1、MIL-STD-1234NOTICE 118 December 1965MILITARY STANDARDPYROTECHNICS: SAMPLING,INSPECTION AND TESTINGTO ALL HOLDERS OF MIL-STD-1234:1. The followinglisted:New Pageiiivv2. The followingRevised Method101.1.1101.2.1101.8.1101.4.1102.1.1102.2.13. The followingMethod No.101.5pages of MIL-STD-1234 have been
2、revisedDate Superseded Page18 December 1965 ii18 December 1965 iv18 December 1965 vand supersede the pagesDate22 June 196222 June 196222 June 1962methods have been revised and supersede the methods listed:Date Superseded Method Date18 December 1965 101.1 22 June 196518 December 1965 101.2 22 June 19
3、6518 December 1965 101.3 22 June 196218 December 1965 101.4 22 June 196218 December 1965 102.1 22 June 196218 December 1965 102.2 22 June 1962method has been added:Title DateMoisture (Kari Fischer Distilation Method) 18 December 19654. Retain this notice and insert before the Table of Contents.FSC 1
4、370 Project No. 1370-0205 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-DEPARTMENT OF DEFENSEWashington 25, D.C.Pyrotechnics: Sampling, Inspection and TestingMIL-STD-12341. This Military Standard has been approved by the Department of Defense and i
5、smandatory for use by all Department and Agencies of the Department of Defense.2. Recommended corrections, additions, or deletions should be addressed to Command-ing Officer, Picatinny Arsenal, Dover, New Jersey 07801, ATTN: SMUPA-DC7.ii Supersedes Page ii of 22 June 1962Provided by IHSNot for Resal
6、eNo reproduction or networking permitted without license from IHS-,-,-MIL-STD-123418 December 1965 ALPHABETICAL INDEX OF TEST METHODSContinuedTitle Method No.Hygroscopicity (Equilibrium Method) . . . . . . . . . . . . . . . . . . . . . . .Impact Sensitivity (U.S. Bureau of Mines Apparatus) . . . . .
7、 . . . . . .76C. International Test . . . . . . . . . . . . . . . . . . . . .Iron (Jones Reductor Method) . . . . . . . . . . . . . . . . . . . . . . . .Leaching . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .Lead Sulfocyanate (Silver Nitrate Method) . . . . . . . . . . . .
8、 . . . . . . . . . . . .Magnesium (Audiometer Method) . . . . . . . . . . . . . . . . . . . . . . . . .Magnesium (Pyropophosphate Method) . . . . . . . . . . . . . . . . . .Methyl Orange Indicator Solution . . . . . . . . . . . . . . . . . . . .Methyl Red Indicator Solution . . . . . . . . . . . . .
9、 . . . . . .Moisture (Desiccation Method) . . . . . . . . . . . . . . . . . . . . . . . . .Moisture (Karl Fischer Extraction Method) . . . . . . . . . . . . . . . . . . . . . . . . .Moisture (Karl Fischer Distillation Method) . . . . . . . . . . . . . . . . . . . . . . . . .Moisture (Karl Fischer Me
10、thod) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .Moisture (Modified Karl Fischer Method) . . . . . . . . . . . . . . . . . . . . . . . . . . . . .Multiple Solvent Extinction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .Nickel (Dimethylglyoxine Method) .
11、. . . . . . . . . . . . . . . . . . . . . . . . . .Nitro-Compounds (Titanous Chloride Method) . . . . . . . . . . . . . . . . . . . . . . . . . .Organic Destruction and Sample Dissolution . . . . . . . . . . . . . . . . . .Perchlorate (Ammonium Chloride Method) . . . . . . . . . . . . . . . . . . .
12、. . . . . . .Phenolphthalein Indicator Solution . . . . . . . . . . . . . . . . . . . . . . . . . . . .Potassium and Barium Salts (Flame Spectrophotometric Method) . . . . . . . . .Potassium Dichromate (0.1N Standard Solution) . . . . . . . . . . . . . . . . . . . . .Potassium Permanganate (0.1N Sta
13、ndard Solution) . . . . . . . . . . . . . . . . . . . . .Potassium (Tetraphenyl Boron Method) . . . . . . . . . . . . . . . . . . . . . . . .Potassium Thiocyanate (0.1N Standard Solution) . . . . . . . . . . . . . . . . . . . . . . .Reactivity Test . . . . . . . . . . . . . . . . . . . . . . . . . .
14、 . . . . . . . . . . . . . . . . . .Selective Solvent Extraction (Extraction Method) . . . . . . . . . . . . . . . . . . . . .Selective Solvent Extraction (Insoluble Residue Method) . . . . . . . . . . . . . . . . . .Selective Solvent Extraction (Leaching) . . . . . . . . . . . . . . . . . . . . . .
15、 . . . . . . . .Selective Solvent Extraction (Soxhlet Method) . . . . . . . . . . . . . . . . . . . . . . . . . .Silver Nitrate (0.1N Standard Solution) . . . . . . . . . . . . . . . . . .Sodium Diphenylbenzidine Sulfonate Indicator Solution . . . . . . . . . . . . . .Sodium Hydroxide (0.1N Standard
16、 Solution) . . . . . . . . . . . . . . . . . .Sodium Oxalate (Potassium Permanganate Method) . . . . . . . . . . . . . . . .Soxhlet Extraction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .Starch Indicator Solution . . . . . . . . . . . . . . . . . . . . . . . . . . . .Strontium Nitra
17、te (Sulfate Method) . . . . . . . . . . . . . . . . . . . . . . . .Sulfur (Carbon Disulfide Insoluble) . . . . . . . . . . . . . . . . . . . .Sulfur (Carbon Disulfide Soluble) . . . . . . . . . . . . . . . . . . . .Titanous Chloride (0.2N Standard Solution) . . . . . . . . . . . . . . . . . . .Titan
18、ium and Titanium Dioxide (Jones Reductor Method) . . . . . . . . . . . . . . .Total Lead (Chromate Method) . . . . . . . . . . . . . . . . . . . . . . . .Total Lead (Sulfate Method) . . . . . . . . . . . . . . . . . . . . . . . . . .100C. Vacuum Stability Test . . . . . . . . . . . . . . . . . . . .
19、 . . . . .Volatiles (Oven Method) . . . . . . . . . . . . . . . . . . . . . . . .Volatiles (Vacuum Method) . . . . . . . . . . . . . . . . . . .Zinc Oxide . . . . . . . . . . . . . . . . . . . . . . . .Zirconium or Zirconium Hydride (Cupferron Method) . . . . . . . . . . . . . . .203.1506.1501.1414.
20、1301.4406.1412.1412.2704.1702.1101.1.1101.4.1101.5101.2.1101.2.1301.7411.1420.1301.5403.1703.1421.1605.1606.1416.1608.1604.1204.2204.4204.1204.9607.1707.1602.1416.1301.6701.1418.1409.1409.2601.1413.1408.1408.2503.1102.1102.2.1419.1416.1ivSupersedes Page iv of 22 June 1962Provided by IHSNot for Resal
21、eNo reproduction or networking permitted without license from IHS-,-,-Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-Method No.101.1.1101.2.1101.3.1101.4.1101.5102.1.1102.2.1201.1202.1203.1204.1204.2204.3204.4301.1301.2301.3301.4301.5301.6301.7401.1
22、402.1403.1404.1405.1406.1406.2407.1407.2408.1408.2409.1409.2410.1411.1412.1412.2419.1414.1415.1416.1417.1418.1419.1420.1421.1MIL-STD-123418 December 1965NUMERICAL INDEX OF TEST METHODSGROUP 100 GENERAL TEST METHODSMoistureMoistureMoistureMoistureMoistureVolatilesVolatiles(Desiccation Method)(Karl Fi
23、scher Method)(Modified Karl Fischer Method)(Karl Fischer Extraction Method)(Karl Fischer Distillation Method)(Oven Method)(Vacuum Oven Method)GROUP 200 PHYSICAL TEST METHODSGranulationAverage Particle Size (Fischer Subsieve Sizer)Hygroscopicity (Equilibrium Method)Selective Solvent Extraction (Leach
24、ing Method)Selective Solvent Extraction (Extraction Method)Selective Solvent Extraction (Soxhlet Method)Selective Solvent Extraction (Insoluble Residue Method)GROUP 300 SAMPLE PREPARATIONSDissolutionDissolution ExtractionExtractionLeachingOrganic Destruction and Sample DissolutionSoxhlet ExtractionM
25、ultiple Solvent ExtractionGROUP 400 CHEMICAL TEST METHODS -Chloride (Silver Nitrate Method)Chlorate (Ferrus Sulfate Method)Perchlorate (Ammonium Chloride Method)Hexachlorobenzene (Parr Bomb Method)Lead Sulfocyanate (Silver Nitrate Method)Barium Salts (Sulfate Method)Barium Salts (Chromate Method)Alu
26、minum (Ammonium Hydroxide Method)Aluminum (8-Hydroxy-quinoline Method)Total Lead (Chromate Method)Total Lead (Sulfate Method)Sulfur (Carbon Disulfate Insoluble)Sulfur (Carbon Disulfide Soluble)Antimony Sulfide (Permanganate Method)Nickel (Dimethylglyoxime Method)Magnesium (Audiometer Method)Magnesiu
27、m (Pyrophosphate Method)Titanium and Titanium Dioxide (Jones Reductor Method)Iron (Jones Reductor Method)Potassium Salts (Tetraphenyl Boron Method)Zirconium or Zirconium Hydride (Cupferron Method)Sodium oxalate (Potassium Permanganate Method)Strontium Nitrate (Sulfate Method)Zinc Oxide (Formic Acid
28、Method) Nitro-Compounds (Titanous Chloride Method)Potassium and Barium Salts (Flame Spectrophotometric Method)vSupersedes Page v of 22 June 1962Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-Provided by IHSNot for ResaleNo reproduction or networking
29、 permitted without license from IHS-,-,-MIL-STD-123418 December 1965MOISTURE1. SCOPEMethod 101.1.1(DESICCATION METHOD)4.1 Place the specimen in the weighingdish and weigh the dish, contents and cover.1.1 This method is used for determiningthe moisture content of pyrotechnic compo- 4.2 Place the dish
30、 with cover removed insitions on a basis of loss of weight in a the desiccator maintained at 25 degrees plusdesiccated atmosphere. This method is used or minus 5 degrees C.on compositions when it is undesirable to Note. Vacuum may be applied to the desiccatoruse heat due to the sensitivity and volat
31、ility to shorten the period of drying. The desiccator isof the material being tested. .2. SPECIMEN2.1 The specimen shall consist of approxi-mately 2 gm of the pyrotechnic weighed towithin 0.2 mg or as the applicable specifica-tion specifies.3. APPARATUS3.1 Weighing dish with tight fitting coverand o
32、f suitable diameter so that the speci-men can be spread out in a thin layer.3.2 Desiccator containing a suitable desic-cant such as anhydrous calcium sulfate, oras specified in applicable specifications,4. PROCEDUREevacuated to a pressure of 380 mm plus or minus20 mm of mercury and maintained at a t
33、emperatureof 25 degrees plus or minus 5 degrees C. Results obtained in this manner are usually reported as loSSon vacuum desiccation, percent.4.3 Weigh the stoppered dish and contentsat intervals until the loss in weight betweenweighings does not exceed 0.5 mg.4.4 Determine the loss in weight and ca
34、l-culate the loss as the percentage moisturein the sample.4.5 CalculationPercent moisture = A100Wwhere:A = loss in weight, gm.W = weight of sample, gm.1 Method 101.1.1Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-Provided by IHSNot for ResaleNo rep
35、roduction or networking permitted without license from IHS-,-,-MIL-STD-123418 December 1965MethodMOISTURE (KARL1. SCOPE1.1 This is a general method for determin-ing the moisture in pyrotechnics which donot react with the Karl Fischer reagent andfrom which the moisture is easily extract-able.Note. Al
36、though the application of the Karl Fischerreagent for determining the moisture content ofpyrotechnics is general in scope, its chemical activi-ty with materials other than moisture imposes cer-tain limitations that must be taken into account bymodification of the method for the purpose of adap-tion
37、to specific applications. Detailed specificationsshould be consulted for adaptations to materials thatrequire modifications of the procedure listed herein.2. SPECIMEN2.1 The specimen shall consist of approxi-mately 8 to 10 gm of the pyrotechnic.Note. The specimen shall contain not more than0.01 gm o
38、f water, The specimen weight should beadjusted after a preliminary determination, so thatthe water will not exceed 0.01 gm.3. APPARATUSThe arrangement now used at PicatinnyArsenal will be described although numerousmodifications, which give equally satisfac-tory results, may be used. There are alsoa
39、vailable automatic titrimeters and aqua-meters especially designed for use with theKarl Fischer dead-spot end point method,which are compact and satisfactory.3.1 Titration assembly consisting essen-tially of:(a) Burets, automatic, Machlett auto-buret, 50 ml capacity, 2 required,one left and one righ
40、t.(b) Titrator stand.(c) Magnetic stirrer with Teflon coatedstirring bar.101.2.1FISCHER METHOD)3.2 Titration flask (fig. 2) consistingessentially of:(a) Beaker, Berzelius, 200 or 300 mlwithout spout, at least 4 re-quired.(b) Rubber stopper to fit beaker, pre-pared as shown in (fig. 3).(c) Glass stop
41、per for sample portholeof rubber stopper (fig. 3).(d) Iron ring support (fig. 2).(e) Drying tube, calcium chloride, 3required.(f) Weighing bottles with cap-styleground covers, 2 required.3.3 Direct dead-stop circuit assembly (fig.1) consisting essentially of:(a)(b)(c)(d)Dry cell battery, 1.5 volts.R
42、heostat, 250,000 ohms.Micro-ammeter, Weston Model 440,resistance 164 ohms, or equal.Platinum electrodes, 2 required.3.4 Over3.5 Assemble the apparatus as follows:(a) Attach each buret to the titratorstand.(b) Clamp the iron ring support to thetitrator stand so that it holds therubber stopper firmly
43、in place,allowingthrough(see fig.(c) Pass theholes inconnectcircuitthe buret tips to passthe designated holes3) in the stopper.electrodes through thethe rubber stopper andthem to the dead stopwith electrical wire asshown in (fig. 1).Method 101.2.11Provided by IHSNot for ResaleNo reproduction or netw
44、orking permitted without license from IHS-,-,-MlL-STD-123418 December 1965(d) Insert a drying tube in the hole inthe robber stopper and attachthe other two drying tubes to thevents of the burets.(e) Place the glass stopper in the sam-ple port hole.(f) Place the magnetic stirrer so thatwhen the rubbe
45、r stopper is firm-ly fitted in the mouth of thetitration beaker, the beaker willrest on the magnetic stirrer.(g) Place the required number of beak-ers in the oven maintained at 100degrees plus or minus 2 degreesC. to dry.(h) Fill the reservoirs of the buretswith the required reagents.4. MATERIALS4.1
46、 Karl Fischer reagent, stabilized singlesolution, placed in the reservoir of a buret.4.2 Standard water-in-methanol, 1 mg ofwater per 1 ml of solution, placed in thereservoir of the buret.Note. The Karl Fischer reagent and standardwater-in-methanol solution are commercially avail-able as standard st
47、ock items. If it is desirous toprepare the reagents, their preparation can be foundin Mitchell, John Jr. and Smith, Donald Milton,“Aquametry”, Interscience Publishers, inc., NewYork, 1948, Chapter IV and ASTM Method E203-62T.4.3 Sodium tartrate dihydrate, primarystandard for Karl Fischer reagents co
48、ntain-ing 15.66 plus or minus 0.05 wt percentwater.4.4 Special solvent as indicated in the applicable pyrotechnic specification.Note. The special solvent or advents employed foreach material will vary depending on the natureof the ingredients. Some of the solvents commonlyemployed are methanol ethan
49、ol, dioxane, acetic acid,dimethyl formamide and pyridine: methanol (1 vol:3 Vol.).Method 101.2.15. PROCEDURE5.1 Reach a preliminary end point asfollows :(a) Dry thetainedminus(b) Removebeakers in an oven main-at 100 degrees plus or5 degrees C.one of the dried beakersand attach it, while still hot,firmly to the rubber stoppe
