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Disclosure to Promote the Right To Information
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है”ह”ह
IS 4667-3 (2001): Chemical Analysis of Silver-CopperBrazing
Alloys, Part 3: Determination of Nickel [MTD 8:Copper and Copper
Alloys]
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IS 4667 ( Part 3 ) :2001
*wkfT %5-lFTmfTqT-l R&ww17r3k75rfaqhJl
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 )’.
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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
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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
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Bureau of Indian Standards
p!
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Review of Indian Standards
Amendments are issued to standards as the need arises onthebasis
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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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