1、MJL-P-13298&(kU) 30 NOVEMBER 1963 SUPERSEDING 11 MARCH 1954 MIL-P-l3298(ORD) MILITARY SPECIFICATION POLYISOBUTYLENE (FOR AMMUNITION USE) 1. SCOPE . 1.1 This specification covers one type of stabilized polyisobutylene of 99,000 to 120, O00 average molecular weight for use in Polyisobutylene Binder. 2
2、. APPLICABLE DOCUMENTS 2.1 The following documents of the issue in effect on date of invitation for bids or request for proposal form a part of this specification to the extent specified herein. SPECIFICATIONS MILITARY MIL-P-10025 -Packaging, Packing, and Marking For Interplant Shipment of Inert Amm
3、uni- tion Components.: General Specifica- tions For STANDARDS FEDERAL Fed. Std. No. 791 “Lubricants, Liquid F u e I s, and Re- lated Products, Methods of Test- ing MILITARY MIL-STD-105 “Sampling Procedures and Tables for In- spection by Attri- butes MIL-STD-109 -Quality Assurance Terms and Defini- t
4、ions MILSTD-1235 -Single and Multilevel Continuous Sampl- ing Procedures and Tables for Inspec- tion by Attributes (Copies of specifications, standards, drawings and publications required by suppliers in connection with specific procurement functions should be obtained from the procuring activity or
5、 as directed by the contracting officer.) 2.2 Other publications. The following docu- ment forms a part of this specification to the extent specified herein. Unless otherwise indi- cated, the issue in effect on date of invitation for bids shall apply. AMERICAN SOCIETY FOR TESTING AND MA- TERIALS (AS
6、TM) D460 -Chemical Analysis of Soaps, Iodine Number (Wijs) Meth- od D1524-Visual Examination of Used Electrical Insulating Oils in the Field. (Application for copies should be addressed to the American Society for Testing and Materials, 1916 Race Street, Philadelphia 3, Pa.) 3. REQUIREMENTS 3.1 Mate
7、rial. The material used in the man- ufacture of polyisobutylene shall be such as to produce a finished polyisobutylene con- forming to the requirements of this specifica- tion and all applicable specifications and drawings. The polyisobutylene shall be stabi- lized against depolymerization at 125 Fa
8、hr- Licensed by Information Handling Servicesenheit and shall be in the form of consolidated be greater than 6% when determined as spec- crumbs to aid in incorporating the material ified in 4,3,1J, in the binder composition. colop than the standard when determined as Properties of the PolYisobutYlen
9、e shall be in specified in 4.3.1 or the color value shall not accordance with table I. 3.2 Color. The color shall not be darker in 3*3 properties* The TABL I Properties Biinimum Intrinsic Viscosity 3.15 Iodine Number - Chlorine, percent . Acidity (as HCI), percent Insoluble matter, percent - 4, QUAL
10、ITY ASSURANCE PROVISIONS 4.1 .General quality assurance provisions. Unless otherwise specified in the contract or purchase order, the supplier is responsible for the performance of all inspection require- ments specified herein. Except as otherwise specified, the supplier may utilize his own or any
11、other inspection facilities and services acceptable to the Government. Inspection rec- ords of the examinations and tests shall be kept complete and available to the Govern- ment as specified in the contract or order. The Government reserves the right to per- form any of the inspections set forth in
12、 the specification where such inspections are deemed necessary to assure that supplies and services conform to prescribed requirements. Reference shall be made to Standard MIL- STD-109 in order to define the terms used herein. Inspection shall be performed in ac- cordance with this specification and
13、 other specifications referenced in any of the con- tractual documents, 4.1.1 Contructor quality ussurnce system. If the contractor desires to utilize a quality assurance system, which is at variance with the qualigy assurance provisions of 4.2 and 4.3 and other documents referenced herein, he shall
14、 submit a written description of the system to the contracting officer for approval prior to initiation of production. It shall in- clude a description covering controls for lot formation and identification, inspection to be performed, inspection stations, sampling pro- Y q . :.- Maximum Aplicable P
15、araDrapha 3.72 4.3.2 1.32 4.3.3 0.10 4.3.4 0.01 4.3.5 0.20 4.3.6 cedures, methods of inspection, (measuring and testing equipment,) and provisions for control and disposition of nonconforming ma- terial. The written description will be consid- ered acceptable when, as a minimum, it provides the qual
16、ity assurance provisions re- quired by the provisions of 4.2 and 4.3 and the other documents referenced herein. The contractor shall not be restricted to the in- spection station or the method of inspection listed in this specification provided that an equivalent control is included in the apprbved
17、quality assurance procedure, In cases of dis- pute as to whether certain procedures of the contractors system provide equal assurance, the comparable procedure of this specifica- tion shall apply. The contractor shall notify the Government of, and obtain approval for, any changes to the written proc
18、edure that effects the degree of assurance required by this specification or other documents refek- enced herein. 4.1.2 Submission of product. At the time the completed lot of product is submitted to the Government for acceptance the contrac- tor shall supply the following information ac- companied
19、by a certificate which attesfs that the information provided is correct and ap- plicable to the product submitted : (a) A statement that the lot complies with all qyality assurance provi- sions of the approved current written description of the system. (b) Quantity of product inspected. . . Licensed
20、 by Information Handling Services(c) Results obtained for all inspection performed shall be made available upon request by the Resident Ordnance Inspection. (d) Specification number a.nd date, to- gether with an identification and date of changes. (e) Certificates of analysis on all mate- rial procu
21、red directly by the con- tractor when such material is controlled by Government specifi- cations listed in any of the con- tractual documents shall be made available upon request by the Res- ident Ordnance Inspection. (f) Quantity of product in the lot. (g) Date submitted. The certificate shall be s
22、igned by a responsi- ble agent of the certifying organization. The initia.1 certificate submitted shall be sub- stantiated by evidence of the agents author- ity to bind his principal. Substantiation of the agents authority will not be required with subsequent certificates unless, during the course o
23、f the contract, this a.uthority is vested in another agent of the certifying organization. 4.1.3 Government verification. Using the contractors written quality assurance proce- dure (see 4.1.1), this specification, and other contractual documents as a guide, the Govern- ment inspector shall verify a
24、ll quality assur- ance operations performed by the. contractor. Verification shall be in accordance with (a) OF (b) below as applicable, the decision being the responsibility of the procuring activity. In either case, the inspector shall also ascer- tain, prior to acceptance, that all quality as- su
25、rance provisions of other specifications referenced in any of the contractual docu- ments have been complied with. Deviations from prescribed or agreed upon procedures discovered by the Government inspector shall be brought to the attention of the supplier. Disposition of the product and remedial ac
26、- tion shall be as directed by the Government inspector and depending on the nature of the deviation, ma.y consist of lot rejection, screening, re-sampling, re-instruction of the RIL-P-zA(MU) suppliers employees, OF other appropriate action : (a) Verification at the point of manu- facture shall be a
27、ccomplished at unscheduled intervals in accord- ance with 4.1.3.1 and 4.1. (b) Verification at the point of delivery shall be in accordance with 4.1. 4.1.3.1 Szc.1.veiZknce. Surveillance shall in- (a) Observation of procedures concern- ing lot fornlation and identifica- tion. (b) Observation of samp
28、ling procedures and application of acceptance criteria. (c) Determination that all required ex- aminations and tests are per- formed in accordance with the prescribed procedures of this specification, or approved equiv- alents thereto. (d) Review of procedures for control and disposition of nonconfo
29、rming material. clude, but is not limited to: 4.2 Inspection provisions. 4.2.1 Lot formcction. A lot shall consist of polyisoubtylene from the same batch or blend- ing operation from one manufacturer, in ac- cordance with the same specification, OF same specification revision, under one unchanged pr
30、ocess. In event of a continuous process, a lot shall consist of material subjected to the same processing opcrations and condition. 4.2.2 Exctwiruttion. Sampling plans and procedures for the folloving classifications of defects shall be in accordance with Standard MIGSTD-105 except that inspection f
31、or critical defects, when listed, shall be 100 per- cent. Continuous sampling plans in accord- ance with Standard MIL-STD-1235 may be used if approved by the procuring activiw, AQLs and sampling plans may be applied to the individual characteristics listed using an AQL of 0.25 percent for each major
32、 defect and an AQL of 0.40 percent for each minor defect. 4.2.2.1 Container, sealed. -3 Licensed by Information Handling ServicesCategories Defects Critical: None defined. Method of Code No. Major: AQL 0.25 percent 101. Container damaged to the extent that the contents are exposed, or likely to beco
33、me exposed or leak out, in subsequent handling . . . , . , . . . .Visual O001 Minor : AQL 0.40 percent 201. Marking misleading or unidentifiable. . . . . . , . . . . . . . . . . . . . . . , . . . . . . . . , . . . , Visual O002 4.2.3 Testing. 4.2.3.1 Sampling by lot. A random sa.mple of 8 containers
34、 shall be selected from each lot. When lots are comprised of 8 containers or less each container shall be sampled. 4.2.3.2 Prepurution of composite. Approxi- mately two ounces of polyisobutylene shall be removed from each of the 8 containers by means of a sharp metallic instrument or oth- er suitabl
35、e tools in order to equal 16 ounces, and if there are less than ten containers, equal primary samples in sufficient quantity to equal 16 ounces, shall be removed from each container, The individual primaly sam- ples shall then be combined in order to form a homogeneous composite sample of 16 ounces
36、and subjected to the tests specified in 4.3. If the composite sample fails to comply with any of the requirements specified, the lot shall be rejected. 4.3 Test methods and procedures. 4.3.1 Colo?*-Code numbe?. 02001. A stand- ard COIOP solution shall be prepared by dis- solving 0.0075 plus or minus
37、 0.0001 gram of potassium dichromate in a small amount of distilled water in a one liter volumetric flask and diluted to volume with distilled water. A solution shall be prepared by dissolving 5.00 grams plus or minus 0.01 grams of the sample in 100 milliliters of diisobutylene. If the sample is not
38、 uniform in color, the darkest portion of the sample shall be used, in the preparation of the solution. A I00 milliliter portion of each of the above solutions shall be transferred to Nessler tube and placed be- side each other on a white surface. The solu- tion of the sample shall be no darker in c
39、olor than the standard solution. 4.3.1.1 Altemate method. The color inten- I sity can be determined by using a modified Hellige Aqua Tester, Model 611A. The color disks used in this instrument are standard disks known as Standard Varnish Color Disk #G20 C40. Colors on this disk are graduated from 1
40、to 9 and can be read to the nearest half color unit. Lower numbers indicate lighter color. Further details on test proce- dures can be found in ASTM method D1526 58T. 4.3.2 Intwhsic viscosity-Code No. 03001. One gram of the sample (cut into approxi- mately 1 centimeter on a side) shall be dried in a
41、 vacuum oven at 70 Centigrade and re- duced in pressure to 25 inches of mercury for a minimum of 24 hours. An accurately weighed portion of approximately 0.05 grams of the sample shall be transferred to a clean, dry, glass stoppered 50 milliliter cylinder. Fifty milliliters of diisobutylene (boiling
42、 point 10lo-104“C.) shall be added to the cylinder by means of a calibrated pipette. The cylinder shall be tightly stoppered and placed in an end-over-end rotating device. The cylinder shall be allowed to rotate at approxi- mately 2 revolutions per second for 40 hours OF as long as necessary to effe
43、ct a complete solution at room temperature. The kinematic viscosity of the solution and of the solvent at 20 plus or minus 0.lo Centigrade shall be determined by means of a number 1 Ub- belohde viscosimeter, in accordance with method 305 of Standard Federal Standard 791. The kinematic viscosity in c
44、entistokes from each of the above determinations shall be recorded. The intrinsic viscosity shall be calculated as follows : Intrinsic viscosity =+T log lo B A = viscosity of solution 2 303 where : Licensed by Information Handling ServicesB = viscosity of solvent C = grams of polyisobutylene per 100
45、 milliliters of diisobutylene 4.3.3 Iodine number, Code number 04001. 4.3.3.1 Reagents. The Wijs, potassium iodide and sodium thiosulphate solutions shall be made in accordance with ASTM method D460-58 iodine number Wijs method. 4.3.3.2 P?-ocedure. An accurately weighed specimen of approximately 0.5
46、 grams shall be transferred to a 500 milliliter Pyrex, glass stoppered, vapor-release iodination flask (see 6.2). Fifty grams of pure para-dichloroben- zene shall be added to the flask and the flask placed on a hotplate with the vapor release of the flask lined up to release pressure. The solution s
47、hall be allowed to boil gently, and the flask and contents swirled from time to time. Care shall be taken to prevent particles of the sample from adhering to the sides of the flask above the solvent and scorching. When the sample has completely dissolved (approximately 20 to 30 minutes is usually re
48、quired), the flask shall be removed from the hotplate and allowed to cool to room temp- erature. Fifty milliliters of chloroform shall be added before clystallization of the para- dichlorobenzene is complete (i.e., when a small amount is still in the liquid phase). Five milliliters of the Wijs solut
49、ion shall be transferred to the flask by means of a pipette and a thin film of the potassium iodide solu- tion placed on the stopper, care being taken that none of the solution enters the flask. The flask shall be stopped with the vapor release closed, placed in an ice bath, and allowed to stand in a dark place for 2 hours. After re- moving the flask from the ice bath 25 milli- liters of the potassium iodide solution and 50 milliliters of water shall be added. The excess iodide shall immediately be titrated with the sodium thiosulphate solution. Near the end- point, 5 mi
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