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IS 4667-3 (2001): Chemical Analysis of Silver-CopperBrazing Alloys, Part 3: Determination of Nickel [MTD 8:Copper and Copper Alloys]

IS 4667 ( Part 3 ) :2001

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CHEMICAL

Indian Standard. . .

ANALYSIS OF SILVER-COPPERBRAZING ALLOYS

PART 3 DETERMINATION OF NICKEL

ICS 77.120.01

(3 BIS 2001

BUREAU OF INDIAN STANDARDSMANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

April 2001 Price Group 1

‘“ “-d

Methods of Chemical/ Instrumental Analysis of Non-Ferrous Metals Sectional Committee, MTD 28

1’

\f,:

r:

t.,’FOREWORD

~.~

1!This Indian Standard ( Part 3 ) was adopted by the Bureau of Indian Standards, atler the drafl finalized by the

‘,

Methods of Chemical Anaylsis of Non-Ferrous Metals Sectional Committee had been approved by the Metallurgical! ‘.

Engineering Division Council.

IS 2927: 1975 ‘Specification for brazing alloy s’covers 22 grades of silver-copper brazing alloys. In order todetermine correctly the composition of different copper-silver brazing alloys, method of analysis have been describedin various parts of this standard.

The determination of silver and copper in silver-copper brazing alloys except BACuAg7 and BACuAg8 iscovered in IS 4667 ( Part 1 ) : 1968 ‘Methods of chemical analysis of silver copper brazing alloys: Part 1 Analysisof silver and copper’.

The determination of silver, copper and tin in BACuAg 7 and BACuAg8 alloys are covered in IS 4667( Part 2 ): 1969 ‘Methods of chemical analysis of silver copper brazing alloys: Part 2 Determination of silver, copperand tin’.

The determination of silver, copper, cadmium and zinc by ~ectrolytic method are covered in IS 4667 ( Part 4 ) :2001 ~.

‘Chemical analysis of silver-copper brazing alloys: Part 4 Determination of silver, copper, cadmium and zinc —Electrolytic method’.

,’

This part covers the determination of nickel by dimethylglyoxime method.

In reporting the result of a test or analysis made in accordance with this standard, if the final value observedor calculated, is to be rounded off, it shall be done in accordance with IS 2: 1960 ‘Rules for rounding off numericalvalues ( revised )’.

f ,.—

IS 4667( Part 3 ): 2001

Indian Standard

CHEMICAL ANALYSIS OF SILVER-COPPERBRAZING ALLOYS

PART 3 DETERMINATION OF NICKEL

1 SCOPE

This standard ( Part 3 ) describes the method fordetermination of nickel in silver-copper brazing alloysin the range from 0.5 to 3.5 percent by thedimethylglyoxime method.

2 REFERENCES

The Indian Standards listed below contain provisionswhich through reference in this text, constituteprovisions of this standard. At the time of publication,the editions indicated were valid. All standards aresubject to revision, and parties to agreement basedon this standard are encouraged to investigate thepossibility of applying the most recent editions of thestandards indicated below:

IS No.

266:1993

1070:1992

2927:1975

4667(Part l):1968

3 SAMPLING

Title

Sulphuric acid ( third revision)

Reagent grade water— Specification( third revision)

Specification for brazing alloys (jirstrevision )

Methods of chemical analysis ofsilver copper brazing alloys: Part 1Analysis of silver and copper

The sample shall be drawn and prepared as per themethod specified in IS 2927.

4 QUALITY OF REAGENTS

Unless specified otherwise, analytical grade reagentsand reagent grade water shall be employed for thetest (see IS 1070).

5 DETERMINATION OF NICKEL BYDIMETHYLGLYOXIME METHOD

5.1 Outline of the Method

After removal of silver, copper and cadmium, nickelis precipitated by dimethylglyoxime, filtered, dried andweighed.

5.2 Reagents

5.2.1 Sulphuric Acid ( see IS 266).

1

5.2.2 Hydrogen Stdphide — gas.

5.2.3 Hydrogen Sulphide Wash Solution — Acidi@1000 ml of distilled water with 10 ml of sulphuric acidand saturate with hydrogen sulphide gas.

5.2.4 Dilute Hydrochloric Acid— 1:1 (v/v).

5.2.5 Tartaric Acid Solution (250 g/1) — Dissolve250 g oftartaric acid in 600 ml of water and dilute to1 litre with water.

5.2.6 Ammonium Hydroxide Solution — rd = 0.90.

5.2.7 Dimethylglyoxime Solution (10 @l)— Dissolve10 g of dimethylglyoxime in ethanol and dilute to1 litre with ethanol.

5.3 Procedure

5.3.1 To the electrolyte after removal of silver andcopper as per 5.4.3 of IS 4667 ( Part 1 ) :1968, add8 ml of sulphuric acid and evaporate to dense whitefumes. Cool to room temperature, dilute to about100 ml with water and heat to boiling and pass arapid stream of hydrogen sulphide gas for about20 to 30 min. Allow the precipitate to settle for about3t04h.

5.3.2 Filter through medium textured filter paperand wash with hydrogen sulphide wash solution for5-6 times. Preserve the filtrate.

5.3.3 Dissolve the precipitate in warm dilutehydrochloric acid (1 : 1) and collect the solution inthe original beaker in which cadmium was precipitated.Wash the paper thoroughly with hot water till acidfkee. Add 8 mI of sulphuric acid and evaporate towhite fhmes, cool to room temperature and dilute toabout 100ml. Heat the solutionto boiling. Reprecipitatethe cadmium by passing a rapid stream of hydrogensulphide gas for about 20-30 min. Allow the precipitateto settle.

NOTE — Proper safety precaution shall be taken while

handling hydrogen sulphide gas,

5.3.4 Filter through medium textured filter paper andwash hydrogen sulphide wash solution for 7-8 times.Preserve the filtrate.

5.3.5 Combine the filtrate from 5.3.2 and 5.3.4 and

IS 4667( Part 3 ) :2001

boil to remove hydrogen sulphide. Adjust the volumeto about 150 ml and add 10 ml of tartaric acid solution,neutralize with ammonium hydroxide solution, add10 ml of ammonium hydroxide solution in excess andheat to about 80”C.

5.3.6 Add 25 ml of dimethylglyoxime solution, stirvigorously and allow to cool to room temperature,stirring occasionally. Let the precipitate settle overnight.

5.3.7 Filter the precipitate through a 30-ml sinteredglass crucible of medium porosity and wash with coldwater. Preserve the filtrate for the estimation of zinc.

5.3.8 Dry the precipitate at 150°C to constant mass.Cool in a desiccator and weigh as nickeldimethylglyoxime.

5.4 Calculation

m x 0.2032Nickel, percent by mass= x 100

M

where

m = mass, in g, of nickel dimethylglyoxime; and

M = mass, in g, of sample taken.

.

2

Bureau of Indian Standards

p!

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‘\

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Review of Indian Standards

Amendments are issued to standards as the need arises onthebasis of com~ents. Standards are also-reviewedperiodically; a standard along with amendments is reaffirmed when such mdviewindicates that no changes areneeded; if the review indicates that changes are needed, it is taken up for revision. Users of Indian Standardsshould ascertain that they are in possession of the latest amendments or edition by referring to the latest issueof ‘BIS Catalogue’ and ‘Standards: Monthly Additions’.

This Indian Standard has been developed from Doc : No. MTD 28 ( 3887 )

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

..

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