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1、J I S Z*390b 88 4933b08 0077bb3 b -. UDC 621.791.36.04:669.234.5:543 JIS JAPANESE INDUSTRIAL STANDARD. Methods for Chemical Analysis of Palladium Brazing Filler Metals Translated and Published by Japanese Standards Association Printed in Japan 11 s Copyright Japanese Standards Association Provided b
2、y IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/16/2007 00:06:09 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S Z*390b 88 m 4933608 0077664 8 I In the event of any doubt arising, the original Standard in Japanese is
3、 to be final authority. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/16/2007 00:06:09 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S Z*3Ob 88 4733608 0077665 T U
4、DC 621.791.36.04:669.234.5:543 JAPANESE INDUSTRIAL STANDARD J I S Methods for Chemical Analysis of Z 3906-1988 Palladium Brazing Filler Metals 1. Scope This Japanese Industrial Standard specifies the methods for determination of palladium , silver , copper , manganese, nickel , and lead specified in
5、 JIS Z 3267. 2. General Matters General matters common to the methods for chemical analysis shall be in accordance with JIS K 0050, JIS K 0115 and JIS K 0121. 3. SamDling. and Treating. of Analvtical -Samde 3.1 Sampling Method 3.1.1 A sample shall be taken in accordance with JIS Z 3900. 3.1.2 The sa
6、mple shall be made to represent mean quality, and cares shall be especially taken for segregation , contamination , etc. therefore. 3.2 Weighing of Sample 3.2.1 When a sample is weighed out, cares shall be taken for the sample to represent average composition by sufficiently mixing by stirring and f
7、urther, no mixing with foreign matter shall be confirmed. 3.2.2 The sample shall be weighed out to the nearest 0.1 mg by using a chemical balance. 4. Arrangement of Analytical Values 4.1 Number of Times of Analyses The same sample shall, as a rule, be analyzed not less than two times. 4.2 Blank Test
8、 When a sample is analyzed, a blank test shall be per- formed through all operations and the content shall be corrected. Applicable Standards : See page 18. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Res
9、ale, 03/16/2007 00:06:09 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S Z*390b 88 m 4933608 0077bbb L m Type (1) 2 Z 3906-1988 Component system Pd-Ag-Cu system Pd-Ag system 4.3 Indication of Analytical Value An analytical value shall be expressed by mass percentage.
10、Palladium, silver, copper, manganese and nickel shall Pd-1,2,4,6 be rounded off to one place of decimal, and lead to two places of decimals in accordance with JIS Z 8401 after averaging not less than two analytical values. palladium determination - filtrate (B) - ( 7 . 2 . 4 . 1 ) 5. Classification
11、bv Analvtical Samtde and Procedures of Analysis ( 2 ) Since the methods for chemical analysis of palladium brazing filler metals are in accordance with a systematic analytical method, the analytical sample of palladium brazing filler metals shall be classified into four types, and the sequence of an
12、alysis thereof shall be as given in the following table. Pd-Ag-Mn system Table. Classification by Analytical Sample and Sequence of Analysis (3) Pd-Cu-Mn-Ili System I Pd-Mn-Ni system Pd-Ni system Class of pal- ladium brazing Sequence of analysis Silver determination - filtrate (A) - (6.2.4) copper d
13、etermination I (8.2.4) Silver determination - filtrate (A) - palladium determination B Pd-7 (6.2.4) ( 7 . 2 . 4 . 1 ) (6.2.4) palladium determination - filtrate (B) - B Pd-9,10 ( 7 . 2 . 4 . 1 ) manganese determination (9.2.3.1 or 9.3.3) Palladium determination - filtrate (B) - ( 7 . 2 . 4 . 2 ) B P
14、d-12 copper determination - electrolytic residual liquid - manganese determination - sample ( 8 . 2 . 4 ) (9.2.3.2) solution (D) - nickel determination (10.2.3.2) Palladium determination - filtrate (BI - manganese determination - sample solution (Cl - ( 7 . 2 . 4 . 2 ) ( 9 . 2 . 3 . 1 ) B Pd-11 nick
15、el determination ( 1 0 . 2 . 3 . 1 ) Palladium determination - filtrate (BI - B Pd-14 ( 7 . 2 . 4 . 2 ) nickel determination ( 1 0 . 2 . 3 . 1 ) Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/16/2
16、007 00:06:09 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S Z*3Ob 88 4933b08 0077bb7 3 W 3 Z 3906-1988 6. Method for Determination of Silver m U 6.1 Determination Method The method for determination of silver shall be in accordance with silver chloride gravimetric me
17、thod. to types (1) and (2). This method applies 6.2 Silver Chloride Gravimetric Method 6.2.1 Summary Decompose a sample with nitric acid, and make palladium the ammine complex by adding aqueous ammonia in excess. . acidify slightly by using acetic acid and deposit silver chloride by adding hydrochlo
18、ric acid. glass filter. After drying, weigh the mass thereof Take the filtrate and washings as a filtrate (A), and use it for determination of palladium. . Thereafter, Filter the generated silver chloride by using a sintered- 6.2.2 Reagents The reagents shall be as follows: (1) Hydrochloric acid (1
19、+ 9) (2) Nitric acid (1 + 1, 1 + 100) (3) Aqueous ammonia (1 + 1) (4) Acetic acid 6.2.3 Weighing-out Amount of Sample 0.5 g of a sample shall be weighed out. 6.2.4 Operation The determinating operation shall be carried out in accordance with the following procedures : (1) Decomposition of Sample Wei
20、gh out a sample, transfer to a conical beaker (300 mi), add 20 ml of nitric acid (1 + i), cover with a watch glass, and decompose by heating. (2) Generation of Silver Chloride Precipitate a watch glass and the inner wall of a beaker, add water to the amount of liquid about 150 ml, and slightly alkal
21、ify by adding aqueous ammonia (1 + 1). Thereafter, add acetic acid (1 + 1) until the solution is slightly acidified. Add little by little hydro- chloric acid (1 + 9) with mixing by stirring the solution, and generate precipitates of silver hydrochloride. becomes to be generated, further add 1 ml the
22、reof in excess, sufficiently stir to mix, wash the bottom face of the watch glass and the inner wall of the beaker with water, and gently boil by heating for about 5 min. Wash the bottom face of After no precipitate (3) Filtration and Washing of Precipitates a dark place for one night, filter by usi
23、ng a sintered-glass filter (1 G 4) which has been preliminarily made constant mass, and sufficiently wash initially with nitric acid (1 + 100) and then with cold water Take the filtrate and washings as filtrate (A) and use it for determination of palladium of types (1) and (2). 1. After standing as
24、it is in Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/16/2007 00:06:09 MDTNo reproduction or networking permitted without license from IHS -,-,- 4 2 3906-1988 (4) Drying and Weighing of Precipit
25、ate Dry the precipitate together with the sintered-glass filter in an air bath at about 13OOC for about 1 h, and let stand to cool in a desiccator for about 1 h. Thereafter, weigh the mass, and repeat this operation to constant mass. 6.2.5 Blank Test Use only reagents, and operate in parallel to a s
26、ample in accordance with the procedures on and after 6.2.4 (1). and washings for the blank test of 7.2.5. following formula: Use the filtrate 6.2.6 Calculation Calculate the content of silver in a sample from the o - (.ni-mz) X O. 752 6 mo Silver wt /o - where ?fil: mass of silver chloride obtained
27、in 6.2.4 (g) m2: mass obtained in 6.2.5 (g) mo : weighing out amount of sample (g) 7. Method for Determination of Palladium 7.1 Determination Method The method for determination of palladium shall be in accordance with dimethylglyoxime palladium gravimetric method. method applies to the types of (1)
28、 and (2) and the types of (3) and (4). This 7.2 Palladium Dimethylglyoxime Gravimetric Method 7.2.1 Summary For the types of (1) and (2), add hydrochloric acid to the filtrate (A) obtained in 6.2.1 and boil. Thereafter, dilute with water. For the types of (3) and (4), decompose a sample with aqua re
29、gia, evaporate by heating to a sirupy state, add hydrochloric acid, and remove nitric acid by repeating this operation. Then, add hydrochloric acid, and dilute with water. Add dimethylglyoxime to the solution obtained by either of those operations, precipitate palladium complex, filter by using a si
30、ntered-glass filter, and dry. Thereafter, weigh the mass Take the filtrate washings as filtrate (B), and use for determination of copper or manganese, and nickel. 7.2.2 Reagents The reagents shall be as follows: (1) Hydrochloric acid (2) Hydrochloric acid (1 + 1) (3) Aqua regia (3 parts hydrochloric
31、 acid and one part nitric acid) (4) Dimethylglyoxime solution Dissolve 1. O g of dimethylglyoxime in 100 ml of ethanol (95 vol %). (5) Ethanol (95 vol %) Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale
32、, 03/16/2007 00:06:09 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S Z*390b 88 4933608 0077bb 7 m 5 2 3906-1988 7.2.3 Weighing-out Amount of Sample For the types of (1) and (2), use ail the amount of filtrate (A), and for the types of (3) and (4), weigh out 0.5 g of
33、a sample. 7.2.4 Operation 7.2.4.1 For Types of (1) and (2) For the types of (1) and (2) , . perform the determining operation in accordance with the following procedures : (4) Hydrochloric Acid Treatment Add 10 ml of hydrochloric acid to the solution (A) obtained in 6.2.4 (3), and gently boil by hea
34、ting for 5 to 10 min. with water. Thereafter, dilute to about 700 ml Generation of Palladium Dimethylglyoxime Precipitate Add dimethylglyoxime solution C7.2.2 (4)l by a rate of 3.0 ml per 0.01 g in palladium content with mixing the solution (l). After heating at 70 to 8OoC for about 20 min, allow to
35、 stand in a warm place for about 2 h. Filtration and Washing of Precipitate using a sintered-glass filter (2 G 4) which has been me- Filter the precipitate by liminarily made costant mass, wash sufficiently with arm water Take the filtrate and washings as filtrate (B) , and use for determination of
36、copper of type (1) and manganese of type (2). 1 , and further wash once with ethanol. Drying and Weighing of Precipitate with the sintered-glass filter in an air bath at about llOC for about 1 h, and allow to stand to cool in a desiccator for about 1 h. Thereafter, weigh the mass, and repeat this op
37、eration to constant mass (2). Dry the precipitate together Notes (l) Though the required calculated amount of dimethyl- glyoxime solution is 2.2 ml per 0.01 g of palladium, it is in excess required for complete precipitation. Since palladium dimethylglyoxime is slightly dissolved in water, when it i
38、s required to enhance precision, perform a parallel test by using a known synthetic sample, and correct a measured value of palladium. (2 ) 7.2.4.2 For Types of (3) and (4) Perform the determining operation for the types of (3) and (4) in accordance with the following procedures: (1) Decomposition o
39、f Sample Weigh out a sample, transfer to a beaker (200 mi), add 20 ml of aqua regia, cover with a watch glass, and decompose by heating. Thereafter, gently evaporate by heating to a sirupy state. (2) Denitration Add 10 ml of hydrochloric acid, and evaporate by heating again to a sirupy state. Repeat
40、 this operation 3 or 4 times. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/16/2007 00:06:09 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S Z*390b 88 M 4933b08 00
41、77b70 3 . 6 Z 3906-1988 (3) Hydrochloric Acid Dissolution Add 35 ml of hydrochloric acid (1 + 1) ( 3 1 , and dissolve the deposited salts. Thereafter, transfer to a beaker (1000 mi) by using water, and dilute to about 700 ml with water. ( 4) Generation and Separation of Palladium Dimethylglyoxime Pr
42、ecipitate Hereinafter, operate in accordance with the procedures of 7.2.4.1 (2) to (4). However, use the filtrate (B) obtained by the operation of 7.2.4.1 (3) for determination of copper of type (3) or manganese and nickel of type (4). Note ( 3 ) Acidity for generation of precipitate is preferably a
43、bout 0.3 mol/ i of hydrochloric acid because nickel coexists. 7.2.5 Blank Test Use only reagents and operate in parallel to a sample in accordance with the procedures on and after 7.2.4.1 (1) or 7.2.4.2 (1). Use the filtrate and washings for the blank test of 8.2.5. 7.2.6 Calculation the following f
44、ormula: Calculate the content of palladium in a sample from where ?HI : mass of palladium dimethylglyoxime obtained in 7.2.4.1 or 7.2.4.2 (g) m2: mass obtained in 7.2.5 (g) ?HO: weighing out amount of sample (g) 8. Method for Determination of Copper 8.1 Determination Method The method for determinat
45、ion of copper shall be in accordance with copper electrolysis gravimetric method. applies to the types of (1) and (3). This method 8.2 Comer Electrolvsis Gravimetric Method 8.2.1 Summary Add nitric acid to the filtrate (B) obtained in 7.2.1. After concentration, add sulfuric acid, evaporate by heati
46、ng, and generate white fume. and weigh the mass of copper deposited on a cathode (Use the electrolytic residual liquid for determination of manganese and nickel. ) . 8.2.2 Reagents The reagents shall be as follows: After standing to cool, add water and nitric acid to electrolyze, (1) Nitric acid (2)
47、 Nitric acid (1 + 1) (3) Sulfuric acid (1 + 1) (4) Ethanol (95 vol %) Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/16/2007 00:06:09 MDTNo reproduction or networking permitted without license fro
48、m IHS -,-,- JIS Z*3906 B B E 4933608 0077673 5 7 Z 3906-1988 8.2.3 Devices The following devices shall, as a rule, be used. (1) Electrolytic beaker (see Attached Fig. 1) (2) Platinum electrode A (see Attached Fig. 2) (3) Platinum electrode B (see Attached Fig. 3) (4) Semicircular watch glass (see Attached Fig. 4) 8.2.4 Operation The determining operation shall be carried out in ac- cordance with the following procedures : (1) Acid Treatment of Filtrate Respectively transfer the filtrate (B) obtained in 7.2.4.1 (3) fo