Document XOBR1Vv72rLEbENB7jb98wR7w

E. I. DU PONT DE NEMOURS & COMPANY PIGMENTS DEPARTMENT 256 VANDERPQOL STREET NEWARK, NEW JERSEY u m n P-52'19 Copy No. / j i i NEWARK PLANT CHEMICAL DIVISION - COLORS NON REACTIVE MEDIUM YELLOW Y-662-D FOR USE IN I.P.I'S 'K6" AND 'VAt 'OSET'' VEHICLES Priod Covered May if 1952 * September 15, 1952 PILE: DATE; <=?//./ 1A/53 j i I NJ 5747 4 #1 - Numerical File 2 - Research File 211.1 3 - Library File 211.1 4 - H. Arnoul/Plant File 5 - J. N. Tully/A. Siegel 6 - W. F. Spengeman/Library Files 7 - Extra 8 - Extra KN-52-19 Copy: NEWARK PLANT PIGMENT COLOR RESEARCH REPORT FINAL REPORT TITLE: NON REACTIVE MEDIUM YELLOW Y-662-D FOR USE IN I.P.I.'s wK6n and "Vaposet" Vfehicles PERIOD COVERED: May 1, 1952 - September 15, 1952 CHARGE: 1101-11, 12 -3 SUBMITTED APPROVED B DATE SUBMITTED: 12/1/52 DUP050069113 -1- SUMMARY AND CONCLUSIONS: 1 - Modification of X-469-D "Ftt process has resulted in the production of a non-reactive type medium yellow similar to Imperial's X-1810 or Imperial^ S-3268, 2 - These modifications involved the following changes expressed in terms of lhs/raol of lead nitrate struck, (a) Reduction in use of Aluminum sulfate (N15) from 48 lbs. to 16 lbs, (b) Reduction in use of titanyl sulfate (N390) from 6.8 lbs* to 3*4 lbs. (c) Reduction in use of "2ndtt lead nitrate from 34.73 lbs. to 30.5 lbs, (d) Ommission of all petronate (K390) (e) Use of tetra sodium pyrophosphate (N479) at the rate of 6 lbs./mol lead nitrate struck, 3 - A degradation in lightfastness versus Y-469-D has resulted because of these changes. This is not serious since all competitives of the non-reactive type are markedly inferior to T-469-D in lightfastness. 4 - The product produced and standardized as Y-662-D lot 765 is superior in lightfastness to Y-661-D or the competitive pigments. 5 - Investigations have revealed that zirconia treatment of Y-469-D processes will result in products of improved lightfast ness. 6-- The use of recirculation of 68 centrifuge fluid discharge to 66 and 67 centrifuge feed lines offers definite possibilities for improved washing of #12 Building products. PATENT STATUS: studies. Nothing of a patentable nature was developed during these REFERENCES; N.B. 1356 - 1437 DSN 52-8, 52-6 KN 52-18 KN 52-20 I. DISCUSSION AND BACKGROUND: The introduction of new vehicle systems in the paint and printing ink fields imposes frequent adjustments in the chemical and DUP050069114 -2- and physical characteristics of chrome yellow pigments* This is not a new situation in the pigment field but is a chronic condition that must be faced as progress is made in the consuming industries. Accordingly, constant revisions and adjustments in our pigment formulation must be made in order to manufacture products suitable for use in these fields. During the years 1949-1950 it became apparent that our medium yellows Y-469-D or Y-6619D were inadequate to meet the competition of Imperial's X-1810 and S-326# in rheological character istics in various vehicles. Complaints were received from the Socony Paint Products Company concerning Y-469-D reactivity in a phenolic modified alkyd system* The International Printing Ink Division (IPI) of the Interchemical Corporation stated that *-469-0, Y-434-D and Y-661-D were unsatisfactory in reactivity for use in their "Kb" lithographic varnish and "Vaposet" vehicle systems. Minnesota Mining and Manufactoring Co. reported that Y-469-D and Y-661-D were excessively reactive in their traffic paint systems. In May of 1952, the problem of developing a medium yellow satisfactory for use in the IPI "Vaposet" systems was assigned to the writer, (For a review of this subject see American Ink Maker 2^ No, 4 33 April 1949)* lb is obvious that an economic solution for this problem must involve an evaluation of the working properties of any experimental pigments in all of the fields involved, since continuous manufacture of many different specials would not be a practical solution for the reactivity problem* The goal was set up of a pigment satisfactory in all vehicles mentioned hut with emphasis placed on IPI's requirements, 2. EXPERIMENTAL: A. Evaluation of Standard and Competitive Samples Investigation revealed that IPI was using a special medium yellow coded S-3268 for "Vaposet" use* Our examination of this product in the customers YV-1304-H vehicle see TF (2403-2) gave the following results versus our standards and various competi tive products, when tested according to TF-2403-2. See table t-JFSie 3. This test has been modified in accordance to Dr. Larsen's instruction to be ground with a roll setting of 120F in order to minimize effects of moisture variation in the atmosphere. Since the vehicle is sensitive to water, it is imperative to control that factor as rigidly as possible. Considerable variations in values for "good" pigments result in duplicate tests. High viscosity pigments always give no flow on the 45 inclined plane. The test has been simplified in this work to consist of a flow reading alone, instead of the usual body, length and flow measurements. No evidence of "reactivity" in the usual sense, i.e., increase in viscosity with time, has been noted. Usually viscosity drops (flow values increase) with time. DUP050069115 po XI P xo> & Mt0o) I <D TbtOO Cv I pd to ON On to CO*N- t<om ft, C oo o HCHO s tNoO Conn- OC*- CJMN 00 C TJOSfx. TO o ON O NO Xf tUoN CTH I Ch p OTO fNI- ON NO UfN VO1 4 o n -4 UN UN TO Of s CM < |X4 ON ON UN -4 -4 rH I 1 1 cd to to O CM H -4 ON ON 1 1 1 COMPARISONS OF VAPOSET FLOW OF EXISTING STANDARDS T!>O*Pu COIMN o (0 XI r- o O C*--Mi -4f CM uTO P(0 lx, p XI <t TO H r-l C!>MI i rH o CM H XO3 s I iH pTO lx. TOPOj TO >03 P H ,C--Mi Ii o ON o o ON HC to ON CM to o o UN ON NO o ON [> ON *--i -4 UN UN oi NO UN ON r4 u\ -4 UN NO UN oO UN M to o 1--1 NO to CM i--1 -4 3 UN -4 W ft} m - TO XI O O 1 ON rH NO NO -4 NO 11 tH !m ON A 1 X to CM O O rH ft. UN TO a I *M O TO PTO TO P PTTOO Q. TfOt Cm O rH TO Orl P, >s P 2 TO O .TOO TO Wa) rl XI TTOO DUP050069116 -4- Inspection of the above data and other tests revealed that both I-469-D and Y-661-D standard, as well as typical products, were unsatisfactory in I.P.I. Vaposet and K-6 tests. In addition, the customer stated that Y-661-D was excessively sensitive to darkening on drying. The latter is known to be associated with the use of cobalt drier in the customer's vehicle. B, Laboratory Studies a - Factors Found to Increase Vaposet Flow to 1. Decrease in Alum usage 48 mol/16 mol NB 1358,55,56, 57 a) effect on K6 Reactivity - beneficial - lower initial consistency also. b) effect on Socony Paint Products Reactivity beneficial. 2. Decrease in titanyl sulfate usage NB 1358,57,60 , 1437,1, 4 a) effect on K6 Reactivity - ineffective on reactivity but lowered initial consistency. b) effect K6 Socony Paint Products - ineffective on reactivity. 3. Ommission of Petronate NB 1358-55,56 a) effect on'K6 reactivity - harmful in high alum processes b) effect on Socony Paint Products Reactivityprobably slightly worse 4. Use of tetra sodium pyrophosphate NB 1358-55,56 1437-1,3,7,11 a) effect on K6 reactivity - beneficial b) " " Socony Paint Products Reactivity- beneficial c) effect on Minnesota Mining & Manufacturing Reactivity - beneficial 5. Use of Lustrex 820 NB 1358-62 1437-1,8 a) effect small-inadequate to justify cost b) products do not disperse in Varnish Drier. 6. Sequence of Treatments NB 1437-3,8,12 a) best sequence alum, ,rLM liquor, sodium pyrophosphate, 2nd PB b) effect on K6 reactivity - nil C. Factors Found to Decrease Vaposet Flow 1. Treatment with fatty acids 40Bs/mol NB 1358-55 al effect on K6 reactivity - worsened 2. Use of Zirconium hydrate NB 1358-57,60,63 ' 1437-1,7 , a) effect on K6 reactivity - beneficial(when DUP050069117 -5- alum replaced with zirconia) similar in behavior to Ti02 treatment. The simultaneous use of zirconium and pyrophosphate was not satisfactory for Vaposet usage. Products could be made exhibiting excellent lightfastness and a low level of reactivity in K-6 using 3*4 gr. TiOjj and 6 gr. Zr02 per mol in place of the usual AlsOj/TiOz treatment. Future study of this treatment, in conjunction with variation in alum (N15), "L" liquor (N390) ratios should be undertaken if the problem of improved lightfastness is reopened. 3. Use of Wetting Agents - Aerosol OT, Dupanol WA, Potassium Daxad KB 1353-62 a) very little or negative effect, , 4. Use of High 2nd lead KB 1437-3, 12 2) effect on K6 reactivity - si worse higher quantities second lead give products of better lightfastness. s 5. Increased Final pH KB 1437-6,6 As pH increased Flow decreased pH o.O better than higher pH's 6. Underdevelopment of fellow KB 1437-9 As percent underdevelopment increases viscosity rises 7. Casein Wash of Finished Press cake KB 1437-1,2 (studied in connection with thixotropy) 6. Nopco 2125 Treatment KB 1437-13,14 (studied in connection with thixotropy) 9. Effectiof Washing on Vaposet Flow DSN-52-6 Complete absence of washing of #12 Building material results in very small Vaposet flow figures. The standard repulp water flow rate is 20 gallons per minute. Lesser quantities have not been ex tensively studied in #12 Building. In addition to the previously outlined studies, the effect of redrying was studied. This was found to be ineffective. Data illustrating these points are given in Tables on Pages 5A,5B, #12 BUILDING STUDIES: 1, The first attempt (see 1437-2 DSN 52-6) was to make Y-469-D in #12 Building, testing the alum/Na4P207 variable. These products coded Y-662-D (6756-6761 inclusive) were made on standard formula except- Condition (1) Slum used at 6 Ibs/mol N-479 used 4 lbs/mol no petronate lots 6756, 59, 60 DUP050069118 TABLE 2 ~ EFFECT OF VARIABLES ON REACTIVITY AMD PLOW eol m -v:-l *'3 43 (A fil v-t -P ,.p) U i! S$ 0 i> 4.3 itf a V f *H: *. si U\ ts 0 0* P0f SSE H fS1 f -*i | 1 Sri f som xQ 0SfOCf.-sS M3- ** kHgS| sO lr. /S. 4\ xO so V(SVtNlf\vS> f t ff f t $>* hs I -P W enjr ,:f fa r*^ cncM^ cvm J- 4.3 O # i.i.4 0. s"l| as| \0 *(* P. "1* /no CSO- ra capv /sV^|- 0rtj- CM O: sOsO-C.svO 8s H j'OSfsOf'*! J- rf>CM (* '* HC r4 IfN g O g* p- ...,, H m! 0'S Os YrsVK 11 CM <M/'Off? O SN J- CM m Ps- Csj: CO CM Ms CvO {M W CO s4 -P O 68 O CM 8 4H oo ,Psr 1 If-co,l > . vof Ss - .m' o i-i O P*mj a4fHe, S. h ca]l m CM rairs o P'1 $ o ert k -PL 43 cgf. f,Pt, afS vw* ,, m r-t ri O O H a CO On t o H CM op.so c\- o c j CO s0 l\4* rA r`( ft CM^-sH O r"4 0 o H: a o `?0. ^ rtOOOH A p,, P^l ;00 o.. pf- e> OcoJ> OOO so J' JrlOO Jl CM o -is4 Ef m. ?>. o fpft-"i o Ss cu n0'-1s *4 S"?| eocooscoco \Q vO M5 s0 so coo <r. <* s0v0 COCO >; 9 vOsC CO CD CO co 0 co CO CO CO CO CO CO *- 1 n s. < vOvO'OvO -OMO SO so sO vO vO sO @ 4Jn*3` A $& -W COCOop co eo CM CM CM Oi ora CO m CM sO- vO sO vO > sp r4 r % r-$ r I: r 5 >H: Cs' COiOCOCOO fi O' 5^> *c*' rft. $<< Wfp tf\ CM r*i i ICs V\> ir , 4 w\ 005. i>i-00S lf\ mU\ cIrossctor1s- Vc^trs ss VCSU\ lt coco UMfs ,w<4 c5 U\ 1- CD 1TN pa CS U*s } 1 5- CM CM MMi-S r*S r^sOsO sr"'l vUOsSIOArtl HIVCNN. co4- 1 1f1 * sststNeec ifs m m m>csics f cMoIr\c'i.otc\fOa?:fs>.'i8sS'M.ero*s Cm @ Or! fe.8r"!` cS sC-O3- C0O m r-| pj- m mm mm r~! t""! fH r-{ i" ! rM rO r"t t--l r-! t'! j --! m.- t mcM ro ;~nJ .0 t-.J r t '.'I r~t rr4: DUP050069119 pft a> s p as 0 ft Eh O O8 <y to X X 0ft 0ft p p OftJ rH r\ 'S& CA ft W PrltOP <D 05 Nil *H (0 o cy ft OP,O <t*\P 0J I 00 <v > . CH H O C, I Hft,frr.H.HEVN| CVtQ C\j-4 1 0ft 0 pp 0ft ft 0ft 0 ft 1 f8t5r)\ 0 p- s$s 0OO0 35 35 3: 3! is 0 N ft. o| Eh w P cy ft, 0000 01 Pk as os a. 1--1 -3; O >E 3: ft tf) o ffl Oh OJ CO M SO rH T-f <0 tO* tO*-CO rH r Eh NO NO NO NO PQ -< s > ft, a co Eh Eh !3 O M ft,ft, Eh <4 w Eh CA Mi w rH Eh CQ co m < t=> Eh rH 35. CV CVNOsO CA CA 1--i rH "4 ft, I I W *T> CM 2 I -ft NO rH II to t> CAS CAE CA -4 rH P a$ CJ > P1 n- ft CNJ H H O 0) P 03 0ft Eh 1 f0t 0 ft OO W 35 3; XS an {V rH (4 rt 44 oT-O Pft fc ft ft 60 rH s0 O CO eft 0 5031 H rH CO <P rH a8s M Qf MI 1Eh "ft <ty cm M nn- Cft CACA rH rH rH <30 m rH 1 0 fHt 0 m mft 5h P O 0) 01 0 mP P 0 01 ft 0 P X) X 0 1 ft ft 0 ft 0 0 ft Ch . 0 P +* / P ft P P P ft P 0P 0 0 h P 0P P P rl PrO rH 0 rH , +0* t. PEW -HWP +| * O rH ft, rH as H 60 rH t>- O IA CN1 CNi IA O P cvNOtN-tocH-LAC^-eo rt C H I--1 60 rH P1 ft, M X3 0) ft > cy ra ft w 00 P ft hOp H H PP rH ft ft ft 00 pp 0 L 0 p p ft P 000 p p P PP p 0 ft, 0 P 0 CA P rH rH 0 0> m P ft 35 1--( W a K > l> E ft 0 P P P H W f <A CANO O IA H vO -4C^o a n O NO 0 0 cy rl 0 O' T3 ft ft rH ft O o Eh P 35 CO -4-60 60 tO ft o ft ON -4 ON O a IN N {ft rH rH I (ft ft, (ft 1 CA as 35 Cy cy cy 35 35 S rH s ft On X) P H N ft (fts as to P s -4s cy (ft p I rH cy s 35 s p as bo S <ft rl ec o X) 60 -4 60 -4 I *I ! 1 I NO 0A I I n o oA I P P - ON `a E ft s -4* E. rH rH rH I rH P S < S 35 2 S fH0t, T3 ^ ON 0n0 n O nD NO to 60 tO 01 as H ""? rH rH ri --4 rH rH rH rH ft Ht 3; s6 4 4 CM 0 ft H BSftODPMfe I I I I I I I IQ -4t S S' 'I (N CAS 6 -4 rH pi 8 M CO t=> rH O s o o <{ (3IQ OI{IP ft1j CA I IN CA -4 rH ft, I DUP050069120 -6- Condition) Alum used at 16 lbs./mol 2. ) N-479 8 lbs./mol no petronate Lots 6?6l Tinctorial comparisons of these lots follow: 6758 vs Y-469-D-658 s.It--s.grn.s.dull 59 s.dk- " n 60 s.dk- 61 vs.dk- 11 tt 6758 vs T-66I-D 59 95500 60 61 s.lt-s.grn s.It-s.grn vs.lt-s.grn.s.dull s.lt-vs.grn. 6758 vs Imperial 59 X-1810 60 54336 61 grn.-s,dull vs.dk-grn.s.dull si.dk-s.grn.s.dull ys.dk-s.grn.vs " 98 s grn. * vvs red vvs red * vvs red * ws red 97 s.grn. 97 s.gnn. 97 s.grn. 98 vs, gm 98 vs.grn 98 vs.grn. 98 vs.grn. much worse It ! tt t W II vs-s. better s.better s.better s, worse vs.better s. better s.better vvs worse K-6_________ 6758 59 60 61 I-66I-D 95500 Imperial 3-3268 34 35 34 31 42 26 40 45 54 42 106 39 REACTIVITY TESTS IPI VAPOSET Initial Flow 0 .1 1 1 1 5 Final Vat Control condi(l) Lab. washed and dried 8 alum 4 M479 7 FVC condi{2) Lab. washed and dried Y-661-D 16 alum 8 N479 1S; alum r " ; '? 21 0 These studies show the beneficial effects of the alum/pyrophosphate variable in K6 reactivity. Vaposet flow was Inadequate to meet competition except in the case of the final vat control from coiid n2a which was excellent. Analysis of Lot 6761 showed 1% Po45content while final vat control from cojad "2" showed 1.62% Po>,~. This probably accounts for the difference in behavior of the plant product and the final vat control, and indicated the necessity for longer experimental runs to permit attain ment of equilibrium conditions in the plant. DUP050069121 It is suggested that the Quality Control Group might Undertake a further trial of this type process which was made without recirculation of centrifuge effluents and which did not show excessive bleed. The attainment of good Vaposet reactivity, which seems possible judging from results of the evaluation of the final vat control from condition 2, might be a desirable simplification of the processes ultimately used for standardization, 2. The second plant run, Y-662-D, A-6988, 89, 92, was based on a modification of the previous procedure in corporating the effects ' of reduced "L" liquor and 2nd lead studies and differed from that of Y-469-D in the following respects: N-15 (alum) N-390 N-490 Petronate) N-479 Na4P207) "Second Lead" Tank 58 used Standard wr 6.8 " 1% none 33 no Experimental 16# (per mol lead nitrate struck) 3.4 " " "" none g# "" t It "" ft II " t 26 ti it tf it yes (for better aging) Some difficulty was experienced .during the run due to peptization of the color during washing and resultant centrifuge bleed. Raising repulp temperatures to +140P and reducing the amount of N-479 to +6.3 lbs./mol eliminated this problem. follows: Comparisons with Y-661-D and Imperialfs S-3268 are as (a) Rubout in Varni3h Drier Y-662-D-6988 vs Y-661-D-95500 6989 " 6992 " Wet MT lt-grn lt-grn s lt-grn Dry MT s itIs grn si lt-s grn vs dk-s grn L/F vs worse + equal vs worse 6989 6992 Wet MT Dry MT lt-grn s grn-s dull s lt-s gr * vs grn-s dull t n Str. 97 95 Tint s grn w L/P *equal tr bet- ter s tr ws Rubouts show that color undergoes slightly greater change in drying or baking in this vehicle than does Y-661-D or S-3 (b) Rubout ih CPV-8677 (I.P,!, Robout Vehicle) ^;------ ------------------ tfet MT 6988 vs Y-661-D-95500 6989 * 6992 " v lt-grn-int v lt-grn-int v lt-grn-int Dry MT v lt-red-viint v lt-red-v int v lt-red-v int DUP050069122 (b.) Rubout in CPV-8677 (cont.) $-662-D-6988 vs Imp. 3-3268 6989 " 6992 Wet MT lt-grn-int It-grn-int It-grn-int Dry Ml s lt-red-int s lt-red-int s lt-red-int These rubouts in this vehicle show that the experimental lots are light, red and intense after drying in the customer's vehicle and appear to be more color stable on baking at 100F, Reactivity - K-6 - ManMichael Readings Initial 3 davs 158F Y-661-D-95500 48 Y-661-D A-7007 fcurrent prod.) Y-062-D-6988 33 30 98 65 6989 32 54 6992 Imp.S-3268 C$54709 " X-1810 C$54336 32 30 35 78 44 61 Increase ' 21 65 more 35)made with / 32)N-479 than (6992 46 14 26 The products are approximately equal in reactivity to Imperial's X-1810 but inferior in this test to Imperial's S-3268, the special for Vaposet. litial KU HH KU after 3 days ~T7ir KU after 14 days im. 4 weeks Y-661-D-95500 Y-662-D-6988 Y-662-D-6989 Y-662-D-6992 Imp.X-1810 C#54336 Y-469-D-658 71 68 69 69 70 71 79 91 99 75 86 94 75 85 94 78 101 140* 75 81 . 87 87 121 140 Vaposet I.P.I. - YV-1304-H Initial Body Length Y-66I-D-955OO Imp.S-3268 C$54707 Y-662-6988 Y-662-D-6989 Y-662-D-6992 Snheavy vs neavy vvs heavy ort Flow (initial) 0 8 6 5 11 Flow (7~days/l20) 0 18 15 15 13 These results indicated that material of the type of lot 6992 was satisfactory for use in IPI vehicles, but unsatisfactory in the Socony Paint Products Phenolic-Alkyd. A sample was sent to DUP050069123 i. -9- IPI for test. 3. The next run Y-662-D-7386 was designed to overcome the Socony Paint Products reactivity exhibited by Y-662-6992. Sister lots from the (Y-662-D, 69$8, 89) but made with higher N-479 content than the Y-662-D-6992 were satisfactory in this vehicle, but less desirable in the Vaposet vehicle. An attempt was made in this #12 Building run, to obtain material satisfactory in all three uses. Considerable bleed occurred during portion of the run which used an alum/Na/^Oy ratio of 16/6.3 per mol lead struck. The bleeding does not occur from the dewatering step, but only from the centrifuge used after repulping of the dewatered color. During considerable periods of the run, no bleed ing occurred. Control of treating agent flow was not good. It was also noticed that the load on the centrifuge was intermittent (as judged by filtrate effluent and ammeter reading variations). These * variations cannot be explained unless the pumps from the repulp vats to centrifuge lead tank were partially air bound. These surges probably caused a loss of color from the centrifuge, since the press cake is thixotropic. Attempts were made to decrease bleeding of centrifuge by: 1. Studying repulp temperatures and volumes of water. 2. Alteration of point of entry of N-479 (increased time interval between N-390 and N-479 addition points.) 3. Variation in amount of N-479 used. 4. Ommission of T-58 in connection with point 2 above. Complete control of bleeding was not obtained during this run which lasted only 11 hours. Longer time intervals between N-479 and N-390 addition points seem to improve both color properties and Vaposet flow as judged by evaluation of Fin Drum samples and plant grinds. The treating stages of medium and light yellows were studied in the following runs to determine optimum methods of handling alum and "L" liquor so as to get maximum lightfastness and color stability with minimum use of agent. 4. In the interim period, while the results of IPl*s evaluation of Y-662-D-6992 were awaited, work was concentrated on the known deficiencies of the product which involved: 1) A tendency to bleed while centrifuging the washed material. 2->, Excessive reactivity in Socony Paint products vehicle. These problems are inter-related since the known variable for correcting excessive reactivity (use of increased quantities of sodium pyrophosphate) is also the cause of thixotropy of precipitates and centrifuge bleed. Laboratory studies revealed that thixotropy of the press cake can be eliminated by means of a treating agent Nopco 2125 (non ionic agent) and also by means of washing with dilute solutions of DUP050069124 -10- electrolytes such as aluminum sulfate or magnesium chloride. Unfortunately the use of electrolytes seem to have detrimental effects upon reactivity and does not offer a practical solution to the problem. The use of Nopco 2125 in amounts from 1-3% does not appea^J$a3%iful to Vaposet viscosity. Reactivity in K-6 has not bean evaluated. A plant trial (Y-662-D - 765$) of the concept of recirculat ing the discharge of 68 centrifuge (wash centrifuge) back into the feed line to 66 and 67 centrifuges (dewatering centrifuges) has led to an apparently satisfactory solution to the bleeding problem. A tendency to the formation of a very high solids discharge from 68 centrifuge was noted. This results in a higher load on No. 68 centrifuge motor, and a tendency to hard stick formation on the fin drum. The dryer bed is only lightly loaded because of the high density of the solids. The process appears to be operable. Lower speeds on 68 centrifuge may result in a softer discharge cake. The products obtained as a result of this run which differs from lot 6992 in (1) addition point for use of sodium pyrophosphate (greater time period between Ti0S04 entry point and pyrophosphate entry point); (2) use of recirculation of 68 centrifuge effluent have shown definite advantages in quality. Improvements have been made in * 1) resistance to darkening 2) lightfastness 3) Initial Vaposet Flow 4) Socony Paint Products Reactivity SOCOKY PAINT PRODUCTS REACTIVITY Y-662-D A-6992 (not recirculated) Y-662-D A-7665 (recirculated) Y-662-D A-7667 (recirculated) Imperial X-1810 C/f54336 5-3268 C#54709 (Vaposet Special) INITIAL 65 67 72 70 DAYS 77 70 69 73 71 .1 WEEK 80.... 72 71 74 72 2 WEEKS .... 75 73 78 75 4 WEEKS W ' 77 76 82 77 Readings in KU by Stormer Viscosimeter. K-6 REACTIVITY Imperial S-3268 C#54?09 Y-662-6992 Y-662-D-7664 7665 7667 INITIAL 31 30 30 29 26 DUP050069125 -11 VAPOSET FLOW Imp, 3268 - C#54709 Y-662-6992 Y-662-7664 7665 7667 INITIAL ' 10" 5 15 18 22 7 DAYS/120F 21 16 16 31 40 A 15,000 lb. blend of Y-662-D production (95662-6) was then prepared for shipment to IPI. This material was a blend of the type made in the run {Y-662-D, A-7658) (araeireulatlbntofg 68 centrifuge effluent to prevent bleed loss)and earlier materials to make up to the 15,000 lbs. required. As expected, the blend was not fully equal in quality to the best material produced in Y-662-D-7658 run but was superior to Y-662-D, A-6992, and competition in rheological and tinctorial properties. A sample of the material made in the run Y-662-D-7658 was also submitted to Dr. Larsen (IPI) for his comments. Our eyduation showed it to be superior to lot 6992 ( first sample sub mitted) in all respects. To date no comment has been received in the latter samples, and favorable comment was received on the 15,000 lb* mix. 5) In view of the good results from the Y-662-D-7658 run, it was decided to standardize on this type material. A final standardi zation run Y-662-D lot 7961 was made 10/13/52 duplicating Y-662-D 7658. The run did not show any particular difficulty and a mix for standard was chosen from the production of this run and run 7658. Y-662-D SD-765 is comprised of Y-662-D lots 7665,6,7,9 7964,7, 7970,3,7, 7960, 7982,4 and 6. letter. jest data on this mix can be seen in the attached In addition to these studies work was also conducted on the Vaposet characteristics of Y-434-D. This code was found to respond to similar variables, in particular to the use of tetrasodiunr pyro phosphate, with or without a cut in alum. This work will be reported by J. E. Bishop in KN-52-20 and DSN-52-6. See also NB 1358-1417, The standard formula for this new process coded Y-662-D will be issued by J, E. Bishop. 6) Recommendations for future Study - The attached letter covers the recommendations.of writer to those concerned with #12 Building operations. DUP050069126 J S Booge f WllMagton D. B, lil'Hsffl* F S* Bolt-on* ** M* McLain* * 1* Tallys Iswark ,1,, -Siegel ,, * S* -H* Parkins* ** 4* B* Bailey* ^ C. 1% OsScine* 9 H. Hughes, ** B* JLn&ul, * t* Bagsves* * I* Js Hughes,, * 4* Bishop, * mmm, m mmm Mommu 12, 1952 tf. F,, flf) Sfi-Ul ll-lXiflCM OF T-66a-i 18-765 We-are ^emitting, for your approval* $-662~B H3-965* This iiatra is a mix f'v* sttter of lots taken froa two ooa aeea&lva plant iPmsu It Is fait that this lot is representative of what em fea prr4m atl is the plant* $hs attached Suwary gives the results or testing on this lot ' S***' . S*. ;BISHOP ; CBBMtC&l' MflSXQI DUP050069127 mSTWQ HISOLTS OS 1*662=B IS ?6S u S m u0 *c<. rtts Pa* S3 H ,. 4 o m m %r\ O &oH 8 frj Bg I s-> H ta m +3 & H > * I Sifcp H il I H A0oot' $H . 'mSt 2 S3 m 2 fit I f <3 *i >^'ri n t} ?4~,35 ,+H3 H49 > HP <S *O*4 * v ieg Ch* ~StsAnV4isS-v-Po 8CWA\\ o ft 0 ,4aNtOv*Mk*\ ^i>OvO*>O<*> b 5$ ? so 4> ** IS ;C3 JK> 4' j,!Wi o4n sa :^ig H *frojN.Ht i * Jw tsvO N 5 V DUP050069128 i St <8 s iS f> p Ti m $ is Mm is OISI'fNs"*j3f%f.Stfs. JO f<S 45J3* SB 0og >#t $4 a g* 4o *S,,| f#-! m 38 ssg |SW|r~i -H if~S iH! >*N *ri rt Isfa fci v9N0S> ~35 iC~O5 CO 5 O aHps l>a0C\OhvO^O|v *3 OOr~n wOnsv Oy^wtn' VNNN0*Ste n Ov o i s o ** w SS$ 535 ?} 5*? c*>5 QCJ *? pfl 4 8 03 a v *6 3V "tt L *4v*S -'i" 83* 45! $S Sn3 % M *aV*t^ S3 3*3 8H^-vWOWnOV'NnOO K' H. es DUP050069129