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. Page 2 of 2 BCS/SS-CRM No. 290/2 (ECRM 253-1) 13% MANGANESE STEEL NOTES ON METHODS USED CARBON Analysts Nos. 1, 7 and 8 determined carbon gravimetrically by the British Standard Carbon Method 1*. Nos. 2 and 4 used a non-aqueous titration method (Jones et al., Analyst, 1965, 90, 623; 1966, 91, 399). No. 3 used a low pressure method (Cook and Speight, Analyst, 1956, 81, 144). No. 5 determined carbon coulometrically. No. 6 absorbed the carbon dioxide on a molecular sieve, released it by heating and carried out the final measurement by thermal conductivity. Analysts Nos. 3 and 5 also determined carbon by both non-aqueous titration and infrared absorption. Results were as follows:- non-aqueous titration 1.15% (No. 3), 1.16% (No. 5); infrared absorption 1.15% (No. 3), 1.16% (No. 5). SILICON All Analysts determined silicon gravimetrically using the British Standard Silicon Method 1*. Analysts Nos. 3, 4 and 7 also used photometric methods depending on the formation of molybdenum-blue and found 0.32%, 0.33% and 0.34% respectively. MANGANESE All Analysts determined manganese titrimetrically. Nos. 1, 2, 4, 5 and 8 used the British Standard Manganese Method 1* which includes a zinc oxide separation. No. 3 titrated with permanganate in fluoride solution (Headridge and Taylor, Analyst, 1962, 87, 905). No. 6 used a bismuthate method. No. 7 titrated potentiometrically with permanganate in tetra-sodium pyrophosphate solution, the method being modified to eliminate chromium interference (Scribner, Anal. Chem., 1960, 32, 970). Analyst No. 3 used two alternative methods: (a) British Standard Manganese Method 3* (b) the same method modified to eliminate chromium interference (Scribner, loc. sit.); these gave results of 12.64% and 12.57% respectively. No. 5 also used a photometric periodate method in conjunction with an automatic analyser and found 12.52%. PHOSPHORUS All Analysts determined phosphorus photometrically as phosphovanadomolybdic acid according to the British Standard Phosphorus Method 2*. Analyst No. 5 also used a photometric molybdenum-blue method in conjunction with an automatic analyser and found 0.044%. SULPHUR Analysts Nos. 1, 6 and 8 determined sulphur gravimetrically according to the British Standard Sulphur Method 1*. The remaining Analysts determined sulphur by combustion in oxygen and titration with sodium borate solution (No. 7 carried out a potentiometric titration). Analyst No. 5 also used the British Standard Sulphur Method 1* and found 0.018%. No. 6 also determined sulphur by combustion and found 0.019%. CHROMIUM Analysts Nos. 1, 4, 5, 7 and 8 determined chromium titrimetrically after oxidation with persulphate/silver nitrate. Nos. 1 and 7 titrated with ammonium ferrous sulphate solution using sodium diphenylamine sulphonate indicator and applied corrections for the small amount of vanadium present. Nos. 4 and 5 titrated with ammonium ferrous sulphate/dichromate. No. 7 titrated with ammonium ferrous sulphate/permanagante according to the British Standard Chromium Method 1*. Nos. 2, 3 and 6 determined chromium photometrically with diphenylcarbazide., Analysts Nos. 2 and 3 also determined chromium titrimetrically and found 0.18% and 0.17% respectively. NICKEL Analysts Nos. 1, 2, 4 and 7 determined nickel titrimetrically after precipitation with dimethylglyoxime. No. 1 dissolved the precipitate in sulphuric acid and boiled with excess of ferric sulphate: the ferrous salt thus formed was titrated with dichromate solution (Analoid Method No. 62). No. 2 titrated with EDTA. Nos. 4 and 7 titrated cyanometrically according to the British Standard Nickel Method 1*. Nos. 3, 5, 6 and 8 determined nickel photometrically with dimethylglyoxime/iodine. No. 3 used a modified version of the British Standard Nickel Method 3*. Nos. 5 and 6 first separated the nickel with dimethylglyoxime before determining it photometrically. No. 8 used the British Standard Nickel Method 3*. Analyst No. 4 also used a modification of the British Standard Nickel Method 3* and found 0.28%. No. 5 also used a photometric method in conjunction with an automatic analyser (without previous separation of the nickel) and found 0.29%. No. 7 also determined nickel gravimetrically with dimethylglyoxime and found 0.29%. MOLYBDENUM Molybdenum was determined photometrically as the oxythiocyanate after extraction into butyl acetate (Analoid Method No. 63). COBALT Both Analysts determined cobalt photometrically with nitroso-R-Salt. No. 1 used the British Standard Cobalt Method 1* whereas No. 7 used a modification of the British Standard Cobalt Method 2*. COPPER Copper was determined photometrically with bis-cyclohexanone oxalyldihydrazone. (Analoid Method No. 65). NITROGEN The sample was fused in a current of helium and nitrogen determined by thermal conductivity. VANADIUM Analyst No. 1 separated iron by extraction into diethyl ether and determined vanadium photometrically as phosphovanadotungstate according to the Analoid Method No 59. Nos. 5 and 7 used the British Standard Vanadium Method 1*. *Methods for Sampling and Analysis 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.

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