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'"w ... '*, :*r-. ' "- -V> .', ' - - *"&? *> * -X-* : * . : * * ,, ,, $ -S*?' ` < 'V.*.>?:. -.. V.&j/`9sr*vr< -'i;<,.' ' ., ..... -- j-- *k r>-- ' '' :; ..v-.; ' . "%? ' ;N'" - .- ; ,- . x-' r- "^--i rv % ., xv.. * vj-: V . ,:/ '.:; VflBTOSftK PLAHT'^ . ' -pxQrHSHT. ..COLOR RESEARCH REPORT 'l/: JAHUARY 1935 . .. v - $ i^ \V, " . 'd.^V*;' -V.?*i. ' > <;- .- :- - - :*.->''.'", 'su*`V wv' N36962 PIGMENT COLOR RESEARCH REPORTS JANUARY - 1935 I - IRON BLUES Yield Study - Iron Blues................................................ II- LITHOL REDS (a) Lithol Red RT-379-D - Plant (WNH).................... (b) Barium Lithol RT-365-D (ADR) ....... III- LIGHTPAST CHROME GREENS (a) Chr. Greens of Improved Lightfastness - Lab. (b) Lt.Past Greens - Kilori Type. CS-7764 (ADR) Meadows Type, CS-7694 IV - CHROME YELLOWS (a) Prep, of Primrose & Lemon Yellows of Improved Lightfastness (SCH, HCM) .................... (b) Primrose Yellow - Semi- Works Study (PLP) . (c) Study of Lithographic Breakdown & Lightfast ness of Y-359-D (Laboratory)(SCH) (d) C.P. Medium Yellow Y-359-3 (PLP).................... V - JACKSON LABORATORY STUDIES (a) Special Organic Pigments (AS)........................ .... (b) Permanent Red 2B (A3) ................................................. VI - EMULSION TREATMENT OP PIGMENTS Pigments in Oil (GWJ).......................................................... VII- RUBBER COLORS (AJS) ............................................................... VIII- PIGMENT GREEN B (a) Pigment Green B (AAB)................................................. (b) Pigment Green B. GT-68-P Semi-Works (WNH) IX - PHOSPHOTUNGSTIC ACID PIGMENTS PTA Yield Studies (EJH)..................................................... X - DISPERSION & TREATING AGENTS Treatment of para Toners with Buponol (EJH) . . XI - MISC. ORGANIC PIGMENTS (a) Toluidines (APCP)................................................ (b) Azo-Sulphite Derivatives (AAB & SWR) . . . c) Duol Red RT-283-D (ADR)............................................ (d) NBS Maroons Improved Maroon Toner of the RT-297-D Type Maroon Toner RT-399-D - Semi-Works (WNH) (e) Rubber Colors - Red for Lake C (AAB) . . . (f) Misc. Toners Pigment Rubine Toner RT-359-D (ADR) . . Maroon Toner - RT-354-D (ADR) ..... (g) Misc. Lakes Peacock Blue BL-151-D (EJH) '......................... Violet Lake BP-69-D (EJH)............................. Zinc Silicate (EJH) . . . .......................... .... 1-2 3 4 5-7 8-11 12-16 17 18-20 21-22 23-25 26 27-31 32-35 36-38 39-40 41-42 43 44 45-47 48 49 50 51-52 53-54 55 56-58 59 60 DUP050315433 2 XI - HISC. ORGANIC PIGMSNTS (Cont.) (h) COLORS POR TAT3R DISPERSION G3-363-D & G3-364-D (3JH).................................. Green Lake G3-388-D CS-7683 {ADR) .... Red Lake for TTater Dispersion - RE381D Type Page 61-62 63 64-65 XII- 1113G. INORGANIC PIGJ.3NTS Chrome Greens - Strong Type C5-7192 (ADR) ... 66 XIII- RA7/ MATERIAL TESTING (APCP) ............................................ 67 XIY - 3SI.H-7/0RK3 PRODUCTION (HA)............................. .... 68-73 DUP050315434 SUBMITTED BY: APPROVED BY: PIGMENT COLOR RESEARCH REPORT YIELD STUDY - IRON BLUES f il e * monaestDATE: JANUARY - 3.935 INTRODUCTION: Yield studies or iron blues were continued with a series on each of two Milori Blues, 3-66-D, and 8-57-D, following the work done on Chinese Blue, B-63-D, reported last month. SUMMARY AND CONCLUSIONS: Three batches each of B-66-D and B-57-D were made in the semi-works on standard formula, careful attention being given to operating conditions* Mechanical losses were avoided by all known means; filtrate at the beginning of the pressing operation was collected and returned to the press vat. The usual amount of washing (to ws sulphates) was carried on. The press cake was dried in plant dryers at 150- 155 F, for 30 - 40 hours. Results obtained to date are tabulated below, on a one mol of Y.P.S. basis (0.4 mol batches were made). These are lump yields. Code Yield Obtained Anhydrous Ayr. Moisture Content B-63-D OK lacquer B-63-D NG lacquer B-66-D B-57-D 310 1 ' 310 2 314 3 293 307 299 305 2# 0.99$ 3.65$ 2.69$ 2.78$ The "anhydrous" figures obtained in the laboratory were 320 IbB. for B-63-D and 306 lb3. for B-66-D (see December - 1934 report). Tinctorial testa and ink properties on the Mileri Blues, B-66-D and B-57-D were reasonably close to standards. One of the three B-63-D batches made was O.K. in lacquer and close to standard in rubout, with a moisture ef 0.99$. The others with higher moistures were deep and brown in lacquer, probably because of insufficient drying. Since the moisture contents of the batches made were not abnormal (except in two batches of B-63-D), the actual yield obtained may be used as an in dication of possible large scale goal yields, without any radical change in equip ment or operation. The indicated yield increases are:- for B-63-D, 33*1/3$ in one case; 4*1/2$ for B-66-D; none for B-57-D Results for B-63-D were not satiefactory because the anhydrous yields did not check well. m DUP050315435 j-7* - 2- l'*:' '..':1-'Jv>"Vii^ BXPBR3MITAL DETAILS; Notebook 428, page 54-63 Type Pigment SW-No. B-66-D 6661 (CS-6705) 6662 26684 Drying Temp. Time -- 150F 29 h. 150 F 41 h. Yield {2 hr.at 110F) unc orr % HaO lump wt< 3.28 128 2.16 2.64 125 125 Yield recal. to avg. -water content. 127.2 125.6 125 feicmlatedf tovSSr ;.r ;. 317 m312 310 B-57-D 6697 (CS-6933) 6710 6716 155 41 H. 155 43 h. 155 40 h. 2.09 2.56 2.91 118 118.4 294 119 119 297 116 115.4 -.269 2The very slightly colored filtrate at the start of pressing and washing mas collected and filtered in the laboratory; it amounted to 130 grams Of drycolor; this loss iaabout 0.25% and can be considered negligible!. Varnieh Rubouts 1x2 Transparent Varnish Vs. B-66-D \ Vs. B-57-D SW-No. 6661 6662 6684 6697 6710 6716 Masstone Undertone dark, black va str. brt. tt s str & grn. tt vs green dark s dark dark e str. s str. str. Strength equal vs str. vs str. str* str. str. vs green vs green vs green vs green : TSSgreen vs green S-. The low yield of B-57-D is probably due to decomposition of Y.P.S. as the strike is carried out at a temperature of 205 F over a period of 45 minutes* %n- DUP050315436 PISMBNT COLOR RESEARCH REPORT LITHOL RED RT-379-3 PLANT SUBMITTED BTi oO v\ \Aju-&9j u l APPROVED BY: -s '/-j -- .+3-2- f/ PILE: 3ATEs JANBARY-19S5 INTRODUCTION "" I Because of the plant need of OK depth, -weak blue material for shading, the Semi-Works were requested to supervise the production of this material. SUMMARY & CONCLUSION Three hatches were made in the plant under the supervision of the Semi-Works. The first hatch was a cheek run to previous dark, strong material (Lot 40659) and was a satisfactory check. In order to decrease this depth and retain the hlueness a redaction in TOB-W and an addition of Mono Acid F was tried, the first batch was not made according to plan and dark, strong material was obtained. The third batch, made as just described gave material s.light and flat, s.blue, a.strong, and si. blue and vs dirty. Further work was dis continued at the plant's request. EXPERIMENTAL PBTAIIS Notebook 433, pp. 49 -51 i Lot Formula Size VS . RT-379-B . Mass. Und. Str. Tint 41501 Check 40659 9-15 dk vs brn vs bl OK vs bl 41524 Check 41501 except decrease " TOB-W and add Mono Acid F (Not carried out as planned) dk vs y. s.str vs cl 41546 Check 41501 except decrease 0.5 sl.li s.bl TOB-W and add Mono Acid &flat s.str s.bl vs dty. DUP050315437 PMMBSr COLOR RESEARCH REPORT SS^3 BARIUM LITHOL RT565D SUBMITTED BY* CULSj^Jcj^ Ql APPROVED BY: 6 PILE* U :DATSi JANUARY-1935 INTRODUC TI ON Three featch.es of RT-365-D were made in the Semi Works to consume some special TOBR left over from previous experimental work. This type contains 10f^ Naphthionic acid. Two hatches were made on the standard alkaline coupling and one on the old acid coupling procedure* SUMMARY & CONCLUSIONS The material on the standard formula, was slightly darker and yellower than standard hut can probably fee consumed in blend* The acid coupling gave a muddy weak product, difficult to shade* t" .EXPERIMENTAL DETAILS F.B. #394. p. 16 0.3 mol charges were made. Gradings are vs* RT-365-D #12417 SW-6651 - SX SW-5810 Grading - Dark s.fert; s.yel; s.str; s.yel. SW-6654 - Cheek 6651 Grading - Dark s.fert; s.yel; s.str; s.yel. . SW-6658 - Acid coupling as in SW-5671 Used 3-6,3# special TOBR and 19.45# ordinary TOER Grading - muddy; yel & wk; weak; dirty v,.; * DUP050315438  PIGMENT COLOR RESEARCH HEPORT CHROME GREEKS OF IMPROVED LIGHTFASTNESS s u b mit t e d b y APPROVED BYs LABORATORY J% c /L^ , ^ f il e : mmem-mmgs DATE: JAFCJARY-1935 HfTRODPCTIOK ' The wrk on chrome greens during the past month has been of a miscellaneous nature. Some attention has been given to the problem of preparing an improved green for use in lacquer. TJie investigation of the effect of the blue on the lightfastness of the green has been continued. A study is being made of numerous reducing agents to deter mine their possible value as restraining agents. STTMMARY & CONCLUSION Chrome greens, of the improved, more lightfast type, when ground in lacquer are c onsiderably worse in lightfastness than the same greens rubbed out in oil or ground in oil in the paint laboratory. From previous work it appeared that the poor lightfastness was not due to any of the ingredients used. During the past month it was found that if a chrome green pigment was rubbed out in the lacquer mill base on a glass slab, instead of ball mill grinding in thd mill base, apd then finished in the usual manner, a considerable improve ment in lightfastness over the ball mill ground product was obtained. It appears that ball mill grinding reduces the lightfastness of the t pigment. A study is being made of the restraining action of various re ducing agent's* The agents studied included stannous chloride, stan;pour sulphate, stannous chloride plus sodium acetate, stannous chlor ide followed by tannic acid, tannic acid, ferrous sulphate, titanous chloride, vanadium pentoxide reduced with zinc and hydrochloric acid, sodium sulphide, sodium selenide. ammonium polysulphide, formalde hyde, sodium thiosulphate, sodium sulphite, sodium hydrosulphite, sodium arsehite. sodium hypophosphite. hydroquinone, pyrogallic acid, and Captas. Because of the acidity of the titanous chloride and re duced vanadium solution?- soda ash was added to a pH of about 6 after the addition of these agents, Captax. sodium hypophosphite, sodium sulphite, sodium hydrosulphite, formaldehyde, and sodium selenide have a negligible restraining action in the process used. The other reagents had a sufficient effect to be classed as restraining agents. From the standpoint of lightfastness tin salts, sodium sulphide, and ammonium pfclysulphide are superior to tannic acid. The other agents from the standpoint of lightfastness seem either inferior or not ap preciably superior to tannic acid. A further study of the effect of the blue on the lightfastnes's of a green indicates that B-103-L and B-10S-D give slightly better lightfas fness than B-66-D. ''EXPRRTiffEKTAL DETAILS Notebook 439 '>: -v:,-:;TM" Restraining Agent Study. 439-63, Study the effect of various reducing agents used &3 restraining agents. - . ``r1' 1 -`' a--' DUP050315439 In this experiment both stannous chloride and sodium sulphide had: a strong restraining effect. The stannous chloride gave a product much superior to tannic acid products in lightfastness. 439-64. Study the effect of using Titanous chloride, ferrous sulphate, sodium sulphite and sodium thiosulphate as restraining agents. In this experiment it was observed that ferrous sulphate can be used as a restraining agent, but g&vt a product poor in lightfastness. Sodium sulphite resulted in a flopped pigment, while Sodium thiosulphate was on the borderline of flopping. It appears that Ti tanous chloride was too acid, thereby causing the yellow to flop. 439-65. Study the effect of Ammonia pblysulphide and sodium arsenite as restraining agents; also study what results will be ob tained when no reducing agent is used. Both Ammonia polysulphide and sodium arsenite had sufficient effect to be called restraining agents, but sodium arsenite gave a product with very poor lightfastness. Omitting the use of a restraining agent resulted in a flopped color. 439-66. Study the effect of neutralizing the Titanous chloride with soda ash; also study quinhydrone and stannous chloride plus sodium acetate*: neutralizing titanous chloride gives the titanous chloride a stronger restraining effect. The addition of stannous chloride plus sodium acetate had a restraining effect but produced poor lightfast ness. Quinhydrone had a strong restraining effect, but gave a produot poor in lightfastness. 439-6"?. Study the restraining effect of v&nadous chloride, for maldehyde,' pyrogallel, and also adjusting with soda ash to a pH of 6 after adding titanous chloride. Titanous chloride gave its best restraining effect when the 'strike was adjusted with Soda ash to a pH of 6. Yanadous chloride, when followed with soda ash to obtain a pH of 6 had a strong restraining effect, but like titanous chloride gave a product poqr in lightfastness. , Byrogallel had a strong restraining effect, but produced a dirty pigment with poor light stability. formaldehyde had a negative restraining effect, giving an olive and very changeable product. 439-68. Study effect of using Stannous chloride and sodium ace tate together as a restraining agent; also try sodium hydrosulphite, sodium hypophosph-ite and Captax. In this experiment sodium hydrosulphite, sodium hypophosphite and Captax had a negative effect as a restraining agent. It was in teresting to observe that Captax gave a product of which the inks did not' dry after several days. ' Stannous chloride used with sodium acetate had a strong restrain ing effect, but produced inferior light stability. 439-69. Study the effect of sodium selenide and stannous sul phate, "as a restraining agents. Stannous sulphate had a strong restraining effect, but did not improve the lightfastness as well as stannous chloride. DUP050315440  iy:..... :v. vl ' v 1. ' ' fc*-. ^- 7 5 Sodium selenide did not reveal any restraining power when used under the conditions of this experiment. _ 439-70. Study the effects of Hydrazine sulphate, Hydroxylamine Hydrochloride, phenylhydrazine hydrochloride and accelerator #552 as restraining agents. Phenylhydrazine hydrochloride had a strong restraining effect. Hydrazine sulphate had a fair restraining effect. Hydroxylamine hydrochloride had a slight restraining effect, and accelerator 352 had a very very slight restraining effect. Hone gave products equal to 63C. using stannous chloride, in lightfastness. Miscellaneous 439-6133. Dry mixes were made of the following blues, using the^ yellow"of 16E (yellow from plant hatch 40706): B-3-D- B-30-D, B-60-D. B-83-D. B-95-B. B-103-D. B-109-D, B-147-D and B-148-3K After being exposed for 168 hours B-109-3) gave the best lightfastness of the group. 439-60. Study the effect of salt (sodium chloride) on the Milori green of improved lightfastness. . It appears that salt tends to give a brighter .product, but does not seem to have any appreciable effect on the lightfastness. 439-62. Try checking 32C and 47C, the strong Meadows greens of* improved light stability. Hot'^ery good checks were obtained on the above-mentioned pro cedures. ' - DUP050315441 PIGMENT COLOR RESEARCH REPORT SUBMITTED BY: APPROVED BY: LIGHT FAST GREENS MILORX TYPE. CS-7764 : MEADOWS TYPE -- - ' ^rr T CS-7694 &- i PTLE: GgRaifZ; G3SSKS DATE: JANUARY - 1935 INTRODUCTION: : 'ST An intensive study of the SsLlori type of Light Fast Green was carried on in the semi-works. Further work was done on the modification of CS-7728 tried last month and a-new formula, CS-7664 was investigated# BsSR gte;1. ' pne plant batch of the latter type was also made. Three batches of CS-7694, Meadows Type, were made in the plant on a process study.of the recently standardized formula. - SUMMARY AND CONCLUSIONS: The modification of CS-7728 (SW-6646 made la3t month) has been dropped for the time being in favor of the cheaper and perhaps more stable formula used in SVJ.-6652, .Laboratory 439-56A. The former appeared to be a little duller in masstone and unless tin crystals Were added both after strike and to the washed yellow there was a tenden cy toward oliyehess which was objectionable on a largerbatch. Omitting sodium sulphate and finishing the yellow with a lead excess gave unstable results, one batch being olive on control and the other becoming so in proces sing* Addition of all the nitric acid before the bichromate instead of splitting it, resulted in an olive changeable green. The formula which appears most promising (i.e. the SW6652 type) has all the nitric acid before the strike but U3es a lower total amount due to omission of the caustic soda. Both formulas gave bluer undertones and tints than desired in a Milori Green and improvement in this respect together with increase in stability on large batches were the objects of the study. Omitting the sodium sulphate from the 6652 type increased oliveness but ,li V had no effect on light stability. &< figr Reduction of strike volume to 50% resulted in poorer light fastness altho it had little effect bn shade. A 75% reduction caused instability in the green. A change in acidity of the formula was detrimental, a 10/i reduction caus ing dullness and a 10/ increase causing oliveness and weakness and both resulting in poorer light stability* Addition of alum and soda ash and of cupric hydroxide as in the Meadows ' type of light fast green appeared to have no advantage. Light stability was slightly . inferior. .... Replacing the bichromate with an equivalent amount of chromate liquor re' ,eultgd in an olive changeable green due to the fact that no adjustment was made for the difJOrence in acidity until after the strike. The above variations were made on 0.1 mol charges. DUP050315442 T" - 2An increase in batch size to 0.5 mol gave a slightly more olive green still brighter, however, than G-317-D with light stability equal to the smaller charge. Doubling the amount of NasS on a large batch, altho causing some dirtiness of masstone and tint, added slightly to light stability. Use of more tin crystals, i.e. added after strike as well as to the washed yellow, gave inferior light stability. & check on this variation is probably needed before positive conclusions can be drawn. Other variables which also should be checked are addition of the bichromate thru a Bprinkler and Reduction in amount of bichromate. Beth changes would appear to be desireaole from the joint of stability but on each run light fastness was poorer. A plant trial of this formula was slightly olive and dirty compared to U-317-U standard but in relation f masstone and undertone was closer to standard than the semi-Works runs, light stability was not as good as obtained in the semi works out was better than G-317-B standard. Work on this type will be continued; Production of the Meadows type, CS-7694, was resumed in the plant to obtain further information about the process. An attempt was made to eliminate the use of cupric hydroxide in order to shorten the process. One batch was made which was slightly oixve bat it may still be possible to make this change. A second batch on standard formula was quite olive due partly to the slight redness of the yellow but chiefly to redness in the blue. use of the sprinkler for adding the bichromate as previously tried helped sombwhat but the finished product was still slightly olive. , Further work will be necessary to obtain better control of this green, a fC' ' semi-works study is being made for this purpose but no results are available yet. DUP050315443 Notebook JF436 p. 100- a p rrrtt 3^ u p p A) t P P .Q a pH >9 43 P fa H 0 .sS -P fa ex P a t, X. sm iH fa in iH oa p fa > P *p fa fa P p P H pH p 43 rl rH O oP p fa 43 > 44 H fa <ri rH 0 S > O xs frH CO I C3 - O P u 6= po CO 8 <D >i * > <H -P S O>$- O a Jf3t h ID 0 r0l f3fl X0 C rH HP >* S3 *3 rl (If PUD # H O r-* a .g m on +> * is -a |o"a -h P to *rt *0 P 4J to *0 43 tO ai* P H* p 1 O b to rto ^ to to CO to 44 to 3p & <o O 0 Al P 44 rt OH fa o xt ^ t-H AS P 43 Ss O O >* X Pp fa fa H H rH pH O 42 k > W> 44 rt g fa rH o c *o fa o H 43 o 0 o rt P H P 0 *0 0 P P 43 Oo to to to to to to 4J 4d o -frat P pto5 ^ 44 X O in fa u 4* fa pH PP P p p P PS 0 3s O* S 43 43 43 f3 W > u 4 Ps xa s . .. a * e * xa `S& * v^SS .. rsS c <d a 3 P P P P p rH rH fH pH pH rH P rH 43 43 . , 43 43 pH 43 43 fa fa fa fa fa fa fa fa P P P P P pP P X. X. X X XX X m in in in fr. 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'3 0 03 45 faP rrt o ft *o0 O 0 ^ C3 fa s H 0 0 *M 0 fa o ej 60 O ,,a t* P t P P g P &0 rl <Ht! 42 P 4> 43 43 g.*.43 43 43 43 H p ao CM CM o CM a& rl CM in in CO in CO C\2 a 03 <D CS) CM in in S in >*m c in fa tn tO s to to iSIJiBK P to to to to to to to p to to to & to to rt to 1 w AS3 P 41 44 44 Ai=fcA4 CO A! H *&4 rt 44 b o &SH O O O a if) u o rrt rH 44 5.J5 o 0 to -* Ja , rH 3 43 43 43 JS CM X -p 43 AJ 43 p X <d < OO O e> o oO o fa IS e pP rH H 4> 42 * ffl + !> A! rH rt fa rH 0 o *0 44 O 44 Jpa c ^3 < X oo 1 . v.._ ' .... .'M' :y J? ; ''Sv- -fr* t o tn o9 rH fr- CM a% 0* Ci rH in CM m CO CO CO 3 oto to t> fr- to tn to CH CO fr- Ok CO Cft rH CM fr- fr- CD to to to to to to to to to fr- to tO to to fr- fr- to to to 39 to to to to to to to tO to to to to to to to to to to to jSXhiiih i MENTAL DETAILS DUP050315444 & S 3 o* > 3P 3 JrH3 `HP H3 p X> 3 ,0 3 J-. Cfi H *rt > =$ 0) X) 3 u UU hi t 3 P P u VL Vi. VL in CO CO rl pH rl P TO in rH 3 s o 8 p b& <D hO u 33 3C rH O rH r-l O 3 & t, ^0^3 J3 P +5 rH > a ra fi Cff u P d &P- 4> > 3 bO 3 O u p a oS3 bO 3 a 3U rH P X* ^ 3 P >> p U oy <=$} rH rO H fH P > c 3 OPM > P fH U ffj J> Sm S .rt > Ad rH J} nd *rl rH rH Us > O Q g s t 3 t. H CO B <s P VO P S H *o rl o *3 45 P H p d xx S iJp O -p m > Prt p o rH P 3 o 3< 3 -p *ri P pH H P 4H2 3 3- Hs 3 as SJ * o S* *rl *4 3 O P -p 3 o <0 H * - P 3 d rH ^ t* rt O 3 -P >> P -P r* P 3 3 *3 3 3 3 J2B * 3 rQ <C 42 3 CO O P CO C- p CO W5jk fc-*SfeO n O ho <o H VO 3 VO H VO VO P rl CO O o o ox - * U jrf VO Ad P o *4 p 3 ,3 P 43 iH :> o o O o CO CO 02 CO o 04 VO VO fr- fcCO VO VO vO VO rl o3 1 4d p P P > &h 42 Ih u rH rl d H 3 3 H O > Q t fcrH *? O fcCO M Q O 8 P O CO 55 fc- VD VO J 3 rl bO P d XX o o S VO b* to o & cP CO O rH 4 o" rl U Pi 3 c P *rt E o t 43 03 CO in o Kj H *4 <"N o in m t- 3 H v4* X O 4vo t* I CO 3 s o u H 3 d Un o 3 rl O X P d3 *3 d Pi rH 3P CO 3 c 3 -rl O CO o p ea 5^= O 04 O g-1* o XX 04 o g 44 3 *r| 5Pi 3 A P P ci a o ^3 rH n 3 3 d P 3 XJ t> <3> rH 4d 43 O b- b* VO CO Q> rl CO ca VO * $ - *&. *! . - ';2t; w - r$S DUP050315445  PIGMENT COLOR RESEARCH REPORT PREPARATION OF PRIMROSE AM? ISMON YELLOV/S OS' IMPROVED LIGHT?ASTNBSS SUBMITTED BT: X C. APPROVED BY* c- INTRODUCTION PILE: piS0MEL-SEI*0 f 35ATE: JANUARY-1935 The problem of preparing an improved primrose yellow was con tinued from the past month. A number of large size hatches of the improved product reported last month, have been made in the labora tory and semi-works, but the reason for observed variation between the laboratory and semi-works has not been determined. A start has been made on the problem of preparing a product with the "ink properties of Y-202-D but of superior lightfastness. This problem is being continued. SUMMARY & CONCLUSION A number of strikes have been made in the laboratory to obtain a more stable process for the improved primrose yellow mentioned in last month's report. In the laboratory the batch size, l/2, 1, 2, or 4 moles does not seem important, although the largest batch made success fully using lead nitrate liquor rather than crystals was one mole. The laboratory products check very closely tinctorially although the lightfastness varies somewhat. The use of a large quantity of bicarbonate after washing or a pH of 6.5 - 7.0 at this point results in poor light fastness. A pH control may be necessary at this point. Allowing the pigment slurry to stand overnight had no effect but allowing it to stand over three days resulted in a redder pigment. Drying in the steam .Oven and the electric oven gives equal products. The work on this pro blem is being continued. ,v ' ; A study is being made of products which may be equal to Y-202-D : as, priiiting ink colors but which are superior in lightfastness. Three processes are being studied. In one process a mixture of bichromate and sulphate is added to a soda ash lead nitrate mixture. The product is about equal in strength- slightly light and clean in masstone. and slightly red in tint. It is low in finish and better in lightfastness than Y-202-D, A sample has been prepared for testing in the service laboratory. In- the second process a mixture of sodium chromate and sodium sulphate is added to lead nitrate. The fresh mounts of the best products are equal in masstone and finish but slightly red and dirty in undertone and tint versus Y-202-d . They dry to a green d irty masstone and while better than Y-202-D in ligntfastness are poor versus our prim rose yellows in this respect. In addition the process is unstable. Since this product is approximately equal to Y-202-D in transparency a sample will be prepared for testing in the service laboratory^ In the third process bichromate and sodium sulphate is added to lead liouor plus nitric acid. The product is clean and light in masstone versus Yw 2G2-D but somewhat red and dirty in undertone. The process is unstable and further work is necessary. In all the above processes it was found that as the strength and transparency increased the lightfastness became wp?se and generally the masstone became somewhat dirty. Pox example, # product equal to Y-31B-D tinctorially and containing no phosphate was found to be no better in lightfastness. In addition as the products come closer to Y-202-D tinctorially the process used appears to become H#? stable,;.'.. ./W/:--*. v-`'v'^.V>'"'^vsv ' ' , v;.r'7?r DUP050315446 EXPERIMENTAL DETAILS Notebooks 415 and 453 Primrose Y-315-D shade 453-1. Study method of drying- using material taken from a four mol batch~struck in a barrel. Regardless of the method used for drying and time of washing, very close checks were obtained. The series practically checked 415-50A tinctorially, but was vvs worse in lightfastness. 455-2. Check 453-1 study. Like 453-1 all members of the series were very close checks to each other, but the entire series was a trace dirty versus 415-50A, and also worse in lightfastness. 453-6. Check 453-1 procedure, but split after the second water, allowing one part to stand overnight. In this experiment, the part (A) filtered the same day it was struck was -slightly red versus 415-51A (a check to 50A); the part (b ) which stood overnight grew redder than A, and was worse in lightfastness. 453-8. Check 453-1 procedure but split after the three waters, A filter as in regular procedure; B treat with sodium bicarbonate to ob tain a pH of 6.9; G flood and let stand overnight. In this experiment C, the part which stood overnight, was cleaner and better in .lightfastness than A and B (which were filtered the day of striking). B was a trace worse in lightfastness than A. 453--14. A was a four litre sample of SW-6722, taken from the first water and. finished in the laboratory. B. Sample.of SW-6722 taken after third water, and finished in the laboratory. B & A were very close tinctorialTy; B being better than A in lightfastne^s. Both B & A were a trace dirty and a trace green versus 415-50A, 453-15. Continue the development study of 415-50A; split before treatment and vary the amount of bicarbonate; study use of sulphate in this treatment* It appears that a 20:7 ratio of alum to bicarbonate gives better lightfastness than the 20:5 and 20:10 ratio. No marked effect was ob served when sodium sulphate was used in the afterwashing treatment. Y-305-D and Y-318-D 415-56-57 Study effect of using sodium fluoride for sodium chlor ide; increase the bichromate in the strike. Sodium fluoride tends to improve the lightfastness a very slight amount, but gives a very red yellow. Increasing the bichromate result ed in a redder pigment than Y-305-D. but very slightly green versus Y-318-B. 415-58. Study further increase in bichromate; also use stannous chloride in the 415-573 procedure. Increase in bichromate from 112 parts per mol to 120 parts result ed in a slightly redder and very slightly stronger pigment. The use of 'stannous chloride gave a marked improvement in lightfastness, but gave a dirty pigment. DUP050315447 15-59. Study the Y-305-D procedure using quantities of the 50A type, ant adjusting acidity when necessary. *B,* striking the Y-305-D procedure at 110using salt, result ed in a product somewhat redder than A. (laboratory Y-305-B). C made with sodium sulphate in the strike was a trace worse in lightfastness. D, using sodium sulphate for alum^ otherwise like C seemed to have a trace better lightfastness. 415-64. Study low temperature, low volume and adding all of the soda ash to the lead nitrate on the 415-59C procedure. It appears in this experiment that adding all of the soda ash to the lead nitrate has no appreciable effect on the lightfastness. Striking at 70^ instead of at 110CF resulted in worse lightfast ness. The change in volume did not seem to have any marked effect on the pigment and -light stability. 415-73 Study the use of tartaric acid and citric acid after the three waters as a stabilizing agent. It appears from this experiment that tartaric acid is far super ior to citric acid as a holding agent - for those made using citric acid flopped in the oven. 415-77. Study the effect of omitting the salt on the 64B, and further study of 50A and 59A. When Salt is omitted iri the 64B type the mounts tend to darken upon drying. "When the soda ash - alum treatment is omitted in the 50A type the prints also darken upon drying. Striking 59A at 110 T\ and using sulphate in the afterwashing gave a very red product. 415-80. 'Study 50A using both the semi-works, raw materials, and the crystals in the laboratory. It appears that the lead nitrate liquor and sodium bichromate from the semi-works when iised in the laboratory gave products equal to lead nitrate Crystals. 415-85. Study effect of making larger size strikes cf the 415-50A type in the laboratory; also omit salt in the 415-50A type. The one mol batch was a trace red versus 50A (made on a 0.5mol basis). It appears that salt is very necessary in the 50A type in order to preserve the improved lightfastness. Weutral lead nitrate - light yellow procedure. 415-60. Study effect of Turkey Red oil. Turkey red oil has a tendency to give a green and very dirty product. 415-65. Check 415-601), using salt in the strike, also with Tur key Red oil after the strike to produce a cleaner color. Turkey Red oil when used ithout salt in the strike gives a dirty pigment poor in lightfastness. Salt-has a tendency to lighten and clean the masstone, and slightly improve the lightfastness. 415-67. Check 415-63D. using a slightly higher precipitant bal ance by increasing the sulphates from 4 parts to 10 parts; ako study use of malic acid after washing. These variations had practically no marked effect. ,;y r DUP050315448 4 415-71, Check 415-67A; study use of less salt and of tartaric acid. The use of tartaric acid and decreasing the salt when Turkey Red oil is used had little or no effect on the products obtained. 415-74. Check 415-71 without Turkey Red Oil: also use tartaric acid for malic, acid? study use of Turkey Red oil after the strike. In this experiment it appears that neither malic acid nor tar taric acid enter in.as important factors affecting light stability. Turkey Red Oil used after the strike did not show any marked improve ment, 415-81-85. Check 415-74A. studying the use of diglycol stearate and potassium furacylate. Both diglycol stearate, potassium furacylate and tartaric acid appeared to have no effect on the pigments, 415-90. Try to obtain a cleaner masstone by lowering the amount of chromatei also by lowering the temperature Cf strike. Decreasing the amount of chromate, increasing the soda ash after the strike, and lowering the temperature of the strike had no apprecia ble effect on the products obtained? all were dirty and poor in lightfastness. 415-93. Study on the 85M procedurejfche effect of omitting the sodium sulphate in the afterwushing treatment, and the use of a more acid hydrate. . Omitting the salt in D seemed to produce a redder product. Using a more acid hydrate appears to give a dirtier productthis will be checked. No marked effect was observed when the sodium sulphate was omit ted in the afterwashing treatment. 455-5. Study the use of salt in the 415-92B procedure 1 It appears that salt is necessary in order to retain the im provement in lightfastness. 455-9, Continue the y-202-D study based on experiment 453-3B. In this experiment the more acid hydrate resulted in the cleaner product. Pulped Kadox used in the afterwashing treatment gave a slightly dirty product somewhat worse in lightfastness than the control. tbr'455-10. Gheck 453 3-2, using varied amounts of bicarbonate in afterwashing treatment. The results of the increase in alkalinity in the afterwashing treatment were not in a perfect trend. It appears that the higher the alkalinity before filtering, the worse the light stability of the finished product. Acid lead nitrate light yellow procedure, 453^5. Check 415-87C. study use of tartaric acid and omit the sul phate in the afterwashing treatment. It appears that C made without sodium sulphate in the afterwashing treatment, also using tartaric acid gives a product very close to Y-202-D in tinctorial properties superior in lightfastness. 453-12. Study pH on 453-5C (ending with a pH of 5.6 and 6.6 re- DUP050315449 5 C (pH of 5.6) was a very good check on 5C and has been reserved for ink-mill test3. B (pH of 6.6) was dirty in masstone. and trace worse in light fastness. " ,, Alkaline - lead liquor light yellow procedure. 415-70. Study the Hilori greening yellow as a light yellow of Y-302-D shade. C made with a strong lead excess, and struck with Turkey Red oil in the bichromate appears to he a promising lead. 415-82-86. Study use of salt, sodium chromate, high and low bi chromate in strike. Hone of these variations gave any marked improvement, 415-91. Chedk 82B with less bicarbonate in the hydrate. Study the effect of decreasing the lead excess. This series as a whole was a flop. A1 and B). using tartaric acid gave products dirtier than Y-202-D. but much better in lightfastness. 455-3. Study slight decrease in bichromate and temperature on the 415-91A} procedure. Striking at 70CF instead of 80F using 116 parts of bichromate instead of 120 parts gave a very promising lead towards matching Y-202-D. 453-4. 7, and 9. Continuation of the study 453-3C, studying 60"F strikes, lower acidity- lower bichromate, use of tartaric acid and pulped Kadox, lower volumes, washing four waters, and using a more acid hydrate. , All three series resulted in pigments that flopped in the oven. 453-11. Study a decres.se in temperature, a cut in bicarbonate and volume, adjusting pH. Hone of th variations studied gave products equal to 415-74C-1, The products obtained were better than Y-202-D in masstone and lightfastness, but had red and dirty undertones. DUP050315450 PIGMENT COLOR RESEARCH REPORT 3S' 7 r SUBMITTED BY* %,k APPROVED BY* /. PRIMROSE YELLOW // < / PILE* .SSUMS YELEOWgr DATE* JANUARY - 1935 Semi-Works Study INTRODUCTIONS . A Primrose Yellow of superior shade, strength and light fastness has been obtained in the laboratory. Efforts were made .to duplicate this material in the Semi Works but the product made was red, strong and of inferior light fastness. The dif ficulty in matching the laboratory material is due mainly to its sensitiveness to dry ing conditions* SUMMARY AND CONCLUSIONS* Ten batches of Y-315-D were made in the semi-works based on the laboratory ^experiment 415-50A (a modified formula for Y-315-D). In order to obtain the desired properties, several variables were studied. Adding tin chloride to improve the light /fastness, use of lead nitrate crystals instead of liquor, faster agitation, increased precipitation time, reducing strike temperature, reducing size of batch were tried. .The addition of tin chloride resulted in a distinctly greener darker shade without improvement in light fastness. The batches made with lead nitrate crystals and high . speed agitation showed some improvement in shade and light fastness, but did not equal ...laboratory material. Striking at lower temperature (70 F instead of 110 F) resulted in.greener, dirtier material. No definite conclusions can be drawn, as all these batches were dried as thick press cakes. Differences were noticed on the same material /.dried as thin and thick press cakes. Thin press cakes resulted in light, greenish material .similar to the laboratory product, whereas thick press cake changed to a red, strong.color of worse light fastness. EXPERIMENTAL DETAILS* Notebook 448, page 30-43. Y-315-D - Semi-works batches (Readingsvs. 415-5GA) ' . SW-# Formula Uasstone Undertone Strength Tint Lt* Fast . 6645 6650 6663 ... 6675 6681 Trial of lab. exp. 415-50 red, dirty As 6645 but small amount of grn, dirty tin chloride As."6645 but pressed the day red,dirty of strike As 6645 but use of Lead Nitrate s red crys. & faster agitation. As 6675 but lead nitrate liq. red red, str. str, gr, dirty red, str. s str. red, str. str. str* str. str. str. " 6711 As 6681 but strike over 1 hr. red instead of 30. min. W . 6718 . As 6681 but strike at 70 F dirty,red \s6722 As 6675 but reduced to l/4 red // V. . Made #50 ga./bbl. high speed agitation / 6734 As check on. 6722 : .6738 As check bn 6732 red red ,/.' 8738A -Part of 6738 filtered as thin s green -press cake*, co-vt red,str. str. red,str.drty str. red str. red red vs green str. str. equal red worse gr. worse red worse s red s worse red worse red worse drtyred worse red worse red worse red worse s grn. equal '"V *' . </' '// .V */ / jV-; /.-/ DUP050315451 -sf^sv *Xis, ; S- t:>. afc r #' SB#v'">,*k * -fer? v ^M - > , .i "5>& 3sr;. SvW " . ?r:.v. PIGMENT COLOR KBSEARCH REPORT STUDY OP LITHOGRAPHIC BREAKUPS AND LIGKTPASTICSS OP Y-359-D (LAB.) SUBMITTED BY APPROVED BY : 3- t/. f PILE: GHRGlffi-3$iOTS DATS: JANUARY-1935 INTRODUCTION The work on Medium yellows during the past month has consisted mostly of miscellaneous strikes. A brief study has been made of the I.C.I. process, file Number H-897, and of the Harshaw British patent 416,744* A study- of process variables on the Y-359-D formula has been made. The effect of a number of agents on the lithographic breakdown of Y-359-D has been determined. SUMMARY & CONCLUSION N Several strikes were made using the H-897 process of I.C.I. The pigments obtained were slightly inferior to laboratory strikes of ^Y-359-D both in strength and lightfastness but possessed a better fin*'ish.* The process involves an acid strike and the use of Turkey Red Oil to prevent the formation of large crystals. Purther work on the process is apparently not justified. A brief study was made of the Harshaw British Patent 416,744. Several strikes were made in which litharge or white lead was treat ed with hydrofluoric acid followed by chromic acid. All the products obtained were dirty and no better than Y-359-d in lightfastness. Mod ifications involving the use of a lead versus a chrome excess and neutralizing at the end of the process gave no improvement. Replac ing sodium chloride in Y-359-D with sodium fluoride resulted in a clean weak product no better in lightfastness. Sodium fluoride was tried in several other processes without obtaining improved products. No further work is planned on this patent. A number of strikes of Y-359-d were made in l/2, 1, 2. and 4 mol batches. The size of the strike had a negligible influence on the result. Drying in a thick cake, thin cake, wet thin cake, or wet thick cake had little effect, the best results being obtained with a thick cake. Neither press washing nor amount cf washing had much ef fect ,k Allowing the color to stand overnight in slurry form resulted in a dirtier, s.red. product slightly worse in lightfastness. Pro ducts closer to laboratory material may possibly be obtained by speed ing up the present plant process, x The time of washing had a consid erable effect. A brief investigation of the effect of various agents on the lithographic breakdown of Y-359-D was made. Some high molecular weight organic acids or soaps appear effective in preventing the se paration of the pigment from the oil in the breakdoxm test. Sodium resinate and hydrogenated rosin appear the most effective, para soap and turkey red oil are somewhat less effective. Naphthenates, naphthionates. Neopen SS and numerous other substances were ineffective. Approximately 0.5# of treating agent is required, the effect of the agent decreasing with a decrease in the amount used. All the treat ing agents which were effective gave veryd irty products. 1 *:r.: DUP050315452 2. BXHBRIMBHrAL DETAILS Notebooks 389 and 415. 389-114. Check on laboratory experiment #279 library file #H-897 of Imperial Chemical Industries. The Turkey .Red Oil treatment of the Imperial Chemical Industries appears to give a slightly weaker product, slightly superior to Y-359-D in lightfastness , 389-115. Check on Harshaw Chemical Company. British patent 416,744 (using-litharge and with hydrofluoric and chromic acids). This treatment appears to give a product inferior to Y-359-D in all properties but strength. " i",. 389-116. Cheek on Y-359-D, substituting Sodium fluoride for sodium chloride, and study the use of TRO after the strike. The above treatment appears to give no particularly beneficial results-. Substitution of fluorides for chlorides seems to give a product with'low oil absorption. 389-117. Study variations in Harshaw Chemical Company patent 416,744, avoiding a chromic acid excess at all times, f?It appears that this procedure gives a very inferior product. 389-118. To study variations in 389-117 procedure, substituting white lead for the litharge. This procedure gives a product somewhat inferior to Y-359-D, but which appears to give better results than the 117 procedure. 389-119. To check 116A and study variations using alkaline strike~and after treatment of alum and bicarbonate. Fone of the products show an improvement over standard. 389-120. Preparation of a reverse strike in large batches. Check 38-116A in 0.5. 1, 2 and 4 mol batches. The size of the batch had little or no effect on the results, Brying in a thick or thin cake had practically no effect. The thick cake gave a pigment very slightly better in lightfastness. Allowing the pigment to stand overnight tended to give a dirty pro duct. slightly worse in lightfastness. Oil Retention Study on Y-359-D. 415-76 and 78. To study the effect of various agents on the oil retaining properties of the pigments. Sodium ricinoleates. sodium naphthenate, malic acid, and sali cylic acid seem to have very little effect. Sodium Resinate gives a marked improvement in conjunction with a dirty product. Para soap gives a reasonable improvement. 415-79. To study the effect of sodium resinate on the oil re taining properties of the pigments. With. increasing amounts of resinate the samples are progress ively dirtier. It appears that resinate is approximately the minimum a- mount for beneficial results. With increasing amounts of resinate the oil retention is pro gressively better up to Ifg. 'y ,, ... V- .1 < . .*. -* .* a.- " ...AAs' . sfea > ; ' V. DUP050315453 3% K . Continuation of 415-79. using liquid resin and distilled resin* hydrogenated rosins, sodium resinate, Reopen SS, and Burgundy pitch. * In this experiment it was observed that rosin increases resist ances to lithographic breakdown, but gives a dirty pigment. Oil Retention Study on y-180-D 415-84. To study the effect of various agents on the oil re taining properties of the pigment. Sodium resinate in quantities sufficient to prevent breakdown makes the product red and dirty. 4^5-88. Continuation of 415-84. The products aopeared to "be somewhat cleaner than in the previous studies. The treatment is not satisfactory as a sufficient improvement is not obtained. xm DUP050315454 SUBMITTED BY* APPROVED BYs 'A PIGMENT COLOR RESEARCH REPORT C.P. MEDIUM YELLOW. Y-359-D FILE! &// ( DATE: JANUARY - 1935 INTRODUCTION t Further work was carried on in the semi-works and plant to improve the quality of thisyellow over the present standard. Semi-works study of lead nitrate purification was completed. SUMMARY ft CONCLUSIONS! In the semi-works, standard Y-359-D formula gave a dark, green, strong product compared with standard. Washing the yellow by decantation, with wash water at the usual summer wash water teraperature, gave a lighter, redder product than con trol, with somewhat Letter light fastness. Press washing also gave a lighter, cleaner redder masstone. Neither of these changes improved the lithographic resistance. Addition of small amounts of either sodium hydroxide or nitric acid gave worse light stability, the former resulting in a dark, red, dirty masstone and increased strength, the latter in' a green, silky, weak yellow. . Increased time of strike gave amuch cleaner masstone, and a redder weaker tint; this variation also appeared to improve lithographic breakdown. This product was lighter and cleaner in masstone than stand ard with equal strength and better light fastness. Two semi-works batches finished with lead excesses; both have poor light fastness, and abnormal tinctorial properties. In the factory, material continued to average stronger than standard, probably because of the cold weather. Masstones tended to be green and dirty. The effect of the presence or absence of salt in the strike was not definite; one batch . made without salt had excellent lithographic resistance, but this result could not be checked. An increase in sodium chromate excess appeared to give a lighter, cleaner masstone, redder tint, and improved light fastness. This is being rechecked. Addition of caustic soda gave a stronger, greener, dirtier product. Hydrochloric acid gavea dark, dirty yellow. No definite improvements in litho breakdown were seen. EXPERIMENTAL DETAILS! See Notebook 448. Tabulations of semi-works and plant batches follow. DUP050315455 M *in ikmfat P rC m*at I 41 (# I*uto a tl i IfDa r e ! 01 & fa *to t--> -expressed &b le n g th o f time Inks stands up compared w ith standard DUP050315456 BXGMSHT COLOR RESEARCH REPORT SPECIAL ORGAKIg PIOMBBTS SUBMITTED BIT I APPROVED BY* FILE* mS&^RSBSSS DATE* JASUARY-1935 XHTROPtlOT IQR Investigations were continued in the laboratory this month on the preparation of pigment colors from the new dyes mentioned in the December report, with particular attention being given to the meet promising pigments, namely. Permanent Orange R, the bright red of the 4 ohloraniline 2 sulfonic acid 2 naphthol 3 carboxylic acid combination, and the scarlet red obtained from 2 ehlor aniline 4 amino toluene B Salt. Some worh was carried out on the bright reddish orange of Bed 23 Acid and R Salta and the isomerie amino phthalic acids - B Salt and 2 naphthol 3 carboxylic acid colors in order to obtain sufficient Information ooneerning the merits of these new dyes and pigments, and thus reaeh a point at which the investigation of these new pro* ducts could be discontinued In favor of other more important problems, SUMMARY & SOBOUJaiOB The preparation of a good quality of Permanent Orange R is greatly dependent upon the quality of the 3 ehlor aniline 6 sulfonic acid# The dye coupling proceeds easily and apparently is quite satisfactory, but the laking procedure tends to give inconsistent re sults tinetorially, altho even the poorest products are superior to Fermatone Orange YT-241-D, These inconsistencies have been overcome to & certain extent, but the small samples of laboratory intermediate available and the difference in quality of the various samples did danse considerable trouble. However, a large sample (CS-7808) of a good quality calcium pigment has been prepared and submitted to the Service laboratory, and a sample of the dye soda salt and calcium pigment to the Du Pont Technical Laboratory, for evaluation, Mo further laboratory investigation of this pigment is proposed for the present# Large samples of the strontium toner (CS-7779) of the dye 4 ehlor aniline 2 sulfonic acid BOH were prepared and submitted to the Service Laboratory and the Du Pont Technical Laboratory for eval uation# This pigment is an exceptionally bright red of yellow shade, excellent lightfastness and is non-bleeding in oil. It is much darker, but brighter, yellower and stronger than Toluidine Toner RT-158-B and equal, if not superior in lightfastnesa as fudged by fadeometer tests of dkindowns and extensions In zlno oxide. This pigment apparently possesses real merit and its manufacture presents no legal difficulties since it is covered in the old Lithol Rubine B patent - D,RP, 151,205 of 1903. The calcium toner of this dye resembles the toner of Lithol Rubine 3 tinctorially and bleeds badly la linseed Oil, and consequently possesses only little merit. In vestigation of this product has been suspended, pending the results of Its evaluation* DUP050315457 Considerable time was devoted to the barium toner of the 2 chlor 4 amino toluene R Salt product* with the object of elimin ating the oil bleed if possible. Preliminary orientation experiments Indicated that this pigment was oil insoluble. However, latter re sults have not confirmed this and investigations are being continued with the object f eliminating the oil bleed, The brightness and strength of this pigment have been improved appreciably The lead salt which is a deeper, brighter but yellower and weaker color than the barium, ale bleeds distinctly in linseed oil but slightly less than the barium salt* The substitution of 1 n^phthel 5 sulfonic acid for H salt resulted in products of no promise, owing to the water solubility of the allsaline earth natal salts. A large sample (CS-7807) of the barium toner of 2B Acid S Salt dye has been prepared and submitted to the Service Laboratory for evaluation and filing for future reference* This product is an exceptionally bright reddish orange of good lightfastness and sub stantially non-bleeding in linseed oil, but is appreciably different tinctorially from any of the organic orange pigments with which wo are familiar* The patentability of this new color is under consider ation. The lead salt of this pigment is much redder, brighter and yellow in shade and non-bleeding in oil compared with the bailurn. The calcium and strontium salts are very soluble In water* Ivaluation of the pigments from dyes prepared by coupling B Salt with the Isomeric amino phthalie acids is rather difficult owing to the extremely hard texture of the dry colors and the failure to duplicate results in some cases. However, as judged from the results of investigations carried out to date, it appears that the barium and strontium salts of the dyes from 3, 4 and mixed 3-4 amino phthalie acid possess greater promise tinctorially than the corresponding calcium salts* The. strontium lake of the 4 amino phthalie dye is superior to the corresponding barium and calcium lakes, and the barium lakes of the 3 amino and mixed 3-4 amino phthalie acids are superior to the corresponding strontium and calcium pigments. The strontium lake of the 4 amino phthalie acid dye appears to possess most promise with the barium lake of the 3 amino phthalid next in line. The alkaline earth metal pigments of dyes from Isomeric phthalie acids coupled with beta oxynaphthoic acid present difficulties similar to the above R Salt lakes. The barium lakes of the 3 amino and 4 amino phthalie acids are most promising in this case. The above dyes and lakes from amino phthalie acids possess dis tinct merit as scarlets, superior to Scarlet 2r lakes in lightfastaess and oil insolubility, but it is recognized that considerable work is involved in their perfection. The general characteristics of these new dyes and lakes resemble pigment Scarlet and Scarlet 2R and it re mains doubtful whether satisfactory full strength pigments (toners) can actually be prepared* Investigation of these new products has been deferred until further information has been assembled on the question of hard pigments in general, a patent search is in progress* and consideration will be given to legal protection of these products which are believed to be new. DUP050315458 v-.. f . 'f' ?- V'*f. a. ' *U.V ft S;. 3 Ik An orientation experiment was carried out on lakes of quinoline yellow P. This dye is the enlfonated condensation product of phthalic acid and quinoline, and is soluble in water. The barium salt is insoluble in water and the calcium substantially Insoluble. Toner pigments are extremely hard in texture and poor in tinctorial proper ties thus possessing little promise, whereas the corresponding hy drate lalces are brownish yellow in toptona, very clean and brilliant in shade and tint* and possess some merit. Latex dispersion of the barium salt of this dye is equal to Lithosol Past Yellow H in strength and brightness, and non-migrating in rubber in which property it excels Yellow H* purther Investigation of this product is proposed. Bsmncawa l d e t a il s Permanent Orange R B.B. 416, expts. 40, 44 and 45 pages 178. 192 and 194 respectively.. B.B. 450, expts. 4,5,8,9,11, and 14 pages 16,20,30,32,36, and 43 respectively* Study of effect of lower alkalinity of dye coupling* neutraliaation of dye, direct and reverse strike, variation in para sosp. omission of para soap, cold and boiling strike, quality of 3 chlor aniline 6 sulfonic acid, substitution of barium for calcium, variation in volume of strike, variation in rate of strike and variation in time of development at the boil. Strontium toner ef 4 chlor aniline 2 sulfonic acid--BOB BB* 416- expt." 42, pageH.B. 450 expt. 15, page 44. preparation of 03 sample - 03-7779 and calcium toner. Barium Toner 2B AcidR Salt BB*. 416, expt* 43, page i'55. B*B,,' 450, expts, 3.6,10,13 and 17, pages 12, 22, 34, 40 and 48 respectively* preparation of Ba, Ca, Sr and Pb toners and alumina hydrate lakes, and study of the effect of neutralization of dye, cold and boiling strike, direct and reverse strike, substitution of It 5 xy acid for R Balt, acidification of developed lake, variation in volume and formaldehyde treatment. Scarlet from Q-Cl-P-Toluidine R Salt - barium toner. 45'6, exptTs. 1, 7 and id, pages 4,""24 and 46 respectively. Study of the offset of lower alkalinity of coupling neutraliza tion of dye, heat digestion of dye prior to filtration, increased acidity of diaao and variation in diazotization operation, variation in time of development at the boil, reverse strike, omission of para soap# substitution of lead for barium and acidification of finished lake. - fradmailne Yellow P. Jf,B^ 400 expt. 12, page Orientation experiment on preparation of Ca and Ba toners, and corresponding alumina hydrate lakes. Amino phthalic acid R Salt pigments Il6. expts* 37 and 41, pages 166 and 180 respectively. Barium, strontium and calcium pigments of 3, 4 and mixed 3-4 amino phthalic acid. Study of direct and reverse strike. Evaluation of the various products, etc. tfc DUP050315459 vmwm COLOR HS8SABCH REPORT PERMAHEHT RHP 2S 3<T'I/ & * v-y' V 'v ^ ' s u b mit t e d BY* APPROVED BY* J... 0 immmm. PILE* MiaO-TOS5SRS" DAEEl JAHUABY-1935 `t lakes of Rod 2B were prepared for evaluation as printing ink and rubber colors, and the pulp of toner GS-7745 was tested in latex for use la rubber. SUMMARY & COKCLUSIOES CS-7745 'dry pigment in rubber is weaker than the corresponding pulp dispersed in latex, all other properties remining unaltered. The alumina and alumina blane fixe dry lakes give slightly better strength in rubber than the corresponding dry toner, but are still slightly weaker than the latex dispersed material* The Alumina Epdrate and alumina hydrate blane fixe lakes of Red 2B, on an equivalent aniline content basis, axe much brighter in mas stone and much yellower and more brilliant in shade and tint than standard Lithol Rublne lake HP-S57-D. K.B. 438, expt* 12, page 48, & DUP050315460 PIGMENT COLOR RESEARCH REPORT PIGMENTS IN OIL SUBMITTED BY APPROVED BY: FILE; PIGMSNPS-IirniL DATE: JANUARY-1935 INTRODUCTION A sample of treated Opaque Blue CS-7469 -was prepared in the SemiWorks. utilizing the "Newark Direct Process" castor oil-dibutyl phthalate treatment. Themeated product was shipped to Parlin for enamel and lacqudr evaluations? The Semi Works treatment was duplicated in the Laboratory, the treatment being made on Opaque Blue slurries having pig ment contents of 2&%, 17,5% and 12.5^ respectively. B-63-D was treated in the laboratory with castor oil and dibutyl phthalate. Both the direct and indirect processes were used and very close attention was paid to microscopical examination of the slurries at every possible phase of the treatments. In an attempt to produce "super-dispersible" and quick mixing pig ments, BT-125-D, 33-66-D and RT-283-D were treated with Diglycol Stear ate. With the same idea in mind. Y-12-D was treated with small amounts of Nujol. The methods used in the treatments were identical to the direct treatment, differing only in the type of treating agent used. Qualitative tests were made on the possibility of treating B-66-D with Beck-Koller's "Beckolin" (a synthetic 100?? binder vehicle) and two of Barrett* s Paracauraarone-indene resins. *P-10Oftand "P-SS0.** Proper ink evaluations of many of the above treated pigments could not be made because of congestion in the Service Laboratory*s experimen tal program. To prevent a too rapid accumulation of research samples, it was therefore decided to discontinue the laboratory work until the samples could be evaluated either in the Service Laboratory or in the Research Laboratory itself after the proposed installation of an inkmill. It was. obvious that, excepting for brief statements, many of the experimental results obtained during the month would have to be omitted from this report because of the above-mentioned lack of evaluation of prepared products. SUMMARY & CONCLUSIONS A comprehensive castor oil - dibutyl phthalate treatment of B-63D was made in the laboratory in or^er to determine, if possible, the use fulness of microscopical examinations in the t>reparatiorj of oil treated pigments. Two types of procedures were carried out: (a) Newark's Dir ect Process, using no emulsifying agents and (b) Farlin's process, us ing Triethanolamine Oleate as an emulsifying agent. Both processes were used tc^theat B-63-D. Three different blue slurry concentrations were used, namely, a normal slurry from the plant, a 1:1 dilution and a 2*1 dilution. Examinations of the slurries were made under the mi croscope at all possible stages in the treatments. The following con clusions were reached:- DUP050315461 2 1. Colloid milling of the slurry gives increased fineness of dis persion and causes greater resistance to reflocculation than in unmilled slurries. 2. Triethanolamine Oleate gives increased fineness and dispersion in the oil treatment. Resistance to flocculation is more pronounced. 3. In the Direct Process, the second pass of the oil treated slurry thru the mill gives little or no advantage over the first pass, 4. Increased dilution of slurries tends to produce greater floc culation. 5. Under (80X) magnification, the main difference in the appear ance of the slurries seems to he that of flocculation. However, as the interior of the flocculates are examined under higher magnification (400 X) these flocculation differences seem to disappear. 6. The flocculated masses under higher magnification (400 X) are resolved into loose aggregations of small pigment-oil droplets. The sizes of these droplets are practically the same regardless of the size of the parent flocculate. 7. Plocculation of the slurries does not tend to harm the quality of the final treated pigment. 8. A photographic study of the oil treatments would probably be meaningless because of the ultimate similarity of the slurries. 9. Average yields of products give the direct process a 2-3% edge over the indirect process. Treatments of RT-283-D. BT-125-D and B-66-D were made, using di glycol stearate as the treating agent, the procedure being the same as in the castor oil treatments. Rubouts of the treated products seemed to point to a greater ease of dispersion of the diglycol stearate treat ed pigments. BT~?.25-D in particular, seemed to give very promising re sults. 2% stearate gave a vvs weak and green tint against standard the masstone was v.s. brown. It was evident that amounts up to 5% di glycol stearate could be added without materially reducing the strength of the pigment. In the r t -263-d - 'rubouts, c-_ the DGS seemed to give a quicker and easier dispersion. The DGS additions deepen the masstone quite strongly? in the tints, there was a more pronounced loss in strength in the stearate treated RT-283-D than in the treated 3T-125-D. However, nothing definite can be stated insofar as fineness, dis persion and mixing are concerned until proper ink evaluations can be made. Rubouts of BT-125-D and RT-283-D pulps were made and compared with standard dry control. The flushed BT-125-D ink gave a v.s. strength advantage, but on the flushed RT-2Q3-D the conditions were reversed. The flushing of the duol was very difficult, probably due to the low pigment content of the pulp (10^) STujol was added to Y-12-d in order to increase the ease of wetting, decrease mixing time, and possibly improve lightfastness or other pro perties. Controls were run thru the colloid mill before and after the - . ' `"if-. . * DUP050315462 2 3 treated samples to check up on any contamination that might have oc curred in the milling. The action of the mill seemed to darken the shade of all the samples, treated and untreated. Samples containing 8% Fujs&l seemed to he about .5^ weak in tint. The presence of the Fujol (8%) with the pigment seemed to increase the lightfastness some what, but not to any great extent. Ink property tests have not been made as yet. Treatments of B-66-D with 'Beckolin and Paracoumarone resins, P-10 ani-P-25. did not seem to give very promising results. In the first place, the Beckolin-treated- pigment could not be dried without polymerizing the varnish. The water could be removed by flushing it out on an ink mill, but this usually indicates the production of an ink, which in this investigation, is not desired. The Couraarone resins were too heavy and viscous to be used in their natural state. Treated samples of B-66-D were prepared by thin ning the resins with hi-flash naphtha, but they were very inferior in properties - hard, difficult to disperse and dull in tone when incor porated into an ink. The fire hazard plus the added expense of the hiflash naphtha makes these resins of doubtful value as treating agents. Opaque Blue, CS-7469- was treated with castor oil and dibutyl phthalate, duplicating the method used in the semi-works in the prepara tion of SW-6698. Treatments were made on a press cake and a 12.5 slurry of blue. Both treatments seemed to work fairly well, although handling the 12.5$> slurry was difficult because of its soupy character istics, The filtration was accomplished with great difficulty - evident by a dense cake first forming over the filter paper, clogging the pores and preventing further filtration. It was thought that operation losses could be reduced materially by making the treatment on a 17.5^ pigment slurry A hatch of Opaque Blue was treated in the Semi Works using the same process as was used in the preparation of SW-6625. The blue slurry at 12.5^ was in a very soupy condition, filtration was extremely slow, and there was a pronounced loss of blue in the filtrate. The yield was 60% less than theoretical due to the filtration .losses and losses due to splattering when the press cake was removed from the cloth. Samples of the treated product were sent to Parlin for evaluation. They report ed back that a sample of the blue, dispersed in a laboratory Banbury mixer, gave a grit free enamel with a high gloss and a hiding power double that of Chinese Blue. ADDENDA Results obtained from 359-83 (oil treatment of Chinese Blue), evaluations of which were not included in December - 1934 report: According to Parlin. it seemed evident that 17-45 parts of oil (to 100 parts of treated pigment) was not sufficient because it did not pre vent agglomerates from forming during the drying process. The agglo merates could not be dispersed at a colloid consistency suitable for handling in the factory Banbury Mixer. These amounts of oil were con siderably less than the minimum indicated by previous semi-works experi mentation for parlin. l DUP05031 5463 4. There seemed to be practically no difference in the amount of grit, whether the direct or indirect method was used. In one case, at 45$ oil* the indirect method gave superior gloss, but no other differences were noted. EXPERIMENTAL DETAILS 359-84. Treated B-63-D for special micro-examination (p. 191). B-S3-D slurries with a (100 g. dry) pigment content were exam ined systematically as follows: 1. Preparation of the Blue. a) Examination of the original slurry bj Run (a) thru colloid mill and examine for dispersion c) Let (b) stand and watch flocculation 2. Preparation of emulsions d) Make castor oil-dibutyl phthalate emulsions without emulsifying agent. e) Emulsion prepared using Triethanolamine Oleate. 3. Treatment f) Mix (b) and (S) and run thru mill - examine. g) Mix (a) and (d). and examine (1) after first (2) after second pass. DlCC.+ 4. -Dr-i-ed- method repeated with three different concentrations of pigment (original (7.5#), 1:1 dilution, 2:1 dilution). 5. Indirect method (Pariin's) repeated with the same slurries. Oil Content of treated products - 54$ (Castor Oil - 40$ (Dibutyl Phthalate - 60$ 451-1. Preliminary Treatment of B-66-D slurry with diglycol Stearate (p. 1) Samples of B-66-D were treated with 1$, 5$. 10$ and 25$ diglycol stearate (based on 100$ treated product). Two passes were given thru the colloid mill. Rubouts were made and samples sent to the Service Laboratory for evaluation. 451-7. Treatment of BT-125-D with Diglycol Stearate, (pp.ifc) The treatment was identical with (451-1) except that 2$. 8$ and 20$ of diglycol stearate were used in the treatments . 451-8. Treatment of RT-283-D with diglycol stearate (p. 20) The treatment was the same as (451-7) 451-5. Y 12-D treatment with Nujol (p. 14) The yellow slurry was treated according to the "Newark Direct Process" with 1$, 3$ and 7;-, Nujol. Control samples were run thru the mill before and after the treated samples. Rubout and fadeometer tests were made. Samples were sent to the Service Laboratory for evaluation. 451-3. B-66-D treatment with synthetic resins of the paracoumarone indene type (p. 9). Samples of B-66-D slurry were treated with Barrett's "Cumar Resins, P-10 and P-25. Procedure was the same as an ordinary dirdct N - .. DUP050315464 3/ 5. process oil treatment* The process was repeated, thinning the resins with hi-flash naphtha. Rubouts were made on the treated samples. Resin Content - 45^ Pigment - 55$ 451-6. Treatment of B-66-D with Beckolin (p. 16). Treatments were made on B-66-B using 2% and 25% Beckolin synthetic varnish. Rubouts were made on the treated samples. 451-2. Opaque Blue CS-7469. Ip.7) The blue was treated with a castor oil dibutyl-phthalate mixture according to the method used in SW-669B. Treatments were made on slur ries having pigment contents of 24^, 17*5# and 12.5%. ( Castor Oil -40% Y/ ''vji.-- Oil Coifent - 54^ ( Bibutyl phthalate 60^ SW-6698. Opaque Blue CS-7469. *>. ` The amount of slurry equivalent to 25# dry pigment weight was treated with castor oil and dibutyl phthalate according to the method used in SW-6625. Two passes were given thru the colloid mill, the milled sample filtered, and the cake dried in an. electric oven at 140P. The treated sample was shipped to Parlin for evaluation. (Castor Oil -40^ Oil Content - 54^(Bibutyl Phthalate 60% DUP05031 5465 m ffei;ti|w K it* I: $:,v TO-.! '(/w' Sjsfl fiSeisA', r- *;:; I:. <& - PIGMENT COLOR RESEARCH REPORT jir-/3 SUBMITTED BY: APPROVED BY: RUBBER COLORS 7 / *r---- ------------- * n ^' FILS; RUBSESUGOLOfeDATE: JANUARY-1935 INTRODUCTION Laboratory work on the general problem of Rubber Colors has been continued the past month. Four phases of the problem have been studied. 1. Diglycol Stearate treatment of PTA colors. 2. Green Lalce to match Imperial's X-1292 3. Lake Red C 4. Pigment Green B The last two are covered in separate reports. SUMMARY & CONCLUSIONS 1. Diglycol Stearate treatment of PTA colors. The treatment, which is a combination of the use of Gardinol in the PTA, Blanc Fixe extension and Diglycol Stearate, was described in the December report. It has been applied to three of the more likely colors and CS procedures set up as follows. 1. 3T-125-D - CS-7759 2. GT-347-D - CS-7789 3. RT-357-D - CS-7790 Samples of each have been submitted to the Rubber Laboratory for evaluation. We believe they possess a degree of dispersion very close to that of the corresponding Latex dispersed colors and should command considerable attention where the shades are of interest. The same procedure has been applied in a preliminary fashion to a color resembling GT-57-P (Green XD) with substantially the same de gree of improvement. We believe the method is of general application to PTA colors and the only limiting feature will be the stability of the resulting dry color in rubber compounding. We also believe that Cyclohexanol amine Stearate can be used in place of the Diglycol Stearate and that it is highly probable that other agents of the same general classes can also be used. These^treated colors exhibit a remarkably soft texture and are very easily ground in oil on the rubout bench. This property suggests their applicability to other situations in which the commercial prac tice includes incomplete grinding such as- for instance, carbon paper inks and the ordinary types of paint grinding. Tc test this out fully, control samples corresponding to the three 33 numbers mentioned above have been prepared as follows: A - Toner control like standard color B - " containing Gardinol in PTA C - As 3 but extended with Blanc Fixe These are being tested by the Service Laboratory and will be reported later. DUP050315466 2 2. Green Lake to match Imperial's X-1292. The December report tells of submitting; certain samples to the Rubber Laboratory for evaluation. They refused to approve any of the four submitted.. In order to use Lithosol Brilliant Blue 3. if possible, the Byeworks lias submitted not 28, their latest improvement. ,7e find it to be inferior to Alphazurine but not markedly so and we have de cided to try to develop a satisfactory color from it. We have also obtained samples of Naphthol Yellow from National Aniline, from Calco and from General Dyestuffs. One of these, from Rational, is much cleaner in combination with the blue than the others but also somewhat weaker. These two dyestuffs will be the starting point for addition al work. The original sample (C-36780) is exhausted and a new sample (C-37280) has been obtained from the manufacturer. There is also a third sample (C-36807) available. No two of these samples are alike and the first one is decidedly the best of the lot. Inasmuch as we have ample supply of the latest sample, and as it is intermediate be tween the other two in properties, we have decided to devote our future efforts to matching it (C-37280) and we feel that it will be a fairly simple task. 3. Goodrich Lithol The customer has given CS-7758 a tentative approval and has ordered 100 lbs. for further tria1. Sufficient amounts of the ingre dients of this CS are available and the order will be made up promptly. 4. Miscellaneous Fairfield has complained of poor dispersion of Y-299-D. This was surprising in the light cf our limited experience with the color and we were unable to obtain any indication of the same. However, we did determine that y-366-D represented a further improvement in Chrome Yellows and have suggested its trial at Fairfield. There was also some complaint from the same source on the shade of. BP-69-D. Laboratory experiments have indicated that this can be corrected by using a small amount of a. greener dye in the strike (An- thraquinone Blue B as u^ed in 3F-79-D) and this procedure can probably be used in case of similar trouble in the future'. Satisfactory material, however, has since been made in the plant from the regular dyestuff used in BP-69-D. ECFBR IMS ITTAL DETAILS See notebook 435. pp. 116-145 435-50. RT-357-D with Gardinol, Blanc Fixe and Diglycol Stearate treatment, variable in amount of Gardinol. The series indicates an op timum in 50 C-l which uses 1.5 gm. Gardinol to 12.5 gm. dye. 455-51. The series represents an attempt tc reduce the amount of Blanc Fixe in the 48 3-1 method (treated GT-347-D). The nethodsused were: 1) Use of deficient amount of 3aCl2 to precipitate all the sulfate ion. 2) Use of a mixture of sulfuric and hydrochloric acids. The yields were reduced as desired but at the same time, the dispersion in rubber became less satisfactory. Hence no change is contemplated. DUP050315467  435-52. In order to test the applicability of the special treatment developed in C3-7759 (see Dec. report' certain controls were prepared so that the colors could be tested in printing inlc a.nd in paint with a view to determining possible patentable features in the process . A - Toner control as 3T-125-D B - As J but containing Gardinol in the PTA C - As B * " Blanc Fixe. C3-7759 is like C with the addition of Diglycol Stearate. "'osts are in progress. 455-53. The effect of adding diglycol stearate at different nieces. A - Bo DGS B - DGS at end C - DGS to toner before extending D - DGS to PTA before toner strike D is definitely inferior and there is no apparent advnatage in C over 455-54. Vary amount of DGS used- also try Cyclohexanolamine stearate and Sodium Stearate in treated GT-347-D. Sodium Stearate is inferior. Cyclohexanol&nine stearate is sub*. stantially like DGS. There is no outstanding difference between Ifand 5; of the latter. 435-55. Test of various samples of Naphthol Yellov; in the Green Lake to match Imperial's X-1292. A - Paper Yellpw L Cone. - D-1859 B - Naphthol Yellow SG - Calco - D-1898 C " S" D-1899 D * S National L-1900 E n S Cone. National D-1901 All used Alphazurine as the blue component. It appears that all the nev: dyes give slightly cleaner products than Paper Yellow L Cone. However, only D-1900 is outstanding in cleanness, but it is also weak. It is possible that an increased a- mount may be used and obtain the desired shade while maintaining the cle anness . 435-56. This series is a preliminary comparison of the various methods of treating GT-347--D. A - Toner control B - As A but Gardinol in PTA C - As B but struck with 3aCl to give 3aS04 in color D - As C but add DGS {5ft) at the end. Rubout strengths are very close to toner content. In rubber, there is a definite improvement in 3 over A and in C over 3. D and C are almost identical but the DG3 will be continued as r safety factor. 435-57. This series represents an attempt to adjust the dyes in 48E to match GT-57-P in shade and to treat the resulting toner? for use in rubber. The desire'.' re.nge is obtained but all the colors are much cleaner than Green HD (Later, dispersion of GT-57-P' . Also Green XD did not fade in cure in this experiment so that the treated pro ducts are somewhat weaker. Any further work will be based on 57 C-l. _k DUP050315468 4. 455-58. To compare colors like 564 < 563 with Latex distercions of the same. In this case the treated dry color shows better strength in rub ber on a toner basis than either its own latex dispersion or that of the toner. This confirms our opinion that the method of treatment gives substantially perfect dispersion with PTA colors. 455-59. 600 grams of color like 483-1 was made up in four charges. mixed and set up as CO-7789. It compare? with. GT-347-B as follows. By rubout 255 parts CI-7759 = 100 parts GT-347-3 In rubber 12.0 " "= " " and the resulting slab is much cleaner than GT-347-3. It is being submitted to the Rubber Laboratory for evaluation. 435-60. A lar-e sample like 50C-1 (RT-357-3 treated' was set un as CS-7790. In rubout 180 parts C5-77SG_= 100 parts RT-357-3 In rubber 100 " " is stronger and much cleaner than 100 parts RT-357-3. It is being submitted to the Rubber Laboratory for evaluation. 435-61. Further study of dyes in the Green Lake like 55 ser ies . A - Control - Alphazurine - paper Yellow L Cone. B - Lithosol Brilliant Blue S- Lot 28 - Paper Yellow I, Cone. C - Alphazurine - Laphthol Yellow SXX - Genl. Bye. D-1904 D- " " S 3-1900 Check to 553 E - As 3 but increase yellow dye 2Of? The Lithosol Brilliant Blue 3 (Lot 28) is not quite equal to Alphazurine but it will be used in future work. There is nothing of interest in General's Yaphthol Yellow. The increase in yellow in E gives good strength but the product is still blue. Future studies will be devoted to attempts to use Lithosol Brilliant Blue 3 (Lot 28) with Uaphthol Yellow S of National (3-1900). A new sample of the com petitive product (Imperial's Rubier Green X-1292 C-v37280) is inter mediate between the two previous samples and much inferior tc the one we had previously tried to match. Inasmuch as the old sample is ex hausted and there is ample of C-37280 which was obtained from the manufacturer, we will set it up as the standard to match. 435-62. Controls for testing CS-7789 in paint and printing ink. A - "Toner as GT-347-3 B - As 4 but Gardinol in PTA C - As C but extended with 31anc Fixe 435-63. Control? for testing C3-7790 in ps.int and printing ink. A - Toner as RT-357-3 3 - As A but Gardinol in PTA C - As B but extended with Blanc Fixe D - As C but treated with 3GB - Check to C3-7790 except for using different dye. < DUP050315469 PIGMENT COLOR RESEARCH REPORT 3r-/y PIGMENT GREEN B SUBMITTED BYY: ^~. APPROVED BY: v ** . 7 / PILE: JSSSx=SES6 DATE: JAMJARY-1935 INTRODUCTION The problem of developing a dry pigment Green 3 for rubber was continued this month along the lines of the diglycol stearate method 444-2D. Some time was also devoted to the testing of plant and sani- worlcs pulps for rubber and paper purposes. SUMMARY & CONCLUSIONS The lead uncovered last month on the striking effect of digly col stearate in improving the dispersion in rubber of the dry green toner, was followed during this month. Variations in the amount of D.G.S. from 0.5 g. to 2,0 g. per 0.1 mol showed that apparently the optimum effect was obtained with 1.0 g. The resulting dry color, milled in rubber, is about 15% weaker than the later dispersion of General's Pigment Green B and is somewhat dirtier. The method (4442d ), also, is not very consistent. However, the products obtained are consistently and decidedly better than those of the cadmium - Turkey Red Oil method (406-66C), It was thought that possibly the use of diglycol stearate toge ther with the cadmium soap of Turkey red oil might yield cleaner col ors. Accordingly, a study was made in which the Turkey Red Oil was reduced from 3.0 g. to 0.0 g. the cadmium sulphate kept constant and the diglycol stearate also maintained constant. Improvement in disper sion was obtained as the turkey red oil was reduced from 3.0 g. to 1.0 g. but f&ien the turkey red oil was omitted, a very we&k and dirty color resulted. These results suggest another experiment in which the cadmium sulphate should be varied. The addition of blanc fixe to method 406-66C gave an improvement in rubber dispersion but not sufficient to equal 444-2D. The run, in which extender was added to method 444-23. was very unsatisfactory for some unknown reason and will be repeated. In order to obtain information which might be of some assistance in the semi-works development, the effect of making the bisulfite ester alkaline with caustic soda and with soda, ash and the effect of omit ting the alkali from the ester, was cheeked. The results were in line with what had been previously obtained. The best method was the regulargstandard procedure, 406-66-C, in which the ester is made alkaline with caustic soda before the ad-'.ition of the cadmium soap, etc. The worst results were obtained with the acid ester method. These results were found to be true whether tested as pulps in rubber or in paper. A report was received that GT-68-P lot 13915 was weak by the paper test. Lot 13915 was a mix of lots 40823 and 40942 which had been Mr. previously approved by the Paper Laborator;;-. Consequently, it was be lieved that the condition of the pulp might have changed on storage. Therefore lot 13915 was treated in the laboratory for the purpose of .'r . i- DUP05031 5470 improving its dispersion in paper. No improvements were obtained bycolloid milling or by treating with dispersing agents such as glue, Leukanol, Bindex and Duponol and subseouently massing thru the colloid mill. An experiment was run in order to obtain additional information for the Legal Department. It was found that ferric oxalate and ferric chloride were very unsatisfactory substitutes for ferrous oxalate whether used with an alkaline or an acid bisulfite ester. The use of the acetic acid treatment prior to filtration did not improve the pro duct obtained by the use of ferrous sulphate in theoretical amounts, i.e. 1 Je to 2 BN. EXPERIMENTAL DETAILS Notebook No. 444 Series 444-4 and 5 varied the amount of digljrcol stearate in method 444-2D from 0.5 g to 2.0 g per 0.1 mol. Prom the results it appeared that the optimum effect on disper sion of the dry color in rubber was obtained when 1.0 g of D.G.5. was used. Lower or higher amounts decreased the strength. The 444-2D method seemed to be unstable. Unsatisfactory checks to 2D were obtained in series 4 and 5, However, the products obtained by this method were all far superior in rubber dispersion to the 444-66C (CD-TRO) method. Series 444-7 studied the effect on 444-2D of omitting the caustic soda from the~~ester; of developing to the boil; and of omitting the acetic acid treatment. The check to 444-2D was very unsatisfactory, therefore no conclu sions could be drawn. This series will be repeated. Series 444-8 studied the effect of adding blanc fixe extender to 406-66C and 444-2D methods. The addition of extender to 406-66C improved the dispersion of the dry color in rubber but the improvement was not equal to the 4442D product. In this series, adding blanc fixe to 444-2D gave a very weak and dirty color. The latter should be checked. Series 444-12 checked effect of variation in Turkey Red Oil from 3.0 g to 0.0 g. in method 444-2D. Reduction in turkey red oil from 3 g. to 1 g. gave a decided improvement in dispersion; but when the turkey red oil was omitted a very weak, dirty color resulted. In this series the cadmium sulphate was maintained. Series 444-11 checked the effect on the pulp color for rubber of making the ester in 406-66C alkaline with caustic sods, with soda ash and the effect of omitting the alkali from the ester. When the alkali was omitted from the ester, the resulting color was weak and dirty. The method in which the ester was made alkaline with soda ash gave fair results but not so good as those from the me thod in which the ester was made alkaline with ce.ustic soda. The re sults corresponded in the rubout test, the paper dyeing test and in the rubber test. Series 444-13 was an attempt to improve GT-68-P lot 13915 for use in paper dyeing. Treatments such as colloid milling with Duponol, Bindex, Leukanol and Glue were ineffective for improving the strength in paper. DUP05031 5471 3* 3 Series 444-9 was a miscellaneous experiment to obtain additional data for tEe~Patent Application. It was found that ferric oxalate and ferric chloride were very unsatisfactory substitutes for ferrous oxalate whether used with.an allsaline or. aeid bisulfite ester. The use of the acetiig acid treatment prior to filtration did not improve the product obtained by the use of ferrous sulphate in theoretical amount, i.e. 1 Fe to 2 BN. I ,i DUP050315472 PIGMENT COLOR RESEARCH REPORT Jf'-Aar ^7 Submitted by: Approved by: PIGMENT GREEN B GT-68-P SEMI-WORKS ---------------------------------------------- viO . v\. _, -v *> 3 . / ' FILS: mt s o . t d t o p r DATE: JANUARY-1935 INTRODUCTION Development work in the Semi-Works was resumed this month. It was desired to improve cleanness and tint for use in rubber, and the application of this pigment for paper work made it desirable to improve, besides the previous mentioned properties, the pulp proper ties - that is, uniformity and dispersibility. SUMMARY & CONCLUSIONS Semi-Works development work consisted of nine runs; the process selected was SW-6526 which had previously yielded material satisfac tory tinctorially in rubber but not satisfactory in pulp properties. It was thought probable that an increase in acetic acid after the strike would improve the flocculation of the pigment and hence its pulp characteristics. Increases in acetic acid of 10$, 50$, and 100$ were carried out; this increase did not affect the tinctorial or pulp properties appreciably for rubber; however, for paper the large increase of acetic acid caused a 10$ loss of strength. De creasing the amount of acetic acid 50$ decreased the strength in rubber (5$) and gave a poorer pulp while in paper there was little tinctorial difference* Paper tests as reported here may not be reliable, as a new testing method is being investigated. In the previous development work, indications had been obtained that yellower and cleaner material was obtained if carbonate instead of caustic alkalinity was used in the ester. Checking this variation gave a product with an improvement in pulp and rubber properties, but 20$ weak in paper tests. The omission of any neutralization in the ester and use of all carbonate alkalinity after the strike did not improve its properties. Similarly, indications of improvement in cleanness and tint had been obtained by increasing the caustic alkalinity of the ester. In order to further study this variable, two batches were made, one with a 10$ and the other a 20$ increase in caustic. The 10$ increase in caustic gave an appreciable increase in cleaniaess and yellowness, the 20$ increase gave a product OK in strength but very blue in tint'. A comparison of the results of the paper and rubber tests shows wide discrepancies; these are due to the method of t esting in paper which is unreliable. An improved method of testing in paper is being developed and it is hoped such a method will more closely correlate paper and rubber results. Pulps for paper trade will require very close standardization to a 25$ pulp, probably to obtain this from a washed pulp will require treatment in a pulp mixer or pulverizer. A brief summary of the mixes made this month will be found under Experimental Details, DUPO 50315473 *iflS*SS$g$ EXPERIMENTAL DETAILS. Notebook 351, p p . 147, 149, 154-159 CM .t H X Id *. E .O r3o3 H a 9 Id P 03 r*H l fl W > C3 rH X9 (X, s- s rT3H3 O P H X rH <e> g Id P Vt X aO4 *4 o *c2t4f ao4 k 4cC4dD o XO oX 03 CO S -s s* d >uo 43 rH X Ma% sBrHt Ab0HdO nIh o 0 4043 bO 4^3 MO* 'rjXSHS0HSI 0O VBSHi xdSoJ Ob 4Id oI* 0 A8S *sfOl gB- -t0H* VrHi m3> n 0*3 tpHo mOa) <SSHH MAIatJ oP 02 \ OH0Ib* O P< CO rH MOc*d Pd p4to2 V+oIod>* rP0pH*d. at>* > p Id > H p X <3 Id H * i-4 X fi pId mO rT=9HS? a p-HO aod*% >CoO. Xo o 3d*3o. n AdnSrJ pIdp* O >b V_arCH, rs3H* ho *Sr3 Pk as Ph * &P Oc S3 m 0H J4 CO Qo3 * Xo rH O* rH *2 a O 24 O rH -0 > fn. o 44 OS O<{4 O 0O3 O0 CO o a* 00 03 Oh O >e xt* CO tO c? in uD i fe: <o CO to oo o 43 O 0> >0 P Oi CO o * X 00 CJ> o Cv? N2 03 02 0 o CO 0 CO 0 O CO CO 02 rH rH CO H CO CO ^4fc Id ro O TO P H +> -p ^ O o CO X w*a O rH o S X B <JS 1 t > o pH ro -o Ifc m i po H -P p Ifc Pd O CO ^ K ^ O a* un <o lO to tj J 33 CO Id X J fcX '0 0 03 CO ^ & 0 1 co H -P PO Pd C**O+ 9X, Q O 0 rH 02 40 U 0 3 j5 CO 00 4* o Id 43 o O o 0 0 CO <?> 03 9 Ih P Pd P 'T' Ik Xo C rH rl *3> < 0 t0%a Id 0a O J Vi gs Id ^ 0 Ste Vi CM 0 O CO * 43 ' O 3b 0 0 0 0 CO ft--s 1^ 0 V rH po PP oo X CO H' O Jb 0 0 01 ^O EB X 0 A! Si 9 X T3 C 0 0 Ob i--1 CO CO s p d a p p V X p 44 rH P ! <d* t J P Ob 0S 0 I. J I. P 0 p Vd n 44 ro E TVS rl 2S O 5^ O 0 02 # rH CO >$k lO P rH *rl Id p Pi P O X c H 0 03 33 to Q 0 Of 12 35 0 a 44 o Id 43 o a rH 02 0" 0 X ft CO CO w fo fl 02 H Id p PP o X o *H 0 02 X 0O 0 i as 3s 0 44 O l Xo o CO 4* 0 HPi O P o i~H M a ft _ro ro > > > a & 03 rH A >* p I* > -H >X ft. *} fc4 O rH CO uo P0 ft H* 03 o Q 4* o8 CO 02 X o 9 ^**S X p rl 3 rH rH Cm > . XX H in rH Oi CO rH ?! 02 oo 02 03 TJ P rl -- X 'H rH S 44 43 p V 4> S VU T3 13b M CO H O l 9 ro rH > P P r9H ISd O P ^ >4} 0 03 13b CO rH CST rH tf> oC^ft o0c>o3 H P 3S aoVl P P 002 CO DUP050315474 PIGMENT COLOR RESEARCH REPORT ff PTA YIELD STUDIES - 5 . ~> / SUBMITTED BY: 6 APPROVED BY: INTRODUCTION Production on RT-329-D and RT-3S2-D was continued during this month, five batches being made. Also included in this month's PTA toner production was three batches of RT-330-D, three batches cF BT-125-D. and one batch of BT-92-D. The Development Section continued to observe yields on these toners. SUMMARY & CONCLUSIONS Yields on RT-329-D and RT-392-D showed a slighljimprovement over last month, the average being 1$ under estimate as compared with 1-1/2$ under estimate/the average yield for last month. Quality tests on these batches were satisfactory. The three batches of RT-330-D showed a satisfactory average yield of 101$ of.estimate with rubout results also satisfactory. The BT-92-D batch gave a fairly satisfactory yield of 98$ of es timate together with satisfactory rubout results. This yield is con sidered satisfactory because of the fact that small losses occur when `color is passed through freshly cleaned press cloth which do not take place when the cloth has been thoroughly impregnated with the color. Yhen this loss on the first batch is averaged off over a number of batches it is practically nullified but when only one batch is made as in this case the loss must be taken up by that batch. The BT-125-D- CS-7609 formulation still remains a sore point as far as yield is concerned. The dye-precipitant balance was adjusted in these batches so that a clean strike was secured and the quality was satisfactory. The average yield, however, on the three batches made showed no improvement over a batch reported in the November yield study report, still remaining 90$ of estimate, pressing, at the start, was satisfactory shewing only a trace color bleed which ordinarily clears up as a cake builds on the cloth providing the color is not pumped into the press too rapidly. Check laboratory strikes made exactly on this formula and with the same dye as used in the plant showed an average yield of 100-1/2$ of estimate, which is equivalent to an 88-1/2# yield in the plant. Prom this result it would seem that the only possible source of loss is in the press-room especially since the three batches made on exactly the same formulation, with the same materials, and showing practically identical rubout results showed as much as a 10$ difference in respective yields. Por rubout and yield results on these plant batches see Table I. DUP050315475 Color Yield Batch Est. Lump RT-329-D 41218 99# 106# If 41233 99# *99# RT-392-D 41252 99# **85-1/2# W 41264 99 98 RT-329-D 41291 99 100 RT-330-D 41507 96 96 If 41531 96 96 II 41588 96 100 BT-92-D 41662 96 94 ET-125-D 41550 88 74 If 41587 88 82 tv 41616 88 78 Grind Rubout vs. Standard Mass. Und. Str. Tint die yel. s .str yel. It vs bl vs wk vs bl die yel -- -- It very dark vs bl v.yel. vs wk -- vs bl&dirty -- vs dark vs yel s .str s'. ye 1 vs It(brn) s .bl vs str bl vs dark s.yel yel ft vs str str vs green s ,dk It s .str n v>5 SfV tt s .str Str n t* i * note. **Hote. This weight includes 3# transferred to Sales Service. This weight is actual lump weight of this batch. Lump weight of 90# as reported by plant includes 4-1/2# from RT-392-D batch 41182 returned by Sales service. DUP050315476 PIGMENT COLOR RESEARCH REPORT TREATMENT OP PARA TONERS WITH DUPONOL J<*C SUBMITTED BYs O-W APPROVED BY: PILE s TREATIBG-AQ^ DATE: JANUARY-1935 * 'h- INTRODUCTION A series of Para Toners were run in the laboratory to determine in the case of RT-70-D and RT-280-D, the effect of substituting Duponol for the Para Soap as used in the standard formulae, and in the case of RT-22-D the effect of adding a small amount of Duponol to the Betanaphthol solution before coupling. SUMMARY. & CONCLUSIONS Substitution of Duponol for Para Soap in the RT-280-B formula using one half the formulated amount gave unsatisfactory results. The masstone was quite bright, but the Duponol had only a slight effect on the strength and tint, the Duponol treated toner being much weaker and bluer than the control made on the standard RT-280-D formulati on. Addition of an identical amount of Duponol to the Beta-naphthol solution before coupling in the RT-22-D formulation gave a v.s. light and bright,vvs strong and a.yellow product versus the control. This product is an improvement over RT-22-D in masstone but the yellow tint may not be desirable in this Para toner. The use of Duponol as a replacement for Para Soap in the dark Para toner. RT-70-D. gave unsatisfactory results, the product being light and flat> weak, and blue versus the control. EXPERIMENTAL DETAILS 440-37 A. Control RT-280-D. CS-5996. (2 gms. Para Soap in coupling) B. As A replacing Para Soap with 1 gm. Duponol. Rubout Results: B vs. A: bright - blue - weak - bl A vs RT-280-D Std: vs It, flat - yel - str - yel Bw w lt-brt - yel - vs str - s.yel 440-38. A. RT-70 control, CS-6300 (4 gms Para Soap in coupling). B. As A replacing Para Soap with 2 gms. Duponol Rubout Results: B vs. A: s.lt&flat - bl - s.wk - bl A vs. RT-70-D Std: brt - yel - str - yel B * s.lt - " " 440-39 A. RT-22 control. B. As A using 1 gm. Duponol in coupling. Rubout Results B vs. A: vs lt&brt - vs yel - vvs str - s.yel A vs RT-22-D Std: It - yel - str - yel T5 a n *i *t < DUP050315477 PIGMENT COLOB RESEARCH REPORT TOLUIDINBS SUBMITTED BY APPROVED BY: FILE: TOiUB&HSS DATE: JANUARY-1935 INTRODUCTION In order to observe the effect of contamination in the diazotization of Meta-nitro-paratoluidine. experiments were carried out in troducing various degrees of impurity in the form of decomposed MNPT diazo. SUMMARY & CONCLUSIONS A sdries of toltiidines were made on the RT-386-D formula. Lab oratory conditions were compared with those in the plant as nearly as possible by using all glass equipment in contrast to wooden paddles, one set of paddles new, another set allowed to soak overnight in a diazo. and the use of a beaker containing a small amount of decom posed diazo. The results indicated that contamination in the forms mentioned, while appearing to cause progressive degrees of sedimenta tion in the diazos, did not affect the finished product with any marked difference in brightness of shade or strength. EXPERIMENTAL DETAILS 440-35. RMS made on laboratory RT-386-D formula. A. Control - using laboratory procedure; glass stir. B. Clean wooden paddles. C. Wooden paddles soaked in a decomposing diazo D. Five cc of a day old diazo placed in beaker before diazotization. Results: B vs A - vs dark & briglnt - vs wk, vs blue CH ws It - OK - OK D* dark - vs weak - s. blue DUP050315478 PIGMENT COLOR RESEARCH REPORT AZO-SULPHITE DERIVATIVES v SUBMITTED BY APPROVED BY* FILSs LSTHGL-REDDATE: JANUARY-1935 INTRODUCTION A procedure for the preparation of the soluble azo-eulphite derivative of Lithol Red and its subsequent conversion into the calcium toner was set up and as signed CS-7801. This method has been submitted to the Jackson Laboratories for their evaluation. SUMMARY & CONCLUSIONS It is evident from the results of our studies on the problem of preparing the soluble azo-sulphite derivative of Lithol Red, that at least three factors are veryimportant s 1. The ratio of sodium bisulphite to caustic soda; 2. The amount of sodium bisulphite; 3. The temperature of reaction. It has been demonstrated that sulphurous acid, or sodium bisulphite or sodium sulphite alone will t. '.I not effect complete conversion of the sods, salt of Lithol Red to the soluble azo-sulphite derivative. Complete conversion occurred between 'ratios of 1.4 and 3.62 of sodium bisulphite to caustic soda, provided 6 to 8 times ' the theoretical amount of sodium bisulphite was employed. It waB also necessary to raise the temperature to 80-85C to complete the reaction. The addition of Leukanol in the coupling of the soda salt facilitated the conversion. Lower amounts than 3.5$ (based on dry pigment) were less effective, higher amounts were without advantage. Since complete solubility was obtained on lowering the volume from 5 to 2 liters, the latter volume being more convenient was adopted as standard procedure. Also somewhat better results were obtained in the calcium toner preparation from the lower volume. A 15$ concentration of salt was found to give substantially complete separa tion of the azo-sulphite compound on standing overnight at room temperature. Norit and filtercel purification of the azo sulphite solution ^assists in eliminating any colloidal unconverted soda salt or impurities, although it appears to be accompanied by an appreciable loss in yield and in strength of thB calcium to ner. A higher amount of calcium chloride was found to be required in preparing the calcium toner in the case of the azo-sulphite method than in the RT-379-D standard procedure. In order to obtain satisfactory yield and the maximum strength it was shown that the calcium toner slurry must be submitted to an acid treatment before filtra tion. The slurry must be slightly acid to Congo red in order to insure the .solu tion of the calcium salts precipitated during the reaction, probably calcium sul phate, calcium bisulphite and calcium sulphite . The calcium toner prepared by the CS-7801 procedure is dark and bright, strong and clean versus the laboratory control on RT-379-D and the RT-379-D standard. The CS--7801 process was submitted to the Dyeworks for their evaluation. DUP050315479 2. EXPERIMENTAL DETAILS Notebook 446, pp. 32-83 Series 446-9 was a yield study on the acid type coupling of RT-364-D, CS-7290 by the conversion of the azo-sulphite compound to the azo red by the caustic soda method. The total regenerated azo red was approximately 96$. Series 446-10 prepared azo sulphite derivatives of Red for Lake C, Lithol Ru bins, Permanent Red 2B They were analyzed for the total $ recovery. Red for Lake C gave approximately 95$ recovery while Lithol Rubine and Per manent Red 2B.gave only 50-60$. Further work will be carried out. Series 446-11 was disregarded due to faulty conversion of the soda salt. Series 446-12-13 tried the use of Leukanol, 1$872, a dispersing agent, to determine"its influence, if any, on the conversion of the soda salt to the soluble azo sulphite compound. Leukanol gave a, more rapid and a more complete conversion of the soda salt. Amounts of Leukanol lower than 3.5$ based on tthe dry pigment content were less ef fective while higher amounts had no advantage. Approximately 15$ salt concentration was found to give substantially complete separation of the azo-sulphite compound on standing over night at room temperature. Series 14-15-16 carried out a study of the SOs - caustic relation in the con version of the soda salt thru the stages of all sulfurous acid to all sbdxum sul phite. It was found that sulphurous or sodium bisulphite or sodium sulphite alone did not give complete conversion. Between the ratios of 3.62 and 1.4 of NaHSOa to NaOH complete conversion occurred provided the sodium bisulphite was 6 to 8 times the amount of soda salt. The water solution of azo sulphite was stabilized with a small amount of so dium bisulphite. Heat or the addition of alkali or merely the solution itself on standing will regenerate the azo-red. Series 446-17 tried the reduction of the amount of sodium bisulphite, keeping the ratio of bisulphite to caustic soda constant. It was found that the ratio of sodium bisulphite to soda salt can be reduced from 8il to 6:1, but it appeared evident that the ratio 6:1 was too close to the lower limits of complete solubility to work satisfactorily. The 8:1 ratio was ac cepted as the most logical amount. Series 446-18 tried the formation of the chromium complex of th,e azo-sulphite compound. No valuable results were obtained. Series 446-19 varied the volume of soda salt from 2 to 5 liters. It was found that complete conversion ms obtained between the two points. In the lower volume the azo-sulphite compound began to precipitate out of solution on cooling to approximately 35 . The higher volume seemed to contain a small amount of fine red precipitate indicating the higher limit of dilution. Ravi as 446-20 prepared calcium toners from the previous series. It was found that the lower volume gave nearly the srune yield as RT-379-D laboratory cohtrol. The others gave approximately 20-25$ higher yields with corresponding decrease in strength. The lower volume was chosen as the best. Series 446-21 tried the purification of the previously prepared azo-sulphite derivatives. A sulphate free product of azo-sulphite was not obtained. DUP050315480 3 Series 446-32 reduced the CaCla from the regular procedure to the theoretical amount. The amount of CaCl2 was found to be 40 grams per .05 mol strike. Higher amounts had little effect while lower amounts gave inferior results. Series 446-24 studied the effect of the acid treatment of the calcium toner in the laking procedure. Finishing the calcium toner slightly acid to congo red gave very good results. The yield was reduced to about equal to laboratory control RT-379-D. The product was dark, strong, clean versus control RT-379-D and also versus standard. Series 446-27 tried the effect of a norit-filtercel treatment of the soluble azo sulphite. Undoubtedly, the norit-filtercel treatment aided the removal of the colloi dal or finely suspended particles in the soluble azo sulphite. It appeared to be accompanied by an appreciable loss in yield and a decrease in strength. fwt: iJJfe' . 'dt- DUP050315481 PIGMENT COLOR RESEARCH REPORT DUQL ESP RT-283-D -V * ' } ' 1 SUBMITTED APPROVED BY: PILE: TftJOBg-9 DATE: JANUARY-193 5 INTRODUCTION One "batch of RT-SSS-D was made in the plant in which sodium resinate purchased in dry form was substituted for I Rosin. The mater ial is obtained from B.M. Spencer. SUMMARY & CONCLUSIONS Substitution of Sodiiim Resinate for I Y/ood Rosin in equivalent amounts gave a product slightly liglter and bluer than RT- 283-D Standard. A closer match could probably be obtained with more sodium resinate but inasmuch as no new tinctorial properties are given by use of this material, no further work is planned. EXPERIMENTAL DETAILS K.B. 385, p. 120 41549 - 1 mol charge. Std. formula but substituted 165# Sodium Resinate for 150# I Food Rosin. 13# Caustic Soda added to Resinate. vs RT-283-D - s.light; s.blue and s. bronzy. Yield 616# DUP050315482 PIQMSST COLOR RESEARCH REPORT IMPROVES KAROOS TOBER Qg TBS RT-297-D TYPE SUBMITTED BY; APPROVED BYI p il e i BBfr-ssfiaeess SATE t tTABUARY-1935 nriRODUOTiOH A number of samples of regular and purified STaphthanil B.S. were tested for Jackson Laboratory. SUMMARY fe COBCLUSIOSS The samples were tested on the improved formula GS-7S23 and confirmed previous findings, namely that purified 5.B.S. bleeds appreciably less in lacquer than the unpurified material. The majority of purified samples resulted in pigment equal to CS-7623 in white lacquer overstripe bleed. EXPERIMENTAL DETAILS JT.B. 416* fixpt. 38, page 172. H.B* 450* 2, page 10. DUP050315483 PIGMENT COLOR RESEARCH REPORT MAROON TONER RT-399-D SEMI-WORKS SUBMITTED BY: Ul ,V\. W APPROVED BY: PIKE: RDS MAR06NE DATE: JANUARY-1935 INTRODUC TION Development work was discontinued last month until du Pont Naphthanil B.S. equal to General Dyestuff Kaphthol AS-BS can be obtained. SUMMARY & CONCLUSIONS The material produced in the Semi-Works from General Dyestuff's Kaphthol AS-BS was assigned the CS-7782, and later coded as RT-399-D. To produce this standard the Semi-Works batches were mixed and shaded with a master-batch containing Pigment Green B. This compares to RT-297-D as follows; vs deep and bright, better bleed; to CS-7623 deep and bright, bleed equal. EXPERIMENTAL DETAILS RT-399-D. lot 3938. RT-7782-D. DUP050315484 PIGMENT COLOR RESEARCH REPORT ^*--33 SUBMITTED BY: APPROVED BY: RUBBER COLORS - RED FOR LAKE C nN ^ V FILE: LAICS RBB-0 DATE: JANUARY-1S35 INTRODUCTION Further studies were made to improve the dispersion in rubber of the dry calcium toner of Red for Lake C. Some work was also done with the strontium toner. SUMMARY & CONCLUSIONS It was pointed out last month that the diglycol stearate treated calcium toner seemed promising but that the method, 284-30D, had proved to be very unstable. Attempts during this month to render the formula stable were also unsuccessful, therefore, it was decided to abandon the D.G.S. method at least for the present. Drying time and drying temperature studies demonstrated that the calcium toner of Red for Lake C was apparently not affected tinctorially by drying at tem peratures between 60C and 9CTC and by drying for 20 to 48 hrs. Also, subsequent exposure to humidified atmosphere at room temperature had a negligible effect. The observation, made last month, that the calcium toner appeared to be affected tine-- torially by changes in the moisture content, was probably due to tests which were made on an incompletely developed toner. The changes which were observed were pro bably due to a continuation of the development of the toner in the dryer. Comparisons of dry millings in rubber of the sodium, barium, calcium and the strontium toners with their respective latex dispersions were made. The results showed that the dry sodium toner was approximately 40$ weaker than its own latex dispersion, the barium toner about 30$ weaker; the calcium toner about 30$ weaker, an d the strontium toner about 35$ weaker. In rubber the barium is the bluest and the cleanest. The strontium is intermediate in shade between the barium and the calcium but slightly dirtier than either. It was decided to discontinue the study of the strontium toner and to prepare samples of the calcium toner and of an extended pro duct for evaluation tests by the Du Pont Rubber Laboratory. Accordingly, a large sample of the calcium toner was prepared and assigned CS-7804. A lake consisting of 70$ calcium toner and 30$ blanc fixe was also pre pared and assigned CS-7805. The lake showed no color advantage over the toner. EXPERIMENTAL DETAILS Notebook No. 284 Series 284-37 was a study of drying time and drying temperature on method 284-28C. Temperatures of 60C and 90C and drying times of 20' and 4S hrs. made prac tically no difference tinctorially in method 284-28C (calcium toner). Series 284-42 was the preparation of CS samples on the 284-28C calcium toner and a lake consisting of 70$ calcium toner and 30$ blanc fixe. The toner was assigned CS-7804 and the lake CS-7805. The lake showed no improvement in dispersion in rubber over the toner. Series 284-40-43-44 were studies on the effect of varying the pH of strike of the diglycol stearate treated calcium toner. One experiment indicated that in rubber an alkaline strike gave improved dis persion in rubber. A series on variation in the degree of alkalinity showed a marked DUP050315485 2 improvement in strength by oil rubouts at a pH of 10.0 but in rubber the high alkaline run was -weak. Another attempt to-match this product was unsuccessful both by rubout and in rubber. Series 284-38 & 41 were studies on the strontium toner. The strontium toner is dark and blue and some-rfiat dirty compared with the calcium. Striking at the boil gave darker, bluer and weaker colors by oil rubouts. In rubber the results were not in line. Diglycol stearate gave no particular improvements. The addition of 20^, 20% and 4-0% blanc fixe gave only a slight improvement in dispersion in rubber. Series 284-39 compared the dry milling in rubber of the sodium, barium, cal cium and strontium toners with their respective latex dispersions. The dry sodium toner was about 40^ weaker than its own latex dispersion; bar ium - about 30^; calcium - about 20%\ and the strontium - about 35j. In rubber, the barium toner was the bluest and the cleanest; the strontium toner is intermediate in shade between the barium and the calcium, but dirtier than either. ........ DUPO 50315486 J2T-^ fj-- PIGMENT COLOR RESEARCH REPORT PIGMENT RUBINE TONER RT-359~D SUBMITTED HVPILE: APPROVED BY: I BAT3: ^3 <"Y . v la&^TTYTNSS JANUARY-1935 INTRODUCTION Production of this toner was resumed in the Semi Y/orks to fill orders and to build up stock. Seven batches were made. Variations were made to obtain material on both blue and yellow sides of stand ard. Two batches were made in a trial of ohlormetanilic acid supplied by Chemical Mfg. Co. Tnc. as a solution of the soda salt. SUMMARY & CONCLUSIONS A mix sufficiently large to fill an order was made up by shading substandard stock with a dark blue batch. This type of material was ob tained by striking the toner at a lower alkalinity adjusted by addition of acetic acid after coupling. A lower temperature of strike (155 instead of 170) added to blueness of tint but did not give the corresponding depth of masstone. This 'out of line' relation of top and undertone occurred in the rest of the series. At equal or even slightly lighter depth the under tone and tint were somewhat bluer than standard. An increase in the amount of soda ash used in the coupling to gether with a higher strike temperature lightened the masstone but did not make the tint sufficiently yellow. Use of Turkey Red Oil instead of Para Soap may have a slightly beneficial effect in obtaining yellower tints and should be tried again. Treatment of the finished product by redryin:: at a higher tempera ture (190P) and by exposure to humidified atmosphere was tried. The former increases depth and blueness although the change in tint iw great er than the change in.depth. The latter treatment results in a slightly lighter yellower product. Other batches will be .treated by this method in order to obtain a blend from the material made". Soda Salt of ohlormetanilic acid in solution gave products of less brightness than the intermediate used at present. Both batches were dark and muddy compared to standard. An increase in alkalinity of coupling did not make sufficient difference. Use of this type of inter mediate for making 1T-359-D is not very promising. However, it may be suitable in extender colors such as R3-6857-D. DUP050315487 EXPERIMENTAL DETAILS N .B . #298 if Ss Oin rH Off m tO m C* HH* CM m 9 t- H O to CM CO to d -p d iH GG H r4 f & x> s iH 43 2 43 d s H > 43 * s* p 5+a u -p u <p V^ CO O U -P J* Jh -rPa fPa bd > o d iH 43 12 > > u Jh *p *P G cd d rH < <* rH d H H XJ G 43 rH G 43 2 O ds 43 iH 43 0 u -p d rH 43 > P >> * CmO .H Tf m > V(Di MXUfiIj 44 x* ^SU ddG <rHH S *3 XJ 8 *p tn H > >* Xxsd SP i-H * t3 j Vw. aE * (S T3 XJ 44 E X3 i4H> n P. 4C3O 4a3 OH 43 A to s Vi d hGO rt O QOm 5 H +C/33 6,,t O oo o -0P< *H o + XoJ TJ XJ cd g O 43 s o CO a * cd Joh *GH, Jh co Sgh dofo ' xcOd* *ori 3 cd u o ^ -o&p tCOM o *p o 0> rH dc .p Pt Jh +3 tPf +> -S P, P. (D O <D <: O 03 5 +s - V* >. a cd p G Jh u >* & C/3 e*J a* g G o Ov rH X O -P X5 X P X O &4 X X O x <S O ri o3+ cd d > Oinff Vi O rH G P d J3 H O in 03 u3 m HCM* a Vi P O H in o Or X -P in Sz* X* to cd G s Jh H & m o c- H OJ m CO CM O %o J Vi B rH d S X* dB cn Jh V & s o rH o> M t- X B O Vi xd *H VO P CO 0 i JOh -P o Vi & o o V -p rH ID e O, G rt _CM G \ *H rH XJ O 44 Sh Vh 44 44 a m c Cd *r-i Jh H TS "O xJ 44 Jh a o h u U o 1 P 43 H a s * 43 G V CM 03 O pG o Jh &d in O Jh CM rH S rH O 43 o o 2? O in CM s o CO CM rH o rH ft- oo s H X5 Jh o sd V fH fo XJ CMO 00 g * lO Ok 3 < rH G CO i-B o -p c- rH CO fe O CO Vh XJ m xj << rn iD fi oa CO X* s2 ! s* c r le f `W c- o o O S 1 +9 Jh to o g Jh XJ 5 PL, 3 &2 M 63 to co o CO CM CO in o ferH CM feCM in CO CO ov rH rH -p M3 fe~ C- fe- c- fi- fi t> o to to to to to to to le to h 4 <4* to <n CO -p o h3 * K '< '. art DUP050315488 SUBMITTED BY APPROVED BY: FIGMENT COLOR RESEARCH REPORT MAROON TONER - RT-354-D 3s'- FILE? 4fiSCT-TeNESS" DATE: JANUARY - 1935 INTRODUCTION: Three additional batches of CS-7685 were made in the Serai-Torks in an attempt to obtain greater brightness and to check previous results* A slight increase in fine ness of pulverization was tried. SUMMARY AND CONCLUSIONS: All the material made was slightly lighter and duller than the batch made last month. This includes a check run on the same formula. Closer duplication might be obtained by use of more Pigment Green B. Replacement of sodium acetate and increase in amount of B.O.N. from the theoretical amount used in theCS formula to a 5% excess gave no improvement. The first variation was tried under abnormal operating conditions and the result is not conclusive. An increase in grinding speed from 3300 to 4460 R.P.M. had only a slight effect on fineness and none on depth in laccjuer. Grinding at the lower speed gave prod ucts grading from 93 to 99^ of SO mesh fineness. EXPERIMENTAL DETAILS: Notebook 3 51, p. 42. SW-6649 - Check 6577 except add 12.5$ sodium acetate to the B.O.N. solution. Lot 3918 (ground at 3300 R.P.M.) vs RT-354-D - s* light & muddy Lot 3919 (ground at 4400 R.P.M.) vs RT-354-D - s. light & muddy SW-6666 - Check 6577 but increase 3.O.N. from 47.5 to 49.5# Lot 3923 vground at 3300 R.P.M.) - si. light & dull Lot 3924 (ground at 4400 R.P.M.) - si. light & dull. SW-6672 - Check 6577 Lot 3925 aground at 3300 R.P.M.) - si. light & dull Lot 3926 (ground at 4400 R.P.M.) - si. light & dull U. DUP050315489 PIGMENT COLOR RESEARCH REPORT PEACOCK BLUE BL-151-D 5^. SUBMITTED BYs \-ekM, / . APPROVED BY* PILE: MI&&v--5S3&~ DATEs JANUARY-193 5 INTRODUCTION Work on this color during the month consisted principally of plant production using humidified drying. A few miscellaneous lab oratory experiments were run to complete the study started last month. SUMMARY & CONCLUSIONS Modifications of the standard formula which were studied in the laboratory were as follows: 1. Tripling the dye volume before adding to base showed no effect. 2. Heating the base to strike temperature before adding the dye showed no effect. 3. Use of a small amount of Duponol in the dye solution gave weaker but greener results. This product does not disperse well in rubber. 4. The stronger lakes show less rubout change on drying than the weaker lakes Humidified drying of this lake in the plant as reported last month continued to give satisfactory results. Ink mill grinds and rubouts showed satisfactory quality and the yields averaged 113$ of estimate. The drying temperature used was 140P at 40$ relative humidity and the drying time averaged approximately thirty hours. A satisfactory blend totalling 728 pounds has been made using one of these recent batches together with a quantity of red and dirty sub-standard material. Ink mill grinds and rubout results on the last series of plant batches will be found in Tables I and II and the composition and rubout results on the plant blend made will be found in Table III. EXPERIMENTAL DETAILS 440-17 A. BL-151-D. Control CS-7633 B. As A but dye volume before adding to base increased to 3 times formula size. (300 cc instead of 100 cc) C. As A except base at 110CE when adding dye (instead of 80rP), cooling to 110P. if necessary, before strike. D. As A except 1.9 gms. Duponol added to dye solution before adding to base ( =o= l/2?f Duponol for plant size formulation) . Rubout Results: B vs A: C D n * C vs B: D vs B: OK- OK- OK- OK OK- OK- v.s?str- vvs red s It- green- vs wk- green OK- OK- vs str- ws red s It- green- vs wk- green D vs Cs s.It- green- wk - green DUP050315490 . *1 2 A vs BL-151-D Std: B" * C * 3) * dk- atrn * *n atr H - red * f t s red & clean Rubber Test: 440-5-7D versus BL-151-3) Std. and BL-143-D Std* 440-17D showed no improvement over BL-151-D Std. in rubber* Neither 173) or BL-151-D Std. disperse as well as BL-14S-D Std. in rubber. 440-26 A. BL-151-D control CS-7633; 4 gms. dye - 3.45 BaCl2- 1.7 AlsClg B. As A except 5 gms dye - 4.31 BaCl2 - 2.12 AI2CI6 Rubout Results: Red wet B vs As dk- str- str- red & dirty A vs B1-151-D Std: It- wk- wk- vs red & clean B* * dk- str- red, vs dirty Tints read dry B vs A: vs red & clean A vs BL-151-B Std: red & dirty B* red. s.dirty #- rl-sS-f- DUP050315491 >* t rl to >I T? s^ ? S ft m P p33 *> <n q uC9D <cOD s99 PCIN S> P3O P&9 7Zq33 t9j id 9 > a9* *mq4 M793 id IS 03 > 7S93d C>D g 7P>UH3* TuBS c i uu pp 99 7U93 79l3*#v id p9 = id pto CQ *g --O4 OB > id P id p9 3 CO ca ta 35 35 tn 35 sa 2P CO 8 o o ^3 Q o Od >^ Or OO 7ft * CD * 9 9 9 M 13 9 1 U 1 ti 1 i 1 S * fa 9 r E&. E* U3 > 9 C3 O o oo > CO ) tO ) CO CM o CM O 3 44 U CM rH rH rH ^*1 * rH -H 9 73 73 73 73 TJ a 9 P <D P 9 P 9 P 9 p 9 H 9 H 9 rt 9 rl 4 H 9 fltf h ia PPPQ g 3 CO 3^ CO 9 H 1= >* P CD SS &5 CO m 3* rH 4 o CM <o co 3 CO X ID SI > CM CO oO CO CO 1ft to 3 ir> rH O o1 CM o o CO 3 65 t/i m <o m d* <o CM CO s 9 ft CM X .*"* * > 9 9 73 9P 33 sO g s arH rH * CO CM i 3 SJ 3 33 3 X! rH CO 4! 9 10 3 CO n oP H iH CM CM 9 rH rH rH rH S3 d4 d* d* s|* 7ft uQ i9* P<O9o Po p-H P -Hf5t* P7993 S9< Pd P P <90 2h W Sr3f 7993 P9 t K HTx99Ji o iod iOd iOd oX Xo * 3 g s Pl S3 rl l iod rtH>* 49c U bO Po * 3 i PCi*O t f9at i Pid iOd p9 CQ Id PCO CD 9 > 999 C9Q sft PmH >U<P9 * w rPrll 1 t fl O 73 pL9. 1 1 IoSpft >* 499P4 PO P9* HO MP 5bH40 9 79id3 X4bH?O 79V3ri P9 ti9dS a > CQ > fCtD* a> CO > u i, 73 49 CC Ubr0l U9CD 5 3os P 7ft 5, CO 3 P OL 3p q rj #; r* OP3 3 83 m P Cm P CM CM CM CM 9 9P P <4* P n n HM H aw an 9 i? P l>~ CH n p om P in ^ p Ii id o rH O 9^ XI fi t c m1 P P1 xl oX X X X O Oo 9 > > 73 O1 23 >> ft ft > P4 M xt 9 9 r* O 9 XJ 9 9 -9 9 & 49 9 9 > XI >" % m 9 g,E O a 3*3 S3 9S m mo Oo id CO p p CO CM CM 9o > p < CM 7ft * m P CO O CM CH O CO n ** !J Tl 2: P 3 e 8 ti g mn o3 oS % in S3 -H p p CO n CM 7ft rl Sr 9 i. U3 X <n p p 7ft P CM DO O p P P &** Sr 9 99 P rH 9 b0 bd 9C 03 *rl id 9 P 93 l n 8 n ot 3 m 4* O P -- * CM P "--4 n p p CO P CM > 73 P W P n P CO 7ft a* P Ol TO 3* CO n P fr* P P CM CM o OPPPP p 2a 7ft tft tC9h3 >8 p>% .T&3 9 > 4<If u/ > I Pq P9 P9 P aO 9 > Si | id 9 9 ioon P jQ 7ft b rH TJ 73 9 > P XJ TJ Ps 1 P n p i p 35 3ft 1ft Ho CO o; to !> to CM O CO CM a i p n rH 4 CO s CO CO p 9 GO n tO > rt P CO CO P P o CO 9 P 7ft 7ft p P 9 <#* 9 noo O td *ft O.JS TJ 9 p aO p >> P oo P t o 35 9p Pp ss o as 9 9 p S3 P 9 sh p pp n si po x P9 25 2J DUP050315492 PIGMENT COLOR RESEARCH REPORT VIOLET LAKE BP-69-D SiT-AI V1 a SUBMITTED BYs APPROVED BYs DATE s JANUARY-1935 INTRODUCTION Because of the difficulty experienced by the Semi Works and plant in matching BP-69-D with present shipments of Helio Past Violet AL. all the shipments giving too red a product, work was started in the laboratory to discover a means of securing a bluer tint on this color. SUMMARY & CONCLUSIONS Board mixes were made in the laboratory using as a toning color a Semi Works lot of BP-79-D.'a lake containing the same type base as BP-69-D with a blue rather than a violet dye. Five percent of this blue lake was sufficient to tone the red Semi-Works lot of BP-69-D to practically a match for the standard. A small mix of these colors was sent to Fairfield for their approval. Meanwhile an attempt was made in the laboratory to natch the BP-69-D Std. using the dyestuffs as used in the above mix rather than using the prepared dry colors. Strikes were roade using these dyestuffs, Helio Fast Violet AL and Anthraquinone Blue 3, and a board mix was successfully prepared using these products. On grinding and screen ing a larger mix, however, a loss of + 5$ in strength was obtained which will be adjusted for when another mix is prepared. From these results it appears that this is a satisfactory method of toning the subject color when a bluer tint is desired. EXPERIMENTAL DETAILS (95$ BP-69-D lot 3297 Initial Board Mix ( 5% BP-79-D lot 3915 vs. BP-69-D Stds s.dk - vvs dirty - vvs stx - vvs red & dirty 440-30 A. As CS-6978. 3P-69-D except use 95% Helio Fast Violet AL and 5% Anthraquinone Blue B, thus 14.82 gins . Helio Fast Violet AL - .78 gms. Anthraquinone 3lue B. B. As A using 10$ Anthraquinone Blue B and 90$ Helio Fast Vio let SL. ^ C. As A using 10$ total increase in dye and using 8$ Anthra quinone Blue B instead of 5% as follows: 14.04 gms. Helio Fast Violet AL and 1.37 gms. Anthraquinone 31ue B. Rubout Results: B vs A: vvs red- vvs wk,bl - vvs wk - bl A vs BP-69-D Std: deep - red.vs str - vvs wk - red B" * * vvs str,vvs clean - s.wk - s.bl C* " dark ----------- s.str - str - vs bl,vs dirty (33-1/3$ 30A x Board Mixt * 303 (* 30C vs BP-69-D Std: s.dk - vvs dirty - OK - ws dirty x Note: A large check mix lost approximately 5$ in strength when ground and screened. DUP050315493 PIGMENT COLOR RESEARCH REPORT Jj'- X& ^0 ZINC SILICATE ^ SUBMITTED BY: C.5.?i*v) APPROVED BY: PILE: MISC, LAPS&-- DATE: JANUARY-1935 INTRODUC TI ON During the last few months a number of experiments have been run to determine the possibility of preparing a zinc Silicate base suit able as a substitute for Alumina Hydrate in lake making. (Ref. Paint Manufacture 4. 240 (1934). SUMMARY & CONCLUSIONS After a number of unsuccessful experiments in which the product was a hard, semi-transparent mass which would not break down it was found that the best result was obtained when the strike volumes on the Sodium Silicate solution and the Zinc Sulfate liquor, the raw mat erials used to prepare the Zinc Silicate, were kept as low as possible. The resultant product broke down easily to a fine but hard and sandy white base. This strike would be difficult of manipulation in the plant because of the fact that the base slurry formed is so thick as to make efficient agitation almost impossible. On preparing a Scarlet Lake and a Peacock Blue Lake from this Zinc Silicate slurry and comparing them with lakes made in the same manner from Alumina Hydrate it was found that this zinc Silicate was practically non-absorbent and gave very weak lakes. Prom these results it would appear that this type base is unsuitable for lake making al though further work may develop a more absorbent, softer base. EXPERBQBNTAL DETAILS For orientation work on Zinc Silicate see 417-86 and 88 For Zinc Silicate used in preparing lakes see 440-13. 440-21 A. Scarlet 2R lake from Alumina Hydrate (30:15 washed base) B. * * * '* Zinc Silicate (washed S04 free) Rubout Results x B vs A: dk- bl. wk- wk- bl x Note: Apparently only reason that a c.olor was secured was that the Scarlet 2R was precipitated as a toner and extended with the Zinc Silicate base. 440-23. A. BL-72-D control using Alumina Hydrate. B. As A substituting Zinc Silicate for Alumina Hydrate. Rubout Results: x B vs A: practically no color to B A vs BL-72-D Std: It- clean- vs wk- green & clean B* * " practically no color to B x Notes As this dyestuff does not precipitate as a toner the resultant rubout on B of this series had only a faint blue tinge. DUP050315494 PIGMENT COLOR RESEARCH REPORT GE-363-D & GS-364-D JS-J-f ;/ SUBMITTED BY: APPROVED Bit y. PILE: WATER- COLORS'* DATE: JANUARY-1935 INTRODUCTION Work was started during the month in an effort to improve the cleanness of tint of both of these colors versus their standards. Recent plant batches have tended toward dirtiness in paper coating tests. SUMMARY & CONCLUSIONS In an effort to prevent the dirtiness caused by the decomposi tion of Auramine when dissolved at high temperatures as in the GE363-D formulation a strike was made in the laboratory striking the dyes separately on one-half the formulated amount of clay, dissolv ing the Auramine at 110"P instead of 180 P, the Victoria Green being dissolved at the formulated temperature. These slurries were then mixed to produce the finished color. No apparent improvement in tint over the control was effected by this variation. Variation in pH of the clay slurry before addition of the dye was then tried on both the GB-363-D and GE-364-D formulation with the results showing that the use of a neutralized clay slurry. pH of 7.0, gives the brightest and cleanest results. This point will be checked in the Semi-Works in an effort to solve this plant problem. BXPERIM3NTAL DETAILS GE-363-D 440-22 A. GE-363-D control. B. Materials and weights as A but strike Victoria Green and Auramine (dissolved in full formulated amount (600 cc.) of water at 180rF and 110F respectively) separately each on one-half the amount of Dispersing Clay (100 gms). Stir each 10 minutes, mix the slurries, stir one-half hour and filter. Rubout Results: B vs A: It - OK-- OK - vs yel A vs. GE-363-D Std: It - yel.str - str- yel 23 # * it w 440-36 A. GE-363-D control Pii= ( s B. As A except add C. gms. Na2C0s to clay before dye is added pH=9.3 HC1 lOOfi pH= 7.1 D. " 5 gms, " 11 pH= 2, Brushout s i B vs A: It,vs yel - OK - vs yel D dirty - OK - dirty C vs B: brt - OK - vs clean D" olive.dirty - OK - dirty D vs C: H * tt C vs A: It & brt - OK - vs yel&clean _ All much more olive in full strength brushout and yellower in tint than GE-363-D Std. DUP050315495 4^ 2 GE-364-D 440-28 A. GS-364 control CS-7349 B. As A except add 5 gins KffiOH 28% to clay "before dye c. n " HaHCOs " W D. * IV 2 gins, soda ash " " II E. M " caustic soda n 11 E. G. * n " acetic acid 100^ " it " muriatic acid " " n n Brushout Results: G vs A: Tort - OK - vs yel&clean A vs GE--364-D Stds lt&brt - s ,wk - bl,v3 dirty B" G* u dk - wk - s.bl vs brt - vs wk - bl D It " s .bl E* E" G* tt lt.wk.brt - wk - s.bl VI brt - -s.wk - bl n aa m D vs A: dk " VVS str - s.yel,vs clean * G vs D: brt - TVS str - vs yel. pH= 8.1 is added " 9.5 It II " 8.1 9.1 n " 11.1 n " 7.5 u " 7.1 DUP050315496 sf-30 C3 PIGMENT COLOR RESEARCH REPORT SUBMITTED BY APPROVED BY: INTRODUCTION GREEK LAKE GE -388D CS7682 n1 PILE: WATER COLORS DATE: JANUARY-1935 One Batch, of CS-7682 was aa de in the Semi Works. This is a lake of GE-353-D type having better flinting properties developed for Louis de J onge . SUMMARY & COYCLBSI PITS A 100# shipment was made to the customer. The product was very slightly yellow and dirty compared to standard. EXPERIMENTAL DETAILS . IT.3. #309. p. 40 SW-6725 - 0.12 X CS-7682 Brushout vs. CS-7682 vs dark, s.blue - Elinted vs dark, OK s .blue ws dirty s.blue . DUP050315497 PIGMENT COLOR RESEARCH REPORT S<3/ R5D LAKE FOR WATER DISPERSION - RE-381- 3 TYPE & C4- SUBMITTED BY: '/ twf-Z**^^**1--* APPROVED BY: PILE: CCUJORS^EDRD^ATER^^ DAL']: JANUARY-1935 INTRODUCTION This report covers the experimental work done on this color since October 1st, 1934. The problem involved the matching of C# 36452 submitted by Louis de Jonge. SUMMARY & CONCLUSIONS The experimental work continued varying the dye proportiais in the formula for RE-381-D, but the results failed to show the brightness characteristic of the C#. The addition of Crocien Scarlet Cone., re placing part of the Scarlet F.P.Y.. seemed to be necessary in order to approach the hue of the competitive color, but in itself was not suffi cient to procure a substantial match. At this point work was reverted to experiments with the substrata. At first the original dye propor tions were used, omitting Crocien Scarlet Cone., and all of the China Clay was replaced by Blanc Fixe. The result was a brighter product, but too light and yellow. Using the new substrata, Crocien Scarlet was again introduced, and with quite favorable results. Temperature of strike variations were then tried on this new formulation and it was found that by using a lower temperature the brightness seemed to be consistently retained. A sizeable amount of the color was made incorporating thesg variations in dye- substrata, and strike temperature, and a sample was submitted to Louis de Jonge under the CS;?7802. EXPERIMENTAL DETAILS 417-59. Check to RE-381-D but using 100.0 Scarlet f .P.Y. dry basis 174.0 Orange II 60.0 Crocien Scarlet Results: vs RE-381-D v.s. blue & bright 417-61. Check to 417-59 Results: vs. RE-381-3 v.s.yell - equal vs. C$36452 " vs dull 417-75. Check to 417-61 except using 90.0 Scarlet F.P.Y. dry basis 70.0 Crocien Scarlet Cone. Results: vs. RE-381-D vs blue - vvs dull vs. G4 36452 vvs blue - vs dull 417-76. Check to 417-18' except that all China Clay replaced by Blanc Fixe. Results: vs. RE-381-D yell - It .- vs bright vs. C$36452 " " equal DUP050315498 ^jr 2 417-91 Same as 417-76 but using 90.0 Scarlet F.P.Y. dry basis 70.0 Crocien Scarlet Cone. 174.0 Orange II Results; vs. KS-381-D vvs blue & bright vs. C#36452 vs It - bluish - vvs bright 440-11. Same as 417-91 but striking at the following tempera tures: A 120 F B 150CF C 170 3? Results: AhvsIB: a.It - vs brighter B vs C: vvs darker & brighter A vs RE-381-D vs brighter B vs M vvs brighter G vs . " s. lighter A vs C#36452 s.dark - vvs brighter B" it n G" " vs- dull 440-24. Check to 417-91 except using the following temperatures: A - 80 CF B - 100F G - 120F and 1000# BaCl2 used instead of 950# Results: A vs 3 - ws dark - trace bright A vs G - s.dark - vs bright B vs C - ws dark & bright A vs RE-381-D - s.dark - vvs bright B" " vvs dark, vvs bright G " vvs light A vs C#36452 dark - vvs bright 3" " s.dark - vvs bright C" " vs dark - 440-29. To prepare a 03 based on 44G4B. Results: vs RE-381-D vs It & bright - vs blue vs C#36452 OK- trace bright & richer The formulation, 440-24B. differs in the following respects to the original RE-381-D formula: 44% of the Scarlet F.P.Y, dry basis, is replaced by Crocien Scarlet Cone., All the China Clay is replaced by Blanc Fixe, and the original 31ane Fixe retained; Strike temperature 100CF instead of 150"i7 and 1000# 3arium Chloride used instead of 950#. DUP050315499 SUBMITTED BY: APPROVED 3Y: PIGMENT COLOR RESEARCH REPORT Chrome Greens - Strong Type CS-7192 <A. 6 -S / tj~ FILS: CmQIS-JMaSWSDATE; JANUARY - 1935 INTRODUCTION; Two batches of CS-7192 were made in the plant to obtain material for use in mixes. A modification of the formula used last month was tried in order to obtain the proper relation of masstone and undertone. Two batches were also made in the Serai-Works to determine the effect of dif ferent rates of agitation. SUMMARY & CONCLUSIONS; Both plant batches were olive. In one batch only part of the yellow was shaded. A 50>t reduction in amount of soda arsh may have contributed to the oliveness but the main cause ms probably the redness of the blue in one case and poor agitation on the other batch. A sprinkler was used for addition of the bichromate and the standard amount of tannic acid was employed. Results of the semi-works batches indicate that good agitation is necessary to obtain a bright masstone. A reduction in speed from 25 to 10 R.P.M. gave an olive product* A further study of this point is being made but in the meantime efforts will be made to obtain the best possible agitation in the plant. EXPERIMENTAL DETAILS; Plant - Notebook 437, p. 8. Semi-Works Notebook 436, p. 11 Lot 41520 - Like 40846 {Dec. Report) except use only 67^ Sods. Ash and add bichromate thru sprinkler* Use new lot of Tannic Acid RMC-71S. Blue Liquor MK 6 (greening test- s It, olive, dirty; vs dirty. VS CS-7192 - vs light, v. olive; yellow & rusty. Lot 41610 - Check last but increase soda ash to 12 lbs. as in 40846. Agitation poor. Pressed out as yellow. Lot 41647 - Part of 41610 shaded. Vs. CS-7192 - s dark, olive; blue & dirty SW-6731 - Check SW-6501 using new lot of tannic acid RMC-718. Agitation - 25 R.P.M. Vs. CS-7192 - vs It. <fc nrt; vs blue; O.Kt vs blue & clean SW-6745 - Check 6731 but reduce rate of agitation.to 10 R.P.M. Vs. CS-7192 - s olive; s blue; vs strong; s blue DUP050315500 St t bmITTED BY: APPROVED BY: PIGMENT COLOR RESEARCH REPORT RAW MATERIAL TESTING / V^5 ' >* PILE: CR-2 DATE: JANUARY-1935 The two items indicated as unfinished in analysis and test last month, have been satisfactorily reported. This month 82 shipments of raw materials were received and sampled, and have the following status: 27 tested in the laboratory and found to he satisfactory; 5 OK in the plant; 8 awaiting report from the Analytical Laboratory; 3 whose testing is incomplete; and 39 reported without test. RAW MATL, SAMPLES There are no samples outstanding from previous reports. Pour samples were received this month. RMS 1373. Green Earth from m. H. Mftller; unsatisfactory, poor disper sion. RMS 1374. Patent Blue A Ex. Cone, from General Dyestuffs Corp. Unsat isfactory - weak RES 1375. Erio Glaucine A.M. from Geigy Co. Satisfactory RMS 1376. Lithosol Brilliant Blue E from du Pont - satisfactory. DUP05031 5501 PIGMENT COLOR RESEARCH REPORT cy SUBMITTED BY: APPROVED BY: SEMI-WCRKS PRODUCTION ft1 PILE: OR GOO DATE: JANUART -1935 INTRODUCTION 95 batches of 20 different colors were made during January; these included 9 batches of RT-359-D, 4 batches of RT-265-D, 22 batches G-317-D, 9 batches GT-68-P, 9 batches of Y-315-D, and 10 batches Y-359-D. S TOMARY RT-359-D, Pigment Rubine Toner - Nine batches were made for pro duction of stock. RT-265-D, Calcium Duol - Pour batches were made for production of shading material. RT-7685-D- Maroon Toner. Two batches were made in development of this more finely pulverized product. RL-360-D Ext. Alizarine Lake, One batch was made to fill an order. RT-126-P, PTA in pulp form. One batch was made for use in prepar ation of finely dispersed pulp by pulverization. Y-315-D, Primrose Yellow. Nine batches were made in development of an improved formula. Y-359-B, Med. Yellow . Ten batches were made in study of the process. G-317-D, Milori Green. Twenty-two batches were made in develop ment of a Lightfast Green of the Hi lori type. G-7192-D, Strong Meadows Green . Pive batches were made in fur ther study of this process. G-7694-D. Lightfast Green. Pive batches were made in a study of the process. GT-68-P, Pigment Green 3. Nine batches were made in a develop ment and process study. GE-7692-D, Ext. PTA. One batch was made to fill a trial order for this improved GE-353-D. B-57-D, Milori Blue. Three batches were made in a yield study. B-63-D. Chinese Blue. Pour batches were made in a yield and process study. B-66-d Milori Blue. Two batches were made in a yield study. B-7469-D. Opaque Blue . One batch was made for use in emulsion treatment. 33-149-d , Ext. PTA. One batch was made for production of stock. 3kL-6618-D Treated Black. One batch was made for Parlin. BkL-6619-D Treated Black. One batch was made for parlin. Sixteen mixes were made during January 1935, for the plant, in the Semi-Works. Mixing Charge Batch lbs Red Toner 751 s 1 130 PTA TONERS 751 s 2 482 Extended Greens 752 s 2 324 CP Yellows 753 s 5 1772 CP Greens 755 s 5 1983 CP Blue 756 s 1 100 16 4791 DUP05031 5502  tit 0 {J ' O O O -) JH H3> 1 a O~f o--i p0 o3 o0*p* AS O 2 Crf j~t. a,. MH cff 0 H^ 'O-O HO Wro N'-ft noO'rtO P O tjt POP Mj --* --*-*** f t #1 wrH --0oI 5*a.nH0^>~o0--O* 0--OJ 0*CH 0rWH0rHO0HOHH3VJHQ|JOrl2> <-H 0 t t H Cff 0 Cff M 8$ s BONNinOWH(3^ id w fn 2 <0 n en *<o TQi rH Cff rH Cff rH f 30 Cff ro o3 -Q iH P: . <05 a; o' 22 o MS u |/>WO>*-(OOWO o OHcnMW'O2C)f0?Q'OH?0C0 r-l ,-J mH Cff t H w H 02 m| fO CO W ro rH H <D 3 0 rH Aa C3 aa Q CU Q Q aa a 1 f 3 1 a, 1 1 1 Q 1 Q 1 1 s 1 } l 1 1 1 1 m -n t -O 1 n 3* a t =3 n < <0 1 *t Off 1 0 3k <0 n t Cff 3k 1 m 1 3k n <0 vo Off 55 Cff 3k & 3k 1 Ok uo vo (W 3k 3k n ro H ro <0 1 ro ID ro 1 H ro n so CO iD <D sO tfff 11 VO e- rH CO fc- t m CO 1 vO t- rH 5-- rH 0 n JO Off H 11 ro rH t-. VO O m es CO i rH b- 10 fts. ast t &M l C-h 1 1 1 1 Eh e-< 1 &q 1 - I | 1 1 Em =h w 1 t f 11 >H >* at: >< >* 33 O CC O CD 5m ac: 5m >H Q5 a: 0 C3 O > * as Off ro CO CO CO in co ?o i> CO cO no 00 0 rH Cff t CO t St1 in t t fi- 00 t 3> t O n rH UO Off (JO co in aS n n V0 n O n 00 nm 0 VO rH vO ?- O fc- t- O vo *0 VO 0 rH cd P O c- n CO Ok rH HI - -?M 3* Ok O oo^cooo O cc 1 <rf 3 CO in 3k fr- Cff rH * <n *H CO Ok 1 JO CO rf* 0 Ok o> rH vO 0 tJk JO 3k O !> r-H rH rH 00 VO n JO VO 3} sf D O T' O O OD 1 H i/> a) ift *1 1 3k a> CS2 3> Jk 3> vjv 3 co O sH 3k n co j> n o_ ift O <ft O H W rH rH rH rH rH rH 0 30 rH <4 -3 pSd CO Cff rH V0 Cff rH m0 rH Cff CQ co rH !> CO <n CO CO O erf rH rH h S| rH a, Cff in m CO CO <rf rH CO CO rH n CO CO rH rH rH rH rH rH rH rH 6* CO VO en as !U a 0M O n r g o CO w Oh O O Cff in VO 3 0 Cff O O e- O 0 0 U- OQO ro&q ss Cff ?> Cff CO rH CO O* CO VO CO Cff t Cff CO O 00 CO Cff CO co as J2 rH p H 'rf rH r-f rH rH 1--I rH rH rH rH I H rH p rH CO aq 35 CO 0 p * a aM * a. rH &4 3 n O a a a a 0 rtW>rlm!<l in rHas 0 0 a PH t rH rH Q rH a 1 3k vO CO 5^ t> ^ JJW n vO to > rH 0 in e- *0 rH JO in t- CO O aa aa a a, a *? s* ? -HO? a m rfv n O t m 1 nn 1 t- I co I in a 1 51 in 3> I <o t* 01 Q w1 ri :W 3>c j 2* rH rH rH CO rH CO rH CO H Pl < in t> ro rJ CO 'D CO CO m CO 1 CO CO n t CO CO 1 00 10 t 1 i*> 1 .16 3 <n O' t fiM M Pm Ch 1 w H1 < PH 1 E-i t IEh HIEh IHI I PXMttJPPai P><P >4 33 n p >M 3* X) 0 as O a as >t as O ^iftD&COOOHH ri rff 0 3k CO 3> O rH OO Cff O CO 0 O tn VO 00 3> O O rH rH Cff CQ rH rH H <* m rH rH rH >* rH P o rH rH O Cff VO c- fr* t- C- C- H <0 3 VO 0 33 O n Ife- 73 rH O O Cff trfv vn O O 0 VO n * O 1 00 rH n O CO Cff 0 n rH a t> rH HI O Cff rft H O O Cff O sjv rH Si -rf* H vrf* x> Jk >+ rH rH O p rH 00 rH rH O rH O rH O rH CO rH 3 Pd (0 O r rH Jk m m h * Off off n Cff 0 0 0^0 rH rH co<cjmocofr.aoooi>PooicocaMioojcooo^d*in Cff0CO0>-0<ffCff:>^00 0tf>0flff^0fffE'-0Cff:O0>*tfffCff-H At O ro O 3 0 0 n nO or 3D l> e- O fr* co CO rH t> Cff O p H 0 O O 0 t> C- !> c- 0 Cff Cff co rH co JO *t rH 33 rH er 02 rt JO co CO rH rH CO CO Cff t- rH ro CO CO n rH rH Cff rH JO JO Cff rH 0 rH CO Cff 0 0 0 rH Cff 0 rH rH S rH <E> O a rH a, 3m 0+ a. o, t a3G| | Q cq a a a a a a aO Q n Q rH a n rH a 1 rH Q rH n 0 p H rH a03 O O Z* 1 n *. H H a ro JO N. rH fr0 rH m 0 H* O Si > H t rH s 1 O 62 n n tow t t- n H co rH rH CO t- rH 01 6- rH S 0 &- t- m 1 00 co l CO "l co JO JO CO ro co 1 JO ro 1 t CO .1 0 Cl> *M 11 c m -M rH 1 "l 1 9h * *7? Pm &H t &H T At t * M *0 3S P ^3 M a -3 M M 3S P 2 P aa p IW a Cff 0 2; i Cff .O n !> g rH Cff CO t r> O 0 O 0 -O b 0 0 0 N. O 0 rH 0 Cff 0 JO 0 t 0 n 0 0 t* 0 0 0 0 0 rH 0 n 4? vgjfry DUP05031 5503 3 SU10IART OF #10 BLDG. PRODUCTI OF REPORT FOR JANUARY - 1935____ Fo. Batches. Code lbs . S truck 9 RT-359-D 827 4 RT-265-D 944 2 RT-7685-D -280 1 RL-360-D 130 1 RT-126-P 5 9 Y-315-D 235 10 Y-359-D 320 22 G-317-D 2169 5 G-7192-D 834 5 G-7694-D 175 9 GT-68-P 254 1 GE-7692-D 126 2 GE-364-D 198 3 B-57-D 360 4 3-63-D 471 2 B-66-D 240 1 B-7469-D 78 1 EB-149-D 900 1 BkL-6618-D 17 1 BkL-6619-D 15 8578 lbs. Packed 818 972 281 130 5 240 307 2028 836 155 258 121 179 352 484 250 78 896 16 14 8420 % Yield 97.3 103.1 100.4 100.0 100.0 102.0 95.7 100.2 88.7 101.6 95.7 90.4 97.7 102.7 104.1 100.0 99.5 94.1 93.9 98.9 DUP050315504 MATERIAL TRANSFERRED DURING JANUARY 1935 - RESEARCH SEMI-WORKS Lot 3909 3910 3911 3920 3936 3942 3943 3947 3948 CR-200 1 1 1 1 1 1 1 1 1 Color Code RT-365-D to if RT-284-D RT-359-D to it to 3789 3 , Y-299-D 3707 3737 4 4 G-20to9-D 3786 4 to 3928 4 G-7772-D 3933 4 G-317-D 3934 4 n 3960 4 G-7192-D 3953 5 B-57-D 3954 5 m 3955 5 ft 3956 3957 3958 5 B-66-D 5 to 5 to 3959 5 B-63-D 3917 6 RE-398-D 3945 6 GE-388-D 3952 6 BE-149-D 3927 10 BP-69-D 3916 3930 11 BL-151-D 11 RL-360-D 3938 3939 12 RT-399-D 12 ft 3921 127 BT-7337-D 3913 3914 3937 129 GX-309-D 129 to 129 B-7469-D 3931 3932 132 G-317-D 132 G-7678-D rbs. 146 146 119 18 128 52 62 63 151 Group 2 ,2 2 2 2 2 2 2 2 Cost Unit 93 2 222 199 143 87 243 79 166 2 2 2 1 2 2 2 119 2 119 2 119 2 126 2 126 2 125 2 472 2 49 1 118 1 965 1 16 2 269 2 131 1 388 1 28 2 47 2 95 1 95 1 22 1 215 2 227 2 Total Cost DUP050315505 RECAPITULATION Colors transferred from Semi-Works to Plant during January, 1935, Toners Yellows Greens Blues "RE" Lakes RP" Lakes **RL* Lakes Maroon Toners PTA Toners Green Pulps Total 885# 93 1581 1228 1132 66 400 416 47 190 6038# f *K sf-. J1--v: DUP050315506 "V- " ''-.rv >-. MATERIAL*^ PROCESS" AS OP FEBRUARY 1, 1935 - RESEARCH SEMI-WORKS jflO BLDG. 64 60 sc* o O o VO o fH| H VO fc- rl Qa cs a I C| a i 1 i C4 * i o oe- N* CO H 1 iH H *$* VO Taj oj C2 1 CO 1 l>* 1 C4 H tf fr 1 T3I .a O O O 00 O Ct UO uO C4 Q 1 av CV2 C1O Eh 04 n| ol o o O o tn fc- o o o 99 i-il 0> H H Cl Cl C* O Cl %111 l i/IOl/J a* co o[ H VO O O 4 dl CO CO CO CO CO of f 1 1 1 1 O! >4 >* >*> < C-- o a> c4 o Cl Cl H 1t VO co H to trt ct" > 11 QU IX< 2O fr- 3? CO Ok C4 a a H ti Ok 3* O VO CO & *?*" 1 o OQ C- CO ro ^ & <4 rH C3 Q1 O <0 O 3> rH 11 Eh Eh 33 03 Si H \VnO 99 o odff!f om?ot O 00 > CO Ao Ao O ol O O v0o 0 pH 33 Hi 3* m CO Q d QQ 1m t tn VO :0 O Ok tn t<n0 1 C4 CO <0 dl 1 1 1 oi ol a: Sh as: =H 3tf ESh o CO vO sat CHOIO O in 30 vrt Q 1 SO <0 1 X O O C4 1 ocj co fr- CO VO to to 4 VCV!>I?IOO*l VVvaIOOo I a! a! O VO 03 30 O HI C3 1 CO vO 1 Eh 0 0 C4 1 05 O H 4 C4 09 CO HQ t S* H <0 1 O O <4 1 X 0 DUP050315507