Document nkb66ypB2yoZjEQRw7jGdzwdX

3S~- 3 7? 3s~ -- y/<7 3 jf- /-" mWARK PLA3ST PIGMBET COLOR RESEARCH REPORTS NOVEMBER- 1935 .3 J 1 i i N36975 DUP050316451 iimmts c o m r e s e a r c h b b p o r t s H0TOBBR - 1955 K - CBR0MB SMS Study of Chrome Greens of Improved Ltfastness (SCH) Chrome Green G-389-D Strong Type (ADR) ...................... * * (AMi) .................................................. Page 1-3 4 5-6 II - CHROME TUiOWS & GRASSES Improvements in Lt. Chrome Yellows (SCH) ................. Excelsior Yellow Y-8021-D ........ Primrose Yellow Y-7888-D (JDM) ........................................ Medium Yellow Y-299-D - Fashing Study (JDM) .......... Y-316-D (JDM) ...........................-i.................. Y-359-D * ................................................ (OCT.) Medium Yellows Y-299-D. Y-316-D, Y-359-D (JDK) .. Chrome Oranges Y0-34-D - Y0-38-D * ... Study of Y0-38-D " .... Study of Molybdate Chrome Orange (SCH) ..................... Molybdated Chrome Orange Y0-8074-D (JDM) ................. 7 8 9 10 11-12 13-14 15-20 21-22 23-24 25-28 29-30 III- LEAD & LEAD MATERIALS Lead nitrate Purification (SCH) ...................................... * Liquor Purification (JDM) ............................. 31-32 33-34 IV- IROH BLUES Yield Study of Iron Blues (HCM. SCH) .......................... B-66-D Moisture Study (JEL) ................................................. B-140-D " * ................................................ 35-37 38-39 40-41 V- LACQUER MARGOES Maroon Toner RT-219-D and RT-297-D (AAB) ................. * RT-399-D (BJH) ................................................ 42-44 45 VI- PIGMEHT RUBIRE G Pigment Rubine G Lake (AAB) ................................................ 46-48 VII- VAT DYE PIGMERTS (AAB & SIR) ........................................................ 49-50 VIII- PIGMBHT GRIER B Pigment Green B Lakes (AAB) ................................. ............. ' " Pulp GT-68-P (EJH) ............................... 51-52 53-56 IX- PIGMENTS nr OIL Flushed PTA Pigments (HEB) ................................................. Evaluation of Competitive Flushed ?TA Ink3 (SCH). Flushed Colors, Ba Lithol (AJS) ...................................... 57-66 67 68 X- PRIHTDTG IRK STUDIES Hew printing Ink Pigments- Rotogravure Inks (AJS) 69-73 XL- RUBBER COLORS Rubber Colors (AJS) ................................................................ .. Barium Lithol for Rubber, RL-407-D (ADR) ................. 74-75 76-77 DUP050316452 2 xn - mis c . 6S0HIO Fimra (a) Para Bed - Blue Slade (JYS) .......................... .. (h) Lithols Calcium Litkol (HP) ;........................................... Ga Lithe 1 Toners RT-379B & RT-300-D (BJH) Ba Lithol Toner RT-364-B (BJ'S) ...................... (e) Misc. Toners Red Toner. K-7843 (AS) ...................................... Lithe sol Red 2B Lake RM-7909-B and (EJH) Toner RT-7853-B (d) Bordo Maroons laroon Toner RT-354-B (ADR) ............................. (e) Miss. Lakes Misc. Lakes & Toners (AS) ........................ .. Barium Lake of Orange II (I'Ll*) ...................... Analysis of Peacock Blue Lakes (RHB.SWR) Peacock Blue Lake BL-164-B (1JH) ................. (f) Dispersed Clay Color GE-405-B (ADR) ................... XIII - SEMI-WORKS PROBUCTIOR (HA.) ........................................................ 78-83 84-86 87-89 90-91 92-94 95-96 97-100 101-104 105-108 107-113 114-117 118-119 120-127 DUP050316453 33r^- 3*1 / wmmm &Qtm r e s e a r c h r e p o r t STUDY OF CHROIIS GREENS OF IMPROVE!) STR^GTH SUBMITTED BY: APPROVED BY; INTRODUCTION * ** JL/fC FILE ;-^SHWg~8S^aDATE: NOVEMBER 1935* Xu view of tile fact that a number of competitive samples have been received which are frcsa 5% to 15% stronger than similar greens in our G-589-B line, a laboratory study has been started in order to Improve the strength of this line, An improved process has been developed and a semi-works study has been started* SUMMARY AND CONCLUSIONS The present G-389-D process possesses a very low acid balance and because of this a low precipitant balance* It was found that if part of the soda ash added before the strike was added after wards, the precipitant balance could be increased without obtaining an unstable process. Increasing the strike volume and at the same time decreasing the strike temperature seems to increase the strength very slightly. Reducing the quantity of sodium chloride in the strike solution increased the strength slightly* It was then found that with the above modifications both the sodium sulphide and copper hydrate added to inorease the stability of the formulae could be omitted with a resultant slight increase in strength. It seems desirable to draw two waters after the strike and one water after the treatment and before adding the blue* This modification results in a very very slightly stronger, slightly cleaner tint in the green* The treatment after the strike was revised to consist of the addition of the slum and tin chloride followed by bicarbonate to a definite pH* This change may not only reduce the flooding by reducing drier absorption but may also increase the stability of the process, Titanyl sulphate may be used in place of alum with apparently a slight decrease in light fastness and a slight increase in strength. The revised laboratory G-389-D formula differs from the original process in that copper hydrate and sodium sulphide are omitted while the strike temperature, volume, acid balance and pre cipitant balance are altered* The various changes suggested have individually only a very slight effect but taken together they appear to result in a stable process with the desired increase in strength* EXPERIMENTAL DETAILS Notebook #439* 459-8E. Study on the G-389-D procedure the use of' titanyl sulphate, the use of lower amounts of sodium sulfide and cupric hydrate* DUP050316454 In this experiment the use of titanyl sulphate gave a chalky product - very slightly worse in light fastness. Decreasing the sulphate and cutting the sulphide and cupric hydrate resulted in a more olive masstone; none of these variations seem to have an appreciable effect on the strength. 439-88* Study variation in volume; in temperature, and the use of sulphuric acid in place of sodium sulphate* The effects from changing the volume and temperature were too minute to draw any definite conclusions; these will he given further study* 439-85* Study effect of increasing volume of the lead nitrate solution; decrease the salt in the strike solution; also use sodium acetate in the lead nitrate solution* In this experiment an increase in volume and a cut in sodium chloride each gave a very very slight improvement in strength. However, in the case of the increase in volume, it was also observed that a fei&ght decrease in light fastness was obtained* Sodium acetate added to the lead nitrate resulted in a chalky product with poor light stability, 459-84* Study omission of tin after the strike; check use of sodium acetate; and study effects of striking at 110F. All the members of this series showed a very slight increase in strength. The omission of tin and the use of sodium acetate gave products very slightly worse in light fastness versus the control* 439-85* Study use of sodium bicarbonate for soda ash after the strike; study cutting and omitting the soda ash. The replacement of soda ash with sodium bicarbonate resulted in a very very slightly more olive product and a slight increase in strength. Gutting the soda ash and omitting it caused the color to flop. 0 459-86, Study a slight reduction in tin; striking at 100 J instead of 80UF and a still further increase in volume; also use alum for titanyl sulphate, A slight reduction in tin helps to improve the strength; striking at 100F gave a dirty tint. It was observed that those made with alum instead of titanyl sulphate gave weaker pigments, but were much better in light fastness* 459-87* Stxidy again the use of titanyl sulphate, sodium acetate and a variation in temperature* In this experiment titanyl sulphate again gave a very slight increase in strength accompanied by e very slight decrease in light fastness. DUP050316455 Striking at 80F instead of 100F gave a very slight increase in strength. The addition of sodium acetate to the lead nitrate liquor had little or no effect on the strength. 489-*88. Study striking into a more concentrated lead titrate solution, also precipitate all the lead as chromate and sulphate# A cut from six to four litres in volume resulted in a large decrease in strength. Increasing the sodium sulphate (88C) in order to precipitate all of the extra lead resulted in this experiment in a dull, flat pigment, hut gave an increase in strength# 459-89 . using 880 as the control further increase the sodium sulphate after the main uart of the strike; use hydrochloric acidwith the tin crystals; also try the use of cupric hydrate as in G--389-B* in strength# All of these variations favored a very slight decrease 439-90 Study variation in pH after the strike# Both an increase in soda ash and a decrease tended to give a more olive product, hut had little or no effect on the strength. 439-91. Continue the study of using hydrochloric acid with the tin crystals; also omit the sodium sulphide. Omitting the sulphide favored a very very slight improvement in strength; this was accompanied by e decrease in lightfastness# Ho marked improvement wa-s obtained by using hydrochloric acid with the tin crystals. DUP050316456 FIG&KHT COLOR RESEARCH RSFOORT mom g e e ee L ewass*! s t r o s g t y p e SUBMITTEB Wi%6M>**S APPROVED BT: C&U INTROSPECTION FILE: DATS: NOVEMBER 1935* Several sew modifications were tried in tie Semi-works in tie study being mad to increase strength - one a variation of standard formula employing high bichromate plus addition of part of the soda ash after the strike; the other a new laboratory formula, Exp.439-89A similar in this respect but with additional features found to give additional strength* SUMMARY AND CONCLUSIONS Ho increase in strength was obtained by employing the higher amount of bichromate* Splitting the soda ash was for the purpose of increasing the amount of soluble lead while the bichromate is being added* The formula appears fairly stable since the highest amount of bichrome did not cause changeability although it did result in an olige product* The new laboratory formula gave a product of good strength but considerably bluer and cleaner in mas stone and tint than either our present standard or the competitive sample. Strength equalled the latter* It appears to be necessary to draw a water after treatment of the yellow as omission of the extra water gave a product ju3t equal in strength to standard* Work is being continued* EXPERIMENTAL RETAILS N.B. 436, p63* clean. SW-7411 - 0.1 mol charge 2$> of CS-7874 - Control. Vs GT-389-D - blue and brt; blue and clean; 0.K*, s.blue, SW-7416 - Check SW-7411 but use 4.32# soda ash; 18*1# Bichromate of Soda; 0*75# Soda Ash replacing final sodium sulphate Vs G-389-D - blue & clean; blue & clean, O.K. s.blue and clean* SW-7420 - check SW-7416 but use 12*8# Bichromate of Soda* VS G-389-B - s*lt,, olive; blue, v.s*str., s.clean. SW-7486 - 0*5 mol charge as in Exp. 439-89A* Vs - G-389-D- s.dark blue & cl; s.blue & clean; strong,s.It. Vs - #37984 - clean & brt; clean; O.K; clean SW-7492 " Cheek SW-7486 but draw 3 waters before treatment and none afterwards* Vs G-389-D - v.s.blue,s.clean; s.bl.&cl; s.str; s.clean. DUP050316457 mmxrsTSB m% aBPROYBB BY* */ f il e : c ^s o me-s e s s ?* BA! HOYEMBSB 195S. *988?mi `PPTOK Plant production of the G--4SS9-B line of Greens was kept under observation of the Development Section in order to eorreot difficulties which have arisen in manufacture of all shades, a number of batches were followed closely * operation and control points being checked# The types of abnormality which are causing trouble were changeability varying from slight to positive; a difference in flooding characteristics of rubouts making standardization difficult} an outoffline relation of masstone and undertone {blueness of undertone}and more recently too great blueness of masstone (lack of oliveness)* 3PMMABY ASP OCBCUJSIOMa Considerable progress has been made in correcting some of the trouble but the blueness of masstone which is possibly the result of variations now being used still requires attention# During the month covered by this report (Oct# 31 to Nova 34=) thirty batches of U-389-D, five of G-39G-D, seventeen of G-391-D and nine of CL-392-D were made# Cross comparisons have not been obtained on all variables tried but the following conclusions appears to be safe* Changeability - Usually only slight in the two light shades of the line, this has practically disappeared* More rapid addition of the bichromate through a sprinkler is believed to be helpful and was adopted in most of the series# It was thought that because of the better agitation being employed now, the yellow might have a freater tendency to change its crystalline form* Lower strike temperature 90 and 75<*F instead of 11QF) is also being used* The effect of increasing sodium sulphide is doubtful. Changeability was observed in a batoh in whleh copper hydroxide was omitted* In the dark shades a few batches were very changeable but none of this type has been obtained recently* Flooding - Lightening of masstone occurred after the mount has stood* Actually this amounts to less darkening or flooding and should be desirable* It appeapo4 to be the normal tendency at present although recent production has shorn, less difference* Use of some soda ash in treatment of the yellow probably has helped in bringing present material closenrto standard in this respect. The amount used is below that employed when the standards were set up as the full amount sometimes causes oliveness and poor light stability* Blueness of undertone and tint# This was corrected by reduction in strike temperature (75F instead of 110F) and by increase DUP050316458 in amount of bichromate used, The changes brought the tinder tone over to the yellow side ^Blueness of Masstone, This was probably increased to some extent gy the lower strike temperature. At ?5F increases in bichromate from S3S to 242 lbs, per 8 mol charge were not sufficient to`equal standard in oliveness and use of the higher temperatures may he necessary. At the present time this is the chief difficulty in blending standard material especially in the dark shade. Red types of blue are being tried for shading but no results are available yet, SXPBRlIffiNTAL. DETAILS Reeord of variations and gradings in N,B, 437, DUP050316459 jr- 3^ PIC-MBHT COLOB RESEARCH REPORT IMPROVEMENTS IN LIGHT CHROME YELLOWS SUBMITTED BY: ^ f MrPrv^ APPROVED BY: &//'/ PILE; 9B30MS.&&Qm DATE: HOYEHBEH 1935. IRTRODPCTIOF A few additional experiments on the Excelsior and Primrose Yellows were made during the past month, A study of these processes in the Semi-works and plant is being continued# SUMMARY AND CONCLUSIONS A study of the Primrose Yellow process, K-7975*. indicated that a part of the alum can be replaced by a small amount of zirconium sulphate with 9 decrease in the livering tendency. This change probably results in a slightly less stable process. Several experiments on an improved Y-180-B process confirmed previous results, A high development temperature and a strong lead excess during the development period seems necessary to obtain a clean masstone. BsrraiinarrAL d e t a il s ___ 481-34, Study reduction of alum and use of Zirconium Sulphate in the K-7975 procedure {primrose yellow). It appears that Zirconium Sulphate can be used for part of the alum without affecting the tinctorial properties* An improvement in the livering properties was observed, Y-180-P, 481-25, Study omission of sodium sulphate after development; also vary the development temperature* Omitting the sodium sulphate after the development resulted in a slightly stronger product; no other marked change was noticed* o Reducing the development temperature to 140P from 180F greatly reduced the light stability and gave a dirty pigment, while developing at 200P had no appreciable effect other than produce a slightly cleaner masstone# experiment* 481-26, Continuation of the studies made in 481-25 While the effects from the variations in this'series were not marked enough to make any definite conclusion it was nevertheless observed that a strong lead excess during the development period was essential to obtain a pigment clean in masstone. DUP050316460 PIGMENT COLOR RESEARCH REPORT 35*-3?/ SUBMITTED BY: APPROVED BY: 4 j A ESC1LSIOR YELLOW. Y-B021-D Cx5HjUQJLO '... ........ . '"' Jt/f'f FILE: ^SfflQlffi-YSiDGSS DATE: N07EMB1R 1935. INTRODUCTION One batch of this titanyl sulfate - treated Excelsior Yellow was struck in the plant during the month. SUMMARY AND CONCLUSIONS The plant batch was struck on a formula checking on a larger scale the original one which gave satisfactory material in the semi-works. The only difficulty in operation encountered was the in adequacy of the plant equipment for rapid heating, the time for development of the eolor requiring considerably more than double the time specified on the formula. The color, nevertheless, against Y-3G9-D standard, was clean in mass tone with a strong, clean tint. Against the semi-works control the masstone was v.v.s.flat and dirty, the tint being v.s.strong and clean. Light fastness was considerably better than that of Y-3Q9-B and a little better than that of the semi-works material. In ink mill tests the plant batch was found to be inferior to the semi-works color, but better than Y-309-B in most respects. With a zinc etch the plant batch (lot 46190) was inferior to both Y-309-D and the semi-works material (SW-7384). In the case of the chromic acid etch, it was superior to standard althougi not as much as SW-7384. While resistance to livering was excellent compared with Y-309-D, the ink became appreciably heavier than that from the semi-works bateh. It is interesting to note that this batch of the special Y-309-D is markedly superior in resistance to lithographic break down to a number of batches made at approximately the seme time on the standard Y-309-D formula. Additional material will be made in the plant upon arrival of a shipment of titanyl sulfate, now on order. EXPERTSWTAL DETAILS See n*b. 492, p. 20. DUP050316461 S4T-3*** '' -Mmm cmm r e s e a r c h r e p o r t e SSJ8MXTTED BY: APPROTO BY: * & gj DBJflir. T-7888-P FILE: fSReMB~YSELOW~ DATE: BOYEKBER 1955. MML Tills Primrose ^ellow was first tried in the plant last May and proved unstable to drying. As a consequence, additional work was done in the seal-works to overcoats this difficulty. After asking satisfactory material in the semi-works in September, the new formulation was tried again in the plant during the last month. s u mmar y jrn oommsiom.... The formulation tried in the plant differs from the one formerly used in two primary respects; namely, that the nitrogen oxides were not removed from the lead nitrate liquor, and that the bichromate was reduced about fifteen percent, thh sodium sulfate in the strike being increased on approximately equal amount In order to retain the correct precipitant balance. Against E-7888 the plant batch was slightly dark and red in mas a tone and red in drawdown and tint. The masstone was slightly green and clean against Y-505-D, the tint being a little strong ana rea. Light fastness was a little worse than K-7888, but better than that of Y-305-D standard. In ink mill tests the color was distinctly better than Y-305-D both tinctorlally and in light fastness, but was somewhat re&dSr than a competitive Imperial Primrose. Aithou^i resistance to lithographic breakdown was good in all cases, less bleed was noticed with the ink from the plant batch. Further work is being done on this color, results of which will be available next month. DUP050316462 PIOMBJT COLOR RESEARCH REPORT Z/'' ^ MEDIIM YELLOW, Y-S99-D - WASHING STUDY SUMITTID BY: APPROVED BY: ZJ/- / f il e : ' esiesffi^ffifcLews DATE: NOV3MB1R - 1935 INTRODUCTION: This study was conducted to determine the optimum point in the washing cycle to obtain a yellow of the most desirable properties* StMMAKY & CONCLUSIONS: Two batches of oolor were struck in this study on identical formulae: namely, the base Y-359-D formula consisting of running a lead nitrate liquor into a dilute solution of sodium chromate. In the case of the first batch, a portion was pressed before flooding, and one after each of five waters. On the second batch a portion was pressed before flooding, and one after the second, fourth and fifth waters. The results are indicative of the fact that these yellows are subjected to more washing than is necessary. In the series in which a portion was pressed after each water, the best product was ob tained after washing but one water. The yellow at this point wasdefinitely cleaner and of better light fastness with, however, a slight decrease in strength against further washed yellows. The yellows be came progressively dirtier as washing continued. In the second series the optimum point in the cycle was not so clearly defined, the yellow pressed with no washing at all, having, however, very, very slightly better li$it fastness than the other samples. This fact together with the accompanying very sli^it decrease in strength in the case of the sample in question, would indicate that this checks the results obtained in the first series. It can be concluded, therefore, that, for optimum tinctor ial properties, it is sufficient, and moreover,advisable to draw one wash water only on this yellow. EXPERIMENTAL DETAILS: See Notebook 448, p. 104-105. DUP050316463 -iv S. $$mmm m% tttOfiJO ^ J2^/ mi: novpssaa iss* fit# development section continued its supervision f this color during the month. Tremble is still being experienced with weak tints and poor light fastness although msstones on the whole, have been satisfactory# A mall i^rease in bichromate and caustic soda was made on the first hate# of the month. It was a trifle on the red clean side of standard with v.s. morses light fastness. The tint was a trace strong and dirty. On cheeking this hatch except for using the standard amounts of bichromate and caustic soda, the color was a little greener in masstone ant on extension, with a little improvement in light stability. A fifty percent increase in volume reddened the produett a little with a small decrease in strength# A check on this last hatch was practically identical except for being a trace cleaner with v.s. worse light fastness# Doubling the time of strike improved the strength but the mass ton became a little green and dirty against the control with a little worse stability to light, this batch was v.v.a. red, clean, and weak against Y-Slt-B standard with slightly worse lightfastness. this batch was eheeked with an increase of one third in the amount of alum. It was' a little red and dirty with slightly worse light fastness. Coincidental with the decrease in this respect there was a small increase in strength. Doubling the volume of the striking solution gave a greener product with.improved strength and light fastness as compared to this last batch. Against standard, however, it was a little grama and dirty with definitely worse light stabiiity* Two batches were made to determine the effect of a further increase in volume over this formulation utilizing the short time of strikes and the already increased volume. By mistake these two batches were mixed, being a little red and clean in mas stone with a slightly red weak tint and v.s, worse light fastness. This variable w$s reehecked, one batch being run as a control, the ethers have a fifteen percent increase in the base volume* The control was a little on the red, dirty side of standard with a somewhat weak, red tint and slightly worse light fastness. The batch struck more diluted, was a little cleaner in masstone and tint with a small increase in light stability. This study is being continued as production permits* DUP050316464 b e tte r. s .w o rs e vs, v .s .g r* v.s.g r, vv ..ss ,.ss ttrr ., v .s .g r.& c l. n v *v .5 ,g i*.&dy0 s*gr a*33-5-sH 43 fr< ft 4UH3 fflCO 4> uP3i P Sf w J Ho u8 a $3 s A ea m ffl ffl m J> ffl nOffl ffl Pff*li +3 0 > P ffl t> & m *u > P0i ffl 0ffl 03 co i* > a ftft * S P*i 4>*P.i Ho ffl ffl to* *hrt n + ffl o t>+ pi > p< ffl ffl i> # > S3 88 8Pof>fil 4P3i to * 4n9 CO f*t > J> eg 8 <2 I 4 o H 8 tS P* ffl * C> ft to 03 * ^ {> > <cf >0 $ff4l **4 *0 ffl ffl ts P*i ffl ffl ffl ffl ffl ffl ffl *? *?<0 tt0-iH e*?O t HO atHoI tOto I 31 31 31 * to (0 caea4 to 03 CM* <M0 I as 3 il*sa it |r eaigs Sli'g?g Hi I*!* ts 1.*4f-fl I". 4>|-g 8|8 GeS*)-r* M EJ O *9. dm f<isis r4* "* ft 8 2< % 8o* o SI Os | S ii Pi 8? frfa0l (0 > ^0 s 1* to to "ft<(4 to %*. P i ffl <0 8* . 4h GQ 03 ff*l ffl ffl a eg +P>i :<Pdi M ffl 65 ff*l fSf3l h& < < tPf*filr40 ffttf**tl4*t>.Urtt ePtC>g**S04tt>>HS** fg *1 r-4 * . rsg XJ t *4 a -F* 4* * p3a e3d ^ '.8 M M V)4r4^ ? I ii II P0t ff0l G 8 ffl Sf3fl ffl j+PffaP>ff*lli Pofftl 65 ff0l Poi ffl 0 > P*t ffl ff*l P4 * 4 * to0 > Pi 4f>fl ffl 0 t* 00 > 8<Gt Pi 03 w* tS Pi 0 ffl 8 0 > &H I g a03 *u -- > o <*} 8It`s *4 ffl 0 111* {*a ffl Pt Pi > ffl ffl 0 ffl > t>0 f0* *00 I t to to 3OS f 2 &00 CO CO 0 to tO tO0 to <0 fffffflll 6*8 8$ i; 'll 8 ii 3a Ml Y-516 48801 * uble sol do ng t i bu rik t 46oSfKIs1 #'S0fe v o lu m e 4--: /'la::--, DUP050316465 i, SUBMITTED BY: APPROVED BY: PIGMENT COLOR RESEARCH REPORT J6~~ A MEDIUM YELLOW Y-5S9-D dXwlreiujtOLoJ Aod- &^s*-****ip** AS/'/ fiLE: DATE: NOVEMBER - 1935 INTRODUCTION: Production was continued during the month, no difficulties being encountered. SUMMARY & CONCLUSIONS: A total of seven batches were struck on the same formula: namely, a dilute solution of sodium chromate acidified with a small amount of muriatic acid (l.S#/mol) and struck with a relatively con centrated lead nitrate solution. According to control laboratory tests these yellows were practically all very slightly darker and dirtier than standard, with a tendency in some toward changeability. These properties were not evidenced in semi-works tests the masstones being generally very slightly red. Tints were slightly strong, green and clean in both tests and light fastness was in nch case# better than that of stand ard, varying amounts of improvement being noted with different batches. color. The development section will continue supervision of this EXPERIMENTAL DETAILS : See Notebook 448, p, 76. DU P050316466 BATCH_ _ DATE FORMULATION CONTROL MASSTONE UNDERTONE STRENGTH TINT LIGHT STa B I I - LITHO ________ ______________________________ _ ___________________ _________________________ ___________________________BREAK _ > oo S4 05 + v> 05 A r4 flj md cr* > ffl r4 ffl r-4 ^ ffl eg S4 63 h w ra J4 i4 * +* to in m tn f4 t-4 43 14 ffl ffl +* y * ffl ffl u CO 5*0*0 !> to f4 Axi o 03 u > . + 13 f> * +* * ua O tags: O *4 03 d *d 43 + 01 03 O u0 43 + ffl 14 ,ffl ffl > 43 03 43 ffl A r-4 O ffl <*} > * Blr-3 O cB u 43 h to m ca rl .ss * GO k t& 03 A CO 0* >u p EG K*i P GO |> 03 * |> M O P ffl 43 43 m ffl a> A P9 43 CO J> CD S3 ' y-i U +3 P 03 CQ CQ CQ 1 * t& P t 60H * 0 *o CQ 03 * <1 rH > VO 03 r0 d 0 8 rcJ GO <D *c5 W! & > O M h ffl m o ri u m J> . o 0 03 t> 83 ffl > "* a * J > " i * > 4--r P Bs fes j -- GO O GO OPO'-- to 0 C3 rl A*"l SBffl'd S3 4 10 43 P GO CQ 'if 05 CO CB to r4 % 3 43 +3 -rl + H 3 Is. a p ! oBS 1-3 * 4> pen ffl ffl *H O O *4 01 CO & ffl 3 =Zite *s *-rtslO ao o a r-3 ffl rt O) IO -Ki A O eO H 9O) A4 O ffl J O 0 H (4 ffl ffl 43 43 43 43 ffl ffl A A9 ffl ffl i-4 fM OO r-J e> eg & & n m t?D ft a 03 >4 P 4 GO n 0) a 1 eg !4 da 43 ,-1 ffl 0 >4 43 1 ffl ffl > ffl eg <g eg 43 & *d r4 ffl Vt Ml fj H a * rtf 0 03 O 03 *> 0 P a 6= 0 CO o- 5 Jd p 43 00 to CQ O to 9 50 r4 o> in M o ffl A O 0to Qi CO CV5 v. 'Ny 0 HH H r4 r4 <> r4 (SO3 CB EO es 85- A, 05 HI H S3 flfl 10 <0 o 9 10 \03 H H 0 0 9 v5 V DUP050316467 tt) Pt &E QuB a** H S t J H 4* ffl a o o 05 E-< .fit 6 S' <D -3 r s u p CO H <j rH CO OJ I--I O oP p li il rH 02 <COS H > rH o p N *s Po rH O r-v CO -0w0 o rH M V<1 rH < 00 rH rH C>l H 03 pCw O to -fi4 CO p oo 03 w) 03 te H p rt rH It slj CO rH al rH g rH 03 CO > rH > H *P &0 Jh CO o O rH p OX rH P U O A g >P 11 > 00 < H CO rH > 51 t> wO CO rH P rM -y O P V. Vi. rH rH II 03 =ti fed 03 CO * VL 03 rH H 02 O P rH rH 03 CQ 02 rH > O *P N * S3 11 p o rH JL, > #* > CO CO rH rH SS rH rH 02 > rH aP 03 O > 11 3 03 rH SP c* O -P ts Vi. CO t rH 5 02 O p fl r*\ CO rH * o t>o > o rH cm o S rH a 03 O P u p s CsJ o p rH =J av rH 2 O -P rH 5o>$ rH o p II s rH 3$ G> ptHo t> H4 OCO <? a H to txO C rH to 5oS to s> 'I Vi. to ffl rH -p o pp pH o 03 O P u >O' O' vO_^' O' v^ O' ID CO o c- rH <C O 03 G*O 03 oI p 3 02 O P 3< O 03 m r--1 3$ |S* aj4 E O o 03 bO o E 03 rH O rH O b&, P n P F 11 rH O03 <? GO > 03 Sh o P t 03 PCO p I CD. R rbri G> rH + <3> t- 0 rH rH in P ^ o ?ru rH 12 prrf O o fH O 03 O rH O rH O CO o I-- o k o VV V rH O M rH S+ B t> *) rH rH P Jh P P ca rH 03 03 H rH O OOO v 02 O _ ***** 03 'CJ E ^ rH H o> CM m tO' o o o n rH <J> CQ o> o o p co o> O t o CO o ej* w* CO O in CO 00 o 00 O * CO O' <T O' O' rH O O' O' rH O' O' o <r> cr rH rH rH |M rH rH rH o H rH rH rH 03 c4 rH rH 03 03 O at CO CO o 03 rH rH 03 rH rH 03 ol i CO r--. CO rH rH O rH 00 rH CO rH oo rH H 03 H 03 t rH 1 11 rH H 03 03 11 rH 02 I * CO CO << ca O' O' O' O o O rH iH fH 03 03 03 03 cje CO CO 1l 1 CO CO "d* DUP050316517 Cf 8 HOTES to TABES III (1) "A8* samples are laboratory dry control inks. *B" " " flushed (on ink mill) inks "C" 88 " plant ground dry control inks (S) The % yield varies greatly with the care taken in scraping th<5 ink from the apron of the mill, and is not reliable in the ear lier experiments. (3) B4 is stronger than As and Bs because the pulp stood over night before it was weighed. (4) The ink mill rolls were not previously wet with ink. (5) Determined by S. W* Runibel using toluene distillation method. (6) Since some flow measurements were made on different days, they are not very significant. (7) The flushed water may have carried with it several percent of color. (8) Inks were thinned down to 2s3 inks for flow test. {g) i, n n i. 4 n n (10) Series 18 and 19 were rated for body, length, flow and texture after standing for 3 weeks. In general, the results so far obtained indicate tentatively that a flushed PTA pigment ink has equal strength, very slightly better tex ture, slightly better flow, similar masstone, equal length, equal body and equal lightfastness to a corresponding dry control ink. Both flushed and dry control types contain only a negligible amount of water. Work is in progress preliminary to analyzing these inks by extrac tion and ashing in order to check the toner content. Additional information is given by an analysis of the properties of each PTA pigment investigated. RT-329-D flushes into #0 regular varnish quite cleanly but there is some color in the flushed water so it is best to evaporate all of the water on the rolls in order not to lose any color. If any water becomes emulsified in the ink, it seems to be negligible. RT-329-D will flush not only into varnish but also into blown castor oil, dibutyl phthalate and a mixture (isl) of Hujol and blown castor oil. It will not flush into Jffujol of mineral spirits alone even when kadox is added. When flushed into blown castor oil (lsl), there was no isesdase in strength. (See 483-16C, B.) Considerable confusion arose from the flow measurements of RT-329-D inks. Four flushed ink^had greater flow and one flushed ink had less flow than the corresponding dry control inks. The flow varied greatly from day to day so comparisons were always made on a single day. DUP050316518 9 The writer 'believes that the multiplicity of factors which affect the flow &ak& satkesflow test almost worthless at least until a better understanding of these factors is obtained. The reason for reaching this conclusion is because duplicate experiments under quite care fully controlled conditionej&o not give duplicate results on flow determinations. RT-329-D pulp mixes intimately with dioxan which becomes yellow-colored when filtered and the pigment is weakened considerably. Although dioxan is miscible with water and with mineral spirits, the ternary mixture produces two layers. The dioxan-treated RT-329-D (dried at 140P overnite) is very soft, very weak, and has much better flow as compared to standard. BT-IOO-D flushes fairly cleanly into #0 regular varnish appar ently without producing a w/o emulsion but BT-125-B which contains gallic acid and para soap produces a w/o emulsion (crepe-like mass) which means that some of the water does not flush out but becomes em ulsified and must be evaporated. There was more difficulty in obtain ing check analyses for BT-100-D than for the other colors. BT-125-D was a semi-works pulp and was thicker and quite granular (dry content 28.50$). BT-125-B ink (isl) was much thicker (possibly caused by para soap) than Bf-100-D ink, so a 2:3 ink of BT-125-D waB prepared for evaluation. Hand flushing of BT-100-B Spatula flushings of BT-100-D have indicated that with #0 regular varnish as the vehicle, the strength of the ink is influenced by the time it is left spread out on the board. Extensions with ainc oxide have shown increases of about 10-15$. Further quantitative work is planned in an effort to explain this observation. It is a factor neglected in the earlier work and which may account in part at least for apparent increases in tinting strength obtained in hand flushing of PTA pigments. Pellet technique applied to flushing of PTA pigments(See 469-3,11,13,14) This technique which has given results of some interest with Lithoi Red comprises stirring the varnish into the slurry by means of mechanical stirrers such as wooden paddles, with PTA pigments it is considered impractical for the following reasons: l) "Ink.balls" in place of pellets are obtained, 2) the incorporation of varnish is difficult and incomplete (some improvement was noticed if the slurryoil mixture was heated, and 3} the settling was poor,leaving an upper layer containing suspended pigment. RT-529-33. RT-329-P slurry containing- 10$ color was stirred with an equal weight of #0 regular varnish for 15 minutes. Water was added to give a 3$ slurry which was stirred with wooden paddles far a total of 20 hours. Buring this period it is possible that some very small pellets were formed which however later coalesced in part to form a thin ink. At no time was there a formation of pellets simi lar to those formed when a Lithol Red is treated in the same manner. The mixture settled to half the total volume in 10 minutes but the upper layer was not clear and contained much pigment in suspension DUP050316519 10 that was not wet with oil. The lower layer was. a mss of ink which was not homogeneous, i.e. some parts contained more oil than other parts. BT-125-B. Since there was incomplete incorporation of oil in the above experiment, it was decided in this experiment to obtain the optimum conditions for wetting of pigment by oil and subsequent pellet formation at room temperature. A 5$ slurry of BT-125-B (240 g. color) was passed twice thru the colloid mill and on the third and fourth passes 100 g. each of #0 regular varnish was slowly added. On the fifth pass 160 g. of oil was slowly added to give a 40*60 pigmentoil ratio. The mixture was passed thru the mill once more. Although the mixture seemed quite homogeneous, a large amount of ink remained in the mill and there was a tendency for the rotor of the mill to gum up. After stirring 30 hours with wooden paddles, the mixture settled to half its volume overnight, the upper layer being clear and containing no pigment in suspension while the lower layer was a homo geneous suspension of ink in water. At no time were pellets formed. The mixture filtered in 45 minutes leaving an ink-water press cal that seemed to be homogeneous. It is possible that by varying the above experimental condi tions, pellets similar to those obtained with lithol red might be ob tained. However, in view of the unfavorable results obtained so far, further investigation with PTA pigments does not seem warranted. EXPERIMENTAL DETAILS Notebook #483. 483-16 8. 35 g. RT-329-B plant dry ground color + 25 g. H-120 4x hot mill. B. 100 g. RT-329-B pulp + 25 g. H-120 4x hot mill. 1633 was t t s heavy, vvs short, s.light and dull and 3% weak vs. 16C - Neither 16C nor 1633 had any flow. B. 200 g. pulp was treated with 200 mi dioxan, filtered and dri< 483-17, 18, 19, 20, 21. See details in Table III. 483-22. Board flushings of BT-100-B. A. Dry control rub out. B. Flush on board - large area- remove water as quickly as poss C. * " small * - work fast B. * " large * - let dry one hour. 332 Repeat of B. Bs Repeat of 33 - only dried 1.5 hours. Rub all above 2 varnish (#0 reg.)sl color (as pulp). Tint 0.1 to 5.55. Strength of tints* A=B=C=B2. B and Ds approximately 10$ strong. 483-23. pellet technique experiment. For details see main body of repc DUP050316520 PIGMENT COLOR RESEARCH REPORT SUBMITTED BY: APPROVED BY: INTRODUCTION EVALUATION OF COMPETITIVE FLUSHED P.T.A. INKS v FILE: SIiSMENTS-~IN--DSr- /6f/ DATE: NOVEMBER 1935 A. number of samples of flushed competitive P.T*A inks have been obtained and are being tested versus dry color inks prepared from our toners* The results to date do not indicate any marked superiority in the competitive samples# SUMMARY AND CONCLUSION Flushed colors may give a better money value because of increased strength over the dry control# To determine the approximate strength of the flushed colors a determination was made of the ink composition necessary with our standard pigments to give equal strength versus the competitive samples* Since light fastness and strength are related in F.TA pigments the lightfastness was also determined* The results obtained to date are listed in the following table# Some of these inks are to be subjected to accurate analyses for pigment, oil and water contents# EXPERIMENTAL DETAILS Notebook #483. C~# Standard Ink Composition Tint Lightfastness Source at Equal Strength vs Std* vs std. _______________________________ ^ Standard ________________ |J88$K 38208 BT-1G0-D BT-122-D 66# 55* dirty,v.s.red poor. s#dirty it HiIton-Davis n 38209 GT-337-D 52* sdirty,s*blue it Tf ft 38210 GT-347-D 53# yellow tt tf ft 38211 BT-125-D 45# dirty,s.green ^ " Vavr a,Frey-McGruden 38212 BT-100-D 60# dirty,s.green ft ft " Sfterwin- Williami 38213 }I Evaluated 3/29/35 by Sales Service {Department CH-16 38236 j 38230 38231 38232 3823? BT-125-D BT-100-D BT-122-D BT-125-D 52# 60 55* 61* equal v.s.better Sodirty poor vs*red " vv*s*dirty " Sherwin-Williams ft ft tf ft Adco The above results are recorded in notebook #483 under experiment #24* DUP050316521 PIGMENT COLOR RESEARCH REPORT FLUSHED COLORS BA LITHOL SUBMITTED BY: *y/' APPROVED BY: FILE: DATE: NOVEMBER 1935 /6t * INTRODUCTION One series was run in the laboratory the past month In an effort to make a "Duol" with less than the usual amounts of rosin when treated with varnish* SUMMARY AND CONCLUSIONS In view of the fact that the addition of varnish to the Na salt results in a lithol having some of the characteristics of a "Duol" a series was run using various amounts of rosin in addition to the varnish as used in the Na salt of previous series* The results, however, were disappointing. In the first place even the dry controls failed to show the desired "Duol" characteristics. All of the rosin treated products were brighter than the untreated ones and in every case they were weaker* Nothing of interest was disclosed in this experiment* EXPERIMENTAL DETAILS See Notebook #469, pp. 174-176, 469-52 Series, A - Dry control like 50-A (Acid coupling "lithol.") B - Asa but add 5$ Rosin to Na salt* Q_ It It IT U * It P_ " * "50$ " I* n E - As'A but 75$ Varnish added to Na Salt* F- *B w tt n w t? ti it G " C tt tt ft n n H <** " D n tt tt tt tt tt DUP050316522 3S~--^ c J FIGMENT COLOR RESEARCH REPORT HEW PRINTING IKE PiGMawra ROTOGRAVURE INKS SUBMITTED BY: $'% APEROVED BYt <$< INTRODUCTION /FA S' FILES SSf-STBBESS DATE: NOVEMBER 1935 The demand for quick drying inks for the newer and very rapid type of printing equipment has placed a larger burden on the pigment* This project, on which active work was begun this month, is designed to broadly cover the field but the specific attack at present has been on pigments to be used in inks for rotogravure printing. The work to date has been devoted to an effort to improve the pigment by incorporating the resin in it* SUMMARY MB CONCLUSIONS The Technical Laboratory at the Dyeworks was asked in February 1935 to recommend an ink for use on a new type of rotogravure press by one of their customers* They selected the recently introduced resin of R & H (RH^35) as the vehicle for the ink, using Solvent Naphtha (H*504) as the solvent* After considerable investigation they changed to the higher melting form of the resin (RH35D) and succeeded in formulating an ink using Hansa Yellow as the pigment which pleased the customer very much* The approximate composition is Hansa Yellow 7*0$ RH35D 45*0 Solvent Naphtha 48*0$ This ink was prepared by pasMBgthe yellow with part of the solvent and adding the resin dissolved in the remainder of the solvent* No grinding was necessary and the ink prints with a very desirable gloss* This laboratory took up the problem with the idea of incorporating part or all of the resin with the pigment in the hope that it would greatly facilitate the mixing into an ink and possibly eliminate tW grinding in many cases* Attempts were made to incorporate the resin by adding a solution in mineral spirits to the color in process, finishing by the usual development, filtering and drying* the solvent evaporating along with the water* In the first experiment the solution of resin in mineral spirits was added to the finished color (Ba Lithol) slurry in a colloid mill* The resin appeared to be successfully incorporated as evidenced by the increased yield but when the resin added reached any appreciable amount there was considerable gumming up of the mill* Another method of adding resin to the lithol was to add the solution in mineral spirits to the Na salt as wqs done with the varnish in some of the experiments on flushed colors* Again the resin was successfully incorporated* Rubout tests indicate little tinctorial effect by adding the resin solution in the colloid mill* On the other hand when the solution is added to the Ha salt, a dark, blue strong DUP050316523 10 *2* product results with the effect increasing as the amount of resin increases* It is known that mineral spirits alone will give this effect to some extent and it will also give a very soft product* These products with mineral spirits and resin* were tested by making inks as noted above for Hansa Yellow and found to give satisfactory dispersion in eaoh case* It was found, however, that a very different ratio of pigment to resin was necessary to obtain the desired gloss on the print* Similar experiments were tried on Bt 100*D by adding mineral spirits alone and with dissolved resin to the slurry Just after strike* The amount of resin was also varied by stepping up to very large amounts* In an amount up to that of the pigment itself the incorporation was substantially complete and dry products readily obtained which showed little tinctorial change* In larger amounts Of resin the amount of solvent required was so much that some came through the filters* with some loss of resin* and the drying process was quite slow and tedious* nevertheless, the effect of the added resin was quite definite for the product without resin but treated with mineral spirits showed very poor dispersion in the ink formulation whereas those containing resin were much better and the effect seemed to increase with the amount Of resin* Again a different formulation was necessary to obtain the desired gloss on the print* It is planned to investigate the merits of these inks when given some grinding sueh as a short ball mill cycle and it will be necessary to more accurately evaluate the inks before final conclusions are possible* We hope to be able to make printing tests of some value in the near future hut a good test for grit is very necessary* We believe it has been shown that RH**35 resin and probably any ordinary resin can be incorporated into pigments in some such manner as described above* The method of adding the resin may and, in most cases, probably will have some effect on its tinctorial properties* We have also shown that in one color (Ba Lithol) the resin treatment does not seem to improve its dispersion in the resin solution whereas in another case (BT**100I>) the resin treated colors do show better dispersion* The future work involves first of all a study of methods of evaluation of the pigments; second, the use of modifying agents in the inks, possibly incorporated in the pigaent as a means of obtaining dispersion; and the study of other representative pigments* We also expect to prepare large samples with ball mill treatment for evaluation by the probable user* DUP050316524 tittle* 7/ TOERIMETTAL DETAILS See notebook #493, pp* 10-24* 493-1* To treat RT-S64-D (acid coupled) with Mineral Spirits and RH35 resin* A - Dry control* B** 1Q% resin in mineral spirits solution added in colloid mill* c 25% ttnti n " "" D - 50% " It W it W tt H E Mineral Spirits added to Na salt E * 10% resin in mineral spirits solution added to Na salt# G 25% w it it tt H ** 50% ttwwtt w it B, C, D tended to gum up the colloid mill, D very badly. All but D were quite soft* Tinctorlally A, B, C, D were very much alike when allowance was made for the resin present* E, G* H were darker,stronger, bluer, and cleaner# It appears possible to incorporate the resin in either of the ways used in this experiment* The method of adding and the amount of the resin determine the change in the tinctorial properties# 495-3 Barge samples for testing* A * Large sample like 493*11 B- " " " 493-1H These are fairly close to their controls asd will be preserved for future tests* There is some evidence that B is no better in dispersion than A# 495*3# To treat BT-100-D with Rh *35 in mineral spirits* A Untreated control like BT-100-D* B Treated with Mineral Spirits alone# C - Treated with 50% RE-35 in MinesallSpirits* JTeither treatment appreciably altered the tinctorial strength of the colors* The incorporation of the resin was successful but no further conclusions are possible# 495-4* An attempt to treat BT-100-D with large amounts of RH35D in Mineral Spirits* A - Mineral Spirits alone* B * 50% resin in mineral spirits C - 100% w"w ' D 500% w it n 1 - 600% " (actually used 550% resin) DUP050316525 7^ i I Gt Ba and 1 filtered and dried very slowly, especially E which did j not become entire dry after 65 hours in the oven* j The only evaluation thus far has been to attempt to disperse in resin solution as was done with, the Hansa Yellow, A and B give very poor dispersion, 0 is slightly better than B and D is quite good though hardly equal to the yellow or to the red in 493-2 series* * ' : N*B* 493, pp. 20-24* j The following preparations were made in the Technical Laboratory at the Dyeworks under direction of Mr* Martone, together with printing tests of the inks prepared* Ink $1 493--4A - 12 gms* RH-35-D - 75 " Solvent Naphtha - 92 ec Ink #2 493-2A - 12 gms* K5-55-D * 75 gms* Solvent Naphtha - 92ce Ink #3 Ink #4 4932B 18 gms* (12 gms* pigment-6 gms* .RR-35) RH* 35 --D -- 69 gms * Solvent Naphtha - 92 ec Ink #2 50 gms* Resin solution - 10 @ms (75 gms* Resin ] (69 cc solvent Naphtha] Ink #5 Ink #2 - 50 gms* Resin solution - 40 gms* j j i \ j J * s j \ ( I Ink #6 493--4D - 45 gms* (12 gms* pigment 53 gms* RH-35) RH-35-D 42 gms* Solvent Naphtha - 92 ec Ink #7 Ink #6 - 85 gms* Resin solution - 20 gms* Ink #8 Ink #6 ** 25 gms* Resin solution * 25 gms* Inks #1 and #2 were smooth in texture but gave a dull finish* By increasing the resin in the mixture as in #4 and #5 the finish wqs greatly imprbved until #5 represents the desired finish as near as can be told with the available tests* Likewise Ink #5 was quite dull but it also was poor in texture due to poor dispersion* Ink #6 was obviously dull and was not printed while #7 and #8 were definite improvements and #8 again appeared to have th4 desired gloss* DUP050316526 The inks showing the desired gloss show the following . approximate compositions;- Color BB55--D Solvent STaphtha Hansa Yellow 7*% 45*0% .j MLM . 100*0% 493--SA 4*0% 50*0% 46*0% To6*o% 493-4 3*6% 50*4% 4Q*Q$ ido.0% DU P050316527 PIGMENT COLOR RESEARCH REPORT SUBMITTED BYi APPROVED BY: RUBBER COLORS / 7'3-" PILE: RBBBSR"C0LRS~ DATE: NOVEMBER 19 35, INTRODUCTION Laboratory work on a dry substitute for Rubber Blue YD was completed this month and semi-works development was begun. In response to a request from the Rubber Laboratory, a sample of Nsphthol Yellow Lake especially treated for use in rubber was prepared and given to them for examination. SUMMARY AMD CONCLUSIONS g study of the amofint of dye to be used in the Victoria Blue R Lake as a substitute for Rubber Blue YD was made and a slight increase over that previously used seemed to give the optimum combination of strength and yield. This formula was checked and then repeated again with a new shipment of dye and gave excellent results with tinctorial properties very close to that of Blue YD on an equal weight basis. It was set up as K-8047 and given to the semi-works for development* The first semi-works batches were tested as vat controls and found to be considerably stronger than the laboratory product, A lake of Naphthol Yellow S was prepared on the GM-401-D formula (50> lake on washed 30/13 alumina hydrate and treated with "Du Ponol WA Gone." and Diglycal Stearate). Part was saved as pulp and milled directly into rubber. The pulp was also made into latex dispersed color and all were tested against Rubber Yellow RD, The dry colors were green and clean against Yellow RD, The pulps were cArtier than the dry colors and the latex dispersed colors were very weak. This last was probably due to bleeding of the dye from the ammonia treated latex. Samples were left with Mr.A.J.Northem of the Rubber Laboratory for examination. EXPERIMENTAL DETAILS See notebook #461. pp. 170-178, 461-56. A further study of increasing the dye gave the expeeted increase in strength as well as higher yields. C (15 gms dye) appeared to be the optimum and wss chosen for semi-works development, 461-57, A check to 560 was very stood in all respects and was given K-8047. 461-58, Checks to 461-57 using a new shipment of dye were satisfactory end the shipment ws O.K. for semi-works use. The series also investigated the toner yield and resulted in the following approximate analysis:- DUP050316528 IS" -2< Precipitated Aniline Matter " Blanc lixe Special Base 54*0% 40*0 6.0 100*0% formula 461-59. A lake of Naphthol Yellow S on GM-401-D A & B finished, as dry lake* 0 and D saved as pulp and a mixture was made up into a latex dispersion which proved'to be quite weak probably because the ammonia in the latex stpped the dye. A and B were green and clean vs Yellow RD* DUP050316529 3*r~ -?' PIGMENT COLOR RTSSEARCH REPORT SUBMITTED APPROVED BT: BARIUM LITHOL FOR RUBBER. RL~407~:D <A ' 0 FILE: RUBBBR-eBORS DATS: NOVEMBER 1935. INTRODUCTION A series of ten batches of RL-407-D was made in the semi-works in an attempt to correct Yellowness being obtained in Rubber tes on plant and recent Semi-works batches. SUMMARY AND CONCLIJS IONS None of the Semi-works batches showed the yellowness or strength to which objection is had* On the contrary all batches were close to standard in tint or even somewhat blue. The product obtained on standard formula was about 3% weak; some of the"variations added to weakness in rubber although aril were strong and yellow by rubout* Batch size may be a possible explanation of the blueness obtained in this series. 0*1 mol charged were made as compared to the 0.6 mol featch last made in the semi-works and 1.0 mol plant charges* Increasing para soap lQOyb and reducing sodium acetgte both gave weaker rubber tests. A similar result was obtained by making the tonefon the acid coupling formula, K-7290* Developing at 170 instead of 150F added &o strength to a very slight degree. A 50c/& reduction and omission of ammonium chloride increased blueness without effecting strength. This may be worth a trial in the plant. An attempt was made to duplicate the highly alkaline coupling which has been found, to give blue dirty products by rubout probably more suitable for rubber. In rubber this reduced strength .. slightly. Of three other lots of Tobias acid used, none showed any difference in rubber test when tested at the same time. Two of the lots are graded slightly yellow versus standard but were er.ua 1 to the control batch. DUP050316530 O d 13 rH O 43 ffl rH di rH d <G <H 6 43 J> a0 m> * *> A * 44 O d rH 43 6a >M 0: r (D 44 & O rH rH 0 t>9 0 ra m p ffl & tn 10 ffl 44 44 44 44 0 0) t> FH CS ffi ffl i> 3gR 0 & & Pi era rH 0 c<3 rH 43 d H l &g rH 0 d i--i d f3 0 O 43 >> w rH rH 1--1 a 0 t rH H r--1 0 a. !>a r3 H , O 0 * w 0 S3 g ffi O rH rH rH O rPjc^ rH O O pH l O He u S-4 UD W UD +=* -R i3 S P +3 CQ O O Ow o P P P 4 Hi 0 rH e p P P O0 0 83 0} > u p ffl * > ffl I& e' w <=8 en & S3 & f3 g: rt o 0 6C P O O O cti 1--f Pi g S rH 1--1 rH 0 i--1 t p ffi O rH rH rH rH rH ^ ffi O rH rH JCj >> ra * ffi * 1--1 CQ O h rH PO m . O (SH 0 # 0 1--1 O >c*5 i> P P Pi P 'ffl 43 Pi P pp 43 % P eg 43 . 43 p<*S 43 1, t 44 UP 44 c 43 44 P 4-3 pp DC w g Pi <H Pi P rH MC Pi 43 rC 43 43 s W H 08 P p rH Pi d 43 Pi x) 4D P P >H H ffi oD d ih Wj H US) UD nH -H 02 tH d 6 i--1 0 <* *e D 6 rH * Pi rH U 1 d O 03 O O W ! C8 > )> O 43 43 CC 4= Pi d c3 i'~4 ffl d m 43 d P Pi Pi O ffl <t-i O M O O E- lO ra ffl=3te O Pi * O IP S3 H 0 P P P4*$ 02 0* K 02 cs 0 <a P nj H1 Pi ra p t> Pi O^. WO 10 OJ >3 r3 t O l> o 0 02 t> r 1 r3 W (K Sh p O *rH 43 PE O rH \M t fl O a R Sfe tra 0 3 ra d t> Pi -J*. p0 dm H O sh |T[ P H a 0 p 0 SM O PI m -h 0a 0 tjDQ 0 CH Pi PM-H T*J P* O O ffl P O rH $3 f3| Pi*fH dda O 1H O ra p 0 rH PC 0 Bh 2d P rH S3|IP ffi rH d cc lO _ t H 02 Pi m 43 rH -H 43 d * 43 t?> o So3 -4* ^ Sh *rl C- <Pl c- E> 4h h, 0 >d 43 to H 1 1O 1 Pi tP O 03 d e- to rH o 45 iff <8j CO fee CO 'O' &! ffi ac 0 a. CO 4S S3 S3 O cc U OO 02 di a H ra fi P rH Pi M 44 M 44 O 43 rH ta 43 0 oCQ r-l a'* d> O tH 42 OP ta O CQ Pi O <13 44 44 O O_ 44 0 & 43 O 43 j 3 43 43 p rd S O BH O -rl O Pi 0 t0o ^ 5 43 d O "rl 43 O M O IP cd rH d * o- 0 co <m 02 m * 0 C c- 0 d *rl O 03 P P ffl O ffl P ffl d w 43 w fl O OOlH M S 02 C- 44 O ffl 43 Ll Bf- Ol Cti e- o> era CS CO CV2 W CO tO era m * "41 Hi H* -4> <# CO > ts frp O E- O c- O 3 -4t e- 7461 check 7427 except use TGb l o t s * lig h t 156 b rig h t y e llo w s 0s tr * & clean y e llo w v as . s t r . , s .y e llo w & clean I DU P050316531 7^ PIGMENT COLOR RESEARCH REPORT PARA RID - BLUE SHADE SUBMITTED BY: APPROVED BY:.-; <BsOC<d* FILE; BtfWfc-ffflB* A,3/^ DATE: NOVEMBER 1935. INTRODUCTIOM- lines: Investigation was conducted along the following A - The function of Para F; B - Its relation to filtration* G - The replacement of Para F hy structurally similar dyes. D - Formulation. SUMMARY AND CONCLUSIONS A* From evidence presented in previous reports and certain data included herein, it is concluded that Mono-sulfonic-acid F imparts a dark shade to Para Red as a result of its coupling with the. diazonium salt of F.N*A* forming the soluble dye,Pars F. The dypstuff is carried down in co-precipitation hy the Psra Med, and the darkness of the product is, among other things, a function of the amount of Para F present, and the pH of the medium* The pH of the medium determines not only the color of the Para F by nature of its indicator action, but also the amount of the dye retained. Solid solution^, or sub-mieroscopic mixed crystals of Para Red and Para F, is postulated* No experimental proof of homogeneity is planned although x-ray patterns would furnish further insight into the nature of the micelle, Para Red and Para F were shown to possess, under certain conditions, similar crystalline form. No doubt this similarity is an attribute of the similar molecular, or spatial structures of two substances, which governs very largely the solubility of the one substance in the other* It seems not improbable that these substances could form mixed crystals, if the variables of composition, etc. were such as to fall into an appropriate part of the phase diagram* It is well knownn(Freundlich: Kspillarchemie, pp*457-66; Leipzig, 1922) that foreign substances which are adsorbed but which canhot enter the crystal lattice will impede the velocity of crystalli zation, and further that such dyestuffs which inhibit the velocity of crystallization may color the crystals* Apparently, dyeing of the crystal and diminution of particle size go hand in hand. If there is a change in'par tide size involved in Pore Red B, it is difficult to say just how significant it is tinctorially. At the present time it ap-nesrs quite unimportant, not only because RT-7Q-D types may be converted to RT-22-D types without a change in particle size, but primarily because other factors afford more ready and promising sources of study (see part D), B* It has been reported tht the rate of filtration diminishes with increasing Para F content*In the eases to be cited in part (C) it was observed that the rate of filtration of a dark Para Red practically parallels the rate of filtration of the soluble dye used* For s slow filtering dyestuff, the Para Red acts as an assistant and filtration proceeds more rapidly than for the dye itself but much more DUP050316532 7f -2- slowly than for BT-22-D. For the rapid filtering pigment dyestuff PNa BOH, the Para Red behaves as a slight retardant in flltretion end the resulting rate of filtration is slightly more rapid than that of RT-22-D* Time measurements were not accurately taken, but it is planned to do so in the future. Further, it has been observed that when a Para Red Pare F pigment is developed and filtered hot, the filtration is rapid, but on adding cold wash water, the rate of filtration falls off markedly* Since soluble salts ore not precipitated, and Para Red is not soluble in hot or cold water, it appears that only the dyestuff and possibly the Para oosp are concerned. When Pnrp^Soap is omitted entirely, the rote of filtration is not increased^Wn^e it is probably not a governing factor. The temperature drop upon adding wash water is sufficient to cause some precipitation of dyestuff, at least to a point of turbidity and this is collected in the interstices in the filter paper forming gelatinous film which retards the rate of filtration markedly. This is observed on filtering hot pseudo-solutions of pure Par E While it is entirely possible that the Pars F in solution may prevent agglomeration, the behavior of hot filtration appears to indicate that Para F itself is responsible for the tedious-' ness of filtration of dark Para Reds* Hot filtrations with hot water washings, and salting out experiments are planned. 0. Several dyestuffs were prepared es possible substitutes for Pare F. These were in all cases benzene-azo-naphthalene derivatives in which there was a hydroxy group ortho to the azo bridge. This requirement permits the use of alpha or beta naphthols. It was further required that there be a nitro group ortho or pgra to the nzo link. In accord with the rules of Koenig and Angeli, and Bison's principle of Vinylogy, the placement of the nitro group in the ortho or para positions should not markedly alter the characteristics of the compound. This arrangement of functional groups constitutes the unit which gives rise to the purple-blue coloration in the alkali test for Para F* Indeed all the substances prepared gave this color test, presumably through double qulnoidization and nitrolio acid formation (J.Soc.Chem.Ind. Japan 29, 132; C.SJ.20, 3000)1 Para Red differs from these dyes in not having a solubilizing group, and while it*does not give this color in aqueous caustic, it will if first dissolved or 'wet with alcohol. These dyes were expected to give the same type of indicator action and it was hoped that they might be sufficiently similar structurally to form mixed crystals with Para Red. Table of dyes studied' PHA Schaeffer's lait 2 PHA Chromotropic Acid, MHPT ~> " EKA * BOH) MHPT Mono Acid F FHA ->HBS) PNa -> Chromotrpic Acid - PNA -*NAS) All substances used were retained by Para Red and produced dark masstones of the RT-70-D type. PHA - Schaeffer's salt was not incorporated due to its extremely tedious rate of filtration. The last three substances are pigment dyestuffs and were therefore necessarily incorporated in a manner xmlike that used for the soluble dyes. The soluble dyes were DUP050316533 dissolved with the B.N. prior to coupling whereas the pigment dyes were prepared and incorporated simultaneously hy mixing the B component in with the BN Using PITA-> NAS and PNA -">NBs, dark Para Reds wees obtained* These filtered rapidly, but were too yellow in undertone. They may be of interest if a yellow undertone is desired. The same is true of the products obtained when the two MNPT dyes were used. Acid dyeing and top chroming on wool of Para F, and the MF1PT dyes indicated that ahelation does not readily occur in these dyestuffs. This is in agreement with publications (Mason: J.Soc. Dyers & Colourists, 48 295 (1932) etc.) on the internal chelation of Para Red# From preliminary studies of the coupling of FNA to ehromotropic acid it seemed possible to obtain a blue dye which could be formed at a rate comparable to the formation of Para Red. Since the supply of ehromotropic acid was smsllqi it was decided to replace the Mono Acid F in K-6673 by this substance. The product obtained was distinctly brown. Coupling under these cohditions the dye was then prepared separately and the reddish-brown mono-szo dye was isolated. In order to prepare the blue dye desired, two moles of PNA diazonium were used, and the product, apparently not recorded in Colour Index was isolated as a ourple-blue dyestuff* (.probably the blsazo dyef# This substance dyes wool a bluish red and on top-chroming gives a blue-black color. It precipitates on alumina hydrate giving violet to blue tints. It proved to be very powerful in altering the shades of Para Reds. Unattractive browns were obtained. However, it is planned to incorporate minute amounts in future runs since this dye produces an increase in filtration rate and softness of texture. It is inexpensive and effiesrious in minute amounts. PITA--frB.OIT was incorporated by mixSLng the BOK with the BN prior to coupling. Replacement of the soTuble Pars F by this pigment dyestuff gave a product which was very soft in texture and filtered very rapidly without any bleed. Only one-third of the amount equivalent to Mono-Acid F was required for equal darkness of. mssstone. Development is desirable, alkaline washing is definitely to be q t o ided. The product appears to hsve nearly everything but brightness. It is too brown in masstone. Further experimentation will be conducted along these lines* From the foregoing data it appears conceivable that dyes or insoluble colors containing fibaadttcaad.1 groups properly arranged spatially may be used more extensively in blending colors, and that the results may be expected to differ widely from thoseobtained by dry mixing. A dry mix of Para Red and Para F produces barely discernible results as compared with the standard Para Red B preparation. DUP050316534 4 D St appears that the depth of color is determined hy the mount of Para F retained more than by any other single factor. If Para F is incorporated prior to coupling and the BN is kept in solution during coupling in a medium of NaOH and NagGOg, dark masstones are obtained. If, however, all other things being equal, the BN is precipitated from the NaOH solution by NaHCOg, the Psra f may be seen to occlude to the Bn , statistically offering greater opportunity for co-precipitation and actually darker Para Beds are obtained. By the same reasoning, if Para F is present prior to the precipitation of the BN by NaHCO,,, darker products should be obtained than when mono-acid F is used. This argument in favor of replacing Mono-Acid F by Par F has not yet been tested. The amount of Para F retained was studied more quantitative ly and the results show a relation between depth of color and the amount retained. In a consistency series, the average loss of Psra F by bleed in an NaOH - NaHGOg coupling medium was determined by precipitation methods and was found to be 0,8 grams per M/10 coupling. In a con sistency series the coupling medium (#270-600) which was reported last month as showing promise, the average loss of Psra F was found to be 1.7 grams. The difference in these figures is sufficiently wide to be significant despite the inadequate control of temperature, pH and salting-out effects. Bata along these lines have indicated scans information with regard to Para Soap retention. The masstones of the 276-6QC type re correspondingly lighter than those for products of alkaline coupling media. Qualitatively this difference in masstone may be expressed in terms of the amounts of Pars F used, 1*5 grams of Psra F in the alkaline coupling method produces darker masstones than 2.5 grams of Para F per M/10 in coupling method #276-600, The advantages of this latter method, viz,, rapid filtration rate, softness of texture and a questionable increase in brightness, become meaningless in view of these data, insofar as these same properties obtains;?/ when a diminished amount of Para F is incorporated in an alkaline coupling medium. The inefficiency of method 276-600 necessitates its dis continuation. It is difficult to say how significant the indicator action of Para F is, since alkaline treatment not only darkens the color of the residual Para F but removes definite amounts at the same time. It is evident that the extent of washing an alkali treated Psra B will influence the final color and texture. In a series with varied washing it was found that the smaller the extent of washing, the darker and harder the product. The darkness is probably governed by Para F alone, whereas the hardness of texture may be due partly to salt as well as Psra F* In a series studying the inflxience of development and alkaline treatment, the decrease in yields correspond to the loss in Para F; i.e. the higher the temperat/ure of development, the greater the bleed in filtration and. interestingly enough the darkness of masstone fell off correspondingly. Assuming that yielfs indicated the amount of Para F retained, a just comparison was available in this series, whereby the influence of the indicator action could be determined. The alkaline washed sample presumably containing an equal amount of Para F ws darker than the sample developed in slightly acid medium. It appears that the indicator action of Para F is a real factor but that the amount of Para F retained is a more \ DUP050316535 kignifleant one* Actually, a very dark Para Red was obtained by coupling in an HD1 medium. It is known that Para F may be salted out by HC1, and this might appear to indicate that the darkness was due to a very complete retention of Para F* The yields and bleed are in agreement with this. However, just how much brownness resulted from decomposed diazo, etc* is indeterminate. It seems evident that darkness is among other things very largely a function of the amount of Para F retained and it is planned to study methods of increasing Para F retention to a maximum* Para F control is of utmost significance insofar as it appears &t the present time that increasing amounts of Para F increases hardness of texture, brpwness* time required for filtration, and the bleed in filtration.' All these objectionable properties are properties of Para F itself* The incorporation of PHA ~*BON in plsee of Para F avoids all these difficulties with the exceution of brownness, but it gives somewhat browner masstones than Para S' at equal depth. It is hoped that brightness may be imparted to the BOH product. It is of technical interest that it is unnecessary to warm the BF into caustic solution. The Para Soap may be used for a two fold purpose. It will disperse the BF sufficiently so that it will dissolve in the caustic under standard conditions by simply stirring 10 - 15 minutes at 26G* Further investigation of the Uhlichsample C-38319 afforded additional informations Extraction with caustic showed the C number to contain Para F. Assuming that extraction is a measure of Para F content it appears that the Uhlich sample contains about as much Para F as RT-7Q-D {The relative figures are 1:1 gr,,, 0*9 gr The difference probably lies within the experimental error)* It is now possible in the laboratory to match the darkness of the Uhlich masstone with considerably less Para F which not only represents a saving, but increases the rate of filtration and the softness of texture. Brightness has not been matched as yet and for that reason the attractive features of PUA --*B0N warrant further study. C-38319 is not as bright as the previous Uhlich C-36670; nor is the blueness of undertone as deep* This blueness is patently not due to the use of some other dyestuffs as initially suspected. It has been found possible to approximate this blueness in the usual manner bp baking of the dry pigment* Drying overnight at 105G produces pronounced changes. The nature of the change produced by baking is not clear at the present time. Investigation is to be continued* DUP050316536 6 Series 490-5. The influences of alkaline washing and development in coupling method #276-600* Page 20 - Rubout comparisons of various samples, including Paul Ohlieh's 0-36670, > Para Red B Series 490-4,, The influence of washing an alkali treated Page 26 Preliminary studies of the coupling 6f PEA to Schaefferrs Salt, chromotropic and Metsnilic Acids. Series 490-5* Consistency series in coupling method (with development). #376-600. Series 490-6* Comparison of Para F loss in method 276-60C and completely alkaline coupling media* olive oil* Series 490-7* Para Boap. Turkey Red Oil and Bulfonated Series 490-8*. Tfce influence of alkaline washing and development in coupling method #276-600 using Mono Acid F* Series 490-9* Consistency in alkaline coupling and the effect of developing at the boil* Series 490-10* The coupling of MEPT to Mono Acid F, and Schaeffer's Spit* Series 490-11* Aeid dyeing and top chroming on wool of Pontaehrome Blue Black, Para F, MNPT - Mono Acid F and HNPT Schaeffer's Salt* Page 50* '^he purification of samples of Para Series 490-12. The incorporation of PEA - chromotropic acid, M38PT - Mono Acid F, MEJPT - Schaeffer's Salt in Para Red pro ducing dark shades* Series 490-15* The dis-azo dye from the coupling of two moles of FNA to chromotropic acid. BON* Series 490-14* Coupling PNA to Sehaeffer's salt and Series 490-15* Incorporation of the dis-azo dye from chromotropic acid in Para Sed# Series 490-16. Replacement of Mono Ajld I by BOH* Series 490-17* The incorporation of PE'* - NAS and PITA - 5TBS in Par a Red* Series 490-18. The baking of dry pigments and further investigation ol Paul UHlich's sample o-aasls. DUP050316537 fo? PIGMENT COLOR RESEARCH REPORT CALCIUM LITHOL SUBMITTED BY:IP?.A APPROVED BY: JU FILE: L^SGLS- % X A,// DATE; NOWBER 19 35. INTEQDU CTTON With the stabilization of the straight TOB-BN formula 472-55 (a light mssstone Salcium Lithol for rubber) work was resumed on the TOB - BN plus Mono Acid F formula, a dark mssstone Calcium Lithol for printing ink and paint purposes. SUMMARY AND CONCLUSIONS Modifications (increase in time and temperature of coupling) which were of advantage in the straight TOB - BN formula, were employed in the TOB - BN and Mono Acid F formulae The duplieability of this formula was unsatisfactory. This seemed to be due to a faint excess of diazo which remained after coupling in spite of a slight excess B.N* The duplioability was improved to o certain extent by a 2$ increase in B,N?, this causing, however, a loss in depth of mssstone* The desired depth of mssstone was regained by an increase in Mono Acid F but with a sacrifice in brightness of mssstone; also bronziness of undertone was caused. It seemed that the less in brightness was due to precipitation of a part of the excess BN during strike with calcium chloride. An effort was made to prevent this. By increase in volume of strike, also by striking at slightly higher temperatures, no advantages were gained* An increase in alkalinity would make a proportional increase in ammonium chloride necessary (to prevent forming of calcium hydrate) which also would throw B.N. out of solution. Material of very dark masstone with blue tint was obtained on the straight TOB - BN formula by (1) adding an alkaline solution of TOB to a beta nsphthol solution containing nitrite, and then obtaining immediate coupling by acidification. (2) coupling at 0C; in both cases normal yields were obtained but these products were very poor in light fastness* Bluish material for shading of the rubber Calcium Lithol, 472-55, was produced by striking at the boil. The maximum blueness seems to depend on volume and time of boiling. Further studies are required to develop this formula (472-65) which is rather inconsistent at the present time* The latest formula for the dark masstone, blue tint Calcium Lithol for printing ink and paint is 472-61C* Compared with RT-379-D standard, this product is dsrk in masstone, about 15% strong, cleaner in tint, softer in texture, and slightly better in oil bleed. Suhequent studies will be directed towards stabilizing formula 472-610. DU P050316538 vwuwr' 9<" -2- reyp-aqiimiTAL DETAILS Notebook #472. 472-460 Developing the diazo in the combined alkaline solution of T.OiB. B.N. end sodium nitrite by addition of Hydrochloric acid# This resulted in a very dark bright masstone of good strength, bluish tint but very poor light fastness* 472^58* Duplicability test on the T*O.B, - B.N. Mono Acid F based on 472-44 with modifications of 472-55 such as increase in coupling time from 5 mins, to 15 mins* ito avoid local zone action) and increase in coupling temperature from 5 C to 10C Consistency was unsatisfactory. 472-59* Variations in the amount of B.N* formula). A - 2*0% below theoretical amount of B.N* (control B - 3*2% excess over n " "" C - 8*3% "" " "" D -16 *6$ w" " " " * (based on 58 The endpoint after coupling and digestion for one hour showed a strong excess diazo in A, faint excess diazo in B, and strong excess B.N. in C and D0 A being only very slightly lighter and slightly less bronzy than B. Increase in B.N. resulted in an increase in lightness of masstone p and bronzier undertone. 472-60* Duplicability test on 59-B. Two couplings on straight 59B and two couplings with an 1*7% increase in BN* Endpoint on the straight 59B formula showed a faint excess diazo besides a slight excess B.N. The 1.7 Increase in B.N. showed a slight but distinct excess of B*N. and no excess diazo. The lower amount of B,N resulted in a darker product but of poorer duplicability. The duplicability was satisfactory with the increase in B.N. but the masstone changed to a lighter shade* 472-61. Increase in Mono Acid F (on 472-60C formula?* A 20% increase in Mono Acid F darkened the masstone, contracting the lightening effect of the larger excess of B.N. The B.N. was proportionately reduced with the increase in Mono Acid F figured as 70%. Te 610 and D (40% increase in mono acid S') ended with a faint excess in diazo* 472-65* Duplicability test on 472-61C but with a 1*7% Increase in BN to avoid the ending with a faint excess in diazo. Four couplings, three of them checked substantially, one resulted in slightly darker products. 472-65* Duplicability test on a formulation of 478-55 (T0E-BN) but sodium salt diluted and struck at a boil to produce a dark bluish material suitable for shading rubber colors. Consistency series was poor* DU P050316539 -3' 472-66* Duplicability test on 472-63 (three couplints) Consistenoy was fair* 472-67* Variation in boiling time of sodium salt studied on 65-A formula: 5 minB, 10, 20, 30 minute boiling; 10 minute boiling resulted in the darkest and bluest products, 472-68* Duplicability test on 472-63* To check results of 472-66 series* 4 couplings# Duplicability was fair* 472--69* Variations in strike volume* A higher strike volume was considered to prevent precipitation of free B.N* which seems to cause silkiness and fullness of masstone# Results: no considerable improvement* ''w w mmms u . DUP050316540 FISMMT COLOR RESEARCH REPORT CALCIUM LITHOL TQ3SBRS, RT-379-D ABB RT-300-D AT- BATE: NOVEMBER- 1935 IBTRQPPCTIOBr Pour batches of RT-379-D were made in the plant under Development Section supervision, reports on only three of which are available. As sub-standard stock is quite low on this color there were no special requirements for shading material. One batch of RT-300-D was made in the plant with material satis factory for rubber being required. SUMMARY & CONCLUSIONS There are two basic formulae on RT-379-D being used in the plant at present. The first, used to give dark material, introduces the following variables (on a 1 mol batch si2e): 65$ TOB - 35$ T0BT7 in the diaao, 82 lbs. caustic soda in the Beta Haphthol solution, 320 lbs. cal cium chloride, struck after bringing to development volume, development temperature 140P. The second, used to give light material, is varied from the above as follows: 75$ TOB - 25$ TOBlf in the diazo, 79 lbs, caustic soda in the Beta Maphthol solution, 160 lbs. calcium chloride, struck in coupling volume (before dilution), development temperature 160P. The first batch made this month was made to check the basic for mula for light material. The customary light and flat masstone, OK strength material was secured. The next batch was made to check the formula giving dark material except that the calcium chloride used was cut 50$ (as used in the light type formula). The resultant color was s.dark and muddy in masstone and strongerfthan the RT-379-D standard. The third batch was made to check the second except that the diazo variable of 75$ TOB - 25$ TQBW was introduced and the color was struck in the coupling volume, before dilution. This material was only v.v.s. light on slurry control but the grind sample rubbed out s.light and flat vs, the standard. Part of this change was probably caused by in complete quenching of this batch after development (quenched to 130P instead of 110115P) due to lack of space in the development vat. This difficulty is sometimes encountered when making 3/4 mol batches which are developed in a 5000 gallon vat. A sufficient quantity of ice in the quenching water to bring the temperature to 110- 115E must always be used in such cases. A satisfactory 1517 lb. mix has been made consuming all sub standard material outstanding from last month. Results on this month's production are tabulated in Table I and the mix in Table II. DUP050316541 2 The RT-3Q0-D hatch for rubber ms made as usual using the standard K-7038 formula. The resultant color tested satisfactorily in rubber, and has been placed in standard stoclc for rubber shipments * Results on this batch are tabulated in Table III. BEPBRIMEHTAI, DETAILS ET.B 433, pages DUP050316542 fblOooPKC H CO ft P P 3 & cr 4 1 ca O 02 3 O rH O rH ft CO <ef< CO H >H +S tn p ft a O rH 0 CO <w p p rl Eh *P CO v 4? O ft 1 CT> frCO Io Eh ff? P > Hf a > >% 4 tf H T* W O rH S3 >> $ rH O> U 4* >> t a "O rH ft "8 O H -p U is g eg| u 4S rH > > 09 S$ fPt S3 o C5 -gp Ih . .OA <H f-pt X} 8 44 Xas) *0 tg rV-il Vo "fP*t > 0 i p 1 H S S > 1 P Eh *3 *0 <0 O rH g 0 g1 a* tro- o OO 03 <0 t 4* Ai rt rH cPa .S3 H WD 0O *H 0 > M ft ft P BW O H O O rH ft rH ft St to ca -H K ra 01 -a S3 *H O* ft i*3ss 0 EH -p 0 ft *MP Eh -P O ft CV? CO ft l> ft ft ft pa rH t CQ ft CO tO V. ft ft CO 03 CO f CO ft ft to to & ft H & sq.<MK>.>>,, 0t-.j4 CO O ft CfOt OS tD ft co <0 a IEh p o rt 4 rt 6jO W o *fHt H 4* .O 13 T3 JU u "d -p p CO <ri *P CO ft 6 <^1 t~ a 2* W O <D 3 to p cs o -p & T3 P m > -P W d p V? 09 i> > ft ii Eh I trH in rH I I CO m o o C3 m *4* tO CO S \ t g; CO to C3 00 CO fgt 3fr 33 frCO O f fCtQ CO om co t> CO o tn *11 d 1-3 4 *K CO ft *4 Jft3 fPt S5 O tj M Eh 0$3 ft sffMtt 8 o t! t o ou cn -p S sft Q " OS ti m 3ra 1 s a; OgHiNsl @ +?} g3! <0 J3I puIl 46277 Check K-7038 156 11.4 vs I t , s.brown w s y e l. w s wk. s td . RT-300D vs y e l. OK- vs y e l, s .d rty 305 298 OK fo r rubber & d irty & muddy DUP050316543 BISMBHT COLOR RESEARCH REPORT BARIUM IITHOl TOHER, RT-364-B s^~~ joy SUBKITTEP BY* t KBmOVm BYi , ISTRGDUGTIOI? VXUSs ^hPTSGLS- -? d a t e s mmwmR- 1935 Production on this toner -mas continued in the plant under Devel opment Section supervision and a total of three hatches are available for report. Slightly dark, slightly yellow, and strong material was desired far shading purposes. SUMMARY & CONCLUSIONS Because of the fact that the recent modification of the acid coupling formula on this toner (addition of the ammonium chloride after completion of the coupling with caustic soda) gave weak results it has been found necessary to revert to the standard procedure of adding the ammonium chloride to the neutral Beta naphthol solution before coupling. The first batch was made to check the standard K-7290 acid type formula except that the caustic soda to complete coupling was increased by 2 lbs. per mol (55#- 57#). The resultant color was dark and weak vs, the RT-364-D standard. In the next two batches the standard formulation was followed except for a 33-1/3^ cut in the para Soap in the coupling (32#/mol in stead of 45#/mol). Both batches were fairly satisfactory being dark, v.s. strong and v.s. yellow vs. the standard. It may be noted here that plant batches at present are being dried at 165F because of lack of room in the Hurricane dryers which are set at 140F. This higher drying temperature is responsible for the slight ly out-of-line depth of masstone, and the lower drying temperature should be used when possible. Production is tabulated in Table I. DUP050316544 A BXPSRIMBHaL 1STAILS H.B. 385, pages 162-163 0 43 mp tO 4* ofe, in *o A 0 43 in P to -P rH HO H flj p *P 4 1C?d r4 JS P csj H S O o *d p-4 *d P O o h a H 4* ss; t. t* T3 rH P (O 1 xs 9 rH >4 H >< .p 03 63 O in CO O <> CO *P S3 e-* p Q *4 4< tO CO _ A.e J o o* oi i* Ol (0 P rH tPfi SQ3 m .p & 89 $ p jh H TJ 44 <d > TJ T3 i M *T3 P & _ a ss p o CO H rH P *> *8 P fc* + 4? r*? x` sf 'r O tn CO O to CO rH >v TO & Jh s u t u 4 m > > tj d 2 44 s44 U T5 *p fc* tn 50 S= *rl &3 H P -p O a$ i--4 2sS o &t 43 p -p m0$ fc" <o tn in r*4 6- oO> S215 CM C- rH ,1 O s*j a * 'tS fcp tn to 44. *pp< o o 43 K o ov O O to <J> to g o> CO O1 O* S3 CM fcia1 roH g S* P CO TO p 44 P< O O 43 X O m to rH to sh * to to iH m to H tO H* 44 P Si P in tn CM to DUP050316545 FIGMENT COLOR RESEARCH REPORT BED TONER. &-7S43 SUBMITTED BY: APPROVED BY: , FILE: Mieev-TeiigSS DATE; NOVEMBER 12, 1935, INTRODUCTION Ortho-chlor-para toluidine is an intermediate prepared for the manufacture of 2 chlor 4 amino toluene 5 sulphonic acid (Red 2B Acid)* Owing to the commercial availability of this intermediate, which apparently would be reasonable in cost, attempts were made to find a possible use for it in dyes for color lakes.* A number of combinations were made of which the R salt product possessed greatest promise* A search of the literature disclosed U*SF. 765.,079 issued July 12th, 1904, to BA and SF, covering the preparation of the combination of diazotized ortho chlor para toluidine and R-salt for the preparation of lakes* Therefore confronted with no legal difficulties, further orientation experiments were earried out* CONCLUSIONS Early orientation experiments resulted in a deep bluish red similar to Para Red but very much weaker than the latter* The possibilities of this product as an oil insoluble pigment, deeper in shade and faster to light than Para B appeared to be good, but the ex tremely hard texture and poor strength of the new pigment were obstacles which had to be overcome in order to make the product commercially attractive* Experimental studies on the action of variables were carried out with the object of improving texture and strength. These properties were greatly improved but only at a sacrifice of depth and blueness of the product* Pigments which, in dry form, were hard and gave inks of deep masstone, gave very much lighter masstone, very much stronger and very much yellower inks when flushed toto lithographic varnish. The flushed inks tinetorially were similar to inks prepared from soft dry pigment, which were very much lighter in masstone and yellower than Para Red B* The exceptionally bright dark masstone and blue shade of the hard texture original product, K-7843, gave merit to this pigment but since its inherent tinctorial properties appear to be light masstone and yellow shade, it now appears to be of no especial interest. This dye apparently possesses characteristics similar to Scarlet 2R (m-xylidine - R-Salt) and it may be that it requires a substratum in order to obtain a dry pigment of good tinctorial and desirable physical properties. Alumina hydrate-blane fixe lakes, although faster to light than lakes of Scarlet 2R, are much lighter in masstone than the latter. DUP050316546 - EXPEHIMEHTAL BETa ILS^ K--7843 the barium toner of ortho ohlor paratoluidine R-Salt was prepared from plant crude 0.C1.P.T, purified in the laboratory by steam distillation. K-7844, the alumina hydrate - hisue fixe lake was prepared from toner K-7843, 72 end 36* Expts. 1, 7, 19 ^ S3 and 261 NB 45Q, PP* 4. 24| 52j Preparation of dye of K-7843 from plant crude 0*C1*P.T* charge #la purified in the laboratory 10/9/3S by steam and vacuum distillation* Bxp. 58^ N.B. 476, p. 198* Dye 476-58 was employed in all subsequent studies* Acidification of the dye prior to laking results in weaker pigment than that obtained byaelftitloatfdnof the lake subsequent to development* Direct strike results in a very slightly darker but softer product than reverse strike but the differences are only slight* Para Soap improves the texture of the dry pigment* the omission of para soap resulting in a product even harder than K-7843* Expt. 5, N.B. 487, p.18* Increase in the quantity of para soap from 40 grams per mol to 60 grams per mol tends to give slightly aeftsran&d slightly stronger dry pigment* This slight Increase in strengtlLis apparently due to the decrease in hardness of the dry pigaent, since"fforrespohding pulp pigments flushed into lithographic varnish do not. show this increase in strength* Boiling strike results in an appreciably softer dry pigment than one prepared by 65C strike and subsequent boiling development The farmer is much lighter in masstone, stronger and yellower than the latter* However, no great tinctorial differences between these two pigments are apparent in the flushed inks. Even though the dry pigment struck at the boil is soft, as judged by touch test, the ink therefrom is very such weaker then the corresponding flushed ink. It may be that this dye possesses characteristics similar to those of Scarlet 2R dye end requires a substratum* Expt. - 9, NIB* 437* p* 32* Increase in volume of dye solution has no appreciable effect on the tinctorial and physical properties of K-7843* k lake prepared by the Pigment Scarlet RL-211-D pro cedure is very hard in texture and poor tinetortally* The flushed inks are much lighter and yellower than Para Red B, RT-70-D and since the tinctorial properties of the flushed inks may be assumed as the inherent tinctorial properties of this pigment, DUPO 50316547 the merit possessed by the original dry product appears to exist no longer* Ixpt. 10* JF.B* 487, p* 36* - SUMMABY The preparation of a dry toner pigment from ortho chlor para toluidine and R-salt as an oil insoluble faster to light product than Para Red B, but at least equal to Para Red B in depth and shade does not appear practical since the apparent inherent tinctorial properties of this new pigment are much lighter and yellower than Para B* Although the alumina hydrate**blenc fixe lake of the new pigment is oil insoluble and much faster to light than lakes of Scarlet SR the former is much lighter than the latter in masstone* REG OMMSHBATIOHS It may be possible to obtain an oil insoluble, fast to light Scarlet Lake of the Scarlet SR type tinctorially by shading the lake Of subject pigment with Lithol Red Deep, RT-284-D or with Maroon Toner, RT-365-D* DU P050316548 mamws c o l o r r e s e a r c h r e p o r t LITHOSOL RKD 2B LAKE KM-7909-D AND TOMR RT-7853-D /% STXBIffITYKD BY: C.y^kw APPROVED BY* ^a<Ce^^^r PILE: KSS^r-~W51ffiBS` DATE: NOVEMBER- 1935 INTRODUCTION Production in the Semi-works this month on the toner and lake of Lithosol Red 2B consisted of test hatches made on the new lot of dye* lot 4, preparatory to starting plant manufacture. Two batches of the lake were made and one batch of the toner. SUMMARY & COITCLPSIOB'S Both lake batches were made on the standard K-7909 formulation. Toner vat control results in both oases were light versus lot 4319, RT-7853-D and the respective lakes were also considerably lighter than K-7909. The two lake batches checked each other very closely. A small toner batch was made in the Semi Works using the old standard toner formulation K-7745 in order to check Raw Material lab oratory results using this formula. Results on this toner were sub stantially the same as the toner vat control results in the case of the lakes, the material being considerably lighter than lot 4219. The Raw Material testing laboratory secured slightly dark results using this formula, but a check run made on the K-7853 formulation was light in masstone versus the control. As two different samples of dye were used to make these laboratory tests, the wide variation in results is no doubt due to non-uniformity of the dye pulp, which fact has been noted in Semi-Works results on previous lots of this dye. On reeeipt of a special lot of dye to give darker material, test batches will be made in the Semi-Works and, if satisfactory, depth of masstone is secured, production will be started in the plant. Results on the toner batch are tabulated in Table I and on the lake in Table II. DUP05 0316549 c* * *4 rH *W >H -P CO i H CN2 J5* I 3 C GW II coj 9 totn>ofli a] (4! *P E EH-i Os *8 H '" e p O 113 r-l ^ -P *% CO co m co c- "e S3 O > S3 Cj * G +3 03 It *P * *P u *p 3: bO SO Us *f* H bO flf o. fr- in 00 in I Q Q fltf *H S *H m <* bb- i PS p* O to to b- w M a CcOv o o O s *H E-i CSV 9CSV -*p* fr eft & g* ra A 3 OaS w o 0 iH *0 % < 0 8 *Q ^*ri sI 9 4 r4-5i CO *H rl 6-i co* 4V* CO> o b- t &* ed . 1 > H > >% U P t* P P H 8 J! I r-4 ,4Q0 s Q oo> o* b L H Sf PS o f**< g CO I in in b- DUP050316550 r? PIGMENT COLOR RESEARCH REPORT SUBMITTED BY; <$>&isCck, APPROVED BY: MAROON TONER. RT-354*D jj? Ji PILE: Mm. '/ DATE: NOVEMBER 1955* INTRODUCTI ON Work on this oolor was continued intrthe Semi-works* further study was made of the use of mixtures of Bremers Acid and ToMas Acid Regular to replace T.O*B*yy, A few other variations were tried to increase depth and brightness and several batches of light bright shading material were made* In addition, two batches were shipped to Parlin in pulp form as RT^ISQ-P.. In the plant two batches of RT-354-D and one batch of RT-130-F were made* SUMMARY AMD CONCLUSIONS Ko new variation of any value was discovered this month* Cheek results were obtained on the most promising modifications tried during October - a 50^ increase in calcium chloride gave a darker product with another lot of Tobias Acid and use of triple amount of sodium acetate consistently gave light bright material* Three batches of the latter type were made for shading SSS material* However, using only a double amount of sodium acetate had no beneficial effect, the product being sdark and brown* A recheck of the comparison in methods of employing the excess BON showed no difference between addition of the extra BON after coupling or addition to the main portion of BON, The latter procedure has been used throughout the series* Raising the temperature of strike from 85 to 122F gave a slightly darker but definitely browner product. Lowering the temperature to 6QF resulted in a lighter but not much brighter product* The difference is possibly due to the better development of the iron toner at the higher temperature* In connection with temperature it should be noted that it is now possible because of low water temperature, to reach 60 F specified for the addition of excess nitrite by dilution with water. This may have a favorable effect on depth* Trial of intermediate amounts of Brommers Acid showed that maximum depth is reached at 6fa which is the amount used in TOBW, All lesser amounts were lighter and browner. At 7fo the product was only slightly lighter than 6$* Higher amounts with the exception of 7*5^ were lighter and browner again. In no case was greater brightness together with depth obtained by use of Brommers aeid as compared to TOBW. Gradings on the complete series are given vs RT-354-B* ^SXii^xJKi^mKXXXXXXXXXXXXXXX^XX^^XX^x1^^^ DUP05Q316551 3% - light & browil** 4% - v*s.light, muddy W> - v*s.d,ark, s*brown 6% - dark, s.brown 7% - dark, s.brown. 7.5% - light 0% - s.light, s.hrown 10% - light, s.brown Two batches of RT-130-P were made on the Semi-works standard formula (SW-7305) with the exception that in one case sodim# acetate was doubled and the final boiling was omitted* Both appeared to be normal* In the plant an attempt to obtain depth equal to standard by increasing the BON resulted in a dark but brown product* It is possible that the alkalinity of coupling was too low* All precautions mentioned in the last report were observed - rapid processing of both halves of the soda salt, six hour washing, drying in thin (l/2 to 1 inch) cakes at 140? and grinding in the Semi-Works 12" pulverizer* A portion of this batch dried in the Semi-works was a trace darker but practically a cheek to plant dried material* A second batch was made on the plant standard formu lation (Lot 44076) with a 50% increase in calcium chloride in one half of the batch* Washing time was reduced to five hours and drying time was varied to give underdried, dry, and overdried material. On vat controls no difference was observed with the increased calcium chloride* However, it is believed the effect of the increase in precipitant would show up only in washing and drying. The drying experiment showed no differences between the various portions when tested side by side* All contained the same percent moisture (9 * 10%)* Some variation in testing was observed on this batch but when made uniform the final lacquer test was darker and only slightly browner than standard. It is readily shadeable material* Mixes totalling 3500# have been made up which although s*brown have been 0*Kfd for DuPont Plants* The plant batch of RT-130-P was made on the above formula except the extra ealcium chloride was split and a 25% increase made in each half batch. Control samples were dark and 0*K* in bright ness* The high moisture content of the last plant batch of RT-354-D (9-10% by toluene distillation) led to further study of this point* By loss in weight method a figure of 6,7% was obtained when dried at 190 F* At 155I only a 2% loss was observed* Standard RT-354-D was found to lose 8.4% on drying at 190F* It was observed that the redried sample absorbed moisture rapidly when exposed to air and in 4-l/2 hours had regained all but l-l/2% of its original weight* In the ease of the plant batch a very slight increase in brightness on lacquer test was noticed on the thoroughly redried material but a brown substandard lot showed no improvement by this treatment* DUP050316552 Oi Fittoo 30*6-*1 opt; a! *4 91 > o Fi x> pg- o +Fi o 4s XFIi xz rf-f4i > 133 >i AFdi a* (ft Ad & i3 o Ad. ft ft ra m t> Ad f *u F0t p A 6rHD H *> P Fi , ra rpt-4cft t> Ad 6e UO ,FQhft i0 ffi p affl I H'hH W >p ID A to ft 01 toft 01 ft# e O toft Ol <D c toft 0> 1#ft 01 to to OS to to ft a CD CD CO 0 CO $ o -tt) j>) H >>i*j Pi PP r-4 03 Pi o o ftd pq pq O C*O H03 O w Ora r-f H (3 30 K PP co co PO ft (J wH 0 Pi Cd t4 s CQ 9 OH A* CO cd S 3 p0 CO Pi Pd CG ffi OH Pi w s3w CO . ra *4 1-4 OP 03 AtO) a 3 ft X3 6D t t)0 ffl ffi ft--1. p Pffi ffi 91 3 CO K 03 P Ft P 3 p p +3 P t to t Pi O H PQ O 64 m 0 64 Q0 64 m O -ISPft^ ft# W S if t*4 O CM CM P=i 0 O to 6 'd 0 P o * o $ 3 9 a ft# to GQ P* O 13 o H >5 O ft. O P 8fes H P 1 If ft CO i4 9 &CO i> 1# CD 3 P, Pi 13 P OO M< U3 Ft O to a et=oa BS 3 Ad^S. <0 to CD ra 3 p PtP 0 0 <1 M Fi to O3 to 3 ECO t Fi isod * Ad ft# a> l to o> 3* P 13 Pip pj M Ft r-4 ffi ci n to 3 ECO *U m cq CO M* o Xl Om to r p PU OO iJ H A O CQ _ 604 sP P bD O pdffi 0 3 3 d* p t> to t- w Aad F-i Ji Osi OP to Pft-- 0 W) 1-i 3 P 1--f CQ Pi O3 64 O O to 33 p MP p <+-i ffi O CO <3 O C-- Ad *ffi & ^3 O O (Q H O P P ffffii XI P Ad PtP U OP w 3 to 0 O Vi to IN (fc) O Ad tO ffl 00 3 U OO p ffi M H P3 ffi Pp. W to 0 to O fti O Ad lO O 00 3d Vi 00 CO +3 g # cO X GQ <0 tft cAd jd 0 <0 ft# E1 ffi i ffi CQ tO <0 ft# E01 as CO 0 p| 0P3 PP U O Pf4fi 03 ffi uo <n 3 * 3 P 1--4 f-l CM f-i o Po p to #3 H 1 <0 64 * tN 01 Oto CO I?- * o co r-*4 E-i P5 Ad xozmPu o if ffl xz w d -- . 66 03 H O r-4 EftS# fftt## Eft#- CeHO- ttoo c- tCoM cft#- CM tOft>#p GO <0 IS tt>o ft# fis CtoO eft#- ttoo tfts# to to 0ft# DUP050316553 PLANT - N.Bo #475 Lot #45963 - Check present plant standard formula (Lot 45559} except increased BON from 192 to 195#* Alkalinity of coupling - very slight on Brilliant Yellow* Washed 6 hrs* Dried in 1/2 to 1 inch even cakes at 140%# At 30% humidity for 30 hrs* Ground in Semi-Works# Lacquer test vs HT-354-D - very dark, o Lot #46017 - Part of 45963 dried in S*W. fneas Dryer at 140 F Lacquer test vs 45963 - trace dark* Lot #46008 - Check 45559 (192# BON) except made a 507s increase in calcium chloride in one half of hatch. Processed as in 45965. Dried 50 hrs* Lacquer test vs BT-354-D - v,,s*light, s*brown (Retested s.dark) Lot #46035 - Part of #46008 taken from dryer in 26 hrs# Lacquer test vs RT-S54-|J - v.s. light, s.brown. " " 46008 - eaual Lot #46036 - Part of #46008 left in`dryer for 72 hrs* Lacquer test vs RT-354~-u - dark* " " 46008 - v#v,sdark Lot #46584 - RT-130-P for Parlin# Check 46008 except a 25% increase in calcium chloride made on each half of hatch# Slurry control vs RT-354-D - Both parts s. dark* Lot #16026 - Mix of 46008-035-036* Lacquer test vs RT-354-D - dark* DUP050316554 ) /*>/ J,S~-y?s*v PIGMMT COLOR RESEARCH REPOST MISCELLANEOUS LAKES AND TONERS SUBMITTED BY: APPROVED BY: BILE: JLSO*~LAS~ DATE: iTOY. 1935 IMTRODUCTIOH Research studies at Jackson Laboratory this month were confined entirely to the investigation of new intermediate produets for the preparation of color lakes* These studies included evaluation of new dyes for lakes, the preparation of azo dyes and corresponding lakes from new intermediates, the preparation of lakes from copper phthalocyanine, attempts to prepare the nitroso compound and iron salt of beta-thio naphthol, and the preparation of a lake from Ponsol Jade Green Supra for rubber* SUMMARY AND CONCLUSION'S Dyes and corresponding calcium and barium lakes were prepared from 3:4 dichloraniline 6 sulfonic acid combined with beta naphthol, betaoxynaphthole acid and R-salt* The resulting pigments in general possess no outstanding merit and apparently warrant no further consideration* The calcium toner of the betaoxynaphthoic acid dye is much darker, duller but much weaker and yellower than Para Red B, RT70D* The deep masstone of this product, which is non-bleeding in linseed oil and fast to light compared with RT-70-D, may mgke it of possible interest* Dyes and corresponding calcium and barium lakes were prepared from 3 nitro aniline 6 sulfonic acid combined with beta naphthol, betaoxynaphthoic acid and R**Salt* The beta naphthol and R**salt produets possess no outstanding merit* Lakes of the betaoxynaphthoic acid dye, including strontium and manganese toners, range in shade from an orange similar to Permatone Orange to bluish red* While the lakes of this dye are of definite interest, the outstanding product is the calcium toner which unlike the great majority of betaoxynaphthoic aeid dyes with which we are familiar, is a bright orange resembling Permatone Orange tinetoriall3 This apparently new pigpaent is non*bleeding in linseed oil and very fast to light, being very much more light fast than Permatone Orange, YT-S41-D in tint* Calcium and barium lakes of the dyes prepared from 6 ohlor 2 amino toluene 5 sulfonic acid (an isomer of Red 2B Acid) and beta naphthol, betaoxynaphthoic acid and R~salt possess no especial merit, the products being very much inferior to the corresponding pigments prepared from Red 2B Acid* Identification of Kentucky Maroon 0^37914, has been definitely established as approximately 75$ Toluidine Red (Meta-nitro- para-toluidine beta naphthol) and 25 percent mixed calcium and strontium salts of Lake Bordeaux B Maroon (Tobias acid beta oxynaphthoic acid)* Synthesis of such a product has resulted in a pigment resembling the competitive material* DUP050316555 -2 Aluraina Hydrate lakes of Ponsol Jade Green Supra were prepared from regular standard paste dye and the corresponding water dispersible dye# at the request of the Dyeworks "Rubber Laboratory* The samples made from the dispersible dye gave cleaner and brighter shades in rubber than the lakes made from the standard paste* The Bubber Laboratory is definitely interested in this product* Acid coupling in the presence of sodium formate of meta^nitro-para *anisidine and beta naphthol results in an appreciably darker and somewhat bluer product than the alkaline coupled product KV7699* Beta-thio-naphthol coupled with diazotized meta@nitro paratoluidine results in a soluble dye, the barium and calcium toners of which are very fugitive to light, oil soluble and poor tinetorially* The dye apparently is unstable, and attempts to condense the dye with sodium chlor&oetate and by oxidation of 2 moles of the azo combination have been unsuccessful* Attempts to prepare a nitroso compound of beta** thio-naphthol have been unsuccessful owing to formation of the nonreactive disulphide compound in the presence of nitrous acid* While this type of work is of interest the products obtained do not appear promising* Two new dyes, Sulfonated Lithosol Blue 6G (sulfonated Rhoduline Blue 6G) and Sulfonated Lithosol Blue G (sulfonated Aoronol Blue), have been investigated with the object of obtaining a Past Peacoek Blue# Alumina hydrate lakes and lakes of the phosphotungstic acid pigments, although faster to light than Peaoock Blue BL*72**D, are inferior to the latter tinetorially* The phosphotungstic acid pigments precipitate with difficulty, owing to increased solubility of the dye caused by the sulfonic acid group. These toners are much weaker, duller, and much greener than those of the corresponding unsulfonated basic dyes* Sufficient orientation work has been done to indicate that these new dyes possess no promise as straight P.T*A* pigments and dyes for lakes# With the cooperation of Jackson Laboratory a large ,, laboratory sample of Copper Phthalocyanine has been prepared for /'Bulux and Lacquer, durability tests* Blanc fixe lakes were prepared with the assistance of Jackson Laboratory chemists, by several procedures* Addition of blane fixe to the acid pasted pigment prior to preoipitation gives results tinetorially superior to those obtained with lakes prepared by precipitation of blane fixe in the presence of the precipitated pigment slurry and by slurry mixing blane fixe and pigment* The latter two show no appreciable improvement over a dry mix of blane fixe and pigment. Further studies along this line have been jr oposed* DUP050316556 TOBBIMUAL DETAILS Barium and Calcium pigments of . ( beta naphthol 3:4 dichloraniline ( * beta oxynaphthoic acia ( * R**salt N*B* 487, exp* 13 and 18, pp 46 & 68 respectively. Barium, calcium, strontium and manganese pigments of ( beta naphthol 3 nitroaniline 6 sulfonic acid ( beta oxynaphthoic aci ( Rsalt N*B* 487, exps* 14, 19, 23, & 25 pp* 52, 72, 90 & 94 respee tively* Barium and calcium pigj&ents of (beta naphthol 6 chlor 2 amino toluene 5 sulfonic(*beta oxynaphthoic ao add (-Basalt H*B* 487, exps* 87 & 28, pp, 102 & 106 respectively. Alumina Hydrate Lakes and P.T*A, pigments of Sulfonate Lithosol Blue 6(1 and Sulfonated Lithosol Blue G* H*B* 487, exps. 26, 29, 31 & 32, pp. 98* 110, 118, & 122 respectively* Meta-nitro*para-anisidine beta naphthol (K>7699) Acid sodium formate coupling* H*B* 487, exp. 16, p, 60* rubber* Alumina Hydrate Lakes of Ponsol Jade Green Supra for N*B, 487, exp* 17, p, 64* Calcium and Strontium toners of Lake Bordeaux B (T0B BOH) and Synthesis of Maroon, C-37914* B*B* 487, exp. 20, p, 76* Azo dye, nitroso compound and iron salt, condensation products of betathio*naphthol* respectively* N.B* 487, exps* 21, 28, & 24, pp. 80, 84, & 92 DUP050316557 Pbthalocyanine Lakes and Pigments* N*B. 487* exps. 30 & 33 pp. 114 & 1S4 respectively. Preparation of lakes for paper coating from water dispersible pigment of Pigment Green B and Blue 3!oner, BT*1S5D. M,B 487, exps, 15, p* 56* DUP050316558 /a S PIGMENT COLOR RESEARCH REPORT SUBMITTED BY: APPROVED BY: BARIUM LAKE OF ORANGE II, /-/Arc. FILE: OR-AH&S `LAKES DATE: NOVEMBER 1935. , */ INTRODUCTION Work on barium lske of Orange II to match G-38038 was continued during this month. SUMMARY AND CONCLUSIONS. A sample of Orange II Gone. (D-2232) was received from the Dyeworks. A "barium lake made with this dye gave a fairly close match to C-38Q38 in masstone by dry mixing with blanc fise and Y-299-D. This lake,was, however, much yellower in tint. Mixtures made to match C-38038 in tint were off shade in masstone. Material of bluish tint was needed to give a perfect match. Studies were made on the straight barium toner with the object of producing a bluer tint. Variations in pH showed no considerable change. An increase in temperature of strike resulted in 8n increase in the blueness of tint but with a tendency to a darker masstone and lower strength. Decrease in rate of strike resulted in duller masstone and yellower tint. Quick strike (by dumping) gave a slight increase in blue ness of tint and a brighter masstone. A dry mixture made with this material with blanc fixe and Y-299- was close to 0-38038, 80 parts of a 51$ barium lake on blanc fixe mixed with 10 parts of blanc fixe and 10 parts of Y-299-D gave material of cleaner, v.s. lighter and higher strength than C-38038. Reducing the strength by an increase in blanc fixe lightens the masstone markedly# An analysis of G-38038 reveiled - 40$ Aniline matter calc, on barium toner of Orange II, 49$ Barium sulfate 10$ Lead chromate. An effort was made to prodtice Calcium Strontium and Aluminum toners of Orange II# The Calcium and Strontium precipitates were soluble in water. The Aluminum toner has a redder, darker,masstone * more strength, a yellow dirty tint and is of inferior light fastness com pared with the barium toner. The Aluminum toner bleeds in oil whereas the barium toner is non-bleeding. A Barium toner of Orange RO was dark, slightly brownish in masstone, of high strength and yellowish tint. A resinated Barium Toner of Orange II was of yellow masstone and tint. DUP050316559 2 - / * ix p s r t mr t it a l d e t a il s > "".... ............'""'**............................... ' 387-191 Test on a preliminary sample of Orange II Dr2S32, analysis revealed 86.32# of sodium salt of Orange II. Material 41 of tlie Barium lake mixed as follows: 387 - 19 76 parts Blanc Fixe 19 " Y-299-D 5" This mix versus C-38038 was v.v.a.dark in masstone, s. yellow in shade and tint and v.s.strong. 387-30. Evaluation study of Bariu^Strontium, Csleium9 ana Aluminum Toners. ' Dye solutions of Orange II, D-2232 (L-2757) were struck with the Chlorides of Barium Strontium, Calcium and Aluminum* Strontium and Calcium Chlorid&s merely gave ^saltingout effect. Flushouts of pulp material of the Barium and Aluminum toners showed no increase in strength versus dried material. 587-21* Variations In pH* Addition of Aoetio Acid or HaOH to the <?ye solution* Final pH values of 4*5, 5.2, 6*8, 7.2 and 7.5 were obtained. A slight tendency to a more bluish shade with higher pH. 587-22* Hasrresse in strike temperature 55C, 80C, and 100G* Increase in blueness of tint and loss in strength. Addition of sodium resinate to dye solution. Yellower masstone and tint* yellow tint. Barium toner of Orange OR - darker, dirtier masstone, 387-25* Variations in rate of strike. Dumping - 5 and 15 minute strike. Dumping brightens masstone and gives a slightly bluer tint-* slow strike gives duller masstone and yellower shade and tint. Material miewed under the microscope showed small crystals in the case of quick stiike and very long ones st slow strike, oo 387-24* Quick strike of barium lake at 55 C, 80 0 and addition of caustic soda. Material struck at 55 mixed with an additional amount of blanc fixe and Y-299-D.Matches 38038 fairly close. Addition of caustic was without effect. Strike at 80oc resulted in dark er masstone, bluer tint and loss of strength.- DUP050316560 3*r-V/7 /67 StJBMITfED BY: APPROVED BTs _Tmwm c o l o r r e s r a r o h k b p o r t AimiSIS OF PEACOCK BLUE LAK1S *s^u,,aJ FILE: MTS: HOY, 1938, 3,/* MBai At the request of the Sales Department a laboratory study was undertaken to determine the possibility of analysing Peacock Blue Lakes for their dye content and to correlate the results with the tinting strength shown by our usual pigment testing methods* ggLiB-SiOMOi,., Two analytical methods were investigated, 1) a Kjeldahl procedure, similar to that used in determining the blue content of chrome greens and 2) titration of a solution of the lake with titanous chloride. Results with the KJeldahl method were unsatisfactory for the following reasons. Analysis of dyes of the Brio-glaucine type gave widely different factors for conversion of the nitrogen content to 100$ dye. With Lithosol Brilliant Blue S and Alphszurine the figures were 13,49 and 22,27 respectively compared with 28*29 calculated from the formula of the soda salt of the dye. It was sub sequently learned that Lithosol Brilliant Blue is an ammonium salt standardized at a 72$ dye content. Analyses of various lakes gave irregular results considered not only from the standpoint of strike formulas and yields but also from careful determinations of their relative tinting strength on extension with zinc oxide. This is attributed to variations in the amount of dye in the final lake and to the fact that ammonium salts are used in the laking operation* More satisfactory results were obtained by the titanous chloride titration method a procedure suggested by the Technical Laboratory of the Orofrem Dept* and subsequently modified for the sake of simplicity and greater speed. The figures which were found are given below in comparison with those from the Kjeldahl analysis for nitrogen and the tinting strengths* As a result of the work to date, the following con clusions have been drawn: 1} The Kjeldehl procedure is unsuitable in giving a basis for classifying Blue Lakes, 2) A modification of the Dyeworks* TiClg titration method gives results which are more nearly comparable with the strengths obtained by our present rubout testing methods, 3} Rubbing out the lake, extending with white by a carefully standardized procedure and comparing with a properly chosen standard furnishes, in our opinion, the best basis for comparison. DU P050316561 Sample aismaT, Calc,of Dye*See Hot I* d a t a , s s e n o t e b o o k #327. xm.rn % Dye by T1C1* ti tration See Note 2. % Dye by Kjeldah! See Note 3* "Dye 0< Tiolg--rjSSSSbi Method Method Figment Strength by rub- out* BL~72-D,SD-46744 3 43 1, W- SBL-70S8-B * SW-4367 19.0 21*1 80*8 BL-143-D SD-36362 " lot 43661 "" 45171 15*0 14*9 13*6 BL-X51-D * SR-46978 SW-6877 7019 19*0 17*1 1SS 12.13 13*74 13.50 7*92 3*30 5*59 10,11 11,37 3*89 14.57 16*38 19*16 10.10 14*64 9*77 13*90 15*80 10*49 100 113*3 111*3 100 115*8 131*5 65*3 63*4 44*4 69*3 100*4 67*1 33*4 93*4 93*7 108*4 73.3 72*0 100 105 105 71,5 71*8 46*0 80*0 91*0 70*0 Dyes Llthosol Brill* Blue 2 Alphazurine Special s AMSrieglaueine D-19QS * 67.36 73*21 309*97 127,14 101*39 - - m 4ft . Note 1) These figures represent wt, dye/yleld x 100 and are not necessarily directly related to the rata in the other columns# Hot 8) Modified fcyeworks Procedure 00 TiCl x normality x *391 x 100/ wt of sample - % dye* Hot 3) Dry Color Mfrs. Assoc, Method* $ Hs x 28,89 - 56 dye .mtm. of A* - Copy submitted method "Determination of Hltrogen in Blue Lakes from Srioglauolne"- (Imperial Color Works)* (See Appendix to this report) B* Copy of submitted method from T,A, Martone "Analysis of Blue Lakes, Llthosol Brilliant Blue "*" Dyeworks Technical Lat (See Appendix}* 0* Modified Dyeworks Method* Similar to B with the exception of treating a 1 gram sample and filtering the residue thru a gooeh crucible containing a #40 Whatman filter paper with the aid of suction, D Rubout method (Krebs) (See Testing Method Ho*TF41-l ) DU PO50316562 /? 3" Masstone 1 gnu color 1 gat* varnish drier Intension (1S30) 1 g.ink 2*5 g* ZnO Presactions 1* Keep away from sunlight as necessary* 2* fork as rapidly as possible with as few samples 5* Keep inks covered at all times when not in use* DUP050316563 Ajz.mmit- DETERMINATE0Hf OF NITROGEN IN BLUE LAKES 3BS^JBgSaMBSfflS Weigh accurately 1 gram^sampl of the pigment and transfer very carefully to a dry KJeldabl flask of 500 ml. capacity containing eight glass beads. Add to the flask 5 ee of 80$ %0,, (Superoxol). Add SO mil* of concentrated sulphuric acid and digest over a flame for two hours, the neck of the flask being at an angle of 60 during the digestion. After two hours add another S m of 30$ HgQg and digest for three hours more. It may be necessary to add concentrated sulphuric acid during the digestion in order to keep the volume at 20 ai* At the end of five hours* digestion the residue will be nearly white. The flask is cooled to room temperature and about 150 ml. of eold distilled water is added. Cool the flask to room temperature under the water tap. Put the flask on the distillation apparatus and add 100 ml. of 40$ caustic solution. Pour solution down the side of the flask, so that It does not mix at once with the acid solution. Attach the flask to the condenser and apply the heat to the flask. The distillation apparatus consists of a KJeldahl bulb or other suitable scrubber to prevent contamination by sprayed sodium hydroxide, having one end attached to the Kjel&ahl flask and the other end attached to a vertical condenser. At the exit end of the con denser is attached a 500 ml. Brlenmeyer flask to which is added a measured amount of 1/10O normal sulphuric aeld to react with the ammonia that is to be evolved* The flask is so placed that the end of the condenser Just dips into the aoid. Add Methyl Bed indicator to the aoid solution. The Methyl Red is greater the the amount* of N/IOO sulphuric aeld in the receiving flask and is also the Indicator in the final titration. The amount of N/1QQ acid used in the flask varies with the amount of dye present. For the usual strength Peacock Blue it will be about 50 oe. Mix the contents of the Kjeldehl flask, which has bean attached to the condenser, by gentle shaking. Heat to boiling, and distill until all ammonia has passed over into the standard acid. Fro 100 - 160 ml. of distillate is sufficient. The presence of the glass beads prevents the bumping of the solution in the KJeldahl flask, as it is concentrated by distillation* After the distillation 1 complete, lower the Srlcnmeyer flask, remove the source of heat, and rinse the condenser with distilled water. Titrate the solution in the irlemeyer flask with an alkaline solution (N/100 NeOH) that is equivalent to the acid solution used. Subtract the volume of N/lQO alkali required from the volume of N/lOO aoid used. One cc of N/100 acid corresponds to 0.00014 gma. of Nitrogen. DUP050316564 ifSSMV . JK // / Grams of nitrogen obtained X 88.29 s amount of sodium dye of Brioglauolne present in sample, Briogl&ucine has the formula - S7 HM %9 s5 NAg {Mol. wt. 798,87) Experimental analyses which have been run on the above method indicate that: the experimental error will be less than oneone husdradty of one percent, so that it would seem that this method offers possibilities, The principal differences between the method suggested above and the one used for iron Blue are - Superoxol is used instead of Copper Sulphate as a stranger oxidizing agent is required, Ji/lQQ HgS04 and NeOB are used instead of w/lO to insure greeter accuracy in titration. The digestion period Is increased to five hours. DUP050316565 /.ft^ B ~ METHOD AHALSSIS OF BLUE LAKES LnjaBKfflOL"- b r il l iu t o b l u b d la reply to your letter of October 89, w are submitting herewith, a formula which the plant has found to give the most consistent results for determining the purity of "Llthosol" Brilliant Blue 1 Lakes* 2,0 grams Peacock Blue Lake finely ground is added to 50 ee distilled water 5 oe aequa ammonia (28$) Digest for 50 minutes at 70-?6C, It is then filtered and the filter paper and residue are put back with 50 ee distilled water 5 oo aequa ammonia (28$) Digest for SO minutes. The filtration is repeated end the filtered solution is added to the first filterse solution* The filter paper and residue are again put in 50 eo. distilled water and 5 oo. acqua ammonia 28$* Repeat filtration* After the third filtration there is practically nothing left on the filter paper but the inert base. Take the filtrate from the three filiations (approx* 155 oe) 9 place over flame or hot plate and evaporate to 50 or 50 ee* (ammonia should be all driven off* If still present boil solution until practically free of ammonia). Then add 50 oe denatured alcohol 50 oe of 25$ sodium tartrate solution* Boll one minute sweeping with carbon dioxide , Titrate hot with N/20 tltanous chloride solution, sweeping with carbon dioxide. TiCls X Normality x 591 Wt* Lake used (l/8 molecular wt, of "Llthosol* Brill, Blue S) is Brilliant Blue 1 in lake. DU P050316566 i Would like to call to your attention the molecular SKStg&t of *Lith@solw Brilliant Blue I is 788 and the color is only Bare* This is also the approximate purity of Alpftawuriae lm 10 and Heptune Blue BB. We mention the purity as your results will he based on a 100$ color basis and you will hare to allow for the color being only 72$ pure* T.a . MART0H1 DUP050316567 PIGMBETT COLOR RESEARCH REPORT JjT- 35*6 X \y MEDIUM YELLOWS Y-299-D, Y-316-D, Y-359-B . Cj<jh SUBMITTED BY APPROVED BY! *t/// PILE! <8fiR!ffi~YLLeWS BATS: OCTOBER- 1935 INTRODUCTION The study of the development of a lead nitrate formula fcr Y-299-B was continued during the month. in the in the plant. The development section is continuing supervision of Y-359-D plant, and at the same time is carrying on a study of the color semi-works. Little difficulty is being encountered in the Trouble is being experienced in the manufacture of Y-316-B with satisfactory properties* dark masstones of poor light stability predominating, SUMMARY & CONCLUSIONS Y-299-P The semi-works studies of Y-299-D and Y-359-B are being con ducted simultaneously because of the close similarity of formulation. Two batches of Y-299-D were made. In the first, hydrochloric acid was added to the chromate, the batch was struck at an elevated tempera ture, and caustic soda was added after strike. The result was a green, dirty strong product against both Y-299-D and Y-359-B stand ards. Lightfastness was equal to Y-299-D standard. The other batch, made with lead nitrate crystals and a small amount of caustic soda added after strike, was slightly flat and v.s. light against Y-299-B with a strong green tint. Against Y-359-D, the masstone was red and slightly dirty. The tint was strong and green; lightfastness was v.s. worse than Y-359-D and equal to Y-299-B standard. Y-359-P One batch (SW-7336) was run on the semi-works control formula for this color. Against standard Y"359-D it was slightly green and dirty in masstone with a strong, slightly green and v.s. dirty tint with v.s. wcrse lightfastness. Against a former control batch (SW-7302) the masstone was green and dirty, and the tint slightly strong and green. Lightfastness was worse than that of the control. This control against standard was v.s. light and clean in masstone with a v.s. strong and v.v.s. green tint with vvs better lightfastness. Two other previous control batches were tinotorially intermediate between the two given above. Another batch run as a control except for striking thru a sprinkler was still on the green and dirty side of standard but was slightly light and clean in masstone against the control batch run on the same materials. The tint was v.s. strong, green and clean agains standard and v.s. weak and red against control. Lightfastness was sligh ly better than control and equal to that of Y-359-D. A check on these controls was made using lead nitrate crystals instead of liquor. The results on this run were quite close to those of the former control. Against that of the present series, the masstone was light and clean, with a slightly weak, red tint and vs better light stability. The DUP050316468 s masstone was v.s. red arid clean against Y-359-D with a slightly strong, v.s.green and clean tint. Lightfastness was equal. These results would tend to indicate that there are other impurities than copper present in lead nitrate liquor which may have a detrimental effect on the yellows. This is supported by the fact that all of the eontrol^mentioned were run on lead nitrate liquor free of copper according to the ammonia test. An investigation is being made on the quantitative determination of the amount of free oxides of nitrogen in the liquor. This investigation may throw some light on the variance noted in these yellows. An increase in chromate excess from 5 to 25^ gave a v.s.green and dirty masstone and a v.s. strong green and dirty tint against standard Y-359-D. Light stability was v.s. worse. The masstone was slightly light and clean against sw-7336 with a ws red and weak tint and s.better light fastness . The addition of 5 lbs. per mol of sulfuric acid after strike to the control formula gave a v.s. light and clean masstone against standard. The tint was vvs clean and lightfastness was equal. The masstone was ws green, flat and changeable against SW-7302 with equal light fastness. Adding the same amount of acid in the base rather than after strike, pro duced a vvs dark and dirty masstone that was vvs strong and slightly red on extension. The color was a little red and clean against standard with a small improvement in lightfastness in each case. Doubling the amount of acid added after strike put the masstone on the green dirty side of standard and slightly dark ;and green against the corresponding batch using half the acid. Tints were green, and lightfastness was equal to standard and vvs better than that of the batch made with the reduced amount of acid. This batch was a little light, green, flat and weak against SW-7336 with slightly superior light stability. One batch struck with nitric acid (6# per mol) added to the lead nitrate solution was green and dirty against Y-359-D standard with a small increase in strength and instability to light. It was also a little on the green side of both control and the batch struck with the higher amount of sulfuric acid in the base. Lightfastness was equal in both instances. Compared to the batch in which stllfuric acid was added to the lead nitrate it was dirty and green. A smaller amountjof acid might give more benefi cial results judging from the above comparisons. Two batches were struck on the present plant formulation; namely, a solution of lead nitrate being run into a sodium chromate solution con taining 1.2 lbs. of muriatic acid per mol, and a 10% chromate excess. Both were a little red in masstone and strong in tint against Y-359-D standard with lightfastness varying from equal to vvs better. The first of the two against control was light and clean, and'a little weak and red with v.s. better light stability. The second batch was a little red and clean against the first. Plant Y-359-P The majority of the Y-359-D made in the plant was struck on the 1C$ chromate excess formula with 6 lbs. of hydrochloric acid added to the base Eleven batches were struck on this formulation. Most of these were a little on the red clean side of standard with slightly to v.s. better strength and tints tending to be slightly green and clean. One batch made with double the amount of hydrochloric acid usually used was very ' similar to the ones struck on the regular formula. DUP050316469 Two "batches were Bade with sulfuric acid (5#/mol) added after strike. One was dirty and v.s. green in masstone with a slightly strong and vvs green tint, with v.s. "better lightfastness. The other "batch was t v s dirty and red in masstone with a slightly strong and green tint, and satisfactors'- lightfastness. The development section is continuing supervision of this color. Y-316-D Difficulty is being encountered in producing Y-316-D of satis factory lightfastness. The first batch of the month was struck on a for mula checking that used for previous strikes. A vvs red and dirty mass- tone with a v.s. strong tint was the result. Lightfastness was s.worse than standard. Reduction of strike time to 10 minutes gave a v.s. red, flat, and dirty masstone in conjunction with a slightly strong tint and v.s. worse stability to light. The result on increasing the striking time to twenty minutes was to give a v.s. dark, green and dirty masstone and a slightly strong, green, and clean tint. Light stability was s.worse than standard. Increasing the time of strike an additional 10 minutes put the color off a little more in the same direction. Three more batches on the same formulation checked these results. In the case of the next lot, the striking time was reduced to 15 minutes, and a cut of 25% made in the amount of alum. This batch was vvs dark, red and cbirty in masstone with a v.s. red and strong tint, and slightly worse light stability. Two more batches struck on a check formula were v.s. dark and slightly red in masstone with a v.s. weak tint that was red and slightly dirty. Lightfastness checked the preceding batch. One batch of this color was press wahhed to determine the effect of such treatment on the color. The vat washed control was slightly ied and dirty in masstone with a slightly weak, red tint. The press washed portion was a little cleaner. Lightfastness was worse than stand ard in ea-ch case. Supervision of this color is being continued. Increased dilution of materials during the strike will perhaps circumvent the difficulty now encountered. Results of this will be given next month. BSCEERIMSHTAL DETAILS. See U.B. 448. Sks " Plant Y-399-D Y-359-D Y-359-B Y-316-B p. 96 p.102 p. 76 p. 62 )i DU P050316470 I r+P p H2h h0 +3 H ffl ft>eo s<f&0t ipf>t *d +> S3 rl ffctfl a ffl CO ft rH. +> 0} + 2&,x> <0 ^ Id w> ffl ffl >> ft n PH^ " S P &3 a4 43 <n >> pft ^3 > H Ti o V ft ffl fti bo rs e cr > l> ft ft ft -P ft -P <D P -P u ffl Jh CO p -P P P p H 43 -P aJ 43 4* S p p rH ffl I? CO ffld to 4> a1 t> m di P 43 ffl'0 > > t> > > a* O' P w p> >> rH O S>* eg P rH *d O ti e8 * * is a ft 6bo n 8 ft ftd rH d ft d ft ffl bt<O btJi) !> ffl bo ft ffl s> o s< bD N U > bO ffl bfl tffl ft g g fS i f<t & ffl ft. p u p^ ft. p u pto u p to ffl > CO ffl ffl ft* p ffl ffl >> w oo AS A ffl ft* P AS ffl d ffl > PS > o ffl * ft* ft* P P ffl ffl ffl ffl > J> > ft AS P erf CQ ffl > > ffl M {> O ft ftp* p ffl AS ffl ^ ffl ffl > ffl ft AS P cS I? ffl CF* > ffl ft. p ffl *8 ft T3 d ft ft* P rH ffl O ffl ffl >> rH ft. O p ffl 8 <8 ft AS & ft. P ^ rH ta p> > ffl > rH O ffl > * fofl c fe u d bO a AS ju a ? AS 8 (rf fcb i I ft ASl bO p e P ^ rl P K P d ^ o0x> * 5- d pd ii * ffl roffl P> ffl & >o ffl > o5 d rH no ft* b,60 Q> d co p ft e-dy .>> ft P bOft `rl 03 *d ft U ft 8 ft 49 S to p uu pp TJ -p ffl eg ffffll V. rH * > 2>>> offtl 'du pffl ^ og n sd ^ pffl +3 >i ft P a aT3 * ft > K X H rH TS &3 * CO >> p a *d e8 fc>8 ft bO 3 P -p > S p ha h erf a 3 O rH O *8 *Ch ffl H +> bb rH >> P rH ft-p>* * ^ *8 rl ft >d bO ft bfl *{je * p ft AS rH b0T5 ffl ffl ffl > l>v p rH ft o *o eg d AS T3 ^ g$ >4 P u H nd ft* ^ 8 a bO > P ft U ffl 3 bfl > H *d ft C bO ft 8 ffl g t; P A d d "8 rH ft &b 8 >> p u H g s d TO d P ffl erf ft ft H ^ f>fl f>fl ft* *d P P tn >>TS PT. 14 u j* hfl'd rH CM C) to Q n to Q CM to O Io CO 1 CO CT> CO I 1 co 31 CO 1o CF* CO CQ -P in t- in o in o fc- m c- t- g o CO ^ co J 1 fel >-4 CO co CM 1 [it *? ^ >H CO g erf rH d a ft ftH CM O rH CO o e- u JELP S*3* CO o u AS _ to AS rl ft* P ffl -P ft d 43 rH AS to CQ b* < W* p <0 si AS d XP o> t o rl a d 43 dVe. to a tn CO ft t- M o top *5: CO to as a ffl ft ft fi 0<M AS rl d ft* dP erf f P ft d 43 P to erf to tn Ai^fe: e in X CM O in m in co CO C0 o NlO ID 03 CM CM \ o *s o> t rH IIS CO CO CM CQ CO CO CQ t- b- b- 3 CM Q t o> in co >s fe r~* Idf r IM C? 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O P rH \ o P CO V o1--i <0 o *5fn CO CO to s & in CO CO in to O/0s3 GO Si CM Ph fc CO P in iH 53 O O Os 43 O 00 s. 0 p d4 CO tn tn 'd* CM tCO 2 in <d* 44 O $ 43 O s O IO CO P j-H ^rH^ \\ OOO P P r-l <> o> O b~ l t> in to tO m in tn <qj o M CM t* P CO 43 m pi axs 44 p 3 43 43 O frrH V 0 p o in * <o a> tin- CM CM 43 t- t> p co CO P in in ^ TJ Mt> 9 4d O -Kr4 43 43 e O 0 " --' P CO CM CM V\ OO PP O CM tf> U t- ttn in *d* * CM fc~CO in -c3* 43 O S3 q H CO o t~ in M* 'H p CoJ is uo IS DU P050316472 to51 -PH *rt . SbCi H CD JU O Jh 0 02 > PC O*ri Eh o 54 = o & a u o a TQ3> roH <6 r^a *ft & " ft* p14^ *C4D I H tfl T*> * A * to E O em (4 P w pCO CO > to Ad s 54 p X 0bO Ro OU P5h Pw M& aK to * *4 P -3 TJ su > > *4 0 b <S5 0 P <o > >1 *3 >% 0 o n to L P0 TJ *s $4 CD p p P oJ pH m >i * 5* -0P *ri d > P$4 H 'C <' no T3 $4 0 <3 & * AC +r3hr *& u rt TJ P$4 0 * eg, 0 bD Ad TS >* 43 p H CM o co ffi to K in d d B l to p H CO %I JtSo 0 i5 rl A* Ad Ad -f*HA4 54 i P00 *H4 P m 5r4l P P0 T0d *rt B P0 P IS 0O H o> CO " -g CT> & CO aS o CO CO > * t- P*0SH3 & tt-- p Cft pH rH d tn d LO m in o in in 0 in 3 Q Ad o rH Ad d r! P Ad 54 d* o CM A4 d* H 0 Ad _ d* Ad 5o4 0 rl O p* C *H O CO O AS o 43 O 43 O 6 CO P \ o a r-J CO o t-- p in *in& d1 CO O pH d \ o X d w rH o rH ao rH H l> o CO CT pH eo d t> O* CO in m m in to to tn m tn in d* d< d* d* d s rOl > > P s5 t(0o > P H S CM Ad co *tJ to * in H d >B u ^043 p ro i> t> t** P54 *H TJ c *rJ 54 5h > m rH ti > f>> P *u 54 ,0 P V ?H6 no ts nr io =3 t> X in > P 3^ 9 *5 CM CO CO CO to tn to in d* d* 33 T! A -p S' pr3O d TJ fr- <$ t- tn f3 d* *rj Ad m to rH 43 O in ibnd Ad B rH CM CM CM \\ O pH O pH tpnH tr cr to fc- io in d * o ts tin d pp it-oh #& ?(M DUP050316473 ^ JZf PIGMENT COLOR RESEARCH REPORT SUBMITTED BY: APPROVED BY: INTRODUCTION CHROME ORANGES. Y0-34-P - 10~38~D ifcKMAA CkX*- J "tST" FILB: GiSRQME - ORANGES' DATE: NOVEMBER 1935* ^2- Trouble is being encountered in the manufacture of standard material of these two codes. Masstones have been running definitely inferior to standard and it was deemed advisable to check the process in the semi-works* SUMMARY AND CONCLUSIONS Y0-54-D* A total of five batches of YD-34-D were struck during the month. 7he first was a variable of the formula of a previous semi-works batch(SW- 4928), the base being heated to a higher temperature, and the sodium bicarbonate reduced a little* The color was light and somewhat flat against standard with slightly increased strength and a yellow tint. It was much lighter and stronger than SW-4922. One batch was run as a check on the standard formula of April 7, 1927* This was similar to the previous batch being a little darker and flatter in masstone and v.s. bluer and weaker in tint# A eheck on th current plant production formula (as of 11-5-35) gave a dark, muddy, masstone against I0-34-D standard. It was a little brighter and weaker than the material struck on the standard formula. This batch, i*e. the one made on the current formula, was checked using sodium bichromate crystals rather than liquor. It was slightly flat and a trace strong against standard. Referred to its control it was lighter and a little flat* A batch made on a laboratory formula (421*96) was light, yellow, and flat* Y0-58-D* Two batches were struck under this code, the first being a check on a former saai-works batch (SW-49&5),, It was a little dark against standard with a stronger somewhat yellower tint. It was also stronger and yellower in tint as compared to the former semi-works material* It was found that small amounts (t 1%) of diphenylguanidine materially increased the brightness of the orange when rubbed up in varnish with the color. This apparent increase was evidently due to the higher finish as theve was no appreciable differences reading the masstones through glass* One batch was struck with 0*5$ diphenylguanidine added to the base, otherwise checking the previous batch.Against this bate)* it was dark in masstone and a little red and weak in tint* DUP050316474 +l* f-i > ft +J3H f9-t1 3 0* H rH P rH H *4 r4 > > E* A P id GO t(0l4D) 03 U 43 CO 0 (h 4 cq 0 P CO H * JO rH a -i <n - (D * !> t* e id ft fs 43 * 9 W ft %? H /a to >J H > rQ 03 1 >3 H |> l>a A 03 A ft 43 ft * 43 9 l co > (> 9 H r-i * r-f H ft rH H 0) f-t >> >3 * * 03 * A id u ft p 4 to 14 43 <*3 +ffom3tt ft 4 to tiHo 4fot to CO ft s<d ICM o to rH rH O t ft &- 3 to a rH 0 0 m Pt P< *1 9* S3 O m rH + Ss rH 0 tn fi O N CQ *-3 M d E-< fact O | a 3 C-| O M c& r-4 0 # H >4 O H <fc * $ < 43 id rH iS m iH ft> & a> 14 & -p r-t iH r P * > r 43 ja 99 p CO CO * *3 CO * 4SS A ft CO SS P rH CD pp <0 CD rH rH 0 S3 ofc, * pp rH tH +3 -P f--1 *-4 S-i <5-) cj$ <d 9O P J4 1--f ft O ft? * 43 A ft (4 03 a3* * < A P *e . fe id > rH * < " Vi P *M w ft * rH to rH P Vi #* *H rH cj$ 03 >> 44 * *3 P H 03 ft + ft H <t3 9 * id ft ft to Q IO 1 to to c- O to i to 9jt E0 O14 iss a> tO D*1 to a o 1 ts 9l t to & 1 CQ h! iS 55 CQ W CO ts 10 1 t 1 f 11 0 0 4 43 Pro ps 0=^ s to ftV P^ H CQ rH 3! P& PtO $ rH ffi 43 e ft ^i03 _ to 'ft id q> ft -p 1 CS +30 H a 45 ft rH 30 SH to tM O _ 0 1 43 9i* 43 <SdH ft 43 -tf rH & 1 r-- O ^4 HH PtrH ft 0 ,Q 9 feS<4> h CO CC Sh P t--i c- ft O tO rH to 9# O * 1 03 -* a o> c- F4 43 43 p, ffi St ft > 0 <h r >H p Cl P W C" + r ft ft 1 f4 O pS id e j. ee eea ft CO 0 to O 33 co t--t 03 ext , r-4 to *r< rH 94 id^ St 9-4 9 Jiti JO S CP *rt * ijSH OO id ft Og M ia O 9 43 id O id 0 ft rH JO 4H * U '5^fc Mfe-P Oo JS ft id 0 'ft w id 0 a id id id 0 t H O rH i> -- (0 W M 0 O S-t -rH 0 to to tO to to to to to 8 * to to to $ to i to ift co t (M 1 to t> CQ rH cs H rH * *1 iIt rH rH rH rH rH rH rH rH H rH rH H H 9 id |s to pi 43 to &4 te 9# PS tapQ t> 9* to H to to 'd* - N C> CO 03 8 o> 9# d> 9# 4P e- u- e- DUP050316475 3*r PIGMENT COLOR RESEARCH REPORT SUBMITTED BYi APPROVED BY: INTRODUCTION STUDY OF Y0-38-D " I- . // FILE: DATE: NOVEMBER 1935, A study of the Y0-38-D process has been continued from the past month. The results to date have been negative and additional work appears necessary, SUMMARY AMD CONCLUSION The work during the past month on Y0-38-D was mostly of a miscellaneous nature* Experiments using a small amount of sodium molybdate in the Y0-38-D strike or dry mixing with a molybdate orange gave negative results. A study was made of the effect of developing Y0-38-D in an Autoclave st increased pressures to obtain a higher development temperature. The products obtained were dull versus the eontrol which may mean that development was incomplete or that increased pressure during development is not desirable. A study was made of the acidity of plant bichrome liquor. It was found that plant bichrome liquor is substantially neutral EXPBRIMENTAL DETAILS Notebook #486. 48657 - Study use of sodium nitrate in the strike solution to influence crystal shape; use of molybdate. Sodium nitrate in the bichromate gave a darker mas stone and very slightly redder and very slightly weaker undertone versus the control. The use of molybdate tends to lighten the pigment but does not improve the brightness of the masstone. 486-59 - Study the use of sodium nitrate in lead nitrate liquor; sodium acetate in strike solution; strike at slightly lower temperature. No marked improvement was obtained by the use of sodium nitrate in the lead liquor. Sodium acetate, if anything, tends to weaken the product. Striking at 170F versus 200QF resulted here in a darker product with no improvement in brightness. 486-58 - Study the development of Y0-38-D under pressure (auto clave study)* Developing Y0-58-D under pressure gave very very poor results? (see notebook 486 page 85 for further details of this experiment DUP050316476 -2- L->/- 485**48 Study the accuracy of the method used for Analyzing bichrome liquor Samples were made up with a known amount of acid added* The analytical results indicate the method used, to be satisfactory in determining the percentages of KagCr,,07 (JSBgO and percent acidity since these results practically check tne originally calculated percentages DU P050316477 PIGMENT COLOR RESEARCH REPORT 33~ STUDY OF MOLYBDATE CHROME ORANGE SUBMITTED BY: t/* APPROVED BY; cZ&ccts&r 3//> 3 f il e : Gmem~oKm?z DATE:' NOVEMBER 1935a INTRODUCTION The laboratory study of preparing a product equal to C-38022, the Imperial Red Orange, was completed during the past month. Several Semi-works strikes indicated the process was satisfactory from an operating standpoint* SUMMARY AND CONCLUSIONS A brief study was made of the effect of varying ratios of sulphate, chromate, and molybdate on the tinctorial properties of the molybdate orange.' As the amount of lead precipitated as lead molybdate is increased from 6,5$ to 12$ the pigment becomes lighter, brighter, and stronger and the process probably becomes more stable. Larger amounts seem to give a muddy masstone. As the amount of lead precipitated as lead sulphate is increased from one to two times the amount precipitated as lead molybdate, the pigment becomes slightly lighter and weaker. The optimum ratio for the molybdate orange seems to. be 6 PbCr04 PbMo04 PbS04 A study was made of the effect of variations in the temperature and volume of the solutions used. With a low temperature, 50 F, and a high volume, Sllifres per half mol lead nitrate, a slightly brighter product is obtained than with more concentrated solutions at a higher temperature. The time of strike does not seem important between 30 minutes and one hour. The precipitant balance and the acid balance are important factors in determining the character of the final.product, A lead excess is necessary at the end of the strike to prevent the formation of flat dull products but to obtain a strong pigment, as much lead as possible must be precipitated by the strike solution. It appears that 95$ of the lead can be safely precipitated without obtaining an unstable process. The acidity of the strike solution may be important. Sodium chromate could not be used but a mixture of sodium bichromate and sulphuric acid seemed only slightly better than a mixture of sodium bichromate and sodium sulphate. The molybdate was present as sodium molybdate in both cases. As the acidity at the end of the strike increases the pigment becomes redder and weaker. The acidity desired is obtained by adding the correct amount of soda ash to the lead nitrate before the strike* At the end of the strike, in the present process, the lead remaining in solution is precipitated with alum., The slurry is then neutralized to s. pH of 6,0, Varying the pH from 5,5 to 7,0 seems to have little effect. Replacing the alum with titanyl sulphate seems to give a very slightly brighter product, somewhat worse in lightfastness. DUP050316478 1XPBR MENTAL DETAILS 452-48Study the importance of the final pH, time of strike, and low volume* la this experiment adjusting to a final pH of 5,6 instead of 6,# resulted in a trace red, slightly fist, and very slightly weaker pigment than the control. Striking in 50 minutes instead of 60 minutes, and using more concentrated solutions had no appreciable effect on the brightness of the pigment produced, 452-49> Study the use of1 sulphuric acid for sodium sulphate, increase the molybdate from 6,5% to 12$, also study the strike temperature* Using sulphuric acid for sodium sulphate gave a red, flat pigment slightly weak and blue in tint* Increasing the molybdate from 6,5fa to 12$ resulted in a yellow-bright pigment, verg slightly stronger than the control. Increase in temperature from 70 F to 110F gave a lighter pigment* 452*50* Study washing two waters before the alumbicarbonate treatment, study replacing alum with titanyl sulphate, also increasing the soda ash in the lead nitrate when striking at 11QOF, Washing before the alum-bicarbonate treatment gave a slightly redder pigment. Using titanyl sulphate for alum gave a slightly yellower masstone and very slightly brighter pignmnt* In creasing the soda ash and striking at HQoF gave a light, dirty and dull product. 452--52* Study lower precipitant balance; higher bichromate with low molybdate end sulphate, study titanyl sulphate and low precipitant balance* Cutting the precipitant balance by decreasing the amount of bichromate resulted in only a very very slight change in masstone but a marked decrease in strength was observed. _l , Increasing the bichromate and lowering the sulphate and molybdate resulted in a pale-dull red and weak pigment. Titanyl sulphate gave a very slightly brighter pigment, very slightly worse in light fastness* 452-55* Using 452-52C as the basic procedure to increase the bichromate to 56 grams at the same time decrease both the molybdate and sulphate, also use less soda ash. Increasing the bichromate when cutting the molybdate and sulphate resulted in a slightly redder pigment, weak and blue in tint* DUPO 50316479 Cutting the soda ash increases the acidity at the end of the strike; this rewalts in a somewhat redder and weaker produet* 453*54 Study washing conditions and after treatment variations in the laboratory on semi-works slurry. Allowing the slurry to remain over night on the third water here gave a very slightly lighter pigment, equal in strength to the control, and trace better in light fastness* Treating semi-works material in the laboratory with Titanyl sulphate (replacing alum) resulted in a stronger pigment with poor light fastness* Omitting the after treatment resulted in a very dirty pigment, poor in light fastness* 453-55* Study the effect of omitting the soda ash in the lead nitrate base both when sulphuric acid and sodium sulphate are used* Omitting the soda ash in the lead nitrate gave a dark weak pigment. However, the one made using sodium sulphate was cleaner and lighter than the one made using sulphuric acid* Striking at 50F instead of 70F resulted in a bright product, somewhat stronger and bluer in tint versus C-38022, and better in light fastness* 453-56* Study varying the amount of soda ash used in the lead nitrate solution* It appears from this experiment that high sods ash in the lead nitrate tends to increase brightness and the strength; lower amounts of soda ash resulted in dirtier duller and weaker pigments* 452-57, Study influence of volume and temperature; also increase molybdate beyond the amount used in 49C {34*4 gms. per mol}* Here the five litre volume struck at 70]? gave a brighter and stronger product than the four litre volume struck at 70F However, the five litre when struck at 50F resulted in a weaker and bluer tint* An increase of molybdate (beyond the 55D and 49C amount) gave a slightly dull and dirty product versus the control, 551* 453-59* Study using lead nitrate liquor instead of lead nitrate crystals; also study striking in ten minutes; study cutting the soda ash in nitrate from 12# to 6# per strike. The use of lead nitrate liquor gave products a trace lighter in masstone, trace stronger and yellower in tint versus the control made from crystals. Striking in ten minutes gave a produet yellower in masstone, weaker and yellower in tint than striking in thirty minutes* DUP050316480 Gutting the soda ash fiftk percent resulted in a slightly weak and blue tint* ' 458-6Sa Study a slight cut in molybdate in the 55D procedure , also an increase in temperature, double time of strike* A slight reduction in molybdate tends to give a redder mass tone, weaker and bluer tint# Striking at 65F instead of 50F resulted in an "-- increase of strength, the other tinctorial properties were not affeeted* Mo marked differences were observed between striking in. thirty or sixty minutes* DUP050316481 PIGMENT COLOR RESEARCH REPORT gS~-39& '3^7^ MOLYBDATED CHROME ORANGE Y0-8074-D dJM SUBMITTED BY: o&>UkCtJjJ APPROVED BY: \J f4. Cj\ st/A 3 FILE: -MOIiga&afflPED ORANGES DATE: NOVEMBER - 1935 INTRODUCTION: After a semi-works trial of the I.C.I. formulation for their Scarlet Chrome A-35 the color was taken to the research laboratory for development of a formula for a similar color of slightly different tinctorial properties. On completion of this study, the semi-works again began work on the color during the last month. SUMMARY & CONCIPSIQNS: The research study of this orange was made to develop a pro duct somewhat yellower and stronger as compared with the I.C.I. Scarlet Chrome A-55, and to match competitive domestic products. After success fully accomplishing this aim In the laboratory, the semi-works began its study based on the new formulation. The first batch was yellow, flat and muddy against the laboratory product. A slight adjustment of the molybdate-sulfate ratio gave material that was very close to the desired shade and equal in light stability. Substitution of lead nitrate liquor for crystals in the formulation gave a color a trace yellow and a little strong against the control. The grind of this latter batch was set up as K-8074. Reducing the time of strike to one-half had very little effect other than increasing a trifle the yellowness of tint. An increase in batch size to four times the K-8074. formula gave a small increase in strength and trace of dirtiness in masstone. Doubling the time of strike over the K formula darkened the masstone very slightly with a trace yellower tint. Raising the strike temperature gave a somewhat flat and dirty masstone with yellower tint, light fastness was a little worse than control. A reduction in strike volume impaired the stability to light similarly. The masstone, in the case of the latter variable, was on the bright, blue side of control. Strength was satisfactory and the tint was a little blue and dirty. A little difficulty is being encountered in obtaining con sistently good yields as the wash waters are, as a rule, decidedly cloudy. It being possible that press washing might obviate this dif ficulty, one batch was treated accordinglyi, Masstone was very close to control, the tint was slightly strong and yellow and light fastness was somewhat improved. Data is not as yet available on the effect..of this treatment on the yield. Such results will be reported next month. ETPERTMEETAL DETAILS : See notebook 448, p. 184-188 DUP050316482 r M H? Eh IH H pq S ? M Eh t-I CQ Eh fej H Et :.i ffi ffi Ft O >& . rH O t> > |t | |h rK 3 PS CQ E- CO > > p p rH ffl ffi O si * c ffi > rH 0 0M cq 0 * M* & Ft P ffi ffi * > to e Ft ffi P i> P >43 --1 1--1 r-t O >> ffi * 03 > O I--1 d (P 0 r-\ O M > > O Ft r-t P M CO u pffi 4 fH 03 >4 rfHfl >> > CQ +F3t > 01 01 Ft p > to 01 > to ><& > a BP O ffi Ft ffi 0 P rH SjJ --1 o r-t P Eh r-t p > CO 0 4i4 Ft P rH * p U CO <} ffi t>> - P Ft ffi *P * u a ffi ffi ffi > ffi 03 CQ > >> > > > > 03 t4 03 o <# O o> K IS IS (O to ts o O H< I* o O < ? f o o J ? o M Sts W CQ >_ w ffi CO Q 03 CD O to H Ft P 0) 1-->I to Jl? CQ t 3 Ft CM o to tf 03 01 CM P SI soi v- pM P *rl Si r-t p r-t Cl P Ft P* CD g P aw IO P O o> w w ft to 03 ffi to , M H* >Vt p ft si) V *Eh pffi IS * Fot Et p cs o Ft f=t Ir p IS i 4 CQ CQ f--4 CQ a p <e S3 IS BM offi M o- pFt p^fejrj r>-tCQ 9 ffl o 8? MP o P O P' o -H S3 O op a 03 0 . w PP oP * > Ft *9 > r> rH P * CQ > > V Ft P ffi CQ > Ft p 03 cS Ft ffi P > ffi rH >V rjt IS O *? CQ to o> CS 1 Js CQ M H< M P O O CQ H^ CD O 0^ C7* 0 CQ > > *H 00 0 H j>,o * 0) p CQ ^ 03 O > {> * Ft P to CQ > > > P P Ft Ft -rH P c^3 ^ ^ rH P ffi *t3 > ffi > to ^fi ts vjt O C*?* WCO rH P Si o > P P P c q jy to t H Ft C- P CO Vi 0 O & P -rH O Eh w Ft O S. * in > 0 rH H 0 r* +> CQ to t> o ri---t1 rH rH 0 > k p CD >1 rH P V U -H W CJ > o> to H1 ts I E CQ M JN HO Ft O P IO U PO SI _ p ffi CQ CO +3 Hi ffi <S G I rt f?CQ fe 0 *} 0 O ts PP O ffi Ft. O i > CQ >^ > H P rH p Ft P *rt ffi > ffi P O P 0 & CQ 0 > 0 rH rH O 03 1 OU P > * PO CQ 0 Ft CQ H P *4} r-t r-t PP m CO 01 > rH 3 p * Ft CQ P > > 0 ffi Ft P ti > M H CQ P ffi Ft CQ P > H< CO ts 0to3 ts o t-tsfl H* ts II E= CQ CQ Ft P to Si"> PH CQ to e H* 3 tS H IO &> CO M O Tt ffl Ft PP O ffffii Ft P- p s a h JI H* H* IS IS IS ts CQ "v. r-l H (0 O* H IS DUP050316483 PIGMENT COLOR RESEARCH REPORT LEAD NITRATE PURIFICATION SUBMITTED BYt, .v- , t. APPROVED BY: FILE: DATE: NOVEMBER 1935, INTRODUCTION A brief investigation has been made of the effect of copper in lead nitrate* In the absence of copper satisfactory chrome yellow is obtained but *01% or more copper*on a lead basis is detrimental to tinctorial properties of Y**359D! SUMMARY AND CONCLUSION Several experiments indicate that plant lead nitrate made frtxn pig lead or lead nitrate liquor purified to equal average plant practice for Y-359-B give in the laboratory a dirty masstone versus that obtained with lead nitrate crystals* It was.found that *01% copper on a lead basis added to lead nitrate crystals caused a very slightly dirty masstone while *02% gave a dirty masstone versus the control* Lead nitrate liquor made in the laboratory from plant pig lead was about equal to lead nitrate crystals containing #01% copper on s lead basis# Several experiments were made purifying plant lead nitrate for various periods with feathered lead* The lead nitrate liquor samples which gave a (test for copper gave pigments with a dirty masstone while those giving only a very faint or negative test for copper were satisfactory for the production of Y-359-D* The results to date indicate that lead nitrate liquor purified copper free is satisfactory for Y-359-D and that the presence of *01% or more copper on a lead basis is definitely harmful# EXPERIMENTAL DETAILS Notebook #452* 452-58-60 - Determine effect of purifying lead nitrate liquor and degree of purification necessary* 58 plan --make a batch of lead nitrate in the laboratory and treat as follows 58A. - as is* 58B - purified l-l/2 hours with feathered lead* 58C - purified over night with feathered lead# 60 plan - crystals* 60A - cheek plant formula (Y-359-B) using lead nitrate 6OB - check plant formula using 58A liquor* 600 - ** "" 58B 60D - "" '* 58C DUP050316484 **2- From this experiment there is s marked indication that the feathered lead treatment will work satisfactory as a method of purification to produce copper free material free enough for making clean Y0-559-D* 458-61 - Check 452-60 series except strike at 130F instead of 90F In this series D made from the lead nitrate purified over night gave a product practically equal to the control (made from lead nitrate crystals* 452-63 - o A eheok 61A (lead nitrate crystals at 130 F. B check A, except use plant lead nitrate liquor, made from pig-lead* B check A except use plant lead nitrate liquor, purified copper free* In this experiment C made from plant lead nitrate liquor purified copper free gave a product practically equal to the control (made from lead nitrate crystals)* 452-64 - Determine amount of copper that can be present in lead nitrate liquor without affecting the finished pigment* It was observed in this experiment that a lead nitrate liquor containing 0*01$ of copper on a lead basis would produce a very slightly dirty yellow, while a contamination of 0*02$ copper on the same basis would give a pigment decidedly dirty in masstone* From these results it is necessary to purify lead nitrate liquor so that the percentage of copper is less than 0*01$ (in terms of lead) in order to obtain a clean product equal to pigments made from - lead nitrate crystals* DU P050316485 SUBMITTED BY: APPROVED BY: PIGMENT COLOR RESEARCH REPORT 3S~~ LEAD NITRATE LIQUOR PURIFICATION /-*/ / --/ FILE: EEAU fiATERIA DATE: NOVEMBER - 1935 INTRODUCTION: A Yew attempts were recently made to purify contaminated lead nitrate liquor in order to determine the possibility and feas ibility of such purifications in existing equipment with minor mod ifications . SUMMARY & CONCLUSIONS: Five purifications were attempted using air agitation rather than the "Lightning, mixer.formerly used. None of these was brought to the desired end point; namely a negative test for copper with ammonia* To the first batch, additional copper nitrate was added to the impure liquor to duplicate approximately the worst conditions likely to be encountered when using sludge in the manufacture of the liquor. About 30$ of the copper present was removed. Toward the end of the purification, the metallic deposit began to flake off, and further progress was stopped. No additional copper was added in the next three batches altho the amount of impurity was comparatively small, and approximately equal, in each. The first was treated at the usual temperature of 145F, the second at 160 F, and the third at 1300 F. About thirty five per cent of the copper was removed from the first two batches. The deposit on the lead sheets was spongy and muddy. There was no evidence of any appreciable purification in the last batch, the temperature in all prob ability being too low. In the last purification, only two small lead sheets were used. These were immersed in the impure liquor, removed at intervals when a deposit had formed and replaced. This cycle was performed a total of seven times, approximately one fourth of the copper being removed. Complete purification was not attempted as too much time was consumed in the cleaning operation. Air agitation gives highly localized action as evidenced by the copper deposits on the lead sheets, andwill, therefore, hardly be suitable for the process at hand. The deposition of copper on the lead is strongly Inhibited by the formation on drying of a film over the surface of the lead. This film resists scrubbing and can be removed only by dissolving with acid. Work on the problem is being discontinued for the present for investigation of other means of solving the difficulties encountered in purification as now attempted. DUP050316486 Purification of Lead. Nitrate Liquor Batch I - Temp. - 145o - Steam valve cracked to maintain temperature. Copper nitrate present initially 14.9# " added ff M removed . #32.4# - 37.3# total 11 2 ?f fi tf 30% Batch II Temp. - Initial 145 Final - 185 Copper nitrate present initially " " removed 5.6# 1.9# Time of nitrification - 4 hours. Batch IllTemp. - Initial 16 0W F Final - 130 T Copper nitrate present Initially " M removed n rt n 5.6# 1.9# 34% Time of purification - 4-1/2 hours. Batch IF - Temp. - Initial 130 F. Final - 115 F. Copper nitrate present initially 5.6# " " removed approx. 0# Time of purification - 5 hours. Batch V Temp. - 140 F throughout ourification Total lead area Lead Immersed seven times. Copper present Initially '* " at end " removed 60 sq. ft. 5.22# as Cu 3.86# 1.36# Lbs. Copper removed per sq. ft. per immersion - 0.00324# DUP050316487 Purification of Lead Kitrata Liquor Batch I - Temp. - 145o r Steam valve cracked to maintain temperature. Copper nitrate present initially 14.9i " " added " " removed 2121..42## 37.3# total rt tf ti 30% Batch II Temp. - Initial 145 Final - 125 Copper nitrate present Initially n " removed % Time of purification - 4 hours, 5.6?; 1.9j| 34% Batch IllTemp. - Initial 160u F Final - 130 F Copper nitrate present initially " " removed oSL ti ti H 5.6# 1.9# Time of purification - 4-1/2 hours. Bateh IV - Temp. - Initial 130 F. Final - 115 F. Copper nitrate present initially 5.6# " " removed approx. 0# Time of purification - 5 hours. Batch 7 Temp. - 140 F throughout purification Total lead area Lead immersed seven times. Copper present initially " "at end " removed % * 60 sq. ft. 5.22# as Cu 3.86# 1.36# 26% Lbs. Copper removed per sq. ft. per immersion - 0.00324# DUP050316488 PIGMENT COLOR RESEARCH REPORT YIELD STUDY OF IRON BLUES ^ SUBMITTED BY: APPROYED BY: ./ f FILS: ffiON~T38E8~ DATE: NOT?EMBER 1935. i Mt r o d d c t i o n _________ The yield study on Iron Blues was resumed at the beginning of the past month* Goal yields have been determined for B--57-D, B-85-D, and B-103-D. The study is being continued, SUMMARY AND CONCLUSIONS In determining goal yields it has been found that, while both the yield and tinctorial properties can be duplicated within a series or from one series to the next, the tinctorial properties do not check the standard and that a change in operating conditions may change both the yield and tinctorial properties considerably. It is also knownthat the plant process and the standard process for a given color on file in the research office frequently differ and that several plant processes are sometimes available for the same product* These factors make the goal yields obtained somewhat uncertain. The goal yield for B-57-D struck at a boil is 899.5 per mol of yellow prussiete of soda, and for B-57-D struck at 205F is 308 per mol* The goal yield for B-83-D is 899*2 and for B-105-D is 31$Ul grams per mol of yellow prussiate of soda, all on an anhydrous basis* EXPERIMENTAL DETAILS Notebook #468. B-57-D Blue. 468-44 to 45 Two series made according to standard procedure on record in research files, i,e. strike at 205F and maintain this temperature throughout the development. $ HgO "As is" yield Anhydrous Toluol Method per 0.4 mol Yld. per mol of t.PTsT' Hours in Elec$* oven at 140 F. 1 468--44A 4*9 44B 4.5 440 4.4 45A 1.0 45B 1*5 450 1.8 B-57-D Std.4.4 SD--46810 130.00 128.30 128,80 124,00 124.50 125,50 309,08 306,33 309.12 306,90 306*58 308,10 72 72 72 88 88 88 Average 308*01 grams per mol of Y.PS, In rubouts all were black in masstone, strong and green in tint versus standard B-57-D, DU P050316489 -2' 468-52 - B-5?-c made striking at 212 F and maintaining this temperature throughout the development like the present plant procedure. "As is" y$eld $HgO Toluol Anhydrous Yield Hoir s in Elect. per 0.4 mol_____ ^Method per mol of Y.P.S. oven at 140F 468*52A * 52B 52C 123.6 122.0 123.5 3.0 299.73 3,2 295.25 2,9 299.30 72 72 72 * 52-B is not included in the average; some of the pigment was lost during drying process. t Average 299.30 grams per mol of Y.P.S. In rubouts all were somewhat black versus the standard but red versus the previous two series (44 and 45). B-83-D Blue 468-47 and 48. Two series made on standard B-83-D procedure; dried for 72 hours at 140F instead of at 160 F as in the plant. "As is" yield $ Hp0 Toluol Anhydrous Yield Hours dried in per 0.4 aol Method_______ per mol of Y.P.S,Electric Oven. 468-47A 47B 47G 468-48A 48B 480 B-83-D Std. SD-46263 129,00 127,00 127.00 126.00 187.30 128.00 7.10 6.80 6.04 4.50 6.20 6.20 6.40 299.50 298.00. 298.25 300.70 298.50 300.15 72 at 140F SI tt 9? n f? n nn ft Average 299.18 grams (Anhydrous) per mol of Y.P.S. In rubouts all were on the black and weak side of B-83-D standard. DUP050316490 -3- B-1Q5-D Standard Blue B-103-D, 468-49 and 50. Two series based on plant formula of "As is" Yield % HgO Toluol per 0,4 mol Method Anhydrous Hour s dried Yld. per mol at 140F in of Y.P.S. Elect, oven 468-49A 49B 490 50A SOB 50C B-103-D sta. SD-46948 134,00 134.00 133,00 134.50 132,80 131.00 6.00 4.80 4.20 5.80 4,00 3.80 5.20 314.90 318.75 ' 318.52 316.75 318.70 315.05 72 72 72 72 72 72 basis. Average 317,11 grams per mol of Y.P.S. on Anhydrous B-103-1)* In rubouts all were on the black side of standard DU P050316491 PIGMENT COLOR RESEARCH REPORT B-66-E - MOISTURE STUDY SUBMITTEE BY; APPROVED BY; a/3 FILE: 5ftN-RBESDATE: NOVEMBER 1935, INTRODUCTION TWo series of laboratory experiments were conducted in order to establish the connection between the moisture content of B-66-D and its masstone in lacquor and "Dulux," SUMMARY AND CONCLUSIONS The moisture content of samples of material from B-66-D, lot 15833 was varied* Moisture determinations were made by the toluene distillation method. A tendency toward increased depth and blackness in lacquer with decreasing moisture content was noted. Below a certain moisture content (about 4*5$) there was a pronounced tendency for the formation of a clean bluish cast in the lacquer masstone# Material testing v.s. deep and black to deep and black vs standard was obtained with moisture contents from 4.6 to 8*9$. - Under intense illumination these variations show up as a trend from a brownish through a purplish to a bluish hue with decreasing moisture content* In "Dulux" the tendency was towards increasing redness of masstone with decreasing moisture content. At high moisture contents greenness was obscured by dirtiness. This dirtiness was an intensification of a variation from standard which was noted in all samples of the batch studied. Material testing v*v,s, green vs standard was obtained with a moisture content of 7*2 percent and testing v.v.s.red with 6.6 percent* EXPERIMENTAL DETAILS See notebook #=363, pp. 106-107* Exp, Treatment Moisture "Dulux" Reading Laequor Reading Method Period Content VS i vs standard_____ 1 A 47 hrs. 2.3fo red black (bluish) D A 23 w 3,0 red black (bluish) C A 7" 4.3 red black (bluish) B A 4 * 3,6 red black (bluish) AB 6.6 v.v.s, deep and black dirty F C 3 hrs. 7*2 v.v# s, ?reen ,-v s.deep & black dirty G G 4-1/2 hrs. 7,2 v.v, s. ;reen sdeep & black dirty I C 31 hrs 8*9 dull v.s.aeep & black DUP050316492 HA MD LD KD JB 0C PG 4 hrs* 4 2 n n 1w 4 hrs* 8 ft 2.6% 4.6 4,7 5*3 6.7 8*6 8*8 very red red red red v.s.red & dirty dull dull deep and black s.deep & black s * deep & black So deep & black s.deep & black s.deep & black v#s.deep & blaek Order of blueness in lacquer under intense illumination - least blue, I, G, F, A, B, C, 1, D, bluest, least blue, F. 0. K. L. M, K, bluest* o A - dried at 180 F in Research Lab. steam oven* B - sampled from barrel & immediately canned. C - heated over water in desiccator at 140F in $2 Lab. D ~ dried at 140F in #2 Lab. oven# oven* DUP050316493 ' gHByw Uu>i--'*Y ' $$$' ' s j t - 3 9S~ PIGMEFT COLOR RESEARCH REPORT S-140*D - MOIS TUBE STUDY / / ,.s s' SUBMITTED BY; Z M\ : APPROVED BY; > *M*&*'** _ f*-/3 FILE: ifteFHBKJBlT DATE: NOVEMBER 1935 HITRQDUCTION Two series of experiments were conducted in the laboratory to determine tiie connection between the moisture content of E-140-D and its ameft^i'ssttnon^ee. in lacquer and "Dulux." SUMMARY AMD COFCLUSIONS The moisture content of samples of this color was varied* Moisture determination were made by the toluene distillation method. In one series material from lot 15879 was used; in the second, material from lot 14766. When the lBCquer panels made from these samples were ree^isved- under intense illumination, the variation in hue was found to be more important and more easily observed than the variation in depth* The trend of lacquer masstone was found to run from a brownish through a purplish to a. bluish tone (the last for low moisture contents)* These changes in hue complicated the estimation of color saturation* The tendency toward increasing blueness with decreasing moisture content becomes most pronounced for moisture contents slightly above 5 percent* As read under the usual illumination there is a tendency for decreasing depth with decreasing moisture content, the depth falling off most sharply at moisture contents slightly above 5 percent and increasing slightly for further decreases in moisture content* Material testing v.s. deep and black to deep and black vs standard was obtained with moisture contents from 7*4 to 14*8 percent, Fo material was obtained testing red vs standard under the usual illumination* The trend of masstone in "Dulux" was toward increasing greenness with increasing moisture content. For very low moisture contents the masstone passes through dirtiness to paleness, dullness and grittiness* Material testing v,vs. green in "Dulux* was obtained with moisture contents from 9*9 to testing v*s,green from 12*4 to 12.6and testing v*v,s* red at 10,2$. DUP050316494 EXPERIMENTAL DETAILS See notebook 365, pp^-109-111. Expo D C B A 1 F a H Treatment Moisture Method Period Content "Bulux" Reading Lacquer Reading vs.Standard vs Standard A 23 hrs, 3 58# pale,dull, gritty v.s.It, v.s.blue A 6-1/2" 3.9 pale, dull, gritty v.s.It, v.s.blue A S 5.0 pale, dull. gritty s.lt. s.blue B - 10.2 v.v.s,red & dirty v.s.deep & black C 2 hrs. 11.0 v.v.s.green s*deep & black C 4-1/2" 12,4 v.s.green c 8 " 12.6 v.s.green c 23 " 14.8 s, green 3.deep & black s.deep & black s.deep & black M B 3 " 7.4% v.s.dirty* deep & black L D 2 " 8.0 v.s.dirty deep & black K B 1M 10,0 v .v.s* green deep & black I D l/2 " 9.9 v.v.s.green deep & black 1 B * 12,4 v.s.green deep & black * Gloss -- v.v.s . low. Order of increasing blueness in lacquer under intense illumination - least blue: H, F and Ci E, A, B, C and D, bluest* least blue: I, J & K, 1, X, bluest. Method of treatment: A - heated at 180F in Research Laboratory steam oven B - sampled from barrel & immediately canned. C - heated in desiccator over water at 140F in #8 Lab, oven* B - heated in #2 lab. oven at 140F. DUP050316495 ter3*"0' PIGMENT COLOB RESEARCH REPORT SUBMITTED BY: APPROVED BY: MAROON TONER. RT-219-g AND RT-397-D ? At* o? PILE: M^-rS-f-MAROCHS-. DATS: NOVEMBER 1935. I1TBOPTIC TI ON In view of Parlin's anxiety over the observation that several batches of RT-297-D had shown "blooming" on aged lacquer panels, and because of the known bad behavior of RT-219-D in this respect, it was decided to attempt to develop formulas for RT-219-D and RT-297-D which would be free from "blooming" tendencies* SUMMARY AND CONCLUSION'S Parlin has expressed a belief that the light Maroon Toner, RT-219-D, would probably be in demand by the automotive trade at some time in the future and that, therefore, some attention should be given to the problem of making RT-219-D non-blooming. Consequently this problem was started in the laboratory with a view towards decreasing to a minimum, or eliminating entirely, the free Naphthanil Bs from RT-219-B, since it has been shown that this ingredient is the material which "blooms" to the surface of lacquer panels. The question of an accelerated and reliable test for "blooming" was given some consideration. Lacquer panels were prepared in varijou ways, including spraying and pouring, air drying of the several coats, drying at 60C and drying in a humidified atmosphere. None of these methods proved to be a satisfactory accelerated test. Only in cases where the N.B.S. content was extremely high did "bloom" develop in a few days. In view of the above^ it was decided to concentrate on the elimination of free N.B.S. from the final pigment and the development of a satisfactory test for N.B.S. in a plgmeny. It was fo$nd that DioxSn (Carbide and Carbon Chemical); was a good solvent for N.B.S., and that small amounts were effective in assisting solution of N.B.S. in caustic soda. It was also shown, when a solution of N.B.S. end B.O.N. (in NaOH) was acidified with acetic acid, that the B.O.N. remained in solution while the N.B.S. was precipitated* From these observations a semi-quantitative method was developed for determining the amount of N.B.S. in a maroon pigment. Briefly it consists in treating a powdered pigment with a solution containing caustic soda and Dioxan. The filtrate from the mixture is acidified with acetic acid and the resulting precipitate (N.B.S.) is filtered and weighed. While on the subject of tests and analyses it should be mentioned that in a previous report it was erroneously stated that N.B.S. upon heating bet\?een 1100 and 190oC, was decomposed into metanit-r.an:ixine (M.N.A.) and betaoxy naphthoic acid (BON) and that the M.N.A. sublime. off as yellow crystals. It has been found that purified N.B.S. does not mublime or give off sublimation products when heated to 190C* The early erroneous observations was based on tests made on impure N.B.S. which contain appreciable amounts of both B.O.N. and M.N.A. I DUP050316496 The use of Dioxm allows very rapid and complete solution of N.B.S. in a 1$ caustic soda solution at room temperature, thus producing very little hydrolysis. Couplings of RT-219-D made with the assistance of Dioxan ana by using purified N.b .S. were brighter and, fatter in lacquer bleeding than RT-399-D. From these results it seems probable that the coupling from MNFT - N.B.S. is inherently non-bleeding in lacquer but that the ease with whioh N.B.S. is hydrolyzed Is responsible for the slight bleed obtained (M.N.P.T - B.o.N.^.2 An experiment on reduction in the amount of N.B.S. in the coupling, showed that it was possible to reduce the amount frost 35 g to 29 g per 0.1 mol coupling and still apparently obtain satis factory coupling. The final pigment still showed a test for excess N.B.S* A caustic soda {Clayton Yellow) treatment of the slurry at about 50C prior to filtration practically eliminated all of the excess N.B.S. Lacquer grinds confirmed previous conclusions that the extent of the "bloom" is proportional to the amount of free N.B.S, in the pigment. The pigments which contain larger amounts of N.B.S. showed "bloom" after a few days, while those with lesser amounts required a larger time to develop "blooming." It is hoped thst those pigments which contain practically no free N.B.S, will never develop "blooming," As a supplement to the above experiment on reduction in the amount of N.B.S., half of each of the above slurries was treated with acetic acid to determine the effect on "bloom" of N.B.S* present v#sthe free hydroxy compound as well as the soda salt* A sample of RT-219-D nfcioh contains no free N.B.S, as well as controls containing about 7% of N.B.S, present as the free hydroxy and as the soda salt will be submitted to DuPont Philadelphia for "Bulux" durability tests. It is believed that possibly the free N.B.S, in the RT-219-D and RT-297-D might be influencing the durability of these Maroons in "Dulux." e x p e r ime n t a l d e t a il s Notebook No. 419. Series 419-27 investigated various methods of pre paring lacquer panels with a view towards finding an accelerated test for blooming. Various methods, such as air drying of each coat (pour-out) for 5 minutes and 30 minutes, air drying in a humidified atmosphere, and drying at 60C , were tried, but no bloom was obtained after a period of about three weeks even in the case of a Maroon to which N.B.S. was added in the grind. Series 419-26 was a comparison of various methods of dissolving N.B.S. in formula RT-219-D; as well as an attempt to extract free N.B.S. from the pigment in slurry form. The methods of dissolving N.B.&. included (a ) the RT-297-D (boiling) procedure, (B) the RT-399-D (90C) method and (G) a room temperature solution with the aid of Dioxan as a wetting agent. In the latter case, solution of N.B.S. takes place readily and completely in a dilute caustic soda solution. DU P050316497 Lacquer bleeds decreased from A to C, brightness increased from A to C, yield increased from a to 0* After three weeks it seemed that bloom was appearing in C, slightly in B and absent in A* These facts are probably explained as follows; the amount of hydrolysis of ^.B.S, was decreased from A to 0, thereby resulting in lower^lacquer bleed (less M.N*P.T* - formation) and in more excess H.B.S* which would increase the yield correspond** ingly and cause blooming* Addition of caustic soda to the slurry at the end of coupling dissolved some of the excess ^.B.S. which was precipitated from the filtrate and identified* Lacquer panels on these Maroons did not bloom after three weeks* Series 419*39 reduced the amount of H.b *S. in the coupling from 17*S g, to 14.5 g per 0*05 mol M.H.P.T. Apparently the coupling was complete in all oases* The yields deereased in proportion to the decrease in N.B.B. and the blooming was apparently in accordance with the amount of .B.S. in the pigment. After four days, Af which contained the greatest excess of N.B.S., showed a distinct bloom; within two weeks, B and G showed slight bloom; D (which contains a slight amount of free K*B*S.) has not developed a bloom as yet. Half of D was treated in slurry form (D-l) at 50C with caustic soda and filtered* This pigment (D-l) does not contain free Jf.B*S. according to qualitative tests* Series 419-20 & 58 were preparations of samples qf RT-S19-D, for "Buxux" durability purposes, which contained free ^.B.S* present as the sodium salt and as the free hydroxy compound and a sample practically free from excess NJB*S* Series 419*31 was a study of the effect of varying amounts of K.b .S. on blooming present as the sodium salt and as the free hydroxy compound. According to semi-quantitative analyses, the above samples varied from 4.5% to 0 JT.B*S* The lacquer panels will be watched earefully for blooming* DUP050316498 397 PIGMBHT COM RESEARCH REPORT MAROOH TOBBB RT-399-B 3 rf/, sumsiTTED b y * CA.liuo . m,i! i8--s88es APPROVED BY: /AMj BOYSMBSR- 1935 IHTROBTJCTIOB One Batch, was made in the plant under Development Section super vision using lots 8 and 9 of Haphthanil BS purified, pre-shipment samples of which had given satisfactory resultsfin the Raw Material testing laboratory. SUMMARY & COHCLUSIOHS This batch was made to check the standard formula RT-399-D, K-7782, except that no Pigment Green B was added for shading. The standard process worked quite smoothly, a satisfactory KBS solution being secured with standard conditions using the purified HBS; this was not possible previously, using the special lot of KBS (lot 308). (In the case of this special lot it was found necessary to increase the concentration of caustic soda in the original HBS solution which is considered undesirable when attempting to produce low-bleed mater ial) . The lacquer bleed on the batch made this month was undesirable, the bleed being as bad, if not worse, than any batch of RT-399-B made in the plant heretofor. Otherwise, the product was satisfactory, test ing v.s* light, bright in lacquer vs. RT-399-D standard. This type material gives standard RT-399-D when shaded with dark brown shading batches containing Pigment Green B provided bleed is satisfactory. There is only about 5 lbs. more of the purified KBS available, so that no test can be made in the Semi-Works to check this result. Serious development work cannot be done until a reasonably largamount of intermediate (+ 1000 lbs.) is supplied to us by the Dyeworks. This substandard batch has been transferred to RT-297-D sub standard stock and as such is easily shadable. Results are tabulated in Table I. BXPBRUBKTAL DETAILS H.B. 473, page 54 HBS Rubout Results Lacquer Results Yld. Hote Batch Formula ___ Lot Amt, vs. RT-399-P Std, vs. RT-399-P Std. Bst Lump 40348 Check std. 8 formula K-7782. Ho 9 pigment Green I53 172 s.dk,vs brt-vs str & yel -t v s str - s.yel. v.C.jvs lt,brtbleed worse Grind: vs It,brt- bieed worse 455 418 HBS solu tion satisfactory with std. procedure. DUP050316499 PTflMTCWT COLOR RESEARCH REPORT PISMSNT RUB IKE G LAKE SUBMITTED BY: APPROVED BY: -- FILE: PIGMENT-.RUBINES'-fT* DATE: NOVEMBER 1935* INTRODUCTION- The problem of preparing a lake of Pigment Rubine G was completed in the laboratory this month. A formula and sample were set up as K8G8S* SUMMARY AND CONCLUSIONS In the September report, mention was made of the discovery that increase in the amount of soda ash in the alumina hydrate base diminished the difference (by rubout) between the slurry mixed lake and the corresponding dry mix* However, it was found that beyond a 30:81 ratio (on an "as is" alum to soda ash basis), no appreciable effect was obtained, and that the product was still somewhat dark and muday in mgsstone, blue and dirty in tint compared wi-th a dry ml&o It was further shown that the use of a large excess of strontium in the precipitation of the toner in addition to the use of a 30:SI alumina hydrate gave a lake which matched a corresponding dry mix* This lake, K-8082, was evaluated in printing ink versus a corresponding lake containing a regular 30:15 alumina hydrate and versus corresponding dry mixes. The results showhd all to be satisfactory in the general printing ink properties including livering. In proof prints all were practically equal to each other. However, by rubout, the lake containing the 30:15 base showed considerable difference compared with the dry mix, in favor of the dry mix* In the case of the 30:21 hydrate product, only a slight difference was noticeable by rubout. E-8082 contains approximately*46% strontium toner, 24% barium sulphate and 30% alumina hydrate* Compared with RT<-359*D, it is lighter in masstone, higher in printing tone finish, distinctly less bronzy, about 54% weaker and about equal in tint* Although the results show that there is apparently no advantage in K-8082 over a dry mix of RT-359-D and the proper extender, it would seem advisable to include in our line of colors a lake of Pi^uent Rubine G corresponding to the lekes of Lithol Kubine (RM-257-D) and of permanent Red 2B (K-7909) (See page 1-A) EJPERIMENTAL DETAILS Notebook No* 463. Series 463-35 studied the effect of decreasing the amount of alumina hydrate in Pigment Rubine G lake frcm 55% to 15%} also DUP050316500 >1-A* 7 The other experiments, which were found to be without merit in eliminating the reaction between the alumina hydrate and the strontium toner in slurry form, included: preparation of hydrate from alumina chloride; treatment of the toner slurry with zinc oxide; reverse striding of the dye solutionminto strontium; The reverse strike resulted in a very dark masstone, bronzeless printing tone, blue tint and slightly inferior lightfastness. It was also demonstrated that the extended color exhibited the same property of absorbing moisture as the strontium toner, with an accompanying tinctorial change# Consequently the lake, K-8082, should be dried in a humidified atmosphere similar to the toner. DUP050316501 -a- effeet of aluminum chloride base; and the effedt of treating the strontium toner slurry with zinc oxide; and the effect of using a large excess of strontium in the strike* The use of a large exoess of strontium in the strike together with a 30:SI hydrate gave practically the same result as a dry mix* All of the other experiments gave darker, browner masstones, with bluer tints* Series 465-54 was a check run on 463-33E (large excess strontium - 30:21 hydrate) and a comparison of this lake with one prepared exactly like it except for a 30:15 hydrate base* The previous results were confirmed,, It was also shown that these lakes behave similarly to the strontium toner with regard to absorbing moisture and changing tinetorially from dark - blue to light-yellow colors* Series 463-55 were preparations of samples of a toner, lakes containing gloss white bases and dry bases for purposes of evaluating in printing ink* The results showed very little differences according to proof prints, livering, etc* between the dry mixes and the slurry mixed products* Series 465-56-37 tried reverse striking of the dye into the strontium; also effect of varying the elum-soda ash ratio from 30:22: to 30:25* Reverse striking gave a very dark, blue tint prodiict with slightly inferior lightfastness* No advantages were obtained by the use of more alkaline bases* Series 465-38 was the preparation of a largd sample of 463-35C (46$ P*A*M, 24$ blanc fixe, 30$ alumina hydrate) which was designated as K-8082* I 1 DUP050316502 n9f +7 PIGMENT COLOR RESEARCH REPORT -SUBMITTED BY APPROVED BY: VAT DYE PIGMENTS ~.y-- S j iA3 Cf FILE: #6~?Se d a t e : NOVEMBER 1955* INTRODUCTION Work wss resumed on tlie vet dye problem this month with the main object of preparing lakes of Ponsol Blues GZ, Gl , BCS, end Ponsol Violet AR for durability testing in "Dulux" and in ,,Duoo.,t These lakes habe been prepared and heve been set up as K-8059 to 8066 inclusive* SUMMARY AMD CONCLUSIONS In a previous report which covered the evaluation of several vat dyes for pigment use, it was mentioned that the most promising dyes of those tested were Ponsol Blue Gl , Ponsol Blue Bcs and Ponsol Violet AR* Therefore, lakes were prepared this month from these dyes both on alumina hydrate and on blanc fixe* Similar lakes from Ponsol Blue GZ were also included for control purposes* These lakes were prepared primarily for T,Dulux" durability tests but they will be submitted to Parlin for "Duco" exposure tests as well* The blanc fixe lakes were included because recent "Dulux" exposure tests have shown indications of slightly better film durability in the case of Kentucky's Century Blue, which is known to bd a blanc fixe extension of a Ponsol Blue* The use of blanc fixe alone did not coagulate the vat dye suspension completely, so it was found necessary to employ small amounts of alumina hydrate in addition to the blanc fixe* KNo* The following is a description of the lakes: Composition Lab, No* DyeAM*$ Blanc Fixe Alumina Hydrate K-8059 K-8060 K-8061 K-8062 K-8063 K-8064 K-8065 E-8066 470--2lA 21B 21C tt 21D 2IE t? 21F tt 21G t 21H Ponsol Blue GZ GZtt Tt n t GL GLTt tt Tt ft BCS tt Tt BCS Tt Violet AR tf tt fr 13 13*5 13*5 14 12*5 13*5 13*0 15*5 7? - 76*5 *> 73*7 * 77 - 10 '86*5 10,0 86*0 13*8 86 5 10 86*5 * A.M. s Aniline Matter or dyestuff content* The Ponsol Blue GL lake is very close tinctorially to BP-121--D (from Ponsol Blue GZ), and according to fadeometer tests is equally as fast* The GL dye costs about half as much as GZ* The lakes, K-8061 and K-8062, should therefore prove to be interesting substitutes for the present BP-121-D* The BCS lakes are redder in tint than GL and DUP050316503 cost about the same. In light fastness BCS is about equal to GZ and 0L The lakes, K-8063 and K-8064 should be valuable for matching redder shades, as will be seen later. The Ponsol Violet AR lakes are distinctly violet in shade but the dye is about as expensive as GZ and its light fastness is not the equal of the GJg; type* However, K-8065 and K-8066 might prove beneficial where very red shades are desired* DuPont Philadelphia is now using mixtures of BP-121-D (from Ponsol Blue Gz), B-lll-D {Prussian Blue, BS-92-D (P.T.A* Toner of Crystal Violet), Ti02 and Timinox for matching Ultramarine Blue shades. Their Special Sign Blue enamels, BDR 87731 and BDR 87745, are made up from such mixtures and are only approximate matches for Ultramarine Blue, lacking in brilliance and cleanness* We were able to match BDR 87'731 with K-8064 (Ponsol Blue GL$ and white; as a matter of fact the vat dye combination is cleaner and distinctly superior in light fastness* BDR-87751 Match BP-121-D - 71*3$ B-lll-D 7,8 BT-92-D *** 7 6 TiOg 8*1 Timinox 5*2 K-8064 - 94$ TiO - 3,6$ Timfnox - 8*4 In the case of BDR-B7745 (redder shade), it was not possible to obtain a good match with vat dye lakes alone. Ponsol Violet AR was too dirty* Ponsol Blue BOS was not red enough* However, a fair match may be obtained with a mixture of K-8064 (BCS) , K-8066 (AR) and white* A good match may be arrived at by substituting K-8064 (BOS) for B p-lSl-D, which allows the use of much less BT-92-^ and consequently better light fastness* For example - BDR-87745 BP-121--U BT-92-D TiOg Timinox _ 53,6$ - 37*7 ` - 9*4 5 - 103 \ Match K-8064 -80$ BT-92-D - 10$ TiO,, - 5$ Timinox - 5$ The above information will be submitted to Philadelphia for their use* EXPERIMENTAL PET AT IS Notebook No. 470 - pp. 72-91 incl* DUP050316504 3S~- ffoo - PIGMENT COLOR RESEARCH REPORT * SUBMITTED BY: ,, APPROVED BY: '' PIGMENT GREEN B LIKES .-------------------------------------------- <**3.7/ -- FILE: BKSfl^-GRSHi-~B- ' DATE: NOVEMBER 1935 INTRODUCTION The problem of developing a dry Pigment Green B lake for paper coating was given consideration this month* SUMMARY AND CONCLUSIONS The superior strength, yellowness and cleaness of GL-407-D over GT-68-P by the EHspear dyeing test is likewise exhibited by the casein brushout test. The preparation of a lake, by adding a base (baryteshydrate) to a slurry of rosin soap treated GT-68-P, salting, filtering and drying, was unsatisfadtory frcsn the standpoint of wetting with water. Likewise, the use of GL-407-D in the above procedure, was unsatisfactory. Increasing the amount of rosin soap in the lake improved the wetting with water but did not improve the dispersion, A simple dry mix of GL-407-D, barytes and hydrate gave very good wetting and good dispersion by the brushout test, a corresponding wet mix which was dried without filtration, was very unsatisfactory in dispersion. It was belieged that the wetting, and redrying of the GL-407-D was responsible for the poor results in water dispersion. Accordingly the method of adding the base to the pulp of GL-407-D before drying, was tried and satisfactory results were obtained. However, when the amount of hydrate was increased to correspond to that employed in the RS-325-D base, poor dispersion was again obtained* It is believed, now, that the reaction between the alkaline rosin soap in OL-407-D and the hydrate is responsible for the poor results. This point will be checked in future studies,, In an attempt to obtain a more satisfactory full strength brushout color, china clay was substituted in various amounts for barytes in the barytes-hydrate mixture. It was found that a combination of clay and hydrate in the ratio of about 6:1, gave a satisfactory color with respect to depth on a full strength brushout. This method 483-25F, will be used in future studies on suitable methods for preparing this lake which consists approximately of 10% F.G-.B, 10% sodium rosinate, 10% hydrate and 70% clay. This lake, by dry mixing of the hydrate and clay with GL-407-D, gives satisfactory brushout results, but its dry appearance is very undesirable* ,fTi-*Bar" was found to decrease the strength con siderably compared with clay* It was interesting to observe that the addition of rosin size to GT-68-P prior to dispersing in casein solution, gave DUP050316505 3 results which approximated those from G-L-407-D, Bosln size had the effect of increasing the strength;s slightly\';making the tint yellower end cleaner* / EXPERIMENTAL DETAILS Notebook Wo a 483* Series 482-20 were preparations of 5, 10, 15$ Pigment Green B Lakes on barytes and hydrate following method 482-18B (rosin soap treated GT-68-F added to base and then salted)* These lakes were poor in t o ter wetting and gave poor dispersion by brushouts* Series 482-"21 increased the rosin soap content of 482-20-B {10$ lake); also tried preparation of a lake starting from Gb-407-D, All were poor in dispersion by brushout test. Series 482-32 compared dry mixing of G^-407-P, barytes and hydrate with wet mixing followed by drying without filtration* The dry mix gave very good strength by brushout; the wet mix gave poor dispersion. In dry appearance* the dry mix wv.s very unsatisfactory. Byjes 482-25, In this experiment it was found that Addition of barytes and hydrate to the pulp of GL-407-D before drying gave satisfactory dispersion by brushout, in fact equal to a dry mix* Series 482-24, Tried decreasing the Pigment Green B content with a corresponding decrease in rosin soap* Poor wetting and poor dispersion {by brushout tent) resulted. The full strength brushouts were all too dark and nonuniform in color. Series 483-25 substituted china clay for bsxy-tes in 482-23G also substituted "^i-Bar" for barytes. In these lakes s 6jl ratio of barytes to hydrate was used as in the RE-385-D base* The lake containing Clay and Hydrate gave a satis factory full strength brushout with respect to depth. ftTi-Bar" gave decreased strength. The clay and hydrate lake, however, did not equal the strength of the corresponding dry mix* This was probably due to the higher amount of hydrate used than previously. DUP050316506 PIGMBHT COLOR BBSBARCH REPORT PISMBHT GBESBT B PULP, ST-68-P 3S~-of StMITTSU BY: Cb-. APHtOTSD BY: /- FILl* B DATS* MOTOMBSR- 1935 IMROPPCTlOlSr Production on GT-68-P in the plant was continued under Develop ment Section s upervision. Pour hatches were made to build up a stock of 1500 lb. dry for rubber. All remaining stock of both rubber and paper material has been shipped to fill existing orders. A pressing study was made in the Semi-Works in an effort to find means of increas ing the dry content on the pulp. STTWARV & GOSTOLUSIOlfS All four batches made during the month were made to check Lot 41873, the paper standard. This formula has consistently given satis factory material for both paper and rubber. All four batches were satisfactory in both paper and rubber on the basis of tests in the Krebs laboratory. Samples have been forwarded to the Paper laboratory for their test in order to make the material available for either paper or rubber stock as required. The problem of increasing the dry content of the pulp has been solved by using the steam pump when washing the pressed color rather than using only the ordinary water pressure. This causes an apparent loss of color at the start of the wash, but final yield is improved as handling losses are decreased when a firmer pulp is secured. It may be noted that it has been deemed advisable to revert to the use of 40 cakeB in the 30 x 1" press as explained in last month's report. Yields on these four batches showed a considerable improvement over those secured in the past two or three months. A yield averaging 96-1/2# of estimate was secured as compared with 91# and 93#, the aver age yields of previous months production. Loss of yield on re-working in the straub-mill on this month's production was lower than average, bei ng about 1-1/2# average loss for the four batches. The average loss for the previous six months (May to October) was approximately 2.3#, the losses varying between 1/2# in May to 4# in June. The probable explanation for this seemingly considerable grinding loss in June is the faulty dry content results on the original pulp due to lack of uniformity of the pulp coming from the press. The same reason can be given far the extremely low loss in May. On checking the final yield results on the production for these two months, they were found to be equal to each other and to the over-all average yield on this color (96# of estimate). These results would seem to prove the above point. A pressing study run in the Semi-Works using plant slurry gave interesting results. A control pressed in the manner that had given a3 high as 35# pulp with Semi-Works batches of GT-68-P gave the low percen tage dry content of 23.8#, which ohecks plant results using the sane DUP050316507 .2 pressing method (gravity pressing, washed under ordinary water pres stare). treating the slurry before pressing with 5% (based on dry pigment pre sent) of Turkey Hed Oil gave a firmer pulp with a higher dry content,27$. yield on the second batch was considerably higher than the first, show ing a 10$ increase. As considerable care was exercised in splitting the slurry when pressing, this increased yield is probably die to lower handling losses with the firmer pulp. These two experimental batches when tested in paper on an equal toner basis gave practically equal re sults . Shipments have been large this month, a total of 1617# dry having been shipped for rubber and 4150# pulp (1049# dry) shipped for paper. Production results are tabulated in Table I, shipments in Table II, and the Semi-Works pressing study in Table III. BXPERIMEarTAL BBTAlIS JT.B. 473, pages 97-100 DUP050316508 <0 fr *p 00 0 r- 0 4f* fH P ti O 0 r--1 P` cS 0 cu > ft xm> *t m <s> tk iH * tu OS Q <D PI rl fr- * bOO P H ^ Ih K &d ^o cb H o uo u H>Cm t1hs CfeO 43 t+ in o W co -p O TO 40 0 h 0 P 0Pi fcrf o Ih m & W O P 0 H id 0 1 M p X v}- O 1 44 P Vi. o> CO O lid -P o 0uft jmo 0 gw fc" %& OS *H ,r* <,36 Mo St>> TS 35-. IU . O^ <0 I to ft *D CO u H t t* Q i*5 1s*4 T>1J -"H5O2 =tfc I CM O ft Pi 0 *rt W ftj O p Q H 43 bd 00 > 11 & & VI V. fr- in to CM O* -0p Cr*Of' E-i +' o 1 -!P 43 0 S* & O &d o M O u 0 *p 1% 0 H 85 3U ft G$ H &B h P 0l5 to 4* 43 6(daHn C* }> j* 44 U I PS VS 3 fist* ft jg as 53 H &0<-' *r! b v>* 0 t3 44 ctf 0 p 44 -P 0 f-. O 43 m tn CO 1 in 0 a* 00 CM CO---- "2? CM in CO CM CO in CO CO ^4* CM 00 44 t 3 g 3 44 0 0 'CJ a 43 Xi 0 O CO CO o> <0 CO a* in C3 to frCO <0 CM CM 00 1 00 0 *d< CO 00 co *--' 0 in CO rH <0 CM tn CO 05 in CM O 0c0o m frco CO ID CM in 03 CO fr *> CM 00 fr ee rH 44 CJ *8 ex* to to CO fr- H 0* tn 0 to 0 to <sH 00 d* H to o 8 o 43 0 4s! ffl 0 f40 44 0 orf -p t> b S3? m 0 0 t* P P in o S0 -P 42 bO <ri to p H 0O 0 *4 i fe ft as o 8 43 f-4 0 2 8 # ma aM a: u H > VI- fH Q VI CO TS 56*31 CO c- :> ' CO TJUj fr- CM CM *tS CM r4 rH 0 ut *0P tO1 H rf rH >* o> rl in to <0 <0 i-4 t 0 to 0 SU 0P 0 bO 0P o tn n 0 45 0 O "8 *P4i Sfe a pp .0 t> 44 0 U0 P r-i in 0 *C <--I *rl cbtf0 43^ OP tn a co m 3 rH p H &o oP p t& ^ -p fr- PO O oCM O ^ 02 AP H 0 *r! 4(04 00 V, ts ffl B 5^ o H -P >> m43u*b0 P P 0P0OP 00 0>m*. O$h in O 0%; 0 d CO 43 CQ 40 C rl tn fes d4 trs O CM tn *4' fr- DUP050316509 S~& 4 TABIE II GT-68-P SHIPMENTS Paper Rtiber Test Test Biapo- Weisht skipped and Lot Composition t t S * 13926 vs.41873 sition destination 43799 44332 44521 -- OK- ws bl & clean t s str- OK OK- vs bl 15$ weak v.we ate IT OK rubber 1236# at 25.8$ = HG paper 319# dry. Skipped for rubber. * 1459 at 25.1$ = 366# dry. Shipped for rubber 1338 at 26.1$ = 350# dry. Shipped for rubber. 44547 *" *** s.wk.s.drty v.dirty accepted rubber. KG paper 994 at 25.1$ = 249# dry. Shipped for rubber. 44916 0 1 o weak OK rubber 1434 at 23.1$ = KG paper 331# dry. Shipped for rubber 45333 ''*** * t v s wk.OK 45379 OK - OK 15415 44999 leaf filter ed to raise dry content. 5$ wks .drty 8$ wk vs drty OK rubber OK paper Hr 1387 at 24.6$ = 341# dry. Shipped for paper. 1507 at 24.6$ = 371# dry. Shipped for paper. 5$ wk- OK 1329 at 25.15$ = 334# dry. Shipped for paper. DUP050316510 -BWmm GOLOR RESEARCH REPORT 3S~~ o %- PLUSHES) PTA PIGMENTS SUBMITTED BY*X.-8M&dik APPROVED BYs f*/ PILE* ramfflBTB-^rTEP. b a t e : No v e mb e r - 1935 HTTROBUCTICM Investigation of the flushing of PTA pigments has been started with special emphasis on a careful comparison of flushed inks with those made by grinding dry colors. An attempt was made to apply the ^pellet** technique to phosphotungstic acid pigments. SUMMARY & GOHCLUSIOHS As a result of considerable work, a method has beendeveloped whereby inks can be made from pigment pulps, substantially identical in percentage composition with those from a dry color control. While not absolutely quantitative, the procedure has been perfected suffi ciently to a point where the uncertainty with respect to composition is of the same order as the precision of the tinting method. Thin work has shown very definitely that in the case of the pigments inves tigated to date, RT-329-D, BT-100-D and BT-125-B, flushing on the ink mill gives no improvement in strength. While slight differences in consistency and flow have been noted, in view of the inadequacy of the testing methods, their significance maybe doubtful. The "pellet" technique, i.e. stirring the pigment slurry with the vehicle to give small granules of ink, has been studied in the attempt to prepare flushed inks of PTA pigments analagous to those made from Lithol Red. While partly successful, it is evident that the method is not equally applicable to all types of oolor and may in fact, only be practical with those like Lithol Red which flush very easily. In view of the importance of these conclusions, the evidence on which they are based is outlined in considerable detail below* REVIEW OF PREVIOUS WORK Previous work on flushing of PTA pigments Since the decision was reached to exhaustively investigate this problem, a complete survey was made of the experimental work that has been carried out in these laboratories. The immediate effedt of treat ing these pigments with oil as recorded in the various experimental notebooks is summarized in Table I. It appears that the following conclusions are justified although they may be subjected to revision upon completion of further experi mental investigations*1 1. When treated with a vegetable oil, either on the ink mill or with a spatula on a glass plate, the PTA pigment transfers from the water phase to the oil phase but this flushing operation is not complete as the flushed water still contains some of the pigment. DUP050316511 p H H O A P rH 1 t H O ud p Ch rl s? O H 44 r-3 4s P H P *rl TO op a to *d CO H a o rH bO ak rH O O f# fc 3 P*HH *s O P COhS H *H *H pp O 44 it H P P -P ft P *rt a TO 5h a to O rH O O r--l H *0 a P O % o S3 O 5 AP t* p 0 TO rH H p rH O TJ 43 43 49 a a rl s to m rH UP P TO P H 42 -rl rH rH tfi H p a 41 *H TO 44 t o a rH H ft t, H H o .a p t &d Bf *ri U ^9 rH rH TO Cm TO a9 g 423 CO TO H s ' O ri HP O O T3 fe ffl M O 43 + S3 a *H O3P u j t-< e w ffl -rl P B 3 S3 O K> 43 <rt to H ^ B1 T3 *H W B C !-) -H n) ro '4a3s CBi U iH3 3a H U -P P4T3O 44 ** *pf TO p *w o rH rH ft a pa 49 O O >p 5 P O rH O 0 *rJ 43 a 02 H ch P 5p ^ ffl p *rl ^ 41 d Sp 2 CD rf H Jh I aI 4o3 PO ^ p bO TO3 aO S T*{ t. 49 Ou Ota a -p p I COm r-l r-l TO 44 to 4* p O PP ft Coh M P4a2 PrrtQPHHo>* pO P&O 4*Pr4l O .PO60, rTOl m o toToO ro 4=5 a rfHt O *PTO?P0fHOHt rP0H fP4T<<Q3ODD HCt$uaC,H>HOO HH COOU *rOHH P 42 43 44 S rH rl rH ft <Oh om P ,n 49 bfl o 53 03 CO *> O CO rH 1 10 09 tO b- oi to CM o * b- T0O rv 1 CM rH 03 tn rH lO CO in t- b Oi 4 to rH CM to cs * * 1 CM ~ t *cH to t to 1 p H* rH <0 0* co to 0 *vO O t> CO to 0 44O O 4Q P CO 03 k k O CO CO rH rH 1 t| O rH CO <0 <0 | 09 O CO 1 G> CO A O CO os 11 a> io to 03 CO to rH CM 8k ft n <0 CM CO rH ft 8v (J to CM CO tb rH 1t 1tl 09 CO <D H rH CO tO rH r. ft to rH tl rH eo rH > rH rH 1 09 co> . to CM CO O0 to CO ft * CO rH 1 t <1 t 09 09 rH 09 09 CO I rH CO 03 1I 09 rH o &q co<4153 in to CO CO ^ ^ in CO in CO in 03 CO ^ in 0 <0 eo tn co co 00 =}* ^ to *sH in co tn co CO to to ^1 mm Q o1 1 525 8 r-l T5 O 6-1 O Q0 pR 1t11 H os in O 0 0d CM rH rH rH 1--1 l e- CQ CQ CQ CQ O -P ea I r! TOO (Si ts H>t .P P <D 6* ^ 3 *H a^ HO C3 P CT> r-l lo p cq o rl > TO 3 %4 P iw| 03 S-i Cu 03 3 *H rH (h mO I -p P* O* -1 P rH a0 rH -H > H * 3 O * *"** Eh p rH a0 rH *H CQ S> t4 +o> CoC a rs ' P O Eh ft CQ R 1 09 CM CO 1 Eh 05 r--i Q d 0 p *r4 Ps PS Eh t j 0 05 ' RR 1! O t> CO tn CO co & D5 R 5U 3 TO *iH pa O TO Eh n Q n 43 53 R d to TO P rl a TO nro 0 RR 1t E' C- en co 1 h Eh PJ O a t in co fifc d j ti 1 o rH p rH 0 O rl m P TO pp H B P nd as TO H Ih O 5h TO > B rH O TO Jh TO B O TO P TO P d rH S3 CiS r OUO O > h TOj h S.3 Eh rH rH rH rl P P TO P 43 P *rl P P TO TO H Eh TO TO U TO CQ 3 P fi B <3 CJ & DUP050316512 U 3 2. Upon stirring with oil, PTA pigments may form small pellets which, however, on long stirring coalesce to gobs of fluid ink. This transfer to the oil phase is not uniform or complete at room tempera. ture as there is some pigment still wetjby water even after long stir ring and some of the ink is abnormally high in oil content. , 3. If equal weights of pigment (in slurry form) and oil are passed thru the colloid mill, an ink is formed which tends to gum up the mill. This tendency can be minimized by adding the oil in small portions but son ink coheres to the mill making cleaning very diffi cult. In regard to evaluation of the inks produced prior to the pre sent investigation, no definite conclusions can be drawn as to the relative advantages of flushed and dry control PTA pigment inks be cause of the fact that these previous experiments were not run in du plicate and no one was sure of the actual pigment content. Indications were that the flushed inks showed some improvements in physical proper ties such as flow and texture. As far as strength is concerned, the evidence was not at all conclusive since some experimental flushed inks exhibited greater ana dome less strength than the corresponding dry control inks, while in many of the experiments the inks have never been evaluated. In the future, all experiments will be run in duplicate and no conclusions will be drawn unless the duplicate experiments check one another. REVIEW OP BXPBRIMBHTAL WORK Rather than make an attempt to evaluate these inks that had been standing on the shelves, the decision was reached to semi-quantitatively evaluate ST-329-D, BT-100-D* BT-125-D and GT-347-P. Samples (press cake and dry ground color) jof the. other PTA pigments that are produced in the plant and semi-works are being saved in case the results obtained are promising enough to ejvaluate them. pending the standardization of a reliable method for the analysis of inks, it is imperative to limit the accuracy of the experimental technique so that the maximum error in the pigment:oil ratio of the finished ink is known. '& technique has been developed in which the max imum total percentage experimental error in the pigment:oil ratio is 1.5$. The probable error should be approximately half of the maximum total error. This technique is described in the following procedure in minute detail so as to avoid future confusion. Detailed Procedure for preparing comparable flushed and dry control inks. Watch glasses are tared to the nearest 0*05g. Plant press cake is mixed thoroughly on the glass plate and 100 + 0.05 g. samples are rapidly weighed on the tared watch glasses. The "A" samples are spread ,out on the watch glasses and are dried to constant weight (24 hours is usually sufficient) in the electric oven (140oE). The *B" samples are 3tored overnight in a desiccator over water. The proper number and size of empty ink cans are weighed to the nearest 0.1 g. DUP050316513 Lb |I 4 Before grinding the inks on the mill, a preliminary sample is run over the mill in order to coat the rolls and apron with the same amount of ink that will he left at the end of the experiment. To each of the "A* samples (dried lumps on watch, glass) is added an equal weight (+ 0.05 g.) of Carter's #0 regular varnish and mixed well with a spa tula on the watch glass, pulverizing as much as possible without losing any color or oil and transferring completely onto the hack rolls of the mill. Bo not grasp the rim of the watch glass during this operation as it may break. Weigh the watch glass in order to be certain that no excessive amount of color or oil is left upon it. Adjust the tempera ture of the water running thru the mill to 160 +5 F. Adjust the tight ness of the rolls to a definite setting which is duplicated throughout the whole experiment except when the water is being flushed out of and evaporated from the wBm samples, when the setting of the rolls must be looser in order to avoid having the pulp or ink run off the edges of the rolls. Place a receptacle under the apron of the mill in order to catch any ink which may drop from the apron. Give the ink six passes over the mill watching closely to avoid extrusion of the ink over the edge of the rolls (it may he necessary to loosen the rolls slightly to avoid this). Scrape practically all of the ink from the apron (in cluding the under side of apron), guards and rolls of the mill. In this operation, the personal equation affects the yield of ink tremen dously. Extreme care and patience must be observed in order to scrape the same amount (+ 0.2 g.) off each time and after the ink is weighed, one must never go"back to scrape off more ink in order to increase the yieId. The **B" samples only lost 1/2^ of water on standing overnight in a desiceator over water. Garter's #0 regular varnish equal to the average weight of the "Aa samples is added and mixed thoroughly with the pulp. The rest of the procedure is the same as above except that the rolls are set looser during the flushing and evaporation of all of the flushed water which usually requires 6-8 passes. During this per iod, it requires an experienced operator to keep the pulp and ink from running off the edge of the rolls and it is well to practice several times flushing the pulp before running the semi-quantitative experiment. Some water, color and oil drop into the pan beneath the rolls and into the receptacle beneath the apron and as completely as possible are re turned to the rolls. After evaporation of the water, the rolls are tightened to the designated setting and the ink given six passes over the mill. Extreme care must be observed in the above procedure in order to duplicate results. The grinding of three "A" samples and three "Bw samples should require 4-5 hours. An attempt has been made in T&bH IX to indicate the maximum total percentage experimental error in each of the steps of the above procedure. See Table II. In one case, namely that of BT-100-D, difficulty was encountered in sampling because of the non-uniformity of the pulp. For this pig ment, the maximum total percentage error would probably be higher than the above figure. Evaluation of dry control and flushed inks The evaluation of RT-329-D, BT-100-D and BT-125-B inks is summar ized in Table III. DUP050316514 V bO oG Pu rl rd -P r-f d <0 -H Vi > to c$ H p <ps> o V fl> Pi VI. 03 o r-t -p o M-H op S3 O a O C -P 05 r-t ffl a! t<alj **-4 P-* 03 03 03] m 03 VL .\ "2 r-H 03 MM a I /? bS3O **Hd *&0d p d tfd **-v 0 d O ,0 V P P, u si a p rl H Vi 0O ___t d +to <0 p aa JU 0 d t* VP V 0 u V w> H S3 rl to P a 3 bO to J3 H --p" bO P bD tHo cd .P 1--t bO p p P P PP 0 P Vi O P d OS-, H 0 0 rl P P P Pi Pi & rl rH rH d 23 p jj3jj c& rH bO r-H V P & Vi Vi H 'ifVi O O d s J3 cd @ Ou M p .1 a3 sP cd H Vi 0 tH s0 aO 1-1 s s rl & <3 V O A? P M c P O V 0 p 0 p O O 0 H rl . & p 6-1 H 0 0 & hO P bO bO bD bD ft am p 49 P cd P Vr P P bD P 3 h2 0 g 3 H to bO to O bO H u a H p d cO & S 0 CO O a oS E3 1-1 03 <n e$i in kD E> GO P o> DUP050316515 EVALUATION OF FLUSHED AND DRY CONTROL FPA PISMSKT IHKS RT-339-D C<O0 *p P5033 p* A H <0 p*bdo "-- do pCO ss i--i P a i tt AT3d 02 P S rH ro PP PP rS PO D **9! P 35 PbdO iH rH nd ppp CrQH O P It in <rEHl > P 4 *d >p <i<n 9 P po H rH P > <o TpoH to a> pCHO ^< g*1^. o02 C^O Cr*OH to fO rH to rH rH to O02 *--* *C7POQ3* -<--Pr3*- 11 PSbS-3330 --iCp*-O r=S 1q5) *3 S* H<&f --P* tl (1 PCQ <HT->> rH r*H rin--' pJ3 u p ppe$ os? -H O V 034 O V PoM 11 r$d WP PPd* pQ > dPpri 11 Co H p u bOO rH PP f5Oe=O rH P b0 S3 O rH PP bdO> rH 11 bO so rH P > CO u a 11 fi u t H d > Ad s it VmL 03 VL rH co rH Chr*t rH t- rH o+ rH C+O rH CO rH cHr- rH o02 a rH rH 02 rH OOO VVV Oo? rH* o 0O3* 02 O 02 o V VVVV d S3 .rH -H |Mrl CmO r--* rH rH i t/a cC&r>* -5/ ; <*13--1 CrHiO CO CO o CrO-H rH 1 S"4w** iConf>c cr> 0cr3 ftH04 CoO am? rH ir># fat>- o CoO* to4 oo 0c0r24* rH rH rH rH Ol <fc:rHl CHCc>lQ-3 09 ft-* rH 1 C0 pm*H1 fCtH-OP* rH 1 m <fi5rH1 frCHtmQ- to e rH to- rH 1 DUP050316516 PIGMENT COLOR RESEARCH REPORT 3$r-- `fsf' /' PEACOCK BLUE LAKE, BL-164-D ^SUBMITTED BY: APPROVED BY: A El LE MI S0-*~--TlAT`T-'PjS~ DATE: NOVEMBER 1935 t INTRODUCTION: Production on this high finish Peacock Blue Lake has been started in both plant and semi-works on receipt of an order for 00 lbs. of this color from F. H. Levey. Four batches were made in the semiworks and one batch in the plant and the order has been satisfactorily filled by mixes made from these batches. SUMMARY & CONCLUSIONS: Preliminary to starting regular production a five pound sample of semi-works batch 72 70, our match for C-37745, had been sent to Levey for their test. This material was accepted and was set up as K-7986 and finally coded BL-164-D standard. On receipt of a 200 lb. order from Levey production was started in the Semi-Works. The first batch made in the semi "works during the month was made to check the standard K-7986 formulation except that the amount of dye used was increased 10$. Du Pont Brilliant Blue E, lot 28 was used as in the standard formula. With the advent of colder weather and lower humidity, it was also necessary to dry thiis material in the controlled humidity P. & S. dryers in order to secure satisfactory tint. A drying temperature of 140 F with 30$ humidity has been set up as giving satisfactory results. This batch was strong, v.s . red in tint and v.s. low in finish versus the standard but was easily shadable, being consumed in a satisfactory mix with a weak sub-standard batch of BL-151-D (a lake of the same general type). Production was then shifted to the plant and a batch was made checking the standard formulation except that it was found necessary to make weight on the dye used with Alphazurine Special as the satisfactory lot (lot 28) of Brilliant Blue E was practically all consumed. The re sultant color was low in finish and weak in drawdown on machined paper, altho v.s. strong in tinting strength vs. BL-164-D standard. A labor atory drying study was made to determine the effect on the finish of drying the product more thoroughly. No apparent improvement in finish was secured and the tint was affected adversely. A second batch was then made in the semi-works to check the standard formula exactly, including the use of Brilliant Blue 1, lot 28 which entirely consumed this satisfactory lot of dye. This semi works batch shewed an improvement in finish over the plant batch but was still considerably below standard requirements. A drying study was then made in the semi-works in an effort to discover if drying variables were responsible for the coMstently low finish material being secured. Variations in humidity and length of time of drying were made using a formula to check the first semi works batch (10$ increase in dye). A new lot of Brilliant Blue E, lot 31 was used in this batch. This dye gave satisfactory material in the laboratory when tested on the BL-72-D formulation using Alphazurine as DUP050316568 ur' - 2the standard dye. Hone of the drying variables used had any apparent effect on the finish and the batch in general seemed to be redder agt dirtier than previous batches. Ink mill grinds on the various sections of this drying study checked the rubout results. A batch was then made in the Semi-Works using an increased amount of soda ash in the base. The. substituents of the base were analyzed and used on a 100$ basis. Alphazurine Special dye was used in order to insure satisfactory tint. The resultant lake was high in finish, strong and v.s. red versus the standard. One third of this batch was used to mix off one of the semi-works sub-standard batches and sufficient satisfactory material was secured to ecaplete the 200 lbs. order from Levey. The two satisfactory mixes secured totalled 261 lbs. of which 200 lbs. was sent to Levey. There is enough high finish material on hand to blend off approximately 60 lbs. of sub-standard stock, to give 125 lbs. of satisfactory material. Two more high finish batches are in process in the semi-works and work will be continued in the plant on receipt of further orders. Production in the Plant is tabulated in Table I, mixes in Table II, and semi-works production in Table III. DUP050316569 ** rH <D 09 JEt T3 t2 S-B & SSf.. I! .* < * Ob I J fc* 03 O s ifi if CO o p O Sr rl wo Is 8 6 8 *P CO 'P -P ca o W a A * S m: * m C *: P 03 $ >, S ; > gKf>gcod h t P d A >aS CO O H H cJ H cn 2* UV CO W D CO 09 3-4 l->t 5 CO C<v03 wr->i CQ <0 fcO a 8 133 SE WI g 9 A SS ti I Jftf P w fcg 3* s ^ 4* iS to o g >> **C3 "C at*s mn* M 03 *& o X feO sj to t=> p t> 1 go. 8 g 'S co 1*1 a * p o g <0 ll Jh -0P3 J> *P cS f>* o -p c -3 Es> 8% V st Sb g g ]> t H z**^J *iA w =h fs t d<55 * O* 09 J* 3$ 7// S o s p o V ri *P rt o* 03 0 o 15 CO Ife5 CO o g I <T* fc- A DUP050316570 $o, / I ,,* O JZ 03 cn co H8 -p "p'-' 9A * 73 & o * U*v tPe iii &* O l> -p r-l rH El 'CJ * *4 at s 73 PA m& m> fe fi a* >* 73 St (D A *tf A 83 -cP t > ta et *<* ->P*Mw -P5315 tt s a - ~r 73 tJ U A t* * : F 73 (9 !r ^ t BO *H *?3 ins ; tS gM 73 to > u *tpo CO - rJ ** 4u 51 *H O VO -* * MO oJ8 i-4 I a* Om fr it to iH ' !3s ccvoa 3 1I. m4 WH gp S8 M h s >* 73 s O fc- ca fc- 44 fc 44 r O O P g 6* * 73 2 SIS t? feO ss O Q 6 >% *o <0 p gt Cm fcO SZ t *-* SSt <S3 m <s t- $ Cl sbl? H - 0 -H A g* A) <D 1 & CO C* g s 1 A, ^6"* o4tt>~o fctd~>- t- t~ CO < fe-- fefe- fe- CO <5* 5* o0* DUP050316571 p io ms n t c o l o r r e s e a r c h r e p o r t DISPERSED CLAY COLOR, QE-405-.D SUBMITTED a p p r o v e d BY: <A ' 0 /?// FILS; DATS: NOVEMBER 1935* INTRO DUCTIQH Standardization and production of this clay color was begun in the plant to fill orders from Louis Be Jonge* It was necessary to vary the ratio of- dyes used to obtain proper shade and to obtain clean shading material. Sewn batches were made* SUMMARY AND CONCLUSIONS All except two batches were readily shadeable* These two were very dirty because of over-drying due to neglect to remove from the dryer at the proper time* Drying in the plant brick dryers appears to be satisfactory provided these conditions are maintained* However, material dried in the Semi-Works' Freas Dryer at 140F was slightly cleaner on brushout. A. temperature of 140F for 48 hours is necessary* As in G-e -363-D, complete replacement of Auramine with Thioflavine gave a blue elean product when dried properly. Most of the material was made using a 50-50 mixture of the two dyes in addition of course to Victoria Green* In the plant acetic acid was added to the dye solution or to the water before adding the dye to obtain cleanness* Either method of adding the acid is probably satisfactory. The pH of the finished color slurry should be 7,0 to 7*1* DUP050316572 C*IM /v o CM rH CM O -* o 6=p c- N CN t> a *% a O 4-3 u 6s r-i o & *>* & *d P 4k 1H o H p * r4 r--I * p 43 +3 f--1 --1 c<^ <D rH P *H *S >> h *d 4o3 cfl > P P p ffij * s> * 03 Sr CO 43 * ISO P X c8 J4 P IfiP P *s fc P U A CO * M <D CO *H dNi a t(iir3l<do<d* P H CD P P o 1--t to Of b aa> &o E-< rp0pE3i ef,>ie>aP 'll- P EH & r * p Sd 0 CO H >> O ft) a o tHO S * m a 4 ft o O P 9 <o0 CM C<O# O 0 O CO rH rH rH rH rH O P :1fe -r O !> tO to H Vl ES3 O & PP O p=Hte4q O 03 ft rH 0 CO rH CO rH H rH * Pt d m 1g a p g CO IN p IO p p <tj to O 00 O ^=s* p q rH OS rH P p is; J> O CO A * +9 *s 'UP* 0 *H P H *Ci h rH * *H to d M P 03 * >> * t> r* 0<> S a 0 ^Hrj rH ^HH rH d 05 * d >5 F^fed >s u < * CO CO 0 rr fcJ 0 co CO H p rH tO s ft to t to 0 IM Sr p fc CM 0 to IN p to H 'tp to to to to 00 CO 0 *> % co H 0a CO 03 O 1 rH O CM * tN 01 H tO }> ra fc w 0 H to <tH P O P P ffi Pt O IN O tO P 3 . * d 43 P tjD fj *rl dffi O p Pi p 0fpf3i 03 43 P O 'rodd d 03 0m p ^ > p 0 03 K CC ffi O PP 1=4 P ffi 03 O .M ffi P O ffi 4r IP P a CO 43 0 pp p ffi 42 d ffl p Pp t5p p p ui ffi 1--1 4 P P O 03 03 O O P P . tJ **H Ft <E P O P. 3 ffi d g 4<3D IB & 43 =!fc CM sj> 02 to tJD P tH rH rH 05 O P rH CD H ?* CD P, O & O JH O GO CD rl DUP05 0316573 t1 / Zto PIGMENT COLOR RESEARCH REPORT i SUBMITTED BY: ) APPROVED BY; SEMI-WORKS PRODUCTION' FILE; -GR~8G^ DATE; HOYEMBER 1935. INTRODUCTION 81 "batches of 17 different colors were made during Novembers these included IS batches of RT-354-D, 10 batches of RL-407-D, 9 batches of Y-180-B, 9 batches Of YO-8003-D, and 9 batches of BL-164-D. RT-354-D, Maroon Toner - Twelve batches were made far production of standard or shading material to help in blending Sss. -} RT-130-P, Maroon Toner in Pulp Form - Two batches ware made and shipped to Parlin. RT-7853-D, Permanent Red 2B toner - One batch was made to test a new lot of dye. RM-7909-D, Permanent Red 2B Lake - Two patches were made for the same purpose. RT-139-D, Maroon {RT-297-D} in Pu^p Form - One batch was made for Parlin. RL-407-D, Barium Lithol for Rubber - Ten batches were made in a study of the formula for the" purpose of increasing blueness on rubber test. Y-180-D, Light Yellow - Nine batches were made on development of a new and improved formula. Y-359-D, Medium Yellow - Four batches were made in continuation of the process study being made on this shade. Y-299-D, Medium Yellow - One batch was made in connection with development of a lead nitrate formula. Y0-54-D, Chrome Orange - Five batches were made in a process study of this shade. Y0-38-D, Chrome Orange - Two batches were made in a preliminary study of this process. YO-8003-L, Molybdated Orange - Nine batches were made in development of this improved product. G-S89-D, Chrome Green XL - Tjptree batches were made in continuation of the development of a stronger product. BT-125-D, P.T.a , toner - One batch was made to obtain material in pulp form. DUP050316574 -s BL-164-D - Peacock Blue - Mine batches were made in a study of the process for this new shade ana to obtain material for shipment to Levey. BL-8#47-D, Lake for Rubber - Three batches were made in a trial of the rubber color formula employing Victoria Blue R. BB-114-D. Dry Dispersed Lake - one batch was made for production. 28 grinds'of dry color, 6 grinds of pulp colors and 12 mixes were made in the Research Semi-Works for the plant during November 19 55, Dry Grinds Red Toners Green Bulk Lakes Blue PTa Toner C.P.Blues Charge rt 742-S Batches 6 12 1 7 Lbs. 1462 6992 50 5381 Pulp Grinds Green Toner Red " Charge 73?-S 26 Batches 4 13,885 Bbls. Lbs. 16 1449# ! 8 100# 6 24 2007# 100# Mixes Red Bulk Lakes Yellow ** " Red Toners Blue PTa Toners C.P. Yellows C.P. Greens G.P.Blues Ghiaage 751-S ft ft tt 753-S 755-S 756-S Batches 1 1 2 2 1 3 2 12 Lbs 324 500 365 508 578 1510 345 4130# DUP050316575 Batch b 7420 ' 21 22 23 24 7425 20 27 28 29 7430 31 32 33 34 7435 36 37 38 32 7440 41 42 43 44 7445 46 47 48 49 7450 51 52 53 54 7455 56 57 58 59 7460 61 62 63 64 7465 66 67 68 39 7470 71 #10 BLDG. PRODUCTION REPORT FOR NOYEMBRR 1955 God Lbs Struck Lbs. cL Packed Yield G-389-D 35 BE-114-D 617 RL-407-D 69 B-68-B liquor RT-354-D 27 109 Y-1S0-D 31 RL-407-D 69 Y-359-D 97 ft 20 Bt 20 CT 20 RL-407-D 69 Y0-34-D 135 ft S t? 135 135 RT-354-D 109 RL-407-D 69 Y0-38-D 135 RL-407-D 69 BL-16.4-D 90 Y0-54-D - 155 - RL-407-D 69 RT-554-B 109 YO-800 3-D 30 Y-180-D 30 RL--407-D 66 RM-7909-D 100 Y0-38-D 135 RT-13Q-P 109 GT-68-P am ft - RT-130-P 109 BL-164-D 90 RM-7909-D 100 Y-180-D 31 RT-129-P 200 RL-407-D 69 YO-8003-D - RL-407-D n 69 69 YO-8003-D 30 RT-354-D 109 Y-180-D 153 Y-299-D 160 RT-7853-D 22 RT-354-D 109 ft BL-164-D 109 22 Y-180-D 30 BL-164-D 20 32 581 63 - 27 120 31 67 100 19 21 18 70 133 130 134 120 70 131 70 96 131 am 67 108 30 29 66 92 131 115 - - 120 99 90 31 209 67 -- 67 68 31 112 149 154 22 117 110 21 31 19 91.4 94.2 91.4 - 100.0 110.0 100.0 97.2 103.0 95.0 105.0 90*0 101.5 98.6 96.3 99.2 110.0 101.5 97.1 101.5 106.7 97.1 - 97.1 99.0 100.0 96.6 95.7 92.0 97.1 105.5 - 110.0 108.8 60.0 100.0 104.5 97.1 -- 97.1 93.6 103.3 102.7 97.4 96.3 100.0 107.2 101.0 95.4 105* 3 95.0 DUP050316576 Batch 7872 > 7S 74 7475 76 77 78 79 7480 81 82 85 34 7485 86 87 88 89 7490 91 92 93 94 7495 96 97 93 99 7500 Coda BT-125-D TO-8003-D ft Y-180-D BL-164-D IT 17 71 BL-8047-D YQ-8003-D BT-354-D BL-8047-D TO -S005-D RT-354-D G--389-D Y-180-D BL-S047-D Y-180-D TO-8003-D RT-354-D G--389 -D Y0-34-D Y-180-D ET-354-D TO-8003-B ft BL-164-D ft RT-354-D Lbs. Struck 20 30 120 30 21 19 9 9 34 30 109 34 30 109 176 30 34 30 30 109 176 135 30 109 30 30 45 45 109 6069 Lbs. Packs d 20 31 118 30 21 19 9 9 31 30 115 31 31 117 174 30 35 31 31 116 175 113 31 118 31 31 4749 116 6059 % Yield 100.0 103.3 98.3 100.0 100.0 100.0 100.0 100.0 91.2 100,0 105.5 91.2 103.3 107.3 97.8 100.0 102.9 10St5 103.3 106.3 99.5 83.7 103.3 108.2 103.3 103.3 104.4 108.8 106.4 10S.1 .M*S. DUP050316577 r v7 -5- SUMMARY OF #10 BLDG. PRODUCTION REPORT FOR NOVEMBER 1935. CODE LBS. STRUCK LBS. PACKED 1 YIELD RT^3B4-D RT-7855 RT-130-P RT-129-P RL-407-D RM-7909-D Y-18Q-D Y-359-D Y-299-D 10-34--D Y0-38-D Y0-8003-D G-389-D. BT-125-B BY-164-D 3^-8047^ B1-114-D 1226 22 218 200 690 200 395 157 160 675 $70 360- 387 20 370 102 617 60 1296 22 235 209 675 182 392 158 154 641 263 334 381 20 389 97 581 6059 . 105.6 100.0 107.8 104.4 97.8 91.5 99.5 100.6 96*2 95*0 97.4 101.2 98.5 100.0 105.4 95.0 94 #2 99.4 /Z.y DUP050316578 -6 Mtrial Transferred During November 1935 - Research SW ...... . ........... LotOR-800 Color Code Lbs. Group Cost Unit Cost 4354 4360 4361 4370 4371 4388 4389 4390 4391 4398 4388 4349 4363 4364 4565 4366 4368 1 1 1 1 1 1 1 l 1 1 1 4 4 4 4 4 4 RT-554-D n Tf tt Tt f* tt tt tt tt RT-219-D GY-7925-B G-389-D If ft tf tt 119 2 180 2 180 2 121 2 128 2 111 2 31 2 114 2 117 2 111 2 26 2 157 2 169 2 171 2 172 2 171 2 168 2 115.13 203.46 7.90 11.40 4380 5 B-63-D 93 2 27.10 4319 4367 6 6 RE-341-D BE-114-D 104 1 582 1 25.11 15.18 4386 4387 8 8 YQ-34-D Y0-38-D 536 2 259 2 7f4 7.70 4384 4385 9 9 RM-79Q9-D 92 1 93 1 72.69 4381 10 IP-324-D 150 2 122.51 4378 4395 11 11 BL-164-D GL-407-D 119 1 358 45.70 36.52 4368 4369 4374 4375 4376 4377 13 13 13 13 13 13 BT-S42-D tt RT-13Q-P ft RT-129-P 41 2 57 2 85 1 ISO 1 109 1 101 1 48,15 116.66 195.83 4350 85 BT-7982-D 99 1 338.47 4383 115 RT-7853-D 45 2 135.47 4372 4379 185 125 RL-400-D RL-407-D 219 1 472 8 46.80 46.15 Total DUP050316579 7 RECAPITULATION COLORS TRANSFERRED FROM SEMI-WORKS IN NOVEMBER 1935. Toners 12S9# Yellows 157 Greens 851 Blues 93 "RE" Lakes 636 Oranges 789 "RM" Lakes 185 "RP " 150 "RL" " 1168 Maroon Toners 86 P.T.A. Toners 69 Toner Pulps 705 Maroon Toner Pulps Sll Total - 5, /H DUP050316580 --8 Material in Process as of December 1 1935 Research Semi-orks. OR-200 1 Cod Lbs* RT-359-D 184 RT-354-D 571 3 Code Lbs. Y-299-D Y-180-D Y-202-D Y-359-D Y-309-D 930 731 25 313 450 11 GL-407-D 40 BL-164-D 287 25 BL-125-D 25 4 Code Lbs. 0-389 -D 435 8 Code Lbs. Y0-34-D 135 Y0-38-D 500 YO-8005-D 60 115 RT-7853-D 22 125 PiL-407-D 202 BL-8074-D 93 129 GX-309-D 377 151. Y0-8003-D 390 :tHiP 'V DUP050316581 %TJBMITTEr APPROVED BY: PIGMENT COLOR RESEARCH REPORT RAW MATERIAL TESTING FILE: PB^-MATERI'AL DATE: NOVEMBER 1935. Both items indicated as awaiting completion of analysis in last month's report have been satisfactorily cleared* This month 110 shipments of raw materials were received and sampled and have the following status: 67 tested and found to be satisfactory; 1 satisfactory when previously tested; 1 O.K, in the plant; 1 awaiting completion by analysis; 2 remaining to be tested; 3 used without test; and 34 reported without test, A shipment of Lithosol Red 2B Paste from duPont turned out to be un satisfactory because of apparent ununiformity. This matter was the subject of an investigation. Raw Material Samples light samples were received this month: RMS-1465 - "Lithosol" Acid T.0B. from du Pont. Satisfactory. RMS-1466 - Lake Red CR Pulp #282 from Sherwin-Williams. Satisfactory. RMS-1467 - Lake Bed OR Pulp #282 - Unsatisfactory, Too Dark* RMS-1468 - kake Red OR Pulp #282} Satisfactory. RMS-1469 - " " " w " ) RMS-1470 - Sod. Molybdate Tech, from Molybdenum Corp. Satisfactory. RMS-1471 - H,C, Alumina Hydrate Pulp from Grasselli, Unsatisfactcsry. RMS-1472 - P.C.0,N,A. Crude Press Cake from du Pont, Unsatisfactory - failed to completely diazotize. DUP050316582 OIL RBTEHTIOH OP PIGMENTS NewarkJan. 22, 1935 PILES OIHIOME -iLLLOW- DUP050316583 Me> * Jtei* 2t 1009% . a b analynla is given bnlor af eertai iteeteiieml mrnM<mn%&mM bih we a tearing <m ite oti-MrtnBt&oft properties f pkattsli i general. Bseattaa f eur wtianter interest la elar yellow, viewed ftrnm this angle, iwassrioal. mlmslatieiia hern teen m&@ stewing ill appraxiwata magnitude of the mxtnm nod eapillary force affecting the paropnrtim of than* pJUjnonttt la itdc vehicles. it i imm that thnir ' oil is related to 4te letter ratter than tins fiMf* The effect of particle sine, steps and distribution la relation te ink properties Is disci*sued briefly* The relation between viscosity ate degree of dispersion Is pointed oat* fte maeJiaaleal properties of % dispersion of lead hreiBai la sa oil vehicle son be calculated approximately from the teoas proper* ties of tit vehicle ate the lead ehrasate partleles* The partial* else of Chron* Tolleir pigment* can be estimated la eeverai ways* From the ewrve of ftletel* ate Baitegr it appear* ttsl ooiMereial pigments will temt a partial* radiua of % ac 1Q~ to 4 x IQJ* u lira this curve. p!a**t with a partial eia tm& or greater than this sill have a strength less than 1/3 the obtainable* in Alexander*8 Colloid Chemistry* Vol* X* page 14, raicrossopic limits of resolution are given as 1*115 x l-**5 o c t u m about the middle of this range* A atiexoeoopia exattlaatlen of standard pigments suck m Y-202 B mad Y~UHd iteieatee that so are aasily resolvable at 8065 tegalflmtloM and are mar the neper lia&t given* while otters mm diffieulttf* tesolva&l* or way tbs lower l!t% given, oenerally, all particles wo aypMKiHhtolar tlai tss*e site* Timm particles will possess a Mnimm crurfoea if they are esterleal, and a samwkat larger surface if they have saw.otter shape* The surface of a sphere of unit voltnw ia 4 "{3/4 V)*v* or 4*84 aq# cm* Tte ourfae* of a oabe of unit volusw ia 6 sq* ea or 4*84 x 1S4 an surfaoe of a square ^risquof unit wlum-vith a length five tins* the diaaater will be Sfl/lg)"/3 4- 4(5}f*5 sq e. or 4*SdK(l^} An increase in tte tnniber of faces will- in e&oh esse deerease tte dlf* fertmoe in surface between tte eptere and the prises* In the following calculations? the asstoiiption is node th&t the swrfftee of the uartiele la 1*25 times that of a sphere of equal radius* the surface of a lead chromate pigment with particles of a given . radius osm easily bo ealcrulated For oxsaple in 3 graaw of lead chms~ ate of specific gravity 6*123 and therefor a volume of *49 oo there ore 49/(4/5} fte3 partielee of aarea (125) 4 Is8 aq* n* For E * 2 x 10-4 we teve ( x *-*)] 4*(2 x 10-^)2(l*2)eq*6* or >*5(1*25} (#49) x 10^ or t2 x 108 aq ea* mr l#4s 10-5 we teve (*75} (1.25) (*49} x 10 or 4*0 at 10* eq. au A motto molecular fit of vehiele my be adsorbiHi at tte sSxsf&m of the mrtiele* Tte tMelmese of thin layer will be appruximtely 3 x 10*"? * (Applied X-Reye, Clash, lft4} In organi eonpetmas tte Increment per oorbon ate ia 1 to 1*3 A#g, giving for a thielctees about 3 x 10-T, it i obviow that tte immmm in DUP050316584 m%iol ratios Swsti this etofftot film is mml%* mm 'mtmm f the fito is 3 x 19~f x 4*3 x 10 m m *014 e is e eae* arct 3 x 10^ x 9*2 x 10 ee or.27* e is tto Om ease. SiaxrsmitKg this *41 etoarot plgpont will fee as ataitioaal lam f 41 toM hy tto forooa f apIXlary attraction* If tto tSwg gwa of M atooaata ** dispersed in one grass * 1*#30 tojtf II tto tktekMM ef this layer will to (1*035 - *014)/ 4*3 s l .1#4 e. or 2*3 x itH e* is a eaae and (1*038 #876)/ *2 as 10 m* m a3 x itr* m is tto other mmm* ^Tto term is tan per an* rmi4 to teealt Hit file is aar/R (y * awrfao# tesoloa) (See Atomndor, colloid Ctoatistry* VOX# 2, Pag 24? ani Swottor, CelleM cmeaistry* Pag 184} la tto nrnmrn&k of ctoafatry and PbysiUsa tto tension af alir ail ia given mi 33*3* Assuming tlse mesfmm tottaion of llaMOi 11 |a SO, we get an a sals for tlw breaking (2(S0)/2*3 x 1#**} draw #* (Halt&sIkaplMe by @m x llnH 2*3S la one am mH (2(30)/8.3 x %#J x .99TM 10^ mi m ia the ettor# fte tore analysis isdle&toa that if In tto printing praai peeeraree of frw 10 to 2 wm mmmt&m4 mmm mar M la mm ease a eenutatioa of tto meest and oil while is tto ttor no oopHmtioa will to noted* Finish or tto tondoiiey of tto papoy t r@*aew oil from tto Ink is also related t tte partielo also* Pigment* of largo p&rtiole sis will tare a low finish, and ttos# of small partiol* ofso a high finish, AMoa agents rail as hydrate me aloitaa toalmte will is* ereae* th finish if tter haw a groator earfaeo pox salt moo the xoplsooa pigMSt* ft I otalMisly Iwnatoxial tteidioy thmy aaaa wot or 3*jr if @ ehaag is partiolo also ooosrs* nmj will to isoffootlwe If tto pigwst mtsrally pooiwases a high finish or If po@sasa _ m ....... . ' ` tto pApwst For two pigasssts# harisg partiolos of Hfforant sis tot ^0 mmm top sad grosaai Is auffleleBt roMol to giro Moatioal mmiX* Isry form* ton 4a& tometeristios will to dJyfforost, tto lrgor partial** will giro rolatiwoly etort oaady isks, tto sailor portioloo losgp ooft iste# Vo Waiasena* (oe ColloliSo tgr Hodgor# mgs 203,) classifies dispsrsioas hy ttoir ptiysiosl nropeftlas* Mieroosystallino partloloo giro past jellias* sltmsiawoorystalliB# partial* giro soft olastlo For tm pimmtes having the si^ sortlot swefam tot m ilfforont psrtlel stop tlfforoat ink propawlios ore posoihlo. B^la ho^ or thixotropy am tto wlsoooity of tto ink say to IwttmmM hj Ito partiolo stops (colloid Ctoa&atiy* Hoigor p711}. Has* of fldxiag me wotting my to misted to tto partial sa?~ fao la ^rogatm of asall partloloo and therefore mil par ri&dLlnis, large capillary force will to to tooak up tto a^^egata, la aggrogatas of largo partioiee of large par radius only small capillary fames will to arailahlo to towels up tto ag^ro- gaio* DU P050316585 3* Xm pigments aemt&inim psrtioleo of various aia, the 001 ferae will to & fanetioa of ih total surfas, a pro** 9d is im lie is less Ham Hits oapillary fore them win tot * tet- deney for the into to separate into %w3m of similar partial si#* For exanple, if Hie ink eestaiae a few grains f mmM %her mmM toe a tendency for prssswrs to eeparat the Ink leading the and wu* lee wet with a little oil* la other words, sine fate wd fvtm large partieles are sandy and wiseoas while inks wad from wall pariteles are fluid and soft, pressure and mot lea will tend to - mere the small partial* hw the larger prtieles# As the msp in partial sis decreases this tendency will obviously bMM less. Helm work a a yatesi tends? ts ras<* tfao stropy or sepamts tin partial** la the atoow# analysis it was aawa4 that Hie first mono- wioottlar layer of ell differs fro the remainder* it is gemrally ssswBed that w ill solids, a amwaoieeular layer of the mttim is Mid with a feres tee t a saeoodiwiy walette, and that the reminder is Mid* if at all, toy capillary feres* ISm work f Bartsll on Hie tension of solids and liquids tndts&tes on tbs ether tend that the first layer it Mid only toy mptllary fares* me eapillary feroe however is greater then tftw* in the liquid itself. If a mnevotim is not md for tbo ncmeEsoleenlar film a mine of 31 Instead of d9 atmospheres is obtained in em ease tolls in the other the oorreetion is nsgligitol, Sine the eapillary f ores is oertaialy greater at the partial surface then within Hat liquid sew oorroo- tftoa should too made* and it is probable that a min of say so at* phores is loser to the true wains* 'mile it is evident that sstrfao* foroes play a minor part la the oil retention of etonase yellow* saw protolests ars probably mere Hms * ly related to this tbss id the apilliry pressures within tbs oil* For oasssplo, flosealstis* and dispersion and the replaeoment of ess liquid toy another at a pigment eurfaee do not appear to too ps*tolw related to ths quantity of vstolsl* present* Although load dramto protoatoly <mt toe prepared in a state of sUtodlwialon, toy ordinary methods, with a partiel mlm of loss Ml 2 x 1CH* on* radius, it is of interest to mmiMr the theoretieal ease of a pigment with part isles 1/4 this is or 5 x !~f m rsiiw and a spooifto gravity of one* the pignsni am will toe [1(1.25) AW8 X 1*-*)^ 4^(5 X lo-9')* oar 5 (1*85){*2) x 10T 7*5 x 1@~4 aq. em. Assuming 1 grsmiof the pigment is gram* of mmisto we tew 2*85 x ICT"7 si tbs film radius* This value It thine approximate - thlelratss of a wnawleeular film* it would appear that an into; of this typo would tot more similar to a solution thus to a @11Mai dispare ion, iron tolue* PSA pigments to* may too in this lass. loaording to ^imstoin (SwodMrg Colloid Ohomitsiry, p. ,q0 H wisooslty of a eol is a fsnstlMi of we t u Iu m of the disperse phw and iMepsMeitt of ths partiole sis. Tba wiseesity of a sol (7s) oan too expressed toy the following equation*** 7 * 7y(l + 2*5 p) (7v ** wisoosity of vohiolot P wol* of diepowed pigment). The DUP050316586 riaoooity ef an ink nhml& tfcoraforo is stomt Mat that f tito n vhiola Tfco aturro aquation in Ias9i on t2* asona^tion ilmt tk paartiolos ar sufficiently far apart so that no iatoyforaao 'feetooon paartialoe **tiXts ana tkat tSw individual portSole ar not &jmm"- eisS>ly o&angodi in ais ky aagr adMtfbedi film of vehicle, tho ir$iij#~ tty f an ink is thersfer a as&imr of th extent to t& #* aawt diaaolwe * tlaparsea la itt oil* a wry flixM ink idioaiiii& at Xa@i an apjnrnofe to Im oolut&oa. s* c. mmim' sm*s DUP050316587