NAVY MIL-I-85492-1981 IMINE CURING BONDING AGENT《亚胺固化 粘接剂》.pdf

1、/ MIL-1-85492 b8 W 7977706 0323b07 O MI L- 1-85492 (AS) 6 October 1981 MI LI TARY SPEC1 FI CATI ON l-t- 1.5- 2/ IMINE CURINGJBONDING AGENT This specification is approved for use by the Naval Air Systems Command, Department of the Navy, and is available for use by all Departments and Agencies of the

2、Department of Defense. 1. SCOPE. 1.1 -. Scope. . This specification establishes the requirements for two types of imine curing/bonding agents to be used as ingredients in case liners and propellants of solid rocket motors. following types: 1.2 Classification. The imine curing/bonding agents shall be

3、 of the Type I: 1 , 1 - (1,3-phenyl ene di carbonyl ) bis 2- methyl -az i ri di ne Type II: 1, 1 I ,l1-(1,3,5-benzenetriyl tricarbonyl) tris 2-ethyl -aziridine 2. APPLICABLE DOCUMENTS. I 2.1 Issues of documents. The following documents of the issue in effect on date of invitation for bids or request

4、 for proposal form a part of this specification to the extent specified herein. STANDARDS MILITARY MIL-STD-129 Marking for Shipment and Storage. (Copies of specifications, .standards, drawings and pub1 ications required by contractors in connection with specified procurement functions should be obta

5、ined.from the procuring activity or as directed by the contracting officer. ) Beneficial comments (recomnendations, additions, deletions) and any pertinent data which may be of use in improving this document should be addressed to: Comnanding Officer, Naval Air Engineering Center, Engineering Specif

6、ications and Standards Department (ESSD) Code 93, Lakehurst, NJ 08733, by using the self-addressed Stan- dardization Document Improvement Proposal (DD Form 1426) appearing at the end of this document or by letter. FSC 68lOl Provided by IHSNot for ResaleNo reproduction or networking permitted without

7、 license from IHS-,-,-MIL-I-85Ll72 68 = 7777Ob 0123608 2 Pro per ty Type I .Min Max Imine equivalent weight, 129 145 g/g equ i val en t percent Hydrolyzable chlorine, - o. 9 Moisture, percent - O. 25 MIL-I-85492 (AS 1 Type II Min Max 135 155 - o. 9 - 0.25 2.2 Other publications. The following docume

8、nts form a part of this soecification to the extent specified herein, Unless otherwise indicated, the issue in effect .on date of invitation for bids or request for proposal shall apply. American Society for Testing and Materials (ASTM) ASTM E 203 Water Using Karl Fischer Reagent, Test Por. Applicat

9、ion for copies should be addressed to the American Society for Testing and Materials, 1916 Race Street, Phfiladelphia, PA 19103.) 3. REQUIREMENTS. 3.1 Product characteristics, The imine curing/bonding agents chal 1 be amber, viscous liquids. 3.2 Chemical properti es .* Chemical properties of the imi

10、 ne curing/ bonding agents shall conform to Table I. TABLE I. Chemical properties. 3.4 Stability. When stored in accordance with 3.3, the imine curing/ bonding agents shall have sufficient chemical stability to permit storage for a minimum of 12 months without exceeding 150 grams/gram (g/g) equivale

11、nt for Type I and without exceeding 170 g/g equivalent for Type II when retested in accordance with 4.3.1. . I 2 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-I-85LI92 68 W 9999906 0323609 Lt 3.5 Toxic products and safety. Safety regulations an

12、d guidelines applicable to the use of imine curing/bonding agents should be complied with to preclude personal injury and damage to equipment and facilities. 3.6 Workmanship. Workmanship shall be such that the imine curing/ bonding agents are uniform and of consistent high quality. 4. QUALITY ASSURA

13、NCE PROVISIONS. 4.1 Responsibility for inspection. Unless otherwise specified in the contract or purchase order (see 6.2.1 1 the contractor is responsible for the performance of all inspectionrequirements as specified herein. Except as Otherwise specified in the contract or purchase order, the contr

14、actor may use his own or any other facilities suitable for the performance of the inspection requirements specified herein, unless disapproved by the Government. The Government reserves the right to perform any of the fnspections set forth in this specification where such inspections are deemed nece

15、ssary to assure that supplies and services conform to perscribed requirements. curing/bonding agents shall be classified as follows. 4.2 Classification of tests. Inspection and testing of the imine 4.2.1 Quality conformance inspections and tests. Quality conformance inspections and tests shall consi

16、st of the following: a. Tests of Table I properties (see 4.3). b. Inspection of filled containers (see 4.5.1). c. Visual inspection (see 4.5.2). 4.2.1 . 1 Sampl i ng. A representati ve sampl e 1 arge enough to perform all tests and a retain sample shall be taken from each lot of material. 4.2.1.2 Ac

17、ceptance criteria. .Failure of any sample to pass all of the requirements specified herein shall cause rejection of the lot represented. 4.3 Test methods. Tests shall be performed using apparatus, reagents, and procedures specified herein. or procedures shall require prior written approval of the pr

18、ocuring activity. The use of al ternate apparatus, reagents , 4.3.1 Imine equivalent weight. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MI L- 1-85492 (AS) I 4.3.1.1 Determination of imine equivalent weight. Add 50 milliliters (ml ) of methanol i

19、c potassium thiocyanate (KSCN) solution (prepared by dissolving 160 grms (gm) of potassium thiocyanate in methanol and diluting to 1 liter) into a 125-ml Erlenmeyer flask fitted with a nitrogen purge. Pipet 10.00 ml of 0.4 Normal (N) methanolic hydrochloric acid (prepared by thoroughly mixing 34 ml

20、of concentrated hydrochloric acid in methanol and diluting to 1 liter) into the flask and thoroughly mix the two solutions. Weigh, to the nearest 0.1 milligram (mg), 0.3 to 0.4 gm of sample into the flask and str 5 to 6 minutes. Add 3 drops each of 0.1 percent alcoholic bromothymol blue sodium salt

21、and 0.1 percent alcoholic phenol red sodium salt indicators. Titrate to a purple end point with standardized 0.1 N a7cohol ic potassium hydroxide (KOH) (prepared by dissolving 6 gm of potassium hydroxide in methanol and diluting to 1 liter). Determine two reagent blanks following the above procedure

22、. Cal cul ation: w x 1000 WN mine equivalent weight, g/g equivalent = Where: V1 = volume of alcoholic KOH used for blank, ml V2 = volume of alcoholic KOH used for sample, ml N = normal i ty of alcohol ic KOH W = weight of sample, gm Report the imine equivalent weight to the nearest whole unit. 4.3.2

23、 Hydro1 yzabl e chlorine. 4.3.2.1 Determination of hydrolyzable chlorine. Weigh, to the nearest 0.1 milligram (mg), a 1 gm sample into a 250-ml flask with a ground glass neck, Add 50 ml of-0.5 N alcoholic potassium hydroxide (prepared by dissolving 30 gm of potassium hydroxide in methanol and diluti

24、ng to 1 liter) and a few boiling chips to the flask. Insert a condenser into the flask and heat to maintain a steady drop rate for 45 minutes (start timing when first reflux begins). cool , rinse the condenser with approximately 50 ml of methanol and disconnect flask. Quantitatively transfer the sol

25、ution to a 400-ml beaker using small portions of methanol. neutralize the solution by dropwise addition of concentrated nitric acid solution, then add 3 ml excess. Titrate potentiometrically with stan- dardized 0.02 N silver nitrate (prepared by dissolving 3.4 gm of silver nitrate in distilled water

26、 and diluting to 1 liter) using a combination of silver-billet/double junction glass electrode and auto- matic titrator. Run a reagent blank using the same method. Allow solution to Using methyl red indicator, Calculation: Hydrolyzable chlorine, percent = 3.545(v1 - V2) N W 4 Provided by IHSNot for

27、ResaleNo reproduction or networking permitted without license from IHS-,-,-there: V1 = - y2 - Ns w= 3.545 = MIL-I-85LI72 68 W 7777706 OL23blL 2 W volume OP standardized 0.02 N silver nitrate used for sampl e, ml volume of standardized 0.02 N silver nitrate used for blanks, ml normality of standardiz

28、ed 0.02 N silver nitrate weight of sample, gm 0.1 atomic weight of chlorine Report hydrolyzable chlorine to the nearest 0.1 percent 4.3.3 Moisture. The moisture content shall be determined in ac- cordance with ASTM E 203 using a 5.0 plus or minus 0.1 gm (weighed to the nearest 0.1 mg) sample titrate

29、d to a 30-second end point. shall be methanol-chloroform, 1 :1 by volume. Report moisture content to the nearest 0.01 percent. Solvent 4.4 Stability. During the first 12 months of storage in accordance with 3.3, the material shall conform to Table I. Shelf life may be extended for an additional 6-mo

30、nth period by verifying conformance to Table I. 4.5 Exami nations. 4.5.1 Inspection of filled containers. All filled containers shall be inspected prior to shipment or use for accuracy of markings and for defects in containers and closures. shall be repaired or replaced, and contents therein shall b

31、e reinspected prior to shipment or use. Al 1 defective containers and closures 4.5.2 Visual inspection. All samples shall be visually inspected to determine conformance to the requirements of 3.6. 4.6 Records. Certification and test data shall be prepared as required - by the procuring activity (see

32、 6.22). 5. PACKAGING. 5.1 Preservation-packaging and packing. Unless otherwise specified in the contract or purchase order (see 6.2.1), packaging and packing of the imine curing/bonding agent shall be in accordance with commercial practice to insure carrier acceptance and shall be of such constructi

33、on and materials that the contents will be adequately protected against loss or contamfnatton. Protection from loss shall include packing in dry Ice to prevent temperature degradation during transi t. 5 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,

34、- MIL-1-85492 68 W 9979906 0123612 MIL- 1-85492 (AS) 5.2 Marking for shipment. Unless otherwise specified in the contract or purchase order see 6.2.72, each shipping container shall be marked in accordance with the requirements of MIL-STD-129. shall include the following: Container markings a. The s

35、uppliers lot number. b. Storage conditions. CAUTION SHIP AND STORE AT TEMPERATURES BELOW -18C c. Toxicity warning. d. Date of manufacture. e. Manufacturers Code Ident. f. Net weight of contents. g. Material name. 6. NOTES AND CONCLUDING MATERIAL. 6.1 Intended use. The intended use of the materials d

36、escribed herein are as a bonding agent between ammonium perchlorate and polymer for Type I, and as a bond promoter in a liner composition for Type II. 6.2 Ordering data. 6.2.1 Procurement requirements. Procurement documents should specify the f o1 1 owi ng : a. b. Title, number, and date of this spe

37、cification. Responsibility for inspection and inspection facilities, if different than 4.1. Special packaging, Racking, or marking requirements, if applicable (see Section 5). c. 6.2.2 Data requirements. When this specification is used in a pro- curement which incorporates a Contract Data Requiremen

38、ts List (DD Form 1423) and invokes the provisions of 7-104.9(n) of the Defense Acquisition Regulations (DAR) the data requirements identified below will be developed as specified by an approved Data Item Description (DID) (DD Form 1664) and delivered in accordance with the approved DD Form 1423 inco

39、rporated into the contract. When the provisions of DAR-7-104.9(n) are not invoked, the data specifiedbelow will be delivered by the contractor in accordance with the contract requirements. Del iverabl e data required by this specification is cited in the following paragraphs: i Provided by IHSNot fo

40、r ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-I-Sq92 b m 7797706 0123b13 b m - M 1 L - I -854 92 (AS 1 Paragraph Data Requfrement Appl i ca bl e DID 4.6 Cert i f fcat ion UDl-A-23264B Test Data DI-T-4024 (Copies of DIDs requtred by the contractors in connection wit

41、h specific procurement functtons should be obtained Prom the procurtng activity or as dfrected by the contracttng officer.) 6.3 Suggested source of supply, Products that haue met the requtre- mentc of this spectftcation in past procurement acttons are manufactured by Minnesota Mining and Wanufacturi

42、ng, Code Ident 28112 as HX 752 (Type I) and HX 868 (Type II). This information is for the convenience of the procuring acttvity and is not to be construed as a waiver of any require- ment of this specification nor as any limttation of additional potential source of supply. Pr epar i ng act i v i ty : Navy - AS (Project 681 O-NB1 7) *U$. GOVERNMENT PRINTING OFFICE: 1981-505-022/8504 7 ,- Y+ Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-