ARMY MIL-C-13613-1954 CARBAZOLE《咔唑》.pdf

1、d-77-58 MIL-C- 13613 (Ora) 3 September 1954 SUPERSEDING PA-PD-185 (Rev i) 27 April 1954 MILITARY SPECIF I CATI ON CBRBAZOLE 1. SCOPE 1.1 This specification covers carbazole for use in the manufact- ure of tetranitrocarbaeole (TNC). 2. APPLICABLE r)Nmm!m 2.1 The following specifications and standards

2、, and all specifica- tions, and drawings referenced thereon, of the issue in effect on date of invitation for bids, form a part of this specification: SPECIFICATIONS MILITARY MIL-G-2 550 -General Specification For Ammunition Except Small Arms Ammunition. STANDARDS MI LI TAY MIL-STD-129 ,Markhg for S

3、hipment alid Storage. (Copies of specifications, standards, drawings, and publications re- quired by contractors in connection with specific procurement functions should be obtained from the procuring agency or as directed bythe contracting officer.) 3. REQUIREb4ENTS 3.1 Purify.-The purity shall be

4、97.0 percent, minimum, when de- 3.2 Freezing Doint.-The freezing point shall be 244.0OC, minimum, 3.3 Ash content.-The ash content shall be 0.10 percent, maximum, termined -as specified in 4.4. when determined as specified in 4.5. when determined as specified in 4.6. . THIS DOCUFWUT CONTAINS PAGES.

5、o Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,- MIL-C=13613 68 9777906 OLL6472 1 3.4 Moisture content .-The moisture content shall be 0,lO percent 3.5 Color.-The color shall be white to grayish-white, when deter- maximum, when determined as specif

6、ied in 4.7. mined as specified in 4.8. 4.1 Lot.4 lot shall consist of material from batches which have A batch shall be defined as that quantity of material which been manufactured by the same process by one manufacturer. has been subjected to some unit chemical or physical mixing operation which se

7、rves to make the product substantially uniform. rubber stoppered bottle labeled to show the name of the material, manufacturer, plant, contract or order number, lot number, and lot size. All acceptance tests shall be made on this sample. 4*3 Ins ection.-Inspection shall be made inExccordance with Sp

8、eci- . f icat ion _E1_s MIL-G-2 50. 4.4 Determination of Duritg.-An accurately weighed portion of 2.0 3. 0.5 gm of the sample shall be transferred to an 800-ml Kjeladhl digestion flask. Ten gm of powdered potassium sulfate, 0.3 gm of crystallized copper sulfate, and 50 ml of concentrated sulfuric ac

9、id shall be added. Several glass beads shall be added to the flask to avoid bumping. The flask shall be placed in an inclined position and heated belon the boiling point of the acid until frothing ceases. heat shall be increased until the acid boils briskly, and digested for 4 hours. The contents of

10、 the flask shall be cooled to room temp- erature and diluted with 200 ml of.water. 50-percent sodium hydroxide solution (equal weights of sodium hydroxide and water) shall be added slowly. shall be poured down the side of the flask so that it does not mix with the acid solution. The Kjeldahl flask s

11、hall be connected to a condenser by means of a Kjeldahl connecting bulb and the tip of the condenser shall be extended below the surface of a 100-ml solution of kpercent boric acid contained in a 500-d. Erlenmeyer flask. contents of the Kjeldahl flask shall be mixed by shaking. $50 ml of the liquid

12、shall be distilled into the boric acid solution. methyl red indicator. made, and the purity of the carbazole calculated as follows2 4.2 Sam lin .-A sample of approximately 1 pound shall be taken from . one of t e containers in the lot. This sample shall be placed in a The A 100-ml portion of a This

13、sodium hydroxide solution The Approximately his new solution shall be titrated with 0.3N hydrochloric acid, using Correction for a blank determination shall be Purity, percent i 16.72 AN w where: A I ml of hydrochloric acid used in sample titration i? 8 Normality of hydrochloric acid. W minus ml of

14、hydrochloric acid used in blank titration. Weight of the sample on a moisture-free basis. . 4.5 Determination of freezing point.-The equipment (see figure i) shallbe assembled with the Inner test tube, thermometers, and stirrer 2- Provided by IHSNot for ResaleNo reproduction or networking permitted

15、without license from IHS-,-,-MIL-C- 13613 (Ord) withdrawn to allow the carbazole to be placed in the test tube and melted with the aidoof a Bunsen burner. thermometer (with 1 C subdivisions) shall be about 1 cm from and adjacent to the middle of the exposed mercury co.1umn of the ther- mometer immer

16、sed in the sample. in the test tube to cover the standardiped thermometer (calibrated for total immersion and having 0.2OC subdivisions) to at least 3 inches above the bulb. Shortly after the thermometer is adjusted, the carbazole shall be completely melted again, care being taken not to heat the ca

17、rbazole over 26OoC, and the smaller tube shall be in- serted into the larger one. The carbazole shall be.agitated vigorously with the metal stirrer as it cools. lowers, the thermometer shall be read every 1/2 minute until the temperature remains constant, or practically so, and then begins to drop a

18、gain. cause the temperature to drop below the freezing point, and then rise to the freezing point. temperature obtained after the temperature starts to rise shall be taken as the uncorrected freezing point. Should no supercooling occur, the temperature shall be recorded as the uncorrected freezing p

19、oint when it becomes constant, or nearly s, during the freezing of the material. The reading of the correction thermometer shall be recorded, and considered the average temperature of the exposed mercury column. The emerged stem correction shall be calculated as follows: The bulb of the correction S

20、ufficient carbazole shall.be placed As the temperature Occasionally supercooling may occur which will Should supercooling occur, the highest Correction (degrees C) I N(T - t) (0.00016) where: N O Number of degrees in the exposed mercury column. T I Uncorrected freezing point. t = Average temperature

21、 of the exposed mercury column. The corrected freezing point shell be calculated by adding this correction ta the uacorreoted ireeeiqg point. approximately 10 gm of the sample shall be transferred to a tared porcelain or platinum crucible. The crucible and contents shall be ignited by means of a gas

22、 flame or muffle furnace until all combust- ible matter has been removed,.cooled in a desiccator, and weighed. The weight of the residue shall be calculated as percentage of ash. 4.7 Determination of moisture content.-An accurately weighed portion of approximately 5 m of the sample shall be transfer

23、red to a tared moisture dish. !he dish Snd contents shall be placed in an oven maintained at looo to 105 C for 2 hours, cooled in a desiccator, and weighed. shall be calculated to percent moisture in the sample as follows: 4.6 Determination of ash content.An accurately weighed portion of The loss in

24、 weight of the dish and contents Percent moisture I .w 100A 3 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-C- 13613 (ord) where: A 0 Loss in weight of moisture W = Weight of the sample. dish and contents. 4,8 Color.-The color shall be determin

25、ed by visual inspection. 4.9 Retest.-Should a lot fail to pass the specified tests, It shall be rejected, but it may, upon application from the manufact- urer and approval of the contracting officer, be retested once. . 5. PREPARATION FOR DELIVERY 5.1 Packing.-Unless otherwise specified, carbazole s

26、hall be de- livered in standard commercial containers, so constructed as to insure acceptance by common or other carrier for safe transportation, at the lowest rate, to the point of delivery. S.S.Markinq,-In addition to any special marking required by the contract or order, shipments shall be marked

27、 in accordance with Standard MIL-STD-129. 6.- NOTES 6.1 Orderine: data.-Procurement documents should specify the title, number, and date of this specification. Notice.-This specification, together with specifications and draw- ings pertaining to it and bearing a ?Notice? of similar restrictions, is

28、intended for use in connection with procurement by the United States Government; and shall not be reproduced either wholly or in part except when authorized in connection with Government procurement nor be used for any other purpose except when specifically authorized by the Chief of Ordnance, Custo

29、dian: 4 Army-Ordnance Corps o Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-.1;1i CA LARGE PAC I MOUTH T Y & /WITH LOOP END a MIL-C-13613 (ord) CORRECTION THERWMEXR STANDARD THERMOMETER L STIRRING ROD CORK STOP PERS GLASS TEST TUBE DIA X 6“ LONG GIA55 TEST TUBE I IDIA x 7“ LONG & & SOLIDIFICATIN POINT APPARATUS FIGURE. I 5 o Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-