1、DOD-M-82730 68 797770b 01123274 T W H-2445 DOD-$i-82730 ( OS ) 17 AUGUST 1984 Superseding WS 14412, dated 27 April 1973 MILITARY SPECFI CATION 4,h-METHYLENEBIS (2 , 6-DI-TERT-BUTYLPHENOL) This specification is approved for use by the Naval Sea Systems Command, Department of the Navy, and is avail- a
2、ble for use by all Departments and agencies of the Department of Defense. 1. SCOPE 1.2 Scope. This specification covers the minimum requirements for the procurement of a low yolatile, temperature stable antioxidant, 4,4*-meth- ylenebis(2,6-di-tert-butylphenol) (see 6. I ) . 2. APPLICABLE DOCUMENTS 2
3、. I Government documents 2.1.1 Specifications, standards, and handbooks. Unless otherwise spec- ified, the following specifications, standards, and handbooks of the issue listed in that issue of the Department of Defense Index of Specifications and Standards (DoDISS) specified in the solicitation fo
4、rm a part of this specification to the extent specified herein. STANDARDS MILITARY MIL-STD-105 Sampling Procedures and Tables for Inspection by Attributes MIL-STD-I 29 MIL-STD- I 21 8 ACS Chemicals Marking for Shipment and Storage * Beneficial comments (recommendations, additions, deletions) and any
5、 pertinent data which may be of use in improving this document should be addressed to: Commanding Officer, Naval Ordnance Station, Stand- ardization/Documentation Division (524), Indian Head, 1.ilD using the self-addressed Standardization Document Improvement Proposal (DD Fom 1426) appearing at the
6、end of the document or by letter. iL, 20640 by THIS DOCUMENT CONTAINS .-$ PAGES Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-DOD-M-82730 b = 7779706 0323275 3 = DOD-M-82730( OS ) (Copies of specifications, standards, handbooks, drawings, and publi
7、cations required by manufacturers in connection with specific acquisition functions should be obtained from the contracting activity or as directed by the contracting officer.) 2.2 Other publications. The following documents form a part of this specification to the extent specified herein. which are
8、 indicated as DoD adopted shall be the issue listed in the current DoDISS and the supplement thereto, if applicable. The issues of the documents AMERICAN SOCIETY FOR TESTING AND MATERIALS ASTH D 1744 Water in Liquid Petroleum Products by Karl Fischer Reagent (Application for copies should be address
9、ed to American Society for Testing and Materials, 1916 Race St., Philadelphia, PA 19103. ) NATIONAL MOTOR FREIGHT CLASSIFICATION RULES (Application for copies should be addressed to the American Trucking Associations, Inc., Traffic Department, 161 6 P Street, NW, Washing- ton, DC 20036.) UNIFORM CLA
10、SSIFICATION COMMITTEE RUUS (Application for copies should be addressed to the ITniform Classification Committee, Room I 106, 222 South Riverside Plaza, Chicago, IL 60606. ) (Industry association specifications and standards are generally avail- They are also distributed among technical groups able f
11、rom libraries. and using -Federal agencies. ) 3. REQUIREI4ENTS 3.1 First article. When specified (see 6.21, a sample shall be subjected . to first article inspection (see 4.4 and 6.2). 3.2 Composition and purity. The 4,4-methylenebis( 2,6-di-tert-butylphenol) shall be a dry crystalline solid at room
12、 temperature and shall be of 98 per- cent minimum purity (see 4.6. I ) . 3.3 Melting point. The melting point shall be not less than 154.0“ Celsius (C) nor greater than 155.2“C (see 4.6.2). 3.4 Benzene insolubles. The benzene insolubles shall be not greater than 0.2 percent (see 4.6.3). 2 Provided b
13、y IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-4 DOD-M-2730 68 9797406 0123276 3 W DOD-14-82730( OS) 3.5 Water content. 3.6 Workmanship. The 4,4 1-methylenebis( 2,6-di-tert-butylphenol) shall be uniform in quality and free from materials that could adversely
14、affect. its use. The water content shall be a maximum of 0.05% (see 4.6.4). 4. QUALITY ASSUR.A.?.?CE PROVISIONS 4. I ResponsibiIity for inspection. Unless otherwise specified in the contract or purchase order, the contractor is responsible for the perform- ance of all inspection requirements as spec
15、ified herein. Except as other- wise specified in the contract or purchase order, the contractor may use his own or any other facilities suitable for the performance of the inspection requirements specified herein, unless disapproved by the Government. in the specification where such inspections are
16、deemed necessary to assure supplies and services conform to prescribed requirements. The Government reserv.es the right to perform any of the inspections set forth ka 4.2 Classification of inspections. The inspection requirements spec- ified herein are classified as follows: a. b. First article insp
17、ection (see 4.4). Quality conformance inspection (see 4.5). 4.3 . Inspection condi tioh. Unless otherwise specified (see 6.21, inspec- tion conditions shall be as specified in the applicable test method. 4.4 First article inspection. First article inspection shall be performed * br the contractor, a
18、fter award of contract and prior to production,.at a loca- cion acceptable t the Government. First article inspection shall be performed on material which has been produced from raw materials with equipment and pro- cedures normally used in production. When specified in the contract (See 6.2), the c
19、ontractor shall prepare a report giving the results obtained for all insp- ectons and tests performed. ACS grade in accordance with MIL-STD-I218 and distilled water shall be used. Where applicable, blank determinations shall be run and corrections applied where significant. which it is granted, unle
20、ss extended by the Government to other contracts. (see 6.2). plus any additional tests specified by the procuring activity (see 6.2). Unless otherwise specified all chemicals shall be P I First article approval is valid on the contract under 4.4.1 SaIilple size. Sample size shall be as specified in
21、the contract 4.4.2 Inspection routine. The sample shall be subject to the tests of 4.6 3 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-DOD-U-2730 68 9779906 0323277 5 DOD-M-82730( OS) 4.4.3 Failure. Failure of the sample to pass any test shall be c
22、ause tor first article rejection. 4.5 Quality conformance inssections. The material shall be subjected to all the following inspections and tests for acceptance. contract (see 6.2), the contractor shall prepare a report giving the results obtained for all inspections and tests performed and a certif
23、ied statement that the lot meets,all the requirements of. this specification. otherwise specified, all chemicals shall be ACS grade in accordance with MIL-STD-1218 and distilled water shall. be used. Where applicable, blank determinations shall be run and corrections applied where significant, When
24、specified in the Vnless 4.5.1 Sampling. 4.5. I .I - Lot. For the purpose oft sampling, a lot shall consist of material of a single form manufactured under one set of conditions from one production batch and offered fr delivery at one tiame. 4.5.1.2 Sampling for examination of product. A random sampl
25、e of filled containers shall be selected from each lot in accordance with WL-STD-105, inspection level II. 4.5.1.3 Sampling for tests. A representative sample of sufficient material to perform the required tests shall be taken from each lot. 4.6 Test methods. Tests shall be performed in accordance w
26、ith the flllow- ing methods. 4.6.1 Purity 4.6.1.1 Apparatus. a. p. Absolute ethyl alcohol c. Bechan DK2 recording spectrophotometer or equivalent The usual laboratory equipment for weighing and diluting the samples. ( 4.6. I .2 Procedures a. Weigh 400 I milligrams of the antioxidant sample into a 50
27、0- milliliter (mi) volumetric flask and fill to the mark with ethyl alcohol. Allow the sample to dissolve in the alcohol. b. Dilute the sample 1:lO by pipetine; 25 ml into a 250-ml volumetric flask and diluting to volume with alcohol. c. Prepare a series of standards from the sample from step I1bl1
28、as follows: 4 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-DOD-M-82730 68 W 9777706 0323278 7 W DOD-!G 82730( OS) 5 nil aliquot to 50 ml with alcohol 10 ml aliquot to 50 ml with alcohol 15 ml aliquot to 50 ml with alcohol 20 ml aliquot to 50 ml wi
29、th alcohol 30 ml aliquot to 50 ml with alcohol 40 ml aliquot to 50 ml with alcohol sample with no dilution. d. Place ethanol in matched I-centimeter cells and set the instrument from O percent transmittance at 277.5 millimicrons (mu) in accordance with the manufacturers instructions. e. Scan each of
30、 the samples from step I1cl1, and determine its absor- bance at 277.5 mu by formula 1 O0 A = log T - Where: - A = absorbance T = percent transmittance f. Plot the absorbance values from as ordinates and concentrations from IIc as abscissa on graph paper and draw the best straight line through the po
31、ints using the origin as one point. from the point of intersection of the line at the most concentrated sample. g. Read the absorbance at the highest concentration. This is obtained h. Calculate as follows: A 3567 x I .88 x 10-O % purity = Where: A = absorbance from step ligll Y 7: 3567 = molar abso
32、rbance index determined from a pure sample of 4,4“-me thy lenebi s ( 2,6- di- ter t -butylpheno 1 ) I .88 = concentration factor in moles per liter 5 I Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-DOD-M-82730 b H 777790b 0123277 7 DOD-M- 8273 O (
33、OS ) 4.6.2 Melting point. 4.6.2. I ADparatus. a. A certified thermometer graduated in 0.2“ in the 150“ to 155“ range, b. c. An oil bath. A second short thermometer to monitor the oil bath temperature. (A 250-ml metal or wrapped glass beaker with mineral oil and an overhead stirrer is satisfactory.)
34、A heater in series with a variac to control heat input to the bath. d. e. Capillary melting point tubes. u 4.6.2.2 Procedure. a. Place the bath on the heater and with the short thermometer in the bath and with continous stirring stabilize the temperature at near 150C so that there is no rapid rise o
35、r fall in temperature over a 2 or 3 minute period. b. Place antioxidant in a capillary melting point tube to-a depth of about 5 millimeters and fasten the tube to the thermometer with a collar cut from a piece of rubber tubing of appropriate size. c. Lover the thermometer into the bath at about 150C
36、 and slowly increase the heat to give a temperature rise of about 1“ per minute. d. Read the temperature at which the sample is completely melted. should be not less than 154C nor greater than 155.2“C. This e. If the melting point is not within the required range, repeat steps Iiari through lldil un
37、til a melting point has been determined with certainty. Make a stem temperature correction if the thermometer used has not been calibrated for the emergent stem. The melting point shall be the average of two determinations. 4.6.3 Benzene insoluble material. Take a sample of material whose weight is
38、between 9.500g and 10.500g. Filter the mixture through a fluted filter paper which has been dried to constant weight in a steam heated oven. benzene. steam heated oven. following fornula: Dissolve the sample in 102.5ml of benzene. Wash the residue with 50 ml of Dry the fluted filter paper and residu
39、e to constant weight in a Calculate the percent benzene insoluble material by the 6 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-DOD-M-82730 68 7797706 0123280 5 W DOD-M- 827 30( OS ) Where: R = weight of residue in g to the nearest milligram (mg)
40、 W = weight of sample in g to the nearest milligram NOTE: All operations using benzene shall be performed in a hood. 4.6.4 Water content. Determine the water content of the sample by method of ASTM D-1744. Sample size shall range between 5 and 10 grams. Commercial Karl Fischer reagent with a minimum
41、 titer of 5.0 mg of water per ml may be used. 4.6.5 Examination of product. The samples taken in accordance with 4.5. I .2 shall be inspected to verify compliance with the requirements of section 5 and other requirements of this specification not involving tests. 5. PACKAGING 5. I Packaging. 5. I. I
42、 Unless otherwise specified, the material shall be packaged in accordance with the manufacturers best accepted commehial practice. Commercial. 5.2 Packing. 5.2.1 Commercial. Unless otherwise specified, the material shall be packed in shipping containers in such a manner as to insure safe transportat
43、ion by comon carrier. Classification Rules and the Uniform Freight Classification Rules or regul- ations of other carriers applicable to the mode of transportation. or order, packages and shipping containers shall be marked in accordance with Containers used shall comply with National Hotor Freight
44、5.3 Marking. In addition to any special marking required by the contract MIL-STD-i 29. 6. NOTES 6.1 Intended use. The 4.4-methylenbis( 2,6-di-tert-butylpheno1) covered by this Specification is intended for use in the manufacture of liner material for torpedo warheads and as a component of plastic-bo
45、nded explosive formulations. - 6.2 . Ordering data. Acquisition documents should specify the following: 7 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-DOD-il-82730 68 777790b CIL23281 7 - DOD-M-82730( OS) 6.2. I Acquisition requirements. a. Title,
46、 number, and date of this specification b. Quantity desired c. d, e. f. g. h. Inspection conditions, if other than as specified (see 4.3) First article sample size, if required (see 4.4.1) Additional first article tests, if any (see 4.4.2) First article instructions regarding arrangements for examin
47、ations, test and approval Request for tests results, certificate, if required, (see 4.4, 4.5 and 6.2.2) Any special marking required ( see 5.3) 6.2.2 Contract Data requirements. When this specification is used in an acquisition which incorporates a DD Form 1423, Contract Data Requirements List (CDRL
48、), the data requirements identified below shall be developed as specified by an approved Data Item Description (DD Form 1664) and delivered in accordance with the approved CDRL incorporated into the contract. the provisions of 27.410-6 of the DoD FAR Supplement are invoked and the DD Form 1423 is no
49、t used, the data specified below shall be delivered by the contractor in accordance with the contract or purchase order requirements. Deliverable data required by this specification is cited in the following paragraphs : Paragraph Data Requirement Appicable DID When 4.4 Test report DI-T-2072 4.5 Certification data/report UD1 -A- 23 264 (Data item descriptions related to this specification, and identified in section 6
