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.

View certificate