Document 4oB98rw3pgyNxvXXYkmgVGmp

PIGMENT COLOR RESEARCH REPORT'S AUGUST - 1935 I- PIGMENT GREER B Pigment Green B Lake for Paper GL-407-D (EJH) Pigment Green B Pulp GT-68-P (EJH) II- LITHOL REDS Calcium lithol (PLP) ......... ......................................... Calcium Lithol Toner RT-379-D (EJH) .................. Barium Lithol RT-364-D (ADR) ................................. III- CHROME YELLOWS & ORANGES Study of Light Chrome Yellow (SCH) .......... Medium Yellows - Y-299-D, Y-359-D (JDM) ......... Primrose Yellow K-7888 (July) (JIM) .................. " * " (Aug.) " .................. Excelsior Yellow Y-7903-D (JDM) ......................... Metal Protective Pigments (SCH) ......................... IV - IRON BLUE Study of High Copperas Excess on B-63-D (HCM) V - PHYSICAL PROPERTIES OP PIGMENTS Dry Pinenea3 of Pigments (RKH, RED) ........... .. VI - VAT DYES POR PIGMENTS Vat Dye Pigments (SWR) ..................*................. .. * " (AS) .............................................. VII- PIGMENT-OIL MIXTURES Plushed Colors (AJS) ................................................... Lithol Red in Castor Oil (HBB) ............................ VIII- PHOSPHOCTJNGSTIC ACID PIGMENTS Blue Toner K-7983 (EJH) ............................................ IX - MISC. ORGANIC PIGMENTS a) Para Red - Blue Shade (JVS) ............................. b) Toluidine Red RT-232-D (ADR) .................. c) DuoIs Barium Duol Toner RT-283-D (EJH) ........... Med. Calcium Duol Toner RT-265-D (EJH) d) NBS Maroons Mareon Toner RT-219-D (AAB) ...................... w* " (ADR) .................. e) Alkali Blue (AAB & SWR) ..................................... fj Maroon Toner RT-347-D (ADR) ...................... g) Pigment Rubine G (CKB) ...................... ................. Dye RT-359-D (ADR) .................. h) Particle Size and Texture (HEB, SCH) ......... i) Misc. Lakes Misc. Lakes & Toners (AS) .................. .. Pyrazolone Dyes (AAB) ................................... Peacock Blue Lake- Development of High Pinish(CKB) Permanent Peacock Blue Lake - Comparison with FugitiveType (CKB) 1-3 4 5-7 8 9 10-11 12-14 15 16 17 18 19 20-22 23-25 26 27-31 32-33 34 35-36 37 38-39 40-41 42-44 45-46 47-49 50 51-54 55 56 57-59 60-61 62-64 65-68 DUP050316038 2 IS - MISC. ORGASTIC PIGMBHTS (Cent.) i) Mis. Lake3 (cont.) ^IfSrathreno Pink SV Lake (CKB) .............. Sulfegene Color Lakes (CKB) ......................... (Jraan Lakes from Acid Tripiienylmethand Byes (CKB) 2 - SEMI-WORKS PRCmJOTIOir (HA) ................................................ -'''BgHNty' -- 69-70 71-72 73-74 75-80 "lifer- DUP050316039 PI^MBBT COLOR BgSgARgB REPORT PIGMENT SHSBH B LAES JOE PAPER SI-407-B j>_sr- 2-6 ? t SUBMITTED UY| tAFIIEt M13G. LAKES" APPROVE BYl DATE: AUGUST - 1935 INTRODUCTION A total of a 1even batches have been made in the Semi-Works on this Pigment Green 3 Lake for paper. Variations introduced have been, in the main, changes in the milling of the slurry, and grinding studies on the dry color* The K- sample, K-7906, has been set up as a standard and coded GL-407-D. SUMMARY & C0HCLP3I0B3 The first series of batohes was made using material amounts as in the K-7906 formulation. The slurry was then split into five parts and the following variations introduced! one, two and three passes through the Charlotte colloid mill and one and two passes through the 8 inoh mikro-pulverizer These five batohes were each split into two parts and grinding studies made. Tests made on these batches gave weak results versus the pulp control. On investigating the materials used, it was found that the rosin size used was material made by the Hercules Company whereas all laboratory work was carried out using rosin size from the Kalbfieisch Corporation. The second series of batches was made on the K-7906 formulation using rosin size from the Kalbflelsoh Corporation of the same type as that used In the laboratory work* The slurry mixture was divided into two parts and one part passed through the Charlotte mill three times and the other passed onee through the 8 inoh Hikropulverizer. fine and coarse grinding studies .wore also made on eaeh of these two batches. All of these dry colors* including both types of grinding gave sub stantially the same results in paper as secured with the pulp control (all run on equal toner basis). A mix of the coarsely ground material from these two batohes was made and set up as K-7906. On receipt of an order for 250 lbs* of this Figment Green 3 lake from the Philadelphia Dyestuffs Sales two more large size batches were made to oheck the K-7906 formula* One pass through the Charlotte mill together with eoarse grinding of the lump material have been in corporated in the standard formula as giving satisfactory results* Both of these batohes were 15# stronger and yellower and cleaner than GT-68-F lot 41673. the pulp paper standard, and were satisfactory ver-' sus K-7906. A mix of these two batohes testing 3# strong and OK shade versus K-7906 was shipped to fill this 250 lb. order. Yields on these two large batches were low, averaging 88# of estimate. This loss of yield was expected as water cannot be used to wash out equipment after oolloid milling because of the fact that this diluted material disperses very poorly after drying. In tthe Semi-works compressed & was used to blow out the lines thus saving as much yield as possible, but this may not be feasible In the plant. It maybe DUP050316040 z mentioned here that no water should he used at any time in this for mula* The use of a small amount of rosin size when breaking down the Pigment (Jreen pulp gives a smooth* uniform slurry and no water need be used. The remainder of the rosin size is then added slowly in order to secure the smoothest slurry possible. Production is tabulated in Table I and mixes in Table II. DUP050316041 7105 c o irs * g rin d , 7106 *c o st s grind -- s tr,jr*l,e ls a a sot up as K DUP050316042 7*19, 7244 3jC str-OK -- shipped to PIGMENT COLOR HESSARCH REPORT PIGMENT GREEN B PULP GT-68P SUBMITTED BYl APPROVED BY: INTRODUCTION <2*3. ?/ PILE* PIGMENT BHMMI B DATEt AUGUST - 1935 Beoause of difficulty in securing satisfactory quality and yield on this color which has recently "been encountered By the plant* super vision of production on this color has been transferred back to the Development Section* Production for the month is quite low; due to plant shut-down only two batches being made on neither of which are results available. SUMMARY A CONCLUSIONS The last batch made under plant supervision during July (44581) has been accepted and shipped for paper. The two batches made during the month will be reported in the September report. Shipments made during August are tabulated in Table X. TABLE I GT-68-P. shipped during August Lot 44581 Rubber Test vs Lot 15926 QE Paper Test vvaa LLoott441L887733 OS by Paper Lab* Remarks and Disposition OK for paper. Consumed in shipmsnt for papsrr 1401# at 25.4# * 366# dry DUP050316043 PlgBBHT COLOR HgggiBeS REPORT CALCIUK LITHOL SX- > 7/ SUBMITTED BY: APPROVED BY: FILE: MTHOEB DATI AUGUST- 1935 IHTRODPCTIOH Study of tlie T.O.B. regular - Beta naphthol + Schaeffer salt formula has "been continued with emphasis on improvements in brightness of masstone and softness of texture. SUMMARY ASP COHCLUSIOBS Material made on the TOB regular - Beta naphthol + Schaeffer- salt formula had a tendency to be slightly brownish in masstone. Brightness was slightly improved by a modification (increase in para soap 472-17D) as summarized in the July report. The product thus ob tained is equal in brightness to RT-379-D. Check runs made on 472-1735 during this month demonstrated the good duplieability of this formula. It seemed that further improvements in brightness could be obtained by improved coupling conditions. Studies were made along these lines by: 1) Decrease in BIf. A slight decrease (3.3#} resulted in a slight gain in brightness which seemed to be due to elimination of free BH in the final product. 2} Variations in alkalinity of coupling: slight decrease pro ducing a larger excess of BEET after coupling and resulting in loss of brightness. Slight increase resulting in a slight increase in bright ness with a slight increase in depth and softness of texture. 3) Variation in amount of ammonium chloride: Increase producing incomplete coupling (larger excess diazo). Decrease gradually produc ing more complete coupling and slight increase in brightness of mass- tone'. The optimum conditions were found with 5.4 gr. ammonium chlor ide for 0.2 mol coupling, this being 45# of the original amount used. Further decrease and emitting of ammonium chloride was found to be detrimental to depth of masstone and softness of texture. 4) Variation in alkalinity of coupling (studied on formula with reduced ammonium chloride), 5$ and 10# increase increasing final pH from 7.4 to 9- 9.8 is detrimental to depth of masstone and strength. 5) Increase in alkalinity during development seemed to have a brightening effect upon mas3tone but this modification had a tendency to impair the stability 'Sr this formula. Improvements in softness of texture Slight improvements in texture were already obtained by increase in para soap, reduction in ammonium chloride and increased alkalinity. A series varying the temperature of development was run. Lower temper atures resulted in harder products, higher temperature gave softer texture. This aeries was ground in rubber and 3howed plainly the im provement in dispersion. At a development temperature of 90C (70cC being standard procedure) a product was obtained which was found equal DUP050316044 .2 in dispersion to RL-408-D and of satisfactory shade (s.blue and v.s. clean)* Rubouta on the series with increased development temperature showed an increase in lightness of masstone* It seems advisable to develop two types of toners* one for the printing ink and one for the rubber trade. Variations in the amount of Schaeffer salt Increase in Schaeffer salt from 1 gr. - 1,6 gr. per 0.2 mol coupling resulted in inorease in depth with a tendency towards a brown ish cast in the masstone and an inorease in blueness of undertone and tint. Increase to 1.9 gr. resulted in a duller lighter masstone with blue undertone. Material made on a formula combining the favorable modifications of these studies resulted in a product which is slight ly superior in brightness with equal depth to RT-379-D, and of equal strength, bluer shade and tint and of softer texture. The TOB + TOOT buffered alkaline coupling (461-23A) still gives a si. brighter and stronger product but of inferior texture. Further work The coupling conditions have been favourably adjusted by recent modifications. A possibility of further improvement in brightness seems to be rather dependent upofc modifications in the development procedure. Studies should be made such as rate of addition of calcium chloride, influence of variation in temperature, volume, heating rate, effect of quenching etc. BXPBRIHBRTAL DBTAIIB Notebook 472, page 48-68. Series 472-18. The purpose of this experiment was to test the duplica'bility or a slightly improved formula (increased para soap 472-173)) as well as to test a new sample of Schaeffer salt. The dupllcabillty seemed satisfactory. The material made with the new sample of Schaeffers salt was also satisfactory. Series 472-19. Decrease of Beta naphthol in`"472-173). Reduction in BN seemed to be desirable as a considerably large exoeas can be noted after coupling* A 3.3# reduction produced a more balanced coupling (i.e. endpoint v.s. excess BN and v.s, exoeas Diazo). This reduction produced a very slight improvement in brightness of masstone, while decrease of 6.6# and 9.9# gave no further Improvements but were detrimental to the strength, yield and texture. 472-20. Study variation in alkalinity of coupling (decrease and increase of NaOH in BN Solution). This study was based on 472-19D for mula with 3.3# reduction in BN. The control checked very closely. 5# decrease in NaOH resulted in a dull changeable masstone, this appar ently being due to incomplete coupling (BN in end pradjust). 5 and 10# increases in NaOH resulted in slight Increases in darkness and bright ness of masstone. The final pH was very little influenoed, this being due to the buffer action of ammonium chloride. 472-21. Decrease in ammonium chloride. Study was based on 472-SOD. (Formula 10# increase in NaOH). Control gave a substantial check. 20# and 40# damgease seemed to give a more complete coupling DU P050316045 3 *7 resulting gradually In an Increase In brightness of ragstone and v.s. increase In strength. 472-23. Study on TOB Schaeffer salt coupling. Based on 21A formula except replacing BH with Schaeffer salt. The coupling pro duct is a soluble dye which precipitates only partly as a calcium, bar ium or lead toner. The barium toner is about equal in depth to the cal cium toner but brighter, of softer texture and less soluble, however, decidedly hard versus TOB Hi material. The superiority of the barium toner gave catise to an experiment 472-23A-2 of striking with barium chloride after crarheriug calcium chloride to precipitate some Schaeffer Balt dye as a barium salt. This resulted however in a much lighter mas stone. The lead toner is of maroon shade and extremely hard. 472-23. Decrease and omitting ammonium chloride. 472-21 series showed advantage in a 40# decrease. Further decrease of 55# and 70# as well as omitting BH4C1 were studied. Study baaed on 21a formula. Control checked very closely. 55# reduction resulted in a v.s* darker brighter masstone with OK strength and tint. 70# reduction as well as omitting ammonium chloride resulted in lighter masstone and harder tex ture . 472-24. Variation in alkalinity of coupling. Based on 472-23B (formulation with reduced BH*G1) a) decrease in sodium hydroxide (BIT Solution) by 10#. Bo appre ciable influence (t v s duller masstone). b) increase in BaOH by 5# obtaining final pH 9,2 C) " * 10# * 9.8 Both -{,) and c) resulted in higher masstone and yellower tint. 10# in crease is detrimental to strength* (apparently formation of calcium hydrate acting as extender). 472-25. Variation in alkalinity of development. Adding increas ing amounts of HaOK as in 472-24 series after strike. Slight improve ment was obtained with addition of HaOH corresponding to 5# increase. This affects, however, the stability of the formula as seen in later studies. 472-26. Increase temperature of davalopmentrloss in depth of masstone increased softness of texture. 472-27-28. Study increase in Schaeffer salts based on 472-25 formula (addition of sodium hydroxide after.strike). These series were not conclusive as luplicablllty was unsatisfactory in the oase of the eontrols. 472-39. Inerease in Schaeffer salt. Series .1 gr., 1, 3 to 1.6 Increase in depth of masstone - v.sl. tendenoy to a brownish oast, increase in blueness of shade and tint. Increase to 1.9 - dullenss of masstone. DU P050316046 PTflWBTirg COLOR RESEARCH REPORT CALCIUM LITHOL TfljgBR RT-379-D SUBMITTED BY: APPROVED 3Y: INTRODUOTIQg FILE: LITHOLS" DATS: AUGUST- 1935 Production on this color during the month was low due to the plant shut-down, only one batch, being trade. Also Included in this report was one batch outstanding from last month. Light, blue nnH weak material was the type product desired to be used for shading purposes. SUMMARY & C0BCLU3I0B3 Both of the batches reported were made using the old standard formula -7365 except for a 20# cut in development volume and a 4# and a 9# cut in the caustic soda in the coupling respectively. The result ant coupling pH tests were on the first batch 11.6 and on the second 10.8. neither of these batches gave quite the results desired as both were yellower than standard, but the fact that the second batch was weak and slightly blue versus the first indicates ^hat variations are being made in the right direction. ' A satisfactory 1677 lb. mix has been made consuming most of current production. Production results are tabulated in Table I and mix result 3 in Table II. SXPERIMSBTAL BBTAILS .3. 433, page 188 TABES I Batch TGB T.at Amt `r T-379-D Production for August BO- Coup- Grind Rubouts vs. TCBW -7 ling RT-379-D Std. Yld Lot Amt in BH pg Mass. Draw. Str. Tint Sst 44713 149 fSj* 39 25# 75# 11.6 lt,fl. vs yel. OK yel 410# 413# weak Modified std. for mula. 44759 k * 71 10.8 It. vs bl. s.wk v.s. 410# 388# yel as above except cut in 7 TABES II RT-379-D Mixes Results VS, RT-379-D 8td. Total Bispo- LotCompositionMass. Draw. str. Tint Wt. sltion TB553 44429 301#, 44480 310# vrs It ws yel 2# wk v.s. 1677# OK (RT-7594) 3817 45#, & flat yel. 43358 181#, 3892 165# 44759. 380#, 3894 160#, Blanc Fixe 135# DUP050316047 Picanntg COLOR HESEARCH REPORT BARIUM LITHOL RT-364-D S~- -3 7 3> SUBMITTED BYl APPROVED BYl IHTRODUCTIQg A ' PILE* LITHOESf DATE* AUOUST-1935 Production of this lithol during July and August consisted of the manufacture of four batches on the standard formula except for the lover amount of Para Soap now being employed. amntABT COHCLPSIOHB One batch was OK to ship without blending. The others ranged from t .s . dark to dark. The extra depth may have been caused by use of the Steam Dryer on this series. This has been found to darken the color more in drying than the Hurricane or p & s Dryerg. All were slightly yellow ii^tint as usual. BXPBRIMBHTAI. DETAILS H.B. 385, p. 152 Batch size and amount of Para Soap were varied. r 44699 - 1 mol - 24# Para Soap - ws dk & brt; vs yel; vs str; s.yel. 44737 - 1 * 34 * a.4k, brt; " ws str; * 44949 -0,75 *18 * vs dk, s.brt; s.str.yel; s.str"* 44997 - * * 18 " dark; vs cl yel; s.str; s.yellow DUP050316048 PIQMBBT COLOR RESEARCH REPORT STUDY OP LIGHT YELLOW J.SUBMITTED BY* APPROVED BYs HrmoBucyioar PILE j DATE* AUGUST -1955 Laboratory work on the Y-180-D and Y-309 D processes being studied in the semi-works has been resumed by the laboratory. The new Y-309-D (CS-7903) seems unsatisfactory from the standpoint of ink properties, such as livering and high body. The new Y-180-D was in addition poor in lithographic breakdown. A large 3ize laboratory standard will be set up on these products as soon as satisfactory material is obtained. A laboratory standard has been prepared for the primrose yellow now active In the development section. SUMMARY ASP CONCLUSIOH The Y-180-D process has been returned to the laboratory for further study because of the unsatisfactory lithographic breakdown resistance shown by the semi-works material. A laboratory investiga- r tion indicates that the lithographic breakdown resistance is influended greatly by the pH after the alum- bicarbonate treatment. It appears that in both the new Y-309-D and Y-180-D processes a low pH after the alum - bicarbonate treatment results in a softer body and better resistance to livering with low resistance to lithographic breakdown. With a high pH a heavy body, livering, and better resistance to lithographic breakdown is obtained* To obtain good resistance to lithographic breakdown a large amount of alum and bicarbonate seems desirable* A number of experiments mads during the past and previous months indicate that the replacement of the alum by tltanyl sulphate or by zirconium sulphate results in a pigment with lithographic breakdown resistance equal to that which can be obtained with^alum and without the heavy body and livering tendencies introduced by alum. Because of the poor ink properties of both the revised Y-180-D and Y-309-D it will probably be necessary to replace the alum with titany1 sulphate to obtain a product satisfactory in al respects. A study is being made of the use of tltanyl sulphate and on completion of the work a large laboratory sample will be prepared as a temporary standard. A number of strikes were made on t he primrose yellow prooess now being studied in the semi-works to obtain a large size K sample* The revised process appears to give a product approximately equal tinctorially to the prooess first developed but with slightly worse lightfastness. This is possibly caused by the use of citrio acid in the revised process but part of the difficulty may be due to the Higher temperatures encountered during the 3unmex months* A 1100 gram sample has been set up as a temporary working standard. EXPERIMENTAL DETAILS See Notebook #452, 481 Expt. 453-83, Preparation of a large size sample of improved Y-202-D to check 453-21B. DUP050316049 "rjsamf .2 Results. Material did not Check 453-2IB, discarded. Bxiot. 453-81, 89. Study of pH after alum 'bicarbonate treatment Of CS-7903^ Results. High pH6,l vs. 5,5 seems to give a slightly redder product. A high pH seems to give better lithographic breakdown resist ance . Expt 453-78. Preparation of a large laboratory sample of CS-7903. Results. Material did not eheak previous strikes, discarded. Bxptg. 453-93. Effect of using less alum in CS-7903. Results. Decreasing the alum seemed to have little effect. Bxpts. 453-90, 481-4,6. Effect of replacing alum with varying amounts of titanyl sulphate and zirconium sulphate. Results. A small amount of titanyl sulphate or zirconium sul phate seems equivalent to a much larger amount of alum in obtaining products of good ink properties and good lithographic breakdown. Bxpts. 453-77. 80. 86, 94. Preparation of a large sample of Primrose Yellow as a temporary laboratory standard. Results. A large size sample has been set up as a temporary standard. Exnta. 79. 84. 87. Preparation of a laboratory sample of Y-180-D prepared bythe revised process. Results. Ink mill grinds indicated that only the material finished at pH 6.1 was satisfactory in lithographia breakdown. SW-7207 prepared by the new process was unsatisfactory in lithographic break down. Samples were unsatisfactory for use as a standard. ' Ex p . 481-1. Effect of using Turkey Red Oil* oltrio aeid and an increased amount of alum in the revised Y-180-D. Results. Use of an increased amount of alum seemed to result in slightly better resistance to lithographic breakdown, Bxpt. 481-2. Effect of final pH on lithographic breakdown. Results. A higher pH ^pre better lithographic breakdown. DUP050316050 HBDIUM YBLLQWS - Y-299-D, Y359D SUBMITTED BYt C|. APPROVED BTt JIIB - CTTROVR-YBUiOff DATE: AUGUST-1935 IUTRCDUCTIOU A study Is being conducted, in the semi-works on the development of a lead nitrate formula for Y-299-D. The starting point of the study was the Y-359-D formula* consisting of running lead nitrate liquor into a dilute solution of sodium chromate* The main varia tions have been in acidity and temperature of strike. The operating variables for Y-359-D are also being studied in the semi-woSks, and in the plant as production permits. SUMMARY AHD COHCLUSIOUB Eleven one tenth mol batches of Y-299-D were struck during the month in the semi-works without obtaining the desired tinctorial properties. The results obtained with this size oT batch are appar ently inconclusive as they are not as a rule duplicable on a larger size batch. As a consequence * the semi-works study of. this color will in all probability be carried on at the one-half mol size in the future. The base formula* mentioned in the introduction, gave a batch that was on the strong green dirty side of both Y-299-D and Y-359-D standards with light stability equal to the latter and very slightly better than Y-299-D. The addition of a small amount {five pounds per mol) of oaustio to the chromate gave a dark red dirty strong product against both standards, with worse llghtfaatness. The re duction of the amount of oaustle to three pounds per mol put the oolor back on the green dirty side of Y-299-D with very slightly inferior stability to light. The addition of oaustio after strike to pH 8.5 gave a result similar to the latter, duplicating the re sults obtained on one batch struck on the base formula at an elevated temperature. The addition of oaustio to the ehromate, together with a higher temperature of strike, gave a dark, dirty produet, with slightly inferior lightfastness against the Y-299-D standard. The addition of seven pounds per mol of muriatic acid to the sodium chromate gave a light masstone, and a slightly strong green tint with better stability to light than Y-299-D standard. Against Y-359-D standard, this batch was slightly red, flat, and dirty, with a v.v.s. green tint and v.s. better stability to light. Striking at an elevated temperature with acid in the chromate gave a somewhat similar product, being slightly light and green, with lightfastness equal to Y-299-D, and s$gp$ktly worse than Y-359-D, with a slightly red silky masstone and a red tint against the latter standard* The addition of muriatic acid after strike gave a batch pr&etieally iden tical to the one last mentioned except for being slightly clean with slightly better stability to light than Y-299-D standard. Against Y-359-D, this batch had a red masstone and a v.v.s, clean tint, with equal lightfastness. DUP050316051 2# Some material from the "batch in which the pH was adjusted to 8*5 with caustic soda, waa treated in the laboratory, the pH of dif ferent samples being adjusted in seven steps between 4.6 and 12.0. From a pH of 8.2 to 12.0 the yellow becomes progressively redder, finally approximating YO-27-D depth* The Y-299-D shade evidently falls between a pH of 8.8 and 9,5 although the samples thus treated were dirtier than control or standard. A continuation of this study is planned. One batch of Y-359-D was struak in the semi-works on the baseformula previously mentioned in this report, except that 5 lbs. per mol of sulfuric acid was added after strike. This batch was v.s. red and clean against standard with slightly improved light stability. It is planned to try this variable on a larger size batch to deter mine whether or not the results are duplicable. Three batches were made during the month in the plant on the Y-359-D formula. Two of these were made during the shut down, one of them being for Y-78-P. All of these were struok on the same for mula} namely, 3 lbs, per mol of muriatic aoid, and a 10$ chrome ex cess. By eemi-works rubout, these batches were on the red, clean 3ide of standard. BXEBRISBHTAL DETAILS H.B* 448, pp. 88-93 p, 100 p. 74 H.3. 386i p. 22 DUP050316052  fa 4 A 1 Aa 38 r -< a(aa 1? aa aau a m _ > sUto o . 6lb lb * fa> 8 h A 0 I i 15 ft* ft* i ofa 0 O Ua sis o A fa aa 1 a lb s & 8 0 & lb I 0 MO fa 8 Hl*Uaa. 0o U\aa b aua %am u aa 8 s a gn i8 l8 8u i *. u * g t g8 a g IS A a > '* 82 I A 0 s *& r4 s M O w o * h !fe 8 I8 0 * e f7t <5 A 2 1" 3 a A aa AA A s I A *d 0 8 CM - I s l <aM1t anint H > J> a* m ia 22 < fa* J. CM afa. $ s CM fat 3 lb AA at d> a in nn fa* fa* A A l Jfi*. 6! * t b * a 8 iI lb k 0 A 4 I) O $ a? 1 sA A A at 2a 22 J i A I A AA CM A. AA J.<A AA V7 fa* fa* 2 e 3 P Si 41 fa o 8 O m g < 8A t *.s r-* 8 Mi * % -8 8 IS x Td VMk M o oo 5 1of*t*-_ M ,,0 A0t H Im ' 0 0 fal tg S 5 B niO s t a* MM I g n o tf Sii I5s*0 Is S fa 15-2 5tn *o 1) o -g -g * g *<2 * *J8 a 0 * ?! 5 J5 10 O H + CM IP* O J4 iis 10 %4 HO CM a* a i! o 10 _ CM O f-l g it a fj CO 4 8g T* 8Sofc 5 o| isi! H i i$ e g iinn fHa fa * N0 4 fe *5 o s i i -r s SO a AS go a a -5H a a mn 8 a O -4* a g I * Ag 8s *,4* <1 id o> to CO CO in 10 i m j) CM in JO 4TV JM in M in JO in > m JO N < IA m W CO n \VN < GO CD Cu CO it m H < jtinoi tn jo jmn in JO ccT > GO a o s 11-g 3ica S38 CO CM CO CO fr* CM t* g s t- 3 8 fc S fc Am t <o *5 A DUP050316053 PIMBBT COLOR BBSBABCH REPORT HtmaOSB YBLLQW - 03-7888 SUBMITTED BY* d.juQuOOlUOttT APPROVED BY* A//-/ PILE* gmOMB YBLBOWg DATE: JULY-1935 INTRODUCTION The study of this oolor in the semi-works was resumed this month on a modification of the formula previously used. The former process, after having been found to give instability in the drying operation, was sent back to the research laboratory in May for revision. SUMMARY & CONULOSIONS Three one-tenth mol batches of the color were made on tthe re vised formulation. The changes made in the new formula were as follows* A., sodium Bichromate reduced 2% B. Soda ash after strike reduaed 20# C. Sodium Sulfate after strike omitted. D. Amounts of alum and bicarbonate increased. B. Amount of citric acid doubled. It is probable that C and D are the factors responsible for the im provement noted in the batches made. All three batohss were very close to each other tlnotorially, averaging very slightly green and strong against C3-7888, with somewhat inferior light stability. All were green and strong against Y-305-D standard; lightfastness in this case being superior. Against the laboratory standard for this color, the Semi-works batches were slightly dirty and strong with worse light stability. The instability of this color in drying as formerly noted, has not been observed as yet. It has, however, been &ied under optimum conditions, results on plant drying not being available until next month at which time the effect of increased batch size will be report ed. Ink mill grinds of the final semi-works batch against a labor atory sample and Y-305-D standard are in process. Results on these tests will be available next month. EXPERIMENTAL DETAILS ^ See N.B. 448, pp. 82-84 DUP050316054 PXGIQ2BT COLOR RESEARCH REPORT mimom TBiaoif + k -t b s s -p 77 ,4. SUBMITTED BYi APPROVED BY* PILE* 8BR0ME1 YBLI16WG DATE* ATJQ-UST-1935 INTRODUCTION An increase in size of batch, was attempted on this color during the month, drying the material in the plant to determine its stability under other than the most favorable of drying conditions. The results show that more work is evidently required to overcome the instability noted. 3TTMMART AMD CONCLUSIONS Two batches were made during the month on a half mol charge instead of a one tenth mol size as formerly* The first batoh made with raw water and dried in the plant was red against K-7888 with worse lightfastness* Against the previous one tenth mol control batch it was red with a slightly strong dirty tint and very very slightly superior fastness to light* One pan of press cake dried in the semiworks Proctor and Schwartz dryer was slightly light and green against the plant dried material* This batch was strong, clean and green against Y-305-D standard with slightly better light stability. The next batoh was identical in formulation except for the use of filtered water* This batoh showed a marked instability in drying, being quite red and dirty against K-7888 with worse lightfastnesa . Results will be available next month on a batch in which the bichromate was rsduced five percent, the sodium sulfate increased a like amount and the press cake dried in the plant under controlled conditions of humidity and air speed* EXPERIMSBTAL DETAILS See ff*B* 448, pp* 85-88 DUP050316055 %S~- > 7? /7 picntsarT c o l o r r e s e a r c h r e p o r t SUBMITTED 3Yl APPROVED BYs OTCROBgCTlOB EXCELSIOR YELLOW Y-79Q3-P odtuoti /. - *Ct *pLl~0*/ FILS l mill! IIIHTl DATS: JULY- 1935 Work on this color is being continued in the plant, the ten dency still being to the dark red side of standard. STHIMARY AMD C OE'CLU'SIOBS Three batches were struck during the month on identical formu las, with a cut in bichromate of 5# and a corresponding increase in sodium sulfate over the control batch (43917). These batches were still on the red strong side of standard Y-309-D, and close tinctorially to control, the first batch being slightly green, and the second very, very slightly red* Difficulty Is experienced in vat washing this color as the second and third waters settle very poorly. It was thought that per haps the agitator running with low volume in the vat flocculated the color, preventing settling on the second and third waters. The third batch was washed by flooding the vat and then stirring, without, however, obtaining beneficial results. r The first batch made during the month was compared to the labor atory controls and found to be quite close in shade, very* very Slightly dirty, and somewhat weak. The light stability was dseide'd&y worse', A proportional part laboratory mix was made of the six batches from 43818 to 44262 inclusive, mix was vs dk. against Y-309D std. and 44367* Batch Ob.lect s'td. Check 43917 but 44367 decrease IT-8 5% Y-3Q9-D increase IT-108 5#. Bass. s.red chg. 44473 Check 44367 * t v s dk red 44605 44367 * vs dk red Under* Stx* Tint red a.str, red Light Stability OX s.red strred " red-el red ns worse DUP050316056 Pitagffg COLOR RESEARCH REPORT METAL PROTECTIVE PIQMBNTS SUBMITTED BY* APPROVED BY: INTRODUCTION PIIE t CHROME.ORANGE DATE! AUGUST- 1SB5 During the past month about seventy pounds of samples have been prepared for use in the seaend exposure series planned by the Experimental station. (See letter of S.C.H. to C.K.S. 8/27/35). In addition* four samples of treated talc have been prepared and sent to the Experimental Station. (See letter of S.C.H. to C.K.S. 8/28/35). 3UMM&BY ASP CONCLUSION Samples of basio lead chlor chromate* flake basic lead chromate, basic lead chromate plus talc* and basic lead chlor chromate plus tale were prepared and sent to the Experimental Station. The various pro cesses used have been described in previous reports. A basic lead sulphate chromate was prepared during the past month by striking a mixture of sodium bichromate and sulphuric acid* containing a small amount, of hydrochloric acid* into a hot slightly alkaline slurry of litharge. Two samples were prepared varying slight ly in lead oxide content and were sent to the Experimental Station. Samples of talc mixed with precipitated lead hydroxide and white lead were prepared and sent to the Experimental Station. These samples are to be calcined and tested for possible increased impermeability. EXPERIMENTAL DETAILS See Notebook 421 Bxots. 78.87. Study of calcium chromate and preparation of a sample of calcium chromate for the Experimental Station. Results. The calcium ahrornate prepared has small particles but cementation oocurs on drying. Sample sent to Bxperipjental Station. Sxpts, SO. 8H. 82. 84. Preparation of a basic lead sulphechr ornate for testing at the Experimental Station. Results. Two ten pound samples were prepared and sent to the Experimental Station. Bxnts. S3. 85.86. preparation of additional samples of basic chromates for use at the Experimental station. Bxnt. 88. Preparation of a struck mix of talc and basio lead carbonate and tale plus lead hydroxide. Results. Samples sent to Experimental Station for calcination experiments. DUP050316057 PIQMBBT COLOR RESEARCH REPORT 3TITDY OF Hlffg COPPERAS gyflgfls PIT B-63-D /9 SUBMITTED BY> APPROVED BTi HfTRQDUCTI Qg <7 FIIS| b IOb 'b LUB DATE I AUGUST- 1935 At the request of the Industrial Engineering Division two experiments were made on the B-63-D formula to study the effects of a large copperas excess, the object being to increase the yield with out sacrificing tinctorial properties in lacquer. 3TTMMART & CONCLUSIONS The results from these experiments were inconclusive because the very humid weather affected the drying conditions. All of the samples were high in moisture content, even on prolonged drying, and all were poor in lacquer, and red and weak in tint. It is planned to give this problem further study after better drying condi tions are available. EXPERIMENTAL UBTAT7.3 N.B. 468 % of Filtering Anhyd. Excess property % field Lacquers vs. 488 Copperas vs.control HaO 0.4 mol B-65-D 3td. Readings vs. Std. B-*63-d (rubout) 12A 123 12C 13A 13B 130 Control 5 10 15 20 25 m OK ws better tt tt t s bettor 9.0 6.1 9*0 7*2 5*5 5*0 122.4 red,bronzy-greatly black; ws wlc. 123,8 tt blushed vs an " black { ws weak 123.8 tt ws red " black; vs wk red 128.1 ft tt n an 128.1 tt f - - N 127.8 ft tt " weak " DUP050316058 P13MBHT COLOR RESEARCH REPORT p r y gummas tre p is k b u t s SUBMITTED BY* APPROVED BY: FILBt PHYSICAL STUDIES DATS: AUGUST - 1935 HTPROPPCTIOjET The question of the' fineness of our dry colors in compariao n with competitive types and also its relation to the quality and proper ties of our pigments has Been a subject of dispute for some time. Very little specific data has been accumulated on this problem in the past due to the lack of a satisfactory method of determining fineness and also due to lack of an organized attempt to obtain the necessary data. The advent of the Mioroharmoniaed colors and the belief that some com petitive types are superior to ours, and also specific requests far finer pigments, led to the neoessity for an examination of our colors aid the perfection of a satisfactory method of testing. Considerable work was done during the month to develop a testing method and this was followed by the examination of a number of samples of iron Blues, Chrome Yellows and Red Lakes. SUMMARY & C0HCLP3I0H3 The ideal method of screening or separation into coarse and fine particles of limited sizes to obtain a true picture of their relative amounts is by a dry method. However, it is impossible to make sueh a separation by dry screening on any but the coarsest or largest eereens due to packing or filling of the screens* Other methods of air separa tion have too many practieal objections to make their trial worth while. A wet method of separation by washing the pigment suspended in mineral spirits thru screens of various sizes has worked very satisfac torily on iron Blues, and organic pigments sueh as HE-3B1-B, RL~211-D, RA-85-B BT-100-D. This method has not been satisfactory however with Chrome Yellow Y-318-B due to excessive "balling" of the pigment into aggregates. By careful manipulation and regulation of quantities, a suspension of this pigment in water has given satisfactory cheek results. The mineral spirits method is as follows* A suspension (S - 10 gr. pigment in 200 eo) of the pigment is stirred 10 minutes and then transferred to $* screen, and the screen washed with a fine stream of mineral spirits until no more color passes. The material on the soreen is brushed lightly and the process repeated. The material on the screen is then dried and weighed. A determination on one screen takes 10 - 15 minutes or less depending on the amount retained and requires 500 to 1000 cc of mineral spirits to wash the pigment thru. The solvent is re claimed by filtering and used again* Due to excessive "balling" of Y-318-D in mineral spirits this method gave very inconsistent and illogical results* However, by making a heavy paste of the color in water and then slowly breaking down this paste and washing with 750 oe of water, satisfactory check results were obtained. Many of the samples tested ware from plant or semi-works grinding studies and will not be recorded here. However, the results of the tests DU P050316059 on our standard Iron Blues and several competitive types are Interest ing. They are tabulated below and also shewn on the attached graph. The latter is H||^explanato]ry and shews the relative coarseness of our standard Bides In comparison with the competitives. The following tabla shows the peraent of material held by the size soreen indicated and passed by the next larger size. To obtain the total amount held by any individual soreen it is therefore necess ary to take the sum of the figures for eaeh soreen up to and including the size in question. In the case of B-63-D* lot 3272 for example, the percentage held on 150 mash would be 37.4$. B-104-Q is double pulverifld 3-103-B. Lot 15307 B-63-B ia material pulverized at high spaed by the procedure recently recom mended by the Pulverizing Machinery Oompany. The other blues of our manufacture were ground in the usual way. It will be noted that in general* competit%, blues are finer than ours pulverized is the ordinary way. Vith the wxoeption of the mieroharmonlaed blue* which is in a olaea by itself* Imperial's are the finest* each of the samples being about equal to the high-speeded B-63-B (Lot 15307). percentage Retained(see above) Code Lot or SB 80 meeh IBP mesh 200 mesh 328 meah ' B-6-B 3D-46S46 B-63-B let 3272 B-57-B 30-48810 B-103-B SB-48948 B-104-D SB-47082 B-147-B lot 12673 B-123-B lot 12672 B-68-B lot 13957 46.1 14.6 27.7 27.3 1.7 32.3 10.5 18.0 21.1 22.3 22.1 25.3 15.7 20.5 22.3 26.3 8.7 14.0 13.3 13.4 15.4 12.0 14.3 14.0 Kentucky C#35843 11*9 Kohnetaam G#37831 3.9 United 0#36866 1.4 Imperial A-4356 0#36219 0 X-640 @#37437 0 * A-1S35 @#37208 0 B-63-B lot 153#7 (high speed) .3 B-83-D lot 1282S QP#2607 13*8 * " micro-harmonized, am GP-2606 11.8 16.0 10.7 .9 1.5 3.9 3.9 23.2 .34 11.5 _14.-&-' 11.1 , 7.9 8.3 13.0 7.8 15. .66 18.9 19*5 19.3 16,3 15.6 1.4 DUP050316060 A DU P050316061 ' t Etauwe anm agaaoa antom: ***''* TAT DYE RrajgUBPPa 3UB5ITTED BTj S*^^J^SL: APPROVED BYt IHTROPaCTIOB -----" & 9% 3. 6 PILE: TAB DYED-- DATE: AUGUST 1935. Tbs general problem of evaluating rat dyes for pigment purposes has been held up pending the arrival of samples of various vat dyes which should prove Interesting from the cost standpoint. ?or example it has been found that the starting point in the preparation of Ponsol Blue GZ. is Foneol Blue R. The treatment5 affeot the physiol characthristios 'of the vat dyes and render them suitable for textile dyeing purposes* These treatments stay or may not be necessary ftps the pigment standpoint. Consequently Ponsol Brilliant Blue B sho^M^I^-f^ldcrablzlles#' expensive and any prove to be satisfactory flM^eiMUrpoftes.. 'Ida the ether hand, information from the Byestuffs SSpfiEfmldt.swanw^l years ago indie ated that Pifhsol Blue GZ was d,evelApwt pzlme^^ilr pigment uses.) . An evaluation of Ponsol Blue BP double paste and grains me mad*. was prepared for usAelsionatilnatkien,gH*7P9-7664-,DfrtoOmmPaotcnhsoBlPV-1iBo1le-Dt . AH***&rf, has built up a considerable stock of BP-85-D and the -biggest, purchaser, DuPont Philadelphia, has reformulated thin enamels on the baste (Ur Bp-lBl-D, at our insistence. BP-181-D is about equal In strength but redder in tint than BP*8dP* Therefore mor* thought wets -given -44^.tags- ' possibility of toning BP-8B-D with * Ponsol Violet AH Irifc*. It was found mat a 30*fousel 'W.Olet AH lake (-7974), dry mixed with BMM in the ^portion of g|j4.-tO:,.Hl. WA respeotivsly, gave o...eloo:. mateh in tint t6 1B-l8l--B. A eahffeof *7974 was sot Up and t*T"- formula was submitted to tho ^veiopiiBt Section. V. . ....... .. 5- ^ ,2*.". " ''v-||?oompp|^on of the dry 'lake.witir^hi^fliiihed pulp showed a -.**HSiideraw' tms $a strength and in cleanness of due to the r,3&* tint also became A comparison of alt end hydrate aetbodi lereparing'.l^MI from no* supply Of Ponsol Blue Q& double p$?t an advantu&lpSi s in the ease of t&*. hydrate method b^ only about 8*. Br,. '"6 a ^CiSferesst'batoh of dyes'a " strength advdrog* was tfnjSvpr of the hydrate metho threrefere sOMis nptttfftfc in strength- may be due to some ifregufarltyia the dyeahipment*. An evaluation was made of'ponsol -.ifau HP grains and double paste for pigmeai*U^3aa*- #Ubls past* resulted in an appreciable loss in CtSatoftii power as Judged by rubout comparison with the boafd flushed .likes ware also weaker then the It wan wpafcer than t#e JteaZsk-i#' ip find that the flushed out lakes pulp Vhen compared on an equal DUP050316062 dye basis. Sr The lake from the grains was about 10# weaker than the lakerfrom the double paste both when compared as dry colors and vs, flushed out pulp. Consequently It may be concluded from the above that the Fonsol Blue BF double Paste is apparently more suitable for pigment lake purposes than the grains, EXPERIMENTAL DETAILS * S.B. 470, Pv 36-47, Series 470-10 evaluated Ponsol Blue BP double paste D-2081 against Ponsol Blue BP sprains by the alum and hydrate methods. Due to seemingly incorrect results in the yields from the alum method they were considered "void" and the evaluation was made on the hydrate method only. Prom the rubout'results on the dried out toner and lakes and the flushing out of the toner and lake pulps, in varnish, the following conclusions were ^dTawn (1) The dried out toner end the grains were very ' weak versus the flushed out toner pulp in varnish, (2) The lake obtained from the Ponsol Blue BF paste was approximately 10# stranger and greener than the lake Ponsol Blue BP grains,, (3) The flushed out. lakes were weaker than the flashed out toner pulp# _ 1 V, Series 479*11 A 13 prepared a 13 and 5# 3teke of Ponsol violet AR to tint BP-83-D in order to match BP-1S1-D tinetorially/ a mixtureof 15# FonsolVlolet AEt lake and 85 matched BP-121-D very close tlnotorially but it was weak and red (100 pts, of the mix * 96 pts. of BP-121-D). Due to the of the match a 2#' lake of Ponaol Violet AEt was.made* This nm~" up aw K-7974. A mix of 91.6# BP-86-D (std,) and 8t# K-7974 close match to BF-121-D in strength, v.s. red end v.s.dirtf in ti the Ponsol to standard., evaluation decreased the amount of dye up to CJZ U- The control gave a vessr close re a sox (salam mebhod)-waa not inoluHd an not bemad*'. ____ the, results obtained from thW addition of dye uhibfi ' *s''8LU2&e< at the boil and in the cold both in alum and hydrate method of K-7974. Ponsol Violet AS gave practically no difference between the alum and hydrate method In each ease the hydrate method wa*" _ to the alum method, the dye which was slurried at. tf slight!? better results than the cold slurried dye. It u?st jpSsel Violet AEt lakes dry out green and weak versus the oBb toner pulp* This difference appeered worthy of future co: regular procedure result# than the a; modifications of the hydrate method gave slightly better `at the boil gave DUP050316063  / v-".:, :s- better reaultir toaa the dye slurried la the cold. The addition of slurry9 t0 UawB8lld h7drat* slurry was inferior to the washed hydrate t ) t ** - ` fe. DUP050316064 SUBMITTED BYl APPH073D BY* 3*~~ xS>3 ^ PKHD8BT ggLea HBgBApflH REPORT ?at ms pioasma JZ&3. & FILS* VAT DYB PIGgggTg DATS* AUGUST - 1935 IYTRQDUCTTOUT Very little attention was giren to this problem this month at Jackson Laboratory* Bxperiaental work was confined to a study of the effect of oxidizing agents os the alumina hydrate Lake of Ponsol Blue GZ. Severer, considerable information of importance was obtained thru the Syeworfes concerning the chemical composition and physical proper ties of a number of Ponsol rat dyes. This information is recorded in our correspondence files (August*). SUMMARY & COBOLtrSIOSB Qkidation of alumina hydrate lakes of ponsol Blue GZ with strong oxidizing agents has no effect upon the tinctorial or light fastness properties. Treatment of the lake with saleium hypochlorite results in a much greener, duller and weaker produet, presumably owing to ohlorination and not oxidation of the dye. ' 30/15 and 30/17 alumina hydrate bases yield lakes similar tinctorially; they are somewhat stronger than a lake prepared from a 30/13 base, Bolling the Tat dye 30/13 alumina hydrate base has no effect upon the tinctorial properties* BXEgRlKBargAL 03TAILS Oxidation of alumina hydrate lakes of Ponsol Blue GZ crude with, sodium perborate, sodium peroxide and ealoium hypochlorite* See Bxpts* 3 and 4, Sf.B. 477* pp* 12 and 16* Alumina hydrate base studies on ponaol Blue GZerude. see Sxpt. 3, H.B. 477, p. 12. DUP050316065 a :7 SUBMITTED BY* APFR0V3U BY* PIGMBffl? gOLOR BSSBARGH REPORT ffLUSHEB COLORS /cs PIIBt g63@BTS Tff Oil' BATEt AUGUST 1935. IHTRQmCTIQg This problem has been continued actively in the-laboratory during the past month with considerable emphasis on the duplication of results previously obtained and also on a critical evaluation of the properties of the oil pastes* SUMMARY ASP CqgULUSIQH3 Any final conclusions as drqwn in the July report were subject to some doubt because almost all the dry controls mere considerably weaker than starfard RT*364-D The method of developing at the boil is partly responsible for this but it oan not aacount for all the weakness and in 469-27 aeries the normal development temperature gives weak products. The early work this month waa directed toward duplicating 469*27 series* all the varnish in the strike, with a study of development temperature (65G * 82C * 100C) . A total of three series e|KS&antially alike were run. Pellet formation was readily obtained-but with a long stirring period of 6*8 hours after drawing 2 waters from the slurry. This requires at least a two day oyele for the process. TlnOtorially one series had controls fairly close to standard but the other two were quite weak* The flushed colors were in all oases dark and bright* strung & blue with a very high finish against the corresponding dry control. The higher temperatures of development gave lighter and weaker products in both dry colors and flushed colors* Store was no>ehoiae possible as to the effect of temperature on the ease of pellet formation for in each aeries a different one finished first* All the colors flushed easily on the ink mill and were readily milled to apparently constant properties. ^ A series nas run to eheek 469*25 which was a study of the effect of mineral spirits and zinc Haphthenati (?) as assisting agents. In this series only 1/4 of the Varnish was in the strike and the remainder was added to the washed slurry, Aifter reheating to 60. There was mueh more rapid pellet .format Ionian this series ( 2*4 hours) and the Baphthenate seemed to give the most rapid and most uniform formation and the mineral spirits treated product was better than the untreated oontrel* Tinctorially the whole series is poor with dull masstones and weak* dirty tints* although the control is fair* They did not mill as wall as the previous series. One member of the series was given additional milling from 10X to 25X. The mas atone and finish ware materially improved but moisture analyses fail to show any significant reduction* hence the improvement noticed from long milling in thi3 and previous eases must be due to some change in the vehicle. DUP050316066 2 Is this last connection a sample of pellets which had not been milled was given a careful study as to the relation between amount of milling* change in tinctorial properties and loss of moisture* The pellets showed 61# moisture which dropped to 8*9# on the second pass* The analyses on the 5th and 10th passes were wail?-- of line being quite low* At the 15th pass there was 4*0# which remained substantially unchanged until the 25th pass* We feel safe in concluding that from 5 to 10 passes is sufficient to remove the moisture. An attempt was made to repeat 469-19C which was prepared on a 4)3 pigmenfiwoil basis and appeared to have interesting properties on thinning to 1*1 basis* This particular sample was prepared with part of the varnish and some mineral spirits in the strike* developed at boil* and the remainder of the varnish added to the washed and reheated slurry* The repeat experiment also included one developed at 65C ana one in which the total varnish was added to the finished aldrry with a Lightning Xixer, The first two stirred vefiy quickly to large balls of ink with oonsiderable fine material which was not readily taken up* The last one stirred to fine sandy pellets quits readily but further coalescingr-appsared to be very slow and all were finally filtered (a very rapid operation) and flushed on the ink mill* The inks were very stiff but on thinning to 111 they were soft and fairly long* Tinotorially they were fairly close to standard* The next series was prepared by adding all the varnish to the finished slurry with the "Lightning" agitator using 5t&, 4*3, and ltl Pigment-oil ratios* The slurries were split and half reheated to 65G before stirring* The reheating seemed to accelerate the incorporation of the vehicle slightly but to detract from the tinctorial value* After about 4 hours stirring* the 111 colors had a large ball of ink with considerable fine materialj the 4t3 colors were small sandy pellets* those which had been reheated being larger and more eompaotf the 5t3 colors were very fine pellets* All were filtered and flushed on the mill* The body of the resulting ink was proportional to the amount of varnish but on thinning to 111 they were very much alike and stlffer and shorter than 33B* The most interesting thing in the series was the obtaining of a lithol ink of workable characteristics with only 37*5# vehicle. One series was run to duplicate the previous work on GT^347#D which Indicated that a very stiff Ink (2il) could be prepared that would have desirable softness and length when thinned to 111/ The experiment this month appears to check the previous one in a general way but not in every respect- as to degree since the inks were all stiffer and shorts? than the earlier ones. An attempt was made to flush RT-347-B in Castor Oil for Parlin* It is obvious that the amount of castor oil which is permissible 1b not enough to flush the oolor* In fact there was very little evidence of flushing and it was necessary to mill until the water had simply evaporated* leaving a rather heard brittle material which was slightly oily* By adding some of the plasticizer (Bibutyl Phthalate) sufficient vehicle was used to make a plastdu. ink hut there was no flushing, just evaporation* DUP050316067 In general certain conclusions now appear fairly safe. 1. The only advantage in stirring until the colors coalesce to relatively large pellets is the ability to remove the water without filtration* The long stirring period required makes the process of somewhat doubtful economy* 2. Nearly all the products go through a stage of fine sandy pellets when they filter very readily but do not form the usual compact, pasty cake* This stage is reached rather quickly and the filtration is very rapid* The produots appear identical with those from the larger pellets and subsequent work will use this method of separating the water* 3. The presence of any considerable amount of varnish during the strike and development results in a substantial tinctorial change which seexas to be largely proportional to the amount of varnish present. Adding varnish after development has a very slight tinctorial effect. 4. Assisting agents such as mineral spirits and a zinc treated naphthenate have interesting effects which should be studied in more detail* 5. Very heavy inks can be obtained by flushing and seems to offer some advantage in body and length when thinned to a working consistency* EXPERIMENTAL DETAILS See Notebook #469 pp. 94-125. All see Ink Grinds #4505 to #45X5. 469-28 ) 469-29 } 469-30 } These three series ware alike in plan and procedure except that 469-29 used different materials and was run on a smaller batch size than the others* They were run to check 469-27 as follows $ A - Dry control --Develop at 65C. B - Develop at 65^0 with 1Q0 Tarnish in the strike. C - Develop at 838 - dry Control D- w " 82G with IOO56 Tarnish in the strike. E - Develop at 10Q6 - Dry Control. y " 100 C with 100S6 Tarnish in the strike. 469-31. This series was run to oheok the effect of Mineral Spirits and Zinc Naphthenate (?) used as assisting a&ftnta in the strike with 2536 Tarnish; the remainder of the varnish added to the washed and reheated slurry. It was a cheek on 469-25 series. This treatment gives more rapid coalescing to pellets and. less tinctorial change than Is obtained by t&e method used in 28-30 series. The mineral spirits does not seem to give quite as good pellet formation as does the zinc treated Naphthenate. DUP050316068 469-32. A Study of flushing 0T-34?M> as is 469-3 series. B - 5oj^ttlek - 2*1 Ink C - 75% Vfcrnish - 4;3 Ink D - 100% Varnish - 1*1 Ink. There is saae evidence that the stiff ink as in B gives a softer and longer ink when thinned to 1:1 basis than is obtained by grinding directly at the 111 ratio* 469-33. This is a cheek to 469-190 with some variations. A - Dry control B - 756 Varnish added to finished slurry in Lightning Mixer. 0 - 756 Varnish - 25% varnish* 15% Mineral 3pirits added to Na salt Developed at boil and remainder of varnish added to washed s lurry- - D - As 0 but develop at 65 6. B gave the best evidence of incorporation of the varnish. All were finally filtered and flushed to stiff inks which did, however, appear to have a soft body and good length when thinned to 111 basis, 0 and D did not give very good pellet formation and were considered * less satisfactory than B* 469-34. This was an attempt to flush HT-347-D into Castor Oil for Berlin. The amount of oil specified was too small to flush the color.- A sample of pulp was milled and the'wtfcer removed almbst wholly by evaporation. Another sample of pulp was mixed with seme Dibutyl Fhthale and milled. There was little evidence of flushing but on evaporation of the water a very stiff oil paste resulted, 469-35. This was a check to 33B with variation Ip the amount of varnish and a study of the effect of heating after adding the oil on the : lightning mixer, -'k": The heating seems to eld in the incorporation of the oil but to have an adverse effect tinetorially. The really Interesting thing about the series' Is that an ink containing only 37,8 % vehicle has been, obtained (36B) end ism workable1 properties. It is of sufficient interest to Uee as a basis for one line of future work, TnV Grind - jjlfiiF A study of the inks from 469*26 series, (Srind - 4806; A Study of the inks from 469-29 series. Grind - 4S0V A study of the inis from 469-30 series. Whereas 28 end 29 series showed natisfeetofy millingT and 9 passes, this series seemed to require from 16 tovl6 passes to give the same properties. i4 DUP050316069 A study of the inks from 4^1-31 aeries. Again a large number of passes (10-20) seem bo be necessary to show complete milling. Grind - 4801 A study of the inks from 439-32 series. The stiffer inks required more passe* to seem properly milled. Grind - 4510 A study of the inks from 439-SQ series. This series had relatively large amounts of mineral spirits used as assisting agent and it does net show any substantial increase in yield or difference In ink properties. Grind - 4111 A study, of the inks from 499-33 series. Grind - 431& A study of the reduction in moisture at various stages in milling the pellets from 17k. Results follow Ramilied 2X ex 10X lex sox 31J| 3.9* 2.34 1.44 4.04 4.1| 3*3* There is considerable doubt as to the accuracy. of these two results. Grind - 4811 Report of. Castor oil. 4i8M& series Lithol Red treated util Grlnd^ vpert -of grinding 483-5 series Castor 911. Lithol Red treated with Grind * 4515 1 A study of the inks from 439-33 series. DUP050316070 PlgMBBT COLOR BBSSARCH REPORT LITHOL BSD HT CASTOR OIL 3UBMITTSD BY: 7<-APPROVED BY{ IETRODUCTIOEf , FILE : riOMBHTS Hf-OIB DATE: AUGUST- 1935 A study of various procedures for preparing castor oil inks of RT-364-D has been made. Samples of inks made from plant batch 44949 have been prefared for testing at Philadelphia. SUMMARY ASP OOgCLPSIOBS Laboratory strikes on CS-7514 (RT-36$-d formula) were made in order to study the effect on blown castor oil - pigment (ltl) *n> of the following variations in procedure* A. Pry control mixed with castor oil in change can mixer and passed over ink mill. B Added 12,5 - 15$ oil (dry color basis) to developed sLurxy in colloid mill, filtered# washed# completed flushing with remainder of castor oil in change can mixer and passed over ink mill. C. Filtered and washed slurry, flushed water press cake with oil in change can mixer and passed over ink mill. D. Added 15$ oil j&.5$ oil of cloves) to developed slurry in colloid mill, filteredSwashed, dried overnite at 140F# mixed with remainder of oil in change can mixer and passed over ink mill. Blown castor oil inks (ltl) from plant batch 44949 of RT-364-D to be sent to Philadelphia for testing were prepared as follows: A. Slurry (before flooding) passed through colloid mill with 14$ oil# filtered, washed, dried overnite at 140-160F# mixed wtith remainder of oil in change can- mixer and given two p&sses ever -ink mill. 3. later press cake (22$ dry color) flushed with oil in W & P mixer and given four passes over ink mill. C. Dry ground eolor mixed with oil by hand and given four passes over ink mill. D. Dry ground color to be used as a control. Evaluation of inks has not as yet been completed, but there is no evidenee to date indicating that the flushed or oolloid tallied pigments give appreciably superior inks. BXEERDtBHTAL DETAILS Hotebcok 483. Exp, ffUifel-. Effect of adding 15$, 30$ and 100$ castor oil (dry pigment basis) to developed slurry of CS-7514. Adding 100$ and DUP050316071 3 2* Z0% of oil formed inks which gummed up the colloid mill, but 15^ of oil was satisfactory and two layers were obtained. The upper layer was a mixture of pigment, oil, water and some air while the lower lay er was clear water. Bxo. 483-3. Series of blown castor oil (H-120) inks (1*1) of CS-7514 prepared. Exp. 483-3. Cheek on 483-2. Bxp. 483-4. preparation of samples to be sent to Philadelphia. DUP050316072 FIOMBST QQTQR BB3BARCH REPORT 3-- Sl & BIOS TOKBR K-7983 SUBMITTED BY* CA Ih^ APPROVED BY* &A3. 3- / FILE* PgA-TTffW3Tfffq-- DATS* ATOSST---4935 iisrTRODPCTicar Production was continued in the Semi-Works on the improved BT-125-D type color in order to build up a stock of satisfactory strength direct strike material preparatory to making a mix to be set up as standard. SUMMARY & OOKGLB3IQE3 Three batches were made during the month all being made on the direct strike formulation. The first batch was made using a 14-1/3# increase in dye over the amount used in the 3W-6940 formulation, and the last two used a 16# increase in dye over this standard amount. This considerable increase in dye was found necessary because of the tendency of those direct strike batches to give weak results on grind ing* The current lots of Victoria Pure Blue BO have also shown a tendency to give weaker results than is desired. Satisfactory strength was secured on all three of these batches with light stability tests approximately equal to BT-100-D. Mixes are now in process preparatory to sotting up a standard with better strength than BT-125-D standard and equal lightfastness versus the BT-10G-D standard. Production is tabulated in Table X. BYPraiMBIWAl DETAILS M.B. 408, pages 98-99 3W Lot Formula BT-125-P production Results Vs SW-5940 Light Yield BY! Stabil Draw Bat. Lttm Lot 100# wt. ity tests down Str. Tint. 7290 Check 7235. Direct 84 18.01# BT-100* el.rod CM red 30# 30# strike* 14-1/8# in vs better vs drty crease in dye over SW-6940 7254 Check 7290 except " 18.25 vs BT-100* clean * red 30# 32# increase dye. Direct strike* 16# increase equal 1 in dye over SW-6940 7262 Check 7254 vs BT-100* t v * worse 9 s.str 30 31 vs red DUP050316073 The problem of producing a darker and brighter, ashless Para Had which possesses better hiding power than RT-70-D was begun* 3TTMMABY ASP COKCLURlOHS & eomparison of the RT-70-D end C3-6673 formulae Indicated the latter to be the more satisfactory, the product being aafclesa, softer in tbocture and haring a higher oil absorption. Zt la d^H^'and stronger in masstone and tint* since ttagt d^aza^petien. process insoluble impurities, rerioUO1 ^rd*iiis were comp ties in the CS-6673 iBtazotlsation appear to The nature of thbse impurities will b# educed darker d. Variations in nitrite and Acid eoncentratlona wefe'-'htudied for purposes of correlation with the di^etlsatlio Decrease in nitrite or increase of acid concentration tends 'the product light in masstone* Bromma (Ber. 21.398 (1888) attempted to aniline and alpha-nitroso-beta-naphthol in a manner analogous ill-known condensation ofaniline and nitroao benzene* ^.stance of the nltroso-naphthol largely in the qulnoid m -1-4 naphthoquinone-d-anil^ were obtained* Zt wen he trongiy acid solution, the tautomeric hydrogen would r< ills position and permit-`^smati.ott of Para Bo**- 0dn \ and nltroso-naphthol were condensed in aqueous acid* Para Red was net obtained* and sineothe product oen, the investigation eae discontinued, no,s,ttampt badug-1----establish the structure of the product- obtained. ' v Procedure <^8*73 permits hot filtration aif mo product, On the':-^iltrat a rli product crystallized* This was is . as p-^troneh!see*^azo- naphthol-s- sulfonic ac: tke coupling of" diazotised PHA with Bono Acid ? a: b" ubsta * warranted investigation a number of rojMOSSJ (A) It eafep3 the ash content of the Ca -shfl' Of Para P ljfepig ftd by the Whiting* Zt is intarocMs to' note that the Jjfc ' Salt is more . 'ti&le, end that the TJhlich sample IMN# -th, to.Jn tble to duplicate Q*40m- by w Of Whiting tip 1 . _ {&) Further, Para 'P giVae a deep blue-purple coloration with al'ka''li, The eolor is slight w|*b soda ash, but .pronounced With caustic, indicating tautom#lsm Of the Hej&iheiie hydrogen. The radieal change in color appears to involve ^ai9H^i!zation in both parte of the molecule thru '"M -4'*,.4, IV. V; DUP050316074 nitrolie acid formation. Treating a known weight of samplev with a fixed volume ij$? a*NaOH affords a qualitaiil> color test for -Para F: RT-22-D shows no color; C-36670 seise* and RT-7Q-D most, (me absence of this color indicates the' absence of Para F, bat the converse is not necessarily true. However, if this color is obtained and Para F is absent, it may be inferred.that characteristic groupings are present in the unknown). (C) It is possible that the blue shades imparted to Para Had by the incorporation of small amounts of Mono Acid Fmay be due In part to copreeipltation of blue Para F with Para Red in alkaline media. Ep^garimeats are designed to test this possibility, it having been observed that BN and Mono Acid F will ccufile in acid media^ ; In this connection it is interesting to note that In the standard diazotisations of PKA, a solid yellow insanity separates on standing, the amount increasing with time and tsmperature. mis substance also gives a violet tint with NagCO* and a deep purple with NaOH although the product is quite insoluble. The substance appears to be p-nitro-benzone azo amlno-p-nitro benzene. Its structure will be more definitely determined. (This is probably the seme impurity which occurs in the CS-6673 diazotisatioa). mcpTCRiMENTAL DBTAIL3 - Notebook #276. 3eries 276-38: - a comparison of procedures. nitrite concentration .ificreaslng'acid concentration mre. studied* Page 119: - Attempted Condensations of PSA DUP050316075 SUBMITTED BYt APPROVED BYi PIGHBUTT COXCR RBSBARCH REPORT TOLtriDIHS men RY-gsg-n ^FIEB* YOT.TrmTpg w w t su -- ' DATEi AUGUST-1935 IHTROSUCTIOK Further study of the RT-232-D formula was made in the Semi works in the attempt to obtain standard strength. Five batches were made. SUMMARY ABED COHCLPSIOUB A greater increase in nitrite excess was tried with little ef fect except where para soap was also increased* In this case the greatest difference was a more pronounced muddineas of masstone. A still higher amount of nitrite gave a definitely muddy mass- tone accompanied by slightly greater strength* Clarification of the diazo did not improve masstone but added somewhat to the strength. Use of urea was not tried. Mixes of some of the stronger but duller batohes made recently with earlier bright but weaker batches gave material very close to standard. However, it is doubtful if the use of higher amounts of nitrite would be successful in the plant* mnara rimerat , t u c t a na h .b . 455. p. 165 3U Variation> und. 7531 cSct: SW-^Sstd (mb f t Lot 43d) but increase nitrite from 17*5 to 19# sVd&rk star* Tint vs blue rs wk. blue ft weak 7234 7236 Check SW-7231 but increase Para - Soap from 1*75 to 2*5# s.dark muddy Cheek SW-7231 except reduce coupling vol. from 550 fb R75 gals* Coupled in 15 min* vs blue we blue war wk * s.blue 7259 7260 Check SW-7234 except increase nitrite from 19 to 20# s .dark muddy s.blue ft weak Check SW-7259 but clarify dia- s.muddy ws yel. zo using norit and filtered 0 s.str ws blue ft dirty vs yel. DUP050316076 PIQHB5T SQLQH HBSEARCH HBPORT BABIHM DPOXt TOSm RT-283-P SUBMITTED BY* APPROVED BY: ' PILE* BU6E3-- DATE: AUGUST- 1935 USTERQDUQTIOM Production of this color during the month was low due to plant shut-downi only one batch being made. Also included in this report are four batches outstanding from last month. SUMMARY fe OOMCLPaiOHS All five of the batches reported this month were made to se cure dark, strong material for shading purposes. The first two batehesi both outstanding from last month, were too light, the first being y .s . lighter than the standard and the second practically equal in masstone versus the standard. In both of these batehes the alkalinity of the coupling was kept just below the 11.3 pH limit (pH of each coupling 11.5) in an effort to make vary slightly dark material,but results were unsatisfactory. The amount of rosin was increased 8-l/2$ (175# - 190#) in the second batch but was unsuccessful in securing the desired result. The next three batehes were then made using the higher alkali nity of coupling (pH above 11.6) and dark material was A satisfactory 3300 lb. mix has been made consuming practically all of currant production on this aolor. Production results are tabulated in Table I and mix results in Table II. DUP050316077 DUP050316078 PISHSHT COLOR RESEARCH REPORT KEPIUK CALCTOM DPOL TOHBH RT-265-D SUBMITTED BY* APPROVED BY: j l **, /vv FILS* DO0SSDATE* ADGTJST-1935 ISTRQDUCTIOH Production was continued on this toner, a total of three batches being made during the month. Also included in this report are two batches outstanding from last month. Blue, equally clean and OK strength material is still desired for shading purposes, SUMMARY & COHCLP3IOH3 The two batches outstanding from last month were made using lowered development and strike volumes and a cut in the time of strike in an effort to secure blue material. Another variation introduced in the first of these batches was to substitute 18% of B Wood Rosin for. the I Rosin the calcium toner development. Results were unsatis factory, the material being yellow in tint versus the RT-265-D standard. In the second batch, 35-1/2% of B Wood Rosin was used and the develop ment temperature lowered to 200 F. These variations gave bluer results but the material was too weak and dirty to be considered satisfactory. / The first batoh made during August was made to check the first of the two batches reported above, except that the caustic soda in the coupling was cut 7-1/2%. Results continued unsatisfactory, the mater ial being yellower than standard. In an effort to secure a variable that would give satisfactory tint a series was run in the laboratory to check the possibility of using mixtures of TOB and T03W for this purpose. A mixture of 75% TOB and 25% TCOW gave bluer results than the control (all TOB) .although still giving yellow results versus the standard* The second plant batoh was made UBlng 75% TOB and 25% TcijBW in stead of all TOB in the coupling otherwise checking "the first hatch outstanding from last month. Results secured were not quite as good as expected, the material being weak, vs blue and s.dirty versus the stand ard . The third and last batch was made using a variable that has given bluer results in the plant* that of increasing the aalcium chlor ide 100%. w&B batch was otherwise a cheek to the first batch outstand ing from Iasi month. Little if any increase in blueness was noted, the product being yellower than standard. The only possibility that may be advanced for the consistently yellow results on this product is the quality of tho raw materials being used with the TOB being the most likely offender. The quality and ap pearance of this product has changed since the time when blue plant batches op RT-265-D were the rule rather than the exception. Two successful mixes totaling 1771 lbs. have been made consuming practically all of current production. RT-284-D and Mapico Red have been used as shading colors to secure the desired bluer tint. Results on production are tabulated in Table I and mix results in Table II. DUP050316079 TABUS I N.B. 385, pages 186-188 a '3? $ 8 I 84* 481 jH 1 Ht3 Ml b. soi <T JO 4&) I *4 h &_ % li 8gtoo J1S $ I > #Oe4l M *t * 33 j *1 k ! I $.4* *1*1' 'Sg * i5 7 I* I *4 * ` *4' *S2SK -t 1. t M o a J* l J*lla..1S0 tC<JnC* -Is os M8 & mt .* 1 <3 it it s -I I > &o w ' B 85 al If *te*H ;t CO *v p4 * jr a-1 t CO t e 8& -p 3 I Hien Ii m 1 25 PS 4H H4S* B B ei e * * * * A* 4 J <8 * * * * i g * * * r-* q t>m *3??.^** *- 35 *60 O 1Q Htin* Oo a* s aH sJoS i sa"8 Ht1O0 &ert- 3 J5 EXPERIMENTAL DETAILS U, ig aH S 84 Ifc a s <* il!! <e 3 1 I S w 1 ! I M1 l3. s M fl s Sna t\ < * * 0 J_ S ih rf 0 $ 'miSf 15710 44757 465#, 44893 4 5 # , 44849 10#, (RT-284) 43107 1 # , n 327- 1 # , Blase f lx s 26# TS dk,blulsh VS r t r . changeable clean vs s tr t s yel DUP050316080 PlfflBW COLOR BBSSARCS BEPORT maocar msm r t -219-d 3&~- 9/ SUEKITTSD BY* APKEtOVED BY* FILE* BBQ-ittROOSODAYS* AUGUST - 1935 lOTRQDTJCTIOB Parlin and Flint have found it necessary to use the old Haroon Toner RT-219-D for automotive lacquer purposes; in fact, our semi-works and plant hare Been manufacturing RT-219-I> against orders from the above Du Pont plants* Hlndful of the past difficulties with this pigment with respect to "blooming9, Parlin is oonoerned about the future behavior of our present production upon exposure. Consequently some attention was given to this important problem in the laboratory during this month. smnrARY & c o b g l u s io b s It will be of interest to review briefly the history of the development of the oeta-nitro-para-toluidine (HHPT) - Haphthanil BS (BBS) maroons. The first product developed, RT-219-D, was a simple coupling at 30C in an alkaline medium, which was filtered after a stirring period of one hour and washed ehloride free in the press. This pigment was a light maroon which frequently caused "blooming" on lacquer panels, i.e. a cream colored deposit which came to the surface of the panel and which could be rubbed off* It was later found that heating of the BT-219-d slurry to the boll, increased the depth of the pigment and the luster of the lacquer enamel. This product, according to the records, also exhibited "bloom ing" . A modification of the above formula, in which the coupling was acidified with acetic acid, then heated to the boil, filtered hot and washed in the press, gave a pigment (BT-259-S) which was apparently satisfactory in "bloom*. ~ Increased demand for more depth in maroons led to the development of r t -297-d which contained a small amount of B rosin soap in the coup ling subsequently precipitated with calcium* The alkaline coupling was ao id ifie^^'made slightly alkaline, heated to the boil and acidified prior to fi&Gpetlon* RT-297-B was darker than RY-259-B and has proven very satisfactory from the standpoint of "blooming*. Buring the development of b t -399-d with improved lacquer bleed, some interesting observations were made which might help to explain the cause of "blooming". The principle difference between BT-297-D and RT-399-D lies in the method for dissolving BBS* In the former ease, the BBS is dis solved at the boll in an &% Caustic soda solution while in the lat formula, solution takes place at 90 C in a A% caustic solution. ___ fp^pared by the above methods of dissolving BBS and starting with the same amounts of BBS, behaved differently in lacquer * RT-297-D gave no bloom while- BT-399-D bloomed badly* It was suspdeted that BBS was DUP050316081 2. responsible for the "blooming* and that no excess or at least a smaller excess of BBS *as present in RT-297-B than in BT-399-D due to the different treatments of the BBS solutions* In RT-297-D, the severe treatment probably caused hydrolysis of BBS* thereby reducing the amount of BBS in the ooupling. In fact* simple reduotion from 33.5 g. to 32.5 g. BBS per 0.1 mol ooupling* eliminated the bloom in BT-399-B. Furthermore,, the addition of a small amount of BBS in the lacquer grind of a non-blooming maroon* caused blooming* while additions of betaoxy-naphthoic acid or metanitranillns produced no effects. During this month* it has apparently been fairly definitely established that the "bloom" on these maroon panels* consists of BBS. The "bloom" was rubbed off and examined very carefully. All the reac tions coincided very closely with those of BBS. A review was made of old lacquer panels in the files and some very interesting facts were learned. For example* it was noticed that laboratory prepared BT-219-D bloomed while semi-works batches were free from bloom. This might probably be due to the faet that the BBS solution is boiled for a longer period in the semi-works than in the laboratory* therefore leas excess BBS may be present in the semi-works maroon* , It was of interest to note that in no case* laboratory* semiworka or plant* did RT-297-D show "blooming.* A semi-works lot of RT-219-D which had been insufficiently washed in the press because of some operating difficulties* exhibited "blooming.* Ooupling at 15C showed praetioally no bloom while a laboratory RT-219-D coupled at the standard temperature of 30C bloomed. It was also observed that higher temperatures of ooupling seemed to cause worse blooming. The ooupling at 150 was probably more complete * there fore ending with less excess BBS* At higher temperatures* MBPS diazo is more apt to form with alkalis the sodium nitrosamine salt which does not coupls. Increased volume of coupling seemed to prevent blooming. All of the above observations seem to point to the prosense of excess BBS in the pigment as the factor which is responsible for "bloom ing" . The superiority of RT-259-D and RT-297-D over RT-219-D might be explained as followst When the MBPT diazo is added to an alkaline sol ution some of the diazo is converted to the sodium nitrosamine salt which does not soppier ikwiiiftfbatiGn of the coupling after all of the diazo has bean adftfdt liberates the diazo which couples with the BBS* In the ease of BT-297-9 whieh is heated at the boil in an alkaline medium* it is possible that any free BBS is farther hydrolyzed into BOB and metanitraniline. It is difficult to understand how the acidifi cation* which precipitates the BBS* is of any assistance in eliminating bloom in the case of RT-297-33. On the*basis of the above discussion of the factors which hare been observed to influence blooming* it seems possible to formulate a DUP050316082 mathod which would match RT-219*D tinetortally and which should be free of "'blooming1* tendencies. 3uoh a formula shonl^ include a alight re duction in the amount of KBS, high volume of ooupling( 15C coupling* alow acidifioation after coupling, subsequent alkaline treatment, heating to about 40c, filtration and very good washing. It is planned to try such a formula in the laboratory. It might be of interest to mention that Parlin*3 enamel which is likely to be seleeted for automotive use, consisted of about 75# BT-219-D and 25# RT-297-B. This combination was found to be only slightly darker than RT-259-D by laoquer grind, therefore it would seem that Pari in could use RT-259-D for this purpose. Certainly, RT-259-D would be a safer pigment to use, judging from past experience. This information has been submitted to Parlin. The question of a reliable and quick test for bloom has been given some attention. At the present time, panels are placed in an oven at about 606 and observed from time to time. "Bloom" usually ooaurs within several days under these conditions whereas at roam temperature months may be required* However, this method is still too slow. Parlin has suggested a sublimation tost which consists in heat ing the pigment to high temperatures at which sublimation ooeurs. ' Parlin has claimed that the sublimed product was BBS which caused bloom ing. Our investigation of this method has shown that the sublimation product was apparently metanitraniline split off by hoat from free BBS. in the pigment. However, RT-297-D,''which for all practical purposes is considered non-blooming, also gave off the same yellow sublimation product by Parlin*s suggested method* Therefore, it is evident that this sublimation method is unreliable for detecting the "blooming" tendencies of a maroon* BvwaRinignTAL BBTAILS notebook BO* 419* series 20 to 22} pp. 56-05. DU P050316083 PlftMTOlljg dQBOR RESEARCH REPORT IttBOMT TOMR Rg-S19-I> Jir- ^5- IHTRgDBCTIOH H3A 3/ FILS: BBS MAiiUUK5~* DATE* AUatJST-1935 Due to renewed demand for this type of maroon by Pari in and Flint, production was begun in the Semi-works and plant. The present book standard formula, >5947, was used except for the increased coupling volume recently used to obtain a lighter mas stone. Six batches were made in the 3emi-works and two in the plant. SUMMARY & C0BCLU810HS All the Semi-`works material was satisfactory for shipment, being of equal depth and slightly greater brightness than the old standard HT-219-D. Brightness was slightly less than the small lot reoently made and shipped to Farliu (SW-8987). A bleed equal in intensity to standard but of a pinker tint was observed. Bo signs of 'blooming* have been observed to date but not sufficient time has elapsed for this to appear. Especial care is being taken to wash the color thoroughly to eliminate this objections! feature. After the first batch a slight increase in soda ash was made to obtain a more definite test for alkali after coupling. This raised the pH from 7.0 to 8.3 or higher. Ho difference was observed on the final grinds although control samples showed a slight increase in brightness as a result of the change. Similarly a slight reduction in amount of nitrite had no noticeable effect. On the first plant batch, additional soda ash was added after coupling to bring the pH up to 8*2. The extra soda ash was emitted on the second batch and an appreciable reduction watrmade in amount of nitrite used. Final tests in lacquer show the first batch to be slightly dark but OH in brightness while the seeottd one was very slightly light and slightly brighter. Both were shipped without blending. DUP050316084 DUP050316085 EXPERIMENTAL DETAILS #190, p . SI PigilSFI COLOR HSSBARgg BR-POUT SUBMITTED 3Y| APPROVED BYs A1EALX mm A*3 fflESs ICE80. IOM& DATSi AUGUST-1935 ISTRODUCTIOU Samples of green and red shades of Alkali Blue pulp were ob tained from three different suppliers to determine the applicability of the 307-530 method (mineral spirits - diglycol stearate - colloid mill) of treatment for improving the texture and tinctorial powers of the dry pigment. Press cakes of Chinese Blue B-63-D and Milori Blue B-66-D were treated similarly. SUMMARY & CONCLUSIONS The following samples were treated by the 307-53C methodj Alkali Blue Pulp, Red Shade (B#2154) and " , G-3 (D#2155) from The Caloo Chemical. Company. Suco Alkali Blue Pulp 3B (D#2152) and * R (B#2153) from The Standard Ultramarine Company. Alkali Blue Pulp G (B#215d) and K (D#2157) from The New York Color and Chemical Company. The 307-530 method oonsiets briefly in oolloid milling the alkali blue slurry treated with a solution of diglycol stearate in mineral spirits, filtering and drying * In eaoh ease a rubout compari son was made of the dried out untreated pulp* the "flushed out* pulp and the treated color* . D#2154 dried out to a very hard, low strength produet. The treated oolor was considerably softer in texture and stronger however it was still-about 38$ weaker than the flushed oolor on an equal ani line basis. D$S159 dried out considerably softer than D#2154 and was only 17$ weaker than the flushed oolor. In this ease, the treated oolor gave substantially equal strength to the flushed color on an equal ani line basis. D#2152 and D#2153, on drying, gave exceptionally good strength versus the flushed colors. The corresponding treated colors showed no strength advantages over the dried out pulps. D#2156 and D#2157 dried out very hard* Appreciable improvements in texture and strength were obtained by the 307-53C treatment* D#2156 was about 26$ weaker and D#2157 was more than 45$ weaker than the corresponding flushed colors when compared on an equal aniline basis. h. DUP050316086 . ?8r 2 From the above results we may conclude that the mineral spirits** diglyool stearate - colloid mill treatment gave improvements in texture and in tinctorial power in every ease where loss in strength and hard texture resulted from the drying of the untreated pulps. However, in a few oases, the treatment failed to equal the strength of the flushed oolora by an appreciable margin. Consequently, more work will be done in an effort to obtain further improvements in texture and tinctorial power. The results of this work on Alkali Blue may possibly find ap plication in the problem of preparing pigments from vat dyes. Press oakes of Chinese Blue B-63-D and iflloxi Blue B-66-D were given the 307-53C treatment and the treated colors were evaluated by the General Laboratory for texture. The results showed no advantages in ease of grinding or in dispersion, therefore the treatment was con sidered apparently valueless in the case of iron blues. Ho further work along these lines is contemplated. BXPBR1BBHTAL BBTAIL3 JT.B. 307, pp. 166-173 Series 307-54 tried the diglyool stearate, mineral spirits and colloid milling treatment on Xilorl Blue, B-66-33, press cake. The B-66-D press cake, reslurried and treated as above, gave an improvement in "breaking down" under the finger although the dried pulp was not r very hard. The treatment gave a low finish, slightly red masstone and low bronze. The apparent dull finish was tarmad detrimental for com mercial application* Series 307-55 repeated 307-54 treatment on Prussian Blue B-63-2> press cake. The product was turned Over to the Serviee Laboratory for evaluation. The treated product appeared better than the dried out toner although the service Laboratory texture evaluation showed no apparent improvements in ease of grinding or dispersion. Series 307-56 determined the effect of the diglyool stearate, mineral spirits and eolloid milling treatment on #2154 alkali blue pulp, red shade and B#2155* Alkali Blue Pulp 9-3 from the Caloo Chemical Com pany. D#215.4 dried out to a very hard metallic like product with very weak strength* The treated product gave eonaiderable improvement in strength although weaker than the flushed out control* D#2155 dried out considerably better than B-2154. The treated product was slightly better than the dried out pulp and slightly weaker than the flushed out pulp in varnish (100 pts* flushed out pulp = 110 pts* of the treated material = 120 pts* of the dried out pulp bn an equal color basis). Series 307-57 repeated the 307-56 treatment on D#2152, sue Alfagfli Blue smp 3B and D#2153 suoo Alkali Blue Pulp R from The standard Ultramarine Company. The dried out pulpa D#2152 and 2153 were exceptionally good ver sus the flushed out pulps. The treated samples were el ightly weak due DUP050316087 3 to tbs 10^ diluent notion of tha diglyool stearate. Therefore tbare was no apparent improvement Obtained from the treatment of these particular samples. Series 307-58 repeated the 307-56 treatment on D#2156 Alkali Blue Pulp a and D#2157 Alkali Blue Pulp H from the Few York Color & Chemical Company* The dried out palp in both oases was very hard. The treatment gave an improvement although it was wefek versus the flushed out pulp. Zn the oase of 2)^2156 150 parts of the treated product was equal to 100 parts of the flushed out, while in the case-of D#2157, 200 parts of the treated material was still weak in comparison with 100 parts of the flushed out pulp. (Parts on an equal color basis). 0 N DU P050316088 PIGMBHT COLOR SSaBARCH REPORT TOKBR RT-347-B SiT- A?/ j-Z> SUBMITTED BY* APPROVED BY: eA. uCz^eSt-- C/CiUi ' ' - g PILE: DOKDO MAROCBTO DATE: AUGUST-1935 IHTRODUCTIOH Because of continued difficulty in the plant in obtaining proper depth on this maroon formula* a series of fire batches was made in the Semi-works to obtain shading material and to study the formula and check raw materials. SUMMARY ASP GOUCLUSIOUS All the Semi-works batches were darker than standard by rubout and by lacquer test. Of two control runs, one was considerably darker than the other. The only observed difference in operation was a higher temperature for dissolving B05 in tha case of the darker batch. Compared to the lighter control, a 20# incre^fe in Turkey Red Oil, believed to be of benefit in the plant, showed no improvement; TOBW Lot 31 gave a v.s. darker and brighter lacquer than Lot 29 previously used; a 26,5# reduction in amount of manganese sulphate resulted in a slightly lighter and duller product. All were developed at a pH = 8.2 - 8.4 instead of 6.3. This my have added somewhat to depth. An OK mix was made containing about 40# of plant substandard stock. BXEBRIMEHTAL DETAILS H.B. 480, p. 5 0.25 mol charges were made. Gradings are on lacquer tests. SW-7243 - Check SW-5177 except final pH of development was raised from 6.3 to 8.3. Use TOBV Lot 29. vs RT-347-D - dark " SW-7247 - Cheek SW-7243 vs. RT-347-D - dark vs. SW-7243 - light SW-7246 - cheek 3W-7243 except increase Turkey Red Oil from 15.6 to 18.67#. vs. RT-347-D - dark vs. SW-7247 - vs light, s.dull SW-7251 - Cheek SW-7243 excapt use TOM Lot 31. vs. RT-347-D - dark vs. SW-7247 - vs dark & bright SW-7258 - Cheek SW-7251 except reduce manganous sulphate from 75 to 55# vs. RT-347-D - s.dark vs. SW-7251 - si. light & dull Lot 15275 - Mix SW and Plant material vs. RT-347-D - t v s light, vs bright DUP050316089 35~- A&S & - SUEMITTED BY;V APPROVED BTt k. >a a .^ f il e ; Ercffimn?- ib j h f w v n DATE: ABGOST - 1935 (1) Obieet of the Ini jLLJul&8&S& The objaot of tMs investigation Is to develop an Isolated sodium salt dye which will be satisfactory for making pigments at Newark. u> qariaL8sssn*,jfeMamSi April 15* 1935 to August 15* 1935 (3.) Historical ,Baek^o^ At the preidht time this pigment is made at Newark bp syn thesizing the dps from Its Intermediates and 1aiding directly, without isolation of the dye. Purchased dye from General Dyestuff corporation is unsatisfactory. Since the present policy Is to make an dyes whenever possible at the Dye works* work was undertaken toward developing a formula for producing isolated soda salt, f U) Summary and Conclusions A process for making soda salt satis factory for Newark has been developed end carried successfully thru the Ereba seal-works. This dye made from Bye works intermediates will be set up as a tentative standard for future manufacture at Deepwater. Indications are that the Isolated soda aalt may he dried without harming W Shis point has. not bean definitedly proved* however. Highly purlfift intermediate gives only very slightly betterproducts then average plant production of Intermediate. is beet ifpnfcad cold, salting causes difficulty in redissolving ;^^;dsrker maaatones . couplings using aJ;gda aih ape satisfactory. They are prac tically equal in quality to ^plings using theory of caustic to diisolve the Beta Oxy Naphthoic d ant soda ash for coupling. greens B.O,N. NagCCs and variations in volume have little effect on the coupling. Drying the toner at 1*0 F in an air dryer produces more strength and darker masutenes than drying in a humidified dryer. Dry ing at IOC C produces darker maBstones* greater strength and much leas bronze-. The addition of s 3 ohlor aniline 6 sulfonic acid or 5# DUP050316090 * ji 4 chlor aniline 2 sulfonic acid to the iafc exmediate has little effeet on the r esultinfitoner. Genetli Dyeetuff Corporation Pigment Rubina 3G and ICI Monolite Rubin 03 ire both unsatisfactory aoda waits, producing dark, dull toners. (4A) Pateat Situation This type of color was disclosed In German Patent Application in which apparently was never granted. (5) Plana for Future Work Production in the Jackson Laboratory semi-works of dye equal in quality to the tentative standard will be attempted. Further exper imentation on producing a dry powder soda salt will be carried out. (6.) Experimental Results which is as follows? Grama Material 00 sm 10*38 Caustic Soda 105 p-chlor aniline a-sulfonie acid - 4.38 501.100* 310 3,7 Sodium Hitrite 12,5 w-- Procedure Dissolve at 15 C. Add stir 1/2 hr* to soIn* lee to 5 o Add Make to at 0F 0 with lee and water. Add rapidly stir 29 min. and couple f j 'i J 'j 3*08 10 4*75 2 1*8 20 Tied* * Caustic soda 82*8 Beta Oxy Haphthele 146 sedlw|fc Carbonate 31 3ErV 80ft Sodium sulfite Para samsp 1500 8 18 StrontiumNitrate 625 4850 g* Dissolve. Add Seat to solution at 69C Dilute with water to Add w*ma water* Then mike to at if 0 'mtfc Ice and water, couple it 28 min* t*l. piki Brill* Yellow) n&eietes dlaxo), stir- x hear* Make to at'77' 84* dissolve, Add stir- 18 min* Add Stir 5 min. Strike In 5 min. at 77* c with A at 77 C. Hold at 77 C for 15 min. Hood to Brew water* niter* Wash chloride ikes. Dry at 150-160 F, Pulverize, DUP050316091 rV . S 1 S~3 Crude :|piermediate, Lot IS was purified by elarifying alkaline with Hosrlte, precipitating with acid, radlaaolving, elarifying and salting the material out* This salted intermediate was again dissolved and clarified and precipitated out as a white solid with acid* When made into^i^fieat on the above formula the resulting toner was only slightly lighter in masstone than toner made from the original Lot of p - Chlar Aniline - M - Sulfonic Acid* Dye was next made by the above formula, half of it filtered and redissolved and the other half laked directly. The toner from isolated dye was lighter and brighter in masstone and considerably stronger than the control. PHWt.har exp primeata ohow ad that thia isolated dye was lighter find bright hr In mncntriTiP nnif ernwiHtTahly ntremor than, the controlr Further experiments showed1 that this isolated dye eould be kept for at least one month without harming it and that if dried the resulting toner was only slightly darker and duller than the toner from paste sample. The isolated dye, particularly if dried, does not redisaolve ' to as clear a solution as the unisolated dye, but lakes satisfactorily ` nevertheless. Attempts to dissolve it completely by the addition of canstie, soda ash or acetic acid result in inferior toners. r Variations in the alkalinity of coupling the isolated dye had *. only slight affect. Couplings in theory of caustic (8.18,) 5.1 g. soda ash and couplings in all. soda ash IV*6 ,g* -as in the^X.a.1. process are both satisfactory* This all soda ash coupling can be made with 8.5 g. soda SSH satisfactorily* This method is the one written up and turned ever to the semi-works* '\ 10$ access B.O.K. over the process was found to have but little effect* s The soda salt was isolated as follows; (a) filtered.cold {h} heated to 70 0 ceded to 3* ({.filtered mid U) heatdd'to. boll, salted 10 and filtered Hot* (a) and lb) were very close. (o> was darker in masstone and bluer in shade than (a)* Method (a) was adopted as stand ard procedure* subst^^ton of SlC of the P Chidr Aniline M Sulfonic Acid with 3 chlor anilinesd sulfonic acid dr 4 ehlor aniline 2 sulfonic acid had but little affect on the resulting pigments. Samples of dye from l.G.I* and General Dyestuff Carp* were re ceived and tested. Beth prodeued very dork, dull unsatisfactory toners, Mr, Brizssolara of the Krebs staff bad baen working on an im provement of the laMng formula. The two new formulas were combined for semi-works trial. Differences from the original formula ware briefly as follows: all soda ash coupling, isolation of soda salt, elimination of sodium sulfite, decrease in. amounts of para soap and strontium nitrate, increase in volume, and elimination of the wash of the final toner. I<S*70 Semi-works trials were made on the attached formula and the Aliening variations tried (a) aging of soda salt paste one week. tj? DUP050316092  3*' f I--*. ' *. ' ?. 4r> (b) drying ani^rlading of soda salt and (c) drying tosar with and with oat controlled humidity, a s a result of these experiments it was decided that tie isolated soda salt paste is satisfactory. The qual ity of the dried material is somewhat doubtful and will he cheeked further. Drying the toner without humidity produces darker masatones, stronger tints and less bronze. The semi-works products are lighter In masstone, stronger* yellower and higfpr in bronze than standard h t -359-D. Krebs will decide on restsndl^Lzlng, Reference Z1M& 1740 pp* 101 to 119 \ 'V r i p1 i & DUP050316093 PTBIffiffP flQLQR RESEARCH KBPORT PISMBST RUBIBS MB RT-359D mt IRTRQDUCTIOK &Ucyt>s^' si * *i 3 PILE i PIGMBHg-fiUBBBS- QDATEi AUGUST-1935 One batch of RT-359-D was made in the Semi-works to teat ^re made on the formula described last month but dried and pulverized before striking the toner, STIMBARY AID COHOLPBIOflS An increase in amount of soda ash to obtain a more positive alkalinity of coupling and irregularities in drying conditions due to shut down of steam pressure, make a direct comparison with pre vious batches uncertain. However, the finished product was very satisfactory, being OK in mas atone and aLIghtly yellow and strong against RT-359-D standard. Under these conditions, drying out the dye appears to have no harmful affect, Further stock is being bu$lt up by a mix of material made on the new formula. In addition to this, a 300# lot of substandard material which was too blue in tint when made up has changed to OK in tint, and will be placed in standard stock, BXESRIMBRTAL DETAILS 5.B, #455, p. 133 SW-7842. Like 7230 except increase soda ash in coupling from 17 to 19#, Dye dried at 140 F. Pulverized. Used 65# to make toner, Balanee held in paste form. Toner dried at 140F and below in Electric Dryer. Redried in P A S Dryer at 140P - 40# humidity. vs. KT-359-D - CK? s.yel, s.bronzy} a.strongT s.yellow DUP050316094 SUBMITTED APPROVED BY: ^ PIGMENT COLOR RESEARCH REPORT 3S~- z 17 PARTICLE SX25 AND TEXTURE / 7/-/ PILE: 3EATBR COLORS1 DATE: AUGUST- 1935 ,,\ INTRODUCTION An attempt was made to gain some idea of the approximate per centage of larger particles on a brushout that is objectionable because of a sandpaper-like or gritty texture. SUMMARY AND CONCLUSIONS When screened with a dry brush, plant barytes passed completely through a 325 mesh screen. Then 1$ of larger particles of ground lump barytes (passed 250 mesh - retained by 325 mesh) was mixed with 99$ plant barges, the resulting brushout was noticeably more gritty and was approximately the upper limit for a satisfactory dry dis persed color. Then 5$ of these larger particles was mixed with 95$ plant barytes, the resulting brushout had a definite sandpaper-like tex ture . Particles of ground lump barytes that passed a 325 mesh screen were rougher than plant barytes, but there was no evidence of poor dispersion or grittiness. Since as little as 1% of slightly larger particles produces definite grittiness in a brushout, methods of screen analysis for satisfactory dry dispersed colors giving analytical results consider-. ably greater than 1$ retained on a 325 mesh screen only furnish a relative measure of the texture of the pigment. In order to have a significant correlation between the quality of a brushout and the particle size of the pigment used, as determined by screen analysis, the latter should be one which gives with a satiafaerfrory color, fig ures in the approximate range 0-2$ retained on a 325 mesh screen. EXPERIMENTAL DETAILS See Notebook 466, Exp. 14, p. 76. DUP050316095 .V ,r REPORT 11 ' 1113 C. LAMS3 ASBy T0HSB3 J<S~- 3-9# i SUBMITTED BY: APPROVED BY: FILE: MTer*7, TifiTTTiTi DATE: AUGUST-1935 lETRODUOUOH; studios on the development of lakelng procedures and improve ment of the original products, range Toner, K-7807 and scarlet SYL`, K7779, were completed this month* Orientation experiments were carried out on the preparation of a green pigment from 2 nitres 1 naphthol S sulfonic acid; lakes of Pontaeyl Brilliant Blue A, Pontaeyl Brilliant Milling Green B and Pontaeyl Wool Blue SL; new mono az dyes from 6 sulfo 2 naphthol 3 carboxylic acid and 4 iso propyl 2 naphthol 3 carboxylic acid; new blue plgoents from nitroso aceto-aoetyl arylides; and evaluation of a new red pigment--the condensation produet of dlbrem is atin chloride and meta nltro aeeto acetanilide. aMUm*MWn(W . An. improved prooesa for Orange Toner, K-7807 has been developed which giree good duplieability and a produet lighter and brighter than . the original K sample. Development of the pigment at the boil under acid conditions is essential-in obtaining the improved product consistently. The pigment is slightly sensitive to grinding which tends toward slightly deeper masstone upon severe pulverization. A large K sample of the im proved material has been prepared. Continued study of the effect of .variables on the hard texture of the deep masstone K-7779 product has resulted in no improvement* softer texture products tend toward much lighter masstones. Flushed inisare much lighter in masstone than inks prepared from the dry pigment,. othS: properties remaining substantially unaltered. The deep maestoso pigment is sensitive to grinding, the finer the pulverization the lighter ad bluer the tinctoria 1 properties. The . softer pigments^ye lass sensitive to grinding. sUM^tutioa of a smell quantity 'of para chlor aniline for 4 chlor anilin#i2 sulfonic sold in the coupling results in a deeper mesatone and yellow shade and tint, but this subterfuge is undesirable since para chlor aniline causes severe bleeding of th$ pigment in lacquer and linseed oil. pared A large K sample of the deep masstoiftp product has been pr a- A sample of 2 nitroso 1 naphthol 8 sulfonic acid, prepared by Dr, Jackson Laboratory, When reacted with ferrous iron resulted in a Very soluble green dye similar to Kaphthol Green B. The dye cannot be precipitated as a toner and only with difficulty as a lake. The Hike has poor light' fastness and tinctorial properties, and therefore, this sew green possesses no apparent merit. DUP050316096 Alumina Hydrate lakes were prepared from the triphenylmethane dyes Pontacyl Brilliant Blue A {Patent Blue A], sad Du Pont Brilliant Milling Green ffeosd on azlne dye Pontacyl Wool BL* Blue A yields a lake practically sHilar to Peacock Blue BL-72-B prepared from Blue S, in all properties. Killing Green B yields a lake much greener than BL-72-D hut otherwise similar in general properties* The latter appears to he as brilliant as BL-72-D. Both Blue A' and Green B precipitate completely and are superior to Blue E in this respect* The greens might he helpful in obtaining greener shades of BL-72-B* especially in rubber colors* Blue BL is very much redder# almost violet* compared with BL-72-D, hut appears to be Just as brilliant * stronger and somewhat better in light fastness than the latter* Blue 81 precipitates very easily and completely and much stronger lakes than can be prepared from Blue E should be poss ih le Dye8 and the corresponding barium and calcium toners and alum ina hydrate lakes were prepared by combining diazotized para nitraniline* meta nitre para toluidins, anthranlllc add and para toluidine meta sul fonic add with the new intermediate 6 sulfa 2 naphthol 3 carboxylic acid. : The pigments are exeepti onally deep yellowish reds which bleed slightly 1 in linseed oil* The P.N.A. * M.H.P.T* and enthranilic acid pigments pos sess no apparent merit* The P.T.M.S.A. pigment possesses some merit but 1 not sufficient to warrant further investigation* Byes and pigments of I 2 naphthol 3 oarboxy q sulfonic add resemble thosa of Schaeffer's Salt t \ (2 naphthol 8 sulfonic acid) more closely than those of B Salt (2 naphthol j 3:d disulfonic add) in solubility and pigment properties* | Byes and the corresponding barium and calcium toners* and altp** j lna hydrate lakes were prepared by combining diazotized para toluidine. . jj meta sulfohle add# 4 Shier aniline 2 sulfonic aeid and chlor 4 amine 1 toluene 5 aulfodn aclCwlth the new intermediate 4 iso propyl 2 naphthol 1 3 carboxylic add* The'pigments are exeeptipnally deep yellowish red^. */ fwhich'bleed badly in.linseed oil* The F*1MISA* calelum lain is and brighter than Mizarlne KL*33J$-B in toptonc Cad slightly yellower 'Hy': -j shade dkptint* fiblng.to the. pronounced Cll solubility of pigments pro* | pared rc@& iso propyl 2 naphthol 3 carboxylic tails intermediate apparom^ : ly possesses no exceptional merit as a new-jntarmediate for azo dyes ttitifl; lakes* -i*-' - j-v....r> - Inrecr&lgatii&s nn tjui. compounds and cor- .''' responding ferrous sdnla'df adito^ddetaallida and aeeto-aeetyi-anthranllie add resulte#^g:brlght blue #e* and pignuts* and not in the expedt^r" green pigm*criifif<3li pigments 'are racy bit flubte and poor in light flit- ness, howeTeri%hC' studies' have .beau onlyn# an orientation nature and . the formation of the pigment and its chemical stricture are not clearly understood* It is that a trie nitrite' compound and eorrespaadi|| 'iron salt of the aeeto-acetyl aryllde is formed, which probably rearrangtis.-"^ into a form differing ffim that of" the true qjilnoneoxime form* These " blue dyes and pigments which appear to be new compounds may warrant fur ther investigation* A new yellowish red pigment, hah been prepared by Dr* A*L* Fox of Jackson Laboratory by condensing dlbrem-isatin chloride with meta nitro aeeto-acetanilide. This new product is dark aha dull In, toptone, and very weak,, but much cleaner in shade and tint compared with Para Bed Y, RT-22-B* It is non-bleeding la linseed all and possesses good light fast ness but bleeds ihl^s^er* -> ** apparently possesses no appre- - Clidilo.merit owing ti 1th poorv:^lnetcrial properties. DUP050316097 EXPERIMENTAL Orange Toner, K-78Q7:- Development of improved laking process and product.Studies on tbseffect of variables. Expts. 15, is, 17. 19, 22, 25, and 27, notebook No.476, pages 42, 44, 46, 52, 64, 74 and 82 respectively. Scarlet 3XL, E-7779t- Development of deep masstone product. Studies on the development of laking ppeoodure and variables. Expts. 18, 20, 21, 24, 26, 29 and 34, notebook No. 476, pages 50, 56, 60, 70 78, 00 and 110 respectively. Iron salt of 2 nitroso 1 naphtho'l 8 sulfonio acid. Exp. 23, N.B. 476# page 66, * Lakes of Foateeyl Brilliant Bine A Du Pont Brilliant Milling Green B and Fontaoyl Wool Blue BL. Exp, 28, H,B, 476, page 84, Evaluation of condensation product of dibramo-isatin chloridjs and meta nitro aeeto acetanilide. Exp, 30, N.B* 476, page'04. , Dyes, toners and lakes of P.N.A* M.N.P.T, Antbranilie Add P.T.M.S.A. ! - 6 sulfo 2 naphtbol 3 carboxylic add Exp. 31, N.B, 476, pago" 94, '" . ' Dyes, toners and lolls Of.. P.T.M.SjA, . - -i 4 01 Aniline 2 sOvl -- 4 iso propyl 2 naphthol 3 carboxylic 2 cl 4 BSjg Toluene 2 ss$i add ~ Exp, 32,N,B,4%76 i page 102, V u * ... I . Iren spt of nitroso aeeto-aOetaniUde and nitroso aeeto* acetyl-ortho carboxyanilide. Expts. 33, 32, 36 end 37, N.B. 476, pages 108, 112, 118 ait 120 respectively. ,VvJ - DUP050316098 PI0MSHT COLOR RESEARCH REPORT PYRAZOLOSE SZSS SUBMITTED Bn APPROVED BY* IBTRQDUCTIOR ------ /Al- 3 y FILE* MIOO* LAESffDATE* AUGUST- 1935 Samples of yellow dyes of the pyrazolone type (Pontacyl Light Yellow 3G) received from General Dyestuff, Rational Aniline and Sandoz Chemical, were converted into hydrate lakes and evaluated. SUMMARY A COKCLUSIOE Lakes were prepared by precipitating the water solutions of the dyes with barium ohloride in the presence of alumina hydrate. The following tabulation lists the dyes which were evaluated and the re sults of the tests (see Table 1). It may be seen that all of the dyes gave greener and cleaner lakes than Du pent's dye except Rational** Yellow 30L whlah was green and dirty. Compared with General's dya, Rational's Yellow 2G and Sandoz' Yellow 20 cone, were close in tint while Rational's Yellow 3GL and Sandoz' Yallow 3G were red and dirty in tint* In addition to being dirty in tint. Yellow 3GL of Rational and Yellow 3G of sandoz were distinctly inferior in lightfastness. Sandoz' Yellow 20 eone, was better in light resistance than Du Post's Pontacyl Yellow while Rational's Yellow 2G and General's Saturn Yellow were substantially equal. Considering the money values of the three dyes which are closest in tinctorial properties, viz. General's Saturn Yellow, Rational's Yallow 20 and Sandoz' Yellow 20 cone., it is apparent, on the basis of the strength relationships and the quoted prices of $1.20 for Rational's 20 and $1.56 for Sandoz' 20, that Rational's 20 offers the better money value, on the earns basis. General's Saturn Yellow should have a sell ing price of about $1.85. The following tabulation`Illustrates the above* Strength quoted Value of Relation- prices dyes on equal t .h w ,----------------------- mh - --at"^tMi< Rational's Fast Yallow (Light) 20 1.58 $1*20 [Q/li/35) 1,86 Sandoz* xylene Light Yellow 20 oono. 1*57 1.5d (8/13/35) 2.45 For comparison purposes, the following tabulation is included to show the comparative money values of all of the dyes in question, when considered on the basis of their strength relationship only* Dves Pontacyl Light Yellow 3G Saturn Yellow GG Fast Light Yellow 20 Fast Light Yellow 30L Xylene Light Yellow 20 Cone. Xylene Light Yellow 30 Strength Quoted Value of Relation- Prices dyes on equal shin of dves strength basis 111 $1.13 (9/17/35]i $1.26 / lb. 100 2.20 (10/9/34 I 2,20 155 1.20 (8/14/35 \ 1.86 180 1.08 (8/1V35 > 2.04 157 1.56 (8/13/35 \1 2.45 168 1.13 (8/13/35;> 1.90 DUP050316099  Sj cz TO H > TO O' S3 e-s w- .P TO O g "* k 1 B u a P TO +3 TO TO ft. P H TO rl TO t> >> u TO +3 TO TO P TO $4 .a O TO o TO rl TO TO TO *4 TO fOt. p > TO TO 1 tag TO TO O TO -C T3 TO p pE| -H 44 1 u TO * r TO TO *3 TO P TO ft* o TO cr u oo 0 TO 0 * TO * TO nfl rl o o"& l *43 O rH O O rl rl O o rl o orl o TO -rl rl >* Cl TO 0 * M M M OH 13 U TO O rH rl O O trt in CO " in CO to 4a OS rt CO p rf rl rl rl rf rl O to rl a >> A TO t i 0 *d -3 rl g O O k c5S d 0 TO rl TO P a1 TO 1 OK TO 2 TO > it f8t. CO p * TO H a TO 43 to TO IS 43 ? C >* a 8 TO TO -rt ft. 6- TO t TO TO rl P TO S> mTO P rl *H rf O d O. P ft *r e H ' O TO <8 Si * TO o ft 8 p TO a9 1 8 1 t ft* o TO 6ft C c ft. TO *H 60 TO TO ft JS & M0 -VPh 8r TO c Q -5 rl a is 1 TO O p So3 3 TO o M TO at t< U TO ft ftCL. H TO a- 3 o TO ft P ex TO TO *-& CO > CO TO TO P >> TO TO <o T3 ft. TO * o rH to <?F l O to rl 02 rf TO lO rl rTOl 00 TO m to rl TO to to tw to rl o 02 a> P TO 2? a a I a A A m .C t43 8 s oi m O P< S3 TO TO H 43 TO TO ft. TO B Ch c*> TOO 60 * -H fO TO H o & 62 cs TO fO TO rl a o rH CS2 ci? * TO -H ft* TO H 00 >THO ffi! C9 C5 rol >> P rl rH rl TO > 8-ft TO * -TO R fi TO ft rl 60 O Jr p TO h ! -W rH O 4 rl rH TO >4 > 53 O TO P g TO Oh P P bO 3 In 5 60 rl TTTOOO rO ft fi* O o /y TO rl TO rf O H ft* fcrl 1 cf (X P4 o> in TO TO rl 5TO CO C-* o cn o is 44 CO 3 Hn JC TO - p &a3 o 2= r3 fa 3 1 M DUP050316100 SUBMITTED BT: APPROVED BY: coi^a Bgg BBPQBT JS~- 3 FXACQGM? BLUB T.n wsmamm og h x s h i m AcXJ. ffXLBl MSEOC, LABB* DAXB: AUGUST - 1935 (1) Object of the Iavastlgstloai Tb0 investigation was undertaken bo develop a Peacock ' Bine lake which when printed oa paper exhibits high finish. (2) Period Covered by the Report Newark, H, T Jase 11, 1935 to August 9, 1933 (3) Historical Background 0& Mar S3, 1938 a Krebs Service to Research report stated that ?. H. lever Company la making thitir o Feaeoek Blue lake bat az# not satisfied with its working properties. They desire a higher flash h than een be obtained with their present lake. It was suggested by tbit Service Labor atory that a strong Feeeoek Lake night be extended with high onelsteney alunina hydrate or that a Peasoek Bine Lake night be * struck direstly on a high consistency base to giro the desired offset. Hr, Bobrlng in the service laboratory had found that the addition of mteh agents as Barium Hydrate, Calelun Sydrats, Manganese Hesitate, Calelun Reainate, Cuner Basin, Conge Eater Gun, Bodied Her seed dl, etc, to our Peacock Blue lake, BL-169-B did not produce high finish, u> *mam.\smwm, A Peacock Bln* lake of higher finish audbetter printing properties than the Levey prodMh has Mean, devaleped In the leboratory and produeed In the seai^aifka,#- Sha swni-wofks lake la toe strong and must be extended with elunlna hydrate or preferably with a weaker lake#., likBroooZ Bfl'lllttat Blue M In inked oa a pheaphated type. alunina hydratklW eehlere tik reiwwl*. A&r drying at turf Is superior to humidity Ifeplp. for predaeias a product of high finish, Vhrlatieas in thoellltllnlty of ths hydrato havo leas ef feet on finish thananisslon afthe phosphate. (*A) Patent Situation No patent situation is intolved* * * (8) Plans for future Work It is planned to make a weaker lake by the same general ferwHa, In the *kl*werks. This material till be blended with the present strong laic# and a large sample submitted to Levey. Mr. Duhring wiH witness the printing testa in the Levey plant* i DUP050316101 ' . . "sfi~ rt^r.-^'-x' .-_ m Mt.'M' (ft), fe^m&iaiy^aia, . `r5WOrklng cm the assumption that the hydrate base is the controlling?'.faster la finish of the resulting ink, th following experimenta were carried out* Alumina hydrate sample* war made in the usual manner with th following proportions of is&red&emts. a - Hegalar 30-15 base Yields. Alton "as is" (106> 883 g Soda Ash 150 g, 86 g. pH of Mother --Masoy.___ 7.e pH Of 6th Water 6.5 B - Regular 39*1$ base Aina "as is" (106JO 28S 8* SodaAsh ISO s* 75*8 8* 8.8 7*1 0 * Phoephated has as in BM0Bt*B. Appro** 30-34*4 Alum *se is* . . 251*8 8* Bisodium phosphate lift 8* sofa Ash f* 8 108.4 g* 6d 5.7 i- - Phoaphated base * Appro*. 30-14.4 Ala* "as is" tl**) *U* 8* Hisodiw phosphata gig. . soli ASh . 4 _ 101.4 8* 5'ft 8* T` b - Phoaphated base * appro** 50-18.5 7.3 6.4 Alas *as is* (XfldjMr 8&*2g* Disodium Pho*plm4# . m 8#' soda Ash ipkg-*. fftS g. 7.4 6.7 These samples wers with fractions of the of eaeh dried* lakes were mods B formula as follows; 1ft g* fimjWt 850 os H80|Wsolw;h4. slurry* ___Poor onto 1/8 of these Adjust temperature to 4411. 64 g 14*8- k + ... ,,,,,,_ 180 e Bel. ' Bihaifere at 40- e. Add to dycNhsaa in 10 min. stir 4 hqurs. - mter. Wash chloride fern** By at Sep^Yi.- These imps wise- dry mixed with the eewwsadire toisd altmdna hy drate to esuslthe. strength'' of the lossy product s*$7745. The lakes from a Tb tregK'^sW^iehd'nosdTeatege in finlalu The lakes, from ev B 4 S t&* S#W material and fairly to sail- pSer* B being wary. 34bhly iafearatcr to 0 and B. "'* 1 -'5s DUP050316102 An attempt was oast made to make lakes of the strength of the Levey product on the & and D formulas by reducing the amount of dye in prouor- ticn to the excess strength Show by the original lakes {8% end 20% respectively). The resulting pigments wore weak t s . ths C number but they did exhibit the desired high finish. 7 A small batch was next made in ths awl-works <m the formula (e) given above except that the amount of dye was reduced from-16 to 14, This batch was split before drying. Half was dried at 140 7 in a humidified drvsr and half at 1*3* F in as air dryer. The air dried pro duct (3W-7215) is superior la finish to the humidity dried material and equal to laboratory samples, it la 8$ strong vs. ths Levey pigment. Reduction with phosphate* hydrate showed it to have higher finish and to print bettor than the C number. Sufficient hydrate waa made in the laboratory to extend 5 Ibe. of material to be submitted to Levey. The mix waa made in the aoal-werks Mlkro Pulveriser and unfortunataly the hydrate was not ground first. As a result the physical appearane# of the mix ia bad, small specks of white ahowing thruout the mass. This effect ia exaggerated oa mixing with ell as the blue lakes mixed before the hydrate. The resulting 9 lb. sample, Lot 4341 while satisfactory in printing properties and finish will net be submitted because of the above mentioned difficulty. Instead it is planned to make a ai-wfs bateh of lake, weaker than the Levey preduet and bland tha strong mater- ial te the proper strength. ./ '. . . Bet. JLBB-17M pp. 1-1S. f 1 i .1 1 -.4 DUP050316103 tOGGNURT CGLQBKaSEARCH REPORT $< PEaHAHEHT PEACOCK BLUE T-AVE ccsmmsos w it h f u q it iv b t y p e 3f- 3*V SUMITTED BY: i^OtSosJe. APPROVED BY! FILE: *09(3. LAggt DATE: AUGUST - 1935 (1) Object of the Investigation This investigation was undertaken, to carefully compare a light fast oaol mBliuxetuarewoitfh phosphotungatle adds of Lithosol Fast Blue 60 and the fugitive barium lakes from Lithosol Brilliant LithBlue 3* in tinctorial properties, strength, light resistance and cost. (2) Period Covered tv the Report July 12, 1^35 to August 20, 1935 (3) Historical Baotamiili It has been known for seme time that a light resistant color/ approximating Peacock Bine Lake in shade can be made from PTAs of Lith osol Fast Blue 6a and Lithosol Bites a. A there investigation into fundamental comparative costs was not made,' however. It was decided to review previous work (done in Krebs Laboratory) and obtain as complete a comparison as possible., *j (4) summary & Conclusions 3 A mix. as felloes : * ` ./ BT-96-D (UthOSOX Fast Blue G&) .72 parts BT-99-D (LithddOl Blue G) v . .29 parts Alumina Hydrate 5.00 parts > ,. is approximately equal in shade and strength but dull vs. BL-151-D (19# lake of Brilliant Blue 2). * ' ' :;3we^*v' .; -v . J- Calculating b*g to the dyes 1 lb. of basic dye mix is eepiv- alent to 3.33 lb*. of BdlllSfct. Bah* B* On this basis and taking into account the prftgppt j*i`*jr Sd&l'snt Blue E dye end the comparative costs of preeilliiahts - wi'mixed basic' dye should cost $3.05 per lb. to be "^^Ppalent hr'tie cost -of Brilliant Blue E* 1 I Ji On a malar basis 1 mole of basic dye is equal tinetorially to approximately 2 moles of the add dye (Brilliant Blue E). Flushing the P.T.A, toners increases the strength approximately 10# over that of the dried pigments. While the fugitive type Is brighter originally, after E hours in the fadeemater it is definitely duller than the permanent type sim ilarly exposed*-'; (4A) Patent Situation patent situatlon is Involved. <-?V DUP050316104 (5) Plans for Eutare Work No &rthr experimental work la planned at this ti cost calculation* will te submitted to the interested parties. (6) Experimental Results In order to develop optimum strength of F.T.a . toners, a series of runs was made In which BT-Ofi-D (Lithosol East Blue 6G) was flushed into oil in Tarioua waps* Erehs regular BT-96-D formula was followed end the pigments treated as fellows: A- Control. Figment dried* then milled into oil in usual way. B- Pigment press cake thoroly mixed with #0 Regular Varnish in 1:1 ratio of drypigment tooll. Flushed m ink mill. G-- Same as R colloid milled, before flushing* D- Varnish added to strike just prior to development. E -Varnish added to p.T.A. solution before strike* B, G, & and %*ere all approximately 106 strong os. a * SanplCB shewed a very slight advantage over the ethers and this method was adopted as standard procedure. simples of KMfc-R, BT-99-D and an alumina hydrate lake of f a mixture of the two (08-7422} were put hru the above flushing operation* The CIS number failad to flush properly due probably to the hydrate and .was discarded. *y These flushed ink* ware mixed with each other and with alumina hydrate ink to approximate a sample of fugitive Fsaooek Blue from F.H. Levey Company. The proportions required were.es follows: more Inlll/.2 ;$&(rs* then goes weak and dull itt 8 hours* It.has- lest nearly all ItiK^^tor id's hours while the permanent type is unchanged in that length ofMitSme* From the proportions of pigment used above* the proportion of dyes required was calculated and a mixed strike made as follows: 33 g# Lithosol-East Blue es 12.7 g. lithosol Blue G When extended 1-6 it equalled the BL-151*g standard and when extended 1-8 it equalled the Levey pro duet which isw& the strength of BLrlSL-D. This experiment sfted as a cheek da previous work and calculations. ccat Wolf the above data the following oaTeulationa were made: DUP050316105 1 lb. P.T.A. toner mist is equivalent to 8 lbs. Brilliant Blue E lake. BL-151-D BL-151-B:'= 19# Brilliant Blue E dye 8 lbs. BLf-lSl-D > 1.52 lbs. Brilliant Blue E dye Therefore 1 lb. P.T.A. toner mix is equivalent to 1.52 lbs* Brilliant Blue 2 dye (1) 46 lbs* lithosol Fast Blue 6G dye to make 1 lb. BT-96-D (Krebs (.46 x .78(proportion of mix}' ) = .33 formula) .44 lbs. Lithosol Blue 8 dye to make 1 lb. BT-99-D (Krebs formula) (.44 x .29 (proportion of mix) ) * .127 Lbs* basis dye mix to make 1 lb* toner - .457 (2) Therefore* .457 lbs. b&sio dye mix is equivalent to 1.52 lbs. Brilliant-Blue B dye (Equations (1) and (2) ) and 1 lb. basis dye mix is equivalent to I.5r_ 3#33 iba*- BrllHant Bine B dye (3) t Precipitant for BT~96-D costs $1*57 per lb* of dye used (Krebs A eost afieet) #1.57 x .72 (proportion of mix) = #1.13 Precipitant for BT-99-D costs #1*82 permit. of dyo used #1*88 x .29 (proportion of mix.) Cost of precipitant for 1 lb. basic dye mix * _ *53 #1*65 (4) Precipitant for BL-151-D costa #.562 per.lb* of dye used Cost of precipitant for f*93" lbs. Brilliant Blue* # *088 x 5".S3 $0*81 (5) Precipitant fSHf.l 2fe basic dye mix costs in exeats of prodfidget for. eaiUiva|sMfc amount of Brilliant Bloc 2 - - #i*4. (J&jpatieas 4 lt 5) 3*33 lbs* Brilliant Blue 2 costs (Krebs cost sheet 0 $3US$ per13*.. Klaus excess precipitant cost #4.50 31*45 Cost that mixed basic dye Should be, to be equivalent to Brilliant HueB #3*05 The alumina hydrate has not been considered in the above calculation** As a matter of interest chemically the mole formula ratio of basic dye and Brilliant Blue 2 has been worked out. DUP050316106 ' Eelmlar Purity of 22* _ Wtight Standard (TlClg) Lithoaol Brilliant Blue S 78* 72.296 Lithosol Fast Bins 80 899 73.996 Litbosol Blue 0 427 92.196 1 lb. basis dye is equivalent to 3.33 lbs. Brilliant Blue E (see above} .789 lba. 100# Fast Blue 60 la equivalent to 2.90 lbs. 100# Brill. .00254 moles Fast Blue 60 is equivalent to .0047 moles Brill. Blue E 1 mole Fast Blqe 60 is equivalent to 1*85 moles Krill. Blue E .981 lba, 100# Blue 0 is equivalent to 2.90 lbs. 100# Brill. Blue E 1 lb. Ido# Blue 0 is equivalent to 9.15 lbs. 1.00# Brill. Blue s 400234 moles Blue 68 is equivalent to .0047 moles Brill. Blue E 1 mole Blue 8 is equivalmt to S.0X molts Brill. Blue 2 Ref. fZSB 1793 pj>. 25*3? r DUP050316107 fef*' 3S~- 3*>- VIWSSS COLOR BgSEABCH REPORT 3ITg'AKT5RBNS FIKK 37 LAKE SUBMITTED BY: QJfd&Q*Jk APPROVED BY: 22 (e PILE: MISC J.tittmDATE: AUGUST - 1935 * (1) Object of the Investigation This investigation was undertaken to develop a process for making a lake of Sulfanthrene Pink SV tor addition to Krebs line. (2) Period Covered by the Rencct , Newark, BF.J. August 3, 1935 to August 21, 1935 (3) Historical Background * A previoria report (JTLR June, 1935} on SulfantKrone Pink colors stated that the toner exhibited as much strength as the ink a when compared on an equal dye basis, At that time there was not a great ' deal of interest in this color. In the meantins a service problem arose in which sulfenthrone Pink was found desirable for or chid shades in paihr and it was decided to add a lake (toner is too high priced) to the Krebs line. ' * I 1 1 I 1 I t Ur*. Siegel had found in his work on rat dye lakes that better products were usually obtained" by mixing the insoluble dye and washed hydrate base* than those obtained by the old procedure of slurry* ing the dye in the alum solution and striking with soda ash. These ex* perlments were tried with Sulfanthrenf Pink 3V. 1 A (4) summary & Conclusions A satisfactory inking formula has been developed and a final sample K-7971 set iq n Cold mixing of th# dye paste and washed hydrate produces stronger, more light fast colors than those made by precipitating the hydrate in th^iN^jiMU^- of' the dye. (4A) Patent a^fia^en Hone is involved, (5) Plana fee future Wark Manufacture of the lake in the Krebs semi-works will be started in the near future. (6) Experimental Results 25^ Alumina Hydrate lakes of Sulfanthrana Fink SV, Lot 9 were made by the following procedures. DUP050316108 ~fO *z A * Dye paste slurried in alum solution, soda ash solution added. Filtered. Washed sulfate free* Dried. B - Dya paste at toil added to washed 30-15 hydrate. Filtered, washed, dried. C - Cold dye paste added to washed 30-15 hydrate. Filtered, washed and dried. Samples B AO were very close to each other and strong, clean and superior in light fastness to A. Method C was adopted as standard procedure and a S sample made on that formula as follows? 430 g. Sulfenthrone Pink 37 paste. Lot 9 (13*97$ solids) 1100 ee Water* Slurry well at room temperature. Add to 8033 ee Alumina Hydrate slurry (washed 30-15 base) equivalent to 180 g* dry. Stir 1 hear* Filter - Wash with 800 ee water. Dry overnight.in air at 1409 F. Yield - <249 g, " This sample cheeked the above sample (e) very closely. It was given K-7971 end the process filed under that number. Befereaee JUHB 1740, pp, 1^9, 181, . j i DUP050316109 ~^sr 4Fr" 33 "7/ ,* I?/ SjnwwJ?> AFPHOVED BY: PicaaasHT c o l o b aganARgB b j p o bt SULF03BB1 COLOR T.AjTKg , mjs, matlLsia- DATS: AUGUST - 1935 (1) Object of the Inreatlgatlan* Certain, sulfur colors are water soluble and capable of being lakad with hoary natal salts* This investigation, was undertaken to make and evaluate acne of these lakes, (g ) Period Covered hr the Report Newark, N, J, June 18 , 1935 toAugust 13, 1935 t3) Historical Background Previous work in 1aokson Labor atery (JXR * ' ) and at Newark on Sulfogene Brilliant Blue SOGF lakes sheared it to he of some interest, altho inferior in brightness and light fastness to Ponsol Blue GZ lakes * The sulfur solor is of course much cheaper than the Ponsol color. Dr* Strease of Jackson Laboratory submitted for test four sulfogene Greens similar in properties to the Brilliant Blue 5G0Pt Their water solubility is due to a' sulfonic told group in the molecule instead ef a carbonyl group as, in the blue* y {4 ^ and nrfwftlnitl .l t; '- Sulfogene Green 4GX, Green M Gan,Brilliant Green oc? and Fast Green BCF, produce lakes of $0r tinctorial properties* The blanc fire lakes are mere light fdst them the' alumina hydrate lakes, Sulfogene Brilliant Blue 530? lakes* wfciih. appear to bo as light resistant in tints as iron blue, have been eubmittad to Philadelphia Jfcr outdoor exposure teste.,' > UA) Patent Situation Nona h- far as now known*. ' t&\ Plana WktJt Be further work .oh the greens is planned* Further work on the bind is dependant on the results of outside exposure tests. These results will not be available for a year cor mere, tin axperinymtal Results Sines the molecular weight and purities of these eolors are uncertain the following procedure wdstfolloirod in making lakes. Samples of standard dye washed praetieoXly: salt free were furnished by Dr* *streuse of the Miscellaneous Dyas' BiVision#- Toner* were made by preoipit&ting 10 g* of each dye with barium chloride solution. These toners had such DUP050316110 * r- ?oor texture thnt they were net rubbed out. The weights or toner ch ained wore aflrrbllCMs: Sulfogene Green 43X 8.5 g. " " M 6enc. 9.8 g. " Brill, Grow. SCOT 9.4 g. * Fast Green BOF 9.7 g. Using these toner yields as a guide, 13# barium -lakes of each color were made on frsafely precipitated, trashed blanc fixe and 30-15 alumina hydrate. It was found that alumina hydrate would precipitate the dye without the addition of barium chloride. The resulting lakes were slightly weals:, however, when compared with the barium lakes. ill the lakes were dull and weak tIn etortally, ranging in shade from a greenish blue to a green. The light fastness of the blane fixe lakes was superior to that of the hydrate lakes but all were itueh inferior to Chrome Greens, 3-39S~D and GdRHB, Sulfogene Brilliant Blue 5GCF A lake containing 11.2$ color was made as follows: -t 8.1 g. Sulfogene Brilliant Blue 5GCF (8-1988) MBB-8.) 400 oo water. Dissolve at 80* 0. Add to 380 ee freshly preeipitated and washed blane fixe (equivalent ' ^ 88,5 g. dry) Adiust temperature to 43 0, Add 41 ec 10# Barium Chloxl do solution during 1 minute, stir SO minutes, Filter, Wash chloride free* Dry at 140 ?* . ,,'" - ` ? $ This lake, was tinted with ftO* in Bulnx to approximate iron blue, 1 part of lake * Z parte TiOkheiag equal in strength to 1 pg$- B-140-g (iron blue"toner).f;^p) parfe TiO^ the Inks waa transparent and res but equal in light ss on hours fadsoneter asposura . Sinoe tho result* of this experiment looked somewhat promising far obtaining light fast blue tints in Dulux, large samples of lake were made upon blaprfixo 'and aliwtnsr"" 'tcitiu Tgtcse ware given K numbers 7931 and 76#1cspeetiv*Xy.* 'T' its hern submitted to Philadelphia for outside expamiii.'tests. Hef. J1HB 1793, pp, 101~i0i ; V-. DUP050316111 3j T- 30^ 7? 3UH4IWED BTS APFRGYBD BTs y.3.3. / ms* taac. iaarar- BUE: AWT33T - 1955 {1} Oblaat of 'Phi* `1: _ from Ba Pont 3*13$! to nisk* and eraluata lakes and Pentacyl Oram BL Gone, (2> ?*!<*Qererad ter liwgt .^**5** SV|, JT. J. O * 3.0* lfJSg (3) Hlat^,#, ' :Utboa#%l Brilliant Bln* S dye which contains thraa sulfonic ald groups dots Itato cleanly with twins chloride. It *is suggested by Hr. Mhrlag of tin KribS' staff that a similar dye eonti lag only two sulfonic grappa might wad intersat and praelpitata sc oanpietely. conference with B*. Allenen and Br*earleton disclosed fast that Peataeyl Graan Bt Cons la identical with Brilliant Bins that It tuna tSfaUlfenie acli groups inataad -ef thraa* this dl au$& containing la addition a Florida atm la raddar in shade ae '-Stt. P. ont Beilll; a- t M*illlB. g EbraGa B*' G. ent (4} Steamary and' CacalueiaBS : Lakes from Btt ...... BL Conn* art bright* JUuiaiPeaeocfc Bins Lakne mat 14" on almina hydrastt with;' KlUSi Oreaa B Conn* and Pontaoyl areas sd# Sight fastness Uisiler t at Blu* s). They strike alain%r: end aluminas* shlarlde. (*il * ** 3l<a<U m ttr- a & (5) Blana for ^jture si$Mftis is inyolrad* at present. fgy Bxearl--ntal Basalts 8*~l/*56 lakes an alumina hydrate war# made 'on Krebs BL-159-D formula as fellows* *xm ~ # g. Watar - Bides. Dlaaolya at dS* G Bake to water. BO: minutes. ' Draw $ watera. DUP050316112 m $** 3 g* Bye 120 oa Water* Dissolve at St* C, stir IS minutes. MS to base ar*Wr 10 minutes. Adjust temperature to 44 6. 3.3 g. Alumina Chloride 7.0 g. Barium Ghlorido 60 ee Water. Diesolve at 44 C. Md to dye- base in 10 minutes, stir 1 boar. Filter. Wash chloride free. Dry overnight at 140 7. Dyes used A - Da Feat Brilliant Hilling Green B Cone. Lot 3 B - Peatacyl Green BL Cone. Lot 17 Both 'dyed precipitated completely giving a nearly colorless filtrate. The dried, lathes were rubbed out in oil and read as follows: A * Green masstone and tint vs* BL-150-B (Brilliant Blue 3 Labs) light masstone, yellow slightly weak tint vs* BT-96-D (p .t .a . of Lithe*! Fast Blue 6G) adjusted to sane pigment content* B * A mere yellowish gren than %, Barb saestone very blue tint vs* <SJM54T-D (p*TA* of Brilliant Green B and Thioflavine) adjusted to aano pigment content* The light fastness of both samples is poor* being, approximately equal to that of BL-15t-D. Both skindoens and tints are faded practically whit* in 34 hours exposure, in the fadcodstcr* while BT*t6-Dand GT*34?**B are practically unaffected* sefercace JIHB' 1740 * pp* 1T7-I7fc. DUP050316113 PIGMBBT COLOR RSSEARCH REPORT asm-w o r k s f r q d u c it io h SUBMITTED BY* APPROVED BYl UTTRODOGTlOg f il es t qa-aoo DATES l AUGUST- 1935 40 batches of 18 different oolors were made* these Included 6 batches of RT-2W-D, 5 batches of RT-347-D* 4 hatches each of Y-299D and Y-7888-i). There was a two week shut-down during this month. SUMMARY RT-232-d i Toluidine Toner, t w o hatches were made concluding for the present work on this color* RT-219-D, 3SBS Maroon - six hatches wore made to fill voders from Parlln. RT-347-D Manganese Maroon - Five hatches were made to produce dark shading material* RT-354-D, Bordeaux Maroon - Two hatches were made to test a lot of Tohiae Acid. RT-359-d , pigment Ruhine Toner - One additional hatch was made on the new aoupling and laklng formula, 03-7970, RP-7971-D, sulphanthrcne pink Lake - One hatch of this new lake was made and split into two parts for drying study* GY-344-D, Greening Yellow - A small batch of yellow was pressed out and dried for shipment to Philadelphia* *- Y-78S8-D. Primrose Yellow - Four hatches were made in development of this yellow formula* Y-299-D, Med* Yellow - Four hatohes were made in o cut lunation of thin problem* (Development of a load nitrate formula)* Y-3S9-D, lied* Yellow - Two hatches were made in the study of this process* Y0-38-D, Orange Yellow - One hatch of a special shade was prepared in the Semi-Works for use by the Sxperimsntal Station* BT-125-d * PTA Toner - Two hatches were undo in continuation of the development work done last month. BL-159-d * Cerulean Blue - One hatch was made in preparation of material to submit to customer* B-Q3-D, Chinese Blue * Two hatohes were made in a send-works Check on the formula * OL-7906-D, Treated pigment Green- Two batches were made in preparation--- of material and in a study of the operation* seven grinds of dry color* 5 grinds of pulp eolor* and 3 mixes were made in the research semi-works* for the plant during August* 1935* Drv grinding CP Blue CP Yellow CP Orange gPfo grading Red Toner palps Green " " o p Yellow Mixing Blue toner CP Orange Charge 743-a 739-0 740-3 737-S 737-3 737-S BKtohes g Total 1 1 2 2 500 2509 987 B"Tjbj!.l.a.. 8 1 Total if lba* S ioo% 708 43d * 1319 751-a l 754-s Total 164 3715 3379 DUP050316114 42 43 44 7245 46 47 48 49 7250 51 52 53 54 7255 56 57 58 59 7260 61 62 63 64 7265 66 67 68 69 7270 71 72 73 74 75 7276 77 78 79 7280 #10 BLDG. PRODUCTION R3P0RT FOR AUGUST. 1935 Code Y-299-D RT-359-D RT-347-D GL-7906-B GY-7925-D RT-347-D It Y-299-D GX-344-D 3T-125-D RT-347-D Y-7888-B Y-299-D BT-125-I> Y-7888-D ft Y-299-2) RT-347-D RT-232-rr It Y-359-D BT-125-D Y0-38-D RT-2I9-D It n it Y-359-D GL-7906-D 31-159-D RT-219-D B-63-D RT-219-D RP-7971-D n RT-354-D B-63-D RT-354-D Y-7888-B n Lba. Struck 31 35 125 160 9 125 It 31 7 30 125 155 31 30 19 t| 31 125 75 75 31 30 4 115 115 It It 157 45 60 115 121 115 6 6 87 120 87 ) 155 ) Lbs. Packed 30 35 133 146 9 134 133 30 7 32 131 107 29 32 19 tt 31 133 74 74 31 31 54 117 118 It 117 158 42 53 119 123 118 5 6 90 123 90 ) 150 ) Yield 96.8 100.0 107.2 91.3 160.0 107.2 106.4 96.7 100.0 106.6 104.8 71.1 93.5 106.6 100.0 It K 106.4 98.7 98.7 100.0 104.2 100.0 101.6 102.6 It 101.7 100.6 98,7 88.4 103.5 101.7 102.6 83.3 100.0 96.7 102.4 96.7 96.7 Total 3009 3007 100.7 DUP050316115 Su mma r y o f #10 b l d g , h io b b c t io h r e p o r t f o r a u g u s t 1935 Fo. of Batohoa 2 6 5 2 1 2 1 1 4 4 2 1 2 1 2 2 Code RT-232-D RT-219-D RT-347-B RT-354-B RT-359- RP-7971-D GY-7295-D aY-344-B Y-7888-1) Y-299-D Y-359-D Y0-38-D BT-125-D B1-159-D 3-63-D 0L-7906-D Lbs* Struck 150 690 625 174 35 12 7 9 348 124 188 54 90 60 241 205 Lbs. Packed 148 717 664 180 35 11 7 9 295 120 189 54 95 53 246 188 Yield 101.4 104.0 106.2 103*5 100.0 91,7 100.0 100.0 84.8 96.8 100.6 100.0 105*5 88,4 102.0 91.7 Total 3009 3007 99.5 DUP050316116 4. bsc ap: ION Colors transferred from semi-works in August , 1935. Toners Bxt, Colors Tallows Croons "BP" Lakes RL* Lakes Maroon Toners P.T.A. Toners Toner Pulps Maroon Toner pulps 1688# 56 835 130 343 281 684 127 79 7 7* DUP050316117 Material transferred during August* 1935 from Researah Semi-works Lot 4228 423# 4231 4232 4256 4257 4258 3259 4280 4223 4235 4236 4237 4238 4239 CE-200 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 Color Code BT-232-D It ft ft II n ft tf it ft RT-359-D RT-34If 7-D II ' `1 .se.i-.y Lbs 75 75 78 78 78 74 77 72 73 77 187 137 139 137 136 135 Cost Group unit 2 $109.11 2 2 2 2 2 2 2 2 2 1 137.43 2 114.83 2 2 2 2 Total Cost 4242 2 01-512-2) 56 2 5.12 4245 3 Y-299-D 361 2 9.30 4246 3 Y-7888-D 312 2 8.61 4247 3 Y-180-D 112 2 ? 4220 10 YP-324-D 569 1 131.83 4229 4248 11 GT-68-P 79 100# 1 56.29 11 GL-7908-D 281 1 36.57 4224 4233 4253 4299 4261 12 RT-399-D 12 ST-129-P 12 ET-219-D 12 ft 12 n * 123 ? 100# 226 109 226 2 1 1 1 1 211.37 197.08 205.74 4234 25 BT-7967-D 10 1 284.08 4249 25 BT-122-D 29 2 143.01 4250 25 II 29 2 4251 25 It 30 2 4252 25 It 29 2 4221 125 OP-399-D 225 2 130.25 4232 125 n 49 2 4226 4227 132 G-7891-D 132 G-7193-2) 79 2 15.89 41 2 14.69 DUP050316118 "T^-TT 8. MATERIAL IS PROCESS AS 07 SEPTEMBER 1, 1935 ___________ RESEARCH SEMI-WORKS OR-200 1. Coda IbSj RT-359-D 359 RT-354-D 174 3. Cod* Lba. Y-788S-3) 155 Y-202-D 25 Y-359-B 157 5. Code lba. 3-63-3) 240 10. Coda lba RP-7931B 12 BL-159-D 130 11. OL-407-D 44 12. RT-219-D 115 25. BT-125-D 226 BT-7923-D 08 115. RT-7745-D 50 129* 0X-309-D 377 DUP0503161 19