ARMY MIL-Z-399 D-1971 ZIRCONIUM (GRANULAR AND POWDERED)《(粒状粉末)锆》.pdf

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1、_ MIL-Z-377D 68 777770b 0113853 7 1 October 1971 SUPERSEDING MIL4-399C i9 February i969 MILITARY SPECIFICATION ZIRCONIUM (GRANULAR AND POMERED) This specification is mandatory for use by all Departments and Agencies of the Department of Defense 1. SCOPE 1.1 Scope. This specification co-vers two type

2、s of zirconiyn for use in the manufacture of ordnance materials. 1.2 Classification. The zirconium shall be of two types as follows: Each type shall have 3 classes as indicated in tables I and II. me I - Granular Type II - Powdered 2. APPLICABLE DOCUEmTS 2.1 The following documents of the issue in e

3、ffect on date of invitation for bids or request for proposal, form a part of this specification to the extent specified herein. SPEC IFICATION .RR-S-366 - Sieve, Test FSC 6810 M THIS DOCUMENT CONTAINS %_7 PAGES. Licensed by Information Handling ServicesMIL-Z-397D 68 W 9979906 011385L1 O W SWDARDS MI

4、LITARY MILSTD.105 - Sampling Procedures and Tables for Inspection by Attributes MILSTIL129 - Marking for Shipment and Storage. MIL-STD-1233 - Procedures for Determining Particle Size, Particle Size Distribution of Packed Density of Powdered Materials (Copies of specifications, standards, drawings, a

5、nd publications re- quired by suppliers in connection with specific procurement functions should be obtained from the procuring 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. Unle

6、ss otherwise indicated, the issue in effect on date of invitation for bids or request for proposal shall apply. AME;RICAN SOCIETY FOR TESTING AND MATERIALS D 1193 - Reagent Water (Application for copies should be addressed to the American Society for Testing and Materials, 1916 Race Street, Philadel

7、phia, Pa., 19103.) (Technical society and technical association specifications and standards 8re generally available for reference from libraries. distributed among technical groups and using Federal agencies. ) They are also DEPARTMENT OF TRANSPORTA TION 49-CFR Transportation Parts 1-199 (These reg

8、ulations may be purchased from the Superintendent of Documents, Government Printing Office, Washington, D. C. 202.) 3.1 Particle size requirements. Type I zirconium shall conform to the particle size requirements specified in table I, and type II zirconium shall conform to the particle size requirem

9、ents specified in table II. The tests for these requirements shall be as specified in k.3.3. 2 Licensed by Information Handling Services_ MIL-Z-377D 68 m 7779706 OLL3855 2 MIGZ-3 99D hable I. Particle size requirements for type I zirconium Sieve class 1 class 2 class 3 Thru No. 20 sieve (840 microns

10、), mru NO. 60 sieve (250 microns), Thru No. 80 sieve (i77 microns), hru NO. i00 sieve (i49 microns) , Thru No. i70 sieve (88 microns), Thru No. 200 sieve (74 microns), Thru No. 325 sieve (Y, microns), percent by weight 99 Qb. percent by weight 5 =. percent by weight 100 percent by weight * i percent

11、 by weight 100 98 min. percent by weight 50 -. 98 min. percent by weight 25 ma. Subsieve J Less than 20 microns, percent by weight Less than 10 microns, percent by weight 10.0 max. 2.0 max. Table II. Particle size requirements for type II zirconium Sieve Class 1 class 2 Class 3 Thru No. i20 sieve (I

12、25 microns), hru NO. 200 sieve (76 microns), Thru Buckbee Mears No. 26 sieve, percent by weight percent by weight (20 microns), percent by weight Subsieve Less then 9 microns, percent 3 microns, percent by weight 0.75 microns, percent by weight by weight 100 100 99.5 min. 99 min. 99 96 min. 96 mui.

13、85 min. 85 Biin. 70-90 7wQ 1230 12-30 Average particle size, microns 2.91.0 2.0 f 0.3 3.0 * 1.0 3.2 Chemical requirements. The zirconium shall conform to the chemical requirements as specified in table III. 3 Licensed by Information Handling ServicesMIL-Z-379D 68 m 797970b OlL385b moo8 ? gooo c ci (

14、r (r I C (r c 0- (r In formula 2, is density of sample at same temperature as Nn“ acceleration ue to gravity = 980 cm/sec2 in formlas I ad 2 Percentage of particles of = fraction pawing No. 325 sieve wt. of withdrawal x 100 wt, of initial withdrawal lC.3.3.2 4.3.3.2.J Sieve sizing. Typ e II airconum

15、 (see 6.9) 4-3.3.2.2 Sieves No. 120 a,n8 200. Weigh 20 gm, or the dry a bred No. 120 sieve. Rest this sikm on a tared No. 200 sieve, ff the Eatter sieve is Co be used (see tab fortype II, weigh 2 gm. of the original dried sample into a watch glass. Add a few ml, of 5 percent sodium pyrophosphate sol

16、iution, paste with a rubber policeman and wash into the sieve with water from a wash bottle. sodium pyrophosphate solution (20 ml. of 5 percent pyrophosphate solution per liter of water) and a camels hair brush. allow the sieve to dry in the air. weighing bottle, dry at 80% (1760) for 1 hour, cool i

17、n.a desiccator, and weigh. Disperse the sample to a smooth Wash the fine particles through the sieve, using dilute Wash with acetone and Transfer the residue to a tared Calculadie the percent of the material passing through the sieve. Licensed by Information Handling ServicesMIL-Z-377D 68 W 7777706

18、OLL3861 8 W 4-3*3.2*4 Subsieve. The particle size distribution of type 11 sir- Conhm Shall be determined by use of the Eagle-Picher mrbidheter (see 6.5). 4.3.3.2.4.1 Preparation of sample. Place approxiniately 0.1 gm. of the powder sample on a clean watch glass and add 5 drops of 0.11 molar aqueous

19、sodium pyrophosphate solution. rubber policeman until thoroughly blended, and all aggregates broken down. Place a 20 micron sieve in a funnel whose stem leads to a 250 ml. graduated cylinder, fitted with a ground glass stopper. Pour a quantity of saturated sodium pyrophosphate solution onto the 20 m

20、icron sieve sufficient to give a total of 2.4 ml. of solution on the watch glass and sieve. Mash the sample carefully from the watch every 0.5 minute for the second and third minutes; every minute up to 20 minutes, and then every 5 minutes until 80 minutes have passed. 4.3.3.2.4.5 Calculation of res

21、ults. Using Keuffeland Esser Ho. 46-100 (old No. 358-81) graph paper, or equivalent, plot the data points. Plot the percent absorption on the linear axis and the time in minutes on the logarithmic axis, points extending the curve at the upper end to the 0.05 minute interval. Draw reference marks on

22、the curves at the time at which the microsizes have fallen past the reading level. The time of fall values are given in table IV for the different size particles. Using projection and work sheets or equivalent, obtainable from the Joplin Printing Company, Joplin, Missouri, Lay out a graph in the rig

23、ht hand section plotting the percent light absorbed values from each particle size from 0.5 to 8.0 microns inclusive. curve #2152-19 or equivalent and project the curve smoothly to the origin, Draw a best fit smooth curve through the data Draw a smooth curve through the points using a Dietzgen In th

24、e first column of the lower left hand corner, record the radius intervals listed in table IV with the smallest radius interval at the top. Record the percent absorption values for the different radius intervals in the next column head PA (prior absorption - the percent ab- sorption prior to the inte

25、rval in question). above 8 microns will be taken from the original plot of R mi. of aagnctnium hydroxide (i to i) to the 175 ml. of solution in the 430 mi. beaker. Digest to 95 OC (203OF) for i5 minutes, filter through a “kshan No. 42 filter paper into a 800 ial. beaker, and wash dkh water. Discard

26、the first 25 mi. of Licensed by Information Handling ServicesAdd 30 mi. of nitric acid to the solution (contained in a 800 ml. beaker) and proceed with the evaporations and development of the color as described under the preparation of calibration curve. of calcium by referring to the calibration cu

27、rve. calcium as follows: Convert the reading to mg. Calculate the percent A Percent calcium = - low where: A - mg. of Ca as read from curve W = gm. of sample in 50 ml. volume on which color measurements are made (ordinarily, W = 1/2 x 0.4 = 0.2 gm.). 4Q3.6 Determination of iron (see 606). 4,3.6.0i S

28、tandard iron solution (1 ml. = 0,100 mg. of Fel, Dissolve 0.1000 gm. of pure iron in 100 ml. of hydrochlaric acid (1 to 1) by warming on the hot plate, cool, and dilute to 1 liter in a volumetric flask. rC.3.6.i.2 Hydroxylamine hydrochloride solution (10 percent) Dissolve 4.3.6.i.3 Tartaric acid sol

29、ution (50 percent),. Dissolve 250 gm, of 50 gm. of hydroxylamine hydrochloride in water and dilute to 500 ml. tartaric acid in water and dilute to 500 ml. I+.3.6.i0L+ Ortho-phenanthroline . Dissolve b gm. of ortho-phenanthroline cool, and dilute to 500 ml. 4.3.6.2 ?reparation of calibration curve. T

30、ransfer 0.5, 1.0, 2.0, 3.0, and 3.5 ml. portions of standard iron solution to 250 ml. beakers. Carry along a reagent blank. Dilute to about 50 ml. with water and add 5 ml. of tartaric acid solution (50 percent), 1 ml. of hydroxylamine hydrochloride solution (10 percent), and 5 ml. of ortho-phenanthr

31、oline solution (0-2 percent). hydroxide (1 to 2) using pH paper. Transfer to 100 mie volumetric flasks and dilute to about 90 d. with water. Heat in a water bath at 60 %o 70C (14Oo to i58OF) for 30 minutes, Measure the absorbence at 5lO nm in a spectrophotometer that has been set to 100 percent tran

32、smittance with the reagent blank. against percent transmittance. Adjust the pH to about 5.5 to 6.0 with ammonium Cool, and dilute to the mark. Plot mg. of iron Licensed by Information Handling ServicesMIL-Z-377D b8 W 777770b 03338b8 O W 4.3.6.3 Procedure. Transfer a 0.5 gm. sample to a platinum dish

33、 and Add 50 mL. of water, warm to dissolve the salts add i5 ml. of water and 7 ml. of sulfuric acid. fluoric acid in 0.5 ml. portions. Evapcrate to strong fumes of sulfuric acid at sioderate heat. if necessary, cool, and dilute to 100 ml. in a volumetric flask. Trans- fer a 20 ml. aliquot to a 250 m

34、l. beaker. (50 percent) and proceed as in the preparation of the calibration curve. Carry along a reagent blank. Convert the reading to mg. of iron by con- sulting the calibration curve. Calculate as follows: Add 2 ml. of hydro- Add 5 mi. of tartaric acid A Percent iron = - f;aining not less than 25

35、 percent by weight of water* 1% must be packed fn wooden boxes, Department of Transportation Specification b5A or 15B, with inside containers of glass or non-carbon polyehylene kving net weight of not over 10 pounds each. In order to prevent free2ing &ring shipment or storage in low temperature clim

36、ates, the zirconium slurry shall contain not less than 25 percent by weight of methyl alcohol-water solution or other anti-freeze mixture approved b the contracting officer, an& which has a freezing point of -30F (-34 C). The zirconium shall be packed for shipment in accordance with the latest Depar

37、tment of Transportation rules Snd regulations for the transpof%ation of hazardous mat erials. B 5.2 Labeling and markinp,. Fach container should be Cfurably and legibly marked to read: (a) Zirconism Mdal Poder (iirini!mm 25 percent *ter). (b) Danger! Flammable solid. May explode if water content is

38、10 perceni m below. (c) Keep et 5n storage - ry poder may be ignited by friction, static exectricity, or heat. (d) Do not attempt to loosen or remove mterial from container with any tool. (e) Keep &way from heat, sparks, and open fleme. (f) Keep from freezing. (g) BI case of spillage, keep wet anci

39、remove carefully. (h) in case of fire, smother with foam-type fire extulguisher or sand. (i) Do not use carbon tetrachloride, CO2 extinguishers or water. (j) Wear goggles or face shield and fire-retardant clothing when handling. in addition to any special marking, marking shall be in accordance with

40、 MILSTII-129. 60 NOTES 6.1 Intended use. The zirconium covered by this specification is intended to be used in pyrotechnic and special ignition compositions. Licensed by Information Handling ServicesMIL-Z-399D 6.2 Orderin,? data. Procurement documents should specify the following: a. b. Title, numbe

41、r and date of this specification Type aiid class of zirconium 6.3 The principle, technique and calculations for the Andreassen pipet method are described by C. Orr and J. M. Dallavalle in “Fine Particle Measurement: Andrsassen Pipets may be purchased from Fisher Scientific Company. Size, Surface and

42、 Pore Volume“, MacKillan Co, New York, 1959, 6.4 Buckbee Mears Sieve. The Buckbee Mears sieve may be ob%ained from the Buckbee Mears Company, St. Paul, Minnesota. 6.5 A booklet en titled ,?Turbidimetric Particle She Analysis“ by Dr. J. R. Musgra:.ie and H. 2. Harrier my be obtained from the agie Pic

43、her Co., P. O. Box 47, Joplin, Mo. 6.6 Alternate methods for calcium, iron, aluminum, silicon, and tin. Calcium, iron, aluminum, silicon, and tin may also be determined by satisfactory spectrographic or atomic absorption methods. 6.7 This is essentially the procedure recommended by ASTM for the dete

44、rmination of hydrogen in zirconium and eirconiwn-base alloys in E 146-6511. 6.S Alternate method for hydrogen. The hydrogen may also be determined by a satisfactory combustion method. 6.9 Zirconium is a hazardous pyrophoric material, particularly when dry. Handle with care avoiding open flames and u

45、nnecessaly friction. Type II zirconium is especially pyrophoric. - Custodians : Navy - OS Air Force - 68 Army - MU Review activities: Navy - OS, AS Air Force - 68 Amy- ND, MU Preparing activity: Project No. 68104904 Amy - MU User activities: Amy - MI, SM 26 Licensed by Information Handling ServicesM

46、IL-Z-377D 68 7777706 OL13B77 5 C-Molybdenum crucible. 8-Fore pump. *Iron guide tube. I-hducthn heating cd. M-McLeod gage. Di-hmefer dinusion pump. &-Evacuation dinuaion pump. FIG. 1.-Hot Extraction Apparatus for O-Quartz furnace tube. P-Mechanical pump for McLeod gage. &-Sample tube. T-Cod trap. TC-Thermocouple gage. V-Small volume. VrLarge volume. Determination of Hydrogen in Zirconium. Licensed by Information Handling Services