MAIN EDITION

BUREAU OF ANALYSED SAMPLES LTD

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

BRITISH CHEMICAL STANDARD CERTIFIED REFERENCE MATERIAL

CERTIFICATE OF ANALYSIS
BCS†/SS‡-CRM No. 453/1
CARBON STEEL (Residual Series)
Prepared under rigorous laboratory conditions and, AFTER CERTIFICATION ANALYSIS IN GREAT BRITAIN AND
NORWAY, issued by the Bureau of Analysed Samples Ltd.

CO-OPERATING ANALYSTS
INDEPENDENT ANALYSTS ANALYSTS representing MANUFACTURERS and USERS (cont.)
1 PICKERING, J. L., CChem, MRSC, Ridsdale and Co. Ltd., Middlesbrough. 7 DOUGHTY, A., APV Paramount Ltd., Crawley.
2 SMITH, P. B., BSc, PhD, CChem, FRSC, BCIRA, Birmingham. 8 DYSON, R. W., BSC Sheffield Laboratories, Sheffield.
3 SNEDDON, J., BCIRA Scottish Laboratories, Blantyre. 9 HOBSON, J. D., BSc, PhD, AMet, CChem, FRSC, Hadfields Ltd., Sheffield.
GOVERNMENT DEPARTMENT 10 HUGHES, H., BSc, PhD, BSC Teesside Laboratories, Middlesbrough.
4 NICHOLLS, H.A., CChem, FRSC, 11 JENKINS, R. H., LRSC, BSC Welsh Laboratories, Port Talbot.
Bragg Laboratory, Materials Quality Assurance Directorate, Sheffield. 12 KIDMAN, L., AMet, MIM, BSC Rotherham Works, Rotherham.
ANALYSTS representing MANUFACTURERS and USERS 13 MATHIESON, V., BSC Craigneuk Works, Motherwell.
5 AMBROSE, A. D., BSc., BSC Corby Works, Corby. 14 SEWELL, M., AMet, BA, BSC River Don and Associated Works, Sheffield.
6 CUNNINGHAM, A., LRSC, BSC Ravenscraig Works, Motherwell. 15 TORDHOL, L., A/S Raufoss Ammunisjonsfabrikker, Raufoss, Norway.

ANALYSES
Mean of 4 values - mass content in %.
Analyst
C Si Mn P S Cr Mo Ni As Cu Sn Ti W Pb
No.
1 0.157 0.34 1.40 0.041 0.026 0.26 0.078 0.107 0.050 0.104 0.023 0.074 0.29 0.0001
2 0.167 0.35 1.35 0.047 0.026 … … … … … … … … …
3 0.164 0.33 1.39 0.043 0.027 … … … … … … … … …
4 … … … … … 0.27 0.084 0.115 … … … 0.075 0.30 …
5 … … … … … … … … 0.053 0.097 0.022 0.072 … …
6 … 0.35 … … 0.026 … … 0.107 … … 0.024 … … …
7 … … … … … 0.25 … … … … … 0.071 0.30 …
8 … 0.34 … … … … 0.077 0.105 … … 0.022 … … …
9 0.157 … 1.37 0.043 … … … 0.107 … 0.098 0.021 … … …
10 … … … … … 0.26 … … 0.056 … … … … …
11 0.159 … … … … 0.26 … … … … … 0.073 0.31 …
12 0.155 … 1.38 … 0.026 0.25 0.079 … 0.053 0.097 0.022 0.071 0.28 …
13 … … … … … 0.27 0.090 0.108 … … … … … …
14 … … 1.37 0.043 0.027 … 0.076 … 0.049 0.100 … … … …
15 … 0.34 … 0.045 0.027 … … … … … … … … …
MM 0.160 0.34 1.38 0.044 0.026 0.26 0.081 0.108 0.052 0.099 0.022 0.073 0.30 …
sM 0.005 0.01 0.02 0.003 0.001 0.01 0.006 0.004 0.003 0.003 0.002 0.002 0.02 …
The above figures are those which each Analyst has decided upon after careful verification.
Figures in bold type certified, figures in small italic type only approximate.
MM: Mean of the intralaboratory means. sM: standard deviation of the intralaboratory means.
CERTIFIED VALUES (Cv)
mass content in %
C Si Mn P S Cr Mo Ni As Cu Sn Ti W
Cv 0.160 0.34 1.38 0.044 0.026 0.26 0.081 0.11 0.052 0.099 0.022 0.073 0.30
C(95%) 0.005 0.01 0.02 0.003 0.001 0.01 0.006 0.01 0.004 0.004 0.002 0.002 0.02
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.

N.B. Due to slight segregation of certain elements an area 6mm in diameter in the centre of the disc samples should be avoided
for emission spectroscopy.
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 BCS/SS-CRM No. 453/1 CARBON STEEL (Residual Series)
NOTES ON METHODS USED
CARBON
Analysts Nos. 1, 2 and 3 determined carbon by non aqueous titration according to the British Standard Carbon Method 4*. Nos. 9 and 11 used coulometric methods
according to Hobson and Leigh, Analyst, 1974, 99, 93 and Boniface and Jenkins, Analyst, 1971, 96, 37 respectively. No. 12 used the low pressure British Standard Carbon
Method 3*.
Analyst No. 9 also determined carbon by non aqueous titration and found 0.157%. No. 12 also used high frequency combustion/infrared absorption and found 0.155 %.
SILICON
Analysts Nos. 1, 2, 6 and 15 determined silicon gravimetrically after dehydration with perchloric acid. Nos. 1, 2 and 6 follo wed the procedure of the British
Standard Silicon Method 1*. Analyst No. 3 precipitated silicon as potassium fluorosilicate and completed by alkalimetric titr ation (Sneddon, Foundry Trade Journal 1966,
120, 605). No. 8 used a molybdenum blue photometric method.
Analyst No. 6 also determined silicon photometrically as molybdenum blue and found 0.34 %. No. 15 also used a potassium fluorosilicate titrimetric method and
found 0.34%.
MANGANESE
All analysts except No. 2 determined manganese photometrically after oxidation with periodat e according to the British Standard Manganese Method 2*. No. 2 used
the British Standard Manganese Method 1 * in which a zinc oxide separation is carried out before oxidation with persulphate/s ilver nitrate and titration with ammonium
ferrous sulphate.
Analyst No. 9 also determined manganese by AAS and found 1.37%.
PHOSPHORUS
Analysts Nos. 1, 9 and 14 determined phosphorus photometrically as phosphovanadomolybdate according to the British Standard P hosphorus Method 2*. The
remaining analysts used titrimetric methods after separation as ammonium phosphomolybdate (Nos. 2 and 3) or quinoline phosphomolybdate (No. 15).
SULPHUR
Analysts Nos. 1 and 6 determined sulphur gravimetrically according to the British Standard Sulphur Method 1*. The remaining a nalysts used combustion methods.
Nos. 2 and 3 used air combustion (Green, BCIRA Journal, 1968, 16, 244), Nos. 12 and 14 used high frequency combustion with infrared measurement and No. 15 used
high frequency combustion with oxidation/reduction titration.
Analyst No. 6 also determined sulphur by high frequency combustion/infrared absorption and found 0.025 %.
CHROMIUM
Analysts Nos. 1 and 13 determined chromium titrimetrically with ammonium ferrous sulphate after oxidation with persulphate/si lver nitrate. No. 1 followed the
procedure of the Analoid Method No. 37. No. 4 used a method involving removal of iron by solvent extraction and photometric m easurement of chromium in the
hexavalent state. Analysts Nos. 7, 11 and 12 used the British Standard Chromium Method 2* in which chromium is determined photometrically with diphenylcarbazide.
No. 10 used ICP-OES after dissolution of the sample in phosphoric acid.
MOLYBDENUM
All analysts except No. 8 determined molybdenum photometrically as oxythiocyanate. Nos. 1, 4, 12 and 14 follo wed the procedure of the British Standard
Molybdenum Method 1* in which the oxythiocyanate complex is extracted into n -butyl acetate. Analyst No. 8 used AAS.
NICKEL
Analysts Nos. 1 and 8 determined nickel by AAS. The remaining analysts used dimethylglyoxim e photometric methods. No. 4 carried out a preliminary separation
of iron by solvent extraction and Nos. 6 and 9 used the British Standard Nickel Method 3*.
Analysts Nos. 6 and 9 also determined nickel by AAS and found 0.095% and 0.106% respectively.
ARSENIC
Analysts Nos. 1 and 14 determined arsenic photometrically as the molybdenum blue complex after extraction as iodide into chlo roform (Fogg et al, Analyst 1972,
97, 657). Nos. 5 and 12 separated arsenic as arsine by reduction with zinc and completed photo metrically after absorption in a chloroform solution of silver
diethyldithiocarbamate. Analyst No. 10 used ICP -OES after dissolution of the sample in phosphoric acid.
COPPER
Analyst No. 1 determined copper photometrically with biscyclohexanone oxalyldihydr azone according to the Analoid Method No. 65. No. 5 used AAS. Analysts
Nos. 9, 12 and 14 used the British Standard Copper Method 3* which involves extraction of the 2, 2' diquinolyl complex into p entan-2-ol and subsequent photometric
measurement.
Analyst No. 9 also determined copper by AAS and found 0.099%.
TIN
All analysts except No. 8 determined tin iodimetrically after dissolution in hydrochloric acid and reduction with aluminium. No. 8 used AAS.
TITANIUM
Analysts Nos. 1, 5 and 12 determined titanium photometrically with diantipyrylmethane. Nos. 4, 7 and 11 used the British Standard Titanium Method 1* in which
titanium is separated by precipitation with cupferron and the determination completed photometrically with hydr ogen peroxide. No. 10 used ICP-OES after dissolution of
the sample in phosphoric acid.
TUNGSTEN
All analysts determined tungsten photometrically with thiocyanate according to the British Standard Tungsten Method 2*.
LEAD
AAS after solvent extraction of iron.

*Methods for Sampling and Analys is of Iron, Steel and Other Ferrous Metals, B.S. Handbook No. 19, first published in 1970 by the BSI, 389 Chiswick High Road,
London. W4 4AL.
Abbreviations:-
AAS: Atomic absorption spectrometry with synthetic calibration.
ICP-OES: Inductively Coupled Plasma - Optical Emission Spectrometry with synthetic calibration.

DESCRIPTION OF SAMPLE
† British Chemical Standard – bottles of 100g chips graded 1700 - 250µm (10 - 60 mesh) for chemical analysis.
‡ Spectroscopic Standard – 38 mm diameter x 19 mm thick discs for spectroscopic analysis.

INTENDED USE & STABILITY

The chip sample, BCS-CRM 453/1, is intended for the verification of analytical methods, such as those used by the participating laboratories, for the calib ration 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.
The disc sample, SS-CRM 453/1, is intended for establishing and checking the calibration of Optical Emission and X-Ray Spectrometers for the analysis of similar materials. The
“as received” working surface of the sample should be linished before use to remove any protective coating. It will remain st able provided that it is not subject to excessive heat (e.g.,
during preparation of the working surface). An area 6mm in diameter in the centre of the disc should be avoided for optical emission spectrometry.
This Certified Reference Material has been prepared in accordance with the recommendations specified in ISO Guides 30 to 35, available from the International Standards
Organisation in Geneva.

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 .............................................................................................................................................................................................................................................. May 1981

Main Edition .............................................................................................................................................................................................................................................. September 1984
Main Edition (revised with C(95%) and sM values for each element) ............................................................................................................................................................ August 2010

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