Document kmXQKez5kRLB83bGqD4DaxOn

>' ^ ^CONFIDENTIAL DU FONT TECHNICAL INFORMATION" : ***' REPORT D.S.C. #67-2 CC: J. W. NESTOR, WILM. CC: C. W. STAHL, TOLEDO F. H. BEADLES, WILM. F. S. BAKER, TUCKER C. F. KALB, WILM. G. I. MULHOLLAND, FLINT E. T. BRENER, WILM. '. H. BULLITT, JR., LAB. C. W. THEOBALD, WILM. . W. LAURRELL., LAB. R. B. DAVIS, WILM. R. E. PIKE, LAB. P. J. GRAHAM, EXP.. STA. C. N. SWINEHART, JR., LAB., R. A. DE WALL, CHICAGO J. W. BASTIAN, LAB. P. 0. PEASLEY, EVERETT W. H. EDWARDS, PHILA. PLANT C. H. THOMPSON, FORT MADISON R. H. VINING, PHILA, -PLANT J. F. MC GETTIGAN, PARLIN JT. E. ABBMCNDJ, PHILA. PLANT W. H. BEUTEL, PHILA. PLANT K. E. ACKLEY, SO. SAN FRAN. TO File: 1705 O' Ma r s h a l l ia b . Marshall Laboratory July IS, 1967 \ E. I. DU PONT DE NEMOURS & COMPANY FABRICS. & FINISHES DEPARTMENT if DIVISIONAL PLANTS CHEMICAL GROUP# ^' - - -.......... 330-LINE DISPERSION STABILIZATION CONCEPT FINAL DURABILITY REPORT PERFORMANCE IN ALKYD, NITROGEN-ALKYD AND THERMOSETTING ACRYLIC ENAMEL SYSTEMS PREPARED BY: ' DATE ISSUED: PROJECT NO.: PREVIOUS REPORTS; C. L, DAWKINS JULY 17, 196? P-63, DISPERSION STABILIZATION^ v CONCEPT MARCH, 1964; AUGUST 1965; MAY, 1966. ABSTRACT: Product systems containing 330-Line Dispersions are equivalent in durability performance to systems containing conventional base analogs. Data demonstrate! that 330-Line Dispersions are satis factory replacements for conventional base analogs in alkyd, nitrogen-alkyd and thermosetting acrylic enamel product systems. Conclusions are based on .the analysis of data compiled, from the evaluation of over 120 exposure series (approximately 6,000 panels). These exposure series include data on the twenty-four 330- ? Line Dispersions scheduled for commercialisation in September, 1967./ in- w 2 D.S.C. #67-2 OBJECTIVE: Determine if 330-Line Dispersions are satisfactory re placements for conventional base analogs in alkyd, nitrogen-alkyd and thermosetting acrylic enamel product systems with respect to . durability performance, CONCLUSIONS: ., 1) 330-Line Dispersions are satisfactory replacements for their conventional base analogs in alkyd, nitrogen-alkyd, . and thermosetting acrylic enamel product systems with respect to durability performance, 2) Use of Dispersion Stabilization Concept (DSC) technology as a formulating tool produces dispersions which are .... ; equivalent in durability performance to dispersions................. formulated by use of conventional technology* From this conclusion, it is predicted that dispersions formulated with DSC technology will give satisfactory durability ........ . performance in many product qualities. This prediction, is supported by durability data covering a wide spectrum of product qualities, 3) Batch-to-batch variation in pigment has a greater effect on durability than does the technology, either DSC or conventional, - applied in development of the dispersion, - REASONS FOR REPORT: This report is issued to: (1) Indicate the successful completion of the durability phase of the P-63 Project, (2) Present the conclusions derived from the evaluation of over 6,000 exposure panels, (3) Act as a durability reference for the full scale 330-Line commercialization proposal, (4) Serve as an across-the-board final report for all exposure series in the P-63 project in lieu of individual reports for each series, (5) Delineate future action. (6) Up-date previous durability reports by intro ducing data covering longer term exposure. DUP030001681 3 D.S.C. #67-2 FUTURE ACTION: (1) Twenty-four 330-Line Dispersions are scheduled for commercialization in place of their 42, 732 and 743Line counterparts in September, 1967 (2) Based on the information now available, no extensive durability evaluations are planned for new dispersions which may be added to the current 330-Line Dispersion gamut. Routine, high-spot evaluations will be made where deemed necessary. (3) Evaluation of active exposure series will continue according to standard procedure until normal lengths of exposure are achieved. PREPARED APPROVED BY APPROVED BY C.N. SWINEHART, JR SUPERVISOR DUP030001682 " 4" Dj mSj .G_.__^62^2 DISCUSSION: Background: Commercial application of 330--Lime Dispersions involves the elimination of several dispersion lines by replacement with a single dispersion line. Before implementing commercial application it is necessary to show that the durability performance of a partic ular vehicle system is not adversely affected by use of 330-Line Dispersions. Satisfactory durability performance was established based on exposure data presented in M. H. Schaffer's report of May 3, 1966. At that time, the duration of exposure of 330-Line Dis persions was sufficient to support durability conclusions. With longer term exposure data now available, earlier results are re inforced and previous conclusions are confirmed. Experimental Procedure: The entire gamut of 330-Line Dispersions was considered in the durability evaluation phase of the P-63 Project. The following general procedures apply to the bulk of these dispersions concerning levels of exposure, locations of exposure and evaluations of exposure, etc.: (1) Colorants were exposed in masstones, tints and mixed color active product formulas. (2) Matstones, tints and mixed color active product formulas underwent exposure by Accelerated Weatherometer (X-l Cycle) at Philadelphia and exterior exposure at the Florida and/or Delaware Exposure Stations. (3) Metallics as well as non-metallics were exposed. (4) Experimental exposure panels were examined and evaluated at regular intervals for all film failure characteristics, i.e., gloss, waterspotting, exudation, mildew, dirt collection, chalking, checking, cracking, blistering, flaking, bronzing, rusting, color-change, et.al., as compared with controls. (5) Recommendations regarding levels of exposure (P/B) were derived from the formulating tables and correlated with the levels of commercial usage. Tables used are as follows: (a) The 15 and 93-Line Formulating Tables were used in formulating straight alkyds. DUP030001683 -5- D.S.C. #67-2 (b) The 780-Line Formulating Tables verb used in formulating nitrogen-alkyds. (c) Performance Criteriaf The 938-Line Formulating Tables were used in formulating thermosetting acrylic enamels, (TAE). 1) Durability was based on results obtained at the Florida Exposure Station, 2) Conclusions are based on the active scaled-up 330- Line Dispersions in alkyd, nitrogen-alkyd and thermo setting acrylic enamel product systems, 3) Durability was based on interpretation of gloss unit differences, since differences in other film failure properties were insignificant. Description of Tables: Table I, "330-Line Dispersions", lists the 330-Line dis persions scheduled for commercialization and shows the 42, 732 and/or 743-Line conventional dispersions which are being replaced. Table II, "330-Line Dispersion Durability Table", shows the durability ratings of 330-Line Dispersions after Florida exposure. Table II shows only 30 of the exposure series covered in this durability study and should therefore be considered only repre sentative of the durability performance of 330-Line Dispersions. All ratings in this table refer to the durability performance of 330-Line Dispersions (experimentals) as compared with conventional dispersions (controls). Batihgs are based on interpretation of gloss unit differences and are as follows: (1) + means better than control or superior by 10 or more gloss units at one exposure leveJand at least equal in the other (s). (2) E+ means marginally better than control or superior by o to 10 gloss units at one level(s) and at least equal in the other(s). (3) E means + 5 gloss units at all level(s). * (4) E- means marginally poorer than control or inferior by 6 to 10 gloss units at one levelCSJ and equal (+ 5) gloss units in the other(s), ' a' - ' (5) means poorer than control or inferior by ^ or more gloss units at one level(s), and de ficient at least 6 gloss units in the other(s). DUP030001684 -6- D.S.C, #67-2 Table III shows, "Statistical Curve For Durability Per formance Of 330-Line Dispersions", as compared with conventional dispersions. Results of earlier {shorter term) and current (longer term) exterior exposure of the basic formulating gamut indicate, statistic ally, a Gaussian type distribution with respect to durability per formance. The percentage distributions are as follows: Equal to Control Better than Control Poorer than Control Earlier Results Current Results 56$ 74$ 30$ 14$ 14$ 12$ Both "Earlier" and "Current" results correlate with accelerated weathering results. Table TV lists numerically, "Exposure Series In Alkyd Product Systems". Table V lists numerically, "Exposure Series In Nitrogen*. Alkyd Systems", Table VI lists* numerically, "Exposure Series In Thermo setting Acrylic Enamel Systems." Each series in Tables IV, V and VI was exposed in at least 4 different sets. Information pertaining to "Completed Exterior Exposure" and "Disposition" is omitted for certain series. In such cases the durability performance is based on the most upto-date information regarding the particular series. Several series are omitted because they are not within the specific range of this report. For instance, there is limited, but satisfactory durability information on 330-Line replacements in vinyl enamels, acrylic lacquers and Trimethylolethane (TME)-Benzoic Acid formulations. DUP030001685 TABLE I 330-LINE DISPERSIONS DS.C #67-2 330-LINE COLORANT 42, 732 AND/OR 743-LINE CONVENTIONAL DISPERSION ANALOG 330-3243 ----- ~ 330-3300 --------- -----------330-2312 --------- ------------ 330-1327*---- ---------330-1355 --------------- 330-1362 ---------- :---- 330-1364 ------ -----------330-1393 ---------- 330-1505 ------------ -- 330-1550 (40-B-6640) 330-2562 ----------330-1566 (40-B-6641) 330-1606* --------330-1612 ----------------- -- 330-1622 ------- ------ 330-2630 ------- ------- 330-1655 ------ ---------330-1656 ------------330-1679 --------------- 330-1666 ---------------- 330-1667 ----------------330-1765 ----------------- - 330-1616 330-1619 --.-- 330-1630 ------------------- -224 W-225 -243 W-253 W-300 -312 W-300 W-355 W-362 W-364 W-393 -505 W-556 W-562 W-519 -606 -612 W-622 W-630 -655 -656 -679 -666 -667 -750 -765 -616 -619 -630 *Not scheduled for commercialization DUP030001686 c o n tro l m a rg in a lly poorer than poorer than c o n tro l E means e q u iv a le n t to c o n tro l E+ means m a rg in a lly b e tte r th a n c o n tro l + means b e tte r th a n c o n tro l OCMI^vtOte .4 * to co O ooo SSI CO OHO CO CM CO CO to CO CO aO aO aO Qa HHO H CM CM co CM m co co co ; oa ao oa o HOOO CM CO co CO M0sOO'O'0Ov O'MS O' o>o.os H CM H iii ii ii ii I.sOoN {os 1 Os i & *a -CO-co OstO I >0 s) SO s0 I ms ms Ox ms I OOOsO .* s`SOsOsOSO I MS O'O'O' I o OS 0`s os CM CM H CM CMHHH g aI taiaia <e-4i taI ta ta tataI ta ta ta i+a i. a 5HH.:: w to w <o co to to to to <0 to to co to to co co co co co to ta l a I i i aia i i 0a a0 a0 a0 0a a0 0a a0 a0 6a 0a 0a i a*-> sO-CO CMtO CMH-H- h *^ I CM-4 IMS-4-.A-CM O H"-4-4-4-4-4-4 I HHCMHHCMCMHCM H CM HCMCMHf'SCMtNtCMCMCMCMCi ta p<q E- oMs CO0MO3h CO aH, fvNUSNNCMHHH Cs- Os -4- OS -4-co CM 00*60 C- OssO OssO OSCM tO OOsOOsO OsOsOOs CM H CM H CM H H CM H -4* sp I 4`H I to ms | OO CM CM I tO CM VS-4- Os OS CM to CM OStv Cv. I 6- OsOssO sO Os os<0 OstO Os Os Q 6s Os O Os Os 6s Os 6s 6s 6s Os CM H H NHrlrlrlrlnrln + t+ai+atataiatat+ai1a tata i ta tai ta ia + ta ta i taI t+a taI M of: OCOS co cocowcocococotoco 0a a0 0a 0a 0a 0a a0 0a 6a OCO, COO aa MS-4-4-4H -4-4 H CM CM CM CM c* CM I CM H H CM CO 01 PI CO to to to tO tO (0 Ml (0 0a 0a 0a 0a 0a 6a a0 a0 a0 0a 0a 0a 30 H-sOtOtO C^s6 O-4-s6-4t0 -4-CM CM CM H H CMCM CM CM CM CM H CM H 0C 4s--Ot*OS&-#fentOOisrvO^sCo>4stOCtsotCrt1MoCtOSoSl II *,-0440vm0<ns I I -4 MS CM -4 CM vsosovuvdito CM os O <4i CM O Os -4sO CM -4 O O H tO OstO ms >2) to to to to tO JAtOtO OOsOsOsOOsOsOsOS I OO I OS Os O Q 0> O' O' Os os OS O Os O CMHHHCMHHHH CM CM H H CM CM H H H H H H CM H CM I t=q + ta MKs ta tata +. + ta ca tata ta ta ta ta tar-"! ta ta ta ta'f *i t^O CM CV Ms CM -4OSMS0 -40 H CM MSSO tO OSO MS CM0So\o\0S0S0S0SM\MS OMSStCoM ttoo tO O MS MS MS>0 CM H SO CM CM SO o ro MStO MS MS Of-stsOO SO SO SO SO SO tStovOtMtosS-HttOo tHOosrtOos OSOSH H H H H H H H II III ItIII OOOOQOOOOO HI NI rIlHI HI HI WI IHIriIrlri lHt r1lHI HI rIl oooooooooooooooo os os os os oSosos ososos OS P'S OS OS P'S OS OS OS P'S 0'S os 0'S OS PS P'S OS ovos <*s .ns o\oyos os os os OS OS os cm OS OS PS OS OS OS o\ OS OS OSOS OS means means E-- DUP030001687 TABLE III D.S.C. #67-2 STATISTICAL CURVE FOR DURABILITY PERFORMANCE PERCENT OF INDIVIDUAL EVALUATIONS* Based on 200,000 individual gloss readings. DUP030001688 TABLE IV D.S.C. #67-2 SERIES EXPOSED IN ALKYD VEHICLE SYSTEMS EXPOSURE SERIES ' PIGMENT REPLACED B1r 330-LINE LEVEL 19655 19667 19634 19692 19760 19735 19303 19312 19323 19329 19345 19364 19369 19393 W-735 W-505 W-63O W-735 W-224 W-679 W-655 W-735 W-735 W-735 W-393 W-505 W-312 W-636 W-300 W-334 W-612 W-653 W-630 W-63? W-636 W-622 < W-735 ' W-612 W-225 W-655 W-300 W-224 W-262 W-630 W-362 W-679 W-336 W-319 W-653 W-362 W-224 W-505 W-225 (M) Masstones; (T) Tints; (X) Mixed. M. T, X. M. M. T. M. T, T. M. T. M. T. M. T. M, T. M. T. M. T. X, M. T. X. , *Re-ex. =* Re-exposed, !$ COMPLETED EXTERIOR EXPOSURE 30 mos. DISPOSITION Retired 30 mos. 30 mos. 27 mos. 30 mos* 27 mos. 24 mos. 24 mo s . 26 mos. Re-ex,* 6 mos. Re-ex. 6 mos. Re-ex. 3 mos. Retired Re-ex. 3 mos. Re-ex. 3 mos. Re-ex. 6 mos. Retired 24 mos. Re-ex. 3 mos. V*.* 12 mos. 24 mos. Re-ex. 3 mos. Re-ex. 3 mos. DU PQ30Q01689 Table IV (cont.) D.S.O. #67-2 r ' series Exposed m AxKyd venicie Systems (cont.) Exposure Series ' 19904 19951 19970 19974 20507 20508 20516 20522 20530 20547 20565 20545 20613 20631 20704 20722 20742 Pigment Replacement by 330-Line ' Level W-785 -312 -259 W-622 -608 -224 W-362 -785 -819 -630 -505 M.T. T T -679 -582 -224 - -612 -818 -819 X M.T. -622 -630 -582 -355 -630 -224 -785 -386 -819 -505 -785 -259 -658 -362 -622 -686 -622 M.T. M.T, X X X M.T. -630 -679 -686 M.T. 1M IM ' Completed Exterior Exposure *-- Olspobition 24 mo. 24 mo . 24 mo. Reex, 6 mo. Reex. 6 mo. Reex. 6 mo. 21 mo. 18 mo . 21 mo. 21 mo. 21 mo. Reex. 6 mo. Reex. 6 mo. Reex. 6 mo. Reex. 3 mo. Reex. 6 mo. 18 mo. 18 mo. 18 mo. 18 mo. .. Reex. 6 mo. Reex. 6 mo. Reex. 6 mo. DUP030001690 Exposure Series 20756 20764 20775 20816 20839 20844 20845 20863 20883 20900 20913 20949 20962 20992 20993 21003 21010 21027 21046 21049 2IO59 21201 21202 21242 21246 21252 21258 21268 21290 21311 21321 21324 21337 Table IV (coni;,) D.S.C. #67-2 Series Exposed in Allcyd Vehicle Systems (eQnt. ) Pigment Replacement by 330-Line Level -686 -224 -362 -686 -658 -559 -505 M M M.T. M.T, T M.T.X. -686 -830 -312 ' -355 -686 -6 79 W-785 -785 -393 -505 -582 -819 -559 -819 W-505 -582 -785 -785 -679 -582 -550 -686 -505 -550 -679 -630 -622 -655 -355 -519 M M.T.X. M M,'.. M.T, X M M M M M M X M.T, M M M M.T, M.T, M.T, M.T. M.T, M.T. M.T, M.T. M* Completed Exterior 'Exposure Disposition 18 mo; 15 mo, Reex. 6 mov Reex. 3 mo. 12 mo. 12 mo . 12 mo . Reex; 6 mo; Reexi 3 mo; Reex. 3 mo. 22 mo. 12 mo; 12 mo. Reex; 3 mo. Reex; 6 mo. Reex. 3 mo. 9 mo. 12 mo. 9 mo. 9 mo . 9 mo. Reex. 6 mo. Reex. 3 mo. Reex; 6 mo. Reex; 3 mp. Reex, 3 mo. 9 mo. 9 mo. 9 mo. Reex. 3 mo. Reex, 3 mo. Reex. 3 mo. 9 mo. Reex, 3 mo. 6 mo . 3 mo . 3 mo. 3 mo. 3 mo. Reex. 6 mo. Reex, 3 mo. Reex. 6 mo. Reex, 6 mo. Reex. 6 mo. DUP030001691 TABLE V D.S.C. 07-2 SERIES EXPOSED IN NITROGEE-ALKXD VEHICLE SYSTEMS Exposure Series Pigment ^ Replacement by 330-Line Level Completed Exterior Exposure .......... Disposition ' 195^3 19568 19655 19666 19667 19684 19692 17905 19715 19791 19804 19B43 20647 20722 20741 20749 26756 20767 -612 -384 -612 -630 -785 -224 -785 -505 -384 -630 -785 -224 -679 -655 -612 -655 -312 -224 -384 -300 -505 -785 -658 -819 -687 -630 -679 -300 -630 -355 -679 -224 -687 -686 -655 : M 36 mo. M.T.X. 30 mo. Retired Retired M.T.X. 30 mo. M 31 mo. M.T.X. 30 mo. M M.T, M.T. X 30 mo. 30 mo. 24 mo. *33 mo. Retired Retired Reex. 3 mo, Reex. 6 mo. Reex. 6 mo. Reex. 6 mo. Retired ,M M M.T. 27 mo. l8 mo. M M.T. M M M - 18 mo. 14 mo. Reex. 6 mo. Reex. 6 mo. x.' ;i"} . Reex. 6 mo. Reex. 4 mo. V DUP030001692 Table V (cont,) D.S.C. #67-2 Series Exposed in Nitropen-Alkvd Vehicle Systems (Cont.) Exposure Series 20777 20781 20786 20806 20815 20816 20822 20831 20836 20844, % 20876 20882 20514 20920 2093I 20949 20979 20993 21003 21010 Pigment Replacement by 330-bine -224- -785 -224 -630 -384 -679 -612 W-608 -687 -686 -686 -362 -393 -630 -362 -582 -312 -505 -785 -559 -559 -505 -686 -679 -582 -224 -686 W-785 -785 -224 W-505 -312 -630 -305 -582 -819 I 1 Level M.T. M.,X Completed Exterior Exposure 16 mo. .......... Disposition Reex. 3 mo. M.T, M.T. M M.T. M.T, M X .14 mo . 12 mo ; 12 mo. 12 mo. Reex; 4 mo; Reex; 3 mo; Reex . 06 .:.mo. Reex, 6 mo. M.T.X. 12 mo. M M M M M.X. M.T. M 12 mo. 12 mo . 12 mo. 9 mo. 9 mo. Reex, 3 mo. Reex, 6 mo. Reex. 3 mo. Reex. 3 mo. . Reex. 3 mo. Reex. 6 mo. M M 9 mo . Reex. 3 mo. M 9 mo. Reex. 3 mo. DUP030001693 r- * f. j. I 1 : i : ;. ' Table V (cont. ) D.S.C. #67-2 Series Exposed in Nitroeen-Alkyd Vehicle Systems (Gont.) Exposure Series 21020 21027 21049 21094 21095 21192 21251 21252 21268 21275 * 21311 21321 Pigment Replacement by 330-Line w -393 w -559 w-505 w-582 W-785 W-224 W-224 W-582 W-686 W-505 w-679 W-505 W-550 W-622 W-655 Level M M X Completed Exterior Exposure 9 mo. 9 mo. 9 mo. Disposition Reex. 6 mo; Reex. 3 mo. Reex. 3 mo. M M.T. M M.T. M.T. M.T. X M.T. M.T. 6 mo; 6 mo ; 6 mo. 3 mo. 3 mo. Reex. 3 mo; Reex; 3 mo; Reex, 6 mo. Reex. 6 mo. Reex. 6 mo. { ! DUP030001694  TABLE VI SERIES EXPOSED IN TAE SYSTEM D.'SYC.'#67-2 Exposure Series Pigment Replaced by 330-Line Level Completed Exterior Exposure .... ... . . Disposition 19688 (acrylic lacquer)1 W-630 19887 (vinyl enamel) -750 -253 W-630 -243 19926(vinyl enamel) -362 -750 -608 W-253 -551 -243 -630 -362 19949 -819 W-818 19969 W-505 -224 -785 W-63O -818 -582 -312 20538 (vinyl enamel) W-687 -750 -687 20561 20568 W-608 W-5P5 ^ -686' W-622 -243 W-300 -655 20607 . -612 -312 20643 2064^ W-785 W-505 -224 1) -754 W-551 W-253 M 30 mo . Retired X 34 mo* Retired X 24 mo. Reex. 6 mo. T X 30 mo. Retired X T 18 mo . Reex. 6 mo. X 21 mo. Reex. 3 mo. M.T. ,x X DUP030001695