Document r2BVKKqNOv9MjB3xgXnn2yaa

^ W NEWARK PLANT p PIGMENT COLOR RESEARCH REPORT $ FEBRUARY 1935 PIGMENT COLOR RESEAROii REPORTS FEBRUARY - 1935 I - IRON BLUES Yield Study B-63-D (FLP) ........................................ ....................... Page 1-2 II - LITHOL REDS (a) Calcium Lithol Toners, RT-300-D & RT-379-D {EJH) (b) Barium litnol RT-365-D (.ADR) ............................................. 3 4 III- LIGHTFAST CHROME GREENS (a) Improvements in Chrome Green Pigments (SCH & HCM) (b) Light Fast Greens - Milori Type CSr7764 (JDM & ADR) Meadows Type G-389-D (CS-7694) 5-6 7-10 XV- CHROME YELLOWS (a) Improvements in Lightfastness of Lt.Chr. Yellows (b) Primrose Yellow (FLP) ................................................. .. (c) Medium Yellow Y-359-D (FLP) ....................... ...................... (d) Excelsior Yellow Y-309-D (FLP) ........................................ 11-15 lb-17 18-19 20 V - CHROME ORANGES (a) Preparation of Rust Inhibitive Pigments (SCH) ... (b) Chrome Orange YO-27-D (FLP) .......... .................................... 21 22 VI - JACKSON LABORATORY STUDIES (AS) (a) Special Organic Pigments............ ......................................... (b) Permanent Red 2B Pigments (Feb. 18) ....-................. (c) Permanent Red 2B .......... ......................................................... (d) Fire Toner RT-208-D ............................................. ............... (e) MNPT For Toluidine Reds ............... ........................ ............. (f) Pigment ftubine G RT-359-D.................................................... 23-25 26-30 31 32 33-34 35 VII - RUBBER COLORS (AJS) ....................................................................................... 36-39 VIII- PIGMENT GREEN B (a) Pigment Green S (AA3) ........................... (b) Pigment Green B, GT-68-P......... 43-44 40-42 IX - PHGSPHGTUNGSTIC ACID PIGMENTS (a) Improvement in Lightfastness of Victoria Pure Blue BO Toner (SCH) (b) PTA Yield Studies (EJH) .......................................................... 45-46 47 X - MPG. STUDIES Grinding of PTA Toner Pulps (JDM) ............................................ 48 XI - MISCi ORGANIC PIGMENTS (a) Azo Sulphite Derivatives (AAB & SWR) ................. (b) Calcium Duol RT-265-D (ADR) .......... ........................... .. (c) Yellow Lake YP-324-D (ADR) ............ ...................... ................ (d) Rubber Colors - Red for Lake C (AAB) ..... (e) Misc. Toners Lithosol Red 2B (Calcium) (AAB) ............... Lithosol Red 2B Toner, RT-7745-D (EJH) ................. Para Chlor Ortho Nitro Aniline (AAB) ............ .. (f) Peacock Blue Lakes, BL-151-D and BL-7427-D (EJH).. (g) Dispersed Clay Colors, GE-363-D and GE-364-D (ADR) 49-51 52 53-54 55-56 57-58 59-62 63 64-65 66-67 DUP050315509 2 HI - MISC. INORGANIC PIGMENTS (a) Chroma Greens - Strong Type CS-7192-7193 (ADR) (b) Strong Milori Green CS-7834 Sloane Blabon Green CS-7838 (ADR) ................. .. ... Hli- RAW MATERIAL TESTING (AFCP) .......... ...................... .................................... XLV - SEMI-WORKS PRODUCTION (H. Rotherham) .......... ....................................... Page 68-69 70 71 72-77 DUP05031 5510 PIGMEHT COLOR RESEARCH REPORT YIELD STUDY B-65-D SUBMITTED BY APPROVED BY: FILE: IROH-BLUE DATE: FEBRUARY-1935 IHTRQDUCTIOH Yield studies on this color were continued to establish the possibility of an increase in yield by slight variations of stand ard f ormuia. SUMMARY & CONCLUSIONS Six batches of B-63-D were made on standard formula with the following variations:- 1) Quenching to 120F after strike. 2) Quick heating (heated to 180F in 15' instead of 1 hour). 3) Use of special copperas (copperas stood for 10 days in con tact with iron to obtain material of higher pH). 4) Adding sulfuric acid after heating to 180F instead of be fore digestion. 5) Increasing copperas by 10$ (extra copperas added to second addition). Batches were carefully supervised and precautions taken to avoid mechanical losses^ washing was done in the usual way, to v.v.s. sul fates. Press cakes were dried in the plant dryer at temperature of 150-165 F for 40-42 hour . Results obtained are tabulated below, on a one mol YPS basis ( .4 mol batches were made). These are lump yields. Moisture 1) SW-6723 Yield Obtained Anhydrous 305 300 2 hrs. at 110F 1.63$ 2) 6728 306 303 0.9 3) 4) 5) ( 6736 6740 6777 309 312 322 305 1.5 295 5.57 314 2.41 ( 6801 324 316 2.41 B-63 Standard formula ( 310 recorded in Jan. Report( 310 + 2 307 299 .99 3.65 The first four variables showed no marked deviation from standard in tinctorial properties. Additional copperas gave redder weaker tints, altho masstones and lacquers were satisfactory. The 10$ increase in copperas was the only variable which result ed in an increase over the highest yield obtained on standard formula. The possibility of some correlation between redness of tint and in creased yield should be investigated. EXE5RIMSBTAL DETAILS notebook 428, pages 64-69. as? ,v--i>r .7 DUP050315511 Tp J3i CtJQ11QO) id Mr0o3H ir003dH *3 3(>O 'Oo0s cSrahl .o X0C5m S 5 a3 T0Of0SVt 0ft tj f> fi 33od 3 xi pn &H t0uJ . >0 rH Scr oc8 rOH >to ro33Hcr TS03m T03 Ts333 S ACVOt|OOQ 3U>D00O 0 PH3a0 13 905m i3d > Ea* ta i0d %> c 3 I 0 PM x0mi 3 2ee3 0UW> m> iHiO3dsI a i*d >0 iraodH3 ATS3 0Uto to A&UJ > Mi--0O3I 30 rOH Haio3d i*P3d0 0 kb 0Uto t0> a i0d iod AA a0 0 o P-c3o3Od a xPa: +S3Z & 0032 rH 0C3O rH 0pH3 lO 03 rH o0>3 rH oCO rH C00Om 0hO p>003H HS303O tT00333; ePft U* 03 -+o> 60 *xSoH:3 3 o3 cy 0tHo P030 id O 3trt O' 3Uffoo0tt r3H rt 0C Oh CO V1<T|03o033(Ht0Hom03.o*xpb300r4t:O>OrxH>0o50ff3hS3Ho00Uo0ram=O>ttl. 5>0O id 00 Xj o -C 5^ at s a <n CO <0 O H as 3 <*> ^ 03 -4> 0t-3 CO 0e- H* 0* < 5- !> < O 20 VO ^2, DUP050315512 PIGMENT COLQH RESEARCH REPORT CALCIUM LITHOL TONERS, RT-300-D AM) RT-379-D 3 SUBMITTED BY* APPROVES BY: PILE: LIgHOLS DATE* FEBRUARY-1935 INTRODUCTION One batch, of RT-379-D and two batches of RT-300-D were made dur ing the month. These batches were supervised by the Development Sec tion. at the request of the Plant in an effort to secure satisfactory shading material for use in mixing off sub-standard stock. SUMMARY & CONCLUSIONS The first RT-300-D batch was made as previous plant batches on a modified RT-379-D formula except that the para soap and ammonium chloride were each cut 25$ to give light and blue results. As this change gave a product with a slightly muddy masstone, the next batch was made without introducing this variable, also increasing the dev elopment volume 25$. This batch was dark, blue and weak by rubout, Neither of these batches were light in masstone ad desired. The RT-379-D batch was a check to the previous supervised plant batch (41546) except that the Mono Acid F was omitted. It was noted that the diazo showed a slight brown tinge and upon investigation it was found that the plant had been neglecting to thoroughly clean out the diazo vat with hot water after every batch, as had been the custom heretofor. This omission will be rectified in the next batch of Lithol toner manufactured as even a trace of decomposed diazo in Lithols or Duols tends to give a muddy masstone. The results on this batch were unsatisfactory, the color being dk, vs brown-blue- vs dirty and blue versus the standard RT-379-D. A satisfactory mix, however, of 2500 lbs. has been prepared from recent manufacture of RT-379-D and released to standard stock. For tabulations on the RT-379-D batch see Table I, and for the tabulation on the RT-300-D batches see Table II. EXPERIMENTAL DETAILS N.B. ^3 page 52 Batch TOB _________Lot Amt TABLE I RT-379-D NaoH TOBW in Rubout Results Lot Amt BN Mass. Draw. Str. Tint Yield Bst. Lump 42022 130 75$ 23 25$ 41# dk,vs blue brown vs dirty, 205 194# bl TABLE II RT-300-D TOB Devel- Bateh Lot patent ________ Volume 42004 103 1200" 42046 133 1500 NaOH NH4C1 in Para JBN_ Soap___ 35F 5-172# Rubout Results Mass. Draw. Str. Tint Yield Bst. Lump 34# dk,muddy blue - - blue 205# 184# 35# 7-1/2 45# dark s .blue wk s.bl. 205# 206# DUP050315513 PIGMENT COLOR RESEARCH REPORT BARIUM LITHOL RT-365-D SUBMITTED BY: APPROVED BY: ^ 0 PILEt LISHSiS* BATE: PEBRUARY-1935 INTRODUCTION Three batches of this d ark barium lithol were made in the plant. Standard alkaline coupling formula was used. SUMMARY & CONCLUSIONS Only 75$ of the standard amount of Mono Acid was employed as this appeared sufficient on a former series. One batch was slightly yellow in tint but the others were bluer than standard and can pro bably be shaded. Use of the full amount of Mono Acid may be desir able . EXPERIMENTAL.: DETAILS N.B. #335. p. 88 All made as in Lot 37923 {April 1934)- 0.75 mol charge 41725 - dark; vs blue; OK; s.blue 41745 - dark; vs yel; str; s.yellow 41769 - dark; s.str; str; v.s.blue s.brown DUP050315514 PIGMENT COLOR RESEARCH REPORT 3JT-3 7 SUBMITES) BY APPROVED BY: IMffiOVBMBNTS IN CHROME GREER S. PIGMENTS t </ PILE: CHROMB1l,~gfggBNS~ DATE: ESBRUARY-1935 INTRODUCTION The study of the effect of various factors on the light fast ness of chrome greens has been continued from the past month. A study of the flooding of chrome greens has been resumed. SUMMARY & CONCLUSION During the work on the chrome greens of improved lightfast ness it was noted that greens in a lacquer vehicle were worse in lightfastness than when ground in oil. Previous work indicated that the difference in vehicle was not the chief cause. During the past month it was found that the lightfastness could be improved by grinding with glass balls rather than steel balls or by decreasing the grinding cycle. No further work is planned on this problem. A study of the effect of the blue on the lightfastness of a ohrome green was continued from the past month. Different batches of B-103-D and B-109-D were tested and found to vary in their effect on the lightfastness of the green. The problem of obtaining a better blue for greens appears impractical, and no further work is planned. A study of the flooding of chrome greens has been resumed. It has been found that a recent laboratory process gives a chrome green showing less flooding than our Milori Greens. Semi-works material shows a similar effect. The test used was the regular puddle test. These greens are yellow, clean and weak in tint versus our Milori Greens and about equal in lightfastness. It seems pro bable that the improvement observed is caused by a smaller particle size of the yellow pigment. A possible improvement in flooding might be obtained by increas ing the particle size of the blue component of the green. Iron blue treated with 10$ of #1 Regular varnish showed a considerable improve ment in flooding over a control dry mix. but was only equal or slight ly better than a Milori Green control. :7here a dry mix is usually used, as in the case of the Pullman greens, this device might produce a decided decrease in flooding. Treatment of a green slurry with 5$ to 10$ of linseed oil gives a practically non-flooding green with the puddle test, but the ink has a very heavy body. Several of our standards and a number of competitive samples were analyzed for phosphorous or tin or both. The results are tabu- lated below: C-32930 Old Sample Imperial Green No Tin C-36S77 Recent Sample " 1.27$ Sn C-36916 w n .38$ Sn C-37270 C-37271 *tt Unitedtt Green .40$ Sn .39$ Sn G-37407 * Kentucky Green C-37730 w Sherwin Williams Green G-208-D Present Standard No tin 1.58$ Sn No tin CS-7694 Improved more lightfast type Green .23$ Sn "~r.A DUP050315515 2 C-36877 Recent Sample Imperial Green C-36916 " * CS-7694 Improved more lightfast green .54% P2O5 .40% trace * BXPRRIMSHTAL DETAILS N.B. #439 459-61B and 6135. Study the effect of grinding with glass or steel "balls in the lacquer process. It was found that using glass "balls at 15 hours of grinding gave "better results in lightfastness than using steel balls for 5 hours of grinding. It was alsco observed that lightfastness grew very slightly worse the longer the pigment was ground with steel balls. This would indicate that by decreasing the grinding cycle better lightfastness would be obtained. 439-61C. Study several batches of B-103-D and B-109-D blue used in dry mixes with the greening yellow of the new improved lightfast green for lightfastness. It was found that different batches of the above blue varied in their effect on the lightfastness of the green. 439-71. Preparation of samples of B-66-D containing 3%, 6%, and 10$ of linseed oil- to be used in the study of the flooding of chrome greens. It is quite noticeable that linseed oil has some effect on the flooding properties without producing an appreciable effect tinctorially. 459-73. Study the effect of #1 Regular Varnish on the 439-37A procedure nade with and without sodium sulphate in the strike. Those treated with #1 Regular varnish were better than the con trols . Ho marked difference was observed between the controls made with and without sulphate in the strike. 439-74. Study of treatment of G-209-I} with linseed oil to re duce flooding. 2) treated with the highest amount of linseed oil was practically non-flooding. The degree of non-flooding was in direct trend with the amount of linseed oil used. 439-75. Study the effect of Gelatin, agar agar, glue and Daktose treated G-210-D as coating agents. Gelatin and Glue had very slightly better coating agent effects than Agar Agar, and Daktose. DUP05031 5516 PIGMENT COLOR RESEARCH REPORT LIGHT-PAST GREENS MILORI TYPE CS-7764: MBADCWS TYPE G-389-D (CS-7694) 7 QLuJ*Ql SUBMITTED BY APPROVED BY: INTRODUCTION A continuation of the study of the previous adnth of the Milori type of green, GS-7764, was carried on in the Semi-works, a total of seven hatches being made during the month. An intensive process study of the Meadows type green .G-389-D (CS-7694) was ns.de, including variables both in mechanical operation and in treating agents. Fifteen batches of this color were struck. In the plant, three batches of G-389-D and one batch of G-390-D, the next darker shade, were made. Efforts to obtain greater bright ness were continued. SUMMARY & CONCLUSIONS I. CS-7764 The 1% increase in acidity of the reduced bichromate formula tried last month was checked using 3-66-D liquor. Greater brightness was obtained on this run. A further increase of the same amount of nitric acid was made to restore the original acid balance present in the initial formula: namely, SW-6673. A bright, clear color was obtained, with somewhat reduced lightfastness. The effect of doubling the amount of sodium sulfide was negli gible, except for giving a slightly darker product, with light sta bility slightly superior to control. The most promising variable was the addition of tin crystals di rectly after strike as well as after washing. In previous work, the amount of bichromate was reduced in order to give a bluer brighter product, the light stability, however, and as was to be expected, the strength, being decreased. The addition of tin crystals after strike had no detrimental effect on the blueness and brightness, and increased the light stability to a marked extent. The bichromate was then in creased to its original amount as in S7/-6673, and with the tin crystals added after strike, the strength desired was regained without affecting the blueness and brightness. An increase of 10 degrees in strike temperature appeared to have no beneficial effect, actually giving a product slightly yellow and dirty against control, with good lightfastness. Work on this color is being suspended until the products ob tained this month are evaluated. DUP050315517 2 S' II. G-389-D (CS-7694) The control for this series was a 0.02 mol charge based on the formula for CS-7694, now coded as G-389-D. The control was slightly on the blue strong side of the G-389-D standard. A decrease in speed of agitation to a point where there was little turbulence, had very little effect on the color, the lightfast ness being very slightly decreased. An increase in the speed of agita tion on the other hand gave a product blue and bright in masstone. One batch of the color was struck, washed, shaded, and pressed the same day. ITo beneficial results were noted. A decrease in the number of wash waters from three to one resultid in an inferior product, that was slightly light and dull in masstone and yellowish in undertone and tint. Lightfastness was very slightly superior to control. A reduction in strike volume of 50$ had little effect on the color. A dark bluish masstone was obtained when the strike tempera ture was reduced from 1103? to 75P. A two hour strike instead of the normal half hour one, resulted in a color with olive masstone and dirty undertone and tint. On the other hand a five minute strike increased the brightness, and the light stability was a little better than both control and standard. A five minute strike with reduced speed of agitation gave a product comparable to the two hour strike. The amount of sodium sulfide was doubled in one batch, but the color was inferior to the control, being rusty in masstone and dirty in tint with a slight decrease in light stability. Doubling the tin crystals, however, had an opposite effect, giving a bright product with a slightly better light stability. A number of variables in treating agents after washing were tried. Omission of cupric hydroxide appeared to have no adverse effects; a lower gloss was observed in the dry masstone in varnish. Use of alum and tin crystals alone resulted in a bright clean product with light stability somewhat superior to control. This study is being continued. PLAHT Difficulty is still being experienced in obtaining brightness equal to the standards recently set up. A check run of G-389-D with a sprinkler for addition of the bi chromate gave an olive product. Reduction in amount of bichromate from 78 to 73$ of lead coverage gave only a slight improvement, but the same formula with a 50$ great er amount of tin crystals added after strike showed a distinct increase in blueness of masstone. However, there was some loss in brightness during drying. DU PO 50315518 3. One batch of the darker shade, G-390-D, was made on the last variation described, plus a 5# reduction In soda ash to bring the acid balance in line* Although shaded too dark, this batch when lightened in a board mix was satisfactory in masstone and light stability, but was slightly dirty in tint* Work is being continued and it is hoped that results of the Semi Works study may be of help in controlling this eoler* EXPERIHBjnfAL 3BTAIIS SEMI-WORKS H.B. 436, pages 133 and 160 S Variation CS-7764 Std. Hass* Und. Light StabiStr. Tint litv 6785 Check SW-6736 but use G-317-D s.dk Be e.bl. s.str s.bl B-66-D liquor instead lot 47001 hrt, of B-63-D 679S Check SW-6678 using 21# * H blue str blue blue 6796 Check SW-6785 but increase " n * M s.bl nitric acid from 15#-16#. Use 19# blue. 6803 Gheek SW-6796 but use " s.dk,s.bl. * s.str blue double amt. of sod.sulfide 6808 Check SW6796 but add 2# tin - Be brt. vs blue It M bl.& crystals to yellow after & brt. clear bichromate 6825 Check SW-6673 but add tin bl & brt N str. blue crystals after strike as in SW-6808. Use 22# blue. n 6830 Check SW-6825 but strike at * s.dk, bl ft a 80e instead of 70F. G-389-1) & brt. -X 6732 Control - 0.02 x CS-7694 G-389D bluish clean t v s str s.bl va (Agitation 29 BEK) lot 13794 Seal worse 6744 Check SW-6732 but reduce * bl,s.brt s .bl s.str * speed of agitation to gel. 16+2 BEK 6749 Cheek"*SW-6732 but reduce s.dk s .str OK cl. m strike volume by 50# & bl. & el 6757 Gheek SW-6732 but in- m *bi. 8 ebl s.str bl Be si. crease speed of agita & cl el. worse tion to 40 BEK 6761 Check SW-6732 vs dk clean ft el. equal & bl 6765 Check SW-6761 but use s.dk. bl s.yel. vs str s.cl v.s. double amt. of sodit&n s.dull &cl worse sulfide. 6773 Check SW-6761 but use dou- " s.dk & s .str n cl. equal ble amt. of tin cjypstals blue s .cl s.bl after strike blue 6780 Check SW-6761 but strike in " vs It, s.yel. OK cl. equal 5* instead of 301 (2 hole blue distributor) s .brt ,... DUP050315519 4 SW Variation G-389-D (cont.) , Std. Mass. TJnd. Str. Tint Light Stahilitv 6783 6793 6795 6802 68X9 6826 6828 Check SW-678 hut G -389-D reduce spaed of lot agitation to 13794 16 + 2 RPM Check SW-6761 hut * wash,shade and press color on the same day. Cheek SW-6761 hut n strike in 2 hrs. instead of l/2 hr. Check SW-6761 hut wash it one water instead of three Check SW-6761 hut strike at 75 P instead of t 110P Check SW-6761 hut add only alum, soda ash f and tin crystals after washing. Check SW-6761 hut add only alum and tin crystals after wash ing VT3 hi s .hi o k : s.bl equal s .dk. s.hl. dull s.yel. OK drty vs yel vs dirty worse s.dk & yel. OK yel. equal olive s.drty s .drty ws It vs yel vs & dull str dark & sc 1 blue M s.yel. equal s.hl s.worse &cl s.dark & hi. s .str s .str vs hi vs worse vs dark vs hi OK & hi. & cl. vs hi vs & cl better PLAHT H.B. 437, p. 55 Lot 41719 41857 it 41973 n 42143 G-389-3). Check G--389-1) olive yel.& lot 41611 lot rusty 13794 G-389-D. Check 41611 except N vs olive vs vs wk si. reduce hichro & dirty dirty drty mate from 232 to 218# G-389-D. Check dark blue 41857 hut in R bluish vs str crease tin crys dirty tals 50$ G-390-D yellow as G-39CJD dark blue in 41973 except lot blue reduce soda ash 3928 from 103 to 98# si. worse v.s. worse equal DUP050315520 PIGMENT COLOR RESEARCH REPORT H/EPH0VBM5HTS IN LIGHTEASINESS OF LIGHT CHROME YELLOWS // SUBMITS) BY: S.C. APPROVED BY: BILE: CIS^ffi^YBKeO^S C f DATE: EEBRUARY-1935 INTRODUCTION T3is study of the primrose yellow of improved lightfastness was continued from the past month. A further slight improvement in tinc torial properties and lightfastness has been obtained. The study of Y-202-D has been discontinued pending the evaluation of three samples submitted to the General Division laboratory. A brief study of the effect of various rubber accelerators and of various tin compounds on chrome yellows is practically complete. No improvement was observed except in the case of the rubber accel erators, Captax and Altax. Altax and in a few cases Captax improved the tinctorial appearance and lightfastness of several chrome yellows when added in a 1% dry mix. A new process has been obtained for the preparation of chrome yellowB in the range from a light medium to Y-309--D. This process is receiving intensive study. SUiaiARY & CONCLUSION During the past month a laboratory study was made, using 4 mol strikes, of the effect of process variables on the tinctorial proper ties and lightfastness of the improved primrose yellow. It was found that the pH after the soda ash should be about 5.2 - 5.4 for maximum lightfastness, and that from 35 to 45 grams of alum per mol should be used to obtain consistently good results. A 15 to 35 minute^ stirring period after the alum seems desirable. The temperature at the time of the alum treatment is about 50E. Increasing the temperature re sults in a slight decrease in lightfastness. Citric acid has a slight stabilizing action, but decreases the lightfastness. Excessive wash ing may decres.se the lightfastness slightly. Omitting the sodium sulphate added before the alum had little effect. Work on this problem has been discontinued fxor the present. During the previous month three processes were developed for the preparation of pigments approximately equal in shade and strength to Y-202-B. During the past month this work was completed and samples rep resentative of the three processes submitted to the General Division laboratory for evaluation. Captax, 2 ITercapto Benzothiazole, and 2 Mercapto Naphthylene were precipitated with both stannous chloride and stannic chloride, and the resulting products mixed with Y-305-D. No improvement was noted. A dry mix of tin oleate and tin tetraphenyl with Y-305-D showed no improvement in lightfastness or tinctorial properties. Dry mixes of Y-202-D with Triphenyl Guanidine. Thionex. A.ltax. Captax. Tuads, and Accelerator 552 were made. An improvement in lightfastness using Captax and Altax was noted. A number of other miscellaneous mixes were made and in general only Captax and Altax improved the DU P050315521 /*2 lightfastness and in all cases Altax was equal or superior to Captax as a treating agent. In general- Captax gives a product with a dirty masstone, particularly when the mount is wet,while *ltax gives a clean masstone versus control or is without effect. A new process has "been developed which is especially suitable for the preparation of light, medium, and excelsior shades. The pro cess involves the addition of sodium chromate plus sodium sulphate to lead nitrate. Soda ash is then added)and after drawing three waters alum and bicarbonate are added. Products superior in lightfastness to Y-309-D have been prepared by this process. EXP5RIMBMTAI DETAILS BT.B. 453-452 415-50A primrose of improved lightfastness 453-18. Study the importance of the pH after the finalt reatment. and its effect in lightstability. It was observed in this experiment that a final pH of 5.7 showed a decided improvement in light stability. A final pH below or above 5.7-5.8 appears to be detrimental to the light stability and clean ness Of the pigment. 455-20. Study the effect of citric acid on the light stability and the effect of omitting the sodium sulphate in the afterwashing treatment. Citric acid appears to have a slight stabilizing effect, but decreases the lightfastness. Omitting the sodium sulphate in the final treatment appears to have very little effect on the product obtained. 453-22-25. Study effect of an additional washing before and after the final treatment. Washing an extra water does not seem to have any effect on the product obtained. 453-24-25. Study laborator}' drying conditions on Semi Woik s batches of improved Primrose Yellow (415-50A) to determine where S.W. color may go red. The unwashed sample dried in one thickness of wrapping paper was only a trace dirty, versus A, the washed pigment. D, the unwashed sample, dried in two thicknesses of wrapring paper v;as red and pro duced a pigment very very slightly worse in lightfastness. D was very red versus C. which, with the exception of being unwashed, received the same treatment. In this experiment, it appears that the time of drying is very important. 453-26. Study effect of increasing the amount of alum in the final treatment. In this experiment, an increase of alum resulted in an improve ment in lightfastness and a very slightly cleaner product. This in crease in alum did not appear to affect the strength. 453-27. Study the effect of varying the amount of sodium chlor ide in the bichromate solution. It appears from this experiment that it is possible to use an op timum amount of salt in order to get a clean product. The omission of salt gave a dirty red product with poor lightfastness. ' >-'; trr DUP050315522 3 453-28. Study drying conditions by varying size of cake, using 26C (high salt) as the basic procedure. It appears that the thicker cakes grew more red upon drying than the thinner cakes. Hone of the members of this series were equal to 26C in lightfastness. 453-29. Increasing temperature of the final treatment to 7C5\ stir l^T minutes between the alum and bicarbonate in final treatment; study diluting to double the original volume. Increasing the temperature of the final treatment resulted in a slight decrease in lightfastness. Stirring 15 minutes between the alum and bicarbonate treatment gave a clean product in conjunction with a very very slight improvement in lightfastness. 453-30. Study washing after the final treatment, also stirring for thirty minutes before filtering. Washing after the final treatment has little or no effect on the products obtained. Stirring before filtering resulted in a very very slight improvement in lightfastness. 453-31. Study th4 alkalinity after the strike, and time of strike. A pH of 5.3 after the soda ash appears to be necessary for ob taining the maximum lightfastness. The time of strike does not seem to be of any specific importance. 453-52. Determine the optimum amount of alum necessary to ob tain the greatest improvement. It seems that 35 to 45 gms. of alum per mol tend to give regu larly very satisfactory results. Improved Y-202-P 453-16. Using 453-11A '{alkaline type procedure) as the control, study the effect of a variation of pH after the final treatment. In this series C, made by adjusting to a pH of 5.7, gave a very promising product, which mounts, contrary to previous conditions, do not grow dirty upon drying. 453-19-21. Study on 453-13A (neutral type procedure) variations of pH after~final treatment, and tartaric acid, also use sodium bi carbonate for soda ash in the strike. In this neutral procedure, a PH of 5.7 appears to give the best results. It appears that tartaric is very essential in order to keep the pigment from going too red while drying in the oven. Bicarbonate substituted for soda ash gave a somewhat dirtier product. Rubber Accelerator Study 453-17. Study various rubber accelerators. STo improvement was observed except in the case of Captax and Altax. Altax and Captax in some of the members of this series showed a slight improvement in tinctorial appearance and lightfastness. 453-37. Study effect of 2 mercapto benzothiazole and 2 mercapto naphthylene when precipitated with stannous chloride and stannic chloride. DUP050315523 4 Ho improvement was noted. A dry mix of tin oleate and tin tetraphenyl with Y-305-D showed no improvement in lightfastness or tinetorially. Light, medium and excelsior shades 452-1. Try to obtain Y-1S0-D shade, 10(H lead chromate, with improved lightfastness and improved strength, using 389-109A as the basic procedure. (This consists of striking salt and chromate into lead nitrate at 70 F. then follow with soda ash, ending with a lead excess). In this experiment increasing the salt from 10 to 20 resulted in a slightly cleaner product. Omitting the sodium sulphate in the afterwashing treatment re sulted in a very dirty product poor in lightfastness. However, amitting the sulphate, but increasing the alum not only gave a cleaner pro duct, but also improved the lightfastness. 452-3. Study on the ID procedure the effect of Altax, striking at 130^7 and omitting the use of salt. Striking at 130and using Altax gave dirty products. In this experiment, C made without salt, was the lightest and cleanest of the series. 452-4. Study the importance of the final pH on the 3G proce dure . It appears that the more alkaline the pigment is before filter ing, the greater is the decrease in lightfastness. The use of sodium chromate in the final treatment resulted in a red product. 452-5. Study possibilities of lightening the tinctorial pro perties of 3C, by using sodium sulphate for part of the precipitants. Using sodium sulphate for part of the sodium chromate resulted in a lighter masstone without affecting the light stability. Substituting bichromate for part of the sodium chromate, and using acid in the base resulted in a redder product. Heating to 105P and 140P before filtering gave clean products, better in lightfastness than the control. 452-7. To lighten the masstone of 5C by increasing the amount of sodium sulphate in the strike, keeping the same precipitant bal ance , An increase in sulphate resulted in an increase in lightness of masstone and a decrease in strength, with no appreciable effect on the light stability. These products possessed considerably more strength than Y-190-D. 452-8. Increase further the sulphate content of 452-7D; also study 453-12C procedure. A large increase in sulphate content resulted in a very light product poor in lightfastness, the mounts of which darkened upon dry ing. Striking the 7D type at 110`T instead of 70"F resulted in a slightly dirtier product. JTo improvement was obtained by cutting the precipitant balance of the 453-12C formula. My 7' .viz__ DUP050315524 5 452-9. Study the 8C formula, using less sulphates. Decreasing the sulphates in the 453-12C formula gave a redder product. 452-10. Study TO, using magnesium sulphate, salt, and less alum; also check 9D omitting the alum treatment. Using salt in 7D tends to produce a slightly cleaner product. Decreasing the alum resulted in a dirty green product poor in lightfastness. Magnesium sulphate gave a slightly dirty product with a de crease in lightfastness. Omitting the alum treatment in the 9D and using chromate in stead gave a changeable product. 452-11. Try to improve the strength of 452-10A by washing after the'"alum treatment, also treat with sulfuric acid. Study treating at 130CF. hashing after the alum treatment gave a dirty product. Using sulphuric acid for alum reddens the pigment. Heating to ISO0? before the treatment gave a slightly dirty product versus 10A. 452-12-13. Continue the study of trying to improve the strength of 10A. Heating to 130rF after the alum treatment gave a slight improve ment in lightfastness. Increasing the precipitant balance by increasing the soda ash resulted in a dirty green product with very poor lightfastness. C, made with 70 parts of sodium chromate and 20 parts of salt was red tinctori&lly and better in lightfastness than Y-309-D. The use of alum and sodium sulphate after the soda ash in the strike gave no marked improvement. 13D, made like 10A, but struck at 110 F was v.v.s. red, 452-14-15. Increase the amount of salt in the 10A procedure; use bicarbonate for carbonate in the strike, add part of the soda ash to the lead nitrate before striking; in 15 series heat to 180CF after the treatment; omit the bicarbonate in the treatment; increase the amount of alum-bicarbonate in the af'terwashing treatment; also try using ammonium sulphate fox the alum and bicarbonate treatment. Hone of the above variations showed any marked improvement in lightfastness. Bicarbonate substituted for soda ash gave a slightly dirty pro duct with a slight decrease in lightfastness. Increasing the salt and adding same of the soda ash to the lead nitrate seemed to increase the strength, with no appreciable effect on the lightfastness. Keating to 180 F after the final treatment gave a changeable product. Omitting the bicarbonate, and increasing the alum resulted in a slightly redder product. Ammonium sulohate did not seem to be very promising. DUP050315525 PIGMENT COLOR RESEARCH REPORT PRIMROSE YELLOW SUBMITTED BY: f*l APPROVED BY: pil e: DATS: PEBRUARY-1935 INTRODUCTION Development work was continued in the semi-works on a Primrose Yellow of improved lightfastness^ and color. SUMMARY & CONCLUSIONS Following a series of small hatches made in a 50 gallon cask, work was resumed in 0.125 mol batch sizes. Careful eontrol of acidity during washing, and conditions of drying, gave a number of interesting products, with little or no change in formula from that used in pre vious work. In all cases, the yellow when dried slowly in extremely humid atmosphere "'flopped* to a very red shade. However, drying in ordinary press cake form at 140F. 2,0% relative humidity, gave satisfactory products which were then quite insensitive to baking at 200-220cF. Addition of small amounts of citric acid or stannous chloride did not have any appreciable restraining action on the change during drying. Omitting sodium sulphate after the second water, and increasing the amount of alum added at this point showed little or no effect on tinctorial properties but showed a distinct improvement in lightfast ness. The use of lead nitrate liquor instead of crystals gave a somewhatfradder, dirtier masstone; however, this difference was not a very great one. EXPERIMENTAL DETAILS Notebook 448. p. 43-49 A tabulation follows: DUP050315526 to p o jQ 3 oc: p E a bO a bO E H C H <3 s a 34 icnn U a -o p (-( 0$ cd 0 P i 8*t * & 0 n -4 -1 -3 (t i"4 S-. rH -3 s* a au 0>0 a TJ p U t* P o oEs a i o 73 E a 9s a o * cr i Ea a a a > > a SJtho3 EH c r> P o X3 d & Ea Pc a a > 2d O o a aa > bO a #S bO E o u > > r. id a > > <A * /. T3 -P X3 a a > > Sjj P o 0E O Id id o o *> > $3 O a r> TO 0 tx 4-r Id o * Ea *a a > N w *r c C X5 T3 bO o s J* c aa X3 a t-, bO t* tn r> rH a E x> rS a h g s a0> P a > U > c** o rH > >> JO HH a rH n H H 'X) 1 n rH CM D00 CM co CM CO co ro 4fc- Xi o CO CM X <43 to to to >H to -3 a u a * TJ a ai % bd oi *> T3 a s TJ T? aa Jk MTi T3 U * a -3 uH o * S- l a > * XJ a a (-4 a a> > r r> u -p P aa V a > a xJ r> *#> Id E bd O O fk X3 TO > bTdJ >* 8 E t u H bO X3 b> 8> a a a > > > u P rH a e 0 st <H a XJ 0 H ss P -H u mm CM CM * rH to O aaa w a P u P pa a M H p a U a t4 Pa 0 a rH Ah * 9s a E a0 0 (4 P00 Ah Ah *r d a (4 9 s t tO PH ffM s O Sm a CM G <n 0 to to f O G CM rH in CM 0 0 t 0 0 CM m <0 to tO m m fc- to to to m in in m in in in in in CM in CM o H 3> Cf 00 O O 3 O in m in XJ rl o a Jh p Cm O a o X4 TJ aS +*'s O > Ah pH + PP a0, 1h S0 &P ai in a c- gd lO p if T3 ^ U * 3O in HCO a1^ co H rH lO JO & +9 4^ n t<nS o -ow TJP5S <Mp- soOs TS cd si ai O0 H0 * m0 O * 0ss 'Qcd rH 00 r& O* & t? 4 0 P rH X X rH <Ti rH X CM P CO to * H X in n 0 a X X X X X X !<0 a to O 0 0 0 0 0 0 DUP050315527 FIGMENT COLOR RESEARCH REPORT MEDIUM YELLOW Y-359D a*--# SUBMITTED BY APPROVED BY: 1/ PILE: C3RO-YEOW DATS: FEBRUARY-1935 INTRODUCTION Work in the semi-works and plant was continued in order to im prove this color over the present standard. SUMMARY & CONCLUSIONS /v- Semi-works studies were made on standard formula with varia :4'-\ tions in volumes, time of strike, increase in sodium chromate- and "better distribution of the precipitates (lead nitrate solution run in through sprinkler). A batch previously made with increased time of strike resulted in material of lighter cleaner shade, better lightfastness and satis factory lithographic resistance. Two batches were made as checks; both, however, finished without excess chromate, probably because of incorrect analysis. The material obtained was slightly better than standard but did not equal the quality of the previous batch (SV/-6747, recorded in January Report). Increase of sodium chromate by 10# resulted in a si ightly light and clean masstone and v.s. better lightfastness compared with con trol. The control batch showed better ink properties than the ones previously made. This may be due to a larger excess of sodium chro mate, as the third watershowed a faint excess of chromate. Adding -\.r - . lead nitrate in a thin spray resulted in material almost equal to the control. This should be repeated with a sprinkler with finer spray. Seven batches were made in the plant on a modified formula, which 'tjf differed from the standard formula in omitting salt, increase in sodium-chromate by 5#, and longer precipitating time. All these batches were superior to standard in masstone, lightfastness and lithographic resistance. Tabulation of Semi-"Works and Plant batches follows. EXPERIMENTAL DETAILS Notebook 448. cages 58. 59 and 70-71 'ir *; Jr U DUP05031 5528 (>/ g io* -p s JQ u +3 <pD S<9D3 bO *C5 U m > xu$ fed o > s u bO Js$ 3 S3 -P ttS ^ bHO rOH C H ,, cJ > rOH ir O > ccoo i<no >ctf>j m 1c* > o CFv cr> 60* 63' 7.4 vs lig h t clean 7.5 vs lig h t c le a n v s green OK c le a n v s c le a n OK a .g re e n vs b e tte r OK v b c le a n v beTTs-l OKi 92*' ^.%$SaBm ' '4^ ;>"; *** " 93"' * 4214X * 42189 * cmCJov a* a* DUP050315529 &-* <u> PIGMENT COLOR RESEARCH REPORT KBttSIOH YTOOT Y-309-D ^ /! 1 SUBMITTED BY:kPILE: h t t r o t /t r APEROVED BY: DATE: [FEBRUARY-1935 INTRODUCTION An additional factory Batch of Y-309-D was made in this study, previously reported in December 1934. SUMMARY & CONCLUSIONS Batch 43020 was made like the previous plant batch (41762) ex cept for a slight reduction in soda ash. The pH of the finished pro duct was lower, and was not adjusted. Since the previous batch had shown that the yellow could be left in the press oversight before loading into the dryer without harm, the batch made this month was left in the press, after being struck, washed, and treated during the same day. The resulting pigment was not satisfactory, being green and poor in light stability. "i The relationships between pH of wash waters, temperature of waters, rapidity of washing, and "turning" of the yellow must appar ently be worked out in the factory in order to obtain the desired pigment properties. BXE8RIMBNTAL DETAILS See Notebook 448. p, 22. .tt-' "IV .3f DUP050315530 PIGMENT COLOR RESEARCH REPORT PREPARATION OP RUST INHIBITIVE PIGMENTS SUBMITTED BY: APPROVED BY: INTRODUCTION PILE: CHROME -eRfeN9B DATE*. FEBRUARY-1935 __e_ In connection with a project on Corrosion Resisting Pigments at the Experimental Station it has Been proposed that Newark supplysuch pigments as may he necessary in their work. A start has been made on the preparation of these pigments. SUMMARY & CONCLUSION Previous work at the Experimental Station has indicated basic lead chromate is low in acid accepting'properties and develops water impermeability less rapidly than red lead. It has been pointed out that a rapid development of high water impermeability may be related to poor film adhesion and poor durability, to low can can stability, and to the acid accepting properties of the pigment. In view of the probable use of talc to obtain high water impermeability it has been decided to limit the preliminary work to a. study of various substances which could be added to basic lead chromate to improve its acid accept ing characteristics. In addition to the available acid acceptors, zinc oxide and red lead, the study will include laboratory samples of 2 PbO.PbCrOA, Pb0.PbS04, PbO.Pb(NOs)2, PbO.PbCl2, 5 FbO.FbCl2 and an acid alumina hydrate. All of these samples were prepared by pre viously described processes except the dibasic lead chromate. This was prepared by the simultaneous addition of lead liquor and sodium chromate to a solution of sodium hydroxide. The can stability of those substances showing acid accepting properties is to be deter mined . EXPERIMENTAL DETAILS N.B. #421 421-18. Preparation of a corrosion resistant basic lead chromate.- 421-19. Preparation of corrosion resistant pigments for Exper imental Station. The products obtained from these experiments have been submitted to the Experimental Station for testing. DUP050315531 PIGMSHT COLOR RESEARCH REPORT CHROME! ORANGE Y0-27-P 2^ s u b mit t e d APPROVED BY* ^ CJLuLf^ p il e ; c h e s s --eftOTSss - BATE; FEBRUARY-1935 IM-RODUCTIOH Assistance was requested by the Production department in con trolling Y0-27-D. Eecent manufacture has been light and strong, and when variables were used, a bricky masstone resulted. A study was begun in the factory to attempt to correct these conditions. SUMMARY & CONCLUSIOHS Pour batches were made on a formula which resembled both the Y0-27-D and the Y0-263-D formulas; a comparison is shown below; YO-27-D Y0-263-D lot 42083 mols chromate (per mol lead) -- ------- 764--------- .50 .61 mols acid 1.278 0.969 1.155 YD-27rB is struck direct (chromate into lead) and developed at a boil, some of the lead being added during the boiling period. Y0-263-B is reverse precipitated and developed at 200F. The four batches made during the month were struck reverse and developed at a boil. Ho shading lead was used. Decreasing amounts of aeid (by chromate ; bichromate adjustment) gave darker masstones, but all the batches made were stronger than Y0-27-D, resembling Y0-263-B. In two batches, the color was not flooded after strike, but was allowed to settle without quenching for four hours. Succeeding waters were heated to lOO^P. This procedure apparently gave a somewhat weak er product. Work will be continued in the plant, studying direct precipita tion and strike temperatures. EXPBRIMEHTAL DETAILS notebook 448, p. 150 Batch Ho. 42083 42110 42184 42221 Hols Formula aeid T.TS'S (See Summary)' 1.033 Like above, except reduce acidity. 1.125 Change in acidity, and color not quenched after boiling; wash waters heated to 100F. 1.164 like 42184, but acidity changed Rubouts VS Y0-27-D & Y0-263-D vs "YO'-S1? v s It,clean; strong; yellow vs Y0263 vs red; OK; trace red vs YO-27 red; strong; red vs YO-263 red; OK; red vs Y0-27 red; strong; red vs YO-263 red; weak; red vs YO-27-D s.red; s.strong; ws red vs YO-263 s.red; weak; red in above, total chromate held constant at .61 mols 42221 vs 42083 s.red; weak; red * s.weak; yellow DUP050315532 f? l PIGMBHT COLOR RESEARCH REPCRT SPECIAL ORGASTIC PIGMBSTS ^3 SUBMITTED BY* APPRO?- BT* p il e * s ees o *--y o be r s - *"v DATE* EEBRUARY-1935 ** IHTRODUCTIOS Investigations were carried out this mouth on lakes of Quino line Yellow Pj vattlug of Ponsol Blue GD in the presence of lanuginie acid and Inorganic substrata* and the preparation of new dyes and color lakes from 1*5 disulfo 2 nsphthylamine combined with beta naph tha1 and beta oxynaphtho ic acid? from 2 chi or 5 amine toluene 4 sulfo nic acid and $ Chlor 2 amino toluene 4 sulfonic acid combined with R Salt* and ortho nitraniline para sulfonic acid* ortho nltranlline para sulfonanilida and 2 nitro 4 benzoylsunino aniline combined with beta naphthol* The investigation of the barium toner of 2 chlor 4 amino tolu ene R Salt, Continued with the object of eliminating the oil bleed, has been Successfully completed* SUMMARY & COHCLUSIOBS Ortho chlor oara toluldlne R Salta further improvements in tinctorial properties and texture of the dry barium toner of the dye combination orthoohlor 4 amino toluene and R Salt have been made by modification of the laklng procedure* The resulting product Is non-bleeding in linseed oil as judged by paper spot and shite overstripe tests* Calcium and Strontium toners and lakes prepared by the improved procedure possess no especial merit, which confirms previous results and conclusions. Investigations to date have been strictly of an orientation nature and It is likely that considerable improvement ean be effected by a systematic study of this color. One pound samples of the toner and corresponding 30J5 alumina hydrate- blane fixe lake prepared in the laboratory* have been submitted to the General Division for eval uation* The tenor* OS-7843, is appreciably darter, eleaner, and weak er than Bara Red RT-70-D, but is appreciably faster to light and non bleeding In oil* The lake, CS-7844, is much lighter, slightly bluer and faster to light than Scarlet Lake RL-10-D. Lakes from 1*5 disulfo 2 nanhthvlamlne Barium and ealeium toners were prepared from dye obtained by coupling diazotlzed 1*5 disulfo 2 naphthylamine with beta naphthol and beta-oxynaphtholc acid* The beta naphthol combination yields calcium pigments which resemble Toluidine Red tinctorially and are much light er, yellower and weaker but appreciably faster to light than the cor responding pigment of Lithol Red RT-379-D. The barium pigments are extremely hard In texture and apparently possess no merit. The betattaphthol dye and color lakes of the above intermediate are not new, being covered in tr*8* P. 718,356 of March 1902 by B.A. & S.F. Color Lakes from the beta-oxynaphthoie acid combination are bluish maroon reds of the Lake Bordeaux B type (Tobias Acid BC8? RT-33-D) and are non-bleeding in lacquer These pigments show no DUP050315533 '2 -'f 2 apparent advantage over the lake Bordeaux b colors. The beta-naphthol and beta-oxynaphthoie aeid lakes of the above intermediate, altho possessing some merit, do not appear to be of especial interest at the present time* 2-ehler 5 amino toluene 4 sulfonic acid and 6 ohlor 2 amino toluene 4 sulfonic acid B Salt Lakes 'The bright orange toner, CS-7807, obtained from the dye of 2 ehlor 4 amino toluene 6 sulfonic acid (2b Acid) and B Salt, prompt ed an Investigation of the isomeric subject intermediates with the object Of obtaining a yellower orange, similar to Persian Orange. However, subject intermediates coupled with R Salt and laked with barium, strontium, calcium and lead resulted in redder and bluer colors than CS-7807, and are of no interest. Pigments from ortho-nitro-aniline parasulfonie aeid and ortho-nitre aniline para aulfonanllide beta-naphthol Barium, strontium, calcium and lead toners were made from the dye obtained by coupling orthonitraniline para sulfonic acid with beta naphthol* rdth the object of obtaining an orange toner similar to Shawnee orange (orthonitraniline and beta-naphthol) tinetorially but superior in other properties. The resulting pigments were much dark er, duller and bluer than the ortho-nitr&nillne product and possessed no especial merit* Ortho-nitro aniline para sulfonanilide di&zotizes with great difficulty and altho the beta naphthol combination gives a dull orange pigment, the latter bleeds badly in linseed oil, which makes it of no interest* 2 nitro 4 beneoylamlno aniline beta naphthol The pigment dyestuff obtained by this combination is a deep reddish brown of bluish ehade which bleeds in linseed oil. The ben zoyl group apparently has an effect similar to the methexy group when substituted for the methyl group in meta-nitro-para-toluidine, namely, that of increasing the depth and blueness of the eolor. Subject pro duct possesses only little merit and further investigation Is not recommended. Quinoline Yellow P I^tkea and Toners Barium and calcium toners and lakes of subject dye are brown in masstone but clean lemon yellow in Bhade and tint, poor in lightfastness and oil bleed, and extremely hard in texture. The Du Pont Rubber laboratory has reported that the latex dispersion of the barium toner is similar in shade said strength to Hansa Yellow H but nonmigrating in rubber. The dry pigments apparently possess very little promise as printing ink colors, but night find use in rubber provided the texture is improved sufficiently to give good dispersion. Wowaol Blue TO watted on substrata and use of lanugtnic acid Ponsol Blue CO) when ratted with hydrosulphite and laked on alumina hydrate yields a lake superior to one prepared by striking DUP050315534 $ s, the hydrate "base In the presence of the ordinary dye paste. 'The use of lanuginic acid (dissolTed wool) in the preparation of rat dye lakes shows no advantage over the lakes prepared with the hydrosulfite vatted dye* The above experiment was strictly orientation in nature, and further investigation along these lines is recomended, especially with Ponsol Blue (BL-86-13 type), fright Orange CS-7S07 An additional one pound sample of the barium toner from 23 Aold and R Salt has been prepared for Bawark'a evaluation studies. gXESRBmagAl BBTAIL3 2 chlor 4 amine toluene Salt barium toner* Dxpts. 19. 21, 23 and 26 - B.B. 450, pages 52, 64, 72 and 86 respectively. IsS disulfo 2 naphthylaalna -A. m and BOB' Bxpt* 20 * B.B. 450, p.B4 Red 0 acid and 6 chlor 2 amino toluene 4 sulfonic acid Sxpt* 24 - B.B. 450, p.76 Salt OKI - OKAPSA and GBA para sulfonanllide 2xpt* 89 * B.B. 450, p.96 BB 8 nitre 4 benaoylaaino aniline --j^BH Bxpt* 30 - B.B. 450* p.102 Quinoline fellow P lakes and Toners Bxpt, 18 -- 9.3. 450, p*50 Ponsol Blue OB vatted and use of lanuginic acid 3xpt* 22 - B.B. 450,p.68 DUP050315535 plttUianC CQLCR HESBARCH BSPQRT ^^ IAS35HT RED 2B PXGMSHTS SUBMITTED BY* AKPROVSD BY* v f x l e i mao. iuUEKs BATS i KSBRUAEY 18, 1938 mmcmQTtm The bjeet of this report is a discussion of the metlxods for laking Lithoaol Red SB (Permanent Red 2B) and the effect of variables on the properties Of the pigments. It is recognised that the quality of the intermediate and dye is an important factor in the determina tion of tinctorial and bleeding properties cf the pigmentsj however, the general properties may also be altered appreciably by variations in the Taking procedure. SUMMARY & COffCLtreiOSa Intermediate and aye Soda Salt In order to Obtain pigments of optimum brightness and non-bleed ing In lacquer a high quality of 2 chior 4 amine toluene S sulfonic acid, free from any unsulfonated intermediate, is essential. Optimum tinctorial properties are obtained with the raonoelinie crystalline form of dye soda salt which results from digestion at TCr'CJ of the alkaline coupled dye and subsequent filtration. Direct lading results in undesirable tinctorial properties. The dry dye powder and corresponding paste give equal results but the paste is desirable for obvious reasons. Volume for taking The calcium pigments of Red 2b require high lairing volumes in order to obtain consistent duplication, which apparently is character istic of most beta-oxy-naphthoic acid lakes, 3000 cc per 0.05 mol ap pears to be the minimum volume which can be safely employed in the laboratory. Early studies indicated that exceptionally high volumes were essential in order to obtain optimum brightness; however, latter investigations showed the volume to be a factor but not as important as believed in the early work. Variation between 4600 and 1150 oe per 0.05 mol was made and all lakes were quite similar tinetori&lly. 3000 oc was selected as the volume for safe operation and consistent duplication, lower volumes tend toward a slight increase in depth and blueness* and inconsistent results. The early studies were carried out on alkaline developed dye, which is less soluble than the acidified dye, and which my account for the wide variations in tinctorial properties upon variation in vol ume of the former. Acidity and Basicity of Development Pigments struck at 40 C and developed acid result in appreciably lighter, brighter, cleaner, yellower and more transparent products than those attack and developed under alkaline conditions. The preferred method is to acidify and thus solubilize the dye, at 40C, with acetic acid prior to the strike in order to obtain a SH of + 5.0 for the nonstyraTand + 6,0 for toe styra* lakes. meSurcTafter the strike and . 'I DUP050315536 2 prior to development. Increase in acidity in either ease has no dele* terions effect* whereas a decrease tends toward Inconsistencies. Al kaline developed pigments. pH 7.5 to 11*0 are appreciably darker* dull er, bluer and more opaque than the acid developed lakes. Hon-styrax and styrax lakes struck and developed at the boil under alkaline con ditions are brighter than the corresponding acid pigments, but are much lighter, duller and bluer than the pigments struck at 40C under aoid conditions* The substitution Of hydrochloric or sulfuric acid for acetic acid is very- unsatisfactory, since pigments acidified with mineral acid are dark* brown, blue, very weak and poor in lightfastness, yeape.ratum.itC., gftCltt, The temperature of strike is important, an increase in tempera ture from 25 to 100eC In both the styrax and non-styrax acid developed lakes resulting in a decrease is depth, brightness, yellowness, strength and transparency, a sharp break occurring between SO and 60cC. Tem peratures above 60C result in very light, dull* opaque, blue and weak pigments* 40C was selected as strike temperature in the laboratory. Temperature of Development Decrease in temperature of development of the lakes decreases the depth, blueness and strength, which apparently is the result of Incomplete conversion or development of the calcium salt. Zt is essen tial to develop the styrax pigment at the boil in order to obtain the full effect of the styrax. Increase in time of development at the boll, from 10 to 30* in the laboratory* increases the depth and blueness of the styrax lake, having practically no effect upon the non-styrax pigment. One half hour boiling development is probably desirable in large scale operation* para scan Para soap added to the dye of the non-styrax lake, prior to aci dification, increases the brightness, strength and cleanness of the color* 3*0 grams per 0*05 mol dye gives optimum results in the labor atory* The use of para soap in the styrax lake has no beneficial ef fect upon tinctorial properties but does increase the yield appreciably* The use of ammonium chloride in place of acetic acid in both styrax and non-styrax lakes, results in pigments similar to those pre pared with acetic acid* Since the latter has a greater solubilising effect upon the dye it has been preferred to the ammonium chloride. ^IgtiM^Styrax.^akcs The use f Liquid Styrax tends to increase the depth and yellow ness slightly, and decreases the strength In direct proportion to the quantity of styrax employed. Liquid styrax apparently functions chief ly as a dispersing agent, giving pigment not greatly different frees the 1 -7 DUP050315537 3. non-styrax product. Of the 7.5 grams of styrax used in a 0.05 mol strike, only 3.0 grams are retained in the pigment as calcium styrax. The styrax* however* appears to impart better working properties to the pigment but this should be determined by actual application tests. The styrax under acid conditions of strike and development* which conditions are essential in order to obtain optimum brightness and yellowness, appears to be much less potent than under alkaline condi tions. The latter conditions result in a much darker, duller, more opaque and much bluer pigment. Variation in the quantity of styrax indicated that in the labora tory 7*5 grams per 0.08 mol dye gives optimum general properties. 4.0 gras, per 0.05 mol dye results in a stronger pigment and is prefer able provided the working properties of the pigment are not altered appreciably. Quantities above 7*5 gms. par 0.05 mol are not recom mended owing to an appreciable loss in strength. Variation in the quantity of styrax and the use of G-ar&inol WA makes it possible to al ter the tinctorial properties of the styrax pigment appreciably. Liquid styrax dissolves completely with the exception of only a slight residue of inert material, in concentrated caustic soda solu tion at the boil. The addition of a small quantity of alcohol just prior to adding the styrax to the dye aids the solubility, but is not essential. A mister of samples of liquid styrax. soma obtained fresh and some aged several years, gave similar results which might be taken as indicative of no great variation in this natural product. f frate of strike, # The rate of strike, studied over a range of 5 to 30 minutes in the laboratory, has no appreciable effect upon the styrax or non-styxax pigments. The use of Gardinol VA in the styrax lake increases the depth, strength, cleanness and bronze (a clean golden bronze) appreciably, apparently Owing to its dispersing action on the styrax soap. Sardine1 has no effect on the non-styrax pigment. 1.0.1. I&jclng Procedures Several ICX procedures for the preparation of the non-styrax cal cium toner were investigated, but 3how no advantage in operation or properties compared with cs-7745. irffyoggagioity of Calcium Pigments The calcium pigments of Bed ZB are hygroscopic and absorb moisture vdaen exposed to ordinary atmospheric conditions. The non-styrax lake upon absorption of moisture changes appreciably lighter* yellower and weaker, thus making standardisation difficult. The styrax pigment ab sorbs an average of 5.8# moisture but does net change tincterially. the calcium styrax apparently having a stabilizing effect. The non-styrax lake absorbs an average of 7.3# moisture, which is reduced to 3.18 by at DUP050315538 4* precipitation with a mixture of calcium chloride and strontium chloride In the proportions of 4 CaCls 75# to 1 SrOls.SHeO, without altering the tinctorial properties of the original calcium pigment. The resulting product does not change tinctorially as determined by aging the pigment under ordinaay atmospheric conditions for three month*. The use of the shore mixed salts as the precipitant for the styrax pigment is objeetionalbe. since in the presence of styrax the strontium alters the original tinctorial properties deleterioualy. Sryjng cf Calcium pigments Since the calcium salts of Red 2b are hygroscopic and the reten tion of appreciable moisture in the nen-styrax product alters the tinc torial properties* it is essential to dry the pigments thoroly. This has been accomplished in the laboratory by drying the pigment at 140F for + 12 hours and then at 180<VP for + 4 hours. Pigments dried in this manner contain approximately 2-3# moisture. The calcium pigment paste flushed into lithographic varnish is very much lighter and very such yellower than the corresponding dry pigment ground into ink. Zn this respect the calcium pigments of Red 2B resemble those of Lithol Rubine B* Aging of Bye.. Pasfo Aging of the dye soda salt paste has been found to have no deleterions offset upon the tinctorial properties. Pulverization Pulverisation of the calcium pigments has no apparent affect upon the tinctorial properties as judged from the results of laboratory tests. Other Metallic salts of Red 2B 3a* Sr* Pb, Be* Co, 31, Bn, Cr. Mg, Zn* Cd and Ha salts of Rod 2b of the non-styrax type range in shade from very dark bluish reds to light yellowish reds* The barium pigment la a light yellowish rod resembling the barium salt of Lake Red C* but possesses better lightfastness. The Ca and Ba pigments of Red 23 are the only ones *hieh possess appreciable merit. The Sodium salt is much darker, stronger* bluer and much fsister to light than the soda salt of Lake Red c bleeds profusely in linseed oil and is quite soluble in water. Extended lateas The alumina hydrate and alumina blanc fixe dry lakes of Red 2B, Oh equivalent aniline content basis, are much brighter in mas stone much yellower and more brilliant in shade and tint and faster to light than Lithol Rubine Lake KP-237-1) nag in Rubber . alitai styr&x and non-styrax dry toners and lakes milled int rubber are much bluer, cleaner and mere brilliant, and stronger than Rubber Red BG (RT-372-1) Barium Lithol Toner), and much yellower, cleaner and more brilliant than Latex dispersed Rubber Red CRD (Lithol Rubine R Calcium Toner) on an equal aniline basis. The non-styrax . ..uz- DUP050315539 s pigment is superior to the styrax product and both are non-migrating and faster to light than Hod BC and Red CRB* The latex dispersed nonatyrax Red 23 paste of CS-7745, is stronger than the corresponding dry pigment in rubber, all other properties remaining unaltered. Roainated Pigment The substitution of rosin for liquid styrax and subsequent al kaline development results in pigments of the styrax type tinctorial- ly, which unlike Duel Reds, give inks of exceptionally good flow. The roeinated pigments are low in bronze and high in finish when pre pared into ink. but are weak owing to the high quantity of calcium roainate retained in the pigment which also gives to this product an exceptionally high yield. BXSSR1HS5TA.L KSTAXIfl Sxperimeatal Beta! Is are covered in the monthly reports for August, September, October and December 1934 and January 1935, filed under ''Miscellaneous Toners'*, and in notebooks 487 and 438* CS GS-7743~- r*rtjk* _ 7747 7748 7749 - * * 8-9 A - non-styrax * - low styrax - no Gardine1 * C- - Gardinol B - high styrax - * * s - rosinated DUP050315540 PIUMSHT omm RESEARCH REPORT SUBMITTED BY I APPROVED BY! ^ > ~> p il e * m&a^-s&smm DATE! FEBRUARY-1935 IUTRODUOTIOB The study of the determination of the stability of Permanent Rod S3 calcium pigments under ordinary atmospheric conditions was completed this month, SUMMARY & COUCLUSIOBS Son-styrsx calcium toner prepared with a mixed precipitant of calcium and strontium chlorides, the styrsx tenar, and the rcsinated fiigomnsenftowra1re21agdeadysi,n the laboratory under ordinary atmospheric eondiBona of these pigments exhibited any objectten able alteration tinctorlally and it has, therefore, been concluded that these dry pigments are stable under ordinary storage conditions. Additional one -half pound samples of CS-7745, 46, 47 and 46 ware prepared for the Service Laboratory, BXEgRXHBBYAL BBTAHA Bxpt. 7* S.B, 438, p. 28 e STon-styrax, styrax and rcsinated dry pigments were aged in open paper envelopes for 121 days in the laboratory under ordinary atmos pheric conditions, being taken out, mixed and then returned to the envelopes each week, under these conditions, the pigments were found to be stable and no noticeable or objectionable tinctorial change occurred in any ease# Bxpt. 13, H.B. 438, p.52 Additional samples of CS-7745, 46, 47 and 48 were prepared using D,W, dye let #1 in place of charge 25. The non-styxax pigment was slightly lighter and bluer than the original CS sample, and the atyrax pigments were darker and bluer than the original CS samples owing to the difference in the quality of dye* DUP05031 5541 f imb c t bo l o b k bs babc h r e p o r i TUBS TOBBR RT-208-D Jf-f? s t ibk it t s b by * APPROVED BY* FXISs PIHB TGHSR MTEj PSBRBAHY-1935 IHTRODtTCTlO* Du Pont rtho-ohlorparaaitraniline, of plant mqpufacture, mam tested far use in Piro Toner, Ri-208-2), 3TIMMARY & COgChtfSIOBS Dyeworfcs plant manufactured intermediate, prepared by direct amidation of 3*4 diahlornitrobenzene, charges #1 and #8 in paste form and charge #2 dried in the laboratory, have been found satisfactory for the preparation of RT-208-D. The pigments from these materials are superior to standard RT-208-3 and the corresponding laboratory control in tinctorial pro perties , linseed oil bleed and turpentine insolubility. The plant intermediate is similar to the laboratory prepared material, which was reported upon in December, The dry intermediate exhibited no advantage in wettability, diazotization or pigment properties ever the paste, and either can be employed in the preparation of RT-208-D, 1XPBHIMSSTAL DETAILS Bxpt, 25, 2T.B. 450, p. 82 DUP050315542 PXQaSHT COLOR KSSBARSH HBPOBT MSPT FOR fOLUXDISB BEEPS & SU3HITTBD WTi APEROVBD BT* IBTHOBtaffgtOg Investigation of meta nitro para toluldine wet crystals and crude paste for the preparation of Toluldine Reds has "been resumad. The poor settling of suspended matter is plant diazotized MHPT was investigated* SUMMARY & (KgfgLtJSXOBS Clarified MSPT wet crystals give satisfactory color and yield of Toluldine RT-386-J5, The crystals are very large and require a longer time of diasotlzaticn than standard intermediate* Crude SBTPT paste diazotizes slowly, owing to the large size ef the crystals, and results In considerably lower yield and poor color* Ball milling of the crude paste material and filtration of the diaso resulted in complete and rapid diazotisation, substantially standard yield and color* which was only very elightly dull versus laboratory control but equal, to slightly superior, to standard RT-S86-B, The Baring effected by using clarified wet crystalo would not . be appreciable compared with the standard dry material now employed, whereas the possible saving by the use of crude paste, taking into account the necessary f iltration of the diazo, apparently would be substantial* further investigation on the use of crude intermediate is being continued* K8BT prepared with Gardinol WA as a wetting agent in place of Alkanol B* results In poorer settling apparently owing to decomposi tion of the Gardinol to the free alcohol, which is an oil-non-miscible with water and which apparently coats the suspended particles and prevents settling. gXEBRXmm aSTAiLS . Rscpts* 27, 28, BO and 31 -- JB 450, pages ^0, 94, 102 and 106 respectively. DUP05031 5543 DUP050315544 SUBMITTED BT APPROVED mt . "V v PUB* ]fflESCTTf03RSDATE* FEBRUARY-! 935 m^mja Investigation of the tinctorial change whieh occurs in litho graphic prints of Figment Rubins G, RT-359-D, upon exposure to light* has been completed. sxmms^ & mw&xm Fade-0-Htar and outside exposure tests under glass were made on rubout mountb of standard RT-359-35, laboratory control samples and similar pigmenta prepared by modifications in tbs laklag procedure. The change from a yellowish to bluish shads* -which the prints of RT-359-3S undergo upon exposure to light, appears to be due to the T" loss of the yellowish bronze, thus exposing the true blue undertone of the color* Altho a number of -variations were made la the laJcing ?rooreleadl uarelt,ernaotnieonre* sbuulttedininsomtheeeeasliems inaantiootniceoafbtlhyeleosbsjecchtiaonngaebwleaB tineap parent after exposure* Zn these oases, the bronze was higher than the standard pigment after exposure* Apparently the only solution to this problem would be the prep aration of a pigment possessing no brenzehut this would probably in volve considerable change in tinctorial properties, this investigation has resulted in a product practically iden tical with standard RT-359-2) tinctorially, but which upon exposure exhibits much less change. This is accomplished by digesting the coupled dye at 60CP until an acicular form is obtained} the dye thou being strucb at this temperature, and subsequently developed at the boil* wpmmKW.jmxui Hxpt. 29, H.B. 416, p. 128 DUP050315545 PIGMENT COLOR RESEARCH REPORT RUBBER COLORS SUBMITTED BY: APPROVED BY! INTRODUCTION The Rubber Laboratory has examined, the extended Lithols and specially treated PTA colors which were submitted in January, and has submitted reports as to their use in rubber, A further report on the Goodrich Lithol CS-7758 has also been made. The laboratory work has been largely concentrated toward the development of a Green Lake to match Imperial's Green X-1292 and the solution appears to be in sight. SUMMARY & CONCLUSIONS Imperial's Green X-1292 has been discussed in previous reports. It is a lake of a mixture of Lithosol Brilliant Blue E and Naphthol Yellow^and preliminary experiments had given results very close to the competitibn. Competitive samples from three sources were not uniform, however, so a sample (C37280) (1 lb,) obtained directly from the manufacturer was selected for matching. After some study, we selected Du Pont Lithosol Brilliant Blue E and National Naphthol Yel low S as the dyes to use. Suitable adjustment of the amounts of the two dyes was quickly made to approximate the competition in strength and shade, but we were consistently dirty. A study of special treating agents showed that treatment with a combination of 5^ Duponol WA Cone, and 5% Di glycol Stearate added to the mixed dye solution gave much cleaner products. They were also slightly weaker, but the yield was corre spondingly increased, Further adjustment of the dye amounts and some increase in the BaCl2 used has given a product, 77C, which is satis factory in strength and shade and definitely cleaner than C-37280. A large sample will be prepared and set up as CS. Some study has been made of the use of quinoline Yellow F as the yellow component of a similar green lake and also as a self col or. It is too expensive for use in the green lake, thoggh it does give a stronger, more brilliant and yellower lake than the same con centration of Naphthol Yellow. As a self color it is much cleaner and greener than Naphthol yellow and somewhat faster to light. In the two or three experiments that have been carried out, the products have been very hard and gritty and not at all suitable for use in rubber. However, the color appears to be desirable both in shade, lightfastness and freedom from migration in rubber and some further study is planned. Some study has been made of the possibility of obtaining bene ficial effects in Lithol Reds (both toners and extended colors) by the use of Gardinol and Diglycol Stearate. The combined use gives a pronounced effect of depth of masstone and cleaner, stronger tints ; in rubber the degree of dispersion is actually DUP050315546 2 diminished. Diglycol Stearate alone may have some merit in rubber Lithols, though the evidence to date is rather limited. B. 3?. Goodrich Company has examined the shipment (100 lbs.) of R1-400-D (CS-7758). They find it quite satisfactory for many of their formulas, and are well pleased with its working properties. However, they criticise its shade in a special formula of which they sell considerable amounts in an uncured state. We recognize that R1-400-D is- slightly bluer than customer's standard under these con ditions, though during the cure this difference largely disappears. Customer's reports have been somewhat inconsistent inasmuch as they selected the bluer end of the range first submitted, CS-773$5 7734, 7735. However, we believe that the difficulty can be appreciably lessened by further study of the mixes submitted, and we hope that a substantially perfect match ispossible. The rubber laboratory has reported evaluations on the follow ing products. Lithol Reds CS-7758. They have examined the Goodrich Lithol and are in substantial agreement with our evaluation of it. They desire to make further tests on the components of this mix (CS-7664 and CS-7665) looking toward using them to replace our present Lithol toners which are unsatisfactory in dispersion. CS-7759. Extended BT-125-D. The tests show this product to be entirely satisfactory in itB behavior as regards dispersion in the rubber, but there are certain properties such as a pronounced parchment paper bleed which make it inferior to Blue ]Q). We will probably attempt to overcome this by the use of Victoria Blue R in a similar lake. CS-7789. Treated GT-347-D. This product is commended very highly both for its physici.1 properties and its brilliance of shade. It does, however, show slight crocking and some effort will be made to correct this, before Semi Works trials, by the use of Alumina Hydrate in the extender. It is felt that there will be some call for a bluer shade of Green. We will, therefore, do some work on developing a similar color based on GT-354-D (Brilliant Green Toner). CS-7790. Treated RT-357-D. The rubber laboratory praises this color in its physical pro perties, but states that there is very little call for the shade. Ho further work will be done unless there is a demand for the color. RT-359-p. Pigment Rubine G - was recently milled into rubber. It is much yellower and somewhat weaker than a Barium Lithol, but is also much better, in lightfastness and is non-migrating. Although we have no call for it at present, it will be kept in mind as a possible rubber color. ;V;!MSsr .--I 2^ ~v DUP050315547 3 EXPERIMENTAL DETAILS See notebook 435, pp. 146-173 435-64. Variation of dyes in an attempt to match Green Lake C-37280. The results are encouraging, though not an exact match. 435-65. Treatment of Green Lake with A - control B - Na Stearate C - Gardinol D - Diglycol Stearate The effects were slight, but there was some evidence of better dispersion and cleaner shades. 435-66. Quinoline Yellow Lake based on CS-6389. Different dyes were used and the colors varied in strength and shade but were fairly close to CS-6389. They were all too hard to be of interest in rubber. 435-67. Gardinol and Diglycol Stearate were used in extended RT-364-D (CS-7664). In inks they each had some effect, and the com bination of the two gave a dark, bright masstone, a high finish and a clean, strong tint. In rubber the products had poorer dispersion than the control, a result wholly unexpected. 435-68. Gardinol and Diglycol Stearate treatments applied to toners of RT-364-D. The combination treatment is definitely harmful to dispersion in rubber as is the Gardinol alone. Diglycol Stearate alone shows some slight superiority over the untreated control. In inks the results are similar to those obtained in the 67 .series. 435-69. Purther variation in dyes in the Green lake like C-37280. ' The results approach the competition in strength and shade but are still dull. 435-70. Green lake like 69c but treated with Gardinol, Digly col Stearate and combination of the two, the treating agents being added to the dye solution. The last gives definitely cleaner tints with some weakness but increased yield, 435-71. Lakes of O.uinoline Yellow F on Alumina Hydrate and on Blanc Piss, The lakes on Blanc Fixe are worthless, but those on Alumina Hydrate are strong but much redder than those obtained in the 66 series. They were all very hard and were not tested in rubber. 435-72. Lakes of G,uinoline Yellow p on Alumina Hydrate and on Gloss White with varying amounts of dyes and some study of develop ment . The development at the boil gave nothing interesting. Gloss White base gave very weak products. Decreasing dye gives cleaner tints with little change in strength over the range studied. The products are quite hard, though they milled into rubber fairly well. . xr.i'sffi- DUP050315548 4. 435-75. A preparation of a Haphthol Yellow Lake and one shaded with 30|T*QuTnoline Yellow, P. The latter gives a definitely greener and cleaner color, bast both are much redder and dirtier than Quino line Yellow lakes. 435-74. further study of the Gardinol-Diglycol stearate treat ment of the Green lake as in 70D, but with adjustments of the dyes to increase the strength slightly. The beneficial effect of the treatment is confirmed and a pro duct obtained (74D) which is 5% strong, v.s. yellow and clean versus C-37280. 435-75. A study of substituting Quinoline Yellow P for the Haphthol Yellow in 74D. 20$ substitution gives a much yellower and cleaner product with some increase in strength,and the effect in creases with larger amounts of Quinoline yellow. Inasmuch as Quino line Yellow is mueh more expensive than Haphthol Yellow, it is not attractive in this formula. 455-76. An attempt to further adjust the strength and s^iade of 74L~*by variations in the dyes used. The products, 76B and 76D, are very close to C-37280, B slightly blue and D slightly yellow, both definitely clean, strength OK. * 435-77. Checks to 76B are not perfect but are quite close. Increasing i'he BaCl2 has little effect on the finished product, but did reduce the backwater bleed and will be adopted. 77C will be the basis for a large sample for a CS. Vy\ . "^ 5 V"" ' DUP050315549 PIGMENT COLOR RESEARCH REPORT FIGMENT GREEN B SUBMITTED BY APPROVED BY: PUB: ?>aSr0. TOffiSllDDATE: FEBRUARY-1935 INTRODUCTION Work on the Pigment Green 3 problem during this month may he divided into three parts: 1. Continuation of the rubber testing of semi-works and plant batches; 2. Study of the paper dyeing method; 3. Study of the 444-1*20 method for preparing a dry color for rubber. SUMMARY & CONCLUSIONS 1 Rubber Testing of GT-68-P The results of the rubber tests on semi-works and plant batches are reported in the Development Report on this problem. It is of interest to mention that the first shipment of GT-68-P. lotJl3926, has practically received the approval of the DuPont Rubber Laboratory and has been tentatively set up as the new standard (latex dispersed) replacing General's Pigment Green B. Final approval is awaiting fur ther tests, such as aging, soap bleed etc. 2* Paper Dyeing Test. Progress with this phase of the problem has been delayed due to. the uncertainty of the paper dyeing method employed at the DuPont Paper Laboratory. After spending considerable time in testing samples of our GT-68-P, the Paper Laboratory admitted that the ori ginal testing method was inconsistent and unreliable. A new method for testing green pulps for paper dyeing was then developed, and it was reported that our lots 13915 and 13925 were about 5% stronger than General's recent deliveries which in turn are about 20% weaker than the original standard. We will attempt to produce material which will be about equal to General's original standard. Much time was spent in attempting to duplicate the Paper Lab oratory's latest dyeing method. We have been successful in duplicat ing all steps except that of drying the finished paper. This angle of the test is being studied carefully. Our results, while not wholly in accord with those obtained by the Paper Laboratory, are fairly satisfactory. 3. Improvement of method 444-12C The 444-12C method is similar to the regular GT-68-P formula in all respects except that it contains a lower amount of turkey red oil and in addition diglycol stearate. The dry color from method 444-12C gives almost equal dispersion to the latex dispersed color but is dirty in tint. The addition of blanc fixe to 444-12C gave only a slight im provement in strength and cleanness. Freshly precipitated barium sul phate showed no advantages. DUP050315550 Modifying the place of addition of the diglycol stearate gave no improvements. It was found that the final color must be washed thoroughly in order to obtain maximum dispersion. Slight.variations in the amount of cadmium sulphate were effect ive. The results from the cadmium variation went through an optimum in dispersion, beyond which a very dirty color was obtained. Appar ently, some cadmium is necessary because attempts to omit the cadmium were accompanied by very weak colors (i.e. poor dispersion). Likewise the turkey red oil apparently goes thru an optimum in the effect on dispersion. A comparison in rubber of the pulps of methods 406-66C (standard GT-68-P) and 444-12C revealed that the dirty color of the latter was inherent in the process and not due to the drying step. An attempt to improve the dispersion of the dry color from method 406-66G by reslurrying the washed toner, passing thru the colloid mill, refiltering and rewashing was unsuccessful. Addition of blanc fixe and diglycol stearate to the above gave some improvement but not enough to approximate the dispersion of latex dispersed color. EXPBRIM3MTAL DETAILS H.B. #444 Series 444-14-16-18 were paper dyeing tests on semi-works and } plant batches of GT-68-P. The results of these tests were inconclusive since the method employed was found to give inconsistent results, and was therefore abandoned after considerable study by the DuPont Paper Laboratory. Series 444-26-27-29-30-31 were additional paper teats on GT-68-P semi-works and plant batches following the latest method developed by the DuPont Paper Laboratory. The testing method has been duplicated in our laboratory f airly satisfactorily up to the drying step, which has presented some diffi culties. At the Paper Laboratory the papers are dried for about 15 min utes in a drum drier under considerable pressure and at a temperature of 90-100''C. This method of drying produces a flat paper with a smooth finish. Our method has consisted in placing a stack of papers in an oven at 60C and covering with a glass plate on which was placed a heavy weight. This gave papers quite similar to those dried in the drum drier but it required about 20 hours to dry. A comparison of our results with those obtained by the Paper Laboratory did not show agreement in all cases. The testing method will receive further study. Series 444-15-22-52 were preparations of nitroso compounds for use in the following experiments. Series 444-17 was a study of the 444-12C method for preparing a dry Pigment Green B for rubber. It was found that a combination of diglycol stearate, turkey red oil and cadmiflm is apparently necessary for good dispersion in rubber. Omitting the oil and the cadmium gave an inferior dirty product. The use of D.G.S. and T.R.O. without cadmium gave very poor dispersion. DUP050315551 3m Series 444-19 varied the cadmium sulphate in method 444-12C-. The results went through an optimum in dispersion, beyond which very dirty colors were obtained. Series 444-20 varied the turkey red oil in method 444-12C and tried the effect of adding blanc fixe. The results went through an optimum in cleanness and disper sion, beyond which the color became weak but remained clean. The addition of blanc fixe improved the cleanness of tint only. Series 444-21 tried the addition of D.G.S. in various places of the 444-12C procedure. The check to 12C was quite dirty and the results showed no advantages. Series 444-23-24 studied the washing of the final toner of method 44'4-2'dD-^extended 444-12C). It was shown that incomplete washing gave weak dirty colors. Series 444-35 studied modifications in the preparation of bar ium sulphate in method 444-20D. Freshly p recipitated barium sulphate showed no advantage over slurried blanc fixe. The color prepared by the 444-20D method was demonstrated to be about 5% weaker than the latex dispersed Pigment Green B but distinctly dirtier. Series 444-28 compared methods 406-66C and 444-12C as pulps milled into rubber to determine difference in cleanness of tint. The results showed that method 444-12C 1b inherently dirty compared with 406-66C and that the dirty tint of the former method is not the result of the drying. Series 444-33 tried the effect of reslurrying a washed toner of 406-66C, passing tliru the colloid mill, refiltering and rewashing; also the effect of adding blanc fixe and diglycol stearate in the above procedure. Advantages were obtained but not sufficient to even approximate the latex dispersion. ;-:y. . DUP050315552 PIGMENT COLOR RESEARCH REPORT SUBMITTED BY: APPROVED BY: Y" PIGMENT GREEN B, GT-68-P . .' . -> -i. -It PILE: DATE: FEBRUARY-1935 INTRODUCTION Development work in the Semi-'Works was concluded for the time Being during the month. Impr&yejl cleanness of tint and uniformity and dispersibility of pulp are t!* .desired results of this work which would give a product suitablwrfor both rubber and paper. A single batch was mad% in the plant checking one of the best of the Semi-Works strikes of last month (SW-6721). SUMMARY & CONCLUSIONS Two batches were made in the Semi-Works during the month. The first was made on the SW-6721 formulation and split in two parts for the purpose of running a washing study, the halves being washed sixteen and forty-four hours respectively. These two parts (SW-6767 and SW- 6768) checked each other in uniformity of pulp both giving a firm, slightly lumpy pulp which did not break down on handling. In rubber, both halves of this washing study were very slightly dirty versus the rubber standard (D#1832) but in strength the longer time of washing (SW-6768) gave slightly strong results versus the rubber standard, and the partially washed product (SR-6767). The second batch made in the Semi-Works studied the effect of decreasing the Cadmium Sulfate crystals used in the Cadmium Turkey Red Oil soap by 50$. This cut in cadmium sulfate did not affect the stability of the cadmium soap, and the usual firm but slightly lumpy pulp was secured. In rubber test, this product (SW-6783) was slightly strong, vvs. blue and vvs dirty against the rubber standard (D#1832) and v.s. clean versus a product made using the standard amount of cadmium sulfate in the soap (SW-6768), This result will be checked on a plant batch in the near future. The plant batch (41873) made on a 2. mol formula to check SW-6721 gave a satisfactory product tinctorially. the rubber test giving vs strong, vs blue and clean results versus the rubber standard. The pulp, however, broke down on stirring to a thin slurry containing approximately 21$ solids. On treating part of the pulp in the labora tory with 1% of salt a smooth, firm, pulp was secured, which gave OK. vvs clean results in rubber versus d #1832. An attempt will be made to increase the solid content of this pulp and improve its firmness by treating with l/2$ of salt, re-pressing part of it to a 40$ dry content with subsequent mixing of the 21% and 40$ pulps to secure a dry content of 27$ (the required standard dry content). This treatment is still in process and will be reported next month, A portion of this plant batch treated with salt was mixed in the pulverizer with a strong, dirty semi-works batch (SW-6676). the result being a 24$ pulp OK in strength, but blue and slightly dirty in rubber versus d #1832. No attempt has been made to secure paper dyeings on these pulps during the month as the method of test is still in process of revision, A summary of Semi-Works strikes will be found in Table I. and Plant strikes will be found in Table II. The mix of SW-6676 and part of Batch 41873 has not been assigned a mix number, and is not summarized. '%.. DUP050315553 >> 5h rl TJ CM CO 03 GO rH t =gr S CO > tH G 03 > e-< >> p CO ;o5 h3 to to F 1 bo E= G CO 50 o J3 P Sh fe-6 oG ,o o o pu CD P3 a W o CtoM ( P co > rOHl to o <D c H P 6550 Ph -H P< rH P <2 *T5 > 5G0 P*H s-ar--1 ff rtoo o ctf u a o.G CmH oC n> j Hx JEC3hD & v: .0X ft H 1 O.3aS>^U CO o o 4; ~jfc CO (aAt 11 u? mCO rH rH rH CM oa> CO Cc Om X5-! u t1--oi CJ T3 AX m a* 9> CM >svH rH c- to l> * to rH e\? Cm t- O to CM < pH c-- CO to to o- fcto to aatt tao* CM <tCCo4OO* rf-oN'S* to 31 aCTO* N O p CM G rH O *' *--p oP K pLi m o XA o rH CM to *o G <C rl CO CO eto CM CO CO "g >ra .eh-< X ,3 G > lP CM a> E-t P d3 b P G r P A p3Q- P co is a: CO CO 50 G O U n > CQ o 55 *H P H c 5cH0 $ Pi P rH o TGO GP Ph o a} P ttf J} cO O.G u O MH 3 9H PCUXO pca r0H* P> o i cmo J5 > O CO aCO* ' rH CM rH CM tn to I o CO o o o-p 00Sffe Au ro o P rH m SXP3RIMSNTAL DITAILS < DUP050315554 PIGMENT COLOR RESEARCH REPORT riWPROVEMBSr'IN l ig h t e a s t b s s s o p v ic t o r ia p u r e b l u b b o t o e e r SUBMITTED BY: S APPROVED BY PILE: DTA-- DATS: PEBRUARY-1935 INTRODUCTION It was suggested by Jackson Laboratory that we again exchange samples of FTA toners to compare the relative merits of the toners from the Newark and the Dyeworks Halopont processes. Since the Halo- pont products are chiefly 24 toners, a new process was developed for the preparation of a similar product utilizing existing information. The new process gave a considerable improvement in lightfastness over CS-7736. Pulp samples of Methyl Violet. Victoria Pure Blue 30 and .Ethyl Violet toners were prepared by the new method and sent to Jackson Laboratory for conversion to Haloponts and testing in paper. SUMMARY & COBGLUSION In developing a new process for the preparation of the 24 PTA toners, CS-7736 was chosen as the best starting point. The direc tion of precipitation was reversed (dye added to PTA solution) to insure more complete conversion to the 24 toner. The quantity of molybdate was reduced to conform more closely to the Halppont colors. Several series werethen run to determine approximately the optimum quantity of dye and of acid. The quantity of Gallic acid and Gardinol used was decreased, but the optimum quantities necessary were not d etermined. The use of the usual amount of Gardinol resulted in the formation of a very weak pigment. When only a small amount was * used the effect on the Methyl Violet, Ethyl Violet, and Pure Blue BO toners was negligible. Large pulp samples of the Ethyl Violet, Methyl Violet, and Victoria Pure Blue BO toners were prepared and sent to Jackson Laboratory. BXEERIMB1TAL DETAILS See Notebook 426 Bxpt. 21. Effect of variation in acid and of reverse strike on CS-7736 type procedure. Results. High acid seems to decrease the lightfastness while a reverse strike results in improved lightfastness. Sxpt. 22 Effect of Gardinol and Gallic Acid on CS-7736 proce dure. Results. Gardinol improves the lightfastneas but decreases the strength considerably. Gallic acid improves both strength and lightfastness. Bxnt. 23 Preparation of a PTA toner of Chrome Blue G.C.B. Results. The toner obtained was weak, dirty, and poor in light fastness versus BT-115-D. Bxpt. 24. Study of precipitant balance on reverse strike of CS-7736. Results. A considerable reduction in the precipitant balance without a corresponding reduction in lightfastness is possible. DUP050315555 .% 2 Expt. 35. Further study of Gardinol, Gallic acid and preci pitant balance on a reverse strike of CS-7736. Results. A further decrease in precipitant balance is without effect. A small amount of Gardinol seems to have no effect. Bxpt, 26. Reverse striks similar to Exp. 25 using Methyl Violet and Ethyl Violet. Results. The toners obtained were weak but slightly better in lightfastness than BT-122-D. Expt. 27. Further study of acid and precipitant balance of re verse strike of OS-7736. Results. Approximately optimum conditions have apparently been obtained. Expts. 28, 29. 30. 31. Preparation of large samples of Methyl Violet, lthyl"~Violet and Victoria Pure Blue BO Toners by the process of Sxpt. 27. Results. All sent to Jackson Laboratory for evaluation. Bxpt. 52. Revision of the Sxpt. 28 process to conform more closely to 0S-7736 except using reverse strike. Results. Use of increased quantities of molybdate and dye improves the lightfastness slightly. Bxpt. 35. Study of direct and reverse strike of Methyl Violet. Results. Inferior results were obtained with the reverse 'strike . , DUP050315556 9 9 * 'a |gv fljfefc.'- PIGMENT OOLOR RESEARCH REPORT SdT-^ y.7 SUBMITTED BY* 6. .9fa APPROVED BY: PTA YIELD STUDIES i > i / > v - c ft1* PILE: PTA COLORS. DATE: FEBRUARY-1955 INTRODUCTION PTA toner production was quite high during the month, a total of fourteen batches being made. These included two batches of BT-125-D, four batches of RT-330-D, six batches of RT-392-D, and one batch each of BT-100-D and BT-122-D. These batches were not super vised by the Development. Section in any way except for the following yield tabulation. SUMMARY & CONCLUSIONS The estimated yifcld on BT-125-D has been revised downward by the plant to 80# from 88#, Average yield on the two batches made was thus brought up to 104$ of estimate, although actually amounting to 94$ of the old estimated yield. This is a 4% improvement over the yields secured on this color last month. These batches were satis factory tinetorially The average yield on the four RT-330-B batches made during the month gave a more than satisfactory average yield of 118$ of esti mate, an improvement of 17$ over last month. Rubout results were also satisfactory. The reason for the abnormally high yield is not known. Yields on the six batches of RT-392-D made were also satisfac tory r amounting to 105$ of estimate, an improvement of 6% over last month. All these batches were satisfactory tinetorially. Yields and rubout results are not available as yet on the BT-100-D and BT-122-D, and these will be reported next month. For tabulated results see Table I. EXPERIMENTAL DETAILS N.B. 434, pages 41-44 TABLE? I Color Batch Yield Grind Rubout vs . Standard Est.# Lump# Masstone Under. Str. Tint BT-125-D RT-330-D ft B RT-392-D m n 9 41890 41911 41940 42003 42054 42064 41982 42029 42081 42100 42128 42151 80 84 80 82 96 108 96 114 96 116 96 114 96 96 96 104 96 102 96 100 96 102 96 100 s.red red dk vs dk. vs dk. B ws red vs str. s .yel yel. H ft s.dk. s.bl. dk. V3 bl. It s .bl dk,vs brn . s.yel. dk yel B >1 ws wk vs red vs str. vs green OK s .yel -*- yel. ~- ft s.str. ft a it str bl. vs bl & cl. bl s ,ye 1. ft yel. Ui- 4?:%' -.* "2 . >-* r-- DUP050315557 PIGMBST COLOR RESEARCH REPORT GRINDING OP PTA TONERPULPS SUBMITTED BY Qj l APPROVED BY: X?C PILE: -IBG. CTUDIEBDATE: FEBRUARY -193 5 INTRODUCTION One batch of RT-126-P was ground wet thru a pulverizer during the month, to attempt an improvement in smoothness of the pulp for Joliet Wa.ll Paper Company. A 5.1b. sample was submitted to the custo mer. One batch of GT-66-P was processed in the same way for A. M. Collins. SUMMARY & CONCLUSIOHS Two-thirds of SW-6779 - RT-126-P was put thru the Mikropulverizer to attempt to get rid of lumpiness in the pulp. The pulp after going thru a 3/32* screen was much smoother than the unground pulp, although a low yield was obtained due to material clogging in the machine. A batch of GT-66-P, (SW-6822) was put thru the Milropulverizer, but a great deal of material stuck in the machine and would not go thru even a i/4* screen. As much as possible was washed thru but / there was a big loss in yield. C /; It would appear that it is impractical to grind small amounts of pulp in the Mikro pulverizer as it is unavoidable that a large amount, comparatively, will be lost in the mill. On a larger batch, If it would undoubtedlyprovepractical, as a decidedly smoother pulp vF' results. P EXPERIMENTAL DETAILS See N.B. 291, pages 70 and 72. V-;.v j DUP050315558 PIGM3ET COLOR RESEARCH REPORT AZO-SULPHITE DERIVATIVES SUBMITTED BY APPROVED BY FILE: LITIIGL REDDATE: FEBRUARY-1935 IMTRQDUOTIOSr Further work on the preparation of sulphite esters of azo reds was carried out during this month. SUMMARY & COUCLUSIOBS A substantial tinctorial match for the barium toner of Lithol Red RT-364-D was obtained by the use of a procedure similar to CS- 7801 (calcium toner by azo-sulphite process) which includes an acid ification treatment prior to filtration. The yield of the barium toner was satisfactory. CS-7801 was found to possess poor dispersion in rubber. Con sequently an attempt was made to improve the dispersion of CS-7801 in rubber by passing a washed reslurried toner through the colloid mill, refiltering and rewashing. This treatment was practically without effect. Likewise, extending the colloid milled toner with blanc fixe and subsequently treating with diglycol stearate, gave a product which was considerably inferior to CS-7665, the special extended calcium lithol for rubber. A toner, 446-23C. made by the azo-sulphite process, but which used a lower amount of calcium chloride in the strike than employed in CS-7801, was found to give equal dispersion with a slightly bluer and cleaner tint than CS-7665. However. 446-23C was slightly weaker than CS-7801 by printing ink rubouts. An attempt will be made to duplicate 446-23C. It is probable that two formulations maybe ne cessary, one for printing ink and paint purposes, and the other for lubber color use. A completely soluble azo sulphite compound of Red for Lake C was obtained by reducing the amount of caustic soda in the sodium bisulfite-caustic soda treatment. Substitution of pyridine and soda ash for caustic soda likewise gave complete conversion to the soluble azo sulphite. The barium toners prepared from these azo sulphite compounds were weaker than RT-313-D. The soda salt of Lithosol Red 23 offered more difficulty. Contrary to previous experience, higher yields of soluble azo-sul phite compound were obtained by the use of sodium bisulfite-hydrochloric acid treatment than by the usual sodium bisulfite-caustic soda method of treatment. About 94% conversion of the soda salt to the soluble azo-sulphite derivative was obtained, and only about 93^ of this compound was recovered as the calcium toner. Apparently there was still some amino compound formed as a result of the bi sulfite treatment. The calcium toners were very weak tinctorially. cLerivati-ye was obtained in the case of Pigment N.B. 446, pp. 76-114 DUP050315559 .2 Series 446-25 tried the formation of the azo sulphite deriva tive of Lithosol Red 2B by varying the amount of alkali. Complete conversion was not obtained, although it appeared evident that the higher amount of alkali gave the worst results. Series 446-26 prepared- the calcium toner of Lithosol Red 2B from the azo-sulphite derivative. The result showed a considerable lower yield, a light and weak product. Series 446-29 prepared Lithosol Red 2B soda salt with and without Leukanol. Corresponding azo sulphite derivatives -were formed and converted to the calcium toner. Leukanol had no advan tageous properties. It was demonstrated that the conversion to the azo-sulphite derivative was not complete, and that the soda salt of Lithosol Red 2b was apparently split off at the azo linkage giving amino compounds. Series 446-57 & 40 studied the effect of reducing the amount of alkali in the bisulfite-caustic treatment of Lithosol Red 2B and the effect of using a mixture of bisulfite-hydrochlorig acid. Reduction in caustic soda increased the conversion of soda salt to a soluble compound -from 43$ to 68$. The use of acid with bisulfite increased the conversion from 68$ to 94$. It was also observed that the amount of amino compounds, which were formed, was appreciably reduced. The calcium toners were distinctly inferior to CS-7745. Series 446-27 and 28 tried the norit-filtercel treatment of Lithol Red summarized in January*s report. Series 446-30 prepared the barium toner of Lithol Red fro m the azo-sulphite derivative following the acid treatment as in CS-7801. The resulting product liras approximately equal to control in yield and was slightly dark. s.strong, clean and blue versus standard RT-364-D. Thus, it is evident that the final treatment must be definitely acid to Congo red in order to obtain the lower yield; insufficient acid gives a high yield and a correspondingly weak product. Series 446-51 prepared 30$ extended barium and calcium toners of Lithol Red by the azo sulphite process with and without diglycol stearate, and tested the results in rubber. The rubber tests were very inferior to our regular extended rubber colors CS-7664 and CS7665, being very weak. D.G.S. gave no marked improvements in di spersion. Series 446-35-36-38 studied various methods for obtaining a soluble azo-sulphite derivative of Red for Lake C, e.g. reducing the amount of alkali in the sodium bisulfite-caustic soda mixture, sub stituting soda ash. ammonia and pyridine for caustic soda. Reduction in caustic soda gave complete solubility; omitting the alkali gave only 70$ conversion to the soluble compound. Ammonia gave incomplete conversion. The barium toners prepared from the azo-sulphite compounds were weaker than RT-313-2>. Series 446-39 varied the calcium toner of Lithol Red treatment in order to try to obtain better strength in rubber. DUP050315560 jr7 3 Reslurrying the toner pulp and putting it thru the colloid mill, filtering and again washing well was slightly better than control. Making the slurry alkaline had no advantages. Reslurrying the pulp by means of the colloid mill and extend ing with blane fixe had a decided increase in strength over control. Blanc fixe and D.G.S. gave a still better improvement but was infer ior to CS-7665, a regular extended Lithol Red. A sample (446-23C) previously prepared by loiajer calcium than the regular CS-7801 gave a very good test in rubber. It was approx imately equal to CS-7665 in strength and blue. Series 446-32 prepared the sodium, barium, ealcium and stron tium toner from the azo-sulphite derivative of Red for Lake c. The soda salt was not completely converted to the soluble azo sulphite compound even on prolonged heating at a high temperature. The yields of the toners were considerably low. and the resulting products were all inferior to the control color 284-39 both in rubouts and lightfastness. Series 446-53-34 prepared RT-359-D (pigment Rubine Gr) both for a Service to Research request and to try the conversion to the azo-sulphite compound. A sample of toner pulp was turned over to the Sales Service Department. The remainder of the pulp was treated with sodium bi sulphite. It went completely into solution without heating or al kali. Id did not salt out as an azo-sulphite derivative formation. % DUP050315561 PIUMBHT COLOR RESEARCH REPORT CALCIUM DUOL RT-265-D SUBMITTED BY APPROVED BY: RILE: SUeBS DATE: PEBRUARY-I935 INTRODUCTION 3?ive 'batches of RT-265-D were made in the Semi-Works to pro duee light yellow shading material suitable for blending with plant sub standard stock. SUMMARY & CONCLUSIONS All but one batch made were of the type desired and were con sumed in a mix with a blue tinted plant batch. Standard development volume was used instead of the reduced volume recently employed and, with one exception, all were struck at 200F. One batch struck at a boil did not show the usual increase in depth. EXPERIMENTAL DETAILS N.B. #441, p. 60 0.4 mol charges were made. 2X SW-5833. Development and strike temperature was 200E except in SW-6762 which was struck at boil. SW-6742 - s.light; vs clean; vs strong; vs yel. & clean SW-6748 - s.light; vs yel & cl; s.strong; s.yel & clean SW-6753 - light; vs clean; vs wk; s.yellow SW-6759 - light; vs weak; vs wk; vs blue SW-6762 - light; s.yellow; OK; s.yel & clean DUP050315562 PIGMBET COLOR RESEARCH REPORT YELLOW LAKE YP-324-D jjr-s? SUBMITTED BTl APPROVED BY: PILE: HAEQA YEESOW DATE: FEBRUARY-1935 IKTROBUCTIOE A run of this color was made in the Semi-Works to build up stock. Twelve batches totalling 1447# were made using the CS-7657 procedure standardized September, 1934. SUMMARY & GOECLUSIQ38S All batches were normal with the exception of the first batch which was slightly dark. All were greener in masstone and cleaner or greener in tint than standard. One exception was a batch in which the resinate was added after the coupling instead of before as is the usual procedure. This was lighter and cleaner than standard, but of about equal redness. Strength and opacity were equal to standard. To correct the depth obtained on the first batch an increase in the amount of hydrochloric acid from 3.25 to 5# per 0.25 mol was made. In order to anticipate any loss in strength in processing,two batches were made with a lower amount of resinate - a 15^ excess over t the original standard instead of the 30% now used. These showed little, if any, difference in strength and no further reduction was made. An old lot of acetoacetanilide (Lot 16) was chiefly used with satisfactory results. This lot contains some insoluble residue. A lot of better material (#564) gave a lighter greener product. A shipment of MHPT, Lot 405. which gave a clearer diazo showed no improvement in the finished color. Actually these batches were slightly darker and greener than usual. A reduction in excess nitrite showed no improvement. DUP05031 5563 EXPERIMENTAL DETAILS N.B. 430 PS > a1 fi o' ft A a p A S3 c A a Aa? p as at at U ' H O Ao H A O j- rH p u P St P u8 p 03 3 a 03 c* 3 e e o4 > p o> > >>> > 3 Si bO r > $ S3 S3 S3 S3 Si o U bO * b*fl 1 03 > S3 S3 fait Pp P -c * p p G W i-4 Si rH rH rH bO o bO O Si Si r--t =e bO c9 <6 > bO "8 O >m O > l> > Si + Cfi I t<| pj > co| s Si u Si Jm +9 p p up (Q CD > > > }> O > JO ! o 3 T3 P O P HCO +O. oX tmo CIoco 3fi P P P Si S Si P bQ Sh + bO Si bO * P CQ 3 >> > H Po o <8 S d 3 Si fi n bO p |JH o Si a u bO to a b- Ea P G 53 Si bJJ i-t o G E i PP u u P bO b0 bO 4S a A* 4$J Sj 3 P fpi Tfi rH M iH rH P 8P Si P tfbO rH Si p bO P s *3 8 c8 Si S 3A fi Si fibO P -P rl rH +9 Si bO bO Si uat rH bO rH bO bO rl > n .> rH > <0 > g o M o in -p o b0 p P e P o +> H CO ^ TO CO rH P rH P P AD P aS PO O a o S -p CO a o o Si Si XJ o o o p P * ^4* pp Si fi H bO H CO T3 p * o T3 O P <P p rl P rl fi to CO <N? fi 4fc + CO CO J *P TJ <o Si Si *rJ rH P P rH JH Po H *iH +9 g a *rt H PP o 35 3 CO rH O P P m3 to O i-3 p P "3 o +9 CO fi A Eh CL. g g W TO n uP Si J 33 &= *rl * to id o o <c S< sp3 OO PP TO TO o Si t* Si l S & CO Si 1 c TO H TO p xt TO p P p T> P *H P CO H ^ a % 49 irt o Si U P S p P g CO P AXt A OPq a. >i bO > Si P^x A AS P X rl X S3 O S3 05 + ^ o a o P to o% <0 to X X p to X CO a> CN? rH i/3 in pCO eC*"- o> Ok o to P to to P to 30 W 10 to <0 to J, o a i tesi Si H P 1 O 1 co 1 O 00 30 1 & J & Ss J S-Xc- =&-& 1 flits J & J3 fe rao H CQ CO a co to n to tn co o rH cvz rH -X y JA < & X bo ca rH CQ H Jrf H AS O M O bO Sp -rl m TO 5> o <C o <H o < o o r> fi fi fi fi fi fi o o o 00 o o fi o OOP o -fi fi fi o ^ 'J jj a w Si op o <o to CO o> 33 e- O o> w 55 CO to > <o tto 00 o to CO e-- to 30 o Osk. to o 35 to **H 35 o rH 35 o CO -O 03 00 to 01 05 to : r' S, * .si DUP05031 5564 PIGMENT COLCR RESEARCH REPORT RUBBER COLORS - RED FOR LAKE G ------------- ----------------------------------------------- , *- * SUBMITTED BY* APPROVED BY* FILEi EE&-SfflKE"7f" DATE: FEBRUARY-!935 INTRODUCTION Work on the Red for Lake C Rubber Colors problem was continued during this month with a study of the barium salt. Some attention was also given to matching Goodrich's Pigment 1442. SUMMARY & CONCLUSIONS Barium: It had previously been found that the barium toner pre pared from Du Font's Lithosol Red CLE paste was substantially equal to RT-313-D standard in rubber dispersion and that both of these dry colors were about 30# weaker than a latex dispersion of the barium toner. During this month it was found that by extending the toner with barium sulphate, and by treating with diglycol stearate in addi tion, a decided improvement in rubber dispersion was obtained. The product, CS-7836. shows about a 20# color advantage in rubber over RT-313-D and is only about 15# weaker than the latex dispersion of the barium toner. A sample was submitted to the Du Pont Rubber Lab oratory for their evaluation. Calcium: Our own tests on CS-7804 and CS-78C5, the calcium toner and the 70# lake respectively, had demonstrated that they were yellower and somewhat dirtier in tint and worse in lightfastness than Orange YO-D (latex dispersion of the sodium salt). Similar results were obtained with these samples at the Du Pont Rubber Laboratory. On the basis of these tests it was decided to abandon work on the calcium toner as well as the strontium, which is bluer than Orange YO-D, as possible substitutes for Orange YO-D. The study of the cal cium toner was continued at the recommendation of the Du Pont Rubber Laboratory. Apparently an error was made either in the testing or in the interpretation of the tests which were nade by the Rubber Laboratory on the original calcium toner prepared by Mr. Siegel. It is believed that a satisfactory tinctorial match with superior properties can be obtained by a mix of Permanent Orange R (CS-7808) and Barium Red for Lake C. Goodrich Pigment #1442: This product (C#37144) was analyzed and found to contain chlorine, barium, zinc and chromium, indicating the possible presence of a mixture of Red for Lake C, barium or so dium salt and zinc chromate yellow. Chemical spot tests showed also the probable presence of a mixture of Red for Lake C and Lithol Red. A fair match was obtained by the use of a mix cf CS-7805 (70# Calcium Red for Lake C on blanc fixe) and CS-7836 (68# barium Red for Lake C on blanc fixe). However, this mix was inferior in lightfastness. This problem of matching C#37144 will be taken over by the Du Pont Rubber Laboratory. EXPERIMENTAL DETAILS Notebook #284 DUP050315565 J3sr 2 Series 284-45 was a raw material test on a new supply of Lithosol Red (JIM. paste, D#1923. The new shipment, D#1923, was found to be satisfactory and was adopted as laboratory standard for future work. Series 284-46 compared the addition of slurried blanc fixe with co-precipitation of barium sulphate and the barium toner; also studied the effect of adding diglycol stearate. Extending with slurried blanc fixe had no apparent advantage over precipitating barium sulphate during the strike. D.G.S. in addition too precipitated barium sulphate gave an improvement in rub ber dispersion. Series 284-47 studied the effect of adding blanc fixe to the strontium toner; D.G.S. was also tried. Blanc fixe improved the dispersion of the strontium toner. D.G.S. gave no apparent improvement in dispersion, but altered the shade. Series 284-48 was the preparation of a large sample of the extended""barium Red for Lake C. The sample was assigned CS-7836 and was submitted to the Du Pont Rubber Laboratory for evaluation. Series 284-49 was an attempt to match Goodrich's Pigment 1442 (C#37144J7 By analysis, C#37144 contains barium, chlorine, 2inc and chro mium, indicating the probable presence of a mixture of Red for Lake C, barium or sodium salt, and zinc chromate yellow. Chemical spot tests showed the probable presence of a Lithol Red. A fair match was obtained by a mix of 284-42C3> .{70% Calcium Red for Lake C on blanc fixe) and 284-45D (68% Barium Red for Lake C on blanc fixe). How ever, this mix was inferior in lightfastness. Series 284-50 was a study of the comparative lightfastness of the barium, calcium, strontium toners of Red for Lake C and Orange YO-D (latex dispersion of soda salt). The following was found to be the order of decreasing light fastness of the above toners when dispersed in rubber {Du Pont com pound ). 1. Barium toner 2. Strontium toner; Orange YO-D 3. Calcium toner DUP050315566 PIGMENT COLOR RESEARCH REPORT <ri LITHOSOL RED SB (CALCIUM) j SUBMITTED BY! APPROVED BY: ' ~ -v ^ PILES MS6t -T*BBRSLATE: FEBRUARY-1935 INTRODUCTION The first shipment, lot 1- of Lithosol Red 2B soda salt paste was received from the Dupont Dyeworks and was tested in formula CS-7745 * Samples of sub-standard dye, which were manufactured in the course of development, were also tested in various formulas, with the object of finding a possible outlet for these dyes. Some work was also done on the Calcium Lithosol Red 2B as a rubber color. SUMMARY & CONCLUSIONS Lot 1 of Lithosol Red 2b was tested in CS-7745 and found to be satisfactory. It tested slightly light and flat, about 5$ weak and OK in lacquer bleed versus CS-7745. For the information of the Development Department- it was found that a 50$ reduction in the volume of strike gave a slight improve ment in brightness of masstone and in strength. Development at 90cC gave a practical check to the standard procedure (100cC). Apparent ly, strontium nitrate may be substituted for strontium chloride with out affecting the tinctorial properties. During the development of the coupling formula for Lithosol Red 2B soda salt paste, considerable material was manufactured which was substandard in quality. This material was sorted into three groups, and samples were submitted to Newaik for tests in various formulas in order to find some possible outlet. The dyes were converted into cal cium toners, with and without styrax, barium toners and dry disper sible eolors, and were evaluated by varnish rubouts, casein brushouts, lacquer and rubber grinds. The results showed that only one sample gave non-bleeding lac quer colors, and that all three samples of dyes (D#1879. D#1880, D#1881) were rather poor tinctorialiy according to rubouts and lacquer grinds. In rubber, all three dye samples were non-migrating but somewhat dirty compared with standard dye. However, representatives of the Dupont Rubber Laboratory agreed that these dyes could be gradually consumed in future shipments. 7$ dry dispersible eolors (on barytes-hydrate base}' were prepared from the above samples of dye and. tested by casein brushouts. D#1880 gave the weakest and dirtiest color; D#1879 and D#1381. although dirty compared with standard, were considered satisfactory by Mr. O.F. Lane of Sales Promotion from the standpoint of color, strength and fadeotneter tests. Accordingly, a sample (C3-7776) was prepared from a mix of D#1879 and 3>j?1881. A sample of the calcium toner pulp from these dyes was also prepared and submitted to the Niagara Wallpaper Company &B SS-7S47. s-r. - i . , .jvnijfSfeSSk DUP050315567 2. I;, . fvv * wi- i.'t. . "t<:: 4 |' ,"3 Rubber testa showed that a laboratory toner (447-10B) and two semi-works batches (SW-6827 and SW-6834), all made on formula CS-7745 and from lot 1 dye, were substantially equal in dispersion to the la tex dispersed color. Extending with blanc fixe and diglycol stear ate, of course, showed no improvement in dispersion. Some considera tion will be given to the question of employing extenders because of the crocking tendencies of the toner. EXEERIMgETTAL BETA IIS JT.B. #447 Series 447-1, 2. 3, 4. 5, 6, 7, 9 were evaluationsof the sub standard dye paste samples B#T8797 D#1880 and D#1881. These dyes represented substandard soda salt pastes of Lithosol Red 2B, which were manufactured by the DuPont Dyeworks in the course of the dev elopment of the coupling formula. The above dyes were tested as calcium toners with and without styrax, barium toners and as dry dispersible colors. The results demonstrated that only one sample, D#1881, gave colors which were substantially non-bleeding in lacquer, and that all three samples, including D#1831, were unsatisfactory because of poor tinctorial results according to rubout tests and lacquer grinds. . In rubber all three dye samples gave calcium toners which were non-migrating and satisfactory in lightfastness, but somewhat dirtier than standard. It was agreed, however, by representatives from the Du Pont Rubber laboratory that these dyes could be consumed in future shipments. Dry dispersible colors {1% calcium lakes on barytes-hydrate) were prepared from the above dyes and tested by casein brushouts: D#1880 gave a very weak, dirty color; D#1879 & D#1881 were considered satisfactory from the standpoint of color, strength, and fadeometer tests by Mr. O.F. Lane of Sales Promotion. Accordingly, a CS sample (CS-7776) was prepared from a mix of D#18?9 and D#1881 and will be submitted to customer. A sample of a calcium toner pulp from the mix of D#1879 and D#1881 was also prepared and submitted to Niagara Wallpaper Company as CS-7847. geries 447-8 was a raw material test of the first shipment (lot 1") of Lithosol Red 23 paste. Also some studies were carried out for the information of the Development Department, The raw material test was satisfactory versus CS-7745. bei ng very slightly light and dull, and about 5% weak. It was found that cutting the volume of strike in two gave slightly superior results; also that development at 90C was practically without effect tinctorially. Series 447-10 were rubber tests of the CS-7745 product to deter mine ease of dispersion. It was found that the toner dispersed practically as well aa the latex dispersed color, and that extension with blanc fixe gave no advantage. Two semi-works runs, 6827 and 6834, were substantial checks to the laboratory toner in rubber. DUP050315568 PIGMENT COLOR RESEARCH REPORT SUBMITTED BY APPROVED BY: # LITHOSOL RED 2BT0RER, RT-7745D -v 'V p il e : msc-r-reiEKis DATE: FEBRUARY -193 5 INTRODUCTION Semi-Work3 studies on this new toner were started during the month for the purpose of checking laboratory variables and setting up a satisfactory manufacturing formulation. A total of fourteen "batches were made; grind results are available on nine of these. Vat conjrrol results are reported on the remaining five batches. ork on this toner will be continued on receipt of a new lot of Lithosol Red 2B dye. SUMMARY & CONCLUSIONS Lithosol Red 2B, lot 1 was used in all of the semi-works batches. This batch of dye tested somewhat light and weak. A check run on standard (CS-7745) formula gave a product which was light and muddy in masstone and blue and weak in tint, compared to the laboratory standard. The lacquer test was similar tinctorially, and was satisfactory in overstripe bleed. Reduction in dye volume to 50, 37-1/2 and 25$ of the formula vol ume apparently gave improved results. The 50$ reduction gave a d arker and brighter masstone than the control run; however, this batch was muddy and blue compared with the laboratory standard. Further reduc tions improved brightness of masstone; the batch using the lowest vol ume has not yet been ground out, and the results reported are controls. The 50$ volume wa3 adopted as standard practice for all the following runs. TP In order to improve brightness, the strike temperature was re duced from 105 to 75 i?. Altho bright on control, this batch was some what brown when ground; contamination may have caused part of this change. A check run was somewhat better tinctorially, the grind being ws dark, s.brown; ws weak; s.blue compared with the laboratory stan dard, CS-7745. Both batches were browner, bluer, and weaker when ground out than indicated on control. A double size batch (45 lbs.) made by the same procedure resulted in a very satisfactory batch, which was v.s.lights ws flat; ws weak; v.s.blue compared with CS-7745. The lacquer test gave dark, v.s.bright results. The reduction in strike temperature was used in all subsequent batches. Omitting the Para Soap gave a lighter, brighter, weaker, yellower product. Increasing the amount of Para soap had approximately the same effect. Striking with calcium chloride only, omitting the strontium chloride, was tried. The fresh vat control was excellent tinctorial ly; an experiment is now in progress to determine the hygroscopicity of this batch, and its effect on the tinctorial properties. Variations in amount of acetic acid over a fairly wide range show no marked changes, on control results. DUP050315569 C 2 Development at 180F instead of a boil gave a lighter, bright er. yellower product on control. It appears that low strike temperatures and low dye volume give the brightest results. Cheek runs to determine consistency of the low er volume will be made when a new lot of dye is received. Fone of the variables so far studied have given a control of depth of masstone. *-r ' 'if'.-,** -7 . DUP050315570 CO l toI tn <bDC p* Si s> i 3 iH ~f*fe H C0O3 2I0 cm & N rH t 3 CM CM i ca CM pH I SC A CM 49 o M 02 CM CM N H 8t rH f CM n CM CM sH CM H ix, PJ >> &o in t- CO o cr H o 3 in e& CiO o CO ** T3 P to 3 rt CO > <a %4 CO i cej s o roH .a > Of CM U a N H1 \rH1 CO H CM \a 3) CO n u P n0* cs> N rH1 CO CO CO CO CM CM \ PM H* H |I 3 o> X) I H a s s rt O O fV as aVi .a jj J; oE-Pf Cm 00 XS > P r 3 S -H 3 Tf J4 to > 4 >O > 3 a to > M U TO3S 3 rH n td o >t p c rH HI rH S* H rH TJ a nn O CO xs xs p 43 p 43 p J5 1453 hO to to to H H rl H 3 U Sh & JO S3 44 _n j 0 to 44 >u xs to .X >U xs <n c3 T3 to 44 > (4 TJ to > rH H > B > Jd A4 ># > >P ISn is f p OB 8 0 rH H h rH JO n P n > > tn >>>> g 5. al <H Cm t ^Oj'-wp*v *>go> c Sa '-m1 a Io ID h >Q H O a 11 at O a Vi m XI > *8 v rH Vh S'* O CB P P N *rf W JS P NH raOH in o n oCC--IO Mo Xo3 bOO. Ts3 Po3 or3H3 rH ttoo Ch c!3 PXPo< <3 stok g to a10 c--o** on i3 s: H TP3 g OPSO3 toC(o0M T5 xs u to uH * Hpr3Ba H O 'S3O r.m^. um PPoXi pO n faStofrc H0ig50l05 MJOC o P -bsHO i> i*1 JH4 pUto 'i OH^** a i O O43 'sd>&^ rnH 1--o1 +> +> r3H 4* 1 1PeCt03oPOXo1M50- iCCiHnrnoC3HtHQMDo^. -X 4O3 rO>H o3 a xi *H PPOXi rOH a n C0<M00 &eo oto 4o3 13 n 4JOE43 Voi aori rr. -3od f--^ce>jr +Po>.^Ote-PPoi tPoti. x e> CC<1Ooi ^^o--!nfe* aOPtfi 0tCt1o-O3 " d Cu3L. =H rr o4434 03-t 44o34 PBs n CO s <o rt0Ho> CCtoMO 0ttC0>3M CCOO St o t0o0 s <o Oin GtoO ImH CtoO Vm`5 *.'V- ' r 1--'v.- -' `rfAs-.S *..:* DUP050315571  *H JH 9 3 -C"4 o cm t to <H (ft 4> to a #v in in H4 2* & 1 -q to H a> H P CO &a * N H 1 cm CM 1b CM \ rH 1 CM CM 9s 4b & \ rH rH t1 CO X CM rH r>H I CO CM c9$ Sf CM s a Ji Eh 3 O to ^ P rH H b m ^P C- P b *H l h to o jq pbi p rH Ob bp p 03 Po o c 4* O M to P< 5to rH 0 CQ a; $2 po SIS 5 3J 3 H ,Q rl b 5 *> * sa u 43 H* n t to a* 0 H -Q O 0 rH rO > P > <rt b 43 > V CQ P rH g.s O b o 09 * o S3 rl 2X bo 1 CQ rH rH b 4o3 Q CM CO p g co 3 H* J *H rH ^03 iSf3 03 O rH ,M b O P o o43 m in CO to <o Vi u 43 45 CM CM \ Sft rH 1 rH 1 43 to o t> 1ft CM a rH rH > OO rH rH rH rH s b > as 12 $b > g rH rH b* > p > P *rl rH * P <! P 0 O r-j PO < o rH O S3? b rH CM CO to _ 41? K-- Om 45 O b in ao vO 0 rH 43 > P 4: to rl i> to H rH *B< O O rH iH=*b 43 to 0 J. -Oa %tfT p Pi P C X < b 0-1 CM O CO to ki m O 43 p O43 co to X to 4>a > p p^ -0 43 to H H$ b b a. o o rH *0 > P rf q p *tH Ox 1o X rH b* N -P CO ai rl ClO -rl O &s P -> CO *rl S at o o rH -p aj 43 O ttoo CO to ft Q b CM \ rH t CM tb rH >* b 44 1 b P to C o u p b pp )& rl P rH b 43 > r^ >% to 73 O P <r> 0 P* Pt rH o to o X b rH CM --' to - to ft rX rH ob o43 CM Q0 to ^7 * S bo <M b* b b 5 to S3 Pi rH 0 P C rl to p p p b 43 o p jO tt S p o >1 b to n rH bH P*4 pO 35 % 'S . M \-jiR ' V ' ^ .3 a" ' ft'' DUPO 50315572 PIGMENT COLOR RESEARCH REPORT SUBMITTED BY* APPROVED BY* PARA CHLOR ORTHO NITRO ANILINE G --y'-g* v -v f' V` ' t b '3 p il e s ligac^aaaaas. DATE: PEBRUARY-1935 INTRODUCTION A new sample of para-chlor-ortho-nitranlline from the Du Pont Dyeworks was tested in formula 307-41C (coupled with beta naphthol) . Samples of the coupled product (CS-7837) were submitted to Du Pont Philadelphia and Parlin for durability tests. SUMMARY & CONCLUSIONS The new sample (d #1927) of para-ehlor-ortho-nitraniline was a composite of plant (Du Pont Dyeworks) crude charges. It was tested in: formula 307-41C (coupling Y/ith beta naphthol) and found to be prac tically equal to the original sample, D#1850. *V-;. *; ; i A large sample of the coupled product was prepared and assigned CS-7837. Samples were submitted to Du Pont Philadelphia and Parlin for Dulux and Duco durability testing purposes. EXPERIMENTAL DETAILS N.B. #307 `&y Series 307-44 was a test of a sample (our D#1927) of para-ehlor ortho-nitraniline in formula 307-41C. This sample was a composite of plant (Du Pont Dyeworks) crude charges 7, 8 & 9. ' May'-i D#1927 gave a product (coupled with beta-naphthol) which was a fair match to that prepared from the original material, D#1850. y. Series 507-45 was the preparation of a CS sample for Dulux and My Duco durability testing purposes. This sample was assigned CS-7837 and was submitted tc Du Pont Philadelphia and Parlin for durability tests. DUP050315573 PIGMENT COLOR RESEARCH REPORT sr-6f PEACOCK BLUE LAKES, SUBMITTED BY: APPROVED BYs B1-I51-D AND BL-7427-D a > 2, / V PILE: MXSC-r--BHIE-LAKES DATE: FEBRUARY-1935 INTRODUCTION Laboratory work on these lakes have been discontinued for the tiine being. Plant production on B1-151-D consisted of three batches made in an effort to secure green and clean material for shading. A batch of very strong BL-7427-D was required to use in shading a Pea cock Blue Lake to match BL-7573-D for Chicago stock thus necessitating the manufacture of the batch made during this month. SUMMARY & CONCLUSIONS V Humidified drying of the BL-151-D lakes was continued using 140J. 40$ humidity for + 30 hours as the standard method of drying. *; Both rubout and ink mill"grinds on the three batches of BL-151-D made during the month were unsatisfactory, all being red and dirty versus the standard. These results may be accounted for by the fact that Lithosol Brilliant Blue E Lot 4 was used as the dye rather than Alpha- zurine Special as used in the standard formula. Yields on these batches were quite high, averaging 127$ of estimate which is due to an excess of moisture present which may be dried out by a longer time of drying, or by spreading the press cake thinner on the drying pans. The grind results on the BL-7427-D are not available as yet, but a rubout on a lump sample gave v.s. weak, red and dirty results. Lithosol Brilliant Blue E, Lot 4, was also used in this lake as com pared with Lot 1 as used in previous manufacture of this color, which was strong,''red and v.s. dirty. Difference in yield may not be consi dered as the reason for the difference in strength, as the average lump yields of the three previous batches (37930, 38140, 38156) checked within two pounds of the lump yield of the present batch (42217). Thus the poor quality of the dye can be the only reason for the unsatisfac tory weak results secured, especially in view of the fact that a 5$ increase of dye was used over the previous batches in manufacturing this lake. Tabulations on rubout and ink mill results on BL-151-D will be found in Tables I and II respectively. '4 DUP050315574 EXPERIMENTAL DETAILS H .B . 318, page 84 T3 & Q rifIH5 t-H r-1 CQi 03 U >P CQ 03 P3O O3S3 Tg3 >* >> >* t ptH. t t! 8 d TJ 'd t0- 0 u pm Md Md s 0 ts 0 S3 OK! O i3 O 43 I I I GO t. Ctf 1 M | 03 &i CeO*i .(* Q0 d0P* d o^ -oo>3< H O *H r- -H iH a: XuJ H Tu3 J CoO o lO 03 CO d rH p o O O rt d Tt* >-* W CO CO CO p o CO *3* *4 =ffe c0o2 O AO m AO r1 H ft CO X g % ff d 00 43 CQ CS2 &* fr- P to o t- rl H H CO d< OS* ($D4 4J rOH *iHJ 0h 5 W o Mo +>> o o _Oa 'HT_aO +tVi tJ>+fa PC U f>fl fa TO "-dH fa -TH3 > > 05 u fa 8 a> fa "8 fa e ni 0ft H rm-- rH CQ 00 P403 T0O ft p 5 >1 5 *4H3 PS3 & p< pc0 Ht, oEs d >>d >d > 0pp p J^h** *dH*-r Jd*HJh >Tk1 *THO, o 5o >* pJh dH * TO *-. 8 CO > o02 * in 02 xCQ S fr* X MM ft=*CfQc a 9 CO i a j Sofc- -tdn* o fOed % ra ! a &0 U >P o OH mo >> d 1 aJ 2 43 H o c o l > o 1 f > m ^u O T3 pH O aS - s s 5 O o O in in > 3 L, CO H ? o 42 u c* Tt< 03 rH 'd O O C\2 CO -* s So *d p -I H tf oOm _c O H m t. ^ d 43 03 CO O 02r-i CO pH rH O frA *d p S3 bO 9sS s pH P P O o O in 02U H o rt K^ CO 0$ m CO O bO rH rH rH H UP So --1 d pH E-* ^ bO t> TO Sd H in CO OJ P i--4 1 b<o O E> t> o *4 - r-i rH iH *3 CO rH Ti* d4 DUP050315575 PIGMENT COLOR RESEARCH REPORT DISPERSED CLAY COLORS, GE-363-D AKD GE-364-D SUBMITTED B! appr o ved by IHTRODUCT 3E03ST PILE* WATER COLttnr DATE: EEBRUARY-1935 A Semi-Works study of the GE-363-D formula was carried on this month to eliminate the oliveness and dirtiness obtained in brusihout tests of practically all material made in the plant. Eight batches were made. Two batches of GE-364-D were made in the Semi Works to check the formula and one batch was then made in the Plant. SUMMARY & OOHCLUSIOHS In the Semi Works, standard GE-363-D formula gave the very yel low tint regularly obtained in both laboratory and plant. An adjust ment of the ratio of Victoria Green and Auramine brought the tint fairly close but did not correct the oliveness in full strength brushout. A light clean blue product was obtained by substituting Thioflavine TCT for Auramine. This type is very suitable for shading the yellow substandard material. An approximate match for standard was made by replacement of about 30^ of the Auramine. An exact match could be obtained by use of proper ratio of dyes. The raw material cost on this formulation is about ^0.45 per 100# higher than is an Auramine formula adjusted to equal shade. This is not believed to be an objection. Light stability is slightly inferior to standard. Slurrying the clay with a hand paddle instead of with a Light ning Mixer had no effect on rubout tests but showed a loss in bright ness on full strength brushout. In each case the clay was screened. .A Semi Works control run on GE-364-D (Victoria Green alone) was lighter and cleaner than standard. The clay was pulped with an Elec tric mixer. A batch made by dispersing the Clay by running it thru a centri fugal pulp which is the usual plant practice was darker and dirtier than control although still a close match to standard. It is- not definitely established whether the difference obtained above is due to poorer dispersion of the clay obtained with the cen trifugal pump or to greater opportunity for contamination. A similar improvement was obtained in a plant batch of GE-364D in which the clay was dispersed with a Lightning mixer. Both rubout and brushout showed greater cleanliness. The procedure is however too laborious for regular operation. DUP050315576 d * -2 73 Q 0 5 8 T3 bo s cd rf 43 iH *2 >> 0 d S3 --f < O . 5ho C3 -8 ite od O_ rH 8 P * *C* oW >1 &o TS & H fr- 0 rH om <0 (H * 0 -* -h >* 0o " Ml fc. p p cs H fik rH s > o d 8 m H H iH 8o8O rH 8 l* 24 p o 3> O rH 8 t <^j *> ^ 8 ffl 3 t j rl PH > U 1 r-i HJJtl 33 O H > O *t Pa Ml id Ml o id rH a SS e* bO c rH iH rl >* 8 iH 8 O '73 to to >* U P U >> rH P 9 p0 5 O S3 T5 H 2 O rH b H rH u H rH rH H 8 8 p 9-H iH > 0 H 0 rH >2 * 4$ 8 o . >> a > > > > o p S* at s* p P a 44 E* x > s= '0 {0U 2 P a id 54 d m > tfc o O O > U 44 P flJ rH O tQ O i & & rH O rH O rH 8 1 rH rH rH T5 8I iH >> rH 8 rH rH 0 3f >. 8 >> 0 aj -H rH a> 3 ~ O g-3 * CQ T3 c 25 rl d ns o (3 03 d co +* 0 03 CO 1 p S3 O S3 1 T3 -H 8 da Pp < OJ o dX Q l CO X to H CO S3 42 'd lb rl J* 8 Sto o p 8 44 &0 J82 o p4b3O <g S r*f S 0 * 44 Sh 3 txO d 8 d 43 d ri rH rt rH d *8 rH 0 rH 3 u taO >> rl > b* CSj Cm O3 H O 8 5-* 1 1 w % rH 10 rH 10 o o t CNJ o C\? o rH rH O rl S3 H -p o8 4-3 WH5 O8 P d dp 3 43 P CO -Prt SOU t d *s3 e0 vO oo H d H 7J 3 H| t s] Oi 8H s o 1 p I Cs? 0) oa * H* * S-* 8 o u! rH H H rH H H H rH PrO H <5 0 >1 'ite 08 'a <8 8 d Sh H8 i ro 3s 1 to r^* -H s 5- 0 i> O o> >- o o 0 0 O 0 H* rH 0 O 23 8 ^P | 0 0 0 0 0 0 08 CUrH >9 r-t O 3 d,<e H 0 P4 A) to o> f j3 O1 P 8 1 4 o 3 *8 to o ra t* -Q 8 e- 3 U <o ec; 0 i s 03 3 44 a to k M O 1 4 8 1 po 8 ^2 10 O 10 0 8 0 tn 0 03 0 1 CO P la n t L o t 41824 - Standard fo rm u la . C lay pulped w ith L ig h tn in m ixe r in s te a d o f being ru n th ru c e n tr ifu g a l pump as in usudl plant p ra ctice . Rubout - vs lig h t (r re d ; s .y e llo w ; vs s t r ; s .c le a n brushout - ~ '-"^vp DUP050315577 PIGMENT COLOR RESEARCH REPORT CHROME GREENS - STRONG TYPE CS-7192-7193 SUBMITTED BY: APPROVED BY* t oh 0#' PILE* -CHROME GRESES' DATE* PEBRUARY-1935 INTRODUCTION Further study of this formula was made in the Semi Works. Six hatches of the lighter shade were made. Three hatches of CS-7192 were struck in the plant, two of which were split and part brought to CS-7193 depth. SUMMARY & CONCLUSIONS Two control runs on CS-7192 showed some variation from the con trol biade last month in the Semi Works, one being olive and the other too bluish in masstone. Reduction of the time of strike from 30 to 5 minutes gave bright products on duplicate runs while an increase in time to 2 hours result ed in a very olive product. Apparently, best results are obtained with most consistency when the yellow is struck and treated *with the restraining agent as rapidly as possible. Such rapid addition of the bichromate requires very good agitation. An increase in strike volume from 500 to 650 gallons per 0.5 mol charge gave a weaker product with a darker masstone. This is not in accordance with previous experience as the higher volume was uBed in. the plant to obtain the opposite effect. Use of the lower strike volume gave promising results in the plant, with one batch finishing close to standard, CS-7192. A check run was somewhat olive. Good agitation was obtained by careful adjust ment of the belts. If this type of agitation can be maintained, it is believed that a rapid s trike such as tried in the Semi Works would be of benefit in the plant. Lowering the strike temperature from 90 to 50F gave a slightly chalky masstone and a very yellow clean undertone and tint. DUP050315578 S. EXPERIMENTAL DETAILS SEMI WORKS N.B. 436, p,14 Lot Variation Mass. Und. Str. Tint SW-6756 6760 6750 6766 6799 6772 Check SW-6731 (CS-7192) olive s .ygrl* s.dirty SW-6731 & 6756 s.dark & s .clean bluish Check SW-6731 except increase strike vol. from s.yellow & clean 500 to 650 gallons Check SW-6731 but add bi-- s .blue s .blue chromate in 5 min. in & brt. & clean stead of 30 minutes. Check SW-6766 s.blue ft & brt. Check SW-6731 but add bichromate in 2 hours v.olive dirty instead of 30 minutes vvs str s.yiel. & clean vs str vs blue clean vs wk clean s.wk OK vs blue & clean s.blue & clean PLANT N.B. 437, p.10 ,41755 41913 41947 GS-7192 - Check 41610 exeept reduce strike vol. from 5000 to 4000 gals. (Std. volume). Check 41755 except that strike temperature was 50 instead of 90F Check 41755 41914 41971 CS-7193. Part of 41913. Added lead tannate and more blue CS-7193. Part of 41947. Added lead tannate and more blue vs dark vvs drty vs str vs blue (Bldg.10) s .clean dark s.blue vs light s.yel. olive dark s.blue vvs dark vs blue vs olive dirty Note: All plant "batches were made in Vat 260 (special baffles) with agitation maintained at 18 R.p.M. DUP050315579 PIGMENT COLOR RESEARCH REPORT SUBMITTED BY APPROVED BY: STROMS MILORI GREEN CS-7834 SLOANS BLABOR GREEN OS-7858 vf PIES: QBROffi-GREENS DATE: FEBRUARY-1935 INTRODUCTION Two additional "batches of the strong Milori Green of the CS7728 type were laade. These were shaded somewhat darker than the "batch made in December. es#7834 was given to this shade. One hatch was used in a mix to prepare an offering for Sloane Blabon C#36876. SUMMARY & CONCLUSIONS Both plant hatches represented an improvement over the first plant trial of this type of green. The better results are due to con trol of the acidity after the strike. The first "batch in which a fair ly large increase (33$) in nitric acid was used was too blue and chalky hut by reducing the final addition of acid to but 10^ extra as compared to CS-7728, a very satisfactory product was obtained. This batch when blended with regular Milori Green and a alight amount of Chrome Orange gave a close match to the sloane Blabon stand ard. An offering was submitted as CS-7838. EXPERIMENTAL DETAILS N.B. #437, p. 132 41797 - Yellow as in 41072 (Dee. Report) except increase final nitric acid from 30 to 40# Blue used = 150# vs C-36876 - vs dark blue; blue & clean 41843 - Yellow as in 41072 except final nitric acid was 33#. vs C-36876 - ws dark & cl; vs blue; s.strong; clean Exp. 363-36 (CS-7838)- 2# mix of 41843, G-317-D, G-318-D, Y0-263-D. vs C#36876 - vs light; vs clean; OK; vs yel. & cl. Linoleum grind & light stability - close DUP050315580 SUBMITTED BY: APPROVED BYt JS'-^ 7rt PIGMENT COLOR RESEARCH REPORT RAW MATERIAL TESTING } v PILE* RtfV-MSTEftlALS BATE: PEBRUARY-1935 The eight items indicated as unfinished in analysis and test last month, have been satisfactorily reported. This- month 79 shipments of raw material were received and sam pled, and have the following status: 40 tested in the laboratory and found to be satisfactory; 6 OK in the plant; 3 used before test ing; 2 satisfactory when previously tested; 2 awaiting completion of test; 2 awaiting report from the analytical laboratory; 2 handled by the Research Department; and 22 reported without test. RAW MATERIAL SAMPLES ft? There are no samples outstanding from previous reports. Eleven samples were received this month: RMS 1377. Azo Bordeaux #37464 from Rational Aniline - Satisfactory. RMS 1378. Mauve for Lakes. Yellowish from Geigy. Unsatisfactory, too light and weak. RMS 1379. Mauve for Lakes. Yellowish from Geigy. Supplementary to RMS 1378. RMS 1380. Calco lake Bordeaux BxL 90$ from Calco; unsatisfactory, too weak and blue. RMS 1381, Lake Red CR Pulp #282 from Sherwin Williams. Satisfactory. RMS 1382. Lake Red CR Pulp #282 S & W } El 1383. ".*) Unsatisfactory - too muddy and bronzy. RMS 1384. Azo Bordeaux B-26565, from Rational Aniline, Satisfactory. RMS 1385. Lake Red GR Pulp #282. S.W. RMS 1386. * * ** R3 1387 " " Supplementary to RMSs 1381-82-83. C: DUP050315581 PIGMENT COLOR RESEARCH REPORT -7 SUBMITTED BY: & APPROVED BY: SEMI WORKS PRODUCTION Itl FILE: -OR-SeeDATE: FEBRUARY-1935 INTRODUCTION 89 batches of 20 different colors were made during February . These included chiefly 8 batches of RT-7745-D? 12 batches of YP-324D; 8 batches of GE-363-D} 13 batches of chrome yellow and 24 batches of chrome greens of various types. SUMMARY RT-265-D, Calcium Duol - One batch was made completing the series begun last month, RT-219-D, Maroon Toner - One batch was made to fill an order from Pariin. RT-354-D, CS-7685, Maroon Toner - One batch was made in a further trial of the improved maroon formula designed to permit finer grinding. RT-359-D, Pigment Rubine - One batch was made in an attempt to produce yellow tint material. RT-7745-D. Perm. Red 2B - Eight batches were made in development of this new type of color. YP-324-B, Hansa Yellow Lake - Twelve batches were made for pro duction. Y-315-D. Primrose Yellow - Seven batches were made in continuation of this development problem. Y-359-D, Med. Yellow - Six batches were made in further study of this process. YL-64-D, Tartrazine Lake - One batch was made to fill an order for this color. G-389-D and G-7694-D, Lithtfast Green - Fourteen batches of this color were made in the study being made of this formula. G-7192-D- Strong Meadows Green - Three batches were made con cluding for the present work on the stabilization of this color. G-317-D, CS-7764. Lightfast Milori Green - Seven batches were made in development of this type of green. GT-66-P, PTA Pulp - One batch was made to study pulverization of the pulp. GT-68-P. Pigment Green - Three batches were made concluding the series begun last month. GE-363-D Dispersed Clay Color. Eight batches were made to im prove cleanliness and brightness of the product. GX-7826 to 7829-D - One batch of each of these extended greens was made to obtain standards of these types. 11 mixes and 1 grind were made for the plant in the research semi-works during February. Grinding CP Green Batche s 1 Charge 741-s lbs 6 Mixing Red Toners PTA Toners Toner Lake CP Green 5 751-s 710 1 2 *1 n 104 336 3 755-s 817 DUP050315582 -71 as as cn o cn CSS OS Os a3 <3 <1 to vC tD vC tC to tC to 09 Co a OC CC CD a 3 oc a <1 --s < <3 <1 *3 " 3 ^3 *3 -0 -0 OS cn as Os Os cn OS cn <1 os tn 4 CO co X o to cc -3 cn cn 4 CO to X o tC cc <3 cn cn 4s* CO to M o <o CD -o Os cn 4* CO to K fe fe HC fe Cl K fe fe 1 1 1 1 1 CO <3 CO 3 CO CO 1 Os H os CD O M H CO 4 1 T to 4 to <o 4 -3 y. Os CO fe ] fe fe fe fe fe fe / K fe K fe : fe Oc c fe Q fe K K tc Q Q CP k ; O a O Q >< P fe ns MS i Hi *n Hi ^3 *-3 1 tFl *-3 3 co CO 1 <n a*. <1 3 es co co -0 41 CO i CO cn CO X cn O. CO O. Os X CO CO CO cn Os CO cn CO Os as H Os H* CO to 3 20 tc to --3 o OC tC tc cn w tO 20 to ul- o> <> to CD CD to <p cn cn cn 4 44 tr fe 4 ns CO fe OS 4s* to to 4* to CO cn 1 fe fe ** fe fe M3 fe i fe fe fe fe fe fe fe *T* fe fe fe a fe fe fe O te X 3 x X XX XX x X H H H + M H M to to 3 CO CO CO 3 CO to to CO CO 3 CO to 20 X CO OS tc CO to CO CO Os to CO to Os CO -* to co O tn cn M CJI CO tC 00 O 4 cn 4* cn CO 09 o *o cn <J oc o 4^ to 9 cn -O 00 to Jg to <3 cn O CD os o 1 OS -0 sX X XX XX X H H b-> H* J-4 H* to X <5 CO CO CO <3 CO oc X X CO 20 3 CO CO to W to 4 O CO 3 cn cc cn D CO tO O to o to CO Ov tc to to CO 4 Os o to to M oCO CD to CO to M os CO >-> to CO cn cn M M 4:* cn 4 CO o cn 4> CD o o o a* <s c/3 C+* M fe fe CO a PT* s* M fe o CO fST XXX to to to tp tC cc oc to to to to tc O o O cc -3 4s* 4 tc to to os cn 4 OC cn o 3 3 V CO X <3 co 4 <3 to cn o CO CO cn o co cn tC to to o to to 3 tc M -3 a: Os X CO 00 cn CO <3 MM M O H to to to O O O to CO o O o 03 to -3 4^ o MM O to o to to o 4 o as to o CO o O *-<J H* CD M (X #10 BUXCDINQ PRODUCTION REPORT FOR FEBRUARY 1935 OS os o> OS OS as as cn os CD CO OQ a fe co CD CD 3 CO CO CO to to to to to to to to to to M to M o to CO -3 Os cn ip CO to o tD fe M H* H* X O o O o o o o o o O o to os cn 4* co to H- O o fe -3 Os cn 4 CO CO X O to fe K <p 3 <p W G2 Q 99 S3 Mi P fe < !=2 2 o a Q o Q *< CP w Q a 03 o K 1 CO CO -3 I CO co .fe fe HX*XX t *T3 ted X ted MJ CO -3 CO 1 CO CO c CO -3 Os to 1 CO H* J-* CO Os S3 CD H 03 3 Cfs CO Os H* CO CO -3 CO -3 **3 -3 -3 -3 M CO co cn CD M Os CO LO cn CO to cn -3 CO 4* to 4*> *S* 4^ to 1 -3 20 3 4" 4s* as cr> os CO fe 4* cn 4* to S 33 4> Os CO fe 20 CD 20 fe CD to to -3 4 -3 to 4 as co to P -3 SP 4 O as to tD to 4 fe fe fea a f cn fe fe i cn *TJ tt fe cn tC -3 OS in fe fe 1 afe fcj fe JL fe fe fe fe 1 fe fe fe *2 fe fe fe fe fe fe fe fe fe OH* H* I-* H* MH M H* to CO -3 tD cn CO cn to to CO cn --3 3 to f- 4s W H* H CO to o CD CO cn CO to 20 to VP* 4=* to to $ cn O cn O cn 3 --3 O to to -3 cn to 4 to CD CO to H* X 3 co CD CO 20 cn cn fe to 4 S3 fe o sg o o Os o CO c+ hi GO O ?r M >-* HH I-* H M K* s CO cn -3 < to co 4^ to w 4* cn S tO hrf to 20 H* cc cn to 4 CO CO to to CO 20 to to CO tc 4* 4= to 4 O 4 -3 4 -3 to to -3 to o CO CO CO to K M M -3 co CO -3 CO to to cn o cn M to MJ H P* oa Pc* H to cc to to to o O O <D O tc to to -3 to o O CD O * o -5 M O M o cn co o *- o: to to oc tc to a o CC a a to cn 3 to tc oc 4* o 4 o CO 3 33 H* o o cc cn o o o 4 X so to tD o -3 -3 o o o Os O CO o M feto O O CD o to o CO feVO to as tD CO w- H CD H* P- os Cs as os t25 s 4 <o 4 cc s 3 4 a*. 4 cn 4 4 4 CO 99 4 to 4 H* 4 o co to CO CO CD CO 3 CO as CO cn to 4 CD CO CO o PO fe so fe W 3 so fe fe fe so fe *-< SO fe fe SO w i-3 1 CO HI CO CO X X 1 CO CO CO *-3 V ? H 1 Os fe3 cc to a 3 X to 3 3 CD 3 CD X to 3 3 3 as o -3 3 to cn to 3 cn cn CD VO 3 VO cn M CD fe 3 i o PO c+ 4 4 4 to to to 4 to to to 4 fe cn fe fe cn fe tD 00 a cn fe fe 3 Os cn pa> i fe fe fe tr4 fe fe fe fe fe fe fe fe H- o> o os 5 to to CC cn 4 O CO tn 4 <n WccCoJulOi^vWwWwW'oWcMo CoO 3H* ttOo M O' Q9* CO Os| 4 n't w a oi w m oM W *Ptnf to to 4 CC 4 CC CP- t> CD to w w w to os cn to w to W -O t> O CD w tOoD I- H- K XX COIt-OKOKMCWOtf P0u0i0<90 o os X BCOO VO O cn 4 .:* H^} 4 < v tDio O e$ o oif*00tn CmO <n tn OS'<S2> ?*r * K DUP050315583 3. StJMARY OP #10 BLDG. PRODUCTION REPORT FOR P5BRU4RY- 1955 Goda Wo. lbs. Batches Struck lbs. Packed % Yield RT-265-D 1 RT-219-J) 1 RT-354-D 1 ST-359-31 1 RT-7745-D 8 YP-324-D IS Y-315-S 7 Y-359-U 3 &r> YL-64-D G-389-B 1 S G-7192- 3 G-7694-B 9 G-317-B 7 GT-66-P 1 GT-S8-P 2 GS-363-B 8 GX-7825-D GZ-7827-D S s GY-7828-D 2 GX-7829-D J3 236 28 140 60 189 1480 244 192 20 175 501 350 1231 11 57 780 141 137 195 150 234 29 144 62 195 1455 270 186 15 165 518 305 1217 11 59 710 115 116 170 137 100.8 103,5 102.8 103.5 103,2 98,3 110.0 96,4 94,3 103,5 87. 1 98,9 100,0 103*6 91,1 81.0 84.7 87*1 91.2 81 6677 6451 96,8 7 s/ mm 7m. DUP050315584 MATERIAL -JRABSBEERED EORIBB 2EBRUARY 1935 4* RESEARCH SEMI-"WORKS IiOt mi 3951 3964 3977 3981 3939 3968 3969 3970 3971 3972 3996 3963 CR-200 1 1 1 1 1 1 1 % 1 1 1 25 125 Color Coda RT-365-0 RT-359-D 9 m * RT-265-D 9 9 m RT-126-P RL-400-D 3935 4001 3985 3986 3987 3988 3992 3993 3994 3995 3 3 Y-359-D * 10 10 YP-*324-D 10 n 10 9 10 n 10 * 10 * 10 * 3991 11 Y1-64-D 3962 4 0-7192 D 3965 4 m 3966 4 n 3967 4 n 3982 4 * 3983 4 9 3984 4 m 3978 3979 .3980 132 6-317-2) 132 m 132 4008 4 0-389-1) 3998 6 GB-364-D 3989 3990 108 0T-68-P 108 9 4010 127 BT-96-D 3997 5 B-66-B 3973 5 B-63-D 3974 5 * 3975 5 91 3976 4009 5 5 * * lbs* Grour ~55 2' 60 2 75 2 58 2 158 2 24 2 241 2 246 2 242 2 243 2 243 2 5#100g 1 96 1 Cost Uait 65.28 132.49 49*39 311.72 45*72 302 486 123 124 124 121 117: 123 122 123 2 2 2 2 2 2 2 2 2 2 8.92 133*56 15 1 34*66 167 2 162 2 168 2 169 2 169 2 187 2 166 2 10*35 1256 526 448 2 2 2 11.31 378 2 12*09 187 2 9.57 25#100# 1 25#100# 1 64.21 36 2 347.95 165 2 123 2 122 2 114 2 126 2 375 2 27.45 26.19 Total Coat =^g^g5W|ffa.r- DUP050315585 s HSCAPITULATIOS Colors transferred from Semi-Works to Plant daring February, 1935* Toners Yellows Greens Bines "KB" lakes Bp * BL* PTA Toners Toner Pulps PTA Toner pulps 1665# 788 3796 1025 187 977 111 36 SO ___ 5 Total 8640# 7^ 7 DUP050315586 AS QT KAROS 1935 RKSSAR6H SOa-VORKS #10 B U .t *l S S3 2 8 tt) i n ft A** OH (S 04> *???? eoooo Htf* iQ m n i !I C >9 Q0 6t*- oToiOl0l!o Ok CO Ok It* nnnwn Heo 1 ft 5 X o o H W <o tit cina l< e~ <0 a tatooi to S3 SI 5 l: I Ht> no 3"SS3Si eo 9 OI f_5$ AI A f_t_ AI mt iatt>mto o HAk AAk eoeaeo Hit leg lAi S$8 rt _n ??A KSS to J&g Ok M_ f to 1 a t t k ao-* ft 3$* sOB h 6. Ok ll 5 2 S tit m 8 a3 qn oi> oi ?s KO 1tf) *S 5 aE i ?Sr J5jg rKt?$p>- * .> >% ftij -A DUP050315587