DLA MIL-DTL-12468 E-2009 DECONTAMINATING AGENT STB.pdf

1、Comments, suggestions, or questions on this document should be addressed to Defense Supply Center Richmond (DSCR), ATTN: DSCR-VEB, 8000 Jefferson Davis Highway, Richmond, VA 23297-5610 or e-mailed to STDZNMGTDLA.MIL . Since contact information can change, you maty want to verify the currency of this

2、 address information using the ASSIST Online database at http:/assist.daps.dla.mil. AMSC N/A FSC 6850 METRIC MIL-DTL-12468E 30 June 2009 SUPERSEDING MIL-DTL-12468D 12 August 1998 DETAIL SPECIFICATION DECONTAMINATING AGENT, STB This specification is approved for use by all Departments and Agencies of

3、 the Department of Defense. 1. SCOPE. This specification covers one type of decontaminating agent called Super Topical Bleach (STB) for military use. 2. APPLICABLE DOCUMENTS 2.1 General. The documents listed in this section are specified in sections 3, 4 or 5 of this specification. This section does

4、 not include documents cited in other sections of this specification or recommended for additional information or as examples. While every effort has been made to ensure the completeness of this list, document users are cautioned that they must meet all specified requirements of documents cited in s

5、ections 3, 4, or 5 of this specification, whether or not they are listed. 2.2 Non-Government publications. The following documents form a part of this document to the extent specified herein. Unless otherwise specified, the issues of these documents are those listed cited in the solicitation or cont

6、ract. ASTM INTERNATIONAL (American Society for Testing and Materials) ASTM D1193 - Standard Specification for Reagent Water ASTM E11 - Standard Specification for Wire Cloth or Sieves for Testing Purposes (Copies of these documents are available from http:/www.astm.org or ASTM International, 100 Barr

7、 Harbor Drive, West Conshohocken, PA 19428-2959.) Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-12468E 2 2.3 Order of precedence. Unless otherwise noted herein or in the contract, in the event of a conflict between the text of this document

8、 and the references cited herein, the text of this document takes precedence. Nothing in this document, however, supersedes applicable laws and regulations unless a specific exemption has been obtained. 3. REQUIREMENTS 3.1 Material. The decontaminating agent STB shall be an intimate mixture of calci

9、um oxide and bleaching powder (chlorinated lime). The bleaching powder shall have a maximum moisture content of 1.0 percent by weight. Calcium hypochlorite (high test hypochlorite or HTH) shall not be used as a substitute for bleaching powder in the manufacture of the decontaminating agent STB (see

10、6.4.2 and 6.5). 3.2 Physical and chemical characteristics. The decontaminating agent STB shall conform to the physical and chemical characteristics of table I when tested as specified therein. Table I. Physical and chemical characteristics. 3.3 Bulk density. The decontaminating agent STB shall have

11、a minimum bulk density of 0.8 gram (g) per milliliter (ml) when tested as specified in 4.4.2.5. 3.4 Setting characteristics. The decontaminating agent STB shall not set when tested as specified in 4.4.2.6 (see 6.4.3). 4. VERIFICATION 4.1 Classification of inspections. The inspection requirements spe

12、cified herein are classified as a conformance inspection (see 4.3). Characteristics Percentage by Weight Test Minimum Maximum Paragraph Available chlorine 28.0 - 4.4.2.1 Water - 1.0 4.4.2.2 Loss of available chlorine - 4.0 4.4.2.2 Calcium oxide 3.0 6.6 4.4.2.2 Iron (as ferric oxide) - 0.2 4.4.2.3 Pa

13、rticle size: Through 1.40 mm (No. 14) sieve 98.0 - 4.4.2.4 Through 600 um (No. 30) sieve 60.0 - 4.4.2.4 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-12468E 3 4.2 Inspection conditions. Unless otherwise specified, all inspections shall be p

14、erformed on a lot. A lot shall consist of the decontaminating agent STB produced by one manufacturer in no more than 24 hours, 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 a batch proc

15、ess, each batch shall constitute a lot (see 6.4.1). 4.3 Conformance inspection. Conformance inspection shall be performed in accordance with inspection provisions set forth herein. The characteristics shown in table I, when tested in accordance with 4.4, shall constitute minimum inspections to be pe

16、rformed by the supplier prior to Government acceptance or rejection by lot. Sampling shall be conducted in accordance with table II. The inspection set forth in this specification shall become a part of the contractors overall inspection system or quality program. The absence of any inspection requi

17、rements in the specification shall not relieve the contractor of the responsibility of assuring that all products or supplies, submitted to the Government for acceptance, comply with all requirements of the contract. Failure of any test, by any sample, shall be cause for rejection of the lot represe

18、nted. Table II. Sampling. Number in a Batch or Lot Number of Samples 2 to 25 2 26 to 150 3 151 to 1,200 5 1,201 to 7,000 8 7,001 to 20,000 10 20,001 to 35,000 15 over 35,000 20 4.4 Test methods and procedures. 4.4.1 Test specimen preparation. See 6.7 for sampling and testing precautions. A represent

19、ative specimen of approximately 0.45 kg shall be removed from each sample container and placed in a suitable, clean, dry container labeled to identify the lot or batch and the container from which it was taken. Each sample specimen taken shall be tested as specified in 4.4.2. 4.4.2 Tests. See 6.7 fo

20、r sampling and testing precautions. Water in accordance with ASTM D 1193 and reagent grade chemicals shall be used throughout the tests. Where applicable, blank determinations shall be run and corrections applied where significant. Tests shall be conducted in accordance with paragraphs 4.4.2.1 thru

21、4.4.2.6. 4.4.2.1 Available chlorine. Place an approximate 5 g specimen in a porcelain mortar and grind with a pestle to obtain a uniform powder. Weigh out approximately 0.25 g of the uniform powder to the nearest milligram into a 250 ml Erlenmeyer flask. First add 25 ml of potassium iodide (KI) solu

22、tion (made by dissolving 50 g of KI in 1 liter of water) and then add 10 ml of Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-12468E 4 glacial acetic acid to the flask. Swirl until all solids have dissolved. Titrate the resulting solution wi

23、th 0.1 N sodium thiosulfate solution until the solution color is light yellow. Then add approximately 2 ml of starch solution and complete the titration with 0.1 N sodium thiosulfate solution until the solution reaches the clear, colorless endpoint. Calculate the percent by weight available chlorine

24、 as follows: Percent available chlorine = 3.5453A W where: A = Total milliliters of sodium thiosulfate solution added to starch endpoint times the normality of the solution, and W = Weight of the specimen added to the flask in grams. 4.4.2.2 Sequential determination of water, loss of available chlor

25、ine, and calcium oxide. Weigh, to the nearest milligram, approximately 10 g of specimen into a 50 ml, low-form, preweighed weighing bottle with cover. Record the initial specimen weight (A). Place weighing bottle with cover removed in an oven at 100C for 2 hours. Always replace the cover before remo

26、ving the weighing bottle from the oven and allow to cool in a desiccator containing “Drierite” before each weighing. After cooling, weigh again and record the specimen weight after drying for 2 hours at 100C (B). Remove 0.25 g of specimen and weigh to the nearest milligram (C) and place it in a 250

27、ml Erlenmeyer flask. Determine the available chlorine (Y) by the procedure specified in 4.4.2.1. Place weighing bottle containing (B-C) g of specimen in an oven at 100C again, then raise the temperature of the oven slowly to 270 5C and hold at that temperature for at least 1 hour. Cool in a covered

28、desiccator and weigh. Continue heating at 270 5C to constant weight and record the weight (D). Add 10 ml of freshly boiled distilled water to the specimen in the 50 ml weighing bottle and stir for at least 15 minutes with a glass rod fitted with a rubber policeman. (Inconsistent results will be obta

29、ined if the slurry is not thoroughly stirred and care is not taken to scrape the policeman clean on the weighing bottle and to rinse the rubber policeman with a small amount of water into the weighing bottle.) Evaporate the slurry to dryness in an oven set at 80C. Transfer the bottle containing the

30、dry slurry to a 270 5C oven and place on an insulating sheet in the oven to prevent the bottle from cracking. Dry to a constant weight and record the weight (E). Calculate the percent by weight water as follows: Percent water = 100(A - B - Z) A Calculate the percent by weight loss of available chlor

31、ine as follows: Percent loss of available chlorine = 100(X - Y) X Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-12468E 5 Calculate the percent by weight calcium oxide as follows: Percent calcium oxide = 311.1(E - D) B - C where: A = Weight

32、of original specimen in grams, B = Weight of specimen after drying at 100C in grams, C = Weight of 0.25 g of specimen removed for available chlorine analysis in grams, D = Weight of dried specimen before slurring in grams, E = Weight of dried specimen after slurring in grams, X = Percent available c

33、hlorine determined on as-received specimen, Y = Percent available chlorine after heating at 100C, and Z = A(X - Y). 4.4.2.3 Iron (as ferric oxide). 4.4.2.3.1 Indicator solution. Dissolve 0.32 g of barium diphenylamine sulfonate in 100 ml of water. Add 0.5 g of sodium sulfate, mix, and allow the bari

34、um to settle. Decant and use the clear solution as the indicator solution. 4.4.2.3.2 Stannous chloride solution. Dissolve 60 g of stannous chloride in 60 ml of concentrated hydrochloric acid and dilute to 1 liter with water. 4.4.2.3.3 Procedure. Weigh to the nearest 0.01 g approximately 20 g of spec

35、imen into a 600 ml beaker. Cautiously add 50 ml of concentrated hydrochloric acid until effervescence ceases. Dilute to 250 ml with water and add 5 ml of concentrated nitric acid. Boil 2 to 3 minutes. Precipitate the iron with concentrated ammonium hydroxide while the solution is still hot. If only

36、a white precipitate of aluminum hydroxide is obtained, the ferric oxide present is negligible (less than 0.01 percent). If a reddish-brown precipitate is obtained, filter through filter paper and wash the precipitate three times with hot water. Dissolve the precipitate in hot 1 to 4 hydrochloric aci

37、d and wash the filter paper three times with solution prepared in 4.4.2.3.2; then add five drops in excess and allow to cool. Add 25 ml of a saturated solution of mercuric chloride and 15 ml of a phosphoric-sulfuric acid mixture (150 ml concentrated sulfuric acid and 150 ml concentrated phosphoric a

38、cid per liter). Add five drops of the indicator solution prepared in 4.4.2.3.1 and titrate with 0.025 N potassium dichromate solution to a purple end point. Calculate the percent by weight of iron, as ferric oxide, as follows: Percent iron = 7.984AB W where: A = Milliliters of potassium dichromate u

39、sed in the titration, B = Normality of the potassium dichromate solution, and W = Weight of specimen in grams. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-12468E 6 4.4.2.4 Particle size. Use sieves conforming to ASTM E 11. Nest a 1.40 mm

40、(No. 14) sieve in a 600 m (No. 30) sieve and place a receiving pan at the bottom. Weigh 200 5 g of the specimen into the top sieve, cover, and assemble in a mechanical shaker geared to produce 300 15 gyrations and 150 10 taps of the striker per minute. Vibrate the sieves for 5 minutes with the tappe

41、r in operation. Brush any residue remaining on the sieves with a camels-hair brush until no appreciable quantity of material passes the sieves. Weigh and calculate the percentage of specimen passing through each sieve. 4.4.2.5 Bulk density. Weigh approximately 40.0 g of the specimen, which has previ

42、ously passed through a 1.40 mm (No. 14) sieve, into a 100 ml graduated cylinder from which the lip has been removed. Stopper the graduate and pass a closely fitting glass sleeve, approximately 76 mm long, over it. Clamp the sleeve to a ring stand. Place a large rubber stopper under the cylinder and

43、adjust the sleeve so that the graduate will be 100 mm above the rubber stopper when the base of the graduate touches the lower edge of the sleeve. Raise the graduate until it touches the sleeve, then release. Continue raising and dropping the graduate until 100 cycles are completed. Read the volume

44、of the sample and calculate the bulk density in grams per milliliter. 4.4.2.6 Setting characteristics. Place a solution of 0.25 g of citric acid in 75 ml of water in a 250 ml beaker, add 50 g of the specimen with constant stirring during a period of 2 minutes, then stir the mixture constantly for 5

45、minutes to break up lumps and to insure as uniform a slurry as possible. Place a suitable thermometer in the mixture and place the beaker in an ice-water bath. Stir occasionally until the temperature of the slurry falls to 4C or less. Hold the slurry below 4C with occasional stirring for 15 minutes.

46、 The specimen shall be considered as failing the test if the slurry sets during any phase of the test (see 6.4.3). 5. PACKAGING 5.1 Packaging. For acquisition purposes, the packaging requirements shall be as specified in the contract or order (see 6.2). When packaging of materiel is to be performed

47、by DoD or in-house contractor personnel, these personnel need to contact the responsible packaging activity to ascertain packaging requirements. Packaging requirements are maintained by the Inventory Control Points packaging activities within the Military Services or Defense Agency, or within the mi

48、litary services system commands. Packaging data retrieval is available from the managing Military Departments or Defense Agencys automated packaging files, CD-ROM products, or by contacting the responsible packaging activity. 6. NOTES (This section contains information of a general or explanatory nature that may be helpful, but is not mandatory.) 6.1 Intended use. The decontaminating agent STB is military unique. It is intended to be used as a decontaminating agent in chemical and biological warfare for the military. It is used in destroying or converting certain chemical and bio