1、i rBeneficial comments (recommendations, additions, deletions) and 1 any pertinent data which may be of use in improving this document s hou1 d be addressed to : Comnandi ng Off i Cer , Naval Ai r Engi neeri ng Center, Engineering Specifications and Standards Department (ESSD) Code 93, Lakehurst, N3
2、 08733, by using the self-addressed Stan- dardization Document Improvement Proposal (DD Form 1426) appearing at the end of this document or by letter. MIL-C-85q93 68 997990b 032363LI 8 MI LI TARY SPEC I F I CATI ON CATALYST , BURN-RATE 2, 2- BIS (ETHYLFERROCENYL) PROPANE MIL-C-85493(AS) 6 October 19
3、81 1-1 - f5-2 I This specification is approved for use by the Naval Air Systems Command, Department of the Navy, and is airailable for use by all Departments and Agencies of the Department of Defense. 1. SCOPE. 1.1 Scope. This specification establishes the requirements for a burn-rate catalyst for u
4、se in the manufacture of solid rocket propel- lant, referred to herein as the catalyst. 2. APPLICABLE DOCUMENTS. 2.1 Issues of documents. The following documents of the issue in effect on date of invitation for bids or request for proposal, form a part of this specification to the extent specified h
5、erein. SPECIFICATIONS FEDERAL BB-N-411 Ni trogen , Techni cal . MI L ITARY 14 I L -A- 1 84 5 5 Argon, Technical. STANDARDS MILITARY THIS DOCUMEN CQNTAPMS /s PAGES. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-C-5473 b m 9777706 OL23b15 T m MIL
6、-C-85493( AS) 2.2 Other publications. The following document forms a part of this specification to the extent specified herein. Unless otherwise indicated the issue in effect on date of invitation for bids or request for proposal shall apply. STANDARDS American Society for Testing and Materials (AST
7、M) ASTM D-445 Kinematic Viscosity of Transparent and Opaque Ltquids (and the Calcu- lation of Dynamic Viscosity), Test For. Applications for copies should be addressed to the American Society for Testing and Materials, 1916 Race Street, Philadelphia, PA 19103.) 3. REQUIREMENTS. 3.1 Chemical and phys
8、ical properties. Chemical and physical prop- erties of the catalyst shall conform to Table I. TABLE I. Chemical and physical properties. Property Viscosity at 25“C, centistokes Iron content, percent Moisture, percent Ac i di ty , mi 1 1 i equi val ents/gram Insolubility, percent Evaporation 1 oss, p
9、ercent Assay by titration) , percent Min 23.3 97.5 Max 2 , 200 24.3 0.10 0.025 o. 1 4.0 - Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MI L- C-85493 (AS ) Number of containers (primary sample) 10% (nearest sampled who1 e number) 10 10 ALL 3.2 Stab
10、ility. When packaged in accordance with 5.1.1 and stored at 27 211 degrees Celsius (OC), the catalyst shall have a storage life of 12 months from date of delivery to the procuring activity. The shelf life may be extended for 6-month intervals after reacceptance testing for conformance to vi scosi ty
11、 and moisture 1 imi ts, Number of composi - e samples 5 4 3 2 3.3 Toxic products and safety. Safety regulations and guidelines applicable to the use of the catalyst should be complied with to pre- clude personal injury and damage ti equipment and facilities. uniform in appearance and free from visib
12、le contamination. 3.4 Workmanship. Workmanship shall be such that the catalyst is 4. QUALITY ASSURANCE PROVISIONS. 4.1 Responsibility for inspection. Unless otherwise specified in the contract or purchase order (see 6.2.1), the contractor is responsible for the performance of all inspection requirem
13、ents as specified herein. Except as otherwise specified in the contract or purchase order, the contractor may use his own or any other facilities suitable for the performance of the inspection requirements specified herein, unless disapproved by the Government. The Government reserves the right to p
14、erform any of the inspections set forth in this specification where such inspections are deemed necessary to assure that supplies and services conform to prescribed requirements (see 6.2). 4.2 Sampling. The lot shall be sampled in accordance with Table II. TABLE II. Sampling plan. in lot 100 or more
15、 51 - 99 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-C-85493 68 m 9999906 0123617 3 m I 4.2.1 Primar sam les. Physical properties tests shall be run on each primary -Y+- sample see Table II). The material container may be sampled by use of a
16、clean glass tube, rod, or pipet. is small enough to be handled safely, the sample may be obtained by pouring. The smallest sample size possible that is consistent with test requirements shall be taken. The minimum sample size shall be two ounces. Glass containers shall be used for all liquid samples
17、. Each sample shall be labeled with date, lot number, and manufacturers container identification number. all of the physical-properties tests herein shall result in rejection of the lot represented. If the container Failure of any primary sample to pass 4.2.2 Composite samples. Chemical properties t
18、ests shall be run on each composite sample. number of composites shown in Table II. by manipulation of the container. Label each composite with Roman numerals, also include date, lot numbers, and manufacturers container identification numbers. The remainder of the primary samples shall be retained p
19、ending acceptance or rejection of the lot. Failure of any composite sample to pass all of the chemical-properties tests herein shall result in rejection of the lot represented. Divide the primary samples equally into the Blend each composite thoroughly 4.3 Quality conformance inspections. Quality co
20、nformance tests and inspectiwinq for each lot of catalyst material (see 6.3.1): - - a. Tests of Table I properties (see 4.4). b. Inspection of filled containers (see 4.6.1). c. Visual inspection (see 4.6.2). 4.4 Test methods. Tests shall be performed using apparatus, reagents, and procedures specifi
21、ed herein. or procedures shall require prior written approval of the procuring activity. The use of alternate apparatus, reaynts, Al1 American Chemical Society (ACS) reagents shall conform to MIL-STD-1218. 4.4.1 Viscosity. 4.4.1.1 Apparatus. a. Cannon-Fenske viscometer as specified by ASTM D 445, or
22、 equal. b. Water bath with thermostatic control to +0.05“C in the range from 20 to 50C. 4 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-FI MIL-C-85473 b8 W 77777Ob OL23bL 5 W I MI L- C-854 93 (AS ) 4.4.1.2 Reagents. a. Standard viscosity oil, type
23、as specified by ASTM D 445, or equal. 4.4.1.3 Determination of iriscosity. Position the appropriate visco- meter in a 25C constant temperature water bath. section to vertical, Using a pipet or syringe, place 7 to 8 milliliters (ml of sample in the viscometer reservoir, Allow the tube to remain in th
24、e constant temperature water bath for 15 minutes. to adjust the head level of the sample to approximately 5 millimeters (mm) above the upper timing line. Release the vacuum and measure the time required for the meniscus to pass from the first to the second timing mark. Calculate the average of at le
25、ast two readings on the sample in the tube. Align the measuring Use a rubber bulb Cal cul at ion : Viscosity, 25“C, centistokes = T x C -. Where: T = average efflux time, seconds . C =calibration constant provided with the instrument or obtained with standard oil at 25C Report the viscosity to the n
26、earest one centistoke. 4.4.2 Iron content. 4.4.2.1 Apparatus. a. Funnel with Tygon, or equal, tubing connected to water aspirator. b. Meeker burner, or equal. 4.4,Z.Z Reagents. a. Hydrochloric acid, concentrated, ACS reagent. b. Nitric acid, concentrated, ASC reagent. c. Sulfuric acid, concentrated,
27、 ACS reagent. d. Perchloric acid, 70 percent, ACS reagent. e. Stannous chloride solution, 5 percent (25 grams (gm)/500 ml of 10 percent hydrochloric acid plus a few granules of tin). f. Mercuric chlorfde solution, saturated. / -. f- t, i Provided by IHSNot for ResaleNo reproduction or networking per
28、mitted without license from IHS-,-,- 7 MIL-C-5473 b = 7999706 0123617 7 MIL-C-85493( AS) g. h. i. Potassium dichromate, primary standard, 0.1 Normal (N). Phosphoric acid, 85 percent, ACS reagent. Sodium diphenylamine sulfonate indicator solution, 0.4 percent. 4.4.2.3 Determination of iron content, A
29、ccurately weigh 0.50 gram of sample into a 250-ml Erlenmeyer flask. Add 10 mi of distilled water and 15 ml of concentrated nitric-acid. CAUTION Add water prior to acid or sample ignition will occur, Swirl to complete dissolution. while adding 5 ml of concentrated sulfuric acid. 70 percent perchloric
30、 acid and several boiling beads. over the flask and connect the funnel to a water aspirator with Tygon, or equal, tubing. Heat the sample slowly over a burner and increase the heat to digest at dense white fumes for 2 to 3 minutes. concentrated nitric acid and five drops of perchloric acid and heat
31、to fumes again. Cool to safe temperature, add 25 nl of distilled water and reheat until precipitate is completely dissolved. While solution is hot, add 10 ml of concentrated hydrocholoric acid and then 5 percent stannous chloride solution, dropwise, until one drop changes the color no more. (The sol
32、ution may be light pale yellow or colorless.) Add one to two drops in excess. solution, add (at one time) 10 ml of saturated mercuric chloride so- lution and let stand 10 minutes. Add 5 ml of 85 percent phosphoric acid, 100 ml of distilled water, three drops of sodium diphenylamine sulfonate indicat
33、or solution, and titrate with standard 0.1 N potassium dichromate solution to a violet end point. Swirl contents carefully and constantly Add 1 ml of concentrated, Invert funnel Add 1 ml of Fume for 3 to 5 minutes. While stirring the Calculation: V x N x 5.585 Iron, percent = W Where: V = volume of
34、standard potass-ium dichromate, ml N = normality of standard potassium dichromate W = weight of sample, gm Report the iron content to the nearest 0.1 percent. 4.4.3 Moisture. 4.4.3.1 Apparatus. a. Beckman “Aquameter“, Model KF-4, or equal. Provided by IHSNot for ResaleNo reproduction or networking p
35、ermitted without license from IHS-,-,-MI L-C-85493 (AS) 4.4.3.2 Reagents. a. Karl Fi-scher (KF) reagent, comercial strength. b. KF reagent, stabilized, water equivalent of 2.0 to 3.0 mi 11 i grams/mi 11 i 1 i ter (mg/ml ) . c. Pyridine-chloroform, ACS reagent, 1 :1 by volume. 4.4.3.3 Determination o
36、f moisture. Add 10 gm of sample to a reaction beaker containing 60 ml of neutral p-yridine-chloroform solution. The stirrer should b off while adding the sample. the same position used for neutralization. pressing the titrate button to a 30-second end point. Turn on the stirrer to Titrate automatica
37、lly, by Ca 1 c u1 at i on : Moisture, percent = VxE Where: Y = volume of standard KF reagent, ml E = water equivalent of KF reagent, mg/ml i4 = weight of sample, gm Report the moisture to the nearest 0.01 percent. 4.4.4 Acidity. 4.4.4.1 Apparatus. a. pH indicator, Leeds and Northrup, number 7664 equ
38、ipped with glass electrode standard 1199-30 and calomel electrode standard 11 99-31, or equal. b. Magnetic stirrer, variable speed, with Teflon coated stirring bar, or equal. 4.4.4.2 Reagent s. a. Methanol , ACS. b. Standard sodium hydroxide solution, 0.1 N. 4.4.4.3 Determination of acidity. Accurat
39、ely weigh 2,5 gm of samDle into a 250-ml beaker. Add 50 ml of methanol , 50 ml of distilled water, and stir to disperse. Titrate potentiometrically with standard 0.1 N sodium hydroxide solution. Determine a reagent blank in like manner. Determine the end point graphically by plotting the volume of t
40、itrant versus millfvolts, taking the midpoint of the straight section of the curve as the end point. 7 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-I ,I_ MIL-C-85493 68 = 9999906 012362L 5 MI L-C-85493 (AS) Calcul ation: V - B) N. W Acidity, milli
41、equivalents/gram of sample = Where: V = volume of standard sodium hydroxide for sample, ml B = volume of standard sodium hydroxide for blank, ml N normality of standard sodium hydroxide W = weight of sample, gm Report acidity to the nearest 0.001 milliequivalents per gram sampl e. 4.4.5 Insolubility
42、. 4.4.5.1 Apparatus. Filter paper, Whatman number 1, or equal. 4.4.5.2 Reagents. Chloroform, ACS reagent. 4.4.5.3 Determination of insolubility. Accurately weigh 10 gm of sample into a 250-ml beaker and dissolve in 100 ml of chloroform. Filter the dissolved sample through an accurately weighed numbe
43、r 1 Whatman filter paper, or equal. to remove any soluble sample. oven for 1 hour, cool in a desiccator, and reweigh. Wash paper and contents with chloroform Dry filter paper and contents in a 105C Cal cul ation: A - B) 100 W Insoluble material, percent = ( Where: A = weight of filter paper and resi
44、due, gm B = weight of filter paper, gm W = weight of sample, gm Report the insoluble material to the nearest 0.1 percent. 4.4.6 Evaporation loss. 4.4.6.1 Apparatus. 8 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MI 14-85493 (,AS) a. Aluminum weigh
45、ing pans, disposable, b. Vacuum oyen. 4.4.6.2 Determination of evaporation, Accurately weigh 10 gm of sample into a disposable aluminum pan and place in a vacuum oven at 80C and 15 mm mercury for 22 hours. Remove from oven, cool i.n a desiccator, and reweigh. Cal cul ation: Evaporation loss, percent
46、 = (W - A) 100 W Mhere: A = weight of sample after heating, gm W = weight of sample before heating, gm Report the evaporation loss to the nearest 0.1 percent. 4.4.7 Assay. 4.4.7.1 Apparatus. a. b. C. d. e. Titrator, Flethrohm E-436 or E-536, or equal, with combination platinum electrodes and 10 ml b
47、uret. Beakers, 1 O ml and 1 O0 ml . Graduated cy1 inder, 1 O0 ml . Syringe, tuberculin, 1 ml. Glass frit filter, medium porosity. 4.4.7.2 Reagents. a. Cupric perchiorate, 0.1 N standardized (see 4.4.7.3), reagent grade. b. Tetrahydrofuran (THF). c. Acetonitrile, reagent grade. d. Ferrocene, reagent
48、grade. f. Perchloric acid, 1 N in water. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-C-85473 68 m 7779qOb 0323623 7 m MIL-C-85493( AS) 4.4.7.3 Preparation of standard 0.1 N cupric perchlorate. a. Weigh 37.0 gm of cupric perchlorate into a 1-l
49、iter bottle and dilute to the mark with acetonitrile. Shake to dissolve. b. Filter through a medium porosity sintered glass filter. Mix well andstore in a bottle with a screw cap polycone liner This solution must be filtered prior to each standardization i.f any turbidity or solids are noted. Set up the titrator according to the manufacturers instruc- tibns. Typical c
