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. 381
BASIC SLAG
Prepared under rigorous laboratory conditions and, AFTER CERTIFICATION ANALYSIS IN GREAT BRITAIN,
issued by the Bureau of Analysed Samples Ltd.

CO-OPERATING ANALYSTS
INDEPENDENT ANALYST ANALYSTS representing MANUFACTURERS and USERS (cont.)
1 COPPINS, W. C., MSc, FRIC, Ridsdale and Co. Ltd., Middlesbrough. 5 GALE, P., BSc, ARIC, BSC, Port Talbot Works, Port Talbot.
6 MUIR, S., BSC, Corby Works, Corby.
ANALYSTS representing MANUFACTURERS and USERS 7 PADGET, H., AMet, ARIC, FIM,
2 BORROWDALE, J., BSc, BSC, Redbourn Works, Scunthorpe. BSC, Ebbw Vale Works, Ebbw Vale.
3 BURNLEY, H., BSC, Skinningrove Works, Saltburn. 8 SKINNER, J. M., BSc, PhD, MIWM, FRIC,
4 DUNNILL, P. B., BSc, BSC, Rotherham Works, Rotherham. Imperial Chemical Industries Ltd., Billingham.

ANALYSES
Mean of 4 values - mass content in %.
All results relate to the dried (105ºc) sample.

Analyst Fe P2O5 P2O5

No.
SiO2 TiO2 Al2O3 Total
FeO CaO MgO Cr2O3 MnO V2O5 Total Citric Sol.
S

1 8.73 0.32 0.72 13.22 3.59 49.2 0.95 0.32 3.17 0.94 15.78 15.42 0.19

2 8.91 0.34 0.62 13.32 3.60 49.6 0.93 0.33 3.07 0.93 15.61 15.21 0.19
3 8.68 0.39 0.62 13.21 3.76 49.3 0.98 0.31 3.19 0.96 15.75 15.00 0.16
4 8.77 0.35 0.74 13.47 3.81 48.8 1.12 0.33 3.10 0.92 15.83 15.00 0.20
5 8.75 0.36 0.73 13.24 3.58 48.8 1.02 0.37 3.30 0.93 15.73 15.32 0.20

6 8.68 0.33 0.66 13.26 3.60 49.0 1.11 0.30 3.08 1.00 15.78 15.13 0.18
7 8.78 0.30 0.64 13.40 3.87 48.9 1.03 0.36 3.29 0.90 15.83 15.42 0.18
8 8.96 0.38 0.66 13.22 3.71 48.6 1.12 0.34 3.10 0.98 15.68 15.15 0.20

MM 8.78 0.35 0.67 13.3 3.69 49.0 1.03 0.33 3.16 0.94 15.7 15.2 0.19
sM 0.11 0.04 0.05 0.1 0.12 0.4 0.08 0.03 0.10 0.04 0.1 0.2 0.02

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.

CERTIFIED VALUES (Cv)

mass content in %

SiO2 TiO2 Al2O3 Fe FeO CaO MgO Cr2O3 MnO V2O5 P2O5 P2O5 S
Total Total Citric Sol.

Cv 8.78 0.35 0.67 13.3 3.69 49.0 1.03 0.33 3.16 0.94 15.7 15.2 0.19

C(95%) 0.09 0.03 0.05 0.1 0.10 0.3 0.07 0.02 0.08 0.03 0.1 0.2 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.

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 BCS-CRM No. 381 BASIC SLAG
NOTES ON METHODS USED
SILICA
All Analysts determined silica gravimetrically. Nos. 1, 6, 7 and 8 fused the sample with sodium carbonate and dehydrated by double evaporation with perchloric acid
(Nos. 1, 6 and 7) or hydrochloric acid (No. 8). Nos. 2, 3, 4 and 5 dissolved in hydrochloric acid and dehydrated by double evaporation with perchloric acid.
TITANIUM DIOXIDE
All Analysts determined titanium dioxide photometrically with hydrogen peroxide. Nos. 1, 4, 7 and 8 carried out preliminary separations with cupferron. No. 2 carried
out a preliminary Group III separation followed by fusion of the ignited precipitate with sodium carbonate. No. 5 separated the titanium as phosphate.
Analyst No. 5 also used atomic-absorption spectroscopy and found 0.37%.
ALUMINA
All Analysts except No. 3 separated iron from aluminium with sodium hydroxide, precipitated the aluminium as oxinate and completed titrimetrically. No. 3 carried
out a basic acetate separation and determined aluminium gravimetrically as phosphate.
TOTAL IRON
All Analysts except No. 4 determined total iron by the Standard method for iron ores B.S. 4158: Part 1: 1967 which depends on reduction with hydrogen sulphide and
titration of the reduced iron with dichromate. No. 4 determined total iron photometrically with 1,10-phenanthroline.
FERROUS OXIDE
All Analysts dissolved the sample in hydrochloric acid in a closed vessel, allowed to cool in an atmosphere of carbon dioxide and titrated with dichromate.
LIME
All Analysts except No. 5 determined lime titrimetrically after separation as oxalate. Nos. 1 and 3 first removed manganese from a nitric acid solution of the sample by
treatment with bromate, then precipitated lime as oxalate from a slightly acid solution. Nos. 2, 4, 6 and 7 separated Group III elements with ammonia and manganese by
oxidation with bromine before precipitating calcium as oxalate. No. 8 used a direct oxalate separation in weakly acid solution. No. 5 determined lime titrimetrically with
EGTA after complexing interfering elements with triethanolamine.
MAGNESIA
All Analysts except No. 7 determined magnesia gravimetrically by precipitation as magnesium ammonium phosphate and ignition to the pyrophosphate. No. 1
precipitated the magnesium from ammoniacal citrate solution after separation of manganese with bromate and calcium as oxalate. Nos. 2, 3, 4, 5, 6 and 8 separated Group III
elements with ammonia, manganese with bromine and calcium as oxalate before precipitating the magnesium in ammoniacal solution. No. 7 fused the sample with sodium
carbonate, dissolved the melt in hydrochloric acid and determined magnesium by atomic-absorption spectroscopy.
Analysts Nos. 5 and 8 also used atomic-absorption spectroscopy and found 0.91% and 1.0% respectively.
CHROMIC OXIDE
All Analysts except No. 8 determined chromic oxide titrimetrically by oxidation with persulphate/silver nitrate and titration with ammonium ferrous sulphate. No. 8
determined chromic oxide photometrically with diphenylcarbazide.
Analysts Nos. 5 and 8 also used atomic-absorption spectroscopy and found 0.33% and 0.34% respectively. No. 6 also determined chromic oxide photometrically with
diphenylcarbazide and found 0.31%.
MANGANOUS OXIDE
All Analysts determined manganous oxide titrimetrically. Nos. 1, 2, 3 and 8 used direct methods involving oxidation with persulphate/silver nitrate and titration with
sodium arsenite/sodium nitrite (No. 1), sodium arsenite (Nos. 2 and 3) or ammonium ferrous sulphate (Nos. 6 and 8). Nos. 4, 5, 6 and 7 carried out preliminary zinc oxide
separations before oxidizing with bismuthate (Nos. 4 and 5) or persulphate/silver nitrate (Nos. 6 and 7) and titrating with ammonium ferrous sulphate.
Analyst No. 5 also used atomic-absorption spectroscopy and found 3.12%.
VANADIUM PENTOXIDE
All Analysts determined vanadium by oxidation with permanganate and titration with ammonium ferrous sulphate. Nos. 1 and 7 dissolved the sample in phosphoric
acid and used Analoid method No. 34. Nos. 2, 5, 6 and 8 used methods similar to the British Standard Vanadium Method 1 for iron and steel †.
Analyst No. 5 also used atomic-absorption spectroscopy and found 0.99%. No. 8 also determined vanadium photometrically with benzoyl phenylhydroxylamine and
found 0.99%.
TOTAL AND CITRIC-SOLUBLE PHOSPHORIC ACID
Analysts Nos. 1, 2, 3, 6, 7 and 8 determined the phosphoric acid titrimetrically. Nos. 1, 2, 6, 7 and 8 used the Statutory method * which depends on precipitation of the
phosphorus as quinolinium phosphomolybdate. Nos. 3 and 5 precipitated as ammonium phosphomolybdate; No. 3 used Analoid method No. 30. No. 4 determined total
phosphoric acid photometrically as phosphovanadomolybdic acid and citric-soluble phosphoric acid by the Statutory method. *
Analyst No. 1 also used the Analoid method No. 30 and found 15.53% for total phosphoric acid and 15.26% for citric-soluble phosphoric acid. No. 4 also determined
total phosphoric acid by the Analoid method and found 15.85%. No. 8 also used the Statutory method* and found 15.66% for total phosphoric acid and 15.22% for citric-
soluble phosphoric acid.
SULPHUR
All Analysts except No. 6 determined sulphur gravimetrically as barium sulphate. No. 6 used a combustion method.
Analysts Nos. 1 and 4 also determined sulphur by combustion and found 0.16% and 0.20% respectively.

* Statutory Instruments 1968 No. 218: The Fertilisers and Feeding Stuffs Regulations.
† 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.

DESCRIPTION OF SAMPLE
Bottles of 100g powder graded < 200μm (80 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 be en 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 1971

Main Edition ............................................................................................................................................................................................................................. July 1973
Main Edition (revised with C(95%) and sM values for each constituent) .............................................................................................................................. October 2012
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