Document Je57mQZxrdoZebo5k4kELQJK

..... * E. I. DU PONT DE NEMOURS & COMPANY KREBS PIGMENTS DEPARTMENT 256 VANDERPOOl STREET NEWARK, NEW JERSEY Serial No. k m-53-30 Copy-No. I B, F. KLENKE, JR., NEWPORT RETURN TO JACKSCN LABORATORY FILE ROOM Period Covered NEWARK PLANT PIGMENT COLOR RESEARCH REPORT Progress Report FLOCCULATION RESISTANT PHTHALOGYANINISS II TEXTURE IMPROVEMENT JURE, 1952 - JULY, 1953 FILEt DATE, 223 A 9/15/53 S '3 '3 D NJ 44r DUP050069532 Copy No Copy to* 1 * Numerical File 2 * Research Office (223*+) 3 - Library File (223 o1*) b - J. N Tully/A. Siegel 5 E. F. Klenke 5 Newport 6 - M. A. Perkins, Jackson Lab , Orchr~ 7 - W, j Clem, Chaammbbers Works, 11 8 - #1**- Building File 9 - J. H. Cooper 10 - Extra 11 Extra 5 NEWARK PLANT CHEMICAL DIVISION - COLORS Progress Report H.CggaLATXON RESISTANT FHTHALPCYANINES II > TEXTURE IMPROVEMENT. m^as^sjms^ m CHARGE* A-II-C278, 303 SUBMITTED BY* S. F. Kudzln Ap p r o v e d BY* J. H. Cooper 9/1/53 DATE SUBMITTED* 7/2V/53 DATE ISSUED* 9A5/53 DUP050069533 IIXSOESSSfiSL. In an earlier report; (KM-53-29) three processes were described for the preparation of flocculation resistant phthalocyanine toners. All of the resulting products exhibited extremely poor texture, as manifested in inferior roller mill dispersion in ink and in alkyd. This report deals with the improvement in texture realized with one of the products described in the aforementioned report, viz., the co-synthesized toner consisting of 93-9!?# Blue IB. and 7-5# CPC monosulfonle acid. This type of product has been desig nated "Monastral" Blue BMP. Three approaches were Investigated in attempts to improve the texture of Blue BNF* I - Treatment of the Blue BMP slurry <33-739) with agents prior to drying. II - Treatment of the Blue Buy slurry by laklng. Ill - Modifications in the milling operation of the BNF crude. mm. I - Treatment of N-739 with various agents prior to drying was found,in practically all cases, to be ineffective as a means of Improving the texture of "Monastral" Blue BNF. II - A "Ramapo" treatment of Blue BMP, similar to that employed in the preparation of BP-173-D, effected a pronounced improvement in texture. The resulting product, coded as BP-366-D, was only slightly inferior to BL-282-D and BP-173-P in texture. In money value It showed a marked advantage over BL-282-D. Ill - incorporation of various agents into the acetone milling of Blue BMP failed to improve the texture of the final products. The substitution of solvents such as carbon tetrachloride, perclene. orthodichlorobenzene and trichlorobenzo a for acetone in the milling operation resulted in a Blue BMP of superior texture. Salt and dispersion milling of Blue BMP yielded products of good texture. misomas* Nothing of a patentable nature has been disclosed by this work. The preparation of soft phthalocyahine powders by intimate association with various metallic rosinates Is covered in U. 3. 2,173*699* issued 9/19/39 to A. Siegel of DuPont. DUP050069534 --2 -- mHBMMU I - The relative effectiveness of various agents incorporated into a BNP slurry prior to drying is test illustrated by the following tables EFFECT OF VARIOUS AGENTS ON THE TEXTURE OF BLUE BNP #1 TRANS. jTM 22 CC14. 5 NaphthaleneTEA~CTo ester 0 (Rfef)2C03 ** 0 CCl^-TEA-C^ ester 0 Diglycol Stearate Untreated Control BT-3<*~D, SD-90719 0 0 6 ...... 32 St 22 6-1/2 6-3A 6-3A 5-1/2 5 7 6-3A 7 6-3A 6 5-1/2 5-lA 7 6-3A 7 7 6-1/2 6 6--iA 7-lA RATE OF STRENGTH DEVELOPMENT BT-30^-0, SD-90719 cc% Naphthalene-TEA-C*. p ester (N%)2C03 CCl^-TEA-C-^ ester Diglycol Stearate Untreated Control 12 2t 112 100 v.weak v.weak v.weak 120 v.weak v.weak v.weak v.weak 110 120 115 112 52 100 115 115 105 110 no 10k n' vs 100 * 22 100 167 130 109 115 150 170 *Grit Elimination data are obtained by use of a Hegman gauge calibrated from 0 to 8 in the case of dispersions in #1 Transparent lithographic Varnish and from 0 to lo in the case of alkyd dispersions. Progressive improve ment in grit elimination is indicated by increased numerical readings DUP050069535 3 Varying percentages of the agents listed were employed* Whenever possible, the agent was dissolved and added to the N-739 slurry prior to drying* In other cases, emulsification or colloid milling was used to effect maximum dispersion of the treating agent* In addition to the agents listed in Table 1, the following were also employed and found to be relatively ineffective: 1. Fluffium - a hydrolyzed polyacrylonitrile soil conditioner* 2* p-toluane sulfonic acid* 3* Toluene TBLMJjg ester 4* Barium hydroxide 5* 2-Ethyl hexoic acid 6. Triethanolamine titanate-oleate. 11 - The following tables illustrate the effectiveness of the "Remap" treatment when applied to Blue BNF. WMLM rmrm m mmm 4o PIGMENT/VBHICLE m 20/60 BP-366-D Blue BNF(DBT-348-D) BL-282-D BP-173-D BT-284-J) MJas., 3X 5X 7X 2-1/2 1 4 5 1 5-1/2 1-1/2 5-3A 1-1/2 6-1/2 3 7 8 2-1/2 7, 3-3A 7-3A 8 3-3A . 3% 7X 6 2 6 ?-1/2 4-1/2 6 4 6-1/2 8 6 RATE OF STRENGTH DEVELOPMENT 3X vs 7X 7X vs 7X. CBT-284-D) BP-366-D Blue BNF(DBT-3*+8-D) BX.-282-D BP-173-D BT-284-D 5^ weak 20% weak equal equal 10-15# weak equal v.weak vs weak eaual One of the more important variables in the "fiamapo" treatment of Blue BNF was found to be the nature of the pre cipitating ion* Thus, the following table shows calcium to be the preferred precipitant* DUP050069536 -b mm RATE OF GRIT ELIMINATION IN #1 TRANS. b b mb b, CLB.,S,2Q)^a ____IT ___ MttalgB Sen. Keg. 1 Al 7+ 2 Ba 7- l Zn Kg 10 5 5 Ca 10 BP-173-D 10 i). 5-1/2 7 V-l/2 6-1/2 7-lA 3? Sen. Heg* 10 6-1/2 10 6-1/2 10 7 10 6 10 7 10 8 5T 8&. , 10 10 10 10 10 10 2Ltt,gHi73sft , gSEIg& ...%___ 10 7 . 125*100 10 6-3A 115*100 10 7-3A 115*100 10 6~lA 165*100 10 7 105*100 10 8 100*100 RATE OF STRENGTH DEVELOPMENT 1 v*v*weak 12# weak equal 100 2 v.v.weak 10# weak 1# weak i 15# weak v.v.weak equal 10# weak equal 2% weak i 10# weak 2# weak 2# weak equal equal equal A determination of the lower limit of rosinate essential for satisfactory texture was carried out* As the following tables illustrate, percentages of rosin approaching those specified for BP-173-D were found to he necessary* jMuy. S inw b k #1 TBAK3JL V 31 5 1-3A if 5-3A 6 10 if 5-1/2 6 6 25 5 6 6-1/2 6-1/2 Further investigation demonstrated the preferred conditions to consist of striking at room temperature followed by development at the boil* pH adjustment after the strike had no detectable Influence on the nature of the final product* Physical conditioning of the slurry after the strike, e*g. homogenisation or colloid milling, provided only a minor advantage over an untreated sample* DUP050069537 The preferred product, HBP-366-D, prepared according to the procedure appended, showed a marked advantage in money value over BL-282-D as can be seen from the following table: ItfULZ Product ^.isaagx SBP-366-D 1.1755 BP-173-D 1.00 BL-282-D 1*3168 Svntex 55 (Bajl mined) 1.05U 1.00 1.3503 1.6 57 1.00 2.129 StrgBgjih. **> 7X 1^37 1.00 1.848 1X1 - Acetone milling of Blue BNF in the presence of various agents was found to be Ineffective as a texturing treatment In all cases the final product dried as a hard bronzy material, dispersible in ink or alkyd systems only with difficulty* the following agents were tried: 1, ftopco 2125 Ethylene oxide condensate ex ffopeo Chem. Co* 2 Trimethyl ammonium chloride* 3, Vlctayet 12 A nonionic wetting agentof the^general formula* ex Victor Cnern. Works* OB* ft R-O-P=0 0 OH1 4*. Polyoxyethylene lauryl alcohol* *>. Ethofat CA5 reaction product of coconut oil add with 5 moles of ethylene oxide, ex Armour & Company* 6. Sta-sol - Soya Lecithin ex A. E. Staley Company. 7* Nitrobenzene 8. Carbon tetrachloride* * 9, Indulin - lignin from Pine wood ex W, Va. Pulp & Paper Co* 10. Acetoacetanillde* 11* Bow Corning Fluid No* 200 silicone polymer ex Dow Coming Corp* 12. Psrclene + Span 80 - latter being sorbitan mono-oleate ex Atlas Powder Company. 13. Triethanolamine titanate - oleate ex Du Pont* DUP050069538 - 6 * The failure of various agents and treatments subsequent to the milling operation aroused suspicion as to the effect of Idle milling per se on the texture of Blue BNF. Consequently, solvents other than acetone were used for BNP milling. The most promising results, summarized in the following tables, were obtained with carbon tetrachloride, Perclene, ortho-dichlorobenzene and trichloro benzene. .JflgJUBL TEXTDRE TESTS I!? SYNTEX 46 PIGMENT :CLE 20/60 RATE OP OMT ELIMINATION. BMP Acetone cei4 Perclene ODCB TCB BL-282-D BP-366-D BT-284-D W' r 1 7 7 6 7A 4--1A 2-1/2 1 MILL BASES 2ST ST aM* V-l/2 5-lA 8-1/2 9-lA 8 g-1/2 6-1/2 7 2 8-1/2 8 8--1/2 7-3A 7-lA 2-1/2 9-lA 8|-_1_/2__ 3-3A . _Si si 7-3A 7-3A 7 7-1/2 7 6-1/2 2 mBBSS'"* 8 8 8-lA 8 l RATE Qg STRENGTH DEVELOPMENT BNF. MlIiUBO-lS... Acetone CCI4 Perclene ODCB TCB BL-282-D BP-366-D BT-284--D aLJBLJBL 205? weak 10% weak *>% weak 5% weak 10$ weak 10% weak 5%, weak 10% weak 7X vs BP-366-D at 73 20-30$ weak 7-8$ weak vs strong, green vs weak, green 10$ weak 5$ weak, red *.* ee 10-19$ weak, red Compared on an equal toner basis. DUP050069539 TAELS VII FLOCCULATION RESISTANCE AM) COLOR READINGS IN GB-2*54- FLOCCDLATION RESISTANCE*(1) COLOR READINGS* (2 ) Acetone CC14 Perclene ODCB TCB BL-282-D BP-366-D BT-284--D BT-3U-8-D, Lot 0 9W ?w* 7W P m 8w m 3S 7W equal, green equal, green equal, green equal, green vs weak, green Control equal, green very weak equal, green (1) Tested by rubbing. (2) Sprayed portions were read* * The following numerical system has been used to designate the degrees of flocculation observed: 10 - no color change ** - bad color change 8 - slight color change 2 * v.bad " ** 6 - considerable color change 0 - extreme tt S - strong, l.e* rubbed area Is stronger than sprayed area (l.e* flocculation)* W = weak, l.e* rubbed area is weaker than sprayed area (l.e. flooding). Increase In strength on rubbing Is the phenomenon commonly associated with flocculation, whereas flooding is recognised by a lighter (l.e*, weaker) rubbed portion* It was demonstrated that flooding, in the case of CPC, is essentially the reverse of floccu lation. Consequently, it is possible to combine a flooding pigment with one that flocculates in proportions that are empirically determinable and obtain a product that is flocculation resistant* Kerosene, water, ethyl alcohol and mixes of acetone + kerosene and acetone + carbon tetrachloride were unsuitable grinding media* Further modifications in the milling of Blue BHF consisted of dispersion and salt milling* The following tables summarise the comparative evaluation of Blue BNF toners finished by the methods indicated* DUP050069540 HBJLTO MSB Solv.Mill (acetone) Dispersion Mill Salt Mill BT-30M-D, Std. IT 3 6.5 6.5 5 32 3 6.5 7 6.5 5S 6 6.75 7 7 a 6^5 7 7 7.25 RATS OF STRENGTH DBVELOFMEffl?. METHOD IT 3T 5f 7$ Solv.Mill(Acetone) v.v.weak Dispersion Mill vv .weak Salt Mill v.v.veak BT-304-D v.weak v.v.weak 3% weak weak weak v.weak 100 5% weak I 1% weak 1 3% weak 4^ 7T .weak (30%) weak (20%) weak (10?) -imsix.. ORIT SLIMXHATIOH Iff SYHTEX fO PIGMENT/VEHICLE 20/60 METHOD Solv.Mill(Acetone) Dispersion Mill Salt Mill BT-284-D U 1 3 3 1 MILL BASE ft S 2 if *f.5 2 2.5 5 5.5 3 3.5 5.5 6.5 h ENAMEL 33 23 32.5 5 2 43.5 5.5 3.5 RATS OF STRENGTH DEVELOPMENT METHOD Solv.Mill(Acetone) Dispersion Mill Salt Mill BT-28*f-D xx.muff;.. 10-15% weak 20-30% weak 10% weak 10? weak 7X vs BT-2&-D 7X v.v.weak (*fO-50%) 1Q% weak 10% strong DUP050069541 -9- I - Treatment of Bln BNF with Carbon Tetrachloride Emulsified in TEA-C-^. Ester Solution. Into a filter beaker was weighed 256 grams of N-739? S.W.3073 (60 grams dry weight)* The volume was adjusted to 1200 ml. with water and the slurry then agitated by means of a "lightnin* miser. The pH was then adjusted to 5*35 with dilute HC1. The slurry was heated to 90C and to it was added an emulsion prepared as follows? 1.2 grams of TEA-C^ ester was added to 125 ml. of hot water. The solution was agitated vigorously and to it was added 3.0 grams of carbon tetrachloride. The mixture was then heated to 90C* The resulting slurry was held at 90C for 30 minutes with continued agitation. It was then filtered, washed free of chloride, and dried at lWP. II - Preparation of BP-366-D A quantity of W-739 equivalent to 100 grams on a dry weight basis was added to an 8 liter jar. The volume was adjusted to 2 liters with water* To the resulting slurry was added a solution of Staybelite rosin containing 31.2 grams of rosin. The slurry was agitated and to it was added,in a dropwise fashion, 120 mi. of a solution containing 12*0 grams or calcium chloride. At the completion of the strike the slurry was brought to a boil and maintained at a boil for 30 minutes. To it was then added 17.8 grams of Blanc Fixe, and the slurry agitated and boiled an additional 15 minutes. The slurry was filtered, washed free of chloride and dried at 140F. Plant formula is appended. Preparation of Staybelite Rosin Solution. 60 grams of Staybelite rosin was dissolved in 510 ml. of water containing 8 grams of sodium hydroxide by heating to a boil* The solution was allowed to cool, and the volume adjusted to 600 ml. with water. DUP050069542 - 10 in - mvrnkMmm. Use of Agents - A 1/2 pint jar was charged as follows; 600 grams steel shot - 1/8" 12 grams crude Blue BNP 100 ml* Acetone 1*2 grams indulin The sample was milled for five days on the semi-works roller mill. It was then screened free of steel shot, toiled till free of solvent, and then acid extracted and finished in the usual way. Use of Different Solvents. - The procedure in these experiments is identical with that described in the preceding paragraph except for the substitution.of acetone with another solvent, and the elimination of the use of agents. Salt and Dispersing Milling Salt Milling - A one quart paint can was charged as follows* 16 grams crude Blue BNP 100 grams salt (N-71) 150 grams roofing nails 1500 grams steel shot (lAw - 1/2") The sample was milled for 2b hours on the semi-works roller mill. It was then screened free of shot and roofing nails, and extracted and finished in the usual way. Dispersion Hilling - k one quart can was charged as follows* 16 grams crude Blue BNP 135 grams salt (N-71) 150 grams roofing nails 1500 grams steel shot (lA" - 1/2") 3 grams Perclene 0ol5 grams Span 80 The sample was milled for 2b hours on the seal-works roller mill. It was then screened free of steel shot and roofing nails, and extracted and finished in the usual way. DUP050069543 Additional data may be found in the following referencess I * Treatment of N-739 with agents prior to drying; .B, 1436 Expt* No. 30 - Fiuffium 32 * pH 15 - H-623 + N-639 - Acetone U * Ammonium Carbonate * p-toluene sulfonic acid I? - Colloid milling - Toluene + TEA-Cnp 39 - CCI4 + TEA-C12 4l - klWta + 43 TT - Ammonium Carbonate 46 - Diglycol Stearate 47 - Barium Hydroxide - 2-Ethyl Hexolc Acid - Titanium dispersing agents IX - Treatment,of Blue BNF_byJUfldbaa 1 N*B. 1^-36 Expt. No, 4o - 50# Bamapo Lake 42 - Aluminum Rosinate Lake 48 - Ba, Al- Zn, Mg, Ca. 49 - Bamapo + CCI4, 50 - Bamapo + Naphthalene 51 - Blancol + Bamapo 52 - Bamapo - Reverse Strike 55 - Zn Besinate 56 - Ca Besinate 57 - Ca Besinate - Variable study 60 - Ca Besinate d* Naphthalene 61 - Ca Besinate - Variable Study 62 - Ca Besinate - " n 63 - Ca Besinate - " " 65 - ABP-366-D for evaluation 66 - ABP-366-D - pH variable 68 - BP-366-D - money value 69 - BP-366-D - Period of Development 70 - BP-366-D - N-739 vs N-739 homogenised 73 - Lake of lignin sulfonic acid 78 - BP-366-D - ex lot 0-5, N-739 82 - BP-366-D - ex lot 0-5, N-739 homogenised DUP050069544 12 - W.B. l4S2 Expt.. No. 14 - BP-366-D ex Orchera samples< 18 BP-366-D ex crude lots 841-845 19 - BP-366-D ex N-739, lots 6-9 22 - BP-366-D Evaluation 111 - Milling Modifications Agents inthe grind!. W.B 143-6 Expt. No. 67 ** Titanium Dispersing Agents. 75 - Nopco 2l25 trlmethyl ammonium chloride. 76 * Victawet, polyoxyethylene lauryl alcohol. ethofat C-15. 77 - Sta-sol nitrobenzene, carbon tetrachloride. 83 * Indulin, acetoacetanilide N.B. 14?2 Expt. Mo. 1 - Perclene + Span 80 8 - Dow Coming 200 Fluid. age, sy,en.t,Jolyeuts. N,B. 3.452 Expt. Mo. 10 * Kerosene and CClj. 11 - Mixed Solvents 15 - H20 and CCI4 16 - Ethyl Alcohol and aeetone/CCl. mix 28 - Perclene, ODCB, TCB * 34 - Acetone and CClv 35 - CC14 and ODCB 57 - Perclene milling 58 - " 80 - " Salt and Dispersion Milling M.B.__1436 Expt. Mo. 58 - Salt and Dispersion Milling 71 - Semi-Works Salt Milling 72 - Semi-works Dispersion Milling 80 - Semi-Works -B. l*fS2 Expt. No. 2 - Semi-Works Dispersion Milling 5 - Semi-Works DUP050069545 * 13 QftHER REFEREHCES 8 1* Sales Service Report 20-40 and 20-41 2* Exposure Series 10368, 10383 DUP050069546 J-53-eM30116 OITTOtoraj u,s, Pat. 2,1739699 2,556,727 COPS:. ABP-366-D GOAL:. ..133.2#- .SIZE*. BL5ZO VAT:_____ COUPLING VAT:. SimS YJBXii___ jtctbjax (3607) ATPaOVEDBI: IHC 10/17/52 w NAME: "BAMAPO" BLUE BHP/CG-20 msmucnONS PREP. to,.l/2!L-4teter or,,,,less,,, gfg|b ..ggfl lo at vat 313 for step S, Stayhellte Boaln 2. Weigh and hold at vat 307 for step lE. USB LBS. 3KT ~120~ HOOPS '52E' 20 Acer. LBS. "JET Tg" s.v. 2o Puma or m into strike vat thru 20 mesh screen JUflQQg*JUKai ieSiL Lot. 2H 1000' m Bun 21w (6l5 G.) water into vat 313 Weigh In drum and pour In 1, Turn on agitation and steam o. Dump in N-528 prepared in step 1. 9. Heat to boll' iO. Boil 10 minutes 11* Test and Record: Cl Hftist to vvs * I2b If necessary^ adjust to ws T4 CY with!.'g~7 fiieofaVCtas&masmssi IA..Reheat to holl, ....... .. . 14. Stir an additional 10-20 minutes at boil to 'ctlssolvi" , ____________ __S.V, 1>>. ana vat 313 into strike vat thru 20 mesh screen 4 W"|C6. Run 1^" (176 0.) watar into vat 3~07~ 5. 17* -XT.^4t.ato.r..ana steam,,, 1.9,.................................................................... P.iL-AAlua-t_to li.lLA.23Q G).-gt.JL$Q~15ggE s.v. '21 Etrike.vat 307.. at l$Q^p^_lnto at^ke.;^ 6o on the surface in 10-15 minutes 22, -S.tjg.3Q mj.3a^tes , .A CONTD ON PAGE 2. DUP050069547 !! pBoass_._sBiip5-._, EST.LOSS REMARKS MAKING AREA MOTES LBS. PRESSING AREA MSTRUCHONS vat ' d at e................ . ... PBESSING AREA NOTES DESCRIBE YOUR YIELD RECOVERY CONDITIONS RBISASHD BY .mm.no,......` 91......................... 92..... . MO. OF c ak es ^ x 70 3 X 70 EST.LOSS c akesused LBS. PRESS WUHOUt ASTTATIOH WASH TO 5000 OHMS HOURS WASHED OHMS MAKB FIRST TESTAFJSR 1 HRS, LOAD ON 5 cars DRYER CARS ACTUAL OR PULP CONTAINERS s pec ial in s t r u c t io n s Non-'bieeAlng MOTES ON SPECIAL INDUCTIONS Must not contaminate with any Sli e SAMPLES DELIVER TO SAMPLED m RELEASED BY DRYING AREA MSTRUCEIONS TYPE L.V. H.V. HURRICANE HOURS H-5 30 5-5 ------------- 3350------- ----------------I*FU~~ Do not dry ih brick dryers ~ DRYING AREA NOTRS LUMP ~ OK - WET ~ SALTS *- CONTAMINATED WITH REMARKS l u mp c o n t ain er see chars* s pec ial in s t r u c t io n s Noii-bleedlng East not contaminate with any Biu >* MO. DRYER CABS PULLED Cool in dryer to loowF* Nuet not" send to Grind Shop unless loO^k cr EST.LOSS IBS. ' SAMPLES ~r"' ~ DelOW. SAMPLED BY DELIVER TO LUMP WEIGHT RELEASED BY GRINDING AREA INSTRUCTIONS GRINDING AREA NOTES GRINDER HO. 7 L.S.Po LUMP -- OK -- WET -- SALTS SPECIAL in s t r u c t io n s Ufon-bleedlne REMARKS Must, not oontaml nate with any BlU ) SSK LOSS LBS, REMARKS s ampl es 2 envelopes CONTAMINATED WITH d el iv er t o Control tab* DO MOT MIS BEFORE SAMPLING pac k ag in g See chart* SAMPLED BY SATE MCKED QOinrY REMARKS LUMP WEIGHT CHECK DUP050069548 MOTES ON ABP-366-D The present formula consists simply of an adaptation of the BP-173-D(J) formula with the following modifications: 1. N-739 ("Monastral" Blue BNP Paste ex Newport) is used Instead of N-623* 2* Staybellte Rosin is employed in place of K-wood rosin., 3. The preferred precipitating cation for the rosin was found to he Ca"H' over Ba**, 41+++, Mg-H- r Zn++ 4. The neutralization step employed in BP-173-D following the strike has been omitted in the present formula* N-739, when dried, yields a product of most unsatisfactory texture, taking with rosin, as described in the present formula, greatly improved the texture. Furthermore, this procedure enhances appreciably the dispersibility of the parent pigment in lacquer, whereby It can effectively display its inherent resistance to flocculation. SFKj CC 10/20/J>2 SIGNED 8. F. KNDZIN - 10/17/52 APPROVED: J. H. COOPER 10A7/52 DUP050069549 4-53-CM8unow Diiiuiommaj n.s. Pat. 2,173,699 2,5561727 2,526,34.5 c o dr .... GOAL- 1^90^ K-p BBP-366-D s izr MAZO VAfc .......... COOTMN VAR...... ............... SIfltgB VAT:--------209. 211 (3608) AEgBCOTJBK JHC - 11/6/52 '* VAT JEEP* SAME: "RAMAPO" BLUE BJSF/CG-21 INSTRUCTIONS 1. Chou tol/S1* diameter o p less, weigh and hold At.-Mt 313 for 3ten 8. atastmliteJEOfflB. usEias. 312 code 528 acc t . IBS. US 2 . Weigh and hold at vat 307 for ste 17a : 320 ip : W"" S.V* 2a ..3.-. Pnnrn or run Ipto strike vat thru26, mesh. screen. (1000#, 100%) '. . # Lot . . 739 lodo 4. Adjust to 35" (1312 G.) in-- 5 Run 21" (815 G.) mtep into vpt 313 3* 60 Welsh In druMLand nour in M 7. Turn on astitgtion and steam .. ._Jt 1 ? "TJF 3.T. 4. Qf Heat to boil in 20-30 mins* lb. Boll 10 minutes li.....Test....and_j!.ehord: Cl .... ..... ...must be ws 12. If necessary, ad .lust to ws + CY with l?-7 .... ..... ..... ....... .................... ............ . ... . . Records CY.................. 13* Stir an addiMona^lO^^Mrmi* to. dissolve. 14. Rian vat 313 into strike yat thru 20 mesh screen, 11 '!" " '. JO? 15. Run 14M (126 G.) water ipto vat 307 5 16. Turn on agitator 17. Dump in H-20 weighed in step 2 l8- Adjust to 1.8".. (230 G). 19*..Stir until dissolved. . ._ s.v. 6a 20. Strike vat 307 at room temp, into strike . . .... vat op the surface in 10-15 mins. 2i. Bring to boil .in.20-3p mins. 22- Stir 30 minutes at boll. 23. Dump In rr,.. ___ ?fi; Stii* an additional 15 minutes. 25. Press with agitation. . ... r 178 65 17k .... 4. ' COW'D ON PASS 2, DUP050069550 CODS. PROCESS;.. BP~;3>o6"D g o at - l400^ r DA3-llA/52..................... EST.L0SS REMARKS MAKING AREA NOTES LBS. PRESSING AREA INDUCTIONS VAT DATE TIME BBTWHgSp B7 PRESS NO, 91 n o . o f c a s es 3 x 70 92 3 x 70 PRESS WITH AGffAYJQN WASH TO 5000 OHMS MAKE FIRST TEST AFTER 1 HRS. l o ad o n 5 cars s pec ial nsiOTcnoHs Non-bleeding "Must ndt coritainlnats with any Blu^ PRISING AREA NOTES DESCRIBE YOUR HELD RECOVERY CONDITIONiS ESA LOSS CASES USED LBS. HOOTS WASHED OHMS DRYER CAPS ACTUAL OR PULP CONTAINERS NOSES ON SPECIAL INSTRUCTIONS SAMPLES DELIVER TO SAMPLED BY RELEASED BY PRYING ARM INDUCTIONS TYPE L.V. H.V. HURRICANE HOOTS 4? 30 M TEMP. 140 140 140 - Do loot dry in trick dryers*. . __ _ PRYING AREA NORBS XDMP -- OK -- WET -- SALTS -- CONTAMINATED WITH HRMgg-g l u mp c o n t a in e r See chart s pec ial nis&OTcnoHs Non-bleeding Must not contaminate with any Bin NO. DRYER CARS PULLED Cool in dryer to 100UF,, Must not 1 0 sent to Grind Shoo unless 100dF ei ESI. LOSS LBS. SAMPLES helOW. SAMPLED BY DELIVER TO ' LUMP WEIGHT RELEASED BY GRINDING AREA INDUCTIONS GRINDER NO. 7 Ii.S.P* s pec ial iNsraucnoNS Non-bleedine Must not contaminate with any BXu< s ampl es 2 Envelopes GRINDING AREA NOYES LUMP --OK -- WET-- SALTS -- CONEAMIKAXSD WITH REMARKS EStLOSS IBS. ftgmMUWTO : .. d el iv er t o Control Lab. DO NOT MLS BEFORE SAMPLING PACKAGING See chart. SAMPLED BY DATE MOLED QUALITY REMARKS LUMP WEIGHT CHECK DUP050069551 NOTES ON BBP-366-D The present formula differs from the "A" formula In two respectsx (1) The "B" process incorporates quantities of Blanc Fixe required to yield a final product calculated to he of the following composition! Toner CaRx Blanc Fixe (2) The strike is carried out at room temperature in the present formula and is followed hy a period of boil, as opposed to the ''A11 formula wherein both the strike and the development were conducted at the boil. This change results in a further improvement In texture. SFKiCC SIGNED : S. F. KODZIN ~ llA/fc APPBOVEDs J, H. COOPER - 11/6/52 DUP050069552