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

SPECTROSCOPIC STANDARD CERTIFIED REFERENCE MATERIAL

CERTIFICATE OF ANALYSIS
SS-CRM No. 219/4
Ni-Cr-Mo Steel
Prepared under rigorous laboratory conditions and, AFTER CERTIFICATION ANALYSIS IN GREAT BRITAIN,
issued by the Bureau of Analysed Samples Ltd.

CO-OPERATING ANALYSTS AND FIRMS

INDEPENDENT ANALYSTS ANALYSTS representing MANUFACTURERS and USERS
1. COPPINS, W.C., M.Sc., C.Chem., F.R.I.C., 4. BOTT, F.R., Rolls-Royce (1971) Ltd., Derby.
Ridsdale & Co Ltd., Middlesbrough. 5. CHAMBERLAIN, B.J., M.Sc.,
2. SARGENT, M., Ph.D., LGC Ltd, London. B.S.C. Bilston, Wolverhampton and Birchley Works, Bilston.
6. HOBSON, J.D., B.Sc., Ph.D., A.Met., C.Chem., F.R.I.C.
GOVERNMENT DEPARTMENT Dunford-Hadfields Ltd., Sheffield.
3. NICHOLLS, H.A., C.Chem., F.R.I.C., 7. KIDMAN, L., A.Met., M.I.M., A..M.Inst.F.,
Bragg Laboratory, Materials Quality Assurance Directorate, Sheffield. B.S.C. Rotherham Works, Rotherham.
8. MATHIESON, V., B.S.C. Craigeneuk Works, Motherwell.
9. MUIR, S., B.S.C. Corby Works, Corby.

ANALYSES
Mean of 4 values – mass content in %.
Analyst C Si Mn P S Cr Mo Ni Cu Sn
No.
1 0.318 0.076 0.81 0.011 0.025 0.67 0.58 2.54 0.086 0.010
2 … … 0.82 … … 0.67 0.58 2.56 … …
3 0.310 0.074 0.80 0.011 0.028 0.65 0.58 2.57 0.085 0.010
4 0.317 0.085 0.82 0.012 0.026 0.66 0.57 2.54 0.089 0.009
5 0.315 0.079 0.80 0.011 0.028 0.65 0.60 2.54 0.088 0.013
6 0.313 0.08- 0.81 0.011 0.027 0.65 0.57 2.56 0.082 0.011
7 0.308 0.074 0.82 0.011 0.027 0.65 0.57 2.57 0.085 0.010
8 0.312 0.089 0.83 0.012 0.026 0.66 0.58 2.54 0.093 0.012
9 0.317 0.076 0.81 0.012 0.026 0.66 0.57 2.57 0.093 0.010
MM 0.314 0.079 0.81 0.011 0.027 0.66 0.58 2.55 0.088 0.011
sM 0.004 0.006 0.01 0.001 0.002 0.01 0.01 0.02 0.004 0.002
sW 0.003 0.002 0.01 0.001 0.001 0.01 0.01 0.01 0.002 0.001
(Additional Information:- Analyst No. 1:- Total Al 0.003%)
MM: Mean of the intralaboratory means. sM: standard deviation of the intralaboratory means. sW: Intralaboratory standard deviation.
The above figures are those which each Analyst has decided upon after careful verification

CERTIFIED VALUES
mass content in %

C Si Mn P S Cr Mo Ni Cu Sn
MM 0.314 0.079 0.81 0.011 0.027 0.66 0.58 2.55 0.088 0.011
C(95%) 0.004 0.005 0.01 0.001 0.001 0.01 0.01 0.02 0.004 0.002

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.

DESCRIPTION OF SAMPLE
Spectroscopic Standard – 38mm diameter discs for spectroscopic analysis.
 SS-CRM 219/4
Ni-Cr-Mo STEEL
NOTES ON METHODS USED
CARBON
Analysts Nos. 1 and 8 determined carbon gravimetrically using the British Standard Carbon Method 1*. Nos. 3 and 4 determined carbon by infrared measurement
of the evolved gases. Nos. 6 and 9 used coulometric methods, No. 6 according to Hobson and Leigh, Analyst, 1974, 99, 93. No. 5 determined carbon by non-
aqueous titration and No.7 used a low pressure method.
Analysts Nos. 6 and 8 also determined carbon by non-aqueous titration and found 0.31% and 0.311% respectively. No. 7 also used an infrared method and found
0.310%.
SILICON
Analysts 1, 7 and 9 used molybdenum-blue photometric methods; No. 1 used the Analoid Method No. 43. Nos. 3, 4, 5, 6 and 8 determined silicon gravimetrically
after double dehydration with perchloric acid, according to the British Standard Silicon Method 1*.
Analysts Nos. 1, 7 and 9 also used the British Standard Silicon Method 1* and found 0.070%, 0.075% and 0.074% respectively.
MANGANESE
Analysts Nos. 1, 5 and 8 determined manganese titrimetrically after oxidation with persulphate/silver nitrate. No.1 titrated with arsenite/nitrite according to
Analoid Method No.53 and Nos. 5 and 8 titrated with arsenite. Analyst No. 2 used ICP-OES, calibrated with pure manganese. Analysts Nos. 3, 4, 6, 7 and 9
determined manganese photometrically after periodate oxidation according to the British Standard Manganese Method 2*.
Analyst No. 6 also used a periodate photometric method with an automatic analyser and found 0.81%. No. 9 also used FAAS spectroscopy and found 0.80%
PHOSPHORUS
Analysts Nos. 1, 3, 4, 6 and 7 determined phosphorus photometrically as phosphovanadomolybdate according to the British Standard Phosphorus Method 2*.
Nos. 5 and 9 determined phosphorus titrimetrically after precipitating as phosphomolybdate. No. 8 used the British Standard Phosphorus Method 1* in which
phosphorus is determined gravimetrically after precipitation as phosphomolybdate and conversion to lead molybdate.
Analyst No. 6 also used a molybdenum blue photometric method with an automatic analyser and found 0.011%.
SULPHUR
Analysts Nos. 1 and 6 determined sulphur gravimetrically according to the British Standard Sulphur Method 1*. All other analysts determined sulphur by
combustion methods. No.3 completed by borate titration, Nos. 4 and 7 by infrared absorption and Nos. 5 and 8 by iodate titration.
Analyst No. 6 also determined sulphur by combustion and found 0.027%.
CHROMIUM
All analysts except No.2 determined chromium titrimetrically after oxidation with persulphate/silver nitrate. No. 1 used the Analoid Method No. 37, Nos. 3, 5, 7,
8 and 9 used the British Standard Chromium Method 1*. Analyst No. 2 used ICP-OES, calibrated with pure chromium.
Analyst No. 9 also used FAAS and found 0.65%.
MOLYBDENUM
All analysts except No.2 determined molybdenum photometrically as oxythiocyanate. No. 1 measured the colour directly using Analoid Method No. 42. Nos. 4,
5, 6, 7 and 8 extracted the coloured complex into butyl acetate, Nos. 5, 6, 7 and 8 according to British Standard Molybdenum Method 1*. Analyst No. 2 used
ICP-OES, calibrated with pure molybdenum.
Analysts Nos. 6 and 8 also used alternative oxythiocyanate methods, No. 6 with an automatic analyser, and each found 0.58%.
NICKEL
Analysts Nos. 1, 3, 4, 5, 6, 7 and 9 used methods involving precipitation with dimethylglyoxime. No. 1 dissolved the precipitate in dilute sulphuric acid, boiled
with an excess of iron (III) ammonium sulphate and titrated with dichromate (Analoid Method No. 61). No.4 dissolved the precipitate and titrated with EDTA.
Nos. 3, 5, 7 and 9 dissolved the precipitate and titrated with cyanide according to British Standard Nickel Method 1*. No.6 completed gravimetrically. Analyst
No. 2 used ICP-OES, calibrated with pure nickel. Analyst No. 8 used a photometric dimethylglyoxime method.
Analyst No. 6 also determined nickel photometrically with dimethylglyoxime according to British Standard Nickel Method 3* and found 2.57%. Analyst No. 9
also used FAAS and found 2.55%.
COPPER
Analyst No. 1 determined copper by FAAS. No. 3 used a photometric bis-cyclohexanone oxalyldihydrazone method. Nos. 4 and 5 separated copper as sulphide
and completed titrimetrically according to British Standard Copper Method 2*. Nos. 6, 7 and 8 determined copper photometrically as 2-2' diquinolyl according to
British Standard Copper method 3*. No. 7 used a photometric diethyldithiocarbamate method.
Analyst No. 1 also used a direct bis-cyclohexanone oxalyldihydrazone photometric method and found 0.098%. No. 5 also used a diethyldithiocarbamate method
and found 0.087%.
TIN
All analysts determined tin by reduction with aluminium and titration with iodate solution. Nos. 4, 5, 6, 7 and 9 used British Standard Tin Method 1*.
* Methods for Sampling and Analysis of Iron, Steel and Other Ferrous Metals, B.S. Handbook No. 19, first published 1970 by the British Standards Institution,
London.

INTENDED USE & STABILITY

The disc sample, SS-CRM 219/4 is intended for the 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 stable 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.

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 …. …. …. …. …. …. …. …. …. …. …. …. …. …. …. …. …. …. …. …. … … … … … … … … … … ...May, 1977
Main Edition (revised with additional values for Mn, Cr, Mo & Ni and with C(95%), sM and sW values for each certified element) … … … … … … … … … ...February, 2003
Main Edition (relating to the disc sample SS-CRM 219/4) … … … … … … … … … … … … … … … … … … … … … … … … … April 2014