BRITISH STANDARD BS 3727-6:

1964

Methods for
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The analysis of nickel

for use in electronic
tubes and valves —
Part 6: Determination of Copper
(Photometric Method)
 BS 3727-6:1964

Co-operating organizations

The Telecommunication Industry Standards Committee, under whose

supervision this British Standard was prepared, consists of representatives
from the following Government departments and scientific and industrial
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organizations:

Admiralty*
British Broadcasting Corporation*
British Electrical and Allied Manufacturers’ Association
British Institution of Radio Engineers*
British Radio Equipment Manufacturers’ Association*
British Radio Valve Manufacturers’ Association*
British Railways Board
Cable and Wireless Ltd.
D.S.I.R. — Radio Research Station
Electrical Contractors Association (Incorporated)
Electrical Research Association
Electricity Council, the Generating Board and the Area Boards in England and Wales
Electronic Engineering Association*
Electronic Valve and Semiconductor Manufacturers’ Association*
Institution of Electrical Engineers
Ministry of Aviation*
Ministry of Labour (H.M. Factory Inspectorate)
Post Office*
Radio and Electronic Component Manufacturers’ Federation*
Relay Services Association of Great Britain
Telecommunication Engineering and Manufacturing Association

The Government departments and scientific and industrial organizations

marked with an asterisk in the above list, together with the following, were
directly represented on the Committee entrusted with the preparation of this
standard:

Scientific Instrument Manufacturers’ Association

United Kingdom Atomic Energy Authority
Manufacturers of nickel alloys

This British Standard, having

been approved by the
Telecommunication
Industry Standards
Committee and endorsed
by the Chairman of the
Engineering Divisional
Council, was published
under the authority of
the General Council on
13 April 1964 Amendments issued since publication
© BSI 12-1999
Amd. No. Date Comments

The following BSI references

relate to the work on this
standard:
Committee references TLE/5,
TLE/5/3 and TLE/5/3/1
Draft for comment AB(TLE)4922

ISBN 0 580 03587 5

 BS 3727-6:1964

Contents

Page
Co-operating organizations Inside front cover
Foreword ii
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Introduction 1
Apparatus 1
Solutions required 1
Sampling 1
Calibration 1
Procedure 2

© BSI 12-1999 i
 BS 3727-6:1964

Foreword

This standard makes reference to the following British Standard:

BS 1499, Sampling non-ferrous metals.
This method for the determination of copper is the sixth of a series of methods
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which will form a complete British Standard under the collective title “Analysis
of nickel for use in electronic tubes and valves”, each method being published as
a separate part. Other parts in the series are as follows:
— Part 1: Aluminium1);
— Part 2: Boron1);
— Part 3: Carbon1);
— Part 4: Chromium;
— Part 5: Cobalt;
— Part 7: Iron;
— Part 8: Manganese;
— Part 9: Magnesium1);
— Part 10: Silicon 0.020–0.25 per cent;
— Part 11: Silicon 0.001–0.020 per cent1);
— Part 12: Sulphur1);
— Part 13: Titanium1);
— Part 14: Tungsten;
— Part 15: Zinc1).
These methods have been found to give reliable and reproducible results and are
primarily intended as reference methods to be used in cases of dispute.
A British Standard does not purport to include all the necessary provisions of a
contract. Users of British Standards are responsible for their correct application.

Compliance with a British Standard does not of itself confer immunity

from legal obligations.

Summary of pages
This document comprises a front cover, an inside front cover, pages i and ii,
pages 1 and 2 and a back cover.
This standard has been updated (see copyright date) and may have had
amendments incorporated. This will be indicated in the amendment table on the
inside front cover.

1) In course of preparation.

ii © BSI 12-1999
 BS 3727-6:1964

Introduction Solutions required

a) Principle. The sample is dissolved in nitric All reagents shall be of suitable purity2), distilled
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acid, sulphuric acid is added and the solution is water shall be used throughout and the solutions
evaporated to fumes of sulphuric acid. The cooled shall be freshly prepared.
residue is diluted with water, the solution is Standard copper solution. Dissolve 100 mg of pure
adjusted to pH 6.8–7.0. The copper is reduced to copper in 5 ml of nitric acid (50 per cent v/v), boil
the cuprous state and 2 : 2½ diquinolyl, in gently to remove nitrous fumes, then dilute with
iso-amyl alcohol, is added. The coloured copper water to 1 litre in a graduated flask.
complex is extracted into the iso-amyl alcohol and
Dilute 50 ml of this primary copper solution
the optical density is determined.
to 500 ml with water in a graduated flask to give the
b) Range. 0.002 to 0.20 per cent copper. standard copper solution (1 ml contains 10 4g of
c) Reproducibility. Experiments have been copper).
carried out independently by a number of Nitric acid (50 per cent v/v). Dilute 500 ml of nitric
analysts, using the method recommended in this acid (sp. gr. 1.42) to 1 litre.
standard. The degree of reproducibility that can
Sulphuric acid (50 per cent v/v). To 50 ml of water
be expected is shown by the following analysis of
add, cautiously, 50 ml of sulphuric acid
the results obtained:
(sp. gr. 1.84), mix and cool.
Copper content Standard
per cent deviation
Buffer solution. Dissolve 10 g of tartaric acid
in 50 ml of ammonia solution (sp. gr. 0.88) or 70 ml
0.02 0.002 of ammonia solution (sp. gr. 0.91) and dilute the
0.20 0.01 solution to 100 ml with water.
d) Application. This method is applicable to 2 : 2½ Diquinolyl (0.05 per cent w/v). Dissolve 50 mg
nickel primarily intended for use in electronic of 2 : 2½ diquinolyl in 100 ml of iso-amyl alcohol.
devices. Such nickel contains not more than:
Sampling
Aluminium 0.1 per cent
Recommended methods of obtaining a suitable
Chromium 0.03 per cent
sample for the analytical procedure given below are
Cobalt 1 per cent described in BS 1499, “Sampling non-ferrous
Copper 0.2 per cent metals”.
Iron 0.25 per cent
Manganese 0.25 per cent Calibration
Magnesium 0.15 per cent Weigh 100 mg of copper-free nickel (e.g. carbonyl
Silicon 0.25 per cent nickel powder) into each of six 100 ml beakers.
Dissolve each sample in 2 ml of nitric
Titanium 0.03 per cent acid (50 per cent v/v), add 0, 2.0, 4.0, 6.0, 8.0
Tungsten 5 per cent and 10.0 ml of the standard copper
solution (1 ml N 10 4g of copper) to the separate
Apparatus beakers, then proceed with each as follows:
a) Grade A graduated glassware shall be used Add 2 ml of sulphuric acid (50 per cent v/v) and
throughout. evaporate to fumes of sulphuric acid. Cool, dilute to
b) Any instrument suitable for measuring the about 10 ml with water, then warm gently to
optical density of the solution at a wavelength dissolve salts. Cool and adjust the solution to
of 550 m4 may be used. pH 6.8–7.0 by the addition of ammonia solution
(sp. gr. 0.88 or 0.91) and sulphuric
If a filter photometer is used, the filter combination acid (50 per cent v/v); use indicator paper with a
should conform as closely as possible to the above range of 6.6–8.0 pH. Add 1 g of hydroxyammonium
wavelength. The following conditions have been chloride, heat on a steam-bath until the solution
found suitable: reaches the temperature of the bath, then heat for a
Mercury vapour lamp with Wratten 74 and Hilger further 5 minutes.
H503 or equivalent filters. Cell size 1 cm.

2) Analytical grade reagents have been found suitable.

© BSI 12-1999 1
 BS 3727-6:1964

Cool in a water-bath to room temperature, Plot the optical density values obtained against
add 5.0 ml of the buffer solution, readjust the percentage copper (based on the sample weight
solution to pH 7.0 with sulphuric subsequently used) and prepare calibration graphs.
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acid (50 per cent v/v), transfer to a separating

funnel (100 ml) and dilute to 60–70 ml with water. Procedure
Add 10.0 ml of 2 : 2½ diquinolyl
a) Up to 0.10 per cent copper. Weigh 100 mg of
solution (0.05 per cent w/v) from a burette, stopper
the sample and transfer to a 100 ml beaker.
the separating funnel and shake vigorously
Carry a blank determination through the entire
for 2 minutes. Allow the two layers to settle
procedure. Add 2 ml of nitric
for 5 minutes, then run off and discard the lower acid (50 per cent v/v) and warm gently until the
aqueous layer; dry the inside of the separating sample has dissolved. Add 2 ml of sulphuric
funnel stem with a roll of filter paper. Transfer the
acid (50 per cent v/v) and proceed as described
coloured organic layer, via a dry filter paper3), into
under “Calibration”.
a dry 1 cm cell.
Obtain the percentage copper in the sample by
Measure the optical density at 20 ± 1 °C
reference to the calibration graph.
immediately, using the conditions specified under
“Apparatus”. Use the blank solution in the b) 0.10 to 0.20 per cent copper. Weigh 50 mg of the
compensating cell. sample and continue as a) above.

3)
A Whatman No. 541 : 9 cm paper has been found suitable.

2 © BSI 12-1999
 Licensed copy: I P, The University of Leeds, Version correct as of 07/04/2013 09:53, (c) The British Standards Institution 2013

blank
 BS 3727-6:
1964
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