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MAIN EDITION

BUREAU OF ANALYSED SAMPLES LTD


Directors:-
R. P. MEERES, BA (Oxon), MRSC (Managing)
G. C. FLINTOFT, ACMA, CGMA (Company Secretary)
J. C. MEERES
M. S. TAYLOR, PhD, CChem, MRSC

BRITISH CHEMICAL STANDARD CERTIFIED REFERENCE MATERIAL

CERTIFICATE OF ANALYSIS
BCS-CRM No. 180/2
COPPER-NICKEL
Prepared under rigorous laboratory conditions and, AFTER CERTIFICATION ANALYSIS IN GREAT BRITAIN,
issued by the Bureau of Analysed Samples Ltd.

CO-OPERATING ANALYSTS
INDEPENDENT ANALYSTS ANALYSTS representing MANUFACTURERS and USERS
1 COPPINS, W. C., MSc, CChem, FRIC, 4 BALFOUR, B. E., AMet, MIM, Henry Wiggin & Co. Ltd., Hereford.
Ridsdale and Co. Ltd., Middlesbrough. 5 CADZOW, N. G., BSc, CChem, MRIC, Weir Pumps Ltd., Glasgow.
2 GOVENLOCK, R., CChem, MRIC, MIM, 6 CROSS, J., BSc, Yorkshire Imperial Metals Ltd., Leeds.
Midland Metallurgical Laboratories Ltd., Birmingham. 7 SAYCE, E. J., Serck Tubes, Birmingham.
GOVERNMENT DEPARTMENT 8 SALE, G., MIM, Thomas Bolton & Sons Ltd., Stoke-on-Trent.
3 NICHOLLS, H. A., CChem, FRIC,
Bragg Laboratory, Materials Quality Assurance Directorate, Sheffield.

ANALYSES
Mean of 4 values - mass content in %.
Analyst
Cu Ni Fe Mn S C
No.
1 68.13 30.33 0.68 0.75 0.007 0.039
2 68.11 30.38 0.68 0.76 0.007 0.042
3 68.14 30.39 0.67 0.76 0.006 0.038
4 68.20 30.26 0.67 0.77 0.008 0.039
5 68.13 30.44 0.67 0.74 0.006 0.037
6 68.09 30.41 0.71 0.75 0.006 0.05
7 68.13 30.30 0.68 0.76 0.006 0.039
8 68.03 30.32 0.69 0.74 0.006 0.038
MM 68.12 30.35 0.68 0.75 0.006 0.04
sM 0.05 0.07 0.02 0.02 0.001 0.01
The above figures are those which each Analyst has decided upon after careful verification.
The following additional information was supplied by Analyst No. 7:
Si 0.018%, Pb 0.003%, Co 0.005%.
MM: Mean of the intralaboratory means. sM: standard deviation of the intralaboratory means.

CERTIFIED VALUES (Cv)


mass content in %

Cu Ni Fe Mn S C

Cv 68.12 30.35 0.68 0.75 0.006 0.04

C(95%) 0.05 0.06 0.02 0.01 0.001 0.01


t sM
The half width confidence interval C(95%) = where “t” is the appropriate two sided Student’s t value at the 95% confidence level for “n” acceptable mean values.
n
For further information regarding the confidence interval for the certified value see ISO Guide 35:2006 sections 6.1 and 10.5.2.

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BCS-CRM 180/2 COPPER-NICKEL
NOTES ON METHODS USED
COPPER
All Analysts except No. 4 determined copper by electrolysis from an acid solution. No. 4 used a direct iodimetric method.
NICKEL
All Analysts except No. 6 determined nickel by precipitation with dimethylglyoxime after prior removal of copper. No. 1
dissolved the precipitate in dilute sulphuric acid, boiled with an excess of ferric sulphate and titrated the ferrous salt thus formed
with potassium dichromate. Nos. 3 and 4 completed by cyanometric titration. Nos. 2, 5, 7 and 8 completed gravimetrically by
filtering and weighing the organic complex. Analyst No. 6 determined nickel by electrolysis from an ammoniacal sulphate
solution.
IRON
Analysts Nos. 1 and 8 determined iron photometrically on the electrolyte from the copper determination. No. 1 used 1:10
phenanthroline after first separating iron by ammonia precipitation; No. 8 used a thiocyanate method. Analysts Nos. 2, 3, 4, 6 and
7 determined iron titrimetrically with dichromate solution after separation with ammonia, dissolving the precipitate in
hydrochloric acid and reducing with stannous chloride. No. 5 used atomic absorption spectroscopy.
Analyst No. 4 also used a thiocyanate photometric method and found 0.67%.
MANGANESE
Analysts Nos. 1, 6 and 7 determined manganese by oxidation with persulphate/silver nitrate and titration with arsenite/nitrite
(No. 1) or arsenite (Nos. 6 and 7). Analyst No. 2 used atomic absorption spectroscopy. Analysts Nos. 3, 4, 5 and 8 used
photometric methods involving oxidation with periodate (Nos. 3 and 8) or persulphate/silver nitrate (Nos. 4 and 5).
SULPHUR
Analyst No. 1 determined sulphur gravimetrically as barium sulphate after chromatographic separation on an alumina column
(Nydahl, Anal. Chem., 1954, 26, 580). All other Analysts used combustion methods. Nos. 2 and 4 analysed the evolved gases by
infrared absorption. No. 3 absorbed the sulphur gases in hydrogen peroxide and titrated with sodium borate solution. No. 5
absorbed in iodate/iodide solution and titrated with thiosulphate solution. No. 6 used the Strohlein method. No. 7 absorbed the
sulphur gases in hydrogen peroxide and titrated potentiometrically with sodium hydroxide solution. No. 8 completed
photometrically with rosaniline (Barabas & Kaminsky, Anal. Chem., 1963, 35, 1702).
CARBON
All Analysts determined carbon by combustion. Nos. 1, 3 and 5 completed by non-aqueous titration, Nos. 2 and 4 analysed
the evolved gases by infrared absorption, Nos. 6 and 7 used a titrimetric method with the Ströhlein apparatus and No. 8 completed
gravimetrically.

DESCRIPTION OF SAMPLE
Bottles of 100g chips graded 1700-250 micron (10-60 mesh) for chemical analysis.

INTENDED USE & STABILITY


The sample is intended for the verification of analytical methods, such as those used by the participating laboratories, for the
calibration of analytical instruments in cases where the calibration with primary substances (pure metals or stoichiometric
compounds) is not possible and for establishing values for secondary reference materials.
It will remain stable provided that the bottle remains sealed and is stored in a cool, dry atmosphere. When the bottle has been
opened the lid should be secured immediately after use. If the contents should become discoloured (e.g. oxidised) by atmospheric
contamination they should be discarded.

NEWHAM HALL, NEWBY, For BUREAU OF ANALYSED SAMPLES LTD


MIDDLESBROUGH, ENGLAND, TS8 9EA
Email: enquiries@basrid.co.uk R.P. MEERES,
Website: www.basrid.co.uk Managing Director

Preliminary Edition June 1975


Main Edition March 1976
Main Edition (revised with sM and C(95%) values for each certified element) August 2012

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