BRITISH STANDARD BS 3727-21:

1966

Methods for
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The analysis of nickel

for use in electronic
tubes and valves —
Part 21: Determination of Magnesium
(Atomic Absorption Method)
 BS 3727-21:1966

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:

British Broadcasting Corporation*

British Electrical and Allied Manufacturers’ Association
British Radio Equipment Manufacturers’ Association*
British Radio Valve Manufacturers’ Association*
British Railways Board
Cable and Wireless Ltd.
Crown Agents for Overseas Governments and Administrations
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
Institution of Electronic and Radio Engineers*
Ministry of Aviation*
Ministry of Defence, Navy Department*
Ministry of Labour (H.M. Factory Inspectorate)
Post Office*
Radio and Electronic Component Manufacturers’ Federation*
Relay Services Association of Great Britain
Science Research Council Radio and Space Research Station
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

This British Standard, having United Kingdom Atomic Energy Authority
been approved by the
Telecommunication Industry
Manufacturers of nickel alloys
Standards Committee and
endorsed by the Chairman of
the Engineering Divisional
Council, was published under
the authority of the General
Council on
31 January 1966 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,
TLE5/3, and TLE5/3/1
Draft for comment D64/10211

ISBN 0 580 03687 1

 BS 3727-21:1966

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
Notes 2

© BSI 12-1999 i
 BS 3727-21:1966

Foreword

This standard makes reference to the following British Standard:

BS 1499, Sampling non-ferrous metals.
This method for the determination of magnesium (atomic absorption method) is
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the twenty-first of a series of methods 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 methods in
the series are as follows:
— Part 1: Aluminium1);
— Part 2: Boron1);
— Part 3: Carbon1);
— Part 4: Chromium;
— Part 5: Cobalt;
— Part 6: Copper;
— 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 cent;
— Part 12: Sulphur1);
— Part 13: Titanium;
— Part 14: Tungsten;
— Part 15: Zinc1);
— Part 16: Determination of Free and Combined Magnesium1);
— Part 17: Not yet allocated;
— Part 18: Not yet allocated;
— Part 19: Not yet allocated;
— Part 20: Spectrographic methods;
— Part 22: Zinc (Atomic Absorption Method)1).
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

Introduction
a) Principle. The magnesium is determined by
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measurement of the absorption of magnesium
radiation, at 2852.1 ,, when a solution of the
sample in nitric acid is sprayed into a flame.
Strontium nitrate is added to the solution to
minimize interference from aluminium.
b) Range. 0.002 to 0.15 per cent magnesium.
c) Reproducibility. Experiments have been
carried out independently by a number of
analysts using the method recommended in the
standard. The degree of reproducibility that can
be expected is shown by analysis of the results
obtained to conform to a standard deviation
of 0.001 per cent magnesium over the entire
range.
d) Application. These methods are applicable to
nickel primarily intended for use in electronic
devices. Such nickel contains not more than:
Aluminium 0.1 per cent
Chromium 0.03 per cent
Cobalt 1 per cent
Copper 0.2 per cent
Iron 0.25 per cent
Manganese 0.25 per cent
Magnesium 0.15 per cent
Silicon 0.25 per cent
Titanium 0.03 per cent
Tungsten 5 per cent
Apparatus
a) Class A volumetric glassware shall be used
throughout.
b) An atomic absorption spectrophotometer
capable of selection and measurement of the
intensity of magnesium radiation at a
wavelength of 2852.1 ,. This apparatus consists
of a light source, an atomizer and burner
assembly, a monochromator and a detector.
The light source shall be a hollow cathode lamp,
with a magnesium cathode supplied with a
stabilized but adjustable current.
The burner should have a slightly air-rich flame and
burn either coal gas, butane, propane or acetylene.
(No single burner will burn all these gases
successfully.)
The monochromator should permit resolution of the
wavelength of interest from other radiation in the
region; a half-band pass of 5 , is adequate.
2) Analytical grade reagents have been found suitable.
© BSI 12-1999
BS 3727-21:1966
The detecting system shall be capable of responding,
with adequate sensitivity, to the radiation from the
lamp after passing through the flame and
monochromator. It shall be capable of detecting a
change in intensity of incident radiation
of 0.2 per cent.
The complete apparatus shall be capable of
measuring a content, or a change of content,
of 0.01 p.p.m. of magnesium in an aqueous solution.
Solutions required
All reagents shall be of a suitable purity2), distilled
water shall be used throughout and the solutions
shall be freshly prepared.
Standard magnesium solution. Dissolve 375 mg of
pure magnesium metal in 5 ml of hydrochloric acid
and dilute to 1 litre. Pipette 10 ml of this solution
into a 1 litre flask, dilute to the mark with water
and mix (1 ml contains 3.75 Èg Mg).
Nitric acid (50 per cent v/v). Add to 250 ml
water, 250 ml nitric acid (d 1.42) and mix.
Hydrochloric acid. d 1.16 to 1.18.
Strontium nitrate solution. Dissolve 0.25 g
strontium nitrate (anhydrous) in 1 litre of water.
Sampling
Recommended methods of obtaining a suitable
sample for the analytical procedure given below are
described in BS 1499, “Sampling non-ferrous
metals”.
Calibration
Weigh 25 mg of magnesium-free nickel
(e.g. carbonyl nickel powder) into each of six 50 ml
beakers. Dissolve each in 2 ml nitric
acid (50 per cent v/v) by gently warming and
transfer the solutions to six 25 ml volumetric flasks.
Make additions of standard magnesium solution to
the six flasks as follows: 0, 1.0, 2.5, 5.0, 7.5
and 10 ml.
Add 5.0 ml of strontium nitrate solution (Note 1) to
each flask.
Dilute to the mark with water and mix (Note 2).
Spray water into the flame and adjust the
measuring system to give a full scale reading. Spray
in the standard solutions in turn and record the
change in reading (Note 3). Spray in water between
each standard solution.
Prepare a calibration curve; the change in reading
being plotted against percentage magnesium.
1
 BS 3727-21:1966
Procedure
A sample of magnesium-free nickel shall be carried
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through the entire procedure and, where necessary,
appropriate correction for the magnesium in the
reagents made to the results.
a) Samples containing < 0.05 per cent silicon,
tungsten absent. Weigh 25 mg of sample into
a 50 ml beaker, add 2 ml nitric
acid (50 per cent v/v) and warm gently to
dissolve. Transfer to a 25 ml volumetric flask,
add 5.0 ml of strontium nitrate solution (Note 1),
dilute to the mark with water and mix.
Spray water in the flame and adjust the
measuring system to give a full scale deflection.
Spray in the sample solution and record the
change in reading (Note 3).
Obtain the percentage magnesium in the sample
by reference to the calibration graph.
3) A Whatman 540 paper has been found suitable.
2 © BSI 12-1999
b) Samples containing tungsten or > 0.05 per cent
silicon. Weigh 25 mg of sample into a 50 ml
beaker, add 2 ml nitric acid (50 per cent v/v) and
warm gently to dissolve. Add 2 ml hydrochloric
acid and evaporate to dryness. Dissolve the
residue in 2 ml nitric acid (50 per cent v/v), dilute
with about 10 ml water, filter3), wash with water,
transfer filtrate and washings to a 25 ml
volumetric flask add 5.0 ml strontium nitrate
solution (Note 1), dilute to the mark with water
and mix. Continue as in a).
Notes
1. With some types of flame, there is no interference
in the magnesium determination from amounts of
aluminium up to 0.1 per cent. In such cases, the
strontium nitrate addition may be omitted.
2. With many types of flame, there is no interference
in the magnesium determination from the nickel. In
such cases, the nickel may be omitted from the
solutions used in the calibration.
3. Further readings may be required according to
the stability of the apparatus.
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blank
 BS 3727-21:
1966
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