1、INCH-POUNDMIL-DTL-398D12 December 1996SUPERSEDINGMIL-R-398C22 August 1962DETAIL SPECIFICATIONRDX(CYCLOTRIMETHYLENETRINITRAMINE)This specification is approved for use by all Departments andAgencies of the Department of Defense.1. SCOPE1.1 Scope. This specification covers the requirements,examinations
2、 and tests for two types of RDX for use in explosivecompositions as follows: (see 6.1).Type I - RDX made by the nitric acid process (see 6.8).Type II - RDX made by the acetic anhydride process (see 6.8).2. APPLICABLE DOCUMENTS2.1 General. The documents listed in this section areneeded to meet the re
3、quirements specified in sections 3, 4 and 5of this specification. This section does not include documentsin other sections of this specification or recommended foradditional information or as examples. While every effort hasbeen made to ensure the completeness of this list, document usersare caution
4、ed that they must meet all requirements documentscited in sections 3, 4 and 5 of this specification, whether ornot they are listed.Beneficial comments (recommendations, additions, deletions) and anypertinent data which may be of use in improving this document, should beaddressed to: Commander, U.S.
5、Army ARDEC, ATTN: AMSTA-AR-EDE-S, PicatinnyArsenal, NJ 07806-5000 by using the Standardization Document ImprovementProposal (DD Form 1426) appearing at the end of this document or by letter.AMSMC N/A FSC 1376Distribution Statement A. Approved for public release;distribution is unlimited.Provided by
6、IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-398D22.2 Government documents.2.2.1 Specifications, standards and handbooks. Thefollowing specifications, standards and handbooks form a part ofthis document to the extent specified herein. Unless otherwise
7、specified, the issues of these documents are those listed in theissue of the Department of Defense Index of Specifications andStandards (DODISS) and supplement thereto, cited in thesolicitation (see 6.2).SPECIFICATIONSFEDERALRR-S-366 - Sieves, Standard for Testing PurposesSTANDARDSDEPARTMENT OF DEFE
8、NSEMIL-STD-1168 - Lot Numbering of AmmunitionMIL-STD-1235 - Single and Multilevel ContinuousSampling Procedures and Tables forInspection by AttributesMIL-STD-1751 - Safety and Performance Tests forQualification of ExplosivesDOD-STD-2101 - Classification of Characteristics(Unless otherwise indicated,
9、 copies of the above specifications,standards and handbooks are available from DODSSP - CustomerService, Standardization Documents Order Desk, 700 RobbinsAvenue, Bldg. 4D, Philadelphia, PA 19111-5094).2.2.2 Other Government documents, drawings and publications.The following other Government document
10、s, drawings andpublications form a part of this document to the extent specifiedherein. Unless otherwise specified, the issues are those citedin the solicitation.DRAWINGSHolston Defense Corp. Engineering Drawing No. 7651-1028.48, 7651-1028.49 asterisks(*) indicate one hundred percent inspection. If
11、sample sizeexceeds lot size, perform one hundred percent inspection. Accepton zero and reject on one or more for all inspection levels.b. Alternative conformance inspection provisions. Unlessotherwise specified herein or provided for in the contract,alternative conformance inspection procedures, met
12、hods orequipment, such as statistical process control, tool control,variables sampling or other types of sampling plans, etc., may beused by the contractor when they provide, as a minimum, the levelof verification required by the provisions specified herein.Prior to applying such alternative procedu
13、res, methods, orequipment, the contractor shall describe them in a writtenproposal submitted to the Government for evaluation (see 6.14).When required, the contractor shall demonstrate that theeffectiveness of each proposed alternative is equal to or betterthan the specified conformance inspection p
14、rovision(s) herein.In cases of dispute as to whether the contractors proposedalternative(s) provides equivalent assurance, the provisions ofthis specification shall apply. All approved alternativeprovisions shall be specifically incorporated into thecontractors quality program or detailed inspection
15、 system, asapplicable.Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-398D104.5.2.1 RDX (cyclotrimethylenetrinitramine). (Classification ofCharacteristics)Conformance Requirement InspectionCriteria Paragraph MethodReferenceCritical None defin
16、edMajor101 Melting point determination 4.6.1 3.2 4.7.1102 Insoluble particles 4.6.1 3.2 4.7.2103 Acetone insoluble material 4.6.1 3.2 4.7.3104 Inorganic insoluble material 4.6.1 3.2 4.7.4105 Acidity determination 4.6.1 3.2 4.7.5106 Granulation determination 4.6.1 3.3 4.7.6107 HMX content 4.6.1 3.2 4
17、.7.7108 Impact sensitivity 4.6.1 3.2 4.7.8Minor201 Workmanship 4.6.1 3.5 4.7.94.6 Sampling and inspection equipment.Hazard NoticeThe materials described herein are flammable or explosive orboth. Consequently, they present hazards in manufacture,handling, storage and shipment. The contractor should r
18、ecognizethese hazards and take appropriate measures to guard and protectagainst fire, explosion, adverse environment, corrosiveatmosphere, rough handling and electrically-induced incidents.4.6.1 Sampling. The tests depicted in paragraphs 4.7.1through 4.7.9 shall be performed on an approximate twelve
19、 (12)ounce sample representative of the batch and taken in accordancewith ASTM Procedure E300-70 for solids. The selection of batchesfor inspection sampling and testing shall be in accordance withMIL-STD-1235, CSP-1, Plan, Sample Frequency Code Letter B, AQL6.5%. If any sample fails to meet any test
20、 requirement, thebatch represented by the sample shall be rejected. All batchesproduced between the time that the last batch was tested andaccepted and the batch which failed shall be tested in accordancewith the applicable methods given in paragraph 4.7. If any ofthese batches fail to meet any of t
21、he test requirements, thatbatch shall also be rejected. In addition, after any failure ofa batch the contractor will return to 100% inspection until “i”successive batches are accepted as required by MIL-STD-1235. Theclassification shall be as given in Table 4.5.2.1.Provided by IHSNot for ResaleNo re
22、production or networking permitted without license from IHS-,-,-MIL-DTL-398D114.6.2 Inspection equipment. Commercially availableinspection equipment shall be used for all examinations and testsspecified in 4.5 and 4.7. The contractor is responsible to havethe necessary equipment available, use it co
23、rrectly and to assurethat proper calibration procedures are followed. The designationof an instrument of a particular make or model number is notintended to preclude the use of an equivalent make or model whichis capable of performing the required test. Government approvalof all inspection equipment
24、 is required prior to its use foracceptance purposes. Inspection equipment designs shall besubmitted to the Technical Agency (see 6.12).4.7 Methods of inspection. The following tests shall beperformed using prescribed analytical procedures for replicatedetermination given in standard and analytical
25、textbooks. Also,unless otherwise specified herein, all chemicals and reagentsshall be ACS Grade or reagent grade chemicals (see 6.13 for useof equivalent test methods).4.7.1 Determination of melting point.4.7.1.1 Apparatus. A melting point bath equipped with amechanical stirrer and a source of heat
26、that can be easilyregulated shall be set up. A beaker of 1 to 2 liters capacityabout 3/4 full of clear paraffin oil is suitable. An accuratelystandardized total immersion Centigrade (C.) thermometer shall besuspended in the bath so that the bulb is not less than 1.5inches from the bottom of the bath
27、. If the mercury column is notcompletely immersed at the temperature of the observed melting, asecond thermometer shall be suspended about 0.5 inch from thefirst thermometer with its bulb approximately at the height ofthe middle of the exposed mercury column of the firstthermometer.4.7.1.2 Procedure
28、. A thin-walled capillary tube of uniformdiameter, long enough to extend beyond the top of the bath shallbe used. The tube shall be filled with a dry portion of thesample to a depth of approximately 4 millimeters (mm), the samplecompacted by tapping, and the tube fastened to the standardizedthermome
29、ter so that the lower end of the tube is in contact withthe bulb of the thermometer. The stirrer shall be started andthe bath heated rapidly to approximately 180 degrees C., thengradually heated so that the rise in temperature is not less than1 degree in 3 minutes nor more than 1 degree in 1 minute.
30、 SinceRDX does not melt sharply or give a definite meniscus, themelting point of the material shall be observed at the point atwhich the sample first gives evidence of movement in thecapillary, exclusive of shriveling. There is an increase involume caused by decomposition and evolution of gas. This
31、isespecially marked with Type II. The beginning of gas evolutioncauses the sample to rise slowly in the capillary. Thetemperature at which this occurs shall be taken as the meltingpoint.Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-398D124.
32、7.1.3 Report. If the mercury column is completelyimmersed at the melting point temperature, this temperature shallbe reported with calibration corrections applied, as the meltingpoint of the sample. If part of the column is exposed, thefollowing correction shall be added to the observed temperature:
33、Correction = n (T-t) 0.000159Where:n = number of degrees C. in the exposed mercury column.T = uncorrected melting point in degrees C.t = average temperature in degrees C. of the exposed mercurycolumn.4.7.1.4 Alternate method. The Fischer-Johns hot stagemelting point apparatus shall be used as an alt
34、ernate method todetermine the melting point of RDX. The thermometer of thisapparatus shall be calibrated using appropriate melting pointstandards. A portion of the sample shall be ground in smallagate mortar and a very small quantity (approximately 0.05 gram)of the finely pulverized sample placed be
35、tween two clean 18millimeters (mm) diameter cover glasses. These shall be gentlybut firmly pressed together and placed in the circular depressionon the stage. The powerstat shall be turned up and the unitallowed to heat. The heating rate may be very rapid to within 15degrees C of the melting point.
36、Thereafter a heating rate ofapproximately 1 degree C per minute shall be used. When thesample begins to melt, the thermometer shall be read and thetemperature reading adjusted to reflect the thermometercalibration correction shall be reported as the melting point.4.7.2 Determination of insoluble par
37、ticles. A 50 gm + 0.5gm portion of the sample shall be weighed to the nearest 0.01gram in a 600 ml beaker. Three-hundred ml. of acetone shall beadded and the beaker and contents heated on a steam bath untilall lumps are broken down and all soluble material is dissolved.The mixture shall be poured th
38、rough a small U.S. Standard No. 60sieve. Care shall be taken to wash all the insoluble matter fromthe beaker with acetone. The residue in the sieve shall then bewashed with acetone to remove the RDX. The particles retainedshall be counted. Sieve shall comply with the requirements ofSpecification RR-
39、S-366. The residue from the sieves and thefiltrate may be retained for acetone insoluble and inorganicinsoluble analysis in 4.7.3 and 4.7.4 respectively.4.7.3 Acetone insoluble material. Use the residue andfiltrate from 4.7.2 or weigh an approximate 10 gram portion ofthe dried sample accurately to t
40、he nearest 0.01 gram, place thesample in a 400 ml beaker and add 200 ml of filtered acetone.Place the beaker and contents on a steam bath (cover with a watchglass if necessary) and stir occasionally until all of the RDXhas dissolved. Filter the RDX solution through a 25 ml mediumProvided by IHSNot f
41、or ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-398D13porosity porcelain filtering crucible, which has been ignited at700 + 20 degrees C, and tared to the nearest 0.1 milligram.Transfer any remaining insoluble material from the beaker to thecrucible with the aid
42、 of a stream of acetone from a wash bottle.Wash the material remaining in the crucible three times with 20ml portions of acetone and aspirate until the odor of acetone isno longer noticeable. Dry the crucible in an oven at 105 + 5degrees C for thirty minutes, cool in a desiccator and weigh tothe nea
43、rest 0.1 milligram. Reserve the crucible and contents fordetermination of inorganic insoluble materials given in 4.7.4.Calculate the acetone insoluble material as follows:Percent acetone insoluble material = (A-B) x 100WWhere:A = The final weights of the acetone insoluble materialand the crucible in
44、 grams.B = The tare weight of the crucible in grams.W = The RDX sample weight in grams.4.7.4 Determination of inorganic insoluble material. At atemperature of approximately 700 degrees C., the material in thecrucible obtained as directed in 4.7.2 shall be ignited, cooled,and reweighed. The increase
45、in weight over the original tareweight shall be calculated as percent inorganic insolublematerial.4.7.5 Determination of acidity. A 10 + 0.5 gram portion ofthe sample, weighed accurately to the nearest 0.01 gram, shall betransferred to a 400 ml beaker, 150 ml of acetone added, andheated on a steam b
46、ath until the RDX is completely dissolved.One-hundred ml of distilled water shall be added and the mixturecooled and titrated with 0.05 N. sodium hydroxide usingphenolphthalein or methyl red indicator. A blank shall be runand the results of the titration of the sample corrected foracidity of reagent
47、s. The acidity shall be calculated on a drybasis to percent nitric acid or acetic acid for Types I or II,respectively.CALCULATIONS FOR ACIDITYPercent Nitric Acid = 6.3 (S-B) NWPercent Acetic acid = 6.0 (S-B) NWWhere:S = ml NaOH used in test determinationB = ml NaOH used in blank determinationProvide
48、d by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-398D14N = Normality of NaOH solution used.W = weight of sample, dry basis4.7.6 Determination of granulation. A 50 + 0.05 gram sampleof RDX (dry weight), weighed accurately to the nearest 0.01 gram,shal
49、l be transferred to a 600 ml beaker containing approximately300 ml of a 2 percent solution of a suitable wetting agent suchas dioctyl sodium sulfosuccinate (see 6.5). With the aid of arubber policeman attached to a glass stirring rod, the mixtureshall be stirred for a few minutes wetting the sample thoroughlyand breaking up as many of the aggregates as possible.a. A spray nozzle (
