1、MIL-A-47059 (MI ) 10 May 1974 SUPERSEDING MIS 14156A 29 December 1965 M I L IT ARY S PE C I F I CAT I ON ACETYL TRIETHYL CITRATE This specification is approved for use by all departments and agencies of the Department of Defense. 1. SCOPE 1.1 Scope. This specification covers one grade of acetyl trie
2、thyl ci trate. 2. APPLICABLE DOCUMENTS 2,l Government documents. The following documents, of the issue in effect on date of invitation for bids or request for proposal, form a part of the specification to the extent specified herein. SPECIFICATIONS Mi 1 i tary MIL-P-14232 Parts, Equipment, and Tools
3、 for Army Material , Packaging and Packing of STANDARDS Mi 1 i tary MIL-STD-129 Marking for Shipment and Storage (Copies of specifications y standards y drawings, and publications required by suppliers in connection with specific procurement functions should be obtained from the procuring activity o
4、r as directed by the contracting off i Cer. ) FSC 6810 -_ THIS DOCUMENT CONTAINS PAGES. (N Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-A-47059( MI) - Characteristic Assay (total ester) , percent Moi s ture , percent Color, APHA number Acidity
5、 (as citric acid) , percent 2.2 Other publications. The following documents, of the issue in effect on date of invitation for bids or request for proposals, form a part of this specification to the extent specified herein, American Society For Testing and Materials ASTM D 1209 Color of Clear Liquids
6、 (Platinum- Coba1 t Scale) Minimum Maximum 99 .o - - O. 3 - 50 - o .o2 (Application for copies should be addressed to the American Society for Testing and Materials, 1916 Race Street, Philadelphia, Pennsylvania 19103 o ) Technical society and technical association specifications and standards are ge
7、nerally available for reference from libraries. distributed among technical groups and using Federal agencies. They are also 3. REQUIREMENTS 3.1 Preproduction sample. Unless otherwise specified (see 6.2) , a preproduction sample shall meet all the requirements of this speci- fi cat ion. 3.2 Chemical
8、 and physical properties , Chemical and physical properties of the acetyl triethyl citrate shall be as specified in Table I. Table I, Chemical and physical properties 3.3 Workmanship. The acetyl triethyl citrate shall be uniform in quality, free from foreign materials, and shall be manufactured unde
9、r conditions and procedures standard in the industry. 4, QUALITY ASSURANCE PROVISIONS 4.1 Responsibility for inspection, Unless otherwise specified in the contract or purchase order, the supplier is responsible for the perform- ance of all inspection requirements as specified herein, wise specified
10、in the contract or order, the supplier 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 inspections set forth in the specification where
11、such inspections are deemed necessary to assure supplies and services conform to prescribed requirements. Except as other- 2 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-A-q7059 b8 m 7777706 0320803 7 m MI L-A- 47059 (MI ) 4.1.1 Acceptance ins
12、pection, Acceptance inspection shall, at the option of the Government, be performed either by the supplier or by a Government representative., acceptance rests with the Government representative. In either case, responsibility for final 4.2 Preproduction sample. The preproduction sample shall be pre
13、pared using the same methods proposed for the preparation of subsequent production lots of acetyl triethyl ci trate. The preproduction sample shall be subjected to all the examinations and tests specified herein. Unless otherwise specified, the Government will perform the examinations and tests for
14、preproduction sample acceptance at the con- tractors plant, Preproduction samples which do not meet all the require- ments of this specification shall be rejected and returned to the contractor. Subsequent quantities will not be considered for acceptance until approval of the preproduction sample ha
15、s been obtained. 4,3 m. A lot shall consist of actyl 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. A batch shall be defined as in 6.3. the are sha s ha The 4.4 Acceptance samplinq, The number of
16、 containers to be chosen at random for acceptance sampling shall be equal to the square root 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 high whole number. In no case, however,
17、shall number of containers to be sampled be less than seven (unless there less than seven containers in the lot, in which case each container 1 be sampled), 4,4,1 Primary sample. From each selected container, a sample 1 be taken from three or more places throughout the container. total weight of the
18、 samples taken from each container shall weigh at least 50 granis (g)u placed in a clean, dry container, and labeled to identify the material name, original container designation, contract number, and lot number, Eacn sample thus taken shall be mixed thoroughly, 4,4.2 Composite sample. Each primary
19、sample shall be subdivided to prepare a composite sample (not in excess of 500 9). material not used 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 the
20、material name, container designation, contract number, and lot number. All specified chemical and physical tests shall be made on this composite sample representing the lot, Failure of the composite sample to pass all of the tests herein shall result in rejection of the lot represented, Primary 3 Pr
21、ovided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-A-47057 68 7799906 OL2OO4 9 4.5 Classification of tests. Inspection and test triethyl citrate shall be classified as follows: ng of the acety a. Preproduction tests. b. Qual i ty conformance tests o 4
22、.6 Preproduction tests, Preproduction tests shall be conducted only on the preproduction sample and shall consist of all the examinations and tests specified herein. 4.7 Quality conformance tests. Quality conformance tests for acceptance of the acetyl triethyl citrate shall consist of the following
23、examinations and tests: Characteristics Test - Assay (total ester) 4.8.1 Moi s ture 4,8.2 Color, APHA number 4.8,3 Acidity (as citric acid) 4.8.4 4.8 Acceptance tests. The following procedures shall be used to determine that the requirements of this specification have been met. Any changes in the te
24、st procedure employed shall be subject to prior approval of the procuring activity Unless otherwise specified, all tests shall be run in duplicate. The average of the two results shall be taken as the test result. 4,8.1 Assay (as total ester). 4.8.1.1 Reagents. a. b. Sodium hydroxide, 0.5 normal (N)
25、. Isopropyl al coho1 , chemical ly pure (CP) . c. Standardized sulfuric acid, 0.5 N. du Phenolphthalein indicator, USP XVI test solution. 4.8.1.2 Procedure. Accurately weigh 1-5 g of sample into a 500- milliliter (m1)ith a 24/40 standard taper ground-glass neck. Add 25 ml of isopropyl alcohol and 25
26、 ml of water. Pipette exactly 50 ml of 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 1-1/2 hours, Cool and wash down condenser with dis- tilled water. Add five drops of phenolphthalein indicator a
27、nd titrate with 0.5N sulfuric acid to a colorless endpoint, A blank using identi- cal quantities of reagents is run simultaneously with the sample. Percent assay equals ( A minus B) N times 0.0796 times 100 (as total ester) C 4 Provided by IHSNot for ResaleNo reproduction or networking permitted wit
28、hout license from IHS-,-,-MIL-A-LI7059 68 9799706 0120805 O MIL-A- 47059 (MI ) Where: A equals volume of sulfuric acid needed to titrate blank, ml B equals volume of sulfuric acid needed to titrate sample, ml N equals normality of sulfuric acid C equals weight of sample, g 4.8.1.3 Acceptance criteri
29、a. For the lot represented to pass the assay (as total ester) shall be not less than the value specified in 3.2. 4.8.2 Mois ture determi na ti on. 4.8.2.1 Apparatus. The appartus used for determination of moisture content of the same shall be Aquameter, Model KF-2 or KF-3, Beckman Instruments, Inc.
30、, Fullerton, Cal ifornia, or approved equivalent. The Aquameter shall be prepared for operation as described in the tech- nical manual furnished by the manufacturer (Beckman Instruments, Inc.). Use of an alternate equivalent item of equipment approved by the procuring activity wi 11 necessi tate use
31、 of the specific techni cal manual prepared by the manufacturer. 4.8.2.2 Reaqents. a. Karl Fischer reaqent. Karl Fischer reagent must have a strength such that each milliliter of Karl Fischer reagent corresponds to 0.0014-0.0023 g of water. Dilute 750 ml of commercially available stabilized Karl Fis
32、cher reagent (with water equivalent of 0.005-0.007 g/ml) to 2000 ml with absolute methanol (0.1 percent water, maximum). Mix well and allow to stand overnight before use. Determine the water equivalent (A) of this solution as follows: 1. Use sodium tartrate di hydrate (Na2CqH406 2H20) as a primary s
33、tandard (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 de rees Celsius (C) (302 degrees Fahrenheit (F 9 ) for 3 hours. Should the value (as determined) differ from the
34、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 transfer 0.090-0.110 g (weighed
35、 to the nearest 0.0001 g) of reagent-grade Na2C4H406*2H20 to the titration vessel. 5 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-A-47057 68 7977706 OL20Ob 2 MIL-A- 47059(NI) 2. 3. Titrate to an endpoint in the same manner as with the sample (
36、see 4.8.2.3). Repeat the standardization procedure until three successive results agree within five parts per thousand. If the indicated water equivalent (A) of the Karl Fischer reagent is less than 0.0014 g of water per milliliter of Karl Fischer reagent, it may be due to the presence of too much w
37、ater 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 equal, may also reduce the water content of the methanol Suff i ciently. 4. Water equivalent (A) equals 0.1566 W Whe
38、re: A equals water equivalent of the Karl Fischer reagent , g/ml B equals weight of Na2C4H406*2H20 taken, g V equals volume of Karl Fischer reagent used, ml b. Water-in-methanol solution. The water-in-methanol solution should contain 0.0015-0.0020 g of water per milliliter of solution. A good grade
39、of comercial absolute methanol contains about 0.0010 g of water per milli- liter of methanol. Water content can be adjusted by adding 1.0 g of water to 1000 ml of the water-in-methanol solution to produce a change of 0.0010 g per milli- ltier. Determine the relative strength of the water- in-methano
40、l solution in terms of Karl Fischer reagent as follows: 1. Put about 50 ml of the anhydrous methanol used in 4.8.2.2a into the titration breaker of the Aquameter. Add a slight excess of Karl Fischer reagent (4,8.2.2a), then back-titrate with water-in-methanol solution (read to the nearest 0.01 ml).
41、Repeat the addition and back-titrating steps twice more to provide triplicate determinations of the equivalency ratio. Calculate the ratio (B) of Karl Fischer reagent to 6 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,- _ MIL-A-47057 b m 7777906 032
42、0807 4 MIL-A-a7059(MI ) that of the water-in-methanol solution. The range of the ratios calculated from the three titrations shall not be greater than 0.04. If the range exceeds 0.04, continue making titrations until three ratios are obtained whose range does not exceed 0.04. Then determine the aver
43、age ratio from all the ratios which have been obtained. 4.8.2.3 Procedure. Determine the moisture content of the sample by the Karl Fischer method using a direct-titration technique. to the titration beaker, through the opening in the diaphragm, approximately 10 g of sample weighed to the nearest 0.
44、001 g. the stirrer and press the titrate button to titrate with Karl Fischer reagent (4.8.2.2a). buret to the nearest 0.01 ml. (4.8.2.2b) may be used to back-titrate. Introduce Close the opening, start When the indicator light glows, read the Karl Fischer Where necessary, water-in-methanol solution
45、100A (VKF minus BVwM) W Percent moisture equals Where: A equals weight of water equivalent to 1.00 ml of Karl Fischer reagent, g/ml VKF equals volume of Karl Fischer reagent titrant used, ml VWM equals volume of water-in-methanol solution titrant used, ml B equals ratio of Karl Fischer reagent to th
46、at of water-in- methanol solution, ml/ml W equals weight of sample taken, g 4.8.2.4 Acceptance criteria. For the lot represented to pass the moisture test, the value obtained for the percent moisture shall be no greater than the value specified in 3.2. 4.8.3 Determination of color. Reference: ASTM D
47、 1209. 4.8.3.1 Reagents and equipment. a. Coba1 t chloride, analytical reagent grade. b. Potassium chloroplatinate, chemically pure grade. c. Hydrochloric acid, concentrated, analytical reagent grade. d. Nessler tubes, APHA standard, high form, 50-ml capacity. 7 Provided by IHSNot for ResaleNo repro
48、duction or networking permitted without license from IHS-,-,-4.8.3.2 Preparation of standards. Dissolve exactly 1.245 g of potassium chloroplatinate and 1 g of cobalt chloride in a mixture of 500 ml of water and 100 ml of hydrochloric acid. Transfer to a liter volumetric flask, dilute to volume with
49、 water, and mix well. This solution has a color of 500 units. Transfer the aliquots of this stock solution, listed below, to 50-ml Nessler tubes and dilute to volume with water. The resulting standards have the corresponding color values in APHA units. Aliquot (ml) 0.50 1 .o0 2 .o0 3.00 4.00 5.00 7.50 10.00 15.00 20.00 30.00 40.00 50.00 Standard (APHA units) 5 10 20 30 40 50 75 1 O0 150 200 300 400 500 4.8.3.3 Procedure. Transfer exac
