1、P 8 28 November 1978 SUPERSEDING 1c-14264 ( CC ) 28 February 1956 MILITARY SPECIFICATION CALCIUM PHOSPHATE, TRIBASIC, TECHNICAL This specifcation is approved for use by all Departments and Agencies of the Department of Defense. 1. SCOPE 1.1 This specification covers one grade of tribasic calcium pho
2、sphate. 2. APPLICABLE DOCUMENTS 2.1 Government documents. The following documents of the issue in ef- fect on date of invitation for bids or request for proposal, form a part of this specification to the eeent specified herein. STANRARDS . MIbSTei05 - Sampling Procedures and Tables for Inspection by
3、 MILSTD-1188 - Commercial Packaging of Supplies and Equipment. Attributes (Copies of specifications, standards, drawings, and publications re- qufred by suppliers in connection with specific procurement functions should be obtained from the procuring activity or as directed by the contracting office
4、r. ) FSC 6810 : Beneflcial comments (recommendations, additions, deletions) and any : pertinent data which may be of use in improving this document should be : : addressedto: Commander, Us Army Armament Research and Development . : Command, Attn: DRDAR-TSC-C, Aberdeen Proving Ground, MD 21010 by us-
5、 : : ing the self-addressed Standardization Document Improvement Proposal : : (DD Form 1426) appearing at the end of this document or by letter. . Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,- - - MIL-C-L42bLlA 68 W 9999906 0438702 1 %- .I .L MIL-
6、C-14264A 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 MATERIALS (ASTM) STANDARDS A
7、STM Di193 = Reagent Water. ASTM Ell - Wire-Cloth Sieves for Testing Purpose. (Application for copies should be addressed to the American Society for Testing and Materials, 191.6 Race Street, Philadelphia, PA 19103.) (Technical society and technical assoeiation specifications and standards are genera
8、lly available for reference from libraries. tributed among technical groups and using Federal. agencies.) They are also dis- 3. REQUIREMENTS 3.1 Physical-and chemical characteristics, Tribasic calcium phosphate shall conform to table I when tested as specified therein. TABLE I. Physical and chemical
9、 characteristics S e . : Requirement : Test : Characteristic :Minimum:Maximum: parragraph: . . . . : : Loss on ignition, percent by wt. : - : 10.0 : 4.3.1 : : Assay, as P205, percent by wt. : 39.8 : 41.2 : 4.3.2 : . : Granulation, percent by wt: e : 4.3.3 : : Through No. 80 sieve : 99.8 : - : . : Th
10、rough No, 325 sieve. : 97,O : - : e e 4. QUALITY ASSURANCE PROVISIONS 4.1 Responsibility for inspection. Unless otherwise specified in the contract, the contractor is responsible for the performance of all inspec- tion requirements as specified herein. Except as otherwise specified in the contract,
11、the contractor may use his own or any other facilities suitable for the performance of the inspection requirements specified here- in, unless disapproved by the Government. The Government reserves the right to perform any of the inspections set forth in the specification where such inspections are d
12、eemed necessary to assure supplies and ser- vices conform to prescribed requirements. 2 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-h 4.2 Quality conformance inspection. 42.1 Lotting. A lot shall consist of the tribasic calcium phosphate produced
13、 by one manufacturer, at one plant, from the same materials, and under essentially the same manufacturing conditions provided the opera- tion is continuous. In the event the process is a batch operation, each batch shall constitute a lot (see 6.3). 4 . 2 . 2 Sampling. 4.2.2.1 For examination of prep
14、aration for delivery. Sampling for examination of preparation for delivery shall be conducted in accord- ance with bL=Sn=i5, 4,2.2.2 For test. Sampling for test shall be conducted in accord- ance with table II. grams (g) shall be removed for each sample container and placed in a suitable clean, aiiy
15、 container labeled to identify the lot and container from which it was taken, A representative specimen of approximately 450 TABLE II. Sampling for test : Number of containers in batch or lot : Number of sample containers : 2 to 25 2 26 to 150 3 . 151 to U00 5 . . 1201to 7000 a . 7001 to 20000 10 .
16、over 20000 20 - . o . . o . . o . . . o . . 4.2 . 3 Inspection procedure . 4,2.3.1 For examination of preparation for delivery. The sample unit shall be one shipping container filled with tribasic calcium phosphate. Each unit shall be examined for the following defects using an AQL of 4.0 percent de
17、fective. (a) (b) Container incorrect or damaged (c) Closure of container incorrect (d) Contents per shipping container not as specified Marking incorrect, illegible, or incomplete. 3 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-I, mT264A 68 999990
18、6 0438704 5 MIL-C-14264A 4.2.3.2 For test. Each sample specimen taken in 4.2.2.2 shall be tested as specified in 4.3. shall be cause for rejection of the lot represented. Failure of any test by any specimen 4.3 - Tests. Water in accordance with ASTM Di193 and reagent grade chemicals shall be used th
19、roughout the tests. blank determinations shall be run and corrections applied where sign- ificant. Tests shall be conducted as follows: Where applicable, 4.3.1 Loss on ignition. furnace to constant weight. approximately 1.0 g of specimen into the tared crucible. fully over a Bunsen flame to prevent
20、loss of specimen. in a muffle furnace at 800Oc for 30 minutes. in a dessicator and weigh. culate loss on ignition as follows: Ignite a porcelain crucible in a muffle Weigh, to the nearest 0.1 milligram (mg), Heat care-. Then, ignite Cal- Cool to room temperature Save the residue for assay, below. Pe
21、rcent loss on ignition = 100(B=T) A-T where: A = Weight, in grams, of specimen and crucible before ignition, B = Weight, in grams, of specimen and crucible after ignition, and T = Tare weight, in grams, of crucible. - 4.3,2 Assay as P,o5. 4,3.2.1 Preparation of ammonium molybdate solution. Dissolve
22、65.0 g of finely powdered molybdic acid in a mixture of 140 milliliters (mi) of water and 145 ml of 28-percent ammonium hydroxide. Cool and add slowly to a well cooled mixture of 320 ml of 70-percent nitric acid and 400 d of water. Allow to stand 48 hours and filter through an asbestos pad. clear, s
23、upernatant liquid, filtering if necessary. (NOTE. This solu- tion deteriorates on standing. sodium phosphate to 5 ml of the ammonium molybdate solution, an abund- ant yellow precipitate does not form at once or after slight warming, the ammonium molybdate solution should be discarded. Store the solu
24、tion in a cool dark place. Use only the If upon the afldition of 2 ml of 1N 4.3.2.2 Procedure. Dissolve residue from 4.3.2.1, above, in a mix- ture of 100 ml of water and 50 ml of 10-percent nitric acid. necessary, filter the solution and wash the filter with severa3 small poreions of water. metric
25、flask. Pipet a 5O-mi aliquot into a suitable size erlenmeyer flask. slight precipitate and then dissolve the precipitate by the addition If Transfer, with several rinsings, to a 250-ml volu- Add sufficient LO-percent ammonium hydroxide to produce a 4 Provided by IHSNot for ResaleNo reproduction or n
26、etworking permitted without license from IHS-,-,-F i of lail of 10-percent nitric acid. Adjust the temperature to 5OoC, add 75 ml of ammonium molybdate solution (4.3.2.1) and maintain the temperature at 5OoC for 30 minutes, with occasional stirring. precipitate to settle, and decant liquid. ml of wa
27、ter, mix well, and let settle. with a second 30 to 40 ml of water. tate with Lpercent potassium nitrate solution until washing is no longer acid to litmus paper. Transfer the precipitate and ftlter paper to the flask containing the washings. and agitate until the precipitate dissolves. acid to a col
28、orless endpoint, using 3 drops of phenolphthaleFn solution as the indicator. Allow Add approximately 30 to 40 Decant liquid and repeat washing Filter off liquid; wash precipi- Add 40.0 ml of lN sodium hydroxide Titrate wyth 1N sulfuric Calculate the percent phosphorus pentoxide as follows: where: A
29、= Milliliters of sodium hydroxide solution, B = NormaJ.ity of sodium hydroxide solution, C = Milliliters of sulfuric acid solution, D = Normality of sulfuric acid solution, and W = Weight, in grams, of residue after ignition (4.3.1). 4.3.3 Granulation. Tare, to the nearest 0.1 g, a No. 80 and a No.
30、325 sieve conforming to ASTM Ell. 325 sieve on a receiving pan. specimen into the top sieve. Wash the specimen through the sieves by means of a stream of water from a Taucet using a piece of rubber tub- ing, attached to the faucet, to direct the stream of water. (Care must be taken not to splash any
31、 of the specimen out of the sieve,) Continue the washing until no more specimen is washed through. to a constant weight, each sieve with residual specimen in a constant temperature oven at 105 + 5OC. Calcate granuation as Follows : Nest the No; 80 sieve on the No. Weigh, to the nearest 0.1 g, 100 g
32、of Dry, Cool to room temperature and reweigh. Percent through No. 80 sieve = W - (X - A)100 W and Percent through No. 325 sieve = W - (X - A +y - B)100 W where: A = Tare weight, in grams, of No. 80 sieve, B = Tare weight, in grams, of No. 325 sieve, X = Weight, in grams, of No. 80 sieve and residual
33、 specimen, y = Weight, in grams, of No. 325 sieve and residual specimen, and W = Weight, in grams, of specimen. 5 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-5, PACKAGING 5.1 Packing:, commercial. Tribasic calcium phosphate shall be comer- cialiy
34、 packed in accordance with MIL-STD-1188. Se2 Marking. Marking shaL1 be in accordance with 141L=STD-ll88. 6. NOTES 6.1 Intended use. Tribasic calcium phosphate, covered by this speci- Marking shall include lot number and date of manufacture. fication, is intended for use in colored smoke munitions. 6
35、,2 Ordering data, Procurement documents should specify the title, number, and date of this specification. 6,3 Batch, A batch is defined as that quantity of material which has - been manufactured by some unit chemical process or subjected to some physical mixing operation intended to make the final product substantially uniform. Custodians: Army - EA Air Force - 68 Review activities: Am - EA, AR DLA - Gs Air Force - 68 Preparing activity: Army -EA Project No. 681-0-0539 6 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-
