ARMY MIL-S-20322 B-1973 STRONTIUM NITRATE ANHYDROUS《无水硝酸锶》.pdf

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1、I MIL-S-20322B b II 9999906 OLL7500 i W MIL-S- 20322B 19 April 1973 SUPERSEDING 17 April 1956 MIL-S- 203228 MILITARY SPECIFICATION STRONTIUM NITRATE, ANHYDROUS This specification has been approved by the Department of Defense and is mandatory for use by the Departments of the Army, the Navy, and the

2、 Air Eorce. 1. SCOPE 1.1 Scope. This specification covers anhydrous strontium nitrate for use in pyrotechnic compositions. 1.2 Classification. Strontium nitrate, anhydrous shall be of the following grades, as specified (see 6.1 and 6.2): Grade A Grade B 2. APPLICABLE DOCUMENTS 2.1 The following docu

3、ments of the issue in effew on date of invi- tation for bids orrequest for proposal, form a part of this specifica- tion to the extent specified herein: SPECIF ICATIQN S FEDERAL L-P-378 - Plastic Sheet and Strip, Thin Gauge, Polyolefin RR-S-366 - Sieve, Test FPP-D-723 - Drums, Fiber MILITARY MIL-D-3

4、464. - Desiccants, Activated, Bagged, Packaging Use and MIL-D-6054 - Drums, Metal - Shipping and Storage. Static Dehumidification. FSC 6810 M O Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-a. MIL-S-20322B 68 7799706 0117501 9 W MIL-S-20322B STANDA

5、RDS MILITARY MIL-STD-105 - Sampling Procedures and Tables for Inspection by Attributes MIL-STD-129 - Marking for Shipment and Storage. (Copies of specifications, standards, drawings, and publications re- quired by suppliers in connection with specific procurement functions should be obtained from th

6、e procuring activity or as directed by the contracting officer.) 2.2 Other publications. The following documents form a part of this specification to the extent specified herein. Unless otherwise indicated, the issue in effect on date of invitation for bids or request for pro- posal shall apply. DEP

7、ARTMENT OF TRANSPORTATION 49 CFR 171-179 - Department of Transportation Rules and Regulations for the Transportation of Explosives and Other Dangerous Articles. (The code of Federal Regulations (CFR) and the Federal Register (FR) are for sale on a subscription basis by the Superintendent of Document

8、s, U. S. Government Printing Office, Washington, D. C. 20402. When indicated, reprints of certain regulations may be obtained from the Federal agency responsible for issuance thereof.) AMERICAN SOCIEXY FOR TESTING AND MATERIAL (ASTM) D 1193 - Reagent Water . (Application for copies should be address

9、ed to the American Society for Testing and Materials, 1916 Race Street, Philadelphia, Pennsylvania 19103. Technical society and technical association specifications and standards are generally available for reference from libraries. distributed among technical groups and using Federal agencies. They

10、 are also 3. REQUIREMENTS 3.1 ryuirementn . The strontium nitrate shall conform to the chemical and physical requirements specified in table I. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-S-203228 68 W 7777906 OLL7502 O MIL-S-20322B TABLE I.

11、Chemical and Physical Properties Property Strontium nitrate (including any barium nitrate), %, min. Moisture, %, max. Hygroscopicity, %, max. Acidity (pH) Water-insoluble matter, %, max. Grit, %, max. Chloride (as Ci), %, max. Ammonium compounds (as “31, %, max. Sulfur (total), %, max. Barium, %, ma

12、x. Calcium, %, max. Magnesium, %, max. Sodium, %, max. Iron, %, max. Bismuth, %, max. Lead, %, max. Copper, %, max. Requirement Grade A 99.5 O .O5 O .O5 6 .O-7 .O o .o2 o .o2 O ,003 o .o1 0.01 O .O5 O .O03 O .O03 O. 003 O. 003 O. 003 O .O03 O. 003 Grade B 99.5 0.05 8 .O5 6 -0-7-0 0.02 0.02 O .O03 0.

13、01 0.01 1.5 O. 003 0.003 O. 003 O. 003 O. 003 O .O03 O. 003 Test larag.raph 4.4.1 4.4.2 4.4.3 4.4.4 44.5 4.4.6 4.4.7 4.4.8 4.4.9 4.4.10 4.4.10 4.4.10 4.4.10 4.4.10 4.4.10 4.4.10 4.4.10 3 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-S-20322B 3.

14、2 Granulation 3.2.1 Grade A. The granulation requirement for Grade A strontium nitrate shall be 95 percent through a number (No.) 100 U. S. standard sieve, min., when tested in accordance with 4.4.11. shall conform to RR-S-366. The sieve used 3.2.2 Grade B. The granulation requirements for Grade B s

15、trontium nitrate shall be 99.9 percent through a No. 50 U. S, standard sieve, min, and 70.0 percent retained on a No. 140 sieve, min. The sieves used shall conform to RR-S-366. 3.3 Workmanship. The material shall be free from grit, dirt, foreign matter and other injurious materials. 4, QUALITY ASSUR

16、ANCE PROVISIONS 4.1 Responsibility for inspection. Unless otherwise specified in the contract or purchase order, the supplier is responsible for the performance of all inspection requirements as specified herein. Ex- cept as otherwise specified in the contract or order, the supplier may use his own

17、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 imspections are deemed necessary to assure supplie

18、s and services conform to prescribed requirements. The test procedures specified hereinafter shall be used in determining compliance of the material with the corresponding require- ments specified in section 3. any requirement of the acceptance test shall result in the rejection of the lot represent

19、ed. Failure of a specimen to comply with 4.2 Lotting. A lot shall consist of strontium nitrate produced consecutively on one shift, by one manufacturer, at the same plant, using the same equipment, under essentially the same manufacturing conditions, with no change in raw materials, provided the ope

20、ration is continuous. In the event the process is a batch operation, each batch shall constitute a lot (see 6.3). 4.3 Sampling. Containers shall be randomly selected from each lot in accordance with MIL-STD-105, inspection level S-4, with a minimum sample size of five containers per lot. The content

21、s of each con- tainer shall be thoroughly mixed and approximately 8 ounces of the material removed from each of the selected containers. Each primary sample shall be placed in an air-tight container, labeled so that the container from which it was taken can be easily identified. A com- posite sample

22、 of approximately 16 ounces shall be made from equal O Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-S-203228 b 777770b 0337504 4 W MIL-S- 20322B portions of the primary samples and mixed thorouglly. sample shall be placed in an air-tight conta

23、iner, labeled to show the name of the material, manufacturer, plant, contract or purchase order, batch number, and lot number. All acceptance tests shall be made on specimens selected from the composite sample representative of the lot. However, if it becomes apparent during sampling that the lot is

24、 not- uniform throughout, the inspector may require that any of the primary samples be tested for compliance with the requirements of this speci- fication. The primary samples shall be held for future examination should the composite sample fail to meet the specification requirements. The composite

25、4.4 Tests. Distilled water in accordance with ASTM D 1193 Type III, and reagent grade chemical5 shall be used throughout the tests. determinations shall be run and corrections shall be applied when necessary. Blank 4.4.1 Strontium nitrate. Place 10.0 k0.5 gm. of tungstic oxide into a platinum crucib

26、1.e and ignite at 700“ f50C (1292O +90F) in a furnace for 1 hour. Place the crucible back into the furnace for an additional half hour, cool in a desiccator for 60 +-5 minutes, and weigh again. Repeat the pro- cedure until constant weight is obtained. Allow the furnace to cool to approximately room

27、temperature and adjust the controls to 690C (1274F). Mix a 2 gm. portion of the sample (accurately weighed to 0.1 mg.) with the ignited tungstic oxide and cover the crucible with a tight fitting cover. rom temperature and heat to 690C (1274F). Heat the crucible for 2 hours after the operating temper

28、ature has been reached, cool in a desiccator for 60 Sr5 minutes, and weigh. Reheat for an additional half hour, cool in a desiccator for 60 f5 minutes, and weigh again. Repeat the procedure until constant weight is obtained. Calculate the percent strontium nitrate as follows: Cool in a desiccator fo

29、r 60 25 minutes and weigh. Place the crucible in the furnace at approximately 195.9A W Percent strontium nitrate = where, A = loss in weight, gm. W = weight of sample, gm. 4.4.2 Moisture. Transfer 3 gm. of the sample to a tared weighing dish (approximately 6 cm. in diameter and 2.5 cm. deep) and wei

30、gh. Dry at 130“ f3“C (265“ +5“F) for 3 hours, cool in a desiccator, and weigh. Calculate the percent moisture as follows: a i 100 A Percent moisture = - W 5 o Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-S-20322B b W 79797Ob 0117505 b U MIL-S-

31、 20322B where, A = loss in weight, gm. W = weight of sample, gm. Save the dried samples for the hygroscopicity determination (see 4.4.3). 4.4.3 Hygroscopicity. Place the dried samples from the moisture determination into a desiccator, 10 liter capacity, containing 1 liter of a sulfuric acid solution

32、 (33.1 f0.2% sulfuric acid by weight) for producing 70% relative humidity at 25OC (77OF). Allow the dishes to remain in the desiccator for 48 hours and weigh. into the desiccator for 24 hours and weigh again. intervals until constant weight is obtained. not change significantly after the initial 48

33、hour period. the percent hygroscopicity as follows: Place the dishes back Repeat for 24 hour Usually the weight will Calculate 100 A Percent hygroscopicity = 7 where, A = gain in weight, gm. W = weight of sample, gm. 4.4.4 Acidity (pH). Dissolve 5 gm. of the sample in 100 ml. of Determine the pH of

34、the solution at 25OC (77OF). distilled water. 4.4.5 Water-insoluble matter. Weigh 50 gm. of the sample into a Filter 400 ml. beaker, add about 300 ml. of water, and stir to dissolve. Heat to boiling and boil for 5 minutes with occasional stirring. through a tared sintered glass crucible and wash wit

35、h hot water. the crucible at 105O +3OC (221O +5OF) for 1 hour, cool in a desiccator, and weigh. Dry Calculate the percent water-insoluble matter as follows: 100 A Percent water-insoluble matter = - W where, A = weight of residue, gm. W = weight of sample, gm. 4.4.6 Grit. Weigh 50 gm. of the sample i

36、nto a 400 ml. beaker, add about 300 ml. of water, and stir to dissolve. Heat to boiling and boil for 5 minutes with occasional stirring. Filter through a Whatman No. 40 filter paper and transfer and wash with hot water. Save the filtrate for the determination of chloride (see 4.4.7). Wash the residu

37、e from the filter paper into a 100 ml beaker with a stream of water from a wash bottle. Add 10 ml. of nitric acid to the 100 ml beaker and evaporate to dryness on a steam bath. Add about 10 ml. of water and break up 6 o Provided by IHSNot for ResaleNo reproduction or networking permitted without lic

38、ense from IHS-,-,- MIL-S-20322B 68 79777Ob 0137506 W MIL-S-203 22B any residue with a policeman. Transfer to a No. 170 U. S. standard sieve with water. well with water, alcohol, and finally ethyl ether. Transfer the material to a tared weighing dish and weigh. f 01 lows : If any solid material is re

39、tained by the sieve, wash Calculate the percent grit as 100 A Percent grit = - W where, A = weight of residue, gm. W = weight of sample, gm. 4.4.7 Chloride. Add 5 ml. of nitric acid to the filtrate from the grit determination (see 4.4.6). nitrate solution, and boil for 5 minutes. Allow to stand in a

40、 dark place overnight at room temperature. crucible of fine porosity and wash with water. Dry at 150 +5OC (302O +goF) for 1 hour, cool in a desiccator, and weigh. chloride as follows: Heat to boiling, add 5 ml. of 5% silver Filter through a tared sintered glass Calculate the percent 24.7A Percent ch

41、loride (as Ci) = 7 where, A = weight of percipitate, gm. W = weight of sample, gm. 4.4.8 Ammonium compounds. Weigh 10 gm. of the sample into a 500 ml. Kjeldahl flask and dissolve in 100 ml, of water, Add 10 ml. of 20% sodium hydroxide solution, immediately connect to the Kjeldahl dis- tillation appa

42、ratus, the outlet tube of.which dips below 50 ml, of 3% boric acid solution contained in a 258 ml. Erlenmeyer flask, Distill about 75 ml., wash down the outlet tube, add about 3 drops of methyl purple indicator, and titrate with standard 0.05 N sulfuric acid solution until the color changes from gre

43、en to light purple. Carry a blank deter- mination through the entire procedure. compounds as follows: Calculate the percent ammonium 1.70 (A-BI N W Percent ammonium compounds (as “3) = where, A = sulfuric acid for titration of sample, ml. B = sulfuric acid for titration of blank, ml. W = weight of s

44、ample, gm. N = normality of sulfuric acid 7 o Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-S- 203 22B 4.4.9 Sulfur (total). Weigh 20 gm. of the sample into a 400 ml, beaker, add about 200 ml. of water, and stir to dissolve. Add 2 ml. of hydkoc

45、hloric acid and 10 ml. of-bromine water. boil 10 minutes. with water. Add 10 ml. of 10% barium chloride solution, heat to boiling, and boil 5 minutes. Allow to stand overnight. Filter through a Whatman No. 42 filter paper, transfer, and wash with water. Place the filter paper and precipitate into a

46、tared platinum crucible. Char and burn off the filter paper at dull red heat and then ignite at red heat for 30 minutes, Cool in e desiccator and weigh. Calculate the percent sulfur as follows: Heat to boiling and Filter through a Wnatman No. 40 filter paper and wash 13.7 A Percent sulfur (total) =

47、where, A = weight of precipitate, gm. W = weight of sample, gm. 4.4.10 Barium, calcium, magnesium, sodium, iron, bismuth, lead, and copper. Determine the calcium, barium, magnesium, sodium, iron, bismuth, lezd and copper contents by spectrographic or other instrumental methods approved by the contra

48、cting officer. 4.4.11 Granulation, Dry the material to be sieved by spreading in a thin layer on a large watch glass and heating in an oven at 57 f3OC (1350 +5OF) for 1 hour. Approximately 100 gm. of dried Grade A material shall be transferred to a No, 100 U. S. standard sieve. Approximately 100 gm.

49、 of dried Grade B material shall be transferred to a No. 50 U. S. standard sieve nested over a No, 140 sieve. The sieve or sieve assembly shall be provided with a cover and a bottom pan. The sieves shall conform to RR-S-366. Shake for 10 minates by hand, or for 5 minutes by means of a mechanical shaker geared to produce 300 +15 gyrations and 150 f10 taps of the striker per minute. Weigh the retained portions on each sieve and ca