Document 4v8rz8peYn1QLmqpDa9DNMwwR

E. I. DU PONT DE NEMOURS & COMPANY PIGMENTS DEPARTMENT 256 VANDERPOOL STREET NEWARK, NEW JERSEY Copy No. 1 2-^ - z NEWARK PLANT PIGMENT COLOR RESEARCH REPORT MEDIUM CHROME YELLOW Y*547-D* DEVELOPMENT OF * CONTINUOUS MANUFACTURING PROCESS - #6 BLDG. PILOT UNIT. Period Covered: October 5, 1945 ~ June 17, 1946. FILE: DATE: 7/5/46 Njaeea Serial Me, KH-46-22 Cej>y Me, 1 Copy te #1 Humerieel Hie 2 - Reeeareh Office {211,1) 3 * Library Hie (211.1) 4 * #18 BullSiag File f-P " 6 Xttperial Sheadeal ls4aetarieev US, 7* * * y * f V, P 6p*mam wm m_ eK--x.at^f-t-i ii* 12 * Sxtra HSffMK PLARf wiomm c o mb r es ear c h r epo r ? Final Reperl miss mam msm uum y -54?-d j wsi^wit cr comimom umm&fsmam pr o c es s - #4 b p s . mm wau Period Qeveredi Oetefeer 5 1941 Jtrae 1? 1944. APPROVED BY* J, 0. Morrison M ISSBEDt 7/5/46 N41555.01 DUP050150511 'JstTOli'SiOtiWS Imolapi#4 otatgoo t' fiM eftlculations I* - Ma&w of S** wait 4* Mgm of 4 Bligt unit* ' 5* i2||F2 Forties b4 Kotos '>. '. l*-::%ratiag truest 2# Gfioretlsg fcsetruotion# ' 3:. : Ggosatiag esleuXaticaaii 4* Iquipmest ciieeli list, ate* KofOrOBOOS t 1 1 19 It al ' r : DUP050150512 -1- I ImmxMmi toe development mrk involved, to making a product equal to the 8sasiork8 improved medium yellow (K-221?, lot @$24) to toe 6 Bldg, eetlaueue aaaufaeiaro pilot unit, la reported below* toe final accepted prestee ms coded 8-8352i tois formula, together with detailed operating instructions, to also toeludsd* Soring toie polled toe K-2352 formula ms developed for Baking material, substantially equal tinetorially to the Ssni-Worke 8-221? (let 324) , to toe 6 %dg, continuous manufacture pilot unit* 8-221?* toe standard set up trm Seminaries continuously manufactured improved Media* fallow, is, to tarn, only slightly inferior to material prepared by the laboratory bagohwiee K-1958 formula* Sines too proposed 12 Bldg, eemtiauaus manufacture unit is to be geometrically toe same as and only twice too siso if tbs 6 Bldg* unit*, it is believed that the development information aeeumulatod to the pilot unit will ho direatly applicable to too full seal plant* Development work in the 6 Bldg* pilot wait ms based cm toe Seed.Work formula for K-221? (see 88-46-6) , By applying variable* evaluated during the Sead-Works development work, and seas developed during toe plant study, a lorumla ms arrived at whioh gave satisfactory material1 this is coded Y-547-D -48-2352), Bub out evaluations of too previously mentioned standards, in H-10S and alkyd vehicles, gave the rose comparisons tabulated below* ni mmmi %m$2 w 8-1958 (lot 33*01) (let ?@9?) 8-2352 w 8-221? (let @314) K-2352 w -54?-C (lot g$4G) 8*221? (let 8314) 8-221? r& 8-lf58 (let ?@9?) m Y-547-D (let 8340) y*54? T9 8-195 (lot S340) (let ?69?) M itLt999Kt9999 Timslml'"'""'' Strength '"'T2S4 Alkyd Masstene ws-ve red, w# to It, s grn ft eloan ve-e red, vs dk s dk, s rtd OK sir w to to OK we red vs grn vs--s it* vs gram 08 e red vs red, vs to. s red, s to vs red to vs red s red, vs to ve dk, vs dull t v s etr 08 ws-ve to DUP050150513 Preliminary printing ink evaluations at K-2352 indicate a tendency toward reactivity} farther study at this property is desirable is connection with pleat manufacture ef Y*547* Compared with s tentative pleat standard sf similar material (1st 8$42) approved by Bales for shipment to Areo* K-2352 was vs It* and vs elsaa ia masctene* OK la strength and tint* (by H-1Q8 rub sat) the plant produced aaterial was considered to he a close enough tiaetoriel cheek to K-2217 to warrant discontinuing dndspntt verb* However* in view ef the existing dempgdfer an improved medium yellow of the T-547* (lot @340) type* te met easterner ecradtssats* the pilot unit K-2352 final formula is being tamed etfer te the Plant toe production use* Additional liaferesttiea concerning continuously manufactured Medium YeHoBrean be fbund in the following rsperta*...(see page 2l).................... DISCUSSIONS The saseessivt basic steps involved in making improved medium Ohreme Yellow* continuously* may be very briefly summarised as follewes- 1* Introduction of Lead Nitrate and Sodium Chromate solutions into a precipitation cone with Intense agitation te precipitate Lead Chromate (slight chrome excess present)* 2* Two stage heat development ef the Lead Chromate crystals at a selected pH* 3* Digestion* or ageing* ef the crystals at the final develop ment trgiparature* 4* Pipe line introduction ef alum (Alg(SO) e*lHsO) and Titanium Bxlde te coat the crystals with hydrous exidss and prevent farther crystal growth and development* 5* `Pipe line Introduction of Lead Nitrate to precipitate Lead Sulfate and Lead Chromate* 6* ' Addition of Soda Ash for final pH control. Although the t Bldg* IHet unit and the Seml-Werks unit are similar in principle* they differ geometrically and* in seem rases* physically* Since this difference prerad te be important* a diagram ef cash unit is included (diagrams I and IX) Alee included is a copy ef the Operating sheet used for opergftiag t|M 6 Bldg* Pilot Unit* together with an explanation of the operation* Because ef its location and its integration with the operation of the Plant Yellow Units* the pilot unit was initially operated and supervised by Plant personnel* The Research department supplied the formulay*. followed each run* collected data and samples? and initiated the necessary changes, for simplicity ef operation It was decided to make the first few runs using pre-diluted Lead and Ohreme solutions instead ef centiaueualy diluting than in the lines* therefore* the formula was adjusted to suit the rotameter limits* To do this seme ef the rat retention times had te be altered* therefor the first Plant Unit formula used did net exactly duplicate all the conditions of the Brad. Works Unit* DUP050150514 -3* Vpjfe&a I tabulates the unit oeaditieas for aoh subsequent image ia formula involving a ehango la rate, and table tX oaatalae the ehangee Involved la 1b development of lit final formula. ^ 1rlaflg. oammrising these tabulations the aajer formula awl processing Qli&ig$? 1* laereasoi concentration of Lead and Chroma solution {$5$ total increase), jwdnsiag lighter nasstono# naanteas, 2* Xnareaasd heat development temperatures, giving redder 3* Imssdiats de watering of slurry front flail treatment vat (fey pooping directly t the centrifuge) to give lighter, leaner meetone. 4* Continuous Potronato treatment, to inereaoo centrifuge rate* mateh. 5# Increase development time (L0^) to give elooor snsstea TABIK I urn 630 i/hr. STRIKE 0.90 1st HEAT SIT. 0.95 2nd1' HEAT MV 11.7 Amim 11*7 T FINAL TREATMENT 8.8 LOT NOS. 26035-28157 80Q#/fcr.* 1100 $/hir. 3.96 3.70 1.1 3.83 13*8 13.8 13.8 13.8 7.8 5#6 27354-27420 27557 *Lad and chrome solution concentration inoreased. DUP050150515 HUJ3. _ H$.. WBE3SSHSISUM"'*-"" ifea&ton.Mraaeth. fist 26035 First plant batch; 630 i/hr, rats 4k inn OK OK 2615! Increased Lead and Shrews sol'n* sene* (133J0 to lighter MSP ws it* OK OK 2735* Shock 26157* but insrsass rats to 800 #/ar* dk* dull str OK 2?b mm Check 27354* but increase cone* ef Lead and Chrome &$/> Check 2?420 but use aeneentrated load and chrome #l*n* and dilute them in lins te strike unit* s It* gn > ws sty OK dfc* dull str s gm* 27592 Check conditions of 27557 but increase rate te 1100 i/hr* ws gra. vs str* OK 27992 Check 27592 but increase development temps* to give redder IT* va It* ws str. OK 28209 Check 21992 but dilute 2nd lead in line) 1 s dk, gra i strs* (SC 29840 Cheek 28289 but continuously Petreaate treat dk, gro str OK 30823 Cheek 28285 but centrifuge slurry as rapidly as it is made * dk, g t str OK 31*51 Check 20023 but continuously Petronatc treat ws dk vs-s str OK An important step in the program of this development work was the transfer of the operation and supervision responsibilities, of the plant pilot unit and processing eguipaeaft to the Research departments This change was aade in recognition of the fact that very close control ef all factors involved in Hashing and processing the continuous unit products ms absolutely essential te the success ef the development work* The results justified tbs change$ thirteen out of twenty subsequent batches being satisfactory checks* It was interesting to note that of the seven unsatisfactory batches, five were cade during the period when Zinc fellows ware being centrifuged immediately before each batch of experimental medium yellow* DUP050150516 8@ai^erk# experience with *22i7 Indicated that* with Lead ate Qh*en* solution* ef accurately pro-adjusted pH, the pH after strike acted be used is indicate the Lend it 9$fsme flew rat* rati rare MmU]r end sere accurately than eeted be dene with rotameters almas* Therefore* ease the desired strike ratten ef Lead it Chroma wet determined* it merely besom aseteeary it measure iht Mi pH and ns* it at a central point for sub* sequent eheek mi provided sufficient tare was enereised Is preparing the eespeaent selutie&e* During iht final stags tf the Float development work the lead, mi Chrome solutions war* analysed and the flew rates ware adjusted solely on ihe tests of analysis* Subsequently a frequent trtriks pH variance ($$ to 6*5) was noted from batch to batch* and sash time this difference occurred, the quality of the resnlting pigmsat was inferior* The method of control was changed* therefore* and ihe chrome solution rate of flow was adjusted wash tine the strike pH was beyond allewahle Units* Using this technique (and continuing to analyso the solutions for cheeking purposes) a series of ouoeoseful eheek batches me run. Analysing this information ate the attending results* it was decided that the solutions (Lead ate throne) could net be sampled and/or analysed accurately enough to warrant operating W calculated flews only* It is therefore established that* for K3352* solution analyses tested be used to eheek the aeeuraoy of eelntien makerap ate provide a calculated flew rate for the Lead solution* the chrome solution flew rate* however* should be regulated by the resulting strike pH* With good sampling sad aeeurate analyses the rotameter adjustment tested rat normally erased |9^ In the early plant development work* the eteer would frequently thicken up in the first and seeead heat development vats* so badly at times that it eaused ths vats to overflew* The cause of this was found to be a lead erases after striking* instead ef a very slight chrome erases* 'Shis was attended in every ease by a lew strike pH* It le therfere reeeamended that the heat not be intro* dueed to the development vats until the strike pH has bsen cheeked and stabilised*. The normal ehroae erases after strike tested be *0*5 #/min* (calculated for *2353) As indicated in the summary ef major formula ate processing change** the final proses sing conditions ted an appreciable affect on the quality of the pigment produced* Olesaly allied With the indicated need fer immediate de watering ef the slurry* was the need fer increasing the solids emitsat ef the finished pulp from 40Jfc to 4$ (vet basis) * te meet the speeifieailens for the continuous dryer guarantee* Te accomplish this* a centrifugation study was made* coincidental with the main study} this is reported in Kti*4&-2? This study indicated that the seeesd*pass centrifugation rate fer *2352 is increased teen the quantity ef re pulp water (equivalent te wash water) is reduced from 1*5 gallons to appreximatel;. 1 gallon per pound (dry eoler) * Tide causes an increase in calculated water soluble salts in the finished pigment* Due to the increased centrifugation rate ate the reduced quantity ef re pulp water* the temperature ef the re pulped material entering the eemtrifuge fer the seemed pass is higher * resulting in the desired higher solids centcut pulp for drier pan loading* There are no data at the present time te indicate the effect of this treatment* If any* on the texture DUP050150517 jf fh$ (irf plpawt# $$ r# nip $$* &M a J|U5 tlMi irif tfintit? f r pslpsd naiejftal i# $& fcafers ib seated eteirifuptiioas yteVLm&mfcy evaluations l&diteted tlat the tlnsteri&l cr^pttHlee ef th >ni sap# net ffi#td* Sine tbs solids eat*nt t tfe final gulp was (oet basis) using tlis grosednr, emtSima&lmvme are planned. Tk ^ jfcitte iini &j&i&ikg^3t? 4*ft %* #<**&>*& ###wftyMyiif ^ AHE n&|i s&i^igi&ftd&a &a aslod &&&&& &k& $iiiaHbs^r^aEW ^rfljp^WPp m imeW n8w^Jp^^iF*FF ^F**^^F^F^^8F8teJHp ^FiW^^WIF^^F ^F fp~ ^W-|F FFCTF^ ^F^lm PWr^wpp FIPpH^ ^WMi9Ww ,PJTmariteF^FF1 PB**P*PipP,P sFWwFF fdratite of tine 6 Bite* pilot unit* Tbl US contains n lift of the its* requiring attentUa* ffe most iagorfcaafc footer iayaiosdf in euffessfully tadnging* , tho nati to e^librite* to making MrtObi the ojamtior kssgs all ft roti* an&srs QJMsriioln adlfasied at aUttaea. There 1 * tenteaoy for new operator# " tO Oeli^ a rotameter tea to sot "tee'sad aoi so more attention a ssry <4jieorreet aeswaptlte* aaijl.iMimi Th# field for continuously namifhciored products tea 0 calculated nest easily By using a n minute tins basis and th respective flew rates ef tfe ingredients* The yield for K-2352 is calculated in this manor* a fellewet Using tb following flow rates (see fomnia) Fb (BOs)s Ba6r0 (as Bafi0rgO?*2Had) Al2(S04)3*lSH8B "I/* biqeor (fiOs eqfuiv*) Sad bead * Fb (fffis)s Petrenate (as is) 17*000 lbs./sdn. 8*220 * 1*823 * *3fl * 1*185 0*Hf 1* PbOrO preeipitated at strike * (l,-w) Cteme assess sill b * (8*22) lM* 2. Sydrat * IPan tin tra%sset (1/3) (1*823) * 3* Hydrate - W Uter w - 0*351 4* *> oro4 1"1 0*541 0*351 l.!7* 5* Pb SO* preoipitated by 2nd bead * [i .j w - (o.m |^a]] j|;gj 8* Petreaat (as is) 0*18| Qaloulatod field per sdnuto "* - o.4Ao Q-i87 19*382 #/Mn* DUP050150518 Oaing th* figura* calculated for prcductlea par admit#, tin 5 peaitioa can 1 calculated a* follow*i im) * (100) (100) 4*60 fRTPMMI MA JtffcaPk&feljdl) " (100) tom* n.9it Ha yield* far eaaiiaucuely manufactured 1*2352 *r* calculated no fttwi flfrfft f-tfrf Mill* the total quantity ef 10<$ Lead Bitrate and* up, by the eoaMeed quentitle* of Finl end Second Load addition* (par minute)j tide U1 determine the total *tm time.* Multiply tA* total *rua tiatf*, toy the caloulated yield par adnata ( Calculation**) to determine the total |1U for the run* Yield of 0 &$aum# MAtHtaX itt feting $& final treating unit at th* and of 40 minutee* Subtract the m adnata* fren the total run tlao (*** above) to dateratna the centrifugation tin*. Multiply the predetermined average eeatriftigatlan rat# (gee J*4ii*2?} of 10.5 ibg/ninute% tin firat faint by the centrifugation tisa* to detem&ae the estimated yiald far eentrifugad material# Fr the** ealealatieiia It oaa bo wan that, If the unit la not brought to equilibrium quickly and maintained tiwri the plaid for centrifuged material sill be lav* DUP050150519 5f i Il 4 DUP050150520 w Hi 1 5? it f. DUP050150521 e*- K-13398 -8FORMULA SHEET COLOR COPgg47D DATE 6/l?/46 NAMfihromO VelioV O_B_J_E_CT . urui,,,nr os K-2J40 but increase batcITsise*" b a s ed ON Plant Production, botch 33603. etc* BATCH SIZE-MOL1|Sft(Hf BATCH No. OF **K SAMPLE" (ml LBS. OR GMS. MATERIAL Aim 100% WT. : GAL* 441 685 C. C. Dissolve " MANIPULATION ~ (Sj5 1/2" Vat 240) at 90-lQQ*F. Pu bp to Vat 344 - Do Mot Washin. s A* Ash ''laaCOa) 826 |52 Wash out Vat 240v then dissolve in it in (17" Vat 240) at 90*-100F , Pfog *1/2 to Vat 238 - Mm uoad iliiFaid Pb (n o s )o 6040 3930 Nitric Acid 2*0 (+60/C HNOs sol'n*) Weigh into Vat 40 Adjust volume to (79* Vat 241) at 79-8lF 8 Adjust pH to 3.15-3*25 with Record pH* Have sol* n analysed for #/gal. Pb (NO8)2 ?^SS-52iISi.i2-^at 872 (see notoe) Sodium. Chromate 2700 (p$ sel'a** Calc* 2H20) 1720 Nitrio Acid *50 (6<$ HNO3 sol*n) Weigh into Vat 356 and adjust volume to (61" Vat 356) at 79*-8lP. Adjust pH to 735-7*45 uith Record pH* Have sol*n* analysed for w/gal.-expressed as Na2Cr2Q? *2H20 a*4mm.m mmm * eseee* ft "V' Liquor (+77I sol'n*) 99 eaa is" 2^ Weigh into Vat 352 Dilute with water to (Id?1 Vat 352) - stir well* Petronato (as is) 30 70 Weigh into Petronate Sol'n* vat Dissolve in water at 140*>l60F and make to Stir well* N# w I to rn DUP050150522 K-13308 ~9~ FORMULA SHEET COLOR CODE OBJECT BASED ON * BATCH SIZE-MOILS. DATE NAME BATCH No* OF *4K*# SAMPLE SOL XXX MANIPULATION K- N# tl&ter Water IfogCrgiO? 2HgO Fb (W03)s Equipment and lines must be properly connected and checked, as directed in KN-46-22. Then proceed as follows- 8.22 17.00 Start agitation in Strike Vat 256. Adjust Load sol'n. diluting water rotameter flow to 10*45 Adjust Chrome sol'n. diluting water rota meter flow to 8*1 Adjust Chrome sol'n. rotameter flow to *1.57 5.3 (actual gal/min. calculated from analysis- soo notos)* Simultaneously adjust Load Nitrate sol'n. rotameter flow to *1.537 +11*0 (actual gal/min. calculated from analysis see notes) Adjust pH after strike to 5.9-6.0 by adjusting Chrome sol'n* rate of flow* After strike pH has been adjusted* turn on steam in ''First Heat Development" Vat 255 and set temperature controller at 165F, Turn on agitator and steam in "Second Heat Development^ Vat 251* and set temperature controller at 205F. A1 a(S04)a.l8K20 "L" Liquor Pb (NOs)a Water Start agitator in "AGeing Vat 252 when slurry reaches sufficient depth. When slurry begins to flow from Vat 252* adjust alum soln. rotameter flow to 1.62 0*692 2.35 Adjust "L" Liquor sol'n. rotameter flov; to 0.351 0.41 0.86 Adjust 2nd Lead sol'n. rotameter flov/ to 1*785 +1*537 +1.16 (actual gal/min calculated from analyses soe notes) Adjust 2nd Lead sol'n. diluting water rotameter flow to -- - 1*1 DUP050150523 K-13398 COLOR CODE OBJECT BASED ON BATCH SIZE-MOLS. LBS. OR GM8. NaaCOg Petronate JDATE -10- FORMULA SHEET NAME___ BATCH No. OF 4*KM SAMPLE ,0J"=1 _5fck__5&c. MANIPULATION 2,84 Lbs/Sal OalA&n Start agitator in "Final Treating!* Vat 254 and adjust Soda Ash sol'n. rotameter flow to 1.21 2.35 Adjust pH in Vat 254 to 6.0 - 6.5 by rogulating Soda Ash sol*n. flow. i When slurry in Vat 254 roaches the level of the stand pipe - start pumping it to i the centrifuge, keeping a 4 inch slurry i depth in the centrifuge head tank. . ?0 18 , Re-pulp the centrifuged material (by < adding 41 /gal. water per lb. color - dry basis) using 1 1/2 opening turns of the re-pulp water valve. Pump re-pulped material into a yellow vat and (after it is all collected) re centri fuge. adding continuously to tho centrifuge head tank 0.40 0.47 through tho rotameter, (see notes) Centrifuge the final material onto dryor pans. CALCULATED COMPOSITION Pb Cr04 * 92.16/ Pb SO 4 2*27# Hydrates 4.6056 Organic Agent - 0.96/ 99.99/ ANALYSED COMPOSITION Pb Cr04 - Pb S04 PACKAGE g o al y iel d LBS. PER COST GROUP SIGNATURE JjJ. F* KLEHKE, JRk 34as is. 6140$ anhydrous, 1*5/ moisture (see KH-46-22 for ealc.) DUP050150524 K-1S399 COLOR CODE 7C- *' ` k NAME -11- failw DATE ^o//<A8 F^f *.-. *' GOAL YLD. f Aft v" *' Jl,_________ ***** .. VAT !&&$ % PREFERRED ALTERNATE VATS H! USE Mm# gfflVAT NO~ AMN,g ft* Vbv VAT NO. GAL./iN. - w$1 Arefrifi Altotm,___ . VAT " 'tf'' Ls r *ogf [SSI# * 24 $&xo....... ------- *zue.d________________ _______ m_____ IEm.1i 'B 3 *$5 30------------ 3M?3--r ^Sr ' * jjjf&o M&rnw . ---- Sw 44o 8 -CaaJN*i______ e a ^mk, mfki Jfih <ft rcrWlTO~ ------------ 1----------------$4p$ftng*)--------------- i4 ...------- ---____ __4-----3----*---4---------- -----------ttjrM.... ___________________________________ __ jfc..Mjjh..... ___________ --f ^ ificlr# Atfrity fr $ji ijW 3LX4 *!nXft a4a 455'252 * **i<r SM5~*4ift ^ 2?3 S^le --.. a..__________________________ A A ____ __________ ,$ *E S# 43 2*&J W^cM PRESSING SPEC I At- CON PCT1QNS DRYING NUMBER OP GRINDER MILL SPEED HAMMER TYPE SCREEN FEED SPEED MINUTES PER BARREL FINENESS SPEC. DRY ICE POUNDS PER PACKAGE PACKAGE TYPE LINER TYPE SPECIAL CONDITIONS Re ma r k s : GRINDING PR^fRBED^ - 2>*Jk 3 Jhi&gf^-gis '*** ^ *Ss vlbS* 3& * .K&it .. -- Si g n a t u r e K % SZS3SSS $ DUP050150525 E-2352 desoribee tt process fey aaa$ Inprewed medico yaUev in the 6 Bldg. emtinuous mmtm*taro pilot ualtji development work oae baaed cst tie Smd-verk# K221f (lot 8314) fiwmli. 24 1 ispemtlve* for goo* masoteao quality, that ik effluent slurry from 254 Vat N dawnsfared iwodlately# BSeauee dr the inadequate oapaelty of the eirntrifttge, a portion (#8 lbs*/ia) of the lf Ibe./sdnute production must lo diverted 4# a yellow vat and vat washed, treated with Pstreaate and pressed. 'fh* portion e treated adll he of inferior quality eespared to the balance of the material, however It is eeaetMahl* ao* or mined with, Y-449-D and/or -424*B. fbt 12 IB#./ ala. rata of coatrtfugatiett was Need eelely on overage eentrignge perforHttaee oat met aot to stood directly to determias or yreilot batch yields. : Several pilot unit yield* for atri#igs material (per >T5B lb# total run jfield) averaged ?00 IN. Mo low yield was duo In tlu& g$ ftn $>#$$ mm toxi normal. Since the time to reach equilibrium (before starting centrlfugatione) la fined* thin time reduction offooto the total centrifugation time * thereby reducing the yield of eeutrifuged material. M solution concentration were abet they should bo* the eonirtfuged material yield averaged lloo IN. (for 271 lb. total yield). The following aotea repreoaat pertinent information gathered Svm 8emi*erks ao veil ae S Bldg. pilot wait experience. The processing netea pertala oily to the eemrifaged portion of the batch, except where otherwise specified. 1. It is aoeoemry that the load nitrate solution and the Sodium Chromate solution be oaalysod for #/gal. fb(80s)g and Kaarav2HsO respectively, and the epeeifle gravity of each Mendaid. This information la necessary to enable oolonlatioo of the reapeotlve rate of flea. 2. ifber the necessary solutions have boon node op* and the Load nitrate and Sodium Chromate solution analyses have boo raoalved* the Loot and krona flaw rates are calculated. Sines the rotameters ware enlibrated vith solutions of different apeeifte gravity from tkooe to be need* ealeolatlono are aloe neeeaaary to oorroot for tkio. d typieal sot of ealsulatieas, pnaoooaafy to fill la the infomntiao needed on the operating sheets (see second page of oaaylo sheet), eeuld be as folloee#- DUP050150526 -13- Using the deirdi lf.O #/ada figure, and the #/gal. esodyeifu the necessary gal/ain flew is calculated. 'Shea, using the equation shew*, the specific gravity eeeipeaaatioa factor is calculated as fellows* % rate of flee of liquid 1 (need fer dalifenatien) nnts * " * * * % (to fee need far ran) density ef retsseter float (7*92 far i Bldg, rotameters) density ef liquid 1 (seed fer calibration) 1.048 retame1ter Calibration fer SMKl 1*044 fer 1HUJ Pta density ef liquid 2 (from anal.) "Performance ef the Rotameter* fear Seheenbera & Qolfeurn Crane. A I Ofe. B* Jf , 359 (1939) Using 1.048 fer Pjjaad 1,142 fer Pa, this equation reselves tei* 0.942 Th& calculated flow (11.05 gal^falm) divided fey this faster (9.942) will give the eerreeted flew rate (ll.fl net shewn is above table). using this corrected new rate figure, and the calibration serve fer the rota* aster involved, the retaaeter reading is detersdnsd. 2 3. Os net turn steam on in development units until strike pH has been adjusted. Xf the strike pH is lev (indicating a Lead eseess) the slurry will thicken la the development unite end the vats will overflow. 4. Provided the strike end final pH have been adjusted, and as rotameter changes have been made in the interval, equilibria material will begin to be discharged from the unit 20 adnutee after the desired development tes$rataree have beem reached sad stabilised. The minimum total time required, to begin to discharge equilibrium material from the final treating vat, averaged 40 minutes from the tine the ehreme end Lead flews were started. DUP050150527 >14~ in 1,11 AirTM WIWp w WlwTM- PPP^. ..^PPpv^PWPfSPHf^^^^P-W ^flpPW|fiMF^WI^^w"^Pfp ^(r tt & ^liw*m tleiiwi"l1WaW1W1** *tfO*q$ii Wo*4r & tiPi`A**".. 'PrWnPJJtKmIBt ^^PdP*uPmmmJmft ' *a* &- m&k3 *--IIMNMRMB V 11441# q # n# fn jSy i^l t^1fclJ&4y# #ssf IH a ate jhfegMKjjfti ia n# <th& %-*** ':***dk *%******* TM ^Wt^pppr ffS^ ^P^ppWWpW#pW-JfT Pff "Pr ^w ^W1 t # wWWiF ^PP^PHIntF ^pjpvmpr PKJMqp 4PJ#Ppr %f|} f&i&ftfaMfll ata&fl Mkmm*M*****/&&* "ppTM wppvwlEiPr "t P? Pf Ww^l|P IPPH# wwllWpWVMFww P* W#w 9m Am 4enfTIIHt A4m, Arnkm^tmAm Hi* fer to Mmr If priatiag iafc wfaicle, Mmmw it ***d to lnprim t* .: y:.- AurttomU-:- ,t# # tt litretrfifnagg, tiMni''l -- V- VTVi ... ItgAt at&MMtyf jagg ft A Hgtl Ml # (aloe to 6*) cause ft decreased wlkW# PflPPtrPfffWiHI PPPP ^w W PP^IPWy #r Jp y- ^PPP'P^WPr 254 Vfttf ift *ilal to pod wasteae fssltiy. ft facilitate tSdf the level of yfyyy lift 4fat ^nf#S 4ii$fe ig f# 4 jlnh#n# SI1 4%#- ilwgy in set le-oate##! ittsKsdietely, the naostea* viH beaaa* dork* greea and dirty. IS* A pigne&t (dry taoSt) will glee vote of 1 test of eah eetor per Sb* of fate* See rsert k h -46-2?. 12i fbe eet14*1* Mi peaiiien off addltiea of the Ingredients i# very Important and eitoali net V* verioi ia the 4 ftlig* ntt* oaooft under i|* IftvtfOOtiMs ill *0pert4a Setoilf ai ^Xneyootien Ml MedsteaseMSt of l^uipHn^t givoa in Booearoli report XB*44t2> met he li *Ei pNfor Petroaate eiZhMm flow fate it determined ]^ gn during %|^ ot eoatrifBCfttiai prii ao that tfeft rate of loamo* i irolino of tho Fotfftnoto al,n ia pregertioa&l to tho deoirsaao la volftfto of the reppulped glm$f* DUP050150528 *15- JAC; JOHj 12*46 i 2 **4 6 CHCKt*D 8Lf .......... ..... coo^'-^I-D SMI Me vArS SST :^00Q ACCT. UB<5. M-CODE US UBS j . INSTRUCTIONS _N/.. 4 MEDIIM YELi CM go^oT... ____ # .........$ pi*-............. Ft-.. ......................... . JUTtt 70" A1 SOV ViT 2?41 ___ ___- ....... ........Ad j u s t p H't o 7.iTlo......R.2.5 w it h ..... . .31..... .Re c o r d p H ", -v * ....:I--________HcoRft..Be.,,...Rec o r d in c h e s ............................ ... . 270O 10 .....-.... A ,,..... 4 H T* _______ Ma k e t o 6Pn m WF Va t R5&.. ____ Ad j u s t p H t o T.Wt o 7.*i*5_w it h __ Re c o r d p H .Re c o r d ip Ch e s Re c o r d Ge "" *** < #* w .** #* ** * ** wr <***; *<. *& * ** ** '*>; >** * m -*a ** ''Mil 15IIHE ,D SSOIVJL ,gUM P..T 0 JAX_3HiL ...i. 3- 1 Ho q Wi *.' * w St ir we11. r. 3,5a, Dissolve ,t N l". A T . Op- 0p*_.!M..VA*Xr 2*40'.' ' 7;'' Po m.-'"t o v a t <3.P. ^Pi;a .p. /. ,v>.$. 0 s.LaPp v..ra Cc h t a 1 ruac.,... Eke ES.fi...St. ORJ'X. .1 S.f>.l`0 Ltv-1 .' . F.mcv .1.0...v at .... ,,... . Adh...f i.(i. Si .0 >:o.a..v--k*t66a.9-^r0ih`:iv2.`i nX UJl P \ 'b..;...j Sa t,/.t_ Cl .- )' . t o Vat 3 L-Ct m ry. r j.i 3 e a n t,. t * r. a .t corfj.iiif.ou-.t J>! ....C.E..N r.U.G.L HE A 3 U I ih JJ S.S.OyV..E.0. ..- W...*15 "5Q-...3 A LL.3.K5....,:..4..,T..... ......... i.:Q~.ipQ JF ui. ,............ ... an.C>h t ? i .t u g c mIp .PAHSij.j.T.H ,,u; t a DUP050150529 TIME Ok S.rta 'ME CCMFi.Ct> -16* UA Ga i-UOMA p& c 1 f 1 c N-IC pH ' -za ,^r* J p m" iME 3TA?.TC TfMt HASHED ^0:3HATCR_._ A. DUP050150530 F85*883 ACCT i.8g. -N-CODC J ,,us? L_ Li -17- APPROVED h a i 6jAd 6- h -46 K: 6-14-^6 CHECKED J&Y, COOJI COOl__ SfAY 3 msrraucriOHs ...M0..i.UM /O.L.CM.. BM..XS^JmD. jfli iEKt Egerss s i iis r y fai muf rura i r ttnrf Jy^Ly7*0i _a-N.,,U- -z JM... O... L>>ftilSJEL AT EQ AHIJLOOO TO tgg''. iSgjw. 3 UTEft VAIS._________________________________ |_________!jftf.IM..................... P_E.*;.M..i.,m..IASI.. MA.T.O..,, ,.HtA.I..,MfiTK__ XL,"jj.~ Bo|I3X7ZZ3rr1^ ...LLT. ... ~t ; - ~ ^yrr-^io irri^fi~Xi^pRss ! i DU P050150531 -18- WL Th* eteps to he followed to alerting tlio wait are listed below ia the order to 'Mr (N^faaaooi (ssseatog the chebka end precautions of fable X3S tow been done) S+ Mwt i|i liifUi# 2* tMrt flew ef mtar for &eed end Ohri, and adtoet* 3* Start Mgi end throne flows* and adjust* 4* (Mk strike pH. after allowing jjr stoats* for unit f toko fihreae now fate ftotosit if aoeesasr?* 6* Uwa Me fS it wltoto Haiti* start stsaa to g$3f#l bw$ #i&$p$gt& $sl# {#' 8%mrt jl'n W&fkm- w& ^ i NNMM ^ d# ft ? " Ipm# m $tl$g; Httt \im8& &WtWf IdfH in . flV tofe *0, iff n.i ,iffMiAifltoik toi .toAMkibntfiMto Hi ,m ifflWHl Ji iQ#- SHmHI niifffii isniwinli ta in int* nt^ybi&$ msi^ 33* mm% mW Mmm tUm %nMM^ mfinr t&* lt Start toe fens lead* and it# dilating water* flow toe *L* LiMr. 13 Start too soda ash flow inemitli after the XMMi# 14 Start too agitator to too final treating unit, toea too itorry towel to high easagh* 15* Start tor pump toon the material to to# final treating wit sowers to staadptf** Id* Qhsok too jgM to too final treating mat* If# tot soda ash adjustment, if aeeeosary* 16* Zf both pB*s are witoto Itoltf} if all the rotameters are at tholr oerroet eettingeg and if too antsrtoi in ws&%& )wi *&ji# yfogpw 411 1s&$ nuMi iffliy In c c$8$4$i,ti i# In i si dtoMM^'l.^lasii.rasi P&fflA&A fid tohtotodtoiidi tomr kind are made er aetiesd* to atoafces toon thie time .the wait toll bo tolled toto and toetomtrgtog aatorial representative to toe oeaditieao to operating erd Sue to eftosmaant iiadtaties the aatorial from too tonal treat ment vat wao disposed to to a o o h bIs k manor* for elarlty too oaboepaent tope will bo preeeedod by m aaplsaation* As todioatod to fable II, tomsdtoto do-watering of too toaishod pigment is essential for goto fwlity* e to this, too material Iron too final treating wait was gaped to a *Btrd" ooatitooae eentrlfuge* DUP050150532 19- fMi mv&mm capacity of the oooirlfuge (at miAwm allowable filtrate blied) ia IMtad ta 4p@ 1** (dry bast*) af S*i|ft por abrade# Tho rate of output fion the uait# hawmri ia 1 *1 Ha (dtf baei#) af 1*2352 per ataata. To M&|| iMMjtWfo imASH? ^ ft l&WMft * ocnraootnd to the exloilag mm too* the wait snap to Up eratrifuge* aad extended to a follow fat# It was tin* peettbla* If regulation of the Inlet mMm to t&o oootitfssB hood ..** to divert, to a follow vat*, the mierial frfoa it4 l^gjlii H^/lililt ftyy' ^f1t *Caeo ilapae XX) The aoatrifuged notarial ea ye-guiped into a fallow aft far oollootlea and, when the run aao fiaiahwi, ro-ca^rifugatioa (with continuous Petroaata treatae*t)t -the final eeairtfugs palp dlaefcarge gftag wm&* , *fca diverted miarialt eellootod ia tha attar follow wts, WMh eastrtfngod portion *!?)* m&&kM idf ffttp thfc S$# f^fft- 41mi rf^|gf t fl!* ggijl lLW?W& i&ltti <8$3>ir& in &*& &ft|ri| (provided conditions of atop IS fcava been fully satisfied) | aft regulate depth ia bead tank to 14 iaolfto* 2I# %oa omtrifugo food talwo aad rapdato ta gioa aooaytafcla filtrata Mood# 22# <^poa tafttlf ftftar wal-va ta daftaad paaitloa (i 1 gaVtt#) 11/2 tmm Car 8li#tly soro) 23# imrt ro*ye2pod elaarry yvn$ 24# ffeas all tbe notarial haa mm eastrifagodt aad ro*f2pad data a follow ftf aoaoiira, aM atari agitator ia tfa yollao mft and opoa tfaa falwai to' tlta aaftrifugo Stet taft* II# Start tho agitator ia tha hm& toad# 2t* Start tfeo Pitroaat# flow ita tho Hoad toad aad rcpiiwt^ wwllTO/ 21# Opea food wolwa ta eaatsdfapi aad rogolato ta give aeeofftahla flltmto blood# 28* Lead tho discharged pulp ante dryer pass* If tho proper eare la tahea ohm adjuotiag the oontrlfu^ food valrea# aad ia raftlag sertaia OQUilihrim has boon reached at tho aeieeted valve peeitiea# there oheuld bo no diffieulty ia ohtaiaijft aatiofaeterily prooMoai nattnrial# DUP050150533 -20- JWftSL u SJH% flf tfcfl ttoi* h h I &tita>M& ami -the reflueetlv* Mma e-ralea tar i.wHMMMrt-ifflB 4m n |44 $# ftaia# HINlI^iljM ^HN>ll# UltiS Wl^w^P^ir '^wiwippiiflppu^w^P^ ^pPHW|r^ ^4PF *** w p-w*11 ^r m ujvwj^m mmwm wj 11'' Jjr*& m TM ";"" ItflBfl m> ft|gj^# H%tw&mwmm 1* Retaaetere ' 2* $$ R4y0|H8 T4f|frf 3* 4# Mr Operate! Steaw Valve* 5* pB Hater 6. A^ios*8 f. s# btaat Pipes & Jeiaiag Uas f* gAanumH In ftg&& 7&S$k$^IIWI-wwPWP vnmm mw^^m'wm w npwp"www 10# Theradeouplefl n# litafepwitl fnff^ Clean Ovt $Nn ^mpi44hbi^ CImmIi 0J$g]| 4 flatten VHm %1,4^h n ^i4# 1 fifuji t$ mmrnmk Irfltf &Jiasa#2ii9 %4# Ciena Out Scale ft MpMWt BuiM Up Clean tut Cheek With Hand Thwr--notar Haatfaly ftftariSaeh Haa IfariBfly %hwM.ly Weekly Routine WfWfcMy After Baflh Slua Veflkly Item <mnss & ireneimmsit c is k c k s s A#4ujfflae44<ii 1. Saw if float* are ft*** afl neter ftp. mat plugged# 2. tcariMdera 9wn * air a*S ** pointer to eee If eeatreUer 3# pH Water 4# 5* Velma 4# Tasaks 7# Csastrifttga 8* trfww 9# io m|d| pH Cheek Operate# ^FtPF^w^^WWt1 ^F Obecfc positions before man# Hah* aertala all are available before starting run# * it it Hah certain lima te awl frea eentrifug eat sadt are properly hooka* ape DUP050150534 gifiiffifi.il wppffffft# iff Q&s&imtm mts^mftwr# $$ wsSti bm ti^#ilffl# ..................KH**4O*X0 0rt* fttfiko Bihoot *proi>ij&t&t4a ftftt <I*fc.) KB*40S5J5 Otaspwfiaww of ftt^lWPffiifiy f$f|f% <yg h k ^^' f&fg&t* 8&Nli#&t Wiwt Hoof tt IBigfltoiiiniMi ftfcwiltw. - - iNNNff * ftSSii* Hfgr* t VtgftMt ColM1** S*44*?8 - Ot*. Bfgp. of Y*46f*f in Mb salt* i0J-44*$0 * ** Sfpr* f ** follow ia 6 Mg* Pilot Mil* S8*4jHI * ftwMff of l*t>* Work m Coat* ltfgr. ofGJttiw* *#Ua* M-45*1Q ft* V* develop* f Seat* pposota fet Ibm&i&o b follow# KH-46-3 * Gent* Sfp* of art* fellow 4a #6 Bldg* Pilot Shit* 8*44<*ft * Gttt* Mffcr* f Improved Bed, follow, K-2H7. Sem-Works t#* DUP050150535