1、- - JAN-S-732 13 I 7779706 0273325 7 JAN-S-7 3 2 9 FSBRUARY 1949 SUPERSEDING U. S, Army 20 NOT. 1947 Picatiany Amenal Tenutire Specification PXS-1186 21 May 1945 50-11-148 NATIONAL MILITARY ESTABLIS“T SPECIFICATION SHELLAC SOLUTIONS -(FOR USE IN AMMUNITION) This specification was approved by the Dep
2、artments of the Army, the Navy, and the Air Force for the use of procurement services of the respective Departppentr. 1. SCOPE AND CLASSIFICATION 1.1 Scope.-This specification covers solu- tions of orange shellac suitable for use in . amunition. 1.2 Classification.- 1.2.1 Types.-This specification c
3、overs two types of shellac solution, as specified (see 6.2) : Type I-Dyed. Type II-Undyed. 1.2.2 0Zmses.-Type I shellac solution shall be furnished in two classes, as specified (see 6.2) : Class 1-For application by spraying. Class 2-For application by swabbing. 2. APPLICABLE SPECIFICATIONS 2.1 Spec
4、ifications.-The following specifica- tions, of the issue in effect on date of invitation for bids, form a part of this specification : AND OTHER PUBLICATIONS FEDERAL SPECIFICATIONS : TT-S-271-Shellac (Orange) and Other Lacs, VV-L-70 1-Lubricants, Liquid Fuels, and Related Products, Methods for Sampl
5、ing aiid Testing. JOIST ARJIY-NAVY SPECTFIC.VIION : JAX+A-463-Alcoliol, Ethyl (For Ord- naiice Use). C. S. .lfJIY PPECIVICATIONS : 50-0-1-General Specification for Amniu- nitioii Except Small Arnis Ammunition. 100-2-Standard Specification for 3;irk- iiig Shipments by Cont ractors. s AY Y I)EP. irr J
6、I EST smci 1.m *.II- I I) s : Geiirral Spccificiitioiis foi. Tilpcction of JIateriaL2 i dppiic:ibic oiiiy to -1rniy piiiciinser. Appliwlic only to S:iry piiwixises. (Army.-Coples of BUREAU OF SUPPLlEE AND ACCOUNTB PWLTA- “IONS : Navy Shipment Marking Handbook. (Copies of the Navy Shipment Marking Ha
7、ndbook may be obtained upon application to the Bureau of Supplies and Accounts, Navy Department, Waehing- ton 25, D. C., except that rictivltiea of the Armed Forces should make applicatiop to the Supply OfBcer in Command, Naval Supply Center, Norfolk 11, Va.) INTERSTATE COMMERCE COMMISSION REUULB- T
8、ION Regulations for Transportation of Erplo- . sives and Other Dangerous Articles, etc. - (Informntion as to the availability of Interstate Commerce Commission Regulations for Transportation of Explosives nnd Other Dangerous Articles, etc., may be ohtnined from the Interstate Commerce Commis- sion,
9、Washington 25, D. C.) 3, REQUIREMENTS 3.1 Material.-The material used in the man- iifnctiire of shellac solutions shall conform to the applicable specifications listed in 2.1. In addi- tion, the following nintreials shall be of the type- or grade specified : - - THIS DOCUMENT CONTAINS 63 PAGES.- - -
10、 - I Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-JAN-S-732 13 7777706 0271326 7 = - Appeuuiee d dne film _-_-_- Nature of vohtile nuttcr- - -_ - - - .- JAN4432 - - Alcohol, etlyl-Joint Army-Navy Specifi- Aniline dye-A commercial grade of pur- She
11、llac, orange-Federal Specification “I!- 3.2 Chemical and physical requirementa- The shellac solutions shall conform to the chem- . ical and physical requirements shown in table I. cation JAN-AA63, grade 5. 5-271, type I, grade A, B, or U. ple dye in powdered form. I % TABLE I.4miecrl and phgM requre
12、mnts Uniform and homogeneoue Shall conform to the ethyl alcohol content .requinment for ite soliitioii :iiid 10 1111. of :L saturated soliitioii of ferric iiiiiiiioiiiiiin sulfate to 50 ml. with distilled water niid mixing thoroughly. 2 - / e Provided by IHSNot for ResaleNo reproduction or networkin
13、g permitted without license from IHS-,-,-4.4.1.1.2 Procedure.-Transfer a weighed portion of approximately 1.0 gm. of class 1 or 0.5 gm. of class 2 material to a lm-ml., glass- stoppered graduated cylinder. Dilute the sam- ple in the graduate with 95-percent ethyl alcohol so that the diluted solution
14、 contains 0.33 gm. of nonvolatile matter per 100 ml. of solution. The volume to which the sample shall be diluted may be calculated by multiplying the weight of sample by the percent nonvolatile xatter as de- termined in 4.4.3, and dividing the product by 0.33. Mix the dilute solution thoroughly and
15、 transfer a 50-ml. portion ta a 50-rnl. Nessler tube; Compare the color of the dilute solution, when viewed by transmitted diffuse white light, with the colors of standrtrds A and B (see 4.4.1.1.1) which are contained in similar 50-ml. Nessler tubes. To pass the comparison test, the solutions shall
16、be approximately the same shade of purple as the color standards, but lighter than standard A niid darker than standard B. 4.4.1.2 Type II.-Determine the color of the undyed shellac solution in accordance with inethod 10.2 of Federal Specification VV-L- 791,. 4.4.2 Xpecifi gravity.-Determine the spe
17、- cific gravity of the sample of the dyed shellac solution at 2Oo/4O C. by means of a Westphal balance or pycnometer. 4.4.3 NonvoZatiZe matter.-By means of a weighing pipet, transfer a weighed portion of approximately 2.5 gm. of the sample for type I, class 1 material, 1.2 gm. for type I, class 2 ma
18、terial, and approximately 5 gm. for type II material to a tared flat-bottomed metal dish approximately 8 cm. in aiameter. Heat the cljsli and contents at 105Ok2O C. for 3 hours, cool in a desiccator and weigh. Calculate the increase in weight as percent nonvolatile matter. 4.4.4 wax.- 4.4.4.1 Reagen
19、ts.- 4.4.4.1.1 Ninety- five percent aZcohol.-Either 05 percent ethyl alcohol or specially denatured alcoliol foriniilas SD-1 or SD-30 shall be used. (See 6.3.) 4.4.4.1.2 ChZoo f orm-Use redistilled chloro- form iii order that the solvent shall not leave a iioiivolatile residue. 4.4.4.1.3 Filter ceL-
20、Extract tlie filter ce1 with chloroforiii before using. 4.4.4.2 Procedure.-Transfer weighed por- tions of approximately 56 gm. of type I, class 1, approximately 25 gm. of type I, class 2, and approximately 115 gm. of type II material, to 200-ml. tall-form beakers. Evaporate the 80- lutions in the be
21、akers to volumes of approxi- mately 25 ml., conducting the evaporation on a steam bath. Add 2.5 gm. of sodium carbonate and 150 ml. of hot distilled water. Immerse the beaker in a steam or boiling-water bath, and stir the contents of the beaker until the shellac is in solution. Cover the beaker with
22、 1. watch glass and allov to ramain in the bath for 2 to 3 hours more without agitation. Remove the beaker from the bath and place it in cold water; The wax will come to the surface of the liquid in the beaker where it will soMG 88 8 layer or float 89 small hard particles according to the amount of
23、wax present. Prepare a Buchner funnel, which shall have an inside diameter of 2.25 to 3.5 inches, as follows: Cover the bottom of the Biichner funnel with a disk of ilter paper; mix 1 gm. of filter ml (see 4.4.4.1.3) with water and pour the mixture onto the filter paper, applyjng suction to remove t
24、 the thermometer should have an auxiliary raser- voir at the upper end, a length of about 39 cm. and a diameter of about 6 mm., and should be certified by tlie National Bureau of Standards (See 6.5.) . The amount of acid in the test tube should be at least double the quantity required to cover the b
25、ulb of the thermometer when the bottom of the latter is 0.5 inch from the bottom of the test tube. Suspend the test tube within a larger test tube by means of a cork, Cool the acid by immersing the assembly in ice mater until the temperature of the acid is loo C. Withdraw the assembly from the ice b
26、ath and stir the acid rather vigorously for a few moments in order to cause the supercooled liquid to partially crystallize and give a mix- ture of liquid and solid acid. Allow the mix- ture to warm, taking thermometer readings every 15 seconds. Note the temperature at which tlie thermometer reading
27、s remain con- stant for at least 2 minutes. Make any neces- sary stem and bore corrections aiid take this corrected temperature as the melting point of tlie acetic acid. 4.4.6.1.2 ChZorofom.-Use U. S. P. grade, acetone-free, chloroform. 4.4.6.1.3 N/O sodium thiosuZfate solution.- Dissolve pure sodiu
28、m thiosulfate in distilled water that lias been -sell boiled to free it froin carbon dioxide, using 24.83 gni. of crystallized sodium thiosulfate per 1,000 ml. of solution. A4dd 0.1 gin. of sodium carbonate per 1,000 ml. of soliition aiid allow this solutiori to stand over- night before standardizat
29、ion. Standardize tlie solution, preferably with resublimed iodine or 4 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,- -*-I JAN-S-732 13 m 9999906 0291329 L1 I c . 8 potnssiuin iotlato. (Sco 6.6.) Keep tho SO- 1ut.ion iii R stock hottlo provided wit
30、h a guard tubo fillcd with soda limo. 4.4.6.1.4 Staivh solution.-Make a pasto of 0.2 gm. of soliihlc (potato) starch in cold water :iiid pour into 100 ml. of boiling. water. Doil tho mixtiirc, for 5 minutes, cool and bottle. 4.4.8.1.5 20 t a.w unr iodide ,?o hton.-Discol ve potrissiiim iodide, freo
31、from iodates, in distilled water, using 10 gm, of potassium iodide per 90 nil. of water, 4.4.6.1.6 Wij8 soZutzm.-Dissolve 13 gm. of rcsiiblimcd iodine in one liter of acetic acid (silo 4.4.6.1.1), heating gently if necessary. Cool the solution and determine its strength by t itraf,ion with N/10 sodi
32、um thiosulfate solution (seo 4.4.6.1.8) as follows: Transfor an ac- curately measurccl portion of 20 ml. of the iodine-acctic acid solution to a 300-ml. Erlen- nicyer Bask, add quickly 15 ml. of potassium iodide solution (see 4.4.6,1.5) and titrate iin- inedintcly with N/lO sodium thiosulfate solu-
33、tion, allowing the solution to run in rapidly wiiilo slinking the flask vigorously until the solirtioii in the flask assuniw a straw color; add 10 ml. of freshly prepared starch solution (see 4.4.6.1.4) and slowly finish the titration, Set itside 50 to 100 ml. of tho iodine-acetic acid so- liition.
34、Introduce dry chlorine gas into the rcninindcr of the solution until a characteristic color change occurs, indicating that the halogen coiitmt of tho solution has been approximately doiibled. Ilctorinine the halogen strength of th cliloi.innted solution by titration with N/lO sodiiiiii t.liiosu1fat.
35、o solution in a manner similar to tlint dcscribcd above for determining the st iaiigtii of the iodinc-acctic acid solution. If tlic Iinlogeii content of the iodine-acetic acid solution IMS beon more than doubled, roduco it by citlding the requisite quantity of the iodine- acctic solution. The final
36、solution should con- .:iin an nmount of iodine and chlorine corre- spciii(1iiifi to iotliric-monochlorido; a slight (!s(:css of iodinc, (lop 110 harki, but any exCo95 of cliloriiic. over tht required tl!eoretically for iocline-moriocliloride must be avoided. As an exnniplc, if tlic titration of 20 m
37、l. of the original iodirie-acetic acid solution required 22 ml. of N/lO sodium thiosulfnte solutioii, then 20 ml. of 1 Iic finished Wijs solution should require be- tweeii 43.5 and 44 ml. of the thiosulfate solution. , JAN-S-732 4.4.6.2 Procedure.-Transfer approximately , 8 nil. of tho samplo by men
38、ns of IJ pipct to IL fltrt-bottomed, glass or porcelnin dish at lenst 8 crn. in diameter. Allow tho samph to sproad evenly over the bottom of the dish, Heat tho dish and contenkq at 85O to 90“ C. for 1h hour. .Scrape the midue from the dish, using a sharp knifc blnde, and discard any chips or thick
39、pieces. At tho dimrotion of the analyst, tlic dry sliellnc may be obtained by the following alternats method: Pour a thin film of the sample on a clean glass plate approximately - 6 by 10 inches and allow the material to drain , for 1 hour, holding the plate in a vertical poai- tion; place the plate
40、 in a horizontd position in an air oven at 43O*5* C. for 18 hours; cool and scrape off the dry shellnc with a shnrp razor blade. Transfer an accurately weiGhod portion of .0.20*0.01 gm. of tho dry shellac to a 300-nil. dry bottle made of clear glass and provided with a ground-glass stopper. Add 20 m
41、l. of acetic acid (see 4.4.6.1.1) and warm the mixture gently on a steam bath until all of the sample except th wax is dissolvod, A pure shellac is rather difficultly solublo; solu- tion is quicker according to.the proportion of rosin present. Add 10 ml. of chloroform (see 4.4.6.1.2) and cool the so
42、lution to 21.6“ to 2%0 C. Allow the bottles to stand half immersed in n slillow pan of water, well insulated or cquipped with a cuitablo thermostat, for at least 30 minutes at 21. to 22.5 C., before adding the Wjs solution. (See 4.4.6.1.6.) Add 20 ml. of Wijs solution (which shall Iiavo a tempera- t
43、ure o 21.5 to 22.5 C.) from a pipet having r?, rather small delivery aperture (delivery time, approximately 30 semids). Close the bottle, imnierso it again in he pan of water, and notetlie time. Keep tho bottle and con- tents immersed in the bath for 1 hour, swirl- ing the contents of the bottle occ
44、psonally. After exactly 1 hour, add 10 ml. of freshly prepared potassium iodie solution (seo .4.4.G.1.5), washing into the hottlo any Wijs solution which may be on the stopper of the bottle. Add 120 ml, of water nnd 40 ml. of , chloroform and titrate the solution immedi- ately with N/lO sodium thios
45、ulfate solution (see .4.4.6.1.3), allowing the solution to run in rapidly while shaking vigorously until the water solution assumes a light brown color. a , 6 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-.-r- .I JAN-S-732 13 7997706 0273330 O W No
46、w tld 18 mi: 8f frctslily prepnred stakh so- lution (eo 4.4.6.1.6) niid slowly finish the ti- tration. llie .endpoint is sliarp sis the anitino dye aiid tlie mctioii prodiicts of sliellac remain dissolved in the ciiloroform; isregard any blue coloration which may roturn after 0.5 niinute or so. Run
47、a blank determination at tlie same timo on.tlio reagents. Calculate tlie idiiie number of tho noiivolatile matter in the sldac solutioii as follows : Iodina number of iionvolatile. matter= 12.69 (V-v)N W - where V=mL of sodium t,liiosulfab solution re- quired in titration of blank. v=ml. of dium tli
48、imulhte solution re- quired to titrate excess halogen in solution coiitriitiing sample. N-normality of sodium thiosulfate solu- tion. IV-gin. of nonvolatile matter tuken for test. The riiicilyst sliould rui) in pnidlel a sample of pire slielliic of known iodiiia iiiiniber as a clicck upon the rolinb
49、ility of t.lic Wijs niid other re- ngciits ; tlic iocliiio iiunilm tlius slioiild be within tlie outside slinll be iii- siil i t et i wit li sheet :isha t os. 4.4.7.2 Pmparation of the fi2tahg unit.-Cut 8 disk of filter pnpei- (Wlintiiiaii No. 41 or ccliiivrilciit) to fit inside the crucible atid tlioii plilce tho disk 011 top of the glass filter. In- trwluce upon the fil
