Document J37bgOzmBQ4wdk9KveK60pn1K
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PIGMENT COLOR RESEARCH R3PORTS
APRIL - 1935
I - PIGMENT GREEN S Pigment Green B Pulp GT-68-P (EJH)................................ * ** for Paper Coating & Eyeing (AS) .
Page
1-3 4-5
II- RUBBER COLORS RUbber Colors (AJS) ................................................................. Ext. Green PTA Colors for Rubber: GP-7789-D and GP-7863D (EJH) Green Lake for Rubber. GL-7854-D (EJH) ................. ..
III- PERMANENT RED 3-B (GW) ............................................................
6-11
12 13-14
15-17
IV - LITHOL REDS
(a) Azo Sulphite Derivatives (SWR and AAB) .......... 18-20
(bJ Caleium Lithol Toners RT-379-D and RT-300D(EJH) 21-22
(c) Ext. Lithols for Rubber - CS-7664 & CS-7665
S3
(d) Barium Lithol, RT-364-D .(ADR) ................................ 24-25 .
V - CHROME GREENS
(a) Lt.Past Greens - lieadows Type, G-389-D (JDM) (b) Light-East Milori Green CS-7764 (JDM) ............ (e) CP Chrome Green. G-365-D (ADR) ............................. (d) Strong Meadows Greens. CS-7192-7194 (ADR) .. (e) Extended Greens - C3-7826-27-28-29 (ADR) ...
26-30 31
32-33 34 35
VI- CHROME YELLOWS & ORANGES (aT'Mediffin Te 11 ow, Y-359-D (ELP) .................................. (b) Primrose Yellow (ELP) ........................ .................. (c) Oil Retention and Lithographic Breakdown
of Pigments (3CH) .......... (d) Lemon Yellow of Improved Lightfastness (ELP) (e) Excelsior Yellow (ELP) ................................................ (f) Improvements in Chrome Yellows (3CH) .......... .. (g) Study of Lead Cyanamide (SCH) ............................... (h) Preparation of Rust Inhibitive pigments (SCH) (i) Y0-27-D (ELP) ..................................................................... (j) Y0-38-D (ELP) .....................................................................
36-37 38-39
40-41 42 43 44 45 46 47-48 49-50
VII- LEAD & LEAD MATERIALS Purification of Lead Nitrate Liquor (EL) .......
51-51A
VIII7 IRON BLUES (a) Iron Blue Yields - Lab. Study (RED & HCM) ... (b) Study of Iron Blue'Pigments (3CH) ........................
52-55 56-57
IX - WORKING PROPERTIES OE PIGMENTS (a) Treatments to Improve Elov of Pigments(RKH). (b) Dry Dispersed Colors (3CE) .................................... ..
X-
PH0SPH0TUNG3TIC ACID PIGMENTS (a) Improvements in PTA Pigments (SCH) .................... (b) BT-125-D and BT-150-D (EJH) ....................................
(c) PTA Yield Studies: Plant (EJH) .............................
58-59 60
61 62-63 64-65
r
DUP050315658
2
XI -' MFG. STUDIES Grinding of* Pulps (jDM)
XII- MISC. ORGANIC PIGMENTS
(a) Para Chior Ortho Nitroaniline (GWJ) ....................
(b) iffltJPT For Toluidine Reds (AS) ....................................
(dC
Duol Toner Light RT-242-D (EJH) ............................. BBS Maroons
Maroon Toner RT-219-D (AAB) ..................................
Lacquer Maroon RT-219-D (EJH) .............................
Purified NBS for Maroon Toner RT-399D (AS) (e) Misc. Toners
Maroon Toner RT-354-D (AAB) .................................
'* " (ADR) ..................................
Pigment Rubine G, RT-359-D (AAB) ......................
Pigment Rubine G Toner, RT-359-D (ADR) ....
Black Pigments (SWR & AAB) ....................................
Zirconium Compounds (AAB) .......................... ..
(f) Misc. Lakes Color Lakes of Vat Dyes; and acid dyes on
Wool Acids (AS)
Extended Pigment Rubine RE-390-D (ADR) ....
XIII- RAW MATERIAL TESTING (AFCP)
XIV - SEMI-WORKS PRODUCTION (HA)
Page
66
67-69 70 71-72
73 74 75
76 77-78 79-80 81 82-83 84
85-86 87
88
89-95
siv-s" '
DUP050315659
PIGMSET COLOR RESEARCH REPORT
?&'/ S
/
PIGMEKT GREER B PULP GT-68P
SUBMITTED BYs APPROVED BY! Gta/of^
JU 3. 7/ PILE: JiaOC. TOKEKS DATS: APRIL-1935
INTRODUCTION
Eive batches were made in the plant to fill an order for 5000# pulp satisfactory for paper. Mixes were also made of all outstand ing Semi Works lots- and the pulp transferred to standard stock as material satisfactory for rubber.
SUMMARY & CONCLUSIONS
Of the first two batches made the latter part of last month the first, lot 42841, made replacing all the soda ash in the lot 41873 formula with caustic soda gave unsatisfactory results in both paper and rubber, being weak and dirty versus the standard in each case. This material, however, can probably be used in rubber by readjusting the latex formula to take care of this weakness. Part of this batch in slurry form was transferred to the Semi Works and pressing studies made. A satisfactory dry content was secured on the first pressing, and the washed material was successfully treated with brine in the press to secure a hard, firm pulp.
The second of these two batches was made on the lot 41873 formula except that the addition of oxalic acid immediately after striking with iron oxalate was omitted. This batch was satisfactory in rubber and indicated satisfactory paper results by laboratory test.
The three batches made in April were made to check lot 41873 ex cept that in the final batch (43342) caustic soda was used to replace the soda ash in the preparation of the cadmium soap. These lots were all satisfactory in rubber and indicated satisfactory results in paper by laboratory test. Pre-shipment samples on the last four batches will be submitted to the Paper laboratory for test before shipments are made
A satisfactory pressing procedure has been set up in the plant during the month of April, the^use of 22 frames in a 36- l-l/2a pres3 giving a dry content of _25-1/?) for a 2. mol batch. Attempts to treat the washed pulp with brine in the press as was successfully accom plished in the Semi-Works were unsuccessful in the plant, the proce dure being too slow when leakage of color is heILd at a minimum. As these pulps must be pulverized for use in paper, the salt can be easily incorporated in the pulp while pulverizing. This procedure was fol lowed in the case of the last plant batch made with satisfactory re
sults. In the case of the first four batches, however, it was neces sary to reslurry and repress the washed material to secure a satisfac tory dry content. This procedure in the plant is as follows: the 2 mol batch is reslurried to a thin pulp in the striking vat, 1/2 of 1% of salt (based on the weight of the water used to reslurry, + 60 lbs.) added and the slurry repressed in 13-20 frames in a 36- 1-1/2" press. The pump can be used to press this salted slurry without undue loss of color although not advised unless absolutely necessary.
DUP050315660
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. *2-
2 Yields on the untreated dolor were fairly satisfactory during the month, averaging 367# dry or 96.6;2 of estimate. Three Semi-Works `mixes were made to transfer outstanding SemiWorks lots to stock. The first two, 4047 and 4048, were OK in rubber and shipped to complete an order. The laatimix- 4049, contained a large amount of plant lot 42841 that was used in the Semi-Works press ing study and was therefore not satisfactory (see above). lot 41873 has been accepted by Philadelphia as satisfactory for paper and has been set up as the paper standard. GT-68-P production for the month is tabulated in Table I and shipments from stock tabulated in Table II.
DUP050315661
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Consumed In rubber shipment* 161# at + 25j. Completee order
fo r 1000$ dry.
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DUP050315662
<3 A
PIGMBPT COLOR RESEARCH EBPORT
IKLSO. FOR PAPER COATING ATTn DYKING
SUBMITTED BYi APPROVED BTt
Jkf jJ' /-
<**3-7/
FILg* i&SG. TOSiffi&-- DATE* APRIL-1935. -
BtTRODUCTIOg
Orientation studies on the preparation of a dry powder of Pigment Green B which, disperses easily and completely In water hare been completed The experimental work on this new product has been sufficient to warrant immediate serai-works development; however* from the viewpoint of economy* it is advisable to carry out some addition al laboratory studies on the product prior to semi-works develop ment* with the object of reducing the quantity of Leucanol and pos sibly eliminating it entirely.
SUMMARY & CdTCLUSIOHS
W & P milling of the treated pigment has been found unnecessary
in obtaining a satisfactory water dispersible dry powder. Results similar to those obtained with the W & P mixer have been obtained by mixing the regular press cake paste with dextrin and leooanol, pass ing this thru a colloid mill and drying the resultant slurry* The powder ground to a granular form disperses well in water and results in paper dyeings equal to those obtained from the w & material* and equal to slightly superior to dyeings of the regular Pigment
Green 3 paste* The eolloid milled dispersible pigment gives results similar to the w & 3? milled product in paper coating* namely an ap preciable increase In strength and brightness compared with the un treated paste*
The use of soluble rosin size as a substitute for dextrin has been successfully applied* thus overcoming the undesirable use of dextrin in pigment colors* particularly in wall-paper use. The dry pigment prepared with rosin size possesses better wetting and dispers ing properties than the dextrin product. In addition* the rosin sine imparts better working properties to the paste* the product drys much faster and to a much easier grinding cake than the dextrin paste, owing to its foaming properties. The rosin size product gives better working properties and a smoother and softer coating on paper than the dextrin pigment* The use of rosin size in place of dextrin may make the use of leucanol unnecessary, which should be determined by laboratory study*
The pigment content of the dispersible Ary powders can be in creased to approximately 50% compared with approximately 25% pigment content of the present standard paste, with satisfactory results.
Treatment of the regular paste with the above-mentioned wetting and dispersing agents results in material of greater strength than the corresponding untreated paste but which is still appreciably in ferior to the dispersible dry powder tinotorially.
DUP050315663
.2
5XPBRIMSSTAX DETAILS
Dextria-Leuoanol Dispersible Dry Powder
Figment Green B pasteequiv. to -- 70 gms. dry pigment
isDextrin (Chlordex) ----------------------------129 (contains + 1$ moisture)
Leueanol ---- ----------------------------------
(dry)
"
* 33.6^ pigment
Rosin Sine - Leueanol Dispersible Dry Powder
Figment Green B paste equlv. to -
giiat jw yigipiiti
Soluble Rosin $iae ----------------------------120 *
leueanol
------------------------------------ 16 " (dry)
* 33,6^ pigment
In each ease the ingredients were mixed to a heavy but workable con sistency with water and then passed thru a Travis Laboratory Colloid
Hill 3 times* The paste was spread on shallow paw and dried at 140 CF, than ground to a granular form, resembling granulated sugar in appear ance* Fine pulverization decreases the wetting properties.
For above see experiment 15, S.B. 460, page 60.
For other experimental data see experiments 52 and 54, R.B.450*
pages 188 and 198 respectively, and experiments 2, and 10, H.B. 460 pages 8, and 40, respectively*
-."SC
DUP050315664
PIGMENT COLOR RESEARCH REPORT RUBBER COLORS
/7SK
FILS:
t?0'L&g
DATE: APRIL - 193 5
During the past month the laboratory has devoted the larger portion of the time to a study of Calcium Lithols in. an effort to im prove the dispersion in rubber. There has also been' some work on Victoria Blue R lakes and on Quinoline Yellow P.
The Semi-Works has started the development of C3-77S9, CS7863 and CS-7854 with very promising results.
SUMMARY & CONCLUSIONS;
Calcium Lithols for rubber have presented a serious problem of obtaining satisfactory dispersion for some time. The past month the laboratory has given considerable time to this problem and some inter esting products have been obtained and, we believe, the foundation is laid for two or three possible lines of attack. However, nothing to date has shown any substantial improvement over C3-7665 which does not, however, give perfect dispersion.
A series with variations in the calcium chloride for precipi tation on the RT-379-D procedure gave no improvement thothe control was better than standard RT-379-D and the corresponding lake was slightly better than CS-7665 when tested in rubber.
A number of variables have been tried using a buffered alka line coupling as has been developed for the Barium Lithol (RT-364-D). The first variable was one in TOB-'.V. As T05-W -was increased the masstone became darker and the tint slightly bluer. The strength increased up to 50$ TQB-Tjf, and then fell off. In rubber, there was a progressive decrease in ease of dispersion tho the inherent strength was shown to be present by refining the rubber which made the poorest one equal to the best. 50$ TOB-W gave a product which was darker, brighter and stronger than RT-379-D but slightly yellow. In spite of its poor dis persion in rubber it was given further study in an effort to improve this property.
Acid development gave some slight improvement as did the addition of 5$ G-ardinol to the Soda Salt, but it was not sufficient to he of great significance. Diglycol Stearate and the combination with G-ardinol gave some improvement but it is even less than the G-ardinol alone.
In another series various treating agents, as Carbitol, Butyl Stearate, Butyl Oleate end Paraffin, as well as those mentioned above were added to the finished toner with negative results. How ever, when the paraffin treated product was heated at 110 C for two hours there was considerably improvement in rubber. As no control was given the same treatment no conclusions are possible as yet.
DUP050315665
-2-
z
Increase in development temperature to tie toil gives some improvement in dispersion but does not equal CS-7655.
Toners from the same type coupling but made from T05 regular were prepared by developing the Ka salt in an effort to give dark, blue products. Up to 60 C development of the soda salt has almost no effect. Above that temperature the toner became duller and weaker.
An interesting procedure was used in which a large amount of whiting was added to the beta naphthol before coupling and the strike made by acidifying to obtain the soluble calcium salt together with a large volume of gas which it was hoped would give a soft product. Strangely, there was no great amount of foaming even during develop ment. A second part containing Gardinol & D.G.3. did not react com pletely to eliminate the whiting and hence had a high yield. There was no startling improvement in texture or dispersion in rubber but there were some properties of interest.
An incomplete series at the end of the month has indicated Jshere may be some virtue in adding small amounts of a volatile sol vent, as kerosene, to the finished slurry. The oil is taken up by the color and finally evaporates after the water has been driven off to give, in theory, soft products. There is some indication that they may also have improved dispersion in rubber and the method is being followed up.
It must be admitted that nothing of substantial value in itself has been developed in this v/ork. However, considerable know ledge of the behavior of Calcium Lithols has been gained and a number of factors shown to give some slight improvements. It is to be hoped that some combinations of these factors can be used to give substantial improvement and it is planned tc continue the 'work.
No work has been done on the Goodrich Lithol except to make a mix of Semi-Works samples of C3-7664 and C3-7665 which was a very close match to RL-400-D. This mix together with RL-400-D and the competitive standard (C-37064) have been examined carefully for stability in var ious types of rubber grinds. We believe.our products to be superior to the competition as more fully set forth in a letter to Hr. E.A. Hoffman under date of April 30th.
The P.T.A. lake of Brilliant Green B was set up as C3-7663. Semi-works development has been started and the first two batches were 15-20$ stronger than the laboratory product in rubber and slightly yellower. The second batch was somewhat stronger and cleaner than the first.
The Semi-Works has also made two batches of C3-77E9 {0T-347-D type P.T.A. lake)- They check each other very nicely and are 10-15^ stronger than the CS, but somewhat bluer. It is planned to make some material well on the yellow side for shading.
The Semi-Works has also sterted development on CS-7254- (Imper ial's Green X-1292). Three batches were very close to each other, equal in strength to the CS, but slightly yellow, Another batch on the blue side will be made for shading.
DUP050315666
3
No work has beer done on a Thioflavine P.7. A., one run was made on Quinoline Yellow to test a new sample of dye. V;e are awaiting
a sample of material representing t'e Rubber Laboratory's production before proceeding further on this color.
A sample of Victoria Blue R was tested and found satisfac tory. A two pound sample was then ordered and a preliminary run has indicated it is also satisfactory. It Is planned*to derelop a P.7. A. lake from It as soon as possible.
Naphthol Yellow 3XX of General Dyestuff was tested against National Naphthol Yellow 3 in C3-7654. The products can be substituted for each other on the basis of 59 ^arts of Naphthol Yellow 3XX for 100 parts of National Nadhthol Yellow 3.
The difficulty with Y-S66-D has been traced to undispersed
pi.;;.;ent which is sufficient reactive to give some lead sulfide during the cure. It has also been shown to be a property of the struck pig ment and in no way related to the processing treatment. No solution is offered and little work has been done looking toward one. One batch which is satisfactory has fulfilled our needs for current ship ments .
One series was run to determine the possibility of using some salt of Lake Red D lAnthranilic Acid - Beta Naphthol) as a sub stitute for Soda Salt of Lake Red C in rubber. The results make it very clear that this color cannot be used for the purpose in mind. However, some interesting facts were developed which will be recorded for future reference. Various coupling methods were tried ranging from a highly alkaline NaOE coupling to the NK4CI buffered alkaline coupling,
and the "acid type coupling11 formerly used vnth Lithols. These last two were far superior in every respect to the straight alkaline coup ling and were substantially alike.* The Ns salts have no application as pigments altho they are quite insoluble. The calcium salt is only a little better giving very unattractive products. However,the barium and strontium salts have good strength and fairly bright nasstones, and tints somewhat similar to Be salt of make Red C (RT-313-D). The stron tium is the better of the two and, at its best, is rated as dull, si. blue, si. weak, blue and dirty against rtT-olo-D; light fastness -.only slightly worse. Altho 'no immediate application is apparent, it is believed that these results represent a considerable improvement over
any previous work on this color.
EXPERIMENTAL DETAILS:
Notebook 461 - pp. 1C-49
461-1 - Orientation studies on coupling of Lake Red D
A - NaOE coupling, high alkali
B - NaOH coupling, low alkali C - NH4CI buffered alkaline coupling D - "Acid coupling" as used in Lithol Reds
A, B, C > D, Al, Bl, Cl, Dl, A2, 52, C2, D2, A3, B3, C3, D3,
Na Salts Ba Salts Ca Salts Sr Salts
All developed at the boil except B A C were filtered cold
y/'; t * -fr
ig#*^
DUP050315667
C2 & D2 were quite yellow and dirty vs. Grange YOD.
All others were too far away to be of any interest. Na Salts are all of no value. Ca Salts are all yellow and dirty and not at all interesting. Ba & Sr Salts are fairly close in masstone but the latter is stronger, bluer and cleaner. C3 vs RT-313-D - dull; s. blue; si. weak; blue & si. dirty.
si. worse in light fastness.
461-2 - Large samples of Brilliant Green B P.T.A. lake was set up as CS-7863.
461-5 - Naphthol Yellow 3XX (Gen. Dye.) was tested in C3-7854 method and found to be*equal to national Naphthol Yellow 3 except that it is slightly stronger so that 89 parts of Naphthol Yellow SXX are equal to ICO parts of National Naphthol Yellow 3.
461-4 - A study of the use of reduced amounts of CaCl in RT-379-D, and the corresponding lakes on Blanc Fixe, showed no improve ment in dispersion in rubber.
461-5 - A new sample of Quinoline Yellow P Ex. Cone, was examined and found to be somewhat weaker than the previous sample but to give slightly superior dispersion in rubber. No further work is contemplated until a comparison with material prepared in the rubber laboratory is possible.
461-6 - A new sample of Victoria Blue R (D-1987) was tested and found satisfactory. Two pounds were ordered for further work.
461-7 - A mix of recent Semi-Works material was prepared to match RL-400-D and was very close. This mix together with RL-400-D and Goodrich Pigment 1440 (C-37064) were examined for stability during
rubber milling as follows:
Six millings of each were made
A - Rolls at low temperature (>100 F) 8 cuts - 8 rolls
3 - Rolls at normal temperature (_+ 160 F) S cuts - 8 rolls
C - Check to B
D - Rolls at normal temnerature
160 F) 5 cuts 4 rolls
E - Rolls at normal temperature
" IS cuts 15 rolls
F - Very hot rolls
(+200 F) 8 cuts - 8 rolls
All the colors vary in shade and strength with variations in milling but C-37064 varies to a larger degree than does RL-400-D or the mix. When the amount of RL-400-B is sterped up lS-EOL it is actually a very close match to C-37064 in a normal milling.
461-8 - Calcium Lithol from NB4CI buffered coupling.
A All T0B B 25# T03-W C 50# TCB-W B 75# TOB-Yv JS All T0B-W
" r-u..
DUP050315668
5
Corresponding lakes {70?!, on Blanc Fixe) .were also nrepared With increase in TOS-W there is an increase in depth of masstone and some increase in blueness of shade. Strength increases up to 50% TC3-W and then falls off. In rubber there is increasing difficulty in dispersion and the lakes are not much better than thi toners in that respect.
C vs. RT-379-D - dark &. s. bright; vs strong; strong; clean, si. yellow. Light fastness - si. better.
Further work was planned to improve dispersion cf C.
3,.-
461-9 - A special method of preparing Ca Lithol was used. A relatively large amount of Whiting was added to the Beta Taphthol
before coupling and the material was subsequently struck by acidify
ing to give a soluble Ca Salt and a large amount of CCg gas In the
hope of getting soft products. Strangely, there was no great amount
of foaming and a second part containing Gardinol and Diglycol Stearate
never completely reacted leaving considerably whiting in the final pig
ment.
It is apparent that the CO2 as such is of little value as the control was very close to 8C in all respects.
461-10 - A Calcium Lithol as in 8C was developed on the acid side as well as the alkaline and both were treated by adding to the 17a salts 5% Gardinol, 5% Diglycol Stearate and a mixture of the two.
The acid development seems to give slightly better disper sion in rubber than alkaline development but all the products are well below the desired dispersion. The treating agents all give some improvement in rubber but the Gardinol gives the most. Here again
the desired dispersion is not attained.
In rubouts Gardinol either alone or in combination with Diglycol Stearate gives light, weal: products. D.G.3. has very little effect.
461-11 - Treating agents added to finished color. In ad dition to those used above (10 series) Carbitol, Butyl Stearate, Butyl Oleate, and Paraffin were added to the finished slurry and stirred until they were taken up. In no cases was the treated pro duct superior to the control. However, the naraffin treated product was subjected to a temperature of 110 C for 2-3 hours and resulted in a marked improvement in rubber. Before definite conclusions are drawn this must be examined more carefully with a control in the
picture.
461-12
study of development temperature is net very con
clusive because of discrenancies in the yield end poor results by rub-
out. However, there is fairly certain evidence of some_improven;ent
in dispersion in rubber with the higher temperatures. nut the pro
ducts are still inferior to C3-7665.
461-13 - A Calcium Lithol yfras in 8A (TC-3 regular) was pre pared by developing the Ka Salt before the strike at various tempera
tures up to the boil. Development at 60 C has little effect and higher erstures give dull, weak products.
i
DUP050315669
*
6 461.-14 - The 461-6 method was used on the two pound samnle of Victoria Blue R (D-2016) vdth variations in the amount of Gardinol. For use in rubber the original amount of 3 gms. with 12 gr.s. dye is considered the optimum.
Sk'ir-y**;
h'i'i*;
`i-
DUP050315670
PIGMENT GOLOR RESEARCH REPORT
3^"''a
EXTENDED GREEN PTA COLORS FOR RUBBER:__GP-7789-D & GP-7863-D
SUBMITTED BY! .3 APPROVED BY:
'
FILE: SUBBER" u&LOR-SDATE: APRIL-T935
INTRODUCTION
Two batches each of GP-7789-D and GP-7863-D were made, and have results available for report. Two more batches on each of these col ors are 3till in process and will be reported next month,
SUMMARY & CONCLUSIONS
The two batches of GP-7789-D were made on a formula 1/5 the size of the standard CS-7789 formulation. Yields were a trifle low averag ing 95/ of estimate, and rubout results were satisfactory, the products being v.s. strong and v.s. blue versus the CS#. In rubber, the pro ducts were also satisfactory, b eing 15/ strong and blue tested against
C3-7789. A batch is in process in which the amount of Thioflavine used is increased to give a yellower product. This product, an extend ed GT-347-D type color, is known as Green EG.
The two batches of GP-7863-D, an extended GT-354-D type color for rubber, were made on a formula l/5 the size of the standard C8-7863 formulation. The first batch ground out 20/ strong, s.dirty and yel low versus the CS# in rubber, but the second batch showed a consider
able improvement over t his result, being 25/ strong and s.yellow with
OK cleanness versus the CS#. By rubout, both of these colors were weak, yellow and dirty versus CS-7863. Yields were fair, averaging 95/ of estimate.
EXHSRIMBNTAL DETAILS
N.B. 408, pages 110-115
Color
Bat eh
Yield
Rubout Results vs. Std.
Sst. Lump Mas s. Draw. Str. Tint
Rubber Results
vs. Std.
Str.
Tint
GP-7789-D EW-6943 30#
28# vs It vs bl vs str vs bl 15/str. blue & drty
6976
tt
29 vs dk
ft
II
II 15-20/ n
str.
GP-7863-D *
6947 6980
2S-1,/2 27 It.
vs wk weak
& drty
It &
26-1/2 muddy vs wk
& yel
s.drty 20/str. s.yel
yel.
s.drty
yellow 20-25/ s.yel. dirty str.
DUP050315671
3 JT'/o $
PIGMENT COLOR RESEARCH REPORT
GREEN LAKE FOR RUBBER, GL-7854S
SUBMITTED BY APPROVED BY:
INTRODUCTION
/ 7^
PILE: SUBBES-COLORS DATE: APRIL-1935
Three Batches of this Green Lake were made in the Semi Works dur
ing the month to check CS-7854 set up to match Imperial's Green Lake X-1292.
SUMMARY & CONCLUSIONS
All three hatches were made l/lO the size of the standard CS-7854 formulation except that in each case the dye volume was cut 10;& to fit Semi Works equipment. In the second hatch a press washed base was used instead of the standard vat washed base.
The three products checked each other quite closely in rubber and were OK in strength, slightly yellow in tint versus CS-7854. Adjustments in the proportions of the dyes used (Lithosol Brilliant Blue E and Naphthol Yellow S) were made in a batch now in process to give bluer results. Results on this batch will be reported next month.
Tabulation of remits will be found in Table I.
DUP050315672
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DUP050315673
PIGMENT COLOR RESEARCH REPORT LITHQ6QL RED 2-B
SUBMITTED BY: APPROVED BY:
FILE: S53C.-TCSERS DATE: APRIL - 1935
5T "1 I;' ijj- _
y;;y >
& 4$
INTRODUCTI OH:
Work was continued this month on the barium toner of Lithosol Red 2-B in an attempt to produce a lighter and yellower pro duct, possibly approaching RT-313-D, Lake Red C, in color value. 'To date, efforts have not been very successful because of the apparent stability of the masstone in the face of all types of operations var iables.
SUMMARY & CONCLUSIONS:
. BARIUM TONER - The formula as it stands at the present time seems to be very dependable, as practically all of the controls give excellent checks against standard. However, most of the dependability of the formula may he attributed to the above-mentioned fact that the toner is practically immune to'the ordinary variables in the prepara tion.
As mentioned in a previous report, the addition of acetic acid before the strike darkens the masstone, develops a slight bronze and makes the tint weaker and bluer than standard. However-^ by neutralizing with caustic directly after the strike, the pigment is made lighter and weaker than the straight acid strike. Neutralization at the boil makes the color still lighter and brighter, but still darker and duller than the neutral control sample.
Addition of 1$ Sodium chloride before striking gives a lighter, brighter masstone, hut a slightly bluer and weaker tint. This masstone was the lightest of any prepared to date.
An attempted zirconium sulfate precipitaticn of Lithosol Red 2-B was entirely unsuccessful because of the excessive spot paper bleed of the product. Increase of precipitant or addition of sodium. acetate had no effect on the reduction of the bleed.
An alum precipitation of the Lithosol Red 2-3 gave a dark brown, dirty product - too dark and dirty to he of any use as a pig ment.
An increase in the time of strike tended to nakethe pigment weaker and bluer - Increase in time from 10 minutes to 30 minutes makes the mas.stone decidedly darker and browner.
An attempt was r.ede tc check the saryle 41C-LL.., prepared at Jackson Laboratory, utilizing their formula. From the extreme difference between the two samples it was concluded that the yellow ness of the 416-22A,sample was*due largely to the hatch of Lithosol a.'-23B from which it was made.
Quenching offered no particular advantage over material fil,tjggrisd.af the boil and for this reason was omitted from the standard
DUP050315674
Concentration of the bErium chloride together with very rapid strikes produced practically no effects except to make the color very slightly weak and blue.
Substitution of Turkey rted Cul for para soap offered no par ticular advantages, except to make the color v.s. light in masstone and vs yellow in tint.
CALCIUM TONER - Work was concluded during the month on the evaluation of the calcium toner lakes (447-17) in ink. Comparisons were made with the toner control, dry extension of the toner and KE-237-D for strength, shade and proofing quality.
It was found that the lakes were 10-d stronger than the toner ground as such, and about 5^ stronger than the dry extension grind of
the toner. The hydrate and gloss white lakes gave better proofs than the corresponding dry extension of the toner. The blanc fixe lake
was only v.s. better than the dry extension. Compared with 311-237-15, the hydrate and gloss white lakes were yellower in shade, brighter, cleaner and better in proofing qualities. On adjusted strength bases, the lakes are equal to'the control toner in light fastness.
From the above tests it may be stated that the hydrate base gave the best results, followed closely by the gloss white lake; the blanc fixe was a poor third.
A report was also received from the Du Pont Rubber Laboratory which confirmed our own rubber tests on the above samples; namely, that all three lakes were practically equal to each other in rubber dispersion and somewhat weaker than the toner. In crocking, all were
equal
EXPERIKENTAL DETAILS:
Notebook No. 447
447-20 - studied the effects of neutralization of an acid strike during the development.
Neutralization of the strike with caustic directly after the
striking operation gave a lighter and weaker product than the straight acid strike. Neutralization at the boil gave a still lighter product, with nractically no strength difference. - However, the masstones in both eases were darker and duller than the neutral control strike.
447-21 - studied the effect of salt on the development and the preparation of zirconium and aluminum toners.
Addition of 1-^ salt before striking gave a lighter, brighter masstone, with a slightly blue ano wea tint.
A zirconium precipitation failed completely because of the excessive bleed of the toner.
An alum precipitation gave a darV brown, dirty and entirely unsatisfactory product.
447-22 - included studies on the time of striking and on the reqhecklng of formula 416-22A.
DUP050315675
Increase in time of strike from 10' to 30' gave a darker, "browner masstone with a weaker, bluer tint.
No semblance of a check was obtained by repeating the 416-22A procedure.
447-23 _ dealt .with the effects of barium chloride concen tration in the strike; with the substitution of Turkey Red Oil for Pare Soap; with effect of quenching.
The effect of barium chloride concentration was oractically nil. Quenching gave no advantage over filtration at the boil. Tur key Red Oil offered no visual advantage as a substitute for Para Soap.
DUP050315676
PIGLEKT COLOR RESEARCH REPORT AZQ SULPHITE DERIVATIVES
Ss'- /o 7
/P"
SUBMITTED BY: APPROVED BY:
iJl
FILE: -MTHOL ft EDO ' DATE: ikPEIL - 1935
INTRODUCTION:
Further work on the preparation of calcium Lithol Red by the CS-7801 (sulphite-ester process) method was carried out with em phasis on the preparation of a suitable rubber pigment.
SUMMARY & CONCLUSIONS:
It has already been explained that while CS-7801 is about 10-15$ stronger than RT-379-D standard by rubout, it possesses very poor dispersion In rubber. In fact, extending with blanc fixe and treating with diglycol stearate produces no advantages. Reduction in e&leium chloride in the strike resulted in somewhat better disper sion in rubber but the inherent strength, of the color (by rubout) was decreased to a point where it is not much better than RT-379-D. Blanc fixe extension of the low calcium toner did not result in any better duplicability than obtained in the case of CS-7665 (present extended calcium lithol for rubber).
Omitting the ammonium chloride from the strike of the low calcium formula gave by rubout darker, bluer and stronger toners with improved light fastness. However, the dispersion in rubber was great ly impaired.
In the case of the high calcium formula (CS-7801), omitting the ammonium chloride made very little difference tinctorially by rub out tests but improved the light fastness appreciably. In rubber no improvement was obtained.
A very interesting lead was uncovered with respect to the effect of temperature of development on texture and rubber disuersion. Increase in the temperature of development from 72 C (C3-7801*) to 100 C gave, by rubout, lighter messtones, slightly weaker and slight ly yellower toners. In rubber, the dispersion was greatly improved. The toner, which was developed at the boil, was practically equal in strength, but cleaner than CS-7665. However, by rubout, this boiled toner was strenger than P.T-379-D, consequently it possessed additional tinctorial power which was not fully developed by the rubber grind. It is possible that, by extending with blanc fixe, this product (44647F) could be made to surpass CS-7665 in strength in rubber.
To summarize the above briefly, it has been found that the sulphite ester process yields a calcium lithol toner which is superior to RT-379-D standard both for printing ink and rubber purposes. How ever, a slight modification of the striking procedure is necessary to obtain a suitable rubber pigment. The latest method (446-47C) briefly, consists in heating to 72o C, a mixture of the sulphite ester of lithol red, calcium chloride and caustic soda, then acidifying with acid before filtration. This product, 446-47C, is darker, about 15$ stronger; slightly bluer and cleaner, and better in light fastness than RT-379-B standard when tested by lithographic varnish rubouts. .
DUP050315677
- %-
In rubber, however, 44S-47C is very poor in dispersion, and blanc fixe
plus digylcol stearate gives no improvement. To obtain a toner which disperses in rubber to give almost equal strength and a cleaner tint than CS-7665 (regular extended calcium lithol for rubber), it is only necessary to develop 44S-47C to the boil instead of to 720 c. The rubber pigment, 446-47F, is about equal in masstone, about 10$
stronger; cleaner in tint and better in light fastness than RT-3 79-D standard by the rubout test.
Printing ink evaluations showed that 446-47C as well as the product made with ammonium chloride (446-47A) were poorer in texture than standard RT-379-D but about 20$ stronger. The 446-47F (boiled) was about 15$ stronger and equal in texture to standard.
EXPERIMENTAL DETAILS;
Notebook 446 (pp. 128-140)
Series 446-45 - prepared toners and extended colors follow ing the low calcium chloride formula, 446-23C, with and without ammon ium chloride. The extended color using ammonium chloride was slightly weak versus CS-7665 (extended calcium lithol for rubber) while omitting the ammonium chloride gave weak results. Both toners were very weak in rubber.
By rubouts, omitting the ammonium chloride gave dark and blue results with considerable better light fastness.
Series 446-46 - repeated the above series but reduced the amount of calcium chloride by 50$. Again, the extended color gave
slightly weak results in rubber while the toner gave very poor results versus CS-7665.
By rubouts, omitting the ammonium chloride gave dark, and strong products with better light fastness, but both were consider
ably inferior in strength to the higher calcium chloride toner.
Substituting acetic acid for hydrochloric gave slightly dark and yellow results.
?/ashing with 1$ soda ash solution, followed with water gave clean, dark and blue results versus control 446-46A.
Series 446-47-48 - prepared samples of C5-7801 with and without ammonium chloride developed at the regular temperature and at the boil, also a sample of ET-379-D for control purposes.
It was found that the boiled samples gave soft products with fairly good results in rubber. They were light and slightly yel low versus CS-7801 and dark and. strong vs. standard RT-379-B by rubout.
Laboratory RT-379-D went off shade for unknown reasons and could not be evaluated for strength and tint.
These samples were submitted for ink grinds.
Series 446-49 - varied the temperature of development from
.,k .
DUP050315678
-f-
'ZsO
7 C to toiling in CS-7801.
Increasing the temperature of development increased the softness of texture.
In rubber the strength increased with the softness in texture, 49D being slightly weak versus CS-7665, while in rubouts the results went light, slightly weak and slightly yellow versus con trol 49A. 446-49B tested O.K. in rubber, versus 446-47E, a previous check.
Sefies 446-50 - prepared oil (litho varnish) treated CS7801. Ho advantage was gained by rubouts. The result was dark, weak and yellow versus CS-7801.
DUP050315679
PIGMENT COLOR RESEARCH REPORT
3 * / & &
CALCIUM LITHOL TOKERS RT-379-P AHD RT-300-D
SUBMITTED BY: C APPROVED BY: #
FILE: ifiSe,-SK8RS DATE: APRIL 195 5
IHTRODUCTIOF
Included in the report this month are one Semi-Works lot of
RT-300-D outstanding from last month and five batches of RT-379-D
made in the plant during April. Bright, yellow, strong RT-379-D was
desired to be used as shading material.
SUMMARY & conclusions
The addition of 20# per mol of sodium phosfate in the coupling in the semi Works RT-300-D gave material bright in top but weak and blue versus the standard. This concludes the work on RT-300-D in the Semi Works for the time being. For tabulated results see Table
I.
The plant batches of RT-379-D were made to check a previous batch, 41501. with slight modifications. Final grind results are available on only three of the five batches made. Yields were fair.
Of the three batches on which grind results are available, the first two were made on the 41501 formulation, except that the sodium salt was struck with calcitim chloride before dilution to development volume. The resultant toner was brown in top, blue and slightly weak versus the standard RT-379-D. Checking this formula but increasing the caustic soda in the Beta Haphthol solution from 61-1/2# to 66-1/2# per 3/4 mol batch gave dark, strong and slightly yellow results versus the standard. The last two batches will be reported next month.
A 2600 lb. mix has been successfully made from material accumula ted oyer the past few months and including the first of this month's batches.
Results on the batches reported and on the mix are tabulated in Table II.
1'
DUP050315680
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DUP050315681
PIGMENT COLOR RESEARCH REPORT
EXTENDED LITH0L5 EOR RUBBER - CS-7654 and CS-7665
SUBMITTED AFPROVED BY:
/? ** ' f*
FILE: LiTEGL REDS DATE: APRIL - 1935
INTRODUCTION:
One additional batch of CS-7665, Calcium Lithol, was made to chock the material found to be satisfactory last month.
Composite mixes of both C3-7664 and 7665 have been made and hre being tested for suitability as standard.
SUMMARY So CONCLUSIONS:
Results of rubber tests on the current batch of CS-7665 were inconsistent but it appears that this run is slightly superior to the former batch. By rubout it was a fairly close check. $
The barium lithol is satisfactory and manufacture of RL400-D from these two colors should not be difficult. A composite of all material on hand (400#) was tested and submitted to the Rubber Division as a tentative standard.
The calcium lithol, while not entirely satisfactory in quality, will also be blended and set up as a tentative rubber stand ,"?U. ard.
EXPERIMENTAL. DETAILS:
Notebook #353, p. 101
SliV-6937 - Check SW-6879.
Rubout vs. CS-7665 - vs dark & bright; vs clean; vs str; vs yellow.
Rubber Test vs. CS-7665 - 5 weak; vs. S'v-6379 - 5>' strong.
DUP050315682
PICrLIEtTT COLOR RESEARCH REPORT BARIUM LITHOL, HT-364-D
SUBMITTED BY: {Wbe~*rs.
APPROVED BY:
^
0
FILE: YITIIOL RfS3 DATE: APRIL - 1935
% ;;; 4:
Wti~
INTRODUCTION:
Production of RT-3S4-D was continued in the plant this month. Two batches of RT-127-P were made and one batch of RT-364-D on the same type of coupling was made for use in rubber. The balance was of the acid coupling type for ink and paint.
SUMMARY & CONCLUSIONS:
RT-127-P, while showing considerable variation on rubout is apparently satisfactory for rubber. The same formula gave a dry product darker than RT-364-D but suitable for use in RT-344-D.
Results on the acid coupling formula have not been entirely satisfactory but the more recent batches are running more normal. Attempts to produce masstones lighter than standard resulted in increase in yellowness of tint. A return to the standard amount of para soap and reduction of alkalinity of coupling are giving bluer products with, however, some increase in depth.
*
:y> '
m
DUP050315683
EXPERIMENTAL DETAILS
DUP050315684
36"-///
lA
PIGMENT COLOR RESEARCH REPORT LIGHT FAST GREERS - MEADOWS TYPE - G-3S9-T;
SUBMITTED BY: APPROVED BY:
). AaJiwwnMO A''
PILE: CkT*OL-. GREET. S DATE: APRIL 1935
INTRODUCTION:
The study of the process variables on this line was concluded this month in the Seni-Vvorks. This report will contain the results on the few batches struck this month* and on a number of them held over from last month because grind results were not avail able at the'time of the last report.
Plant production on this line included five batches of G-38 9-D, 3 of G-39 0-D, seven of 0-391-D and four of G-392-D, a total of nineteen batches. The attempt to secure brightness of
masstones was successful both in the blue and the olive shades, giving satisfactory material for shading.
SUMMARY & CONCLUSIONS:
a---
Semi-Works - The most favorable variable* tried was that of omitting the soda ash in the treatment of the washed yellow. A bright, blue and clean product was consistently obtained with
:i. light fastness slightly superior to standard. Omission of copper hydroxide on this formula, gave a product similar except for increased * rr strength and slightly decreased light fastness. An attempt was made
- to circumvent the instability of the copper hydroxide as used by sub M. stituting the more stable basic copper carbonate. The resulting color
was quite similar tinctorially but the light fastness was reduced.
.u In one hatch, the soda ash was added after the copper hydroxide, only enough being used to assure the precipitation of all the copper. The product altho satisfactory tinctorially was infer ior in light stability. A reduction of 50 in the amount of soda ash used in treatment gave a dull chalky product. Similar results were ob tained by adding alumina hydrate to the yellow instead.of slum and soda ash. The light stability of this batch was inferior.
Hydrochloric acid was substituted for the alum in two
hatches, the acid being added to approximately the same pH as ob
tained by the alum addition. Blue', bright, strong
clean products
were obtained, the light stability decreasing from equality with
standard as the acidity was decreased.
Tinctorially similar products resulted from reducing the alum by 50$, the light fastness being very slightly worse than standard.
The addition cf tin crystals directly after bichromate instead of after the-sodium sulfate gave a dull, chalky product.
Altho satisfactory tinctorial properties were obtained by adding alum and soda ash before flooding rather than after washing,
light stability was materially reduced.
DUP050315685
\
A dark blue, clear, product ruth very slightly inferior
light fastness resulted from the omission of sodium sulfide from the standard formula.
An increase of approximately 4n in bichromate and a cor responding decrease in sulfate to preserve the balance of preeipitants resulted in a superior product considerably more olive than the blue, bright material from the alum-tin-copper hydroxide formulation first mentioned in the summary.
An increase of strike temperature from 110 to 120 in conjunction with the omission of the soda ash treatment gave a color olive and dirty against control and blue against standard with equal light fastness. Striking this color in 5 minutes instead of 30 min. gave s product slightly yellower in undertone and tint.
A combination of favorable variables, namely: the use of double amount of tin crystals after strike, fast strike", and amission
of soda ash treatment, gave a product blue against standard with very slightly superior light stability.
In one batch, the soda ash and copper hydroxide were omitted in the treatment and the tin crystals'were replaced by sodium stannate. The result was dark, blue and strong with, how ever, slightly worse light fastness.
Plant
(1) G-589-D - Two batches struck on standard formula %vith
the omission of soda ash and copper hydroxide in the after-treatment,
of the yellow were light, blue and bright in masstone. The batch
size was doubled to a four mol charge in two batches, the colors being
tinctorially similar to the smaller size strike. The copper hydroxide
was replaced in these to escape the dullness of finish on exposure to
light. The need for bright, olive materiel for shading the blue
material consistently obtained on the above formulation was satisfied
by increasing the bichromate and decreasing the sodium sulfate in the
strike solutions, giving oliveness of masstone, and yellow undertone
and tint. The G-389-D batches are being made entirely in the large
size with the good agitation available from, the fast, direct drive
agitator recently installed.
(2} G-590-D - Cne batch was struck on the high bichromate formulation mentioned in the previous paragraph, and two used an in termediate amount of bichromate in order to obtain satisfactory7 shading material. The colors obtained were slightly olive in masstone and yellow in undertone and tint.
(3) G-391-D - One batch struck or. standard formula, except for a fast strike, was dark, blue end slightly dirty ir. masstone. Cn one batch the amount of soda ash in the base was raised to take cere of an intended increase in bichromate, however, the bichromate was left standard, resulting in a slightly bluer product. The bichromate was increased as intended in the next batch riving e color slightly olive in masstone and blue in undertone and tint. The bichromate was next reduced to standard leaving the soda ash at Its former high value. The 'result of this was a flat, changeable masstone with yellow undertone and tint. This last result was similar to that of one batch
struck on standard formula except for omission of soda ash in after-
DUP050315686
treatment. This omission of soda ash occurred in all hatches but the one first mentioned in this section. One batch struck with increased bichromate but standard sulfate was blue in masstone, undertone and tint. A reduction in sulfate corresponding to the increases in bichromate save a slightly olive masstone with similar undertone and tint.
(4) G-59S-D - One batch struck on. standard formula with omission of soda ash was close to standard. An increase ir. bichro s-':.. mate with corresponding decrease in sulfate resulted in a slightly yellow masstone with blue undertone and tint. Omission of copper hy droxide, also on this formula, gave an olive, silky and changeable v-`. masstone. On replacing the copper hydroxide and increasing the sodium sulfate in the strike solution to standard a product was ob tained with blue masstone and slightly yellow undertone and tint. //:
In all of the four shades of this line, the omission of soda ash in the after treatment of the yellow has materially increased the brightness of the product.
Light stability tests have been made only or. representa tive batches but in these cases results were entirely satisfactory*
DUP050315687
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DUP050315689
PIGMENT COLOR RESEARCH REPORT
LIGHT-FAST MILORI GREEN CS-7764
SUBMITTED BY: MpUUWo*uioj APPROVED BY:
o?/ FILE: ifiie~UHEEN3` DATE: APRIL-1935
7/
INTRODUCTION
Three hatches of this color were struck in the plant during the month, with especial emphasis being placed on the overcoming of instability in the formulation. The improvements made in recent Semi-Works batches were utilized.
SUMMARY & CONCLUSIOHS
Two batches were struck on the same formula, a variation on lot 41367 based on SW-6808. The bichromate was reduced and tin-: crystals added after strike as well as after washing. On both of
these batches the result was a product with a bluish masstone with
clean undertone and tint as compared to G-317-D. In the third run, in which the higher amount of bichromate was used, there was a bi chromate excess after strike, which, contrary to expectations, did not disappear upon addition of nitric acid. The product was very olive, dirty, arid changeable.
Further work will be done on the lower bichromate formula as this appears to be satisfactory in stability both to processing and
in lightfastness.
EXPERIMENTAL DETAILS
N.B. 437, pp. 134-136
Lot
Ob.i ect
Results
Mass.
Under. Str.
Tint
Light Stability
42945
Modification of
s.dk
s.cl.
41367 (Reduced
& bl. *
Bichromate, and
tin crystals after
strike as well as
after washing.
OE vs cl.
vs worse
43162 Check 42945
*v/jZr
5<3t
43283 Check 43162 but
ol.
bl.
increase bichrome, chgble
DUP050315690
PIGMENT COLOR RESEARCH REPORT C.P. CNROnE GREEN, G-565-D
SUBMITTED BY: APPROVED BY: ^'
*
f it v : cftTMnnuip; OR-CTr? DATE: APRIL - 1935
INTRODUCTION:
Production of tMs color has been more olive than standard, and inasmuch as efforts of the plant staff were unsuccessful in controll ing this property, a series of batches was follows by the Development Section.
When the installation of the special direct driven agitator was completed two batches were made with the new equipment.
SUMMARY & CONCLUSIONS:
A control run on standard formula (370/ nitric acid) was olive on slurry and press cake samples. No grind was available due to its being mixed with the following batches.
On all succeeding batches, 355,^ of nitric acid was used. Four batches were made on this formula of which three were slightly olive and the fourth v.s. bluish on control.
A bluer, less clive product was fcJ uuliiwt (J' Ci-O Ot w- J. A. o I. 6 amount of sodium sulphate precipitated with the bichromate. This variable may be worth following un as it has shown a similar effect on G-209-D and GX-312-D.
A batch made with the newly installed agitation (30 minute strike at 16 3.P.M.) was only v.s. olive. Reducing the strike time to 9 minutes appeared to add somewhat to the oliveness althc the dif ference in acetic acid ratio introduces some doubt on the comparison.
No positive conclusions can be drawn as to the effect on this color of the improved agitation. It was not possible to run the agitator at its maximum of 20 R.P.h. due to the sine cf the motor which was installed'.
As G-365-D is being discontinued by Philadelphia in favor of the more light stable G-389-D, no further v;ork will be done. l..ixes totalling about 12,000,- and consuming all the material made were C.P. for Philadelphia. Slightly ever 25>C of blue bright green of washed base type were used for shading.
JWJM.
DUP050315691
EXPERIMENTAL DETAILS N .B . # 2 8 7 , p . 162
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DUP050315692
PIGMENT COLOR RESEARCH REPORT
STRONG MEADOWS GREENS? 05-7192-7194
SUBMITTED BY:--j.
APPROVED BY: A"
.' a
a/ FILE: OIIROkE GREENS DATE: APRIL - 1935
.. . INTRODUCTION:
!?{.' U-r IfF--
' Production of this type of green was resumed in the plant upon installation of the direct driven agitator. Two hatches of yellow were struck employing different speeds of agitation and rates of strike.
SUMMARY & CONCLUSIONS:
|||, No improvement in stability was obtained by striking at ffv 16 R.P.K. on an otherwise standard formula such as has been used Sh. . lately. The yellow was too red to shade.
However, by striking very rapidly thru a sprinkler at 20 R.P.Ivi. a yellow very close to standard was obtained. This is in line with Semi-Works results which showed greater consistency under these conditions.
Sr'' The light shade of Green, 05-7192 was also the most satis factory material produced on this formula.
The dark shade, C3-7194, was more olivex than standard but equally bright. It is suitable for use in G-37E-D, the Fuller Green giving a match for the original C3-7624. The final mix on this color is not completed.
A slight modification of the formula will undoubtedly give the increase in blueness of masstone which is needed in the dark shade.
EXPERIMENTAL DETAILS:
Notebook 437, p. 13
;l:
:fi. p:.;
f&' -4' ' jit:
45131 - C3-7192 - Check 41755 using Vat 261 - equipped with
special agitation. Variable speed and direct drive. Run at 16-17 R.P.il. No sprinkler used for bichromate. Yellow - Red and clean. Hot shaded. 45255 - C3-7192 - Check 43131 except (1) - Sneed of agitation increased to 20 R.P.k. (2) - Strike time - 7 min. instead of 30 min.
(3) - Used sprinkler for addition of bichromate.
Vs. CS-7192 - C.K. ; vvs clean;^vvs str; vs blue; s. clean (v.s. yellov; cast)
Added -
45255 - CS-7194 - 1/3 of 03-7192, Lot 43255 green slurry.
3j Tannic Acid 2# Lead Oxide T.B.L. 266# B-66-D Liquor
DUP05031 5693
PIGMENT COLO3 RESEARCH REPORT EXTENDED GREENS -CS-7826-27-28-29
SUBMITTED BY APPROVED BY:
FILL: HROKE 'CREEPS DATE: APRIL - 1935
INTRODUCTION:
'V ' Gp
jjg-.. v^ \
During February the preparation of several shades of Extended Greens was begun in the Semi-Works for the rurpose of obtaining material for an offering to the Illinois Paint Works. This work was completed last month but results were not available.
:F' SUMMARY & CONCLUSIONS: fr --------------------------------------------
|)T,
Light and dark shades were made of the improved light fast
p ;* (G-389-D) line and of the regular Milori (G-315-D) line. Plant yellow
ry-slurry or in some cases green press cake was shaded and extended in
the Semi-Works to a 30$ Green.
Mixes were made up for standards from which samples -were submitted to the customer. Reports from Sales Service were unfavor able because of too high cost.
The Greens corresponded to extensions of G-389-D, G-392-D G-315-D and G-318-D.
EXPERIMENTAL DETAILS:
Notebook #346, p. 114.
CS-7826
- SW-6810 - 21# G-389-D, P.C. Lot 419 73 ground with Barytes slurry thru pulverizer. SW-6855 - 21# G-390-D Preening Yellow - shaded and extended. Lot 4026 vs. G-369-D .30) s. dark i dirty; s. yel. 1. dirty; Barytes .70) s. strong; s. yellow
CS-7827 - 3W-6811 - 10#G-3S9-D, P.C. Lot 41973 ground with Barytes slurry thru nulverizer. 5W-6836 - 14#G-390-D Greening Yellow - shaded and extended. Lot 4028 vs. G-3S2-D .30) vs light; s. yellow P dirty; vs str; Barytes .70) vs yeiTow 1 dirty; s... dull 'L rusty"5
CS-7823 - SW-6812 - 15# G-318-D Yellow, Lot 419S7 - Shaded end extended. 45# G-315-D P.C. Lot 42159 - Ground with Barytes
W: slurry thru pulverizer. Lot 4027 vs. C-315-B .30) vs dark; s. str; s. str; vs clean Barytes .70)
CS-7829 -- SW-6813 11?G-31-D Yellow Lot 413P7 Shaded sue extended.
& - "
SVv-6843 22# G-315-D P.C. Lot 42159 - Ground with Barytes slurry thru pulverizer.
Lot 4029 vs. G-31S-3 .30)'s. blue L ch Iky; s. blue; C.L; blue.
Barytes .70)
'Si'i
LS*'Ai.
' -ft*.*.
DUP050315694
SUBMITTED APPROVED BY: ^
INTRODUCTION:
PIGMENT COLOR RESEARCH REPORT
3'~/fb
MEDIUM YELLOW'. Y-559-D
2//. / FILE: CiNOMJD YELLOWS DATE: ifiiibL,- 1935
M v '' .** '< * .'-
ksS&rvSi' .sSf'-V'
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Process study was continued in the factory durinr this month. Production was partly made on a slightly modified formula to obtain some darker, redder and weaker material needed for shad ing. Produetion was satisfactory in lithographic resistance and in tinctorial properties and light fastness - fairly close to standard. Most of the batches were made with lead nitrate rrcAiced from pig lead, unpurified.
SUMMARY & CONCLUSIONS :
Fifteen batches were made during this month, eight on the improved standard formula and seven with a slight modification, the addition of hydrochloric acid to the sodium chromate, resulting in a slightly darker, redder and weaker color needed for shading of lighter, greener and stronger material produced last month; shading to standard material was successfully accomplished. One batch was made with ad dition of salt - no effect was noticed. Two batches struck at a ^.ower temperature were of dirty shade and poor light fastness, a press washing study was begun on this color; two of the batches were partly press washed. This material was in both cases slightly dirtier in shade than the control.
It seems that this color needs a certain time for develop ment which occurs during the washing cycles when vat washed. In this case press washing could probably satisfactorily accomplish i$- *he color is struck at a higher temperature or heated before oressing as the development reaction would probably speed up at higher temperature.
EXPERIMENTAL DETAILS:
Notebook 448, page 72-73
Tabulation attached.
S.V'
DUP050315695
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DUP050315696
SUBMITTED BY : fit. ^ APPR07ED BY:
PIGMENT COLOR RF.3B.A8nu REPORT
PHIK30S5 YELLC.V
.a//- / FILE: C&fl&LE YSiih&xi DATS: APRIL - 1935
INTRODUCTION:
Semi-works study was continued on this color. Differences ir. shade which were encountered on previous studies in replacing lead nitrate crystals by lead nitrate liquor were minimized. A plant trial 3& :: was made on a slightly modified formula.
5U1.ILARY & CONCLUSIONS:
<v- Eleven semi-works batches were made based on a formula represented by 3W-6821. This batch, which is superior in light fast ness, shade, and strength, to Y-305-D, was set up as a temporary standard, CS-7888. An effort was made to prevent the sensitiveness to drying by forming a larger amount of lead sulfate and lead, carbon
k'-' ate in the final product. This was without advantage, the material D, ' was inferior in shade, strength and light fastness. 3V*-6821 was made 5t with lead nitrate crystals; check batches made with lead nitrate
liquor resulted in slightly dirty material. This is apparently due i; to the lead nitrate liquor which is not a straight solution of lead 1 nitrate but a mixture of lead nitrate and lead nitrite. Development
of KOg during the precipitation process was noticed on batches made -vgith lead nitrate liquor, and the pigment settled to a larger volume
during washing. Material equal to"3V.'6821 was obtained with treated lead nitrate liquor, i.e., converting lead nitrite to lead chloride by adding hydrochloric acid and driving off MCg. The lead was brought back to its original acidity with soda ash.
A plant batch was made on this improved formula as a 5 mol strike. Press cake samples dried in the laboratory were of slightly cleaner shade than the corresponding samples of the semiworks control and cleaner and much better' in light fastness than Y-305-D standard. The plant dried material was adversely affected by abnormal drying conditions as rise ir. temperature and a leaking steam pipe.
5XPSRIMENTAL DETAILS:
See Notebook 448, p. 53-55
Tabulation of batches attached.
' -
DUP05031 5697
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DUP050315698
PIGMENT COLOR RESEARCH REPORT
OIL RETENTION AND LITHOGRAPHIC BREAKDOWN OP PIGMENTS
SUBMITTED BY: V? APPROVED BY:
'
<2//- i
FILS: tSHttWE YELLOWS DATE: APRIL - 1935
INTRODUCTION
Work has been started on a Service to Research request #246 for a Y-180-D of improved lithographic resistance* The work on the oil retention of pigments has been continued.
SUMMARY & CONCLUSION
The problem of preparing Y-180-D satisfactory in lithographic breakdown resistance presents numerous difficulties. The present process for preparing Y-180-D was developed in the plant from the Y-309-D process and in the laboratory gives material lighter and weak er than standard Y-180-D. It is believed that much of the difference between the laboratory and plant is caused by the more severe process ing and drying conditions encountered in the plant. Modifications of the process to give standard Y-180-D in the laboratory would pro bably result in dark masstone material when the process was transfer red to the plant. On the other hand a modified process resulting in material equal to laboratory Y-180-D in shade and' satisfactory in lithographic breakdown may not equal Y-180-D in shade on being trans ferred to the plant. To obtain the desired improvement in lithographic breakdown in Y-180-D it will probably be necessary to develop a new 1 process in the laboratory and carry it thru the regular development cycle.
Previous work had indicated that the presence of soluble lead or of alumina hydrate improves the lithographic breakdown. These modifications superimposed on the standard Y-180-D process .resulted, as had previously been observed, in light masstone material. It was found however, that if the basic lead carbonate present be removed with acid and the pH after the hydrate be adjusted to 7.0 that a masstone equal in depth to the control is obtained. This material appear ed to be satisfactory in lithographic breakdown.
A few miscellaneous experiments on oil retention have not given results of practical value. The results have been somewhat irregular indicating adsorption at the pigment surface may be a very important factor. Flocculation may be desirable rather than undesirable in some cases since experiments with D.P.G. treated P.T.A. inks indicated that increased dispersion did not result in increased oil retention.
EXPERIMENTAL DETAILS; See Notebooks 453, 426
Exp. 453-48 - effect of hydrate and soluble lead in the Y-180-D process.
Results - Soluble lead and hydrate keep the color from becoming red on drying. The control is light vs. standard Y-180-D.
DUP050315699
2 IxpA_453-49 - Effect of hydrate and soluble lead in v-180-D at a pH of 7.0 . Results - At a high pH there is little or no tendency to prevent a change in shade on drying. The control is light vs. standard Y-180D. Exp. 426-56 - Oil retention of BT-125-D. Results - Treatment with Amyl Alcohol or D.P.G. does not improve the oil retention. Exp., 453-54. Preparation of Y-359-D containing 1, 3 and 5% of #0 Yarnish and 1, 3, 5% of rubber latex. Results - Either the varnish is not permanently attached to the particle surface or the possible increased affinity for varnish has a negligible effect on the oil retention.
DUP050315700
3UHC1TTED BY APPROVED BY:
PIGMENT COLOR RESEARCH REPORT
LEMON TELLO.i CP IMPROVED LIGET FASTNESS
AS/*/ FILE eTtROiMj-sOrLe-rrs DATE APRIL 1935
..."'.O*. >'
?y' *
|v ii ail. y-; ;tL-
;.e
V -f
INTRODUCTION:
This lemon yellow has characteristi calls'" poor light fast ness. A product recently made in tie laboratory showed an imurovement in light stability. An effort was rede to duplicate the materiel in the Semi-Works.
SUlu.-ARY & CONCLUSIONS:
One batch of a special yellow was made based on the labor atory experiment (453-213). This formula differs from tie original Y-202-D formula mainly in the replacement of lead acetate by lead nitrate an<^ disodium phosphate by sodium sulfate. The resulting 3eni-Works material (compared with 453-213) is slightly better in light fastness hut unsatisfactory in shade. The off shade of this hatch is probably due to change during drying process.
EXPERIMENTAL -DETAILS:
The hatch (3,.-o936 was filtered and went into dryer on the day of strike. The material was dried in the Proctor L Schwarz experimental dryer at a relative humidity of 20%.. The color remained in the dryer for 42 hours. The dried lumps were non-uniform (partly changed to a more reddish shade.
Readings: .
S',7-6936 vs. 453-213 - green, dirty; red str; about equal; si. better in light fastness.
" vs. Y-202-D Std. - green, light; red, str; about equal; red; much better in light fastness.
For further details see 'Notebook 446, page 14.
' `V
Hi-
v.
i
DUP050315701
SUBMITTED BY: APPROVED BY:
J4r-;<a O
PIQLBTT COLOR RESEARCH REPORT
EXCELSIOR YELLOW
/ FILE: CEROta TBELOWB DATE: APRIL - 1335
INTRODUCTION:
~ Excelsior Yellow made in a laboratory experiment showed a distinct improvement in light fastness over Y-309-D*. An effort was made to duplicate this material in the semi-works.
STJK&1ARY fc CONCLUSIONS:
Two semi-works batches were made based on an improved for mula for Y-309-D represented by the laboratory experiment 452-25A. The first hatch gave material of dirty shade and poor lithographic resistance due to a too low final pH of 4.6. The second batch was adjusted to a final pH of 5.6. The material is of cleaner, si. redder masstone, higher strength and better light fastness vs. Y-309-D standard, and of satisfactory lithographic resistance. The semiworks batch was made with lead nitrate crystals. A check batch will he made with lead nitrate liquor.
EXPERIKMLrAL DETAILS:
notebook 44fi, page 28, 29.
DUP050315702
PIGMMT COLOR RESEARCH REPORT IMPROVEMENTS II' CHROME YELLOWS
SU3IITTED BY: //(/^ >t h*. APPROVED BY:
A//./
FILL SKRCIiE YEILC'iVS
DATE ^RIL - 193 5
INTRODUCTION:
Several miscellaneous experiments were ran during the past month. A test of Supratol VA, RMS-1406, of the Hart Products
' Co. indicates it has no value when used in Y-359-D.
SUMMARY & CONCLUSION:
A further study of the new Excelsior process indicates that the difference between the alum treated and the zirconium treated products can be reduced somewhat by adding acid with the alum. Slightly lighter and darker shades than Y-309-D can be prepared by
varying the chromate-sulphate ratio. The light products tend to be came dirty in masstone.
* A test of Supratol VA indicates that it is without ef fect in Ifche Y-359-B process. The process supplied by the Hart Company gives a product inferior to Y-35S-D.
An experiment using zirconium oxychloride and other sub stances in a medium yellow gave no leads.
Magnesium hydrate added to Y-359-D and Y-309-D slurry " gave no noticeable improvement.
EXPERIMENTAL DETAILS:
notebook #452
Exp. 452-27 - Use of bichromate in place of chromate in new excelsior process.
Results - Chromate appears equal or better than bichromate in this process.
Ex p . 452-29.50 - Comparison of Titanium, Zirconium and Aluminium salts to equal the acidity obtained with zirconium and tir:- tanium salts.
Results - The titanium and zirconium salts gave slightly better results, zirconium being very slightly more effective in giving
a clean masstone than titanium.
Ex p . 452-51 - Effect of varying the chromate sulphate ratio.
Results - Use of large amounts of chromate result in a carker masstone.
Exp. 452-28 - Use of magnesium hydrate in Y-309-D and Y359-D. Results - Ho marked improvement was observed.
Ex p . 452-32 Effect of zirconium oxychloride, hydrochloric
acid and sodium molybdate in the preparation of a Medium Yellow. Results - No improvement was obtained.
Exp. 452-53 - Test of Supratol VA in a Medium Yellow. Results - Supratol VA produces no improvement.
DUP05031 5703
SUBMITTED BY: ^ APPROVED BY:
PIGMENT COLOR RESEARCH REPORT
STUDY OF LEAD CYANAMIDE
z-so. y FILE: e&ISOME YELLOWS DATE: APRIL - 1935
INTRODUCTION:
The receipt of a sample of lead cyanamide from the R. & E. Division prompted an investigation of this conroo*and and a study of the
t" use of sodium and calcium eyanamides in thepreparation of yellow nigmeats. Nothing of value has as yet been obtained.
SUMMARY & CONCLUSIONS:
A comparison of several samples of lead cyanamide, D-1979 D-1980, and D-1950 with Y-3Q5-D, and Y-232-D indicated that lead cyan amide might possibly be of interest. It is very weak versus Y-232-D and Y-505-D but is practically lightfast, being equal to Y-232-D In this respect. A laboratory strike consisting of the addition of sodium cy
anamide to lead nitrate gave a product inferior to the R. & H. sample.
A number of strikes attempting to prepare mixed crystals of lead chromate and lead cyanamide gave negative results. The use of lead sulphate and lead molybdate to give the light chrome yellows and
chrome reds respectively also failed to give indications of mixed crys tal formation with lead cyanamide.
Hiding power tests with TiCg and lead cyanamide indicate
it is less effective than TiOo in increasing the hiding power of Y232-D and Y-305-D.
The.use of a mixture of sodium cyanamide and sodium chromate
in the preparation of a zinc yellow gave no indication of the formation of mixed crystals.
EJLPERXMENTAL DETAILS:
Notebooks ,'-453 and 177.
Exp. 4S, 47 - Preparation of lead cyanamide. Results - The simple mixture of sodium cyanamide or calcium cyanamide
with lead nitrate gives a yellow inferior to the R. & E. products.
Exp. 43, 44 - Precipitation of mixtures of lead chromate and lead cyanamide.
Results - No evidence of mixed crystal formation was observed.
Exp. 45 - Coprecipitation of lead chromate, lead sulphate, and lead cyanamiaeT
Results - No evidence of mixed crystal formation was observed.
Exp, 46, 47 - Coprecipitation of lead chromate, lead molyb date and lead cyanamide. Results - No evidence of mixed crystal formation was observed.
Exp. 50 - Cryptometer readings on mixes of zinc yellow, and Y-305-D with D-1950 and TiOg. m- Results - Lead Cyanamide apparently has a lower hiding power than TIOg.
ate.
DUP050315704
PIGMENT COLOR RESEARCH REPORT PREPARATION OF BIBT INHIBITIVE PIGMENTS
J>jT
C/4>
SUBMITTED BY: . C. APPROVED BY:
/?
f il e : onnesn o r a n g e s DATE: APRIL - 1955
INTRODUCTION:
The work at the Experimental Station and at Newark on the preparation of Rust Inhibitive Pigments is being continued.
SUMMARY & CONCLUSION:
The results of tests at the Experimental Station on the pigments of possible acid accepting properties indicates that SPbO.PbClp possesses the desired characteristics. The next phase of the problem, A that of preparing talc of improved impermeability, has been undertaken. Samples of talc have been prepared which have been treated with zinc hydroxide, lead hydroxide, basic lead chloride, basic zinc chromate, and basic lead chromate. These samples will be tested for a possible improvement in impermeability.
Samples of Zinc Yellow treated with zinc hydroxide and of Chrome Orange treated with basic lead chloride and lead" hydroxide have been prepared for the Experimental Station.
Mechanical mixtures of the best of the talc treated nroduets with basic lead chloride andwith Chrome Orange or Zinc Yellow are to be made.
EXPERIMENTAL DETAILS:
See Notebooks #421 and 177.
- Exp. 27, 8. 50, 51. 52, 55 (Notebook 421) - Preparation of samples for tbe Experimental Station.
Exp. 57, 58 (Notebook 177) - Preparation of Zinc Yellow samples for the "Experimental Station.
DUP050315705
SUBMITTED BY: APPROVED BY: ^
PIGrNEKT COLOR RESEARCH REPORT
YC-27-D
a//* a FILS: -eest:&-ffsrGE3 DATS: APRIL 1S35
INTRODUCTION:
Recent studies in the plant on this color led to a slightly modified formula by which standard material can be obtained. Further work was done during this month to simplify the formula.
SUMMARY & CONCLUSIONS:
Standard material was obtained on a formulation with a total amount of 0.64 mols chromate per mol lead and 1.228 mols of acid (represented by lot 42812). This batch was made by reversed strike and Bichromate added in three steps. 92.5$ of Bichromate in the strike, 2.5$ after strike and 5$ to shade after heating to a boil; after this a final adjustment was made with sodium chromate to a faint excess of chromate and to a final pH of 7,3
17 batches were made for production, partly as checks on 42812 and some with modification in the addition of bichromate to simplify the working procedure.
Satisfactory material was obtained by striking into 98.5$ of -the required amount of bichromate and adjusting the endpoint at a boil to a faint excess chromate and uK of 7.1 - 7.3 with the necessary amount of bichromate or chromate. The right adjustment of the endpoint is of great importance, as a larger excess in chromate results in strong material which according to the pH will be of either red briekish or yellow'muddy shade. The right endnoint, faint excess chromate, can be easily determined by comparison with a standard filtrate sample.
EZPEfflKBNTAL DETAILS:
Notebook 448, page 152-154
Tabulation of Plant batches attached:
~*
DUP050315706
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DUP050315707
t
SUBMITTED BY APPROVED BY:
FICH/JBKT COLC-H RESEARCH REPORT YO-38-D
3iT-/lS~
A FILE: egaois CRASteS DATS: APRIL - 1935
INTRODUCTION:
Previous and recent production of this color caused con siderable trouble in the plant, material made on standard formula usually resulting in bricky, weak material. Laterial made cn a slightly modified formula was usually light and flat in masstone. Work was resumed on this color during this month in the Semi-Works.
SPI.1IARY & CONCLUSIONS: ;
Seven batches of Y0-38-D were made based on standard for mula; variables were studied, such as doubling volume, addition of sodium chromate, .and increase in sodium bicarbonate. Doubling volume together with the addition of a small amount of sodium chrcmate showed a slight improvement in brightness versus control; the material is however, very light and strong. An effort was mads to darken the masstone by an increase in sodium bicarbonate, which resulted in a darker material somewhat closer in masstone to standard but of less brightness and high strength.
EXPERIMENTAL DETAILS:
See Notebook 339, page 154.
Tabulation attached.
DUP050315708
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DUP050315709
~-/<Z rc JT7
PIGfc
COLOR RESEARCH REPORT
PURIFICATION OF LEAD HIT RATE LIQUOR
SU3LITTED BY APPROVED BY:
MA /-/
FILE: fahAB-fr-TSXD LATERIAL3
DATE: APRIL - 1935
INTRODUCTION:
Purificationsof lead nitrate liquor have been successfully accomplished in the Seni-.-Vorks by deposition of metallic impurities on sheet'lead. New equipment was installed in the plant for large scale
purification of lead nitrate liquor needed for the new medium. Yellow, Y-35S-D and light Fast Greens.
SUNKARY & CONCLUSIONS;
, Four purifications havebeen made during this month in the plant equipment to test its efficiency. Variations in temperature and acidity were studied to find out the test working conditions.None of these purifications were carried to the satisfactory endpoint (negative test for copper with Ammonia) in spite of an increase in lead sheet surfate hy 37-82^ over the one in the semi-works study and extending the time of process from 2-1/2 (for Semi-Works Study ) to 3-1/2 - 4-1/2 hours. Gradual decrease in copper was noticed on sam ples taken at 1/2 hour intervals. The slowness of the purification process is probably due to insufficient agitation.
The agitation in the plant equipment, obtained with a "Lightnin" mixer, is inferior to that by which the semi-works studies were carried out. The metallic deposits on the lead sheets were nonuniform, the heaviest deposits occurred in sections of more efficient agitation, i.e. close to the agitator. The agitation seems to be more important for the speed of the process than an increase in lead sheet surface.
.Vi.''
Increase in temperature - It is not certain whether an in crease in temperature over "140o ? (this being the optimum temperature for SemipA'orks study) is of advantage as the gain in reaction speed is counteracted hy loss in .acidity at higher temperature. A certain amount of free acid seems to be necessary for reaction, therefore, an addition al amount of nitric acid had to be added during the purification pro cess to make up for the loss of NOa. ' at higher temperature.
The addition of acid during the process - is harmful as metal deposits will dissolve especially in the case c? poor agitation.
Addition of nitric acid at the start of -purification - is probably necessary as pH adjustment, if the rh of the leaa nitrate liquor is over pH 4.8
Removing of deposits from lead sheets. This could be read ily done with the hose on sections with heavier deposits whereas the removal of llhin deposits was troublesome and had to be done bv brushing
off.
very"poor, as-.'
DUP05031 571 0
2
agitator was working against the broadside of the lead sheets.
No. 2 Purification - The agitation was somewhat improved by mounting the agitator in a way that' the agitating stream runs parallel with the lead sheets. A slight development of NOg was
noticed during process combined with loss in acidity. Nitric acid was added to balance the acidity.
No. 3 Purification - Agitation as in Mo. 2. The lead nitrate used was heavily charged with impurities and a considerable
amount of sludge entered into the purification vat. The pH could not be sufficiently lowered by the*addition of the nitric acid due to the presence of basic salts.
No. 4 - Agitation as in No. 2 and 3. Nitric acid was adied at start of purification to lower pH to 4.6. Slight NOg dev elopment during process.
The Purification equipment consists of.a 3000 gallon vat in which, 9 lead sheets are'immersed totalling a lead sheet surface of 663 square feet if filled with 2800 gallons. Agitation will be improved by removing some of the lead sheets. Further purification will be made after this modification.
EXPERIMENTAL DETAILS :
Notebook 448.
Lead Nitrate Liquor Purification
1
2
3
4
Amt. of Lead Nitrate liq. in gals. 2750
2800
2600
% Pb(N03)2
19.3
22.05
25.
Specific GravityO
1.194
1.224
1.26
Lbs. of Ph(N03)2 100%
5260
6300
6S30
Sq. feet of lead sheet surface immer . 656.4
663
636
Sq. ft. of lead sheet sufface -oer
100# of Pb(N03)2 100%
12.4-
10.6
9.3
2700 21.55 1.22
5800 650
11.3
Reaction for Copper tested with KH OH before process
Reaction for Copper when process was stopped
sli. vv si.
fairly strong
sli.
very strong fairly strong
slight
pH before purification pH at end of purification
4.8 5.0 5.0 5.0 (4.8)* 4.9 5.0 5o 5.0
Amt of Nitric Acid (60%) added at start of purification
Amt of Nitric Acid 60% added during purification
None None
None 75 lbs.
None 105#
30# * None
Temp* of Lead Nitrate Lie. during purification
Time of Purification in hours
140 F
175 F 4
160 ? 4-1/2
170 F 3-1/2
i--i i
to
*pH was lowered to 4.8 by addition of 30# Nitric Acid
! : A lAt
DUP050315711
PIGMBHT OOLOB RESEARCH REPORT
IROIf BLUE YIELDS IABORATORY STUDY
3*'/A 7
SUBMITTED BY* APPROVED BY*
PILE: fflOH-BLUE DATE: APRIL-1935
IHTRQPUCTIOff
The laboratory work reported below is a continuation of that carried out in December 1934 and covered in the regular research re port for that month. %k' 5V- The Engineering Department is carrying out a critical study of blue yields, under practical operating conditions and requested defi nite information on the goal yields of the more important blues. The recent work is largely a repetition of that carried out before, but was believed necessary because of the doubt existing as to moisture content in the various earlier samples.
Son attention has been given to blue yields in the semi-works (see reports' for January and Eebruary 1935) but in these cases there was also some question as to the water content of the products.
SUMMARY Off RESULTS
1} Determination of "Moisture"
The difficulties in estimating "moisture" were referred to in
the December report. While it is probable that a satisfactory method involving loss on heating could be developed with sufficient study, the results ordinarily obtained are quite unreliable. The Engineer
ing Department therefore took up a study of the analytical method as an early step in their general program. It was found that the A.S.T.M. (Dean & Stark) toluene distillation method gave results which, are ap parently entirely satisfactory with respect to duplicability on a given sample. (See letter IRS, KRJ - F.H.McB 4/1/35). The method gives no information as to' the type of water. In other words, it may be chemically combined, adsorbed etc. Moreover, the figure obtained for a given blue may be different if a liquid other than toluene is used. Some additional investigation of the method was carried out in our laboratory particularly in comparing day to day results with those ob tained by loss on heating. These results also showed the distillation
method to be much the better.
A number of laboratory batches were made of B-63-D and B-66-D. In the former case, some formulation changes were studied to determine their effect- on yield and color. These will be considered in turn. *% H20" refers to the figure obtained by distillation and "anhydrous" to figures also calculated from the latter.
2) Milori 31ue B-66-D
Thft six samples made in December (376-45, 46) were re-analyzed
artrt the observed yields calculated to an anhydrous basis giving an aver age of 305 g./mol Y.P.S. Standard B-66-D (Lot 13957) was found to con tain 3f3% H2O; recalculating to this basis gives 315 g/mol.
DUP050315712
tfe: $
ji
v
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i*.'.
2&
As pointed out in the December report (page 2), these figures were known to he a little low due to slight losses in filtration. In the recent series a special effort was made to correct this by refil tering, and an actual determination of blue in the final filtrate
showed only 0.75 g./mol on an anhydrous basis. This has been neglect ed. The anhydrous yields ran from 313 to 317 g/mol with 315 as an average. it 3.3^ moisture this is equivalent to 325 g.
Two strikes digested at a higher temperature (red masstone) gave an anhydrous yield of 312/mol. It is doubtful whether this difference is significant; in other words, a difference in temperature on B-66-D affects the color more than it does the yield.
3} Chinese Blue B-63-D
The laboratory yields previously reported (August 1934) gave an
average of 320 g/mol on an anhydrous basis or 330 at
H20. The lat
ter analysis is of course open to question, but in the light of the
recent work would appear to be correct since the same average figure
was obtained. On an anhydrous basis, the lowest was 317 and the high
est 322 favg. = 320).
Increasing the copperas excess by 20) raises the yield very near
ly 10 grams/mol. While weak in tint, the batches so made were OK in lacquer.
Digestion at a high temperature (200 vs. 180) was tried both on the regular formula and the one using high copperas. In both cases (the yield dropped 10 grams/mol. Since this was not observed with B-66-D (see above), it was probably due to prussiate decomposition be fore the addition of the second portion of copperas. As might be ex
pected, the high temperature gave redder masstones in both cases; the
lacquers also tended to be red, particularly with the high copperas.
While the various batches made by standard formula gave good re sults in laequer (generally on the deep black side), rubouts were rather unsatisfactory, showing a tendency to be red and slightly weak (+ 3%) in tint. This is attributed to drying conditions and moisture
content of the products, and is discussed briefly below.
4) "Effect of Drying on Color
It is well known that drying has a considerable influence on the quality of iron blues, the various types requiring fairly definite specific conditions. In this general connection, it was observed that the residue from distilling with toluene (moisture determination), and therefore corresponding with severe drying, was red and weak in tint against the original sample.
As in the previous work, all samples were dried at 140 far 72 hours. It is believed that for the comparatively thin cakes obtained on a small seale this was excessive and the chief cause of the infer iority in color of the laboratory strikes in comparison with standard.
"<*v
DUP050315713
In the case of B-66-D, the moisture contents were approximately 2# in comparison with the Z% figure mentioned above.
Standard B-63-D (Lot 3272) from the storage drum was analyzed and found to contain 3.2^ of moisture. Drying at 140 for three days reduced the figure to 1.6^. Both were quite close in lacquer to the lacquer standard (SD-46794), being v.v.s. red and v.v.s. black respect ively. However, by rubout they were distinctly different. Against the original blue, the redried was v.s. dark, slightly weak (+ Z%) and v.s. red, -- in other words, similar to the laboratory blues for which the moisture averaged a little less than 2$. The higher figure ob tained last summer (i.e. Z%) may have been due to the different analy tical method or to higher humidity in drying.
A more comprehensive study is in progress on the relation of moisture content to the properties of B-63-D in lacquer and by rubout. The general procedure is merely to dry plant press cake in the labora tory oven {140;F), taking samples after appropriate intervals, analyz ing for moisture and making color comparisons. The preliminary results are in agreement with the above conclusions. Details will be reported at a later date.
*
BXESIRIMEiKTAI. DETAILS Recorded in notebook 376 as follows* B-63-T) Studies, Expts. 53, 57, 59, 73, 74 See especially pages 176 & 182. B-66-D studies, Expts. 60, 61, 75 See especially pages 180 & 184. Moisture determinations, Expts.. 64, 65, 67, 68, 69, 78 Drying study, Eftpt. 80. (To be reported in detail at a later date) The yield results are shown in the two following tables.
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DUP050315715
PIGMENT COLOR RES BARCE REPORT
STUDY OP IRON BLUE PIGMENTS
SUBMITTED BY: J.C.^ APPROVED BY:
<2/3
FILE: i&GR BLUES' DATE: APRIL - 1935
INTRODUCTION;
It is proposed to make a broad study of iron, blue pigments in order to obtain a better foundation for further work on these produe ts.
SUMMARY & CONCLUSION:
The results to date chiefly confirm previous work -on iron blues. It has been found that preparation of the iron blue under nearly neutral conditions results in the formation of green undertone blues. These products are mentioned in the literature and probably consist of mixtures of iron blue and iron hydroxide. They are brown in masstone and dirty in undertone and are probably of no interest.
A sample of Williamson's Violet was prepared by heating potassium ferrocyanide with sulphuric acid and oxidizing the precip itate with hydrogen peroxide. The product was red in masstone and red, dirty and weak in tint versus B-5-D. It apparently contained larger particles than B-5-D. The color was soft in texture and had a brilliant dry appearance.
One series run by a process somewhat similar to 3-66-D without the use of ammonium salts and using various oxidizing agents gave approximately the same results with sodium bichromate, hydrogen peroxide, and ferric chloride. A hot strike using sodium chlorate gave a stronger product. Striking at an elevated temperature gives a light masstone but the strength may be increased or decreased depending on other conditions. Striking the Y.P.S. into the copperas seems to give a greener tint than the reverse procedure. Ammonium salts are most effective when a small amount of copperas Is used. It is possible that there is less differencetinctorially between the ammonium salts and the .iron salts than between the soda salts and the ammonium salts. It was not found possible to prepare the red shade blues or toning blues in the absence of ammonium salts.
EXPERIMENTAL DETAILS:
See Notebook 376
Exp. 49, 50 - Effect of acidity and temperature of strike. Results - Oxidation under neutral conditions results in a dirty, green undertone. This is accentuated at an elevated temperature.
Exp. 51 - Preparation of Williamson's Violet. Results - Williamson's Violet appears to be a light masstone, weak, red tint blue.
Exp. 52 - Effect of various oxidizing agents. Results - The oxidizing'agent has no effect on the blue.
Exp. 54 - Effect of direction of strike and temperature of
DUP05031 5716
-2
Results - Temperature influences the masstone. Striking the Y.P.3. into the copperas increases the greenness of tint.
Exp. 55, 58 - Effect of ammonium salts and their point of addition. Results - No improvement was observed thru the use of ammonium salts where a large excess of copperas was used, but where a slight excess of copperas was used the ammonia blue was superior.
7, , Exp. 62 - Further study of strike temperature. Effect of washing the white precipitate. Results - Washing the white precipitate gives a dirty undertone. Strik ing at an elevated temperature gave a light masstone.
Exp. 65 - Effect of dilute strike and of ammonium salts. Results - There seems to he little difference between the ammonium blues and the iron blues. Dilution had little effect.
Exp. 66 - Effect of replacing ammonium salts in B-152-D with copperas, stannous chloride and lead nitrate.
Results - Only the ammonium salts gave a toning blue.
Exp. 70 - Preparation of iron blues without going thru the white precipitate stage. Result - The blues were very hard and weak.
Exp. 7E - Yield study of B-152-D. m' Results - The ammonium bicarbonate added decreases the yield.
Be.-.
.
DUP050315717
PIGMENT COLOR RESEARCH REPORT TREATMENTS TO IMPROVE FLOW OE PIGMENTS
jr?
.SUBMITTED BY: APPROVED BY:
PILE: PKtefflff--TREETl MEETS
DATE: APRIL - 1935
INTRODUCTION:
Work on the improvement of the flow of inks by the addition of Barium Hydrate and other basic inorganic materials was continued dur ing the month. The work has been confined largely to tests on Duol Red, RT-283-D and Red Lake C, RT-313-D, with one experiment on BT-122-D and one on Y-309-D.
SUMMARY & COHCLUSIONS:
The addition of 4# and 1% Barium Hydrate to BT-122-D did not affect the ink sufficiently to make it flow but did eliminate to
some extent, the short buttery character. The addition of 4# developed considerable bronze on the color but 1% had no apparent effect on this property.
The addition of 1$ Barium Hydrate to Y-309-D caused an in crease in flow of 26 to 35. It is not felt that this is sufficient
improvement, especially in view of the possible tinctorial effect on the color due to alkalinity, to warrant further consideration at the present time.
On the basis of accelerated livering tests on RT-283-D
containing 1, 2, 3 and 4& Barium Hydrate, it is felt that about
is
the maximum amount that can be safely used on account of bodying with
the greater amounts.
It was found in experimenting with RT-313-D that TriSodium Phosphate inereasedflow considerably#but inhibited drying. Stoichemetrie mixtures of Barium Hydrate and Trisodium Phosphate were tried in RT-283-D but the flow produced was approximately in propor tion to the amount of Barium Hydrate present.
Laboratory prepared Sodium Resinate in RT-283-D tended to decrease flow rather than increase it. Equal part mixtures of Sodium Resinate and Barium Hydrate gave slightly less flow than would be ex pected from the Hydrate present.
Magnesium Oxide, 2$, in RT-283-D increased flow slightly
more than
Barium Hydrate; 4# caused less flow than 2y.. Both
amounts caused very bad livering in 24 hours on an accelerated test.
On the basis of molecular equivalents, LgO would give less flow than
Barium Hydrate.
. Mixtures of Barium Hydrate and D.P.O. {Diphneyl Guanidine) even as high as 1% Barium to 4# D.P.G., were not effective in RT-293-D.
The effect on ifche flow of Bed Lake C, RT-313-D with small amounts of Barium Hydrate is very much greater than is the case with Duol Red, HT-283-D. As little as 0.5$- Barium Hydrate gives an appre
ciable increase in flow over the control and 1$ causes a considerable
DUP05031 5718
2
increase, and 2% a corresponding increase.
As much as 1.5$ Barium Nsphthenate precipitated on RT-313-D was not effective in increasing flow.
Barium Linoleate, equivalent to l$Barium Hydrate, caused only a very slight increase in flow.
Tri Sodium Phosphate, 1$, gave considerable increase in flow, but inhibited drying.
Semi-works grinds of RT-313-D were made containing 0.5$ and 1$ Barium Hydrate for trial by the LeCall Company. This was done in response to the customer's request for a Red Lake C having good flow. The flow of the plant grinds checked the results obtained in the laboratory, and trial shipments were made as RT-405-D (0.5$ Barium Hydrate) and RT-406-D (1$).
The Experimental Station found that Glucamine and methyl
Glucamine were quite effective in increasing the flow of Lithols and
Duols, the former much more so than the latter, but both compounds in
A-t
W
hibited drying. Both will be tried in conjunction with Barium Hydrate
If. in RT-283-D.
A EXP ERIMSiOTAL' DETAILS:
} r:>Vs
Experimental details are covered in Notebook 458-4-7-8-9-13 a- and the following ink grinds.
Ink 3011 3015 3015
5017
3020 3020 3022 3021 3022 3022
3023
3030
BT-122-?D Barium Hydrate
Y-309-D
RT-313-D Barium Kaphthenate-
Tri Sodium Phosphate
Barium Linoleate n Barium Hydrate (McCall formula) ti " " (Reg. vs. Trans. 7ar. formula)
T Barium Evdrate Livering Tests
RT-283-D
4$ " 1,2,3$
ft tt
Tt
tr
n Ba Hydrate k Tri Sodium Phosphate kgO
tr " Sodium Resinate t " Sodium Resinate k Barium Hydrate
tt " Barium Hydrate & D.P.G.
DUP05031 571 9
PIGIvlECT COLOR RESEARCH a SPORT DRY DISPERSED CCLCR3
35^/30
- ***
SUBMITTED APPROVED BY:
FILE: PgaECT" DATE: APRIL - 1935
INTRODUCTION:
An investigation of a nev; process for preparing dry dis persed colors of improved softness has been started. The process in
volves a treatment of the pulp color vdth an emulsion of fe. volatile petroleum distillate followed by drying. Cementation of the particles during the drying process is avoided. The preliminary work indicates some improvement in softness may be obtained.
SUMMARY & CONCLUSION:
A number of toner pulps were treated with emulsions of
varnolene and kerosene prepared with triethanolamine oleate. About 20$ of oil on the solid content of the pulp was used. In all cases, which included RT-332-D, GT-68-P, 3T-37-P, and 3-63-D, the emulsion treated products were softer and showed less grit on brushout.
Treatment of a slurry of GT-68-P with an emulsion followed by filtra tion gave slightly better results than treatment of the pulp color without dilution with water. In the case of the alizarine toner, RT-332-D it was necessary to use a wetting agent to wet the treated scolor before brushing out.
While the preliminary work showed little difference be tween varnolene and kerosene further work to determine the optimum boiling range of the volatile oil is Planned. A study of the quan tity of oil necessary is also to be made.
EXPERIMENTAL DETAILS:
Notebook #466
emulsion cases.
Exp. 1 - Treatment of various toner pulps with a Varnolene Results - An improvement in texture was obtained In all
Ex p . 2 - Treatment of GT-6S-F 'with a varnolene and a ker osene emulsion and also slurry treating with a kerosene emulsion and also slurry treating with a kerosene emulsion.
Results - Treatment of the slurry seems to give slightly better results than treatment of the ruin. The kerosene evaporates less rapidly than the varnolene but no definite difference in texture
of the two products was noted.
si
.. v
DUP050315720
- *1*,^
6'
PIGMENT COLOR RESEARCH REPORT
IMPROVEMENTS IN P.T.A. PIGMENTS
SUBMITTED BY: V' /> APPROVED BY:
3. eX-/
FILE: P~.T.A. PIGCfflTTS DATE: APRIL - 1935
INTRODUCTION:
The laboratory work on a molybdenum toner of Victoria Pure Blue BO containing a small amount of vanadium was concluded during the oast month. One batch was prepared in the semi-works without difficulty.
SUMMARY & CONCLUSION:
Comparison of reverse strike versus direct strike on the molybdenum toner of Victoria Pure Blue BO containing a small amount of vanadium indicated that the reverse strike or dye into the phosphomolybdic acid gives slightly better results tinctorially and in
light fastness.
Several miscellaneous strikes on the effect of formic acid in place of sulphuric acid in the BT-96-D and BT-99-D processes gave products weak versus the respective standards.
A study of the use of hydrate in P.T.A. toners indicated that slurry mixing or precipitation of the hydrate on the F.T.A. pig ment produces a decrease in strength greater than that corresponding
to the Increased yield.
EXPERIMENTAL DETAILS:
See Notebook f4S6
cesses .
Ex p . 53 - Use of formic acid In the 5T-96-D and 3T-99-D pro Results - Week products were obtained.
Exp. 54 - Effect of hydrate in the pigment and effect of use
of mixtures of sulphuric and formic acid. Results - Hydrate weakens the pigment. A mixture of sul
phuric anc formic acid"is equal to formic acid alone.
Exp. 55 - Check on experiment 54. Results - Check those of Exp. 54.
Exp. 57 - Comparison of reverse vs. direct strike on the molybdenum toner of Victoria Pare Blue 30.
Results - The reverse strike seems better tinctorially and
in light fastness.
iblsr*'
v
*>.
DUP050315721
PIGMENT COLOR RESEARCH REPORT
3JT~
7^
BT 125-D AND BT-150-D
SUBMITTED BY: LX U^o APPROVED BY: ^SCiCa^c/^^
*<***/' PILE: PSA--90LQR5 DATE: APRIL-1935
INTRODUCTION
Work was started the latter part of last month, and continued through the month of April on the manufacture of 3T-12D-D for BT-150D, CS-7609 formulation, to determine the possibility of securing satis
factory yields on this color when on a production basis in the SemiWorks. The plant has consistently secured poor yields on this color.
Work has also been started in the Semi Works on a new BT-125-D tyoe toner which is stronger than BT-125-D with a lightfastness equal to'b t -io o -d .
SUMMARY & CONCLUSIONS
Of the five batches of BT-125-D for BT-150-D made, all but one were satisfactory in tinctorial properties, being v.s. strong and bronzy versus CS-7609. The poor batch was slightly weak versus CS7609 but about 15$ high in yield. Yields were satisfactory, averaging 102$ of estimate, thus showing that satisfactory yields can be se
cured oh this formula. A board mix has been made using these batches together with three sub-standard plant batches to make 444 lbs. of satisfactory BT-150-D. This mix will be made in the Semi Works and will be reported next month. Por ctabulation of results see Table I.
Three batches of special BT-125-D were made during the month but final results on only one of these are available. This material, a Vanadium-Molybdenum toner of Victoria Pure Blue BO is stronger than BT-125-D with a lightfastness equal to or better than 3T-100-D. The standard laboratory formulation uses the reverse strike, i.e. dye solution into the precipitant, as the method of precipitation, but study in the Semi Works has shown that the material made using a dir ect strike shows little if any variation in properties. As the latter method of striking is more convenient to use with present plant and Semi Works equipment, this procedure will be followed in all subse
quent work. Rubout and ink grind results on the first batch made on
the standard laboratory formula show satisfactory results. Results on the remaining two batches will be reported next month. Ink mill and rubout results on the one batch are tabulated in Table II.
DUP050315722
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DUP050315723
/
/33
PIGMBffT COLOR RESEARCH REPORT PTA YIELD STUDIES? PLA3HT
SUBMITTED BY APPROVED BYj
INTRODUCTION
PILES: PTA OOLOIl-S PATS: lOTIilf'1 n*K
PTA toner -production remains high during the month with average
yields being fair, but individual batch yields continue erratic. This yield study Is merely a survey of operating data, no attempt having been made to improve the yields obtained.
SUMMARY & CONCLUSIONS
Six batches of RT-329-D are reported this month including one held over from last month. On some few of these batches the plant has been re-estimating the yield downward without making an equivalent de crease in the size of the batch. Average yields are still poor being 92-1/2# based on plant estimated yield and 88# of corrected estimated yield. This is a drop of 8# under last month's production of this color. Tinctorial properties are satisfactory.
Six batches of BT-92-D are reported this month including three batches outstanding from last month. Average yields were only fair, being 95# of estimate, a drop of 11# under last month's average. Rubout results were satisfactory.
Pour batches of BT-100-D were made during the month. Yields
averaged 106# of estimate^ an improvement of 7# over last month's pro duction. These products were satisfactory tinctorially.
Three batches of GT-347-D were made during the month, with yields averaging 98-1/2# of estimate. This is a decrease of 6# under last month's production. Rubout results were satisfactory.
The two batches of RT-330-D made during the month gave satisfac
tory yields but were poor tinctorially. The yields averaged 112-1/2# of estimate, a drop of 5-1/2# under previous production. This yield is still abnormally high, however. 3oth of these batches were light, blue and weak versus the standard by rubout.
Semi-works yields on 3T-150-D were equal to estimate: this work is covered in a separate report.
Yield and rubout results are tabulated in Table I.
DUP050315724
TABLE I
N.B. 434, pages 47-51
caior
YIELD
Grind Rubout vs. Standard
Batch Est.
Lunin % of Est Mass. Draw.
Str. Tint
Remarks
RT-329-D
It
It
It
tt
It
42713
43069 43113 43144 43357 43399
99 90(98) 90199) 90(97) 95(98) 95(97)
96 88 91 80 89 72
RT-330-D 43313 W 43333
GT-347-D 43225 * 43273 It 43294
96
tt
n n m
104 112
82
tt
102
97 90 92 82-1/2 91 73-1/2
It. dk It dk dk dk
vs jrel. bl bl s.bl s.yel yel
we wk vs str
-- s.str
tt tt
yel bl bl bl yel M
108-1/2 It. 117 tt
blue
tt
weak tt
blue tt
85-1/2 vvs dk vs yel
tt vs dk
tt
106-1/2 vs It.
tt
s.str
It
s.yel
It
II
Total average yield of all PTA Toners for March * 98% of estimate.
Total average yield of all PTA TonerB for April =96.8/2.
l.Z% decrease for April under March.
BT-92-D
It
R M
n
n
42913 48931 42938 42971 43048 43204
n
R'
It
m n
86
89-1/2 s.dk s.str str
vs red
It
tt tt
tt
tt s .red
84
87-1/2 dk
vs red
tt
tt
98 102
dk vs red, str "
tt
94 98 s.dk vs red tt vs clean
100 104
It
s.wk
weak
s.green
BT-100-D It
m m
42987 43011 43359 43184
90
100 111
s.dk s.str str
ws red
96
106-1/2
tt
tt
tt
OK
85 94-1/2 vs dk. vs red vs str vs red
100 111
vs It. OK
OK vs green
DUPO 50315725
SUBMITTED BY: APPROVED BY*
PIG-MEM* COLOR RE SEARCH REPORT
/ sy
GRINDING OP PULPS
/'K-^
PILE: IffG, STUDIES DATE: APRIL 1935
a
INTRODUCTION
Two "barrels each of Y-77-P and Y-78-P were ground through the Straub mill. These were shipped as samples to the Lowe Paper Company, who had complained of lumpiness in a former sample,
SUMMARY & CONCLUSIONS ,
The Y-77-P went through the mill with comparative ease, emerg ing much smoother than the unground pulp. The pulp settled somewhat after milling, making it possible to draw off some water.
The Y-78-P gave considerably more trouble, being very sticky and unadaptable to the gravity feed of the Straub mill. A good product was, however., obtained after two days work on it.
EXPERIMENTAL DETAILS
See N.B. 291, pp. 75-76.
DUP050315726
PIGMENT COLOR RESEARCH REPORT
(Z
SUBMITTED BY: ATPRCVED BY:
/?? '4^'"'^ FILL: FIDE TCSSa
DATE: APRIL - 193 5
1KTRCDICTION:
Investigations on p-ehlor-o-nitro aniline were conducted during the month with the purpose of preparing a red toner similar tinctorially to RT-208-D and RT-396-D. During the latter part of the month, C3-7873 was set up and several charges were prepared in the Seri-works under the supervision of the laboratory.
SUI.l.ARY & CONCLUSIONS:
As a basis for the initial attack, formula CS-7837 was used in the preparation of the p-chlor-o-nitro aniline pigment. A complete investigation of both the diazotization and coupling~steps was taken, along vd.th several miscellaneous operation steps. A general classifi cation of the problems was summed up as follows
1. Diazotization (a) Hydrochloric Acid (b) Time of diazotization (c) Sodium Nitrite (d) Urea (e) Clarification (f) Volume of diazo
2. Coupling (a) Hydrochloric Acid (b) Temperature of Coupling (e) Time of Stirring
3. Miscellaneous (a) Substitution of Sulfuric for Hydrochloric Acid (b) Effects of screening - omission cf D-1846 {phenol (sulfonic acid formaldehyde)
Variations in the Hydrochloric acid content of the diazo from 1.0 mol excess to 4.0 mol excess gave lighter masstones, increased blueness but decreased strength. The greatest difference both in masstone, strength and tint was between 1.0 mol and 2.0 mol excess. Beyond the 2.0 mol excess very little change seemed to take place.
The general tendency cf increased time of diazotization was to give lighter and brighter masstones, with practically no changes in strength and tint.
Increasing the amount of nitrite from (theoretical) to (a 30$ excess) resulted in darker, browner masstones, with stronger yellower tints.
Absence of urea after the diazotization gave a darker, dirtier masstone with a stronger, yellower tint. The addition of sbdincrease in amount of urea produced lighter and cleaner masstones, but bluer and weaker tints. The maximum change took place around 7.5 g. -jper 0.1 mol charge.
39:: ,,
- .*
DUP050315727
s
Omission of the clarification step gave about a 7% increase in yield, but a darker, weaker and bluer product.
Up to 900 cc/0.1 mol diazo charge- dilution, very little change is noticed in the masstone. Above this point the masstone became decidedly darker and browner, with a stronger yellower tint.
By. increasing the amount of hydrochloric acid in the coup ling from 0.75 mols to 1.05 mols per 0.1 mol coupling, a darker masstone, weaker strength and bluer tint are produced. A decrease in the hydrochloric acid content below 0.75 mols*to within reasonable limits above zero excess, caused very little change.
Increasing temperature of coupling above 30 C, gave darker yellower and weaker products. Decreasing the temperature to 0 C gave lighter, brighter mas stones - Belcw 20, tine change is reversed because of the extreme retardation of the speed of coupling.
It was found that sulfuric could be substituted in the pro cess for HC1 with practically no color changes in the pigment. At the same time it was shown that temperature development to a boil gave no changes.
In thepreparation of the C3-7873 samples for the files, two 0.1 mol and two 0.4 mol couplings were made in order to check the dependability of the formula in the preparation of different size batches.
It was found that the two 0.4 mol samples checked each other exactly; in the 0.1 mol coupling (d) was vvs darker than (c). From this, it may be concluded that the formula as set up, is stable, but that the masstone is liable to darken somewhat as the size of the charge increases.
EXPERIMENTAL DETAILS: Notebook No. 219
219-51 - dealt with the effects of screening; omission of norit and filtercel; and, omission of D-1846 (Phenol Sulfonic Acid Formaldehyde).
Screening seemed to produce very little effect except to re duce the yield of pigment slightly. Omission of norit and filtercel tended to give a lighter, brighter masstone with a weaker, bluer tint. Absence of D-1846 gave a darker, cleaner and brighter masstone, with a bluer, weaker tint.
219-52 - consisted of variations in the hydrochloric acid content of the diazo, the total acidity of coupling remaining the s o,Tn@
Increase in the amount of hydrochloric acid gave a lighter masstone with a bluer, weaker tint. The greatest difference^in strength, masstone and tint was noticed between 100% and 20 0 excess acid.
219-53 - studied the time of diazotization.
5|g#ill
DUP050315728
C?
-3
Increased time of diazotization lightened and brightened the masstone, the strength and tint remaining practically constant.
219-54 - dealt with the effects of sodium nitrite excess.
Increase in nitrite excess gave a darker masstone with a stronger, yellower tint. Drying at 180 F instead of 140 F had prac tically no effects on the color.
216-55 - was a study of the effects of urea.
Absence of urea gave a dark, dirty masstone with a strong yellow tint. Addition of and increase of urea gave a lighter mass -- tone, with bluer, weaker tints.
219-60 - dealt with the effects of clarification removal.
Omission of clarification gives approximately 0.5# increase in yield, but gives a darker, bluer and weaker product.
219-62 - studied the volume of the diazo.
Within reasonable limits, there are practically no changes in the masstone, strength and tint.
219-56.57 - dealt with the effects of varying acid excess in the coupling.
* Increasing the amount of HC1 in the coupling 0.75 to 1.05 mols per 0.1 mol coupling produces very slightly darker masstones, very slightly less strength and v.s, blue tints. Decreasing the J-IC1 below 0.75 to within reasonable limits ebove zero acid excess, very little changes were produced.
219-58. 59 - dealt with the study of temperature of coupling.
Increasing temperature, above 300 c gave darker, yellower and weaker products. Decreasing temperatures to 20 C gave lighter, brighter masstones - below this point the change is reversed, because of the extreme retardation of the speed of coupling.
219-60 - studied the substitution of sulfuric for hydro chloric acid and the effects of temperature development.
Sulfuric acid produces ver3r fev; changes in the color values of the pigment. Temperature development to a boil shows practically no changes.
219-65 - studied the effects cf coupling time.
Increased time of coupling produced vvs darker, but vs brighter products.
219-61 - tested the consistency of the formula set up as standard (GS-7873).
0.1 mol couplings checked each other, but were lighter, yellower and stronger than 0.4 mol couplings.
is-j,
DUP050315729
P1GM333T COLOR RESEARCH REPORTKHFT FOR TOLETIDIHE REDS
TO.
SUBMITTED BT* APPROVED BTl
f il e s yeastfEBsms DATBs APRIL-1935
umiODiroTioir
Investigations started in February* were resumed and completed this month on the use of erude msta-nltre-para-toluidine wet crystals ffer the.Reparation of Toluidine Reds,
SUMMARY & G0HGLUSIQB3
Six chargea of crude MKPT, material taken after saponification and not reerystallizred from alcohol, were tested for use in our brightest Toluldina Bed RT-386-D. These charges varied appreciably in quality* With the exception of one charge* all resulted in lab oratory toners superior to standard r t -386-D and practically equal to laboratory control.
The successful use of crude SKPT necessitates ball mill grind ing of the crude paste in order to obtain small crystals which diazotize readily, and further necessitates filtration of the diazo in order to eliminate impurities. The ground crude intermediate diazotizes as rapidly ns the regular standard dry material* eliminates the pulping up of the 33BPT prior to diazotization, and gives yields substantially equal to thoee obtained with regular material. Altho ball milling and filtration of the crude intermediate is essential to its successful use in ToluIdins Red. the expense of this operation may possibly be offset by elimination of the cumbersome pulping oper ation and settling difficulties experienced with the present standard
material, and still possibly result in an appreciable saving in materials cost. Semi-work trial of this material appears to be worthy
of consideration.
Direct substitution of crude MHPT for standard KEPT in the Dyeworks Lithosol Fast yellow HR is unsatisfactory, resulting in a deep er and duller masstone. It appears, however, that with further in vestigation it might possibly be u-ei satisfactorily for the prepara tion of Fast Yellow HR.
EXPgRIMBHTAL DETAILS
Sscpt, 33, H.B. 450. page llo, and Expts, 3, 12 and 18, S.B* 460, pages 32, 48 and 72 respectively.
S.
DUP050315730
FIGMENT COLOR RESEARCH REPORT
&--/S7
7/
DUOL TONER LIGHT RT-242-D
SUBMITTED BY: APPROVED BY*
INTRODUCTION
///
FILE: DUOIB-- DATE: APRIL 1955
Ten batches were made in the Semi Works in an effort to make
light, yellow, low bronze material to be used in shading sub-standard stock,
SUMMARY & CONCLUSIONS
The first batch was made to check SW-4071, an old Semi-Works lot that had' given desirable results. As no Hercules B Wood Rosin, one of the components, was available the ordinary Wood Grade B Rosin was substituted for it. The resultant color was light, muddy, weak,
blue and dirty and low in bronze versus the standard, thus differing considerably from the old Semi-Works lot.
Varying the proportions of the I and B Wood Rosins used, and
omitting the Sodium phosphate in the coupling showed some improvement especially in the strength, but the product still remained bluer than the standard.
Omitting the B rosin and replacing with all I rosin tended to give cleaner and yellower results, but the bronze was increased con siderably. This bronze was decreased by adding a small amount of
resinate from B rosin after the development, and holding at the dev elopment temperature a short while longer. This resulted in a de crease in bronze with practically no effect .on the tinctorial proper ties. The product, however, still remained bluer than the standard.
Cutting the Barium chloride 60# in order to get yellower re sults gave unsatisfactory blue material.
Finally a formula using Sherwin Williams TOB with all I rosin gave a bright, yellow, strong batch that was satisfactory in every way except that it was high in bronze. Plant batches will be made on this formula to build up enough stock for shading the light, blue, weak batches in sub-standard stock.
Results are tabulated in Table I.
DUP050315731
N.B. 441, pages 106-116
RT-242-D
A4
C
u H jQ JQ U n
3--1 ii--ni 1 9- oCOt
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HHto 9 >.
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8ss
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t r0t HO >
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-8
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fblb S 2S
&
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pte
fb s> o
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to ja
Uoi 3
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iB-o>t
a
I
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mso^ wa ol* H1-4 J3-t A
at c
Hp >
pJL3
P T>5v
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a
p
r-t
pIh S
P*o *A0
u
Xp0I
i CO o>
HCi3 Q
cm
r-If
C1O
CM
0
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A
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mCO
13 1P5i Sctf c* oCOi CsIM
t H -OoG t0o
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to
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\CM.i*
3 CO
H 0(0
hI 4oj at
0
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CM CM
55
P
iCOnOk
25
p
0(0 o
i-i H
o te c xos c
a>
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fmccv-
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Ss?, HI OI
3feP t> CM P > W S
to dh -0 H *8h) 0OrlS
8
tao* tJo
Ct0oO> toI
s oto*
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CM COtoO*
J
bronze
*
EXPERIMENTAL DETAILS
DUP050315732
PIGMENT COLOR RESFAROE REPORT MAROON TONER RT-219-D
SUBMITTED BY: APPROVED BY:
-- FILE: KE3 LABOURS DATE: APRIL - 1935
INTRODUCTION:
A few experiments were run in the laboratory to determine some variables which would enable the semi-works to match RT-219-B s standard in order to fill a small urgent order from Du Pont - Parlin.
SUMMARY & CONCLUSIONS:
The semi-works obtained, on standard formula, a product which was darker than RT-219-D standard (lacquer grind) and which -Parlin considered too dark for their purpose. Consequently the lab oratory undertook a study of some variables which produce lighter colors by the RT-297-D procedure. These variables, which included dissolving of the NB3 at 90 C, a decrease in caustic soda and a corresponding increase in soda ash in the coupling, and the use of
General Dyestuff Haphthol <*AS-B3, gave equal or darker colors than RT-219-D.
products.
Increase in the temperature of coupling gave darker
The addition of 5 and 1C% of B.C.K. to the KBS solution was practically without effect on the depth.
A 100^5 increase in the volume of the KBS solution before coupling gave a lighter, brighter maroon than standard. This variable was tried in the semi-works and resulted in a substantial match for standard.
EXPERIMENTAL DETAIIS :
Notebook 419
Series 419-17 - determined effect on RT-219-D of dissolv ing NBS at 90u C instead of 100 C; of decreasing the caustic soda and increasing the soda ash correspondingly; and of employing General Dyestuff Naphthol A3-BS.
Nothing lighter than control was obtained.
Series 419-18 A 19 - studied the temperature of coupling in RT-219-D
Lowering the temperature to 15 C was without much ef fect; raising the temperature to 40 - 50 C made the color darker.
Series 419-1S - doubled the volume of coupling and ob tained a lighter and brighter color than control.
Series 419-19 - tried the addition of 5 A 10% of B.C.K. to NBS but obtained very little change.
*5^ vi-v
l'fe-*
DUP050315733
PIGMSNT COLOR RESEARCH REPORT
3<5~~/3? V Vs
SUBMITTED BY: . APPROVED BY: #
LACQUER MA.ROOH RT-319-D
**/.3 >~
PILE: DATS: APRIL-1935
INTRODUCTION
One batch of RT-219-D was made in the Semi Works on receipt
of a special order from Parlin. The material ordered was required to check the RT-219-D standard more closely in depth of top than did a previous shipment (Lot 4014- SW-6837).
SUMMARY Sc CONCLUSIONS
Using a variable developed by the Research laboratory to give
a product lighter and brighter in top, a batch was made checking the standard RT-219-D formula except that the volume of the Kaphthanil ^3S solution before coupling was doubled.
This variable gave material that was ws. deep, s.bright in
lacquer versus standard ET-219-D and therefor was OK to ship. The yield was satisfactory.
Results tabulated in Table I.
EXP3RIMBHTAL DETAILS
Batch
Type Formula
.19jU)
Table I
N.B. 441, page 59
Lac
Yisld
Matl. Lot# Rubout Results vs RT-219D Results
MBS MNPT Mass. Draw. Str. Tint vs RT- ESiLfimp
SW-6984 Check CS5947 305 (lot 4081) except
double NBS vol.before coupling
405
s.dk. vs cl. s.str vs cl.vvs dp.28-1/2
vs brt s.str
yel. s.brt
29#
DUP050315734
PKfMBST COLOR BBSSARCH RBFORI
j<~- /f/o 7>
RUBIFIED BBS KIR mROOT? TfmSR RT-399-D
SUBMITTED BT* APPROVED By*
IBTRODUCTXOH
*>?</ 3 -2~
p il e t lafl-gaRoeas DATE: APRIL-1955
Improved BaphthaniX BS and purified Raohtfaanil BS were tested for use in Maroon Toner RT-399-d .
s u mmar y & comimims
Pigment prepared frost regular BBS, prepared "by an improved
process, is superior to pigment from the Id standard intermediate in white overstripe lacquer bleed, but inferior to pigments from the purified UBS and to General Dyestuff Corporation's intermediate* The purified intermediate is slightly superior to the G.D.C. mater ial and satisfactory for the preparation of RT-399-D*
While the regular improved BBS is inferior to the purified and &,D*C. intermediate, it gives toners in the laboratory which are practically equal in bleed to standard RT-399-D and, therefore, semi-works trial of this qualify of intermediate is recommended*
BXBSRIHSBTAL DETAILS
Expt. 4, B*B* 460. page 18.
DUP050315735
PIGMENT COLOR RESEARCH REPORT MAROON TONER - gr-SBA-T,
7*
SUBMITTED BY: APPROVED BY:
FILE: MIS-O.--TONERS DATE: APRIL - 193 5
INTRODUCTION:
Some assistance was given to the Raw Materials laboratory in testing shipment of TOB-W in RT-354-D.
SUMMARY & CONCLUSIONS:
The Raw Materials Laboratory has had some difficulty in matching RT-354-D standard with standard materials, therefore, the re search laboratory assisted in testing Lots 27 and 28 of TOB-W in HT354-B. A satisfactory match for standard was obtained with the stand ard materials TOB-W and B.O.N. Lots 27 and 28 gave lighter products than the control and standard RT-354-D, therefore, were considered un satisfactory.
Incidentally, the effect of addins from 5 to 2C$ of diglycol stearate before the strike in RT-354-B was tried. No im provement in texture was obtained and slightly browner colors re sulted.
EXPERIMENTAL DETAILS:
Notebook No. 424
Series 424-16 - was the R.M. test of lots 27 & 28 of TOB-W.
Series 424-17 - determined the effect of addins- 5 to 20$ of diglycol stearate in RT-354-D.
'o'
DUP050315736
PIGMEHT COLOR RESEARCH REPORT 1.1ARC PIT TOILER, RT-354-D
s#~-
SUBMITTED BY: APPROVED BY:
A
'
f il l :
TONStg
DATE: APRIL - 1935
II.TRC DUCTION:
Some attention was given by the Development Section to plant production of RT-354-D which has been running light. It was
not possible to follow operation of all batches in~detail but control tests of some of the batches were checked and variations suggested for increasing depth.
SUL-ARY & CONCLUSIONS:
There is some indication that the quality of the TOB-W is responsible for the lack of depth on lacquer test. Of two batches made with Lot 29 instead of Lot 27 previously used, one was dark and the other equal to standard.
However, no direct comparison can be made as other variations were also introduced. Omission of the final gaustic development and increase of strike temperature from B5 to 105 F did not appear to be helpful but results are not conclusive as they were tried on half charges which were pressed out together.
Use of a 20$ increase in Turkey Red Oil should also be re checked. This amount was used in the satisfactory batches obtained with TOB-W*. Lot 29. It may be effective in reducing the amount of change during drying.
A definite increase in depth of lacquer test was obtained by adding Pigment Green slurry to the finished RT-354-D slurry just before pressing. The final grind was dark, but slightly brown, and was consumed in a mix totalling 3195#. A sample ground in the labor
atory to 80 mesh fineness was still ecual to standard in depth hut was too brown.
EXPERIMENTAL DETAILS:
I'ot ebook #55, p. 133
0.9 mol couplings are being made, split into 2.parts for development^and pressed together.
42935 - Standard formula except added 7# Figment Green L (GT-6S-F 100$ weight) to batch before pressing. TC3-U', Lot 27. Lacquer Test - dark
42966 - Standard formula. TCB-W, Lot 27 Lacquer Test - s. light
42991 - Standard formula. TCS-Y.', Lot 27 Lacquer test - s. light
43005 20$ Increase in T.R.G. (Used 65if). TOR-*,, Lot 27. Vat 100 - standard development - s. dk. vs brt; vs yellow Vat 105 - final caustic soda omitted - brown; blue Lacquer test - v.s. light A brown.
43018-- 20$ Increase in T.R.C. (65ff) TOB-V, Lot 29.
Vat 100 - struck at 85 F - dark; vs brown; blue
Vat 105 - Struck at 1050 * - dark, vs brown; blue
DUP050315737
45041 - 20$ Increase in T.R.O. (65$) TOB-W, Lot 29. Standard strike temperature Lacquer test - vs brown (O.K.)
DUP05031 5738
SUBMITTED BY: APPROVED BY:
PICaiaiT COLOR RESEARCH r e po r t
PIGfaiEKT RUBINS G - RT-359-B
PILE: iilBC. TOLERS DATE: APRIL - 1935
INTRODUCTION:
A brief study of the RT-35S-B formula was made in the laboratory in order to assist the semi-works in their difficulties with respect to matching standard.
SUMMARY & CONCLUSIONS:
Semi-works production of RT-359-D has been yielding colors of duller masstones and bluer tints than standard. Consequently the laboratory studies were directed toward obtaining brighter masstones and yellower tints.
Raw material tests were made on lets 1 (standard) 10, 11 and 12 of para ehlor aniline meta sulfonic acid using formula RT-359-D, C3-7260. The results indicated that the intermediate was not respon sible for the difficulty, since all of these lots gave practical checks to each other.
Such studies as the addition of sodium sulfite immediately after the coupling, reduction in the caustic soda in the coupling with a corresponding decrease in soda ash, increase in the soda ash in the coupling were practically without effect in producing brighter masstones or yellower tints.
All tfeercaustic in the coupling made the color very dull.
The addition of small amounts of beta naphthol to the B.O.K. solution gave a dark, bright, blue color.
A small amount of barium chloride in the strike gave a lighter and duller masstone with a slightly yellower tint.
Diglycol stearate, added to the soda salt before strike, gave a duller masstone and increased the bronze.
Acidification of the soda salt before strike made the color very dark and blue.
It has already been observed that the strontium toner of Pigment Rubine G, RT-359-B, varies in depth of masstone and in tint depending on its water content. 'When dry, it is darker in masstone and bluer in tint than when it contains water. The masstone decreases in depth and the tint becomes yellower as the water content increases up to about 4%, Beyond 4^ the color only becomes weaker. Consequent ly in order to match standard RT-359-D, which contains about 4;C water. It is necessary to allow the dry color to absorb moisture to that ex tent or else to dry in a humidified atmosphere In order to prevent overdrying.
Yfhen the above precautions were taken fair matches to standard have been obtained in tints but the masstones have been some-
. ____ ______ . " .. .
DUP050315739
z
what dull and the printing tones have been bbronzy. Recent semi-works batches were humidified in the laboratory and in most cases fair matches in tint to standard have been obtained.
It has been found that a 50$, reduction in para soap and total elimination of para soap have given slightly darker but brighter masstcnes with much less bronze in the printing tone. As a matter of fact, 463-6A-1 (no para soapt was very close match in masstone and in tint to standard, and slightly strong.
EXPERIMENTAL DETAILS :
Notebook 463
Series 465-1 - was a raw material test of lots 1, 10, 11 and 12 of para chlor aniline roeta sulfonic acid on RT-359-D, C3-7260 formula.
i
All lots gave practical checks to each other.
Series 465-2 - studied effect of all caustic in coupling, of adding small amount of B.N. to B.O.K. and of adding small amount of barium chloride to the strontium nitrate solution. The effect of mak ing toner slurry slightly alkaline and acid were also studied.
Nothing of interest was uncovered with respect to obtain ing a brighter masstone and a yellower tint. All caustic gave very
'brown color. B.N. gave a dark blue product. Sari urn chloride gave a duller masstone with a slightly yellower but dirtier tint.
Series 465-3 - tried adding the sodium sulfite immediately after the coupling, also increasing the sods ash in the coupling and reducing the caustic in the coupling with a corresponding decrease in the soda ash.
Practically no differences were obtained. In the case of increased soda ash, the yield was increased and the strength was de creased correspondingly.
Series 465-4 - tried acidification of the coupling before strike; also addition of a small amount of calcium in the strike; and addition of diglycol stearate to the soda salt.
Acidification gave a darker blue product which was quite stable to moisture changes.
The calcium-strontium strike made very little difference tinctorially but seemed to give a color which was more stable to moisture changes.
Diglycol stearate gave a duller toptone and increased the bronze considerably.
Series 463-5 & 6 - studied the variation of para soap in 3T-35S-B,C3-7260, ~ Increase in para soap made very little difference. Decrease
in para soap tended to give slightly darker masstones with increased brightness, less bronze and equal strength and tint.
*85".
DUP050315740
3s--
PIGMENT COLOR RESEARCH REPORT
PIGMENT RU3INE G TONER, RT-559-D
SUBMITTED BY: (jJlSLtt^X c&.
APPROVED BY:
0
^ * 9^
FILE: Mil. ILllSs
DATE: APRIL - 1935
INTRODUCTION:
Work on this color was continued in the Semi-Works. Three hatches were made with special attention being paid to drying conditions.
3UU.ARY & CONCLUSIONS:
A check run on standard formula shaved results such as ob tained previously - dark blue bronzy product. Redrying at 140 F 40/ humidity brought the tint very close to standard but increased nuddiness of masstone and bronziness of drawdown.
Separation of the dye after coupling was repeated on a large charge and together with drying at once in humidified atmos
phere resulted in a light, yellow product.
A very promising lead uncovered in the laboratory, i.e. omitt ing para soap from the strike, was checked in the Semi-works and found
to give less bronze than standard. The product was darker and slightly bluer than standard but more work along these lines should give a closer match.
A 220# mix was made up using the yellow material made this month. While satisfactory in drawdown and tint, the masstone was quite muddy. It will probably be suitable for most customers.
EXPERIMENTAL DETAILS:
Notebook #351, p. 94
SW-6955 - l/20th of Std. formula. Check run. P.C At. o i.* ^ m Ai. Lot 12 Dried in Electric Dryer - dark; blue; strong; blue (lump) Redried in P. &. 3. Dryer - s. dark; mu dry; s. str; s. str; v.s. yellow (grind) (140 F - 40$ humidity)
3W-6967 - 1/3 of SY.-6955 Press Cake.
Dried in P. k 3. Dryer - v. muddy; s. yellow; O.E; s. yellow (140 F - 40/ liumidity.
SW-6972 - EX S'ii-6921 (Dye separated t. dissolved)
Dried as in 3d-6967. Grind - light, cuddy; yellow 6 bronzy; OK; yellow.
SW-6983 - Like 3W-6955 except omit para soap.
Dried as in 6967. Grind - s. dark muddy; s. clean; CE; vs blue.
DUP050315741
SUBMITTED BY: APPROVED BY:
FIGHEET DOLOR RESEARCH REPORT BLACK PIGm^TS
A *3 PIPE: LiZoC. TOir-nDS DATE: APRIL - 193 5
ILTRCDUCTIOI-T:
Laboratory work on black pigments was continued along two lines, viz:
1 - Improvement in the texture of the lead toner of "isrrosine for Du Pont Pariin; and
2 - Preparation of samples of treated carbon black for -print ing ink tests.
SUU-ARY & CONCLUSIONS:
Lead -Toner of Higrosine; - It was reported last montb that Parlin had approved of the lead toner of Kigrosine with respect to color but had criticized its hard texture. Consequently laboratory studies during this month were directed towards improving the texture of the lead toner. These studies i'.cluded the addition of extenders, various dispersing agents and a combination of both. Biglycolo stear ate, carbon black, a combination of blanc fixe and diglycol. stearate and a mixture of carbon black and diglycol stearate gave some improve ment in texture. Alumina Hydrate (10^). turkey red oil, rara soap, Duponol, Alkanol B, Reopen SS, Cadmium soap of turkey red'oil, and treatment with kadox-para soap were practically without effect upon the texture of the lead toner of Nigrosine. a sample (459-11B) of a lead toner containing about lOy of super spectra black and 5% of di glycol stearate was prepared and submitted"to Parlin for their eval uation. An oil treated toner (459-11A) containing about 45 of lead toner and 55% of a mixture of castor oil and dibutyl phthalate was also submitted to Parlin for test. The latter, according to our own tests', was superior in initial luster and in color to the dry lead toner. A verbal report was received from Parlin to the effect that the oil treated pigment shaved considerable promise but that further work should be temporarily discontinued due to the investigation of another type of process which is shewing promise at the Parlin labor atories.
Treated Carbon Blacks - The treatment of carbon black with sodium naphthenate at the boil and subsequent precipitation with bar ium chloride as done in C3-S789, results in considerable improvement of the carbon black with respect tc printing ink properties. There has been some doubt as to whether the naphthenic acid is really the responsible factor in 03-6789, therefore, several sauries of Levey Carbon Black have been prepared with the object of determining the effects of simple water boiling, caustic soda treatment at the boil and treatment with barium hydrate at the boil. A preliminary report frcr. the Service Laboratory has indicated that none of these treatments has approximated CS-6789. At the same time Carbon Black was treated on the mill with naphthenic acid, barium naphthenate and barium hydrate but no improvements were obtained. It appears that the naphthenic acid is essential in the C3-G789 procedure for obtaining improvements in carbon black from the standpoint of printing ink properties.
~ r-" ikStt'd 4&Z A?--' " >__
DUP050315742
2 EXPLRI&SNTAL DETAILS :
Notebook 459 (pp. 24 - 34) Series 459-8-10 - tried to improve the texture of the lead toner of Nigrosine by adding extenders and various types of dispers ing agents and fcomMnations of both. Fairly soft texture was obtained with diglycol stearate, carbon black, carbon black plus diglycol stearate and blanc fixe plus diglycol stearate. Alumina hydrate base, HL-211-D base, turkey red oil, rosin, Duponol WA, Alkanol 3, Neopen 3S, Cadmium-turkey red oil mixture had very little effect, if any. Series 459-9 & 11 - prepared oil treated lead toners of KigrosineT A 45--55 pigment-oil* ratio gave about the best results. A large sample was prepared for Parlin Laboratory tests. Series 459-12 - treated Levey Carbon Black by boiling, addition of alkali and boiling, separate addition of alkali and barium chloride, and a mixture of alkali and barium chloride. These samples were turned over to the Service Laboratory for further inves tigation.
DUP050315743
SUBtdITTED BY: APPROVED BY:
PIGMENT COLOR RESEARCH REPORT
ZIRCCNIUR COMPOUNDS
/ Jl A/ FILE: MIDCt TONERS DATE: APRIL - 193 5
INTRODUCTION:
Zirconium sulphate solution, manufactured by Titanium Alloy Ufg..Company was investigated as a possible precipitating agent for azo reds, and as a substitute for aluminium sulphate for preparing a lake substratum. This work was done in accordance with A.L. Erskine's memo of 2-6-35 and R.R. Denslow's nemo of 2-5-35.
SUMMARY & CONCLUSIONS:
Attempts were made to precipitate the soda salts of Lithol Red and Lithosol Red 2-B with zirconium sulphate. The product obtain ed with Lithol Red was very brown. In the case of Lithosol Red 2-B, incomplete precipitation was obtained. These results might possibly have been due to the strong acidic character of the zirconium sulphate solution.
Zirconium sulphate was treated with caustic soda, soda ash and disodium phosphate. The resulting products were extremely hard in texture, therefore, of no merit as white pigments or extenders.
EXP mMENTAL DETAILS:
Notebook No. 307
Series 307-49 - attempted the precipitation of Lithol Red with zirconium sulphate.
A very brown product was obtained.
Series 307-51 - were precipitations of zirconium sulphate with caustic soda, soda ash and disodium phosphate.
The resulting products were extremely hard in texture.
Notebook No. 447
Series 447-21 - was an attempted precipitation of Lithosol Red 2-B with zirconium sulphate.
No complete precipitation was obtained. It was thought that the strong acidic character of the zirconium solution was respon sible for the bleed, consequently.sodium acetate was added to the strike but no complete precipitation was obtained by this treatment either.
DUP050315744
PIGMSKT COLOR RESEARCH REPORT
J4T- #<7
COLOR LAKES OP VAT DYBSi AHD AOID DYES 03? WOOL ACIDS
SUBMITTED BY* cJ APPROVED BY l ^
PILE:
LAKES
DATE* APRIL-1935
1BTRQPUQTI0B
Investigations were continued this month on the preparation of lakes from water dispersible vat dyes of Ponsol Blue GZ, Ponsol Blue GD* Ponsol Jade Green Supra and Indanthrene Blue 2 GBSL.
The work this month has been confined almost entirely to the vat dye lakes and only little attention has been given to the prepar ation of lakes from acid dyes and wool acids.
SUMMARY & OOBCLUSIOBS
The tinctorial properties of lakes prepared from vat dyes ap pear to be dependent upon the physical form of the dye, such as dis persion, particle siae. crystalline or amorphous character, etc. which affect and determine the physical form of the dye on the substratum of the color lake. This explanation apparently is confirmed by the results of dyeing and printing of textiles, in which case the tinctor
ial properties of vat$res are greatly influenced by their physical properties. In some eases, altho the dyes are similar chemically, they are satisfactory for dyeing and unsatisfactory for printing tex tiles and vlee versa.
Laboratory development of Blue Lake BP-121-D appears to sub stantiate the above* for in order to obtain a lake of optimum tinctor ial properties it was necessary to employ Ponsol Blue GZ crude paste, the regular or double paste having been found inferior. Altho chemi cally alike, the double paste and crude paste differ in physical form.
Dry vat dye powders of a specific physical form which disperse to a clear colloidal solution in water have been prepared by the Dyeworks by W & P milling the regular pastes with dextrin and leueanol. In the ease of Ponsol Blue GD. GZ and jade Green Supra, alumina hydrate
lakes appreciably superior to lakes prepared from the regular pastes,
have been obtained* The superiority is manifested principally by improved depth and brightness of masstone, increased cleanliness and brilliancy of shade, tint and printing tone, and some increase in strength* Whether or sot an appreciable improvement can be effected apparently depends upon the form of the commercially obtainable dye, e.g* Indanthrene Blue 2 GBSL which apparently contains some dispers ing agent, does not exhibit an improvement, in the lake prepared from dispersible dry dye, as great as the above mentioned Ponsol Vat dyes. The improvement in this case is primarily one of blacker and brighter
masstone,
A water dispersible dry vat dye powder similar to the & P
type material has been prepared successfully by colloid mixing the dye
paste and dispersing agents, and subsequently drying the product,
lakes and paper coatings of improved tinctorial properties over the regular paste products, and substantially similar to the corresponding products from W & P dye, have been obtained. The results obtained to date indicate that the successful preparation of the dispersible toy vat dye powders is not specific to r & p milling.
DUP050315745
The substitution of soluble rosin size for dextrin is satis* factory and advantageous* thus avoiding the object!onalbe use of dextrin.
Ponsol Blue GZ, GD and Jade Green Supra dispersible dry ponders
are appreciably stronger and brighter than the corresponding untreat ed regular paste, as judged by paper brushout tests. Indanthrene Blue 2 GWSL dry dispersible powder exhibits only a slight improvement over the regular paste, which is attributed to the excellent dispersion of the regular paste owing to the apparent presence of a dispersing agent.
Investigations are being continued with the object of determin ing the scope of this problem and the application of dispersion prin ciples as herein observed, to existing and speculative problems.
Investigations were continued on the preparation of lakes from
precipitated wool acids. A lake of the BL-79-D type has been prepared from Anthraquinone Blue BIT and while results of interest have been obtained, no prophecy can be made at present concerning the merit of this lake*
Further studies on the preparation of a Cerulean Blue Lake from Lithosol Brilliant Blue S and wool acids have confirmed the results of previous work. The new lakes are appreciably greener, more brill iant, stronger and faster to light than BL-72-D and similar lakes pre pared in the laboratory. The wool acid lakes, however, are Somewhat
harder in texture than the BL-72-B type lakes and this disadvantage must be overcome in order to obtain a product of commercial value.
The use of barium chloride and aluminum chloride has practically no effect on the tinctorial and lightfastness properties of the wool acid
lakes, yet these precipitants are absolutely essential in the success ful preparation of BL-72-I).
Continuation of investigations on the preparation of lakes from wool acids and other protein matter is proposed.
BKISaiMSSTAL DETAILS
Vat dye Lakes
Ponsol Blue GL - Expt. 13 & 17, R.B. 460,
Ponsol Blue GZ - 1, 13 & 14
*
Ponsol Jade Grevn)
Supra)" 5 & 6
*
Xndanthren
11 & 13
pages 52 & 70 respectively.
" 4, 52 & 56
* 20 & 24
"
44 Sc 52
Wool Acid Lakes Lithosol Brilliant Blue 1 - Expt. 51 & 53, E.B. 450 pages. 184 & 194
respectively, and Expt. 7, R.B. 460, page 28.
Anthraquinone Blue BK - Expt. 3. E.B. 460, page 12.
DUP050315746
BLITTED APPROVED BY:
PIGKENT CCLDR RESEARCH REPORT EXTENDED PIGMENT RUBINE RE-39O-D
-s 0
* SLf
i ILj i : itliSC. EAiiTHIS BATE: APRIL - 1935
1 INTRODUCTION:
Two batches of this lake were made to fill an order from Congoleum-Nairn. Variations previously used were made to obtain proper shade.
5DENARY & CONCLUSIONS:
Each batch was a check on a previous run and the products obtained were, about the same as on the last series, i.e. one batch was dark and blue and the other v.s. dark and yellow in tint. The yellowness of tint was due to some extent to an increase in amount of soda ash and para soap hut probably chief^ to humidified drying.
A mix sufficient to fill most of the order was obtained and another batch of the yellow material is in process.
EXPERIMENTAL DETAILS:
Notebook 318, p. 23
42808 - Check 39840 Grading - dark; blue; s. strong; blue
42840 - Check 39960 but increased batch size. 94# Soda Ash.in' coupling; 31# Fara Soar. Struck at 180 7. Dried et 140 y _ 40$ humidity.
Grading - vs dark - muddy; s. strong; stroiv.; s. yellow.
" JjwfSiSS . . *
DUP050315747
SUBMITTED BT. APPROVED BY:
PIGMENT COLOR RESEARCH REPORT
RAW MATERIAL TESTING
/30. A PILE: RAW MATERIALS DATS: APRIL - 1935
All items outstanding from previous reports have been satis factorily tested.
This month 105 shipments of raw materials were received and s sampled, and have the following status: sixty-six tested in the
laboratory and found to be acceptable; 3 satisfactory when previously tested; 4 OK in plant; 4 satisfactory when used without test; one for SW consumption, and 26 reported v/ithout test. A special shipment of Dispersing Clay was tested on several formulae and'proved unsatisfac tory. Its principal disadvantage was in failing to completely "take up" the prescribed amount of dye. The material was rejected.
RAW MATERIAL SAMPLES
There are no samples outstanding from previous reports:
Pen samples were received this month:
RMS 1399. Sod. Sulphate "Natural Product". Satisfactory.
RMS 1400. Ammonium Oxalate, Jungmann & Co. Satisfactory.
RMS 1401. Calco Red Lake C Barium Toner Pulp - Light, Caleo Chen. Unsatisfactory.
RMS 1402. Azo Bordeaux S.3. Cone. National Aniline - Unsatisfactory.
RMS 1403. Lake Red CR Pulp #282. Lot 71. Sherwin Williams - Satis factory.
RMS 1404. Acid Tartaric U.S. F. Powdered. Kallinckrodt - Satisfactory
RMS 1405. KEPT - Calco - Satisfactory.
RMS 1406, Supratol Y.A. Kart Prod. Corp. - Not tested.
RMS 1407. Lake Red CR Pulp CP 282. Lot 71. Supplementary to RMS 1403.
RMS 1408. Anthranilic Acid Technical - Dow Chemical Co.- Unsatisfactory.
aSSSSSSS*
DUP050315748
PIGMENT COLOR RESEARCH REPORT
S^7
SEMI-WORKS PRODUCTION
SUBMITTED BY:"#'APPROVED BY:
/// n il s : -eR-a&e DATE: APRIL 1935
INTRODUCTION
84 batches of 24 different colors were made. These included 11 "batches of RT-242-D, 6 "batches of RT-399-D, 6 batches of RT-7873D. 4 batches of RT-359-D, 3 batches of GL-7854-D. 4 batches of GL-7789D,
4 batches of GL-7863-D* 10 batches Y-305-D. and 7 batches Y0-38-D.
SUMMARY
RT-242-D, Barium Duol - Eleven batches were made in a study of the process undertaken for the purpose of obtaining yellower tints and less bronze.
RT-265-D Calcium Duol - Three batches were made for production of shading material.
RT-359-D, Pigment Rubine - Pour batches were made in a process study and to obtain satisfactory material.
RT-399-D. Improved NBS Maroon - Six batches of this improved product were made in a trial of purified and special Naphthanol BS.
RL-7665-D, Calcium Lithol for Rubber - One batch was made to recheck a satisfactory batch made previously.
RT-7873-D, Red Toner - Six batches were made in denSLopment of this improved red of RT-208-D type.
RT-219-D, Light Maroon - One batch was made to fill an order far- Parlin. A modification in formula was made to obtain standard depth.
KE-253-D, Scarlet Lake - One batch was made to obtain material far an order.
3T-125-D. Blue PTA - Three batches were made in trial of a laboratory formula for a stronger product.
GL-7854-D, Rubber Color - Three batches were made in development of this lake made from Lithosol Brilliant 31ue E and Naphthol Yel lowAS .
BT-150-D. Blue PTA - Pour batches were made in a yield study.
GL-7789-D. Rubber Color- Pour batches were made in development of this extended PTA made from Thioflavine and Brilliant Green B.
GL-7863-D* Rubber Color - Pour batches were made in development of
this extended Brilliant Green 3 PTA. Y-202-D, Lemon Yellow - One batch was made in a trial of an improved
laboratory formula. Y-309-D. Excelsior Yellow - Two batches were made for a similar pur
pose. Y-305-D. Primrose Yellow - Ten batches were made in continuation of
this development problem. YO-38-D, Chrome Orange - Seven batches were made in a study of the
process to correct plant difficulties. G-389-D. Improved Light Stability - Two batches were made concluding
the Semi Works study of this process.
DUP05031 5749
f* 2
G-7192-D, G-7194-D, Strong Green - One batch of the former and two of the latter were made, in production of the darker green for use in the Puller green. G-378-D.
BE-149-D, Dry Dispersed Lake - One hatch was made for stock.
GE-3B8-D* Dry Dispersed Lake - One hatch was made for stock.
BkL-6619-D, Treated Black - One hatch was made for Parlin.
One grind and fourteen mixes were made in the research semi-works for the plant during April, 1935.
Grinding
Charge
Batches
Ihs
CP Green
741-s
1
50
Mixing
Charge
PTA Toners
Red Toners Blue Lake
Red Bulk Lake Extended Yellow CP Orange CP Yellow CP Green
751-s
19
t*
It
752-s 754-s 753-s 755-s
Batches
4 1 1 2 2 1
1
_2
lbs
791 344 203 1167 1975 570 455 430
Total
14
5935
DUP050315750
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DUP050315751
4
SUMMARY OF #10 BLDG* PRODUCTION REPORT FOR APRIL - 1935
No* Batches
Code
lbs* Struck
11 RT-242-D 1619
3 RT-265-D 708
4 RT-359-D 118
4 RT-399-D 272
1 RL-7665-D 118
6 RT-7873-D 180
1 RT-219-D 28
1 RE-253-D 398
4 BT-150-D 161
3 BT-125-D 50
4 (j T-68-P
72
3 GL-7854-D 237
4 SL-7789-D 180
4 GL-7863-U 340
1 Y-202-D
31
10 Y-305-D 390
7 Y0-38-D 610
2 Y-309-D
78
2 G-389-D
70
2 G-7194-D 600
1 G-7192-D 171
1 B2-149-D 900
1 GE-388-U 252
3 BkL-6619-D 42
7625
lbs. Pack.
1565 731 118 276 113 169 29 359 162 46
227 171 324
25 371 529
73 68 610 168 877 242 41
7261
2 Yield
96*7 103.2 100.0 101.4
95.7 93.9 103.6 90.1 100.6 92.1
95.8 95.0 95.3 80.7 95.1 86.7 93.5 97.2 101.7 98.3 97.5 96'. 1 97.6
95.9
DUP050315752
5. MATERIAL TRANSFERRED DURING APRIL 1935 PROM RESEARCH SEMI-WORKS
f?
Lot 4041 4054
55 56 57 59 60 61 62 69 70 4058 4066 4075 76 77 4078 4082 4083 4084
4029 4053
4050
4051 52
4064 4067 4068
4044 4085 4063 4074
4079
4081
4047 48 49
4042
4045 46
4043 4065 4071
72 73
CR-200 1
1
1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1
Color Code RT-300-1) RT-242-D
If
IV
tv
H
II
If
tl
ti
n
RT-359-D RT-242-D RT-265-L
It
RT-300-D RT -405-1) RT-406-I) RT-359-D
2 GX-7829-D 2 GX-312-D
lbs. 319 151 153 154 157 162 156
81 76 147 163 26 100 246 243 242 82 152 23 209
139 355
Group 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 1 1 1
1 2
3 Y-305-D
446 2
4 G-389-D
4 G-207-D
4 B-141-D 4 G-389-D 4 G-7192-D
522 2 66 2 55 2
211 2 166 2
6 GE-388-D 6H
6 BS-147-D 6 RE-253-D
247 1 242 1 875 1 359 2
10 RP-7516-D
38 2
12 RT-219-D
28 1
108 108 108
GT-68-P
fl
tl
Dry Wt 81 96
110
1 1 1
115 RT-7853-D
246 2
11 BL-151-D 11
104 2 110 2
127 129
138 138 139
BT-7737-D B-7469-D BkL-66n19-D
if
38 2 67 2
13 1 12 1 14 1
Cost Unit 52.75 47.05
131.42 47.05 48.91
52.75 104.21 103.83 133.42
8.82 4.88
7.80
11.30 9.82
30.61 11.30 10.17 17.69 17.55 16.49
31.23 203.96
59.80
131.39
43.50
297.84 22.54 61.69
DUP050315753
6
RECAPITULATION
April
Colors 1935.
transferred
from Semi
Works
to
Plant
during
Toners
Ext. Colors Yel loirs (Jre ens
Blues "RE" Lakes "RM* "RL"
Maroon Toners PTA Toners Toner Pulps
3348#
494 446 955 122
1723 39
252 28 38
287
Total 7732#
Ik
DUP050315754
1935 - RESEARCH SEMI-WORKS #10 BLDG
MATERIAL " IN PROCESS" OF MAY I ,
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DUP050315755