ARMY MIL-DTL-244 B-1996 NITROCELLULOSE《硝化棉》.pdf

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1、 INCH-POUNDMIL-DTL-244B12 November 1996SUPERSEDINGMIL-N-244A13 February 1962DETAIL SPECIFICATIONNITROCELLULOSEThis specification is approved for use by all Departments andAgencies of the Department of Defense.1. SCOPE1.1 Scope. This specification covers the requirements,examinations and tests for fi

2、ve grades, four types, and twoclasses of nitrocellulose for use in propellant.1.2 Classification. Nitrocellulose is classified into thefollowing grades, types, and classes.Grade A - PyrocelluloseType I Nitrogen Content 12.6 + 0.10%Type II Nitrogen Content 12.6 + 0.15%Grade B - Guncotton Nitrogen Con

3、tent 13.35% minimumGrade C - Blend of Pyrocellulose and GuncottonType I - Nitrogen Content 13.15 + 0.05%Type II - Nitrogen Content 13.25 + 0.05%Grade D - Nitrogen Content 12.20 + 0.10%Grade E - Nitrogen Content 12.00 + 0.10%Beneficial comments (recommendations, additions, deletions) and anypertinent

4、 data which may be of use in improving this document, should beaddressed to: Commander, U.S. 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 137

5、5DISTRIBUTION STATEMENT A. Approved for public release;distribution is unlimited.Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-244BClasses 1 and 2 - Each of these grades and types ofnitrocellulose will be produced as either Class 1 or Class

6、 2depending on its specific applications (see 3.2 and 6.1).2. APPLICABLE DOCUMENTS2.1 General. The documents listed in this section areneeded to meet the requirements specified in sections 3, 4, and 5of this specification. This section does not include documentsin other sections of this specificatio

7、n or recommended foradditional information or as examples. While every effort hasbeen made to ensure the completeness of this list, document usersare cautioned that they must meet all requirements documentscited in sections 3, 4, and 5 of this specification, whether ornot they are listed.2.2 Governm

8、ent documents.2.2.1 Specifications, standards and handbooks. Thefollowing specifications, standards and handbooks form a part ofthis document to the extent specified herein. Unless otherwisespecified, the issues of these documents are those listed in theissue of the Department of Defense Index of Sp

9、ecifications andStandards (DODISS) and supplemented thereto, cited in thesolicitation. (see 6.2)SPECIFICATIONS (see 6.2)RR-S-366 - Sieve, TestDEPARTMENT OF DEFENSEMIL-C-206 - Cellulose (Cotton)MIL-C-216 - Cellulose, Woodpulp, SulfiteMIL-E-463 - Ethyl Alcohol (For Ordnance Use)MIL-C-20330 - Cellulose

10、, Woodpulp (Sulfate)STANDARDSDEPARTMENT OF DEFENSEMIL-STD-129 - Marking for Shipment and Storage.2Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-244B3MIL-STD-286 - Propellants: Sampling, Inspection andTesting.(Unless otherwise indicated, cop

11、ies of above specifications,standards, and handbooks are available from the DOD SingleStockage Point (DODSSP), Standardization Document Order Desk, 700Robbins Avenue, BLDG 4D, Philadelphia, PA 19111-5094.)2.3 Non-Government publications. The following document(s)form a part of this document to the e

12、xtent specified herein.Unless otherwise specified, the issues of the documents which areDoD adopted are those listed in the issue of the DODISS cited inthe solicitation. Unless otherwise specified, the issues ofdocuments not listed in the DODISS are the issues of thedocuments cited in the solicitati

13、on (see 6.2).AMERICAN SOCIETY FOR QUALITY CONTROLANSI/ISO/ASQC A8402-1994 Quality Management and QualityAssurance Vocabulary(Application for copies should be addressed to American Societyfor Quality Control, 611 East Wisconsin Ave, Milwaukee,Wisconsin)2.4 Order of precedence. In the event of a confl

14、ictbetween the text of this document and the references citedherein, the text of this document takes precedence. Nothing inthis document, however, supersedes applicable laws andregulations unless a specific exemption has been obtained. (Seecontract provisions for additional precedence criteria).3. R

15、EQUIREMENTS3.1 First article. When specified in the contract orpurchase order (see 6.2 ), a sample shall be subjected to firstarticle inspection in accordance with the technical provisionsherein (see 4.3).3.2 Material. The material requirements and test methodsfor specific classes (applications) of

16、nitrocellulose shall be inaccordance with Table I below:Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-244B4Table IRequirements and test methods for classes 1 and 2 applicationsClasses Applications Requirements ApplicableParagraphs Test Meth

17、odParagraphs1 For combustible 3.1 to 3.11 4.5.1 to 4.5.12cartridge inclusive inclusiveapplications2 For all other 3.1, 3.2, 3.3, 4.5.1 to 4.5.9applications 3.4, 3.5, 3.6, inclusive3.7, 3.8, 3.93.113.2.1 Water. The water used at all stages in themanufacturing process shall be clean and free from susp

18、endedmatter or sediment.3.2.2 Alcohol. The alcohol used in the manufacture ofnitrocellulose shall conform to the requirements for Grade 2 ofSpecification MIL-E-463.3.2.3 Cellulose. The cellulose used shall be derived fromcotton cellulose, woodpulp cellulose obtained by the sulfateprocess or woodpulp

19、 cellulose obtained by the sulfite process,fabricated in sheeted or baled form, conforming to the chemicaland physical requirements of Specifications MIL-C-206, MIL-C-20330, or MIL-C-216 respectively except that sheeted or baledmaterial is acceptable.3.3 Chemical properties. The chemical properties

20、shall beas specified in Table II for all classes of nitrocellulose whendetermined in accordance with the applicable subparagraphs of 4.4and 4.5. Blending may be used to achieve the applicablerequirements for each particular grade as specified in Table II.Provided by IHSNot for ResaleNo reproduction

21、or networking permitted without license from IHS-,-,-MIL-DTL-244B5Table II Chemical propertiesEther Acetone Seealcohol insoluble Ash FootGrade/Type Nitrogen solubility maximum Max notecontent %, (Min.) %, (Max.)A I 12.6 + 0.10 99 0.4 0.4 1II 12.6 + 0.15 99 0.4 0.4 1B 13.35 min. 0.4 0.4C I 13.15 + 0.

22、05 0.4 0.4 2II 13.25 + 0.05 0.4 0.4 2D 12.20 + 0.10 99 0.4 0.4 3E 12.00 + 0.10 99 0.4 0.4 4Footnotes:1- The required nitrogen content may be obtained byblending nitrocellulose containing from 12.45 to 12.75 percentnitrogen.2. - The limits for solubility of Grade C nitrocellulosein ether-alcohol shal

23、l be left to the discretion of themanufacturer using the nitrocellulose in the production ofpropellants. However, when nitrocellulose is purchased and usedby a different plant from that producing it, detailedrequirements for solubility shall be as specified in the contractor order (see 6.2g).3.- The

24、 required nitrogen content may be obtained byblending nitrocellulose containing from 12.05 to 12.35 percentnitrogen.4. - The required nitrogen content may be obtained byblending nitrocellulose containing from 11.90 to 12.20 percentnitrogen.3.4 Viscosity. Detailed requirements for viscosity shallbe a

25、s specified in the contract or order (see 6.2h), when testedas specified in 4.5.5.3.5 Deterioration in storage. Nitrocellulose of Grade A(Types I and II), Grade B, Grade C (Types I and II), Grade D, orGrade E for all Classes which has been stored prior to its use inthe manufacture of propellant shal

26、l, within a period of 2 weeksprior to its use, conform to the requirements specified in 3.8.3.6 Fineness. Detailed requirements for fineness shall beas specified in the contract or order (see 6.2i), when tested asProvided by IHSNot for ResaleNo reproduction or networking permitted without license fr

27、om IHS-,-,-MIL-DTL-244B6specified in 4.5.6.3.7 134.5 degree Centigrade (C.)heat test. Nitrocelluloseshall meet a minimum heat test period of 30 minutes, when testedas specified in 4.5.7.3.8 65.5 degree Centigrade (C.) heat test. When specifiedby the procuring officer, heat test shall be conducted wi

28、thpotassium iodine (KI) starch paper. Nitrocellulose shall meet aminimum KI test period of 35 minutes, when tested as specified in4.5.8.3.9 Manufacturing procedure. The following proceduresshall be used for the manufacture of nitrocellulose:3.9.1 Drying. Cotton cellulose conforming to therequirement

29、s of Specification MIL-C-206 may be dried beforenitration when producing Grades A, B, and C nitrocellulose, andwhen producing Grades D and E nitrocellulose in a continuousprocess. Cotton cellulose conforming to the requirements ofSpecification MIL-C-206 shall be dried before nitration whenproducing

30、Grades D and E nitrocellulose in a batch nitrationprocess. The drying temperature at no time shall exceed 110degrees C. Wood sulfate cellulose conforming to the requirementsof Specification MIL-C-20330 and wood sulfite celluloseconforming to the requirements of Specification MIL-C-216 may besubjecte

31、d to rapid drying in a continuous sheet at a temperaturepreferably not higher than 165 degrees C., and shall not behigher than 175 degree C. The time of exposure to temperatureabove 165 degree C. shall in no event exceed 15 minutes.3.9.2 Preliminary boiling. The nitrocellulose shall beboiled in tubs

32、 so constructed that the nitrocellulose shall notcome into direct contact with the heating coils or with the livesteam from the coils. The nitrocellulose shall be entirelycovered with boiling water. During the process, the temperatureshall at all times be kept as close to 100 degrees C as possible.W

33、here barometric conditions reduce the boiling temperature, thetemperature required is the highest that can be attained.Irrespective of the boiling points of water in the particularlocality, the temperature at no point in the tub shall be lessthan 95 degrees C. No alkali shall be used in this prelimi

34、naryboiling. The treatment shall be so arranged with regard to thetype of water used, that the first boil shall be with adistinctly acid water, not less than 0.05 percent acidity andpreferably within the limits of 0.05 to 0.50 percent aciditycalculated as sulfuric acid and tested for acidity atappro

35、ximately 2 hours after commencement of boiling treatmentsand at intervals during the first boil.3.9.2.1 For Grades A, D and E nitrocellulose. For Grade Anitrocellulose, the preliminary boiling treatment shall be notless than 20 hours, followed by two 5-hour boils with a change ofwater after each boi

36、l. For Grades D and E nitrocellulose, theProvided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-244B7preliminary boiling treatment shall be not less than 15 hours,followed by two 5-hour boils with a change of water after eachboil.3.9.2.2 For Grade B

37、 nitrocellulose. For Grade Bnitrocellulose, the first boil of the preliminary boilingtreatment shall be not less than 40 hours, followed by two 5-hourboils with a change of water after each boil.3.9.3 Pulping. The nitrocellulose shall then be pulped inwater to which may be added just enough sodium c

38、arbonate solutionto preserve a slight alkaline reaction to phenolphthalein. Theaddition of sodium carbonate in dry form instead of solution isallowed. The pulping process shall be continued until thenitrocellulose is thoroughly and evenly pulped to a satisfactorydegree of fineness. During this proce

39、ss, the water shall bechanged to the extent which may be necessary to removeimpurities.3.9.4 Poaching. After pulping, the nitrocellulose shall berun to the poachers, settled, decanted, and washed if necessary.The nitrocellulose shall then be boiled for 4 hours in freshwater, and during this time a t

40、otal of not more than 10 gallonsof sodium carbonate solution for each 2,000 pounds of drynitrocellulose may be added at intervals. The solution shallcontain one pound of sodium carbonate per gallon. The additionof sodium carbonate in dry form instead of solution form isallowed. During this and all o

41、ther boiling treatments in thepoachers, the pulp shall be thoroughly agitated by mechanicalstirrers with sufficient water added to mix thoroughly all pulpin the poacher. The water shall be boiled by injecting livesteam into it in such a manner that the temperature at no pointin the tub will be less

42、than 95 degrees C. (without correctionfor boiling water). After each boiling treatment, sufficientwater shall be added to replace that lost by evaporation and thecontents of the tub agitated. The nitrocellulose shall beallowed to settle and the clear water decanted as completely aspossible so that a

43、t least 30 percent of the contents of the tubshall be drawn off. The tub shall then be filled with freshwater, boiled 2 hours, settled, decanted and refilled with freshwater. The boiling shall then be continued for 1 hour and thisprocess repeated, making a total boiling treatment in the poacheras fo

44、llows:4 hours boiling, with or without sodium carbonate2 hours boiling, without sodium carbonate1 hour boiling, without sodium carbonate1 hour boiling, without sodium carbonateEach boiling shall be followed by settling and change of water.However the settling and change of water after the final 1 ho

45、urboiling, without sodium carbonate, may be omitted in plants usingProvided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-244B8a filter method of washing as described in 3.9.5, when approvedby the contracting agency.3.9.5 Washing. After poaching, th

46、e nitrocellulose shallhave a sufficient number of cold water washings (not less than 2)to insure its conformance with the requirements of thisspecification. Each washing shall consist of agitation bymechanical means for 1/2 hour in a sufficient amount of freshwater, with thorough settling and decant

47、ation of the clear water.In decanting, at least 30 percent of the total contents of thetub shall be drawn off. Any other practical method of washingwhich removes an equivalent amount of impurities, such asdisplacement washing by means of a filter, may be employed,provided that the details of the pro

48、cess are submitted to andapproved by the contracting agency.3.9.6 Screening. Nitrocellulose shall be screened toremove fibers not properly pulped. The width of the slots shallnot be greater than 0.022 inch. Only the material which passesthrough the screen shall be offered in the finished lot.3.9.7 Complete process. Written details of the completemanufacturing process (including the boiling schedules forindividual products), and the equipment used by the contractorshall be submitted to the contracting agency. Written approvalshall be received from the contracting