NAVY MIL-A-85501-1981 ANTIOXIDANT N-PHENYL-N--CYCLOHEXYL-P-PHENYLENE DIAMINE《N -苯基-N --环己基-对苯二胺抗氧化剂》.pdf

1、H-7Q-79 MIL-A-5503 68 m 9777906 0323692 6 m MIL-A-85501 (AS) 6 October 1981 MILITARY SPECIFICATION ANTIOX I DANT , /- N-PHENYL-N-CYCLOHEXYL-p-PHENYLENE DIAMINE This specification is approved for use by the Naval Air Systems Comand, Department of the Navy, and is available for use by all Departments

2、and Agencies of the Department of.l)efense. 1. SCOPE. 1.1 Scope. This specification establishes the requirements for 2. APPLICABLE DOCUMENTS. N-phenyl -NI -cyclohexyl -p-phenylane diamine antioxidant material. 2.1 Issues of documents. The following documents of the issue in effect on date of invitat

3、ion for bids or request for proposal form a part of this specification to the extent specified herein. STANDARDS MIL I TARY - MIL-STD-129 Marking for Shipment and Storage. MI L-STD- 1 21 8 ACS Chemical c. (Copies of specifications, standards, drawings and pub1 ications required by suppliers in conne

4、ction with specified procurement functions should be obtained from the procuring activity or as directed by the contracting officer. ) Beneficial comments (recommendations , addi ti ons , del eti ons ) and any pertinent data which may be of use in improving this document s hou1 d be addressed to : C

5、omandi ng Off i Cer, Naval Ai r Engi neeri ng Center, Engineering Specifications and Standards Department (ESSD) Code 93, Lakehurst, NJ 08733, by using the self-addressed Stan- I dardization Document Improvement Proposal (DD Form 1426) appearing lat the end of this document or by letter. IFSC 68101

6、Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-A-8550L 68 M 9979906 O323693 B W 3. REQUIREMENTS . 3.1 Chemical and physical properties, Chemical and phystcal properties 1 of the materal shall conform to Table I. - Property- Mfn Max Nelting point

7、, OC 110 - p-Aminodtphenylarnine, percent - Di phenyl ami ne, percent 5.0 O, 5 - TABLE I. Chemical and physical properties. 3.2 Stability. When stored at 27 +11 degrees Celsius (OC), the material shall have a storage life of 24 months from date of delivery to the procuring activity. 3.2.1 Storage li

8、fe extension. The storage life of an individual lot (see 6.3.11 of material may be extended an additional 12 months provided the material, upon retest, successfully meets the requirements for melting point, p-aminodiphenylamine, and diphenylamine. 3.3 Infrared (IR) spectrum. An IR spectrum shall be

9、made. The IR spectrum shall qual itatively conform to Figure 1. 3.4 Toxic products and safety. Safety regulations and guidelines applicable to the use of N-phenyl -NI-cyclohexyl -p-phenylene diamine should be complied with to preclude personal injury and damage to equipment and facilities. 3.5 Workm

10、anship. Workmanship shall be such that the material is uniform in appearance and free from visible contamination. 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 perfor

11、mance of all inspection requirements as specified herein. Except as otherwise specified, the contractor may utilize his own facilities or any comerclal laboratory acceptable to the Government. The Government reserves the right to perform any of the nspections set forth in this specification where su

12、ch inspections are deemed necessary -to assure that suppl ies and services conform to prescribed requirements. 2 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-A-85501 68 m 7779706 0123674 T MIL-A-85501 (AS) 4.2 Samplfng. The lot shall be sample

13、d in accordance with Table II. TABLE 61. Samplingplan. Number of contalners in lot I00 or more 51 - 99 11 - 50 1 - 10 Number of containers sampled (primary sampl e 1 10% (nearest whole number 10 10 ALL . Number of compost te sampl es 5 4.2.1 Primar Sam les. each primary * sample see Table II). The m

14、aterial container may be Physical properties tests shall be run on sampled by use of a 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

15、 sample size shall be two ounces. Glass containers shall be used for all liquid samples. 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 1 ot represented. If the cntain

16、er Failure of any primary sample to pass 4.2.2 Composite samples. Chemical properties tests shall be run on each composite sample. Divide the primary samples equally into the number of composites shown in Table II. by manipulation of the container. Label each composite with Roman numeral s, al so in

17、clude date, lot numbers, and manufacturers container identification numbers. The remainder of the primary samples shall be retained pending acceptance or rejection of the lot. Failure of any composite sample to pass all of the chemlcal properties tests herein shall result in rejection of the lot rep

18、resented. Blend each composite thoroughly 3 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-A-85501 68 W 7779706 0123675 II MIL-A-85501 (AS ) 4.3 Quality conformance inspections and tests. Qualtty conformance inspecttons and tests shall consist o

19、f the following: a. b. c. Vtsual lnspectton (see 4.5.2). Tests of Table I properttes see 4.41. Inspection of filled containers (see 4.5.1). 4.4 Test methods. Tests shall be performed using apparatus, reagents, and procedures speclf fed berei n. The use of al ternate apparatus , reagents, or procedur

20、es shall require prior written approval of the procuring .activity. Al 1 American Chemical Society (ACS) reagents shall conform to MIL-STD-1218. 4.4.1 Melting point. 4.4.1.1 Apparatus. a. Melting point apparatus, filled with mineral oil, or equal. b. Melting point capillary tubes, 100 millimeter (mn

21、) by 1.5 to 2.0 mm. c. Thermometer, O to 150C, or equal. 4.4.1.2 Determination of melting point. Collect a small amount of sample in the open end of a capillary melting point tube. Pack sample int about 3 mmof the capillary tube. Preheat the bath to within 3OC of the expected melting point. Attach t

22、he capillary tube to the therm- ometer with the sample opposite the mercury bulb and lower the assembly into the melting point apparatus until the thermometer bulb is below the side arm. The liquid level of the bath should be near the 0C mark when melting occurs. Adjust heating so that the temperatu

23、re rise is approxi- mately 1C per minute when approaching the melting point. temperature when the sample becomes completely wet .and mol ten. the melting point to the nearest OC. Record the Report 4.4.2 p-Ami nodi phenyl ami ne. 4.4.2.1 Apparatus. a. Spectrophotometer, Perkin-Elmer Model 350, or equ

24、al , with matched 1 centimeter silica cells, set up to measure in the 450 nanometer (nm) range. . b. Mtcro buret, 10-milliliter (ml). 4 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-4.4.2.2 Reagents. a. p-Ami nodi phenyl ami ne , reagent grade. b.

25、Glacial acetc acid, ACS reagent. c. Saltcylaldehyde, reagent grade. 4.4.2.3 Preparation of standard p-aminodiphenylamtne cume. NOTE: Standardtzatfon must 6e completed tn I day and must be repeated for each new lot of glacial acetic acid. Weigh accurately 0.12 gram Cgm) of p-aminodipheylamine into a

26、100-ml volumetric flask. Dissolve in glacial acetic acid, dilute to volume with glacial acetic acid, and mix well. Transfer, by means of a micro buret, 2.0, 4.0, and 6.0 ml of the solution to a series of 100-ml volumetric flasks. Dilute each to volume with glacial acetic acid and mix well. Prepare t

27、wo 100-ml volumetric flasks, marked A and B, by transferring 10-ml aliquots from each flask. acetic acid and 45 ml of distilled water to each flask and swirl to mix. Fill flask B to volume with distilled water, mix well, and use flask B solution to zero the spectrophotometer. Add 1.0 ml of salicylal

28、dehyde to flask A, dilute to volume with distilled water and mix well. mine the absorbance of the sample solution immediately (absorbance decreases on standing) at a wave length of 450 nm and a slit width no greater than 0.2 mm. Repeat this procedure for the other three sample solutions. the concent

29、ration of p-aminodiphenylamine in gm/100 ml , and draw a line best fitted to the points. Add 40 ml of glacial Deter- Prepare a standard curve by plotting the absorbance versus 4.4.2.4 Determination of p-aminodiphenylamine. NOTE: and requires the same lot of glacial acetic acid used for the standard

30、curve. Analysis must be completed in 1 day Weigh accurately 0.60 gm of sample into a 50-ml volumetric flask, dissolve in glacial acetic acid, dilute to volume with glacial acetic acid and mix well. Transfer 10.0 ml of sample solution to a 100-ml volumetric flask, dilute to volume with glacial acetic

31、 acid and mix well. Transfer 10.0 ml of this solution into each of two 100-ml volu- metric flasks marked A and B. Add 40 ml of glacial acetic acid and 45 ml of distilled water to each flask and swirl to mix. Fill flask B to volume with distilled water, mix well, and use flask B solution to zero the

32、spectrophotometer. Add 1.Oml of salicylaldehyde to flask A, dilute to volume with distilled water and mix well. Determine the absorbance of the sample solution imnediately (absorbance decreases on standing) at a wave length OP 450 nm and a slit no greater than 0.2 mn. concentration of p-aminodipheny

33、lamine in the sample solution directly from the standard curve. Read the 5 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-_ MIL-A-85501 b W 7999906 0223697 5 W MI L-4-85501 (AS) Cal cul at i on : C x 500 p-ami nodi phenyl ami ne, percent = Where: C

34、= concentration from standard curve, gm/100 ml W = weight of sample, gm Report the p-aminodiphenylamine to the nearest 0.1 percent. 4.4.3 Diphenylamine. 4.4.3.1 Apparatus. a. Gas chromatograph, Perkin-Elmer Model 820, equipped with a 12 foot stainless steel column by 0.12-inch outside diameter, pack

35、ed with 15 percent W/W Apieton L on Anakrom ABS, 90 to 1 O0 mesh, or their equal. b. Helium cylinder. c. Syri nge, 5-mi crol i ter. 4.4.3.2 Reagents. ._ a. Diphenylamine, ACS. _r_ _.* b. Acetone, ACS. / J 4.4.3.3 Preparation of standard di phenyl ami ne sol ution. Weigh .- accurately 0.08 gm of diph

36、enylamine into a 100-ml volumetric flask. Dissolve in acetne, dilute to volume with acetone and mix well. 5 microliters of this solution into the gas chromatograph using the fol lowing conditions: Inject Injection port 275 to 300C Column temperature 250“ C Detector 275 to 300C He flow 40 cubic centi

37、meters/rninute Calculate the standard factor from the peak height thus obtained. c Cal cul ation: W Standard factor = 6 i I f Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,- MIL-A-5501 b W 77977Ob 0123678 7 W MI L-A-85501 (AS) Where: W = weight of s

38、ample, grams P = peak height of sample, mm Record the standard factor to the nearest 0.000001. 4.4.3.4 Determination of diphenylamine. Weigh accurately 4.0 gram of sample into a 25-ml volumetric flask. Dissolve in acetone, dilute to volume with acetone and mix well. Inject 5 micro1 iters of sample s

39、olution into the gas chromatograph which has been set to the conditions including attenuation in 4.4.3.3. Calculate the amount of diphenylamine in the sample from the peak height thus obtained. Cal cul ation: F x P x Vx 100 r4 Di phenyl ami ne, percent = Where: F = standard factor from 4.4.3.3 P = p

40、eak height of sample, m Y = volume of sample solution, ml W = weight of sample, gm # Report the diphenylamine to the nearest 0.1 percent. 4.4.4 Infrared spectrum. The infrared spectrum shall be determined using an infrared spectrophotometer in accordance with the following: Set the instrument pen to

41、 at least 70 percent transmittance at approximately 4,000 cml when pel 1 et of spectrographic grade potassium bromide and N-Phenyl-NI-Cyclohexyl-p- Phenylene Diamine (approximately 55:l weight ratio) is mounted in the sample beam (reference beam:air). a. b. Adjust the thickness of the pellet if 70 p

42、ercent transmittance is not achieved. if any major peaks are less than two percent transmittance. Scan the pellet and compare resulting spectrum to Figure 1. The peak position and relative magnitude shall be qualita- tively similar within a 2.5 to 15 pm, scan range. Also, adjust the weight ratio of

43、the pellet c. d. Report conformance to, or deviation from, Figure 1. 4.5 Exami na t i ons . 4.5.1 Inspection of filled containers. All filled containers shall be inspected prior to shipment or use-for accuracy of markings and for 7 Provided by IHSNot for ResaleNo reproduction or networking permitted

44、 without license from IHS-,-,-MIL-A-85501 b 777770b 0123677 7 I l MIL-A-85501 (AS) defects in containers and closures. All defective containers and closures shall be repaired or replaced, and contents therein shall be reinspected prior to shipment or use. 45.2 Visual inspection. All samples shall be

45、 visually inspected to determi ne conformance to the requi rements of 3.5. 4.6 Records. Certification and test data shall be prepared as required by the procuring activity (see 6.2.2). 5. PACKAGING. - 5.1 Packaging and packing. Unless otherwise specified in the contract or purchase order (see 6.2.1)

46、, packaging and packing of the material shall be in accordance with comercial practice to insure carrier acceptance and shall be of such construction and materials that the contents will be adequately protected against loss or contamination. 5.2 Marking for shipment. Unless otherwise specified in th

47、e purchase order (see 6.2.1), each shipping container shall be marked in accordance with the requirements of MIL-STD-129. Container marking shall include the fol lowing: a. The suppliers lot number. b. Procuring activity purchase order number. c. Container identification number (applied in numerical

48、 sequence as the containers are filled). d. Date of manufacture. e. Manufacturers Code Ident. f. Net and tare weight of container. g . Materi al i denti f icati on. 6. NOTES AND CONCLUDING MATERIAL. 6.1 Intended use. The intended use of the material described herein is as an antioxidant in solid roc

49、ket motor propellant. 6.2 Ordering data. 6.2.1 Procurement requirements. Procurement documents should specify the following: a. b. Title, number and date of this specification. Responsibility for inspection and inspection facilities, if different than 4.1. r i I 8 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-I MIL-A-5503 6