1、FSC: 6810 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-V-48773 (PA) 2,2 Other publications,-The following documents form a part of this specification to the extent specified herein. Unless other- wise indicated, the issue in effect on date of
2、invitation for bi or request for proposal shall apply. AMERICAN SOCIETY FOR TESTING AND MATERIALS ASTM-El - Wire-Cloth Sieves For Testing Purposes ASTM-E203 - Water, Using Karl Fischer Reagent ASTM-E300 - Sampling Industrial Chemicals I I (Application for copies should be addressed to the American S
3、ociety for Testing and Materials, 1916 R?ce Street, Philadelphia, Pennsylvania 19103) 3. BEQUIREMENTS 3,l Material,-The material shall be vanadium pentoxide (V2O5) 3l,l Form.-The material shall be in the form of yellow-brown conforming to the following requirements: .crystalline powder and shall be
4、free of dirt, chips, grease and other foreign matter when examined as specified in 4.4.3.1. I 3.1.2 X-ray diffraction.-The material shall conform with the I Data File when determined as specified in 4.4.3.2. following chemical properties: Property Requirement Paragraph Moisture Content,%,max 0.10 3.
5、1.3 Chemical Properties.-The material shall conform with the Applicable Basis) 99 090 I Chlorides (as Cl) .Xmax O. 007 4.4.3.4 4.4.3.5 3.1,4 Particle Size.-The particle szie of the material shall conform to the following when determined in accordance with 4.4.3.9. I -I Tyler Mesh Size: 60 100 %, max
6、, Retained on : 0.0 %, min, Retained on : 0.0 0.0 25.0 50.0 I Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-3 -. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-V-q773 b W 999990b OL2L2b 7 I I c
7、 MIL-V-48773 (PA) 4.4.2.1 Sampling.-Approximately 1 pound of V20 shall be withdrawn from each batch to be sampled using ASTM 2 rocedure E300-70 for solids. Samples shall be selected for inspection in accordance with MIL-STD-1235, CSP-1 Plan, Inspection Level LI, AQL 6.5%. If any sample fails to meet
8、 any test requirement the batch represented by the sample shall be rejected. All batches produced between the time 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 4.4.3. any of the test requirements,
9、 that batch shall also, be rejected,. In addition, after any failure of a batch the contractor will return to 100% inspection until llifl successive batches are accepted as required by MTL-STD-1235. The samples shall be subjected to the tests listed below: Inspection/Requirement Defect Classificatio
10、n Form (see 3.L.L) Major B X-ray Diffraction (see 3.1.2) Major B Properties (see 3.1.3) Major B . Mo ist ur e If any of these batches fail to meet Vanadium (as V20 ) iron (as Fe2031 Sodium (as Na201 Silica (as Si021 Chlorides (as C1 7 Particle Size (see 3.1.4) Major B 4,4.2,2 Inspection Equipment.-T
11、he government reserves the right to inspect the contractors equipment and determine that he has available and utilizes correctly, measuring and test equipment of the required accuracy and precision and that; the instruments are of the proper type and range to make measurements of the required accura
12、cy. Commercial inspection equipment, shall be employed where applicalbe for all tests and examinations specified in 4.4.3. The contractor is responsible for assuring proper calibration procedures are followed. Government approval of inspection equipment Is required prior to its use for acceptance pu
13、rpose. 4.4.3 Test methods and procedures.-(see 6.2) The tests in 4.4.3.2 thru 4.4.3.5 shall be performed using prescribed analytical procedures for replicate determinations given in standard analytical textbooks. I 4.4.3.3. Form,-Spread approximately 1/2 pound of the sample on a flat surface and exa
14、mine the material visually for the presence of contamination and form. 4 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-V-48773 (PA) 4.4.3.4.4 Calc
15、ulation d V2O5 = A x B x 2.021 B = Relation factor I Where: A = Ml of ferrous ammonium sulfate. 4.4.3.5 Chlorides.-Determine the chloride content in accordance with a turbidimetric method described in a standard or reference textbook (see 6.4). 4.4.3.6 Iron,-Determine the iron content as follows: 4.
16、4.3.6.1 Solutions: .2% 1.10 Orthophenanthroline Monohydrate 10% Hydroxylamine Hydrochloride 1 Molar Sodium Perchlorate Sodium Sulfate (anhydrous) Nitrobenzene - Purifed Grade Standard Fe solution - 1 ml = 10 micro grams. Dissolve 0.0702 g pure Fe(NH)s(S04)2. 6 H20 in 100 ml of 5% HC1 and dilute to 1
17、000 ml. 4*4.3.6.2 Procedure,-Transfer 0.25Og of the sample into a 100 mL beaker, Add LO ml of HCl and heat slowly until sample is dissolved. Add 10 ml of H20, cool to room temperature, add 20 ml. of hydro- xylamine hydrochloride and continue as in preparation of calibration curve. Since hydroxylamin
18、e hydrochloride forms a strong complex with Vanadium (IV) which at a pH of 4-5 gives a colorless solution, the use of pH paper is not necessary in the pH adjustment of the sample solution. The correct pH is attained by adding ammonia until the solution is just colorless. A blank should be run along
19、with the sample. Care should also be taken in the selection of glassware. It is often wise to set aside glassware and reagents to be used for this determination of iron only. 1, 2, 4. 6, 8 and 10 ml of the standard iron solution to 100 ml beakers., Dilute to 10 mL with water, add 20 ml of hydroxylam
20、ine hydrochloride and let stand for about 8 minutes. Add 1-1 ammonium hydroxide from a burette until a pH of 4-5 is reached. (pH paper can be used). Quantitatively transfer the solution to a 250 ml 4.4.3.6 3 Preparation of Calibration Curve .-Transfer O (Blank), 6 Provided by IHSNot for ResaleNo rep
21、roduction or networking permitted without license from IHS-,-,-MIL-V-48773 68 M 777770b OL2L287 2 W MIL-V-48773 (PA) separatory funnel, add 1 ml of sodium perchlorate, 20 ml of ortho- phenanthroline and shake. Add exactly 30 ml of nitrobenzene and shake vigorously for 30 seconds. Let the phases sepa
22、rate and draw off the nitrobenzene layer into a clean 50 mL beaker containing lg of sodium sulfate. Shake and immediately filter through a small Whatman #54 paper into a photometer cubette. Immediately cap the cubette and read the absorbance on a photometer at 525 mu, using the blank to zero the pho
23、tometer. Proceed as above on all the calibration solutions and plot the readings against micrograms of iron. The V.C.A uses a spec 20 photometer or equivalent. accrdance with an Atomic Absorption method described in a standard or reference textbook. Convert the percent sodium found to Na20. follows
24、: 4.4.3.7 Sodium.-Determine the sodium content in the sample in 4.4.3.8 Silica.-Determine the silica content of the sample as Transfer a 5.00 gram sample into a 600 ml beaker. Add 80 ml of 1-1 H2SO4 and 20 ml HClO4. sample is dissolved then evaporate until dense fumes of perchloric acid escape freel
25、y from the spout of the beaker. Cool, dilute to about 450 ml with water, and filter through a Whatman #40 filter paper containing a small wad of fi1te.r paper. Wash the paper and precipitate alternat.ely with hot 1:4 HC1 and hot water about 6 times. Transfer the paper and precipitate into a platinum
26、 crucible and ignite in an electric muffle furnace, first at low heat and then at a higher temperature to obtain constant weight. Cool, weigh the crucible, then add 1 ml of water, 3 drops of sulfuric acid and 2 ml of hydrofluoric acid. Place the crucible on a hot plate and slowly evaporate to drynes
27、s, then heat in the blast of a burner. Reweigh the crucible, an record the loss in Cover the heat slowly until the . weight . %Si02 = Loss in Weight x 100 4.4.3.9 Particle Size.-Superimpose the sieves of the meshes required in 3.1.4 as defined in ASTM Ell and attach the receiving pan to the bottom.
28、Place 100 grams of the sample in the top sieve, mount the assembly on a shaker and operate the shaker for 5 minutes At the end of 5 minutes weigh the granules retained in each sieve and in the pan and calculate the percentages of each. 5 7 i Provided by IHSNot for ResaleNo reproduction or networking
29、 permitted without license from IHS-,-,-MIL-V-Ll8773 b 977990b 01123290 9 MIL-V- 4 8773 (PA 5. PREPARATION FOR DELIVERY 5.1 Packing 5.l.l Level A and Level C,-Unless otherwise specified, the V2O5 shall be packed in accordance with manufacturers commercial practice to assure acceptance by common carr
30、ier for safe delivery , at first detination for immediate use, 5.2 Marking,-Unless otherwise specified, the shipping containers shall be marked in accordance with MIL-STD-129, and shall include the lot number. 6. NOTES 6.1 Ordering data.-See MIL-A-48078 (PA) 6.2 Prior approval of the Contracting Off
31、icer is required for use of equivalent test methods, A description of the proposed method should be submitted thru the Contracting Officer to: Commander, ATTN: SARPA-&A-A-P, Picatinny Arsenal, Dover, New Jersey 07801. This description should include but not be limited to the procedures used, the acc
32、uracy and precision of the method, test data to demonstrate the accuracy and precision and drawings of any special equipment required. use in lithium batteries is manufactured by Foote Mineral Company, Exton, Pa. 19341. V205 from other sources should be evaluated by Picatinny Arsenal, Dover, New Jer
33、sey 07801 (ATTN: SARPA-&A-A-M) before being approved as an equivalent. City, New York. 6.3 Vanadium Pentoxide which has been found satisfactory for 6.4 Method available from Hellige, Inc, 877 Stewart Ave, Garden Custodian: Project Number: 6810-AA71 Army-PA U. 8. GOVERNMENT PRINTING OFFICE: 1975.&j3-7&/0474 a Preparing Activity: Arw-PA Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-
