1、MILITARY S PEC IFIC AT ION MIL-E-63218 (AR) 9 December 1980 / 7 EMULSION POLYETHYLENE (FOR USE IN AMMUNITION) This specification is approved for use by the US Army Armament Research and Development Command, and is avail- able for use by all Departments and Agencies of the Department of Defense. 1. S
2、COPE 1.1 This specification covers one type of a polyethylene emulsion used in the formulation of explosive compositions (6.3). 2. APPLICABLE DOCUMENTS 2.1 Issue of documents. The following documents of the issue in effect on date of invitation for bids or r.equest for proposal form a part of this s
3、pecifisaton to the extent spec i fi ed her e in. SPEC IF I CAT IONS MILITARY MIL-A-48078 - Ammunition, Standard Quality Assur- ance Provisions, General Specifica- tion For STANDARDS MIL I TARY MIL-STD-105 - Sampling Procedures and Tables for Inspection by Attributes MIL-STD-129 - Marking for Shippin
4、g and Storage MIL-STD-1218 - ACS Chemicals FSC: 6810 THIS DOCUMENT CONTAINS 13 PAGES. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-flIL-E-b323 b 7777906 0322357 7 = - i r MIL-E-63218 (AR) a MIL-STD-123s - Single ana Multilevel Continuous Sampling
5、Procedures ana Tables for Inspection by Attributes (Copies of specifications, standards, arawings, and publica- tions required by suppliers in connection with specific procurement function should be obtained from the procuring activity or as directea by the contracting officer.) 2.2 Other publicatio
6、ns. 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. ASTM-D5 ASTM-D1386 ASTM-Di505 ASTM-D 28 3 4 ASTM-D2905 ASTM-E 2 8 ASTM-E70 ASTM-E30 O - Pe
7、netration of Bituminous Materials - Acid Number (Empirical) of Natural Waxes - Density of Plastics by Density-Graaient Technique - Nonvolatile Matter (Total Sois) in Water Emulsion Fioor Polishes, and Polymer Emulsion Floor Polishes, Test For - Statement on Number of Specimens Required to Determine
8、the Average Quality of a Textile Material - Softening Point by Ring and Ball Apparatus - pH of Aqueous Solutions with Glass Electrode - Sampling Industrial Chemicals (Application for copies should be addressed to the American Society for Testing and Materials, 1916 Hace Street, Philadelphia, Pennsyl
9、vania 19103.) (Technical society and technical association specifications and standards are generally available for reference from libraries. They are also distributed among technic1 groups and using Federal agencies.) 3. REQUIREMENTS 3.1 Composition. mi 3.1.1 Polyethylene. The polyethylene used in
10、the lsion shall comply with the requirements in Table I 2 a Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-E-b3218 68 7977706 0322358 O m MIL-E-63218 (AR) TABLE I. Requirements for Polyethylene (See 6.5) Applicable Property Hequirement Test Meth
11、od Acid Number 14-17 4.6.1.1 Penetration, mm 0.8-1.4 4.6.1.2 Viscosity 14OoC, cps, max 200 4.6.1.3 Softening Point, OC 95-100 4.6.1.4 Density, y/cc O .90-O .94 4.6.1.5 3.1.2 Emulsion. The emulsion shall be a uniform dispersion of the following materiais, as indicated in Table II (see 6.U.). TABLE II
12、. Compos it ion Polyethylene Tall Oil Fatty Acid Morpholine Stearic Aci (See 6.10) Ammonia (28%) (See 6.10) Water Emulsion Formulation % by Weiqht Notes 20.38 See 6.5 3.57 See 6.6 3.57 See 6.7 1.13 See 6.8 0.50 70.85 See 6.li 3.1.3 Emulsion properties. The properties of the emulsion shall comply wit
13、h the requirements in Table III. TABLE III. Emulsion Properties Property Applicable Requirement Test- Method Chemical Composition (based on total solids) Linoleic Acid, % Oleic Acid, % Stearic Acid, % Polyethylene, % Penetration, mm Viscosity 14OoC, cps, max. Softening Point, OC PH Transmission Valu
14、e, %, min. Dry Weight, %, min. 6.5 + 1.0 4.5 0.5 81.5 5 3.0 2.0-3.0 85 94-98 9-10 50 . 24.5 7.5 T 1.0 4.6.2. 4.6.2.i.1 4.6.2.1.1 4.6.2.1.1 4.6.2.1.2.2 4.6.2.1.3.1 4.6.2.1.3.2 4.6.2.1.3.3 4.6.2.2 4.6.2.3 4.6.2.4 3 Provided by IHSNot for ResaleNo reproduction or networking permitted without license fr
15、om IHS-,-,-MI L-E- 6 3 2 -18 (AR) 3.2 First article inspection. This specification contains provisions for first article inspection. Require- ments for the submission of first article samples by the contractor shall be as specified in the contract. 4. QUALITY ASSURANCE PROVISIONS 4.1 Responsibility
16、for inspection and standard quaity assurance provisions. Unless otherwise specified herein or in the contract, the provisions of MIL-A-48078 shall apply ana are hereby made a part of this detail specitication. 4.2 Classification of inspections. The inspection requirements specified herein are cassif
17、ied as follows: a. First article inspection (see 4.3) b. Quality conformance inspection (see 4.4) 4.3 First article inspection. 4.3.1 Submission. The contractor shall Submit a first article sample as designated by the Contracting Officer for evaluation in accordance with provisons of 4.3.2. The firs
18、t article shall consist of 20 Liters of the polyethylene emulsion obtained by sampiing.as described in 4.5.1. In addition, a one (i) kilogram sample of the poiethyiene used in the manufacture of the emulsion shall aso be submitted. The samples shail be obtained from a production lot which has been p
19、roduced by the contractor using the same production processes, procedures and equipment as wil be used in fulfilling the contract. Ail materials, shall be obtained from the same sources of supply as will be used in regular production. 4.3.2 Inspections to be performe. The sample wil be subjected by
20、the Government to any or all of the examinations or tests specified in 4.6 of this specification. 4.3.3 Rejection. See MIL-A-48078. 4.4 Quality conformance inspection. 4.4.1 Lot formation. A lot shall consist of one or more batches of the polyethylene emulsion produced by one manufacturer, in accord
21、ance with the same specification, or same specification revision, under one continuous set of operating conditions. Each lot shall consist of that quantity of Polyethylene that has been subjecte to the same 4 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from I
22、HS-,-,-MIL-E-63218 b8 9977906 0322360 9 MIL-E-63218 (AR) unit chemical or physical mixing process intended to make the final product homogeneous. The product shall be submitted for inspection in accordance with MIL-STD-105. 4.4.2 Examination. Unless otherwise specified in the classification of defec
23、ts and test tables, sampling plans for major and minor defects shall be in accordance with MIL-STD-105, Inspection Levei II (see MIL-A-48078). 4.5 Test inq; PRECAUTION WARNING This specification covers sampling and testing of toxic or hazardous materials. Accordingly, it is emphasized that all appli
24、cable safety rules, regulations and procedures must be followed in handling and processing these materials. 4.5.1 Sampling. 4.5.1.1 Polyethylene. Two independent representative samples shall be withdrawn from each batch or lot of polyethylene used in the formulation of the emulsion, using ASTM Proce
25、dure E300 for solids. If either of these samples fail to meet any test requirements given in Table I of 3.1.1, the polyethylene shall not be used in the emulsion formulation. 4.5.1.2 Emulsion. Approximately 2 liters of the poly- ethylene emulsion shall be withdrawn from each batch to be tested using
26、 ASTM Procedure E300 for liquids. Samples shall be selected for inspection in accordance with MIL-STD-1235, CSP-1 Plan, Sample Frequency Code Letter B, AQL 6.5%. If the sample fails to meet any test requirement the batch represented by the sample shall be rejected. All batches produced between the t
27、ime that the last batch was tested and accepted and the batch which failed should be tested in accordance with the applicable methods given in paragraph 4.6. If any of these batches fail to meet any of the test requirements, that batch shall also be rejected. In addition, after any failure of a batc
28、h the contractor will return to 100% inspection until “i“ successive batches are accepted as required by MIL-STD-1235. The samples shall be subjected to the tests listed in Table IV: 5 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-E-6 3 218 (AR
29、) TABLE IV. Defect classification Defect Inspection/Requirement (Emulsion) Table IV classification Chemical composition Major Hooo*o*o.oo.o.oeoo Major Transmisson,. Major Penetration, Ma or Viscosity. Major Softening point. t Major Major Dry weight . 4.5.3 Inspection equipment. The contractor shall
30、use commercial inspection equipment for all of the tests and examinations specified in 4.6. The contractor shall have the required equipment available, foliow proper calibration methods and perform the testing in accordance with accepted operating procedures. Government approval of ali inspection eq
31、uipment is required prior to its use for acceptance procedures. 4.6 Test methods and procedures. The foiowing tests shall be performed using prescribed analytical procedures for replicate determinations given in standard analyticai textbooks. ASTM Method D2905 may also be used to determine the numbe
32、r of replicates required. Also, unless otherwise specified herein, ali chemicals and reagents shall be ACS or reagent grade in accordance with MIL-STD-1218. 4.6.1 Polyethylene prior to incorporation in emulsion. 4.6.1.1 Acid number. Determine the acid number of the polyethylene sample in accordance
33、with the method given in ASTM-D1386. 4.6.1.2 Penetration. Determine the penetration value for the polyethylene sample in accordance with the method given in ASTM-D5. 4.6.1.3 Viscosity. Determine the viscosity of the poly- ethylene sample as follows: Place an eight gram sample of the polyethylene in
34、the viscosimeter cup of a Brookfield Thermosei Model LVT Viscosimeter. Attach the large spindle to the viscosimeter shaft beiny careful not to bend the thin wire used for this purpose. 6 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,- MIL-E-6323 68
35、7777706 0322362 2 W MIL-E-63218 (AR) Lower the viscosimeter cup into the heating unit and turn it until the cup firmly sets itself in the heating unit keyway. Bring the heating bath temperature to l4O0C and slowly lower the spindle into the cup in stages being sure the connecting wire does not bend
36、OE bow but hangs straight down. Lower the spindle until the two support arms just touch the flat top of the heating unit ana then back up 1 mm. Set the RPM rate so that the viscosimeter pointer is on scale preferably near the 50 mark. Wait for the sample temperature to stabilize at 140%. Record the
37、viscosimeter pointer reading at five minute intervals over the period of thirty minutes. Average the readings and calculate the viscosity using the following formula: Viscosity, in centipoises = 30RPM X B A Where: A is t,he RPM rate used for the determinations and B is the average of the viscosimete
38、r readings. 4.6.1.4 Softening point. Determine the softening point of the polyethylene sample in accoKdance with the methoa given in ASTM E-28. 4.6.1.5 Density. Determine the density of the polyethylene sample in accordance wi.th the metho given in ASTM D1505. 4.6.2 Emulsion. 4.6.2.1 Composition. 4.
39、6.2.1.1 Determination of stearic, oleic and linoleic acids. Prepare the standard stock solution as follows: Accurately weigh about 60 mg of stearic acid, 70 mg of oleic acid and 60 mg of linoleic acid into a 50.0 ml volumetric flask. Dissolve the fatty acids in chloroform and dilute to the 50.0 ml m
40、ark with chloroform. Prepare the polyethylene emulsion as follows: Pipet 10.0 m. of polyethylene emulsion into a stared 100 ml. beaker. Weigh the beaker and emulsion to the nearest 0.OOlg. Determine the sample weight (W) by subtracting the beaker tare weight from the weight of the beaker and emulsio
41、n. Add LO m. of 7 a PROBLEM HARD COPY Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-E-63218 (AR) distilled water, and 1 ml. of 6N HCL. Stir mixture well with glass rod and allow to stand with occasional stirring or 10 minutes. Quantitatively tr
42、ansfer precipitate into small (60 mi.) sintered glass funnel of coarse porosity, Using suction, wash three to four times with 25-30 ml, of distilled water until filtrate is neutral to pHydrion paper, stirring the precipitate thoroughly during each wash. Rinse once with 20 ml. of 50% methanol/water.
43、Suction-dry precipitate on filter for 10 minutes to remove residual water. Quantitatively transfer the precipitate to glass stoppered 125 ml. Erlenmeyer flask, add 50 ml. of chloroform and place in an ultrasonic vibrator or mechanical shaker until all solids are suspended. Finally quantitatively tra
44、nsfer the solution to a 100.0 ml. volumetric flask and dilute to volume with chloroform. Transfer a portion of the solution to a centrifuge tube and centrifuge until the lower portion of the solution is clear. Pipet 4.0 ml. of the clear solution and transfer to a 10.0 ml. volumetric flask, Into four
45、 appropriately marked 10 ml. volumetric flasks, pipet 2.0 ml., 3.0 ml., 4.0 ml., 5.0 ml. and 6.0 ml. of Standard Stock Solution. Add 1 drop of phenolphthalein (0.1% phenolph- thalein solution in methanol) solution to each flasks, and neutralize each to a pink end point with 0.5% methanolic potassium
46、 hydroxide solution. Evaporate the solutions in the volumetric flasks to dryness in a 45-50C water bath with the aid of a stream of dry nitrogen: Pipet 1.5 ml. of alkylating agent, prepared by dissolving 555 mg of , p-dibromoacetophenone and 53.0 mg of crown ether (1,4,7,10, 13,16-hexaoxacyclo-octad
47、ecane), in 20 ml. of benzene, into each volumetric flask and place flasks in a ultrasonic vibrator for several minutes in order to suspend any residues. (All operations involving the use of benzene must be conducted in an efficient fume hood.) Place flasks in an 8OoC water bath for 20 minutes shakin
48、g frequently, Do not allow to dry out. If necessary add 0.5 ml. of benzene to each flasks. Mix well. Cool to room temperature, and make up to volume with benzene. Draw a line 1.5 cm from the lower edge of a 20 X 20 cm KC18 Reversed Phase Thin Layer Chromatographic plate (with fluorescent indicator,
49、Whatman, Inc.) with a soft lead pencil. Mark points o application at 2 cm intervals along the line and using disposable open-end capillaries (Drummond Microcaps or equal) apply 5 lambda of each sample and standard to the plate. Run in duplicate. Allow solvent to evaporate from spots on plate and place the plates in a filter paper lined developing chamber being sure the developing solvent, acetonitrile: Chlo
