ARMY MIL-C-48038-1972 CALCIUM CHROMATE TECHNICAL《钙铬技术》.pdf

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1、.I I t MIL-C-48038 (MU) 31 May 1972 MILITARY SPECIFICATIOW CALCIUM CHROMATE, TECIMICAL 1. SCOPE 1.1 This specification covers technical grade calcium chromate for use in pyrotechnic ammunition. 2. APPLICABLE DOCUMENTS 2.1 The following documents of the issue in effecr on date of irlvitation for bids

2、 or request for proposal form a part of this specification to the extent specified herein. SPECIFICATIONS FEDERAL RR-S-366 - Sieves, Standard for Testing Purposes . STANDARDS MILITARY MIL-STD-105 - Sampling Procedures and Tables for MIL-STD-109 - Quality Assurance Terms and Definitions MIL-STD-650 -

3、 Explosive: Sampling, Inspection and Testing MIL-STD-1168- Lot Numbering of Amunition MIL-STD-1169- Packaging, Packing and Marking for Shipment of Inert Amunition Components MIL-STD-1233- Procedures for Determining Particle Size, Particle Size Distribution and Packed Density of Powdered Materials MI

4、L-STD-1234- Pyrotechnics: Sampling, Inspection and Testing MIL-STD-1235- Single and Multilevel Continuous Procedures and Tables for Inspection by Attributes (Copies of specifications, standards,. drawings, and publications required by suppliers in connection with specific procurement functions shoul

5、d be obtained from the procuring activity or as directed by the contracting.officer). Inspection by Attributes (ABC-STD-105) II FSC: 810 THIS DOCUMENT CONTAINS 4_ PAGES. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MILiC-Ll038 68 m 0b 0121073 1 MI

6、L-C-40038 -(MU) r O 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 proposal shall apply. AMERICAN SOCIETY FOR TESTING AND MATE!RIALS ASTM

7、-P77 - Atomic Absorption Spectrometry, Rec. Practices for, Proposed ASTM-B212 - Apparent Density.of Metal Powders, Test for (AppZication -for copies should be addressed to the American Society . -for Testing and Materials, 1-916 Hace Street, Philadelphia, Penn. 19103). 3. REQUIREMENTS 3.1 The materi

8、al shall conform to the chemical requirements shown in Table I. TABLE I - CHI!NICAL REQUIREMENTS t fLST 1- HEQIJIRHMENT TEST PARAGRAPH - Calcium chromate, percent, mininum Calcium carbonate, percent, maximum ChloPide (au Ci-), percent, max. Sulfate (as s04), percent, mix. Volatile mat ter, percent,

9、*mx . Aluminun (as Al 031, percent max. Sodium (as Na Of, percent, max. Silicon (as SHI, pereent, max. 96. o .1.5 o. o1 o. o1 0.10 O. 20 O. 15 0.05 4.4.2 4t.4.3 -4.4 b4 4.4.5 4.4.6 4.4.7 4.4.8 4.4.9 3.2 Apparent density.-The technical calcium chromate shall have an apparent density of 0.35 gm/ml, mi

10、n. when tested as specified in 4.4.10. 3 . 3 Particle size.-The particle sise of the technical calcium chromate shall be 2.0 - + 0.5 microns trlieri tested as specified in 4.4.11, 3.4 Granulation.-The technical calciun chromate shall be able to pass, 100 percent, through a 44 micron (Ho. 325) sieve

11、when tested as specified in 4.4.12. 3.5 First article testing.-This specification makes provisions for first article testing. Requirements for the submission of first article samples by the contractor shall be as specified in the contract. c 2 Provided by IHSNot for ResaleNo reproduction or networki

12、ng permitted without license from IHS-,-,-MIL-C-LIO3 68 W 9979906 OLZLOiLI 3 m MIL-C-4 8 03 8 (MU) . 4. QUALITY ASSURANCE PROVICIOMS 4.1 Responsibility for inspection.-Unless otherwise specified in the contract or purchase order, the supplier is responsible for the performance ofall inspection requi

13、renents as specified herein. Except AS otherwise specified in the contract or order, the supplier may use his own or any other facilities suitable for the performance of the inspection requirements specified herein, unless disapproved by the Government. The Government reserves the riqht to perform a

14、ny of the inspections set forth in the specification where such inspections are deemed necessary to assure supplies and services conform to prescribed requirements. MIL-STD-109 to define terns used herein. Reference shall be made to 4.1.1 Submission of product.-At the tire each conpleted lot of item

15、s deliverable under the contract is submitted to the Government for acceptance, the contractor shall supply the following iiiformation acconpanied by a certii icate which attest that the information provided is correct and applicable to the product being submitted: a. A statement that the lot compli

16、es with all of the quality assurance provisions spacif ied in this specification. 1). Specification nunber and date, together with identif i- cation and date of changes thereto. C. Certificates of analysis on all naterials used directly by the contractor when such material is controlled by Governmen

17、t specifications shall be made available upon request by the Contracting Officer . The certificate shall be signeci by a responoihle agent of the certifying organization. substantiated by evidence of the agents aiithority to bind his principal. required with subsequent certif icatan iinlttss, durinq

18、 the course of the contract, this authority is vested in another aqent of the certifying orqanization. d. Quantity of product in the lot. e Date submitted. The initial certificate suhnitted shall be Substantiation of the agents authority will not be 4.2 First article inspection 4.2 . 1 Submission.-P

19、rior to the start of regular production the contractor shall submit a first article scinple (see 6.1) to a Government, approved facility as designated iy the contracting officer for evaluation in accordance with the provisions of 4.2.2. article shall consist of 50 lbs. of calciiirz diroriate in acco

20、rdance The first 3 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-C-48038 (MU) with instructions issued by the Contracting Officer. All samples submitted shall have been produced by the contractor using the same production processes, procedures,

21、 and equipnent as will be used in packing, shall be obtained from the sane sources of supply as will i be used in regular production. The sample shall be accompanied by i certificates of analysis. A first article quantity, or portion thereof, as directed by the Contracting Officer, shall also be sub

22、- mitted whenever there is a lapse in production for a perio in excess of 90 days, or whenever a change occurs in nanufacturing process, material usad, drawing, specification or source of supply as to significantly affect product uniformity as etermined by the Govern- ment. Prior to submission, the

23、contractor shall inspect the sample Co the degree necessary to assure that it conforms to the requirements of the contract and submit a record of this inspection with the sample. A sample containing known defects will not be suhitted unless specifically authorized by the Contracting Officer. 4.2.2 I

24、nspections to be perforned.-The sariple will be subjected by the Government to any or all of the eaninutionc or tests specified in 4.3 and 4.4 of this specification. . fulfilling the contract. All materials, including packaging and 4.2.3 Rejection.-If any sample fails to conply with any of the appli

25、cable requirements, the first article quantity shall be rejected. inspection upon any failure of a sample to conply with any of the stated requirements. The Government reserves the right to terminate its 4.3 Inspection provisions 4.3.1 Tat formation.-A lot shall consist of one or more batches of cal

26、cium chromate produced by one rianufacturer, in accordance with the same specification, or sane specification revision, under one continuous set of operating conditions. Each lot shall consist of that quantity OP calcium chronate that hac been subjected to the same unit chemical or physical rnixinq

27、process intended to make the final product homogeneous. The product shall be submitted for inspection in accordance with EIXJJ-CT1-1O5. The criteria and procedures for the assignment of lot nudiers shall be in accordance with Standard MIL-STD-1168. 4 Provided by IHSNot for ResaleNo reproduction or n

28、etworking permitted without license from IHS-,-,-MIL-C-YBO3B 68 m 9999906 0121076 7 MIL-C-48038 (MU) I 4.3.2 Examination.-Sampling plans and procedures for the MIL-STD-105 (ABC-STD-105), except that inspection for critical defects shall be 100 percent. Contractors sampling plans, if used, shall be a

29、pproved by the Government and shall provide, as a minimum, the protection afforded the Government by the sampling plans in MIL-STD-105. Continuous sampling plans in accordance with MIL-STD-1235 may be used if approved by the procuring activity. Also, at the option of the procuring activity, AQLs and

30、 sampling plans may be applied to the individual characteristics listed, using an AQL of 0.40 percent for each Major defect and an AQL of 0.65 percent for each Minor defect, except where 100 percent inspection is specified. following classifications of defects shall be in accordance with 4.3.2.1 Con

31、tainers, prior to sealing Categories Defects Mzthod of Iilspect on Code No. Critical: None defined. Major: AQL 0.40 percent 101. Liner pierced or tornVisual O1001 Minor : AQL 0.65 percent 201. Marking missing, incorrect o1 002 or illegible . Visual 4.3.3 Sampling.-All sampling of individual containe

32、rs shall be accomplished in such a manner that the sample is representative of the entire contents of the container. Individual or composite samples shall be identified in such a manner as to provide positive identifi- cation as to the container or containers represented by each sample. For the chem

33、ical composition tests, the lot shall be divided up into two (2) parts. From each part, a composite sample shall be prepared in the following manner. A random sample of filled containers shall be selected in accordance with MIL-STD-105. However, if each part comprises less than five (5) containers,

34、all containers shall be selected. Approximately equal portions shall be taken from the selecte containers in such quantities that the aggregate weight of such portions shall be approximately five (5) pounds (lbs.). These portions shall then be thoroughly mixed to form a composite sample. For the phy

35、sical tests, the lot shall be divided up into four (4) parts. For each part, a composite sample shall be prepared in the same manner as described above. shall be approximately ten (10) lbs. If any of the above samples fails to meet.any of the requirements specified in Section 3, the lot shall be rej

36、ected. The aggregate weight of each composite sample 4 5 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-I i MIL-C-46030 (HU) 4.4 Test methods and procedures 4.4.1 Reagents.-The reagents used in testing should conform to the American Chemical Society

37、 (ACS) Specifications as described in “Reagent Chemicals“ . No. 02001.-Jeigh accurately, approximately 2.5 gm of sample. Transfer to a 250 ml volumetric flask, add 20 ml of concentrated hydrochloric aeid, and shake to dissolve. The solution may not be entirely clear, Dilute with water to the mark an

38、d mix well, IJsinq, a 25 ml. volumetric pipette, transfer an aliquot to an iodine flask. Dilute with 100 ml. Of water, add 3 gms. of potassium iodide and allow to stand in the dark for 10 ninutes. Titrate the liberated iodine with IV10 sodium thiosulfate using starch indicator toward the end. Calcul

39、ate the percent of calcium chromate as follows: 4.4.2 Determination of calcium chromate - Major defect - Code 141 of Sodium Thiosulfate X Normality X 0.05203 X 100 Weight of Sample in Aliquot = %calcium Chroniate “A“ 4.4.3 Determination of calcium carbonate - Major defect - Code 4.4.3.1 Reagents 4.4

40、.3.1.1 Ammonium oxalate saturated solution.-Dissolve 50 No. 03001. gmsof ammonium oxalate in 500 ml of hot water, dilute to 1 liter and allow to coal to room temperature. an aliquot of the solution from the preceeding test to a 400 ml. beaker. Dilute with water to a volume of about 75 ml. Heat to bo

41、iling and add slowly 100 ml. of a saturated solution of ammonium oxalate. Add 2 to 3 drops of methyl red indicator solution. Then add ammonium hydroxide dropwise until the solution Just turns yellow, and set on a steam bath until precipitate settles. Filter the precipitate through a Cooch or sintere

42、d glass filter and wash well with cold water (100 - 150 ml.). Transfer the filter plus precipitate to the precipitating beaker and cover with water. the filter thoroughly with a glass rod to loosen the precipitate. Add 3 ml. of concentrated sulfuric acid and heat to 70 - 8OOC. Titrate with N/lo pota

43、ssium permanganate to the first pink endpoint, making sure that the temperature is still at 70 - 80C when the endpoint is reached. Calculate the percent of calcium carbonate as follows: 4.4.3.2 Procedure.-Using a 25 ml, volumetric pipette, transfer Stir M1 of Potassium Permanganate X IJormality X 0.

44、02004 X 100 Weight of Sample in Aliquot = %Calcium “B1 “A“ (from 4.4.2) X .2568 = :6 Calcium, from chromate side = “C“ If “B“ is greater than “B“ - “C“ = Z Calcium due to carbonate = “I)t1 llD1t X 2.5 = XCaCQj the sample contains free Caco3 then: 6 Provided by IHSNot for ResaleNo reproduction or net

45、working permitted without license from IHS-,-,- MIL-C-48038 b = 7qOb 012107B O MIL-C-48038 (MU) 4.4.4 Determination of chloride-Major defect - Code No. 04001.-The chloride determination shall be performed in accordance with Method 401.1 of MIL-STD-1234. 20% (by volume) sulfuric acid. 05001.-The sulf

46、ate determination shall be performed in accordance with Method 411.1 of MIL-STD-650. The leeching solvent shall be 20% (by volume) hydrochloric acid. 4.4.6 Volatile matter - Major defect - Code No. 06001.-Heat a glass-stoppered moisture dish in an oven at 100 to 110OC. for 1 hour, cool in a desiccat

47、or, and weigh to the nearest 0.1 milligram (mg.). Transfer approximately 2 grams (am.) of the specimen to the dry dish, stopper and weigh. Heat unstoppered In an oven at looo to 110OC for 1 hour, cool in a desiccator, replace the stopper, and weigh to the nearest 0.1 mg. Repeat the heating for half-

48、hour periods until successive weighings differ by not more than 0.2 mg. Calculate the loss in weight as percent volatile matter as follows: The leeching solvent shall be 4.4.5 Determination of sulfate - Major defect - Code No. Percent volatile matter = 100 X A - B A-L) Where : A = weight of original

49、 specimen and dish, in gm. B - weight of specimen and dish after drying to constant D = weight of dry moisture dish, in gm, weight in gm. 4.4.7 Determination of aluminum (as Al2O3) - Major defect - Code No. 07001.-Aluminum shall be determined by an atomic absorption method as specified in ASTM-P77. No. 08001.-Sodium shall be determined by an atomic absorption method as specified in ASTM-P77. 4.4.9 Determination of silicon (as Si) - Majo