Document NGBBQD6doGQ8wgpeOV9wVm56w

Mr. W. R. Tome DECEMBER, 1967 RESEARCH REPORT GLIDDEN - DURKEE DIV. S.C.M. CONFIDENTIAL A GLD 045548 C & R RESEARCH CENTER RESEARCH REPORT December, 19^7 TABLE OF CONTENTS TRADE MAINTENANCE Exposure Reports. ..................................................................................... . Fillers - Mastics ................................................ .......... High Body Paints............................................................................................... Latex Paints - Exterior . ........................................................................ Latex Paints - Interior ............................. ........... Miscellaneous..................................... Solvent Reduced - Trade Products................................ M-l Trade Maintenance ..................................................................................... M-2 Industrial............................ Page TM-1 TM-2 TM-3 TM-6 TM-13 TM-17 TM-24 TM-^5 TM-47 INDUSTRIAL IRODUCTS Industrial Can Coating. .................. Industrial Litho Coating ............ ................... Industrial Wood Coating ........................................................ . Industrial Automotive...................................................................... Industrial Electrocoat Formulation and Demonstration. ... Industrial Electrocoating Laboratory. ........... 1-1 1-3 1-6 1-9 1-12 1-15 COATINGS RESEARCH CR-1 POLYMER & PLASTICS (RESINS) Vehicles for Air Dry Coatings . . .......................................... Comparison of Igepal CA-63O vs. Triton X-100....................... . p-i p-2 ANALYTICAL Analyses. ............... ...................................... . NUBIAN DIVISION ............................................................................................................ a -1 N-l GLD 045549 TM-1 TRADE-MAINTENANCE EXPOSURE REPORTS December 1967 SUBJECT Accelerated Testing RS9/000T4U54 KS9S000M1J-54 RS9700IT5054 RS9500el2111 RS9700219054 RS95004I5114 RS97003I6026 RS95006P1101 RS9500714108 CONTRIBUTORS: K. Kramer, H. Lawson SUMMARY Exposures - Exterior Cleveland - 19 series of new exposures - 147 panels. Sub-Tropical - 22 series of new exposures - 101 panels. New Orleans - 2 series of new exposures - 12 panels. Baltimore - 1 series of new exposures - 7 panels. *> Minneapolis - 2 series of new exposures - 12 panels. G.T.M.G.'s Nothing new to report. Weatherometer The weatherometer back-log is remaining steady at 35 panels. Fadeometer The Fadeometer is once again in operation. Salt-Sprays & immersion Tanks Nothing new to report. Demineralizer The Demineralizer is operating to specification with two week intervals between regenerations. GLD 045550 TM-2 TRADE-MAINTENANCE FILLERS - MASTICS December 1968 SUBJECT: Y-5317 Improvement NT23021T3266 CONTRIBUTOR: H. Sheets SUMMARY: This work was started to determine if K-1666 can be replaced by RCR-0108 in the Y-5317 formula. When the K-1666 is replaced on an equal solids basis with RCR-0108 the block filler is too heavy in viscosity and does not level. A reformulation using 20% AC-61 and 80% RCR-0108 gives a 104 KU viscosit and good leveling, but the filler does not have enough body under the brush and tends to brush out too thin. When the filler dries it leaves holes in the block. A formulation was made using 52.8 lbs. of Alsibronz mica per 100 gallons of filler. The N-356 silica was cut on equal volume as the Alsibronz wa added. The Alsibronz was added at th end of the grind and required the addition of some of the AC-61 to get all the mica ground in. The resulting block filler was very thixotropic, filled and leveled quite well, and had a viscosity of 114 KU. After one week at room temperature the viscosity is 116 KU. The filler brushes quite well and does not shrink or develop holes on drying. The filler dries to a relatively hard finish. Water soak and tests for topcoat hold-out will be run. GLD 045551 TM-3 TRADE-MAINTENANCE HIGH BODY PAINTS December 1967 St t o .t e c t * Develop Hi-Gel Thixotropic Water Paints With Application Properties Of Regular Paints. CONTRIBUTORS: V. A. Donegan, H. J. Kreinheder, G. Sweitzer NT26011T3163 NT23029T3263 NT27000T3263 SUMMARY: Reformulation of Ultra Flat continued. Pigment studies for improved uniformity and lap sheen were evaluated. K-1666 from Reading using igepal CA-630 was evaluated versus Cleveland plant K-1666. Only scrub resistance was poorer. Nuvis 44-W, a thickener was tested for improving color acceptance in the revision of Ultra Flat. No improvement was noted. Deefo 97-2 defoamer was evaluated in Y-5118-F as a replacement for E-624 The 97-2 defoamer was poorer than E-624. Painter Latex Paint is being reformulated to use K-7255. Besides chang ing vehicles the product is to be upgraded. An increase of 5 per gallon in latex presents excellent scrub resistance compared to the current Y-5370-J. Equivalent hiding was obtained using Zopaque R-77-S, calcium carbonate, talp, and clay. Brushing properties were poorer than those of Y-5370-J, but acceptable. The best combination of brushability and flow was obtained with a small addition of Kelzan. DISCUSSION: Work continued on the K-7255 revision of Ultra-Flat. A slight lap sheen has been noticed with application over bare Upson board, and a tendency for non-uniformity in the brush tracks. In an effort to improve the uniform, replacement of N--356, (amorphorus silica) with Min U. Sil of several sizes (10, 15 and 30 Micron) was studied. Difficult brushing was encountered with the 10 and 15 micron materials. Uniformity and lap sheen were improved with the 30 micron Min U. Sil compared to a control with N-356. To further study lap sheen a factorial design experiment with five factors was used. Factors studied were P.V.C. - (57-62), thickener type - (cellosize versus Methocel), thickener level - (3# versus 6#), glycol addition for hold-open time -(2800A versus a normal batch of K-7255 at 5500A). The 2800A batch was prepared on the K-7255 formula for use in this experiment. The test paints were shaded a medium blue with Dramatone and applied by brush in a 2-1/2 to 3 inch strip around the edges of a one foot GLD 045552 TM-4 square section of bare Upson board. After drying the center section was rolled with a Dynel roller overlapping the brushed section one inch. Evaluation of the panels and analysis of the data shows no one single factor, other than viscosity (high thickener level) to be significant. Best results were obtained by several factors interacting; they are ceiiosize at the higher level, wirft giycoi and the smaller particle size latex. Further evaluation and study will follow. A special batch of K-1666, P-617331, from Reading using igepal CA-630 in place of Alipal CO-436 was evaluated in Y-5118-F. Room temperature roll, and 140 F. oven stability were equal to, or better than a control using Cleveland plant K-1666. The Cleveland plant material had poorer than normal mechanical stability, coagulating after 4 days roll. A normal batch shows no coagulation after 7 days roll. Color roll stability with the special K-1666 was slightly poorer than the control, showing slight color flocculation between 4 and 7 days roll. Scrub resistance of the "special" was lower than the control at 7 days air dry. Merest Chart Unsealed Japalac Control Special 268 130 245 160 101 84 Results are in double strokes. Further testing for storage stability will follow. Nuvis 44-W, a polysaccharide thickener from Nuodex was evaluated in the K-7255 version of Ultra Flat without RCR-2102. Nuodex claims improved color acceptance and color stability with this material compared to Ceiiosize or Methocel. Rub-up and color roll tests failed to show any improvement over Ceiiosize in the K-7255 Ultra Flat formula. Deefo 97-2 defoamer was evaluated in Y-5118-F as a replacement for E-624. Evaluation was on a pound-for-poursd substitution and at a 3/4 replacement level. Defoamer activity was tested at overnight, 4 days and 7 days storage in a 140" F. oven. Deefo 97-2 defoamer was poorer than E-624 initially and after aging at both levels of substitution, A complete reformulation of Y-5370-J, Painter Latex, is in process in order to upgrade the current product and to incorporate K-7255 as the vehicle. Reformulation occurred initially at an equal PVC of 69.0%. A formula with K-7255 having 10 pounds per 100 gallons of a permanent plasticizer, Eastman 135 and 25 pounds per 100 gallons of BCA gives quite good film formation GLD 045553 TM-5 at 50" F. as Shown by color difference testing. Alipal CO-436 gives the system good stability and adequate color acceptance as initially investigated. The addition of 54.4 pounds per 100 gallons, or 5d per gallon, of K-7255, lowering tne i'-C to 63.4%, gives increased scrubability. Over 500 double scrubs over a Morest Chart and 200 double scrubs over Japaiac are obtained after seven days of drying at room tempera ture. After an eqjivalent dry time Y-5370-J gives 150 strokes over a Morest Chart and 150 over dapalac. The scrub data for the K-7255 paint is quite reproducible. Y-5370-J, however, does not always exhibit the same data as quite low values have been observed. In order to obtain hiding equivalent to Y-5370-J, several extender systems were employed with Zopaqqe R-55, W-755. The addition of Nytal 300 in replacement of CaCC^ produced no increase in hiding. The pigmentation of Y^537QWr involving Mineralite Mica 3X and Hydrite MP showed better hide, however, brushability was sacrificed when used with K-7255. Zopaque R-77-S was introduced to give greater hide. Since enamel hold-out is not a prime prerequisite, the low hold-out characteristics of R-77-S were not considered. R-77-S in combination with Nytal 300, CaCOo, and Al-Sil-Ate, W, clay, was found to give equivalent hide to Y-53/0-J when tinted to the same color. This was determined by light scattering techniques. Brushability is not adequate with the aforementioned pigmentation system. In order to upgrade the brushing characteristics, the HEC level was decreased and various levels of Kelzan were studied. Results show that 1 pound per 100 gallons of Kelzan and 5 pounds per 100 gallons of HEC gives adequate brushing qualities while sacrificing very little in flow and leveling. The most recent formulation will be examined for color and viscosity stability. v. GLD 045554 TM-6 TRADE-MAINTENANCE LATEX PAINT - EXTERIOR December 1967 SUBJECT: EXTERIOR LATEX CURRENT PROBLEMS ill XZ BUZ CONTRIBUTORS: J. Patrick, N. Petro, W. Kirkpatrick, G. E. Pekarek SUMMARY: Water Leachable Staining (Water Spotting) The brown water spotting problem associated with Y-3600-T Spred House Paint has been found to be due to the V-2197 long oil linseed alkyd modifier. Five new Glidden alkyds are being examined as possible replacements for the V-2197. Water spot tests indicated that Y-3600-T based on RE-22484, RE-22485, RE-22486 (safflower aIkyds) and RE-22487, RE-22488 (tall oil alkyds) did not exhibit the typical brown staining associated with V-2197 based Y-3600-T. Water immersion tests on Y-3600-T formulations, based on the subject alkyds, indicate that the tall oil alkyd RE-22488, based system, has the best water resistance. The other alkyd modified systems were judged equivalent to the V-2197 based 3600-T. A test was also min to establish the early wash off resistance of the subject coatings. The coatings were applied at ambient temperature and allowed to air dry for 40 mintues. The coatings were then subjected to a jet spray of water played continuously across the surface of the coatings for 5 minutes. The control (based on V-2197) started to wash Off first, followed by RE-22488, RE-22485, and RE-22486, in that order. RE-22484 (safflower) and RE-22487 (tall oil) based Y--3600--T were not included in this test. These were rejected because of poor roll stability. A repeat of the water spray test allowing an additional 15 minute air dry resulted in the same order of failure. Thirty day viscosity stability of 3600-T based on the subject alkyds has been determined at room temperature, 120 F., and at 140 F. These data are summarized in Figures 1-3. Room temperature storage for 30 days indicates that the control 3600-T based on V-2197 exhibits the best stability. The stability behavior at 120 F. and 140 F. is best illustrated by examining Figures 2 and 3. In general the viscosity stability of the V-2197 control at the elevated temperatures was comparable to or fell intermediate between the other alkyd modified 3600-T systems. Exposure tests were initiated for all the subject alkyds at 1/3 and 2/3 alkyd modification levels. (Reference: 7-313, 7-314, 7-345, 7-346, 7-315, N7-315). GLD 045555 TM-7 Stability of tne alkyd modified 3600-*'? may be related to the degree ar.d ease of emu's iiflcat icr. of the alkyd modifier. A phase separation idy of ur,pigmented batches (all ingredients of 3fe>u0--T minus pigments) was made at alkyd concentrations ranging from j00% alkyd tp 30% alkyd <2 si..vg. . -X 7 re. tr a! AE~2^.43d ' all oil alkyd). Tha L00% alkyd sy *? ems s:io.v ` ilt -e or cr.asa aeparato.cn on standing. As latex 'AC-34) is introduced (9Ofi alkyd, 80%, etc.) the - -ye break occurs. V--2! 4 snows pnase separation tnlougnout tne enure range or concentra tions studied (9iv>4 alkyd through 30%). RE-22488 ftall oil alkyd) also shows a phase separation frbm 9CA tp 40)4 alkyd, but the rate of separa tion is slower. The 30% alkyd, 70/4 latex based on RE-22488 shows little or no phase separation. SVJ?.7E0T i Exterior Latex Product, improvement 11 2 3 v 2 IT 5 21 i SUMMARY: The film bu i id, hiding, arid lap sheen characteristics of Y-36QQ-T Spred House Paint need improvement to increase the market penetration of this product. The following studies have been initiated to improve these properties: 1. High Solids Spred House Paint 2. Thixotropic Spred House Paint ,3. Factorial Experiment - Five Factors at two levels. (1) High Solids Spred House Paint - Y-3600-T Type Four paints have beer, prepared at. incremental solids increases corresponding to a cost increase of 5, 10, 15, and 20b per gallon. Each nickel increase corresponds to a volume solids increase of about w.5 gallons.- The pigment volume concentration was maintained at 30% by adjusting the inert level .'IVeosil k). Evaluation tests are now underway. Reference: {J1431-9C-1, 91-i., 98, 93) (2) Thixotropic Spred House Paint The following grinds have been submitted to Mr. V* Donegan for development of thixotropic house paints based or Tyzor/Kelzan: a) Y-3600-T with reduced Cellosize content. b) Y-3600 based on Strodex/calgon surfactants. Preliminary results indicated that a low degree of thixotropy was induced. These studies are continuing. Reference: (1431-89-1, 1431.-98) GLD 045556 tU K w r y c tf u '-k !2r>/i,7- a TM-8 12/'/ / 7 TM-9 * /g ///J /? // />/<? /? /#/'? ?* 2! 22 21 2f 2rj- 2/ ' /J/3A TM-11 (3) Factorial Design A 25 factorial design has been set up and a series of paints are being prepared. The variables included in the study are: 1. Alkyd type: V-2197 (linseed oil alkyd) RE-22488 (tall oil alkyd) 2. Alkyd concentration: 66.6%, 30% (binder basis) 3. Thickener level: 4.5, 6.0, lbs./gal. 4. Process variable: Alkyd in grind. Alkyd in letdown. 5. Titanium Dioxide level: Standard 0.75 lbs./gal. increase Primary emphasis is being placed on the effects of these variables and their interactions on lap sheen, hide, film build, flow and leveling. SUBJECT: Craftsman Light Tint Base SUMMARY: Eleven Dramatone colors were evaluated for weatherometer fading in two Craftsman tint base formulations;(1 oz. and 4 oz. per gallon). 1. 40% PVC - zinc oxide 75#, TiC>2 165#, Camel White 149#, Binder 1/3 alkyd. 2. 40% PVC - Ti02 175#, Camel White 178#, Binder 1/3 alkyd. After 300 hours exposure the two formulations were judged to be equiva lent. Y-3625 (Gray and Phthalo Green) shows slightly better fade resistance. The following tints were rejected for severe fading after 300 hours Weatherometer exposure: Light Yellow (Hansa), Yellow Green, Orange and Fast Red. The following colors were returned for additional exposure: Violet, Red Oxide, Phthalo Blue, Phthalo Green, Yellow Oxide, Neutral Toner, and Gray. One month package stability tests have been completed on the /tint base formulations. Reference: (W7-394-1) GLD 045560 TM-12 SUBJECT: Complaint Problems HT23027T3154 SUMMARY: San Francisco reported that a batch of 3600-T (34696EG) was returned in a "kicked out state" from Portland and that a batch of Y-3625 (34696EG) was suspect as a potential problem batch. 1) Y-3600-T - The condition of the "kicked out" batch was duplicated by freezing a control batch. Raw materials and maniafacturing procedures are being examined as other possible problem sources. 2) Y-3625 - Quality control tests indicate that this batch is satisfactory in all respects except for viscosity which is below specification. SUBJECT: SUMMARY: Miscellaneous Evaluations 1) Ultra-Adhesive's Deefo 97-2 defoamer was evaluated in Y-3625 and found to be inferior to Defoamer 357# our standard defoamer. 2) Color Corporation's irgazin Violet and 414 Yellow are being evaluated versus Dramatone Violet and Lemon Yellow for Wea^herometer fade resistance in Y-3625. Reference: (W7-413) GLD 045561 TM-13 TRADE-MAINTENANCE LATEX PAINT - INTERIOR December 1967 SUBJECT: New Spred Satin Formulations & Development j n T230j . 7T326J CONTRIBUTORS: R. Ashcroft, M. Cammarato, R. Kreider SUMMARY: 1) Three different samples of Methocel 15000, 90 HGDG were evaluated for the purpose of establishing raw material specifications on the seed content. Although the wet films showed different levels of seed content when filmed from a 2% solution, on drying the seeds could not be visually detected. Paints prepared using these 2% solutions showed the presence of seeds before film drying. After drying, however, tlie seeds left minute holes in the film which reached to the substrate in some cases. 2) Two water dispersed organic red colorants from Hilton Davis were evaluated as possible alternates in Y-3484 Cherry Red. The Toluidine Red cblorant appears to disperse readily but does not have the proper tone and cast to be usable for matching the Y-3484 chip. The Second sample was based on Naphthol Red and, therefore was no match for the presently used toluidine red. In addition the Naphthol Red colorant caused the paint to coagulate on short term aging. 3) The Architectural White (Y-3403) formula was re adjusted to meet the viscosity specification of 85-90 KU. The original formula produced a final paint viscosity of 95-100 KU after viscosity adjustment with water. A reduction in Methocel 15000 90 HGDG was required. 4) A Reading produced batch of Y-3454, P-264 (Green Ice) was sent to the Spred Satin Laboratory from the Quality Control Laboratory for evaluation. This batch was out of specification. 5) Nine defoamers were evaluated for effectiveness in the new Spred Satin. Included in the series was Nalco 121 and Drew 9135X which are; coded under the same code number E-624. Nalco 121 was found to be markedly inferior to Drew 913SX. It was recommended that a separate code number be issued to Nalco 121 and that it should not be used in new Satin. 6) During the month of December 1967 the formulations for new Spred Satin produced in the pebble mill and Cowles mill were re-written to include the manufacturing changes found successful in the regions. These formulas now include the up-to-date raw material costs as requested. GLD 045562 TM-14 DISCUSSION: I) Evaluation of Methocei for Seed Content The purpose in carrying out this work was to determine the effect of large amounts of seeds on new,Spied Satin films. To do this work the Dow Chemical Co. submitted three samples of Methocei 15000 90 HGDG thickener having different levels of seed or gel particles. Two percent solutions were made and films made on hiding power charts. In the wet films it was visually apparent that the seed content varied m the samples. On drying the films showed no signs visually of any seeds present in the films. <? Paints were then made based on Y--3418 in which the thickeners were introduced. These paints were again drawndown over a hiding power chart with a three mil Bird applicator. The wet paint films showed small particles were present but on drying no visual signs of the small seeds or gel particles was apparent. All three paints were equal. Based on the information obtained in this work it does not appear justifiable to set up rigid quality control specifications for Methocei 15000, 90 HGDG in new Satin. 2) Water Dispersed colorants From Hilton Davis Initial manufacture of Cherry Red imposed a supply strain on Holland Color to supply Toluidine colorant for use in Cherry Red (new Spred Satin). Hilton Davis supplied us with two colorants based on toluidine and naphthol red. Both colors failed to approach the color required in order to match the Cherry Red chip. The toluidine colorarit dispersed readily and the paints showed satisfactory stability when heat aged at 140 F* Their naphthol red, however# caused the paint to coagulate on heat aging. The cause of this situation is unknown. No further work is planned with either of these Colorants. 3) Architectural White (Y-3403) The Cleveland plant informed the laboratory that Y-3403 failed to be in the viscosity specification after final adjustment. The viscosity specification of Y-3403 was established by application of the paint by brush to be 85-90 KU. in some instances Cleveland's production of Y-3403 was 95 to 100 KU. Verification of these results were forth coming from Atlanta. Based on those comments laboratory work was done to specify reduced levels of Methocei 15000, 90 HGDG. Reduction of the Methocei amount by 0.25 pounds per 100 gallons allowed the final viscosity adjustment to place thC final paint viscosity on specificatior 4) Evaluation of Reading Satin Production Green Ice Y-3454, P-264 This sample Was submitted to Quality Control and was subsequently sent to the Satin Laboratory because of deviations in physical propertie This batch was compared against Cleveland production Y-3454, P-607. The hide was a trace less than P-607 and the match was a mismatch to the chip. The following physical constants were obtained: GLD 045563 TM-15 P-264 Specification Pounds per Gallon Viscosity pH Solids, weight 11.10 106 KU 7.7 48.6% 11.25 t 0.15 90-95 KU 7.0 - 7.8 50% It was concluded that this batch was abnormal and failed to meet release specifications. 5) Evaluation of Defoamer Candidates for Spred satin A total of seven defoamer candidates and a re-evaluation of Drew 913SX and Nalco 121 which are both listed under the same code number, e -624, was made during the month of December. The defoamers are listed below: E-624 -- Drew 913-SX E-624 - Nalco 121 North G.L.N. Nppco NDW Hodag PV-22 Hodag PV-93 Hodag Q-324 Colloid 600 Colloid 677 Duplicate testing of Drew 913SX and Nalco 121 by roller, brush and heat aging for defoamer effectiveness showed conclusively that these two defoamers are not alternate materials for use in New Spred Satin. Nalco 121 failed to collapse the copious foam generated under the roller. This information and recommendation was made to the plants. Of the remaining defoamers only North's GLN looked equal to Drew 913SX. This defoamer is being aged at room temperature and will be tested for defoaming efficiency after 3 months. 6) Re-Writing Of New Spred Satin Formulations Complete revisions of the Satin formulation was made both on the pebble mill and Cowles procedures for all tint bases and ready-mixed colors. These precedures incorporate the latest manufacturing methods used successfully in the regional plants. SUBJECT: Experimental Latices In Semi-Gloss Latex NT27001T3363 CONTRIBUTOR: H. Sheets SUMMARY: A portion of this work involved the evaluation of experimental latices, 1580-10A and 1580-10B, in the typical semi-gloss latex formula. 1580-10A and B are diacetone acrylamide containing latices. In one set of formulations the 1580-10A and B were used to replace AC-61 only in the semi-gloss, and in another set of formulations they were used as a replacement for both AC-61 and RCR-0108. GLD 045564 TM-16 All semi-gloss paints based on the 1580-10A and B were quite brittle and were quite poor in wet adhesion on the scrub test. The epoxy ester emulsion 611--Q was also evaluated as a replace ment for AC-61 in the semi-gloss formula. The 611-Q gave-good film flexibility and dry adhesion, but was not quite as good as AC-61 in wet adhesion. SUBJECT: Latex Semi-Gloss CONTRIBUTORS: H. Carroll, R. Venus, F. Wickert, J* Scarry SUMMARY: Throughout the month of December 1967 work continued on the stabilization of the Y-3700 line Semi-Gloss, particularly the high hide white formula containing 280 lbs. of Ti02- Work conducted in this area in recent months has revealed fairly conclusive evidence that the stability of the Y-3700 formula decreases with increasing Ti02 levels. It is not completely understood why this is so, but nevertheless a number of surface active agents were tested as a means of correcting the inherent problem. DISCUSSION: Of the surfactants employed, Gafac LO-529, an organic phosphate ester, was of particular interest. When added to the grind at a level of 3 lbs. per 100 gallons it improves the dispersion of the millbase. When used in combination with letdown surfactants E-239 or E-237 and E-133 it aids stability. These con clusions have been confirmed by and observed 9-10 KU increase in viscosity after 14 days in the 140 oven. With the surfactants employed in the current Y-3700 formulas, the 280 lbs. Ti<>2 levels either kick-out or exhibited a significant increase in viscosity. It was also observed that 2 lbs. per 100 gallons of E-133 in the let down gives a definite improvement in oven stability. Both E-237 and E-239 aid oven stability also. E-237 gives slightly increased stability. E-239 gives a little sharper gloss. Initial batches of Y-3700 line were started in Toronto for T. Eaton. No major problems were encountered in the productions made with supervision from Cleveland other than a lower gloss than expected. Later batches made with RA-45 replacing R-900 gave gloss increases of 8-10 units. GLD 045565 TM-17 TRADE-MAINTENANCE MISCELLANEOUS December 1967 SUBJECT: Water Thinned Floor Paint NT241Q0T3364 , CONTRIBUTORS: E. E. Saville, R. W. Kreider SUMMARY: 1. A list of properties to be considered before releas ing a water-thinned floor paint is given. 2. Glidden Polyurethane Florenaxnel will be used as a standard to be matched, if possible, in a water-thinned paint. 3. Sherwin-Williams' Loxon, Pratt & Lambert Floor Paint, Dutch Standard Floor Paint, and Rohm & Haas suggested formula F-254 have been studied for comparative performance. 4. K-7255, Rhoplex AC-61, Arolin 376, Polytex 611-Q, Monsanto RF-6315 and V-6014 are being considered for use. A combination of Rhoplex AC-61 and V-6014 shows potential. REPORT: la) Properties to consider In Floor Paint Formulation A list of properties have been considered in formulating floor paint systems. This check-list will be reviewed before releasing a paint for production. 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. Storage Stability Colorant Acceptance Odor Ignition Temperature - flash point. Application Flow and leveling. Tool clean-up. Drying. Hiding Appearance Performance over substrates. Durability - Interior-Exterior Floor clean-up. Heat resistance. Discoloration Floor wax acceptance. Manufacturing procedure, types of production. Cost control procedures. Limitations GLD 045566 TM-18 2a) Control Paints For Formulating Glidden Polyurethane Plastic Florenamel, a solvent paint, will be used as a standard to approach in formulating water thinned floor paints. This paint does not have the easy brushing or easy clean-up of a waterthinned paint but appears to have other fine properties. 3a) A simple screening test has been used to evaluate paints. Drawdowns are made on glass and one and two coats are brushed on asbestos board, water immersion, abjrasion and clean-up tests are run on these panels. 4a) Combination of vehicles were tested using the same procedures as in 3a). A straight latex paint made with K-7255 blistered and seemed too brittle. K-7255- modified with Polytex 611-Q had slightly better adhesion but slightly greater water sensitivity. Spred Satin (new) C18A is extremely flat and absorbed water rapidly. Glid-Gloss 15055 No. 2 has a suitable gloss but appears too water sensitive. Arolin 376, ADM, remains water soluble. Arolin 376 plus driers reduced the water sensitivity. Arolin 376 made into a paint had a high gloss but also had a high degree of water sensitivity. The high cost of Arolin 376 makes it impractical at this time. Arolin 376 combined with Rhoplex AC-61 had a decided reduction in gloss. Rhoplex AC-61 has good water resistance and is being considered the base latex for further studies. By combining AC-61 and V-6014 a good brushing, fair leveling paint has been developed with good abrasive resistance and good water resistance. A high loading of the oleoresinous binder increases the dry time to 16 hours. However, V-6014 must be made with a non--yellowing oil before it can be practical for a floor paint. At present a combination of high amount of latex with a low amount of alkyd or oleoresinous binder looks most favorable for a floor paint. SUBJECT: Water Reducible Speedenamel NT28002T5362 CONTRIBUTOR: H. Sheets SUMMARY: A blend of Spencer Kellogg D.V. 1695 and ADM Arlon 376 at 12-| to 87^% of each respectively appears to give the best combination of cure and gloss in the water reducible Speedenamel GLD 045567 TM-19 formulation. The initial formulations were adjusted to about 75 KU viscosity. At this viscosity they tended to cause "drag" on the brush, and picked up 9-10 KU in about 1 week at room temperature. The viscosity of later formulations was reduced to 63~64 KU and there was very little viscosity pick-up. The viscosity reduction was obtained with little reduction in solids, by increasing the amount of Cellosolve and decreasing the amount of water used in the. letdown. The lower viscosity formulation brushes much better, but tends to sag at around 3 mils wet. This was overcome by the addition of 6 lbs. per 100 gallon batch of fientone 27. At present the best drier combination appears to be lead, cobalt, manganese, and zirconium, with Exkin No. 2 for anti-skin. A primer based on D.V. 1695 was also formulated. The primer contains 1 lb. per gallon of Busan 11, and can be used on wood or metal as it is reduced in low odor mineral spirits rather than water, but water can be used for cleanup of the equipment used. The primer gives very good hold-out when tppcoated with the water reducible topcoat or the standard Speedenamel. A series of metal and wood Weatherometer panels have been prepared using the water reducible system vs., the standard Speedenamel. A series of metal panels also have been prepared using the water reducible versus standard for salt spray, humidity and water immersion tests. GLD 045568 TM-20 SUBJECT: To Work Out Concentrated Dramatone Colors CONTRIBUTOR: F. Coenen SUMMARY: Neutral Toner, developed. A concentrated Dramatone Red Oxide, 100% stronger than the standard material, and a concentrated 50% stronger than the standard material, have been DISCUSSION: in the realization of the idea to shade deep hues with a concentrated Dramatone color, some facts have to be considered in order to understand the possibilities. Based on the difference of actual pigment-load in each of the standard Drama- tone colors, a uniform increase in color strength of all our Drama- tone colors cannot be achieved. Eight colors of our line will allow a 50% or 100% increase in color strength, whereas Yellow Oxide, Orange and Lemon Yellow do not allow increased pigment loads, for the pigment volume in the standard material is already very high. Any further increase would result in unacceptable con sistencies. This consistency is the most characteristic fact with regard to possible increases in color strength of any given color. For the predispersed material in the Cowles, mixer must have fine flow properties in order to go through the sand mill. Based on these facts. Red Oxide could be made 100% stronger, and Neutral Toner 50% stronger, even though both colors allow some what higher increases. That cannot be done, or should not be done, for the ratios of standard color to concentrated color would give the color lab great difficulties with later work. The ratio of standard Red Oxide to concentrated Red Oxide = 1 to 2, respectively. The ratio of standard Neutral Toner to concentrated Neutral Toner - 2 to 3, respectively. The new Red Oxide would allow an addition of 8 fl. oz. per gallon with a color strength of 16 fl. oz. standard Red Oxide. The new Neutral Toner would also allow an addition of 8 fl. oz. per gallon with a color strength of 12 fl. oz, standard Neutral Toner. F. Coenen GLD 045569 TM-21 (Suggested Code Number: RFT-67005-H-50) ** 50% stronger than standard. RPT-67005-H Concentrated Dramatone Neutral Toner For Production Evaluation 100 Gallons C-711 S-714 0-834 E-133 24.96% 9.62% 6.71% 3.83% B-312 J-4637 .48% 53.53% E-231 .72% E-419 .15% 100.00% Cowles Mixer & sandmill R7M-21C 37.05 Gals. 15.88 It 10.50 It 6.60 II .42 28.22 II ll 1.08 II .25 H 345.00 133.00 92.80 53.00 6.60 740.00 10.00 2.00 Lbs. H II II II II II II ) ) Mix First ) ) Cowles Mixer: ) Up to 120 F. ) Reduce speed and add: ) Mix for 5 minutes. Then Add: ) Mix for 2 minutes. 100.00 Gals. 1382.40 Lbs. Slow Sand Mill Pass Necessary N.V.B. Volume: 45.92% N.V.B. Weight: 64.73% Vehicle Solids: Pigment: Volatile: 10.72% 54.01% 35.27% 100.00% GLD 045570 TM-22 (Suggested Code Number: RFT-670Q3-K-10Q) = 100% Stronger than standard. RFT-67003-K Concentrated Dramatone Red Oxide For Production Evaluation 100 Gallons Cowles Mixer & Sandmill R7M-13A C-711 S-714 E-231 17.14% 10.26% .58% C-834 Aldosperse ML-14 Pegosperse 200-ML Tween 20 5.15% .49% .48% .54% N--413 R-4098 R--509 4.72% 7.00% 50.14% Lee. Ale. W-14-B-X E--133 1.03% 2.35% E-419 .12% 100.00% 31.59 Gals. 21.06 II 1.08 11 10.00 ll 1.00 if 1.00 IV 1.00 II 3.58 2.80 20.04 It If II 2.00 II 4.60 It .25 H 100.00 Gals. 294.00 176.00 10.00 88.40 8.40 8.20 9.20 81.00 120.00 860.00 17.60 40.40 2.00 Lbs. Lbs. II II 11 ft f If It it it it it ) ) Mix First ) Then Add: ) ) ) ) Mix Again ) ) Cowles Mixer: ) ) GO up to 120 F. ) Reduce Speed & Add: ) Mix for 5 minutes. ) ) Then add: ) Mix for 2 minutes. 1715.20 ii Needs A Slow Sandmill Pass N.V.B. volume: 46.20% N.V.B. Weight: 72.05% Vehicle Solids: Pigments: Volatile: 10.19% 61.86% 27.95% 100.00% Lecithin Alcolec W-13-B-X from The American Lecithin Co. GLD 045571 TM-23 (Suggested Code Number: RFT-66041-F-100) = 100% Stronger than standard. RFT-66041-F Concentrated Dramatone Phthalo Blue For Production Evaluation 100 Gallons Cowles Mixer & Sandmill R8A-2A C-711 S-714 C-834 E-133 Lee. Ale. W-14-B-X Flexticin P-1 E-231 C-268 N. Methyl 2 Pyrrolidone 8.90% 19.14% 7.65% 3.37% 1.68% .73% .96% .96% 1.63% N-413 RV-6909 B-4714 17.32% .06% 14.35% C-711 23.06% E-419 .19% 100.00% 10.00 23.91 9.00 4.00 2.00 Gals. II t VI it 1.00 <1 1.08 1.08 2.00 il it it 8.00 .05 11.76 25.87 .25 it it it It tl 100.00 Gals. 93.00 Lbs. ) 200.00 It ) 80.00 IS ) 35.20 II ) Mix First 17.60 If ) 7.60 If ) 10.00 10.00 17.00 II It II ) ) ) 181.00 .60 150.00 241.00 2.00 If It It If Cowles Mixer: ) ) Up To 120 F. > Reduce Speed & Adc ) Mix For 5 Minutes Then Add: ) Mix For 2 Minutes 1045.00 Lbs . N.V.B. Volume: 37.07% N.V.B. Weight: 46.36% NEEDS A SLOW SANDMILL PASS Vehicle Solids: Pigments: Volatile: 14.63% 31.73% 53.64% 100.00% GLD 045572 / TM-24 TRADE-MAINTENANCE SOLVENT REDUCED - TRADE PRODUCTS December 1967 SUBJECT: Exterior Solvent Thinned Paints NT26042T4262 NT24069T4262 NT23051T4268 NT23051T4268 CONTRIBUTORS: W. Green, R. Ruzicka, J. Southwick SUMMARIES: 1. A high hiding gelled alkyd house paint as a sub stitute for y -5003 in the San Francisco plant has been developed using gelled alkyd RCR-6505. 2. competitive House Paint Evaluation of Pittsburgh 1-57 and 1-54, Sears 30-25024, 2301-4, S.W. Kem-l-Coat, National Lead 110 and 111, S.W. 473, S. W. 471, Benjamin Moore 100, DuPont and Pratt & Lambert. 3. A feeder drier evaluation in Y-5003 comparing Nuact Paste and Litharge for improved dry stability. 4. An exposure series comparing mildewcides; Vancide Dow 1013 and Super-Adit at 7.2<=, 9, and 13.5C per gallon in Y-1801, Endurance Non-Chalk and Y-5003 Ultra Hide. Paints were applied to yellow pine and sent to Baltimore and New Orleans. PA, 1) A high hiding gelled alkyd house paint as a substi tute for Y-5003 in the San Francisco plant has been made in the labor atory. This paint is made with RCR-6505 and 3 lbs. per gallon of titanium dioxide. RCR-6505 is a 60% N.V. tall oil alkyd made with 5% Versamide 335. The purpose of this paint is to replace the current oil version of Y-5003 in San Francisco. The high humidity in the coastal areas cause excessive flashing and dry complaints with standard oil paints. Alkyd enamels have sufficient dry to overcome these problems. However, standard alkyd enamels have poor brushing and low build. By gelling these paints with Versamide 335 we are able to obtain excellent brushing paints comparable with Y-5003. We are also able to obtain a measurable increase in film build with no sagging. A sample of this paint has been sent to San Francisco for evaluation prior to issuing a formula. GLD 045573 2) COMPETITIVE HOUSE PAINT EVALUATION The primary purpose of this report is to compare competitive paints to Glidden's four new thixotropic oil paints, Y-1803, Y-5003, Y-1800 and Y-1801. Exposure tests have been made in Cleveland, New Orleans, and Baltimore. A special "wall" has been built with a two foot over hang to give a better evaluation of uniformity Of exposure from over hang to foundation. This test primarily evaluates dirt pickup and general appearance. Blister exposures are also being run on the GTMG units. Formulas have been calculated based on the can analysis. The calculated weights per gallon are then compared to actual weights per gallon to determine reproducability of the product in relation to the published analysis. The Pure Pure White from Sears showed too high weight per gallon. Moore's 100, SW's 471 and Moore's 110^-01 showed lower weights per gallon. All other paints tested showed good correlation between calculated and actual weights per gallon'. Brushing tests were made to show base of application and hiding. One coat hiding was advertised by five competitors. We claim one coat hiding on all four of our paints. Of the paints tested, only three paints show true one coat hiding -- Y-1803, Y-5003 and Kem 1 Coat. Y-1S00 and Y-1801 were very good, but did not equal the top three. Sears Snowhite, Moore's 109-01 and Pittsburghs 1-45 did not give one coat hiding as advertised. The durability of these paints will be evaluated at a later date. Reference is made to the hiding chart attached to this report. Hiding is listed three ways. First by amounts of titanium dioxide, secondly by equal film thickness (3 mil drawdown), third by brushouts. The first method is usually a good indication of the best hiding power provided the paints tested are comparable types i.e. oil, alkyd Thixo etc. It does not take into effect such properties as flow, build, toning, solids, and effects of other pigments. The second method is a good test for hiding provided each paint is similar in film build. It shows the effects of toning, other pigments and solids, it does not take into effect flow and film build. The third method is the best GLD 045574 TM-26 indication of hiding, but is the most difficult to evaluate. All three methods are presented here to show the effects of properly controlling body flow and hiding pigment. The Moore's 109-01 has a very poor dispersion and does not perform in relationship to the label analysis. Likewise the Sears Snowhite performs better than would be expected from the label analysis. Included in this report is a table of estimated costs. These costs were calculated from the label analysis and do not represent actual coat. They can, however, be used as a loose guide to compare relative material cost differences. No consideration was given to driers, mildewcides or special additives which might influence cost. For instance, Kem 1 Coat is known to contain 18$ worth of fungicide. This is abnormally high and would effect the cost above that of a normal amount of additive. Note that paints containing leaded pigments tend to be much higher in cost compared to zinc oxide paints. Wade Green GLD 045575 TM-27 i . so.irs - Pure pure White House and Trim Paint 30-2502 - New label* no formula change - advertizes one coat coverage over any color - 500 scr. ft. per gallon maximum coverage paint was previously sold as Master-Mixed Pure-Pure Wh i te . 2. Sears - Snowhlte One Coat House Paint - Self cleaning White 2301-4 Same label - new formula?' advertises one coat coverage over any color. Coverage recommended as a maximum of 440 so. ft. per gallon. *This formula shows a radical decrease in quality primarily a drop in titanium. 3. Pittsburgh - Sun proof House Paint 1-57 - Chalk Resistant No previous label or formula available - Recommends one or two coats. 4. Sherwin Williams - Kern 1 Cdat Premium House Paint A3W15 - New Paint advertized as exceptional white with guaranteed one coat coverage - flash resistant. 5. National Lead - Dutch Boy 110 Bright White - Self Cleaning New label, same formula. Recommend 2 coats at 600 sq. ft. per gallon. 6. Sherwin Williams - 473 Trim & Tinting White - New label no previous formula available - Recommends 2 coats. 7. Sherwin Williams -471 Gloss White - New label new formula Recommends 2 coats. 8. Benjamin Moore & Co. - 100 Exterior White - This paint is advertised as having exceptional hiding with brilliant whiteness. They recommend two coat work. Same label, same formula. 9. Pittsburgh - Titanic Outside White 1-54 - No label or formula change since 1961. Recommend one or two coats. 10. National Lead - Dutch Boy 111 Gloss White - New label information on formula not available - recommends two coats. 11. Benjamin Moore - One Coat House Paint 109-01 - No data available on old label or formula - Recommended one coat over most repaint jobs. E.I. Du Pont De Nemours - Trim & Shutter Gloss Enamel 800 - New formula New Paint Recommendation 1-2 coats at 350-500 sq. ft. per gallon. GLD 045576 TM-28 A 11. Pratt & r.ambert - 300 Chalk Resistant White - No data on label or formula - Recommended one or two coat work. 14. Benjamin Moore - Moore's House Paint 110-01 - Label and formula data not available - Recommended one or two coat work. 15. Pittsburgh Plate Glass - Sun-Proof one Coat House Paint 1-45 Same label slight change in analysis. Advertizes one coat coverage. This table is a list of estimated material costs is based on the can analysis. The Glidden formulas also list actual cost for comparison purposes. Actual Cost/Gallon Cost/Gallon Dutch Boy 110 2-67 a Dutch Boy 111 2*53 a .n Kem 1 Coat 2*47- 1 9 Moore1s 100 -2-~3-3 *%* Y-1803 2*29 * 3 2.11 SWP 471 2*2-6- I it P & L 303 2--26 go Moore's 109-01 7.22 * y-5003 2*22- > o 2.04 SWP 473 ?-?-<! i . "i- Snowhite 2*28 i. 11 ' Du Pont 800 2.07 Y-1801 J*99~ / 1.84 Moore's 110-01 1*90 &O Pittsburgh .1-54 < ri Pittsburgh 1-45 1.88 YrlSOO J*8 > n / 1.80 Pittsburgh 1-57 X*82r f. ^9 Sears Pure Pure White 1.71 ZNO X X X X X X X X X X X X X Pb-ZNO X X X White X X X The above costs do not include any additives that may have been added to the paint. \<<l t( '/2A* GLD 045577 TM-29 This chart lints hiding by amount of titanium dioxide, 3 mil draw down, and by brushout. hiding as rated by: Amount of titanium dioxide/gal. Du Pont 800 Pittsburgh 1-45 Kem 1 Coat Y-1803 Y-5003 Moores 109-01 *Sears Pure Pure White Y-1801 Y-1800 *Moore's 100 *SWP 471 Dutch Boy 110 Moore's 110-01 P & L 303 Pittsburgh 1-54 Snowhite SWP 473 Dutch Boy 111 Pittsburgh 1-57 4.19# 3.40# 3.29# 3.20# 3.00# 3.00# 2.82# 2.00# 2.00# 2.00# 1.95# 1.88# 1.79# 1.70# 1.61# 1.46# 1.45# 1.38# 1.26# by 3 mil draw down by brushina Kem 1 Coat Y-1803 Y-1803 Y-5003 Y-5003 Kem 1 Coat Pitts. 1-45 Y-1800 Du Pont 800 Y-1801 Moore 109-01 Pittsburgh 1-45 Pure Pure White Sears Pure Pure White Y-1801 Moore's 100 Y-1800 Moore's 109-01 Moore's 110-01 Moore's 110-01 Moore's 100 SWP 471 SWP 471 Snowhite Snowhite Dutch Boy 110 P & L 303 Du Pont 800 SWP 473 SWP 473 Dutch Boy 111 Dutch Boy 111 Dutch Boy 110 P & L 303 Pitts. 1-54 Pitts. 1-54 Pitts. 1-57 Pitts. 1-57 This chart lists products in order of ease of brushing. Y-5003 Y-1803 Y-1801 Y-1800 Kem 1 coat x Sears Pure Pure White Pittsburgh 1-57 P & L 303 SWP 473 SWP 471 Dutch Boy 110 Moore's 109-01 Moore's 110-01 Dutch Boy 111 Snowhite Moore's 100 Pittsburgh 1-45 Pittsburgh 1-54 Du Pont 800 Excellent Excellent Excellent Excellent Very Good Very Good Good Good Fair - Good Fair Fair Fair Fair Fair - Poor Fair - Poor Poor Poor Poor Poor GLD 045578 T M -30 at -rt at A r-t * o fa u IS to in s* ro H r--I r-4 r~I aS rtf r-t & I O' u CM O fa m * * # o' g o nsj* O' CM cm o o m -r*l to in ,c r--l 54 3 t'' ,0 ^ in o CM i> 4J H +j *i"4 \ \ \ fa r~t dt dt= * 3 g o * 54 CM rl o o * fa r-4 CM in at -rt CM at >t> HH + c 01 -rl 3 54 A 5 H o to C at \ r-4 % 3 g 54 O fa m at m r-l rH d*=dt= CM r-4 CM ^ rl at >ir-~ 4-1 r-t -H s 54 5-1 H to f3a \ * iu f3a u CM 00 o fa CM CM \ d* O' <SJ g 'O t4 no 3 *rl, -| Mo <0 <0 AA -rl O r-t rt Ato A 'flu at r4 tJ at g g'H 3 3 X A aS A fa A -rt -rt O G c c c O O coo as u rt aS -rt t A A c r-t 54 H 54 H *rt *rl rt 3 'rt E-t * N w u WO o ri cn r-t \ r-t . r-4 in o p--i 8 \ H m* in c m O' fa o O r- O VD VO r-f 00 CN' Of I G\ 00 r-4 >* IS d* co r .c mr4 h m -co r*- in M CM as CM > o r- CM <d id O' .O' \\ H r--1 r-4 in r- c m io in fa coofficonntsffKDiD -a o CM cd o is o nOihMHH r- in c m O r-4 CM O oo rl ro r- CM r--1 r-4 5-4 o \\ Po rl r^ O' t-* O' 00 fa fa 10 I rl com i 5-1 o mt''mrii-4inf"in-i-4r-4 IS o CM <d in CM fa c m oo r- <3* o ^i* m r-t i--4 n h d r-l r--1 H H .O'O'O'O' a oo cd (d (d (dr^mr'-inin.-i fa to o t ind n h o h i r- nnMftNHrid00 5-1 r OCM O d oooo at r* 1--1 c rt at m 54 \ r--4 fa -r4 4- 0 $4 4-> 5 r-t rs XS Q -rl -rt Ag 3 OH4Jia+l'HH O C <-4 o \ *o 4-) A> 'G3COG4->0^> *o* rl r4 i--I r-t C tJ 54 O'^S >. >1 3 at C >1:0 x r-t -rt --f fa > A A O O r-t rt r-t JZ o > < CJ fa o GLD 045579 at at O i--i at A C at -rt *u Oc rH O ' 4J +> S g en C O mA o B e n ja m in 100 3 1 2 w c0 CO CD P to >,m rH Is- r4 rH O rlrin CM rH H in r- in CM o cd ftJ tT3 ftj ,05\\ ## 3 S CP CPCP 05 O 5-1 i--I I"ro CM rH O * * tnHCKN H O O o id td tp tp \ \ i--f i--i id id tp tp (Pr^mnooNH P co Q O co in cNi-ncocriCNin'd'fn o o n- O O 50 M CO f' n r-fH cr* r- fa c m a oo Leaded Z in c SWP 471 CO >,in rH CM id 5 rH .3 tP fd \ r-i # H g in p CP O fa rH CO r-| to <P >i .H O id CM ,s r- co CO CO r--1 rH 33 CP tP ## CP cO CO CP CM CM * O CO in rtf' CM CM rH id CP cd \ r-l # i co P CO O fa rH rH rH id id 'tP\ in co CM rH CM CM 'X o r rH id cp \ rH id tp 05 o r~ rH - O 05 rH rH rH IP r" rH rH id id ## i--i id tp \ > <--i id tp ID CM <p r> O f-i ID in o o CO rH id tp \ rH id tp 00 o O ^ CO & P VO t* * -H CM o lO COCMr-COCOCOCM i c j i c m co rd 2 CM in'd'COP'COrHtH o CP o CM rH id tp \ rH id IP co r* co r- c m id m * j-i rr-l 10 iH i--1 CO rH i--1 r--1 3* i <t > co m id o ID cn CP 00 CO rH rH CO CO H fa CM 2 o N a tio n a l Lead D u tc h B oy 110 SWP 473 01 -H CO >iC0 rH rH 3 id r* 05 CO CO r--1 3 tp Id\ - 3 g in p^ o fa r-l rH rH rH id id a) tp tp tp \W O CP CO ip c p r~ # CM CM O * c CD <0 e d >4 ftf -o 3 <D <D rl *t C 4 +> Xo -H -OH rf-tJi +> .S3 a u 08 rl ^ 'O to O e g -W QJ 4J 3 3 X + RJ 2 +id '4 0 id C id c CC OO oo id id o -h 43 4J 4J c r-l J-I H *H -H -rl Id -4 X! -I P h id BBN WOOcoU CO CM r" CM t--i rH id id tp tp d \\ O rH rH E> o id id S tP tp ID CM CO To 1 CM r- co P c m in 05 05 rH rH rH CM CO CO rH CO r** co *r4 O in rH in Tf 05 00 CO rH rH id CM 2 fa oo C id -H CD tp 0Q)) P0) ed -h +> id to p r-l 03 'd Q -P CD e to <Drl rl tr> 3 O r-* -P i -p H rH O Id c o 03 ui C -P CD H c s o & > O CD P 4-> id T3 r-l C m c 'd P >i o r--I CD > r--I tPX3 -H CD fa > xi xi U 3O >H id *rt 3P -P tp -r-t i4 rH < x: U o CO > id o fa o < co m O --i CP tP to X3 G (0 4-1 iH d o c x: g1-1 2 CP E to 4-1 P to c o -h co Xt O P * leaded Z in c GLD 045580 >iCO <-{ co CN m s1 S E-* -P c O0i o o 00 3 Q0 3 g 01 5-1 r-i O* Cm <3* [" 10 cn oj r-l i--i 00 0i 81 i--i 00 0i {ji c m in c m p cm 2 i*0 p nO O IQ m (N | | UlOrtHrl I NCOCO O ' 3* i i i-- m c m i--i r--i m r- oo r-' 3t c -j >h oo m -H 10 r--i 0) cn CO Cm >,cn oo rn o r--1 1--1 CM <T> o0 S3 1-1 o c <3 G1 -r-i CTl i--11--11--11--i go rd id <d <d id r--i 0i on 0i O' -n id \\W g r-l # ### 0) %'d' o on o CD Cm io c m on oo O* CC| i--i r--i O i--i Gl co 10 f'- CM i--i m0 01 0i \ r--i cd 0 01 0> in in in vD c m CO P CM 01 (\J * r-i * 0 't cMr-ioocnr'iD'st^t O CM 00 CD 0 CM 2 V0 CO 00 f> CO !--1 r-i Oi id *t Cm oo 01 -h 'd* 0 O 0 >,in *--11--i <u 0 4 >*! 1--1 O <d (D r-i G fd OA 0i -rM o fd \ +1 P r-l # <d 3 3__ 2 Q 6 00 P cn O Cm --i cm m oo oi OJ rM 1--i id id 0i 01 \\ ## O CM co in * CM CM in cn cn cn in in 01 r- r--1 H id id 0> 01 \\ ## rcn co . r-i H rH id 01 \ r-i id 01 in in o CM CM 0M 01 > O \0 r--I 0 Pm 0 (D p 1 io co 0i co in cn ag Cm cn OIHOOHOIN^'# CO 1 OIMO ri nJ in O h io n tji co co i-i i--i ^ 00 V0 CM fa c m 2 o cn io in o- >i r--I CM ^ 10 01 0 CM 1--1 3 'd' S rQ in 01 I P r-l -P it} cS i-i 0 On Oi Oi 341:# g p r-i in o O cn cn o Cm '* ^ CM O id (D 0 PI 0) g r0 3 *H *rl XO O r-i -rM flj *0 O a r0 01 oi g g -I- O P 3 3 X -P id ri-ri O id G id (U 0 Hi -P -H CD p P c o S -p id id c GC OocoO id id -P -P O G -ri r-i A Cm 0 -rl ,Q 01 r-i Cm -r4 r4 -r4 *r-i id 3-h id EMgitsimocncDO 00 t CM -d* cn r--i r-M i--I 00 0i on r-i io f> in co 2 Cm 0 id c m B On tp I | ^rMOICMCM I (J5MM O I I 00 MNH H HMD<t ft O CO in CM oo r-l G -ri 03 0P 00 PJ -,-i 01 P +> 111 id 0i \ r-4 -P 0 ^01- 0 0 1--1 S0 -0 Q rG g \ O -rM -rM 0 0i 3 'O * i-i O r-i -P OS -P 0 -ri r-M 0 -P 0i O 0 G r-i 0 O -P 5 01 *0 01 C -P- 0) O % > 0 'O 0 ,G C 0 -ri C g -ri r-M r-l C O 0 -P -ri 0 >0 P 0 013 >1 rM 3 0 'ri w O C ,C m >1 O > -r! 0 o n n 3 p -rM r-l O 0 C^rlH ft > o r-i M-> 01 > 01 g 3 Hrid O , . _ > > > 0 O p p<ow^^:2a.u< cn c o s t 1.89 tin te d No GLD 045581 G lid d e n from , Y -1 8 0 1 TO CM r- CD >,r-nnN r--1 r--1 1--1 CD CD CD \ \\ 4 \Q r--4 *sj* CO CT> O 0 n (N ro vO iO co rH CD \ r--*1 CD VO . . O 1--I CD \ rH CD m CD ui vo ... CM * VO 00 t- r-l CM 00 in 00 vO CO r-i . O CD TO 0) i--i >-i P itts b u rg h 1-45 TO w *h o j >i O r) (O ' ^ i--t CJl \ rl # 3 go U O Cn CO co r-l rl r-i CD \ 4 rCM * r--I ,, .in.r.~ .vo CD CD CO CM i--I CM HHrIH CD CD CD CD \\\\ i--! r--I r--( r--1 as (D h c m in p co CD tin CD CD 4* "* CO o CO m csno H (N rl n i i i i r- O IdrlH I CM CO CO O r-- co cMH h mr' or* ft rt >i \ O OOO B e n ja m in M oore 110-01 t o co co r- co *r-4 * * t o c m * ' in c m ^>1 rH ro (N H H rH as , r-l 3 g CN VO OT P CD r*. CD CD CM 0 .... feOMHOH VO CD 0 VO ro r-l rH CD CD \\ r--4 rH CD Cd c ^ ro CD monin & p o .... -rl CD 01 00 VO 00 r-l VO as * c m in of CD m^h h CO CO ^ Cm 1--1 J>4 0O P ra tt & Lam bert 303 TO rl VO TO . >1 CM 1--1 r-l 0- in .. 1--1 CO CM CM rH rH *H aS aS CD \ r-l # CD CD w 3 go 00 in P r~ 0 c d co Ua rH CM CM 'O <u g rd 3 -H *iH x0 O r-i -H rd O T3 PI P3 -P rl x: TO -p is -P g___g_ T-Jrl TO -P . S -p -3rl 3 -rl X O -P G G c c 0 0 -rl O GOO -A & -HP *-HP -HC -ri-Hl P T3O r-r-ll p fiHNMOfflWU GO *4* r-l O CO cl rH iH CD CD \\ rH r-l CD CD 00 CM in * m in 00 B *oo ... in on o ro CM I- CM ro 00 r-l CO CO | CD O o 13 in c m in rj* 00 O- ro r-l r-l ^ ffl CO COM * G rl TO H TO P CD \ PS -rl p) *--f ra TO p +J 5 to -r-lI -'OP *0 O r-l 4-1 Q <JS -P ,3 CD g 3 H <--l CD no 4-1 O --1 CD O G rH O P> CD O CQ C -P O & > as T3 ra ,c G -rl c g r-tr-ICUW-P-rl -a p trix: >1 >1 3 -p t o o G ,G >3 >04>-rl A U3P--1 r-iora-P-P -Crl rX-t H, HO B,,i>,, PI < O CO ^ ^ U <1 pi CD C> CD fi 3 TOG P > tl P O -H o,o< fn,Q04J -rl O P *o 1--1 4-1 44 aS co * GLD 045582 Titanium dioxide Titanium Calcium Zinc Oxide Silicates Carbonates Busan Silica White Lead Carbonate White Lead Linseed Oil Alkyd Solids Chlorinated Resin Solvent & Driers % Pigment % Vehicle NV by weight NV by volume PVC Calculated wt/gal Actual wt/gal grind vise gloss 3 month gloss brushing cpst tinted Glidden Actual Y-1801 Formula Analysis 0.85 #/gal 3.84 #/gal 2.00 #/gal 0.47 gal/gal 0.31 gal/gal 82.3 69.0 31.3 1.84 GLD 45583 TM-35 3) A feeder drier evaluation in y-5003 shows an improve ment in dry. Drier studies were made comparing standard Y-5003 with Y-5003 plus 2 lbs. per 100 gallons of litharge and with Y-5003 plus 5 lbs. per 100 gallons of Nuact paste. The litharge shows a 5 hour improvement in dry. The Nuact paste shows a 5 hour increase in dry. The dry recorded here is not dry-to-touch time but is read as complete film dry. All of the paints dried-to-touch in about 7 hours. These paints wm be rested tor io s s or dry in b months. 4) An exposure series comparing Vancide PA, Dow 1013 and Super-Adit at 7.2d, 9b, and 13.5b per gallon has been made and exposed at Cleveland, New Orleans, and Baltimore. This series was exposed on 4 ft. yellow pine siding. Y-1800-G, Y-1803, and Kem-l-Coat were included as standards. The mildewcide ladders were run in Y-1801 and Y-5003. Both the alkyd and oil version of Kem-l-Coat were used as controls. SUBJECT: Glid-Tone Varnish Stains - Y-1201, Y-1202, Y-1203 CONTRIBUTORS: D. Sutherland, J. Davis, J. Southwick SUMMARY: The San Francisco plant has satisfactorily completed the manufacture of the initial batches of the varnish stains that have been revised to comply with Rule 66. This is an entirely new formulation that affords the opportunity to eliminate some specialized varnish cooks from inventory, i.e., V-525 (V-357), V-533 (V-306-C) and V-755 (V-405). The new formulation is composed of V-2390 (V-863) and V-2283 (V-891), both alkyds, in conjunction with V-415 (replaces V-46). A new gilsonite solution, V-739, has been introduced to replace V-755. The V-739 is easier to manufacture and easier to incorporate in the stains. We recommend that the new formula be adopted nationally. Besides the obvious inventory advantages, the new material has a substantially lower raw material cost. If desired the v-415 may be cold-cut in large quantities and used as required, or the resin may be cold-cut in each individual batch this is entirely up to each production man and the economics involved. It will be necessary, however, to deplete the inventories of the obsolete raw materials, or have an alternate disposition, before manu facturing the new varnish stains. / GLD 045584 TM-36 SUBJECT: CONTRIBUTORS: D-142, Burnt Sienna Replacement In Glid-Tone Stains NT26042T4262 J. Davis, J. Southwick OBJECTIVE: To find a suitable replacement for D-142 (Burnt Sienna) which-is becoming increasingly difficult to obtain and is used in a number of the Glid-Tone wood Stain colors. SUMMARY: A sample of D-142 (BS-6653, Lot 26) from the Chas. Pfizer Company, which, according to them is off specifi cation, was tested in Y-244, Modern Red Mahogany Stain and found to be acceptable. Also received from Pfizer was a sample of 7852 Burnt Sienna which was a possible replacement for D-144,old code R-21. This was rejected due to the''dirtier color of the Pfizer material. Four samples were received from Reading where D-144 was used as replacement for D-142. These samples; Y-244 Modern Red Mahogany, Y-245 Walnut, Y-252 Maple, and y -258 Fruitwood were tested versus the standards. Results showed in all cases a slightly dirtier, browner tone than the standard but we feel not enough to bring complaints and, therefore, R-144 is tempor arily approved as a direct replacement for D-142 in pebble mill batches only. Work will continue to find a final replacement for the D-142. SUBJECT: Glidden Manufactured Odorless Flat Wall Resin RCR-6507 & Cargill 72245 Versus Standard F-2233___________________ NT27006T4363 CONTRIBUTORS: J. Davis, J. Southwick SUMMARY: RCR-6507 and the Cargill resin were tested in Y-5718, White Tint Base versus the standard resin F-2233 (ADM). The results show the Glidden material to be equal to the standard in application, enamel holdout, hiding, tint strength, flow, and uniform ity. The viscosity of the paint made using the Glidden vehicle is 90 KU's, the minimum for this formulation, while the standard has a viscosity of 113 KU. The lower viscosity of this material can be corrected with minor formula adjustments if necessary. Another pilot plant batch of this material is to be made. The Y-5718 using the Cargill material has a satisfactory viscosity of 97 KU. As in the Glidden material all properties of the Cargill are acceptable in comparison to the standard with the exception of hiding and tint strength, which is high and enamel holdout which is slightly poorer, indicating the inability of this resin to maintain as high a PVC as the standard. These problems are easily corrected with the addition of 2-1/2% more resin which lowers the PVC slightly. All materials have excellent package stability after 10 days. All paints have excellent odorless qualities. GLD 045585 TM-37 CONCLUSION: Both the Glidden RCR-6507 and the Cargill resins are acceptable as replacements for our standard F-2233 if minor formulation adjustments are made. Special formulas will be written for each resin. SUBJECT: Odorless Alkyd_Flat -_Low Cost CONTRIBUTORS: J. Southwick, D. Sutherland OBJECT: Investigate possibilities of lowering the raw material cost of EGL-64544 and Chicago's A-3000-B. SUMMARY: An investigation into the reduction of the raw material cost of our low cost alkyd flats has been made. The main approach to this reduction has been through pigmentation. By the use of selected extenders in combination with titanium calcium(30%), flats have been made that maintain high dry-hide with no sacrifice in other properties. The combination of extenders showing the best efficiency proved to be Al-Sil-Ate NC, Nytal 300, and Atomite with up to a quarter of a pound per gallon of diatomaceous silica for flatting. By judicious selection of extender pigmentjs, a saving in the raw material cost of $.05 to $.10 per gallon can be realized. With the adoption of a Glidden manufactured odorless alkyd resin, the RMC can be dropped another $.05 to $.07 per gallon. The work on this new vehicle is nearing completion. SUBJECT: Y-5099 Eggshell Stipple Uniformity Evaluation NT23048T4263 CONTRIBUTORS: J. Davis, J. Southwick OBJECTIVES: To test several batch retains for Dramatone acceptance and gloss uniformity and to make necessary formulation corrections to eliminate any problems encountered. SUMMARY: Occasional complaints have been brought to our attention concerning the sheen uniformity of the eggshell stipple after the addition of Dramatone. Several Cleveland batch retains were tested in an attempt to get duplication of the problem arising in the field. One batch which has a gloss of only 10 duplicated the problem others did not. Glosses on batches checked ranged from 20-60 and no uniformity problems were apparent. It was noted that a definite increase in gloss takes place in the package probably due to drier adsorption. CONCLUSION: If the gloss of all batches are kept above the formula specification minimum, no uniformity problems should appear. However, the formulation will be revised to include Nuact Paste (E-396) to combat the increased gloss in the package. The W-137 (RCHT-X Ticol) will be replaced by our W-138 (RCHT Ticol) which has a GLD 045586 TM-38 higher oil absorbtion and gives slightly higher hiding and slightly lower gloss. Thixin will be increased from 7 to 10 lbs. for better stipple effect and our gloss specification will be changed from the present 25-30 to 25-35 to allow a wider acceptance range and to help deter any more uniformity complaints from low gloss stipples. u-tsuj s C*I* : bprea jjuscie - uaotiebs r ictc rtiKyd NT23048T4263 NT27006T4363 CONTRIBUTORS: J. Bednarik, J. Sainsbury, J. Southwick SUMMARY: The Resin Laboratory prepared a batch of experimental Glidden Odorless Flat Wall Alkyd (RCR-6507) with a trace increase in the Glycerine level. The objective was to compensate for a modified manufacturing procedure. This resin (1429-A-43) was evaluated in Spred Lustre Y-4618-J and rejected because of insufficient self-sealing properties. Gloss uniformity over substrates of varying porosity is a necessary function of Spred Lustre. Other properties - gloss, viscosity, sag control, application - were acceptable. SUBJECT: Spred Lustre - Use Of Zinc Oxide NT23048T4263 NT23053T4268 CONTRIBUTORS: J. Bednarik, J. Sainsbury, J. Southwick SUMMARY: Incorporation of zinc oxide (w-514 at 10 lhs. per 100 gallons) into Spred Lustre made with both F-2233 (ADM odorless 5555-MO-30) or RCR-6507 (Glidden Odorless Flat Alkyd) showed very little effect. The W-514 was substituted for the 20 lbs. of N-413 in Y-4600-A. No significant effect was noted on dispersion, viscosity, flow, sag control, gloss, uniformity over substrates of varying porosity, application, dry, or hiding. Periodic examinations of stability, viscosity, drift, gloss retentionhazing, and oven stability are scheduled. Very careful checks will be made into any possible seeding. SUBJECT: Spred Gloss Enamel - Non-Yellowing NT23048T4263 CONTRIBUTORS: J. Bednarik, J. Sainsbury, J. Southwick SUMMARY: Two resin modifications, Damar and Picco 6140-3, are being evaluated in Spred Gloss Enamel White Y-900-A. The objective is the removal of zinc oxide without sacrificing non yellowing, YelloWingtests, gloss retention, haze resistance, and exposure tests have been initiated. These will be reported as con clusive observations are available. GLD 045587 TM-39 SUBJECT: Spred Gloss Enamel - Drier Series NT 23 048T4263 CONTRIBUTORS: J. Bednarik, J. Sainsbury, J. Southwick CONCLUSIONS: Evaluation of Mooney Chemicals recommendations of drier systems in Spred Gloss Enamel Y-900-A showed improved dry with either Taiiates or Ten-cems. However, the increased ary is impractical due to the cost increase or discoloration due to manganese. DISCUSSION: Y-900-A. The solids: Two drier systems recommended by Mooney were evaluated versus the standard system in Spred Gloss Enamel White systems evaluated were: % Drier Metal based On vehicle Standard No. 1 Experimental No. Experimental 0.052% Co 0.052% Co 0,078% Co 0.240% Pb 0.480% Pb 0.480% Pb 0.034%Ca 0.030%Mn 0.102%Ca Both Taiiates and Ten-Gems were evaluated. Drier costs based on Cleveland raw material for the Taiiates are: Standard No.1 Experimental No.2 Experimental 2.99 3.29d 6.20d per gallon per gallon per gallon The Experimental No. 1 system was found to be equal to the standard drier system but was unacceptable due to a brownish-red staining from the manganese. The Experimental No. 2 system improved the dry from 6 hours to 4 hours but this improvement is not practical in light of the extra 3.2d per gallon. ( Comparison of Tallate versus Ten-Cem in each system showed equal dry but a trace less staining for Experimental No. 1, equal to 1/2 hour better dry for the standard, and 1/4-3/4 hour better dry for Experimen tal No. 2. Dry stability will be evaluated to make sure no substantial product improvement is available with these experimental systems. SUBJECT: Spred Gloss Enamel - Post 4 NT23048T4263 CONTRIBUTORS: J. Bednarik, J. Sainsbury, J. Southwick SUMMARY: Due to questions from manufacturing and sales departments we have re-evaluated the use of E-173 (Post 4) in Spred Gloss Enamel White Y-900-A. Our conclusions are: GLD 045588 TM-40 Post 4 additions into the dispersion phase significantly contribute to flocculation. While a noticeable increase is made in the sag resistance, the loss of hide and color due to flocculation rules out the use of Post 4 in this way. Post 4 additions in low levels (1/2-1 liquid ounce per gallon) as a post-additive to a completed batch to further control tne say lesistaui-e .l s dtcepudOie. j.r <ray liutcuiaviu!! j -s evident, but a trace (1-3 KU) viscosity increase and a significant increase in flow control is achieved. SUBJECT: Competitive Product Evaluation - Spred Lustre Alkyd NT24070T4163 Semi-Gloss Enamel CONTRIBUTORS: J. Bednarik, J. Sainsbury, J. Southwick SUMMARY: We have completed our evaluation of the new "partial odorless" Spred Lustre Alkyd Semi-Gloss Enamel versus 6 major competitive products: DuPont Benjamin Moore National Lead Pittsburgh Sears-Roebuck Sherwin-Williams Duco Dulamel Diamond Satin Hide Satin Kem-Glo #260 #207-01 #11-17 #20-6 #7611-4 #391 Satin Sheen Semi-Gloss Semi-Lustre Lo-Lustre Semi-Gloss Semi-Gloss This comparison showed the new "partial odorless" Spred Lustre to be the best general purpose product evaluated. All testing results are based on standardized laboratory tests or, where opinion is required (application, odor, appearance, wet hiding), on tests from unlabeled containers by a panel of four qualified laboratory personnel. Characteristics Rated Superior (X) & Inferior (0) * DuPont Glidden B. Moore Nat.Lead PPG Sears S-W Application XX 0 Odor O XXO Appearance XX X Uniformity X X O X00 Color O 0 X X0 Re fleet./Brightoess X0 Wet Hide X 0X Dry Hide 0X Flow O Sag control XX Dry 0 XX Washability 0X X Burnishing Resistance X XX XX GLD 045589 TM-41 Lap Time Self-Priming Gloss Gloss Retention Film Aging DuPont ' 0 0 Glidden X X B.Moore X X 0 Nat.Lead 0 PPG O X X 0 0 Sears X S-W 0 0 TOTAL RATING -2 +7 0 +3 + 2 + 3 -3 Number of X1s (superior ratings)i minus number of 0* s (inferior ratings). DISCUSSION: Specific Test Comparisons General Characteristics Dispersion(grind) Weight/Gallon Viscosity (KU) %N.V.(Label Anal) Label Description Non-Ye1lowing Odorless Self-Priming DuPont G1idden 4-6^ 10.6# 91 64% 6 11.1# 88 68% Yes Yes Yes B.Moore 5-6 10.9# 79 69% Yes Nat. Lead PPG Sears S-W 6 11.4# 82 73% 5 6 5-6 11.1# 11.7# 11.2# 79 83 72 68% 71% 70% Yes Yes Yes Yes Yes Yes Yes Visual characteristics Color Blued Heavily Lightly Trace Very Heavily Dirty Blued Yellow B lued Blued Dirty Blued Reflectance 85.3 85.6 88.2 85.7 86.1 83.2 85.2 - Colormaster Tri-Stimulus Colorometer - measure of color brightness or cleanliness - 100 maximum. Wet Hiding 800 1050 700 1370 900 1010 970 - Pfund Cryptometer - No. 35 Top Plate , Wedge Constant 0.0035 - Evaluation from unlabeled cans - Sq. Ft. per Gallon Hiding 97.2 98.1 95.5 99.0 97.4 97.7 100 - Colormaster Tri-stimulus Colorometer - Contrast Ratio - 100 maximum. Hiding 99.1% 100.0% 97.4% 101.0% 99.1% 99.6% 102.4% - % of Spred Lustre - based on Contrast Ratio Hiding and reflectance comparisons are dependent upon the color and type of color each product has. The very dirty color of the Sears' Satin is detrimental to the reflectance of the product, but is GLD 045590 advantageous for hiding. Just the opposite is true for the natural color unblued B. Moore Dulame1. Theoretical titanium dioxide level - based on label analysis and actual weight per gallon - expressed as pounds per gallon: DuPont Glidden B. Moore Nat.Lead PPG 2.90 3.00 2.15 4.13 2.92 Sears 3.19 S-W 2.93 Dry-3 mil wet film 4-5/8 6 8| 8 5-5/8 3-3/4 5-3/4 - 12 hour cycle - B-K Automatic Dry Recorder - hours 6 Week Aged film Brittle OK OK OK Brittle OK OK Lap Time Minutes 20 25 25 20-25 10 15-20 10-15 Comparative evaluation - dependent upon conditions at time of comparison. Washability, Gardner Straight Line Scrubber - 3 mil wet film drawdowns aged one month - soiled with four items - scrubbed 35 cycles with Bon-Ami and water - reported as approximate percentage of soiling agent removed. Lipstick Crayon Pencil Ball PointPen 100% 100% 50% 75% 100% 100% 100% 75% 100% 100% 100% 50% 100% 100% 100% 100% 100% 100% 75% 75% 100% 100% 100% 100% 100% 100% 100% 75% Burnishing Yes No No No Yes NO No Application - unlabeled can - panel rating Glidden DuPont Rated best. Rated equal to or trace poorer. PPG Rated good - trace ropy and thin. B. Moore Same as PPG Sears Acceptable - thin. Nat. Lead Acceptable - heavy with noticeable drag. S-W Poorest - rated fair - thin - noticeable drag. GLD 045591 TM-43 Odor - during application PPG and Sears were rated best - completely odorless. Glidden , DuPont and B. Moore were rated good - very mild. Nat. Lead and S-W were the poorest - noticeable odor. Leveling DuPont Glidden B.Moore Nat.Lead PPG Sears S-W 5, 5-6 4 6 2 56 - N.Y.P.C. Leveling Meter - ratings of 0 (no flow) to 10 (complete flow) - normal acceptable range is 4-8. Sag Resistance 11 9-10 12 9 12 10 8 - Leneta Anti-Sag Meter - ratings of 3 (complete sag) to 12 (no sag) normal acceptable range is 6 (3 mils wet) to 10 (5 mils wet). Uniformity & Self-Sealing - brushed over wallboards partially primed with Spred Vapor Barrier and Painter Latex. Over Y-3416 OK Over Y-5370 OK Over unprimed OK Self--primed Good Good Good Good Good Good Good Good Good OK Poor Poor Fair* Good Good Good Good OK Poor Fair Good* Good Poor Fair OK* * Second coat is very high gloss compared to first coat. Gloss Data Gloss - 3 mil drawdown on Leneta Form 3B Opacity charts - 60 Photo Volt Initial 40 49 82 66 1 Month 22 33 53 50 58 57 80 33 42 51 Gloss - 3 mil drawdown on Morest Penetration charts - 60 Photo Volt - sealed background/unsealed background 43/24 55/31 83/61 73/5 63/33 60/17 70/49 Brushed Gloss 28 51 65 59 2nd Coat 31 40 48 54 62 56 47 40 50 49 GLD 045592 TM-44 Non-yellowing tests and gloss stability upon aging have been initiated. Results of these tests will be available in 2-3 months. Specific data and panels on all tests are available for inspection at the Research Center. Work is planned to evaluate two tints (very light yellow and medium green) of these semi-glosses in the near future. GLD 045593 TM-45 TRADE-MAINTENANCE M-- 1 TRADE MAINTENANCE December 1967 SUBJECT: Converted Epoxy iS.M23Ui.iMi3 6B CONTRIBUTORS: E. Hood, P. Begany SUMMARY: 1. Busan 11 In Epoxy Ester Coating Six months Florida exposure panels have been inspected of GL-67299, White Epoxy Ester Enamel, and GL-67299 containing 150 pounds of Busan per 100 gallons. GL-67299 has chalked heavily. The Busan 11 modifi cation has not chalked but does show moderate dirt collection. 11 2. Lubrizol CA-21 Curing Agent A 6 month inspection of a comparative yellowing test of Nu-Pon Cote and a Lubrizol CA-21 cured epoxy show that the Lubrizol CA-21 cured epoxy has yellowed less in the smoke room and window exposures. 3. Evaluation Of Titanox CL-NC Titanox CL-NC is being compared with W-944 and W-948 in both Nu-Pon Cote and Durable Polyurethane on exterior exposure. SUBJECT: Water Reducible Epoxy Ester Primer NM28007M1368 CONTRIBUTORS: E. Hood, P. Begany SUMMARY: 1. H2O Reducible Epoxy Ester Primer is more economical than Y-5570 on a solids basis. Bulk Cost N.V.Volume Y-5570, Metallite Nu-Pon Primer PB43-67, H2O Reducible Epoxy Ester Primer $2.95 $3.13 39.0% 45.9% 2. One hundred-fifty pounds of N-531, mica, per 100 gallons greatly improves salt spray, humidity, and water resistance.3 3. PB43-67, Water Reducible Epoxy Ester Primer, and Y-5570, Metallite Nu-Pon Primer, are being compared for recoatability with Rustmaster, Lifemaster, Nu-Pon Cote, and Vinyl-Cote at varous time intervals (4 hours, 1 day, 5 days, 1 week, 1 month, 6 months, and 1 year). On 4 hours, 1 day, 5 days, and 1 week recoat, Lifemaster, Rustmaster, and Nu-Pon Cote are at least as good over water reducible primer as over Y-5570. The adhesion of Vinyl-Cote is much better over GLD 045594 TM-46 water reducible primer than over Y-5570. The film flexibility of water reducible primer is much better than Y-5570. Nu-Pon Cote has a crawling tendency over 1 month aged Y-5570 but not over 1 month aged water reducible epoxy ester primer. 4. In our work to develop a lead-free water reducible epoxy ester primer, PB91-67, pigmented with RX-2022 Iron Phosphate (Pfizer; is testing out better chan PB63-6 i red lead primer. Active But No Reported Work During Current Month NM25007M1268 NM25009M1268 NM27009M1168 NM27016M1764 NM28001M1168 NM28011M1168 Parlon Block Filler Rule 66 Seamless Floors Demonstration Manual ASTM Dl \ Letters Closed During The Month ' NM24030M1168 Preparation of Detailed Specification For Trade Sales Closed 12-11-67 SM24005M1168 Central Region Requests Closed 12-11-67 GLD 045595 TM-47 TRADE-MAINTENANCE M-2 INDUSTRIAL December 1967 SUBJECT: Lead less Hi-Mil Printer j XM^/OubM2 322 CONTRIBUTORS: F. Jeffers, P. Begany SUMMARY: Tbe condition on the two storage tanks has not changed since last reported. SUBJECT: / Urethane Epoxy NM2 7012M2222 CONTRIBUTORS: E. Hood, P. Begany SUMMARY: Following are the results of Cleveland exposure testing of urethane-epoxy: Coating System 6 Month Cleveland Exposure 1 Year Cleveland Exposure 1. Nu-Pon Cote (Y-5251 & Y-5240) Moderate chalk. Heavy chalk. 2. Vinyl-Cote (Y-5251, Y-5285, Y-5280) No change. Slight gloss loss. 3. Durable Polyurethane (Y-5251 Y EGL-65415) No change. No change. 4. Mobay Durable Polyurethane Moderate yellowing. (Y-5251 & FJ43-66) Moderate chalk. 5. Epon 1009 - Desmodur N (Y-5251 & FJ44-66) Slight gloss loss. Heavy chalk. 6. Epon 1009 - Desmodur L (Y-5251 & FJ45-66) Bad yellowing and moderate chalk. Heavy chalk. SUBJECT: Chemical Resistance Test - Glid-Flake NM28002M2122 CONTRIBUTORS: F. Jeffers GLD 045596 TM-48 SUMMARY: A one month interim report has been submitted which shows that: 1. It is good for acids at room temperature for one month. Other acids at elevated temperatures have not been determined. 2. Alkali resistance is fair to good at room temperature, nowever, at elevated temperature it has no resistance. 3. Solvent resistance is not satisfactory either at room or at elevated temperatures. SUBJECT: Weld-Thru Primers NM28003M2310 CONTRIBUTORS: F. Jeffers SUMMARY: The following primers are being tested in the Weatheromete and Salt Spray cabinets. Sch. No. 258 259 260 261 262 263 264 SF-19196 - Hi-Solids Aluminum Weld Thru Primer Vinyl Alkyd RL-19418 - Zinc Dust Primer - Phenoxy Carbo-Zinc #11 - Zinc Silicate Monsanto - Aluminum Silbond H-6 - Zinc Dust - Ethyl Silicate 178-G-l - Metal Conditioning Primer - Poly Vinyl Butyrol RL-19388 - Zinc Chromate - Poly Vinyl Butyrol Salt Spray - 250 Hours Sch. No. 258 259 260 261 262 263 264 Failed Bad Blistering and Rusting at the scoreline. No change. Bad rusting(scoreline). No change. v Failed Failed There are no results on the Weatherometer panels at this time. SUBJECT: Water Reducible Epoxy NM28010M2222 CONTRIBUTORS: E. Hood, P. Begany SUMMARY: 1. The shading color and Dramatone acceptance is much better when added to the polyamide component than it is GLD 045597 TM-49 in the epoxy component. Therefore, we are going to pigment the poly amide component and have the epoxy emulsion component unpigmented. 2- The addition of 50 pounds of N-413, magnesium silicate per 100 gallons of pigmented base improves sag resistance and anti-settling. The gloss reading is 85. 3. A modification of water reducible converted epoxy with Spencer Kellogg DV-1695 was investigated to improve clean-up with soap and water. It is unsatisfactory because it caused a hazy appearing film. 4. PB82--67, White Water Reducible Converted Epoxy Base, has passed 1 week at 110 F. stability, and 5 freeze-thaw tests. 5. Merginamide L-220 (Stephan Chemical) and also Armocure 100 (Armour) were found to be unsatisfactory as curing agents for our water reducible converted epoxy. 6. Igepal CO-890 and Igepal CO-430 (General Aniline & Film) are not as effective as Triton X-100 as wetting agents in our water reducible converted epoxy. 7. Pot life is extended by blending Epi-Rez 2051, epoxy emulsion, with an emulsion of F5151, Epi-Rez 242. SUBJECT: Statistical Design NM17001M2822 CONTRIBUTORS: F. Jeffers, B. Payne SUMMARY: 1 through 8. acrylic. Sixteen samples were received from the resin group. Eight of these samples represent the OH acrylic numbered Eight samples numbered 1-A through 8-A represent the NCO All 16 samples were at 50% 1 1% NVM. Testing was performed by the Maintenance and Wood Laboratories. Samples when mixed were applied 3 mils wet on tin plate using a bar coater. Pigmented films will not be tested until the results of the preliminary design are known. Following is a list of tests that are to be run. 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. Pot life. Recoat Adhesion Impact Pencil hardness. Dust-free; Tack-free; Film appearance. Film thickness. Flexibility. Chemical Resistance. Dry-through. GLD 045598 1. Samples In Mixing Order Of Design OH Sample No. NCO Sample No. OH % 7 7-A .39 8 2-A .88 6 4-A .83 3 8-A .41 1 3-A .89 5 1-A .38 4 5-A .39 2 6-A .90 2. Samples In Mixing Order Of Design OH Sample No. NCO Sample No. OH % 8 8-a .88 7 4-A .39 3 2-A .41 6 7-A .83 5 6-A .38 1 5-A .89 2 1-A .90 4 3-A .39 Statistical Design Tests NCO% 2.28 4.85 2,62 4.65 2.74 5.00 2.10 4.32 NCO % 4.65 2.28 4.85 2.28 4.32 2.10 5.00 2.74 SEE FOLLOWING PAGE GLD 045599 m I 2: r-t S T A T IS T IC A L DESIGN TESTS m 0) e u Q c as 03 4-1 -i-4 4J o cu -P <D 5-1 O U O 03 3 4-1 4-4 r--I 54 -H -P 0) as a C4 b qj o it II w O *--4 H o i* w t4 m 0) -M m3 54 c 3 .-'j O g. E II H 03 03 5-4 54 0) 03 E3 3C C 03 03 0) 44 g -r-l -p-4 J E4 -P >1 O 54 04 Q GLD 045600 1 11 01 P e rfe ct F a ilu re C H EM IC AL R ESISTAN C E TE S T ON S T A T IS T IC A L D ESIG N 666ddoooooooooo rH r-1 rH rH rH rH iH rH r-4 rH rH rH rH r--I rH rHOOOOr^OOQ.HrHrHrHrHrHO rH rH rH rH rH pH rH **** rH rH O O O O rH rH f--4 pH r--I rH rH r--I rH p--4 O r--I --4 r4 i--4 *** * rH : O O O OO O O * O O --4 O O O O p--l rH rH r--4 i--I p--4 r--I H rH r--4 t--4 rH p--4 r--I i--I r--I rH i--4 p--4 rH rH rH rH rH rH rH pH i--I pH pH rH rH rH rH rH rH rH rH rH rH rH rH rH rH rH rH o o o O rH rH H o rH rH o iH o t rH i-i i-i i-i rH rH rH rH o o o o iH iH o rH rH o rH o rH -I rH rH rH rH i--i rH rH o o o o O o o o o o rH rH o o o i--i pH rH i--i rH i-i rH rH rH rH iH pH rH rH o o o o O o o o o o o o o o o 1--1 rH rH 1-1 rH iH rH iH rH r-i rH rH pH Hi rH II li o r-t rH * o pH o o o o o o rH O o o rH rH o o O --1r i-l rH rH pH rH rH rH rH rH rH rH rH o o o o o o rH O rH o rH iH o o o 1--1 rH --I rH rH r-i rH i--i rH rH rH rH in rH in ID rH r-l 1 5 rH r-i rH rH *H rH rH rH o o o o o o o o o o o o o o o rH rH rH rH rH rH rH rH rH rH rH rH rH rH rH rHoooor^or^ooorHr-ooo rH rH r--I rH rH rH rH rH * rH rH rH rI'(NI ^Io)I MIf-iIunI oIcOI 'tI<NI tIs'VIDiInHI mI rI^oI o^I oIni-iimIrtCl Nl CIorl^fInvIDiInr-I ioIj'^Ii' GLD 045601 TM-53 SUBJECT: Supplement To Statistical Design NMl7001M2822 CONTRIBUTORS: F. Jeffers, B. Payne SUMMARY: The following materials were submitted by the Resin group for possible new coatings by the Maintenance and wood .laboratories. Sample No. 1524A-42 1524A-43 1524A-58 1524A-50 1524A-52 1524A-55 % N.V. Viscosity NCO(100%Basis) Solvents 56.7% A 8.3 S-423 Resin Backbone Epoxy 63.8% V-W 8.3 S-423/ S-614 Epoxy 65.8% S 7.4 S-423/ S-614 Epoxy 68.7% 38.5% U-V D 4.9 4.0 S-423 S-423/ S-614 Polyester Vinyl 61.5% F 3.0 S-423 Polyester The above materials were mixed in proper ratios of NCO to OH with the following Sample No. % N.V. Acid No. Viscosity %OH Solvents Backbone 1524A-54 68.4 .4 B 5% (100% Basis) S-423 Polyester 1524A-57 60.2 1.2 B+ 3.2% (as is) S-423/S-614 Epoxy These materials were handled in the same manner as were the original Statistical Design. Physical and Chemical Tests proved to be unsatis factory. However, 1524-A-58 and 1524-A-50 were mixed in proper ratio with #2 OH acrylic (1524A6) which proved to have excellent acid and alkali resistance. A paint using #2 acrylic has been made and panels are In the process of being prepared. Following are the proposed schedules using Desmodur N, Desmophen 650 as control. Sch. 265 - 1st Coat - Y5251 Nu-Pon Cote Primer 2nd Coat - EGL-65415 Durable Urethane/Desmodur N 3rd Coat - Sch. 266 - 1st Coat - Y-5251 Nu-Pon Cote Primer 2nd Coat - EGL-65415 Durable Urethane/1524a -58 3rd coat - " " Sch. 267 - 1st Coat - Y-5251 Nu-Pon Cote Primer 2nd Coat - 19-A-26 #2 Acrylic/1524A-58 3rd Coat - " "" Sch. 268 - 1st Coat - Y-5251 Nu-Pon Cote Primer 2nd Coat - 19-A-26 #2 Acrylic/1524A-50 3rd Coat - GLD 045602 TM-54 ACTIVE BUT NO REPORT DURING CURRENT MONTH NM24009M2122 - Sinclair NM24011M2222 - Semi-Gloss Water Reducible NM26006M2322 - External Pipe Coating NM27004M2122 - General better NM27005M2222 - Zinc - Phenoxy Primer NM28008M2121 - Krotan NM28009M2122 - BMX Blocks SM25001M2219 - Water Reducible Government SM25002M2219 - Water Reducible Anti-Fouling CLOSED DURING MONTH NM28013M2722 Bendix Panels - Closed 12/11/67 J GLD 045603 CAN COATING LABORATORY INDUSTRIAL PRODUCTS December, 1967 SUBJECT: PRODUCTION CONTROL - CLEVELAND (REACTORS) - SI23009I1103 SUMMARY: We received a wet sample of VR-61015-A, P-371785 from Crown Can's Orlando factory. Our tests showed: 1. This sample did eyehole badly as the customer had reported (worse than our retain). 2. No contamination could be found by infra-red analysis and physical examination showed nothing -unusual. 3. Addition of Modaflow solution VR-67022 (20 liq. oz. per 55 gal. drum) was effective in overcoming the eyeholing condition. Mr. Moyer of Crown Tech. Service and Mr. Keefe of our Atlanta plant were advised of these findings. Mr. Keefe will arrange to supply Orlando with the necessary amount of VR-67022. SUBJECT: PACK TESTS - WHITE ACRYLIC SANITARY ENAMELS - NI28005I1103 SUMMARY: Our laboratory test packs on the white acrylic sanitary enamels are now completed (initial, 6 weeks @ 120F., 12 weeks @ 120F.). All the test ends were reviewed by Mr. Hafeli and resin lab personnel. Detailed gradings are available and will be written up in a final report. General conclusions and inpressions were: 1. SW-7099 and EGL-67350 are about equal in performance, with EGL-67426-A definitely inferioi to the other two. 2. This basic type enamel will be suitable for selected products only (no bad staining products). 3. More work will be needed (if the market for this type product warrants it) to check out performance in other areas. a. Enamel and resin modifications. b. Other plate surfaces (TFS). 4. Competitive white enamels and conventional controls should be run for comparison. SUBJECT: PREPARATION OF SAMPLES AND EXHIBITS - NI24035H103 SUMMARY: We evaluated three enamels on Weirchrorae TFS for process resistance in a pumpkin pack. a. VR66030 (epoxy-urea) b. EGL68392 (acrylic) c. VR55102 (oleoresinous) GLD 045604 1-2 These enamels were selected mainly because the customer (Campbell Soup) desired a baked film with minimum color. Rather surprisingly all enamels passed the processing test with almost perfect ratings. Gallon samples of each coating were made up and submitted to Campbell. Future work is planned to investigate other types of TFS, short bake schedules, and extendec pack resistance. SUBJECT: PAINT CAN LINER FOR SPRED SATIN - NI27053I1203 SUMMARY: We have screened several more lining types for Spred Satin resistance. Thes* included resol phenolic (Ciba), low-bake phenolics (Varcum and UCC) double coat systems (epoxy size, epoxy-phenolic topcoat) and Crown Can #920 lining. None of these linings approached the resistance we have obtained with National Can #7701 on our screening test (half-filled cans @ 120F.). As noted before, #7701 is not a completely satisfactory solution to this problem because of the solvent-soluble dye used as a colorant. In addition, we have heard that National Can would like to see a less expensive coating than #7701. (This fits in with our analysis as a methylon type). Future work on this project will be guided by Messrs. Hafeli and Kingston after they have reviewed results to date. SUBJECT: SAMPLES SUBMITTED - DECEMBER, 1967 DATE 12/12/67 12/12/67 12/12/67 12/13/67 MATERIAL #55102 Sanitary Enamel #66030 Clear NuPon #68392 Acrylic #67022 Flow Control FORMULA VR55102 VR66030 EGL68392 VR67022 AMOUNT 1 gallon 1 gallon 1 gallon 1 quart CUSTOMER Campbell Campbell Campbell Federal Tin CONTRIBUTORS: A. Kukuca, G. TUlk GLD 045605 1-3 LITHO COATINGS LABORATORY December, 1967 SUBJECT: REGULATION #3 REVISION OF VR63013 - CROWN CORK S SEAL CO. - NI27054I1203 SUMMARY: VR67043 has been formulated to meet Regulation #3. The sales department also requested a Rule 66 modification of this formula to furnish to Los Angeles clants, VR67049 has been developed to meet the solvent regulations of Rule 66. This DPR will be returned. SUBJECT: VACRALIN - GENERAL SALES - NI24115I1303 SUMMARY: 1. Vacralin VR-67023 lined cans have been stored at the Research Center for three months at 120F. packed with Orange Drink, Black Cherry and Strawberry Soda. Previous pack openings have shown little change in the can lining or in the product packed. However, after three months storage the Vacralin films now are severely blushed while control cans lined with a commercial vinylite coating (VR67019) show no signs of attack. 2. Two gallons of VR-66014 were prepared in the lab and sent to Aluminum Company of America Pittsburgh laboratory. SUBJECT: PREPARE EGL67350 SAMPLE - CANADIAN CANNERS - SI28070I1103 SUMMARY: Five gallons of EGL67350 white sanitary enamel were made in the laboratory and shipped to Mr. B. Miller in Toronto. SUBJECT: WET INK VARNISH FOR BEVERAGE CANS - GENERAL SALES - NI28006I1303 SUMMARY: Five stearic acid alkyds were evaluated to determine if increasing the oil length or changing the method of cooking would improve the flow of the varnish. None of these revisions improved the flow, but incorporating ethylene glycol as part of the polyol and changing the PE/glycerol ratio stabstantially improved the flow. However, the film hardness was only fair. Three tall oil alkyds (V-2347, V-2373, V-2352) a soya (V-2254) a DCO (V-2462) , a coconut (V-2712), and a castor oil alkyd (F-2777) were evaluated with 20% melamine modification to determine which has the best propeorties for a wet ink varnish. The V-2352 tall oil alkyd had the best combined properties of adhesion, film toughness, and mar resistance. The flow of the varnish was only fair since the alkyd contains xylol. Replacing the xylol in the alkyd with Solvesso 150 gave good flow when rollercoated. The initial color and color retention of the alkyd melamine varnish are as good as the stearic alkyd used by Heekin. Mr. Greulich was advised of our test results. We hope to get a trial run at Heekin Can for a thorough evaluation of this vehicle. GLD 045606 1-4 SUBJECT: LOW COST WET INK VARNISH - GENERAL SALES - NI28011I1303 SUMMARY: Two rosin modified tall oil alkyds (SX5-35 and SX5-44) prepared by the Central Resin Lab were evaluated. Both alkyds; had poor mar resistance and poor toughness. A current production tall oil alkyd (V-2373) has been evaluated with various driers to develop good hardness. The addition of 0.06% Zirconium gives a hard mar resistant film witl excellent color. The alkyd, however, is too high in viscosity to give a varnish with 40-50' #4 Ford cup viscosity at 50% N.V. Two competitive alkyd varnishes were tested and show excellent hardness, mar resistance, adhesion and color. This Ford cup viscosities are 42" and 60" at approximately 50% N.V. In order to compete with this type of varnish, an alkyd must be developed with a viscosity of W-Y @ 60% N.V. in mineral spirits with a maximum color of five. It will also have to cure to a good hard film without the addition of amine resins. SUBJECT: COIL COATING CONTAINERS - GENERAL SALES - NI26018I1303 SUMMARY: Last month we reported that our Gold EGL68342 drifted considerably in color when applied by reverse roll coat at Enamel Products on November 15th. By replacing the Microlith Red RT with Microlith Red BRT color stability of the coating under shear was greatly improved. The plate coated at Enamel Products and fabricated into containers at Campbell Soup failed on processing (250 60 min.). The customer's tests also indicated that the higher the film weight, the poorer the process resistance. Production coated plate at film weights of 11.6, 14, and 22 mgm/4 sq. in., fabricated into domes on the Eriehsen testing unit here at the Research Center and processed were satisfact It was necessary to bake the gold at 525 for 120 sec. to produce process failure on our equipment and our recommended bake of 525 for 60 sec., and also at 525 for 80 sec. proces resistance of the system was excellent. By reducing the epoxy to acrylic level 5% we improved the bake stability of the coating; a decrease of more than 5% resulted in bad blocking of the coated stock. A competitive gold will be run at Campbell and future action on our part will depend upon the outcome. SUBJECT: NEW VEHICLE DEVELOPMENT PROGRAM - NI16011I1303 SUMMARY: The following acid acrylic resins were checked as white roll coat enamel vehicles, 1572A-9, 1572A-1, 1572A-11, 1572A-13, 1572A-34, 1572A-39, 1572A-57 1572A-58 in a project aimed at developing an enamel with better flexibility and block re sistance than EGL67426-B (based on RCR6318 and RCR6319). GLD 045607 The control systems in these tests was EGL67426-B, and screening tests were fabrication into screw caps (dry heat, C14SO4 immersion) and blocking resistance (80#/sq. in. @ 110F.: 11515F2 .*/*15 min.). All resins were checked at: 1 Pigment binder ratios of 60:40, 55:45, 50:50, 45:55%. 2. Epoxy levels of - 25, 20, 15, 10%, 3. With epoxy molecular wt. variations - F-5161, F-5106, F-5158. 4. With and without BDMA (Benzyl dimethyl amine). None of the resins produced a coating equal to EGL67426-B. The best system was resin 1572A-39 (RE23302) at 50:50% pigment, vehicle and 26:74% epoxy to acrylic ratio but it was inferior to EGL67426-B in fabrication. SUBJECT: REVISE VINYL COATINGS FOR RULE 66 - NATIONAL CAN CORP. - SI2709311203 SUMMARY: 1. Five gallons of VR67037 Rule 66 type vinyl spray were prepared in the laboratory and shipped to National Can's Long Island Plant for a trial run. 2. Several solvent suppliers are working with B. F. Goodrich to formulate Rule 66 conforming solvent systems for Geon 222 resin. This work is intended to provide us with solvents to allow reformulation of VR61153 and VR61154. Mr. Prout and Mr. Jimenez of Goodrich visited the Research Center on December 6, 1967 and gave us several suggested solvent combinations resulting from their program. These solvent blends are being evaluated in our VR61153 formula. SUBJECT: PRESHIPMENT SAMPLES TESTED Geon 222 Resin S6171 Resin Soln. Atlanta Vinyl Prod. Toronto Vinyl Prod. Central Enamel Prod. 3 lots 2 lots 2 lots 1 lot 2 lots SUBJECT: SAMPLES SHIPPED 1-5 1-1/4 1-5 1-1 2-1 1-1 VR67037 Beer Can Body Spray VR67046 Clear Can End Varnish EGL67350 White Sanitary Enamel VR65043 Vacralin VR66014 Vacralin Spray Liner VR65044 Wet Ink Varnish National Can (Long Island) Nubian (R. E. Meyers) Toronto (B. Miller) Reading (J. P. Harner) Alcoa International (Bush) SUBJECT: DLR'S ACTIVE BUT NOT WORKED ON NI25026I1303 NI26003I1303 NI27035I1303 NI27042I1103 NI27048I1303 SI27153I1203 Owens-Illinois Closures Coatings for TFS New Geon Resins Vacralin Taste Program Varnish for Miraseam Can Revise EGL65437-A CONTRIBUTORS: W. E. Reich, W. R. Armstrong, R. L. Mandley, R. L. Toth, J. Rebar, R. Woodruff GLD 045608 1-6 INDUSTRIAL WOOD COATINGS LABORATORY December, 1967 SUBJECT:: PAPER IMPREGNATION - NI26022I4308 SUMMARY: In our continuing search for improved properties of the decorative laminates we have been investigating various monomers. The monomers looked at in this last series consist of several "buy-outs" and some experimental systems prepared by the Resin Research Group. Monomers tested were substituted in EGL68300A as a direct replacement for RCR3024 (patent situation). Impregnated papers were prepared and laminated six monutes at 260F. and 200 psi. MONOMER AND MANUFACTURER RESULTS t-stibbene - Shell Chemical para-Diisopropenyl benzene - Shell Monomer X-980 - Acrylic - Rohm fi Haas Monomer X-970 - Acrylic - Rohm & Haas Tri Vinyl Benzene Di Methyl maleate 1316A24 - Epoxy Acrylate - Glidden 957A10 - Epoxy - Acrylic Acid - Glidden 1512A31 - Epoxy Acrylate - Glidden Incompatible Incompatible Paper too tacky Paper too tacky Poor Cure - No mar resistance Poor cure - no mar resistance Bad pitting in laminated film Poor cure - no mar resistance Pure cure - no mar resistance None of the above monomers showed much promise and the epoxy-acrylic types, which with some modification might be interesting are higher in cost than our present system. As reported previously we have been looking for a resin system which will contribute less color in clear overlays and on light colored laminates. Although RCR4238 type resin does give us much better color but a softer film, so it was decided to investigate the manufac turing procedure of RCR4247. A sample of RCR4247 (1253A79) was prepared by the Resin Group which was considerable lighter in color. This sample was prepared by the same procedt: as used in the manufacture of RCR4238. Sample 1253A79 was substituted in EGL68300A as a direct replacement for RCR4247. Clear paper was impregnated and laminates were made over a white background along with our standard clear overlay. The new resin produced a much lighter overlay. If 1253A79 cam be manufactured in the Plant in large volume to the same specifications as the laboratory sample we should have no further complaints about color. SUBJECT: EXTERIOR PREFINISH SYSTEMS - NI27037I4308 SUMMARY: Exterior exposures of wood and, plywood panels sealed with a Polyurea sealer have shown us that durability is greatly improved. The sealer is a low solids wash coat or dip. We have extended this idea as an edge sealer for hardboard, with considerable promise. Polyurea edge sealer not only reduces the amount of water that soaks into the cut edge of the panel, but also controls the edge cracking and delamination of the panels. GLD 045609 1-7 We have coded the 15% N.V. solution EGL68448 Polyurea edge sealer, and EGL68449 converter. SUBJECT: TIBBALS FLOORING - NI28000I4108 SUMMARY: December 14. Because of the excellent abrasion resistance shown by EGL68303 clear Poly-Lure we conducted a test on the Tibbals finishing line at Oneida, Tennessee on The system was as follows: Filler Sealer Topcoat GP53382 type RGL19205 EGL68303 The sealer performed in a satisfactory manner. There was a slight increase in viscosity on the roll, probably due to loss of solvents. The filler obviously did not have the proper solvent system for this line. When the solvent was slowed down with Solvesso 150 to correct poor cleanup, we got blistering and popping. The topcoat EGL68303 Poly-Lure, did not cure completely on the Tibbals line. The lack of cure was evident from the slight hot-tack and lack of hardness in heavy areas. Tibbals will run a blocking test, print test, and wear test on the samples run. The results will be sent directly to the lab. We plan to investigate the filler situation more completely, as we suspect that we did not have standard material. We plan to improve the speed of cure on EGL68303. SUBJECT: NAHB EXHIBIT - NI2803H4108 SUMMARY: booth. The 1967 show was at the International Amphitheater in Chicago. This was the first year that anyone from the Ind. Wood Coatings Section had worked in the In addition to the Polyester bath tub, the item which attracted the most interest was the Poly-Urea coated window. Representatives from nearly all of the large mill-work companies stopped to discuss the window. The reaction was so general that it indicates the industry must be under considerable pressure to come out with completely finished windows. The Decolure panels and the pre-finished hard-board siding attracted considerable attention during the first two days of the show. When the contractors and builders arrived, they were mare interested in the block fillers and trade sales items. GLD 045610 1-8 SUBJECT: SUMMARY: SUBJECT: SUMMARY: TRIPS DURING, DECEMBER December 3, 4, 5 J. Watson to NAHB, Chicago December 6,7 D- Raymond to NAHB, Chicago December 14, 15 B. Payne to Tibbals Flooring, Oneida, Tennessee SAMPLES SHIPPED DURING DECEMBER 12/14/67 to Matt Andrews, 17100 Vein Aken Blvd., Shaker Hts, Ohio 1 qt. EGL68422 Polyurethane 1 qt. EGL68423 Converter 12/26/67 to P. C. Herzog, Portland, Oregon 1 qt. EGL68300A Impregnating Resin CONTRIBUTORS: J. Watson, D. G. Raymond, B. Payne, J. Kerby ; GLD 045611 1-9 AUTOMOTIVE. LABORATORY December, 1967 SUBJECT: IMPROVED BLACK FLOWCOAT PRIMERS FORD MOTOR CO. - SI27168I7207 GENERAL MOTORS CORP. - SI28011I7307 SUMMARY: Evaluation of Central Region Resin Laboratory resins formulated specifically for this project continues. Primary goals are an alternate for F-467 at equal properties and a resin providing improved properties over GRV3480. None of the resins received during the month met these requirements. ' Ford Motor Co. requested information on effect of isopropanol on film build of XM64463-C Black Flocoat Primer. Study was made and results reported. Ten gallons of XM64463-C in which isopropanol replaced part of the water were made and shipped to Ford. SUBJECT : IMPROVE THROWING POWER. AND SALT SPRAY RESISTANCE OF BODY ELECTROCOAT GENERAL AUTOMOTIVE - NI25032I3207 SUMMARY: 1. Slimetrol RX-16 was evaluated as a biocide in EXM67141 bath and found effective. No deterioration of resistance properties was observed. However, a few pinholes developed on throwing power strips run in baths with Slimetrol. This must be checked further. 2. A new approach to a hard resin additive to maleinized oils to upgrade throwing power, corrosion resistance, and gravelometer was initiated. Specific resins made and evaluated were the monoester of Epon 1001 and diphenolic acid, and the mixed diester of Epon 1001, linseed F.A., and diphenolic acid. The monoester proved too reactive with maleinized oils. The diester with maleinized oils yielded electrodeposited films having excellent corrosion resistance on Bonderite and excellent gravelometer, but poor corrosion resistance on C.R.S. Further work on this is planned. 3. Variations of GRV3485 with other resins substituted for F-467 were evaluated and judged not as good. 4. A variation of GRV3485-in which linseed replaced soya and methacrylic acid was increased to 6% showed significantly improved gravelometer resistance. This will be pursued further. 5. A series of four Epon 1004 linseed F. A. esters differing only in the amount of carboxyl introduced through half esterification with tetrahydrophthalic anhydride was evaluated. Ease of solubilization decreased with increasing acid value. The lowest acid value was 42. Those which could be solubilized showed excellent gravelometer and salt spray resistance on Bonderite and exceptional salt spray resistance on unphosphated steel. Sufficiently smooth films on throwing power strips could not be produced,. thus salt spray exposure of these was not run. Baths are being held for observation to establish hydrolytic stability of this type resin. ! 6. Steam hydrolyzed RCR1G70 was evaluated against RCR1070 hydrolyzed in the customary manner with triethylamine and water. EXM64098 samples made from each showed no differences. GLD 045612 I-10 7, Ion exchange treatment of Monroe wheel tank bath was repeated with Dowex 21K in place of Dowex 2X8 as reported in November. Again, no decrease in coulombs per gram was observed, thus introducing a question of whether anionic contamination is a significant factor in the poor electrical efficiency of #70 quality baths at steady state. The next approach planned is a study of different ratios of diisopropanolamine and diethylenetriamine in EXM64090 to determine effects on coulombs.per gram. SUBJECT: ELECtROCOAT FOR GASKETS - DETROIT GASKET CO. - SI28014I3307 SUMMARY: 1. Several other resins were evaluated for resistance to excessive hardening during the five hours at 350F. heat test. None showed any promise. 2. Antioxidants were found ineffective in preventing heat hardening. SUBJECT: TESTING SAN FRANCISCO BATCHES OF K-187 and XM64463-C SUMMARY: XM64463--C P-33373 was tested and approved. SUBJECT: XM67815 ALUMINUM E/C - FORD MOTOR OF ENGLAND - LN18006I3315 SUMMARY: 1. A revised formulation made with dry aluminum powder rather than solvent- wet aluminum paste was made. Metallic brightness was significantly better than that of the original. 2. A study of various solvents in the formulation showed that best metallic appearance resulted from butyl cellosolve and that metallic appearance decreased with decreasing miscibility op the solvent. 3. Temperature at which GHV3389 and GRV3390A are blended was shown to have considerable effect on color. Lower temperature is preferable. 4. A two package maintaining system showed satisfactory solubility 'characteristics. 5. Pump stability testing resulted in some loss of color but little film thickness loss. Color change prevention will be attempted through increasing aluminum content. 6. Conventional methods of pigment to binder ratio determination have proven useless because of partial conversion of aluminum to the oxide during ashing. Separation by filtration or centrifuging was unsatisfactory. A new technique being developed depends on conversion of the aluminum to aluminate through reaction with aqueous diethylamine and subsequent ashing to yield aluminum oxide. SUBJECT: GLOSS AND FLAT BLACK CHROME TRIM ENAMELS - TERNSTEDT - SI28035I7307 and SI28036I7307 SUMMARY: 1. Replicate panels of XM67819 prepared here were exposed simultaneously in Temstedt's and Central Region's humidity cabinets. Only the panels in Temstedt's cabinet, which is a true condensing type, failed. Triple the normal exposure of 96 hours in the local cabinet still did not cause failure. Also exposure in the Cleveland Condensing Humidity Cabinet did not cause failure. GLD 045613 1-11 2. Initial evaluations of a gloss black made from acrylic resin 1522A23 and Cymel 301 produced satisfactory results. Cratering which is a problem with other low bake gloss blacks, was not evident. Work on this will continue after a means -for duplicating failure in the Ternstedt humidity cabinet is found. SUBJECT: IMPROVED ANTI-FOAM SYSTEM FOR XM64407 - WALKER PARKERSBERG - SI18020I7215 SUMMARY: Screening of anti-foamers has begun. SUBJECT: FLAT BLACK E/C ENAMEL - TRICO - SI28066I71Q7 SUMMARY: A black electrocoat enamel was formulated in #83 quality with N-326 Syloid included to Control 60 gloss between 10 and 15. Earlier attempts with surface treatment sylbids resulted in waxy float on the bath surface, a condition not apparent with the untreated N^326. Trico windshield wiper assembly components will be coated and returned to the customer for evaluation. SUBJECT: LETTERS NOT WORKED ON SUMMARY: LN17029I3207 SI27164I7115 SI27162I7315 SI27163I7315 SI27165I7115 NI2702013307 SI28012I3307 LN18007I3115 Merville & Morgan - Peugeot Primer Lear Siegler - Testing Gibraltar Steel - Strap Coatings U. S. Steel - Black Strap Coating Production Plating - Testing Ford - Upgrade EXM64090-C General Motors - E/C Sheet Metal Primer General Industrial Paints - EXM67141 Sample SUBJECT: SAMPLES SHIPPED SUMMARY: XM64463C (Special with S-88) - 2 - 5's - Ford Motor Co. EXM68069 Black #83 Electrocoat - 1 gal. - Research Center (for Tecumseh) Seven Sets of Steel Strap in Six Colors - Gibraltar Steel SUBJECT: TRIPS SUMMARY: J. E. Ruecke - General Motors, Detroit - 12/1/67 Master Lock Co., Milwaukee - 12/6-7/67 CONTRIBUTORS: J. E. Ruecke, R. Hordusky, P. V. Kunz, R. Bukowski, D. Allen, R. Markus GLD 045614 1-12 ELECTROCOAT FORMULATION AND DEMONSTRATION LABORATORY " December, 196? SUBJECT: DETERGENT RESISTANT PRIMERS - ACRYLICS - NI27045I33Q4 SUMMARY: 1. Work has continued on the development of an acrylic laundry primer to meet Whirlpool specifications. The following areas are being investigated for improvement of detergent resistance. a. Styrene Levels - By going to high styrene levels, acrylic systems can be made to pass the detergent and salt spray portions of the specifications. However, these systems are lacking in the flexibility required by the specification. b. Lowering acid no. - This approach has been found to improve detergent resistance. The limiting factor here is the acid no. required to give the stability and solubility needed for a practical system. s c. Melamine levels - The optimum level of Cymel 301 has been determined for best detergent resistance. d. The incorporation of a hydroxyl monomer (HPMA)-the use of the above monomer has been found to improve detergent resistance with a slight loss in flexibility. The optimum level has yet to be established. e. Replacing Cymel 301 with Benzoguanamine Formaldehyde resin - This approach has resulted in improved detergent in some instances where a direct comparison has been made with Cymel 301. Improved flexibility definitely has been obtained with the B. F. resin. The optimum levels have yet to be determined, also the effect of cooking the B. F. resin in the acrylic portion. SUBJECT: DETERGENT RESISTANT PRIMERS - EVALUATION OF F-467 SUMMARY: There had been some indications that F-467, a new phenolic resin, if put into the RCR1083 cook in place of F-460, might provide equal or better detergent resistance and also stop the phenolic bleed through problem which occurs when Whirlpool's EXM66072-A is topcoated with white. A very exacting experiment incorporating three bake schedules was run comparing RCR1083 with F-467 against std. RCR1083 with F-460. No signifi cant difference was found between them in salt spray, pencil hardness, impact and conical mandrel. The detergent resistance of F-460 was much better than that of F-467. it averaged out over 12 conparisons to be 43% better. The F-460 gave slightly less bleed through than F-467 although the untopcoated primer based on F-467 had a much cleaner color. On the basis of this experinient, no further work will be done with F-467 in detergent resistant systems. A full, detailed report on this experiment will be issued. Initial screening has been begun on a maleinized oil-epoxy primer. GLD 045615 1-13 SUBJECT: WHITE ROGERS DIVISION 6f EMERSO& ELECTRIC - SI28058I3312 SUMMARY: A #106 Gray has been formulated for the above customer. The color is #26251 Federal Standard 595. The main requirements are 75-90 gloss, H Pencil Hard- ness, 200 Hrs. salt spray, and 350 - 500 hoars humidity resistance. Of our current resin systems, RCR2106 best fulfills the above requirements as far as properties are concerned., The starting material number is EXM68097. The substrate specified is iron phosphated steel. SUBJECT: SUMMARY: THE WIRBMOLD COMPANY - SI28059I3315 A #102 quality tan starting material, EXM68098, was developed to match the customers color and gloss. Eight gallons were made to coat customer parts. SUBJECT: SUMMARY: ST. LOUIS SERVICE LETTER - SI25178I3115 Technical service was provided Medart Locker on a throwing power problem with their gray tank. SUBJECT: SUMMARY: MIDWEST SERVICE LETTER - SI25187I3115 Technical service was provided to Carnes Corp. on a contamination problem with their white tank. SUBJECT: SUMMARY: READING SERVICE LETTER - SI25176I3115 Several batches made in Reading were tested here. EXM67038B P-101723 - Had inadequate solubility K-1632 P-617583 - Approved K-1632 P-617589 - Approved EXM67025-C P-101793 - Approved SUBJECT: NATIONAL SERVICE LETTER - NI24056I3115 SUMMARY: A program of tightening electrocoat manufacturing quality control tests was initiated. The first "Electrocoat Manufacturing Quality Control Bulletin" was issued. It described the tentative "Deionized Water Reduction & Filtration Test" for feed materials. This is a factory test method for determining whether a production batch of electrocoat feed material has adequate solubility. SUBJECT: SOLVENT FREE ELECTROCOAT ENAMELS - NI27057I3315 SUMMARY: RE22356, Work has begun on developing a solvent-free acrylic. Several resins have been evaluated but they did not deposit properly. These were: RE22355, and RE22357. GLD 045616 1-14 SUBJECT: RCR2106, DEVELOPMENT PROGRAM - NI25005I3313, NI17015I3315, NI27030I3315 SUMMARY: #106 quality turnovers have been conducted on two colors, the General Electric Gray #65194, and the V. E. Anderson White #66051. The G. E. gray turnovers were an attempt to convert a #102 quality tank into a #106 quality tank by introduction of #106 quality feed material. The V. E. Anderson turnovers were an attempt to convert a #104 quality tank into a #106 quality. The appearance of craters has forced both these turnover runs to be discontinued. Apparently, the cratering was caused by the introduction into the tanks, at about 1.5 turnovers, of inadequately mixed gallon batches of feed. #106 quality seems to require better mixing than the #102 quality does. If a bate1 of #106 feed that causes cratering is given additional mixing time or allowed to age about one week, it thins down in viscosity and when introduced into the tank does not cause cratering. To be absolutely certain that the cratering is not intrinsic to mixing #106 with #104 in certain proportions, a second V. E. Anderson turnover run has been started. I This run is using a gallon batch of feed which has been provided to be non-cratering by use during the first V. E. Anderson turnover run. This feed will be used for five turnovers which will bring the tank to a composition of 99.5% #106 quality. If cratering is due only to sub-standard feed, then no craters should appear from 0 to 5.0 turnovers. Note: Low mol. wt. electrocoat resins tend to crater. I Formulation work was begun on a family of #106 quality aluminum extrusion coatings. In trying to raise the B/P ratio it was found that the material had excessive flow. Because I of this and because of difficulties experienced in maintaining voltage stability on steel in certain formulations, we have decided to evaluate higher molecular weight "RCR-2106's." 1 An eight resin, full factorial experiment has been initiated by the resin lab apd ourselves. 1 Most further work on #106 quality aluminum extrusion coatings will be set aside until the high mol. wt, experiment is complete. Three pilot plant batches of RCR2106 have been manufactured. The batches were all quite similar in properties and it appears that we should be able to make the resin successfully. DEMONSTRATIONS SERVICE TRIPS I Singer Company G. E. - Ft. Wayne PARTS AND PANELS International Oil Burner Bendix Corp. John Deere Kewaunee Mfg. Maytag Co. Master Lock Co. Bonnel Co. 12/5 - S. Hinds to S.P.S., Hatfield, Pa. 12/13 to 12/16 - L. Mambuca to Carnes Corp. Verona, Wise. I i CONTRIBUTORS: D. Thrane, J. Erickson, L. Petrak. A. Figoli, D. Shuster, P. Kunz, R. Smego, S. Hinds, L. Mambuca, R. Bair GLD 045617 1-15 f t .r c t r OCO&TING LABORATORY December, 1967 SUBJECT: PATENT WORK SUMMARY: Patent investigations on British patents #665195, #482548 and Japanese patent #144755 were completed. These patents were cited by Japan patent office against the basic electrocoat patent application by Ford Motor Company. British Patent #665195 concerned special alkyd compositions. British Patent #482548 concerned shellack solutions. Japan patent #144755 concerned a Urushiol resin solution. Data was prepared in affidavit form and taken to Japan by Mr. Douthitt. Together with the above data, the electrical equivalent weight of RCR1083 was again determined as an example of our basic electrocoat resin for comparison to other resins. SUBJECT: CHROMATED FATTY ACID SUMMARY: inves tigated. Investigations were carried out on solubilization of fatty acids with chromic acid. A patent disclosure was prepared to cover the data and principle SUBJECT: VARIATIONS OF EUROPEAN AND U. S. RCR1070A' SUMMARY: Investigations were made on five sairples of RCR1070A (Wulfing 10049) resins and two samples of RCR1070A (Salchi SR-53) resins together with four samples of RCR1070A (U.S.) resins. The purpose of this work is to discover reasons for production resins variations found in our recent international electrocoat ooperations. Raw materials as well as process variables are being investigated. SUBJECT: BLACK PRIMER SUMMARY: Work on developing a new black electrocoat primer has been delayed pending preparation of the new resins requested. SUBJECT: TRIPS SUMMARY: None CONTRIBUTORS: A. E. Gilchrist and W. Lehman GLD 045618 COATINGS RESEARCH DECEMBER, 1967 SUBJECT: 100% SOLIDS - NT17002C2376 SUMMARY: Recent results show that diallyl maleate is non-volatile only in the poly ester system and not with alkyds. Therefore variations of the butyral poly ester were prepared to overcome the short, brittle nature of these films. Two variations were made using diethylene glycol at different ratios with maleic anhydride: 1512A2Q resin with 4/3 ratio DEG/MA and 1512A21 resin with 6/5 ratio DEG/MA. Both resins were very poor drying, requiring more than eight hours for set-to-touch. 1512A16 resin was made with TMP in place of ethylene glycol. ably well and is being tested further. This polyester dried reason NEW SOLVENTS Bis (2-vinyl 4-hydroxyethyl) 1,3-dioxolane: Poor solvency and poor drying. Allyl butyl maleate: Reasonable odor and solvency, good drying but with some residual tack. Slower curing and less brittle than diallyl maleate. DiAllyloxyethyl Maleate: Very reactive. Solvent alone gelled in two days without catalysts. It is proposed to attempt to use this structure in the design of new polyesters. SUBJECT: WATER BASED ZINC RICH WELDING PRIMER - SI28022I7307 SUMMARY: A 25 hour study was carried out to determine the feasibility of making a water based welding primer for automotive use. It was concluded that no single package water based vehicle currently available will pass the wash-off test involved in the cleaning and phosphating process prior to baking. Various latex systems were tested and good films were produced. The precipitation of the latex by zinc dust was overcome by pretreating the latter with ammonium dihydrogen phosphate The latex systems did not gas excessively or gell after two weeks. Further tests are in progress to determine the stability of these systems since they may be of value in other are CONTRIBUTORS: R. Gray, P. Abel. GLD 045619 CR-2 SUBJECT: WATER SOLUBLE AUTOMOTIVE METALLICS - NI27021C13Q7 SUMMARY: Several melamines were evaluated for physical properties with a particular interest in the improvement of gloss of water soluble automotive metallic enamels. Melamine QR-483 (Rohm and Haas) gave a measurably better gloss than Resimene 730 while being fairly equal in other physical properties. QR-483 appears to be more compatible with the 10% hvaroxypropyl methacrylate (HPMA) and 10% acrylic acid modified acrylic polymer (RE23178) that we are currently working with. Melamine 27-400 (RCI) showed some interesting properties. The cure at a 30 minute bake at 250F. was poor but the cure at a 30 minute bake at 300F. was slightly better than the Resimene 730 cure at 250F. The gloss of the higher bake was fairly similar to that of QR-483 but with improved , flexibility. Perhaps an acid catalyst might improve the cure while maintaining the other properties. Melamines RI-2027 (Monsanto) and 27-065 (RCI) had very slightly better cures than Resimene 730 but were slightly more sensitive to popping. 27-065 was also slightly less flexibile. Resloom M-75 and Resloom M-80 (Monsanto textile melamines) were faster curing and slightly less flexible. Resloom M-80 had slightly better gloss but was slightly more sensitive to popping. Stability results will determine whether further study should be done on these two melamines. MD-588 and MD-788 aluminums (Alcan) and 7290 aluminum (Alcoa) were treated to impart water dispersibility. They are being checked for stability. MD-588 and MD-788 have similar appearance and gloss to MD-5079 (Alcan water dispersible aluminum). 7290 aluminum is noticeably finer in particle size, grayer and glossier than MD-5079. L-478 (Silberline water dispersible aluminum) was found to be slightly finer in particle size, grayer and glossier than MD-5079. Lt 478 falls between MD-5079 and 7290 aluminums in the above properties. The stability is being checked. j 1 Phthalo blue and carbon black pre-dispersed pigments (powder form) from Holland-Suco were checked for use in tinting pastes. The dispersions were cut into pastes on a mixer. The black paste had a good dispersion and produced a very good gloss in a black enamel. The blue paste was slightly seedy bbt gave good gloss in a blue metallic enamel. Perhaps a better cutting procedure can be found for the blue dispersion. Larger samples have been ordered for further investigation. |J j > In an effort to improve the gloss of the white enamels Titanox CLNC (National Lead) was substituted for TiPure R-960. This produced a noticeable increase in gloss. The additional substitution of QR-483 melamine gives a white enamel with very good gloss. A ten percent addition of Lustrasol 13-402 (RCI water soluble thermoplastic acrylic) was made to the vehicle of a metallic enamel for better oven flow and gloss. The addition produced a lower gloss so it would seem that Lustrasol 13-402 is not conpatible with our vehicle. Diacetone alcohol substituted for butyl cellosolve acetate produced a lower gloss metallic enamel. Tertiary amines, which give better package stability to water soluble enamels, have contribu ted to objectionable popping. Diethyl ehtanolamine (a tertiary amine) was tried in the neutralization of a 6% acrylic acid and 10% HPMA modified acrylic polymer. There was noticeably less popping (not quite free of popping) than when used with a 10% acrylic acid and 10% HPMA modified acrylic polymer. There was a noticeable pH drift, however, that was not encountered with other tertiary amines which have been tried. CONTRIBUTOR: K. Coleman GLD 045620 CR-3 SUBJECT: SUMMARY: SILICONE ACRYLICS - NI26035I2311 Some significant weatherometer studies are now becoming available and are giving some indication of the durability to be expected. RE22898 RE22898 S Silicone 60 Gloss at 1200 hrs. = 17 chalk started at 1200 hrs. 60 Gloss at 1200 hrs. - 75 chalk started at 2600 hrs. RE22899 RE22899 & Silicone at 1600 hrs. = 36 gloss at 1600 hrs = 71 gloss RE2290Q RE22900 & 10%/Z6018 RE22900 & 25%/Z6018 at 1000 hrs. = 72 gloss at 1000 hrs. = 81 gloss at 1000 hrs. = 82 gloss Exterior durability data is not yet available. The above results are obtained from cold blended systems. More recent resin systems have the silicone intermediate reacted with the acrylic. The latest of these is an acrylic having a composition in between RE22899 and RE22900, This resin was then reacted with 10% and 25% Z6018 to produce RE23210 and RE23211 respectively. These two silicone acrylics have, to date, shown the most promise. For example, an enamel based on RE23210 (10% silicone) with 5% of plasticizer produces films curing at a PMT of 450 and having H hardness, 3T flexibility and 30"lbs. impact resistance. On the other hand, RE23211 (25% silicone) with 10% plasticizer will produce a film curing at 450-470F. and having F+ hardness 2T flexibility and 20"lbs. impact on Alodine 1200S treated aluminum. Both full and 30 gloss are being exposed in the weather ometer, Florida and Cleveland. A range of colors have been produced with success in the high gloss systems. These have also been exposed in the weatherometer, Florida and Cleveland. The present work has been confined to an aluminum substrate but further work with different substrates is scheduled. Some enamel costs have been evaluated and it would appear that selling costs on a solid film basis would be in the order of 0.9$ for the 10% silicone acrylic to 0.96C/sq.ft./ml for the 25% silicone acrylic enamel. SUBJECT: COIL COATING CONVENTIONAL TYPE SIDING FINISH SELF-CURE ACRYLICS RCR6322, Self-Cure Thermosetting Acrylic SUMMARY: Further work was curried out with composite grinding of black pigments with DuPont's titanium dioxide, R-960 in RCR6322. Two non-flocculating, easy- grind carbon blacks were tested. They were DuPont's A-43-D and Harmon Color's J1027. Flooding was prevelant in the enamel containing DuPont's A-43-D. Harmon Colors J1027 corrected the problem. Flooding-floating was not evident in the enamel containing this pigment. The following development work was carried out on RCR6322 for weatherometer and exterior exposure. Panels are being exposed in Cleveland @ 45S. Florida exposures are at 5 and 45S. in addition to the weatherometer. GLD 045621 CR-4 LAB CODE 1350A-44 1350A-62 COLOR Olive Tone Olive Tone COLOR PIGMENTS Mapico Tan 15 Chrome oxide Green Carbon Black TI02 __ GLOSS R960 80+ R960 15 The following were exposed to study 3% epoxy modification. 135OH-68 White ---------- R960 10 1350H-70 White R960 10 EPOXY 3% A carbon black shading base was developed for RCR6322 enamels. The shading base was made in the plasticizer, Rohm & Haas Paraplex G-41, and issued as EGL68425. The initial 40 gallon batch of EGL68357 was passed as standard on 12/18/67. The batch (181564) had flexibility equivalent to the control. The weight per gallon and viscosity j i were in spec and the film passed 120 hours Cleveland Condensing Humidity with a rating of 10 RE-23289, Self-Cure Thermosetting Acrylic The above acrylic was submitted by the resin department to see if it could be used as a more flexible version of RCR6322. RE23289 differed from RCR6322 in that butyl acrylate replaced the ethyl acrylate. The supposition was that butyl acrylate would impart more flexibility to the resin. Although greater flexibility was in fact obtained the resin still required plasticizer. The improvement in physicals was not significant enough to amount further development. The results are more fully reported in Coatings Research Report #50. I | SUBJECT: THERMOSET VINYL ACETATE SUMMARY: In November, 1967 the thermoset vinyl acetate resin RE23110 was repeated by the resin department to see if it would correlate with the initial sample of RE23110. At the same time RE23242 was submitted for evaluation. This thermoset vinyl acetate was RE23110 with 1% trichloroethylene as a chain regulator. j Testing proved the initial and repeat batch of RE23110 were equivalent. However, a dis crepancy was found in the original testing of RE23110 cured with Cymel 301 and Cyzac 1010. This system was found originally to pass ninety to one-hundred MEK rubs but in second analysis was found to pass 200+ MEK rubs. ? I The addition of trichloroethylene casued darkening of the resin and loss of flexibility. For complete results on above resins refer to Coatings Research Report No. 49. j GLD 045622 CR-5 Thermoset vinyl acetate resins RE23215 and RE23216 are copolymers prepared by the resin department by grafting acrylate monomers on the vinyl acetate copolymer RE-23111. The purpose of the submission was to see if grafting of acrylate monomers improved on flow hardness and/or flexibility of the thermoset vinyl acetate copolymers. Testing showed that the above grafting did not improve on the physical properties of the thermoset vinyl acetate resin system. For complete results refer to Coatings Research Report No. 48. SUBJECT: COIL COATINGS SAMPLES AND EXHIBITS - NI27038I2111 SUMMARY: The following samples were prepared and shipped during December, 1967. Both samples were based on Aerylure, RCR6322. CUSTOMER CODE TYPE GLOSS PURPOSE SUBSTRATE Kirsch Alcan EGL68357 EGL68428 Aerylure Aerylure 80+ 10 Drapery Hardware Cold-Roll Bond 901 Experimental Exterior Treated Exp. Aluminum SUBJECT: SILICONE POLYESTER - NI26035I2311 SUMMARY: Silicone polyester EGL68424 was prepared and submitted to Alcan for testing as a residential siding finish. This system is a blend of linear polyester RCR6403, Cymel 301 and a Dow Corning silicone polyester R-6-0031. Weatherometer results indicate excellent chalk resistance up to 2000 hrs. No advantage is gained in terms of gloss retention over the straight linear polyester RCR6403 and would not therefore be suitable as a high gloss finish with stringent gloss retention specifications. The low silicone level (7-8% on resin solids) and high volume solids (54.2%) would be advantageous from a cost consideration. The general physical properties of this finish are as follows: Gloss 60-10-14 Pencil Hardness - F+ Flexibility - 2T no tape off Reverse impact resistance - 30 in-lbs no failure Cure - 380F. P.M.T. SUBJECT: THERMOSET VINYL CHLORIDE - NI26035I2311 SUMMARY: Work is being completed on the Thermoset Vinyl Project. The data is being statistically analyzed and should be completed in January, 1968. Selection of the optimum resin, or more probably the optimum conditions for synthesizing a vinyl resin should be finalized at this time. The problem of Humidity failure has not yet been completely resolved due to a suspected deficiency in metal pretreatment. A rather sub stantial portion of this type failure could be due to this factor. GLD 045623 CR-6 SUBJECT: VINYL PEELCOAT ~ NX26034I2211 SUMMARY: Longer term tests are indicating that a system based on Geon 135 and Flexol 1010 (EGL68374A) is superior to a similar system based on D.G.P. in two ways (1 phr of Cyasorb U.V. 24 is required for U.V. resistance). 1. Slightly superior results in the dew cycle weatherometer. After 136 light hours this system completely almost completely peels off whereas the D.O.P. and competitive Conchemco peelcoats only 1/2 peel off. 2. Better initial viscosity at a higher solids occurs when Flexol 1010 is used. A viscosity of 12 secs Zahn #6 at 83% N.V. content is obtained. The results, to date, show that the viscosity stability is equivalent to the Conchemco material. More detailed tests using line run panels from E. G. Smith of Duracron finishes are in progress. Durability studies are underway in Florida, Cleveland, Minneapolis, and the dew cycle weatherometer. The peelcoat applied over standard baked and underbaked Nubelar films have also been exposed. E. G. Smith's aluminum is used as the substrate. The peelcoat passes the "wet towel test," blocking and low temperature peelability (overnight at -10F.). It was observed that when the peelcoat was applied over the Duracron films some gloss increase occurred when the peelcoat was removed. Loss in hardness of the acrylic films was also observed. These effects were also noted with the Conchemco material. Conchemco Peelcoat Geon 135/Flexol 1010 GLOSS OF DURACRON 60 BEFORE / AFTER PEELCOAT 31 50 31 60 INITIAL HARDNESS AFTER PEELCOAT ONE WEEK Conchemco Peelcoat Geon 135/Flexol 1010 F+ 2B F+ B 2B B+ E. G. Smith also supplied stainless steel panels for testing. Application was found to be good over this substrate. It is not clear at this stage, what exactly their durability requirements are. If in fact they are more stringent than are met by our present system it would appear necessary to pigment the peelcoat for additional U.V. resistance. For this reason some dew cycle studies are being made with a carbon black pigmented peelcoat. The carbon black was conveniently added as the Dramatone black Y1782. The formula EGL68374A has been costed and based on Central Region costs a bulk cost of $2.75/gal. was Obtained. CONTRIBUTORS: K. O'Hara, R. Zilke, R. W. Stone GLD 045624 CR-7 SUBJECT: : POLYPROPYLENE - NI27009C1315 SUMMARY: Efforts have finally been successful in making a decent looking polypropy lene topcoat dispersion using the new Hercules PB-774 (lot SP-2447) and the new Hercoprime 292 (now called Hercoprime SA-941). Initially difficulties had been encountered in making a coating that would fuse nicely without blistering or mudcracking. It was found that by increasing the amount of slower solvents (by over 50%) that the difficulties of getting a good film were greatly minimized. Two dishwasher tubs were coated with a polypropylene topcoat dispersion using the new resins. Due to lack of experience with this new material, the results were not exactly first class. However, they were judged adequate for the purposes intended. Since it has become increasingly evident that "Airless Spray" is the desirable way of applying the polypropylene topcoats, efforts have been made to develop a workable material. Some success has been achieved but the main difficulty at present is that the spray gun gets plugged up by the material. This is due largely to the fact that this new lot of solution resin (Hercoprime 292) does not do an adequate job of holding the dispersion together. The resin manufacturer is aware of this and is working on the problem. In an attempt to raise the solids level of the polypropylene topcoat dispersions, efforts have been made to utilize a stone mill (Morehouse) to manufacture this material. The results have been interesting but not too successful. The chief difficulties appear to be results that are not consistently reproducible and too much "debris" in the dispersions which is difficult to remove. A "Bramley Beacon" mixer has finally arrived and attempts to make suitable caulking compound for under the polypropylene topcoats are underway. The chief difficulty at present is making a caulk that is more flexible and still retains the good detergent and adhesion properties of our former materials. Materials were sent to the following places: PreFinish Metals, Inc. - Elk Grove Village, Illinois 7 gals. EGL68302 Black Polypropylene Disp. Bennett Industries, Inc. - Peptone, Illinois 1 gallon EGL67573 White Baking Primer 5 gallons EGL67314 Yellow Baking Primer 5 gallons 1568KA-78A White Rollcoat Polypropylene Disp. Glidden - Salchi S.P.A. - Milan, Italy 5 - polypropylene coated wire racks 25 - 4" x 8" Polypropylene coated panels Hercules Inc. - Wilmington, Delaware 2 - panels polypropylene coating 1 qt. - EGL68437 White Polypropylene Disp. 1 qt. - EGL68446 White Polypropylene Disp. CONTRIBUTORS: J. Witko, G. Hardie GLD 045625 CR-8 SUBJECT: IMPROVEMENT OF NUBELAR (GENERAL SALES) - NI26034I2111 SUMMARY: I. As the result of a reported fading problem with EGL66216, Olive Tone Nubelar Coil Coating/ tests have been initiated to determine the cause of this fading if it occurs in properly applied systems. EGL66065A, EGL67413 and EGL67413 modified by replacing Zopaque R-55 with TiPure R960 were each used under EGL66216 and EGL66216-B. The two topcoats were also applied as single coat systems. The Cleveland Condensation Humidity Test showed the EGL66216-B over EGL66065-A system to be weak (few field blisters). All other systems showed no effect after 240 hrs. The systems are under test in Dew Cycle Weatherometer and Florida (h -7-418, WD-7-418 and F-7-348). II. Kynar 500 Experimental Resins Lots 65-0454 and 67-0454. Lot 65-0454 gave a marginal grind reading on dispersion and smoth, fused films. Lot 67-0459 gave excellent dispersions and films. Penhsalt Chemical Corp. has informed us that we can expect slightly higher viscosities with these resins. The specification are 60-85" #4 Ford and 10.91 lb./gal. for EGL66064-B. On a standard lab batch the constants are 83" and 10.91 lbs. (14 weeks old). The lab batch using Lot 67-0454 is at 86" and 10.92 lbs after four weeks. III. Production of 110 gallons of EGL68377, Caribbean Blue Nubelar Coil Coating and 40 gallons of EGL66064 Mist White Nubelar Coil Coating for Elwin G. Smith were made without any technical difficulty. IV. EGL68434, #68434 Bone White Nubelar Coil Coating, was developed for Inland Steel. This is a different shading of EGL66064-B. SUBJECT: COIL COATING - APPLIANCE - NI27007I2511 SUMMARY: Trip to Glidden (Nubian) Chicago PURPOSE: To supervise production of initial 25 gallon batch of EGL67421C White PolyLure 3000 Finish. CONCLUSION: Batch manufactured to standard using RCR6403 P380075. This batch is to be tested at American Screen on precoated aluminum for awnings. SUBJECT: EXHIBITS AND SAMPLES - GENERAL SALES - NI24034I1111 SUMMARY: I. Organosols - Alcan Brixite EGL68398, Terra Cotta Two Coat Organosol and EGL68400, Dark Gray Two Coat Organosol were developed and sampled to Alcan Brixite. These coatings have excellent low temperature (-10F. ) over aluminum. They have passed 120 hrs .@ 190F. CCH with no effect. They are under test as follows H-7-396, W-7-396, 7-324 (Cleveland), F-7-322, 3, 4. An unpigmented version of EGLS6047 White Organosol Primer, was made and tested in CCH under EGL67440-A, White Two Coat Organosol. No effect was noted after 120 hours. GLD 045626 CR-9 II. Poly-Lure Finishing Systems for Appliances A series of panels of Poly-Lure 1000 and 3000 have been submitted to the Chicago (Nubian) Division for evaluation as coil applied coatings for appliances. PAINTS EGL67314 EGL68426 EGL67673 EGL68457 EGL68458 Nupon Primer (Zinc Chromate) Clear Nupon Primer White Poly-Lure 2000 Primer White Poly-Lure 1000 Finish White Poly-Lure 3000 Finish FIIWS Primer 0.2 mil dry Finish 2 coat 0.9 mil dry Finish 1 coat 1.0 mil dry METAL Aluminum 0.025" Alodine 12Q0S Q Panel v Cold Rolled Steel H.D. Galvanized Steel 22 gauge 26 gauge Bonderite 901 Bonderite 1303 Republic Steel Republic Steel FINISH SYSTEMS SUBSTRATE Aluminum It If It If C.R.S. fl II H.D.G. II >1 II PRIMER No II Poly-Lure 2000 fl NuPon Clear II No II NuPon Zinc Chromate If NuPon Clear It NuPon Zinc Chromate II POLY-LURE FINISH 1000 3000 1000 3000 ! 1000 3000 1000 3000 1000 3000 1000 3000 1000 3000 GLD 045627 vO <jv P <v 1 o 0) Q CT> G -*H X 3 E T3 fftt -H A to x s cn c rt so I--t X 0 M-t 1 I 1 i--i tM X "O' &> O -3" CM X z 01 EM W a M K >s w Q Z < CO fMftt S t Em o w *3 Z co c CD r- rH rH rH r-- r- T" r-i <N <N tn in m CN CN CN \ \ W v. <N <N C4 CN CN rH r-i r-i r--( t--i. rH \\ \ \ \\\\ CN CN CN CN CN CN CN CN CN r--1 rH rH r*H rH rH rH rH rH rt H ri H H X I--( c o p cC 0o u >4 G O W G O H c o u C 0 V4 71 71 0 -P u u 0) P 0) U OJ P 0) P 0) ng. TJ TJ T! n T) rH rH c c c G G C 1 :r^f 4. rA 0 o 71 71 75 71 71 71 fdilii A} nS ft5 !T1 <t 3 E JS rH rH rH rH rH rH # :'St' 2 S; 3: s s X p w a a a a a C c: c < < < <c c c < < 01 0) o e? r (X oi OS & ft C <tJ s G(0 G10 CIts G<0 fet fst sft e.ft Ao Ao Ao Ao rtHli-IHrtrlH"+HH(74H ^^ .Tj ret to to (0 t0 10 t0 (0 t0 <0 <0 G C C G >- G C M vr .si x .4 x x .-4 x x x 3 0 =3 d 0 3 0 4J 4J X 43 X 44 44 44 44 44 44 44 -X -rS -H -X -X -H -X GCCGGGCCGCGC^ftftftftftft U<U C<jB) O U CJ S> O O CJ u u z3 z3 zP zP zP zP zP o ao o C GC CG 44 4-> 44 X X XX XX G 13 13 13 13 ooo o X X X XX x m to to to to to fotEo-toftEO-'UDw10 a(0Htoix1i0iato CCGC -X 'X _x *x 10 10 10 10 X X rX H X XX X ii (0 id id i0 a a a x: aouu to -X -X -X H * a *tZo to ft to ft CGC G OOO O XXX X GG <D r-t r-t X X XX t0 t0 X XS3 CO CQ ^ - 1G0 GtC CO to o o i--t r-i D D << '3,^,'O,"O,OOOO'0,"0*,3' W\W%W\ rX i--I r-t r-i *--t i--t i--t i--t i--I 00 00 \\ r-t r-t 00 co co or <o> -of -or WWW r-t r-i r-t r-t r-t r-t 00 00 ojr <5*1 \ww i--I 1--i X !--I r-t m n to rt h r-t O O <N CM XX CM CM VO + + CM CM t3 *0 vQ DO s ee X t Mft o o o o <o o Z. CM CM CX a> xXX fpt 3 ft 3 ft -X -X X XXX Oi a a oo n n co o X XX rX CM s ^OV ^O' O' o> o> X XXX O ft I 1C >t >r O X X Oi G o _ _ 0) ft O O' X 003 3 < ft z z z o oX z3 z z Q ft o o o ooo o o o ooo o oao OOO X ftCO X CM CM CM CM a XX 33 ft ft XX f3t f3t X- X3 Xft ft O' O' XX oo It I tt >i >. >1 > >i -X >1 >1 S >1 >1 >1 o . * x ft H H X X X XXXXXftUO fot fot fot fot O ft -x CO 00X0003 ft<ftftftftZftft 10 X X3 0 rH p P Oi o Xp 03 o Xp 0) -ri p 0) 0) C{ to p o fto o a> 0) <D ifl 01 0) <u o H 01 -ri p P 0) 0) 0) 0 <u dl p -*H p rH P rH 6 rH X ft P P <u t*: rH P cu p *H pX -rH -X ii o cfl <D ja NX rH P 03 X -ri a P 04 P 04 0) P -r| r\ P -H * p O r( o p -ri X X p -rH Is p -W l3 A E P -ri P -rl >n /d P O p >i 0 <d up Q id p o P -ri -H P p o pP p <0 2 CQ rj O O CO vO X A CD <d Eh Q o >4 W < ^3* O iD rH m CO CO < O VO 'O' rH cn r- CN o CO r- CO rH r*' VO rH in CO rr o vO O CO <y CO r^ r^ > CO 03 vO o vO < ^3* O vO rH CO r*' ro V0 r** o rH CN < in CN in r^ vO CN m r- rH CN CO CM *r ca in CO CO CO CN CD o rH CO in o vO C-* o vO P- vO rH r^ rH CO r- CO a\ CO CO o o CO ^0 i> vO vo \o iO vO vO vO vO vO V0 vO vO vO vO vO vO VO vO vO VO vO VO vO vo vO VO vO 66047 67525A 68433 W h ite W h ite W h ite O rg. P o ly -L u re 1000 P o ly -L u re 1000 4 1 /8 1 A lc a n ,W a rre n E a s te rn M a rw a is E a s te rn E a s te rn S .F ra n . P o h lm a n P o h lm a n G .B ro w lie 1 2 /7 1 2 /7 1 2 /1 5 GLD 045628 ________________________PE G L C O L O R Q U A L I T Y A N E LS G A L L O N S C U S T O M E R D IV IS IO N SALESMAN DATE co O0 0 CO (N \ i-t W CN \ PI M M \ M CN r- ro .TV o lT) <r vO <N CO <, ^*4 H o rH rH r--4 o CO CO CD CO GO 1--1 rp rH H H 0* a* & a* Du a P <U X X Pp p rtS H U C P 0g U cn g CO H t--4 a) p i-H # so <T$ rH 0 o 0 a. ID w XX in c o in o o m p i h ^ co CN iH CN 2 O n E-* a .4 O CD X Q < O uD CN -H X in ro m co CN X o -i nnUOHINPlHi!) CO X U MOinHlNinHH pH CN oo oo o o CN <u 0) pp 3P U 3 >4 HJ hj C I pH r- I O >1 04 r-t n 01 n H> 3 03 3 o 2X22 04 t--a0>i p CQ (0 ai 0 p gP P -.H C -ri fd r; >i <d P a> p CW X o XP -h CO p i4 a* s O CQ ro ^3* m r*4 vO H ro ro O rr- CD co vO v> VO VO vO vO CO 01 w aun^oiNifiOo co CcOa 2 < HHH <N CM LO ^ 04 04 co 1 r* o o o vO o o o ooo H H CN m a> 4) <D H Pi p P P O 0 ca p 3 3 3 p as Ct CQ s* id >4 a X 3 o o P r--i 1 1 <H a v ID ca rH PQ <v >i >i >i >4 IQ H e flj O ca s i--N o p 0 pH o p O r-4 -r-t U -H P -P o Q 2 X cu X < O CO X c m E-i 04 <d x m d co -p <o J3 o X X -p c a <o m o co x o h x x H X 8 GLD 045629 POLYMER & PLASTICS P-1 December, 1967 SUBJECT: VEHICLES FOR AIR DRY COATINGS INTRODUCTION: The first statistical design described in,lab report PP-37B " is nearing completion. The resins were all-successfully pre pared and film tests are almost completed. It Is the the intent of this report to describe the second statistical design and to mention future work which will complete the urethane part of this twopackage air dry project. SUMMARY: The second design is based on an epoxide-monobasic acid adduct back*r bone. The adduct will be reacted with both an aromatic and aliphatic di-isocyanate in order to make the NCO prepolymer. For the two-package mixes, the overall design will be split into four sections described below: ECO PREFOLYMER OH PREPOIYMER 1. Benzoic acid, t-butyl benzoic Styrene:ethyl acrylate acid, DER 332 adduct modified (with) with isocyanate acrylics .2 T tf (with) Benzoic acid, t-butyl benzoic acid, DER 332 adducts 3. Caprylic acid, TOFA, DER 332 modified with isocyanate (with) Styrene:ethyl acrylate acrylics 4. tf ff (with) Caprylic acid, TOFA, DER 332 adducts This will involve 4-X2 unsaturated designs and 32 mixtures to test* but it is hoped that 2 designs will suffice in which case there will be 16 mixtures to test. An example of one of the 2J designs involving the analysis is en closed; this represents the mixture (I.) in the preceding table. Resin preparation will begin on December 4, 1967# to be completed by the week beginning December 25> 1967. Film testing will follow. A meeting to discuss the proposed work will be held on December 1, 1967. Messrs, Tome, Watson, Pratt, Coaster and Backley will be present. By: Leonard Coaster, Donald A. Backley GLD 045630 p o l y me r & p l a s t ic s December, 1967 SUBJECT: COMPARISON OF IGEPAL CA-630 VS. TRITON X-lOO SUMMARY: A careful comparative evaluation was made to determine the suitability of Igepal CA-630 in K-1666 polymerization. Laboratory batches of latex, analytical checks and paint evaluation of the lab batches of showed tha+ the Igepal CA-630 was equivalent to the standard Triton X-100. A trial production run of K-1666, using Igepal CA-630, was made at Reading. The latex passed all of the standard control tests; however, it proved to be inferior to a control batch of K-l66b when tested in Trade Sales paints. Approval of Igepal CA-630 for this use can not be given as based upon test results. INTRODUCTION: past. The use of alternative sources of supply for emulsion poly merization surfactants has been suggested several times in the The nature of emulsion polymerization is such that it magnifies the subtle differences that are inherent to materials produced by different manufacturers who often use different starting materials and/or processes. Our past experience has shown that such alternates must be carefully evaluated. In the case of Igepal CA-630, a complete evaluation was made in 1965 All laboratory tests, including Infra-red analysis and Gel Permeation Chromato graphy, indicated that the material was equivalent to the standard Triton X-100. A production trial at Central Region yielded unsatisfactory latex. Unrelated production problems were later discovered and could explain the poor results of the trial and made this second evaluation desirable. EXPERIMENTAL - DISCUSSION: Due to the failure to find any differences between CA-630 and Triton X-100 in our previous work, only 5-liter size batches of K-1666 latex were prepared. The sample of Igepal CA-630 was especially selected and submitted by Antara Chemical of GAF. Test paints were prepared with the experimental latex and a laboratory control batch of K-1666. Ultra Flat and Dripless Latex paints were chosen as the test systems because both show a high sensitivity to differences in the latex. A production trial run of K-1666, using Igepal CA-630, was made at Reading. A sample of this latex was tested in the same Ultra Flat and Dripless formulations A batch of K-1666 from Central Region production was used as a control. EXPERIMENTAL - RESULTS: I. Polymerization: No measurable or visible dif ferences were found from the use of Igepal CA-630 in laboratory preparation of K-1666. See Table I for physical data. GLD 045631 POLYMER & PLASTICS P-3 December, 1967 XI. Paint Testing - Laboratory Batches: In both the Ultra Flat and the Y-3080B Dripless paint, no significant differences were detected between the control and the test batch of latex. See Table II. III. Production Trial Run: Manufacture of the latex at Reading was reported to he normal. This batch of P-617331, meets all of the K-1666 specifi cations. Examination of the cLear drawdown showed many fish-eves. Subsequent examination of other Reading K-1666 batches also revealed fish-eying. These did not carry over into the paints and probably are not the reason for the poor results. The fish-eying problem may be due to either insufficient mixing of the defoamer prior to the sampling or related to the production problems that plagued Reading during the K-7255 scale up. Table III shows the physicals for this batch. This latex was tested in the same Ultra Flat and Y-308GB Dripless formulations that were used before. A random sample of K-l666 from Central production was used as a control. While the oven stabilities were satisfactory, the scrubability was much poorer with the trial Reading batch. See Table IV for the test results. CONCLUSIONS: While laboratory scale batches and analysis fail to detect differences between Igepal CA-630 and Triton X-100 when used in emulsion polymerization, polymerization at a production level did show differences. These differences, as measured by perofrmance tests, show that Igepal CA-63O does not produce the same product as Triton X-100. Based upon these results, it is not possible to approve Igepal CA-630 for use as a substitute for Triton X-100 in K-1666 polymerization. R. D. Connerth GLD 045632 p-4 / TABLE I K-1666 Latex - Lab Batches N. V. PH Viscosity Particle Size Film Form. Temp. Mech. Stability V Draw Down RE-23008 Std. Control RE-23009 Iqepal CA-630 52.0% 52.0% 4.9 4.9 435 cps 410 cps 3325A 3200A <<45*F. C45*F. SPECIFICATIONS 50-52% 4.5-5.6 200-1000 cps 2300--3500& <46F. >30 min. >30 min. >30 min. Clear, Seed-free Clear, Seed-free Clear, Seed-free GU> 045633 P-5 TABLE IX PAINT EVALUATION & TEST RESULTS Laboratory Batches of Latex Initial Viscosity 24 Hr. Vise., R.T. 7 Day Vise., R.T, 7 Day Vise., 140F. 7 Day Roll Color Stability Scrub (unsealed) UL T RAFLAT RE-23008 RE-23009 Y-3080B Dripless RE-23008 RE-23009 91 Ku 90 Ku 99 Ku 99 Ku 93 Ku 93 Ku 98 Ku 98 Ku 93 Ku 93 Ku 98 Ku 98 Ku 91 Ku 90 Ku 95 Ku 95 Ku 86 Ku 88 Ku 94 Ku 95 Ku OK OK OK,si. chg 0K,sl.chg 238 cycles 244 cycles 68 cycles 66 cycles ... ...... ' 1 ' ,,"w " 1 " GLD 045634 TABLE III K-1666 Production Trial P-617331 with Igepal CA-630 PHYSICAL CONSTANTS; N. V. 51.0% pH 5.0 Viscosity % Free VAc 380 cps 0.8% Particle Size 2920A Mech. Stability 30 minutes Film Form. Temp. 40 *F. Draw Down Clear - Many Fish-eyes GLD 045635 P-7 TABLE IY Paint Evaluation of P-617331 ULTRA P-617331 FLAT Control Initial Vise. 96 Ku 96 Ku 24 Hr Vise RT 96 Ku 96 Ku 7 Day Vise RT 99 Ku 7 Day Vise 140 F 102 Ku 97 Ku 100 Ku 7 Day Roll 96 Ku 101 K.O. Color Stab. N.G. N.G. Scrub (unsealed) 160 245 OLD 045636 anal yses ANALYTICAL LABORATORY DECEMBER, 1967 CONTRIBUTORS: H. D. Swafford, D. Senko, J. Schmittgen, E. White, G. Flood, C. Blake, S. Pitcher, R. Evans Following are listed some of the analyses completed during the month of December, 1967: During the month, a series of experiments were performed to devise simple means for a wet analysis lab to run assay analyses on hydroxypropyl methacrylate monomer batches. Linear concentration plots were obtained versus percent hydroxyl, versus refractive index, and versus weight per gallon over the range 0 to 100% R.P.M.A. in xylene, with and without 2% water present. 1, #29-129 WHITE POLYESTER EN. (STANDARD-T CHEM. CO.--FOR FRANKLIN MFG. CO.) - NUBIAN SOLVENT: Xylene, diacetone alcohol, cellosolve acetate, methyl isobutyl ketone. BINDER: Melamine-formaldehyde modified, neopentyl glycol-adipic acid-isophthalic polyester. TOTAL SAMPLE Solvent Pigment Binder 37.3% 28.1% 34.6% SOLVENT S-423 S-622 S-558 S-614 Unk, 50.3% 23.3% 11.8% 14.2% 0.4% BINDER M.F. Isophthalic Acid Adipic Acid 7.1% 43.7% 20.0% CONSTANTS NV Veh.NV N2 62.7 48.1 1.6 * Expressed on Veh. NV. 2. GLASIMAT TM RED COLORED DISCS (GLASTIC CORP.) - ELMWOOD FILLER: China clay (hydrated aluminum silicate). MONOMER: Styrene, only. POLYESTER: O-phthalic maleic--fumaric--"Het" ethylene glycol. There is also present a small amount of a bis-phenol A based, polyol (thought to be the ethylene glycol diether). "Het" content is largest, and only a small o-phthalic content is present (could not quantitate in this four-way mixture). No calcium or magnesium was found. TOTAL SAMPLE POLYESTER CONSTANTS Filler & Glass Fiber Polyester resin: Styrene 67.0% 30.0% 3.0% "Het" anhydride 48.6% NV Cl 97.0% 27.9%* * On Veh. solids. GLD 045637 A-2 3. CLEAR TOPCOAT AND WHITE TOPCOAT (RELIANCE--FOR EDISON WOOD PROD.) - NUBIAN CLEAR TOPCOAT SOLVENT: Xylene, toluene, n-butanol, isopropanol, butyl acetate. BINDER: Urea-formaldehyde resin and cellulose acetate butyrate. An acid is also present (see Acid No., below). SOLVENT BINDER CONSTANTS S-423 S-416 S-231 S-222 S-522 Unk. #1 Unk. #2 16.7% 30.4% 8.0% 8.8% 35.0% 0.5% 0.6% U.F. C.A.B. 33.3% 66.7%** NV Acid No. N2 14.7% 6.4 (43.5 on NV) 7.5%* * Expressed on Veh. NV. **By difference. WHITE TOPCOAT SOLVENT: Xylene, toluene, methyl isobutyl ketone, isopropanol, methyl amyl acetate, methyl ethyl ketone. BINDER: Nitrocellulose, together with a glycerine--P.E.--cocoanut--o-phthalic alkyd. Ratio of glycerine to P. E. is approximately 1 to 1. TOTAL SAMPLE SOLVENT BINDER CONSTANTS Solvent Pigment Binder 46.8% 44. 3% 8.9% S-423 S-416 S-614 S-222 S-530 S-612 Unk. 22.1% 22.9% 37.9% 4.8% 5.4% 5.8% 1.1% N Nitrocellulose P.A. Cocoanut -F.A. 26.8% 35.9% 25.0% NV Veh.NV 53.2' 16.0- 4. FLOW COAT PRIMER (JONES DABNEY - FOR WHIRLPOOL) - NUBIAN SOLVENT: Xylene, diacetone alcohol, small quantity of unknown naphtha. BINDER: "Epon" - type epoxy resin, urea and melamine-formaldehyde resins (approx. 1 to 1), and a D.C.O. - glycerine--o-phthalic alkyd. TOTAL SAMPLE Solvent Pigment Binder 42.5% 20.1% 37.4% SOLVENT BINDER S-423 S-622 Naphtha 62.7% 28. 3% 9.0% P.A. D.C.O. F.A. U.F. - M.F. Epoxy + Polyol 19.2% 18.4% 27.6% Balance CONSTANTS NV Veh.NV 57.5% 46.8% GLD 045638 i 5. STYPOL 40-2342 (FREEMAN CHEMICAL) -ELMWOOD MONOMER: Styrene, only. POLYESTER: Isophthalic--maleic--fumaric--diethylene glycol--ethylene glycol. A-3 Bx ND.R Isophthalic Acid 34.7% M.A. 21.3% Glycols Balance POLYOU D.E.G. E.G. 89.1% 10.9% CONSTANTS NV Acid No. OH 6. STYPOL 40-2314 (FREEMAN CHEMICAL) - ELMWOOD MONOMER: Styrene, only. POLYESTER: Maleic--fumaric--dipropylene glycol. BINDER M.A. D.P.G. 44.0% Balance * On NV CONSTANTS NV Acid No. OH Ash 74.4% 19.1 0.28%* 0.05% (Co203) 7. CORESYN (LARSON IND., INC.) - ELMWOOD MONOMER: POLYESTER: Styrene. I O-phthalic--maleic--fumaric--diethylene glycol. CONSTANTS POLYESTER SOLIDS NV Ash Acid No. OH 66.1% 0.07% (Co203) 21.9 (as is) 1.3% (on NV) P.A. M.A. D.E.G. 50.2% 7.4% Balance B. CR-101 POLYESTER (INTERCHEMICAL - FOR NOLIN MFG.) - ELMWOOD MONOMER: Styrene, only. BINDER: O-phthalic--maleic--fumaric--propylene glycol. small amount of dimerized fatty acids. Also appears to contain a GLD 045639 BINDER P - A. M. A. P.G. 32.6% 28.4% Balance * Expressed on Veh. NV. CONSTANTS NV Acid No. OH Ash 63.4% 2.4 (as is) 0.98%* 0.08% (Co23> g. CR-102 F. R. POLYESTER (INTERCHEMICAL--FOR NOLIN MFG.) - ELMWOOD MONOMER: BINDER: Styrene, only . O-phthalic--maleic--fumaric--tetra-bromo-phthalic--ethylene glycol-- propylene glycol polyester (approximately 2/1 ratio of E.G./P.G.). Molar ratio of P.A./M.A. is estimated to be approximately 2/1 (cannot be determined quantitatively in the presence of T.B.P.A.). BINDER T.B.P.A. 20.6% * Expressed on Veh. NV. CONSTANTS NV Acid No. OH n2 Br Ash 64.2% 83 0.93%* 14.2%* 0.7% (Si02, Co203) 10. KEMVAR-C, KEMVAR-M, AND CATALYST (S. W. -- FOR BIRCHCRAFT KITCHENS) - READING KEMVAR C SOLVENT: Xylene, toluene, isobutanol, methyl isobutyl ketone, and a quantity of a ketone solvent which could not be identified (no matching reference spectrum available). It is not any of the commonly used ketones. PIGMENT: A quantity of silica is present in this sample. BINDER: Isobutylated urea-formaldehyde resin and vinyl chloride--vinylidene chloride copolymer (approximately 60/40 V.C./VC12). TOTAL SAMPLE SOLVENT BINDER CONSTANTS Solvent Pigment Binder 80.6% 1.3% 18.1% S-423 S-416 S-232 Unk.Ketone S-614 36.5% 15.5% 16.7% 20.6% 10.7% Vinyl Resin 40% Isobutylated U.F. Balance NV n2 Cl Ash 19.4% 7.7%* 25.0%* 1.3% (Si02) GLD 045640 k e mv a r m SOLVENT: Xylene, toluene, isobutanol, methyl isobutyl ketone, and the same unidenti fied ketone found in Kemvar C. PIGMENT: BINDER: Silica is present in this sample, also. Isobutylated urea-formaldehyde resin, vinyl chloride--vinylidene chloride copolymer resin, and a benzoic acid modified, tall oil--P.E.--o-phthalic alkyd. TOTAL SAMPLE SOLVENT BINDER MONOBASIC ACIDS Solvent Pigment Binder 73.8% S-423 1.3% S-416 24.9% S-232 Unk.Ketone S-614 34.1% 24.5% 20.1% 11.9% 9.4% Isobutylated U.F. Vinyl Resin P.A. Monobasics 17% 25% 25.6% 21% Tall Oil Acids 80.4% Benzoic Acid 19.6% CONSTANTS NV N2 Cl Ash 26.2% 3.8%' 15.3% 1.3%' (Si02) KEMVAR CATALYST SOLVENT: Isopropanol, toluene. SOLIDS: Solids of this sample consists of an aromatic acid phosphate. Although no reference spectrum is available for confirmation, it is postulated from observed structures that this may well be diphenyl (or di-cresyl acid phosphate). SOLVENT CONSTANTS S-222 S-416 79.8% 20.2% NV Acid No. 38.3% 149.6 (390.6 on NV) * on Veh. NV. li. TWO FAST-DRYING EN. (TOUSEY AND MOLINE PAINT CO. - FOR HART-CARTER) - NUBIAN #2-3069 DESERT SUNSET F. D. EN. SOLVENT: Xylene, plus some V.M. & P. naphtha, plus some Solvesso No. 100 aromatic naphtha. PIGMENT: Chrome yellow, titanium dioxide, silica. BINDER: Styrenated, D.C.O. - glycerine--o-phthalic alkyd. GLD 045641 A-6 TOTAL SAMPLE Solvent Pigment Binder ' 43.1% 30.1% 26.8% BINDER P.A. D.C.O. F.A. P.S. + Polyol 25.0% 27.1% Balance SOLVENT PIGMENT S-423 S-332 S-446 72.8% 12.6% 14.6% Ti02 PbCRQ4 Si02 PbS04 66.5% 17.9% 10.3% 3.6% 98.3% CONSTANTS NV Veh. NV 56.9% 38.3% JDM-0-10-A YELLOW MPM-2184 F. D. EN. SOLVENT: .Xylene, a V. M. & P. naphtha, and an aromatic naphtha comparable to Solvesso 100 PIGMENT: Chrome yellow, titanium dioxide, silica. BINDER: Benzoic acid modified, soya--tnmethylol ethane--o-phthalic alkyd. TOTAL SAMPLE SOLVENT PIGMENT Solvent Pigment Binder 43.6% 29.4% 27.0%. BINDER S-423 S-332 S-446 73.6% 11.2% 15.2% CONSTANTS PbCR04 Ti02 PbS04 Si02 39.7% 44.2% 8.7% 4.3% 96.9% P.A. Monobasics 37.8% 41.1% NV Veh. NV 56.4% 38.2% MONOBASIC ACIDS Soya F.A. Benzoic Acid 79.4% 20.6% 12. #673 PLATINUM GRAY PRIMER (MINIT SPRAY CORP. - FOR HOTPOINT) - NUBIAN PIGMENT: Talc, carbon black, titanium dioxide. BINDER: Nitrocellulose, resin--maleic adduct ester, tricresyl phosphate plasticizer. PIGMENT BINDER CONSTANTS Talc TiQ2 86.5% 12.9% N.C. T.C.P. Rosin-Maleic 47.0% 8.5% Balance NV Veh. NV 36.5% 20.1% GLD 045642 A-7 13. BLUE VINYL STRIPCOAT (IMPERIAL TYPE METAL) - READING SOLVENT: BINDER: Methyl isobutyl ketone, xylene. Dibutyl p'nthalate plasticizer, vinyl -chloride--copolymer resin. The vinyl resin used is an unusual one (contains little or no vinyl acetate). We do not have a matching type on file. This may contain some polyvinyl dichloride resin. K&eon Type 3005j as homopoiymer, or copolymer with vinyl chloride. In any event, it appears probable that the comonomer used is a chlorinated type (not vinylidene chloride, however). Some "Cab-O-Sil" type silica is present, also- TOTAL SAMPLE SOLVENT BINDER CONSTANTS Solvent 73.1% S-614 S-423 36.2% 63.8% Dibutyl Phthalate Vinyl Resin 17.5% Balance NV Cl Ash 26.9% 52.0%* 0.07% (Si02) * Expressed on Veh. NV. 14. KYANIZE LATEX HOUSE PAINT (KYANIZE PAINTS, INC.) - ELMWOOD SOLVENT: Water, only. PIGMENT: Titanium dioxide, talc. BINDER: Vinyl acetate - n-butyl acrylate* copolymer latex, modified with a quantity of glycerine - unk. type fatty acids** isophthalic alkyd. WATER SOLUBLES: Material recovered appears to be largely a sodium fatty acid soap (No thickener was detected). Also present is a small quantity of an alkylphenol - ethylene oxide adduct (nonionic emulsifier). TOTAL SAMPLE CONSTANTS PIGMENT BINDER Solvent Pigment Binder 50.8% 31.2% 18.0% NV 49.2% Ti02 Talc 69.9% 25.8% 95.7% Isophthalic F.A. Vinyl Copolymer & Polyol 6.9% 6.3% Balance * Too little present to identify positively **Or possible di-butyl fumarate - maleate. GLD 045643 A-8 BAKING ENAMF.T, SAMPLE (MFC-. UNK,) - BALTIMORE SOLVENT: Xylene, BINDER: Melamine- TOTAL SAMPLE Solvent Pigment Binder 52.3% 19.0% 28.7% FATTY ACIDS Caprylie Capric Laurie Myristic Unk. Palmitic Stearic Oleic Linoleic 7.1% 8.4% 23.9% 13.2% 2.3% 7.7% 3.1% 13.8% 8.6% SOLVENT BINDER S-423 S-416 S-438 24.9% 35.0% 40.1% P.A. F. A. M.F. 38.1% '"'`21% 23.8% CONSTANTS NV Veh. NV N-, 47.7% 35.4% 5.36%* Expressed on Veh. NV. 16. ELECTROFAX BINDERS SCM CORPORATION) - ERS-200 RESIN SOLUTION (PLASKON) SOLVENT: Toluene, only. BINDER: Benzoic acid modified, tall oil--trimethylol ethane---o-phthalic alkyd. SOLVENT BINDER CONSTANTS S-416 100% P.A. T.O. F.A. Benzoic Acid 35,8% 32.0% 2.6% NV Acid NO. 52.6% 6.0 {11.5 on NV) Z23PS ELECTROSTATIC PAPER {CROWN-ZELLERBACH) Resin present consists of an approximately 70/30 copolymer of vinyl acetate/dibutyl fumarate* * Or, possibly, n-butyl acrylate. IB-200 ELECTROSTATIC PAPER (PLASTIC COATERS) Resin used is an isobutyl methacrylate-styrene copolymer resin (approx. 3/1 I.B.M.A./ Styr.), together with a quantity of an o-phthalic alkyd (oxidizing type). GLD 045644 A-9 17. ITALVAR ACRYLIC EN. #2 & THINNER (ITALVER S.P.A.--FOR PHILCO ITALIANA) - SALCHI ACRYLIC EN. #2 SOLVENT: Cellosolve acetate, xylene, toluene, cellosolve, aromatic naphtha, and an unidentified solvent which appears to. be an aromatic, chlorinated solvent. PIGMENT: Titanium dioxide, silica. BINDER: Epoxy resin plus a terpolymer of ethylacrylate, styrene and unsaturated acid. Estimated ratio of terpolymer/epoxy resin approximately 60/40. Epoxy resin vised appears to be about comparable to Shell's Epon-1001. Nq acryloid AT--70 was available to examine in order to confirm or deny its' presence. However, Mr. Gordon Phillips said that this sounded exactly like AT-70 (styrene, ethyl acrylate, high acid content--used with epoxy resin). TOTAL SAMPLE SOLVENT PIGMENT CONSTANTS Solvent Pigment Binder 36.9% 41.1% 22.0% A Ar. S-558 S-423 S-416 S-572 Naphtha Unk. , 28.1% 32.7% 2.7% 4.3% 17.2% 15.0% Ti02 SiO,, 91.1% 6.3% 97.4% NV 63.1% Veh.NV 37.3% Acid No. 42.9 (on Veh.NV) Oxirane 1.3%* * Expressed on Veh. NV. ITALVAR DILUENT SOLVENT: Cellosolve acetate, isophorone, Solvesso #150 Aromatic Naphtha. SOLVENT S-558 S-640 S-460 21.2% 15.2% 63.6% 18. ACRYLIC-ACRYLONITRILE LATEX (JOHN DEERE) - ELMWOOD Monomer composition of this sample consists of: saturated acid. (Small amount). Acrylonitrile, n-butyl acrylate, un NV Acid No. N2 44.2% 10.4 (on dried film) 8.6% (32.6% acrylonitrile) GLD 045645 A-10 19. KEL SOL 1000 (SPENCER-KELLOGG) - .ELMWOOD This sample consists of a butyl cellosolve solution of an ammonia neutralized, maleinized, linseed oil. 20. BANSPREP SOLUTION (RANSBURG) - READING SOLVENT: Trichloroethylene, only. SOLIDS: Solids present consists of an alkyl trimethyl ammonium chloride (where the alkyl group consists of a long-chain hydrocarbon (approx. C-12?). CONSTANTS NV 0.5% 21. IMPREGNATED PAPER (RIVERSIDE LAB - FOR STATE OF WEST VIRGINIA) - ELMWOOD I. R. spectra obtained on solvent extracts of this sample of impregnated paper showed the following components to be present. 1. An isophthalic---maleic--fumaric--propylene glycol polyester. 2. Diallyl phthalate monomer. 3. Benzoyl peroxide. (No tertiary butyl perbenzoate was detectable). 22. RESIN IMPREGNATED PAPERS (JAPANESE) - ELMWOOD I. R. spectra obtained on various solvent extracts of this impregnated paper showed the following to be present: 1. Diallyl phthalate monomer. 2. Benzoyl peroxide catalyst. 3. Polyester based primarily on o-phthalate esters, plus (probably) some maleate- fumarate esters. 23. IMPREGNATED PAPER (R.C.I.--FOR STATE OF WEST VIRGINIA - ELMWOOD "\ Various solvent extracts were prepared from this sample of coated and/or impregnated paper. The I. R. spectra obtained on the extracts showed the presence of: 1. A vinyl acetate copolymer resin (approximately 60/40 ratio of vinyl acetate/acrylic). Acrylic used is probably methyl methacrylate and ethyl aerylate. 2. Melamine resin. This is not melamine methacrylate, but more nearly resembles a conven tional melamine-formaldehyde resin. GLD 045646 A-ll 24,. URUSHIOL LACQUER (SEKISAN PAINTS, JAPAN) - ELMWOOD I. r , spectra of eiectrocoated, baked films were rather featureless, and showed little other than C-H and OH groups. No significant differences were noted between the three spectra (from the cathode, anode, and dipped panel). ine r. R. spectra of anodrcaliy plated film and cathodioally plated film (uncured) were compared with the transmission spectrum of the sample deposited on a salt crystal. There were no significant spectral (sturctural) differences detectable between the three samples. 25. GRAY ELECTROCATED PANEL (P.P.G.--FOR WHIRLPOOL) -ELMWOOD The I. R. spectrum of the M.E.K.-toluene solubles from this sample shows the presence of 1. An "Epon" - type epoxy resin (large amount). 2. Benzoquanamine-formaldehyde resin (Est. 10-20%). 3. Ester, groups (Medium amount). 4. Acid groups (small amount). It is thought likely that the epoxy resin (and ester groups observed) are present as epoxy resin --- fatty acid ester, although this is not conclusive (this could probably be determined by saponification + G.C., et. if required). Solvent insolubles shows the presence of pigments (china clay, titanium dioxide, silica) No previously examined P.P.G. electrocoat sample is comparable to this current sample. 26. 1512-A-27 (ALLYL BUTYL MALEATE SYNTHESIS) - ELMWOOD Combined I.R. & G.C. analysis gave the following conposition for this sample: Diallyl Maleate Diallyl Fumarate n-Butyl Allyl Maleate (Product) n-Butyl Allyl Fumarate Dibutyl Maleate Dibutyl Fumarate Maleic Anhydride 16.0% 3.3% 43.1% 5.2% 24.2% 4.9% 3.3% GLD 045647 A-12 27. 1512-A--35 (ALLYLOXYETHYL) MALEATE SYNTHESIS) - ELMWOOD A small free M.A. content is observable in the spectrum*. Toluene is present in small amount. Otherwise, the structures;present are those which would be expected for the di (allyloxyethyl) maleate. Little or no. trans structures are present (essentially all maleate). * Probably less than 5%. 28. 1589AP20 (MANNICH REACTION WITH DIACETONE ACRYLAMIDE, FORMALDEHYDE AND PYRIDINIUM ACETATE) - ELMWOOD The solids of the two submitted samples (viscous liquids) were examined by I.R. and compared to the spectrum of (molten) diacetone acrylamide. It appears likely that the anticipated reaction did take place. The spectra obtained differ significantly from each other and from spectrum of D.A.A. No reference spectra were available for confir mation of structure. Unfortunately, carboxylate groups absorb very close to the amide absorbtion bands, making confirmation of its presence uncertain. 29. CURE STUDY OF UNSATURATED POLYESTER IN DIALLYL MALEATE - ELMWOOD The major changes occuring in the I.R. spectrum with time appears to be the physical loss of diallyl maleate by evaporation (film thickness diminishes with time, and all absorbtion bands due to diallyl maleate diminish with time, such that they are virtually non-existent at the end of 24 hours). An additional change occuring with tine is the increasing amount of OH content observable, as well as some increase in carbonyl groups (oxidative cross-linking?). Unsaturation also diminishes with time, but it is not possible to ascertain how much of this disappearance may be due to cross-linking and how much to evaporation of the diallyl maleate (certainly, mostly due to the latter). 3. 1523A68 (SYNTHESIS N-TERT. BUTYL ACRYLAMIDE) - ELMWOOD The I. R. spectrum of this sample matches exactly the our reference spectrum for this material (manufactured by American Cyanamid, examined 3/19/59). 31. #0S 20637 LATEX (LUBRIZOL) - ELMWOOD Binder solids consists of a diacetone acrylamide--2-ethylhexyl acrylate copolymer. BINDER Diacetone AcrylaMde 2-ethylhexyl acrylate 43.5% Balance NV Acid No. 46.3% 2.0 (on solids) 3.6% (on dried film GLD 045648 A-13 V2. HAZE FROM 15Q7A-66 III & P-75020 - ELMWOOQ The "haze" from this sample consists predominantly of paraformaldehyde {I. R. spectrum obtained also showed some melamine resin structures). ''AINT CHIPS 'FAILURE' - MIDWEST REGION The following is all that could be learned from examination of the two surfaces of the submitted paint chips: RED-BROWN SURFACE: The I. R. spectrum obtained showed the presence of an o-phthalic alkyd, silica, calcium carbonate, iron oxide. WHITE SURFACE: The spectruih obtained showed essentially all pigment (largely silica and silicates). A small ester carbonyl content indicates the presence of some organic ester polymer, but is not present in sufficient amount to characterize. 34* SEDIMENT IN V6105 REDUCED TO Y5Q13 - ELMWOOD Sediment present in this sample consists of pentaerythritol. 35. POLYMER FROM V1118, P-547 - ELMWOOD The I. R. spectrum of this sample of gel is that of (poly) hydroxypropyl methacrylate. Ash from the gel consisted of iron oxide. 36. HAZE FROM RCR3021 - ELMWOOD Haze ("gel") consists of paraformaldehyde. 37. HAZE OF PAINT FILM (Y5634) - MADISON The I. R. spectrum obtained on some of the removed "haze" showed the presence primarily of long-chain hydrocarbon structures (wax and/or mineral oil). Some ester groups are present (small amount), which maLy be glycerol triesters. The overall appearance is reminiscent of a polish formulation. No indications of alkyd could be found. 38. FOREIGN PARTICLES STRAINED FROM Y5067 - ELMWOOD Strainings consist largely of an amorphous silica, together with a lesser amount of TiCal (pigment agglomerates). No aluminum stearate ior other soaps were detected). GLD 045649 NUBIAN RESEARCH REPORT DECEMBER, 19^7 N-l SUBJECT: Food Packs to Qualify Coatings Status: 1. A simulated corn pack was made to determine film quality of NRV4i64 "F" and "C" Enamel when iron drier replaced manganese drier. Based on tne results of tnis test we have determined that tne iron drier range should he greater then 80 + 20 ppm., since adhesion failures were recorded when cans stored three days at 100F. were examined. The range, l40 + 20 ppm., appears most promising. Water pack tests for'bench flavor testing using the two driers at different levels have been initiated. 2. Last month we reported that tinplate ends using our interior systemVR-59045-A Basecoat VR-62151 Vinyl Topcoat had been originally checked by Anheuser-Busch, St. Louis with off-flavor reported. This laboratory coated aluminum foil and tinplate for a re-test vs. the original production samples and Anheuser-Busch flavor results were satis factory. Ends made from a new production run (American Metal Decorating) were also checked by Anheuser-Busch and were satisfactory. Everyone appears to be satisfied that this interior system is flavor acceptable. By: R. E. Meyers, H. C. Snodgrass, T. Dal Cason SUBJECT: Exterior System for Lug Caps Status: 1. Evaluated closures which had been fabricated from both USS #100 and Weirton CP treated 7C# tinplate by White Cap. Our color was excellent but it appears that there is a definite difference in the adhesion to metal of our three-coat white system over these two types of plate. Adhesion over Weirton CP is excellent, whereas adhesion over USS #100 treatment is questionable. 2. We are working on development of a size coat to give satisfactory performance also on USS #100 treatment tinplate. By: E. W. Eubanks, R. E. Meyers SUBJECT: Water Thinned Interior Panel Coating System Status: Four conversion varnishes were evaluated as topcoats for Masonite Corporation's Royal-Cote interior hardboard paneling. Special emphasis was given to testing the non-yellowing properties of each candidate. Other tests performed included pot life, print resistance, sheen stability, cross-hatch adhesion, mar resistance and stain resistance. The four varnishes, 150-T-9G9, GLD 045650 N-2 CL-35883-A, CL-3568I, and CL-3^-^00 were applied over various competitive synthetic groundcoat drawdowns supplied by Masonite. The four candidates were essentially equal, except for non-yellowing properties in which case CL"35883-A showed appreciably less tendency to yellow in the 20 hour liwDF. heat test. Samples of two formulations in CL-35883-A quality, a 10 sheen (CL-36080) and a 30 sheen (CL-36o8l) were submitted to Masonite in mid-December. Based or. +>}? acceptable results of all tests, including good adhesion of a complete system upon refinishing without sanding, large samples were ordered for a limited plant trial to be run sometime in January. By: M. C. Grippo, W. H. Hinckley, L> J. Mattucci, S. J. Biedron, L. Taylor GLD 045651