1、c JAN-S-b27 TH 999990b 0242885 9 W f i . JAN-S-627 14 JULY 1948 NATIONAL MILITARY ESTABLISHMENT SPECIFICATION SOLDER; LOW-MELTING-POINT This specification was approved by the Departments of the Army the Navy and tihe Air Force for use of procurement Perdes of the respective Departments, and supersed
2、es the following specifications: U. S. Army Navy Department 67-98 Bureau of Ordnance 6 Aug. 1931 47547 (Ord) . 26 Feb. 1947 A. APPLICABLE SPECIRICAlIOSS AND OTHER PUBLICALIOHS A-1. Specificatio?zs.-The following specifications, of the issue in effect on the date of invitation for bids, form a part o
3、f this speci- fication : JOINT ARMY-NAVY SPECIFICATIONS JAN-P-105-Packaging and Packing for Overseas Ship- ment-Boxes, Wood, Cleated, Plywood. JAN-P-106-Packaging and Packing for Overseas Ship- ment-Boxes, Wood Nailed. JAN-B-107-Packaging and Packfng for Overseas Ship- ment-Boxes, Wood, Wirebound (O
4、verseas JAN-P-108-Packaging and Packing for Overseas Ship- ment-Boxes, Fiberboard (V-Board and W-Board) , Exterior and Interior. . JAN-P-1%-Packaging and Packing for Overseas Ship- ment - Barrier - Materials, Waterproof, Type). Flexible. JAN-P-138-Packaging and Packing for Overseas Ship- ment-Boxes,
5、 Wood, Fiberboard-Lined. JAN-P-140-Packaging and Packing for Overseas Ship- ment- Adhesives, Water - Resistant, Case- Liner. FEDERAL SPECIFICATIONS NN-Bi591-Boxes; Wood-Cleated-Fiberboard. NN-B-601-Boxes; Wood-Cleated-Plywood, For Domestic Shipment, NN-B-Zl-Boxes ; Wood, Nailed and Lock-Corner, NN-B
6、-631-Boxes; Wood, Wire-Bound, For Domestic Ship- ment. ment). QQ-M-151-Metals; General Specification for Inspection of. LLGB-631-Boxes; Fiber, Corrugated (For Domestic Ship- LLL-B-636-Boxes; Fiber, Solid (For Domestic Shipment). 100-2-Standard Spe$fication for Marking Shipments by -1 U. S. ARMY SPEC
7、IFICATION 1 Contractors. - 1Applicable only to Army purchases. , 801546-48-(E-40 -. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-2 NAVY DEPARTBIENT SPECIFICATION General Specifications for Inspection of Material, and Ap- pendix II, Metals, Part A,
8、 Definitions and Tests. A-2. Other publication.-The following publication, of the issue in effect on date of invitation for bids, forms a part of this specification : BUREAU OF SUPPLIES AND ACCOUNTS PUBLICATION Navy Shipment Marking Handbook. B. COIPOSITIOSS LiD FORJIS B-l. Compositioits.-This speci
9、fication covers the following four compositions of low-nielting-point solder, as specified (see pars. E-1 and H-2) : Cornposition A. Composition B. Composition C. Composition D. in the form of bars, ingots, sheets, strips, and other forms, as specified. I B-2. Forns.-This specification covers low-me
10、lting-point solder O. BIATERIAL AND W0RIEI)IANSIXIP C-l. Muterid-The raw materials shall be such as to produce solders meeting the requirements for the various compositions of this specification. (3-2. Workmanship.-Solder shall be uniform in quality and color, and shall be free from any injurious de
11、fects which may affect the serviceability. Sheets and strips shall be commercially flat, of uniform thickness, and free from scale, laps, twists, and i r damaged ends or edges. D. GEiELAL REQ.UIREMEXTS D-l. See section E. El. Chemical and freezing point requirements.-Solder shall meet the chemical a
12、nd freezing point requirements shown in TABLE I.-Chemical and freezing point .requirements. El. DETAL REQUIREXENTS i ! i table I. 1 Other :I%,“- Tin Lead Bismuth .!?al elements Freez- I ing- Tota- :$! i . Percent Percent Percent Percent Percent DeD. F. i i Y.,“, - - Y.“ i A . 42-44 41-45 13-15 330-2
13、86 C 10.8-13,2 25.2-30.8 45-55 . 9-11 1.00 166-155 D 36-44 18-22 36-44 . 1.00 220-210 i E B 16-18 15-17 66-68 305-200; ! %la. An analysis of each lot shall be furnished by the con- ! ! i tractor, showing the percentage o each element specified. 1 Applicable only to Navy purchases. L 1 f JAN-S-6271 i
14、 t Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-JAN-S-627 TH 777770b 02Li2887 2 fi E-2. Dimens.ions.-Solder in ali forms shall conform to the E-3. Marking.-Unless otherwise specified, each bar, ingot, sheet, strip, or other form, shall have cast o
15、r stamped thereon the specification number, composition, and the contractors brand or symbol. In the case of wire solder, the marking may be placed on -i -1 1 dimensions specified in the contract or order. (See par. II-2.) I the spool. F. METHODS OF SABIPLING INSPECTIONi AND FESTS F-l. Znspect.im.-
16、F-la. Place of inspection.-Unless otherwise specified, inspection shall be made at the place of manufacture. (See par. EI-2.) F-lb. Dimensions and mark.ing.-The inspector shall examine a sufficient number of pieces from each lot to determine compliance with paragraphs E2 and E3. F-2. Lot.-A lot shal
17、l consist of all solder produced from the same melt,. of the same form and size, submitted for inspection at the same time. F-3:Sampl.ing for Government ana at least five pieces from a lot of over 1,000 to 10,000 pounds, inclu- sive; and at least 10 pieces from a lot of over 10,000 pounds to one car
18、load, for use in preparing the composite sample as described in paragraph F3c. F-3b. Other forms.-In case the lot is in any other form, an equivalent quantity of metal representing the lot shall be taken, but in no case shall less than one whole piece (except in the case of wire) represent a lot. F3
19、c. The sample for chemical analysis shall be composed of sawings or drillings taken from each piece selected to represent the lot in accordance with paragraph F-3a and paragraph F3b. Saw- ings or drillings shall be taken so as to represent the average cross section of each piece. The sawings or dril
20、lings from all pieces shall be thoroughly mixed, and not less than 6 ounces of the mixture shall be forwarded by the inspector for analysis. Samples from Navy purchases shall be forwarded to a Government labora- tory. $4. Tests.- F4a. Bismuth.-Transfer an accurately weighed portion of 0.6 gm. of the
21、 sample to an 800-ml. beaker and add 60 ml. of water, 5 ml. of 12 N hydrochloric acid and 10 ml. of 16 N nitric acid. Cover the beaker with a watch glass and heat until the sample is completely dissolved. Add 50 ml. of water to the beaker and make the solution just alkaline with a 20 percent potassi
22、um hydroxide solution using phenophthalein as an indicator. Add 100 ml. of 20 percent potassium hydroxide solution, dilute the mixture to 600 ml. with water and pass hydrogen sulfide gas into the solution for 16 minutes. Place the beaker and contents on a steam bath for 2 hours, allow the beaker and
23、 contents to cool to room temperature and then filter the contents of the beaker with the aid of a No. 42, 11 cm. Whatman or equivalent filter paper. Transfer the residue - JAN-S-6271 t Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-9 4. to the filt
24、er paper and wash thc residue and the filter pager 5 times with approxiniatcly 20 ml. portions of a 0.5 percciit potassium hydroxide solution saturated with hydrogen sulfide. Open the filter paper and place it on the upper inside wall of the original 600-mi. beaker. Wash most of thc precipitate from
25、 the paper into the beaker with a fino stream of hot water, using about 50 nil. of water. Dissolve the precipitate remaining on the filter paper with about 2 nil. of 15 N nitric acid solution, added dropwise. Wash the filter paper with about 40 nil. of 0.7 N nitric acid solution and then discard the
26、 filter paper. Cover the beaker and boil the contents for about 5 minutes. If the sulfides are not completely dissolved, add 1 ml. of 15 N nitric acid solution and again boil the mixture for about 5 minutes. Repeat the addition of nitric acid and boiling until the sulfides are completely dissolved a
27、nd the separated sulfur is yellow to white in color. Filter the contents of the beaker with the aid of a No. 42, 9 cin. Whatnian or equivalent filter paper and catch the filtrate in a 400-nil. beaker. Transfer the residue to the filter paper and wash 5 times with approximately 10-nil. portions of a
28、0.7 N nitric acid solution. Neutralize the solution by adding 15 N animoniuni hydroxide, dropwise, using litmus paper as an indicator and record the number of nil. of IS N ammonium hydrox- ide used2 Add 10 ml. of 16 N nitric acid and dilute the solution to 250 mi. with water. Cool the beaker and con
29、tents to 18 C 2C. Add to the beaker, dropwise, and with constant stirring of the contents, a freshly prepaied solution of 5 percent cupferron in the following amounts: For solder, Composition A, use 10 mi. of cup- ferron solution, for Composition B, use 25 ml, and for Coniposi- tions G and D, use 20
30、 ml. Allow the contents of the beaker to settle for 15 minutes and then filter, using a tared ignited asbestos Gooch crucible. Transfer the precipitate to the crucible and wash 5 times with approximately 15-nil. portions of a freshly prepared solution of 0.1 percent cupferron in 0.15 N nitric acid s
31、olution. (Reserve the filtrate for the determination of the lead content.) Dry the-crucible and contents at 100 -t- 10C. for 30 minutes and then place on a hot plate heated to 225 k 25C. for about one hour to convert most of the residue to bismuth oxide. (On heating, the residue effervesces, turns b
32、lack and eventually assumes the light brown coloration of bismuth oxide.) Heat the crucible and contents at 650 -L 25C. for one hour, cool and weigh. Repeat this pro- cedure until constant weight is attained. Consider the residue in the crucible to be bismuth oxide and calculate the increase in weig
33、ht of the crucible to percentage of bismuth in the sainpie as follows: Weight of residue in crucible x 89.70 Weizht of samde Bismuth, percent = F-4b. Lead.-Transfer the filtrate obtained fkm the bismuth determination to a 600 ml. beaker. Evaporate the solution to about 60 ml. and add 36 N sulfuric a
34、cid in the following amounts: 5 m1. plus one-half of the volume of ammonium hydroxide used in con- nection with the determination of bismuth. (For exnniple, if 12 ml. of aninioniuw hydroxide were used, use 5 plus % times 12 or 11 ml. This value is used In connection with the determinatioii of the le
35、ad content. JAN-S-6271 I ! ! j i 1 i i t i Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,- - JAN-S-b27 TH m 9349b 0242889 b m _._II_.- ! i ; -. i i i i- ,;- : I i ! E 5 of sulfuric acid.) Heat the contents of the beaker until sulfur trioxide fumes a
36、ppear. If tlie residue is colored b the presence of organic matter, add 2 mi. of 15 N nitric acid sofution and again heat the niixturc until sulfur trioxide fumes are produced. Repeat the addition of the nitric acid solution and then heat to sulfur- trioxide fumes until all the organic matter in the
37、 beaker is destroyed and the residue in the beaker is white or colorless. Add 5 mi. of water and again heat the mixture until sulfur trioxide fumes are produced. Add 100 nil. of water, heat the mxture to boiling, and boil for 15 minutes. Allow the mixture to stand at room temperature for at least 3
38、hours and then filter it with the aid of a tsred, previously ignited filtering crucible. Transfer the precipitate to the crucible and wash it 5 times with approximately 10 ml. portions of 1.5 N sulfuric acid solution. Wash the crucible and residue with 3 mi. of water. Dry the crucible as lead sulfat
39、e and calculate its weight to percentage of lead in the sample as fnllowva: - - - . . - . Weight of residue in crucible x 68.32 Lead, percent = Weight of samde - - Fac. Tin.-One-half gram of the sample is placed in a 300-ml. Erlenmeyer flask and 10 mi. of strong sulfuric acid is added. Nearly all of
40、 the excess acid is expelled. The moist residue is allowed to cool, and 100 ml. of air-free water is added, followed by 50 ml. of strong hydrochloric acid and the mixture gently warmed until tlie solution begins to clear. Into the Erlenmeyer flask is placed a 1-hole stopper with a delivery tube exte
41、nding to the bottom of a beaker containing approximately 400 mi. of 10 percent sodium bicarbonate solution. Approximately one grn. of very finely powdered antimony metal (or iron wire or nails) is placed in the flask followed by 10 mi. of saturatcd sodium bicarbonate solu- tion, the stopper being re
42、moved during the addition and then immediately replaced. The air is displaced by the carbon dioxide generated. The contents of the flask are gently boiled for 15 minutes allowing the escaping gases to bubble through the sodium bicarbonate solution. The apparatus is removed from the hot plate and all
43、owed to cool to room temperature, leaving the sodium bicarbonate solution to establish the pressure equilibrim, carbon dioxide being generated in the flask as the sodium bicarbonate solution is drawn into the flask on cooling. When the contents of the flask are cooled the stopper is removed, 5 mi. o
44、f starch indica- tor solution is added, and the solution titrated to a permanent blue end point with 0.1 N iodine solution. One nil. of 0.1 N iodine is. equivalent to 0.005935 grams of tin as metal. F-4d. CarEnifwL (for composition C solder).- F4d(l). Iliethod.-Weigh 1 gm. of the sample into a 250-m
45、l. beaker, add 10 id. of water, heat, and add sufficient HNOS (sp. gr. 1.42), a little at a time, until the alloy is dccoinpose. Evaporate to dryness, digest with 10 ml. of HNOS (sp. gr. 1.42), dilute to 50 nil. with water, bring to boiling and allow to stand, and scttle for one hour keeping the tem
46、perature just below the boiling point. Filter, keeping the solution hot, through a small close- tcxturcd paper to which a little paper pulp has bec11 added aiid wash with hot dilute HNOs (1:49). Reserve this original filtrate for cadmium. JAN-S-627 * c Provided by IHSNot for ResaleNo reproduction or
47、 networking permitted without license from IHS-,-,-i i i Transfer the paper and precipitate to a small porcelain crucible, dry and ignite. Mix the residue with 4 gm. of fusion mixture, cover with 4 gm. of the fusion mixture and heak until in quie6 fusion; heat 20 minutes longer. Cool, leach with as
48、little water.as possible, remove and wash the crucible. Combine washings with the main leaching solution. The supernatant solution should be of a clear, yellow color. Filter and wash with warm (not hot) KSH wash solution. Discard the filtrate. Dissolve the residue from fusion with 16 ml. of hot HN03
49、 (1 :2), wash with hot water, boil to a volume of 25 ml. and allow to stand for one hour keeping the temperature just below the boiling point. If an insoluble residue is present, filter on a small close-textured paper to which a little paper pulp has been added and wash with hot dilute HNOI (1 :49). Dischard the tin bearing residue. Com- bine the filtrate with the original filtrate (from the H2SnOs separation). Boil the combined filtrates
