ARMY MIL-H-235 C-1984 HEXACHLOROETHANE TECHNICAL《六氯乙烷 技术》.pdf

1、MIL-H-235C 68 = 7979706 0113570 3 . i MILITARY SPECIFICATION MIL-H-235C 23 February 1984 SUPERSEDING MIL-H-235B 6 September 1977 HEXACHLOROETHANE, TECHNICAL This specification is approved for use by all Departments and Agencies of the Department of Defense. 1. SCOPE 1.1 Scope. This specification cov

2、ers technical grade hexachloroethane. 2. APPLICARLE DOCUMENTS 2.1 Government documents. 2.1.1 Specifications, standards, and handbooks. Unless otherwise specified, the following specifications, standards, and handbooks of the issue listed in that issue of the Department of Defense Index of Specifica

3、tions and Standards (DoDISS) specified in the solicitation form a part of this specification to the extent specified herein. SPECLPICATIONS FEDERAL NN-P-7 1 - Pallets, Material Handling, Wood, Stringer Construction, UU-S-48 - Sacks, Shipping, Paper PPP-D-705 - Drum, Shipping and Storage: Steel, 16 a

4、nd 30 Gallon 2-Way and 4-Way (Partial) Capacity MLL-B-117 - Bags, Sleeves and Tubing - Interior Packaging - : Benef mal comments (recommendations, additions, deletions) and any perti- : : nent data which may be of use in improving this document should be addressed: : to: Commander, Armament Research

5、 and Development Center, US Army Armament, : : Munitions and Chemical Command, ATTN: DRSMC-TSC-S(A), Aberdeen Proving : Ground, LID 21010 by using the sel-addressed Standardization Document : Improvement Proposal (DD Form 1426) appearing at the end of this document : : or by letter. - - FSC 6810 THI

6、S DOCUMENT CONTAINS -.io-. PAGES “ Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-H-235C STANDARDS MIL I TARY MIL-STD-105 - Sampling Procedures and Tables for Iiispection by Attributes MIL-STD-129 - Marking or Shipment and Storage MIL-STD-147 -

7、Palletized Unit Loads MIL-STD-1168 - Ammunition Lot Numbering 2.1.2 Other Government documents, drawings, and publications. The following other Government documents, drawings, and publications form a part o this spec- ification to the extent specified herein. CODE OF FEDERAL, REGULATIONS (CFR) 49 CF

8、R 171 to 179 - Department of Transportation Hazardous Materials Regulations (The Code of Federal Regulations is available from the Superintendent o Docu- ments, US Government Printing Office, Washington, DC 20402. Orders for the above publications should cite “49 CFR 171 to 179.“) (Copies of specifi

9、cations, standards, handbooks, drawings, and publications required by manufacturers in connection with specific acquisition functions should be obtained from the contracting activity or as directed by the contract- ing officer. ) 2.2 Other publications. The following documents form a part of this sp

10、eci- fication to the extent specified herein. The issues of the documents which are indicated as DoD adopted shall be the issue listed in the current DoDISS and the supplement thereto, if applciable, UNIFORM FRl3IGHT CLASSIFICATION RULES (Application for copies should be addressed to the Uniform Cla

11、ssiEication Committee, Room 1106, 222 South Riverside Plaza, Chicago, IL 60606.) ASTM STANDAKDS D1193 - Reagent Water D2989 Ell - Wire-Cloth Sieves For Testing Purposes E203 - Water Using Karl Fischer Reagent E256 E324 - Acidity - Alkalinity of Halogenated Organic Solvents and Their Admixtures - Chl

12、orine in Organic Compounds by Sodium Peroxide Bomb Ignition - Relative Initial and Final Melting Points and the Melting Range of Organic Chemicals 2 P Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-H-235C 68 W 7799706 0333572 7 W MIL-H-235C o -%

13、- e O (Application for copies should be addressed to ASTM, 1916 Race Street, Philadelphia, PA 19103.) (Industry association specifications and standards are generally available for reference from libraries. They are also distributed among technical groups and using Federal agencies.) 2.3 Order of pr

14、ecedence. In the event of a conflict between the text of this specification and the references cited herein, the text of this speciica- tion shall take precedence. 3. REQUIREMENTS 3.1 Physical and chemical characteristics. The hexachloroethane shall conform to the physical and chemical characteristi

15、cs of table I when testet specified therein. I as TABLE I. Physical and chemical characteristics : idelting point, OC : 183.0 : 187.0 : 4.2.4.1 : : Assay (as hexachloroethane), percent : : by weight1 : 98.00 : : 4.2-4.2 : : Acidity (as HCl), percent by weight : - : 0.04 : 4.2.4.3 : : Iron, percent b

16、y weight . - : 0.07 : 4.2.4.4 : : Water content, percent by weight * - : 0.05 : 4.2.4.5 : : Ammonium chloride, percent by weight2 : - : 0.02 : 4.2.4.6 : lCalculated from the total chlorine after making deductions for the chlorine in the hydrochloric acid. 2This requirement does not apply when the ma

17、terial is to be used in smoke mixtures containing ammonium chloride as one of the ingredients, or if the process used in the manufacture of hexachloroethane does not involve the use of ammonia. 3.1.1 Material. The hexachloroethane shall not be adulterated by the addition of any foreign material. qui

18、rement has been met. The contractor shall certify that this re- 3 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,- MIL-H-235C b 737770b 0333573 7 MIL-H-235C 3.2 Particle size. The hexachloroethane shall conform to the particle size characterisitics o

19、f table II when tested as specified in 4.2.4.7. TABLE II. Particle size : Percent by weight passing : * : Minimum : Maximum : Particle size - : 850 micrometers 95 : 300 micrometers 50 : 150 micrometers - : 75 micrometers - - * 30 10 4. QUALIR ASSURANCE PROVISIONS 4.1 Responstbility for inspection. U

20、nless otherwise specified in the con- tract or purchase order, the contractor is responsible for the performance of all inspection requirements as specified herein. Except as otherwise specified in the contract or purchase order, the contractor may use his own or any other facilities suitable for th

21、e performance of the inspection requirements speci- fied herein, unless disapproved by the Government. The Government reserves the r-tght to perform any of the inspections set forth in the specification where such inspections are deemed necessary to assure supplies and services conform to prescribed

22、 requirements. 4.2 Quality conformance inspection. 4.2.1 Lotting. A lot shall consist of the hexachloroethane produced by one manufacturer, at one plant, from the same materials, and under essentially the same manufacturing conditions provided the operation is continuous. In the event the process is

23、 a batch operation, each batch shall constitute a lot (see 6.3). When specified (see 6.2), lot numbering shall be in accordance with MIL-STD-1168. 4.2.2 Sampling. 4.2.2.1 For examination of packaging. Sampling shall be conducted in accord- ance with MIL-S TD- 1 O 5. 4.2.2.2 For test. See 6.5 for sam

24、pling and testing precautions. Sampling shall be conducted in accordance with table III. A representative specimen of approximately 500 grams (g) shail be removed from each sample container and placed in a suitable clean, dry container labeled to identify the lot and con- tainer from which it was ta

25、ken. 4 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-H-235C 68 m 7977706 0333574 O m MIL-H-235C TABLE III. Sampling for test : Number of containers in batch or lot : Number of sample containers : 2 to 25 2 26 to 150 3 151 to 1,200 5. 1,201 to 7

26、,000 8 7,001 to 20,000 10 Over 20,000 20 4.2.3 Inspection procedure. 4.2.3.1 For examination of packaging. The sample unit shall be one filled unit container, ready for shipment. Sample unit containers shall be examined in accordance with the classification of defects and MIL-STD-105. 4.2.3.2 For te

27、st. Each sample specimen taken in 4.2.2.2 shall be tested as specified in 4.2.4. rejection of the lot represented. Failure of any test by any specimen shall be cayse for 4.2.3.3 For critical defects. Each container in the lot shall be inspected ?or the critical defects listed in the classification o

28、f defects. 4.2.3.4 Classification of defects. (a) Packaging (section 5). Categories Defects Critical: 1 Bag liner not heat sealed, tied, or knotted as specified 2 Container closure not secure Major: AQL 1.0 percent defective 101 Container not as specified 102 Bag liner not as specified 103 Quantity

29、per container not as specified 104 Container damaged or leaking 105 Unitization not as specified 106 Marking incorrect, illegible, or missing 4.2.4 Tests. See 6.5 for sampling and testing precautions. Water in accordance with ASTM D1193 and reagent grade chemicals shall be used throughout the tests.

30、 Where applicable, blank determination shall be run and corrections applied where significant. Tests shall be conducted as follows: 5 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-NIL-H-235C 68 m 7779706 Old35%T I MIL-H-235C 4.2.4.1 Melting point.

31、Determine the melting point of the specimen in accordance with ASTM E324, except that the capillary tube shall be completely sealed approximately 15 millimeters from the specimen. 4.2.4.2 Assay. Determine the percent chloride of the specimen in accordance with ASTM EX Calculate the percent by weight

32、 hexachloroethane as foiiows: Percent hexachloroethane = 1.113A - 1.082B where: A = Percent chlorine and B = Percent hydrochloric acid (see 4.2.4.3). 4.2.4.3 Acidity. Determine the acidity of the specimen as percent by weight hydrochloric acid in accordance with ASTM D2989. 4.2.4.4 Iron. - (a) Butan

33、olic potassium thiocyanate solution. Dissolve 10 g of potassium thiocyanate in 10 milliliters (mL) of water. Warm the soutionto 25OC and add n-butanol to make 100 mL. clear. Shake vigorously unti the solution is (b) Ferric ammonium sulfate solution. Dissolve 0.1727 g of ferric ammonium sulfate in 10

34、 mL of 10-percent sulfuric acid and dilute with water to make 2,000 mL. One mL of this solution equals 0.01 milligrarn (mg) of iron. (c) Procedure. Add approximately 8 g of potassium bisulfate or potassium pyrosul- Weigh 7.00 g of the specimen into a large porcelain crucible. fate, cover with a porc

35、elain cover, heat gradually, and fuse until a clear melt is obtained. Cool to room temperature, add 25 to 50 mL of 1 to 4 hydrochloric acid, boil to dissolve the fusion, and filter. Wash two or three times with 1 to 3 hydrochloric acid. Add a few drops of hydrogen peroxide to the filtrate and then a

36、 slight excess of ammonium hydroxide. Boil until the ferric hydro- xide forms flocks, cool to room temperature, filter through a fritted glass filter prepared with diatomaceous silica, and discard the filtrate. Attach the fritted glass filter containing the ferric hydroxide precipitate to a bell jar

37、 filtering apparatus. Add 10 mL of 1 to 1 nitric acid to the Perric hydroxide, filter, and catch the filtrate in a 250-mL beaker. Wash alternately with 1 to 1 nitric acid and hot water, using the minimum amount necessary to remove the ferric nitrate from the filter. 250-mL volumetric flask and dilut

38、e to 250 mL with water. Pipet a 2.5-mL aliquot into a test tube and add water to make a volume of approximately 10 mL. Add approximately 30 mg of ammonium persulfate and 15 mL of butanolic potassium thiocyanate solution prepared as specified in (a). seconds and allow to separate. layer shall be no d

39、arker than that in a blank in which 5 mL of ferric ammonium sulfate solution prepared as specified in (b) is substituted for the 2.5-nL aliquot and tested in the same manner. Transfer the filtrate quantitatively to a Shake well for about 30 Any red color in the clear butanol (upper) 6 e 8 e Provided

40、 by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-NIL-H-235C b m 7779906 OLL3576 MIL-H-235C 4.2.4.5 Water content. accordance with ASTM E203. Determine percent by weight water in the specimen in 4.2.4.6 Ammonium chloride. Weigh to the nearest 0.01 g approximat

41、ely 25 g of the specimen into a 500-mL separatory funnel. Add 100 mL of water and 100 off the bottom water layer,into a 500-mL Kjeldahl flask. Extract the ether layer twice more with 100-mL portions of water and transfer the water layers to the Kjeldahl flask. Discard the ether layers. Add a few dro

42、ps of sulfuric acid to the Kjeldahl flask to make the solution distinctly acid and heat on a steam bath until only a trace of ether remains. Cool the flask to room tempera- ture and then carefully add 25 mL of 50-percent sodium hydroxide solution down the side of the flask in such a manner that a se

43、parate layer is formed on the bottom of the flask. Immediately add to the flask several pieces of broken unglazed porcelain to promote uniform boiling and without agitation, attach the flask to the condenser of a Kjeldahl distillation apparatus. Extend the outlet tube of the condenser beneath the su

44、rface of a solution of 25.00 mL of 0.1N sul- furic acid and 25 mL of water in a 500-mL Erlenmeyer flask. Quickly agitate the contents of the Kjeldahl flask with a swirling motion and distill until approximately 150 mL have been distilled into the Erlenmeyer flask. Discon- tinue the distillation, dis

45、connect the flask, and wash out the condenser with water, adding the washing to the distillate. Titrate the excess sulfuric acid with 0.1N sodium hydroxide solution using 6 drops o sodium alizarine sul- fonate-indigo carmine indicator solution (O. 9 g of sodiun alizarine sulfonate and 0.125 g of ind

46、igo carmine in 100 mL of water). by a change from green to bluish-gray. ammonium chloride as follows: u mL of ether. Shake vigorously until two distinct layers have formed. Drain The end point is indicated Calculate the percent by weight 5.35 (AB - DC) w Percent ammonium chloride = where: A = Millil

47、iters of sulfuric acid used B = Normality o sulfuric acid, C = Milliliters of sodiun hydroxide solution used, D = Normality of sodium hydroxide solution, and TJ = Weight of specimen in grams. 4.2.4.7 Particle size. Place 100 + 1 g of the specimen on a sieve stack arranged from top to bottom as follo

48、ws: micrometers, 75 micrometers, and bottom pan. Sieves shall conform to ASTM Ell. Place the covered sieve stack in a mechanical shaker geared to produce 300t 15 syrations per minute and 150 + 10 taps of the striker per minute. 5 minutes. culate the percent by weight passing through each sieve. 850

49、micrometers, 300 rnicrorneters, 150 Vibrate for Weigh the specimen remaining on the sieves and in the pan and cal- 7 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-H-235C 5. PACKAGING 5,l Unit packing. Unit packing shall be level A, B r C a specified (see 6.2), and shall be in accordance with Department of Transportation (DOT) regu- lations and any other reg