ARMY MIL-T-47063 A-1991 TRIETHYL CITRATE《柠檬酸三乙酯》.pdf

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1、MIL-T-47b3A 68 = 9999906 048LLBl b I Beneficial comments (recommendations, additions, deletions) and any pertinent data which may be of use in improving this document should be addressed to: Commander, U.S. Army Missile Command, ATTN: AMSMI-RD-SE-TD- ST, Redstone Arsenal, AL 35898-5270 by using the

2、Standardization Document Improvement Proposal (DD Form 1426) appearing at the end of this document or by letter. MIL-T-47063A (MI) 14 June 1991 SUPERSEDING MIL-T-47063 (MI) 10 May 1974 MILITARY SPECIFICATION TRIETHYL CITRATE This specification is approved for use by the U.S. Army Missile Command, De

3、partment of the Army, and is available for use by all Departments and Agencies of the Department of Defense. 1. SCOPE 1.1 Scope. This specification covers one grade of triethyl citrate. 2. APPLICABLE DOCUMENTS 2.1 Government documents. 2.1.1 Specifications, standards, and handbooks. The following sp

4、ecifications, standards, and handbooks form a part of this document to the extent specified herein. Unless otherwise specified, the issues of these documents are those listed in the issue of the Department of Defense Index of Specifications and Standards (DODISS) and supplement thereto, cited in the

5、 solicitation (see 6.2). AMSC N/A FSC 6810 DISTRIBUTION STATEMENT A. Approved for public release; distribution is unlimited. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-T-470b3A b E 9999906 048112 E MIL-T-47 O 63A (MI) STANDARDS FEDERAL FED-S

6、TD-313 - Material Safety Data, Transportation Data and Disposal Data for Hazardous Material Furnished to Government Act ivit les MILITARY MIL-STD-129 - Marking for Shipment and Storage MIL-STD-1190 - Minimum Guidelines for Level C Preservation, Packing and Marking (Unless otherwise indicated, copies

7、 of the federal and military specifications, standards, and handbooks are available from the Standardization Documents Order Desk, Bldg. 4D, 700 Robbins Ave., Philadelphia, PA 19111-5094.) 2.2 Non-Government publications. The following documents form a part of this document to the extent specified h

8、erein. Unless otherwise specified, the issues of the documents which are DoD adopted are those listed in the issue of the DODISS cited in the solicitation. Unless otherwise specified, the issues of documents not listed in the DODISS are the issues of the documents cited in the solicitation (see 6.2)

9、. AMERICAN SOCIETY FOR TESTING AND MATERIALS (ASTM) ASTM D 1193 - Standard Specification for Reagent Water ASTM D 1209 - Color of Clean Liquids (Platinum-Cobalt Scale) (Application for copies should be addressed to the American Society for Testing and Materials, 1916 Race Street, Philadelphia, PA 19

10、103.) AMERICAN CHEMICAL SOCIETY (ACS) Reagent Chemicals, American Chemical Society Speci.fications (Application for copies of ACS publications should be addressed to the American Chemical Society, 1155 16th Street NW, Washington, DC 20036). (Non-Government standards and other publications are normal

11、ly available from the organizations that prepare or distribute the documents. These 2 a Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-T-47063A 68 9999906 0481183 T MIL-T-470 63A (MI) Characteristic documents also may be available in or through

12、libraries or other informational services. ) 2.3 Order of precedence. In the event of a conflict between the text of this document and the references cited herein, the text of this document takes precedence. Nothing in this document, however, supersedes applicable laws and regulations unless a speci

13、fic exemption has been obtained. Minimum Maximum I 3. REQUIREMENTS Assay (as total ester), percent Moisture, percent Color, APHA number Acidity (as citric acid), percent 3.1 First article sample. When specified (see 6.2), a first article sample shall be subjected to first article inspection (see 6.3

14、) in accordance with 4.3 and 4.4, - 99.0 0.3 50 0.02 -_ - - 3.2 Chemical and physical properties. Chemical and physical properties of the triethyl citrate shall be as specified in table I. Saponification number 3.3 Material safety data sheets. A material safety data sheet shall be prepared in accord

15、ance with the requirements of FED-STD-313 (see 6.4). 607. O 611. O TABLE I. Chemical and physical properties. 3.4 Workmanship. The triethyl citrate shall be uniform in quality, free from foreign materials, and shall be manufactured under conditions and procedures standard to the industry. 4. QUALITY

16、 ASSURANCE PROVISIONS 4-1 Responsibility for inspection. Unless otherwise specified in the contract or purchase order, the contractor is responsible for the performance of all inspection requirements (examinations and tests) as specified herein. Except as otherwise specified in the contract or purch

17、ase order, the contractor may use his own or any other facilities suitable for the 3 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-T-47063A 68 E 9999906 048LLB4 I E MIL-T-47063A (MI) performance of the inspection requirements specified herein,

18、unless disapproved by the Government. The Government reserves the right to perform any of the inspections set forth in this specification where such inspections are deemed necessary to ensure supplies and services conform to prescribed requirements. 4.1.1 Responsibility for compliance. All items sha

19、ll meet all requirements of sections 3 and 5. The inspection set forth in this specification shall become a part of the contractors overall inspection system or quality program. The absence of any inspection requirements in the specification shall not relieve the contractor of the responsibility of

20、ensuring that all products or supplies submitted to the Government for acceptance comply with all requirements of as part of manufacturing operations, is an conformance to requirements, however, this known defective material, either indicated Government to accept defective material. 4.2 Classificati

21、on of inspections. specified herein are classified as follows: the contract. Sampling inspection, acceptable practice to ascertain does not authorize submission of or actual, nor does it commit the The inspection requirements a. First article inspection (see 4.4) b. Quality conformance inspection (s

22、ee 4.5). 4.3 Inspection conditions. Unless otherwise specified, all inspections shall be performed in accordance with the test conditions specified herein. 4.4 First article inspection. When specified in the contract or order (see 6.2) a first article sample shall be subjected to first article inspe

23、ction. First article inspection shall consist of all examinations and tests specified herein. The government shall witness the examinations and tests for the first article sample acceptance at the contractors plant. Subsequent units shall not be considered for acceptance until Government approval of

24、 the first article has been obtained. The quality shall be as specified in the contract or order. 4.5 Quality conformance inspections. Quality conformance tests for acceptance of the triethyl citrate shall consist of the following examinations and tests : 4 Provided by IHSNot for ResaleNo reproducti

25、on or networking permitted without license from IHS-,-,-NIL-T-47063A b I 9997906 0481185 3 I- Examination and test MIL-T-47 O 63A (MI) Requ i remen t Method paragraph paragraph TABLE II. Quality conformance inspection. e Assay (total ester) Moisture Color, APHA number Acidity (as citric acid) Saponi

26、fication number 3.2 3.2 3.2 3.2 3.2 4.11.1 4.11.2 4.11.3 4.11.4 4.11.5 4.6 K. A lot shall consist of triethyl citrate produced at one plant with no change in formulation or process. If manufacture is by batch process, each batch shall constitute a lot. 4.7 Batch. A batch is that quantity of material

27、 which has been subjected to one or more chemical or physical processes (or combination thereof) intended to produce a desired product having substantially uniform characteristics. 4.8 Sampling. The number of containers to be chosen at random for acceptance sampling shall be equal to the square root

28、 of the total number of containers in the lot. If the number thus obtained is not a whole number, the number of containers to be sampled shall be increased to the next higher whole number. In no case, however, shall the number of containers to be sampled be less than seven (unless there are less tha

29、n seven containers in the lot, in which case each container shall be sampled). 4.9 Primary sample. From each selected container, a sample shall be taken from three or more places throughout the container, The total weight of the sample from each container shall weigh at least 50 grams (9). Each samp

30、le thus taken shall be mixed thoroughly, placed in a clean, dry container and labeled to identify the material name, original container designation, contract number, and lot number. 4.10 Composite sample. Each primary sample shall be subdivided to prepare a composite sample (not greater than 500 g).

31、 Unused primary material. shall be returned to the primary sample container. After mixing the composite sample thoroughly, place the composite sample in a clean, dry container, seal and identify the composite sample with material name, container designations, contract number, and lot number. All spe

32、cified chemical and physical tests shall be made on this composite sample representing the lot. Failure of the composite sample to pass all the tests herein shall result in rejection of the lot represented. 5 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from I

33、HS-,-,-MIL-T-47063A 68 m 9999906 0481186 5 m MIL-T-47063A (MI) 4.11 Testing. the requirements of this specification have been met. to be specified in accordance with American Chemical Society reagent grade standards where appropriate. appropriate grade of ASTM D 1193. Any changes in the test procedu

34、res employed shall be subject to prior approval of the procuring activity. otherwise specified, all tests shall be run in duplicate. The average of the two results shall be taken as the test result. The following procedures shall be used to determine that Chemical reagents are Reagent water is to be

35、 specified by the Unless 4.11.1 Assay (as total ester). 4.11.1.1 Reaqents. a. Isopropyl alcohol, chemically pure (CP) . b. Sodium hydroxide, O. 5 normal (N) . C. Standardized sulfuric acid, 0.5N. d. Phenolphthalein indicator, USP XVI test solution. 4.11.1.2 Procedure. Accurately weigh 1.5 g of sampl

36、e into a 500- milliliter (mi) flask with a 24/40 standard taper ground-glass neck. Add 25 ml of isopropyl alcohol and 25 ml of distilled water. 0.5N sodium hydroxide into the reaction mixture. Add boiling chips and attach to a water-cooled condenser with 24/40 standard taper joint. Reflux for 1.5 ho

37、urs. Cool and wash down condenser with distilled water. Add 5 drops of phenolphthalein indicator and titrate with 0.5N sulfuric acid to a colorless end point. A blank using identical quantities of reagents is run simultaneously with the sample. Pipet exactly 50 ml of Percent assay (total ester) = (A

38、 - B) N x 0.092 x 100 C where : A = volume of sulfuric acid needed to titrate blank, ml B = volume of sulfuric acid needed to titrate sample, ml C = weight of sample, g N = normality of sulfuric acid 6 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-

39、c MIL-T-47063A b 999e190b 0481187 7 I MIL-T-47063A (MI) 4.11.1.3 Acceptance criteria. For the lot represented to pass the assay (as total ester) test, the value obtained for the percent assay (as total ester) shall be not less than the value specified in table I. 4.11.2 Moisture. 4.11.2.1 Apparatus.

40、 The apparatus used for determination of moisture content of the sample shall be an Aquameter, Model KF-4Bf or an approved equivalent. 4.11.2.2 Reagents, a. Karl Fischer reagent. Karl Fischer reagent must have a strength such that each milliliter of reagent corresponds to 0.0014-0.0023 g of water. D

41、ilute 750 ml of commercially available stabilized Karl Fischer reagent (with water equivalent of 0.005-0.007 g/mi) to 2000 ml with absolute methanol (not greater than 0.1 percent water). Mix well and allow to stand overnight before use. Determine the water equivalent (A) of this solution as follows:

42、 (1) Use sodium tartrate dihydrate (Na2C4062H20) as a primary standard (with a water content of 15.66 percent) for standardizing Karl Fischer reagent. If the water content value is in question, it may be determined by heating some of the salt at 150 Celsius (C) for 3 hours. Should the value (as dete

43、rmined) differ from the theoretical value of 15.66, then the experimental value shall be used in the determination of water equivalent (A) of the Karl Fischer reagent; instead of the 15.66 in the formula below, the factor should be lop, where P is percentage moisture (as determined). Rapidly transfe

44、r 0.090-0.110 g (weighed to the nearest 0.0001 9) of reagent-grade NasC4062H20 to the titration vessel. (2) Titrate to an end point in the same manner as with the sample. (See 4.11.2.3) (3) Repeat the standardization procedure until three successive results agree within five parts per thousand. 7 Pr

45、ovided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-T-47063A b m 9999906 04LL 9 m where : b. (4) Water MIL-T-47063A (MI) If the indicated water equivalent (A) of the Karl Fischer reagent is less than 0.0014 g of water per milliliter of Karl Fischer rea

46、gent, it may be due to the presence of too much water in the absolute methanol used. In this case, distill the methanol from metallic calcium or calcium hydride. Passing the methanol through a column of Molecular Sieves, Type 4A, or equivalent, may also reduce the water content of the methanol suffi

47、ciently. equivalent (A) = 156.6 W V A = water equivalent of the Karl Fischer reagent, g/ml V = volume of Karl Fischer reagent used, ml Water-in-methanol solution. The water-methanol solution should contain 0.0015-0.0020 g of water per milliliter of solution. A good grade of commercial absolute metha

48、nol contains about 0.0010 g water per milliliter of methanol. Water content can be adjusted by adding 1.0 g of water to 1000 ml of the water- methanol solution to produce a change of 0.0010 g per milliliter. Determine the relative strength of the water-methanol solution in terms of Karl Fischer reag

49、ent as follows: Put about 50 ml of the anhydrous methanol used in 4.11.2.2a into the titration beaker of the Aquameter. Add a slight excess of Karl Fischer reagent (4.11.2.2a), then back-titrate with water-methanol solution (4.11.2.2b). Then run in an additional 5 to 8 ml of Karl Fischer reagent, read to the nearest 0.01 ml, and again back-titrate with water-methanol solution (read to the nearest 0.01 mi). Repea