NAVY MIL-C-85498-1981 CURING AGENTS DIMERYL-DI-ISOCYANATE AND ISOPHORONE DI-ISOCYANATE《固化剂》.pdf

1、- I - MIL-C-S49 b 979990b OL23bb4 Z +/5- .I7 Beneficial comments (recomnendations, additions, deletions) and any pertinent data which may be of use in improving this document should be addressed to: Commanding Officer, Naval Air Engineering Center, Engineering Specifications 4nd Standards Department

2、 (ESSD) Code 93, Lakehurst, NJ 08733,- by using the self-addressed Standardfzation Document Improvement Proposal (DD Form 1426) appearing at the end of i this document or by letter. . MI L I TARY SPEC1 FI CATI ON MIL-C-85498(AS 1 6 October 1981 - CURING AGENTS, DIMERYL-DI-ISOCYANATE AND I SOPHORONE

3、DI - ISOCYANATE This specification is approved for use by the Naval Air Systems Conmand, Department of the Navy, and ts available for use by all Departments and Agencles of the Department of Defense. 1. SCOPE. 1.1 Scope. This speciffcation establtshes the requirements for two types of di-isocyanate

4、curing agents. 1.2 Classification. The curing agents shall be of the following types: Type 1 Dimeryl -di-isocyanate (DDI) Type II Isophorone di-isocyanate (IPDI) 2. APPLICABLE DOCUMENTS. 2.1 Issues of documents. The following documents of the issue in effect on date of invitation for bids or request

5、 for proposal, form a part of the specification to the extent specified herein. STANDARDS MIL I TARY M I L- S TD- 1 2 9 Marking for Shipment and Storage. MIL-STD-1218 ACS Chemical s. .- Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-C-85LI78 68

6、7777906 0323665 3 = Property NCO content, percent Moi sture , percent PH Hydrolyzable chlorine, percent MI L-C-854 98 (AS 1 Type I . Min Max 13.50 14.30 - o. 02 5.0 6.5 - 0.05 2.2 Other publications, The following document foms 4 pqrt op tkis specfficqtfon to the extent specified heye, Unless otherw

7、ise indicqted the tssue n effect on date of tnvttqtion for btds or request for proposal shall apply. STANDARDS ASTII1-D-1638 Urethane Foam Isocyanate Raw Matertal s. (Applfcatfons for coptes should be addressed to the herican Society for TestPng and Natertal s , 191 6 Race Street, Phil adel phta, PA

8、 191 03. I 3. REQU I REMENTS . 3.1 Product characteristfcs. The curing agents shall be clear liquids with the color of light straw. . 3.2 Chemical properties. Chemical properties of the curing agents shall conform to the requirements of Table I. TABLE I. Chemical properties. 37.1 I 37.8 f t 3.3 Infr

9、ared spectrum. An infrared spectrum shall be made for Type I and Type II materials In accordance with 4.4.3. The infrared spectrum shall qualttatlvely conform to Figures 1 and 2. 3.4 Stafjiltty. When packaged in accordance with 5.1 and stored n the temperature range of 5 to 22 degrees Celsius PC), t

10、he curing agents shall meet the requirements of thts specification for a minimum Qf 6 nonths after acceptance. The shelf life may be extended for 6- montli intervals after reacceptance testing for conformance to the chemi-cal property requirements in Table I as follows: Provided by IHSNot for Resale

11、No reproduction or networking permitted without license from IHS-,-,-MIL-C-5LI7B 68 7779706 0123666 5 Number of containers Number of containers (primary sample) 100 or more 10% (nearest in lot sampled who1 e number) 51 - 99 10 11 - 50 10 1 - 10 ALL MI L-C-85498 CAS ) Number of Composite samples 5 4

12、3 2 a. 6. Type I - A11 properties, Type rI - NCO content and pH. 3.5 Toxtc products and safety. Safety regulations and guidelines appltca6le to the use of the cnrtng agents should be complied with to preclude personal tnjury and damage to eqntpment and fact1 Wes. 3.6 Workmanshtp. PTorkmanship shall

13、6e such that the curtng agents are unfform in appearance, of consistent htgh qnaltty and free from irtst.61 e contqninatton. 4 QUALITY ASSURANCE PROY TSIONS. 4.1 Responsibil tty for inspection. Unless otherwise specified in the contract or purchase order, the contractor shall be responsible for the

14、performance of al 1 inspection requirements as specified herein. Except as otherwise specified, the Contractor may utilize his own facilities or any commercial laboratory acceptable to the Government. The Government reserves the right to perform any of the tnspectons set forth in this spectflcation

15、where such inspections are deemed necessary to assure that suppl ies and sewices conform to prescribed requirements. . 4.2 Sampl in%. The 1 ot shall be sampled in accordance with Tab1 e I I. TABLE II. Sampling plan. -. 3 - Provided by IHSNot for ResaleNo reproduction or networking permitted without

16、license from IHS-,-,-MIL-C-85478 68 m 7779906 O323667 7 W MIL-C-85498 (AS) 4.2.1 Primar Sam les. Physical property tests shall be run on each primary sample -F- see Table II). The material container may be sampled by use of-a clean glass tube, rd, or pipet. enough to be handled safely, the sample ma

17、y be obtained by pouring. smallest sample size possible that is consistent with test requirements shall be taken. The minimum sample size shall be two ounces. Glass containers shall be used for all liquid samples. labeled with date, lot number, and manufacturers container identifi- cation number. Ta

18、tlure of any primary sample to pass all of the physical propertles tests herein shall result in rejection of the lot represented. 4.2.2 Composite samples. Chernical properties tests shall be run on each composite sample. number of composites shown in Table II. Blend each composite thoroughly by mani

19、pulation of the container. Label each composite with Roman numerals, also include date, lot numbers, and manufacturers container identtfication numbers. The remainder of the primary samples shall be retained pending acceptance or rejection of the lot. Failure of any composite sample to pass all of t

20、he chemical properties tests herein shall result in rejection of the lot represented. If the container is small The Each sample shall be Divide the primary samples equally into the 4.3 Quality conformance inspections and tests. Quality conformance inspectfons and tests shall consist of the following

21、: a. Tests of Table I properties (see 4.4 and 3.3). b. Inspection of filled containers (see 4.5.1). c. Visual inspection (see 4.5.2). 4.4 Test methods. Tests shall be performed using apparatus, reagents, and proc.edures specified herein. or procedures shall require prior written approval of the proc

22、uring activity. Al 1 American Chemical Society (ACS) reagents shall1 conform The use of al ternate apparatus, reagents, to MIL-STD-1218. 4.4.1 Isocyanate (NCO) content. 4.4.1.1 Apparatus. a. b. Iodine flask, 250-milliliter (ml). c. Pipet, 5-ml . Magnetic stirrer, variable speed, with Teflon-coated s

23、tirring bars, or equal. 4.4.1.2 Reagents. f a. Isopropanol ACS reagent., P 4 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-C-85LI98 68 9999906 OL23bb 7 b. C. d. e. 7. i 9. I h. i. 3. k. 1. I i MIL-C-85498(AS) Toluene, ACS reagent (dried oyer si

24、lical gel). Di-n-butylamine (Eastman No. 1260 or equal ) solution, 1 Nomal CN;) (25.8 grams CgmT ln 200.ml of dry toluene). StandardPzed hydrochloric acid ln isopropanol , 0.2 N (use tris tydroxymethyl mino methane (THAM procedure fw standardi - zatfon. Bromphenol blue tndlcator solution (0.01 gm in

25、 25 ml of ethanol). Alcohol ic potasslum hydroxide solution, 0.5 N. Phenol phthal ein. Nitric acid solution, 8.0 N. Standard silyer nitrate solution, 0.02 N. Nitrobenzene. Forty percent ferric ammonium sulfate indicator solution. Potassium theocyanate solution, 0.01 N. 4.4.1.3 Determination of isocy

26、anate. Weigh accurately 0.6 to 0.8 gm for Type I or 0.15 to 0.17 gm for Type II into a 250-ml iodine flask. Add 50 ml of dry toluene to the sample flask and to two other flasks to be used as blanks. Pipet 5 ml of 1 N di-n-butylamine solution into the flasks, replace the stopper, stir with a magnetic

27、 stirrer, and let stand 30 minutes. indicator solution. isopropanol solution to the yellow end point. Add 50 ml of isopropanol and 0.5 ml of bromophenol blue Titrate with standardized hydrochloric acid in Calculation: B-V) x N x 4.202 W Percent NCO = ( Where: B = average volume of standardized hydro

28、chloric acid for V = volume of standardized hydrochloric acid for sample, N = normal ty of standardized hydrochloric acid solution Pi = weight of sample, gm blanks, ml ml Report the NCO to the nearest 0.01 percent. Provided by IHSNot for ResaleNo reproduction or networking permitted without license

29、from IHS-,-,-MIL-C-85478- 68 = 9777706 0323667 O W MIL-C-85498(AS) 4.4.2 Moisture. 4.4.2.1 Apparatus. Beckman “Aquameter“, Model Kq-4, or equal. 4.4.2.2 Reagents. a. Karl Fi scher (KF) reagent, comercial strength. b. Standardtzed KF reagent, stabilized, water equivalent of 2.0 to 3. O mil 1 igramclm

30、ill i 1 i ter (mg/ml. c. Pyridine, ACS reagent. d. Chloroform, ACS reagent. 4.4.2.3 Determination of moisture. To the reaction beaker containing 60 ml of a 1:l ratio neutralized pyridine-chloroform solution, add 9 to 10 gm of sample which is weighed by difference to the nearest 0.01 gm. The stirrer

31、should be off while adding the sample. Turn on the stirrer to the same position used in the neutralization. Titrate automatically by pressing the titrate button to a 30-second end point. Cal cul ati on : Percent moisture = VxE Where: V = volume of standardized KF reagent, ml E = water equivalent of

32、KF reagent, mg/ml i4 = weight of sample,. gm Report the average of duplicate analyses to the nearest 0.001 percent . 4.4.3 Infrared spectrum. 4.4.3.1 Apparatus. Infrared spectrophotometer, Perkin-Elmer Model 21 or equal, equipped with sodium chloride windows. 4.3.3.2 Procedure. Prepare a smear of th

33、e sample to be tested on the sodium chloride windows in a thin continuous film. Scan the infrared spectrum from 4000 centimeters- (2.5 micrometers) to 666 centimeters- (15 micrometers) for the material being tested. Compare the spectrum obtained with Figure 1 for Type I or Figure 2 for Type II. 6 Pr

34、ovided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-C-85478 68 7777706 0123670 7 MIL-C-85498(AS) 4.4.4 pH. 4.4.4.1 Apparatus. a. pH indicator, Leeds and Northrup, No. 7664, or equal, equipped with Calomel electrode standard 11 99-31 and glass electrode

35、 standard 11 99-30 or equal . b. Separatory funnel, 250-ml . 4.4.4.2 Reagents. a. Sodium hydroxide, 0.01 N. b. Distilled water, pH 7.0. c. Hydrochloric acid, 0.01 N. d. Standard buffer solution, pH 7.0. 4.4.4.3 Instrument standardization. Adjust the pH indicator to read a pH of 7.0 using the standar

36、d buffer solution. 4.4.4.4 Preparation of pH of 7.0 distilled water. Adjust the pH of 200 mi of distilled water to 7.0 with approximately 0.01 N sodium hydroxide or hydrochloric acid. 4.4.4.5 Determination of pH. Pour 50.0 ml of sample into a 250-ml Stopper separatory funnel and add 50.0 ml of 7.0 p

37、H distilled water. the funnel and shake vigerously for 1 minute. Let stand for 5 minutes or until separated in definite layers, draw off the lower phase for Type I and upper phase for Type II into a 150-ml beaker, and detemine the pH of the aqueous solution by using the pH meter and following the in

38、structions supplied with the instrument. 0.1 pH unit. Report the pH to the nearest 4.4.5 Hydrolyzable chlorine. 4.4.5.1 Type I. Hydrolyzable chlorine shall be determined in accordance with ASTM-D-1638, Methods 40 through 46. the nearest 0.01 percent. Report hydrolyzable chlorine to 4.4.5.2 Type II.

39、Hydrolyzable chlorine shall be determined as follows: a. Weigh 5.0 gm to the nearest mg sample into a round bottom flask. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-C-85478 b 777790b OL23b7L 7 b. Add 50.0 rnl of 0.5 N alcholic potassium hydr

40、oxide solution and reflux for 45 minutes; cool the solution, add seyeral drops of phenolphthalein, and make slightly acld-ic by adding concentrated nitric acid from a dropping bottle. c. Add 5.0ml of 6 N nitric acid solution. b d. Add exactly 10.0 ml of standard 0.02 N silver nitrate solution from a

41、 buret. e. Add 5.0 ml of nitrobenzene plus 2.0ml of 40-percent ferric amnonium sul Pate indicator solution. P. Back titrate to first reddish coloration with standard 0.01 N potasslum thiocyanate sol ution. g. Calculate hydrolyzable chlorine as follows: Percent hydrolyzable chlorine = (V1.x N1-V2 x N

42、e) x 3.546 W Where: V1 =. volumeof standard silver nitrate, ml N1 =. normality of standard silver nitrate V2 = volume of standard potassium thiocyanate, ml N2 = normality of standard potassium thiocyanate W = weight of sample, gm Report hydrolyzable chlorine to the nearest 0.01 percent. 4.5 Examinat

43、ions. 4.5.1 Inspection of filled containers. All filled containers shall be inspected prior to shipnent or use for accuracy of markings and for .defects in containers and closures. All defective containers and closures shall be repaired or replaced, and contents therein shall be reinspected prior to

44、 shipment or use. .4.5.2 Visual inspection. All samples shall be visually inspected to deterniine conformance to the requirements of 3.6. 4.6 Records. Certification and test data shall be prepared s required by the procuring activity (see 6.2.21. 8 ., Provided by IHSNot for ResaleNo reproduction or

45、networking permitted without license from IHS-,-,-MIL-C-85498 68 m 997770b 0323672 O m 5. PACKAGING. 5.1 Packaging and packing. Unless otherwise specified in the purchase order (see 6.2.1), packaging and packing of the.curing agents shall be in accordance with commercial practice to insure carrier a

46、cceptance and shall be of such construction and materials that the contents will be adequately protected against 1 oss or contamination. 5.2 Marking for shipment. Unless otherwise specifled fn the purchase order (see 6.2.1 2, each shippincl container shall be marked in accordance with the requiremen

47、ts of MTLLSTb-129. the fol lowing: Container marking shall include a. The suppliers lot number. b. Procuring activity purchase order number. c. Container identification (applied in numerical sequence as the containers are filled). d. Date of manufacture. e. Manufacturers Code Ident. f. Net and tare

48、weight of the container. g. Material identification. WARN1 NG Toxic material. Avoid skin contact. Do not breathe vapors. 6. NOTES AND CONCLUDING MATERIAL. 6.1 Intended use. The intended uses of the material described herein are as curing agents in solid propellant and rocket motor case liner formu 1

49、 at i ons . 6.2 Ordering data. 6.2.1 Procurement requirements. Procurement documents should specify the following: a. Title, number and date of this specification. 6. Responsibility for fnspection and inspection facilities if different than 4.1. 9 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,- MIL-C-