to Include 110.0 Test Results 30,9 0.5711 7255 Characteristic .30 Leas terms 5 Pus 992 No Free Add 0.023 Frs. 220,0 19.711 460.2 45,0 440.4 12722 17123 110.1 110.9 0.11 1.4941 Clear end he of sedIrnsat inciter suspended solids The ASOVE ANALY11111 WAS PERFORM, 11Y PirV17131Tesmo owl= can IinE17. THE &AUKS Al TESTED, COMMONS TO ASI.A140 CHIMICAL SPICSICAllOPM Cobb Brad AM is, am Lab Rst 000847-001 -- Dr.ALS- ,4%,_ Ashland Distribution Company, Division of Asblind Ina, Box 2219, Columbus, Ohio 43216 s Cbr Cr..* 1111W SW-Scearce 01333  Loberstoru S 1 3 -1343- -17717-!tr. Ashland Distribut)on Company Division of Ashland Customer Certificate of Analysis Cus industrial Chemical & Solvents Division OATE Apt 19, 2004 Product TOLUENE r.. 0 -- A9 Omer 417 2P21; ass AO lomat Ai . L1 ": 0 IFAINM:75 ArriffifrAKW121-7, A I IC TIZAMSregr i Analysis Analysis Deaa1ption Limits Test Results API &oily 41 80 Deg F (0 4052) 30.9 Spsdfto Gravity p 10 Deg 140-4052) 0.819-0.1113 0.8711 1.8.51GAU80 Deg F (0 4052) 7.255 Odor (134298) Cabs (0 151) CharackelsOs +30 Color Ms (0 1209) 20 mess Lase Ws Copper Ccerosice ID 9419 Pisa Pus Add Wish Color (0 IA 2 ma 1- Ksuri Behind Vain (01133) 90 min 992 Pally (D 84/) No Free kid No FresArid Ado/ (0 OM 041062) SUM (0 353) Waist Coolant (E 1084) (ppm) Ftee 0.23 Free nes mull (MC) (%) Pareirins (G.C.) (ppm) 8MUM Canine (0.C) (ppm) Eihybensene Coolant (3.C.) (ppm) Owes (0X.) (ppm) xoers S Etsybereens (G.C.) (ppm) 994 min 4802 48.0 440.4 12722 17121 DIsUbion (01150) Dog C brae Boling Point 110.1 DIY Palm Total Obillelion Range Refractive Index. 25 Dog C (Q 1219) 1.0 le include 110.9 110.9 0,0 1.4941 Appearance Visual) Clsu mei Erred sediment satifor :winded scads niitelimiLove mouse WAS FOUCIWINDIV KIM% 'TIMMWeetelAtAUS mot The ekuPle, AS Term coseciais Aliee40 CHINO. IFECeneAlgie. Camber* API 19, X01 IA Mt 000147-001 Addend Distribution Company. Division orAsidand Inc., Slott 2219, Cokenbus, Ohio 43216 ' SW-Scearce 01332 Flpr 13 04 201 ISM; Laboratory ',17407 =shlarrt 513-8411174 04...0( P1 Ashland Distribution Company Division of Ashland the. Customer Certificate of Analysis Customer. 509rA Av* 39-re000.2.4wo "hienamo sa4e.r4 ,,deo /7-;/4,,.." amiso -7,jarc Industrial Chemical & Solvents Division DATE Awl 1% 2004 Product TOLUENE Tank 4 a Trinsincntalona, **Albany. Indians Ship Ds* of--,q9---0 41 er/i. SNPOmar saw Order No: iii3/24,9*#41.1171 Customer Order No /45. Lot No Analysis An alysis Dssception Limits Test Results AR Gravity 90 Dag F (0 4052) 30.9 Spade Gravity 0 CO Dp F (0.4052) LOS/GAL/50 Dog F (0 4052) 0.8694.873 0.6711 7.255 Odor (01298) Chametsrtsda Color (0 155) +30 Color PVC* (0 1209) 20 max Lass than 5 Copper CC4104100 (0 549) Pan Pass Add WWI COW (D 1148) 2 man 1- Kiwi &Sand Vitus (0 1133) 93 min 992 Melly (0 547) No Fr Acid No Fms Add Acker/ (0 NT) WINO Sulfur (0153) Fres 0.023 Fm* Walse Carte* (E 1054) (ppm) 220.0 (0Z)(%) Paraffins (043 (WI) 99.5 min 9936 4502 Samna Content (G.C.) (ppm) Ethylbantans Conlon' (G.c.) (ppm) 45.0 440.4 Xylem (G.C.) (ppm) 1277.2 Xylenos Elhylbsrmsno (C.C.) (ppm) 1712.5 Disellation (0850) Cleo C Initial Meng Point 110.1 Dry Point 110.9 Total Olsellation Rangy 1.0 b Include 110.0 0.1 Relmcdve Incluse 25 Dap C (0 1218) 1.4941 Appearance (Visual) Clew and free of ssdimsol and/of suspended sonde MIL THE MOVE NI/J.Y513 WAS pIRFORNED SY INT001017531190 ISAVICZO.C51.15 MEM THE N lapis. Al TESTED. CONFORM/ TO WWI CADSCAL SPEOPICJOKNO. i tP 404 C=MOWN Caleb lime Api 19, 2004 Lab Rot 000147401 Ashland Distribution Company, Division of Asblund Ina, Be* 2219, Columbus, Ohio 43216 SW-Scearce 01331 .ArILANID. Customer Certificate of Analysis Ashland Distribution Company Divioloo of Ashland, Inc. P.O. Hose 3219, Columbus, OH 43316 16.10.04 Pao #: Analysiss 190424 cal rte}) Ton Method Appear' & Gravity, eini. Crow*, patois/plias SayboN Color Pt Co Color (AMA) Add Waal: Color Kaorlantasol Valus Suffer Coapouvids (1123, SO2) Shalfor, ppm Acidity Copper Strip Corrosion smarmy% la. Seaman 114. Tamale, it X3.101 % Xylem., % Udell Soiling Post, C Dry Pout, C blot. Roam C Weber Coldest, ppm visual D-1191 10.4003 CIO D-1514045 D.1200 D44* 131133 0403 D-6453 .13-047 D4301149111311 D-2304 D.3306 04306 12.2306 0.2306 0451 D-150 D.I50 Aquatint Shim Questityi 35M Tick* latti POI Lot No.: 4501195151.a.cnt PO No.: 10233- Sicoificalas 040 to WM report only report oily 10 non moon only report oily report only Mon onlar mon MY report only as mos. 0.03 man 95.6 min 0.9 MUM 0.5 man 109.6 1114 Nan 1 non 500 mu. Tuft Raub Chow 1140sid, Are* it pordoelateo 047111 1.149 30 2 ON 109 Nog 0.0 Neg IR 0.04 0.0S 99.93 0.01 0.00 HILS 1194 .511 . Pow Pass Pats Peas Pam Poo Paso Pus !nu' Pali Pea Pam Pau Pea" Pau Paso Putt Pisa Pus Pus ianWitit MEW A Reepoodbierase Gayety 5-1"1-0k ( 6 .1 Mows ea Mambas AshkodPoreletor LLC, PO Dm 34901 Ceassiberp, Kr/ 4112P, 0064214100 rn m_11 rig," T 1t Nr..1 If.14 . M en nn inn 16 1,017 InT inn SW-Scearce 01330 ALANIX Ashland Distribution Company Division er Asblesd, roc. PA. Boo 22111. C011010111, Oil 43216 Customer Certificate of Analysis Ostontss illasts Ship DEW 044304 Product. Tassels "dm 03110 1000 220G , Kan lase Bose Tank 1410.z 170 Wash GAT7L-53901 Ildorspi. KY 40175 81310 ::otite_ 24712 Ticket Put 0: 4141-7241-0024 wadi PO J Lot )104 45901451.043C2C0 Aft: Deb Nisi Analysis C40113101111 Tod Mcibtel Asoasrsss alumnae Gmily. give. 4001 amity. pessisegalise *phial Oder Pt f co Color (ainLV Acid Wash Cele, Kesti-Detnnsi Yoko Sulfur Camps, ado (1123,1103) Stilfar, ppm, Middy Comer Strip Corrosion Silvana, % Yroassak % 717101016 Itylimpo.% WWI Dallirad PHA C Dry Mat, C Dist. Panne, C Water Cutest, pm Anal D-119110.4032 Cski D456/6041 11-1200 044$ D-1133 D-OS3 1344113 0447 130/149/111311 D2306 043411 11`3300 12-23416 0-2306 D-000 0400 Armies* Cussareir PO 14o. Specie:odes 0360 to 0.273 report only mere orribr 10 mum. revert only revert emir Plot oa1 report saw report oily retort WY 03 was. 043 eon. IL 0.$ insx. 0.0 emu 100,4 eds. 111.4 mom. 1 IDOL 501 mu. T4 itresatte Clear thrw fts et prOadaus. 6a7111 7.2611 30 2 On 100 Nog gut Nog 13 0.00 Not Seises* 90.04 040 110.0 110.4 9.1 412 Post Pao Pus Per PIN PUN PIN Peps Nap Pass Pus Pew Pun PIN Pus PUS Pass Pane Puss Pass Aati-5111addeil A itteletasilis Cars Comm tokliTO 39Vci 57JI 1311U1Et 30-V01041 L9906a719 EiVgl O08Z/SI/9O SW-sceerce 01329 Ashland Dbtribatin C0114111111 Division of Ashland, in& P.O. Du 2219, 0310016001 OH 43216 Customer Certificate of Analysis WIIIIIMENInnoll110s11M1111111M.s1. Ship Daan 04-1444 03-17-1 taa SDOG ..sssMMMIIMrnAlaIL&EPAIEIIL ss....Mm..s..IMsssww Inds Dad. Tack Ns.: 170 Sitio OutritiW: 24764 QA777074 Tick* Pax Or 614-199-424 Inadt Po / Lot No.k Attn: NI Analysis Col Test Method Custom" PO No.: Specification Tad Ratans A peartere SPecilk Gravity, *NIL SW Gerrity, peosasioelleo Sorban Color Pt/ Co Color (AMA) Add Wank Color KaarHletanol Vales Sulfur Catoptends 024 902) &afar, PPE Acidity CORM Strip atirellISO 0otioso400p % Doom* % Totems, A Mu% % > Use% % ldlbl Dediati Pub*, C Thy Point, C Dist. Roam C Water Contost, ppm vteusa D431 I D-4021 elk D-156/4148 114205 D-148 D1133 D4S3 D-4453 D647 D-130/849/11131 13-13041 D4304 D-2324 D-33011. 1`130` 04341 Dan D430 Mesta* -MA iC f 1119 h." AY' W ks' /714 WNW to 0373 mot Doty main only Ift our& Mori 00IY report eel, report oidp report onkr rePort 1111041 0017 0.5 sag. 0.03 saw . ra.4 maw 0.1 ma& 0.8 ow& 101.11 who. 111.4 MIN& 1s SOS sao. if rt g ow -1-4 Cher avoid. *so of pordsodolom Poso 9.37111 Poor 7.260 tea 30 Pap 2 Pant 0a Pass 304 Not P.. 0.0 pi. Nag Past 13 Peet &OS Page Not dowels 90.34 P.. 0.00 Pass torvi PP,0.00 1111.8 ILLS 52 Peer 11 ma'am addod Ilop000kis Cy; compote ti0 /Ect 39'dd APPICAR0 In so srN Meow estP4tremea Maid Teirolowo 11C. PO flat 1191. Oratombeen Ky 41129 6049214403 Idel 417.z1/111611 51.31 CINOlifold PZ9906L015 115) ME-301 0002/5T/90 SW-Scearce 01328 ASHLANCI, Ashland Distribution Company Division of Ashland, Inc. P.O. Box 2219, Columbus, OH 43216 Customer Certificate of Analysis Customer. Sherwin Williams Company Bow Lane South Richmond. KY 40473 Fax *: 614.790-6424 . Mtn: Deb Nbt (IC 1S Columbus) Analysis Teat Method Appearance visual Specific Gravity, ghoL WOW D-891 I D-4052 Gravity, pounda/piloo Cale Saybolt Color 11-15616045 Pt / Co Color (APHA) D-1209 Acid Wash Color D-845 1Cauri-Butanot Value D-1133 Sulfur Compounds (HIS, SO2) D453 Sulfur, ppui D453 Acidity 11-847 Copper Strip Corrosion D-130/349/1831 Saturates, % D-2306 Hosszene, % D-2306 Toluene.% D-2306 Xylem % D-2306 , Xylem, % D-2306 Initial Boiling Point, C 0-850 Dry Point, C D-850 Dist. Range. C D-1150 Water Content, ppm Aquatest Ship Date: 8/24/04 Product Toluene C., 03-17-10 Tank No.: 170 Vessel: 6001 Ship Quantity: 6542 Ticket 28642 IC&S PO / Lot No.: 4501005062-C3C0 Customer PO No.: 10233 S 2300 Specification 0.869 to 0.173 report only report only 10 max. report only report only report only report only report only report only 0.5 mu. 0.03 man. 993 min. 0.5 max. 0.5 mat, 109.6 min. 111.6 mas1 max. 500 max. Test Results Clear liquid, free of porticulatee Pass 0.8715 Pass 7.260 Pass 30 Pass 2 Pass ON Pus 104 Pass Nee Pass 0.1 Pass Neg Pass 1 a Pass 0.06 Pass Not detected Pass 99.94 Pass Not detected Pass 0.00 Pass 110.5 Pass 1104 Pass 0.1 Pass 32 Pass ( 12 - Anti-Sus added 360ns1 of ANTI STAT ADDED A Responsible Cam Company Shipment do Marathon Ashlanu Petroleum LLC, PO Bon 1492, Catlettsburg, icy 41129, 605-9214802 ru-90194 SW-Scearce 01327 ASHLANC). Ashland Distribution Company Division of Ashland, Inc. P.O. Box 2219, Columbus, OH 43216 Customer Certificate of Analysis Customer. Shamir; Williams Company Bow Lane South Richmond, KY 40475 Fax #: 614-790-6624 Attn: Deb Mat (IC&S Columbus) Analysis Test Method A ppeorenee Specific Gravity, giniL 4g6011 Gravity, pounds/gallon Saybeit Color Pt! Co Color (APHA) Acid Wash Color Kauai-Batumi Value Sulfur Compounds (H2S, SO2) Sulfur, ppm Acidity Copper Strip Corrosion Saturates, % Benzene, % Toluene, % Xylone, % > Xylem, % Initial Boiling Point, C Dry Point, C Dist. Range, C Water Content, ppm visual D-8911 0-4052 Cale D-156/6045 D-1209 D-848 D-1133 0-853 D-5453 D-847 D-130/849/1838 D-2306 D-2306 D-2306 D-2306 D-2306 D-850 D-850 0-850 Aquatest Ship Date: 8.27-04 Product: Toluene 03-17-10 HMIS 2300 Tank No.: 170 Vessel: TOLUENE Ship Quantity: 6522 Ticket: 28708 !CM PO / Lot No.; 4501035084-c3co Customer PO No.: 10233 Specification Test Results 0.869 to 0.873 report only report only 10 max. report only report only report only report only report only report only 0.5 mu. 0.03 max. 99.5 min. 0.5 ma:. 0.5 max. 101.6 ml.. 111.6 max. 1 max. SOO max. Clear liquid, free of particulates 0.8718 7.260 30 2 On 104 Nee 0.1 Neg 18 0.07 Not detected 99.93 Not detected 0.00 110.4 110.6 0.2 61 Pus Pass Pass Pass Pass Pus Pass Pus Pus Pus Pass Pus Pus Pass Pass Pus Pass Pass Pass Pass dig ova- 3 10 Ants-Stu added ANTI STAY ADDED!!! D A Responsible Care Company Shipment de Marathon Ashland Petroleum LLC, PO Box 1492, Catlettsburg, Ky 41129, 606 -911 -6502 me-31234 SW-Scearce 01326 ,ASHILAIVEL Ashland Distribution Company Division of Ashland, Inc. P.O. Box 2219, Columbus, OH 43216 Customer Certificate of Analysis Customer Sherwin Williams Company Bons Lane South Richmond. KY 40475 Fax #: 614-7904624 Alen: Deb MU (ICaS Columbus) Analysis That Method Appearance Specific Gravity, g/taL @OOP Gravity, pounds/gallon Saybolt Color Pt I Co Color (APHA) Acid Wash Color ICauri-Butaitol Value Sulfur Compounds (H29, SO2) Sulfur, ppm Acidity Copper Strip Corrosion Saturates, % Barcena, % Toluene, % > xybae, % Initial Boiling Point, C Dry Point, C Dist. Rouge, C Water Content, ppm visual D-841 / D-4052 Cak 0-156/6045 D-1209 0-8411 D-1133 0453 D-5453 D47 0430/849/11138 0-2306 D-2306 D-2306 D-2306 D-2306 0-85$ D-850 0-850 Aquatest Ship Dinvx 8-2744 Product: Toluene 03.17-10 MIS 2300 Tank No.: 169 Vessel: TOLUENE Ship Quantity: 6495 Ticket 28720 IC&S PO / Lot No.: 4501007859-e3c0 Customer PO No.: 10233 Specification 0.869 to 0.873 report only report only 10 max. report only report only report only report only report only report only 0.5 max. 0.03 inns. 99.5 min. 0.5 max. 0.5 max. 109.6 min. 111.6 max. 1 max. 500 mos. Test Results Clear liquid, free of partleulsta 0.5718 7.260 30 2 ON 106 Nag 0.1 Nei 1B 0.07 Not detected 99.92 0.01 0.00 110.4 110.6 0.2 Pus Pass Pass Pass Pass Pass Pus Pus Pass Pass Pass Pau Pass Pass Pass Pass Pass Pass Pass Pau 4 Sam E 674Eintit Anti-Stet added ANT1STAT ADDED gIC A PPROVED A Responsible Care Company Shipment do Marathon Ashland Petroleum LLC, PO BOK 1492, Catlettsburg, )Cy 41129, 606-921-6002 SW-Scearce 01325 omm.1ss ASHLAND. Ashland Distribution Company Division of Ashland. Inc. P.O. Box 2219. Columbus, OH 43216 Customer Certificate of Analysis Customer. Sherwin Williams Company Bonus Lairs South Richmond, KY 40475 Fax #: 614-799-6624 Attn: Deb nit (IC&S Columbus) Analysis Test Method Appearance Specific Gravity, 8/mL 6t60F Gravity, pounds/gallon Sayholt Color Pt / Co Color (APHA) Add Wash Color Kanri-Butanol Value Sulfur Compounds (1125, SO2) Sulfur, ppm Acidity Copper Strip Corrosion Saturates, % Benzene, % Toluene, % Xylem., % Xylem % Initial Boiling Point, C Dry Point, C Dist. Range, C Water Content, ppm visual D-891 I D-4052 Cale D-156/6045 D-1209 D-8411 D-1133 D-853 D-5453 D-847 D-130/849/11138 D-2396 D-2306 D-2306 D-2306 D23116 D-850 D-851 D-850 Aquatest Ship Date: 8-27-04 Product Toluene 03-17-10 HMIS 230G Tank No.: 170 Vessel: TOLUENE Ship Quantity: 6317 Ticket: 28703 IC&S PO / Lot No.: 4501005979-C3C9 Customer PO No.: 10233 Specification 0.869 to 0.873 report only report only 10 max. report only report only report only report only report only report only 0.5 max. 0.03 max. 99.5 min. 9.5 min. 0.5 max. 109.6 min. 111.6 max. 1 max, 500 max. Test Results Clear liquid, fres of particulates Pass 0.8718 Pass 7.260 Pass 30 Pass 2 Pass On Pass 104 Pass Neg Pass 0.1 Pass Neg Pass 1B Pass 0.07 Pass Not detected Pus 99.93 Pass Not detected Pass 0.00 Pus 110.4 Pass 110.6 ZPass Pass 61 Pass Ann-Stat added ANTI STAT ADDEDP 1 03 ISO !OM MI a A Responsible Care Company Shipman tio Marathon Ashland Petroleum LLC, PO Boa 1492, Cadettsberg, Ky 41129, 606-921.6802 ra-setae SW-Scearce 01324 ASHLANI CO, Ashland Distribution Company Division of Ashland, Inc. P.O. Box 2219, Columbus, OH 43216 Customer Certificate of Analysis Customer. Sherwin Williams Company_ Bow Lens South Richmond, KY 40475 Fax 4: 614-790-6624 Attn: Deb Nist (IC&S Columbus) Analysis Test Method Appearance Specific Gravity. g/mi. (6oF Gravity, pounds/piton Saybok Color Pt / Co Color (APHA) Acid Wash Color Kauri-Butanol Value Sulfur Compounds (H2S, SO2) Sulfur, ppm Acidity Copper Strip Corrosion Saturates. % Benzene, % Toluene, 'A Xylene, % > Nylon*, % Initial Boiling Point, C Dry Point, C Dist. !binge, C Water Content, ppm visual 0-891 / 0-4032 Cs is 0-156/6045 13-1209 0-848 D-1133 0-853 0-5453 0-847 D-130/149/1838 D-2306 0-2306 D-2306 0-2306 0-2306 0-850 D-S50 D-850 Aquotest Ship Data: 8-28-04 Product Toluene 03-17-10 HMIS 2306 Tank No.: 169 Vessel: TOLUENE Ship Quantity: 6542 Ticket 28727 IC&S PO / Lot No.: 4501007813-C3C0 Customer PO No.: 10233 Specification 0.869 to 0.873 report only report only 10 max. report only report only report only report only report only report only 0.5 min. 0.03 mu. 99.5 min. 0.5 max. 0.5 max. 109.6 min. 113.6 nn. 1 max. 500 max. Test Results Clear liquid, free of particulates 0.8711 7.260 30 2 ON 106 Neg 0.1 Net 1B 0.07 Not detected 99.92 0.01 0.00 110.4 110.6 0.2 36 Pass Pass Pass Pass Pass Pau Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Anti-Stet added ANTI-STAT ADDED AEU I BB APPROVED A Responsible Care Company S hipmcnt cio Marathon Ashland Petroleum LLC, PO Box 1492. Cadettsburg, Ky 41129, 606-921-6802 SW-Scearce 01323 AS11-11LANIE1 Ashland Distribution Company Division of Ashland, Inc. P.O. Box 2219, Columbus, OH 43216 Customer Certificate of Analysis Ship Date: 08/30/04 Customer Sherwin Williams Company Product: Toluene 03-17-10 HMIS 2300 8020 Lane South Tank No.: 169 Vessel: TOLUENE Richmond, KY 40475 Ship Quantity: 6134 Ticket 28737 Fax 3: 614-790-6624 IC&S PO / Lot No.: 4501007866-C3CO Attn: Deb Nist (IC&S Columbus) Analysis Test Method Customer PO No.: Specification 10233 Test Results Appearance Specific Gravity, g/mL 060111 Gravity,pounds/gl Saybolt Color Pt / Co Color (APHA) Acid Wash Color Knurl-Butanol Value Sulfur Compounds (H2S, S02) Sulfur, ppm Acidity Copper Strip Corrosion Saturates, Benzene, Toluene, Xylem% / Initial Bolling Point, C Dry Point, C Dist. Range, C Water Content, ppm visual D-891 / D-4052 Cale D.156/6045 0-1209 0-848 D-1133 0-853 0-5453 D-847 D-130164911838 D-2306 D-2306 D-2306 D-2306 ['-2306 D-8511 D-850 0-850 Aquatest it 0.869 to 0.873 report only report only 10 max. report only report only report only report only report only report only 0.5 max. 0.03 mu. 99.5 min. 0.5 max. 0.5 mix. 109.6 min. 111.6 max. 1 mi. SOO max. Clear liquid, free of particulates 0.8718 7.260 30 2 ON 106 Meg 0.1 Nag 18 0.07 Not detected 99.92 0.01 0.00 110.4 110.6 0.2 36 Pus Pass Pus Pass Pass Pass Pass s Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Anti-Stet added 360 mt. OF ANTISTAT ADDED 6;5-Y -7 APPROVED ISO 5001:2000 A Responsible Care Company Shipment do Marathon Ashland Petroleum Lir. PO Box 1492. CaUettaburs., Ky 41129. 606-921-6802 131-3SS34 SW-Scearce 01322 ASHLAP JO Ashland Distribution Company Division of Ashland, Inc. P.O. Box 2219, Columbus, OH 43216 Customer Certificate of Analysis Customer: Sherwin Williams Company Boil Lane South Richmond, KY 40475 Fax #: 614-7904624 Attn: Deb Nast (ZCikS Columbus) Analysis Test Method Appearance Specific Gravity, g/mL (4).60F Gravity, poundslgallon Saybolt Color Pt / Co Color (APH A) Acid Wash Color KsuriButanol Valise Sulfur Compounds (1125, SO2) Sulfur, ppm Acidity Copper Strip Corrosion Saturates, % Benzene, % Toluene, % Xylene, % Xyleno, % Initial Boiling Point, C Dry Point, C Dist. Rang*, C Water Content, ppm visual D491 I D-4052 Cale D-15616045 0-1209 0.848 0.1133 0-853 1)-5453 11-1147 D-130/849/11138 D2306 D-2306 D-2306 D-2306 D-2306 D-850 0-850 0450 Aquatest Product: Toluene Tank No.: TI 69 Vessel: 8504 Ship Quantity: 6328 Ticket: 28746 IC&S PO / Lot No.: 45010078711-C3CD Customer PO No.: 10233 Specification 0.869 to 0.873 report only report only 10 mu. report only report only report only report only report only report only 03 max. 0.03 mu. 99.5 min. 0.S max. 0.5 mac. 109.6 min. 111.6 mss. 1 max. 500 max. Test Results Clear liquid, fres of particulates 0.8718 7.260 30 2 ON 106 Neg 0.1 Neg 1B 0.0/ Not detected 99.92 0.01 0.00 110.4 1104 0.2 36 Pass Pus Pass Pass Pass Pass Pass Pass Pus Pass Pass Pus Pass Pass Pass Pus Pass Pass Pus Anci-Star oddest 03-17.10 HMIS 230G 360MLS ANTI-STAT ADDED \y APPROVED A Responsible Cue Company Shipment c/o Menthes Ashland Petroleum LLC, PO Box 1492, Catlettsburg, 14 41129, 606-921 -6802 III-911234 SW-Scearce 01321 "51-111LANIA Ashland Distribution Company Division of Ashland, Inc. P.O. Box 2219, Columbus, OH 43216 Customer Certificate of Analysis Ship Date: 08-31-04 Customer. Sherwin Williams Company Product Toluene 03-17-10 S 2300 Boggs Lane South Tank No.: T169 Vessel: 25241 Richmond, KY 40475 Ship Quantity: 6535 Ticket: 28771 Fax 0: 614-790-6624 1C&S PO / Lot No.: 4501008566-C3C0 Attn: Deb Nist (LC&S Columbus) Analysis Test Method Customer PO No.: Specification 10233 Test Results Appearance Specific Gravity, g/mL (460F Gravity, pounds/gallon Sayboit Color Pt / Co Color (APH A) Acid Wash Color Kauri-Butanol Value Sulfur Compounds (1125, S02) Sulfur, ppnt Acidity Copper Strip Corrosion Saturates, % Benzene, I Toluene, % > Xylene, Initial Bolling Point. C Dry Point, C Dist. Range, C Water Content, ppm visual D-891 / D-4052 Cale D-156/6045 D-1209 D-848 D-1133 D-853 D-5453 D-847 D-130/849/1838 D-3306 D-2306 D-2306 D-2396 D-2306 D-851) D-850 13-850 Aqustest 0.869 to 0.873 report only report only 10 mix. report only report only report only report only report only report only 15 max. 0.03 max. 915 min. 0.5 max. 0.5 mos. 109.6 min. 111.6 max. I max.. 500 mos. Clear liquid, free of particulates 18718 7.260 30 2 ON 106 Neg 0.1 N eg lB 0.07 Not deteeted 99.92 0.01 0.00 110.4 110.6 0.2 36 Pass Pass Pass Pass Pass Pass Pass Pass Pass Pau Pass Pus Pass Pass Pass Pass Pass Pass Pus Pass Anti-Slit added 03-17-10 HMIS 2300 360h4LS ANTI-STAT ADDED ISO VIM 2SOO A Responsible Care Company Slapincnt do Marathon Ashland Penult-ma LLC, PO Box 1492, Catlettsburg, Ky 41129, 606-921-6102 M-- 302O4 SW-Scearce 01320 Ashland Dbtribudon Company Division of Ashland, Inc. P.O. Box 2119, Columbus, OH 43716 Customer Certificate of Analysis Customer: Sherwin Williams Company Boons Lane South Richmond, KY 40475 Fax it 614-7964624 Attn: Deb NW (1CRS Columbus) Analysis Test Method Appearance Specific Gravity, elmL (MOF Gravity, pounde/pilon Saybolt Color Pt / Co Color (APHA) Acid With Color Kauri-Butanol Vales Sun* Compounds (HU, SO2) Sulfas, ppm' Acidity Copper Strip Corrosion Saturates, % Benzene, % Toluene, % Xylene, % > Xylem., % Initial Boiling Point, C Dry Point, C Dist. Bongo, C Water Content, ppm visual D491 / D-4053 Cate D-156/6045 D-1209 D4481 D-1133 D453 D-5453 D447 D-130/849/18311 D-2306 D-2306 0-2306 D-2306 O-2306 D4511 D450 Agitated Ship Debt: 08-3144 Product Toluene 03-17-10 HMIS 2300 Tank NO.: T170 Vessel: 8072 Ship Ouantitt: 6553 Ticket 28774 IC&S PO / Lot No.: 45011108571-C3CE Customer PO No.: 10233 Specification 11.869 to 0.873 report only report only 10 max. report only report only report only report only report only report only 0.5 max. 0.03 amt. 99.5 -in. 0.5 max. 0.5 max. 109.6 min. 111.6 mss. 1 max. 500 mars Test Results Clear liquid, free of particulates 0.0711 7.260 30 2 ON 104 Neg 0.1 Neg le 0.05 Not detected 99.94 Nat detected 0.00 110.3 110.6 0.3 50 Pass Pass Pus Pm Pam Paso Pass Pau Pus Pass Pass Pass Pus Pass Pus Pus Pass Pass Pass Pass Anti-SIM added 03-11-10 HMIS 2300 360MLS ANTI-STAT ADDED :101 Raspaisible Care Company Shipment do Mambo* /WOW Petroleum LLC, PO Boa 1492, CallvElbwi, Ky 41129. 606-921-6102 (9 ra 10 ISO 9 ISIS 1/1-91M94 SW-Scearce 01319 ASHLAND. Ashland Distribution Company Division of Ashland, Inc. P.O. Box 2219, Columbus, OH 43216 Customer Certificate of Analysis Ship Date: 10/05/04 Customer. Shore/in Williams Company Product: Toluene 03-17-10 HMIS 230G Booze Lauer South Tank No.: 169 Vessel: TOLUENE Fax 4: Richmond. KY 40475 614-7904624 Ship Quantity: 6579 Ticket: 29366 [CIS PO / Lot No.: 4501034681-C3C0 Attn: Deb Nist (IC&S Columbus) Analysis Test Method Customer PO No.: Specification 10233 Test Results Appearance Specific Gravity, g/mL MOP' Gravity, pounds/pikes Saybolt Color Pt / Co Color (APHA) Acid Wash Color ICauri-Butasol Value Sulfur Compounds (112S, S02) Sulfur, ppm Acidity Copper Strip Corrosion Saturates, % Benzene. % Toluene, % Xylem, % Xylem*, % Initial Boiling Point, C Dry Point, C Dist. Range, C Water Content, ppm visual D-891 / D-4852 Cite 1)-156/6845 0-1209 0448 D-1133 D-853 0.5453 0-847 0.430/849/1838 0-2306 0-2306 D-2306 0-2306 0-2306 0,.850 0.850 13-858 Aquatest 0.869 to 0.873 report only report only 10 max. report only report only report only report only report only report only 0.5 max. 0.03 max. 99.5 min. 0.5 max. 0.5 max. 109.6 rain. 111.6 max. 1 mitt. 500 max. Clear liquid, free of particulates 0.8718 7.2611 30 2 On 106 Net 0.1 Net 1B 0.04 0.00 99.92 0.04 0.00 110.1 110.6 0.5 137 Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pau Pass Pass Pass Pass Pass Anti-Stu added 360 mt. OF ANTI-STAT ADDED APPROVED A Responsible Care Compesy . Shipment c/o Marathon Ashland Petroleum LLC. PO Box 1492, Catlettsburg, Ky 41129, 606-921-6802 Ili- all 234 SW-Scearce 01318 -iHLANJEA Ashland Distribution Company Division of Ashland, Inc. P.O. Box 2219. Columbus, OH 43216 Customer Certificate of Analysis Customer Ashland Distribution Company Tewksburz MA 01876 Fax 0: Attn: Analysis Test Method Appearance Specific Gravity, ,/ml, (160F Gravity, poundalpilon Saybolt Color Acid Wash Color Kaurl-Butanol Value Sulfur Compounds (H2S, S02) Sulfur, ppm Copper Strip Corrosion Saturates, % Benzene, % Toluene, % Rylene, % > Xylene, % Initial Bolling Point, C Dry Point, C Dist. Hansa, C Water Content, ppm visual 0-891 / D-4052 Colt D-156/6045 0-34$ D-1133 D-853 D-5453 D-130/849/1838 D-2306 0-2306 D-2306 D-2306 D-2306 0-850 0-850 0-850 Aquatest Ship Date: 10-5-04 Product: Toluene PC3001850-8-5 Tank No.: 169 Vessel: TOLUENE Ship Quantity: 6676 Ticket 29361 [CAS POI Lot No.: 4501034676-C3C0 Customer PO No.: 10233 Specification 0.869 to 0.873 report only report only report only repo repo repo repo 0.5 0.03 99.5 min. 0.5 mu. 0.5 max. 109.6 min. 111.6 max. 1 max. report only Test Results Clear liquid. free of particulates 0.8718 7.260 30 On n "106 V...f/(411 -r 0 . 99.92 0.04 0.00 110.1 110.6 0.5 137 Pass Pass Pass Pass Pass Pass Pass Pass Pau Pass Pass Pus Pass Pass Pass Pass Pus Pass CODES03-17-10, HMIS 2300 360 MI. ANTI-STAT ADDED RELIO APPROVED L ISO 9001:2015 A Responsible Care Company Shipment do Marathon Ashland Petroleum LLC, PO Box 1492, Catlettsburg. icy 41129, 606-921-6802 SW-Scearce 01317 ASHILANI CIL Ashland Distribution Company Division of Ashland, Inc. P.O. Box 2219, Columbus, OH 43216 Customer Certificate of Analysis Ship Date: 10/06/04 Customer: Sherwin Williams Company Boggs Lane South Richmond, KY 40475 Fax 0: 614-790-6624 Attn: Deb kW (IC&S Columbus) Analysis Test Method Appearance Specific Gravity, g/mL (gISOF Gravity, pounds/gallon Saybolt Color Pt / Co Color (APHA) Acid Wash Color Kiwi-Butane! Value Sulfur Compounds (H2S, 302) Sulfur, ppm Acidity Copper Strip Corrosion Saturates, % Benzene, % TO11111% % Xylene, % > Xylene, % Initial Boiling Point, C Dry Point, C Dist. Range, C Water Content. ppm visual D-891 / D-4052 Cak 0.156/6045 D-1209 11.848 D-1133 0-853 0-5453 0-847 D-139/849/1838 D-2306 0.2306 D-2306 D-2306 0-2306 D-859 0.850 D-850 Aquatint Product: Toluene 03-17-10 HMIS 230G Tank No.: 169 Vessel: TOLUENZ Ship Quantity: 6600 Ticket: 29390 IC&S PO / Lot No.: 4501035731-c3c0. Customer PO No.: 10333 Specification Test Results 0.869 to 0.873 report only report only 10 max. report only report onl report onl report on report on report o 0.5 111/11.. 0.03 ma 99.5 mi 0.5 ma 0.5 max. 109.6 min. 111.6 max. max. 500 max. Clear liquid, free of particulates 0.8715 7.260 30 2 keg 1B 0.04 0.00 Uul 99.92 0.04 (,ti4. 4:1, 0.00 110.1 O-c) 110.6 pc 0 57 Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pus Pass Pass Pass Pass Pass Pass Pass Pass Pass 0 '1)4 (irr Anti-Stet added 360 mL. of anti-star added rel. x 1 APPROVED 3 150 9001:2111* A Responsible Care Company Shipment cia Marathon Ashland Petroleum LLC, PO Box 1492, Catlettsburg, Ky 41129, 606-921-6802 114- 9 6 234 SW-Scearce 01316 Ashland Distribution Company Division of Ashland, Inc. P.O. Box 2219. Columbus, OH 43216 Customer Certificate of Analysis Ship Date: 10/06/04 Customer: Sherwin WIllients Company Bons Lane South Product: Toluene Tank No.: 169 03.17-10 ELM1S 2300 Vessel: TOLUENE Wantons!, KY 40475 Ship Quantity: 6526 Ticket: 29396 Fax /1: 614-790-6624 1C&S PO / Lot No.: 4501035734-C3C0 Attn: Deb Nast (IC&S Columbus) Analysis Test Method Customer PO No.: Specification 10233 Test Results Appearance Specific Gravity, g/mL (60P Gravity, pounds/gallon Saybolt Color Pt / Co Color (APHA) Acid Wash Color ICauri-Entanol Value Sulfur Compounds (H2S, 502) Sulfnr, ppm Acidity Copper Ship Corrosion Saturates, % Benzene, % Tolman% % Xylem, % > Xy lens, % Initial Boiling Point, C Dry Point, C Dist. Range, C Water Content, ppm visual D-891 I 0-4052 Cale 13-156/6045 D-1209 0-848 D-1133 11-853 0-5453 0-847 D-130/849/1838 D-2306 D-2306 0-2306 0-2306 D-2306 0-850 0-850 D4150 Aqustest 0.869 to 0.173 report only report only 10 max. report only report only report only report only report only report only 0.5 mu. 0.03 max. 99.5 mho. 0.5 max. 0.3 max. 109.6 min. 111.6 mix. 1 mu. 500 max. Clear liquid, free of particulates 0.8718 7.260 30 2 On 106 Nag 0.1 Neg 111 0.04 0.00 99.92 0.04 0.00 110.1 )10.6 0.5 137 Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pm Pass Pass Pass Pass Pass Pass 31((o. Ann-Stat added 360 mL OF ANTI-STAT ADDED REL. Cl OCT - 6 2004 APPROVED A Responsible Care Company Shipment do Marathon Ashland Petroleum LLO PO Hos 1492. Catlettsburg, Ky 41129, 606-921-6102 IN-3111234 SW-Scearce 01315 Ashland Distribution Company Division of Ashland, inc. P.O. Box 2219, Columbus, OH 43216 Customer Certificate of Analysis Ship Date: 10-07-04 Customar Company Bow Lane South Product: Toluene Tank No.: 170 Vessel: TOLUENE Richmond, KY 40475 Ship Quantity: 6366 Ticket: 29435 Fax #: 614-790-6624 IC&S PO / Lot No.: 4501036729-C3C0 Attn: Deb Nht (ICA'S Columbus) Analysis Test Method Customer PO No.: Specification 10233 Test Results Appearance Specific Gravity, s/mL 065F Gravity, pounds/gallon Saybolt Color Pt / Co Color (APRA) Acid Wash Color Kaari-Butssel Value Sulfur Compounds (112S, SO2) Sulfur, ppm Acidity Copper Strip Corrosion Saturates, % Benzene, % Toluene, % Xylene, % Xylene, % Initial Boiling Point, C Dry Point, C Dist. Rings, C Water Content, ppm visual 0-891 / D-4052 Cale D-156/6045 13-1209 D-848 D-1133 D-853 0-5453 D-847 0-130/849/1838 0-2306 13-2306 0-2306 D-2306 0-2306 0-850 D-850 D-550 Aquatest 0.869 to 0.873 report only report only 10 max. report only report only report only report only report only re 0.5 0.03 99.5 0.5 0.5 109 111.6 max. 1 max. 500 max. Clear liquid, free of particulates 0.8719 7.261 30 3 ON 104 Net 0.2 Net 110.4 110.6 0.2 48 Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pam Pass Pass Pass Pass L4 Anti-Stet added 360 WS ANTI SCAT ADDED PER FULL TRU C14 415 APPROVED 151;4 A Responsible Care Company Shipment do Marathon Ashland Petroleum LLC, PO Hoe 1492, Catlettsburg, Ky 41129, 606-921-6102 Eli-- 31134 SW-Scearce 01314 ASHLAND, Ashland Distribution Company Division of Ashland, Inc. P.O. Box 2219, Columbus, OH 43216 Customer Certificate of Analysis Customer: Sherwin Williams Company Bow Lane South Richnsoad, KY 40475 Fax N: 614-790-6624 Attn: Deb Nist (1C&S Columbus) Analysis Test Method Appearance Specific Gravity, g/mL 60F Gravity, poanda/golion Saybolt Color Pt / Co Color (APH A) Acid Wash Color Kauri-Butanol Value Sulfur Compounds (112S, S02) Sulfur, ppm Acidity Copper Strip Corrosion Saturates, % Benzene, % Toluene, % Xylane, "fr > Xylem*, % Initial Boiling Point, C Dry Point, C Dist. Range, C Water Content, ppm visual D-891 / D-4052 Cale D-156/6045 0-1209 13-848 D-1133 13-853 0-5453 1:1-$47 D-130/849/1838 0-2306 0-2306 D-2306 D-2306 D-2306 D-8511 D-850 0-850 Aquatest Ship Date: 1047-04 Product: Toluene 03-17-10 HMIS 230G Tank No.: 170 Vessel: TOLUENE Ship Quantity: 6922 Ticket: 29436 (CNA PO / Lot No.: 4501036736-C3C9 Customer PO No.: 10233 Specification 0.869 to 0.873 report only report only 10 max. report only report only report only report only report only report only 0.5 max. 0.03 max. 99.5 min. 0.5 max. 0.5 max. 109.6 min. 111.6 max. 1 max. 500 max. Test Results Clear liquid, free of particulates 0.3719 7.261 30 2 ON 104 Meg 0.2 Nag 1B 0.05 Not detected 99.95 0.01 0.00 110.4 110.6 0.2 48 Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pus Pus Pus Pass Pass Pau Pass Pass Pass Pass Ann-Stat added 360 MLS ANTI STAT ADDED PER 1RUCK RELI T _11924? . &323`3" APPROVED A Responsible Care Company Shipment c/o Marathon Ashland Petroleum LI.C, PO Box 1492, Catlettsburg, Ky 41129, 606-921-6802 0952: 2011 d 00 WM-31234 SW-Scearce 01313 ASHLAND. Ashland Distribution Company Division of Ashisad, Inc. P.O. Box 2219, Columbus. OH 43216 Customer Certificate of Analysis Customer Sherwin Williams Company Dow Lana Saudi Richmond, KY 40475 Fax 0: 614-7904624 Ann: Deb Nbt (IC31.5 Columbus) Analysis Teat Method Appearance Specific Gravity, g/mi OOP' Gravity, pountWplion &yin's Color Pt 1 Ca Color (APHA) Acid Wash Color ICartri-Butanol Value SulfUr Compounds (1125, 502) Sulfur, ppra Acidity Copper Strip Corrosion Saturates, % ileuena, % Toluene, % Xylem*, "A Xylowit, % Initial Boiling Point, C Dry Point, C Dist. Range, C Water Content, ppm visual 0491 /13-4052 Cale D-156/6845 D-1209 0-840 D-1133 0-853 0.5453 0-847 0-138/114911838 D-2306 11-2306 0-2306 0-2306 D-2304 0-850 p4159 Aquitsst Ship Date: 10-11-04 ri3roduce lkaiiiene4.. N 1' Tank ind 170 Q3-17-10 HMIS 2304 TOLUENZ Ship Quantity: 6180 Ticket 29508 ICU PO1 Lot No.: 450103934 .10 Customer PO No.: 10233-I Specification Test Results Clear liquid, free sr porderdites Pass 0.869 to 0.873 04711 Pus report oily 7.261 Pass report only 30 Pass 10 max. 2 Pass report only On Pass report only 104 Pus report only Nag Pass report only Pass report oily Nag Pass report only 111 Pass 0.5 max. 0.06 Pass 0.03 nuts. 0.00 Pus 994 :rim 99.91 Pass 0.5 mu. 0.01 Pass 0.5 mu. 0.01 Pus 109.6 min. 110.1 Pass 1114 mu. 110.8 Pass 1 ang. 0.7 Pau $ 1T C rte. l i w/ C 56 Pass Ant!-Stet lidded 360 MU ANTI S'L'AT ADDED PER FULL TRUCK APPROVED A Responsible Cons Company Shipment do Monahan Ashland Petroleum LLC, PO Boa 1492, CodetIabmi, Ky 41129, 606-921-6101 SW-Scearce 01312 Ashland Distribution Company Division of Ashland, inc. P.O. Box 2219, Columbus, OH 43216 Customer Certificate of Analysis Customer Sherwin Williams Company Bow Lane South Richmond, KY 40475 Fax 0: 614-790-6624 Attn: Deb Nist .(1054 Columbus) Analysis Test Method Appearance Specific Gravity, g/mL (60P Gravity, pounds/gallon Saybolt Color Pt / Co Color (APHA) Acid Wash Color ifnuri-Butanol Value Sulfur Compounds (1128, 502) Suitor, ppm Acidity Copper Ship Corrosion Saturates, /. Benzene,'/. Toluene,'/. Xyiene, % Xylene, % Initial Boiling Points C Dry Point, C Dist Range, C Water Content, ppm visual 0-891 / 0-4052 Cale D-15616045 D-1209 0448 D-1133 13453 D-5453 D-847 0-130/849/1838 D-2306 O-2306 0-2306 0-2306 0-2306 D-850 0-850 0-850 Aquatest Ship Date: 10-18-04 Product: Toluene 03-17.10 HM1S 2300 Tank No.: 169 Vessel: TOLLIZNE Ship Quantity: 6218 Ticket: 29664 IC&S PO / Lot No.: 4501044266 Customer PO No.: 10233-1 Specification 0.869 to 0.873 report only report only 10 max. report only report only report only report only report only report only 0,5 mos. 0.03 max. 99.5 min. 0.5 mai. 0.5 man. 109.6 mist. Test Results Clear liquid, free of particulates Pass 0.8710 Pass 7.254 Pass 30 Pass 2 Pus ON Pass 105 Pass Neg Pass 0.1 Pass Neg Pass 1B Pass 0,06 Pass Not detected Pass 99.93 Pass 0.01 Pass 0.00 Pass 110.5 Pass 110.6 Pass 0.1 Pass 46 Pass Anti-Stat added ANTI STAT ADDED.. Irg A Responsible Care Company APPROVED ISO seal: COOS /1( Shipment eto Marathon Ashland Petroleum LLC, PO Boa 1492, Catlettsburg, Ky 41129, 606 -921.6802 IN-35284 SW-Scearce 01311 4"Ik' h.SHLANIF). Ashland Distribution Company Division of Ashland, Inc. P.O. Box 2219, Columbus, OH 43216 Customer Certificate of Analysis Ship Date: 11-29-04 Customer: Sherwin Williams Company Boggs Lane South Product: Tolman Tank No.: TI70 03- 17- 10 HMIS 2300 Vessel: 8506 Richmond, KY 40475 Ship Quantity: 6168 Ticket 20552 Fax #: 614-790-6624 Attn: Deb Nist (IC&S Columbus) Analysis Test Method (C&S PO / Lot No.: Customer PO No.: 4501071421-C3C0 10233 Specification Test Results Appearance Specific Gravity, g/naL 60P Gravity, pounds/gallon Saybolt Color Pt / Co Color (APHA) Acid Wash Color Kanri-Butanol Value Saliba. Compounds (1121, S02) Sulfur, ppm Acidity Copper Strip Corrosion Saturates, % Benzene, % Toluene, % Xylena, % > Xyleno, % initial Boiling Point, C Dry Point, C Dist. Range, C Water Content, ppm visuel D-891 / D-4052 Cale D-156/6045 D-1209 D-1348 D-1133 D-853 O-5453 D-847 D-13W349/18311 D-2306 0-2306 D-2306 D-2306 D-2306 D-850 0-850 0-850 Aquatesi 0.869 to 0.873 report only report only 10 max. report only report only report only report only report only report only 0.5 max. 0.03 max. 99.5 min. 0.5 max. 0.5 max. 109.6 min. 111.6 man. 1 max. _.500 max. nn Ho ovei , .1 Clear liquid, free of portico's*** Pass 0.8718 Pass 7.261 Pass 30 Pass 2 Pass ON Pass 103 Pass Nei Pus 0.1 Pass Nei Pass 111 Pass 0.05 Pass Not detected Pass 99.93 Pass 0.01 Pass 0.01 Pass 110.5 Pass 110.6 Pass 0.1 Pass 14 Pass Anti-Stst added 03-17.10 11:MIS 2300 360 MIS AMT-STAT ADDED 1211;2: APPROVED/ Voi A Responsible Care Company Shipment a/o Marathon Ashland Petroleum LLC, PO Box 1492, Catlettsburg, Ky 41129, 606-921-6102 613 ISO 55111:2980 /1 10 WM-36234 SW-Scearce 01310 ASHLIsNICI. Ashland Distribution Company Division of Ashland, Inc. P.O. Box 2219, Columbus, OH 43216 Customer Certificate of Analysis Ship Date: 11-29-04 Customer Sherwin Williams Company Product: Toluene 03-17-10 HMIS 2300 Boggs Lana South Tank No.: T170 Vessel: 3067 Richmond, KY 40475 Ship Quantity: 6755 Ticket: 20550 Fax #: 614-790-6624 IC&S PO / Lot No 4501071414-C3C0 Ann: Doh Nist (IC&S Columbus) Analysis Test Method Customer PO No.: Specification 10233 Test Results Appearance Specific Gravity, g/usL6t6OF Gravity, pounds/gallon Saybolt Color Pt / Co Color (APHA) Acid Wash Color Kauri-Butsnol Value Sulfur Compounds (1125, SO2) Sulfur, ppm Acidity Copper Strip Corrosion Saturates, % 511112161M. % Toluene, % % Xylens,, % Initial Boiling Point, C Dry Point, C Dist. Range, C Water Content, ppm visual 13.0911 D-4052 Cale D-156/6045 D-1209 13-84$ 04133 D-853 0-5453 13447 D-130/849/1833 13.2306 D-2306 13.2306 0-2306 D-2306 0-850 13-350 0450 Aquatest 0.869 to 0.873 report only report only 10 inns. report only report only report only report only report only report only 0.5 max. 0.03 mu. 99.5 min. 0.5 max. 0.5 max. 109.6 min. 111.6 max. 1 max. 500 mos. Clear liquid, free of particulates Pass 0.8718 Pass 7.261 Pass 30 Pass 2 Pass ON Pus 103 Pass Neg Pass 0.1 Pass Neg Pass 1B Pass 0.05 Pass Not detected Pass 99.93 Pass 0.01 Pass 0.01 Pau 110.5 1110.6 Pass A Pus 63 0.1 Pass 14 RECI! E-13 29/004 /22/0 Anti-Star added 43.17-10 AMTS 2341 360 MLS ANTI-STAT ADDED APPROVED .re Company Shipment do Marathon Asidend Petroleum LLC, PO Box 1492, Catlettsburg. Ky 41129, 606.921-61102 ISO 9001:2000 ffi 1 11:111. In-98 2 94 SW-Scearce 01309 Dec 07 04 01:05p Laboratory 513-541-2174 PI Ashland' it c44/64.1 of,v 7-47 Ashland Distribution Company Division of Ashland Inc. Customer Certificate of Analysis industrial Chemical & Solvents Division DATE: December 7, 2004 Customer: , 5,44Al.som, !ter %/, A er, n-Chite/a v, r b Atr/it'A, Cr-4-17001-7 17) 157-PI2'ee,ilvi er 6/4 e$ 396- 441.v-5 .400 .4esee13$ /.410,1 44.140 75- cast codis,0 vg-/7 Product TOLUENE a'rank 4 Trans:00081one, New Albany, Indiana Ship Date: /a.- 2 2 - o 9 . Ship QUentity: GS: va Sales Order No 4/.5-0/4.0-0 q/def C 3 rrci Customer Order No: MfrALSPoota de.O. Lot No: 002658.001 Analysis 350 Analysis Description Limits Test Results API Gravity igr 60 Deg F (0 4052) 30,8 Specific Gravity (I) 50 Deg F (0-4052) 0.599-0.873 0.8717 LBS/GA1150 Deg F (0 4052) 0280 i Odor (0-1296) tharaderlet10 Color (0 156) *30 Color PUCo (0 1209) 20 max Less than 5 Copper Corrosion (0 541) Pass Peas Acid Wash Color (0 848) 2 max 2- Knurl &stand Value (0 1133) 102.9 Acidly (0 847) No Free Add No Free Add AckitY 80) ( 4004(9) Sulfur (0 653) Free 0.019 Free Water Content (E 1064) (ppm) 229.0 Assay (G.C) (1) 99.5 min 99,89 Paraffins (G.C.) (ppm) 356.3 Benzene Content (G.C.) (ppm) 25.5 Elhylbenzene Content (G.C.) (ppm) 230.7 xylenes (G.C.) (ppm) 508,3 Xylenes 1 Ethylbenzene (G.C.) (ppm) MILO Distillation (0850) Deg C Dry Point 109.8 1106 Total Distillation Range 1.0 to Include 110.5 1.0 Retractive Index 25 beg C (0 1218) 1.4540 Appearance (Visual) Clear and free of sediment andfor suspended solids NOE: THE ABOVE ANALYSIS WAS PERFCRMED BY MEM nose Remit CALEB BREIT. me emote. AS TEMP, CONFORMS TOAPILAND CHOAICAL 5PECIFICAT1Ce4S. t9Z/4Po , Coftek,4 letertek Caleb ens11 December 7, 2004 Lab Rd: 002856.001 It Ashland Distribution Company, Division of Ashland Inc., Box 7219, Columbus, Ohio 41216 SW-Scearce 01308 Dec 07 04 01:05 Laboratory 51.3-941 -2174 P Ashland Ashland Distribution Company Division of Ashland Inc. Customer Certificate of Analysis industrial Chemical & Solvents Division DATE: December 7, 2004 aProduct TOLUENE Tank 4 TransmonlaignS, New Albany, Indiana s Ship Data -- zte Ship Quantity: Sales Order No: Customer Order No: Lot No: 002858-001 Analysis Analysis I7escription API Grevity 80 Dag F (0 4052) Specific Gravity 60 Deg F (0-4052) L05/GAL.160 Deg F (0 4052) Oder (0-1296) Color ID 156) Color PtICo (0 1209) Copper Corrosion ID 849) Acid Wash Color (0 648) Kaun Swami' Value (0 1133) Acidity (0 647) Acidity (0 647) (Meg/kg) Sulfur (0 653) Water Content (5 1064) (ppm) --Fergana (G.C.) (plan) ArsiVIT.CME Benzene Content (G.C.) (ppm) Elhylbertzene Content (G.C.) (ppm) Xylenes (G C.) (ppm) Xylenes & Eihylbenzene (G.0) (ppm) Distiliabon (0850) Deg C Ory Point Tolal Distillation Range Refractive Indexa 25 Deg C (0 1218) Appearance (Visual) Limits 0.869-0.873 20 max Pass 2 mu No Free Add Free 99;5min 1.0 to Include 110.6 Test Results 30.6 0.8717 .p2130 Characteristic *30 Less then 5 pus $' 102.9 No Free Acid 0.019 Free 229.0 99.84 356.3 25.5 230.7 50&3 kca *7g 4 1 Maff ci )02 109.8 110.6 1.0 1.4940 Clear and he of sediment and/or suspended solids 0 THE ASOVE ANALYSIS WAS PERFORMED BY INTEATEK TESTING SERVICES, CALEB SRETT. THE SAMPLE, AS TESTED. CONFORM: To ASHLAND CHEMICAL SPECIFICATION& Uk Interlslr COWBee Daaamber 7, 2004 Lab Rat 002858.031 40---. 11114 11 Ro won 6.0" ow* C &NW" Ashland Distribution Company, Division of Ashland Inc., Box 2219, Columbus, Ohio 4 216 SW-Scearce 01373 Oacs 07 04 01:0Sp Laboratory 513-941-2174 p.1 1 2sihriland Ashland Distribution Company Division of Ashland Inc. Customer Certificate of Analysis N. Industrial Chemical & Solvents Division DATE: December T. 2004 Analysis Product: TOLUENE Tank 4 Trartemon New Alban Indiana S. Ship Date: _67 or104 75IShSiaPlesQOuradnetirtyN:o:(.e6fed, -f7 Customer Order No: to.;p Lot No: 002658-001 ail 'Au, Analysis Description API Gravity CA 00 peg F (D 4052) Specific Gravity (1) 50 Deg F (0-4052) LBSIGAU60 Dap F (0 4052) Odor (D-1290) Color (13 156) Color PVC (01209) Copper Corrosion (D 849) Aoki Wash Color (ID 848) Kaun Butenol Value (D 1133) Acidity (0 847) Acidity (0 847) (Meg/kg) Sulfur (0 853) Waist' Content (E 1064) (ppm) Assay (G.C) ('A) Paraffins (G.C.) (ppm) Benzin. Content (G.C.) (ppm) Eltrylbenzene Content (D.C.) (ppm) Xylenes (G.C.) (ppm) Xytenes & EilVbenzene (DZ.) (ppm) Distillation (0850) Deg C Dry Point Total Distillation Range Refractive Index 25 Cog C (0 1218) Appearance (Visual) Limits 0.509-0.873 20 max Pass 2 max No Free Acid Free 99.5 min 1.0 to Include 110.6 Test Results 30.8 0.8717 , ,g1= +30 Less then 5 Pass 102.9 No Fres Acid 0.019 Fres 229.0 99.89 355.3 25.5 230.7 et% 505.3 0 lb 109.6 110.6 1.0 1.4940 1.1 Clear and free of sediment indfor suspended solidi THE MOW ANALYSIS WAS PERFORMED DY INTERTEK TESTING SERVICE% CALEB BRETT. THE well. As TESTED. ClYilkettrill0 ASHLAND CHEMICAL SPODIRCATIONS. AMIWWIWC4.7* C./.14./ !Mattis Cash Brea Dscsoter 7, 2004 eR77-- 13 Lab Reit 002458.001 Ir Ashland Distribution Company, Division of Ashland Inc., Box 2219, Columbus, Ohio 431I6 SW-Scearce 01372 Dec 07 04 01:05p Laboratory 5 13 - 9 41 - 2174 P 1 Ashland I '11-6 Ashland Distribution Company Division of Ashland Inc. Customer Certificate of Anal sls --AWNCustomer. 1 11 Industrial Chemical & Solvents Division DATE: December 7, 2004 Product TOLUENE Tank 4 r Tranimon Ship Oats: / Ship Quantity; re, New Alban Indiana Customer Order No: ".v (3,2 . Lot No: 002858.001 Analysis Description API Gravity a 60 Deg F (D 4052) Speak Gravity ia 60 Deg F (0.4052) Limits 0.889-0.873 LBS/GAU60 Deg F (D 4052) Odor (0-1294) Color (0 156) Color P1/Co (0 1209) 20 max Copper Corrosion (0 849) Pass Acid Wash Color (0 646) 2 max /faun Bulanol Value (D 1133) Acidity (0 847) No Free Acid Acidity (D 841) (Ma09) Sulfur (0 853) Fran Water Content (E 1064) (ppm) Assay (G D) (%) 99,5 min Paraffins (G.C.) (porn) Benzene Content (G.C.) (ppm) Elhylbenzene Content (G.C.) (PP1 11) Xylenes(G.C.) (ppm) Xytenes A Elnyibentene (G.C.) (ppm) Disaliation (0850) Deg C Ory Point Total Distillation Range 1.0 to induda 110.8 Retraclive Index@ 25 Deg C (0 t218} Appearance (Visual) ! vr e 0?i 19 1 Test Results 301 0.8717 8t250 it heracteristIc 410 Loss than 5 Pass 102.9 No Free Add 0.019 Free 229,0 99.69 355,3 25.5 230.7 508.3 5 011p/ ya.o Ili I 109.6 110,8 1.0 1.4940 Clew and free of sediment end/or suspended solids THE AsovE ANALYSIS WAS PERFORMED IIY WTERTEX TESTING SERV/GE% GALES BRETT. THE SAMPLE. AS TESTED, CONFORMS TO ASHLAND OIEMICAL SPECIFICATIONS. !modal! Carob Brett December 7,2004 ,, Labatt: 002158-001 s Ashland Distribution Company, Division of Ashland Inc., Box 2219, Columbus, Ohio 4ii16 SW-Scearce 01371 Dec 07 04 01:05p LabcratcrU 513-941-2174 P1 =nrdA.415611 Ashland Distribution Company Division of Ashland Inc. Customer Certificate of Analysis Industrial Chemical & Solvents Division DATE: December 7. 2004 li 4415AA /7777/ rpci. Lei AO .i Gp- Product TOLUENE Tank 4 c Transition Ship Date: shipQuantity:G L; Sales Order No:~ 42.c.).,,,_,....LtorherOrderNa: , Lot No: 002858-001 Analysis Analysis Description Limits Test Results API Gravity CO 60 Deg F (0 4052) 30.6 Specific Gravity al 60 Deg F (D-4052) LBS1GAt160 Deg F (D 4052) 0.869-0.873 0.6717 11260 Odor (D-1294) Color (0 156) haractedstio +xi Color PVC (0 1209) 20 max Len then 5 Copper Corrosion (CI 849) Pass Pau Acid Wash Color (C) 848) 2 max 2- Kaun Bute:tot Value (D 1133) 102.9 Acidity (I) 847) No Free Acid No Free Acidity (D 847) (tteglitg) 0.019 Sulfur (0 853) Free Free Water Content (E 1064) (ppm) 229.0 Assay (0 C) (%) 99.5 min 98.69 Paraffins (G.C.) (ppm) 356.3 Benzene Content (G.C.) (ppm) 25.5 Elhylbenzene Content (G.C.) (ppm) 230.7 Xylenes (G.C.) (ppm) 1 506.3 ylenes & Ethylbenzene (G.C) (ppm) /9.0 Dishile lion (0850) Deg C 109,6 Ory Point 110.6 Total Distillation Rang. 1.0 to Include 110.6 1.0 Palmolive Index@ 25 Deg C (0 1218) 1.4940 Appearance (Visual) Clear and free of sediment and/or suspended scads 4 N:rS THE Aeove ANALYSIS W45 PERFORMED BY prrekrbi TEBONG SERVICES, CALEB Elerrr. THE SAMPLE, AS TESTED, COMPOIVA5 TO ASHLAND CHEMICAL SPECIFICATIONS, q1D 1)1 Wank Caleb Brell December 7, 2004 tab Ref: 002858.001 -..\ n s tsimmskie Can41, Corwin, Ashland Distribution Company, Division of Ashland Inc., Box 2219, Columbus, Ohio 421166 SW-Scearce 01370 04 01 : OSp Laisorsytor S13-942 -2174 iro 1 Ashland ..somorm- Ashland Distribution Company Division of Ashland Inc. Customer Certificate of Analysis .er. Aa I AN I AA- (/1 a4 frAVIO .47e/ 1/7--cf Analysi 3? 46 Industrial Chemical & Solvents Division DATE: December 7, 2004 Product TOLUENE Tank 4 Trinaman Ship Date: de New Ship Quantity: fieSales Order Nec di Customer Order No: ii9 3 Indiana Analysis Description Limits Test Results API Gravity @ 60 Deg F (0 4052) 30.8 Specific Gravity (I 60 Deg F (0.4052) LBS/GAL/60 Deg F (P 4052) 0 569-0.873 0.5717 Imo Odor (0.1296) orst:teem Color ID 158) +30 Color PVCo (CI 1209) 20 max Less thin Copper Corrosion (0 849) Pass Pau Acid Wash Color (D 648) 2 man 2- Kaun Butenol Value (0 1133) Acidity (0 847) No Free Acid 10x.9 No Free Add Acidity (0 847) (Meq/kg) 0.019 Sulfur (D 853) Free Foie water Content (E 1064) (ppm) 229.0 Assay (G C) (16) 99.5 min 99.89 Paraffins (SC.) (ppm) 356.3 Benzene Content (G.C.) (ppm) 25.5 Eihylbenzene Content (G.C.) (ppm) 230.7 Xylenas (G.C.) (ppm) Xylanes & Ethyibanzens (G C) (ppm) 508.3 tp3,0 Disbilabon 10850) Deg C 109.6 Dry Point 110.6 Total Ordination Ring. 1.0 to include 110.6 1.0 Refractive Index@ 25 Deg C (D 1218) Appearance (Visual) 1.4940 Clear and free of sediment mikr suspended solIds 41QAL THE ABOVE ANALYSIS WAS PERFORMED SY INTERIM TESTING SERVICES. CALEB 5REIT, THE SAMPLE, As TESTED, CONFORMS TO ASMLINO CHEMICAL SAECIFICAT1014. taw* Caleb Brett December 7, 2004 Lab Rd: 0023511-001 A 4.44..A.1s CaMb Co/ftern, , 1. Ashland Distribution Company, Division of Ashland Inc.. Box 2219, Columbus, Ohio 43216 SW-Scearce 01369 Dec 07 04 01:057 Laboracor3 S13-941-2174 ' Ashland' 1191BABEW Ashland Distribution Company Division of Ashland Inc. '"'""Customer Certificate of Analysis 7.1111111.11/ 3 -/ s a so Industrial Chemical & Solvents Division DATE: December 7. 2004 Product TOLUENE Tank 4 Tran Ship Oats: New Alb Indian 4 Ship Quantity: 40. 09 Sales Order No: . Customer Order No: Ae)9, Lot No: 002868-001 Analysis Analysis Description Limits Test Results API &awry a 60 Deg F (0 4052) 30.11 Speck Gravity a 60 0e F (0-4052) 16SIGAU60 Del F (0 40521 Odor (0-12911) Color (0 156) 0.669-0.573 0.8717 .11260 b thuraderisas +30 Color PVCo(e 1209) 20 max Lase Copper Corrosion (0 649) Pass Pass Acid Wash Color (0 344) 2 max 2- Kaun Buirol Value (0 1133) 102.11 Acidity (0 547) No Free Acid No Fres Acidity (0 647) (WOO 0.019 Sulks (0 853) Frs. Free Water Content (5 1064) (ppm) Assay (G.C) 99.5 min 229.0 99.89 Paraffins (G.C.) (ppm) Benzene Content (0.0.) (ppm) Eltiyiberasne Coolant IG.C.) (ppm) Xylenes (D.C.) (ppm) Xylenes 6 ethyibenzene (G.C.) (ppm) 355.3 25.5 230.7 508.3 419.0 Distillation (0650) 0s0C Dry Paint Total Distillation Bangs 1.0 to include 110.8 109.5 110.8 1.0 Retractive index@ 25 Del C (0 1218) 1.4940 Appearance (Visual) Clear and free of sediment Indio! suspended solids gni THE ABOVE ANALYSIS WAS PERFOISIECI WV PITEATEX713reto sERvicEs. craze ssErr. Tme SAMPLE. As TESTED, CCAIPORMS TO ARUM CHEMICAL SPECIFICATION& ,l11.1,1 I 47;q kid A 11.10s11.111. enw.P09 Inisnak Caleb Brod Dicember 7, 2004 Lab Fish 002861401 t Ashland Distribution Company, Division or Mislaid Inc., Box 22)9, Columbus, Ohio 41216 SW-Scearce 01368 u ti c 07 04 02: 05p m.milM.sssssss1111 Laboratory .ss ss 513-941-2174 P 1 Ashland Ashland Distribution Company Division of Ashland inc. Customer Certificate of Analysis Industrial Chemical & Solvents Division DATE: December 7, 2004 c /CP r -11-re; (1.&41 4?*- 03 Cr 5 " a, Air Analysis i')- / 1:41 Product: TOLUENE Tank 4 Tranemon Ship Date: 0, New Alban Indiana 2A.-' Ship Quantity: Sales Order No: .4.1c:e2.,,/,.7.?/..i(479( ..-) 2/ 1/ Customer Order No: /4 .2 Lot No: 002858.001 Analysis Description Li mits Test Results aAPI Gravity 60 Deg F (0 4052) Specific Gravity 60 Deg F (0-4052) 0.869-0 873 30.5 0.8717 LBS/GA1160 Deg F (D 4052) 0260 b Odor (0-1298) theracterlstlo Color (0 158) Color Pt/Co (01209) 20 max *30 Lan than 5 Copper Corrosion (0 849) Pass Pass Acid Wash Color (0 848) 2 max 2- Kauri Sulam! Vskie (0 1133) 102. Acidity (0 847) No Free Acid No Fr Acidity (0 841) (WOO) Sulfur (0 853) Free 0.01A Free water Content (E 1084) (ppm) 229.0 Assay (G CI (1) 99.5 min 99.89 Paraffins (G.C.) (ppm) 356.9 Benzene Content (G.C.) (ppm) 25,5 Elhyibenzene Content (G.C.) (ppm) (G,C.) (ppm) Xylanas & Ethylbenzene (G C ) (ppm) 4 u1'230.7 508.3 toe. Distinalion (0550) Gag C 109.6 Dry Point 110.8 Talai Distillation Range Refractive Index@ 25 Deg C (0 1218) Appearance (Visual) 1.0 to Include 110.6 1.0 1.4940 Clear and free of sediment and/or has_ suspended solid* I)-15 ABOVE ANALYSIS WAS PERFORMED SY INTERTEN TESTING SERVICES. CALEB BRETT THE SAmPLE AS TESTED. CONFORMS TO ASHLAND CHEMICAL SPECIFICATIONS. trunk Caleb Brie December 7, 2004 Lab Ref: 002858.001 ^Ashland Distribution Company, Division of Ashland Inc., Box 2219, Columbus, Ohio 4 ii16 SW-Scearce 01367 Ashland Distribution Company Division of Ashland, Inc. P.O. Box 2219, Columbus, OH 43216 Customer Certificate ofAnalysis Ship Date: 5-2-5 Customer: Sherwin Williams Com an Onus Lone South Product Toluene Tank No.: tk169 03-17-10 HMIS 2300 w Vessel: TOLIJIN9 Richmond, KY 40475 Ship Quantity: 6712 Ticket: 23764 Fax 4: 614-790-6624 !C&5 PO / Lot No.: 4501174709-r3ce Attn: Dab Nist (IC&S Columbus) Analysis Test Method Customer PO No.: Specification 10233-1 Test Results Appearance Specific Gravity, L WO, Gravity, pounds/gallon Saybolt Color Pt / Co Color (APH A) Acid Wash Color Knurl-Bottum! Value Sulfur Compounds (H29, SO2) Sulfas, ppm Acidity Copper Strip Corrosion Saturates, % Bettesse, % Toluene, % Xylano, % > Xylene, % Initial Wiles Point, C Dry Point, C Dist. Range, C Water Content, ppm visas' D-891 0-4052 Cale D-15616045 0-1209 D-848 0-1133 0-853 D-5453 13-1147 D-13011149/18311 0-2306 0-2306 D-2306 0-2366 D-2306 0.850 D-11.50 D-850 Aquatest 0.869 to 0.173 report only report only 10 mos. report only report only report only report only report only 'report only OA max. 0.03 max. 99.5 mim 0.5 ntatt. 0.5 nos. 109.6 Mho. 111.6 max. 1 max. Clear ligaid, free of particulates 0.8711 7.260 30 3 ON 107 Nei 0.2 Net 1B 0.06 Not detected 90.92 0.01 0.00 110.4 110.6 0.2 23 Pass Puss Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pus Pass Pass Pass Pau Pass Pass And-S10 added angslal added z3 V-c- L/ ID 4 Itemnfriihlei rue rnainistv Ship111011 da Meridian Ashield Poralcan LLC, 11631 Rasa 23, Codemburg, Ky 41129. 606 -921 -6102 SW-Scearce 01366 SHLANID. ammE.1s.1. Ashland Distribution Company Division of Ashland, Inc. P.O. Box 2219, Columbus, OH 43216 Customer Certificate of Analysis Customer: Sherwin Williams Company Bons Lane South Richmond, KY 40475 Pax 4: 614-790-3085 Attn: Deb Nist (IC&S Columbus) Analysis Test Method Appearance Specific Gravity, g/mL (g60F Gravity, pounds/gallon Saybolt Color Pt I Co Color (A PH A) Acid Wask Color Knurl-Butanol Value Soifer Compounds (H2S, SO2) Sulfur, ppm Acidity Copper Strip Corrosion Saturates, % Benzene, % Toluene, % Xylene, > Xylem*, % initial Boiling Point, C Dry Point, C Dist. Range, C Water Content, ppm visual D-891 / D-4052 Cale D-156/6045 13-1209 D-848 D-1133 D-853 D-5453 D-847 D-130/849/1838 D-2306 D-2306 D-2306 D-2306 D-2306 D-850 D-850 D850 Aquntest Ship Date: 5.2.5 Product: Toluene 03-17-10 HMIS 2300 Tank No.: TK169 Vessel: TOLUENE Ship Quantity: 6596 Ticket 23766 IC&S PO / Lot No.: 4501174720-C3CP Customer PO No.: 10233-i Specification 0.369 to 0.873 report only report only 10 num report only report only report only report only report only report only 0.5 max. 0.03 max. 99.5 min. 03 max. 0.5 may. 109.6 min. 111.6 max. max. 500 max. Test Results Clear liquid, free of particulates 0.8718 7.260 30 3 ON 107 Nag 0.2 Nag 113 0.06 Not detected 99.92 0.02 0.00 110.4 110.6 0.2 23 Pass Pass Pass Pass Pass Pass Pus Pus Pus Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass 2.314- 1- Anti-Stns added ANIT-STAT YSO 9001:2000 A Responsible Care Company Shipment do Marathon Ashland Pctrolimm LI.C. 11631 Route 23, Caren:Min, Ky 41129, 1406-921-4802 SW-Scearce 01365 ASI-ILAVVE) - cc) Ashland Distribution Company Division of Ashland. Inc, P.O. Dos 2219, Columbus. 1)11 .11216 Customer Certificate of Analysis Ship Date: 8-4-05 Customer: Sherwin Williams Company Boggs Lane South Richmond. KY 40475 Fax iv 614490-3085 Attn: Deb Dist (IC&S Columbus) Analysis cm N,Irthod Product: Toluene 03-17-10 HMIS 2300 Tank No,: 170 Vessel: TOLUENE Ship Quantity: 6350 Ticket: 25904 .,,...-(("Per 1C&S PO / Lot No.: 4501243024-c3co. Customer PO No: 10233 Specification 1 est Results Appearance Specific G ravity. Wm 1.. 0601e Gravity, pounds/gallon Sayholt Color Pt / Co Color (APRA) Acid Waste Color Kauri-Butanol Value Sulfur Compounds (1125.502) Sulfur, ppm Acidity Copper Strip Corrosion Saturates, % Benzene, % Toluene. % Xylene. % a Xylene. % Initial Boiling Point, C Dry Point, C Dist. Range, C Water Content. ppm visual 13-1191 /11-44152 Cale D-156/6045 0-1209 D.414/4 13-1133 D-853 11-5453 9-847 D- 130/849/1838 D-2306 9-2306 9-2306 11-2306 D-2306 9-850 041511 D850 Aqua test 0.869 to 0.873 report only report only 10 max. report only report only report only report only report only report only 0.5 max, 0.03 max. 99.5 min. 11.5 max. 0.5 max. 11)9.6 min, 111.6 max. 1 max. 500 max. C:lear liquid, free of particulates 0.8718 7.2611 30 I ON 104 Neg 0.2 Nag IB 0.07 Not detected 99.91 0.02 0.00 110.4 110.6 -60.2 16 Pass Pass Pass NISS Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass ass ass Pass Anti-Slat added anti stab aitticamwia I 11 , PRtA I 1) 2z. ISO !OM 2000 A Responsible Can ('ompiny Shipment em Kindhon A:4%1mnd namlotto 1.1C. I 1631 Routs 23. Catlettsburg. Ky 41129. 606-921-61102 SW. Scearce 01364 ASHLAND. Ashland Distribution Company Division of Ashland. Inc. PA) Box 2219. Columbus, 01-I 43216 Customer Certificate of Analysis Customer Sherwin Williams Company Bogs Lane South Richmond, KY 40-175 Fax It. 614-790-3085 Attn: Deb NW (IC&S Columbus) Analysis Test Method Appearance Specific Gravity, g/ml, /1.060E Gravity. pounds/gallon Say holt Color Pt/ Co Color (APRA) Acid Wash Color Kaurl-Butanoi Vale* Sulfur Compounds (MS. SO2) Sulfur, ppm Acidity Copper Strip Corrosion Saturates, % Benzene, % Toluene, Y. Xylene, % > Xylene.% Initial Boiling Point. C Dry Point, C Dist. Range, C Water Content, ppm visual D-891 / 0-4052 Cale D-156/6045 0-1209 0-848 0-1133 D-853 D-5453 0-847 D-130/849/1838 D-2306 D-2306 D-2306 0-2306 0-2396 1)450 D-850 D-850 Aquatest Ship Dale: 08/04/05 Product: Toluene 03-17-101-1M15 230G Tank No : 170 Vessel: vy.lf..UENF. Ship Quantity: 6517 Tkket: 25902 t-* 9-r IC&S PO r Lot No.: 4501243027-C3C0 C'ustrimer PO No,: 10233 Specification 0.869 to 0.873 report only report only 10 max. report only report only report only report only report only report only 0.5 max. 0.03 max. 99.5 min. 0.5 max. 0.5 max. 109.6 min. 111.6 max. I max. 500 max. That Results Clear liquid, free of particulates 0,8718 7.260 30 ON 104 Nog 0.2 Ncg Iii 0.07 Not detected 99.911 0.02 0.00 1111.4 110.6 9.2 16 Pass Pass Pass ?ass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Puss Pass A nil-Slat addcd At% I'1-' TA f AD1W1) ii,n1k41 4 A Itcsponade Care Company Nhirrincni du Knathon Ashland IN:trolcuml.l.C. I 1 f)3 I Runic 23. Caltctiqhmu, Ky 41129. 606-021.68112 SW-Scearce 01363 ASHLANI D Ashland Distribution Company Division of Ashland. Inc. P.O. Box 2219. Columbus. OH 43216 Customer Certificate of Analysis Ship Data. 8/8/05 Customer: Sherwin Williams Company Boggs Lone Smith Fax tO Richmond, KY 40475 614- 790.30115 Attn: Deb Nist OCAS Columbus) Analysis Test Method Product: Toluene 03-17-10 HM1S 2300 Tank No.: 169 Vessel: TOLUENE Ship Quantity: (.317 Ticket. 1C&S PO / I sit No,: 45012441941C3C0 Customer PO No.: 10233 Specification Test Results Appearance Specific Gravity. g/m1.. Gravity, pounds/gallon Say bolt Color Pt / Co Color (APHA I Acid Wash Color Kauri-Butanol Value Sulfur Compounds (1125, 502) Sulfur, ppm Acidity Copper Strip Corrosion Saturates, `/.. Senz.ene. % Toluene, 'V. Xylene, % > Xylene, % Initial Boiling Point. C Dry Point, C Dist. Range, C Water Content, ppm visual D-891 / 9-4052 C'alc 9-i 50/60 45 D-1209 9448 D-1133 9-853 D-5453 13-847 D-1311/849/1838 D-2.106 9-2306 D-2306 D-2306 D-2306 0-8541 1)850 D-850 Aquatest 0.1460 fn 0.873 report only report only 10 max. report only report only report only report only report only report only 0.5 max. 0.03 man. 99.5 min. 0.5 max. 0.5 max. 109.6 min. 111.6 max. I max. 500 max. Clear liquid, free of particulates 0.8715 7.260 311 .1 ON 104 Nee 0.1 Neg 1I) 0.08 Not detected 99.86 0.07 0.00 110.2 110.6 0.4 31) Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass AnnSux added AN ti-STAT AD1)1:13 REL tl /2046 JF- APPRoV111 ISO !111: 2001 A RcsponSibtO Care Ci.mpany Shipmeni Mmailion 14111and olvtim 11.C. 11631 R11.114e 23. Calk:11%66m, ky 11129 604-921 -6302 nt-11294 L SW-Scearce 01362 .AS11-11LIVNE) Ashland Distribution Company Division of Ashland, Inc. P.O. Box 2219, Columbus, OH 43216 Customer Certificate of Analysis Ship Dote: 8-9-05 Customer: Sherwin Williams Com Product: Toluene 03-17-10 HMIS 230a Boggs Lane South Tank No.: 1b9 Vessel: TOLUENE Richmond, KY -10475 Ship Quantity: 6355 Ticket: Fax #- 614-790-3085 IC&S PO / Lot No.: 4501244193-C3C0 Attn: Deb Nist (IC&S Columbus) Analysis Test Method Customer PO No.: Specification 102.33 That Results Appearance Specific Gravity, g/mL Gravity. pounds/gallon Saybolt Color P11 Co Color (APHA) Arid Wash Color Kaurt-Butsmol Value Sulfur Compounds (112S, S02) Sulfur, ppm Acidity Copper Strip Corrosion Saturates, % Benzene, Toluene. Vu Xylene, % > Xylene. Initial Roiling Point, C Dry Point. C Dist. Range, C Water Content, ppm visual D-891 / D-4052 Cale 0-156/6045 It-12119 D-848 0-1133 0-853 0-5453 0-847 D-130/84911838 D-2306 0-2306 0-2306 0-2306 D-2306 D-850 D-850 0-850 Aquatest 0.869 to 0.873 report only report only 10 max. report only report only report only report only report only report only 0.5 max. 0.03 max. 99.5 min. 9.5 max. 0.5 max. 109.6 min. 111.6 mac. 1 mac. 500 max. Clear liquid, free of particulates 11.8718 7.260 30 4 ON 104 Nes 0.1 Ns& . 10 0.08 Not detected 99.86 0.07 0.00 110.2 110.6 11.4 30 Pass Pass Pass Pass P ass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Aan-Stai added RI.1.1:1SE NO-1 ANTI-STAT ADDED- 3N1 M1, KR I RUCs( e-* 2 'g3 ( s 6775'0 Mlit0VED ISO 9011: 21100 A Roponsibir Carr Companl 411tipmcm do Marathon A thland PeiroLaim 11.C, 1101 Roma 23,4,'411cuthorg, Ky 41120, 406-021-61102 IU-31234 SW-Scearce 01361 AsPrAiNo Ashland Distribution Company Division of Ashland. Inc. P.O. Box 2219, Columbus. OH 43216 Customer Certificate of Analysis Ship Date: 9/15/05 Customer: Sherwin Williams Company Boggs Lana South Richmond, KY 40475 Product: Toluene rank No.: 169 Ship Quantity: 6351 43-11-10 !MIS 230(1 Vessel: TOLUENE Ticket: 26878 Fax #: 614-790-3085 1C&S PO / Lot No.: 4501270327-C.3C0 Attn: Deb Nist (IC&S Columbus) Analysis Tim Method Customer PO No.. Specification 10233-1 Test Results Appearance Specific Gravity. g/m L ru)60F Gravity, pounds/gallon Say bolt Color Pt / Co Color (APHA) Acid Wash Color Knurl-Batons)! Value Sulfur Compounds (H2S, S02) Sulfur, ppm Acidity Copper Strip Corrosion Saturates, % Benzene," Toluene, 'Ya Xyleae, % > Xylem, % Initial Boiling Point, C Dry Point, C Dist. Range, C Water Content, ppm visual D-1191 / D-4052 Cale D.156/6045 D-1209 D-848 D-1133 0-853 D-5453 0-847 0-130/849/1838 0-2306 D-2306 D-2306 D-2306 D-2306 0-850 0-850 D-850 Aquatest 0.1169 to 0.873 report only report only 10 max. report only report only report only report only report only report only 0.5 max. 0.03 max. 99.5 min. 0.5 max. 0.5 max. 109.6 min. 111.6 malt. 1 max. 500 max. Clear liquid. free of particulates 0.8718 7.260 30 3 ON 145 Neg 0.2 Neg 1B 9.07 0.01 99.67 0.03 0.02 110.1 110.6 0.5 77 Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass ( /0 Ann-Sun added ANTISTA r Aniwri F AppRovi..rs) 150 /11101! ZOOS A Roponsible Cult C'onipan!. Shipment c/u Marathon Ashland Petrol atm 1.10. 11631 Route 23, Catlettsburg, Ky 41129, 6M-921.61402 SW-Scearce 01360 .ASJIALANI Ashland Distribution Company 1)ivision or Ashland. Inc 1'.0 13ox 2219. Columbus. OH 41216 Customer Certificate of Analysis Ship Date: 9- 15- 05 Customer: Sherwin Williams Company Boggs Lane South Richmond, KY 40475 Product: Toluene Tank No.: 169 Ship Quantity: 6366 03 - 17 - 10 HMIS 230G Vessel: TOLUENE Ticket: 26881 Fax 4: 614-790-3085 Attn: fhb Nist (C&S Columbus) Analysis Test Method ICikS PO / Lot No.: C ustomer PO No. 4501270339-C3CO 10233-1 Specification 'lest Results Appearance Specific Gravity. g/mL Ca76OF Gravity, pounds/gailon Saybolt Color Pt / Co Color (APHA) Add Wash Color Kaurl-Butanol Value Sulfur Compounds (1125.502) Sulfur. ppm Acidity Copper Strip Corrosion Saturates. % Benzene, % Toluene, % Xylene, % Xylene, *A, Initial Boiling Point. C Dry Point, C Dist. Range.. C Water Content, ppm visual 0-891 / 0-4052 Cale 1)-156/6045 0-1109 13-841. 0-1133 D-853 0-5453 0-847 0-130/849/1838 0-2,306 l)-2306 0-2306 0-2306 0-2306 0-850 D-850 0.850 Aquatest 0.869 to 0.873 report only report only 10 nu m. report only report only report only report only report only report only 0.5 max. 0.03 max. 99.5 min. 0.5 max. 0.5 max. 109.6 min. 111.6 max. 1 max. 500 max. Clear liquid, free of particulates 0.11718 7.260 30 3 ON 105 Neg 0.2 Neg in 0.07 0.01 99.87 0.03 0.02 110.1 110.6 0.5 77 Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass 1 5953 ip r nitStat added ANTI c rAT Al gmn ISO 9001:2100 A Respnn.ihle Cate Company shipment c'u aturatttott Ashland Petroleum LLC. 11631 Rome. 23, Cmitnihtirg. 14.y 41 I 2t . 606-921-611!72 SW-Scearce 01369 ASH1LANIEP Ashland Distribution Company Division of Ashland, Inc. P.O. Box 2219. Columbus. 011 43216 Customer Certificate of Analysis Ship Date: 9/23/05 Customer Sherwin Williams Company Product: foluene 11F1-17-1011311S 2300 Boggs Lane South Tank No.: 169 Vessel: TOLUENE Richmond. KY 40475 Ship Quantity: 6917 Ticket: 27114 Fax 614-790-3085 !CAS PO / Lot No.: 4501276607-C3C0 Ann: Deb NW (IC&S Columbus) Analysis Test Method Customer PO No.: Specification 10233-1 Test Results Appearance Specific Gravity. g/mL /0601r Gravity. pounds/gallon Saybolt Color Pt / Co Color (APHA) Acid Wash Color Ksturi-Butnnel Value Sulfur Compounds (MS, S02) Sulfur, ppm Acidity Copper Strip Corrosion Saturates, % Benzene, % Toluene. 3/4 Xylem.% > Xylene, Initial Boiling Point, C Dry Point, C Dist. Range. C Water Content, ppm visual 0-891 / 0-4052 Cale D-156/6045 13-1209 9-848 0-1133 13-853 0-5453 0-847 0-130/849/1838 D-2306 0-2306 0-2306 D-2306 D-2306 D-850 0-850 0-850 Aquntest 0.869 to 0.873 report only report only 10 max. report only report only report only report only report only report only 0.5 max. 0.03 max. 99.5 Milt. 0.5 max. 0.5 Inns. 109.6 rain. 111.6 max. 1 max. 500 max. Clear liquid, free of particulates 0.8718 7.260 30 3 ON 105 Neg 0.2 Neg 113 0.05 0.01 99.88 0.05 0.00 110.2 110.6 0.4 51 Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass kati-Star adLkd NPPROV V a t.ISO 9081:2888 A Respormthie Cate Compan% Shipment c/o piarathon Ashland Petroleum 1.1.C, 11631 Route 23. Callet hurg, Ky 4 I 129. 6116-921-68112 IM-3$234 SW-Scearce 01358 As1--stANo Ashland Distribution Company Division of Ashland, Inc. P.O. Box 2219. Columbus, OH 43216 Customer Certificate of Analysis Ship Date: 9/23/05 Customer: Sherwin Williams Company Boggs Lane South Richmond KV 40475 Product: Toluene Tank No.: 169 Vessel: Ship Quantity: 11633 Fax 4: 614-790-3085 IC&S PO / Lot No.. 4501276608-C3C0 Attn: Deb Nis* (1C&S Columbus) Analysis Test Method Customer PO No.: Specification 10233-1 Test Results Appearance Specific Gravity, g/mL 4460F Gravity, pounds/gallon Seybolt Color Pt / Co Color (APH A) Acid Wash Color Katiri-Butanol Value Sulfur Compounds (H25. 502) Sulfur. ppm Acidity Copper Strip Corrosion Saturstes,II4 Benzene, % Toluene, % Xylene, > Xylem % initial Boiling Point. C Dry Point, C Dist. Range, C Water Content, ppm visual D-1491 / D-4052 Cale D.156/6045 D-1209 D-848 D-1133 D-853 0-5453 D-547 D-130/849/1838 D-2306 D-2306 D-2306 D-2306 13-2306 13-850 0-850 D-850 Aquatest 0.869 to 0.873 report only report only 10 max. report only report only report only report only report only report only 0.5 max. 0.03 max. 99.5 min. 0.5 max. 0.5 max. 109.6 min. 111.6 max. I max, 500 max. Clear liquid, free of particulates Pass 0,8718 Pass 7.260 Pass 30 Pass 3 Pass ON Pnss 105 Pass Meg Pass 0.2 Pass Meg Pass I13 Pass 0.05 Pass 0.01 Pass 99.88 Pass 0.05 Pass 0.00 Pass 110.2 Pass 110.6 Pass 0.4 Pass Pass Anti-Slat 4r.lticd Ise 9081:2000 A Responsihk Care Company Shiplricnt clo Mnranion Ashland Petroleum I.I.C. I Ih3I Rome 23, Cailenshilrg.,, Ky 41129. 606-921.61102 ra- 3023.6 SW-Scearce 01357 Oct 05 OS 12:37p Laboratory 513-943 -2174 p. 1 'Ashland Ashland Distribution Company Division of Ashland Inc. Customer Certificate of Analysis Industrial Chemical & Solvents Division DATE: October 5, 2005 Product TOLUENE A Tank 4 fiLl2ensmon a, New Man Indiana Ship Date: 1WerarlaTAIW: cuaxixtr '11 Ship Quantity: -l cSales Order No ...v. .510 d,c) (.0;5 Lot No: 002339.001 OFFAMINIVIIIEFAMMVAESIaillWffer I- Analysis e Analysis Description API Gravity rfl 60 Deg F (D 4052) Specific Gravity@ 60 Deg F (0.4052) LBS/GAU60 Deg F (0 4052) Odor (0-1296) Color (0 156) Color PUCo (13 1209) Copper Corrosion (D 849) Acid Wash Color (01548) Kauri Butanol Value (0 1133) Acidity (D 847) Acidity (D 647) (Meolkg) Sulfur (0 853) Water Content (E 1064) (ppm) Assay (G.c) (x) Paraffins (G.C.) (ppm) Benzene Content (G.C.) (ppm) Ethytbenzene Content (G C.) (ppm) Xylenes (G.c.) (ppm) Xylenes & Ethylbenzene (G.c.) (ppm) Dislillatian (0850) Deg C Dry Pont Total DistIlialion Range Refractive index* 26 Deg C (0 1216) Appearance (Visual) Limits 0.869-0.873 20 max Pass 2 max No Free Acid Free 99.5 min 1.0 to include 110.8 Nom THE ABOVE ANALYSIS WAS PERFORMED SY INTER/EX TESTING SERVICES, CALEB THE SAMPLE. AS TESTED, CONFORMS TO ASHLAND CHEMICAL SPECIFICATIONS. Test Results 30.9 0.8714 7.255 Characteristic *30 Less than 5 Pass 2104.9 No Free Acid 0..188 Free 93 99.91 394.7 48.4 168.4 194.1 360.5 110.3 110.8 0.3 1.4940 Clear and free of sediment mkt suspended solids t 307q? ateb Drell October 5, 2005 Lab Rat: 002339401 A;i1,0041C st Cogvapp Ashland Distribution Company, Division of Ashland Inc., Box 2219, Columbus, Ohio 43216 SW-Scearce 01356 Oct 05 05 12:37p Laboratory 513-541-2174 p.1 'A''''ilsahllialgaEnll.1d61 1 !"1111111111W1 Ashland Distribution Company Division of Ashland Inc. Customer Certificate of Analysis C us er: ( 011-411-426dade: COO YE) industrial Chemical & Solvents Division DATE: Octobe 5, 2005 Product: TOLUENE Tank 4 Trans tai. ne, New Albin Indiana Ship Date: eASOF Ship Quantity: Sales Order No: (J/t2'Reea. Customer Order No: "Cc:A .53 . Lot No: 002339-001 Analysis Description API Gravity t 60 Deg F (D 4052) Specific Gravity 60 Deg F (D-4052) LIZ/GAL/60 Deg F (0 4052) Odor (0-1296) Color (0 156) Color PVCo (0 1209) Copper Corrosion (0 849) Acid Wash Color (0 848) Kaun Butancil Value (13 1133) Acidity (0 847) Acidity (0 847) (Meg/kg) Sulfur (C) 853) Water Content (E 1064) (ppm) Assay (G.C) (%) Paraffins (G.C.) (ppm) Benzene Content (G.C.) (ppm) Ethylbenzens Content (G C) (ppm) xytenes (C.C.) (ppm) Xylenes & Eihybenzene (G.12,) (ppm) Distillabco (0850) Deg C Dry Point Total Distillation Range Refractive indexfa 26 Deg C (0 1218) Appearance (Visual) Limits 0.859-0.873 20 max Pass 2 max No Free Acid Free 99.5 min 1.0 to Include 110 6 THE ABOVE ANALYSIS WAS PERFORMED BY INTERTEK TESTING SERVICES, CALEB BR THE SAMPLE, AS TESTED, CONFORMS TO ASHLAND CHEMICAL SPECIFICATIONS. Test Results 30.9 013714 7.255 Characteristic +30 Less than 5 Pass 2- 104.9 No FMB Acid 0..188 Free 93 99.91 394.7 48,4 166.4 194.1 360.5 110.3 110.6 0.3 1.4940 Clear and free of sediment andlor suspended solids 1 3 0 t.VY 2_ 3-0 3 gob Brett October 5, 2005 Lab Rol: 002339-00 1 4ONNOW.014Cacoll. CAP.Voi. 7 Ashland Distribution Company, Division of Ashland Inc., Box 2219, Columbus, Ohio 43216 03 SW-Scearce 01355 "511-11LP1NE) Ashland Distribution Company Oivision .V.hlond. Inc. PA) [lox 2219. (:olumbus. 1)1-1 41216 Customer Certificate of Analysis Ship Date: 10/22/05 Customer: . Sherwin Williams Company Product: Toluene 17-l0^ 1 ii 5330E MVOs 1.ane South Richmond, KY 40475 lank No.. 169 Ship Quantity: 6389 Vessel: TOLL ENE Ticket: Fax 4: 614-790-3085 Attn: Deb Nist (IC&S Columbus) Analysis req Method IC&S PO / Lot No.' Customer PO No.: 4501298651-C3C0 10233-1 t 2 a.g)9Q Sped lit:81ton rest Results Appeal-erica Specific Gravity, glint, 6060F Gravity, pounds/gallon Saybolt Color Pt / Co Color (APHA) Acid Wash Color Kauai-Butanol Value Sulfur Compounds (125.502) Sulfur, ppm Acidity Copper Strip Corrosion Saturates, % Benzene. % Toluene, % Xylene, % Xytene,% Initial Boiling Point. C Dry Point. C Dist. Range. C Water Content. ppm visnxl D-8911 0-4052 Cale 0-156/6045 D-1209 0-848 0-1133 0-853 1)-5453 D-847 D-130/849/1838 0-2306 0-2306 0-2.306 D-2306 0-2306 0-850 0-850 04150 Aqualest 0.869 to 0.873 report only report only 10 mos. report only report only report only report only report only report only 0.5 max. 0.03 max. 99.5 min. 0.5 max. 0.5 max. 109.6 min. 111.6 mat. I max. 500 max. Clear liquid, free of particulates 0.8718 7.260 30 3 ON 106 Neg 0.1 Neg In 0.06 Not detected 99.93 0.01 0.00 110.4 110.6 0.2 26 Pass Pass Pass Pass Pass Plus% Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass A no-SA.4 44.Idell AN I 1-'.TAT 11/111 A Responsible Carr Company Shipman* ein Mariolum A,IllinitlPulanleum1.1.C. 110;1 Rome 23. C.iikitti,buriL bey 41 1 29, 606-421-FMO2 SW-Scearce 01354 ASPit"NICP Ashland Distribution Company Division of Ashland. Inc. P.O. Box 2219. Colurntrus, OH 43216 Customer Certificate of Analysis Ship Date: 11-15-5 Customer: Sherwin Williams Company Product: Toluene 03-17-10 HMIS 230G Boos Lane South Tank No.: 170 Vessel: TOL UENE Richmond, KY 40475 Ship Quantity: 6408 Ticket 28365 Fax 614-790-3085 IC&S P0/ lot No: 4501315212-CICO Attn: Deb Nist (1C&S Columbus) Analysis Test Method Customer PO No.: Specification 10133-1 Tot Results Appearance Specific Gravity, g/m L r4m01 7 Gravity,pounds/gl Say bolt Color Pt / Co Color (AMA) Acid Wash Color Kn url-Butanol Value SulOar Compounds (1125. SO2) Sulfur, ppm Acidity Copper Strip Corrosion Satu rates, % Benzene.% Toluene, % Xylem!, % > Xylem. % Initial Boiling Point, C Dry Point, C Dist. Range. C Water Content, ppm visual 9-891 / D-4052 Cale 11-156/6045 11-1209 11-848 D-I 133 9-853 D-5453 D-847 9-130/849/1838 9-2306 9-2306 0-2306 D-2306 9-2306 D-850 D-850 D-850 %gustiest 0.1169 to 0.873 report only report only 10 max. report only report only report only report only report only report only 0.5 max. 0.03 max. 99.5 min. 0.5 max. as max. 109.6 min. 111.6 max. 1 max. 500 max. Clear liquid, free of particulates 0.8718 7,260 30 ON 107 Nag 0.1 Meg I 13 0.05 Not detected 99.94 0.0t 0.00 110.5 110.6 6920.1 25. Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass Anti-Mat added AN11-srm Ammin 6 31 g 5 . I. ePfi - APPROVED ISO $001:2000 Responsible Cure Company slupineni Maiinhon Achkintl. Petroleum I IC, 11631 Route 23. CatIcit.iburg, Ky 11129, 606-92 I -6802 En-30234 SW-Scearce 01353 Designation: D841 - 10 INTERNATIONAL Standard Specification for Nitration Grade Toluene' This standard is issued under the fixed designation D841; the number immediately following the designation indicates the year of original adoption or. in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. I. Scope* 1.1 This specification covers nitration grade toluene. L2 The following applies to all specified limits in this standard: for purposes of determining conformance with this standard, an observed value or a calculated value shall be rounded off "to the nearest unit" in the last right-hand digit used in expressing the specification limit, in accordance with the rounding-off method of Practice E29. 1.3 Consult OSHA regulations, supplier's Material Safety Data Sheets, and local regulations for all materials used in this specification. 2. Referenced Documents 2.1 ASTM Standards:" D848 Test Method for Acid Wash Color of Industrial Aromatic Hydrocarbons D849 Test Method for Copper Strip Corrosion by Industrial Aromatic Hydrocarbons D85() Test Method for Distillation of Industrial Aromatic Hydrocarbons and Related Materials D1209 Test Method for Color of Clear Liquids (Platinum- Cobalt Scale) D2360 Test Method for Trace Impurities in Monocyclic Aromatic Hydrocarbons by Gas Chromatography D3437 Practice for Sampling and Handling Liquid Cyclic Products D5386 Test Method for Color of Liquids Using Tristimulus Colorimetry D7504 Test Method for Trace Impurities in Monocyclic Aromatic Hydrocarbons by Gas Chromatography and Effective Carbon Number E29 Practice for Using Significant Digits in Test Data to This specification is under the jurisdiction of ASTM Committee D16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee D16.01 on Benzene, Toluene. Xylenes, Cyclohesane and Their Derivatives. Current edition approved Jan. I, 2010. Published February 2010. Originally approved in 1945. Last previous edition approved in 2002 as D841 -- 02. D01: 10.1520/D0841-10. For referenced ASTM standards. visit the ASTM website, www.astm.org , or contact ASTM Customer Service at service@astm.org . For Annual Book of ASTM Suan-laals volume information. refer to the standard's Document Summary page on the ASTM wchsite. Determine Conformance with Specifications 2.2 Federal Specification: 3 PPP-C-2020 Packaging of Chemicals, Liquid, Dry, and Paste 2.3 Other Document: OSHA Regulations, 29 CFR paragraphs 1910.1000 and 1910.1200 4 3. Properties 3.1 Nitration grade toluene shall conform to the following requirements; Property Nonaromatic hydrocarbons, max, volume % (wt %) Acid wash color, max Copper corrosion Appearance Color, Pt/Co scale, max Specification 1.5 (1.2) pass with 2 pass (1A or 113) e 20 Distillation range including the temperature 110.6C at 101.3 kPa (760 mm Hg pressure), max,' C 1.0 ASTM Test Method A D2360 or D7504 D848 D849 D1209 or D5386 D850 A If more than one method is listed, the producer and user should agree on the referee method. 8 Clear liquid free of sediment and haze when observed at 18.3 to 25.6C (85 to 78F). 4. Sampling 4.1 The material shall be sampled in accordance with Practice D3437. 5. Packaging and Labeling for U.S. Government Procurements 5,1 United States Government procurements shall be packaged and labeled in accordance with the applicable paragraphs of Fed. Spec. PPP-C-2020. 6. Keywords 6.1 toluene Available from Standardization Documents Order Desk. DODSSP, fildg. 4, Section D, 700 Robbins Ave.. Philadelphia, PA 19111-5098, IMO/ www.dodssp.daps.mil . Available from U.S. Government Printing Office Superintendent of Documents. 732 N. Capitol St., NW, Mail Stop: SDP., Washington. DC 20401. hupari www.access.gpo.gov . *A Summary of Changes section appears at the end of this standard. Copyright 0 ASTM international, 100 Barr Harbor Drive, PO Box C700, west Conshohocken, PA 19428-2959, United States. Copyright by ASTM Inf1 (all rights reserved); Mon Jul 12 18:28:35 EDT 2010 i Downlade/pritby Stephen Petty 0 pursuant to License Agreement. No further reproductions authorized ,  D841 -- 10 SUMMARY OF CHANGES Committee 1716 has identified the location of selected changes to this standard since the last issue (17841 - 02 (2008)'') that may impact the use of this standard. (Approved January 1, 2010.) (/) Added method for composition, Test Method 1)7504 in Table in 3.l ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights. and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, at the address shown below. This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States, Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website (wwwastm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/ COPYRIGHT/). Copyright by ASTM Intl (ail rights reserved); Mon Jul 12 18;28:35 EDT 2010 2 Downloadedlprinted by Stephen Petty () pursuant to License Agreement. No further reproductions authorized. NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Contact ASTM International (www.astm.org ) for the latest information. Designation: D 2306 -- 00 INTERNATIONAL Standard Test Method for C8 Aromatic Hydrocarbon Analysis by Gas Chromatography' This standard is issued under the fixed designation D 2306: the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (E) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method determines the relative distribution of the individual C 5 aromatic hydrocarbon isomers in the following xylem products: 1.1.1 Nitration grade xylene conforming to Specification D 843. 1.1.2 Xylenes for p-Xylene feedstock conforming to Specification D 5211, 1.1.3 Ten-degree xylene conforming to Specification D 846. 1.2 The absolute concentration of hydrocarbon impurities typically found in commercially available mixed Cg aromatic hydrocarbons should be determined using Test Method D 2360. 1.3 The following applies to all specified limits in this test method: for purposes of determining conformance with this test method, an observed value or a calculated value shall be rounded off "to the nearest unit" in the last right-hand digit used in expressing the specification limit, in accordance with the rounding-off method of ASTM Practice E 29. 1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appmpriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 9. 2. Referenced Documents 2.1 ASTM Standards: D 843 Specification for Nitration Grade Xylene 2 U 846 Specification for Ten-Degree Xylene 3 D 2360 Test Method for Trace Impurities in Monocyclic Aromatic Hydrocarbons by Gas Chromatography' D 3437 Practice for Sampling and Handling Liquid Cyclic Products = This lest method is under the jurisdiction of ASTM Committee D16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee 016.01 on Benzene. Toluene. Xylenes, Cyclohexane, and Their Derivatives, Current edition approved June 10, 2000. Published August 2000. Originally published as D 2306 --64. Last previous edition D 2306 -- 96. 2 Annual Book of ASTM Standards, Vol 06.04. Discontinued 1991. See 1990 Annual Book of ASTM Stondanls. Vol 06.03. D 3797 Test Method for Analysis of o-Xylene by Gas Chromatography 2 D 3798 Test Method for Analysis of p-Xylene by Gas Chromatography' D 4626 Practice for Calculation of Gas Chromatographic Response Factors 4 D 4790 Terminology of Aromatic Hydrocarbons and Related Chemicals' 1) 5060 Test Method for Determining Impurities in HighPurity Ethylbenzenc by Gas Chromatography 2 D 5211 Specification for Xylenes for p-Xylene Feedstock' E 29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications' E 260 Practice for Packed Column Gas Chromatography' F 355 Practice for Gas Chromatography Terms and Rela- tionships' E 691 Practice for Conducting an Interlaboratory Test Pro- gram to Determine the Precision of Test Methods' 2.2 Other Docuntent: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.12006 3. Terminology 3.1 Definitions: 3.1.1 For definition of terms used in this test method sec Terminology D 4790. 4. Summary of Test Method 4.1 The specimen is introduced into a gas chromatograph equipped with either a flame ionization detector (FID) or thermal conductivity detector (TCD). Either packed or capillary columns are permitted. The peak area of each component is measured and the weight percent concentration is calculated by dividing the peak area of the individual component by the sum of the total individual peak areas. The result is multiplied by 100 to get the normalized C8 aromatic hydrocarbon isomer distribution. 'Annual Rook of ASTM Standanis, Vol 05.02. 3 Annual Book of ADM Standards, Vol 14.02. " Available from the Superintendent of Documents, U.S. Government Printing Office, Washington. DC 20402. Copyright O ASTM International, 190 Barr Harbor Drive. PO Box C702, West Conshohocken. PA 19428-2959. United States. Copyright by ASTM Intl (all rights reserved); Mon Jul 12 18:28:34 EDT 2010 Downloaded/printed by Stephen Petty 0 pursuant to License Agreement. No further reproductions authorized. ,,NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Contact ASTM International (www.astm.org ) for the latest information. cet D 2306 - 00 5. Significance and Use 5.1 This test method is suitable for setting specifications on the materials referenced in 1.1.1 through 1.1.3. This test method may also be used as an internal quality control tool and in development or research work. 5.1.1 Refer to Methods D 5060, I) 3797, and D 3798 to determine the purity of ethylbenzene, o-xylene, and p-xylene respectively. 5.2 This test method does not attempt to determine the absolute purity of the sample, but defines the relative distribution of the C8 aromatic hydrocarbons. 6. Interferences 6.1 If present, nonaromatic hydrocarbons of twelve carbons or greater will he interferences in this analysis. 7. Apparatus 7.1 Gas Chromatograph-Any instrument having a flame ionization detector or a thermal conductivity detector may be used. A flame ionization detector is preferred. 7.2 Columns-Both capillary and packed columns containing a stationary phase of cross-linked polyethylene glycol have been found satisfactory. The column and instrumental conditions described in Table I are recommended. 7.3 Recorder-Electronic integration is recommended. 8. Reagents 8.1 Carrier Gus-Chromatographic grade hydrogen, helium or nitrogen have been found acceptable. 11. Preparation of Apparatus 11.1 The method used to prepare packed columns is not critical provided that the finished column produces the desired separation. 11.2 Follow manufacturer's instructions for mounting and conditioning the column into the chromatograph and adjusting the instrument to the conditions described in Table 1. Allow sufficient time for the equipment to reach equilibrium. See Practices E 260 and E 355 for additional information on gas chromatography practices and terminology. 11.3 The column must be capable of resolving the C 8 aromatic hydrocarbons as individual isomers. 11.3.1 The resolution of two components is defined as follows: ,) R- ' w (I) where: tRm i > tR.p peak resolution, retention time of m-xylene, (m = m-xylene), tR. p retention time of p-xylene, (p = p-xylene), W = peak width at baseline for m-xylene, and W b ,p = peak width at baseline for p-xylene. 11.4 For p-xylene and m-xylene, the minimal allowable resolution is 1.0. If the resolution between p-xylene and m-xylene is <1.0, the chromatographic system must be modi- fied to improve the separation. 9. Hazards 9.1 Consult current 081 -1A regulations, supplier's Material Safety Data Sheets, and local regulations for all materials listed in this test method. 10. Sampling 10.1 Sample the material in accordance with Practice 1) 3437. TABLE 1 Instrumental Parameters Column A Detector Column: Tubing Stationary phase Film thickness, p Length, m Inside diameter, mm Temperatures: Infector,* C Detector, Oven: C Time 1, min Final, C Rate, C/min Time 2, min Carrier gas Linear vol., cm/s Split ratio Sample size, pL Analysis time, min flame ionization fused silica polyethylene glycol 025 50 0.25 200 250 70 10 120 5 0 helium 20 100:1 1.0 20 12. Procedure 12.1 Inject the desired volume of specimen into the gas chromatograph and record the peaks on the sensitivity setting that allows the maximum peak height and minimum baseline noise. The injection volume should be small enough to produce symmetrical gaussian shaped peaks. Fig. 1 illustrates a typical analysis. 13. Calculations 13.1 Determine the area defined by each peak. 13.1.1 In the event that a thermal conductivity detector is used for the analysis, the observed peak areas may need to be adjusted using response factors. Sec Practice D 4626 for a discussion on response factors. 13.2 Calculate the weight percent concentration of each C 5 aromtichydbnsflow: (A; )(100) C, - (As) (2) where: C = concentration of component i, = peak area of component i, and = peak area of all C, aromatic isomers. 14. Report 14.1 Report the individual C, aromatic hydrocarbons to the nearest 0.01 weight %. Copyright by ASTM Intl (all rights reserved); Mon Jul 12 18:28:34 EDT 2010 2 Downloaded/printed by Stephen Petty () pursuant to License Agreement. No further reproductions authorized. NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Contact ASTM International (www.astm.org ) for the latest information. D 2306 - 00 MX 990 I PS E-91912 g . 9.21 OX 11.97 TOL IL 40 1P11 11.27 I MMO 13.92 r-.1--r- T - T-rr-T -77 T-T- 1 - T-T .1- r- r-r -1. , 0 T --r. -1-1- 7-r- r7 -0 -1- 1-1.- r -/ 'T-T- T-T- 7- 'T 'T-1. 'T - i ..-i- T- i 5.0 3.0 7.0 41.0 9.0 10.0 11.0 12.0 13.0 14.0 15.0 FIG. 1 Chromatogram of Mixed Xylenes Using Conditions for Column A, Table 1 15. Precision and Bias 15.1 The following criteria should be used to judge acceptability (95 % probability level) of results obtained by this test method. The criteria were derived from an interlaboratory test amongst 10 laboratories. The data were run on 2 days using different operators using a sample that was gravimetrically prepared from the individual C8 aromatic hydrocarbons to the concentrations listed in Table 2. Fused silica capillary columns TABLE 2 intermediate Precision (formerly called Repeatability) and Reproducibility Component Expected Concentration Weight% Intermediate Average Precision Concentration (formerly Reproduc- Reported called ibility Weight % Repeat- ability Elhylbenzene p-Xylene m-Xylene o-Xylene 17.93 20.16 44.09 17.83 17.92 20.07 43.96 17.98 0.077 0.073 0.101 0.116 0.153 0.193 0.369 0.193 containing a polyethylene glycol stationary phase were used by 9/10 laboratories. Flame ionization detection was used by all 10 laboratories. The results of the round robin were analyzed in accordance with Practice E 69]. Supporting data are available from ASTM International Headquarters. Request RR: D16-1015. 15.1.1 Intermediate Precision (formerly called Repeatability)-Results in the same laboratory should not be considered suspect unless they differ by more than the amount for repeatability shown in Table 2. On the basis of test error alone, the difference between two test results obtained in the same laboratory on the same material will be expected to exceed this value only about 5 % of the time. 15.1.2 Reproducibility-Results submitted by each of two laboratories should not be considered suspect unless they differ by more than the amount shown for reproducibility in Table 2. On the basis of test error alone, the difference between two test results obtained in different laboratories on the same material will be expected to exceed this value only about 5 % of the time. 15.2 Bias-Although the interlaboratory test utilized a sample prepared gravimetrically from individual C8 isomers obtained at the highest purity available, this sample has not been approved as an acceptable reference material and consequently bias has not been determined. 15.2.1 As an aid for the users in determining the possibility of bias, calculated C8 distributed for the round robin sample is listed in Table 2 as the "Expected Concentration." The average value for each C3 isomer as calculated from the reported concentrations is listed as "Average Concentration Reported." 16. Keywords 16.1 aromatic hydrocarbon; aromatic hydrocarbon analysis; C3 ; gas chromatography; isomer;p-Xylene; xylene Copyright by ASTM Intl (all rights reserved); Mon Jul 12 18:28:34 EDT 2010 3 Downloadediprinted by Stephen Petty () pursuant to License Agreement, No further reproductions authorized. NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Contact ASTM International (www.astm.org ) for the latest information. (41114) D 2306 -- 00 ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, at the address shown below. This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700. West Conshohocken, PA 19428-2959, United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above address or at 610-832-9585 {phone), 610-832.9555 (fax), or service@astm.org (e-mail); or through the ASTM website (www.astmorg). Copyright by ASTM Intl (alt rights reserved); Mon Jul 12 18:28:34 EDT 2010 4 Downloaded/printed by Stephen Petty 0 pursuant to License Agreement. No further reproductions authorized. NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Contact ASTM International (www.astm.org ) for the latest information Designation: D 2360 -- 03 INTERNATIONAL Standard Test Method for Trace Impurities in Monocyclic Aromatic Hydrocarbons by Gas Chromatography This standard is issued under the fixed designation D 2360: the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (E) indicates an editorial change since the last revision or reapproval. This slumlord has been approved for use by agencies of the Department of Defense. 1. Scope* 1, I This test method covers the determination of the total nonaromatic hydrocarbons, and trace monocyclic aromatic hydrocarbons in the purity of toluene and mixed xylenes by gas chromatography. 1.2 Nonaromatic aliphatic hydrocarbons containing I through 10 carbon atoms (methane through decanes) can be detected by this test method at concentrations ranging from 0.001 % to 2.500 weight %. 1.2.1 A small amount of benzene in mixed xylenes may not be distinguished from the nonaromaties and the concentrations are determined as a composite. 1.3 Monocyclic aromatic hydrocarbon impurities containing 6 through 9 carbon atoms (benzene through C9 aromatics) can be detected by this test method at individual concentrations ranging from 0.001 % to 1.000 weight %. 1.4 The following applies to all specified limits in this test method: for purposes of determining conformance with this standard, an observed value or a calculated value shall be rounded off "to the nearest unit" in the last right-hand digit used in expressing the specification limit, in accordance with the rounding-off method of Practice E 29. 1.5 This standard does not purport to address all or the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish applypriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statement, see Section 9. 2. Referenced Documents 2.1 ASTM Standards: D 841 Specification for Nitration Grade Toluene' D 2306 Test Method for C i, Hydrocarbon Analysis by Gas Chromatography' This test method is under the jurisdiction of ASTM Committee D16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee 016.01 on Benzene, Toluene, Xylenes, Cyclohesane and Their Derivatives. Current edition approved June 10, 2003. Published July 2003. Originally approved in 1966. Last previous edition approved in 2000 as 1) 2360 -- 00. Annual Book of ASTM Siandards, Vol 06.04. D 3437 Practice for Sampling and Handling Liquid Cyclic Products' D 3797 Test Method for Analysis of o-Xylene by Gas Chromatography' D 3798 Test Method for Analysis of p-Xylene by Gas Chromatography' D 4492 Test Method for Analysis of Benzene by Gas Chromatography' D 4790 Terminology of Aromatic Hydrocarbons and Related Chemicals' D 5211 Specification for Xylenes for p-Xylene Feedstock' E 29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications 3 E 260 Practice for Packed Column Gas Chromatography" E 355 Practice for Gas Chromatography Terms and Rela- tionships' E 691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method' E 1510 Practice for Installing Fused Silica Open Tubular Capillary Columns in Gas Chromatographs' 2.2 Other Document: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.1200 5 3. Terminology 3.1 Definitions: 3.1.1 For definition of terms used in this test method see Terminology D 4790, 4. Summary of Test Method 4.1 A known amount of an internal standard is added to the specimen that is then introduced into a gas chromatograph (GC) equipped with a flame ionization detector (FTD). The peak area of each impurity and the internal standard is measured and the amount of each impurity is calculated from the ratio of the peak area of the internal standard versus the peak area of the impurity. Purity by GC is calculated by Annual Baak of ASTM .57andaids, Vol 14.02. Anima Book of ADM SlawkLmis, Vol 03.06. Available from Superintendent of Documents, U.S. Government Printing Office, Washington DC 20402. *A Summary of Changes section appears at the end of this standard. Copyright ASTM International, 100 Barr Harbor Olive. PO Bon C700, West Conshohocken, PA 1442B- 2959, United States. Copyright by ASTM (all rights reserved); Mon Jul 12 18:28:38 EDT 2010 I Downloaded/printed by Stephen Petty () pursuant to License Agreement. No further reproductions authorized.  D 2360 -- 03 subtracting the sum of the impurities found from 100.00. Results are reported either in weight percent or volume percent. 5. Significance and Use 5.1 The determination of hydrocarbon impurities contained in toluene and mixed xylenes used as chemical intermediates and solvents is typically required. This test is suitable for setting specifications and for use as an internal quality control tool where aromatic monocyclic hydrocarbons are produced or are used. This test method is applicable for determining the impurities from the aromatic hydrocarbon production process. Typical impurities are alkancs containing 1 to 10 carbon atoms, benzene, toluene, ethylbenzene (EB), xylenes, and aromatic hydrocarbons containing nine carbon atoms. 5.1.1 Refer to Test Methods D 3797, D 3798, and D 4492 for determining the purity of o-Xylene,p-Xylene, and benzene, respectively. 5.1.2 Refer to Test Method D 2306 for determining the C g aromtichydbnsruoimxedylns. 5.2 Purity is commonly reported by subtracting the determined expected impurities from 100.00. However, a gas chromatographic analysis cannot determine absolute purity if unknown or undetected components are contained within the material being examined. 6. Interferences 6.1 The internal standard chosen must be satisfactorily resolved from any impurity and the product peak. A peak will be satisfactorily resolved from a neighboring peak if the distance from the valley to the baseline between the two peaks is not greater than 50 % of the peak height of the smaller of the two peaks. 6.2 In some cases for mixed xylenes, it may be difficult to resolve benzene from the nonaromatic hydrocarbons and therefore the concentrations are determined as a composite. In the event that the benzene concentration must be determined, an alternate method must be selected to ensure an accurate assessment of the benzene concentration. 7. Apparatus 7. I Gas Chromatograph --Any instrument having a flame ionization detector that can be operated at the conditions given in Table 1. The system should have sufficient sensitivity to obtain a minimum peak height response for 10 mg/kg n-butylbenzene of twice the height of the signal to background noise. 7.2 Columns--Both capillary and packed columns containing a stationary phase of cross-linked polyethylene glycol have been found satisfactory. The column must give satisfactory resolution of the internal standard from the solvent and the impurity peaks, and should be such that benzene is eluted between n-nonane and n-decane. Table 1 contains a description of a column that has been found satisfactory. 7.3 Recorder--Electronic integration is recommended. 7.4 Microsyringe, 10 and 50, and 500-pL capacity. 7.5 Volumetric Flask, 50-mL capacity. TABLE 1 Instrumental Parameters Detector Column: Tubing Stationary phase Film thickness, p Length, m Diameter, mm Temperatures: Injector, C Detector, C Oven: Initial, C Time 1, min Final, C Rate, C/min Time 2, min Carrier gas Flow rate, mLlmin Split ratio Sample size, pL Analysis time, min Linear velocity @ 145"C, cm/s Flame ionization fused silica crosslinked polyethylene glycol" 0.25 60 0.32 ID 270 300 60 10 150 5 10 helium 1.0 100:1 1.0 30 20 A Polyethylene glycol such as Carbowax 20 M available from most chromatographic suppliers, has been found suitable for this purpose. 8. Reagents 8.1 Purity of Reagent--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where such specifications are available. 6 8.2 Carrier Gas--Chromatographic grade helium is recommended, 8.3 High Purity p-Xylene, 99.999 weight % or greater purity. 8.3.1 Most p-xylene is available commercially at a purity less than 99.9 % and can be purified by recrystallization. To prepare 1.9 L of high purity p-xylene, begin with approximately 3.8 L of material and cool in an explosion-proof freezer at --10 -- 5C until approximately 1/2 to 3/4 of the p-xylene has frozen. This should require about 5 h. Remove the sample and decant the liquid portion. The solid portion is the purified p-xylene. Allow the p-xylene to thaw and repeat the crystallization step on the remaining sample until the p-xylene is free of contamination as indicated by gas chromatography. 8.4 Pure Compounds, for calibration, shall include n-nonane, benzene, toluene, ethylbenzenc (EB), o-xylenc and cumene. The purity of all reagents should be >99 weight %. If the purity is less than 99 %, the concentration and identification of impurities must be known so that the composition of the standard can be adjusted for the presence of the impurities. 8,4.1 Internal Standard--n-butylbenzene (NBB) is the recommended internal standard of choice, however, other compounds may be found acceptable provided they meet the criteria as defined in Section 6. Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by the American Chemical Society, see Aerial- Standards lire Laboratory Chemicals, 13131.1 Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharmacopeia! Convention. Inc. (USPC), Rockville, MD. Copyright by ASTM Intl (all rights reserved); Mon Jul 12 111:28:38 EDT 2010 2 Downloaded/printed by Stephen Petty O pursuant to License Agreement. No further reproductions authorized. (440, D 2360 - 03 9. Hazards 9.1 Consult current OSHA regulations, supplier's Material Safety Data Sheets, and local regulations for all materials used in this test method. 10. Sampling 10.1 Sample the material in accordance with Practice D 3437. 11. Preparation of Apparatus 11.1 Follow manufacturer's instructions for mounting and conditioning the column into the chromatograph and adjusting the instillment to the conditions described in Table 1 allowing sufficient time for the equipment to reach equilibrium. See Practices E 260 and E 355 and E 1510 for additional information on gas chromatography practices and terminology. 12. Calibration 12.1 Prepare a synthetic mixture of high purity p-xylene with representative impurities. The volume of each hydrocarbon impurity must be measured to the nearest 0.1 AL and all liquid reference compounds must be brought to the same temperature before mixing. Refer to Table 2 for an example of a calibration blend. The nonaromatic fraction is represented by n-nonane, while o-xytene represents the xylene fraction. Cumenc will represent the aromatic hydrocarbons containing nine carbon atoms or greater (C, aromatics). 12.2 Using the exact volumes and densities in Table 2, calculate the weight percent concentration for each impurity in the calibration blend as follows: C = ,}(Vi))II(Vp )(Dp ))(100) (I) where: = density of impurity i from Table 2, = volume of impurity i, mLs, DV,,IY = density of p-xylene from Table 2, = volume of p-xylene, mLs, and = concentration of impurity i, weight percent. 12.3 Into a 50-mL volumetric flask, add 50.0 L of n-butylbenzene (NBB) to 50.00 mLs of the calibration blend and mix well. Assuming a density of 0.857 for the calibration blend and 0.856 for NBB, the resulting NBB concentration will be 0.100 weight %, as determined from the equation in 12.2. 12.3.1 All solutions and reference compounds must be brought to the same temperature, preferably 25C, prior to adding the internal standard. 12.4 Inject the resulting solution from 12.3 into the chromatograph. A typical chromatogram is illustrated in Fig. 1. 12.5 Determine the response factor for each impurity relative to NBB by measuring the area under each peak and calculate the relative response factor as follows: (cKRF, (AMC?) : 00,) (2) where: RRF, = response factor for impurity i relative to the internal standard, A, = peak area of impurity, i, = peak area of the internal standard, N1313, C,. = concentration of the internal standard, NBB, weight percent, and C, = concentration of impurity i, as calculated in 12.2, weight percent. 12.6 Calculate the response factors to the nearest 0.001. 13. Procedure 13.1 Bring the internal standard and the sample to be analyzed to identical temperatures, preferably 25C. Make sure that the temperature of the sample is consistent with that of the calibration standard prepared in Section 12. Pipet 50.0 tiL of internal standard into a 50-mL volumetric flask containing 50.00 mLs of sample. Mix well. 13.2 Depending upon the actual chromatograph's operating conditions, inject an appropriate amount of sample into the instrument. Make sure that the injection amount is consistent with those conditions used to meet the criteria in 7.1. 13.3 Measure the area of all peaks except the major component(s). Measurements on the sample must be consistent with those made on the calibration blend. The nonaromatic fraction includes all peaks up to toluene (except for the peak assigned as benzene). Sum together all the nonaromatic peaks and report as a total area. The C9 aromatics fraction includes cumene and all peaks emerging after o-xylene. Sum together all the C9 aromatic peaks and report as a total area. TABLE 2 Preparation of Calibration Blend Compound Density' Recommend ed Vofurne (ul) Resulting Concentration Volume Percent Weight Percent p-Xylene (see 8.3.1) Benzene Toluene Ethylbenzene o-Xylene Cumene n-Nonane 0.857 0.874 0.862 0.863 0.876 0.857 0.714 50.00 mL 10.0 10.0 50.0 50.0 10.0 10.0 99.72 0.020 0.020 0.100 0.100 0.020 0.020 99.72 0.020 0.020 0.101 0.099 0.020 0.017 .4Density at 25 C. Values obtained from Physical Constants of Hydrocarbons to C., a , ASTM Publication Data Series 4A, 1971. ii 5.00 10.00 moo 20.00 FIG. 1 Typical Analysis of Calibration Standard Copyright by ASTM Intl (all rights reserved); Mon Jul 12 18:28:38 EDT 2010 3 Downloaded/printed by Stephen Petty () pursuant to License Agreement. No further reproductions authorized. ARY D 2360 - 03 13.4 Fig. 2 illustrates the analysis of Specification D 841 toluene, Fig. 3 illustrates the analysis of Specification D 5211 mixed xylenes. 14. Calculations 14.1 Calculate the weight percent concentration of the total nonaromatics and each impurity as follows: (A ,)(RRE ,)(C,) CI- (A) (3) 14.2 Calculate the volume concentration of the total nonaromatics, total C9 aromatics and each trace aromatic as follows: V; (4) where: V, = concentration of impurity r , volume percent, and Di = density of impurity i from Table 2. D, = density of sample 14.3 Calculate the purity of the sample as follows: purity, weight percent = 100.00 - C, (5) where: C, = total concentration of all impurities, weight percent. 15. Report 15.1 Report the following information: 15.1.1 Individual impurities to the nearest 0.001 %. 15.1.2 Concentrations of impurities less than 0.001 %, report as <0.001 %, and consider as 0.000 in summation of impurities, 15.1.3 Total impurities to the nearest 0.01 %, and 15.1.4 Purity as "purity (by GC)" to the nearest 0.01 %. iI11 5.00 10.00 15.00 20.00 FIG. 3 Typical Analysis of Specification D 5211 for Xylenes 16. Precision and Bias 16.1 Precision-The following criteria should be used to judge the acceptability of the 95 % probability level of the results obtained by this test method. The criteria was derived from the round-robin between seven different laboratories. The data from five laboratories was used in calculating the precision data for toluene. Two samples were analyzed. Each sample was run twice in two days by two different operators. Results of the interlaboratory study were calculated and analyzed using Practice E 691. 16.1.1 The numbers in parentheses shown in the left hand column of Table 3 are reported average concentrations of the TABLE 3 Repeatability and Reproducibility Toluene Intermediate Precision Reproducibility Nonaromatics (0.023) Ethylbenzene (0.017) p-Xylene (0.010) m-Xylene (0.012) o,Xylene (0.001) Toluene (99.94) Mixed Xylenes 0.0067 0.0041 0.0038 0.0031 0.0003 0.0160 Intermediate Precision 0,0110 0.0063 0.0038 0.0040 0.0003 0.0210 Reproducibility Nonaromatics (2.526) Toluene (0.649) Cumene (0.010) Xylenes (96.82) 0.150 0.052 0.0007 0.180 0.816 0.153 0.0013 0.819 MINUTES FIG. 2 Typical Analysis of Specification D 841 on Toluene impurities. 'Supporting data are available from ASTM International Headquarters. Request RR: Di 6-1020. Copyright by ASTM Intl (all rights reserved); Mon Jul 12 18:28:38 EDT 2010 4 Downloaded/printed by Stephen Petty () pursuant to License Agreement, No further reproductions authorized.  D 2360 -- 03 16.2 Intermediate Precision, (formerly called Repeatability)--Duplicate results by the same operator should not be considered suspect unless they differ by more than - the amount shown in Table 3. All values are in weight percent. 16.3 Reproducibility--The results between two laboratories should not be considered suspect unless they differ by more than the amount shown in Table 3. All values are in weight percent, 16.4 Bias--Since there was no accepted reference material available at the time of interlaboratory testing, no statement on bias can be made at this time. All values are in weight percent. 17. Keywords 17.1 impurities; purity; toluene; xylenes SUMMARY OF CHANGES Committee D16 has identified the location of selected changes to this standard since the last date of issue (D 2360 - 00) that may impact the use of this standard. (1) Corrected Equation 4. (2) Added definition of D, after Equation 4. (3) Corrected Table 2 reference to p-Xylene from 7.3. I to 8,3.1. ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. It you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, at the address shown below. This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States. individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above address or at 610-832-9585 (phone), 810-832-9555 (fax), or service@astmorg (e-mail); or through the ASTM website (www.astm.org). Copyright by ASTM lnt'l (all rights reserved); Mon Jul 12 18:28:38 EDT 2010 5 Downloaded/printed by Stephen Petty () pursuant to License Agreement, No further reproductions authorized. NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Please contact ASTM International (www.astm.org ) for the latest information. Designation: D 4367 - 02 Standard Test Method for Benzene in Hydrocarbon Solvents by Gas Chromatography' This standard is issued under the fixed designation D 4367; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. 1. Scope* 1.1 This test method covers the determination by gas chromatography of benzene at levels from 0.01 to I volume % in hydrocarbon solvents. No-rE 1-For benzene levels lower than 0.01 volume %, use Test Method D 62291) 6229. 1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only. 1.3 For purposes of determining conformance of an observed or a calculated value using this test method to relevant specifications, test result(s) shall be rounded off "to the nearest unit" in the last right-hand digit used in expressing the specification limit, in accordance with the rounding-off method of Practice E 29.E 29 1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 1.5 For hazard information and guidance, see the supplier's Material Safety Data Sheet. For specific hazard statements, see Section 7. 2. Referenced Documents 2.1 ASTM Standards: D 6229 Test Method for Trace Benzene in Hydrocarbon Solvents by Capillary Gas Chromatography' E 29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications 3 E 300 Practice for Sampling Industrial Chemicals' 3. Summary of Test Method 3.1 An internal standard, methyl ethyl ketone (MEK), is added to the material and then introduced into a gas chromatograph equipped with two columns connected in series. The ' This test method is under the jurisdiction of ASTM Committee D01 on Paint and Related Coatings, Materials, and Applications and is the direct responsibility of Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved Dec. 10. 2002. Published February 2003. Originally approved in 1984. Last previous edition approved in 1999 as D 4367 - 99. = Annual Book of ASTM Standards, Vol 06.04. Annual Rook of ASTM Standards, Vol 14.02. Discontinued; see 2001 Annual Book of ASTM Standards, Vol 15.05. specimen passes first through a column packed with the nonpolar phase, methyl silicone, which separates the components by boiling point. After octane has eluted, the flow through the nonpolar column is reversed, flushing out the components heavier than octane. The octane and lighter components then pass through a column with the highly polar phase, 1,2,3-tris(2-cyanoethoxy)propane, that separates the aromatic and nonaromatic compounds. The eluted components are detected by a conventional detector and recorded on a strip chart. The peak areas are measured and the concentration of each component is calculated by reference to the internal standard. 4. Significance and Use 4.1 Benzene is classed as a toxic and carcinogenic material. A knowledge of the concentration of this compound may be an aid in evaluating the possible health hazards to persons handling and using hydrocarbon solvents, but this test method is not intended to evaluate such hazards. 5. Apparatus 5.1 Chromatograph-Any gas chromatographic instrument that has a backflush system and flame ionization detector and that can be operated at the conditions given in Table 1. The detector-recorder combination must produce a 4-mm deflection for a 1-1IL specimen containing 0.05 volume % MEK when operated at maximum sensitivity. 5.2 Columns, one 0.8-m (2.5-ft) length of 3.2-mm (1/4-in.) outside diameter stainless steel tubing and one 4.6-m (15-ft) length of 3.2-mm ( 1/8-in.) outsider diameter stainless steel tubing. 5.3 Recorder, Strip Chart-Potentiometer with a full-scale deflection of l mV, a full-scale response time of 2 s or less, and a maximum noise level of - 0.3 % of full scale. 5.4 Microsyringe, 5-JAL capacity. 5.5 Pipets, measuring 1 and 2 mL, graduated in 0.01 mL; 5, 10, and 20-mL capacity. 5.6 Flasks, volumetric, 25 and 100-mL capacity. 5.7 Vibrator, electric. 5.8 Vacuum Source. 5.9 Evaporator, vacuum, rotary. 5.10 Flask, boiling, round-bottom, short-neck, with 24140 T joint, 500-mL capacity. Suitable for use with the evaporator (see 5.9). *A Summary of Changes section appears at the end of this standard. Copyright *ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States. 1 NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Please contact ASTM Internatio I (www.astm.org ) for the latest information. 1111 D 4367 - 02 TABLE 1 Instrument Conditions Found Satisfactory for Measuring Low Concentrations of Benzene in Hydrocarbon Solvents (Note 2) Detector Columns Length, m Outside diameter, mm Stationary phases Support Reference column Temperature, C Injection port Column, isothermal Detector block Carrier gas Flow rate, mL/min Recorder range, mV Chart speed, mm/min Specimen size, iL Time to backilush, min Total cycle time, min flame ionization two, stainless steel (A) 0.81 (B) 4.6 3.2 (A) methyl silicone, 10 weight % (B) TCEP, 25 weight % (A) acid-washed calcined diatomite, 60 to 80-mesh (B) acid-washed pink diatomaceous earth, 80 to 100mesh any column or restriction may be used 150 100 150 helium approximately 30 0 to 1 10 1.0 approximately 2 approximately 30 5.11 Lamp, infrared. 5.12 Burets, automatic, with integral reservoir, 25-mL capacity. Nora 2-Suppliers of stationary phases and supports can be found in Research Report RR:D01-1038, available from ASTM International Headquarters. 6. Reagents and Materials 6.1 Purity of Reagents-Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where such specifications are available. 5 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination. 6.2 Acetone. 6.3 Chloroform. 6.4 Diatomaceous Earth 6-Acid-washed, 60 to 80 mesh and 80 to 100 mesh. 6.5 Helium, 99.99 % pure. 6.6 Methanol. 6.7 Methylene Chloride. 6.8 Methyl Ethyl Ketone (MEK), 99.9 mol %. 6.9 Methyl Silicone.' 6.10 1,2,3-Tris(2-Cyanoethoxy) Propane (TCEP). 6 6.11 Calibration Standards. 6.11.1 Benzene, 99+ mol %. 6.11.2 Isooctane, 99+ mol %. 6.11.3 n-Nonane, 99+ mol %. s Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by the American Chemical Society, see Analar Standards for Laboratory Chemicals, FIDH Ltd., Poole. Dorset, U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharmacopeia] Convention, Inc. (USPC), Rockville, MD. 6 See Note 2. 7. Hazards 7.1 Many hydrocarbon solvents are flammable and hazardous; use special precautions when handling them. Of the reagents used in this procedure, methanol, chloroform, methylene chloride, acetone, methyl ethyl ketone, benzene (see 4.1), and n-nonane are hazardous. 7.2 Benzene is volatile and highly flammable. Exercise care to prevent accidental ignition. Benzene is also carcinogenic and toxic; acute or chronic poisoning may result from inhalation of benzene vapor, absorption of benzene through the skin, or drinking benzene. 8. Sampling 8.1 Take samples of solvents to be analyzed by this test method using the procedures described in Practice E 300E 300. 9. Preparation of Columns 9.1 Column Packing Preparation-Preparethe two packing materials, one containing 10 % methyl silicone and the other 25 % TCEP, as follows: 9.1.1 Weigh 45 g of the acid-washed calcined diatomite support 60 to 80 mesh, into a 500-mL flask (see 5.10). Dissolve 5 g of the methyl silicone in approximately 50 rnL of chloroform. (Warning-Chloroform is a toxic material and inhalation must be avoided.) Pour the methyl silicone-chloroform solution into the flask containing the support. Attach the flask to the evaporator (see 5.9), connect the vacuum, and start the motor. Turn on the infrared lamp and allow the packing to mix thoroughly until dry. 9.1.2 Weigh 75 g of acid-washed pink diatomaceous earth, 80 to 100 mesh, into a 500-mL flask (see 5.10). Dissolve 25 g of TCEP in 200 mL of methanol and pour into the flask containing the support. Attach the flask to the evaporator (see 5.9), connect the vacuum, and start the motor. Turn on the infrared lamp and allow the packing to mix thoroughly until dry, but do not heat the packing above 180C. 9.2 Column Preparation: 9.2.1 Clean the stainless steel tubing as follows: Attach a metal funnel to one end of the steel tubing. Hold or mount the stainless steel tubing in an upright position and place a beaker under the outlet end of the tubing. Pour about 50 mL of methylene chloride into the funnel and allow it to drain through the steel tubing into the beaker. Repeat the washing with 50 mL of acetone. Remove the funnel and connect the steel tubing to an air line, by means of vinyl tubing. Remove all solvent from the steel tubing by blowing filtered, oil-free air through or applying a vacuum. 9.2.2 Pack the 0.8-m (2.5-ft) tubing (Column A) with the methyl silicone packing (see 9.1.1) and the 4.6-m ( I 5-ft) tubing (Column B) with the TCEP packing (see 9.1.2) as follows: Preform Columns A and B separately to fit the chromatographic instrument. Close one end of each tubing with a small, glass wool plug and connect this end to a vacuum source by means of a glass-wool packed tube. To the other end connect a small polyethylene funnel by means of a short length of vinyl tubing. Start the vacuum and pour the appropriate packing into the funnel until the column is full. While filling each column, vibrate the column with the electric vibrator to settle the 2 NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Please contact ASTM Internatio t (www.astm.org ) for the latest information. D 4367 - 02 packing. Remove the funnel and shut off the vacuum source. Remove the top 6 mm ( 1/4 in.) of packing and insert a glass wool plug in this end of the column. 9.3 Prepacked columns conforming to specifications listed in Table 1, and in 5.2, 9.1, and 9.2 may be obtained from any reputable chromatography supply company. (s) Forward Flow 10. Preparation of Chromatographic Apparatus and Establishment of Conditions 10.1 Column Conditioning--Join Columns A and B as shown in Fig. 1. Connect the inlet of Column A to the injection port of the chromatograph. Pass helium gas through the column at approximately 40 mL/min. Condition the columns in accordance with the following time-temperature schedule. Temperature, C 50 100 150 170 Time, h 1/2 1 3 10.2 Connect the outlet of Column B to the detector port. Adjust the operating conditions to those listed in Table 1, but do not turn on the detector circuits. Check the system for leaks. 10.3 Adjust the flow rate as follows: 10.3.1 Set the value in the forward flow mode (Fig. 2(a)) and adjust Flow Controller A to give the required flow rate (Table 1). Measure the flow rate at the detector vent, specimen side. 10.3.2 Set the valve in the backflush position (Fig. 2(b)) and measure the flow rate at the detector vent, specimen side. If the rate has changed, adjust Flow Controller B to obtain the required flow rate to within t..1 10.3.3 Turn on the detector circuit. Change the valve from forward flow to the backflush position several times and observe the baseline. There should be no baseline shift or drift after the initial peak resulting from the pressure surge with the COLUMN El TcEP _ -- -- --- 1 REFERENCE SIDE 174 FLOW CONTROLLER C) PRESSURE INDICATOR A- PORT SWITCHING VALVE CARLE INSTRUMENTS CO. CAT. NO. NO34. FULLERTON, CA DR EQUIVALENT INJECTION POI; T FIG. 1 Tubing Assembly and Instrumentation (b) Backflush COLA ---0 VENT COL FIG. 2 Flow Switching System REFERENCE valve change. If there is a baseline shift, slightly increase or decrease flow with Controller B to balance the baseline. (A persistent drift indicates leaks somewhere in the system.) 10.4 Determine time before backflushing, which varies for each column system and must be determined experimentally as follows: 10.4.1 Prepare a mixture of 5 volume % isooctane in n-nonane. Using the injection technique described in 11.3 and with the system in the forward flow mode, inject 1 pl., of the isooctane--n-nonane mixture. Allow the chromatogram to run until the n-nonane has eluted and the recorder pen has returned to baseline. Measure the time in seconds from the injection until the recorder pen returns to baseline between the isooctane and n-nonane peaks. At this point all of the isooctane but essentially none of the n-nonane should have eluted. One half of the measured time approximates the time to backflush and should be from 30 to 120 s. 10.4.2 Repeat the run, including the injection, but switching the system to the backflush mode at the determined backflush time. This should result in a chromatogram of isooctane with little or no n-nonane evident. 10.4.3 If necessary, make additional runs, adjusting the time to backflush until a chromatogram of all the isooctane and little or none of the n-nonane is obtained. This established backflush time, including the actual valve operations, must be used in all subsequent calibrations and analyses. 11. Calibration and Standardization 11.1 Standard Solutions--Prepare seven standard solutions covering the range of 0 to 1 volume % benzene as follows: For each standard, measure the volume of benzene listed below into a 100-mL volumetric flask. Dilute to volume with isooc- tane, with all components and glassware at normal room temperature, and mix thoroughly. Volume % Benzene mL 3 NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Please contact ASTM Internatio I (www.astm.org ) for the latest information. D 4367 -- 02 1 0.5 0.25 0.10 0.05 0.01 0.005 1 0.5 0.25 0.10 0.05 0.01 0.005 11.2 Calibration Solutions--Accurately measure 0.5 mL of MEK into a 100-mL volumetric flask, fill to the mark with the first standard solution (see 11.1), and mix thoroughly. Repeat with each of the other standard solutions. 11.3 Chromatographic Analysis--Using the conditions established in 10.3 and 10.4, chromatograph each of the calibration solutions after injecting them as follows: Flush the 5-1.11L microsyringe at least three times with the calibration solution and then fill with about 3 1.1L, avoiding inclusion of air bubbles in the syringe. Slowly eject the material until 1.0 ;IL remains in the syringe. Wipe the needle with a tissue and draw back the plunger to admit I pi, of air into the syringe. Insert the needle of the syringe into the septum cap of the chromatograph and push through the septum until the barrel of the syringe is resting against the septum cap; then rapidly push the plunger to the hilt and immediately withdraw the needle from the injection port. Nom 3--This injection technique is necessary to obtain sharp symmetrical peaks. 11.4 Calibration--Measure the areas of the benzene and of MEK peaks by conventional means (Note 4). Calculate the ratio of the benzene peak area to the MEK peak area. Plot the concentration of benzene versus the ratio as in Fig. 3. The calibration must be done to ensure that the entire chromatographic system is operating properly and that the concentration of any one component has not exceeded the linear response range of any part of the system--column, detector, integrator, and other components. The calibration plot should be linear (Note 5). Determine the retention times for each component for future identification. NOTE 4--The precision statement in Section 15 was developed from results obtained using electronic integrators or on-line computers. The precision statement may not apply if other methods of integration or peak area measurement are used. NOTE 5--If the calibration is linear, a least-squares calculation may be performed to obtain a calibration factor. The precision statement in Section 15 was developed from results obtained from calibration plots and may not apply if calibration factors are used. 12. Procedure 12.1 Test Solution--Accurately measure 0.5 mL of MEK into a 100-mL volumetric flask. Fill to the mark with the material under test and mix well. 12.2 Chromatograph a specimen from the test solution using the conditions established in 10.3 and 10.4 and the injection technique described in 11.3. Nom 6--The valves must be turned to the backflush mode at the established backflush time so that undesirable components do not enter Column 13. EUZON K, VOL, 2 1sss.1.INNFEN.smFIN. EMMIMIL=MELIO11==. ssIM s=.1ss=11IN=IMNWYSISM,11. 1s3/MMM=0MaliMIIMMCMERIMif s sss 1=1=Mi MMERMAXSUItailEVIWaa =UMW O Laboratory A Laboratory B Laboratory C Laboratory o Laboratory E NOTE 1--Determine for each analytical system. FIG. 3 Typical Calibration Curve for Benzene 4 4 NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Please contact ASTM internatio0 I (www.astm.org ) for the latest information. D 4367 - 02 UN IDENTI FIED RECORDE R RE SPONSE 12.3 Identify on the chromatogram the benzene and the internal standard MEK peaks from the retention times of the standards. NOTE 7--The order of elution is nonaromatic hydrocarbons, benzene, MEK, and toluene when using the specified columns, as shown in Fig. 4. 12.4 Measure the areas under the benzene peak and under the MEK peak by conventional methods. 13. Calculation 13.1 Calculate the ratio of peak area of benzene to the peak area of MEK. Read from the calibration curve the volume % of benzene corresponding to the calculated peak ratio. 13.2 If the results are desired on a weight basis, convert to weight % as follows: Benzene, weight % = (1110) X 0,8844 4 TIME, MINUTES FIG. 4 Typical Chromatogram where: V = benzene, volume %, and D = relative density of sample at 15.6/15.6 C (60/60 F). 14. Report 14.1 Report the following information: benzene content in volume or weight % to the nearest 0.005 %. 15. Precision and Bias 7 15.1 Precision--The precision statements are based on an interlaboratory study in which analysts in each of six laboratories analyzed seven hydrocarbon solvent samples, including heptane, VM&P naphtha, mineral spirits, toluene, and aromatic solvent 100 on two different days. To each solvent, initially containing essentially no benzene, 0.1 to 0.5 volume % benzene was added. The within-laboratory standard deviation was found to be 0.0094 % absolute with 42 df and the betweenlaboratory standard deviation was 0.022 % absolute with 49 df. Based on these standard deviations, the following criteria should be used for judging the acceptability of results at the 95 % confidence level: 15.1.1 Repeatability--Two results, each the mean of duplicates, obtained by the same operator on different days should be considered suspect if they differ by more than 0.027 % absolute. 15.1.2 Reproducibility--Two results, each the mean of duplicates, obtained by operators in different laboratories should be considered suspect if they differ by more than 0.063 % absolute. 15.2 Bias--Bias can not be determined for this test method because there is no available material having an accepted reference value. 16. Keywords 16.1 benzene content; gas chromatography; hydrocarbon solvents ' Supporting data are available from ASTM International Headquarters. Request RR:D01-1038., SUMMARY OF CHANGES Committee D01.35 has identified the location of selected changes to this standard since the last issue (D 4367 - 99) that may impact the use of this standard. (1) Added reference to Practice E 29E 29 in 1.3 of the Scope section. (2) Added Practice E 29E 29 to list of Referenced Documents. 5 NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Please contact ASTM Internatio I (www.astm.org ) for the latest information. D 4367 - 02 ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination or the vaiidiry or any such patent rights, and the 1155 of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM international Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you !eel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, at the address shown below. This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above address or at 610-832-9585 (phone), 610-832-9555 (fax), or service eastm.org (e-mail); or through the ASTM website (wwwastm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/ COPYRIGHT!). 6 NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Contact ASTM International (www.astm.org ) for the latest information. Designation: D 6563 - 00 INTERNATIONAL Test Method for Benzene, Toluene, Xylene, (BTX) Concentrates Analysis by Capillary Column Gas Chromatography' This standard is issued under the fixed designation D 6563; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method covers the determination of the total nonaromatic hydrocarbons, benzene, toluene, ethylbenzene, xylenes, and C 9 + aromatic hydrocarbons in BTX concentrates by capillary column gas chromatography. This test method is applicable to materials with a final boiling point below 215C. 1.2 Individual components can be determined from 0.01 to 90 %. 1.3 The following applies to all specified limits in this standard: for purpose of determining conformance with this standard, an observed value or a calculated value shall be rounded off "to the nearest unit" in the right-hand digit used in expressing the specification limit, in accordance with the rounding-off method of Practice E 29. 1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For a specific precautionary statement, see Section 9. 2. Referenced Documents 2.1 ASTM Standards: D 3437 Practice for sampling and Handling Liquid Cyclic Products' E 29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications' E 355 Practice for Gas Chromatography Terms and Rela- tionships' E 691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method' ' This test method is under the jurisdiction of ASTM Committee D16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee D16.01 on Benzene, Toluene, Xylenes, Cyclohexane, and Their Derivatives. Current edition approved June 10, 2000, Published August 2000, 2 Annual Book of ASTM Standards, Vol 06.04, Annual Book of ASTM Standards, Vol 14.02. E 1510 Practice for Installing Fused Silica Open Tubular Capillary Columns in Gas Chromatographs3 2.2 Other Documents: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.120W 3. Terminology 3.1 Definitions of Terms Specific to This Standard: 3.1.1 extracted reformate--An aromatic concentrate obtained by solvent extraction of reformate. 3.1.2 reformate--The product of a catalytic process that increases the concentration of aromatic hydrocarbons. 3.1.3 pyrolysis gasoline--Depentanized by-product recovered from ethylene manufacture. 3.1.4 synthetic blend--Blend of reagent hydrocarbons that simulate a process product. 3.1.5 hydrogenated pyrolysis gasoline--Pyrolysis gasoline that has been treated with hydrogen to reduce the olefins content. 3.1.6 crude ethylbenzene--Product produced from the reaction of impure fluid cat cracking, (FCC) ethylene and benzene. 3.1.6.1 Discussion--It typically contains greater than 40 % of ethylbenzene and benzene. 3.1.7 light blending aromatics feedstock--Light aromatics fraction (with high amounts of benzene and toluene) typically recovered from the isomerization of a p-xylene or m-xylene depleted C g aromatics stream. 4. Summary of Test Method 4.1 The specimen to be analyzed is injected into a gas chromatograph equipped with a flame ionization detector (FID) and a capillary column. The peak area of each component is measured and adjusted using effective carbon number (ECN) response factors. The concentration of each component is calculated based on its relative percentages of total adjusted Available from the Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. Copyright ASTM international, 100 Barr Harbor Dive. PO Box C700, West Conshohocken, PA 19428-2959, United States. Copyright by ASTM Intl (all rights reserved); Mon Jul 12 18:28:40 EDT 2010 1 Downloaded/printed by Stephen Petty pursuant to License Agreement. No further reproductions authorized. NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Contact ASTM International (www.astm.org ) for the latest information. D 6563 - 00 peak area and normalized to 100.00. Results can be reported as either volume or weight percent. 4.2 Volumetric results can be derived by dividing each component's weight percent by its relative density and renormalizing to 100 %. 5. Significance and Use 5.1 This test method was primarily developed to determine benzene, toluene, and xylenes in chemical intermediate and solvent streams such as reformate, BTX extracts, pyrolysis gasoline, hydrogenated pyrolysis gasoline, crude benzene, crude ethylbcnzene, commercial toluene, and light blending aromatic feedstocks. This test method may not detect all components and there may be unknown components that would be assigned inappropriate response factors and thus, the results may not be absolute. TABLE 1 Instrument Parameters Column Carrier gas Flow, linear velocity at 70C, cm/s Split ratio Detector gas Hydrogen flow rate, mL/min Alr flow rate, mUmin Make-up flow rate, rnUmin Sample size, pL Temperatures Injector, "C Detector, Column Initial, C Hold, min Rate, C/min Final, C Hold, min Size of 60 m by 0,25 mm ID pmbonded polyethylene glycol-fused silica capillary, internally coated to a 0.25-pm thickness helium 20 200:1 30 300 30 0.5 250 300 70 10 5 200 24 6. Interferences 6.1 Nonaromatic hydrocarbons may interfere with the determination of benzene and toluene when certain columns are used. 6.2 Styrene may be present in some samples. It, will elute with Cy+ aromatics. 7. Apparatus 7.1 Gas Chromatograph-Any gas chromatograph having a flame ionization detector and a splitter injector suitable for use with a fused silica capillary column may be used, provided the system has sufficient sensitivity to obtain a minimum peak height response of 0.1 mV for 0.01 % of any component of interest in the sample being analyzed or in the system blend when operated at the stated conditions. Background noise should not exceed 0.01 mV. Largest component of interest should not exceed 90 % full scale of the electronic integration device. 7.2 Column-Capillary columns have found to be satisfactory. For example, a 60 m by 0.25 mm inside diameter fused silica capillary, internally coated to a 0.25-um thickness with a bonded (cross-linked) polyethylene glycol can be used (see Table 1 for parameters). Other columns may be used after it has been established that such a column is capable of separating all major impurities under operating conditions appropriate for the column. 7.3 Recorder/Electronic Integration-Electronic integration with tangent capabilities is recommended. 8. Reagents 8.1 Carrier Gas-Helium with a minimum purity of 99.99 mol %. 8.2 Detector Gas-Hydrogen with a minimum purity of 99.99 mol %. 8.3 Flame Support Gas-Air, hydrocarbon free, with a minimum purity of 99.99 mol %. 9. Hazards 9.1 Consult current OSHA regulations, supplier's Material Safety Data Sheets, and local regulations for all material used in this test method. 10. Sampling 10.1 Sample material in accordance with Practice D 3437. 11. Preparation of Apparatus 11.1 Chromatograph-Follow manufacturer's instructions for mounting and conditioning the column in the chromatograph and adjusting the instrument to the conditions as described in Table 1 to give the desired separation. Allow sufficient time for the instrument to reach equilibrium as indicated by a stable recorder/electronic baseline. See Practices E 355 and E 1510 for additional information on gas chromatography practices and terminology. 12. Procedure 12.1 Bring the sample to ambient room temperature. 12.2 Inject an appropriate amount of sample into the chromatograph that meets the criteria outlined in 7.1. See Practices E 355 and E 1510 for additional information on gas chromatography practices and terminology. 12.3 Sample chromatograms are illustrated in Figs. 1-3. 12.4 Measure the area of all peaks. The nonaromatics fraction includes all peaks up to ethylbenzene (except for the peaks assigned to benzene and toluene). Sum together all the nonaromatic peaks as a total area. The Cy+ aromatics fraction includes cumene and all peaks eluting after o-xylene. Sum together all the C9+ aromatic peaks as a total area. 13. Calculation 13.1 Calculate the weight percent concentration of each component as follows: X ECNV - E ECAri) (I) Copyright by ASTM Intl (all rights reserved); Mon Jul 12 18:28:40 EDT 2010 2 Downloaded/printed by Stephen Petty 0 pursuant to License Agreement No further reproductions authorized. NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Contact ASTM International (www.astm.org ) for the latest information. D 6563 - 00 Inj ecttime: 14: 2501 (EL - 9E) twpsmart.60 (96.9T) suatAxoi120 liql) alalraNd (91.9T) onazumn429 4n sr ) !anon o t -- 0. N art N -N - 41} N oit krO CO 1. -- CO L-- eNa -o 2ID N 0 a 0 C.1 _ of aq La, a T. Copyright by ASTM Intl (all rights reserved); Mon Jul 12 18:28:40 EDT 2010 3 Downloaded/printed by Stephen Petty 0 pursuant to License Agreement. No further reproductions authorized.  NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Contact ASTM International (www.astm.org ) for the latest information. (61t D 6563 -- 00 011. 4% V 0 Inject tine: 16: 45: 35 sN N 0 CO" - Itt N GO N 1". LV -N r ital . 771 ont'orthekne. rh (94.8.0 suotampso N N z N NO El C.1 1 Ifs .11.11 (80'L I) ounkeez (or m ) mumueqprm4 CT =nil t (RT'OT) R170711147 -M -- -N -- -- - -- N -- -- (W9) ImPlimpaL2211 iT BT it 41 it sq it it it pt k . 6 enomt -- 471 -W O 171, 0 L ' 6 . 6 . 71,r C k . i- asuodslay aougolaa 10 g Copyright by ASTM Intl (all rights reserved); Mon Jul 12 18:28;40 EDT 2010 4 Downloaded/printed by Stephen Petty 0 pursuant to License Agreement. No further reproductions authorized. NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Contact ASTM International (www.astm.org ) for the latest information. D 6563 -- 00 :1; L Inject t ime: 15: 35: 51 I OT EZI **T2012iXa mmis..1.s N 1. O N N 4. le N es es In AIEN L -- co r L. 1s of ri ' it It it st ft' it sztemi it of rs Copyright by ASTM Intl (all rights reserved); Mon Jul 12 18:28:40 EDT 2010 5 Downloaded/printed by Stephen Petty () pursuant to License Agreement, No further reproductions authorized. wittodurd 222.10zea NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Contact ASTM International (www.astm.org ) for the latest information. 4110) D 6563 - 00 where: = concentration of component in weight percent, = area of component, i peak, ECN; = effective carbon response factor for component, and = (Ai X ECNi) = the summation of all response corrected areas in the chromatogram. 13.2 Calculate the volume percent concentration of each component as follows: V = 1v0, 0 C/D 2,(C/D) (2) where: V = calculated vol % concentration of component, C = calculated wt % concentration of component from 12.1, D = relative density of component, and E(C/D) = sum of the quotients C/D. 13.3 Use the following effective carbon number (ECN) response factors for the calculations: Component Non Aromatics Benzene Toluene Ethylbenzene p-Xylene m-Xylene o-Xylerre C5+ aromatics ECN Response FactorA,B 1.0000 0.9100 0.9200 0.9275 0.9275 0.9275 0.9275 0.9333 Relative Density at 60F 0.7200 (average) 0.8829 0.8743 0.8744 0.8666 0.8694 0.8849 0.8752 (average) AScanlon, J., T., and Willis, D., E., "Calculation of Flame Ionization Dector Relative Response Factors Using the Effective Carbon Number Concept Journal of Chromatographic Science, Vol 35, August, 1985, pp. 333-339. &Response Factors are relative to n.heptane. `DS # 4A Physical Constants of Hydrocarbons C, through C. ASTM, 1971. 14. Report 14.1 Report the following information: 14.1.1 All component concentrations to the nearest 0.01 wt (or vol) %. 14.1.2 For concentrations less than 0.01 wt (or vol) %, report as <0.01 wt (or vol) %. 15. Precision and Bias 5 15.1 Precision-The following criteria should be used to judge the acceptability of results obtained by this test method (95 % confidence level). The precision criteria was derived from an interlaboratory study using data submitted by fourteen laboratories. Each interlaboratory study participant was provided two gravimetrically prepared BTX known samples and three unknown samples of varying concentrations. Each sample was run twice on two days by two different operators. Results of the interlaboratory study were calculated and analyzed using Practice E 691. 15.2 Intermediate Precision, (formerly Repeatability)Results in the same laboratory should not be considered suspect unless they differ by more than the amount shown in Table 2, Table 3, Table 4, Table 5, or Table 6. On the basis of Supporting data are available from ASTM International Headquarters. Request RR:DI6-1025. TABLE 2 interlaboratory Precision and Reproducibility for Synthetic Blend Sample Nom I -This data was calculated after removal of outliers using Practice E 69 1. Component Concentration Weight % Intermediate Precision Reproducibility Nonaromatics Benzene Toluene Ethylbenzene Total xylenes Ca+ aromatics 22,447 42.891 19.961 3.061 7.921 4.192 0.296 0.781 0.212 0.055 0.195 0.169 1.746 1.887 0.715 0.191 0.512 1.009 TABLE 3 interlaboratory Precision and Reproducibility for Pyrolysis Gasoline Sample Nom I -This data was calculated after removal of outliers using Practice E 691. Component Concentration Weight % Intermediate Precision Reproducibility Nonaromatics Benzene Toluene Ethylbenzene Total xylenes Co+ aromatics 17.918 36.580 17.117 1.519 6.271 20.419 0.237 0.666 0.181 0.027 0.154 0.823 1.394 1.610 0.613 0.095 0.406 4.917 TABLE 4 Interlaboratory Precision and Reproducibility for Extracted Reformats Sample Nom 1-This data was calculated after removal of outliers using Practice E 691. Component Concentration Weight % Intermediate Precision Reproducibility Nonaromatics Benzene Toluene Ethylbenzene Total xylenes C o+ aromatics 0,264 21.015 34.516 5.473 24.173 14.744 0.003 0.382 0.366 0.098 0.595 0.594 0.021 0.925 1.236 0.342 1.564 3.550 TABLE 5 interlaboratory Precision and Reproducibility for Hydrogenated Pyrolysis Gasoline Noce 1-This data was calculated after removal of outliers using Practice E 691, Component Concentration Weight % Intermediate Precision Reproducibility Nonaromatics Benzene Toluene Ethylbenzene Total xylenes C D+ aromatics 27.871 61.111 10.966 trace trace trace 0.368 1.112 0.116 2.168 2.689 0.391 test error alone, the difference between two results obtained in the same laboratory on the same material will be expected to exceed this value only 5 % of the time. 15.3 Reproducibility-Results submitted by each of two laboratories should not be considered suspect unless they differ by more than the amount shown in Table 2, Table 3, Table 4, Table 5, or Table 6. On the basis of test error alone, the Copyright by ASTM Intl (all rights reserved); Mon Jul 12 18;28:40 EDT 2010 6 Downloaded/printed by Stephen Petty () pursuant to License Agreement. No further reproductions authorized. NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Contact ASTM International (www.astm.org ) for the latest information. D 6563 - 00 TABLE 8 Interlaboratory 013neC.eI.an and Reproducibility for Standard Sample NOTE 1--This data was calculated after removal of outliers using Practice E 691. Component Concentration Weight % Intermediate Precision Reproducibility Nonaromatics Benzene Toluene Ethylbenzene Total xylenes C a+ aromatics 4.538 50.0655 30.039 5.067 5.069 5.308 0.060 0.911 0.318 0.091 0.125 0.214 0.353 2.203 1.075 0.316 0.328 1.278 difference between two results obtained in different latiorato ties on the same material will be expected to exceed this value only 5 % of the time. 15.4 Bias--Since there was no accepted reference material available at the time of the interlaboratory study, no statement on bias can be made at this time. 16. Keywords 16.1 BTX concentrates; BTX extracts; capillary gas chromatography; commercial toluene; crude benzene; crude ethylbenzene; hydrogenated pyrolysis gas; light blending aromatic feedstock; pyrolysis gas ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and If not revised, either reapproved or withdrawn. Your comments are Invited either for revision of this standard or for additional standards and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, at the address shown below. This standard is copyrighted by ASTM international, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM wabsite (www.astm.org ). Copyright by ASTM lnfl (all rights reserved); Mon Jul 12 18:28;40 EDT 2010 7 Downloaded/printed by Stephen Petty () pursuant to License Agreement. No further reproductions authorized.