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NEWARK PLANT PIGMENT COLOR RESEARCH REPORTS
JANUARY - 1936
DU P050316620
PIGKBHT COLOR RESEARCH REPORTS JAHUABY - 1956
I - CHROME YELLOWS & GRANGES
Light Chrome Yellows (SCH) ..........................
Study of U.S. 2,023,928 (SCH) ...............................................
Canary Yellow (JBM) .......................................................................
Exe. Yellow K-3146 (K-8021) (JDM) .......................................
Primrose Yellow (SCH) ..................................................................
Y-403-D (K-8124) (JPM) .....................................
Med. Yellows of Improved Strength (SCH) .......................
Med. Yellow Y-299-D (JBM) ........................................................
-tr-'!S6Q'-Tl
Dark Medium Yellow (SCH)
I!!!! J
Chrome Orange Y0-38-D (HCM, SCH) ........................................
II -MOLYBOATED ORAHGES Molybdate Chrome Orange(SCH) .................................................. Molybdate Orange K-8074 (HR) ....................................... ..
* * (JDK) ...............................................
III -LEAD & LEAD MATERIALS
Lead nitrate Purification - Ferroeyanide Precipi-
tation (JK)
IV - CHROME GREEKS
CP Chr. Greens G-409D - 412-D Production (JK, ADR)
G-415-D and G-416-D
*
V - PIGMEUT GREEK B Pigment Green B (AS) ...................... .....................................
Pigment Green B Pulp, GT-68-P (EJH) ................................ Pigment Green Lake for Paper GL-407-D (ADR) .............
VI - HEW ORGASTIC PlfflEEHTS - Spec. Organic pigments (AS) ..
VII - PIGMEETS HT OIL Flushed Inorganic Pigments Flushed Lithol Red * PTA Pigments * Lake Red C
(HEB) * * *
....................................... ....................................... ......................... .. ........................................
VIII - PRIHTIEG IKK COLORS Hew Type Printing Inks - Rotogravure Inks (AJS) ..
IX - PHYSICAL STUDIES Spectrophotometric Study - Chrome Yellows (VC,HGY)
Colorimetric Study of Milori Blues (HGY, VC) .......... Physical Laboratory - Progress. Report (HGY) .............
X - mo. STUDIES - Pulverisation Studies (JK) .........................
XI - MISC. ORGAHIC PIGMEEHTS
a) Para Red - Blue Shade (JVS) ............................................ ..
*
- Yellow
...................... .....................
"
RA-26-D
w .................... ................ ..
* Dark, Improved RT-70-D (JVS) .......................
b) Lithols - Ca Lithol Toners RT-379 & 300-D (EJH)
Toner RT-8108-D (EJH) ................. Med. Ca Duol Toner RT-265-D (EJH) ...
Ba Lithol Toner RT-364-D * ...
Page
X 2 3-4 5-6 7-8 9-10 11-12 13-14
16-16
17-18 19-23
24-25 26-27 28-32
33-36
37-38 39-41
42-43 44-46 47-49
50-51
52-54 55-57 58 59-60
61-67
68a- z4 69-75 76-77
78
79-85 86 87-88 89-90 91-94 95-97 98-99 100-101
DUP050316621
2
SI - MISC. ORGANIC PIGUKTS (Cent.) o) HSad. Calcium Duol Toner ST-265-B (EJH) .................. d) Hansa Yellow Lake YP-324-D (EJH) ................................ e) Miser. Toners Red Toner K-7699 (2LP) ..................................... MHPA - IBS Maroon (JS) .................... .............. Alizarine Toner RT-332-D (HR) .......... .. f) Bordo Maroons Lacquer Maroon Toner RT-354-B (ADR) ... * " (PLP) ... g) Green Toner GT-337-B (EJH) ............................................... 2x) Misc. Lakes Orange Lakes K-8098 & 8099 (ADR) ............. Peacocck Blue Lake BL-164-B (EJB) .............
XII - SAW MATERIAL TESTING (AXCP) .............................................................
XIII- SEMI-WORKS PRODUCTION (HA) ................................................................
Page 102-103 104-105
106-107 108 109-110
111-114 115-117 118-119
120-121 122-123
124-
125-131
DUP050316622
PIGMENT COLOR RESEARCH REPORT LIGHT OHROMS YELLOWS
3&~/
SUBMITTED BY; /VFILE;
APPROVED BYt
DATE:
CHROME YELLO?/S JANUARY 1936
INTRODUOTION
In several recently developed develop# processes, such as K-8021, an essential part of the process is heating the pigment in aqueous suspension* Laboratory work has been undertaken with the object of obtaining similar products without including the heating step, since such a modification may be necessary to avoid infringe** ment of U.S. 2,023,928*
SUMMARY AND C (MC U75ION
Several experiments were made striking at an elevated tem perature and omitting the development after the strike, other con ditions being similar to K-8021* The best product, that struck at 180F, was slightly inferior to material made by the regular process* This study is being continued*
EXPERIMENTAL DETAILS
N.B. #481.
481-56. Study effect of high temperature strike in connec tion with U.S. patent #2,023,928*
In running the CS-7903 procedure at increased temperatures (110F, 140F, 160F, 180F) the cleanness and redness of the pigment increased in direct proportion to the increase in temperature.
481-38. Study treatment before washing on high and low temperature strikes; also heat one (struck at 80 F) to 160F after the addition of soda ash.
It appears from these results that treatments before wash ing offer no merit towards obtaining the desired properties. D, which was heated to 160UF before washing, gave a clean product.
DU P050316623
PIGMENT COLOR RESEARCH REPORT s t u d y o f ij .s . 2,025,928
SUBMITTED BY APPROYED BY:
PILE: CHROME YELLOW DATE: JANUARY 1956
INTRODUCTION
An intensive study of U.S. patent 2,023,928 and of prior art references possibly related to it has been started* Some preliminary work indicates that the products disclosed in this patBnt are not greatly different from products obtained by some of the early processes recorded in the literature. This study is being continued*
SUMMARY AND CONCLUSION
A number of pigments were prepared by the processes described in U.S. 2,023,928* They were similar to a previous series, 389*89, run 723~34, following some of the examples in the corresponding British Patent 403,762* A search is being made of the patent and scientific literature for processes likely to give similar production. Several samples have been pre pared not greatly different from the products disclosed in TT.S. 2,023,928, The literature survey and laboratory study are being continued with the object of obtaining products equal to the disclosed pigments by methods old to the art*
EXPERIMENTAL DETAILS
N.B. #481,
481-37^, Check examples 1, 8 and 6 of U.S. patent # 2,023,928,
These products although they were weaker and dirtier than those of the 389*89 series, were of the same type*
481*59, Study examples from the Chemical Journal article. See notebook for clearer details,
481*40. Continue study on 381-59B (example 3 from table I) by increasing the bichromate at the expense of the sulphate content.
Increasing the bichromate at the expense of the sodium sulphate improved the cleanness, greenness and strength of the pigment* Substituting sulphuric acid for sodium sulphate tends to decrease the strength even after increasing the bichrcmate from 76# to 82# per mol.
DUP050316624
PIGMENT COLOR RESEARCH REPORT CANARY YELLOW
3<'*
SUBMITTED BY: APPROVED BY!
PILE DATE
GHROME YELLOWS JANUARY 1936
INTRODUCTION
This titanyl-sulfate treated Y-180-D was given an initial trial in the plant, with subsequent manufacture of sufficient material for standardization as K8153*
SUMMARY AND CONCLUSION
Six batches of this yellow were made during the month on formulae based on those used in the semi-works study* On testing in rubouts, all of this material was a little on the dark side of Y-180-D standard* On reading the dry rubouts, how** ever, the plant material is markedly superior to the standard, indicating instability of the color, a property possessed in all probability by the standard* Light fastness of the plant mater** ial was much better than that of Y180D*
The strength of the color was found to be increased as the amount of salt in the strike was reduced* The reduction in salt, together with a long period of washing gives strong, green and clean tints*
Ink mill tests on two of the plant batches indioate that the color is superior to Y-180-D in resistance to lithograph** ic breakdown, bleed and to livering* The inks were softer, and exhibited shorter mixing time and longer flow than the standard*
A laboratory mix of Y403D and K-8146, the new primrose and excelsior yellows, respectively, was made to Y180*D depth and tested on the ink mill against Y180*D stMttojd* The mix was stronger than the standard and showed bette|^8g^^: stability* In ink tests it was superior to Y-180-D except for tUMBpat that it livered badly*
A mix of four batches of plant material has been made and set up as K-8153. Against standard Y-180-D the mix is dark in masstone and somewhat strong, red and clean on extension with slightly improved light fastness*
EZPERIMENTAL DETAILS
Eor Experimental Details see N.B, #492 p. 45-49*
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DUP050316626
FIGMENT COLOB RESEARCH REPORT KSSSLSIOH XSLLOW K-S146 (.*8021)
SUBMITTED BY: a p p r o v e d b y .:
PILE: CHROME YELLOWS DATE: JANUARY 19S6*
INTRODUCTION
The study of this color w as continued in the semi* works and plant during the month. A mix of plant material has been made and standardized under the.K8146*
SUMMARY AND OOBPLPBIQtt
SeatioWerka *
Til on batch the heating was omitted during the period of development, resulting in an off batch* In the two following batches the additional sodium sulfate was added before the development and in the strike, respectively* Both batches were dirty and had poor light fastness as compared to K-8146* It is evident, therefore that the additional sodium sulfate, used to increase the yield, must be added; just before washing the color#
Plant *
Two batches of this yellow were made during the month on the K-8081 oodd* The first was washed overnight* Its masstone was W*.slight but somewhat flat and changeable with satisfactory light fastness# The tint was a little strong and green and clean compared to K*80S1. It was stronger and redder than Y-309-D with better light stability*
The second batch was made with an increase in the amount of titsnyl sulfate, ^his batch was a little darker and greener than the first, with small improvement in light stability#
These two batches have been tested on the ink mill and are quite similar and superior to the other material made on this code#
A mi& has been made of the first five plant batches of E-80S1 and recoded as K-8146# Against E--8021 this new mix is a little light, green, and flat in masstone, v*s.strong, green and clean in tint, and is inferior in stability to light*
DUP050316627
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DUP050316628
PIGMENT COLOR RESEARCH REPORT PRIMROSE YELLOW
SUBMITTED BY: J' , APPROVED BY:
,,
PILE: CHROME YELLOWS DATE: JANUARY 1936
INTRODUCTION
Satisfactory results having tern obtained in the plant with a new primrose process laboratory work has been resumed with the object of improving its resistance to livering. An improved product with respect to livering has been obtained and a complete evaluation of this product is being made.
.>
SUMMARY AND CONCLUSIONS
1 In the development of a new primrose yellow K 7888 it had been found that stannous chloride gave a product slightly green and slightly dirty in aasstoae with better light fastness# It was found that by using both stannous chloride and disodium hydrogen phosphate at appropriate points in the K-7888 process a product equal to the Imperial primrose C-38349 in mas stone, strength, light fastness, and livering resistance was obtained* Further work is being postponed pending more complete evaluation of this sample*
EXPERIMENTAL DETAIL
N.B#481
481-34. Study of phosphate yellow to compete with 0-38349, using the following variation: Add sodium phosphate to 481-4A procedure {present semi-works procedure), and replace the bicarbonate with soda ash; strike at 70F instead of at 110F; decrease alum*
None of these variations aided in improving the 481-S4A product. Striking at 70F instead of at 110F. improved the strength slightly.
481-35 Study use of stannous chloride; further reduction of alum on the 340 type; reduction of sodium chloride in the strike.
It appears from this experiment with the use of both stannous chloride and sodium acid phosphate added at an optimum point of the process material equal to C-38349 can be made in the laboratory, The use of stannous chloride greatly improved the light stability.
481-41, Study on the 35B (regular S4A with the addition of tin and a reduction of alum) the use of sodium sulphate added after the tin and carbonate; lower temperature strike*
In this series no marked effect was observed by the addition of sodium sulphate after the tin and carbonate* Striking at 70F instead of 11QF resulted in a trace stronger and greener product*
j
j ! I
DUP050316629
m2** 48143 Continue further the use of sodium sulphate; also vary the amount"~of tin used#
Hone of these variations had any appreciable effect on the present laboratory control (35B)* The entire series showed an improvement over C>*58549 both in strength, tint and light fastness*
a>
DUPO 50316630
PIGMENT COLOR -EESEARCH REPORT
PRIMRO.SE y e l l o w
Y~403-D (K<*8134)
SUBMIT TIB BY: .APPROVED BY:
PILE: CHROME YELLOWS DATE: JANUARY 1956*
INTRODUCTION
This yellow has been inactive in the plant since the setting up of the new standard.
A review of yields obtained in the research, semi** works, and plant study of this color showed them to be much lower than desired* As a consequence, some work was don in the semi-works to Improve the process in this respeet#
SUMMARY AND CONCLUSIONS
Two batches of this yellow were made in the semi works to determine the effect on the yield, and also on the properties of the color, of completely precipitating the lead which has previously been rejected in the wash waters# In the first batch an excess of sodium sulfate was added to the color just before washing. resulting color was very light, clean, green and somewhat strong against Y-403-D with equal light fastness# It was even greener then &-788S and the yield was materially increased over that obtained in former batches#
The second batch was similar to standard formula except that the amounts of the striking components were increased to insure more nearly complete precipitation of the lead* A distinct lead edcess was present, however, at the end of the strike* The yield of this batch was equal to that of the first, and it was v*s*redder and v*v#s* Stronger* Against K-7888 the masstone was still a little greener*
It has been recommended that Y~305**D be replaced by Y-403-B; and at such time that production is resumed in the factory, the variable made in the first batch mentioned herein will be tried on a larger scale*
EXPERIMENTAL DETAILS
See N.B. 492, pp. 66*
DUP05 0316631
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3IJBLITTED 3Y: APPROVED 3Y:
:-ia. l i.t c o l o r r e s e ar c h r &pg r t
A2DIUL YiSII0/<3 OF IAFROYED STHJEl'.'GTK
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FILS: CHROME YELLOWS' DATE: JANUARY - 1936,
INTRODUCTION:
The preparation of medium Yellows of high strength by
,
striking in very dilute solution is difficult to carry out on a large
scale because of the high volumes involved. It has been proposed to |
avoid this by developing a continuous process in which the lead nitrate|
and sodium chromate solutions are added simultaneously to a mixing tube |
and the pigment slurry is then pumped to s filter. The results indi- 1
cate that products prepared by this proposed process are about equal j
in strength to those prepared by the normal precipitation process.
I
SUT-ARY Sc CONCLUSIONS:
1
Several samples of Chrome Yellow were prepared by the
simultaneous addition of .L. solution of lead nitrate and sodium chrop-ate to a mixing tube both with and without the simultaneous addition of water to the mixing tube to obtain more efficient mixing. without the addition of water the product obtained was approximately equal to that resulting from a reverse strike. The addition of water to the mixing tube produced a dirty mass tone and a decrease in light fastness but practically no change in strength.
| j f j <
| 1
!3PER1&.SKTAI DETAILS: See Notebook 452
' j
experiment 87 - Simultaneous strike in a mixing tube.
Results - Preliminary results indicate the process can be ; used in place of the usual striking, procedure.
DUP050316633
PIGMENT COLOR RESEARCH REPORT MEDIUM YELLOWS OF IMPROVED STRENGTH
SUBMITTED BTs APPROVED BY:
FILE: CHROME YELLOWS DATS: JANUARY 1936
INTRO DOC TI ON
The study of medium yellows Of improved strength has been continued from the past month* The effect of a number of variables has been determined and the process seems ready for Semi-Works study*
SUMMARY AND CONOID SI ON
The effect of the more important variables in the pre paration of a strong medium yellow was discussed in the December report A few additional variables were studied during the past month* Small amounts of barium chloride added after the strike increase the strength while larger amounts decrease the strength* Heating to 18003? after the strike results in a product equal to Y-328-D in leanness of masstone and only slightly weaker than the pigment finished oold* Decreasing the volumes t equal plant Y--359-D resulted in only a slight decrease in strength* Several exper iments using a Y tube mixing device resulted in products similar to those obtained by the regular procedure* The process seems ready for semi-works study*
EXPERIMENTAL DETAILS
N.B.# 452 and 497*
452-92* Study an increase of chromate and volumes on 452-84B procedure*
No marked effect was obtained by increasing the chromate two grams per mol* Increasing the volume of the chrome solution had no appreciable effect, however, a very, very slight dirtiness was observed*
452-94* Study a decrease in temperature; the addition of Barium chloride after the strike; the effect of heating after the strike*
A large decrease in temperature produces dirtiness, like wise the addition of Barium chrloride produced dirtiness of masstone*
Heating after the strike to 180F resulted in a red masston with a marked improvement in light fastness*
452-95* Compare the effect of increase of volume against standard pisaSt' "volume#
la this experiment increasing the Volume of the lead nitrate resulted in an increase in dirtiness of masatone* Cutting
\
DUP050316634
the volume of the chrome solution gave a product dirty and red in masstone versus control, hut somewhat stronger than B and C made with higher ohrcmate volumes*
497~14. Study effect of adding Barium chloride and sodium chloride when added to higher strength yellow procedure** Using increased amount of Barium chloride tends to increase the greenness of the mas stone and tinto Following the strike with sodium chloride had no marked effect tinotorially on the pi^aent obtained*
DUP050316635
BIGMMT COLOR RESEARCH R1FOET
IKDIPM mil>f Y -2.9 9 ~ D
q.iSUBMITTED BY:
APPROVED BY:
FILE! CHROME YELLOWS FILE: JiSTOARY 1936
IHTRODUGTIOH
The development section began a study of Y"399~D in this plant during the month to obtain a formulation which will give satisfactory material, especially from the viewpoint of light fast* 3X& SSft
SUMMARY AM) OCOTCTBIcafe
Trouble has been encountered in the manufacture of this color for some time, the main difficulty lying tfc-the inability to produce material of satisfactory light fastness*
Two lead nitrate formulae have been given a trial in the factory* The first was a check on the K-7031 formula (an old plant formula for Y-399-D) a mixture of sodium chromate and caustic soda being run in two portions into a lead nitrate solution* It is believed that this process should be satisfactory when pure lead . nitrate is used* This batch was dark and red in masstone against the temporary standard (15115) with a strong green tint and slightly better light fastness* Compared to the real Y-299-D standard (13645) the temporary one is vs green, silky and changeable, vs clean and green, ws weak, and vvs green with slightly worse light stability*
The second plant batch was made on a formula similar to that for Y-359-D except for the addition of csustic after strike instead of muriatic acid in the strike. The masstone of this batch was slightly light and flat and a little red against Lot 15115. The tint was strong, green and clean with slightly better fastness to light*
The study is being continued as production permits*
E3FSRIMEETAL DETAILS
E.B. #448 p 106
DUP050316636
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DU P050316637
PIGMSETT COLOR RESEARCH REPOST MEDIUM YELLOW
ji'1
SUBMITTED BY: APPROVED BY:
FILE t CHROME YELLOWS DATS: JAHUARY 1926
HTTP QDUC TI OH
Fro duetim of this yellow was continued during the month In the plant. The development section tried several changes in formulation to obtain red, weak tint material for use in Y*566D
SUMMARY AM? CONCLUSIONS
Seven batches were struck during January. On the first three, attempts were made to obtain material with red, weak tints by brushout test for Y366**B mixes* In the case of the first, the strike was Made at a higher temperature than ordinarily with a large increase in the amount of muriatic acid added to the chromate* It was a little dark and dirty in mas stone and ws strong, vs green and clean in tint* Light fastness of all batches was slightly better than standard* The second batch was struck at the usual temperature with sodium chloride and muriatic acid added to the ehr ornate* This material was a little redder and weaker than the first* Compared to standard the tint was equal in strength and vs red* The third batch was a check on the second exeept for an increase in temperature* The yellow was similar exeept for being a little dirtier*
A brushout on the first batch made (47028) showed it to be red against YS66*B and strong, green and clean on extension*
The rest of the month*s production was made on standard formula and ran a little flat in masstone, and strong, green and clean in tint* Light fastness was superior to that of standard*
EXPERIMENTAL DETAILS
See W. B. # 448 p* 76*
DU P050316638
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DUP050316639
PIGMENT COLOR RESEARCH REPORT DARK MEDIUM YELLOW
3L'/
SUBMITTED BY: SAPPROVED BY: <3^^^
Fill: CHROME YELLOWS DATS: JANUARY 1936
INTRODUCTION
The dark medium yellows as represented by Y-216-D have not received laboratory attention for some time. A brief study is being made with the object of developing a product similar to Y-S16D but of improved strength and light fastness.
SUMMARY AND CONCLUSION
A number of strikes have been made in Which three in gredients, lead nitrate, sodium chromate, and oaustic have been mixed in different ways* It seems desirable in all oases to strike at 130F or above and to heat to about 15QF to 180F after the
strike* The best results were obtained by adding sodium chromate plus caustic to lead nitrate and by simultaneously striking lead nitrate and a sodium chromate caustic mixture into water. The darker or redder shades are obtained by increasing the amount of
eaustie used* In the simultaneous strike a considerable excess of sodium o hr mate seems necessary to obtain maximum strength*
IXFSRBil^TAL DETAILS
N*B #497.
497-g* To obtain an improved dark medium yellow com parable to Y-2l6D*.
None of the variations studied in this experiment offered a lead towards improving the dark medium yellow Y-216-D*
. .. strike)*
Continue variations on 497-3B (simultaneous
Nothing of any value was obtained from this series* B,
the cheok on 497-3B gave a light, olean, strong pigment which was
much too light to match Y-B16-D* A and 0 made with an increase of Caustic soda in the one chrome solution (strike solution) were too red and dirty*
Study effects of striking simultaneously into varying amounts of chromate; add salt to chromate*
None of the variations made in chromate pertaining to
the material in the strike Jar showed an improvement* The addition of salt to the chromate gave a fair lead; this will be checked*
497<*9* Study a reduction in chromate and oaustic; also
effect of adding molybdate to erne chrome (strike solution) solution; study striking at 130F*
DU P050316640
In this series 0 made at 1S0F, without any molybdate gave the most promising lead, being the greenest and cleanest of the series*. The addition of molybdate resulted in a very red yellow*
49740b Study a reduction of sodium hydroxide and the omission of sodium chloride; also a further increase of strike temperature* Study these same quantities struck in the regular striking manner {chromate, etc* into the lead solution)*
B made without salt resulted in a very red yellow* In* creasing the strike temperature to 150F resulted in a some-* what light product accompanied by on increase in strength* It appears from this series that the regular striking method gives the better product; this being illustrated by 0*
DUP050316641
SUBMITTED BYt APPROVED BYt
PIGMENT COLOR RESEARCH REPORT
3W/
QHROMB ORANGE Y&-58B
S,c//k*^ ^
FILE: CHRCMS ORANGE DATE: JANUARY 1936
INTRODUCTION
Tlie study of YG-38-B has been continued from the past month.
The experimental work has consisted chiefly of a continuation of the study of the effect of possible impurities in the raw materials used and a study of the effect of various treating agents. This work is being con tinued#
SUMMARY AMD OONQLUSICUB
Experimental work on the effect of various possible impurities
was continued from the past month* The conclusion of the December report that impurities seem a minor factor still appears correct* The use of sodium acetate from crude acetic acid resulted in no improvement*
Experimental work on the effect of agents, such as gaxdinol, oleic acid, citric acid, H.T.P* alcohol, amyl alcohol, ammonium chloride and strontium nitrate gave no indication that these agents were of any value. A number of similar products will be tried during the next month*
results*
Lead liquor from plant water and distilled water gave similar
Attempts to prepare a bright TO-38-D by the use of lime were unsuccessful. All products obtained seemed poof tinctorially. A few ex periments on the use of lead nitrate gave negative results.
The effect of treating a washed slurry of Y0-38*D with alum and acid was determined* The results are similar to those obtained several years ago* Either no effect is noted with small amounts of alum or acid or a dark yellow masstone and high finish results* The study of the effect of acid is being continued#
MESRjMENTAL DETAILS
N.B. #486.
486-65* To study the effect of impurities from water* Lead liquors were made in the laboratory using the regular plant water and distilled water#
The lead liquor made using distilled water gave a
foduot which is a little brighter than the other members of this series# is difference, however, may be due ohiefly to experimental conditions and not t the difference in the type of water used#
DUP050316642
486-35 Check results obtained in series 486-65*
It is quite apparent from the results obtained in the series" that lead liquor made using distilled water has no greater tendency to produce brighter pigments than those made using tap and plant >mter*
486-66* Study the effect of dilute strike and of a long stirring period; also add bichromate during development to increase the 0r04* excess*
STo marked improvement was observed from the four hour stirring period after the development. Dilute volumes for the lead liquor resulted in light products. Adding bichromate during development did not improve the pigment,
486-67* Study the effect of the use of white lead, and the use of stannic chloride in the lead liquor*
There was a brightness observed in the pigment made using white lead that was considerably outstanding versus the con trol made from lead liquor. However, the product was very very dark and weak versus I0-38-D standard. It appears an increase in acid (in the white lead base) would tend to produce a lighter pigment. What effect this will have on the brightness cannot be estimated*
486-68. Study long stirring periods as in 66c, also study use oF"""acetic acid in a dilute strike*
There is a slight indication that digesting for four hours at 205F after development gives a product very very slightly cleaner than the control. Acetic acid in the bichromate resulted in a brighter and cleaner product than the control of this series* None were near the standard in brightness. These leads will be cheeked*
486-69* Study further the use of white lead*
Increasing the amount of lead nitrate used with the white lead, here, indicated a very very slight improvement in brightness*
486-70* Study the effect of H.T.P. alcohol, amyl aleohol ana '^SSponol" when added to the lead liquor*
Here, a noticeable improvement in brightness was ob tained from using amyl aleohol in the lead liquor; this will be given further study. H.T.P. aldtiol and "Duponol" added to the lead liquor gave dirty pigments*
DUP050316643
486-71* Study concentrated strikes, with, and without acetic acid, stirred for a long period at high temperatures* Here, a slight inconsistency was observed in the effect of holding for four hours at 205F* A1 and A-2 are very close in masstone, while B-l and C-l are somewhat cleaner than B-2 and C-2* Hone of the variations have shown any marked improvement over the control*
486-78* Study further the use of amyl alcohol in the strike "and lead liquor; study a four hour development period on the 67A procedure*
In this experiment the four hour development period gave a very slight improvement in brightness* Here the use of amyl alcohol did not check the marked improvement obtained in the 486-69C experiment*
486*73* Study effect of purifying the lead liquor with feathered' lend before making an orange; also study the use of amyl alcohol, and Ammonium chloride.
Here, the purified lead liquor gave a product consider ably darker than the control, but no marked improvement in brightness. Following the strike with Ammonium ohloride re sulted In a light pigment, hit with no improvement in bright ness* Amyl alcohol added after the strike had no marked effeet*
486-74* Study consistency of the present laboratory standard prosedure; also add gloss tot to the orange before developing.
The addition of gloss white resulted in a very high finish but dia not add to the brightness and cleanness of the pigment. Very poor consistency was obtained*
486-75* Study again the use of purified lead liquor; also try using crude acetic acid in the lead liquor; study the effect from washing the pigment before development*
Here again the purified lead liquor (purified by passing over feathered lead) gave a dark weak product. Crude aeetio acid resulted in a very dark weak product* Washing the pigment be fore developing resulted in a light dirty pigment.
486-76* Study further the process of washing the struck pigment before developing; add bichromate to the washed pigment be fore developing, also try the use of calcium chloride in the base*
The addition of bichromate to the washed pigment in its unbleached stage resulted in a dull dirty product* Treating the base with Calcium chloride gave a light masstone, but no improve ment in brightness was obtained*
486-77* Study Calcium oxide procedures used in 1918*
t
None of the calcium oxide procedures gave a very deep orange* Another run will be made to study further conditions necessary to obtain greater depth from these me theda
DUP050316644
vT'
486*78. Study the use of calcium oxide when added to Bicarbonate arid struek at a boil; also study the effect of remov ing the carbon dioxide by means of a suction*
Heating the calcium oxide treated pigments tends to produce depth and strength. The addition of the calcium oxide to the lead liquor at very high temperatures gave a much darker pigment than was obtained in the 77 series* Developing by means of a vacuum did not give very satisfactory results.
486-79* Study striking at 140&51; also simultaneously striking sodium bicarbonate and sodium dichromate.
Simultaneous strikes gave very yellow and strong products. Striking at 140F gave a very light orange*
486-60* Study the problem of development on the 67A. procedure, tthe regular laboratory standard procedure).
Here it appears that boilingjdntil the foam breaks helps to brighten the product. Treating after the development period does not seem to be very effective* Striking at 140F, and then bringing to a boil to develop the orange resulted in a light orange*
486~81 Study the part of the procedure pertaining to time of development and striking.
Striking in thirty minutes (810) resulted in the bright est pigoaent of the series? this might only be due to experimental differences. Preparing the white base afc a boil and boiling for 30 minutes did not have any effect on brightness. Stirring for 30 minutes at 200F had no favorable effect on the brightness.
486-82* Check 810, but use the regular procedure for preparing fhe "Tead-base; also study the effect of manganese salts.
Boiling the lead base, otherwise like 81C resulted in a dull dirty product.
Using manganese salts tends to produce very very brown pigments.
486-85, Study the use of Kadox, citric acid and strontium nlirate*
The addition of Kadox has little or no effect on the pigment. Citric acid used after the slurry was heated to 212F gave no improvement in brightness*
Here strontium nitrate appears to give a slightly lighter and cleaner product. This may be only an experimental difference, therefore will be checked.
486-84. Study further the use of strontium nitrate; also molybdate*
DUP050316645
-5-- 2^2 .. The position for adding the strontium nitrate affected the depth hut had little effect on the brightness. Molybdate added at a boil during the development period gave a product ws brighter than the control* 486-86 Study various K procedures in the laboratory {used in plant: io make Y0-58-D). Two K procedures of Y0-38-D made in the laboratory (K 5946 and K7536) gave dull products versus the standard material when rubbed out 486-87. Study effects from Y.P.S. method of purifying the lead liquor} also study the us of a sulphuric acid treatment after washing the pigment four waters. Using lead liquor purified by the Y.P.S. method gave a slightly darker pigment than the control but gave no improvement in ^either brightness and cleanness of masstone* Treating the washed pigment with sulphuric acid gave a brighter pigment with a yellowish cast, and a high finish under tone. 486-88. Study sulphuric acid, alum and oleic acid treat ments on the washed pigment. The use of oleic acid tends to increase the dirtiness of the pigment. Alum gave a high finish, but no improvement in oleanness of m&sstone. Sulphuric acid treated pigments were quite yellow in undertone, with a very undesirable finish. No improvement was obtained from this series.
'
DUP050316646
PIGMENT COLOR RESEARCH REPORT MOLYBDATE PEPQMS ORANGE
jd''*
SUBMITTED BY: S- &< APPROVED BY:
FILE: MOLYBDATE CHROME ORANGE DATE: JANUARY 1936
INTRODUCTION
An intensive study of tills color was undertaken in the laboratory during the past month* This work can be divided into two parts, first a study of the K-8074 process to determine the cause of instability on large scale operation, and second the development of a process giving a produot from 20$ to 40$ stronger than the Rex Orange*
Laboratory work to date indicates that greater variations in tinctorial properties result from slight variations in operating conditions than from slight variations in the quantities of chemicals used*
A new laboratory process has been developed giving a produot similar to the Red Orange C 3B041 but more than 80$ stronger. This study is being continued*
SUMMER-r m> CONOIDS ION
Semi-Works difficulties with the K 8074 process made it necessary for the laboratory to resume work on this process* Lead nitrate liquor and bichrome liquor were found equal to the corres ponding crystals. Slight variations in molybdate had little effect bat l^rg variations influenced the shade and strength* There, appears to., to" an optiaun amount above which the tint is weak and yellow ana below which the tint is weak and blue* Occasional strikes have come tot flat and slightly weak versus a corresponding control indicating variations in operating conditions may be a more important factor in brightness of mas stone than small variations in the quantities of ikgrcdi&his need*
A new laboratory process has been obtained giving a product Similar to the Red Orange but considerably stronger* The process in volves, the addition of a mixture of sodium chromate, sodium molybdate, and sodium sulphate to lead nitrate* Laboratory strikes are in ..pastogjtj.ees to determine the optlmun ratio; the optimun precipitant .hsjfeamce, and the quantity of nitric acid required after the strike to OsbMih conversion to the tetragonal form*
B?AL DETAILS
IT.* #458 and #497.
Ctvuommppjaaxrwe lxau ubvoj j r-ab.tory mtttovlyxbyduatueawb j i.tuhu pj j xlcal nu .*t material oom.pare laborat or y process with the semi-works procedure*
The plant molybdate gave a duller and very, very slightly peg* product than the laboratory material* Using plant lead liquor
DU P050316647
in the K 8074 procedure gave a much stronger and yellower tint than ^ using Crystals* All were worse in light fastness than E 8074* The Semi-Works procedure gave a stronger product than the laboratory formula#
497-1# Study variation in molybdate* In this experiment decreasing the amount of molybdate salts resulted in darker masstones, and bluer tints. However, in some eases no effect in strength was observed; the same was also true with brightness#
497-2* Study a more alkaline strike, making variations in acid after the strike, and study the use of sodium sulphate*
Changing from the use of Sodium Bichromate to Sodium Chromate gave a duller light product greatly improved in strength* A slight variation (in the chromate procedure) of nitric acid, and sodium sul phate had no appreciable effect on the products obtained*
497-6o In this experiment stirring overnight (chromate procedure) and heating to 160oE in 30* had a deleterious effect on the pigment* "D*1, stirred two hours after the strike was the brightest of the series#
497-7* Continuation of 497-6 D# Study variation of hrornate, sulphate, molybdate, ratio; study use of salt in the strike#
The control was a very poor check on 497-6D* A reduction in molybdate and sulphate resulted in a very poor orange* Salt used in the bichromate resulted in a light milky orange* Hone_were very promising*
497-11# Study higher precipitant balance; neutral strike; low molybdate on the bichromate procedure*
Increasing the precipitant balance favored an increase in depth* Replacing the sulphuric acid with sodium sulphate gave a large increase in depth* However, an increase of acid together with a cut in molybdate gave a pigment somewhat lighter than the control * but not as bright#
Continuation of 497-6D* Balance strike to deter mine optimum chromate, sulphate and molybdate ratio to yield maximum strength and bti'lglytness
Hone of the eaabinations of chraaate-sulphate and molybdate studied gave an improvement over the control* All were on the red(top) weak and blue (tint) side of the control*
497-15* Study on 497-2C the stability of the formula, using a slight reduction in molybdate; lower precipitants#
o
lowering the precipitant balance, here, resulted in a very# very slightly weaker and bluer tint*
Stirring 30 minutes before adding the alum had no marked effect on the pigment* Decreasing the molybdate from 10.5 to 10 gave a pigment very slightly stronger than the control*
DUP050316648
PIGMENT COLOR RESEARCH REPORT MOLYBDATES ORANGE g-8074
g 6'/^
SUBMITTED BY: A/.
FILE: CHROME ORANGE
APPROVED BY: ^DATE: JANUARY 1956
INTRODUCTION
A study of molybdated orange, (based on the formula for SW 7540), was made in the laboratory, to determine the factors producing light, flat, and weak semi-works material. Later plant and semi-works runs have been quite close, tinctorially, to the K number (8074) using some of the information developed in this labor atory, study.
J
SUMMARY AND CONCLUSION
This series of experiments included the study of a number of variables. Factors auph as alkalinity of strike, variation in amount of sodium molybdate, delayed addition of treating agents, and variation in the amount of sodium bichromate were studied. No single experiment gave results directly comparable to the previous semi-works batches. However the work done indicates that a combination of several of the variables studied would produce a light, flat and weak pigment; particularly, a large lead excess produces weakness; high acidity gives a weak, blue product; high molybdate results in a lighter, stronger, yellower product.
MPEBIMENTAL DETAILS
N.B. #440 p. 52
Study variation in amount of sodium molybdate
A - Control-check SW 7540 B - Increase molybdate 10% C - Decrease B 10%
Results
B vs A - vs yellow, vvs flat,-; vs str, s yellow - Light fastness vvs better
C vs A - vs red, vs flat,-; s wk, s blue - Light fastness - s better
p. 53
Observe the effect of using different amounts ,of soda ash in the lead base
A - Control-cheek 440-52A B - Decrease soda ash 25% C - Increase soda ash 25%
DUP050316649
Results
-2-
xn
B t s A vs refii vvs flat,-; s wk, blue - Light fastness - ws better C vs A vvs light, vvs bright,-; vs str. vs yellow - Light fastness - equal
P. 54
Study variation in amount of sodium bichromate and excess sulphate in bichromate.
A - Control - check 440- 52 A B - 5 grams extra sulphate in bichromate liquor
0 - Increase sodium bichromate 10$ D - Decrease sodium bichromate 10$
Results
B vs A - O.K., vs flat, vs yellow; vvs wk, vs yellow - Light fastness - equal
C vs A - vs dk, vs flat, vs blue; equal, s blue - Light fastness - vs better D vs A - s It, vs flat, vs yellow, vs wk, yellow - Light fastness - equal
F. 55 The effect of delaying the addition of sodium bicarbonate.
excess.
Due to an error in weighing this series had a strong chromate
Rubouts showed all of the series to be dark and muddy in masstone, poor in light fastness, but much superior to the K number in strength. This information has been passed along to the research group.
P. 56 The effect of delaying the addition of sodium bicarbonate.
A - Control - check 440-52
B - Sodium Bicarbonate added immediately after strike
CP_
n w
"
"10 minutes
"
"
n
tt go
n
n
h
Results
B vs A - O.K., O.K, O.K; vvs wk. O.K. - Light fastness - equal C vs A ws It. vvs flat, o.k; vs wk, vs yellow - Light fastness - equal D vs A vvs It, vvs flat, O.K; vs wk, vs yellow - Light fastness - equal
P. 5? Observe the effect of delaying the addition of alum
A - Control - Check 440-52 A
B - Delay adding alum 10 minutes
G- "
"
"20
"
Results
B vs A O.K, O.K, O.K; O.K, vvs yellow - Light fastness - equal G vs A O.K, ws flat, O.K; vvs wk, ws yellow - Light fastness - equal
DUP050316650
FIOMBHE COLOR RESEARCH RSPCRT MOLYBDATBD CHROME QRAKG1 YD*8Q74*S
3 l-'T
SUBMITTED BY: APPROVED BY:
Ue UJUo .
BILE: MOLYBDATED CHROME GRAMSE DATS: JANUARY 1956
MTEODtJCTIOH
Following an unsuccessful plant trial of this color last month, the formula was returned to the semi-works for revision* A considerable amount of work has been done* Satisfactory material is now being made,on a slightly revised formula in both the semi* works and plant*
A new formula giving an orange of greatly increased strength is being tried in the semiworks*
SUMMARY AMD OOHgLgSMMS
Semi^Works
A total of eighteen mall batches of this color were made in the smi-works during the month* The first six of these were run on variables in molybdate, different lots and quantities being used in an attempt to ascertain the cause of the yellow, weak material being produced* Results were inconclusive, all of the six batches being distinctly yellow flat and weak against K80?4*
The K*8074 formula was then checked using crystalline materials wherever possible, and a new lot of molybdatea This batch was close to the Renumber, being a little on the dark, bright side, with satisfactory strength^ and a somewhat yellowish tint* The institution of lead nitrate liquor for crystals gave a little lighter product that was vs weaker* The further substitution of solium biohrcmate liquor for crystals gave a little cleaner, weaker and bluer color than the previous batch* An increase of ten peroent in the amount of molybdate increased the strength to that of the K-number and gave a somewhat yellowish mas stone and tint* This batch was cheeked except for a five percent increase in bichromate, which gave a very faint biohrcmate excess after strike* The result was a vVs dark, red and bright masatone with a vs strong and blue tint* Light fastness on all of the batches ran ssmewhat inferior to that of K*8074*
Two batches were mad.a. Inwhich the addition of the treat* ing agents, alum and sodium biSsS&aaSlSs, was delayed twenty minutes* "Both batches were a little weak and flat, but not nearly as much so as the material made at the first of the month*
^ A new laboratory formula was given a trial in the semiworks. It differs from the present formula in that the strike is made at a much higher pH which is subsequently lowered by the addition of acid. Material forty percent stronger than K-8074 was obtained in the lab* oratory using this formula* In the semi-works the first trial was blue, flj^and weak* On a slightly revised formula, material about
' >'*
DU P050316651
--8* twenty-five percent stronger than IT-8074 was obtained, the masstone, however, being a little blue, dirty and chromy. A oheek batch was s little lighter and flatter Plant
Three 3-mol batches of this color were made in the factory* The first of these was a cheek on the K-8074 formula* - as was the off-batch made last month, except for a five percent in crease in the amounts of sodium bichromate and molybdate* This batch was on the dark, red, bright side of the K-numbers, with a weak, red tint and y v s worse light stability. We have been unable to isolate the cause of the yellow, flat appearance of last month*s batch except to conclude that it was a result of a combination of unfavorable conditions; ie., too high an exoess of lead, not enough molybdate, and too high acidity* The first two items may have heen the result, of inaccurate analyses*
The second batch of the month was made with an increase in bichromate and molybdate over the former one. It was a little flat, dirty and strong against the former batch. An increase in soda ash gave a lighter, yellower product*
This study will be continued in the semi-works and plant* EXPERIMENTAL DETAILS
Par Experimental Details see N.B. #448, p. 193-195. W.Bj^>#493, p* 75--85
DUP050316652
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DUP050316655
PIGMENT COLOR RESEARCH REPORT LEAP NITRATE PURIFIQATIOM -
TOR0GTANID1 PRECIPITATION
3^/i3
SUBMITTED BY: / > APPROVED BY:
FILE: LEAD & LEAD MATERIALS DATE*. JANUARY 1935*
HISfeODUOTIOK
Work has heen continued in the semi-works on the purification of lead nitrate by the precipitation of the eopper with sodium ferrocyanide.
SUMMARY AND COHCLUSIQHS
Twelve purifications have been carried out. The following variables have been found effective in increasing the f iltrati onr /"<//* /
1* An increase in temperature - 150F is the temperature now being used.
2. A change in filtering medium frcsa single 4/0 duck cloths to doxible XX chain weave cloths.
3. The addition of filteroel to the slurry* One to three pounds of the filter aid were used*
The last variable was also effective in cutting down the time necessary to obtain a clear filtrate at the beginning of the
filtration cycle. No difficulty was experienced in obtaining adequate purification as jtidged by the analysis of the resulting solutions and the quality of the Y-359-D made from them, in which, however, a slight dirtiness was observed, possibly due to a red dye bleed from the filter press used. A series is being run to check this matter.
On the basis of the results of one batch, it appears that "Lightain" Agitation will be satisfactory*
DUP050316656
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MCPBRnflEWTAL DETAILS
See Notebook #492, pp* 99-137* Additional results -are given on the batches mentioned in the December report
Batch
#Fb(N0g}g
SW-7549 7355
7560 7563 7565
7574
7578 7586 7620 7621
7624 7637
7640 7647
7649 7655 7660
7664 7667
7674
265 265 259 248 257
129
196
234 250 250
200 173
196 195
19 196 15 19
164
Iff
# Y*F*S* Filteroel #Filtereel
-... ia
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5*34
6*84 5*34 5*09 5*29 2*67 So 69
0?8 4*84 4*84 3*87
3*56
3*80 3*84 3*78 3*80 3*55 3*55 3*55 4*30
i 3
5
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Volume Gals*
120
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tt
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II
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It tf
W
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tt tt
tt
Batch
749 7555 7560 7565 7565 7574 7578 7386 7620 7621 7624 7637 7640 7647 7649 7653 7660 7664 7667 7674
Precipitation
Temp*
Time
_______
60
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60 110
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n tt 150
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5 30
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Peed Yield
#60'*
*046 #046 *044 *043
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m *053 #048 *055 *031
*0005 *00011 *0003 *0002 *0001
*0091 *00016 *00019 *0001 #0001
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DUP050316657
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R. * rubber recessed plate press* p.F. - $203, wooden plate and flame press.
* gravity filtration. ** s sent to press without dumping residue from previous batch.
Batch
Press
Cloth Agitation Time of Filt*
P.C*
Recycling Rate
Yol*
____________________________ Min*_______ G-al/SQ.ft/hr* eu.ft*
7549 7105 7550 7503 7505 7574 7578s 7586 76 gO
7681 7084 7037
7640 7647
7048 7055 7660 7664 7667 7674
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*19
Yellow
Rubout versus Standard
Batch # Batch#
MasstQneDrawdown Strength Tint Lightfastnea
7554 7556 7561 7566 7572
7579
7584
7588
7625
7639
7638
7043
7549 7555 7560 7565 7565
7574
7578
7586
7620
7621
7624
7637
v.s.red & eln*
sred & oln*
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v*s*dark & red
s.red
v.v. s.dlSrty
v.v.s.red & oln* O.K.
s * str * s*tr* s.str* s*str* s.str.
0*K.
s*red & dirty
s*red & dirty
s*red
v*v.s.red,v.s* dirty v*s.red
dirty,
s .red red,s* dirty s*red & dirty
s*red
s.str. v*s*str* str* s.str.
v.v.s.red s*str.
v.s.dirty & flat s.red
s.str*
s*gm. better s.grn* better
s.cln* s*b"etter
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oln* v*v*s.red better & oln. s*red & s*better cln v.s.clm* s*better
eln*
s.better
s.cln* s.better
sgr*& eln*
s.gr.ft cln.
v.s.better s,better
DUP050316658
Yellow Batch #
7654 7655 769
Parif*
Batch
7640 7647 7649 7653
Rubout versus Standard
Masstone
Drawdown Strength Tint
Light* fastness*
s*grn*& dirty
s#red
s*str*
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s.str*
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s*str.'
v*v,s*grn*vs*dirty v.s*red s*str*
s*grn& clru soln seln
s*ela*
s*better
better better s*better
DUP050316659
FIGMENT COLOR RESEARCH REPORT C.P. CHROME GRl^S. G*409^ * 413D PRODUCTION
SUBMITTED BT: APPROVED BY:
PILE: CHROME GREEN DATE: JANUARY 1935,
INTRODUCTION
One batch of each member of this line was made in the plant for stock.
SUMMARY AND CONCLUSIONS
Difficulty was experience from redness in the greening yellows and the corresponding olive and dirty masstones of the greens* Two of the abovejfreening yellows were improved in a measure by the addition of fifty pounds (actual weight) of acetic acid before greening* It seems probable, therefore, that this trouble can be corrected by an increase in the acid in the strike*
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PIGMENT COLOR RESEARCH REPORT GP CHROME GREENS. G415~P JUMP G~416-D
3<-'n
SUBMITTED BY: APPROVED b y :
& cA.
FILE: CHROME GREERS * DATES JANUARY 1936
3>
ESTROIOCTIOH
Three hatches of each of these colors were made on the formula (439-89A) recently used In an effort to obtain a strong type G*389D* This was done to restandardize G-415**D and G-416-D {G390D and G*391D standardized for rubber)* This was necessary because the original standards contained copper*
SOMMARY AND OONCIUSKUB
The formula actually used was a modification of the lab** oratory formula previously reported as SW 7530 and G-389-D, plant bateh 46839 *
These batches showed a decided tendency to flatness and chalkiness in masstone by rubout against both the rubber ana regular G-389** line standards* Against G*390-D standard a mix of the three G-415**D batches brought to equal depth with a little G-416-D* showed about 5$ extra strength* A similar G*416*D mix was about 10% strong versus G-391*B standard*
Satisfactory new copper-free standard mixes were made using the six batches made#
See Table 1*
Mixes have been made and submitted for standard in rubber as follows, the mixes containing a small amount of lead sulphate to allow for the extra strength of this productian:
G-415>B, 16662 consists of:
G-415--D "
G**844*iiD
Fb34
47118 47156 47183
46618
1330# 1470#
1098# 190# 285#
4363#
G**416*D, 16698 consists of:
G-416-D *
G-415-D <
PbS04
47119 47155
47 205
47183 46682
168031 18351 178C
3713
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DUP050316664
PIGMENT COLOR RESEARCH REPORT
dj.
SUBMITTED BY:te APPROVED BY:
PIGMENT GREEN B
*' PILE: PIGMENT GREEN B ^ DATE: JANUARY 1956
INTRODUCTION
Work was continued in the laboratory this month on the problem of developing a dry lake of Pigment Green B for dispersion in rubber and for general evaluation*
The investigation on the preparation of dry colors for paper coating continues to be delayed, pending completion of the studies on GL-407-I)#
SUMMARY AND CONCLUSIONS
Preparation of a dry lake of Pigment Green B for rubber has been completed* The product K-8172 is a fifty per cent Pigaent Green B Lake on alumina hydrate - barium resinate substrata. It disperses well in rubber, 107 parts being equal to 100 parts of both the corresponding later dispersed pulp and Green IF D Standard, on an equal pigment content basis* A sample is to be submitted to the Rubber Chemicals Dept, for evaluation.
The work this month was devoted chiefly to studies in volving minor modifications of the laking formulation* in order to obtain exactly 50 per eent toner content of the lake and complete precipitation of the water dispersible pigment on the substrata*
The use of barium chloride in place of sodium chloride in breaking the pigment-rosin soap colloid results in complete floceulatian of the pigment and slightly softer texture and consequently slightly improved strength as judged by rubber tests. The rosin in the pigment is in the form of barium resinate instead of the free resin acid or soluble sodium resinate*
Altho diglyeol stearate gave some improvement in previous products the recently improved lakes are not benefited by diglyeol stearate#
Lithographic varnish rubout inks of K-8172 show it to be equal to the best prepared previously and indications are that this one product may be satisfactory for both rubber and general application, excluding paper coating* The problem of development of a Pigment Green B Lake dry powder in the laboratory can be considered complete .and this new pi^aent is now ready for semi-works development, pending acceptance of K-8178 for rubber#
DUP050316665
EXPERIMITTAL 1STAILS Exnt* 34. 55 and 1. N.B* 482 p 106. IIP and 112 respectively* Substitution of BaClg for Had, for precipitation of the
dispersible pigment results in slightly softer texture ana slightly increased strength, and is preferable, especially since barium resinate instead of free resin acids or sodium resinate is present in the lake
The use of "Duponol" WA and diglycol stearate have no benefical effect upon the dry pigment.
Variation in the quantity of precipitant (BaClg) influences the flocculation and physical properties of the pigment* Sufficient BaClg to give complete flocculation is essential in obtaining pigment of the desired texture and strength*
Bxpt* 57 HB. 462 p* lid Tariation in alumina hydrate base from 50/ll to 30/l5 has not appreciable effect upon the pigment* The 30/15 base is prefer able* EXPt* 58 HB 482 p 118
Substitution of CaClg for BaClg as the precipitant results in a lower yield and offers no advantage over BaClg*
The quantity of BaClg*2HgO was varied from 4 to IS grams per SO grams of Pigment Green B dry basis and 6 grams I Wood Rosin. Com plete floeculation and maximum strength was obtained using 8 grams BaClg*2HgO*
Expt* 39 & 40* N*B* 483 p* 130 and 122 respectively.
Variations were made in the quantity of alumina hydrate in order to obtain an exaet 50 per oent Pigment Green toner content of the dry product* The composition of the 50 per cent lake, K-8172 as estimated from the amounts @f Ingredients employed and yield obtained, is probably as fellows:
50 parts Pigment Green B 100% toner basis 30 parts Alumina Hydrate 20 parts Barium Resinate Actual Fe analysis of K-8173 gave 4*29% Re. equivalent to
4*29 x ll*9(factor for P.G.B.) * 51*05% Pigment Green B
DUP050316666
PIGMENT COLOR RESEARCH REPORT PIGMENT GREEN B PULP, GT-68-P
jt-/?
SUBMITTED BY: B APPROVED BY: ^'
PILE: PIGMENT GREEN B DATE: JANUARY 1956
'Tf.
INTRODUCTION
Production, was started in the plant on GT-68-P in order to build up the required stock of 1500 pound dry for rubber, A total of three batches were made under Development Section supervision*
SUMMARY AND CONCLUSIONS
The first batch was made to check Lot 41875 except that a new type Turkey Red Oil (Jacques Wolff) was used in preparing the Cadmium Soap* Because of the partial oxidation of the Sodium Bisulfite used in this batch the Nitroso Beta Naphthol nyas hot fully ester if ied with the result that there is a large excess of Ferric oxalate and of Cadmium Soap in the finished pulp* The resultant color was therefore weak and. dirty in both rubber and paper and with a yield of only 70$ of estimate* In order to oonsume this off batch it will be necessary to mix off small portions of it in subsequent production of rubber material. Steps have been taken to prevent a recurrence of production of sub-standard material by arranging to discard all Sodium Bisulfite that has deteriorated (hard ened in barrels) and by seeuring analyses of ell material under suspicion* It has also been decided that subsequent orders for Sodium Bisulfite will be placed only as needed for current production in order to keep loss of material due to oxidation to a minimum.
The nZt two batches were made to check the first except that in the ease of the last batch the regular General Aniline Turkey Red Oil was used in preparing the Cadmium Soap in order to have a control hatch to use as a cross-eheek on the use of Jacques Wolff*s Turkey Red Oil* Both of these batches were satisfactory in both rubber and paper by Krebs test and cheeked each other almost exactly by rubber test* The Jacques Wolff Tu t key Red Oil is therefore satisfactory for use in GT-68-P on the basis of this test.
Yields were satisfactory averaging 96jb<> of estimate in the use of the last two batches whieh checks the yield on previous plant production
The Dye Works has requested that no more stump barrels or kegs be included in the shipments of GT-68-P* This will of course necessitate the holding of stump batches in stock until enough has been accumulated to make full barrels (a 400 pounds of pulp)* Uniform mixing of these stump lots will be rather difficult as the only equipment available at present for pulp mixing is the Semi-Works Straub-mill or Mikro-Pulverizer which are not designed for work of this type* The Dye Works has returned stumps on six batches of GT-68-P for paper* These have been mixed and there are two more mixes in process which will oonsume all stump material on hand at present*
DUP050316667
Shipments over the past two months have consisted of 2473# pulp (656 # dry) shipped for paper# Stump barrels on the two batches shipped were retained as requested*
Production results are tabulated in-Table I, mixes in Table II and shipments in TA'ble III#.
DUP050316668
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DU P050316669
FIGttNT COLOR RESEARCH REPORT PIGMENT GRIM LAKE FOR PAPER* GL407D
3
SUBMITTED BY! APPROVES BY:
JANUARY 1936 FILE: PIGMENT GREEN B
INTRODUCTION
Three trial batches of this lake were made on the E-81S7 (sodium resinate) formula to test practicability of large scale operation# A plant size Drum Dryer located at the DyeWorks was used.*
SUMMARY AND CONCLUSIONS
Although the material made on standard, formula was
weak on paper test, it is believed that by proper adjustment of the toner content* a satisfactory product ean be obtained with use of drum drying* Analysis of the lakes produced showed only a 44*2% toner content on the two batches intended to be 50$ toner* This discrepancy is explained by the yields obtained which were higher than on small previous batches and much closer to theoretical* Recalculation of the toner content on basis of theoretical yield gives a figure of' 44*5$*
On basis of control tests which indicated the need of a weak shading batehaa third batch was made to be 31% toner and was of course too weak for present use. The toner content by analysis was 36*48$* Dispersion in water was reported as somewhat inferior to the
other "batches*
Operation of the formula appears to be satisfactory* For regular manufacture provision for a vat in which to prepare sodium resinate would be necessary as use of an iron drum as done in other
trial runs is cumbersome and unsafe* An agitated iron vat was used to slurry the green toner and resinate. No oolloid mill was available nsd is probably not required*
The actual drying proceeded without difficulty, the
material coming off the rolls in rather fine condition with only a small amount of wet lumps in the edgings* Approximately 8% of the product is carried into the ducts and scrubber from whieh it can be recovered*
The total yield obtained for the series was 549# or 93*5$ of theoretical* The latter is calculated from the dry weight
of Figment Green, plus the weight of rosin, the sodium equivalent of the caustic soda used and 3-1/8% moisture*
EXPERIMENTAL DETAILS . H*B. #391, p* 30*
The Drum Dryer used is. the one located in the Basic Pink Bldg, (#392) at the Dyeworks* The set up included a 445 gal* iron
vat from which the color is fed to the (foils* A dust collecting system
consisting of flues and a scrubbing tower is used* A drying rate of
DUP050316670
g k
about 100# per hour was obtained,. Steam pressure was from 30 to 40#* um reversed at a rate of 4 R.P,M*
^he Sreen Toner *ulp (GfT-68-P) used in the series was
on lot #45093* This was treated material whieh was
for rubber and
for paper*
Paper tests on final grinds (main portion)
SW-7636 10**15# weafc - Dispersion - good*
SW-7628 *
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SW*7031 - 30$
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DUP050316671
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DUP050316672
PIQMBHT COLOR RESEARCH REPORT SPECIAL ORGANIC
3 6^f
SUBMITTED APPROVED BY:
FILS: MISC. LAKES & TONERS DATE: JANUARY 1936
INTRODUPTION
Laboratory investigation of new intermediates, dyes, lakes, etc* was confined this month to the preparation and evaluation of dyes and lakes of the anilide of beta^oxyaaphthoie acid as coupling component with 2 ehlor 4 amino 6 sulfonic acid {Bet 2 B diazo component) and 4 ehlor aniline 8 sulfonic acid (Scarlet 8 YL diazo component) as diazo components*
Tests were made of 8.5 diehloraniline of Verona Chem* Co* and Lithosol Orange R lot 1 of the Dye Works.
SUMMARY AMD CONCLUSIONS
Dyes and corresponding pigments of the alkaline earth metal salts were prepared in the laboratory from
A-diazotized 2 ehlor 4 amino toluene 5 sulfonic acid combined with the anilide of 2 naphthol 3 carboxylic acid and
B-dlazotized 4 ehlor aniline S sulfonic acid combined with the anilide of 2 naphthol 3 earboxylie acid
The barium and calcium toners f the "A" combination are reds of medium depth and of yellowish shades, the calcium pigment being darker, and bluer than the barium. Both, however, are much darker and weaker than the Calcium toner of Lithosol Red 8 B K7853 and both bleed slightly in linseed oil and distinctly in laoqaer* fhis bleed, however, may result from decomposition products formed during coupling or incomplete conversion of the dye to the alkali earth metal salt* Altho light fastness tests have not been completed the results so far indicate that both the calcium and barium pigments are inferior to &*7853 (CaRed 8 B Toner) in light fastness*
The barium and calcium toners of the "BW combination are deep reds of yellowish shade, the barium pigment being darker and bluer than the calcium* Both are much darker than pigments of the "A" dye and very much darker, duller, bluer: and less clean than the strontium toner of Scarlet 8 YL, K-7985, The calcium and barium pigments exhibit a slight linseed oil and lacquer bleed. This bleed, however, may result from decomposition produets formed during coupling or incomplete conversion of the dye to the alkali earth metal salt* Altho light fastness tests have not been completed, the results so far indicate that both the calcium and barium pigments are inferior to K7985 in this respect*
*
DUP050316673
The work on the above new dyes and lakes so far has been strict ly of an orientation nature and a conclusion at this time as to the merits of any of these products would be premature* Continued investiga tion is proposed*
A sample of 2s,5 dichloraniline of The Verona Chemical Co. appears to be satisfactory for the preparation of Monolite Fast Red 2 R (8:5 dichloraniline -- anilide of beta-oxynaphthoic acid) This color is a very olose match to Toluidime Red RT-586-B*
Tests of laboratory prepared dye and duPont "Lithosol" Oraijge R lot 1 showed indications of the latter being contaminated with black dye. This was subsequently confirmed by The Technical Labofatory* EZPSRXMSHTAL DETAILS
Sxpt. 49 U.B. #487 n. 163 Preparation of Dye: diazotized 2 chlor 4 amino toluene 5 sulfonic acid Maphthanil A.S., and Barium and calcium toners. Series Ag A3 A4 15 and A6* Preparation of Dye: diazotized 4 chloraniline 2 sulfonic acid --& Naphthanll A.S., and Barium and calcium toners. Series Bg Bg B4 B5 and Bg* Exut. 47 NB.#487 P. 164 R.M. test of Verona Chem* Go*s 2:5 dichloraniline BXbt. 45 M.B.#487 v, 160
* R.M. test and investigation concerning off-eolor of duPont "Lithosol" Orange B-lot-1. The dye lot 1 appears to be contaminated with blaek dye* This was confirmed at a later date by the Technical Laboratory of The By Works*
i
DUP050316674
PIGMENT COLOR RESEARCH REPORT FLUSHED INORGAIIIC PIGMENTS
3 O'
SUBMITTED BY: APPROVED BY:
FILE: PIGMENTS IN OIL DATE: JANUARY 1936
MTRQDUCTION
Orientation work on the flushing of iron blues and chrome yellows has been eontinued#
SUMMARY AND gOCCLUSIONS
The effect of the flushing process on the tinting strength of iron blue is still in doubt although indications are that flushing causes an increase in tinting strength*, Metallic oxide (ie* ZnO and MgO) flush** ing assistants decrease the tinting strength probably by reacting with the iron blue and increase the rate of livering of the finished ink#
Long chain alkyl amines and the corresponding quaternary ammonium salts apparently coat the iron blue particles so that they are
no longer wet by water causing a thick iron blue pulp to become thin and watery {this same effect is produced by stearic acid, sodium hexametophosphqte and the sodium salts of lignin sulfonic acids (D-S262) but these agents do not cause the iron blue (in pulp form) to transfer into the oil phase easily in such a manner as, for instance. Zinc Oxide does* In some instances, fixanol has caused an actual transfer but consistent results have not been obtained and it is evident that the optimum condit ions have not been determined# The results obtained at the Experimental Station with a Ifl slurry of iron blue have been confirmed in this
laboratory*
Zinc naphthenate (D-2240) is relatively successful while the
following additional agents are tentatively unsuccessful as assisting agents for the "flushing" of iron blue in pulp form:
1* Active silica adsorbent
(D~224l)
2* Merck*s medicinal charcoal
(D-8&42f
3* Sttlphonated olive oil
(D-SS33?
4* Diglysol laurate
(D-S315)
5 Free lignin sulphonie acids
{D-2261}
6 * Sodium salts of lignin sulphonie
acids
(D~2262)
Crude stearyl amine
(D-2286)
8* Sodium hexametaphesphate
9* Stearic acid
10* Puroie acid
(D-1267)
11 Cetyl trimethyl ammonium bromide (D-SS74)
12# Aqualoid
(D2328f
15# Leeiv&t
(D-2329)
DUP050316675
Y-316AD does not flush Into vegetable oils unless Zinc Oxide is added* B-66--D and Y-516-D will not flush into Kujol even with the addition of Zinc Oxide* Providing sufficient water is present, B~66B and Y-31S-D mixed with Eujol will produce a erude emulsion with water as the continuous phase#
Zinc naphthenate was relatively successful while Zinc Oxide, lead sulphate and soya lecithin (D-1561) were tentatively unsuccessful for flushing Y#Q2*D into #1 transparent varnish* REVIEW OP PREVIOUS YORK
The immediate effect of treating water-wet pigments with oil as recorded in the various experimental note books is summarized in Table I* SAFERIMSMTAL DETAIL
N.B* 483* Expt* 15# Reaction of Kadox with wet and dry B*66AD* Expt* 14 Effect of White Seal SnO and MgO on flushed and dry control inks of B*66-D#, Expt* 15* Orientation experiment on flushing B*66D and Y-316-B* Expt* 33# Fixanol as assisting agent for B-66-P Expt* 54* Affect of fixanol on strength of B-66-D* Experiment to be repeated* Expt* 35*. Affect of various amines and quaternary salts on rate of filtration of B-66-D slurry (1$)# Expt* 4S Flushing assistants for B-66-D* Expt* 46* Flushing assistants for B~66D and Y-S02-D*
DUP050316676
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DUP050316677
PlSKggg COLOR RESEARCH REPORT FLUSHED LITHOL BBb
3^
SUBMITTED BY; ~X appr o ved by*
FILE: PIGMENTS IN OIL b a t e : JANUARY 1936
INTRODUCTION
4*
A consistency study of the effect of flushing on RT-364-D has been made#
. SUMMARY AND C0NCLUSIBH3
Flushed inks of RT*364-D are consistently slightly weak and blue in tint and very slightly light and dull against corresponding dry control Inks# It makes no difference whether the dry control inks are ground from lump dry color or from dry eolor which has been pulver ized on paper by rolling with a bottle* The above relationship of the fresh tints changes on standing* Apparently the masstone, undertone and tint are more closely duplicated for flushed inks than for dry control inks within a single plant batch* Between plant batches, the absolute tinctorial values, of course, vary greatly but the relative tinctorial values of flushed and dry control inks are quite consistent,
A preliminary experiment indicates that RT-364-D can be flushed into RC-203 "Dulux" resin containing thinner on the hot ink mill*
The extraction method of analysis for pigment content of inks does not appreciably affect RT-364-D tinctorially.
Apparently there is less bleed into oil in flushed inks than in dry control inks of RT-364-D since when 483-31 and 483-36 inks (1:1) were thinned down to 2:3 inks and mounted on paper, the oil that soaked into the paper showed less bleed for the flushed inks than for the dry control inks*
REYI5U OF EXPERIMENTAL WORN
A consistency series (483-36) was run in order to determine if the relationship of flushed and dry control inks of RT-364-D would be the same from batch to batch* Apparently this is true since in both series 483-31 and 483-36, the fresh tints of the flushed inks are slightly weak and blue and the masstones slightly light and dull against the dry control inks* Apparently the masstone and tint are more closely duplicated for flushed inks than for dry control inks. The conclusion seems justified that within a single plant batch, the masstones and tints of flushed inks can be duplicated* There is a great variation, of course, from plant batch to batch of RT-364-D. The results of 483-36 series are tabulated in Table I of this report and should be compared with the results of 483-31 series tabulated in Table III of the "Flushed Lithol Red" report for December, 1935*
EXPERIMENTAL DETAILS
N.B* #483*
DUP050316678
Inks*
483*36* Consistency study on. RT*564-B flushed and dry control
4S3*57. Hushing of RT-364-D into BR0-95490 resin,
483*40% flushing of RT-364<*D into #3 regular varnish and into #5 transparent Garnish*
4Q5.tM. Effect of extrati on procedure on RT<i*864*
DUP050316679
EVALUATION OF FLUSHED AND DRV CONTROL LITHOL BED INKS_______________
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DUP050316680
PIGMENT COLOR RESEARCH REPORT FLU5TO P.T.A.PIGMENTS
SOTMITTSD BY!
APPROVED EY:
*
8a **JU+4 .
FILS: PIGMENTS IK OIL DATS! JANUARY 1936
INTRODUCTION
A cooperative study with. F. H. Levey Go, on methods of flush ing and evaluation of flushed inks has been initiated*
SUMMARY AND OQNCHISIONS
A large sample (over 3 pounds) of BT-1S5-D flushed ink and corresponding dry control and pulp oontrol have been prepared so that F.H.Levey Co* can compare their methods with our method of flushing* Also a 3 pound sample of Blue Toner, K-7982, dry oolor ground in an equal weight of #0 regular varnish has been prepared for Levey to compare in properties against competitive flushed inks,
Neither flushed nor, dry control ETA pigment #0 regular varnish inks showed an appreciable amount of livering after standing in cans at room temperature for three months.
Flushed and dry control inks of GT-347-D extended in hydrate ink (1:50 and 1:100) by grinding on the ink mill showed no difference in tinting strength*
KZPSRIMgNTAl DETAILS
N.B. 483
485-41, Preparation of three pound`sample of K-7983: #0 regular varnisS '(1:1) ink for Levey,
K-7982 s stronger and s better in light fastness vs. BT-150-D, 483-43* Preparation of large samples of BT-135-D (Lot #47391) for Levey,
A. Dry Control, Press Cake dried over night in steam oven 140 F and micro pulverized in saai-works*
B. Flushed Ink, 3400 g. pulp (833 g. dry color) * 833 g, #0 regular varnish flushed on large ink mill. Four passes over hot mill after removal of water,
C. Pulp control,
ink.
485-45, Extension of 483-29 inks (GT-347-D) with hydrate
DUP050316681
PIGMENT COLOR RESEARCH REPORT FLUSHED LAKE RIB C
3^
SUBMITTED BY: ~>C - 6*s*M*4 APPROVED BY:
FILE: PIGMENTS IN OIL DATE: JANUARY 1936
INTRODUCTION
An accurate evaluation of flushed and dry control inks of RT-313-B has been made.
SUMMARY AND CONCLUSIONS
On the ink mill, RT-313-D flushes readily into an equal weight of #0 regular varnish with only a negligible amount of pigment remaining in the flushed water.
Duplioate experiments show that RT-313-D flushed inks have no advantages in tinting strength, flow, masstone and undertone and slight advantages in body, length, texture and light fastness as compared to corresponding dry control inks.
The experimental evidence upon which these conclusions are based is summarized in Table I*
DUP050316682
A ll
the masstones became more equal.
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Masstone mounts "
DU P050316683
FIGMENT COLOR RESEARCH REPORT NEW TYPE FEINTING INKS - ROTOGRAVURE INKS
t
SUBMITTED BY; APPROVED BY:
FILE; PRINTING INN COLORS DATE: JANUARY 1936
INTRODUCTION
This problem has been pursued actively in the laboratory the past month* A large number of inks have been prepared and evaluated in so far as we are able to evaluate them and conclusions drawn as to the "formulation of inks with satisfactory gloss* This phase of the invest!** gation appears to be substantially complete* Some investigation of the merits of various resins remains to be done* as well as the final prepar ation of sizeable samples of inks to be evaluated by the user by actual
printing $eats*
SUMMARY AND CONCLUSIONS
The following resume of the prevfcus work is introduced to make this report complete in itself*
The Technical laboratory at the Dyeworks was asked>in February
1935 to recommend an ink for use on a new type of rotogravure press by one of their customers. After considerable investigation* they selected RH - 35 - D (the high melting modification of the RAH Department*s new resin) as the binder for the ink with Solvent Naphtha (H--504) as the solvent* They formulated an ink using Hansa Yellow as the pigment which pleased the customer very much* The approximate com
position was given to us as
Hansa Yellow 6*6$
RH-35-D
40*6$
Solvent Naphtha 52*8$
100*0$
(Attempts in this laboratory to duplicate the above ink have cast some dloubt on the accuracy of these figures) *
The ink was prepared by pasting the yellow with part of the solvent and adding the resin dissolved in the remainder of the solvent* No grinding was necessary and the ink prints with a very desirable gloss*
This laboratory took up the problem with the idea of incor porating part or all of the resin with the pigment in the hope that it would greatly facilitate the mixing into an ink and possibly eliminate grinding where it would otherwise be necessary* Attempts were made to incorporate the resin by adding a solution in mineral spirits to the color in process, finishing by the usual development, filtering and
drying, the solvent evaporating along with the water*
This treatment was applied to a lithol red by adding the
DUPO 50316684
* s
resin solution in a eolloid mill to the finished pigment and by adding the resin solution to the soda salt suspension in the vat with subset quant treatment as if it were not present. The treatment was also
applied to BT-100-D by adding the resin solution just after adding the PTA solution to the dye and before the development at the boil* In ' each case the resin was incorporated and the dry product was somewhat harsh and brittle to the touch but softened very readily when added to solvent naphtha* There was good evidence that these products did in some oases show better dispersion in the solvent without grinding than ' did the untreated products* However, there was also evidence that com*** plete dispersion would be very difficult to obtain without some grinding
action such as a short ball mill cycle* When such a grinding action HI ' was used the effect of the resin in the pigment was no longer apparent*
There was also evidence that such a treatment did in some case result in a marked tinctorial change although in other oases this was not apparent*
It would appear that any resin could probably be incorpor ated in most pigments in some such manner as here described* It was, however, decided to drop this phase of the work and concentrate on a determination of the real merit of RH-35-D with a representative group of pigments and to formulate with each of them a satisfactory ink.
The first preparations made with a lithol red and with
BT-100-D {PTA Blue) lead to the conclusion that each color would require
a different formulation to obtain the desired gloss* This work was done in cooperation with the Technical laboratory but attempts to duplicate it at Newark have lead to a new view of the problem which is more fully set forth in the following discussion of the work undertaken
in January*
During this month two preparations of Para Brown have been made and have shown the process to have satisfactory reproducibility# A large sample is available for a K sample and for preparing an ink for examination by the customer who has expressed a desire for such a
color*
The remainder of the work during the month has consisted of the preparation and testing of roto inks using RH-35-D resin as the binder and solvent naphtha (H-504) as the solvent* The following pig
ments have been examined:
1* RT-242-D 2* RT-232-D 3* RT--329--D 4* YT-291-D 5. BT-125-D
6* Para Brown
Duol Red Toluidine Red P.T.A. - Rhodamine 6 GDN
Hansa Yellow P.T.A. - Victoria Pure Blue BO
A small amount of time has also been given to the examination of other resins in comparison to RH-35-D*
The method of testing the inks is fully described under the Experimental Details* As more fully set forth there, our evaluation of the inks is limited in its accuracy because of the thick film of ink and slow rate of evaporation of the solvent on the cold printing
DUP050316685
5- LJ -
machine* In actual practise a much higher amount of solvent could undoubtedly be tolerated than the maximum permissible under the
conditions which we are using for testing*
A quite exhaustive study has been made of the relations of the three ingredients of the inks using each of the six colors listed above# Contrary to our previous statements that each pigment would require a different formulation# the conclusion now appears unmistak able that a suitable relation between resin and pigment can be found which will apply to all of these pigments without material change* It appears that no gloss can be obtained when the pigment-resin ratio is below 1:4 and that about 6 parts of resin to one part of pigment are required to give the best results* Higher amounts of resin can be used but appear to be very impractical*
With the printing equipment available and using a pigmentresin ratio of 1:6 it is necessaf^ to keep the solvent below 45% of the total and preferably below 40% to give the best detail of print and the highest gloss* As noted above# this factor of solvent content will certainly be influenced very largely by the thin film of ink used
in typical roto work as well as by the very rapid evaporation on the heated presses*
As to the effect of different resins, we have some con firmation of the reported merits of the higher melting varieties of RH resins* The natural resins such as last India Gum and Damar, give visoous solutions with resulting good detail of print but are somewhat deficient in gloss. Other synthetics like Amberol and Cumar show fair gloss and give promise of being quite satisfactory when the solvent is properly adjusted* We are now inclined to the belief that RH-35-D (or RH-211) is probably the best of the resins so far tested* However, we further believe that other resins can be so formulated as
to give results substantially comparable even if slightly inferior* We have ordered and plan to examine a number of commercially avail able products and to select certain of the best from this group to
prepare inks for examination by our customeyalong with the contemplated
inks from RH-35-D*
We are now proceeding to make up one gallon samples of the various colors noted above (omitting RT-329-D) using RH-S5-D and
we will use RT-232-D to make up similar samples using the various resins# These inks will consist of
Pigment
Resin Solvent
8*4
51*6 40*0
we will hope to keep accurate records of the additional solvent# if any* used by the customer*
e x p e r ime n t a l d e t a il s
N.B.#49S P* 50-95* Also - evaluation of inks as reported in December#
All evaluations of rotogravure inks as noted in this report have been carried out on a small textile printer with an engraved roll operating against a rubber roll* The engraving is quite deep in respect to the usual rotogravure etching* The ink is
DUP050316686
distributed from a blade with a second "doctor" blade to remove the excess*, The machine operates at a speed of about SO feet per minute and there is no heat so that drying is by evaporation in the open air,# As a consequence of this situation inks of relatively low solvent content are required to obtain a satisfactory gloss* With higher solvent contents, the solvent penetrates the paper and takes so much of the resin with it that the finish is quite flat* Also inks of low viscosity do not print a sharp, clear design when the engraving is deep* All tests have been carried out on a rotogravure paper obtained from The International Paper Co* Ratings have been based on the clear* ness or detail of the print, on the gloss and on the penetration of the paper*
495*5 series evaluations p. 25*27# These inks were prepared to duplicate the inks prepared in November at the Technical Laboratory of the Dyeworks and also to study the effect of ginding in a ball mill#
It is obvious that all the inks of this series have more solvent than was used in the earlier work* They are thin, give blurred prints with little gloss and considerable penetration*
Grinding very definitely improves the P.T.A. blues but appears to have very little effect on the Hansa Yellow and Lithol Red inks*
495*6 series evaluation p* 28-29* last India Gum vs* Cumar Resin with Hansa Yellow and Lithol Red#
In each case the East India Gum gives a more viscous ink and a sharp print but poor gloss# The Cumar resin gives a thin ink with a blurred print and poor gloss#
495-12 series evaluation p*4647* These inks were prepared from the brown pigments of 495-9 and 495-10 series*
"A* was from 493-90 Basic Brown P.T.A. and was a very poor ink* The pigment was hard and did not grind out* The other inks were from Copper Para Browns* Although all the prints were blurred and showed bad penetration* there was some suggestion of a gloss which gave promise of formulating a satisfactory ink:#
495-15 series evaluation p* 48-49* This series consisted of the Cumar resin inks prepared according to Mr. Duhring's formula* They had no gloss and did not dry completely* The formula is certainly not applicable to the work at hand*
495 p* 50-51# An attempt was made to flush BT-100-B press cake in a mixture of RH-35-B in solvent naphtha (H-504) in a vacuum mixer arranged to recirculate the solvent#
Due to the high rate of evaporation of the solvent it came over much more rapidly than the water and recirculation proved to be well-feigh impossible* The work was stopped because of lack of time* but the resulting very heavy paste still contained a large amount (f 30$)
DUP050316687
of water but only about 12$ of the original solvent. It has since been shown that the remaining water and solvent can be removed on a hot roller mill leaving a slightly plastic mass which solidifies on cooling and can be dispersed in the solvent by heating. The whole process appears, however, to be quite impractical and no further work is planned.
495-14. A study with variations in amount of color and amount of solvent using a Lithol Red as the pigment. This series seems to place an upper limit of 43-45$ as the maximum solvent possible with the present testing equipment to give a print of satisfactory detail and gloss. The variation in piguent over the range selected seems to have little effect*
495-15. Clear varnishes with variation in solvent content. When printed, 40-45$ solvent seems to be the maximum which is possible and still obtain the desired gloss.
493-16. A further study of Hansa Yellow inks on formulas previously used. Ho gloss was obtained and it is obvious the inks have more solvent than the ink obtained from the technical laboratory, as representative of the sample examined by their customer.
495-17. Formulation of Roto ihks from RT-242-D using in creasing amounts of pigment with variations in solvent content*
Where the solvent is kept below 45$ a fair gloss results with fairly sharp prints over the whole range of the amount of pigment used* However, even these inks give too much penetration.
495-18. A study of the use of Alumina Hydrate to give gloss and of increasing the pigment still further
The Alumina Hydrate does not increase the gloss but rather tends to act as additional pigment which is further shown to give reduced gloss but better detail of print. To a ratio of 1 part pigment to 4 parts resin there is some gloss but at a 1:1 ratio there is none and the products are quite thixotropic and require more solvent to have a workable body.
495-19. A further study of pigment-resin ratios with RT242-B varying from 1:1 to 1:3.75. Below 1:3 there is almost no gloss but there is good detail of print. With 1:375 the ink seems to be fairly satisfactory in all respects.
It is 'therefore tentatively concluded that the pigment binder ratio is the deciding factor as to gloss with the amount of solvent a function of the manner in which the ink is to be used, these con clusions assuming the use of RH-S5-D as the resin.
495-20. Formulation of Roto inks from RT-232-D,
This series varied the pigment-binder ratio through equal steps from 1:1 to 1:8. The resin solution was made up to contain 8 parts of resin to 7 parts of H-504 except that additional solvent was necessary in the first two members of the series to give a workable body to the ink.
DUP050316688
6 -
Good detail of print is obtained up to a pigment-binder ratio of 1:6* However, there is no gloss below 1:4 and it requires at least 5 or possibly 6 parts of resin to give the desired gloss and freedom from penetration*
495-21* Formulation of Roto inks from RT-329-D.
The variables were the same as in 20 series and the conclusions are the same except that none of the inks from this series give the de sired gloss*
493-22. formulation of Roto inks from BT-125-D.
The same variables and the same conclusions apply as in 49320 series*
493-23. formulation of Roto inks from YT-291-D.
The same variables were applied as in 493-20* However, there was a much greater thiekenlng effect at the lower ratios than in the previous series. Even these inks left something to be desired*
495-24. Solvent variable with YT-291-D using a pigment binder ratio of 1:6. It is conclusively demonstrated that such an amount of resin will give a print which is excellent in every respect if the solvent is sufficiently low (below 40$)*
493-25. A study of the use of different resins using RT-232-D with a pigment binder of 1:6 and a resin solution containing 8 parts resin to 7 parts of H-504.
Resin
Detail of Print Gloss Remarks
A RH-35-D
B RH-35 C RH--211 D East India Bold
Good Poor
Good Good
E Gum Damar
Good
F last India Fossil
Gum
Good
G Slemi Gum
Poor
H Amberol Resin
Good
I Manila Bold J Cumar Yh
K " wk L Ester Gum M I Rosin
**
Poor Poor Poor Poor
Good
Poor
Low melting variety
Excellent Higher melting than RH-35
Fair
Reauired additional solvent
to grind
Slight
Slight
Hone
Very
Required additional solvent
Slight
to grind
- Insoluble - no tests
Very slight
Slight
Slight
None
The high melting RH resins gave the best prints in every
respect. The natural resins gave good detail but low gloss* The other synthetics as Amberol and the Cumar s were ;promising and should be studied with a view to adjusting to the desired properties if possible. The llemi Gum and the rosins were quite unsatisfactory*
DUP050316689
495-86 > A large sample of Para Brown was prepared on a formula
very muck like that used in 493-10B. The products check the previous work very closely*
493-87* Solvent variable on RT-242-D
493-28. Solvent variable on RT-233-D
493-29. Solvent variable on RT-329-D
495-50. Solvent variable on BT-125-D
These four series are like that of 495-84 in varying the solvent on a pigment-resin ratio of 1:6, The same conclusions hold
in every case, that a sufficiently low solvent content (below 40$) gives an excellent print of good detail and gloss,
Browns.
495-51, The preparation of Roto inks from 493-26 - Para
The same variable as used in 493-20 was applied (variation in pigment-resin ratio). The same conclusions also apply. 6 parts of resin to 1 of pigment are necessary for good gloss*
495-52. Solvent variable on Para Brown.
See 493-27 to 30 above for method ana conclusions.
495-55. Solvent variable using Cumar wir with RT-232-D*
A very respectable print is obtained with solvent below 40$
but the best in this series appears to be somewhat less glossy than the best obtained from RH-35-D*
495-34, An additional large sample of Para Brown was pre pared as in 495-26 series and four samples are very good checks. This material will be used to prepare a large sample of ink for examination by a customer*
DU P050316690
PIG-MEM1 COLOR BESTSARCH REPORT SPECTROPHOTOMETRIC STUDY - CHROME YELLOWS
SUBMITTED BY*.
FILE: PHYSICAL STUDIES DATE: JAM* 22nd, 1936*
INTRODUCTION
Spectrophotometric measurements have been made of a large number of paper mounts ("skindowns") of inks prepared from Krebs
Chrome Yellow standards* various mixes* and several competitive Cadmium Yellows* CI*E* tristimulus specifications were computed from the spectrophotometric curves* and these results, as well as the curves* have been carefully examined*
SMEARY AND CONCLUSIONS
This study gave no unexpected results as to shapes of curves ox the tristimulus color specifications* All of the curves
are of the usual fora for Chrome Yellows, showing strong absorption (even for the thin ink films examined) in the violet, blue, and greenblue, reflecting less than ten percent of the incident light in this region; in the green-yellow* yellow, orange and red, reflectance is
hi$i* about ?585 percent* Spectrophotometric data agrees with visual observation in a qualitative way*
The influence of quality of the pigment preparation and mount on colorimetric measurements was observed, particularly in the case of mounts of identical inks mounted on different paper. It is probable that "skindovm" mounts are not well suited for colorimetric measurements because of difficulty of duplication#
The hue range of chrome yellows runs from 582*5 to 573*0 millimicrons dominant wave length* The sensibility of the eye
to hue change at the average excitation purity of chrome yellows (74-78 percent) may be roughly estimated at 0*1 millimicron in dominant wave
length* (According to extensive data in the literature, the sensibility of the eye to wave length change is at a maximum in the vicinity of 5S0 millimicrons* There is another maximum at 490) *
Because of the similarity of the curves of all the yellows examined, mixes of various of these are very similar to the intermediate yellows in visual appearance and shape of curve*
The curves of mixes fall between the curves of the
individual components of the mixes* in an approximate way* Deviations from this rule are attributed to non-uniformity of ink film thickness in the skindowns*
The three Cadmium Yellows examined are similar to chrome Yellows in their color characteristics but are all higher in purity than corresponding chrome yellows* The spectral curves show more complete absorption in the absorption bands (less than seven percent)
DUP050316691
2
and somewhat steeper slopes than chrome yellows of approximately the same hue*
DETAILS
The Yellows examined fall into three groups:**
I# Chrome Yellow Standards (Krebs)
Am Regular ("nitrate") Yellows* (The following tabulation is arranged in order of hue}*
1* Y**359*D (reddest)
8* Y190--B
3* Y-309-D (high finish)
4* Y~171~D
5, Y180D
6* Y-303-D
7* Y-*305*D (high finish)
8S Y-315-D ("
n )(greenest)
* B* Lemon Yellows.
9* Y318D 10* Y-202-D
11a Chrome Yellow Mixes.
Mixes of various members of the IA group to match other
members of the same group. Mixes were made of standards one step apart to match the intermediate standards; a mix was also made of the extremes to
match a standard in the middle of the range# Several mixes were made of standards two or three steps apart*
III, Three competitive Cadmium Yellows*
Yisual examination of the Yellows were made before the mounts were measured spectrophotometrieally; these results were reported In a letter (Y#C* to A.W* Kenney 1/16/55) a copy of which is appended to this report#
It should be kept in mind that all measurements discussed
were made on "skindowns"; masstones and tints were not considered in
this study, Skindowns were prepared in the usual manner, by scraping a thin film of the yellow inks (made from the pigments ground with lit ho varnish) over two kinds of paper - bond paper and litho label stock. Mounts of the latter are designated by the subscript "A",
CHROME YELLOW STAMPARDS
Skindowns of the ordinary types of Chrome Yellows show an excitation $uritw between 74,51$ and 76,83$, a brightness factor of 43,4$ ~ 48,07$, and vary in dominant wave length between 582,48 (medium) and 57 3*0 millimicrons (primrose), Y-309D has an .abnormally high purity, 78*3$,
DUP050316692
3
(A) Dominant Wave Length. The classification of chrome yellows according to their dominant wave lengths rather than th&ir "Shade'* is an unfamiliar one* The visual color differences, as graded hy the pigment makers* ordinary methods, are compared below with the
dominant wave length differences#
Standards
Dominant Wave lengths
Wave Length
____________________ _________________________________ Differences.
Yisual differences
Y*359D -Y*19Q*B Y*190*D **Y*171*D Y*171*D *Y**180*B Y~18Q~D *Y303D Y**303**D Y305*D Y*305"B *-Y315D
582*5 * 578,1 578#1 577*4 577,4 576#6 576,6 - 575# 5 575,5 ** 573,6 573,6 9* 573*0
4*4 Y*19QD is very much greener,
0,7 Y*171*D is slightly greener#
0,8 y*180*D w i
1*1 Y**303**D is much greener
1,9 Y-305-D is very much greener
0,6 Y"515D is slightly greener#
Y-309-P (577*6) appears slightly greener than Y190**D (576*1} and very slightly redder than Y171-D (577,35); because of its high finish, Y~309D looks more brilliant or stronger than the others*
From this tabulation, the sensitivity of the eye to hue change in this range is estimated to be in the order of 0*1 millimicron; hipping limits would require standardization to within about twice this limit#
(b) Purity and brightness. The variation in purity may be largely accidental , due to variations in quality of the mounts which were measured. Although every effort was made to make these uniform* noticeable visual differences were often seen in duplicate pulldowhs* Accidental variations might be expected in which purity would go up and brightness go down, or vice versa, corresponding to a thicker or thinner Ink film# There is a gradual increase in brightness as we go from the redder to the greener yellows; roughly, the brightness increases with increasing lead sulphate (and decreasing lead chromate) content:**
Code______
Brightness
-percent lead sulphate
YB59-D Y*X9G~D Y|7lD
Y10~D Y303**B Y305-*D Y~S15~B
53*58 64*06 66,00 67,47
68,91 72*97 74#5S
0
28fo
51 42 48 44 52
The spectrophotom@trio curves (Figure 1}* show this as a widening of the absorption band with increasing percentage of lead chromate,
^Figure 1 follows#
DUP050316693
*
r ef l ec t anc e
WAVELENGTH
DUP050316694
4
A tabulation of calculated Dominant Wave Length,
excitation, purity, and brightness factor for the various yellow standards
is given below.
Exoitation
Standard Code
Dean*Wave Length Purity
Brig:
Y-359-D Y-190-D Y-309-D
Y-171-D Y-180-D Y-303--D
Y--305--D Y-315-D
582*48 578,13 577*63
577*35
576,64 575,53 575*55 573*00
76,36 74,61 78,39 76*85 76,76
75,80 76*94 75.02
53<*52 64*06
65*50 66*00 67,47
68*91 72*97 74.55
An examination of the speetrophotometrie curves in : shows nothing unexpected in their general characteristics. The shapes of all the curves are similar, showing a strong absorption barid in the
violet and blue, and having a fairly sharp cut off between 500 (blue-green) and 540 (yellow-green).
The curves for Y-305-D and Y-315-D show lower reflectance in the blue than any of the other yellows* If this is not caused by a
accidental variation in quality of the mounts, it would indicate that there is room for improvement in the other yellows in the blue end of the spectrum. The curves sre approximately parallel, except for the red end of the Y**359~D curvej the arrangement and spaoings are about what would be expected from visual examination.
Lemon Yellows
A tabulation of the two "lemon yellows", Y-202-D and Y-318--D, compared with two regular yellows of similar hue is shown below*
Excitation Standard Code Pom,Wave Length Purity______ Brightness
Y180D Y-318-D
Y-2G8-D Y-303-B
576*64 575.73
575*33 575*53
76.76 78.47
73,03 75*80
67,,47 67,69
65*81 68*91
Lemon Yellows are Chrome Yellows differing from the ordinary type in their working properties when made into printing inks because of
their crystal form and particle size* Y-202-D is a "pure" lemon yellow, while Y-318-D is intermediate between a lemon and a regular type yellow*
Speetrophotometrie and visual examination of these mounts
do not show the expected superiority of the lemon yellows; this may be attributed to the method of preparation of the mount.
Examination of inks made on an ink mill and printed on a proofing press would probably show the lemon yellows to better advantage.
Figure 2* shows the curves of the two lemon yellows*
Three Cadmium Yellows (Cadmium Sulphide)-C-31670, 31671, 31672 - were examined* A tabulation of the tristimulus specifications is given below; several chrome yellows of similar hue are .included*
^Figure 3 follows*
DUP050316695
NCE
WAVELENGTH
DUP050316696
r
~5 -
Bom. Wave Length
Excitation Purity.. _
BSEriUi MMIHH....
C-S1671
577.39
0-51672
574.84
0-31670
573,80
Y-171-B (chr.Yellow)577.35
Y-3Q5-D " "
@73*55
82.91
@1.15
78.62 76.83 76*94
64.48 70.51 72.80 66*00 72.97
Figures 24* and 2B* show the greeter steepness is the curves and lower reflectance in the blue sad violet for the Cadmium Yellows as compared to Chrome Yellows*
Figure 3* shows the chromatieity of all of the yellows discussed above plotted on the C.I.3. coordinates*
Bffee t of quality..of . Paper.
4s discussed previously, "skindowns" were made on two
kinds of paper* a comparison of these is shown in the following
tabulation*
Excitation
Curves
Standard Code
Paper
PQm.Wave LengthPurity___ Brightness
1 14
Y-3it59-B
2 24
Y-1t*9G-B
3 34
Y-3n09-D
4 44
Y-171-D
5 54
Y18G*
tt
bond
582.48
litho label 581.48
bond
578.13
litho label 574.27
bond
577.63
litho label 576.05
bond
77.35
litho label 573.61
bond
576.64
litho label 573.77
76.36 80.06
74.51 69.03
78.39 80.15
76.83 77.62
76.76 73.53
53.52 57.32
64.06 74.15
65.50 69.49
66.00 73.2S
67.47 78.27
6
6A
Y-3QS5- tt
7 74
Y-3tt9S-D
bond
575.53
lith label 574.26
bond
573.55
litho label 571.98
75.88 77.31
76.94 72.06
68.91 73.32
72.97 78.46
@ 84
Y~3tt1S*D
bond
573.00
litho label 571.99
75.02 73.21
74.55 78.30
9
94
Y-3tt18-D
bond
578.73
litho label 574.79
78.47 80.85
67.69 71.64
10 104
Y~2tt02~D
bond
575.33
litho label 574.47
73.03 71.15
65.81 71.17
* Figures 24 and SB follow
* * 2 follows
* **
3*
DUP050316697
'[;f; *_
Sfc-
.. .
<520 640 660
?oa
DUP050316698
DUP050316699
,310 .320
+30 m ATO .ISO
,m ,j
DUP050316700
6
In. the above data the difficulty in preparing satisfactory uniform "skindowns" on the smooth surfaced litho label stock must be taken into consideration; the conclusions drawn are therefore tentative* The following table shows the differences found between the bond and litho label mounts#
Y359**D Y190*D Y*309**D
Y171D Y180D Y-303-D Y305-D Y~315~I> Y~318-I> T~2Q2**D
Differences (litho label vs bond)
Dom*Wave.Length
Purity
Brightne
* 1 * 00 - 3*86 ** 1*53
374 ** 2 *87 <* 1*28
* 1*57
- 1*01 ~ 0*94 * 0*83
4 3*70 - 5*48
*> 1*76
0*79 * 3 * S3
* 1*51 4*88
** 1*81 *- 2*33 * 1*88
3*80 *>10*05 t* 3o90
7 *18 7*80
* 4*41 <i* 5*49 * 3*75 t 3*95 & 5 # 36
The dominant wave length is shifted to the green side in
all oases* Excitation purity differences vary erratically, probably depending on the quality of the mounts (i*e*, the effect of more or less of the white paper showing thru the ink film)* Brightness is increased in all oases by the use of the litho label stook.
The above data emphasizes the importance of the type of pigment mount on the color of the pigment preparation*
Curves for all these yellows are shown in figures 4 to 13* inclusive; in each case the subscript "A" indicates the litho label skindown*
Fig* 4 5 6 7 8 9
10 . 11
IS 13
Curve #1 2 3 4
5 6 7
8 9
10
Y~359~D Y-190-B^ Y~309~D Y-171D
Y-180-D Y*305**D Y~305D
Y-315-D Y~318D
Y*202**D
* Figures 4-15 Follow*
DU P050316701
100
90
80
{' /o
60
50
40
30
20
' .0
#> I
0
41
10 460 480 500 520 540 560 580 600 620 640 660 680 700
61- 1938
WAVELENGTH
Color Measurement
DUP050316702
D** at*e t. aA. pril 6*, 1935
WAVELENGTH
Color Measurement's Lab.
DUP050316703
V5K
90
80
)
70
60
50
40
30
20
ro
0
420 440 460 480 500 520 540 560 580 600 620 640 660 680 700
a April 6, 1935 No.
WAVELENGTH (millimicrons)
Color Measurement's Lab. Mass. Inst, of Tech. ___
DU P050316704
400 420 440 460 480 500 520 540 560 580 600 620 640 660 680 700
Date April 6* 1935
WAVELENGTH
f Color Measurements Lab.
DU P050316705
r e f l e n c e {Percent)A
Date April 6, 1935 Test No.
WAVELENGTH (millimicrons)
Color Measurements Lab. Mass. Inst, of Tech.
DUP050316706
REFJVANCE (Percent)
400 420 440 460 480 500 520 540 560 580 600 620 640 660 680 700
Date April 6, 1935 Teat No.
WAVELENGTH (millimicrons)
Color Measurements Lab. Mass. Inst, of Tech.
DUP050316707
100
90 80 70 60
50 40 30 20
10 0
4<
!>afo April 6, 1935 tot No.
WAVELENGTH {millimicrons)
Color Moasuromonts Lab. Mass. Inst, of Toch.
DUP050316708
REFLECTANCE (Percent)
DU P050316709
100 90 80
)
70 60 50 40 30 20
to April 6, i36 st No.
WAVELENGTH (millimicrons)
Color Measurement Lab. Mass. Inst, el Tech.
DUP050316710
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DUP050316711
QHHOMB TEIXOW MUSS
S@Yen mixes of standard yellows were made to match intermediate shades, fhe composition of these mixes is shorn graphically fcselow.
MIfix t*
11
18
is
n
n n
14 13
IS
ft 7
Yg59~D
Y*171D Y180*>P Y308*B Y~5Q&D Y*51B*
4$>-------- =-x<s-------------X<--------- 63$ ->X <-
6,
6,7 *7*
-> X^-> X
-- 37$ ->X *-
-'WIIIHtx,*-. -itfMtfrm'WV-'
DUP050316712
a
o
1 H
P
0 CB
oP
80 U jVe>h
H M w |Cij
bO 8 O u t
H n as
5* 03 H
0 IQ
f*t f0t
as
I
ft
0 w
if
0ft
'CJ
P
0$
pf bO 8
0 c 0 J
00Oo
Pi 0 V H
&Q &b *VP)
O
0000
0 to 0 0
0
f0t
f0t
0 ft
G) 0 &
P. V T
HP e> *
_*C3. 800 O
U U HW Jh
8S3 V*Hi
P T3 p
3S *pMrl
83 p V 0 0
Hm 0,3
Q
1
0 O 2
aas ano
as s
3
ID
0 S
St 0 Jf* ft- ft* I H G 0 CO ft-
S3
CO 0
ft* ft. in a !
d
fc
0
0 O cd V P
8 0
to (O
CO <2 ft
CO *8 to ft*
& 0 tft ft-
srt m t ft
*2a T
22
i: HI
CQ Hi
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ctf 0.
nc3
$3 WS3)
0O 0 Jm
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o 8
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pP
i;
ft* 1!
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fir- ft- CO to to to
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%
o 0
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g
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to G> fc- ft1* CO
000 <0 to in ft- ft- >
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a
to *
1 00
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.
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i
ft
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I
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in
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o $4 1n2
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f DUP050316713
& ?B
In general. It may tie eoneludeit X) Spectrophotometrio data agree fairly well with visual readings of
mixes and standards* 2) All of the yellows, in the regular line, from primrose to medltna shades
are "compatible" with each. other* giving satisfactory raatohes for intermediate standards in skiadowh mounts prepared as specified earlier in this report*^ Spec trometrie gre'wes of Mixes .and,.OtttgftWUte, Figure 14* shows curves for two standard yellow, Y**359*B and Y17lB, and a curve for the mixtures of these two yellows* As might be expected, the curve for the aix falls between the curves of the two components* A similar set of curves for two other yellows is shown in figure 15*; in this case, the curve for the mix is somewhat above either component from 550 to 660 millimicrons; this is probably due to variation in quality of the pigaeat mounts* Figure 16* shows curves of two mixes (11 and 16) designed to match standard Y*190I> (2>* Mix 11 is good matoh; mix 16 is not as close*
figures Id, 15, end 16 follow*
DUP050316714
DUP05031671 5
^ 90
DUP050316716
REFLECTANCE
TOO
DUP050316717
8 *
r
Dr* &,W, Kenney* Experimental Station* E.I* du Pont de Nemours & Co,*
Wilmington* Del*
CHROME YELLOWS
We are sending you attached herewith forty "pulldowns" which we have prepared for speetrometric examination by Dr. Hsrdy and your subsequent study of C,,IE. curves* These exhibits have been made frcan our important standard Chrome Yellows and mixtures of these standards and also include six mounts of competitive cadmium yellows#
There are two mounts of each pigment or pigment mjt&ture* one an a bond paper (Parohmont Bond) and one bn a ooated paper ("litho
label")* The latter mounts are designated by the subscript "a"* No chrome oranges are included in this series, because visual examination of tentative mixes indicated that differences in oil absorption, finish* etc* between the oranges and the yellows made significant mixtures of the two
types impossible*
The yellows used are tabulated below* with identifying numbers with which the pulldowns are markedf
Pulldown No*
Standard Code
42n9
and la 2 " 3a
3 " 3a
t? 4 " 4a
if 5 " 5a
w 6 " 6a
n 7 " 7a
tt
ft
8 " 8a 9 " 9a
n 10 "10a
n 11 "11a
n 12 "12a
tt 13 "13a
rt 14 "14a
rt t
15 IS
"15a "16 a
it tt
17 18
"17 a "18a
ft 19 "19 a
ft 20 "SOa
Y359D
Y190*D Y*5Q9 <*D Y**17X*D
Y-180-D Y*303**D Y-305-D Y315-D Y--518B
Y-208-D mix to match Y-190-D (4% Y--359 96% Y-171-D) mix to match Y-171-D (37% Y-190-D, 63% Y-180-D) mix to match Y-180-D (63% Y-171-D, 37% Y-303-D) mix to match Y-180-D (6,7% Y-359-D, 93,3% Y-315-: mix to match Y-303-D (50% Y-180-D, 50% Y-315-D) mix to match Y-190 *D (12% Y359-D* 88% Y-303-D) mix to match Y-171-D (6,7% Y-359-D, 93,3% Y-303 C--31671 Cadmium Yellow
C-31672 Cadmium Yellow
C-31670 Cadmium Yellow
Mixes 11 to 17 inclusive were made to be fairly close visual matches for masstone and undertone on bond paper, mounted in the usual manner* In many cases, differences in finish, masstone; undertone relation ship, strength, etc, made close matches impossible. The following list
is a tabulation of readings of the mixes versus the standards they are designed to match. The readings are in the orthodox manner used at Newark;
DUP050316718
3 -9
the abreviations s., v.s*, and v.v.s*, mean "allghtly"* "very slightly", and "very very slightly"* Strength is the apparent tinting power when the pigment is extended 1 part to 15(by weight) with zinc oxide*
Tint is the 'chromatie!ty of such an extension. (These tints were made for general information and are not being sent to you*
Readings - mix versus standard
Mix Standard
Masstone
Undertone
Strength
Tint
11 2 (Y-190-D) ws green
vs strong
vs strong s green & oleai
12 4 (Y-1?1~D) vs red & clean sweak
vs weak
s red
15 5 (Ym18Q*DJ vs green
vs green equal
ws greeq
14 5 (Y-180-D) s red
vs weak & green weak
eaual
15 6 (Y3Q3**D) vs red & clean vs strong
s weak
s net
16 2 (Y-190-D) vs lt*cl.&gra* vs clean
s weak
vs green &
dirty
17 4 (Y-171-D) vs red
s weak
weak
vs ret
The above readings are the writer's, of mounts on bond paper*
In order to give you an idea of other than color differences
between these yellows, the following tabulation indicates the composition and special characteristics of the various pigments*
StdCode Pulldown Ho. $PbCr04 "Shade" .
Type
Remarks
Y**359 D Y-190-D
y**i7i-D Y-180-D Y-*303--D Y--309 --D Y305~D
Y-318-D
Y-202-D
1 2
4 5 6 3 7 8
9
10
100$ 72$
69$ 58$ 52$ 70$ 56$ 48$
85$
79$
Medium
regular regular medium type
dk,,excelsior "
regular excelsior
type; somewhat wk*in
It* "
ft
tint* regular excelsior type
canary lt*canary
tt ft
regular canary type light,weak canary
excelsior high fin . high fin* good str*
primrose
n ft high fin* primrose
lt*primrose "
n high finflight,weak
primrose,
lem. (canary lemon high fin., good prints
shade)
ing tone and oil re
tention*
lemon
lemon good str , poor light
stability*
In most of these yellows, the additional component besides lead chromate is chiefly lead sulphate; in the high finish type, there are small amounts of alumina hydrate; in the lemon yellows there is also lead phosphate*
Pulldowns were made instead of prints because the former are much easier to prepare, and approximate the results obtained in prints* Large pulldowns were made so that they could be cut up, if necessary, for several runs in the spectrophotometer* I am enclosing several sheets of the
DUP050316719
10 ** papers used* In running curves on these mounts* I believe they should be backed by several sheets of paper* to give a non~seleotive opaque backing*
Yisually, Y-359-D is much redder than Y-190-D; Y3O0*D* Y171B* and Y180D are greener in approximately equal small steps; Y*303*D is distinctly greener than Y-*18GD; Y505 is greener than Y*>503*D the difference being Isrge; Y315X> is very slightly greener than Y505~D* Y*318-*D is somewhat greener and more saturated than Y180-D; Y*20B .is much greener, and more saturated than Y*180B
Y. CHAUJPSKI.
DUP050316720
PIGMENT COLOR RESEARCH REPORT COLORIMETRIC STUDY OP MILORI BHJES
SUBMITTED BY: Si APPROVED BY; ^
DATE; JANUARY 1936 PILE; PHYSICAL STUDIES
INTRODUCTION
Speetrophotometrie curves have been obtained on a number of blue ink preparations, with the object of studying their inherent color properties, and to determine the extent to which the
ordinary Milori Blue fall short of the "ideal" minus red* Prom the date obtained, certain conclusions can be drawn as to possibilities of improvement*-
in ARY AND CONCLUSIONS
Two standard Milori Blues (B-57-D and B-66-D) were
examined, let down to approximately printing strength with alumina hydrate ink and printed on a proof press, a curve was also run on Peacock Blue Lake, BL-72-D, for comparison* In the case of B-66-D, curves were run for three different extensions (1:3, 1:9, 1:15), and also on a thin film of ink mounts# between glass plates.
The following is a tabulation of the results calculated to the tt*IE. tristimulus specifications (Illuminant C).
Dominant Wave Excitation Brightness
Length______ Purity
Paotor
BL-7 S-D print
B-57-D ,1:2*3 Al*hydrate)print
B~Q6~D 1:3 n n
n
* li9
w 1:15 *
*
" transmission-film between
glass
" reflection (of above film,
over white paper)
482*70 478*11 478*46 481.76 482*56 478*95
473*98
62*43 58*95 57*15 40*03 31*70 73,07
74*09
17*47 12*95 14.16 29*43 36*05 17.86
7*05
idea) minus red
490*85
30*15
81*82
The color difference between the B-57-D and B-66-D prints is quite small, as might be expected*
In the B-66-D series, successive reductions shift the dominant wave length toward the green. Purity is reduced, and brightness is increased, as expected* The transmission curve of the ink film of B-66-D between glass slides represents the inherent light absorption
of the blue in varnish; examination of the curve and the above tristimulug specifications shows a high transmission in the violet and blue, rapidly decreasing transmission thru the green, a very small transmission in the yellow, and practically zero transmission in the red (less than
0*80 percent}* The reflection curve, made by placing this ink-between-*
'
ss* y
DUPO 50316721
8
glass mount on a sheet of white paper and treating this as a reflection mount, shows no peculiar results; the data from the transmission curve calunlated to such a reflection curve (taking into consideration the reflection characteristics of the paper) agrees very closely with the actual curve, as shown in the following tabulation* This Indicates that there are no complications introduced by bronze or surface color phenomena* The absence of any pigment-air interface would of course prevent any very marked surface selective reflection*
* Cal*Refleotion Actual Reflection
(a) (h) Wave Length Transmission Refl* of |(a) x b) 4> K*
________;______ of Mount_______ paper_______'
from curve
400 43*2% 73% 15*9%
420 53*2 76 23*8 ..
440 60*5
77.6
30.7
460 62*3 79 33*5
480 58*3 80 29*5
500 48*2
80*2
21*0
520 35*0
80*1
12*1
540 21*7
79*8
6.1
560 11*0
80*0
3*3
15*3% 23*6 30*6
33*5 29*1 21*8
11*3 5.7 3*1
*K * constant of reflection from glass-air interfaces, taken as 3.3$, based on reflectance in the red end of reflection curve*
Figure 1 shows the curves far the three extensions of B-66-D, and the curve for Peacock Blue Lake, Bl -72-D* The reflection curve for the paper used is included*
Figure 3 shows the comparison between B-66-D and B-57-D* B-66-D is extended somewhat more than the B-57-D in these prints*
Figure 3 shows the transmission of tbs B-66-B ink diluted between glass slides* The curve for reflection of this film over paper,
and>the curve of a print (same as in Figure 1) is also included* It may be noted that curves B and 0 are both steeper than A*
Figure 4 shows a portion of the Ci*E* triangle, showing the location of these blues on this plot*
\
All of the blues examined fall far short of the ideal
minus red; the spectrophotometric reflectance curves indicate this perhaps more than the 0*1*1* graph* Hone of the blues reflect nearly s 'j enough green; all are very low in the violet, and their maxima are all
quite low* None of the blues has a very steep curve. A comparison of
curves for BL-72-D and B-66-D with a hypothetical blue equal in "chromatic
efficiency" to an ordinary chrome yellow (made by reversing a chrome yellow curve right to left) is shown in figure 5* The inferiority of N the two blue pigments is obvious*
PQ '-^v. V
DUP050316722
% Reflection
7/
DU P050316723
fo Reflection
y'i-
DUP050316724
Reflection 100
T>
700
DU P050316725
X
DUP050316726
DUP050316727
2 0 DIVISIONS *S ft INCH. t& . 3 3 2 6
:<; r
-C. $, & H E W VO M .v. O U
SUBMITTED BY: $JAPPROYSD BY*
3^
p ig mmt cam b s s b a b o e b b p o b t
PHYSICAL LABORATORY - BROGBESS REPORT
^'
Jim i mwxam, s t u d ie s DATE: JASTOARY if36
74
This report covers the work done in the Physical laboratory for the past month. Inasmuch as most of the work now being done is of a continuous or semi-wontinuous nature, no attempt will he made to draw conclusions in this report* The work divides itself naturally into three types* namely, mieroseopic studies, color analysis,
and consistency measurements as a part of the general problem of
fundamental physical measurements of the physical properties of pigment#
vehicle preparations* This latter type was inactive during the month*
Microscopic studies - Considerable work has been done in assisting Dr* J*V, Soudi in his investigation of Para Reds. A
number of samples have been examined by transmitted light, reflected light, polarized light, and dark field illumination in an attempt to
discover the physical nature of the pigment and differences between samples* For a complete discussion of the work done, reference is made to Dr* Seuai's report on Para Red - Blue Shade for January 1936* Ti In this examination, it was found that the us of sodium silicate as an immersion medium was of considerable value inasmuch as Para Reds, in common with many other organic pigments, are somewhat soluble in the
ordinary immersion mediums*
In addition to the above, microscopic examination has been made of flushed inks as compared to regular inks and of a
copper phthaloeyanine ink, for dispersion* Insults in both eases were inconclusive due to difficulties in dispersing a pigmented vehicle and in securing uniform mounts*
Under color analysis, three types of work have been
in progress this month*
mounts have been and are being prepared
for Sr* A*W,, Kenney of the Experimental Station for use in his study
of the possibility of defining numerical shipping limits* Mounts showing
differences within shipping limits have been prepared on masstones,
extensions, and brushouts and mounts on lacquer tests and linoleum tests
are now being prepared* Our part of this study, that is preparation
and visual reading of the mounts, should be completed within the next
two weeks*
Second, continuation of the work on securing physical
data on our more important standards is proceeding* Speotrophotome trio curves have been run on ten red pigments and completion of work on this particular group should occur within the next month* At such a time
a report will be written drawing sueh tentative conclusions as may
be indicated by the data obtained thus far* It may be mentioned that
five curges are being run on eaeh standard, i#e* masstone, skindown* print, 1:3 extension, and 1:100 extension. Calculation of dominant wavelength, excitation purity, and brightness factor from these curves is being delayed by the lack of a calculating machine*
. .r
DU P050316728
- 3 *
7?
Third* work has been done in the study of blues, especially of the copper phthaloeyanine pigments* Prints have been mad and speotrophotometrie curves obtained for several such blues in various degrees of extension with alumina hydrate* A special report on a number of blue pigments is now in the process of preparation*
A report on the spectrophotometrie study of chrome yellows (drawdowns) has been prepared* and is filed under "Physical Studies."
In the preparation of mounts on RT~Sg0 standard fox spectrophotometrie analysis, average thickness of printing ink film was determined by the area-volume method as *00239 millimeters or *000094 inches* This value should* of coarse, be regarded as an approximation* but one which indicates the order of thickness of a printing ink film as applied to litho label paper by the pi atan press in the Sales Service laboratory*
DUP050316729
vtGmm ooim mammon i
1__
BY: APFROYSD BYS
C'
INTRODUCTIOH"
miltWG. STUDIES BAYS! JAMFARY 1956*
A series of grinds was made in th semi-works to match the performance of the usual settling of the semi-works #1
12-inch pulverizer for the grinding of iron "blues with that of a settling of the 8lnch pulverizers*.
SUMMARY AND COHClUBIOirS
A. "batch of B-66-B lump from lot 4489 was ground
in the semi-works #1 12-Inch pulverizer at 6800 R*P*M* through the
#055 inch HB screen and in the 8-ineh pulverizer with various settings* The smaller pulverizer best matched the performance of the larger one when running at 5812 R,P.M, with a 5/64 inch screen*
See notebook #46?, p*110--111*
Speed
Screen
12-ineh pulverizer
Residue on screen in % 80 150 200 325
6800
*055 HB
17*14 11.48
8-inch pulverizer
8566 n tt
.059 in. 3/64 1/16
it 1/4
4980
039
R 3/64
ti 1/16
l/4
5812
*039
n 5/64
it
n lA
46.26 43.78
65.34 79.30 21.12 27*84 46.60
53*20
15.64 19.84 31.96 46.68
12,72 11.96 11.60
9.92 14.56 16.00 11.64
13.26
17.02 15.00
14.28 17.02
12-inch pulverizer
6300
.035 EB
1.04 5.48
10.62 11.48
8-inch pulverizer
4980 5812 5812 8058 8030
8030
039 .039
3/64 3/64 l/l6
1/4
1*08 0.76 0.92 0.52 0.86
4.24
8.00 6.04 5.98 1.32 5.52
12.50
12.04 884
12.94 4,02 7.00
12.54
14.56 17.02 15.00 10.60 13.04
14.22
DUP050316730
PIGMENT COLOR BBflKdBffi REPORT PARA RH mm
FILE* PARA RED DATE: JANUARY 1936
If
Work was continued along the following lines:
A-Phy*ical studies B-Variations in the relative rates of formation
of Para Red aM Para F C-Variations in the concentration and kind of
dispersing agent D-Barium salt formation of the incorporated
Para F 1- Some semi-works observations
SUMMARY AWP CONCLUSIONS
(A) In the course of this work it was believed necessary to obtain certain physical data on the microscopic nature of Para RedBlue Shade* The Physical Department has made these measurements.
Products prepared in the absence of Para Soap are com posed of hard glossy aggregates which may be factored giving irregular particles* The major portion of these particles is optically inactive, that is, amorphous, probably as a result of solid solution* In silicate immersion at 8200 magnifications, anisotropic pin-point spots and occasional needles were observed. Comparison with 0-38319 showed the latter to contain a much smaller amount of optically active spots and practically no needles. RT-70-D contains as few if not less than the C number. From these data it is inferred that the latter two are probably in more complete solid solution than the former*
When dusted on a microscope slide, RT-70-D aggregates appear larger than those of the C number. Attempts to break down the agglomerates caused smearing* These smears are due to the Para Soap present in the pigment since products prepared with out Para Soap do not smear* Oblique illumination of these smears in a dark field showed no scattering* Hence these red smears are true solutions containing moleoularly dispersed Para Red, Para F or both, as well as possible impurities. The Para Soap (c. Zfo by wt.) may merely impart fluidity to the solid solution, acting as a third component. This seems more feasible than a surface coating of the indefinite lumps of solid solution*
The extent of smearing may be considered an approximate measure of the Para Soap content. RT-70-D smears more than C-38319, and both smeared more than a baked sample of 490-20 B which was pre pared initially in the presence of twice the amount of soap used in the preparation of R^-VO-D,
1
DUP050316731
5^
It Is not impossible that plant prosessing ohanges may be concerned with the loss of Para Soap. Forexample, higher temperatures as in baking, or over-drying, or the heat and shear of grinding may
produce a slow evaporation f the Para Soap*
There is no apparent way to determine the nature of these
optically active points and needles whieh appear in the final pigment*
As previously indicated Para F and Para Red are probably isomorphous*
The angles of extinction of the two substances in polarized light are
approximately equal, and equal to the extinction angles observed for
the anisotropic points and needles observed in the pigments. Consequent
ly, these may be crystalline Para Red, Para F or mixed crystals. Con
sidering the relative proportions of the Para Red and Para F, it
appears improbable that these active spots are the result of mixed
crystals* On the basis of proportions, it would seem more probable that
these crystals are Para Red which crystallized by way of the Para soap,
and this aging would be accelerated by heating* The higher the
temperature and the longer the time of heating, the greater the perfection
and the larger the crystals should become* Cementation might even
occur in baking treatments and this would be in agreement with the ten
dency of the products to go weak and blue on baking. This may
possibly account for plant processing ohanges, but would not explain
the occurrence of the anisotropic pin points and needles in laboratory
products, particularly since these action points are observed in
pigments prepared in the absence of Para Soap* It seems most probable
that these crystals are Para T incorporated by nature of the mode of
ooupling* In the methods used, Para F is formed prior to the Para
Red* During the course of coupling there is an increasing formation of
lf&Cl. This may salt out crystalline particles which are mechanically
included in the micelle
standing, the bleeds yield definitely
crystalline Para.F.*}
Such a picture is equivalent to a very fine dry mix of the
Para F with a solid solution. Since dry mixing does not in general attain the maximum brightness of either component, it would appear de sirable to seek a uniform molecular dispersion of the Para F in the Para Red,
Such a molecular dispersion will obviously depend largely on the relative rates of ooupling of P.K'.A. to B.ET. and mono acid F.
The ideal case would probably require that something of the order 50
Para Red molecules be formed per single Para F molecule* Another major factor involved appears to be the Para Soap. Consequently, ex
perimentation was oarried out along these two lines, (see parts B and C}*
(B) Coupling has been carried out in alkaline media; e.g. in
KaOH - NagCOg as per RT-70-D, or in IfaOH - NaHCOg, and these couplings have ended on the alkaline side. Coupling in a medium of HaOH - EFaCgH30g, ending acid to Congo, but not to Clayton Yellow has given certain in teresting results. The products were bright, hut light in masstone
and the loss in Para F was considered wasteful since equal masstones
oould be obtained in an NaOH - EfaHCOg medium with less mono acid F.
DU P050316732
?!
By inverse coupling (adding BN component to the diazo) it is
possible to begin on the acid side and end at any desired pH. Thus we
have an additional empirical method of governing the relative reaction rates.
Ending slightly on the alkaline side gave hard, brown weak products even though T.R.O, was used. These products were not examined microscopically, but from their appearance and yields, it was apparent that the Para F was not satisfactorily dispersed. Ending at a high pH
gave brown products which were improved by acidification, but were not
as strong as those obtained heretofore. There was some blueness of undertone, although this may merely be a result of weakness.
When coupling ended strongly acid to Congo products were ob tained in improved yields* They filtered very rapidly, were soft in
texture and had much more blueness in undertone than has been obtained
heretofore* These products were tinetorially unlike those obtained by
the usual diazo to B.N. coupling method in NaOH-NaCgHgOg only in having more blueness in undertone. They were light and weak vs. C-36670 but
the undertone approached that of the C number somewhat, and appeared to
justify further investigation. Increasing the amount of Para F present gave hard brown products typical of mechanical mixtures of the Para F and Para Red unless the products were developed. When developed and
filtered hot, the strength increased to about that normally obtained
(490-20B) but the masstone remained very light vs. 490-20B. The products have about the same depth as RT-70-D. Theyare light, and very bright in masstone and s. blue in undertone versus 490-20B. These products (490-37C2 and D2) are close to a match for C-36670 in masstone and brightness. In tint and undertone they are strong and yellow. These colors may be expeeted to develop further blueness on processing. However, they may become lighter in masstone, If they do not this may be a method of matching the C number.
Series were run in which variations in final acidity were
studied. In general, increasing the final acidity yields lighter masstones and the strength increases to a maximum.
From an approximate examination of the bleeds it seems that less
Para F is retained by these reverse couplings, but some is definitely retained by the pigment under the experimental conditions. More accurate data will be accumulated. The Para F is present as the free acid and is probably incorporated as such rather than as the Na salt
which is probably the usual case in alkaline couplings. This difference may readily account for the tinctorial differences noted.
The products obtained by this inverse coupling method appear
to be almost entirely crystalline. They smear when rubbed in a slide
due to the T.R.O. present, but the smears contain a large number of
crystals. Since some Para F is apparently retained, it appears that
instead of solid solutions, mixed crystals were obtained. This uniformity
may account for the corresponding increase in brightness. These same
phenomena were also observed for product prepared in the presence of a
large excess of Para F* The average particle size is roughly between
o,5 - l.o
It is interesting to note that 37A, made, under the
same conditions in the absence of mono acid F did not possess blueness
of undertone, and yet the particles were of the same order of magnitude
in size. From this it would appear that the "adsorbed dye" restraining
action is not very great compared to the dispersing power of the T.R.O.
DUP050316733
and further that the blue shade in the Para Bed depends on the incorporation of Para F*
9"^
It is interesting to note that the products are yellow
in the reaction slurry. If this slurry,is smeared on glass and
allowed to air dry the product remains yellow, and possesses no apparent blueness. Tet this blueness develops when the product is finished up as usual. It may be that the dissolved Para F exerts
an inhibition toward crystal perfection (Kolthoff and Rosenblum: J.A.C.S. 57, 607 etc.) but after filtration and washing, the dye
on the internal surfaces is included in the perfection of the crystals on drying at 60C
Thus, it appears that in the inverse method of coupling mixed crystals are obtained whereas in alkaline couplings the products (C number and RT-70-D types) are probably solid solutions* These phenomena may possibly be related to differences in the lattice parameters of the free acid and the soda salt of Para F
In the crystalline product^ the masstones are light and bright with
blue undertones while the products isolated from alkaline media
are dark in masstone and yellow in undertone and tint. The strength, which appears to be concerned with hot development and may there
fore be an aging process, is approximately equal in both types of product* It does not seem highly probable that these two products
will have a common meeting ground in which the advantages of both may be combined, unless it is accomplished by a dry mix*
It is interesting to note that these crystalline products and their aging may be studied quite rigorously, not only by their
optical properties, but also "by ionic exchange and Para F ex traction. These methods would furnish insight into the kind and
amount of surface present. Surface is obviously a measure of
particle size, but the kind of surface appears to be equally signif icant since from the present evidence it appears that the nature of
the Para F incorporated may be ouite important tinctorially. It seems not impossible that incorporation of the free acid of Para F may be responsible for the blue undertone. The influence of this free sulfonic acid group in the pigment may have some affect on the vehicle in which the pigment is used,
(c) Series were run in which a study was made of the kind
and the amount of soap used. In alkaline couplings of the NaOH NaHCO* type it was observed that diminution of Para Soap caused the product to become light and flat whereas increasing the Para Soap caused bronzing* This bronzing may be the result of the solvent action of excess Para Soap on the Para Red as disoussed in part A. It is interesting to note in this connection that bronz
ing is practically eliminated in the semi works during grinding* For a medium of NaOH - NagC03, a large increase in Para Soap caused bronzing, in the masstone the product became weak and flat.
Diglycal stearate gave promising results when used in amounts about equal to those of Para Soap normally used. The
products were slightly lighter but brighter, sodium abietyl sul
fonate gave stronger products which were lighter and brighter than those produced by Para Soap.
DU P050316734
n-5
(D) As indicated in earlier reports the Uhlieh sample C-36670 was shown to contain barium, and certain experimentation was conducted along these lines* The Ba salt of Para F is best prepared in acid media. This requires removal of the excess nitrite in alkaline couplings* This may be accomplished by urea treatment of the diazo, use of insufficient nitrite or removal of excess NOg- from the slurry by washing. All three methods were compared* In general, the yields are increased, but the product is no longer ashless* On the other hand, C-36670 contains 3.38# residue. The product obtained herein contained 3-3*5# residue. In the absence of Ba salt formation the ash content is
0.8#*
As indicated in the December report, the rate of filtration of these products was increased by precipitation of the colloidal Para F as the Ba salt*
In the series in which the excess nitrite was removed by washing, the product acidified and struck with Ba, the products were darker than those not treated with Ba. This may be due to increased retention of Para F sinee the Ba salt is less soluble than the STa salt, although there might have been a trace of nitrite present to form nitroso BIT* Studying the temperature of development, it was observed that there is little tinctorial difference between colors truck at 83C and those at 65G. However when developed ti> 95c the colors become light. Ba salt formation outs down the Para F bleed considerably. Compared to the Ka salt the ratios are:
22o - 1:10 ; 65 = 5:2 ; at 95e = 5:3
In other words at equal temperatures there is a greater loss of the Para F when present as the Ha salt* Thus the additional depth in color may be due to increased retention of Para F* This same observation obtains in comparing the Ba containing product at the three temperatures studied* The higher the temperature of development the lighter the masstone. These colors were all filtered hot.
Colors prepared by coupling urea treated diazo to BIT in the usual way (NaOH - NaHC0,, raeoia and development to 65C) when compared with a similar product which was acidified and struck with Ba 9 were dark and brown* The Ba containing product filtered faster and was obtained in higher yields.
By restricting the amount of nitrite used rather than the urea treatment, striking cold in the usual medium pH = 7 - 7.3 and developing to 65c the brightest product was obtained. {acidifica tion caused browness, due undoubtedly to a slight excess of nitrite. It appears that small amounts of nitroso -BN produce marked tinctorial deterioration.) There was a slight increase in yield and a good in crease in the rate of filtration. The product was softer in texture than 490-20B and appears to be as bright and possibly a trace darker. On baking, this product went light in masstone, weak and blue in tint. The Uhlieh blueness was not reached.
Barium was incorporated in the diazo in the inverse coupling method and the products were filtered cold* The product was light in masstone, and strong in undertone. However, the product was weak versus products obtained by development in alkaline couplings.
DU P050316735
6
No comparison can be made at the present time since these products were not developed* It is planned to study this point further since the products obtained were dark and bright against RT-70-D and bright against 490-SOB, although light and weak*
(E) Two batches were made in the semi-works, and the details will be reported elsewhere, although certain observations may be discussed here*
The outlet surface of the press cakes after washing showed
the greenish fluorescence of Para F* This type of diffusion phenomenon may be related to bronzing, and as has been previously indicated the tedious filtration is related to the Para F present in colloidal suspension in the reaction vehicle* Ba salt formation would probably eliminate both these objectionable features.
It is well known that Para Red - Blue shade is sensitive to development at 95 c* On the other hand, the pigment may be held at 65o for many hours at pH 7 - 7.5 without any great change tinetor-
ially* It is interesting, however, that there is a physical change, viz., an increase in yield. This anomalous increase was discussed in December report, and a possible explanation was given*
EXPERIMENTAL DETAILS
N.B. #490
Series 490 - 50* A non-bleeding Para Red for paper coating to replace RA-26-D* Barium salt formation, its influence on bleed in water, and the rate of filtration* Residue determinations*
Series 490 - 51* Continuation of 490 - 51* Urea treated diazos and those prepared with reduced nitrite concentration* Ex tension of products with Gloss White*
Page 140 - Notes on semi-works trials.
Page 144 - Microscopic examinations.
Series 490 - 58* The incorporation of diglycal stearate and sodium abietyl sulfonate: Barium salt formations and concentration variations.
pH valueso
Series 490 - 55.
Series 490 - 54. medium of NaOH - NaHCOg*
Inverse couplings: decreasing final Variations in Para soap: coupling
Series 490 - 55* Variations in Para Soap: coupling medium of NaOH - NagOOg*
Series 490 - 56* Inverse couplings: final pH values low, intermediate, and high*
DUP050316736
-7*
Series 490 - 57* Inverse couplings: increasing concentrations of mono acid F; the influence of developing at 22 o, 6So and 95c#
Page 17S * Microscopio examinations*
Series 490 56* J concentrations*
of the Para F#
Alkaline couplings with reduee mono acid Inverse couplings with Ba salt formation
DUP050316737
PIGMENT COLOR RESEARCH REPORT PARA RED - YELLOW SHADS
SUBMITTED BY: APPROVED BY:
FILE: PARA RED DATE: JANUARY 1936
INTRODUCTION
In the course of the investigation of Para Red - Blue
shade, it became neeessary to conduct certain experimentation to obtain Borne insight into that nature of Para Red - Yellow Shade* Since, at the present time, certain difficulties are being encountered In production, the following data are presented* No intensive research
was carried out and the results are those of several isolated series*
SUMMAR--Y A--ND----CONCLU--S--IO--N--S
0jk.T
The method of diazotization of F.N.A* used through was
#276-44* Whiting was omitted* Consequently, the yields were diminished
by approximately 10$* ^or that reason, products called ''strong" herein
are approximated only on the strength beyond the initial 10$*
In alkaline coupling media (NaOH - NagCOg or NaOHNaECOg) the presence of Para Soap appears to be contra-indicated. The products are strengthened considerably but the masstones are dark and
brown*
A coupling medium #276-600 (NaOH-NaCgH,,0,,) which is
initially alkaline but finishes acid to Congo, but not tS layton Yellow gave promising results* ^he products were light and bright in masstone and quite strong versus RT-22-D* This formula seems reasonably stable since it was checked in a second run*
Running the diazo into a suspension of B*N. precipitated by HC1 appears to be entirely unsatisfactory* The product is very bright but very weak and the time of coupling unduly long*
It was found possible to use Turkey Red Oil without
the usually accompanying brownness of masstone by an inverse method of coupling #490-37A* The strength was materially increased with the decreasing particle size* ^he crystalline particles appear to be of the
order of magnitude of 0*5 - 1*0 fiau
EXPERIMENTAL DETAILS
See notebooks #276 and #490*
Series 276-44; Series 276-57:
Series 276-60: Series 276-61: Series 490-37:
Method of diazotisation*
Comparison of various alkaline media for the coupling of RT-22-D*
Acid couplings* Notably "A" a check for 276-60C. Inverse couplings using Turkey Red Oil*
DUP050316738
PIGMENT COLOR RESEARCH REPORT
3^
*7
PARA RED RA26D
SUBMITTED BY; APPROVED BY:
FILE: PARA RID DATE: JANUARY 1935.
INTRODUCTION
The preparation of an Ra -26v D for paper coating which is non-bleeding in water*
SUMMARY AND CONCLUSIONS
On the assumption that the water bleed of dark Para Reds is due solely to the soluble Para F contained, it is possible to prevent this bleed by Bariu# Salt formation, since the Ba salt of Para I is more insoluble than the Na salt or the free acid in water and acids* However, it appears to be completely hydrolysed in alkaline
media*
The procedure for the preparation of RA-36-D involves a slightly alkaline coupling bedium* This cannot be directly acidified due to the excess of nitrite present, but it is possible to restrict the amount of nitrite used or to remove this excess by washing of the product prior to acidification, or by urea treatment of the diazo solution* These three methods were used without detriment to the color and the slurries were struck with BaClg in slightly aeid media* The products were studied at this point for a more vigorous comparison of water-bleed, rather than after the extension with the gloss white.
It was shown eolorimetrieally that the bleed at 22Cof the RA-26*D type is approximately ten times that of the product struhk
in slightly acid medium. At 65C the ratio fell to 5 to 2 and at 95C it became 5 to 3. Tbds increasing temperatures cause# a more marked increase in solubility of the Ba salt than for the Na salt, although the Ba salt is always the less soluble of the two salts*
When extended with gloss white, the products were tested for water bleed according to TF-7-2, and colorimetrically* The products struck on the acid side did not bleed (the color test used is sensitive to 1 part in 1,000,000)* whereas those struck on the alkaline side did bleed and the color ratio of the two bleeds was found to be 1 to 10, in close agreement with the values formed fcr the unextended colors.*,
EXPERIMENTAL DETAILS
See notebook 490*
Series 49030i pages 126 - 133*
Study of Ba salt formation, its influence on the rate of filtration, extent of bleed and tinctorial properties* Colorimetric method of comparison of Para F bleeds, and measurement data - for unextend ed products*
Series 490-31: pages 134 - 139
Methods used fSMtereduction of nitrite, their influemce
si. DUP050316739
8-
W
tine tori ally in the toners and lakes. Bleed comparisons and baking influence in the toner#
f
*rr --
DUP050316740
FIGMENT COLOR RESEARCH REPORT
PARA RES PARK IMPROVED RT-70-D
SUBMITTED BY: APPROVED BY: ^
FAR A
FILE: Ml SC. TUftiffiST DATE: JANUARY 1936
INTRODUCTION
Two trial runs were made in the Semi-Works on an experimental Para Red B formula (490-20B), The products were quite bright in masstone (by rubout), but did not have the blue undertone and tint required to match the ccmpetitive product, Further work in the SemiWorks has been postponed because of pressure of more important problems, but will probably be resumed during the next month,
SUMMARY AND CONG LUSIONS
Both batches were made on the same basic formulation, (Onefourth mol batches were made in each case). The formula differs in some details from K-7347, Semi-Works development for ashless para B which has been inactive since 1933, The ehief differences are in (a) method of preparation of the diazo (a modified cold method is used) (b) a very slight increase in Mono Acid F (c) an increase in amount of bicarbonate in the coupling*
One semi-works batch was washed with cold water, and the other washed with warm (150F) water. The latter batch, as expeoted, was lighter, stronger, and yellower than the former. Washing time was of course deeresed (cold water, 212 gallons in 13 hours} warm water 106 gallons in hours)
Results on these two batches were satisfactory versus RT-70D both being darker, vs lighter, stronger and yellower than this standard. Hot water washing gave s lighter, vs brighter, stronger and s bluerresults than the cold water washed material. Against a com petitive sample 0-38319 (Uhlich) this hot water washed material was vs bright, and strong, but yellow in tint Work is in progress in the laboratory in an effort to match the very blue tint of the com petitive sample.
Results are tabulated in Table I
DUP050316741
EXPERIMENTAL DETAILS
N-B. 455, pages 50-51
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DU P050316742
PTrrwrrcT c o l o r r e s e a r c h r e p o r t
CALCIUM LTTHPL TOHT5RS. RT-579-D MV RT-500-P
3L- 3$~
s'
SUBMITTED BY; APPROVED EY; ^
'
BILE: LITHOLS DATS: JAMJARY 2936
I3S7TROBUCTION
Plant production was high on Calcium Lithol Toner, RT-579-D, during the month a total of ten hatches being reported* Bright masstone material was the principal type product required although complaints have been made by the Control Laboratory concerning the high strength of present plant production which necessitates the use of Blanc Fixe as a shading material# Extension of the toner with Blanx Fixe is undesirable because of the difficulty of securing uniform material#
Two batches of RT-SOO-D were also made with material satis* factory for rubber being required#
SUMMARY AMD CCMCPTSIOHS
The first four batohes of RT-579-D are outstanding from the latter part of last month* Control on these batches was satis factory the desired light and strong material being secured in the case of the first batch and three batches of required dark, bright and strong material then being secured* The usual variables (tem perature of development, amount of TOBW used and amount of calcium chloride used) were used to secure the desired results*
The next four batches, made the first part of January, were also made to secure dark, bright and strong material with fairly consistent results# The first three batches were satisfactory but the fourth, made with a new lot of '1Lithosol,f Acid TOB (lot 160) was slightly muddy in masstone*
A complaint was then received from the Control Laboratory that present plant production on this Lithol Toner was too strong, which made it necessary to use Blanc Fixe in shading the color and that there was a possibility of complaint by customers because of the presence of this white pigment in the Red Toner*
The next two batches were made using variables that tend to give weaker material* The first batch was made using 75% TOB 25% TOBW and striking in the low coupling volume* This variation heretofore had the tendency to give weaker material but with the disadvantage of giving muddy masstone. The resultant product was bright but remained slightly stronger than the standard. The next batch was made to check this batch except that the caustic soda in the coupling was cut 4%* The combination of the two weakening variables gave material that was only vvs stronger than the standard RT-379-D but the undesirable slightly dirty masstone was also secured*
DUP050316743
Recent shipments of "Lithosol" Acid TOB (lots 158, 159 and 160) hare shown a tendency to give blue tint RT-379-D a type which we have not been able to make satisfactorily for same time* These results were not oo'nsistently obtained with these lots, however, as yellow tint material was also obtained with practically no variation in the formula used*
Three satisfactory mixes have been made totalling 5767 pounds which consumes a major portion of present plant production There are at present 1846 pounds of RT-379-D in sub-standard stock;
Production is tabulated in Table I and the mixes in Table II* Two batohes of RT-30Q-B were made during the month using the standard K-7038 formulation. Satisfactory rubber material was the type required. Control on this produet has not been very satisfactory the material made with recent shipments of ''Lithosol" Acid TOB (lot 156, 160) giving dirty results in rubber versus Red ST standard* A batch made with lot 159, however, gave satisfactory results. As production is low on this color there is no opportunity to study and check results secured using variations in raw material* A satisfactory 685 pound mix has been secured consuming most of present production* RT-500-D sub-standard stock is low totalling S77 pounds* Production is tabulated in Table III and the mix in Table IV*
DU P050316744
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DUP050316746
PIGMENT COLOB RESEARCH REPORT CALCIUM LITHOL TONER RT-81Q8-D
3 L' ^
SUBMITTED BY; h $ APPROVED BY;
PILE; LITHOLS DATE: JANUARY 1936
INTRODUCTION
Development work was started In the Semi-Works on a new Calcium Lithoi Toner to replace RT-379-D. A 0.2 molar batch size was used in all cases with E-8108 being used as the basic form ulation. A total of five batches were made and studied during the month .
SUMMARY AND CONCLUSIONS
The K-8108 formula differs mainly from that of RT-379-D in that Mono Acid P is used in the Beta Naphthol solution to secure the dark and blue effects desired rather than the use of TOBW mixed with the TOB in the diazo (which gives the same effect in RT-379-D) The use of ammonium chloride as a buffer in the coupling is another variation that may be noted*
The first batch was made to check the standard K-8108 formula using TOB lot 159. Some difficulty was encountered in making the diazo, the TOB precipitating before adding the sodium nitrite when using the formulated Volume of 590 gal/mol. An Increase to 480 gal/ mol was found necessary to prevent precipitation. This last volume was used In all subsequent batches. Because of this trouble or for some other unknown reason this first bateh was off, being consider ably darker, bluer and weaker than either RT-379--D standard or K-8108*
The next batch was made to exactly check the first including the use of TOB lot 159 and the higher diazo volume* Results were satisfactory, the product being darker, stronger and vs bluer than RT-379-D standard and vs light and bright, ws strong, and s yellow versus K-8108*
The next two batches were made to exactly check this second batch except that TOB lots 158 and 160 were used respectively. Fairly good checks to the second batch were secured even when using TOB lot 158 which had given abnormal results when used in making Barium Lithol Toner (see RT-364-D report for January 1936).
TOB lot 160 was selected as satisfactory for use in making a variable study and the fifth batch was made to check the above except that the Mono Acid P was omitted and the Beta Naphthol was increased in molecular proportion. A 2% excess of Beta Naphthol was used in this batch and the Mono Acid P is used as 73$ material* This formula, of course, resembles the RT-300-D standard more close ly than RT-379-D. The resultant product was, as expected, consider ably lighter and yellower than either RT-379-D or 10-8108. Rubout
DUP050316747
aad snubber tests were then made versus RT-300-:d with the following results: by rubout the material was s dark and considerably brighter, s strong and s yellow versus RT-300"D and by rubber test was vs strong, very yellow and clean in tint versus Red SX (the RT-500-D rubber standard)? k rubout was then made versus a competitive sample of Galolua lithol Toner 0-38413 (Sherwin Williams) which is browner in masstone, vs blue in tint but 10$ stronger than RT379~D standard. Our new product was ws light but bright, t o weak and yellow versus this C# It is believed that use of a small amount of Mono Acid # in this type formula will enable us to match the competitive product* A variable study will be made in the SemiWorks before this formula is released for plant production*
Results are tabulated in Table I*
DU P050316748
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DUP050316749
PIGMUSfT COLOR RESEARCH REPORT
CALCIUM LITHOL LAKE RL-S1Q#-D
SUBMITTED BY: .<)0Ao APPROVED BY:
'
FILE: DATE:
LITHOLS JANUARY 1936
INTRODUCTION
In con junction with the Serai-Works development of Calcium Lithol Toner, -8108, a study was made on a Calcium Lithol Lake, K-8109, to replace RL-408-D (extended RT-379-D for rubber)* Two batches were made during the month*
SUMMARY AM) COLLUSIONS
The <*8109 Toner formulation is an exact check to K-810S
except that the Mono Acid F is omitted with the Beta BTaphthol increased
in molecular proportion* The coupled soda salt is extended with
163#/mol of Blanc Fixe and the slurry struck and developed as in
10-8108, The finished RL-8109 contains
toner as compared with
I&OfeS toner in RL-408-D standard*
Two checks to the standard -8109 formulation were made,
T0B lot 159 bdng used in each case. Check rubout results were se cured both batches being dark, strong and vs blue versus -8109 and light, strong and yellow versus RL-408-D In rubber both batches were practically identical to K-8109 and about 12$ stronger and s cleaner than RL-408-D*
Work will be continued in the Semi-Works to secure a com plete variable study before finally releasing the formula*
Results are tabulated in Table I
DUP050316750
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DU P050316751
PIGMENT COLOR RB8HR0H REPORT BARIUM LITHOL TOUR. RT*564~P
J
SUBMITTED BY: S % APPROVED BY:
.
lEffi! LITBPLS DATE:- JANUARY 1936
INTRODUCTION
Production in the plant on this color continued under Development Section supervision. A total of five batches are reported this month inoluding three batches outstanding since December, 19350 Li^ht and strong material was required for shading purposes#
SUMMARY ABB SCNQ-LUBliNE
Control on this oolor remains unsatisfactory the principal difficulty being the production of material no more than very slightly dark in masstone, satisfactory in strength and O.K. or blue in tint versus RT*364D standard#
The first batch reported was made checking the present plant standard formula (check to K-7390 except using 45#/ mol of Para soap instead of 60#/mol) except that the Beta Naphthol used was dissolved at a temperature of 750 ** 80F instead of 160eF* Solution is secured by adding the Beta Naphthol to the cold water with agitation* the caustic soda, in solution, is added to the Beta Mapthol in suspension and the mixture stirred to solution* The mixture may be heated slightly, if necessary, to secure complete sol ution* This variable has given limiter results in a Barium Lithol Lake fRL-dOS^D). The resultant oolor was dark, blue and vs strong, an abnormal result, and was due to the use of"Lithosol"acid TOB, lot 158. This result was checked in a subsequent batch omitting the Beta Naphthol solution variable and cutting the Para Soap which is a variable used to give lighter material* The abnormal dark result was again secured using TGB lot 158#
The remaining three batches were made to secure light material with satisfactory strength# To reserve this result the out in Para Soap (84#/mol and 18#/mol instead of 60#/mol) was used together with TOB lots 156, and 160* Results were normal the resultant products being light, O.K. in strength and yellow versus the standard*
A satisfactory 1635 pound mix has been made consuming part of recent production* Sub-standard stock on this color remains high being 2255 pounds#
Production is tabulated in Table I and the mix in Table II*
DUP050316752
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DUP050316753
PIQMBHT GO LOR RESEARCH REPORT
MEDIUM CALCIUM DITQL TQEBR. RT-gtB-B
SUBMITTED BY; $ APPROVED BY:
?3Be BTJGLS RATE: JANUARY 1936
INTRQDUCTX?
Production on RT265*D was started in the plant to aanufaoture dark and vs blue shading material to mix off approximately 800 pounds of substandard stools averting light and vs yellow versus standard RT-265-D* Two batches were made under Development Section supervision*
s u mma r y Mm cmcinsiONs
Considerable difficulty has been encountered in recent months in securing blue tint RT-265-D. Hie one variable, that con sistently gives blue results, that of substituting'Lithosol aoid TTlDBW for part of the "Lithosol" Aoid TOB used in the coupling, also gives weak and dirty tint and is undesirable for this reason*
The variables used in these batches were those that had given blue results in RT-265-B production during 1934* These variables included use of a mixture of M Gum Rosin and B Wood Rosin, decrease in alkalinity of the coupling by cutting the caustic soda used in the Beta Naphthol solution, and cuts in the volume of soda salt development and strike volume. The first batch was made omitting the out in volume of soda salt but the second batch was made using all these variables to give blueness* Results were un satisfactory both batches being dark and bright, strong, but yellow in tint versus RT-265-D* The only reason that can be given for these consistently yellow results as compared with previous production is changes in the quality of the rosin or Lithosol Acid TOB*
A satisfactory mix totalling 1257 pounds has been made, however, consuming all but @8 pounds of outstanding sub-standard stook together with one batch of this month*s production* A small amount (less than 1%) of Mapleo Red light was used to secure the blue tint required to secure a satisfactory mix* Sub-standard stock is low totalling 529 pounds which includes one of the dark, bright yellow batches made this month (weight 444 pounds)*
Production is tabulated .in Table I and the mix in Table II.
DUP050316754
EXPERIMENTAL DETAILS
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DU PO 50316755
PIGMENT COLOR RESEARCH REPORT HANSA YELLOW LAKE. YP-534-D
fOf
SUBMITTED BY: C.\ .litm> APPROVED BY:
'
TILE: HANSA YELLOW DATE: JANUARY 1936
INTRODUCTION
Production was started in the Semi-Works on YP-334--D to build up standard stock* There is no sub-standard stoek on this color so that satisfactory material was desired. A total of eight batches were made during the month*
SUMMARY AND 0 QNGLTJ SIGNS
All eight batches were made on the same formulation checking SW-7208 which had given satisfactory material in recent production. All eight batches were satisfactory averaging vs green and dirty in toptone, O.K. in strength, and vs green and clean in tint.
A Variation from the standard method of dissolving the aceto acetanilid, that of adding the dry material directly to the dilute alkaline solution without pulping with water beforehand, (as in the standard formula), was tried in two of these batches with practically no effect on the quality of the solution or on the final product* In the case of one batch in which the diazo was contamin ated with lead nitrate it was necessary to clarify the diazo in order to separate the precipitated lead compound (lead chloride?#* This batch was also satisfactory*
Yields were low on these eight batches averaging 96^ of estimate* This is a 3fa decrease in yield under that secured in the last Semi-Works series* The use of a weak lot of MNPT (lot 456) may be partially responsible for this low yield*
A satisfactory board mix has been made consuming all of these eight batches and the mix is now in process*
Results are tabulated in Table I*
DUPO 50316756
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DU P050316757
PIGMENT COLOR RESEARCH REPORT
SUBMITTED BY; fvV L %*k APPROTSD BY:
RED TOMER K-7699
FILE: MISC. TOHERS . DATE: JANUARY 1936
' XMTRODUCTION
Work on K-7699 (MNPA-BF) was concluded during this month. Material very close to the original K-7699 was obtained and a large sample has been prepared for Philadelphia*
SUMMARY AMD CONCLUSIONS
The main difficulties in matching K-7699 were due to low purity of the Meta-nitro para anisidine (D-S334) Increases in depth were obtained by increase in MNPA and decrease in the amount of seoond component. This combined with a slight increase in Hydrochloric and acetic acid resulted in material of satisfactory masstone, brighter, cleaner undertone and an increase in strength of over 10$ compared with K-7699. A composite mix was made of four 05 mol. laboratory batches which checked each other closely* This mixture K-7699 {487-53) tested in lacquer is slightly light and bright versus K-7699. A pound sample was shipped to Philadelphia for evaluation.
e x p e r ime n t a l d e t a il s
487-46. Series.Increase in Meta Fitro Para Anisidine by 5, 10 and 15$,
A 5$ increase resulted in an increase in brightness, where as a 10$ and 15$ increase resulted in increased depth accompanied by a loss in brightness.
487-48. Lowering the amount of second component to balance the Meta Fitro Para Anisidine D-2234, which is of low purity, and in crease in acetic and Hydrochloric acid each by 5$ were studied. Hydro chloric acid was added to the diazo* Distinct improvements in depth were obtained with the inorease in acidity and the depth of K-7699 was reached. Material of a darker masstone but possessing a faint brownish cast was obtained with the inorease in Aoetic Acid.
487-50. Two 0.5 mol. batches were made on the formulation 48D (increased Hydrochloric acid)* Both batches were decidedly lighter than material obtained on the mol. couplings. During coupling the development of carbon dioxide caused severe foaming. Ho development of C0S was observed in the 0.1 mol. couplings#
487-51* Two 0.5 mol, couplings similar to Expt. 50, but with increase in A.cetie Acid. The Sodium bicarbonate was added to the RF solution just prior to addition of the diazo. The Sodium bicarbonate is added undissolved and shall dissolve progressively during the coupling
DUP050316758
i
2*
A7
process so balancing the alkalinity of coupling. No carbonate develop
ment takes place when the sodium bicarbonate is added just before coupling, whereas a strong development occurs when the sodium bicarbonate is completely in solution* At the start of coupling this causes
trouble by foaming and results in undesirable shade.
48752* Check runs on 51* Material close to 51 was obtained,
487-55. Composite mix of 51 and 52,
N.B. 487, page
*
DUP050316759
PIGMENT COLOR RESEARCH REPORT
3
* N.B.S. MAROON
SUBMITTED BY: APPROVED BY:
FILE: MISC. TONERS DATE: JANUARY 1936.
INTRODUCTION
Preliminary couplings of M.N.F.A, to N.B.S. were made witli the object of obtaining dark maroons for MDulux"*
SUMMARY AND CONCLUSIONS
The diazonium of M*N*F*A. was coupled to N.B.S, in an
alkaline (Na003 NaOH) medium* %e N*B*s* was taken into caustie
solution by preliminary wetting with dioxan*
In the presence or absence of Turkey Red Oil, heat development of the product in alkaline media gives improved darkness and brightness* If the medium is acidified the reverse is true* The products tend to become light and flat dn development*, The use of
Turkey Red Oil appears to be advantageous. The products are not only
softer in texture, but darker in masstone. The best product was obtained using T*R*0* and development in alkaline medium.
The products show some promise, '^hey have good hiding power* In this respect they are better than RT-297-D and probably better than RT-354**D* The products are darker than either standard* The increase in depth comparing product lGa with RT-354-D is greater than the increase in depth observed in comparing RT-554D with RT-297-U*
EXPERIMENTAL DETAILS.
Notebook #499, page 8. The influence of development in alkaline eoupled products*
The influence of acidification, and development of the acidified product*
The influence of T.R.O. Development and acidification of T.R.O. containing products.
DUP050316760
PIGMENT COLOR RESEARCH REPORT ALIZARINS TOMER RT-552-D
SUBMITTED BY: APPROVED BY:
FILE: MISC.TONERS DATE: JANUARY 1936
INTRODUCTION
Three laboratory experiments were run in order to produce brighter plant material. Plant production has been lacking in depth and particularly in brightness.
SUMMARY AND CONCLUSIONS
This series included a study of lower development tem perature, shorter time of development and the adjustment to a pH of 6.0 before development. A pigment very slightly dark and slightly bright versus standard was produced by adjusting a sample of plant slurry (Lot 47305) to a pH 6.0 and developing in the laboratory#
EXPERILENTAL DETAILS
N.B. # 440, p. 57
Observe the effect of holding at 165C for three hours, then bringing to a boil
A - Plant slurry (Lot 47274) filtered and washed
B-
" " held at 165F for 1 hr.
c- w
" " " n 165F " g hr,
D~
" '* n n ]_65F for 3 hr.
E ~ D brought to aboil and boil 2 minutes
Results
A vs Std
B vs
tt
C t tf
D M tf
E tt It
dk.
ft
It ft
ft
muddy, T
ft
n ?
blue;
It H
tf
If
O.K.,
ft
ft
tt tt
blue
it tf
ft
ft
-
Light fastness - equal
tt it
ft
tt
ft
?t tt
n it
tt
B vs A
C vs A
D vs ?t
It , n
n
muddy.
It
r!
o*:K; str
YS yellow tt tf
vs clean - Light fastness - equal
str, " tt rt _ ws better
$f tt . n
?t
vs better
E It ii
it
nr *
n equal si yellow - Light fastness vs better
P. 59
Study the effect of adjusting plant slurry to pH 6.0 be fore development
A - Control (Lot 47305)-usual development B - Adjusted to pH 6.0
Results
A vs Std. dk. O.K., vvs. str. -yvs str, s blue - Light fastness - vs better
B vs
vs dk, s bright, vs str. - vs str, vs blue - "
"
n
s-h!; ...... si
DU P050316761
-2-
//<>
B vs A si. It, vs bright, O.K. - O.K, vvs yellow - Light fastness - equal
P. 60
Rapid development of plant slurry
A ~ Control (Lot 47305) usual development B - B - brought to boil as fast as possible and
boiled 2 hours
1 Results
A vs Std. dk, vs brown vs str: O.K, si blue - Light fastness - vs better
B vs " "
"
"
tt H
Tt
tt
_ **
W *
B vs A, vs It., O.K., O.K; O.K., vs dirty - Light fastness - equal
l
j
DU P0 50316762
tit
PIGMENT COLOR RESEARCH REPORT
LACQUER MAROON TONER* RT-554-P
SUBMITTED BY: &.<A APPROVED BY: /
FILE: BORDO MAROONS d a t e : Ja n u a r y 1936*
INTRODUCTION
Work on this problem was continued in the semi-works# Attention was given to materials used and chiefly to seledtion of a suitable lot of T,0*B*W. Batch size was reduced to 0*1 mol to prevent increase in substandard stock. In the plant one batch of RT-150-P was
made for Farlin*
SUMMARY AND CONCLUSIONS
With Lot #34 T*0*B*W., which had been used in most of the work to date, the product obtained on the smaller charge was satis factory in depth and brightness*
However, Lot 33 could not be used although several variations were tfied* The resulting products were too light*
Lot j?35 gave a dark product with satisfactory bright
ness on both 0*1 and 0*2 mol charges although it was necessary to keep
the alkalinity of coupling very low, 2000# of this lot were ordered for use on RT-554-D* Material obtained with this lot was used to make up 2500# of standard material in which was included 1800# of a slightly light "off" mix carried in substandard stock. Substandard is now
2193# and oonsists almost entirely of light material*
The shift to the smaller coupling equipment used for the reduced charges had the effect of giving a slightly lighter and brighter product in lacquer* jgtvthat this tendency was due to the vigor with which the small charge was boiled in the large size
development vat and in latter batches more moderate boiling was employed*
The red appearance of the diazo from T.O.B.W. lot 33
le$ to the erroneous conclusion that this lot contained too much Bronner*s Acid. On this basis, mixture with various amounts of T.0.B* Regular were tried without improving the product* It was learned from the Dyeworks that Lot 53 was actually low in percent of Bronner's, con taining o$ly 5# as compared to 7,4$ in Lot #34 which was satisfactory*
Adding Bronner's Acid to Lot #33 to make up this difference was not
successful*
The mixtures of T*0,B. Regular and 6 or 7% of Bronnerrs Acid which had previously given sufficient depth resulted in light products* However, the poor results of this series can be fairly
definitely Ascribed to the type of B*0,N, {beta oxynaphthoic acid) used* This assumption is supported by the fact that B,o*N, lot #145which was used, also gave the only light products obtained with the satisfactory
T*0B*W. lot f35 while B*0N. lot #154 gave dark products. Further
comparison of these two lots will be made in the laboratory. The first thought that the difference may be due to moisture content was found to be incorrect*
DU P050316763
2 irty
It is Relieved that with intermediates of the type indicated above no further difficulty will be experienced in the semiworks, at least during cold weather, in obtaining depth and brightness. Some doubt is felt about maintaining brightness during summer months due to possible instability of the soda salt* Use of ice on or after coupling may correct this apparent difficulty*
The batch of RT-130-i*, made in the plant, was similar to that made last month in formula and in lacquer test on slurry control* A sample of pulp dried in 8 1 inch cake was slightly light and brown in lacquer* However, the material appears to have been satisfactory for Pariin's needs*
DUP050316764
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DUP050316765
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DUP050316766
PIGMENT COLOR RESEARCH REPORT
LACQUER MAROON RT-354-D
SUBMITTED BY' APPROVED BY:
/
INTRODUCTION
Laboratory work was started this month on RT-354-D with the object of improving the stability of the formula K-7507. Offshade material is occasionally obtained due to difficulties encountered in control of the present formulation.
A further object of this investigation is to improve the depth and brightness of RT-354-D over its present standard, in order to match Harmon's Deep Infrex Maroon*
SUMMARY AND CONCLUSIONS
The difficulties in controlling the process for RT-354-D appear to be in the coupling which does not go to completion* The coupling reaction ends with a slight excess of diazo and a faint excess of B.O.N. The excess diazo remains through the various steps of the process and disappears only when the development temperature reaches approximately 70C* It has not been determined whether the decomposition products of the diazo have a beneficial or harmful effect upon the pigment properties but undoubtedly reactions of this kind are difficult to control* Work was directed to eliminate the exeess diazo. An increase in alkalinity forced the coupling to completion, but resulted, however, in a lighter shade owing to insufficient excess B.O.N. which is necess ary for the formation of the iron salt of Nitroso-B.O,B, upon which RT-354-D is dependent for its depth* However, the depth of RT-354-D was obtained by increasing the quantity of B.O.N.
The T.O.B.W. is another factor which causes inconsistencies in shade: first, through the tendency of the quick crystal growth of the T.O.B.W. diazo which influences the rate of coupling and causes varia tions in the excess of diazo, and secondly, through variation in the amount of Broenner's acid in the T.O.B.W.
Experiments in which the quantity of Broenner's Acid was varied in the T.O.B. regular in the laboratory indicate that the maximum depth and brightness is obtained with 7-8$ Broenner's Acid. This is in agree ment with recent semi-works studies, in which 7.5$ Broenner's acid was found to give maximum depth. Therefore, 7*5 percent added Broenner's Acid is recommended in the ibfcure preparation of RT-354-D* Efforts were made to eliminate the T.O.B.W. by T.0.3. reg. Neither slurry mixes of T.O.B. reg.-B.O.N. couplings with Pigment Green B, nor couplings with T.O.B. reg.-B.O.N. * Mono acid F showed any promise*
No definite improvements in depth and brightness over standard RT-354-D were obtained. However, some promising leads, which warrant further investigation, have been uncovered.
Semi-works trial of the higher alakline complete coupling method, using 7.5 per cent Broenner's and an increase in B.O.N. excess, is
&eommehded*
DUP050316767
EXPERIMENTAL IE TAILS
424-279 Substitution of T.C.3. res. for T.O.B.7. results in very light end flat material versus control on RT-554-D formulation*
Addition of Pigment Green B and Green Toner GL-407-B gave only a very slight increase in depth and caused poor dispersion in lacquer*
424--28* Decrease in volume by 504 had no marked effect. T.O.E. reg. - B.0.IT. Mono Acid F coupling resulted in light and dull material; however, it was darker and brighter than the straight T.O.B. reg - B.O.r. coupling.
Applying modification of alkaline buffered coupling and long digestion Ijadopting working procedure of K-8108 (calcium-LitholJ] material was obtained which showed a distinct improvement over its control. This series, however, was made without the formation of the Nitroso B.O.N. Iron compound and therefore very light versus RT-354-D*
424 -89* Increase in alkalinity of coupling by 5, 10 and 20;'o in NaOE gave complete coupling (absence of excess Diazo) with 10yo increase in NaOE resulting in lighter but slightly brighter material* A 204 in crease in NaOH showed fe tendency toward browness*
424-50* Modifications of the improved Calcium Lithol formula tion (K-8108) were applied to RT-554-B. The variation consisted of an increase in Sodium acetate* slight increase in alkalinity, use of Ammonium chloride and longer digestion time* These variations resulted in light material*
424-51* Increase in copperas* A 10$ and 204 increase in copperas, and an increase of 104 excess B.C.N. in the higher alkaline coupling 29C procedure resulted in no improvement in depth.
424-52* Neutralization of the Sodium salt of the T.O.B.'W.E.O.N. dye with EC1 immediately after coupling (lowering pH from 10.2 to 7.). resulted in slightly darker material versus the control,but lighter versus standard RT-354-B.
Lowering the pH to 6.8 resulted in decreased depth* Addition of the excess B.O.IT. as nitroso compound (formed separately) resulted in decreased depth.
424-55* Study made on 29C formulation* Addition of excess B.O.IT. as nitroso compound resulted in slightly lighter material, checks results of 32. 104 increase in copperas resulted in a slightly lighter material* A 104 substitution of B.C.N. by Mono Acid F resulted in a lighter shade. The dye of T.O.B.W. - Mono Acid F is lighter than the dye of T.O.B.17. - B.O.N;
424-54.59. Adding Broennerrs acid to T.O.B. reg. in various amounts*
T.O.E. reg* Broenner's Acid
984 24
DUP050316768
3* )<7
Increasing amounts of Broennerts acid in T.O.B.W. resulted in an increase in depth, maximum depth being obtained with a Broennerts acid content of 7 to 850.
424-55 Separate diazotisation of T.O.E. reg. and BroennerTs acid, mixed together before coupling, and separate coupling of Broenner*s acid diazo followed by T.O.E. reg. diazo, resulted in no improvements, in the laboratory, which would justify a change from our present standard procedure# However, these changes in procedure are worthy of some consid eration and should be checked in the semi-works* This was however studied on the formulation with high alkalinity of coupling which seems to be less susceptible to the effect of crystal growth of the T.O.B.77.diazo*
424-56* Development of the Sodium salt of the T.O.B.W.-B.O.N. dye at the boil results in an increase of crystal size,of the dye# The fine irregular particles of the sodium salt obtained are distinctly crystal line. Preparation of RT-354 from heat developed dye resulted in very light material* Filtration and reslurrying of the boiled sodium salt results in a much brighter and darker product than obtained with the un filtered dye but which is still much lighter than RT-354-D*
424-37* Increase in Hydrochloric acid in order to balance the high alkinity of the completely coupled 29C dye, and a similar variation on a dye prepared by substituting Nitroso B.O.N. for B.O.N. as coupling component, resulted in darker and slightly brighter pigment than the control* The nitroso-B.O.N. coupling is of interest since all excess B.O.N. is already in the nitroso form, which is necessary for composing the Iron complex. The material is dark, slightly brown versus control but still light versus RT-354-B#
424-58* Readjustment of pH to 9#6 on the 37 formulation# This study was made withe the sodium salts of 37 series* No conclusions can be drawn as the sodium salt was detrimentally influenced by long standing after diluting*
424-40* Addition of the excess B.O.N. as Nitroso B.O.N. dissolv ed in caustic resulted in a slight increase in depth but gave a distinct brownish east. No increase in depth was obtained by this orocedure on the formulation with high alkalinity of coupling (29-C}*
424-41* Reducing the rate of coupling to 1/3 and eliminating the digestion on 29-C formulation showed no considerable chabge. An increase in depth was obtained with an increase in Hydrochloric acid by 10%, this checks previous results (37),
424-42* Pouring the sodium salt of the T.O.B.W.-B.O.N. dye into the water containing Hydrochloric acid and sodium nitrite should assist the formation of nitroso B.O.N} however, no appreciable im provement in shade was obtained in this experiment*
424-45* Increase in excess of B.O.N. by 10%, 20% and 40% A 10% increase gave a slight and a 20% increase a very distinct improve ment in depth. The depth of RT-354-D was reached in the laboratory with the 20% increase in excess B.O.N. in the formulation employing completely coupled dye.
DUP050316769
PIGMENT COLOR RESEARCH REPORT GEE'S!'! TONER. GT-537-D
SUBMITTED BY: C.} ?}{*** APPROVED BY:
. '
FILE: P.T.A.COLORS DATE: JANUARY 1936
INTRODUCTION
Semi-*Works production was started the latter part of last month on the manufacture of clean GT-337-D for shading sub-standard stocks A total of five batches were made with a total estimated weight of 175 pounds,
SUMMARY AND CONCLUSIONS
The five batches were made using Brilliant Green B as a shading dyestuff to produoe the clean results desired*
Rubout results were satisfactory average results being dark, vvs strong and vs blue and clean versus GT-337-D,
Yields were satisfactory, the lump yfeld averaging 103$ of estimate
A satisfactory 306 pound mix has been made consuming the first three batches made in the Semi-Works (total wt. 106$) together with 200 pounds of dirty tint sub-standard material* Sub-standard stock now consists of 531 pounds of dirty tint, O.K. strength material and 75 pounds of clean material representing the last two batches of Semi-Wor ks produe tion *
Production is tabulated in Table I and the mix in Table II,
DUP050316770
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DUP050316771
fl^>
PIGMENT COLOR RESEARCH REPORT
ORANGE LAKE. K-8098 and 8099
SUBMITTED BY: (i <s APPROVED BY:
/
FILBs MISC. LAKES DATE: JANUARY 1936*
INTRODUCTION
Three batches of Orange II lake were made in the semi-works in a trill of the laboratory formula K-8098 This was developed to mateh Ansbacher-Siegle's product, 0*38038* by dry mixing with Y -299-L and blanc fixe*
SUMMARY AND CONCLUSIONS
Semi-works products were duller in mas stone and yellower in undertone than the laboratory standard* This is due to rate of strike us&d* In the semi-works as in the plant, 2 minutes is as fast as the barium chloride can be added thru a line while in the
laboratory the precipitating agent was dumped in. Increasing the time of strike frcm 2 to 6 minutes gave a lighter yellower product with greater strength. Striking at 150 instead of 1300F had a similar effect although the contrary was excpeeted from laboratory results*
Drying at a constant fcpml&ity of 50$ gave a very slightly weaker and slightly bluer product*
All the material made was mixed as K-8099 and will
be submitted to the customer, Binney and Smith. The mix which employed
less Y-299-D and more blanc fixe showed some of the dullness and yellowness of the straight orange lake*
EXPERIMENTAL DETAILS
N*B. #430, p. 57.
All charges were l/20th of K-8098 using 20# Orange II dye lot 17 which was also used in Laboratory work.
SW-7581 - BaClg added in 2 minutes at 130F vs K-8098 - v.s.lt. muddy; yellow, s,strong; yellow*
SW-7591 - BaCl2 added in 6 minutes at 150F vs K-8098 - light and flat; yellow; strong; yellow*
SW-7596 - BaClg added in 2 minutes at 150F vs K-8098 - light and flat, yellow, s.strong, yellow*
The following are portions of the above batches dried in the
P &.S Dryer at 140F 30$ Humidity* Gradings are against the portion dried in the Freas Dryer at 140oF*
DUP050316772
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SW-7582 vs 7581 - s.dark; v.s.bl* & wk+, swk, s.blue* SW-7592 vs 7591 * v*s*dark, v*s.blue, *s. wk*, v.s.blue, SW-7597 t s 7596 - v.s.bright, v*a.blue, v.s.wk, s*blue*
Lot 4458 - YL-8099-D Mix of above (113#) plus Y-S99-D (14#) and blanc fixe (32#) v K-8099 v.s. dark & dirty; yellow; v.s. weak; s yellow vs C-58058 v.s. dark & dirty; yellow; s. str.; yellow, s. clean
DUP050316773
PIGMENT COLOR RESEARCH REPORT PEACOCK BLUE LAKE BL-164-D
3^1
1/
SUBMITTED BY: j) $*** APPROVED BY: ^'
PILE: MISCELLANEOUS LAKES DATE: JAMJARY 1936
INTRODUCTION
Production on this high finish Peacock Blue Lake has been continued at intervals over the past two months in both plant and Semi-Works. High finish material was needed to shade existing low finish sub-standard stock*
SUMMARY AND CONCLUSIONS
Two check batches of BL-164-D were made in the Semi-Works using the following variations from standard K-7986: the soda ash in the base was increased 11% to secure improved finish and the dye was decreased 7% in order to secure a product a trifle closer to stand ard in strength than has been secured in recent production. The reason f.pr this increased strength may be the use of a new lot of 'Lithosol Brilliant Blue E (lot 31 instead of lot 88) or the diffic\ilties involved in controlling drying during the winter months. The use of controlled humidity drying should reduce this last possible variation to a minimum, however. Both batches were dried in the seme manner at 1403T - 40% Humidity and the resultant color in each case was very close to standard in finish but was strong and s red and dirty in tint.
An attempt was made to make a satisfactory mix with this material together with some high and low finish material from sub standard stock but with no success. The material available is, on the average, too high in strength and too low in finish to blend satis factory.
A plant batch was then made to check the standard K-7986 formulation except increasing the soda ash in the base 80% in order to secure improved finish. The product showed the desired Increased finish but was strong and s red and dirty in tint versus BL-164-D standard. Because of the high strength this material was also unsatisfactory for shading present sub-standard stock.
A second plant batch is in process checking the Semi-Works batches reported this month except that the dye was cut 39% below the standard in order to make a weak, high finish batoh for shading material. Results on this batch will be reported next month.
Semi-Works production is tabulated in Table I and Plant production in Table II.
DUP050316774
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DU P050316775
FIGMENT COLOR RESEARCH REPORT RAW MATERIAL TESTING
SUBMITTED BY; APPROVED BY:
FILE: RAW MATERIALS DATE: JANUARY 1956.
The two items outstanding from the November report remain* to be tested.
This month 92 shipments of raw materials were
received and have the following status: 28 tested satisfactorily
in the laboratory; 4 used without testing; 6 satisfactory when pre viously tested; 5 Remaining to be tested; 15 awaiting completion of analysis; one shipment returned, wrong material; and 32 reported without test.
A shipment of M.N.P.T. frcm the duPont Bye works produced a flat mas stone when tested on the RT-386-D formula. 'Ehis
material was included in the investigation mentioned in the December report.
Raw Material Samples
Thirteen samples were received this month.
RMS-1484 F*c.O*N.A. from Verona chem*Co* Satisfactory.
RMS-1485 - Sod. Molybdate, du Font.
RMS-1486 - M.N.P.T, ) Caleo.
RMS-1487 - "
) Unsatisfactory.
RMS-1488 - M.N.P.'1. from Sherwin-Williams* Satisfactory*
RMS-1489 - Bleached Barytes from F.E. Shundler. Unsatisfactory*
RMS-1490 - Naphthol AS-BS from General Dyestuffs orp.
Unsatisfactory.
RMS-1491
RMS-1492 RMS-1493 RMS-1494 RMS-1495
P,c.O.N*A. - Dry - from du Pont*
This material is the dried and ground ^.C.O.N.A. Crude Press cake, RmS-1472* *o be tried on production sdale.
Tri-sulphoil Soap from Scholler Bros* Satisfactory/
Lithosol Scarlet 3BI from du Pont* Satisfactory/
M.N.P.1'* A } from Calco " B ) Unsatisfactory
RMS-1496 - Naphthol AS-BS from General Dyestuffs Corp. Unsatisfactory,
DUP050316776
PIGMENT COLOR RESEARCH REPORT SEMI-WORKS PRODUCTION
3
SUBMITTED APPROVED BY: ^'
FILE: OR-200 DATE: JANUARY 1936
INTRODUCTION
86 batches of 13 different colors, and 13 lead nitrate purification were made during January| these included 11 batches of RT-354D, 5 batches of RT-8108*D, 13 batches of Y-359-D, 17 batches of Y0*8074-D, 8 batches of YP-324-D and 6 batches of GL-407-D*
SUMMARY
RT-554-D, Maroon Toner * Eleven batches were made in a process study on this color with the production of bright material for shading as the principal object* Effect of varying lots of BON was also tested in this series*
RT-8108-D, Calcium Lithol Toner * Five batches were made in a process study of the new calcium Lithol Toner to replace RT-379*D,
RT-70-D, Para Toner, Dark * Two batches were made in a process study of a new formula for aBhless Para Red Dark.
RT-280D, Para Toner, Light Six batches were made in an effort to make bright material to fill an order*
RT-8109-D, Calcium Lithol Lake - Two batches were made in a process study of a new calcium Lithol lake formula to replace RL-408-D*
Y-359-D, Medium Yellow - Thirteen batches were made in connection with the study of lead nitrate purification by the YP5 method*
Y-8021-D, Excelsior Yellow - Three batches were made in a process study of this recently standardized color*
Y-8124-D, Primrose Yellow - Two batches were made in a yield study,
Y0-B074-D, Molybdate Chrome Orange Seventeen batches were made* Thirteen of them in a process study of the color, and the re mainder in a development study of a stronger type.
YL-8098-D, Yellow Lake - six batches were made to use as shading material in manufacture of YL-8099-D*
YF-324-D, Hansa Yellow - Eight batches were made for production of stock,
GL-407-D, Treated Pigment Green - 6 batches were made at the dyeworks in order to try drum drying,
BE-114-D, Extended PTA Toner - One batch was made for stock*
Lead Nitrate Purification - Thirteen purifications were carried out in a study of the IPS method for the removal of copper by precipitation.
DUP050316777
One grind of dry color, 14 grinds of pulp color and IS mixes were made in the Research Semi-Works during January 1936.
Dry Grinds C.P.Yellows
Charge 739-S
Batches 1
Lbs. 100
Pulp Grinds
Red Toners Green n C.P. Yellows
Charge
7 37--S tt ft
Total
Batches
4 5 6
15
Bbls*
14 15 84
53
Xjrto 3*
1044 1320 7024
9388
100> ft ft
tt
Mixes
C .P. Greens C -P. Yellows C.P.Blues C.P.Oranges Ext. Yellow Blue FTA Toner Green " " Red " " Red Toner
Charge
755-S 753-S 756-S 754-S 752-S 751tt *S
ft tt
Total
Batches
e
l
8 1 1 3 1 1 1 13
Lbs .
859 703 382 965 138 423 306 339 255 4364
DUP050316778
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DUP050316779
4BQMMARY Qg #10 BLDG * PRODUCTION REPORT FOR JANUARY 1956
Code
RT354-B RT-8108-D RT-70-D RT280D RL-8109-D Y-359-D Y-8021-D Y8124D YP~324-D YO-8074-D YL-8098-D C-L-407-D BE-114~D
Lbs. Struck
713 415 144 157 330 410 450 310 960 510 120 542 592
5553
Xil^s* Packed
755 411 141 159 226 409 468 302 911 524 119 542 584
5551
% Yield
105*8 99.1 97.8
101,3 97,0 99.7
104.0 97,4 94.9
102.7 99.2
100.0 98.7
99 .8$
DUP050316780
rtf
MATERIAL TRANSFERHEP DURING JANUARY 1956 FROM RE-SBARC H SEMI-WORKS
Lot
CR-200 Color Code
lbs. Groun
Cost Unit Total Cost
4441 42
43 44 49
50 59 60 61 62 63 64 65 4467
1 RT-354-D
1 tt
1n 1 tt 1 rt
1 1
it
tt
1n
1n
1 t?
1 Ft 1 Tt
1 ft
1 RT-70-D
58 2
62 2
60 2
58 2
63 2
58 2
57 2
61 2
61 2
59 2
59 2
119 2
115 2
140
2
110.07 45*40
4445
46 47 48 68
69
70 71 72
3 Y-359-D
3 3
Y-8021-D tt
3 Y-180-D
3 Y-8024-D
3 tt
3 Y-8021-D
3 tt 3 tt
210 2
158 2
156 2 368 2
150 2 153 2
149 2 156 2 164 2
8.80 8*80
8.11 8.70
8.80
4413 4466 4440
4457
8 Y0-34-D 8 tt 8 Y0-38-D 8 ft
45 1 106 2
305 1 288 1
7.29
7.34 7.34
4434
6 BE-149-D
269 2
14.54
4411 4451
4458
11 BL-72-D 11 BL--164--D 11 YL-8099-D
29 1 96 2 157 1
52.82
44.22 20.72
4410 4412 4435
36 37
38
39
25 BT--122--D 25 RT-338-D 25 GT-537-D 85 ft 25 tt 25 tt 25 ft
29 1
31 1 35 2 37 2 35 2 37 2 41 2
150.75 299.41 176.94
4452 115 RT-7853-D
40 2
133.56
4453 125 RL-408-D
48 1
49,25
4455
151 Y0-8074-D
56 151
W
2 13.98 2
DUP050316781
RECAPITULATION
Colors transferred from Semi-Works to Plant during January 1956
Toners Yellows "RE" Lakes Oranges "RL" Lakes PTA Toners
Total
1070# 1664#
157 1503
173 244
4811#
DUP050316782
MATERIAL "H r PROCESS" AS OF FEBRUARY 1 . 1956 RESEARCH SEMI-WORKS-
w in x> tri-3 tn
p 1
rH H tjj 1 o fa O pn
ftt raj to
r-| nil H
i tj|
o O
P t
tO to
1
CD
o o to
P 1
1 in ndj to
Oj
O >h
o Cft to
rH p to 1 i--1
o o CD
1 P r
lO r-l r-|
to P 02 > H co
o rJ4
t p 03
in
w
in P 02 1
in 03 rH
* 6-i CO
to
to
Ip
oo "* P CD
<t>3I> p
nta
0-^0
o co in
P rt< rH P
O
O rH
tO 03
OCft
p 1 pp
CO 1 t o co rH tO CD CJt tO W
o E- E-< Eh o 03 P3 D3
H rH pp
t
o tit
O tO
t Pt
PP
P
O
trH P
w to
1 pi
DUP050316783