1、4 MIL-M- 4 81 4 6 (!T.J) - I* - . 8 March 1973 SUPERSESSIOU (see 6.5) I. .I. MILITARY SPECIFICATIOJI .MOLYBDENUM TRIOXIDE (FOR USE IIJ AI.IMUIJIiIOIi) 1. SCOPE 1.1 This specification covers one gracie of ;.lolybtienum 2 . APPLICABLE DOCUIENTS Trioxide intended for use in anununition .(see 6.2). 2.1
2、The following documents of the issue in effect on date of invitation for bids, or request for proposals, form a part of this specification to the extent specified herein. SPECIFICATIOMS FEDERAL Vv-S-48 - Sacks, Shipping, Paper PPP-D-723- Drums, Fiber PPP-D-729- Drums, Iletal, 55 Gallon (for shipment
3、 of noncorrosive material) MILITARY i , . FIIL-I-112 - Packaging anci Packing for Overseas Shipment Drum, Plywood (for drums whose weight of contents does not exceed 200 pounds. ) STAND AHDS MIL IT ARY MIL-STD-105 - Sampling Procedures and Tables for MIL-STD-109 - Quality Assurance Terms and Definit
4、ions MIL-STD-129 - larking for Shipment and Storage MIL-STD-116 8- Lot Numbering of Aumunit ion MIL-STD-1233- Procedures for Deternining Particle Size, Particle Size Determination and Packing Density of Powder Naterial MIL-STD-1235- Single and Multilevel Continuous Inspection by Attributes (ABC-STD-
5、105). V Sampling Procedures and Tables for Inspection by Attributes FCC: 6810 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-.MIL-M-4L4b b = 7777706 OL2LO2 2 , ,.- k-3 E ! I I I MIL-M-48146- (MU)-, * - - * q- - (Copies -of specifications, standards
6、, drawinfr;s and publications. required by suppliers in connection with specific procurement functions should De obtained from the procuring activity or as directed by the contracting officer.) part of this specification to the extent specified herein. Unless otherwise indicated, the issue in effect
7、 on date of invitation for bids or request for proposal shall apply. 2.2 Publications.-The followTng docunenta form a AMERCIAbJ SOCIETY FOR TESTIEJG AIID MATERIALS PUBLICATION ASTI1 Designation E300-70 - Recommended Practice for Sampling Industrial Chemicals (Application for copies of ASTM Standards
8、 should be addressed to the American Society for Testing and Materials, 1916 Race Street, Philadelphia, Pennsylvania, 19103). UfIIPORM FREIGHT CLASSIPICATIOEJ RIJLES (Application for copies of these freiKht classification rules should be addressed to the Consolidated Classification Committee, 202 Ch
9、icago IJnion Station, Chicaco, Ill. 60606). AMERICAN TRUCKING ASSOCIA“IOF! PUBLICATIOFJ National rlotor Freight Classification Rilles and Container Specifications. (Application for copies should be addressed to the American TruckinE Association, 1424 16th Street N.W., Washington, D.C. 20482.) 3. REQ
10、UIREMENTS 3.1 The requirements for moiybdenum trioxide shall comply with Table I when determined as specified in the . applicable paragraphs of section 4.4. TABLE I Test . Property Percent Paragraph Assay, minimum (min.) . 99.5 4.4.1 Insoluble in ammonium hydroxide, maximum (max. ). 0. o10 4.4.2 Chl
11、oride (Ci), max. 0.002 4.4.3 Nitrate (!JO 1, max. 0.003 4.4.4 Arsenate, p osphate and silicate 0.001 4.4.5 (as Sioz), max. 2 2 1 / Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-. -. k, . . , . ,y: . - _. - . . . ,. . . . . . . . . . -.- I- . . . .
12、MIL-M- 4 814 6 ( MU) Sulfate (SO 1, max. Ammonium (NA4) , max. Heavy metals (as Pb), max. 0.020 O. O02 0.00.5 4.4.6 4.4.7 4.4.8 3.2 Average particle size.-The average particle size of molybdenum trioxide shall be 8 plus or minus 4 microns when dete,rmined as specified in paragraph 4.4.9. 3.3 ,Workma
13、nship.-The material furnished under this -, specification shall be free flowing and free of lumps, dirt, chips and other foreign material. provisiorls for first article testing. Submission of first article quantity by the contractor shall be as specified in the contract. 3.4 First article testing.-T
14、his specification makes 4. QUALITY ASSURANCE PROVISIONS 4.1 Responsibility for inspection.-Unless otherwise specified in the contract or purchase order, the supplier is responsible for the performance of all inspection requirements as specified herein. Except as otherwise specified in the contract o
15、r 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 right to perform any of the inspections set forth in the specification where such inspections
16、are deemed necessary to assure supplies and services conform to prescribed requirements. Reference shall be made to MIL-STD-109 in order to define the terms used herein. 4.1.1 Submission of product.-At the time the completed lot of product is submitted to the Government for acceptance the contractor
17、 shall supply the following information accompanied by a certificate which attests that the information provided is correct and applicable to the product being submitted: requirements and quality assurance provisions specified in this specification. b. Specification number and date, together wi.th a
18、n identification and date of changes. c. Certificates of analysis on all materials used directly by .:2,: . .- . . .-.- i. . Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-M-48346 b 7779706 0323084 b MIL-M-48146 (MU) The certificates shall be si
19、gned by a responsible.agent of the certifying organization. The initial certificate submitted shall be substantiated by evidence of.the agents authority to bind his principal. Substantiation of the certificates unless, during the course of the contract, this authority is vested in another agent of t
20、he certifying organization. .agents authority will not be required with subsequent - ., 4.2 First Article Inspection 4.2.1 Submission.-Prior to initiation of regular production the contractor shall submit a first article sample consisting of i50 grams of molybdenum trioxide in accordance with instru
21、ctions issued by the Contracting Officer for evaluation in accordance with paragraph 4.2.2. All samples submitted shall have been produced by the contractor using the same production processes, procedures, and equipment as will be used.in fulfilling the contract. All materials, including packaging a
22、nd packing, shall be obtained from the same sources of supply as will be used . in regular production. The sample shall be accompanied by certificates of analysis. A first article quantity, shall also be submitted whenever there is a lapse in production for a period in excess of 90 days, or whenever
23、 a change occurs in manufacturing process, material used, drawing, specification or source of supply as to significantly affect product uniformity as determined by the Government. Prior to submission, the contractor shall inspect the sample to the degree necessary to assure that it conforms to the r
24、equirements of.the contractand submit a record of this inspection with the sample. A sample containing known defects will not be submitted unless specifically authorized by the Contracting Officer. (see 6.1) 4.2.2 Inspections to be performed.-The sample will be subjected by the Government to any or
25、all of the examinations or tests specified in 4.3 and 4.4 of this specification and any or al1,requirements of the applicable drawings . 4.2.3 Rejection.-If any sample fails to comply with any of the applicable requirements, the first article quantity shall be rejected. The Government reserves the r
26、ight to terminate its inspection upon any failure of a sample to comply with any of the stated requirements. . 4.3. inspection Provisions 4.3.1 Lot formation.-A lot shall consist of one or more batches of molybdenum trioxide produced by one manufacturer in accordance with the same specification or s
27、ame specification 4 n Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-L /. ( revision under one continuous set of operatini: conditions. Each batch shall consist of that quantity of molybdenum trioxide that has been subject to the sane unit chemical
28、_- or physical mixing process intended to make the final product homogeneous. The product shall be submitted for inspection in accordance with MIL-S?I)-lOS. The criteria and procedures for the assignment of lot numbers shall be in accordance with MIL-STD-1168. 4.3.2 Examination.-Sampling plans and p
29、rocedures for the following classifications of defects shall be in accordance with MIL-STD-105 (ABC-STD-105). Contractors sampling plans, If used, shall be approved by the Government and shall provide as a minimum, the protection afforded the Government by the sampling plans in MIL-STblOS. Continuou
30、s sampling plans In accordance with MIL-S”1)-1235 nay be used if approved by the procuring activity. Also, at the option of the procuring activity, AQLs and sampling plans may be applied to the individual characteristics listed, usinp: an AQL of 0.40 percent for each major defect and an ACL of 0.65
31、percent for each Minor Defect. 4.3.2.1 Drum, prior to fillinl: (Polyethylene liner) Categories Defects Method of Code No. Inspection (see 6.4) Critical: None defined. Major: AQ, 0.40 percent Minor: None defined. 4.3.2.1.1 Drum, prior to filling (alternative method) Categories Defects Method of Code
32、FIO. 101. Liner cut, torn or punctured.Visual O1001 Inspection Critical: None defined. Ma j or : AQL 0.40 percent 101. Laminations or coatings incomplete . . Tisual 01002 Minor : None defined. 5 . 4.3.2.2 Drum, prior to closinF: (Polyethylene liner) . f 5 L o. Provided by IHSNot for ResaleNo reprodu
33、ction or networking permitted without license from IHS-,-,-Categories Defects Critical: None defined Critical: None defined. 6 Method of Code No. Inspection Ma j or : AQL 0.40 percent 101. Liner not completely sealed Visual/ Manual Minor : None defined. 4.3.2.3 Drum, sealed (steel) Categories Defect
34、s Method of Code No. Inspection 4.3.2.4 Drum, sealed (fiber) 02001 Ma j or : AQL 0.40 percent 101. Closing ring damaged or improperly positioned (drum cannot be closed properly). Visual Minor: AQL 0.65 percent 201. Marking misleading, missing or unidentifiable Visual Categories Defects O3001 03002 M
35、ethod of Code Ido. Inspection Critical: None defined Major: AQL 0.40 percent 101. Weight of contents . Baiance(CD) 04001 102. Closure incomplete or damaged to the extent that contents sift out, . Visual 04002 Minor: 0.65 percent 201. Marking rnisleading,missing or unidentifiable.Visual 04003 4.3.2.5
36、 Drum, sealed (plywood) Categories De fe c t s Critical: None defined. II Piethod of Code No. Inspection Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-6:;:. . . .- MIL-M- 4 8 i46 (MU ) .- . . c ,. . . . . . . . , . . , . . . ._ - . . . . : . - . NI
37、L-H-48346 68 m 9777706 0323087 3 . - AQL 0.40 percent Major: .I . . . . . . . . contractor will return to 100% inspection until “i1 successive batches are accepted as .required by MIL-STD-1235. The classification and code 7 . . . - “ . . . . . . . Provided by IHSNot for ResaleNo reproduction or netw
38、orking permitted without license from IHS-,-,-I i MIL-M-48146 (MU) I : Assay Insoluble in ammonium hydroxide Chloride (Ci) Nitrate (NO ) Arsenate, pl?osphate and silicate (as SiO2) Sulfate (SO ) Ammonium (Nh4) Heavy metals (as Pb) Average particle size TABLE II Major Defect Major Defect Major Defect
39、 Ma j or De f e ct Major Defect Major Defect Major Defect Major Defect Maj or Defect Code No. O6001 Code No. 07001 Code No. O8001 Code No; 09001- Code No. 10001 Code No. 11001 Code No. 12001 Code No. 13001 Code No. 14001 4.3.4 Inspection equipment.-The inspection equipment required to perform the ex
40、amination and tests prescribed in this section is identified under the “Method of Inspectiontt heading in 4.3.2 (see 6.3). 4.4 Test Methods and Procedures 4.4.1 Assay 4.4.1.1 Lead acetate reagent (10 percent) solut,on.- Pb- “P Dissolve 100 grams of lead acetate ICH3COO)2 in distilled water. If neces
41、sary, add a few drops o acetic acid to clear the solution and dilute to 1000 ml. 4.4.1.2 Methyl orange indicator.-Dissolve 0.10 grams of methyl orange in 100 ml of distilled water. 4.4.1.3 Procedure.-Approximately 1 gram of sample, accurately weighed, shall be dissolved in 10 ml of distilled water p
42、lus 1 ml of ammonium hydroxide. The solution shall be transferred to a 250 ml volumetric flask diluted to volume and mixed throughly. A 50.0 ml aliquot shall be transferred to a 600 ml beaker to which the following shall be added: 250 ml of distilled water, 20 grams of ammonium chloride, i5 ml of hy
43、drochloric acid and 0.15 ml 8 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-1.31L-M-4til46 (I7U) of methyl.orange Zndicator solution (sec 11.h.1.2). The solution shall be heated nearly to hoilint: and 18 rnl of the 10 percent lead acetate reagent s
44、olution shall be added (see 4.4.1.). To the hot and constantly stirred solution acici slowly a saturated solution of armonium acetate until the solution is alkaline, and then an excess of 15 ml of the acetate solution. I)iF“,cnt on the hot plate in the covered beaker at a temperature just; below boi
45、ling until the precipitate hassettled (from one half to one hour). Filter the mixture throiici1 a Gooch crucible wtiich has been ignited and weighed. ilash the crucible eirht times with a solution containing 10 ri1 of nitric acid and 100 ml of a saturated solution of annonitir? acetate which has bee
46、n diluted to 1000 111 with distilled water, and then wash three times with hot vater. Tgnite the crucible in a muffle furnace at 5G0C to 625C until constant weiht is obtained. The crucible and contents shall be cooled in a desiccator and weif;heti as lead molybdate (fbJ4oO4) . Calculate the percenta
47、ge of molybdenurn trioxicie as follows: Percent Nolybdenum Trioxide = 0.332i x Il x 100 Mere: dl = weight of residue, iri I: 4 . II. 2 il2 W2 = weight of saraple in aliquot; tised, in Insoluble in dilute armoniun hytiro:;icic. - Approxinately 10 crams of sarnple, acciirately wcir,!ieti , shall be di
48、ssolved in 120 rnl of dilute armoriiirm hydroxide (1 plus 6) (see 6.8) and theri heated to boilinf: anti diyested in a covered beaker on a stear? bath for 2 hours. Filter through a tared medium porosity filteririgf crucible, wash thoroughly with distilled water arid dry at 105OC to constant weicht.
49、The residire shall be calculated as percent insoluble in dilute amnoniiin hydroxide as follow : Percent insoluble in dilute annoniiirn hydroxide = 1OOA w Where: A = Ileight of residue, in fz 4 . 4.3 Chloride 4. i+. 3.1 W = Weight of sacple irsed, in Silver nitrate reagent Solutiori.-Dissolve 17 grams of silver nitrate (dried at lO5OC, in a mixture of 800 m
