NAVY MIL-S-487 B-1967 SULFUR GROUND (FOR USE IN AMMUNITION)《硫磺(用于火药中)》.pdf

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1、. .* .- MIL-8-487B 28 June 1967 Superseding 20 October 1965 MIL-8-00487A (MU) JAN-5-487 7 August 1947 MIL ITA R Y SPECIFICATION SULFUR, GROUND (FOR USE IN AMMUNITION) This specification is mandatory for use by ail Departments and Agencies of the Department of Defense. 1. SCOPE 1.1 This specification

2、 covers the requirements for ground sulfur. (see 6.1). 1.2 Classification - The sulfur shall be of the following grades, as specified (see 6.2 and Table I) Grade A - Ground crude Grade B - Ground crude Grade C - Ground crude Grade D - Ground refined Grade E - Ground crude 2. APPLICABLE DOCUMENTS 2.1

3、 The following documents, of the issue in effect on date of invi- tation for bids, or request for proposal, form a part of this specification to the extent specified herein. SPECIFiCA TIONE Federal UU-S-48 Sacks, Shipping, Paper STANDARDS Military MLLSTD-105 Sampling Procedures and Tables for Inspec

4、tion by Attributes Markng for Shipment and Storage MILSTD-129 THIS DOCUMENT CONTAINS cool in a desiccator and reweigh. Calcillate the gain in weight as percent insoluble matter, Calculate percent sulfur as follows: Percent sulfur = 100.00 - (A+B) where: A = Percent insoluble matter and B = Percent m

5、oisture (see 4.5.2) *4.5.2 Moisture - Place about 50 grams of sulfur into a tared dry weighting bottle (75 millimeter (mm) diameter by 30 mm high). Record the weight of bottle and sample and place, with lid removed, in an oven maintained at 80 t: 1C (176 st 2F) for 16 to 24 hours. Remove from the ov

6、en, replace the lid on the bottle, cool in a desiccator and re-weigh. Calculate the loss in weight as percent moisture. 4.5.3 Acidity - Fit the base of the chromatographic tube (see figure i), equipped with a ground glass jqint, into a 500-ml suction flask. Cover the per- forations of the base with

7、a plug of absorbant cotton to provide a support for the column of sulfur. Apply suction and add 100 g of the sample. Tamp smooth with a rubber stopper which just fits inside the tube. Apply suction and pass two 100- ml and three 50-ml portions of freshly boiled (see 4.5) water through the column of

8、sulfur. Allow each portion to drain through the column before adding the succeed- ing portion. Combine the effluents and titrate with 0.1N sodium hydroxide to a methyl red end point. (Retain the titrated solution for the chloride determination, 4.5.5). Make a blank run using the same procedure, with

9、out the sample. Calculate as follows: 4.904 (A-B) N W Percent acidity, as sulfuric acid = 6 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-S-4 87B Ash - Ignite a porcelain or platinum crucible for 5 minutes at - q4.5.4 900 to 1000C in an electri

10、c muffle furnace. Transfer the crucible to a desiccator and allow to cool. After weighing the crucible, add a 20 to 25 g sample to the crucible and reweigh. Heat the crucible and sample under a hood until the vapors continue to burn after the flame is withdrawn. Allow spontaneous burning until the s

11、ample is comumed. Then place the crucible in the 900 to 1000C muffle furnace for 30 minutes. Remove from the furnace, cool in a desiccator and weigh to the nearest 0.0001 gram. Calculate as follows: A-B (100) W Percent ash = where: A = weight of crucible plus ash, in grams. B = weight of crucible, i

12、n grams. W = weight of sample, in grams. 4.5.5 Chlorides - Filter the titrated slution retained from 4.5.3 into a 600 ml beaker. Add 10 ml of concentrated nitric acid and a few crystals of ammonium persulfate. Boil the solution for 5 minutes, cool to room temperature and dilute to 400 ml. To a 40 ml

13、 aliquot of this solution in a 6 inch test tube, add 10 drops of a 10 percent silver nitrate solution and mix. Observe the turbidity and compare to that formed when 40 mi of distilled water, 1 ml of concentrated nitcic acid, 10 drops of 10 percent silver nitrate and 0.5 ml of a standard Na C1 - dist

14、illed water solution (containing 0.0010 gram of Na C1 per mi) are also mixed in a 6 inch test tube. If the turbidity of the sample is less than that of the stanard, report chloride content as less than 0.005 percent. If the turbidity of the sample is greater than the standard, proceed as follows: Co

15、mbine the sample turbidity solution with the original sample solution. Add 10 ml of 10-percent silver nitrate solution and heat to boiling. Remove the solution from the source of heat and allow the precipitated silver chloride to settle for a minimum of 2 hours. Quantitatively transfer the precipita

16、te to a tared filtering crucible and wash the precipitate with 1-percent nitric acid. Dry at 130“ &2“C for one hour, cool in a desiccator, and weigh. Calculate chloride content as follows: 40.78 (A-B) W Percent chlorides, as sodi& chloride = where: A = Weight of crucible and precipitate, in grams. B

17、 = Tare weight of crucible, in grams. W = Weight of sample, in grams (equal to the sample weight for acidity test, 4.5.3) Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-S-487B 4.5.6 Sulfates - Repeat the preparkion of the hot water extract of a

18、fresh 100 gram sample of sulfur as described in 4.5.3. Transfer the 350 ml hot water extract to a 600 mi beaker, add 5 ml of concentrated hydrochloric acid and heat to a rolling boil. While boiling, add dropwise 10 ml of 5 percent barium chloride solution. After precipitation of the barium sulfate,

19、place the 600 ml beaker on a steam bath for 2 hours. Filter the solution through a tared filtering crucible, quantitatively transferring the barium sulfate precipitate to the crucible with a stream of hot distilled water. Then wash the sides of the filtering crucible and the precipitate five times w

20、ith hot distilled water. After drying the crucible and precipi- tate in an oven at 105C to 110C ignite at a cherry red heat for 15 minutes. Cool in a desiccator and weigh. Calculate sulfate content as follows: 60.86 (A-B) W Percent sulfate, as sodium sulfate = where: A = Weight of crucible and preci

21、pitate, in grams. B = Tare weight of crucible, in grams. W= Weight of sample, in grams 4.5.7 Particle Size - Particle size shall be determined in accordance with ASTM Test Method B 214-63T. Two metal washers weighing not more than 15 grams shall be added to a 100 gram portion of the sample in the to

22、p sieve to help break up lumps. *4.5.8 Ammonia and Ammonium Salts - Weigh out approximately 20 grams of sulfur and place in a beaker with 100 f 0.1 ml of reagent grade ammonia free water. The water ehali be prepared and tested in accordance with ASTM D 1426. The water shall be at laboratory room tem

23、perature. Thoroughly mix the sulfur with the water by stirring 5 to 10 minutes. Filter the mixture and then thoroughly rinse the beaker and the filter with three 10 ml portions of reagent grade ammonia free water. Test the effluent for the presence of ammonia or ammonium salts by the Direct Nessleri

24、zation Method of ASTM D 1426. 5. PREPARATION FOR DELIVERY *5.1 Packaging(Bottles only) - 5.1.1 Level A - The sulfur, filled into on- or five pound bottles con- forming to Type I, Class 1 of PPP-C-301, shall be packaged in intermediate containers as specified in PPP-C-301. 8 Provided by IHSNot for Re

25、saleNo reproduction or networking permitted without license from IHS-,-,-b I a-32cm -Chromatographic tube Sulfur rCotton -Perforated base -Ground glass jal Figure i. CHROMATOGRAPHIC ASSEMBLY Suction r- 500 ml filter flask mL-S-487B Provided by IHSNot for ResaleNo reproduction or networking permitted

26、 without license from IHS-,-,-MIL-S-4878 b = 7777706 0333747 O =, MIL-S-487B 5.1.2 Level C - The sulfur shall be packaged in uniform quantities in accordance with the manufacturers commercial practice. Unit and intermediate containers shall be of uniform size, shape and material. intermediate contai

27、ners shall contain only one grade of sulfur. *5.2 Packing - 5.2.1 Level A - 5.2.1.i Bottles - The sulfur, packaged 88 specified in 5.1.l, shall be packed in accordance with PPP-C-301, Level A. 5.2.1.2 - Bulk - Fifty pounds of sulfur shall be packed.in a shipping sack in accordance with construction

28、4x of UUS-48, type of closure optional. The moisture proof barrier paper shall be polyethylene coated and conform to Type E of UUS-48 with a basis weight of 1/15 PE-50. Valve sack closures, when supplied, shall be constructed with moisture proof tuck-in-sleeves, except that the sleeves shall be Poly

29、ethylene coated in accordance with Type E of UUS-48, basis weight 1/15 PE-50. After ffliing, the sleeves shall be heat sealed or closed by tape by the procedure npecified in UUS-48. In addition, both ends of the sack shall be completely sealed by either heat sealing prior to the closing procedures s

30、pecified in UUS48, or by dipping the closed ends as specified in UUS-48. 5.22 Level C (Bottles and bulk) - The sulfur shall be packed to insure carrier acceptance and safe delivery at destination in containers complying with the rules and regulations applicable to the mode of transportation. *53 Mar

31、king - in addition to any marking required by the contract or order, all containers shall be marked in accordance with MILSTD-129. 5.3.1 Additional Marking - Unit conwinern shall be marked with the following: (a) lot number (b) Precautionary instructions to cover hazards that may be encountered duri

32、ng storage or use of the sulfur. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-S-LiA78 68 W 9979906 OLL3750 7 W MIL-S-487B 6. NOTES 6.1 for use as follows: intended Use - Sulfur covered by this specification is intended Grade A- For black powde

33、r Grade B-For pyrotechnic composition Grade C-For pyrotechnic composition Grade D-For nongaseous powder and primer compositions Grade E-For pyrotechnic composition. 6.2 Ordering Data - Procurement documents should specify the following : (a) Title, number and date of this specification (b) Grade req

34、uired (see Table I) and quantity. (c) Levels of packaging and packing required (see 5.1 and 5.2). (d) Additional data, if required (see 3.1) 6.3 Manufacture - 6.3.1 Grade D sulfur is a special high purity grade of refined flour sulfur intended for use in explosive compositions which are sensitive to

35、 small quantities of moisture, acids, and electrolytes. Small lots of this grade have been made by washing refined flour sulfur with water and drying at 70C. The refined sulfur known as ttflowers of sulfurtf containing up to 1.0 percent acidity and up to 30 percent amorphous sulfur is not a suitable

36、 raw material for manufacture of grade D sulfur. 6.3.2 Lumping or caking of grade C sulfur (finest particle size) may be expected inasmuch as the requirements of this specification are intended to prevent the addition of conditioning agents, either organic or inorganic. 6.4 Safety precautions - Sulf

37、ur dust or vapors are flammable and can explode when mixed with air and exposed to heat or flame. The lower limit of flammability in air is 30 milligrams per liter. Adequate ventilation should be pro- vided to keep the concentration of sulfur in air below this limit. Sulfur is not con- sidered toxic

38、, but many of its compounds are poisonous. Contact with sulfur can result in conjunctivitis and irritation to sensitive skins. Personnel who are sensitive to sulfur whould wear protective clothing to avoid skin contact and chemical safety goggles for eye protection and a respirator to avoid excessiv

39、e inhalation. .$- - 11 .* T/r . .I Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-S-Li7B b W 777770b 0333753 7 MIL-S-487B Personnel who must fight fires of sulfur should be protected from the very toxic sulfur dioxide fumes. Water is the best ex

40、tinguisher but small fires may also be controlled by smothering with sand or even with more sulfur. Since sulfur dust should not be scattered when fighting a fire, the use of a water spray is preferable to a solid stream or pressure hose. 6.4.1 Storage - Store sulfur in a cool, ventilated area away

41、from heat, open flame, acute fire hazards and powerful oxidizing agents. Under these ideal conditions, the shelf life of sulfur is indefinite. 6.5 Marginal Notations - The outside margins of this specification have been marked to indicate where changes (deletions, additions, etc) from the previous i

42、ssue have been made. This has been done as a convenience only and the Government assumes no liability whatsoever for any inaccuracies in these notations. Bidders and contractors are cautioned to evaluate the requirements of this document based on the entire content as written irrespective of the mar

43、ginal notations and relationship to the previous issue+ % Preparing A citivity a Custodians: Army - MU Navy - AS Air Force - 68 Navy - AS Review activities : Army - MU, Mi Navy - AS, OS Air Force - 68 DoD Project No. 6810-0431 * U. S. GOVERNMENT PRINTING OFFICE-1867: 301-5092364 12 - Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-