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E. I. DU PONT DE NEMOURS & COMPANY KREBS PIGMENTS DEPARTMENT 256 YANDERPOOl STREET NEWARK. NEW JERSEY Serial No. KN 48-18 Copy No. 1 X NEWARK PLANT l PIGMENT COLOR RESEARCH REPORT Period Covered) REPORT ON THE MANUFACTURE OF IRON BLUES ^ I FILE) 213 DATE) Aug. 10, 1948 N42171 X opj im 01 < Numerical yil ,g * M&gmpzh Office ( 213 I 3 * Library File ^ 213 ) 4- - #3.0 Building, file -< V fv ------*- 'fr! . 1,4.4 . .- 10 * n12 Serial So*' JfcJ* 48-18 Copy 80* is3i.SK mm *13: :' OOiaa Jt&SBftftM BSfOEf 4>99NMc . Pinal Rort <i Title* REPORT OH THE MANUFACTURE OF IROH BLUES Period Covered* Charges NOTE* This report was prepared by Production Division personnel add is being incorporated in the Chemical Division files at the suggestion of J* 0. Morrison to afford greater accessibility of the information for the future* JMT* R. B* MORTON KH BOMROEDl June 25, 1048 dmotso BY # c, W. OSKINS Dim ISSUED s Aug 10, 1948 DUP050067035 4 GO it Messrs -i <. Ii o Chaiupaki I!,, Arnoul 12 r> A a 0StCS D. A. Dear?. t.T* Gemmlll JU O OQ C E Poranski E, A, Tiller c,, w, -q s k b s . mnx sG;>mn&on k a k ih g g :lgmv<nta - 8 ewarte Rewark, lew Jersey June .6* 1948 JUL 5*3 19#tr W,ES, mmrs o h t h e ma ij f a c x t j h s o p p r o m mm Ewing tbs shree and a half -weeks beginning May 27, the svsjor portion of .fifpsjm batches pf Iron blue manufacture were .followed 5r detail the object was to determine if there were any inadequ&ts 5rati notions or eqtti|3*nt, also to ewe if it was possible to adhere to the strike cards. While doing this the deviation froa operator to cperator was observed* The various points will be developed according to the sequence of operation in -tite making of Iron blues* Ftriko ,Vat Cleaning of yate during *hls time was done according to the ?3riie card * 'It was found that the vats on the first floor required ms .hour to run the vfsnty inches of rinse water out .after washing the vat out from within. .To determine if this step Was necessary* samples of the rinse water from vats inspected by the writer were taken which indicated this step was necessary X feel that 'at least one aiaker dees not normally enter the vat to hose it down from within and that at least one maker did not previously rinse the vat with twenty to twriy~flve inches of water after washing vat out from within* This cm -maker believed that the good washing out fraa within covered this point. foughly half of the operators take advantage of the hot water heaters used for* heat ing the water for the one inch hose line used in washing out from within the vat. There were various excuses for not using it,. The stack and agitator water seals for the sealed vats were sufficiently clean with the exception of the stack seal on 280 vat* Two factors cause the seal to be completely flooded with blue pigments they ares 1 Steam and air sparger is located almost directly under this seal and 2, the seal ie so constructed that normal cleaning ; does not olean the seal, outi > . One or both of these conditions will hays to bo corrected to eliminate this condition as it Is possible that a small contamination of the finished pigment trapped in the seal might get into, the slur* Jr being f ' -l DUP050067036 .aeafced prior bo -oxidation which Is undesirable, 2..F.8* Solution! The procedure used 1 handling' the liquid Y.P.h, lies beer. {fcsx.gsd sc many tires in a relative short fcim that confusion existed f'rom shift, to shift os this matter * The colls in the storage tanks i-PP-e to haye been repaired for the time beingf however, any drop in analysis from day to day should be watched closely and the Sead-flnlsh tree questsoned toa'cemlng it Sometime it is difficult to obtain . t-oni Irmatlcn of the storage tank being need due to inability to reach ' qualified persona to check this* ' The strike temperature for the 1f*h.,S. solution for the large siee lllorl blue is approaching, a critical point, As the water hasomoo during tho surauer months very close control will be necessary on the storage tanks for T.P.8.* Even with close control at this point at times che strike temperature may not be obtainable using water alone In making the y,,i?*S* solution for PB-S and B-63, it is neeedsary tc neutralise the cyanide excess with diluted copperas. This is dene by slowly pouring the diluted copper*s Into the with agitation fo re.fi'.. I lor la made on the strike card as to the necessity :f neutralising the e: cess or how to do It. One operate followed t^patently was net In. 'lie habit c>f diluting the copperas The oytnlde excess in the T.P.8., has in the pact varied quite fiddly. One portion p-.3mpod for a batch was found to have an excess of throe -tenths of on percent., Several *ere close to one** tenth of on perernt The scale ?at 380 Used for weighing and diluting the If.P.S* jumps 1 'from stop ago w* a found to be corroding, quite badly. The oxide formed In blisters below the normal liquid level and heavy seal.above that level, especially around 'the manhole and steam sparger Inspectton also revealed that the silent steam heater had been installed in such a manner that it caused erosion on the side of the vat* This was eliminated by turning the sparger slightly*. The outlet plug cook on 30 Vat was found to be leaking. Thirty to forty poinds of solution leaked into the lines going to the first'and second floor r? * This plug cock will be replaced when the new quo on order is recoiled. The scale mechanism for 30 Vat is In need of better support to reduce the wear on the parts of the.scale* Walking along the floor behind the scale and handling of drums of naptheaie acid and ammonium .hydroxide in the vicinity, cause excessive vibrations and therefore wear on the scale mechanism. . Pulling the lever to lock the mechanism Is not practiced as much as it should be* Aaaaonlum Sulphates Dissolving this material in Vat 83 was found to vary from operator to operator* Some methods were a harigover from dissolving hard lumpy material. Using the present ammonium sulphate, the method on the strike card was found to be the beat* The other methods put ,* . ~2~ DUP050067037 too ,auob of a strain a the agitator at the beginning* If wo are foreo'! to us hard lumpy material ia the future a different method may be needed for this* All volumes and temperatures for.this operation were obtainable and in generalt followed by the operators.. Weighing of this material was watched closely and fit was demonstrated again that this step is necessary* Bags varied from tfi pounds to 108 pounds net* Shis resulted in a difference of 26 pounds in one batch, Despite the difference in wights some makers are not: thoroughly cold on the Idea, Some of the makers, I believe, weigh this material for almost every batch and others weigh It when they are being watched* Considerable time was spent by several, makers in figuring out how much had actually been added to the vet* 1 believes, a blackboard mounted on the back of 351 vat scale would be helpful for this job and also remind the maker this material is to be weighed* The board could be used when weighing other materials such as-chlorate and napthenlc aoidc ;> The scale used for .weighing the dry -materials for the blue manufacture was found to be sticking and the weights obtained could not he relied upon* A mechanic mad an attempt to correct this condition but failed* The scale mechanic had previously worked on the scale and put it in order for a short period of time. The scale was removed from service until the scale mechanic returns to correct the condition* Copperas Solution?* . <**.* Oh mW. HI mu . Or; the first two batches followed two mistakes in copperas s weights were corrected One was an error in reading the seal weight that amounted to 1,000 pounds, the second an error in calculation of 500 pounds* Pumping copperas to 382 was done much as it should be but for two exceptions* In most cases no attempt was made to close the outlet valve on 192 storage vat in 36 building whoa finished pumping. Most makers pump 388 vat full and no room is available for diluting the solution if it If above 25 Be*. A job breakdown was written covering the entire operation and circulated to the shift group Supervisors with a memorandum on these two points* Preparation for Striker In all.cases some water was .run in the vat prior to adding the copperas and ammonium sulphate solutions to the strike vat* This volume la not critical as it is made up before the strike is made* Mi Changes in agitation rate in the strike vats was at a minimum during the period covered The one change made was very plainly marked at top of the strike card. This practice should be continued for best results* It appears that no difficulty will be encountered in meeting the strike temperature ip the strike vat, winter or hummer* A suggestion was received prior to this study to reout the cams for the temperature controllers so these instruments could be used to heat the strike vat to the required 78!'* This idea has been accepted and a work order *$**> DUP050067038 i^utvd to c'o the work. Some makers made the vat one Inch short of the required volume and then heated the yat to temperature,, X'hi-s was evidently a carry over of winter operations After the vat was at temperature no measurement was made to check the volume* It ms demonstrated that the vat was not at correct volume using this procedure* Strike of YP*S* .and Sulfuric Acids The time required for YcP.S strikes cn 11 but the large *-ie mil or i blues were obtainable* Strike time for these batches ranged from 40 minutes for strikes in the second floor vats to 43 .minutes for strikes in the first floor vats* The strike was timed from opening of the valve until the .amount left in -380 vat was 250 po-unds, Thi * ebnnps in time has been innorporatnd in the new strike cards for these batches The *?.S. strikes were adequately screened by box screens in the vat openings * Suitable screens for under the surface strikes are not on hand; however, this type of strike Is not contemplated in the immediate future,, The addition of sulfuric acid to the batch proceeded normally on all batches followed and no difficulty is expected in the future* heating 8 truck Slurry? It was found that follow-up on.the progress of the temperature controller during and after the heating cycle Is very necessary* This is a very important part of the making of an IronBlue and occasionally the controllers fail to perform according to the, requirements of the strike card* The instrument giving the most trouble is the one located cn 281 vat* The slurry could not be brought to temperature in the required time using the controller* The controller has been adjusted several times and it now appears to be working as it should for the first time in several months* The instrument on 282 vat was found four degrees high, was corrected and two days later was again four degrees high* After the last adjustment no further change has taken place* . In general the controllers were within plus or minus two degrees... The steam valves operated by the .controllers on 280, 181, and 380 were all leaking through* Work is under way now to repair these valves. The cause for the leak through is wire drawing brought on by the throttling of the valve when close to the control point. The instrument mechanics are investigating the possibility of eliminating this through adjustments to the instruments. It is the writers opinion that more frequent routine checks should be made cn these instruments by the mechanic* -4- DUP050067039 Miscellaneous Solutions; Sodium Chlorate solution was made in two different ways* There was not sufficient instructions for uniform operation One method was to put 8<=>1.0 inches of water in the vat and dump the" chlorate in on this -water then dilute, agitate and heat with steam*, this method resulted in mild solutions of chlorate toeing splashed cut of the drum, ' The other method which was adopted was to add chlorate dry to the vat then dilute, while agitating and heating sift steam.c The bichromate solution was made according to the card except for volume required,, ffee tendency towarde 'higher volumes vas noted. Ho Inches were specified on the strike card to correspond to the 40 gallons figure is in part en explanation of this. The new strife cards are providing this in'V.ma^lGrn It should he noted here -fiat' the,, volumes of the chlorate* bichreme 2nd iamiaonruia aapthenat are not critical as long a& eolation la obtained The amnonima napthena te was mad accord lag to the strike -sard except for .a variance of three to four inches in the volumes 0 Park clear solutions were obtained In all cates, The ammonium hydroxide was not added to the diluted napthenic acid in two to four minutes but dumped in* . Prom observations of air cooling It appears that mechanical agitation for short periods of time would to helpful On batch did not appear to be cooling properly and no mechanical agitation had been applied during the cooling. Agitation was used for three minutes mxd the slurry was found to be thirteen degrees cooler than before the agitation. Just as this hot spot oocurred around the element, cold spots may be around the elements for thermometers In other vatSo Instructions covering this agitation are included in the new strike card, ' Conclusionsi The cases where quality, equipment and safety was jeopard* Iz.ed were corrected. Reasons for doing the job differently were' given the makers at th time. This one correction and explanation is not considered as having solved the problem, Only constant follow-* up on the part of the individual Group Supervisors of the important points will do the job. Attached to this report is a list of important points that can be used as'a guide in checking the making of iron bluea, v DUP050067040 MAIOTO. CHECK LIST IROH BLUE Preparation of Vats I,-. Have maker report; when mt h&a been washed out; from within8 occasionally inspect 2r Check to see if the 20~2S inches rinse water, is used. Check agitation rate on card and at rat, p , P -,S Solution; 1- Analysis in bock, 2,. Strike temperature and volume, Ammonium Sulphate Solution; X, Material weights* 2, Solution screened into strike vat* Copperas -Solutions 1* Sludge washed out of scale vat before pumping* 2* Calculations of weight. Strike * 1* Strike vat to volume and temperature. So Time required to strike, SK Screening of strike, 4, Calculations on Sulfuric acid addition. Heatings 1, Temperature before heating, 2, Time required to heat, -3, Accuracy and conditior. of instruments Miscellaneous Solutions? 1, Spills of chlorate, 2, Ammonium napthenate solution. DUP050067041 Air Co&I&ngs X, Agitation during air sooling and be.fora obtaining final temperature 0 DUP050067042 r.nnF: B-2I6-D K# ROAl ; 4157 SIZE: DIAZO VAT: COUPLING VAT: . STRIKE VAT: 181,182,282 , (B) APPROVED BY: HAj 6-10-48 CM): 6-11-48 NON-BLEEDING JDs 6-1^ ---- ------------- -------- >------- '------'-----'--r------------------------ ----------:------------- ------------ VAT NAME: M1 LOR 1 BLUE INSTRUCTIONS USE LBS, N- CODE ACCT. LBS. S. Pu mp in t o s c a l e t a n k 380 1 _ CNxs . T_______ _____ M ..... _,,................... .......... < 594 5897 QNxs TM * ... 594. Oft ........................ A- By a r t w a t e r in t o s c a l e t a n k 380 B Tu r n o n a g s t a t o r a n d s t e a m. ~ f,. We ig h a n d d u mp in D. Ad j u s t t q 77"(3053ft) a t 104-I06F. 4 E- St ir 20 min u t e s o r l o n g s * t o d is s o l v e . M3 sc. " 2. We ig h a n d mo l d a t v a t 383 f o r s t e p 5 .................... 1700 340 1700 m 3 Ru m 15-20"(+ 2450) h a t e r In t o v a t 383. 5. Tu r n o n a g it a t o r a n d s t e a m. ' 5. Du mp in N-340 w e ig h e d in s t e p 2, 6. a d j u s t t o 4o w (4900) a t 70-7S*F. 7. St ir 20 min u t e s o r l o n g e r t o d is s o l v e . S.V. 4 ""389" 5 8. Re mo v e s t e a m v e n t s e a l in s t r ik e v a t . 0. Ge t in s id e s t r ik e v a t a n d h o s e t o p . w a l l , a g it a t o r THOROUGHLY CLEAN. 10. RUM 20-25" (4 26250.) WATER INTO STRIKE VAT WITH AGITATfOH. 11. Bl o w s t e a m l in e s . 12. Ru n w a s h w a t e r t o s e w e r w it h a g it a t io n . et c . 13. WEIGH AND d u mp in t o v a t 309 14. Ad j u s t t o 24"(400). 15. He a t t o I20-140*F t o d is s o l v e .- 226 12 226 w 6 16. Ro n in t o s c a l e t a n k 307 f r o m v a t M 17. Ad j u s t t o 24" (400). 38. St ir t o u n if o r m s o l u t io n . 343 T 4 8 .JTL "pT 19* We ig h a n d p o u r in t o v a t 388 20 St a r t a g it a t o r . 21. Ad j u s t t o 30" (86g ) b y a g o in g w at er sl owl y. 22. St ir 3-5 min u t e s t o e mu l s if y . 23. We ig h a n d p o u r in in 2-3 min u t e s 24. St ir 5 min u t e s . 25. Ch e c k a n d r e c o r d : s o l u t io n CLEAR, . . mu s t b e d a r k a n d . ... 243 399 243 122 <5 . .. Y* 26. Ho s e t o p w a l l , a g it a t o r e t c . o f s t r ik e v a t f r o m o u t s id e OF VAT AND RUM TO SEWER. 27. Wh e n u s in g v a t l8l o r 282.*s e t a g it a t o r a t 16 RPM. 28. Km 5-15" (+ 10506) w at er in t o s t r ik e *v-ak'-tVv. r CONTINUED ON PAGE 2, DUP050067043 * 0-- <W VAT "lEO 9 Pa c e ; Co o E;8-2I6-D LbS: 4157 in s t r u c t io n s ' USE LBS. 29. We ig h a n d p u mp INTO s t r ik e VAT PROM VAT 382 p H Fe U p H Fe M 30. Wh e n s t e p 7 s t ir r in g c o mp l e t e d . r u n v a t 383 VAT THROUGH SCREEN. 31. In s t a l l c h a r t in t e mp e r a t u r e c o n t r o l l e r . 32. Ad j u s t t o 39" (409f5G) a t 74-76*F. in t o 4 4 s t r ik e NCODE 24 24 ACCT, LBS. 5894 55. Ad j u s t s c a l e t a n k 580 t o 77" f5055<3.) a t I04-I06*F. 54. St r ik e v a t 380 a t I04-106*F in t o s t r ik e v a t a t 74-76F o n t h e s u r f a c e in 40-45 MINUTES. 35. 36. Ru n in t o s t r ik e MINUTES St ir 5>1n o t e s . v at f r o m sc al e t ank M in 5-10 T 4 37. Ch e c k a n d r e c o r d : *F. 38. Te s t a n d r e c o r d : c o r p e r a s XS |(|. mu s t b e +. 39* He a t a t o n c e t o l79"l8l*F in 57-63''Min u t e s . Re c o r d : tiMErSTARTED 40. Ch e c k a r d r e c o r d a c c u r a c y o f c o n t r o l l e r : Lo w it me r mo me t e r F Co n t r o l l e r *F. Hiq h : t h e r mo me t e r .,,... F Co n t r o l l e r ....... F. 4l. St ir 30 min u t e s a t I79-I8I*F. Re c o r d : t ime s t a r t e d 42. Ru n v a t 389 in t o s t r ik e v a t in 2-4 min u t e s . . 43* St ir 1*5 min u t e s . 44. r u m v a t 587 in t o s t r ik e v a t in 2-4 min u t e s . 45. St ir 15 min u t e s . 46. Ru n v a t 388 in t o s t r ik e v a t . 47. St ir 2 Ho u r s . Re c o r d : t ime s t a r t e d 48. Sh u t o f f a g it a t o r . 49. Air c o o l f o r 8 h o u r s o r l e s s t o l40-i45*F. . ... . Re c o r d : Re c o r d : Re c o r o : t ime t ime st ar t ed st o pped *F. 50. 5 h o u r s a f t e r s t a r t o f a ir c o o l in g , t u r n o n a g it a t o r FOR 3-5 MINUTES. 51. 6 HOURS AFTER START OF AIR COOLING. TURN ON AGITATOR? FOR 5-5 MINUTES. 52. Be f o r e r e c o r d in g f in a l t e mp e r a t u r e in s t e p 49. STIR 5-5 MINUTES. 55. CMEOK a n d r e c o r d : ", NORMAL 77"(8085G). 54. IF NECESSARY, FLOOD TO |40-145*F. Re c o r d : Re c o r d : F. 27 *f 2349 55. Pr e s s w it h a g it a t io n . * ' TIME START kw ft tt TIME FIN it tt H ft OPTR tt tt ... O 4f#/ /6S" DUP050067044 S~2X6~D <B). fix i?B5i process replaces the previous standard formula K-2809 and differs as follows4- X The process has been established oa a stepwise basis 2 fbe batch sis has been increased from 3353# to 4X57# ia order to .fill two 60 fleas presses la. place f two 50 frame presses*' .5* Newark manufactured TfS liquor is used in place of purchased TPS crystal, 4* As a result of the increase to batch sis, it was accessary'to change the strike volumes and temperature in order to obtain a temperature after strike of approximately 90F* Higher temperatures* such as XXB^F* result in lull tint* 8* Ifsw&rk TPS (contains high sulfates) gay dull tint m compared to crystal TPS* In order to mini mise the effect* it was necessary to reduce tlx copperas from 215$ to 15$ excess* 9394# copperas is used in place of 4253#* 6* 1 slight reduction in Ammonium Sulfate* 1700# in place of 1762#, was mad in order to control maostone depth* 7 fhe sodium bichromate was -reduced from 234# to 71# without adverse effect* in order to decrease cost* Tea total oxidant has been reduced from 1*50 qui vaXsnts to 1,16 equivalents based on the pigment * 6* The formula does not request the temperature to be held during the stir period after the oxidant addi tion since in plant practice the temperature rise approximately 5F at this point* la the laboratory .however* It may bo necessary to hold the temperature during steps 41 to 47 inclusive* The following calculated composition and goal yield are copied from the IC-2209 formula Sad have been adjusted for batch slas* The goal yield is to b redetermined* CALCULAT'D COMPOSITION GOAL YIELD Iron Blue Complex Organic Agent . 96*7$ 3*3 . msim "as is" 4157# Anhydrous 3957# Boisture? 4*8$ Referencei UB 1115-46 Additional information and variables can be obtained by referring to the K-2209 notes* H* ARWO0L 7-19*48 DUP050067045