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
4004
BRITISH CHEMICAL STANDARD CERTIFIED REFERENCE MATERIAL

CERTIFICATE OF ANALYSIS
BCS-CRM No. 114
LOW ALLOY STEEL
Prepared under rigorous laboratory conditions and, AFTER CERTIFICATION ANALYSIS IN GREAT BRITAIN,
issued by the Bureau of Analysed Samples Ltd.

ANALYSES
Mean of 4 values - mass content in %.
Lab
C Si Mn P S Cr Mo Ni Al As B Co
No.
1 0.4012 0.2990 0.4212 0.0043 0.0044 0.1975 0.1851 1.4939 0.0806 0.0022 0.0006 0.0179
2 0.4168 0.2847 0.4143 0.0051 0.0044 0.1867 0.1866 1.5197 0.0818 0.0023 0.0008 0.0178
3 0.4004 0.3031 0.4216 0.0041 0.0047 0.1889 0.1807 1.5045 0.0746 … 0.0007 0.0168
4 0.4023 0.3004 0.4155 0.0040 0.0047 0.1848 0.1787 1.4993 0.0785 0.0030 0.0008 0.0167
5 0.3970 … … … 0.0052 … … … … … … …
6 … 0.2910 0.3995 0.0041 0.0050 0.1844 0.1878 1.4888 0.0745 0.0026 0.0009 0.0160
7 0.4025 0.2917 0.4218 0.0050 0.0041 0.1800 0.1836 1.5055 0.0771 0.0024 0.0007 0.0172
MM 0.4034 0.2950 0.4157 0.0044 0.0046 0.1871 0.1838 1.5020 0.0779 0.0025 0.0008 0.0171
sM 0.0069 0.0070 0.0086 0.0005 0.0004 0.0059 0.0035 0.0108 0.0031 0.0003 0.0001 0.0007
sw 0.0077 0.0020 0.0026 0.0003 0.0003 0.0022 0.0019 0.0071 0.0010 0.0003 0.0001 0.0003

Lab
Cu N Nb Sn Ti V Zr Pb W Ca Sb
No.
1 0.3639 0.0044 0.0043 0.0458 0.0099 0.0096 0.0055 … <0.001 <0.0001 <0.0025
2 0.3656 0.0040 0.0043 0.0381 0.0098 0.0078 0.0043 0.0002 … … …
3 0.3537 0.0042 0.0039 0.0406 0.0092 0.0087 0.0053 <0.0001 0.0004 <0.0001 0.0002
4 0.3589 0.0045 0.0039 0.0409 0.0093 0.0082 0.0053 <0.0004 <0.0006 <0.001 0.0022
5 … 0.0041 … … … … … … … … …
6 0.3633 … 0.0043 0.0402 0.0097 0.0088 0.0055 <0.001 … <0.0001 <0.001
7 0.3546 0.0046 0.0045 0.0420 0.0094 0.0082 0.0049 <0.0001 … <0.0001 0.0002
MM 0.3600 0.0043 0.0042 0.0413 0.0096 0.0086 0.0051 … … … …
sM 0.0051 0.0003 0.0003 0.0026 0.0003 0.0007 0.0005 … … … …
sw 0.0018 0.0002 0.0004 0.0008 0.0005 0.0004 0.0004 … … … …
The above figures are those which each Analyst has decided upon after careful verification
MM: Mean of the intralaboratory means. sM: standard deviation of the intralaboratory means. sW: intralaboratory standard deviation.
Values given above in small italic type are for information only.

CERTIFIED VALUES
mass content in %
C Si Mn P S Cr Mo Ni Al As B Co Cu
MM 0.403 0.295 0.416 0.0044 0.0046 0.187 0.184 1.502 0.078 0.0025 0.0008 0.0171 0.360
C(95%) 0.007 0.008 0.009 0.0005 0.0004 0.006 0.004 0.012 0.004 0.0004 0.0001 0.0008 0.005

N Nb Sn Ti V Zr
MM 0.0043 0.0042 0.041 0.0096 0.0086 0.0051
C(95%) 0.0003 0.0003 0.003 0.0003 0.0008 0.0005

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

NB: Although widely accepted within the industry “mass content in %” is neither an SI nor an IUPAC supported quantity. Multiplication of the certified value (Cv) by 104
will yield the value in µg/g
 BCS-CRM No. 114
LOW ALLOY STEEL
NOTES ON METHODS USED
CARBON: Analyst No. 1 determined carbon using non-aqueous titration according to the Standard Method BS 6200:3.8.2:1991.
The other Analysts used high frequency combustion-infrared absorption.

SILICON: Analysts Nos. 1, 2, 3 and 7 determined silicon gravimetrically, Nos. 1, 2 and 7 after dehydration with perchloric acid
and No. 3 after a sulphuric acid dehydration. Analyst No. 4 used a molybdenum blue photometric method, whilst Analyst No. 6
used Inductively Coupled Plasma Optical-Emission Spectrometry (ICP-OES).

MANGANESE: Analysts Nos. 1, 4 and 7 determined manganese photometrically after oxidation with potassium periodate.
Analysts Nos. 2, 3 and 6 used ICP-OES

PHOSPHORUS: Analyst No 1 determined phosphorus photometrically as phosphovanadomolybdate with extraction according to

the Standard Method BS EN 10184. Analysts Nos. 2, 3 and 6 used ICP-OES whilst Analysts Nos. 4 and 7 determined phosphorus
photometrically as phosphovanadomolybdate without extraction.

SULPHUR: Analyst No.1 determined sulphur gravimetrically according to the Standard Method BS 1 6200:3.26. Analyst No.6
determined sulphur by combustion, according BS 7020:7.2. The other analysts used high frequency combustion infrared
absorption.

CHROMIUM: All Analysts, except No. 7, determined chromium by ICP-OES. Analyst No. 7 used Flame Atomic Absorption
Spectrometry (FAAS).

MOLYBDENUM: All Analysts, except No. 7, determined molybdenum by ICP-OES. Analyst No. 7 used a photometric method
with thiocyanate in the presence of Sn (II).

NICKEL: All Analysts, except No. 7, used ICP-OES. Analyst No.7 titrated with EDTA.

ALUMINIUM: Analysts Nos. 1, 2, 3, 4 and 6 used ICP-OES. Analyst No. 7 used FAAS.

ARSENIC: Analyst No. 1 determined arsenic photometrically with silver diethyldithiocarbamate after separation as arsine,
according to BS EN 10212:1996. Analysts Nos. 2 and 4 used ICP-OES and Analyst No.6 used hydride generation atomic
absorption spectrometry. Analyst No. 7 determined arsenic photometrically as molybdenum blue.

BORON: All Analysts, except Nos. 2 and 7, determined boron photometrically with curcumin, No.1 according to BS EN 10200.
Analyst No. 2 determined boron by ICP-OES and No. 7 used dianthrimide to determine the boron photometrically.

COBALT: All Analysts, except No. 7, determined cobalt by ICP-OES. No.7 used FAAS.

COPPER: All Analysts, except No. 7, determined copper by ICP-OES. No.7 used FAAS.

NITROGEN: Analyst No. 1 determined nitrogen using an acidimetric titration after distillation, according to the Standard
Method BS 6200:3.22.1:1992. The remaining Analysts used thermal conductivity after decomposition in a graphite crucible.

NIOBIUM: All Analysts, except No. 7, determined niobium using ICP-OES. Analyst No. 7 determined niobium photometrically
with 4-(2 pyridylazo)-resorcinol.

TIN: All analysts, except No.7, used ICP-OES. Analyst No.7 determined tin by FAAS.

TITANIUM: Analysts Nos. 1, 2, 3, and 6 determined titanium by ICP-OES. Analysts Nos. 4 and 7 determined titanium
photometrically using diantipyrylmethane.

VANADIUM: All Analysts, except No. 7, determined vanadium by ICP-OES. Analyst No. 7 used FAAS.

ZIRCONIUM: All Analysts, except No. 7 determined zirconium by ICP-OES. Analyst No. 7 used a xylenol orange photometric
method.
LEAD: Analysts Nos. 2 and 6 determined lead by ICP-OES. Nos. 3 and 4 used FAAS and Analyst No. 7 used electrothermal atomic absorption
spectrometry (ETAAS)

TUNGSTEN: All Analysts used ICP-OES

CALCIUM: Analysts Nos. 1, 3 and 4 used FAAS, Analyst No.6 used ICP-OES and Analyst No. 7 used ETAAS

ANTIMONY: Analyst No. 1 used FAAS, Analysts Nos. 3 and 7 used hydride generation atomic absorption spectrometry and Analysts Nos. 4 and
6 used ICP-OES

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 BCS-CRM No. 114
LOW ALLOY STEEL
CO-OPERATING ANALYSTS
INDEPENDENT ANALYST
1 PAGE-GIBSON, J.E., BSc, CChem, MRSC Ridsdale & Co. Ltd., Middlesbrough.

ANALYSTS representing MANUFACTURERS and USERS

2 CROOK, D., Corus Strip Products, Llanwern.
3 FOX, G., Corus Engineering Steels, Stocksbridge.
4 WEERDT, Miss J A., BRAS, P.W. ten & GULDEMOND, Dr D., Corus Staal BV, IJmuiden.
5 RICHMOND, Mrs H., & RAW, M., Corus Construction and Industrial, Redcar.
6 SNOWDEN, Miss Y.A. and RAW, M., Corus Construction and Industrial, Scunthorpe.
7 WILSON, J., Allvac Ltd., Sheffield.
DESCRIPTION OF SAMPLE
BCS-CRM 114 is a low alloy steel supplied in bottles of 100g chips nominally graded 1700 – 250µm (10 – 60 mesh) for chemical
analysis. The sample is also available in pieces of 44mm diameter as SS-CRM 114.
The preparation of representative samples for chemical analysis and the certification by co-operative analysis was undertaken by
Bureau of Analysed Samples Ltd (BAS).
BAS is a United Kingdom Accreditation Service (UKAS) Accredited Reference Material Producer, No 4004, and, as the Producer of
BCS-CRM 114 as defined in ISO Guide 34:2009 section 3.1, is fully responsible for assigning the certified values and their uncertainties
in accordance with ISO Guides 34:2009 and 35:2006.
This material was originally certified in 2004, before BAS achieved accreditation to ISO Guide 34 in 2006. However, following an
extensive review of the certification of this BCS-CRM, it has been established that the procedures used were exactly the same as those
which have since been accredited and that therefore BCS-CRM 114 can be issued under the ISO Guide 34 Accreditation.
INTENDED USE
This sample is intended for uses such as the verification of the accuracy and repeatability of analytical methods, such as those used
by the participating laboratories, for the calibration of analytical instruments, for establishing values for secondary reference materials
and for training purposes.
In order to ensure that a fully representative sample is taken users should take a minimum sub-sample size of 1.0g. Users of this
material should be aware that the use of a smaller sub-sample size will invalidate the certified values and the associated 95% confidence
limits.
The sample should be mixed thoroughly before each use.
STABILITY
BCS-CRM 114 will remain stable provided that the bottle remains sealed and is stored in a dry atmosphere. When the bottle has
been opened the lid should be secured immediately after use.
TRACEABILITY
The characterisation of this material has been achieved by chemical analysis involving inter-laboratory study, each laboratory using
the method of their choice, details of which are given above.
Most of the analytical methods used in the characterisation of this CRM were either international or national standard methods or
methods which are technically equivalent. All laboratories used either stoichiometric analytical techniques or methods which were
calibrated predominantly against pure metals or stoichiometric compounds, ensuring traceability of the individual results to the SI.
MEASUREMENT UNCERTAINTY
The uncertainty of each of the certified values of BCS-CRM 114 has been established by multiplying the standard error arising from
the chemical analysis by the appropriate two sided Student’s t value at the 95% confidence level for the number of results. Homogeneity
has been assessed on the bulk material and has been found to be acceptable. It has not, therefore, been included in the calculated
measurement uncertainty. The stability of this CRM and its transportation also make negligible contributions to the overall uncertainty of
the certified values.
COMMUTABILTY
BCS-CRM 114 is intended to be used in the same physical form as that used by the participating analysts and therefore
commutability is not of relevance in respect of this CRM.
Further information and advice on this or other Certified Reference Materials or Reference Materials produced by Bureau of
Analysed Samples Ltd may be obtained from the address below.
NEWHAM HALL For BUREAU OF ANALYSED SAMPLES LTD.
NEWBY R P MEERES,
MIDDLESBROUGH Managing Director
ENGLAND
TS8 9EA
email: [email protected]
Website: www.basrid.co.uk
Preliminary Edition…. …. …. …. …. …. …. …. …. …. …. …. …. …. …. …. …. …. …. …. …. ….. …. …. ….July 2004
Main Edition.… …. …. …. …. …. …. …. …. …. …. …. …. …. …. …. …. …. …. …. …. …. …. …. …. ….March 2014

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