1、MIL-DTL-23938B 9999906 205b8U3 921 MIL-DTL-23 93 8B(AS) 28 November 1997 SUPERSEDING 1 September 1966 MIL-F-23 93 8A(AS) DETAIL SPECIFICATION FERRIC OXIDE This specification is approved for use by the Naval Air Systems Command, Department of the Navy and is available for use by all Departments and A
2、gencies of the Department of Defense. 1. 2. 3. SCOPE 1.1 Scope. This specification establishes the requirements for ferric oxide. APPLICABLE DOCUMENTS (This section is not applicable to this specification.) REQUIREMENTS 3.1 First article. When specified (see 6.2), a sample shall be subjected to firs
3、t article inspection in accordance with 4.3. If changes in the process methods and equipment adversely affect the characteristics of the material, additional first article samples may be required. 3.2 Chemical and Dhvsica reauirements. Chemical and physical requirements of the ferric oxide shall be
4、in accordance with table I. 3.3 Workmanship. The ferric oxide shall be free from foreign materials. It shall be manufactured in accordance with standard manufacturing procedures of the industry. Beneficial comments (recommendations, additions, deletions) and any pertinent data which may be of use in
5、 improving this document should be addressed to: Commander, Naval Air Warfue Center Aircraft Division, Code 414100B120-3, Highway 547, Lakehurst, NJ 08733-5100, by using the self- addressed Standardization Document Improvement Proposai (DD Form 1426) appearing at the end of this document or by lette
6、r. AMSC N/A FSC 1336 DISTIUBUTION STATEMENT A. Approved for public release; distribution is unlimited. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,- MIL-DTL-23938B m 9999906 20568VV 868 m I Iron as Fe203 Volatiles HCl solubles Si02 H20 soluble Sie
7、ve analysis - Retained on US standard sieve No. 325 TABLE I. Chemical and physical requirements. 98.70 % - 7 - 0.20% - 0.20% o. 10% 0.20% - 0.20% - - 4. VERIFICATION 4.1 Classification of inspections. The inspection requirements specified herein are classified as follows: a. First article inspection
8、 (see 4.3). b. Conformance inspection (see 4.4). 4.2 Lot size. A lot shall consist of material produced by one manufacturer in one continuous operation employing not more than one lot of each ingredient and with no change in formulation or process. If manufacture is by batch process, batches may be
9、combined to form a lot provided that not more than one lot of each ingredient and no change in formulation or process is used (see 6.2). 4.3 First article inspection. First article inspection shall consist of all the conformance inspections and requirements of this specification, when a first articl
10、e inspection is required (see 3. i). 4.4 Confomance inspection. Conformance inspection sha consist of ail the test methods in 4.5 to determine compliance with section 3. other test methods may be used if they offer assurance of equal results. If test methods differ fiom those specified herein, a cop
11、y of those methods or reference to available source for the methods shall be furnished to the acquiring activity. 4.4.1 Sampling. Sampling for conformance inspections shail be as specified in the contract or purchase order (see 6.2). Ail samples shall be selected at random fiom each lot. There shall
12、 be no defects. 4.5 Test methods. 2 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-23938B m 9999906 2056845 T4 m MIL-DTL-2393 8B(AS) 4.5.1 Determination of iron as Fei0.i. The determination of iron as Fe203 shall be as follows: 4.5.1.1 Prepa
13、ration of reagents. a. 0.1 N Potassium dichromate (K2Cr207) - Weigh out exactly 4.9037 grams of reagent grade or analyzed potassium dichromate. Dilute to 1 liter with distilled water. b. Sulfiinc-phosphoric acid mixture - 150 mL of concentrated sulfuric acid (HzSOd) and 150 mL of concentrated phosph
14、oric acid are mixed together. The mixture of acids is diluted to 1 liter with distilled water. c. Diphenylamine indicator - One gram of diphenylamine is dissolved in 100 mL of concentrated HZSO4. d. Stannous chloride solution (SnC12) - Dissolve 60 grams of SnC12 in 600 mL of concentrated HCl; add 40
15、0 nL of distilled water. e. Saturated mercuric chloride (HgC12) - Place 100 grams of HgC12 in 1 liter of distilled water. Heat to dissolve. 4.5.1.2 Procedure. a. Weigh 0.2 gram to the nearest O. 1 milligram (mg), of sample into a 250 mL beaker. Add 20 mL of concentrated HCl. Heat at 158 “-176 OF (70
16、 “-80 OC) for one hour or until sample is completely dissolved. b. Add stannous chloride (SnCh) solution to the dissolved sample dropwise until the solution is colorless; then add two drops of SnC12 in excess. Cool the solution in an ice bath. c. To e cooled solution, add all at one time, 10 mL of s
17、aturated HgC12; let solution stand for approximately five minutes, then add 15 mL of the sulfuric-phosphoric acid mixture. Dilute the sample solution to 150-200 nL with distilled water. Add three drops of diphenylamine indicator and titrate immediately with the potassium dichromate solution. Near th
18、e end point, the green color changes to a dark blue-green. The dichromate is now added dropwise until the color changes to an intense violet blue. d. Calculations: N (Normality of Potassium Dichromate) O. 1000) (Assay of Dichromate) 1 O0 imL) CI9 ( 7.985) sample weight Percent Fe203 = 3 Provided by
19、IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-239388 M 9999906 2056846 630 M MIL-DTL-23 93 8B(AS) (mL = milliliters of potassium dichromate) 4.5.1.3 Alternate procedure. a. Weigh a 0.5 gram sample to the nearest O. 1 mg in a 250 mL beaker. b. Add 25 mL
20、 of distilled water and 15 mL of concentrated hydrochloric acid. Heat until the sample is completely dissolved. c. Transfer to a 250 mL volumetric flask. Wash the beaker carefully with 5 portions of distilled water. Add the washings to the volumetric flask. Make up to volume with distilled water. d.
21、 Pipette a 25 mL aliquot into a 250 mL beaker. AcidiQ the solution by addition of 5 mL of concentrated HCl. e. Add 30 n with the aid of a glass rod, tear the filter paper. e. Heat to boiling and boil for 5 minutes. Again filter through a No. OOH filter paper or equivalent md wash 5 times with dilute
22、 HC1. f. Transfer the filter paper containing the insoluble residue into a pre-ignited and weighed platinum crucible. Char the filter paper on a Meker burner and place the crucible in an electric mde hace at 1450 *50 OF. Heat for 30 minutes. Cool in a desiccator and weigh. Calculate as follows: perc
23、ent HCl insolubles = B-A x 100 W 5 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,- MIL-DTL-23938B m 7999406 2056848 403 MIL-DTL-23 93 8B(AS) where: A = weight of crucible B = weight of crucible plus residue W = weight of sample 4.5.4- Silica content
24、 determination. The silica content shall be determined as follows: a. Wet the residue from HC1 insolubles with two drops of concentrated sulfuric acid. Add about 15 mL of 48 percent hydrofluoric acid. Caution: Pour the acid directly from the polyethylene bottle and do not measure it in a glass conta
25、iner. If the acid gets on the skin, wash with water and soap to make sure that none of the material remains on the skin surfaces. This acid can cause severe burns. b. Place on a nichrome wire triangle or equivalent and place the triangle on a hot plate. The triangle should be so adjusted that the bo
26、ttom of the crucible is about 1-2 mm fkom the surface of the hot plate. Heat until all of the acid is evaporated and heavy SO3 fbmes are evolved. c. Place on a burner and evaporate the last traces of SO3. Then, place in a muffle furnace at 1450 k50 OF. Heat for 30 minutes. d. Cool in a desiccator an
27、d weigh. e. Calculate as follows: B-A percent Si01 = 7 x 100 where: A = weight of crucible plus residue before HF treatment B = weight of crucible plus residue after HF treatment W = weight of sample 4.5.5 Total water solubles determination. The total water solubles shall be determined as follows: .
28、 a. Transfer about 10 grams of the sample weighed to the nearest O. 1 mg to a 250 mL beaker and add 100 mL distilled water. Bring to a boil and allow to boil for five minutes. Filter while hot using a close grained paper and collect the filtrate in a clean, dry, 250 mL beaker which has been previous
29、ly weighed. b. Wash the residue once using hot distilled water. Place the beaker with the filtrate on a hot plate and evaporate to dryness. The sample may boil while evaporating but not so hard as to aiiow loss by spattering, especially near the end of the evaporation. Ailow to cool and weigh. Calcu
30、late percent water soluble salts. 4.5.6 Sieve analvsis. 6 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-23938B 9999906 2056849 34T MTL-DTL-2393 8B(AS) 4.5.6.1 Procedure. a. Set up the following sieves in order: NQ. 325 Sieve Pan b. Place ap
31、proximately 50.0 gm of the dry sample on the top sieve. c. Shake for 30 minutes. d. Transfer the material on the No. 325 sieve to a weighing container and weigh to the nearest 0.1 gm. e. Calculations: x 100 s retained Sample wt. Percent retained on No. 325 Sieve = 4.5.6.2 Alternate procedure. a. Tho
32、roughly wash and dry a US Stanard No. 325 sieve and set aside for future use. b. Place 10 grams of the sample in a 600 mL beaker. Add enough of Triton 720 or Darvan No. 1 or Naccod to form a heavy paste, and mix well to thoroughly incorporate the sample being tested. c. Dilute the mixture with water
33、 to a volume of approximately 300 mL and pour through the sieve set aside in step a, after the sieve has been weighed to the third decimal place. d. Wash the material on the sieve with a steady, gentle stream of water which has previously been passed through a US Standard No. 325 sieve. Using a smal
34、l camel hair brush, or equivalent, brush the material through the sieve, running the water through at the same time. Continue this operation until no more ferric oxide passes through the sieve. Once or twice during the screening, the sieve may be removed from under the running water and a drop or tw
35、o of the stock dispersing agent solution added, and spread over the sieve with the brush; these personnel need to contact the responsible packaging activity to ascertain requisite packaging requirements. Packaging requirements are maintained by the Inventory Control Points packaging activity within
36、the Military Department or Defense Agency, or within the Military Departments System Command. Packaging data retrieval is available from the managing Military Departments or Defense Agencys automated packaging files, CD-ROM products, or by contacting the responsible packaging activity. 6. NOTES (Thi
37、s section contains information of a general or explanatory nature that may be helpful, but is not mandatory.) 6.1 Intended use. Material purchased in accordance with this specification is intended for use as an ingredient in solid propellant grains. 6.2 Acauisition requirements. Acquisition document
38、s must speci the following: a. b. C. d. e. f g- Title, number and date of this specification. If first article is required (see 3. i). Minimum lot size, if applicable (see 4.2). Conformance sampling (see 4.4. i). Place of inspection. Packaging requirements (see 5. i). Place of delivery. 6.3 Sub-iect
39、 term (key word) listing. Ingredient Propellant grains 6.4 Changes from previous issue. Marginal notations are not used in this revision to identdjr changes with respect to the previous issue due to the extent of the changes. 8 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-23938B 9999906 2056853 TT8 H MIL-DTL-2393 8B(AS) CONCLUDING MATERIAL Preparing activity: (Project 1336-001 9) Navy - AS 9 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-
