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1、 STD-JIS H LqLI-ENGL L77b m Li933b08 05qLi807 3LT “OC 669.35 24:669.018.55 :543 This version is for information only since the original Japanese text IS of this Standard was revised in Mar., 1996 JAPANESE I NDUSTRIAL STANDARD Methods of Chemical Analysis for Copper Nickel Resistance Material JIS H 1
2、413-1976 (Reaffirmed: 1984) This copy is an English version of Japanese Industrial Standard prepared by Japanese Standards Association, the copyright holder. Any further reproduction without permission is prohibited. Translation without guarantee I I I In the event of any doubt arising, the original
3、 standard in Japanese is to be evidence ; ! Translated Japanese Standards Association 1-24, Akasaka 4, Minato-ku Tokyo 107 Japan O JSA, 1986 Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007
4、22:32:21 MDTNo reproduction or networking permitted without license from IHS -,-,- STD-JIS H 1413-ENGL 199b 4933608 0544830 031 This English traslation is prepared at the expense of Japan External Trade Organization (JETRO) Copyright Japanese Standards Association Provided by IHS under license with
5、JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 22:32:21 MDTNo reproduction or networking permitted without license from IHS -,-,- STD-JIS H 3433-ENGL 377b W 4733b08 0544833 T78 UDC 669.3524:669.018.55:543 JAPANESE IXDUSTRL4L SrwDARD J I S Methods of Chemical Analy
6、sis for H 1413-1976 Copper Nickel Resistance Material (Reaffirmed: 1984) 1. Scope This Japanese Industrial Standard specifies the methods of chemical analysis forchemical components (copper, nickel, cobalt, manganese) specified in JIS C 2521. 2. General Matters General matters common to the chenicel
7、 analysis methods shall be in accordance with JIS K 0050 and JIS K 0115. 3. S.=mpling and Treating of Sample for Anaysis 3.1 The sampling shall be in accordance with 2.3 of JIS H 0321. 3.2 When a cast sample is sampled, not less than 2 samples per one fusion (one sample when the amount of one fusion
8、 is especially very little) shall be taken to obtain the sample representing its average material quality. especially free from segregation to obtain the same quality as that of product as perfectly as possible. Cares shall be taken so that the cast sample is 3.3 The chipping of sample shall be as f
9、ollows: When there are adhering substances on the surface of sample, the surface shall be cleaned by removing them with an emery paper or the like. Drills and other tools shall be cleaned by using alcohol and the like. C?hen a cast sample is chipped out, the sample is pierced by perpendicularly dril
10、ling from one side of the part near the central part and both ends or the like, and otherwise it is drilled from both sides till reaching the central core part at least. methods. Otherwise the sample is chipped out by other suitable For chipping out the sample from product samples of wire, band, pla
11、te, etc., they are chipped out in sizes suitable for analytical operation by using a drill or other suitable tools. Applicable Standards: See page 20. - 1 - Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Res
12、ale, 03/15/2007 22:32:21 MDTNo reproduction or networking permitted without license from IHS -,-,- Becatse the surizcec of chips are occsionally oxidized by gensration of heat when drilled, drilling is carried out by giving the drill a pressure and a number of revolutions to the degree not to oxidiz
13、e them. In that case, it is prohibitted to use oils or other lubricants, or otherwise t o pour water or the like for cooling. Further, cares shall be taken so that chips are not mixed with wearing powders of drill. The size of chips shall not be too thick and the length shall be about 5 mm max. Trea
14、ting of Sample Ali the chipped out sample (generally 50 g min.) ar2 collected and the mixed iron powders or th2 like are carefully removed by using a strong magnet. At last, they are Sufficiently mixed to be the sample for analysis. When the sampling of sample for analysis is defficult to conform to
15、 the above-mentioned specification, the sampling can be separately determined depending upon the agreements between the purchaser and the manufacturer. The sample for analysis-shall be put in a desiccator and let stand for 1 h or more. . Thereafter, it chail be weighed out. 3.5 Weighing of Samp1.e T
16、he weighing of sample shall be as follows: (i) On weighing ot the sample, cares shall be so taken that the sample represents average chemical composition by sufficiently mixing the sample. (2) The sample shall, as a rule, be weighed out by using a chemical balance and an anount near as specified amo
17、unt shall be weighed out to necessary places referring to the indicated ntimber of places of analytical value. 4. Expression of Analytical Value and Czution on ODeration 4.1 Expression of Analytical Value The analytical value shall be expressed by percentage and rounded off to places specified in JI
18、S C 2521 in accordance with JIS Z 8401. 4.2 Caution on Analytical Operation The caution on analytical operation shall be as follows: (i) The same sample shall be analyzed not less than 2 times and the result shall be confirmed. (2) When analyzing, a blank test shall be carried out over all operotion
19、s and the measured value shall be corrected. - 2 - Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 22:32:21 MDTNo reproduction or networking permitted without license from IHS -,-,- 5. Meth
20、od for Determination of Copper 5.1 Classification of Methods The method for determination of copper shall be in accordance with electrogravimetric analysis method. 5.2 Electrogravimetric Analysis Method 5.2.1 Summary After decomposing a sample with the mixed solution of nitric acid and sulfuric acid
21、, it is electrolyzed by using a platinum electrode and copper is deposited on a cathode, mass is measured (the electrolytic residual liquid can be used for determination of nickel). Then, its weighed out. Reagents Mixed acid 20 ml of water is added with 5 ml of sulfuric acid while mixing them with s
22、tirring and cooled, Thereafter, it is added with 5 ml of nitric acid and sufficiently mixed. Ethyl alcohol (95 v/v X ) Devices The following devices shall, as a rule, be used. Electrolytic beaker (refer to Fig. i) Platinum electrode A (refer to Fig. 2) Platinum electrode B (refer to Fig. 3 ) Semicir
23、cular watch glass (refer to Fig. 4 ) Weighing-Out Amount of Sample The reagents shall be as follows: 1 g of the sample shall be 5.2.5 Operation The determination operation shall be carried out according to the following procedures: (1) Weigh out a sample, transfer it into an electrolytic beaker, cov
24、er that with a watch glass, add 30 ml of mixed acid and quietly decompose it at as low temperature as possible. I After completion of decomposition, allow it completely to be solution by carefully heating and expel nitrogen oxide, After washing the bottom surface of watch glass and the inside wall o
25、f beaker, dilute it to about 150 ml by adding water. (2) Allow the platinum electrode A the mass of which is preliminarily measured to be a cathode, utilize a platinum electrode B as an anode, cover them with two semicircular watch glasses, apply a current of 0.3 to 0.4 A at a liquid temperature of
26、20 to 30C (when the temperature of liquid decrease to less than 20C, the beaker is heated with a suitable heater) and electrolyze it for one night. - 3 - Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale
27、, 03/15/2007 22:32:21 MDTNo reproduction or networking permitted without license from IHS -,-,- (3) Wash the bottom surface of watch glass, the inside. wall of beaker and the pzrt of the handle of electrode exposed above the liquid surface with a small amount of water, raise the surface of electroly
28、te by about 5 mm with that washing water and further continue to electrolyze it for about 30 minutes. (4) When copper is not deposited any more longer on the handle of cathode newly dipped in the electrolyte, gradually draw up both electrodes while washing them with water as current is applied, at l
29、ast quickly dip them into new water and remove the cathode (the electrolytic residual solution may be used for determination of nickel). (5) Raise and lower the cathode several times and wash it with water, thereafter, sufficiently wash it by using ethyl alcohol, immediately quickly dry it in an air
30、 bath at about 80C and allow it t o stand to cool in a desiccator for about 30 minutes. Thereafter, measure its mass. 5.2.6 Calculation The content of copper in sample shall be calculated from the following formula: W Copper ( X ) = -xi00 . IV where EU: mass of copper deposited on cathode (g) W : we
31、ighed-out amount of sample.(g) Fig. 1. Electrolytic Beaker Unit: 1 L I I 955 mm 7 Fig. 2. Platinum Electrode A Unit: mm I II 1 in dialieter of hole e- , I Cylinder formed from a vire of 120 m in length - 4 - Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS
32、Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 22:32:21 MDTNo reproduction or networking permitted without license from IHS -,-,- STD-JIS H 3433-ENGL L77b 4733b08 0544835 b33 = JAPArdnoE rq =-* STANDARDS ASSOC?IAPi6H Fig, 3. Platinum Electrode B Fig. 4. Sesicircular Watch Glass U
33、nit: mm I i - y f t 6. Method for Determination of Nickel 6.1 Classification of Methods The method for determination of nickel shall be in accordance with either one of the following methods: (1) Titrimetric method (2) Gravimetric method 6.2 Titrimetric Method 6.2.1 Summary Decompose the sample with
34、 mixed acid, electrolyze Add tartaric acid it according to 4 . and separate copper or the like. and ammonium chloride to the electrolytic residual liquid, make it alkaline with aqueous ammonia and deposit nickel by adding dimethylglyoxime. dissolve the precipitate by heating. titrate it with zinc st
35、andard solution. Thereafter, wash it with hydrochloric acid and Add EDTA and EBT thereto and 6.2.2 Reagents The reagents shall be as follows: (i) Hydrochloric acid (i + 1, 1 + 50) (2) Mixed acid It shall conform to 5.2.2 ( 1 ) . (3) Aqueous ammonia ( 4 ) Aqueous ammonia (i + i) - 5 - Copyright Japan
36、ese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 22:32:21 MDTNo reproduction or networking permitted without license from IHS -,-,- (5) hmonium chloride solution (25 wlvX) (6) Tartaric acid solution (25 w/
37、vX) (7) Dimethylglyoxime solution 1.0 g of dimethylglyoxime is dissolved in 100 ml of sodium hydroxide solution (1 w/v%). ( 8 ) M/50 zinc standard solution 1.308 g of metallic zinc (99.99% min., corresponding to extra grade of JIS H 21073 is accurately weighed out, decomposed by heating with as smal
38、l amount of hydrochloric acid (i + i) as possible and cooled. Thereafter, it is transferred into a measuring flask of 1000 ml and diluted u? to the marked line with water. (9) M/50 disodium ethylenediamine t et rzacetat e (EDTA) standard solution 7.45 g of disodium ehylenediaminetetraacetate (2 hydr
39、ate) is dissolved in water and accurately diluted to 1 1 . The standardization of titer is carried out as follows: 25 ml of M/50 EDTA standard solution is separately taken, added with 10 ml of ammonium chloride solution (25 v/vW) and 0.1 ml of EBT indicator and the amount of solution is diluted to a
40、bout 100 ml with water. aqueous ammonia (i + 1) until the solution becomes blue, titrated with M/50 zinc standard solution and the point where the blue of solutidn has turned to red purple is taken as the end point. The titer of M/50 EDTA standard solution is calculated from the following formula: T
41、hereafter, it is dropped with V 25 F=- where F: titer of 81/50 EDTA standard solution v: used amount of M/50 zinc standard solution (mi) (10) Eriochrome Black T (EBT) solution 0.5 g of Eriochrome Black T and 4.5 g of hydroxylamine hydrochloride are dissolved in ethyl aclcohol to 100 ml. This solutio
42、n can be used for about 6 months. 6.2.3 Weighing-Out Amount of Sample 1 g of the sample shall be weighed out. 6.2.4 according (1) Operation The determination operation shall be carried out to the following procedures: Weigh out a sample, transfer it into an electrolytic beaker, cover it with a watch
43、 glass, add 30 ml of mixed acid and decompose it by heating. Thereafter, electrolyze it according to 5.2 electrogravimetric analysis method of copper, as appropriate, and remove ( l ) copper. - 6 - Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/
44、1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 22:32:21 MDTNo reproduction or networking permitted without license from IHS -,-,- Transfer the electrolytic residual liquid into a measuring flask of 250 ml and dilute it up to the marked line with water, Thereafter, separately take a fixed a
45、mount (2) (3) thereof into a beaker (500 m i ) . Add 10 ml of tartaric acid solution (4) and 20 ml of ammonium chloride solution thereto, then drop aqueous ammonia until the solution turns clear blue, further add 5 ml thereof in excess and dilute it to about 250 ml with water. Heat the solution to a
46、bout 90C, add dimethylglyoxime solution at a rate of 7 ml per 10 mg of nickel unticipated content mixing them, further add 5 ml in excess and sufficiently mix them with stirring. Thereafter, let it stand for about 20 minutes and precipitate nickel. Filter the precipitate by using a filter paper (Cla
47、s SA) and sufficiently wash it with warm water. precipitate on filter paper into the original beaker by pouring warm water and 10 ml of hot hydrochloric acid (l+l), wash the filter paper several times with warm water and warm hydrochloric acid (i + 50) and dissolve the precipitate by quietly heating
48、 it. Wash out the After accurately adding 10 ml of M/50 EDTA standard solution per 10 mg nickel anticipated content to this solution, further add 5 ml thereof in excess, mix them by shaking 2 to 3 times, add O. 1 mg of EBT solution as indicator, drop ( 5 ) aqueous ammonia (1 + 1) until the solution becomes blue, immediately titrate (6) it with M/50 zinc standard solution and allow the point where the solution turns red purple to be the end point. 6.2.5 Calculation The nickel content in sample shall be calculated