1、i MIL-D-20305 b 7779706 0337473 3 M s-77-65 . I - i MIL-D-20305 21 November 1951 MILITARY SPECIFICATION DIMETHYLANILINE This specification was approved by the Depart- ments of the Army, the Navy, and the Air Force for use of procurement services of the respec- tive Departments, and supersedes the fo
2、llowing specification: Army 50-11-30C 17 June 1943 This specification consists of this cover sheet and Specification 50-11-30C, dated 17 June 1943, attached hereto, without modification. When a request for this specification is received by a supplying activity it will be necessary to attach this cov
3、er sheet to the pertinent specification before issue. Copies of specifications required by contractors in connection with specific procurement functions should be obtained from the procuring agency or as directed by the contracting officer. Custodian : Army-O A- / LFA GPO 83-40257 -y PHIS DOCUMENT C
4、ONTAINS b PAGES. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-D-20305 68 U 777770b OLL7474 5 U u. s. ARMY SPECIFICATION NO. 50-11-30C June 17, 1943 Super sed ing October 5, 1938 NO. 50-11-30B DIMETHYLANILINE A. APPLICABLE SPECIFICATIONS A-1. T
5、he following U.S.Army Specifications, of the issues in effect on the date of invitation for bids, form a part of this specification: No. 50-0-1, General Specification for Ammunition Except Small No. 100-2, Standard Specifications for Marking Shipments. Arms bunition B. GRADE. B-l. This specification
6、 covers one grade of dimethylaniline. C. MATERIALS AM) WORKMANSHIP. C-l. There are no requirements relative to materials or workmanship 5 applicable to this specification. D. GENERAL REQUIREMENTS. D-l. See section E. E. DETAIL REQUIREMWTS. E-1. Color.- Yellow E-2. Freezing point. - Minhum, 1.9O C. E
7、-3. Residue. -Maximum, 0.1 percent. E-4. Solubility. - 100 percent. E-5. Alkalinity or acidity. .- Maximum, 0.005 percent. E-6. Aniline. - MaximWn, 0.1 percent. F. METHODS OF SAMPLING, INSPECTION, AND TESTS. F-l. Inspection. Inspection shall be in accordance with Specification No. 50-0-1 and shall b
8、e at the point of delivery unless otherwise specified in the contract. . F-2. Size of lots. Maximum 30,000 pounds, if shipment is made in con- tainers other than tank cars. If shipment is made in tank cars, a lot shall consist of one tank car load. F-3. Sampling shall be done-as follows: If the dime
9、thylaniline is chlpped- in drums or smaller containers, select 10 percentbut not more than 10 of the containers so as to be representative of the lot. tents of each selected container, remove approximately 1 quart of material and place this in a tightly stoppered bottle. Mix the con- Label each prim
10、ary sample so Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-D-20305 b 9997906 OLL7V95 7 W that the container from which it was taken can be identified. Make a com- mary sample, and mix this thoroughly. ly stoppered bottle. If the material is sh
11、ipped in a tank car, remove the sample (approximately 1 quart) by means of a thief or a clean weighted bottle the material being sampled. Lower the unstoppered bottle by means of a cord, chain, or rod to the bottom of the tank, and immediately withdraw to the sur- face. In order to obtain a represen
12、tative cross section sample of the mater- ial, raise and lower the bottle at a uniform rate of speed, and regulate the speed so that the bottle is just filled as it reaches the surface of the liquid. Place this sample in a tightly stoppered bottle. Label the sample so as to show the name of the mate
13、rial, manufacturer, plant, purchase order, and number of pounds in the lot. representative of the lot. examination should the composite sample fail to meet the requirements. posite sample of approximately l.quart, comprising equal parts of each pri- 1 Place the composite sample in a tight- Rinse the
14、 bottle, which has a capacity of approximately 1 quart, with Make all acceptance tests on the sample Hold the primary samples for possible future F-4. Laboratory examination shall be made as follows: F-4a. Color. - Determine by visual inspection. F-4b. Freezing point. samle by addina 1 cc. of - Dry
15、a portion of approximately 50 cc. of the absolute alcohol, heating the solution for 1 hour C., and cooling in a sulphuric acid vacuum desi- ccator. Place the dried dimethylaniline in the test tube of the freezing point apparatus shown in Figure 1. Insert the aluminum rod and a standard- ized total i
16、mmersion thermometer, graduated in 0.2 C. or smaller subdivisions and extending over the range -100 to f loo C., into the cork stopper. Fasten a correction thermometer adjacent to the standardized thermometer so that its bulb will be approximately level with the center of the exposed mercury column
17、when the dimethylaniline freezes. test tube, and adjust the standardized thermometer so that its bulb is at least 1/2 inch from the bottom of the test tube. Clamp the tube assembly in the ice water bath so that the level of the dimethylaniline is at least 1 inch below the level of the bath. Stir the
18、 sample throughout the determina- tion, xaking approximately 120 complete up and down motions of the aluminum rod per minute. Watch the thermometer closely to determine when the temper- ature of the sample ceases falling and begins to rise due to the heat of crystallization. Note the temperature of
19、the sample every 15 seconds until the maximum is reached, and record this temperature as the uncorrected freezing point. this value as the average temperature of the exposed mercury column. Celcu- late the correction for emergent stem as follows: ) Insert the cork assembly into the Note the reading
20、on the correction thermometer and consider Emergent stem correction = n (T - t) x 0.000159 where n = number of degrees in the exposed mercury column, T = uncorrected freezing point. t = average temperature of the exposed mercury column. Calculate the freezing point of the sample by adding the emerge
21、nt stem and standardization corrections to the uncorrected freezing point value. For -“- , samples containing more than 1 percent of impurities, add salt to the bath if the dizethylaniline does not freeze in the ice water bath. Provided by IHSNot for ResaleNo reproduction or networking permitted wit
22、hout license from IHS-,-,-MIL-D-20305 b W 9779706 OLL7q76 7 M F-4. the sample the liquid and weigh. . sample. 96 percent F-4d. Residue. to a tared evaporating dish. By.means of a hot plate evaporate rapidly-to dryness. Cool the dish and contents in a desiccator Transfer a weighed portion of approxim
23、ately 100 grams of mlculate the increase in weight to percentage of residue in the Solubility. Add a 1 CC. portion of the sample to 10 cc. of 94 to sulphuric acid solution and shake the mixture. Note if the dime- thylaniline dissolves completely in the acid solution. Pour the solution in- to 50 cc.
24、of distilled water. solid matter, indicating that less than 100 percent of the dimethylaniline is soluble in sulphuric acid solution. Note if there is any separation of an-oil or F-4e. Alkalinity or acidity. Place 20 cc. of neutral distilled water in a 100 CC. separatory funnel and add a 25 gram por
25、tion of the sample. the mixture thoroughxy for 2 minutes and allow it to stand for a few minutes to permit separation into two layers. by means of a pipette transfer 10 cc. of this aqueous layer to a 100 cc. Erlenmeyer flask. Add 3 drops of rosolic acid indicator and titrate the solution with approx
26、imately N/10 hydrochloric acid or sodium hydroxide solutior Calculate the percentage of alkalinity or acidity of the sample. Shake Draw off the lower aqueous layer and Percentage of alkalinity, .as sodium hydroxide = Percentage of acidity, as hydrochloric acid = 7.293 AB C 8,001 AB C where A = volum
27、e of acid or alkali solution used. B-= normality of acid or alkali solution. C = weight of sample. F-4f; Aniline. By means of a pipette transfer 5 cc. portions of the sample toeach of 2 glass tubes. To each tube add 15 cc. of ether and 5 cc. of calcium oxychloride solution. Prepare the calcium oxych
28、loride solution by shaking 200 cc. of distilled water with not less than 35 grams of calcium hy- pochlorite, containing not less than 30 percent of available chlorine, until no further solution takes place. Allow the mixture to settle and filter the solution. The tubes should be such that the two 25
29、 cc. volumes of liquid form columns of equal height. Stopper the tubes, shake thoroughly, and allow to stand for 30 to 35 minutes. Compare the reddish colors produced in the ether layers with those produced in blanks started at the same time with freshly distilled pure dimethylaniline to which 0.1 p
30、ercent of aniline has been added. Note if the colors produced in the samples are no darker than those produced in the blanks, indicating the presence of not more than 0.1 percent of aniline. G. PACKIXG AND MARKING G-1. Packing. Unless otherwise specified, dimethylaniline shall be delivered in standa
31、rd commercial containers such as steel drums or tank cars, so constructed and protected as to conform with applicable regulations of the Interstate Commerce Commission and insure acceptance by common or other carriers for safe transportation, at the lowest rate, to the point of delivery. , / G2. Har
32、king. 1n.accordance with U. S. Army Specification KO. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-D-20305 b 9999906 0117c197 O and applicable regulations of the Interstate Commerce Commission. H. NOTES. H-l. Uses. Dimethylaniline covered by t
33、his specification is intended for use in the manufacture of tetryl. H-2. The use of this specification whenever applicable is mandatory on all procuring agencies of the Army. H-3. If the composite sample.representative of the lot fails to comply with the requirements, the manufacturer shall have the
34、 option of having analysis made of each primary sample at his own expense. place defective portions of the lot represented by the primary samples which fail to meet the requirements, and again submit the lot for inspection and acceptance, providing that the markings on the containers are such that c
35、om- plete replacement of defective portions of the lot can be made to the satisfac- tion of the inspector. The manufacturer may then re- Notice: When Government drawings, specifications, or other data are used for any purpose other than in connection with a definitely related Government procurement
36、operation, the United States Government thereby incurs no responsi- bility nor any obligation whatsoever; and the fact that the Government may have formulated, furnished, or in any way supplied the said drawings, specifi- cations, or other data is not to be regarded by implication or otherwise as.in
37、 any manner licensing the holder or any other person or corporation or convey- ing any rights or permission ta, manufacture, use, or sell any patented inven- tion that may in any way be related thereto. ri ) NOTE: Copies of this specification may be obtained from the Office, Chief of Ordnance, War Department, Washington, D. C. 1 Proof Read 3: /mj p Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-
