Document 7zJa2Qeg2j4KZBLL2D4dm016

E. I. DU PONT DE NEMOURS & COMPANY KREBS PIGMENTS DEPARTMENT 256 VANDERPOOL STREET NEWARK. NEW JERSEY v v, ' L-U--* U' Copy No. 1 Numerical // ^7* 6 / - 4 C - "5 Period Covered: NEWARK PLANT PIGMENT COLOR RESEARCH REPORT Final Report "OS STRAIGHT" STUDY - DRY COLORS MARCH 1941 - MAY 1942 114o01 FILE: DATE: 8/29/46 \ i NJ627S N39991 Serial Ho. KN-46-53 Copy Ho. l Copy tot #1 - Numerical File 2 - Research Office (114.01) 3 - Library File (114.01) 4 - #10 Building File ?-# 6 " * 6 - Imperial Chemical Industries. Ltd. 7. H 3- w H m II N || 9 - W. F. Spengeman 10 - Extra NEWARK PLANT PIGMEHT COLOR RESEARCH REPORT Final Report "OK STRAIGHT" STUDY - DRY COLORS MARCH 1941 - MAY 1942 SUBMITTED BYt APPROVED BYt L. Stewart R. R. Densl J. 0. Jforri 7/30/46 #'* DATE SUBMITTED* 7/23/46 DATE ISSUED* 8/29/46 N39991.01 DUP050150378 .MRT ~.m ^PLQRS This report has been prepared to summarize and consolidate the information developed in the course of a research program which was carried out in 1941 and 1942* It has been designated the "OK Straight Study" since the object was to Improve plant performance In respect to reproducibility from batch to batch. The study as such was discontinued in May, 1942 but has never been formally reported. The following was compiled from a partially completed draft of a progress report prepared by Dr. Stewart at the time, together with copies of memoranda summarizing the status of the work from month to month. Other pertinent information has been Included when readily available. Attention was focussed for the most part on chrome oranges; however, some consideration was given to chrome yellows and to zinc yellow. R.R.D. mMiXoa* Dry color which is not satisfactory for shipment on com pletion of the normal processing procedure must be brought to speci fication by dry blending with other material. Standardization by dry blending is both time consuming and expensive. Because of the increasing demand by the trade for more rigid standardization, the amount of dry color finishing equal to standard without dry blending, known as "OK Straight", decreased steadily from 39# of production in 1930 to an all time low of 14% in 1935* At that time the seriousness of the situation was recognized and steps were taken to Improve the performance. Improvement was shown, until, for the last quarter of 1940, the "OK Straight" performance was 36*9#. Cost calculations made at that time indicated a savings of approximately $40,000 per year could be obtained by increasing this te 85*0. In view of the potential savings involved the Research Department was requested to assign a chemist to full time study of this problem. During 1941 and the first half of 1942 full time was given to the problem* However, during the last half of 1942 little attention, other than that of a general supervisory nature, -was given the problem because of the pressure of other work. DUP050150379 - 2- As a result of the combined efforts of the Production and Research Departments, the "OK Straight** performance on colors was increased from an average of 36.9!* for the last quarter of 1940 (the period immediately preceding the study) to an average of 78.4J? for the last quarter of 1942 when the study was dis continued. This Improvement in performance, 41.5$, was due pri marily to two factors* - (1) An improvement in quality control. (2) An increase in zinc yellow production which usually runs 95-100$ "OK Straight". However, the Increase In zinc yellow production at that time was relatively small and calculations In which correction la made for the effect of the increase in zinc yellow production show that approximately 75$ of the improvement was due to Improved quality control. Further confirmation of this fact is obtained by an examination of the performance of the individual color groups. A decided improvement is to be found on some groups as well as a general improvement on all groups. As is to be expected,the above improvement has resulted in increased efficiency and reduced costs, especially in the grind shop. She amount of color processed In the grind shop increased from 300 lbs. per man-hour to 540 lbs. per man-hour and the labor cost per barrel of color standardized was reduced, roughly, from $1.20 to $0.65. Rough cost calculations show thai these savings amount to approximately $30,000 per year. The individual studies leading to the above described improvement in "OK Straight" were: - 1.A general educational program based on a survey of color shop operations. 2. Revision and standardization of the tri-basic lead acetate process (See KR-41-159 and SF-25 formula, K-1482) 3. Revision and standardization of the lead nitrate process (See KS-44-46 and SF-10 formula, K-1720) 4. A general revision of formulas with emphasis being placed on control points, tolerances, etc. 5. A standard practice manual was written describing in detail the proper method ef performing the various plant operations. DUP050150380 - 3- 6. The chrome orange process was studied in detail and control refinements introduced into the formulas. 7. A general study of the chrome yellow processes was started. 8. A definite system of classification of ground color was established. This system was based on the criterion that color which grinds out "OK Straight" is the most desirable type from an economical standpoint. Items 1 and 8 are discussed in the following section: jmmL. Educational Program. temail_nn. Survey of Color..Shop It was known in the beginning that the properties of a pigment depend primarily on its chemical composition, and the slse and shape of its particles. The problem of improving quality control, therefore, resolves itself into establishing the necessary oontrol over all factors affecting chemical composition and particle slse and shape. In general, the principles governing particle formation were known. For example, it was known that the amounts of raw material, their purity, their acidity, etc., determine the composition of the pigment, while the size and shape of the particles are affected by the rate and temperature of strike, amount of agitation, etc. In other words, in order to produce "OK Straight" material standardized raw materials must be processed under standardized conditions* Bearing this In mind, a program was set up to check the following} (a) Formulas - for dupllcabllity, material balances, control points, equipment limitations, etc. (b) RawMaterials - for variation, purity, methods of analysis, methods of sampling, etc. (c) Equipment - for suitability, mechanical condition, accuracy (scales, thermometers, etc.), etc. (d) Operating Technique - for accuracy, methods, etc. (a) Evaluation of Product - for accuracy of method, choice of standard, practicability of shipping limits, etc. (f) Performance - fcy individual code so that the "bad actors" could be spotted. Normal practice had been to show the performance by group. DUP050150381 -4- All of the lump color ground In the plant falls into one of the following classes: 1. "OK Straight" - Material satisfactory for the purpose for which it was made and shippable without further work being done on it* Material of this type leads to lower labor costs, decreased investment charges, and good customer service* 2. "Shipoable Straight" - this includes material unsatis factory for the purpose for which it was made but satisfactory, without additional labor being expended on it, for another purpose* Material of this type, also leads to lower labor costs, but the amount that can be carried in stock is usually limited and its manufacture is accompanied by poor customer service* 3* "gab-standard" - this includes material which is not satisfactory for the purpose for which it was made and must be blended with other material before it can be shipped* Because of the additional work involved in blending, the manufacture of this type material is relatively costly* The object of this study is to eliminate, as far as possible, the manufacture of this type material* 4. "Component" - in some cases it is more convenient to make a desired product /by blending two or more standard colors. Material falling in this category i3 classed as a "component" since it obviously cannot be "OK Straight" as struck. 5* "Development" - all experimental material falls in this category. It does not affect "OK straight" performance. 6* "Shading Material* - this represents, material deliberately made "off" standard for shading existing sub-standard and comprises 3 sub-groups - a) OK as shading material. Class as (4) h) Unsuitable for shading but shippable straight. Class as (2) c) Unsuitable for either (a) or (b)* Class as (3). The "OK Straight" performance for any given period is obtained by dividing the pounds of color falling in class (1) by the sum of the pounds in (1), (2), and (3)> DUP050150382 5- - MONTHLY PROGRESS REPORTSON "OK STRAIGHT* PROBLEM (Stewart) i - PforeM.Ogamm A. Y0-27-P Observation in the plant has shown the reverse strike to be unsatisfactory from the standpoint of being able to control conditions of temperature, time, volumes, etc. In the laboratory good duplicability has been Obtained using the direct strike which can be controlled* Plant trial of the direct strike shows that conditions can be controlled satisfactorily but lighter material is obtained. Variables are being applied to this type of 'formula to give standard material* B. & This is a chronic `"tick list" color and the OK Straight performance has always been poor* *Observation in both plant and laboratory Indicates that the trouble is probably due to the method (kof making the "white base". In order to make a 6000 lb* batch in the ''plant it is necessary from volume considerations to add dry sodium bicarbonate to the lead liquor when precipitating the base* This method gives a lumpy non-uniform base and its conversion is therefore erratic. Laboratory study shows that check results can be obtained if the bicarbonate is added as a solution instead of dry* This would involve cutting the batch size from 6000 lbs. to 5000 lbs. Other means of overcoming this difficulty were tried but without success. Plant work is now being directed towards determining the performance to be expected with all conditions controlled as closely as possible except for the use of dry bicarbonate* Following this, three batches will be made at a smaller batch size using controlled conditions and the bicarbonate in solution. A comparison of the per formance by both methods will then be made to determine whether the decrease in batch size can be justified. c. Qrawrea,. Plant performance on YO-263-D and Y0-260-D has always been very poor. A laboratory study is now in progress to develop more information and better control of these formulae. Some of the variables being studied are acidity, chrome concentration, and development temperature. No results are available. II - Miscellaneous A. Although the plant OK Straight performance is reported monthly for each group, the performance for each individual code Is not calculated at present* This has been done for January and February and will be done monthly in the future* DUP050150383 6 msuJLm. i - fifeQsg..gxaB&a& The new recording thermometer which was purchased for the chrome orange strike vat has been installed and was placed in service on April 28th. It was checked against a standard thermometer before use. Its use has confirmed our belief that temperature control on chrome oranges, especially YO-38-D, was very poor. With the elimina tion of this important variable and the use of controlled formulae, the one important variable remaining to be controlled is concentration and acidity of lead liquor. Work will be started on this during the coming week. A. XQ-3Z-.B The study of variables to give standard material was continued. Two batches were followed in the plant. Both were just outside shipping limits, one being too dark and the other too light. The study of control variables will be continued. B. Five batches were followed in the plant. Two of these were made with variable changes to adjust the formula to give standard material. One of the remaining three batches, which were made on the same formula, was OK straight. It has been found, however, since the new thermometer was installed, that the temperature control on YO-38-D was poor. Evaluation of the YO-38-D formula using dry bicarbonate is being continued. In connection with the laboratory study of XO-36O -D it was noticed that several of the batches made were quite dark in masstone. Rubouts showed one of these to be quite close to Y0-38-D. This is of Interest as it may be a means of making our Dark Oranges on a formula that can be controlled, that is, eliminate the dry bicarbo nate method. This lead will be investigated further in the near future. C. The laboratory study of the YQ-260-D and YO-263-D formulae has been completed and plant batches are now being followed. No results are available on the bateh of Y0-260-D which was followed. Investigation has shown that practically all Y0-260-D and YO-263-D are sold as "specials". These four or five "specials" are made by shading with small amounts of chrome yellow or other orange. Work should be directed, therefore, towards striking these "specials" OK Straight rather than YO-26O-D and Y0-263-D. The Production Depart ment has been asked to supply a list of such "specials" for considera tion. DUP050150384 - 7XI - ifi3Jf33J>gg Our present knowledge of the zinc yellow formulae Indicates that the controlling variable, provided standard formula Is followed In other respects, is the amount of impurities in the zinc liquor* The amount of Impurities required to give standard material is not known* Variation in quality in the plant is due, no doubt, to the fact that a fixed amount of Impurity is added to the zinc liquor without any consideration being given to the amount of impurities already in the zinc liquor. A preliminary survey shows that the impurities in the zinc liquor vary considerably. Work is being directed towards establishing a relationship between the amount and kind of impurities in the zinc liquor and tinctorial properties. A. Y-232-P Four batches were followed on standard formula in the plant and a close cheek on impurities made* All four batches were OK Straight. This work is being continued. B. Two batches were followed very closely for the purpose of improving the OK Straight performance and also to develop texture equal to our "HY-CAP" standard. Samples of these batches are to be submitted to the Ink Laboratory for evaluation* Wo further work is planned until results are obtained on these batches. Ill - MtaefiAiUfflftRBa A. Plant OK Straight performance has beencalculated for April for each individual code. DUP050150385 -8- gt4Xi.J24.i_ I - QKHfqfM O^flSRga A. XQ-?..Zd2 Three batches were made In the plant using the direct type of strike and controlled conditions, hone of these were OX Straight. These results Indicate that yellower material is to be expected from the direct strike than from the reverse strike* The reverse type of strike Is to be avoided, however, as processing conditions are not readily duplicated due to equipment limitations. Control variables will be applied to the direct type of strike In an attempt to obtain more "in-line" material. B. Xq-MrJB The Initial trial of YQ-34-D in the plant using controlled conditions resulted in OX straight material* This batch will be checked when production is resumed. C. 22=3S= Study of the YO-38-D process In the plant was continued* The first two batches, check batches, made during the month were OX Straight, but, when production was resumed about a week later, using the same formula, very dark material was obtained* Apparently the plant had encountered one of its chromic "off11 periods which necessi tates a readjustment of the formula. The trouble has been traced to a shortage of lead in the strike and an average of bicarbonate of soda, both of which tend to give darker#material. In order to prevent the reoccurrence of this type of trouble the plant has been asked to con trol the lead liquor within definite limits and the bicarbonate is being weighed Instead of being used at the net weight specified on the bag. The formula has been adjusted to give standard material on this basis and a performance series is being run. Thls%0-260-D type formula, which was developed in the laboratory last month for the manufacture of the Dark Oranges, was tried in the semi-works during the month. This formula, since it eliminates the solid phase or "white base" step in the regular process should be much more easily controlled and, therefore, give a higher OK Straight performance* The results of the semi-works batch are quite promising and another batch is to be scheduled as soon as equipment is available. D* M-a&QffiB. Study of the Y0-260-D process was started in the plant. Two batches were made using the direct type of strike and controlled conditions. Both batches, which were made for shading purposes, gave satisfactory mixes. This study will be continued when pro duction is resumed. DUP050150386 - 9S. XQ,".263~P. Study of this formula was also started in the plant* A batch, which was made for use In Y0-422-D, a dry mix, was satisfactory for this purpose* II - 2iUaa.Xs.Ufll.. Study of the zinc yellow processes was Interrupted early in the month while the Development Section at the Operating Depart ment's request, determines the maximum batch size for the present equipment. Before this work was discontinued, however, three batches of Y-467-D with "HY-CAP" texture were made. The develop ment of MHY-CAPM texture on Y-46?D is being carried along as a part of the OK Straight study* This work will be resumed when the study of batch size is completed* m - fi&^aJLtUaia With the discontinuance of the OK Straight work on zinc yellows, attention was turned to Chrome Yellows. Calculations, based on the first four months of 1941, show that the three yellows, Y-403-D, Y-424-D, and Y-490-D, which are dry mixes, comprise 43.5# of the color sold as dry mixes. If these three yellows were to be struck OK Straight, and the problem does not appear too difficult, a savings of approximately $8000 per year could be realized. With this in mind a letter is being written requesting the Research Department to take up the study of this problem in the laboratory. An added reason for the study of Y-490-D, which is a special for Q.P.I. and probably the largest single yellow consumed lm the country, is that we only get a small part of this business. If the yellows were struck direct and OK Straight, it should lead to a much more uniform and satisfactory product* iv - glass,UaaasM... A. Plant OK Straight performance for April has been calculated for each individual code* DUP050150387 10 u im Control of chrome oranges depends on the control of chemical composition and particle size. So control the chemical composition, it is necessary to control closely the amounts of raw materials used, especially those that effect the alkalinity of the system. To con trol particle size, physical conditions, such as temperature, volume, etc., must be controlled. It is felt that the physical conditions and some of the raw materials are now controlled satisfactorily! however, the lead liquor has varied greatly and has been far from satisfactory for use on chrome oranges. Little progress has been made by the plant in meeting the specifications set up In a letter of Hay 21, 1941. During the early part of the month approximately $0% of the lead liquors used contained precipitated material while during the latter part of the month the liquors have been too acid*. Rapid methods for the determination of alkalinity and lead con tent have been developed in the laboratory. It has been suggested that the plant use these methods for control purposes and arrange ments have been made to check all finished liquors in the laboratory by these methods. Attached is a table giving the details on batches of orange followed in the plant and semi-works diving the month. I - Chrome Oranges A. XQ-aZzS All the Light Oranges made in the plant to date by the direct strike have been muddy and yellow. CasparIson of the reverse and direct type of strike, both in the laboratory and the plant, shows that the reverse strike gives cleaner, brighter and redder material than the direct strike. Although the dlreot strike is more desirable from a control and ease of operation standpoint, rather than embark on a long and costly study to eliminate the muddiness, it has been decided to improve the reverse strike as much as possible and deter mine the "OK Straight" performance to be expected. B. IQ-34.dB The three Hitches made were within shipping limits of each other but two were-too dark to be "OK Straight". Lighter material will be made when production is resumed. DUP050150388  11 c. fll-3gr.B In generalj batches made on the same formula were within shipping limits of each other provided the bicarbonate of soda was weighed rather than used at bag weight* Three batches, howeverv made with lead liquor which was found to be "off were quite dark and muddy and did not check among themselves* Trial of the Y0-260-D type formula in the semi-works gave material which, although muddy, was relatively close to YO-38-D in shade. As the direct strike was used, it is believed that the reverse strike will eliminate the muddiness* A batch will be made by the reverse strike method when equipment is available* Ho production in plant* B. IQ The reverse strike gave cleaner and brighter material here too. Variables will be applied to the reverse strike to give standard material and a performance study run. 11 - zim XaUfiga The "OK Straight1" and development of "HY-CAP" texture studies have been inactive pending the completion of the study of batch size in the plant* xxi - PtemJCftiUgaa The Research Laboratory is actively engaged in developing a formula for Y-490-D as a struck color* Y-490-D at present is made as a dry mix. Satisfactory progress is being made on this problem. iv Miasgllflagaaa A* Plant "OK Straight" performance for Hay has been calculated for eSch individual code. DUP050150389 $ CM H d 0 H H Ofa P P o o % *2 1 11 u *<o * m w 8+5 <h ja 28 . o<R Ik OU> ^ 03 ow ui CQ 0 H fa P 0P PP 0 1 "CM * CM `CM1 d PUv P WOO 0 fa Vl VfOa< VOl O 00 gig| o o" H OH PP ?onCM PntplfN* T3VrXJU\ CO woo rf o sas ju s P OP 0 o S O CO CO ao w CO c p w co &CQ oca I t g fa o u * 1 0d fa 2 I b ** P %p A CO A 94 fa 2 0 op 0 TJ K2 * 09 *0* M 9(D4 O n 44 > *ts 0O fa 44 *o 0 P p 0 Pf0a 0 04 *Q H jd Vol 0 *8 i %s po 0 fa H O I* -H ** Hi -P p *5 P p co H19 4CO s* 3p & ca 0 0I M ! V 0 43 0 g OH 8 P0 -HP *8 tv S O O rn S< f-i ON * s OOH P-9 OH HH 4HS0ta0RT0V'SHH VO t I I CV) 0\0\O4 UCMRffVfvV*l coco o 8I0U 1 o 4O4 j o O fa o o " Si 3S oo Mo 0 si a 0 b *eh w o M cB O GO 4O->4H*0 C(1Q0 8 B H & O0 c H 0 9 fa * 0 o w-o 0 > *** fa p p0 *ft 0 AO no f0a *s fa 0 0 -O *o fa 0 > ft p >0 PH0424** 4n4o t> t? H0 m p0 J8oH'"Wc?o Sa* 81* o S 3 -0 4h O H HI 0, H H0 OH 0 5 fa fa W3 P fa 0 0P 0 O 0 > fa O80O _ A fa Vi SS-H 0 P0 0 JS> iPHfa M -<* H fa c?VCONP0 PPH 0 W vO 00 P P0 H SS'-gg ao 3 so n to * Jh I0 fa fa PO Vi C> H l P 0 >4 0 p H Cv oo CCMMUCNv 5s*V 0000 8 ro v0 00 N fO JUTvV 00 00 flOr\ clro\ OV \rTOs cVorv OVO sINOC\O0 ^ JS TO o mmeg oUovolros oirov ovoocvoOcvoO0C*v VO CO vO CO ai a -mnr %CO iI H CQ amI VO CM I gg DUP050150390 - 13 The "OK Straight" work was Inactive during the period July 20th - August 3, 1941 while the staff was on vacation* The control of alkalinity and lead content of lead liquors during the month was satisfactory* The improvement was obtained by adjusting the liquors, as soon as available, using the rapid methods developed in the laboratory for the determination of alkalinity and lead content. Examination of retained samples indicate that all of the lead liquors used during the month were stable, that is, had no tendency to precipitate on standing. Preliminary results indicate that further improvement in the control of chrome orange manufacture has been obtained thru using pH as a measure of alkalinity rather than total pounds of acetic acid* This change has necessitated the readjustment of some of the control variables but it appears to be giving more uniform conditions* Attached is a table giving the details on batches followed in the plant and semi-works during the month* i - chrpqfl ftranseg A* YQr37-p The two batches made were too light to be "OK Straight" and further variable changes must be made to get darker material* B* mrJl-S The single batch made was too dark* A further decrease in alkalinity will be made to obtain lighter material* C* I0=3L--P Five batches were made in the plant* The last three were "OK Straight" and one of the others was OK in depth but was too red* This redness is common to both Plant and Development controlled material and has been a chronic complaint on this orange for several years. It probably will be necessary to make a study of this some time in the near future. Another batch of orange was made in the semi-works on the Y0-260-D type formula using the reverse strike. The material was light and muddy against Y0-38-D. Although it is felt that the product could undoubtedly be improved by changes in formulation, no further work is planned for the present since the regular YO-38-D formula is showing an improved performance* DUP050150391 14 D. gQrlter-g She single batch made finished too light in masatone* Control variables will be applied on the next manufacture to give darker material* E. XQ=g63sB The single batch made was light in masstone as requested but was too dirty in tint for use in YQ-422-D. the purpose for which it was made. It was shaded without difficulty as Y0-263-D. II - Inactive. Still awaiting completion of batch size study. Ill - fi^aas-lflUgga She Research Laboratory has been able to develop a formula for making Y-49Q-D as a struck color* This is being turned over to the Development Section for further study* It is estimated that eliminating dry mixing on Y-49Q-D will result in a savings of approximately $1500 per year* IV - Miscellaneous A* Plant "OX Straight" performance for June has been calculated for each individual code* DUP050150392 CHBOME ORABGES JULY 1941cl net n H o H H O w tJ ct ^ PH W PfcPH S 2a1?K 1 B* 8 ain Sh P d o o H i~SX> bs U* o> HH PO P $4 oH do o pH Q) O WP 2M4wT o P% P P 03 0 P Pi H HO-Hfc uJOC0 sCOo Pi m Apt no o *o H mH WU P* P J?g d n H j Oo ofri PH P Pi o p P p j B to P P o r* tPg.CP0 <HMo p *trS-MP PH *a * H HO OP H TS P *d P P g. PP d OH vo0 \Q ^ \0vOv0 CM AS KS-P mCVmISm.ISPt pU VOX! VO N0 VO HP 00 *? CO 00 CO ht? sg P wC <Q w(0 o P HOP *d p oOd Pt p* s pdQXp3 m 0* d pw d<8n*ao < >p ^w H dOPo OP HP dH m 0**0 MO I O ro *pvo H CM 3 ' Pw A H_ CM d CM P H * AI H S8S Pi P > Po om v <mw w HP 4 P P *4 *-tQ P WP fn + 413 p. S> C9O 8<M a no PC I nCO 2 -nt p co o 2i S1 2 "1!4 2 mh IU HNOOWX3 > J6E0J-P p d So3 p p p w 00 s ca ca 43 a t: CO CO CO H to CO GO 1 CG CO CO I HH 4 M o #0 Ht H *d 9 % *o net I *4 * 'O kH w w S 5-8 m vmt is i p a <<> m H no H pp PHM * o HH <^f W p H dm no u *> tJ U v/ O ct)#ned0t Pi ^ m m 9 no **Q 4P M H w no ktM wp OO >H ccCaaO pto w > & H no i p p H H tH *o O P P H jet tA O O' vO c m mo o p NO OQ CO It s O cs. 00 SCOv NO CM ?8 00 00 CM CM VO 00 COCO OH NOV CVOO 00 CO CO nj- U> vO CO X Cl *? I -nr CM rO t II CO \oo CM t 8 s8 8 ON m vo co a i m no cm & .r DUP050150393 - 16 Supervision and control of the manufacture of lead liquor was continued during the month* Control of concentration and alkalinity was satisfactory. A detailed formula for the manufacture and control of the lead liquor process is being written preparatory to returning the supervision of this process to the Plant staff* Attached is a table summarizing the batches followed in the plant during the month* A detailed discussion of these batches is given below* X- A. 22=32=22 The adjustment of control variables to give OS Straight material was continued. The first two batchesf made on the same formulat checked each other quite closely but one was a little too dark to be OS Straight. The next two batches were made to be lighter but while they checked each other quite oloselyy one was a little too light to be OK Straight* The fifth batch which was made to be a little darker than the two previous batches was still a little too light to be OK Straight* Further changes will be made until OK Straight material is obtained* A performance study will then be run* B. XQ-34ri> Ho production. C. yQ-3QrI* A performance study was run during the month using the formula developed during July* The results indicate that several difficulties must be overcome before OK Straight material can be made consistently* They are* - 1* Bicarbonate of soda which has been stored for two-three weeks becomes hard* This gives a lumpy rtwhite base" and probably erratic results. 2his is the first time this trouble has been encountered and further investigation is necessary* 2. The chronic complaint of red and chrome mass tones was encountered* Several recent batches were satisfactory in depth of masstone but were too red and chromy* This problem has been studied in the laboratory several times during the past few years but little progress has been made in its solution. Since this problem is now on the plant "sick list" and since it must be overcome before OK Straight Y0-38-D can be made| it has been decided to study it in the OK Straight laboratory. Its successful solution will probably require a long and tedious study of the fundamentals involved in the manufacture of YO-38-D. DUP050150394 - 17 - 3* Two "off* batches were made during the performance study. Analyses are now being made on all the retained samples of raw materials, slurries, and backwaters to determine the cause. Pre liminary results indicate that the balance between the lead oxide and bicarbonate is close enough to the upset occasionally by a combination of variations in raw material analysest weights, etc. It is known that an unstable product will result if there is no soluble lead present at the "white base" stage. It has been decided to return this formula to the laboratory to determine definitely the causes of "off batches and to develop a more stable formula. Plant work on Y0-38-D will be discontinued until this work is complete. ---------------- YSs3fe.IL No production. e . Ya=afe8 The adjustment of control variables was continued from last month. The single hatch made was OK Straight. A performance study will now be run using this formula. II. g4Bfl.,MLWL Inactive. Plant OK Straight performance is very good. Develop ment of "HY-CAP" properties is awaiting completion of batch size study. HI* Chrome Yellows The Research Department is now actively engaged in the develop ment of a formula for .making Y-424-D, the duPont medium yellow, as a struck color. xv. %4gpq;HaMan& A. The Plant OK Straight performance by individual code for the first six months of 1941 is being Issued as a matter of general information. DUP050150395 960SK)S0dna Sfiflfi &S& Y0-27-D 87710 dk, red, vs tort; red, vs vk - __ -Cm0MS_ 0RMQES AUGUST 1941 Y0-263-D 88201 s red & tort; w s y e l * w s s tr ; OK Study o f c o n tro l vartables yel & s clean disposition SSS Study o f c o n tro l va ria b le . N0t0OO0000tOo00 -o0ooo0 _ &03occCmoO (Sttor*0 2 (cA+ O OSH 3 0 jfli Ow> ohi wf* o %0Otor ma eO#gO* hpt 9 CD *& OO00tO0J0sp00?, 03 ppH0r* 9 OC0O0sSHT* 00 ufv>>|*O0*O3td*k* whi 0X0T *j? 1arht>** c+ H08H* to cH* < CO wOn (ctot fMto ^a (*to << ** ** a 2 2M & I w3 Kj J VAI* TH3 3 cf cHo+1 rM01 3 00 & W 03 O 86 o* 00>k OKta** wt<!v+**chHpdjr S VCO? H ai.WgHi>f * IT O >000 I oo i ^- sv. .v Remarks W ithin 19 x - frsafl,,UaBSE Study of the lead liquor process has been completed, a process report written, and control of the process returned to the plant staff, the important changes introduced were: - 1* Use of standard batch cards giving detailed operating instructions* 2* Use of more efficient operating conditions* For example, it has been shown that one 1-hour run over the feathered lead gives satisfactory liquor, whereas two runs of 2-3 hours each were formerly used* 3* Conditions under which lead liquor is stable, does not precipitate on standing, have been determined and all liquors are being adjusted to these conditions* 4. Rapid control tests have been developed and are being used for the control of the lead liquor process* II - Chypmg..Qrjaagftg, A* SfislSsB Work on T0-38-D was confined to the laboratory* Two problems were studied during the month. They ares 1. Causes of flopping - Two definite causes of flopping have been found to date* Flopped batches in the plant are probably due to either or both of these conditions. The present formula will be revised, based on this knowledge, to give a more stable formula* 2. Causes of red-chromy masstones - The problem is being attacked from several angles* a. Laboratory study of stflke variables - Ho definite leads have been uncovered to date. b. Particle size, shape and composition - Samples of satisfactory material and red-chromy material have been sent to the Experimental Station for comparison under the electron microscope and a spectrocheaical analysis. e* Testing Method - All complaints to date have been based on rubout results. Paint grinds, etc., are being made to determine whether the redness and ehrominess is evident under actual conditions of usage. Preliminary results indicate that there is no correlation between rubout results and those obtained in other systems* DUP050150397 - 20 B. Two batches ware made In the plant. They were very close checks! one being "OX Straight" and the other a little too dark. A performance run will be made using this formula when production is resumed* III - UfiOlllfiXl The plant "OS Straight" performance continues satisfactory and no work is planned for the present. Iff - fifryoag XfiUflSS Work on the development of a formula for making Y-424-D, the duPont medium yellow, as a struck color, was continued in the Research Laboratory* The results, to date, have been rather erratlo. probably because of the difficulty of controlling the composition by precipitation methods* v - tylPccUaoaflM A. A process report for the control and manufacture of lead liquor has been written. B* The plant "OX Straight" performance by Individual code for the first six months of 1941 has been issued for the guidance of those Interested in the improvement of "OX Straight", DUP050150398 po o p .*&haOt -Hd3 P<p rQHJ J H**CCH<OP o Ho. JB P$2 ut a &1 0oO0*,P23<CO0 <ompa HO 5 si mP fcuO Pco 60 oH pu pa SQ t Prl CO OP 1O4 co 5 H CM 3 o so C i H MmMpIIHI & 10 CO o >CO *C3D CO CO ** |U H 0) 0 JB * MxCOt**mUP** 1UMt* 34 CO CM t x^S m$ Saji <oXo> a <& *C pN 080* 00 DUP050150399 22 - The other r,0K Straight" work was interrupted early in the month in order to give full time to checking the lead nitrate operation* Chrome Yellows made from lead nitrate have been running too dark and dirty in masstone and it was felt that this was due for the most part to the lead nitrate* I - LeM-Iitratfl As a matter of record and in order to avoid their reoccurrence, a detailed discussion of conditions which were responsible for the poor grade of lead nitrate being made are listed below* Recommen dations are also included for further improving the lead nitrate operation* 1* A brown sludge which has been shown to give dark and dirty yellows was found in all tke lead nitrate storage tanks. The tanks have been cleaned and are to be cleaned on schedule in the future* 2* The electric eye which is the sole guard against the brown sludge leaking into the storage tanks was in such poor mechanical con dition that it was useless as a protective device* A new lamp is to be installed and the system rearranged. The electric eye should be scheduled for inspection at least once a month in the future. 3* The pump switch which is normally actuated by the electric eye was too rusty for automatic operation. This has been remedied. 4. Assuming the electric eye to have been in good condition, it would not have been possible to utilise it for control purposes because of the following conditions* - a. One of the glasses in the trough was broken* It is being replaced* b. Too much wood fibre suspended in the solution* The press is in very poor condition. New plates are being made. These should be painted with a protective material to increase their life. o. Too much entrained air in the solution* This was due to the pump needing packing and the poor condition of the press and accessories. The pump has been packed, the press is being re conditioned, and small changes have been made in the pressing procedure. A screen has also been installed in the trough to break up the air bubbles and eliminate the wood fibre* d. Too many lead nitrate crystals entrained in the solution. Conditions under which lead nitrate solutions are stable are being determined and all lead nitrate will be adjusted to these conditions. DUP050150400 - 23 5. The test for iron under the present conditions was found to he worthless due to the relatively large amount of nitrite present in the lead nitrate. A new test is being developed. 6. In general, the operation was sloppy and important differ ences existed in the methods used by the three operators. The operators are being instructed and trained as the work progresses. The following suggestions are offered as a means of further improving the lead nitrate operations - 1. Increase the lead nitrate concentration to an average of 22$. It has been running 18-19# for some time. This is now being studied. 2. Improve the agitation in the purification tank. The poor agitation increases the time of purification and adjustment, and leads to lower lead yields and non-uniformity of reaction. 3* The present press pump has too much capacity for the present system, resulting in leaks in the press, blowing air, and higher maintenance and power costs. A slower speed motor on the pump would lead to more efficient operation. 4. Lack of storage capacity results in hurried operation during peak production periods. This has been exaggerated by the recent Increase in batch sise on lead nitrate colors. Hurried operation is resulting in sloppy operation and poorer quality lead nitrate. Con* sideration should be given to installing another storage tank in the rear of #18 Building and larger scale tanks in #6 Building. It should be possible to use wooden tanks for this purpose. 5. As a check on the lead nitrate operation a continuous sampler should be installed on the line from the clarification press. 6. The present method of adding nitric acid for adjustment purposes should be eliminated due to the hazard involved and higher maintenance costs. ii - ksafl.Ua.uai The quality and control of the lead liquor operation continues satisfactory. h i - ctaoBW,.fiyangfl,a- 22=2Z=e_ Two bbeatches were made for the purpose of studying control variables. Both were a little too dark to be "OK Straight" but were readily ehadeable. B. Y0-38-D A single batch was made to try a new and more stable formula. It was too light and it will be necessary to apply known variables to give darker material. DUP050150401 CHROME ORAMSES OCTOBER 1941- D1bp o s it ion. Code Batch Raboat J tg ia s & l o P w, H,0-HH 961 * s!-* H t3 P85r3' _PW VOi <0 g,-Sw P CO 3coc3o CO 1 * w *** p*d &F 0 k W CO P . U*i MM *0*0 m t P w > k H >* r*l a P rl lf\^ MH Os0v coco a IS CM 1 O * <* cs CO co m i p H DUP050150402 Full tine was given to improving the lead nitrate operation and process. Except for occasional batches, the lead nitrate was satisfactory throughout the month. Elimination of the poor batches and a further general improvement depends primarily on the comple tion of pending equipment changes; The Improvement in lead nitrate quality to date has resulted in much less dark - dirty masstone chrome yellow being made. A brief discussion of the status of the lead nitrate work is given belowi 1. The storage tanks were cleaned during the month. The storage tanks are being cleaned once per month and the scale tanks once per week. 2. The electric eye has been mounted on a permanent base so that it is not affected by vibrations, spillage, and condensation. The old lamp should be replaced and the cover to the lamp and eye locked to prevent tampering. 1 *4 3. The rheostat which controls the eye has been locked to prevent tampering. The present ammeter is to be replaced as it is in need of repairs. When this replacement is made it will be possible *to calibrate C te|*e system go that its efficiency can be checked at any future date. 4. There are ten bad plates in the press. An order has been issued for replacements. 5* The majority of the spigots and hose on the press are worn out. Replacements are on order. 6. The agitation on the purification tank is unsatisfactory. A project has been written to install a larger agitator. 7. The press pump is too large for the present system. The Mechanical Department is trying to locate a slower speed motor for this work. 8* The Industrial Engineers have installed a temperature recorder on the make tank. This will provide a much needed means of control for this operation. 9* A project Is being prepared to install a small pump for use in adjusting the lead nitrate. 10. The lights in #19 Building have been moved so that the spigots and trough can be observed during the night shift. A study is being made for the purpose of providing sufficient light for operation at night. DUP050150403 XI. Consideration Is being given to Installing a continuous sampler on lead nitrate. This would provide a much needed check on the lead nitrate operation. 12. Operating instructions covering the lead nitrate process have been written and posted in the leadshop and #19 Building for the guidance of the operators. 13* A new test for iron has been developed and is now on trial in the plant. 14. Corrosion tests are being run to determine the effect of lead nitrate on iron pipe. The new test for iron is also being used to determine the iron pick-up in the present system. 15* For the present, all lead nitrate is being adjusted to approximately pH 4.0. This appears to prevent the formation of crystals and yet is not aeid enough to attack the iron piping. DUP050150404 - 26 - sasama...im. The lead nitrate operation was checked throughout the month. Although there were several periods of poor quality, in general, the quality of lead nitrate showed an improvement over last month. These ttoffH periods are due to our inability to control the pH of the lead nitrate with the present equipment and methods. The possibility of adapting conductivity equipment from the llthopone plant to the measurement of pH is being investigated. The new iron test which has been on trial during the past month appears to be satisfactory. The test is also proving valuable in the study of corrosion and iron pick-up in various parts of the system. Preliminary results indicate that the pH in the storage tank must be kept above 3*5 to avoid contamination with iron while pumping to the soale tanks in #6 Building. A new lamp and micro-ammeter have recently been Installed in the electric eye circuit. These are now being calibrated so that the efficiency of the system can be checked in the future. After a trial period an inspection schedule will be set up. Several tests have shown that the eye is working satisfactorily and that no solids are passing into the storage tanks. Chrome Yellows have been made in the laboratory from plant lead nitrate containing iron to determine the maximum amount of iron which can be tolerated under present conditions. Preliminary results indicate that the plant is now operating below the maximum amount of iron which can be tolerated, whereas several months ago they fre quently were above the maximum. Several batches of lead nitrate whioh were made on standard formula were followed. When the Industrial Engineers complete their study on nitric acid yidlds, the making operation will be studied further with the object of shortening and improving the control of this operation. DUP050150405 - 27 - She lead nitrate operation was checked throughout the month. Daily samples of the finished liquor Indicated that, except for one day, the lead nitrate was satisfactory. She one exception was due to the mechanical failure of an acid valve. Very little dark and dirty masstone chrome yellow was made as a result of the improved performance on lead nitrate. All of the recommended equipment repairs and Improvements, except the installation of a pH electrometer and continuous sampler, have been made. The equipment is now in excellent condition and little trouble is to be expected in this respect in the future. Consideration is still being given to the purchase of a pH elec trometer and the installation of a continuous sampler. A detailed study of the lead nitrate purification process has been emmplsted and, except for pH control, the methods are now satisfactory. The only dependable method found for the control of pH Is the electrometer. The electric eye has baen calibrated and a method set up for checking its operating efficiency. It is recommended that it be checked at 30 day intervals in the future* At the Plant's request samples of finished lead nitrate were taken throughout the month for the purpose of determining the average nitrite content. A SCR method for the determination of nitrite has been developed and will be used in determining the nitrite content of these samples. A trial run was made at the Plant's request to determine whether it is possible to eliminate the purification step by consuming the lead sludges at rates low enough to keep the Impurities within specifications. Preliminary results indicate that satisfactory lead nitrate can be made in this manner if close supervision is provided. The process has certain weaknesses and it is felt that there may be more desirable means of accomplishing the same purpose. These have been fully discussed under separate cover. As of January 12, 1942 the plant has been using, without research supervision, the Chrome Orange formulas developed during the "OK Straight" study. These formulas specify volumes, times, temperatures, pH, etc., which normally are not controlled. At this time, the results are too few to justify any conclusions. It is planned to give a few days to checking the operation on these formulas during the coming month. DUP050150406 FBBfi9AftX.JS3a - 28 Daily tests made on the finished lead nitrate liquor indicate that it was satisfactory for use in the manufacture of colors* She quality of Chrome Yellows made during the month confirm these tests* A study of the lead nitrate making operation was carried out during the month. A detailed operating procedure has been written, based on this study, and is now on trial in the plant* A trial run has been in progress for the past three weeks to determine whether It is feasible to manufacture satisfactory lead nitrate without purifying and without clarifying in the filter press* During this period pig lead has been the sole source of lead and the liquor has been clarified by settling. The results to date Indicate that satisfactory lead nitrate can be made In this manner provided the following conditions are mett * 1. Pig lead continues to meet specifications. 2. Each batch of lead nitrate is completely finished (pH 4.4) before pumping from make tank. 3 The pH is adjusted within the range 38 - 4*2 before settling. 4. The settling period is held to a minimum of 30 minutes. 5* The tank cleaning schedule, recommendations to be made later, is adhered to rigidly. 6. Close supervision is provided - much more than at present* S.toffs.,graM3g The "OK Straight" study on Chrome Oranges was resumed on January 28, 1942* This study was Interrupted several months ago because of the variable character of the lead liquor. This is the first work on Chrome Oranges since the difficulties on lead liquor were eliminated. During the period January 12 ~ 28th, the "OK Straight" Chrome Orange formulas were used in the plant without supervision by the Development Section. Attached is a table showing the results on all the batches made on these formulas. Batches marked with an asterisk were not followed by the Development Section* A brief discussion of the performance of each Orange is given below. I9.z27.zV This formula appears, except possibly for a few minor adjust ments, to be satisfactory. All the batches made under the Develop ment Section's supervision were "OK Straight" and six of the last eight batches were "OK". The cause of the poor performance at the beginning was located and has now been eliminated. DUP050150407 - 29 0=Mr-B. This formula now appears to be satisfactory - four of the last five batches were "OK Straight"* This formula is still unsatisfactory and has been returned to the laboratory for further study. The plant is also having trouble controlling the regular formula at this time. Apparently there is still some unknown variable in this formula which must be located before consistent results are obtained. Occasional batches will be made in the plant as a cheek on the laboratory work. Y0-26Q-D There was only one batch made. Additional experience will be needed before drawing any conclusions concerning this formula. Although two of the four batches made appear to be "OK Straight" versus the regular standard, the results are too few to justify any conclusions at this time. DUP050150408 p MS P laJS 08P H fid P P "3 MB O. V *o* a*s no o a. a & 15 no 2 >H r"i M. *** AH 5P * J*4*CM VO 43 t 40 40 40 40 14 Pi ? *8 ** *4 tftfH ** SR**" 1^* IO PM* 00 p o #* 0 P 14P HVi P14 j m$ P HP *> rH P H J> w w p P >> a r *o * H 43 +> +>++> lw >k iQ %%% OQ m HJ tn > y~% #(h-p /^l ^N/%*0 r*"S, Mr a lu d o*d r-%43 fe* Ov 14 Hw*4v**4W fU w14 P |>HP N44 434Hw X 43M jM-O * 01 *0 + > p g F g rt > H > > J> 5 00 O P H 43 C0 H S?S P gg H00 O 43 H *D 0) rl g?fe OCt &< 3S 3s 1O4 H00 $4H H i*4S00 CH fe<H *1 14 40 H P*- V ** >0 H 4134 t 8 _SR f H 00 4O3 40 pH cu C-P g g rH 14 &M 14 14 O Pti* H O 8. P P 2 5. *8 O ej ^4 fr + EM O I# 1 H X 1 1 n_o P.g.g .% 2 Vgssss DPbwTuCJ<u0<tO0ux4h +**n O,*# <f*n a *-SPj -fPe *o >o<p,o<a g> (p ijhs n co * 43** n<o *40***0*43JWw* *<*ftnXo U 14 M*0 m fg) ROff*"4 14 t 43 * * M0 Hogt o 'g 1 a 2 H&* rH 4 N > *&o P jj P14*0 43 * XI 14 40 14X1 eg 14 M 4H M 40 J HT1 ^1 P ,* ,,_ . O O rH | H <B SSHgU ^ OO P - & ^ b r.`oWHHoO s&s fR-S \ a * v0 t3 O H<Q h w *H gjQ wH OX O >1**^ O P P no40 *** 14 14 !-4f>lj PrVHiVHf fl ^ H *H > J>VVl W W P H mmmmm* X JH43P43P *a no pH pH pH H l * 8 *a 14 4* P Ja 2 40 2 M no CCOQMC0O0 COOOMMCOOM^MoS0Q0< CO O CQ CQOOGOOOOCQO Wc5i o COi CO is *4 *4*$ oo o is C * JS CQ ## ^ cs.cn 0O0 0O0 0N0 p0HS pOHsOrHv N O# *H ^ OvCMO*vOnt ?? Cvio^SUrvJo Hcsc(MscOsI oCMvc<Mso(MvcCMsaO^loCMv N CM On CO OrH^OCMVOCMSCCMSOCM^CCMS Pi I fr m t 8 JfOSWISNOrvosmo UMrwO Cv OH0N osON ### H 0>0 O rH tN4f CsH CVvO vO CM IN cooomm^r\r\ HOI CM OJ CM CM CM Ov 0h OV Os CS Ov 0v 5 m CM Os H CM Os 5 O SO CM I 8 BiteBas&Ma DUP050150409 CHROME ORAHGES FEBRUARY iqa2 Contd.- Code Batch P isposition Results Y0-263-D 91835* (SSS) red & b rt; s red, vs wk - s tr j s clam Remarks Made fo r Y0-422-D "OK S tra ig h t11 vs regular Std |L| |L w +* m IQ m H' ' H r >> b ** .Q ^ (Q as o >p ii u h Vi IQ > ^ *> -M 4*j H Wrl coca co co coco CO CO CO ** U\mH UNlTNOO CNHCV rlCVIW On On ON "8 m >0 rl <0 u Q*P CO P gw 00 .a* a 4* o 4jl g-r* ow P > 8*9 ^ 8t 32" 1SISs a O *H Vf P O # 0 Q) PXjCO XI p <UH Q * . co o >*>|H Udi ?a% O > fH * *g tgj dad3 s . wd p *OH Hd :04)| d O Pi O 0 09 V DUP050150410 32 MARCH/APRIL, 1942 - He reports) m.im, c,toQigfi..Qy.,aagag_ There was no production on Chrome Oranges during the month* When manufacture is resumed the *'0K Straight" formulas will he used on all Orahges* QhyQfff ,TtUqL, A general survey of the Chrome Yellow equipment and operation has been made* This was followed hy a more detailed study of raw materials and the various operations Involved in the delivery of the proper amount of raw material to the strike vat. A brief discussion of the raw materials investigated and the equipment used in handling them is given below* - gfarmata... analyses - satisfactory uniformity - samples taken from hose to strike vat check those taken from storage tank* alkalinity - varies considerably but majority of formulas now require adjustment before use* $odiqm SlQfeEfiialg, analyses - satisfactory uniformity- '* acidity " ffl.tr 3.ti& analyses uniformity acidity impurities in general good, but several found outside limits* satisfactory at times varies considerably contained too much iron three of the eleven days checked* analyses - satisfactory uniformity - satisfactory impurities - suggest that brown sludge in storage tanks be removed* DUP050150411 - 33 uniformity - contains too many large lumps weights - bag weights are incorrect - should always be weighed* g,,aXfta,.fli^.,,laJlgb.lag Scale Vat #359 - used in weighing sodium molybdate solution* Found to be in good condition* Soale Vat #351 - used to weigh chromate, acids, alum, etc* Found to be in good condition* Scale Vat #356 - an alternate for #351* Sot satisfactory for use on Molybdate Orange, possibly satisfactory for Yellows* Location of beam relative to solution valves contributes to inaccuracies. Scale Vat #354 - used for weighing lead nitrate solution* Inherently a good scale but now sluggish and tends to stick, requiring considerable care in its use. Beam not visible from control value* In weighing it should be made a general practice to balance and read the scale Just before drawing solutions* Several instances were found where the weighing was done some time previous to withdrawing solution and examination before withdrawal showed that the weight had changed* Leaking valves usually are the cause of such changes* During the course of the general survey several conditions were encountered which should be corrected* They are* - 1. Several of the agitator turbines are so badly worn that little or no agitation is supplied in the upper portion of the vat* 2* The practice of re-using paper sample cups should be discontinued. A sample of lead liquor taken in one of these cups showed 7*2 pH whereas checks in glass ran 9*15 pH which is normal for lead liquor* 3* On several occasions it was found that either the late maker or the nightman had not washed out equipment and hose sufficiently* As an example, a sample of water taken from the hose to Vat #351 contained a white sediment and its pH was 10.7. This solution would normally go into Molybdate Orange which is quite sensitive* Work to date has been confined to the making operation. The treating (nightman), pressing, drying and grinding operations are still to be studied* DUP050150412 Experimental work la recorded In Laboratory Notebooks 884 and 932* and DSN 46-26, / DUP050150413