1、MIL- D- 22 346B (OS) 19 March 1973 SUPERSEDING MIL-D- 22346A (Wep) 21 December 1961 MILITARY SPECIFICATION DI-NORMAL-PROPYL ADIPATE This specification has been approved by the Naval Ordnance Systems Command, Department of the Navy. 1. SCOPE 1.1 This specification covers di-normal-propyl adipate for
2、use in propellants. 2. APPLICABLE DOCUMENTS 2.1 The following documents of the issue in effect on date of invita- - -.- tion for bids or request for proposal form a part of the specification to the extent specified herein. ! STANDARDS Mi lit ary MIL-STD- 129 Marking for Shipment and Storage (Copies
3、of specifications, standards, drawings, and publications required by suppliers in connection with specific procurement func- tions should be obtained from the procuring activity or as directed by the contracting officer.) 2.2 Other publications. The following documents form a part of this specificat
4、ion 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 E 200 Preparation, Standardization, and Storage of Standard Solutions for Chemical Analysis 1-1 THIS
5、 DOCUMENT CONTAINS 7 PAGES. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-D-22346B (OS) (Application for copies should be addressed to the American Society for Testing and Materials, 1916 Race Street, Philadelphia, Pa. , 19103.) 3. REQUIREMENTS
6、 f .* - “. . i- ._,_ -. . - -. . . 5- 3.1 Acidity. The acidity shall be 0.1 percent maximum when determined in accordance with 4.4.1. 3.2 Ester content. The ester content shall be 99.0 percent minimiim when determined in accordance with 4.4.2 and corrected for acidity as determined in 4.4.1. 3.3 Spe
7、cific gravity. The specific gravity shall be not greater than 0.982 nor less than 0.972 at 2Oo/2O0 centigrade (C) when determined in accordance with 4.4.3. 3.4 Freezing point, The freezing point shall be not lower than -19O C nor higher than -13“ C when determined in accordance with 4.4.4. AIlf . 3.
8、5 Refractive index. The refractive index shall be not greater than _- 1.4298 nor less than 1,4290 when determined in accordance with 4.4.5. 3.6 Color. The color shall be APHA 30 maximum or natural water white when determined in accordance with 4.4.6. 3.7 - Ash. The ash shall be 0.002 percent maximum
9、 when determined in accordance with 4.4.7. 4. QUALITY ASSURANCE PROVISIONS 4.1 Responsibility for inspection. Unless otherwise specified in the contract or purchase order, the supplier is responsible for the perfor- mance of all inspection requirements as specified herein. otherwise specified in the
10、 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 such i
11、nspections are deemed necessary to assure supplies and services conform to prescribed requirements. Except as 2 - Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-D-2234bB 68 = 9779906 OLL7745 I MIL-D-22346B (OS) 4.2 Sampling. 4.2.1 - Lot. A lot s
12、hall consist of di-normal-propyl adipate manufac- tured in one batch by the same processing, unit, chemical, or physical mixing process, which is intended to make the final product uniform. 4.2.2 Samples. At least 10 percent of the containers shall be sampled and a composite prepared therefrom for a
13、nalysis. 4.3 Acceptance criteria. Failure of any sample to meet any require- ment of this specification shall be cause for rejection of the lot, 4.4 Test methods. 4.4.1 Acidity. Weigh accurately to 0.1 milligram approximately 25 grams of the sample into a 125-milliliter (mi) Erlenmyer flask and diss
14、olve in 50 ml of ethyl alcohol. titrate to a persistant faint pink color with 0.1N sodium hydroxide solution prepared in accordance with ASTM E-200, paragraphs 13 through 18. Make a blank titration on 50 ml of the ethyl alcohol used to dissolve the following: Add 3 drops of phenolphthalein and . (2
15、I the sample. Calculate the percent acidity as adipic acid according to 7.3073 (A - B)N W Percent adipic acid = where A = ml of NaOH solution required for titration of sample B = ml of NaOH solution required for titration of blank N = normality of NaOH solution W = weight of sample in grams. 4.4.2 E
16、ster content as di-normal-propyl adipate. Transfer 1.5 grams of sample to a 250-ml Pyrex erlenmeyer or similar flask fitted with a ground glass joint. Add 50 ml of 0.5N alcoholic potassium hydroxide (KOH) by means of a calibrated buret or pipet. prepared by adding 28 grams of reagent grade KOH to 1
17、liter of 95 percent alcohol.) Fit the flask to a reflux condenser fitted with an NaOH-filled drying tube. complete. potassium adipate and reflux on a water bath for not less than 45 minutes with occasional swirling of the flask. Wash down the sides of the reflux (0.5N alcoholic KOH is Heat on water
18、bath until the precipitation appears to be Add approximately 15 ml of distilled water to dissolve the 3 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-D-2234bB b m 9999906 0127946 3 m MI L-D-22346B (OS) condenser and the ground joints with appro
19、ximately 25 ml of distilled water. Cool the solution to 25 C and titrate with 0.5N hydrochloric acid using phenolphthalein indicator. determination on 50 ml of alcoholic KOH which has been carried through the complete process. propyl adipate as follows: At the same time run a blank Calculate the est
20、er content as percent di-normal- Percent di -normal-propy 1 adipat e = (11.515; - n)N - (A X 1.58) where N = normality of the acid used V = ml of acid used to titrate blank n = ml of acid used to titrate excess of KOH W = weight of sample in grams A = percent acidicy as adipic acid. 4.4.3 Specific g
21、rzvity. Determine the specific gravity at 2Oo/2O0 C by means of a pycnometer or Westphal balance. - e.- .I 4.4.4 Freezing point. Heat a test tube moderately over a flame to remove moisture. Place about 35 grams of sample in test tube and place inner tube in outer tube of apparatus (figure 1). ice-ac
22、etone bath, and stir sample with a reciprocating action until first crystal forms, continuing the reciprocating stirring, note disappearance of crystal. Place assembly in dry This is the freezing point. Remove tube from bath and, 4.4.5 Refractive index. Determine the refractive index at 25 C by use
23、of an Abbe or dipping refractometer. 4.4.6 Color. 4.4.6.1 Standard preperation. Dissolve 1.245 grams of potassium chlorplatinate (KzPtC16) and 1 gram of crystallized cobaltous chloride (CoC126H20) in distilled water containing 100 ml of 37 percent hydro- chloric acid, and make up to 1000 ml in a vol
24、umetric flask with distilled water. This is best done in two steps for colors below 50 in order to avoid measurement of extremely small volumes of the color standard. table I for dilution ratios. Store the color standards in glass-stoppered bottles, preferably Pyrex. See Provided by IHSNot for Resal
25、eNo reproduction or networking permitted without license from IHS-,-,-MIL-D- 22346B (OS) I - -1; 1. . :i F-. . I. -. ! FIGURE 1. FREEZING Aluminum stirring rod loop end Standard thermometer Correction thermometer Cork stoppers Test tube 1 inch X 6 inches Test tube 1-1/2 inches X 7 inches POINT APPAR
26、ATUS 5 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-.- - - MIL-D-223qbB 68 7999906 0117748 7 I Color Milliliters of standards 500 standard ! MIL-D-22346B (OS) Milliliters of dis ti 1 led water Table I 4.4.6.2 Comparison. Compare the color of the s
27、ample visually with an equal amount of the Hazen color standards. done by placing the Hazen standards in Nessler tubes or in a uniformly shaped bottle and by placing the sample in a spare bottle of the same type glass and shape. It is suggested that 125-ml square glass-stoppered bottles be used alth
28、ough any style or shape bottle or Nessler tube may be used for comparison. that most nearly matches the sample. midway between two standards, report the darker of the two. This may conveniently be Report as the color, the number of the standard In the event that the color lies 4.4.7 - Ash. Weigh a p
29、ortion of approximately :O grams of the sample in an accurately tared porcelain crucible. over a low flame or on a hot plate. Ignite the residue to constant weight at a red heat. Cool the crucible in a desiccator md weigh. Calculate the increase in weight as percent ash as follows: Evaporate nearly
30、to dryness Increase in weight X 100 Weight of sample Percent ash = , Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-D-2234bB b W 79977Ob 0337747 7 = MIL- D- 2 2 336B (OS) 5. PREPARATION FOR DELIVERY 5.1 Packing. Packing shall be level C. Unless
31、otherwise specified, di-normal-propyl adipate shall be delivered in standard commercial con- tainers so constructed as to insure acceptance by common or other carriers for safe transportation, at the lowest rate, to the point of delivery. 5.2 Marking. Unless otherwise specified, containers shall be
32、marked in accordance with MIL-STD-129. 6. NOTES 6.1 Ordering data. Procurement documents should specify the following: a. Title, number, and date of this specification b. Quantity required. Custodian : Navy - OS Preparing activity : (Project No. 1375-0401) Navy - OS * U. S. GOVERNMENT PRINTING OFFICE: 1973 -714-544/4574 7 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-
