Spectroscopic Standard – 38mm diameter discs for spectroscopic analysis. Page 2 of 2 SS-CRM No. 225/2 Ni-Cr-Mo STEEL NOTES ON METHODS USED CARBON Analyst No. 1 determined carbon both conductimetrically using the Wösthoff apparatus and gravimetrically; the results were 0.394% and 0.40% respectively. The other Analysts used the Standard gravimetric method B.S. 1121: Part 11 1948. SILICON Analyst No. 1 determined silicon photometrically as molybdenum-blue using the Standard photometric method B.S. 1121: Part 15: 1949. The other Analysts determined silicon gravimetrically. Nos. 2, 4, 5, 6, 7 and 8 used the Standard method B.S. 1121: Part 10: 1948. No. 3 used a nitro-sulphuric acid method. Analysts Nos. 4 and 6 also determined silicon photometrically as molybdenum-blue and found 0.23% in each case. No. 8 also determined silicon gravimetrically by evaporation with hydrochloric acid and found 0.22%. PHOSPHORUS Analysts Nos. 1, 3, 4, 7 and 8 determined phosphorus titrimetrically after precipitation as ammonium phosphomolybdate. No. 4 precipitated the phosphomolybdate according to the Standard gravimetric method B.S. 1121: Part 9: 1948, No. 8 according to the original Standard method B.S. 1121: Part 1: 1943. Nos. 2, 5 and 6 determined phosphorus gravimetrically by precipitation of phosphomolybdate and conversion to lead molybdate according to the Standard method B.S. 1121: Part 9: 1948. Analysts Nos. 1 and 6 also determined phosphorus photometrically as phosphovanadomolybdic acid (Elwell and Wilson, Analyst, 1956, 81, 136; 1957, 82, 453) and both found 0.020%. SULPHUR Analysts Nos. 1, 2, 3, 5, 6 and 8 determined sulphur gravimetrically as barium sulphate. All except No. 3 followed the procedure of the Standard method B.S. 1121: Part 1A: 1957. Nos. 4 and 7 determined sulphur by combustion. No. 4 absorbed the sulphur gases in hydrogen peroxide and titrated with sodium borate solution. No. 7 absorbed in dilute hydrochloric acid and titrated with iodide/iodate solution. Analysts Nos. 1, 6 and 8 also used combustion methods and found 0.012%, 0.013% and 0.012% respectively. No. 5 also used a combustion method on a 10g. sample, but after absorbing the sulphur gases in hydrogen peroxide the sulphur was precipitated as barium sulphate and determined gravimetrically; the result by this method was 0.010%. CHROMIUM All Analysts dissolved the sample in sulphuric-phosphoric acid mixture and oxidized the chromium with persulphate/silver nitrate. Nos. 1, 4, 5, 7 and 8 titrated with ammonium ferrous sulphate/permanganate according to the Standard titrimetric method B.S. 1121: Part 13: 1954, No. 2 titrated directly with ammonium ferrous sulphate (Analoid method No. 37), No. 6 titrated with ferrous sulphate/dichromate. Analyst No. 4 also used a method similar to the Analoid method and found 1.06%. No. 5 also used a method similar to the Standard titrimetric method but with N- phenylanthranilic acid as indicator and found 1.08%. MOLYBDENUM Analysts Nos. 1, 2, 4, 5, 6, 7 and 8 determined molybdenum photometrically as molybdenum oxythiocyanate. Nos. 1, 4 and 6 used methods involving extraction of the coloured complex with butyl acetate. No. 2 used the Analoid Method No. 42. Nos. 5, 7 and 8 used the Standard method B.S. 1121: Part 34: 1955. No. 3 determined molybdenum both photometrically and gravimetrically by means of benzoin α-oxime; the results were 0.34% and 0.33% respectively. NICKEL All Analysts precipitated nickel with dimethylglyoxime and completed titrimetrically. Nos. 1 and 5 used the Standard method B.S. 1121: Part 37: 1961 in which the nickel is titrated with cyanide solution. Nos. 3, 6 and 8 used similar methods. No. 2 dissolved the dimethylglyoxime precipitate in dilute sulphuric acid and boiled with excess of ferric sulphate; the ferrous salt thus formed was titrated with dichromate solution. No. 4 precipitated the nickel according to the Standard method, but completed by titration with EDTA. No. 7 used both the Standard titrimetric method and a photometric method depending on the use of dimethylglyoxime; the result was 1.45% in each case. Analysts Nos. 4 and 5 also used photometric dimethylglyoxime methods and found 1.45% and 1.44% respectively. MANGANESE Analyst No. 1 used both the Standard titrimetric method B.S. 1121: Part 16: 1949 which involves a zinc oxide separation and the Standard photometric method B.S. 1121: Part 23: 1951 which depends on oxidation with periodate. Nos. 2, 3 and 7 determined manganese titrimetrically by oxidation with persulphate/silver nitrate and titration with arsenite/nitrite solution (Nos. 2 and 3) or arsenite solution (No. 7). No. 4 used the Standard titrimetric method. Nos. 5 and 6 used the Standard photometric method. No. 8 used a photometric method depending on oxidation with persulphate/silver nitrate. Analysts Nos. 3 and 8 also used titrimetric bismuthate methods and found 0.57% and 0.55% respectively. No. 4 also used the Standard photometric method and found 0.55%. COPPER No. 2 used the Standard photometric method B.S. 1121: Part 36: 1956. Nos. 4 and 6 used the bis-cyclohexanone oxalyldihydrazone method (Haywood and Sutcliffe, Analyst, 1956, 81, 651). VANADIUM Titrimetric Analoid Method No. 34. TIN Reduction with aluminium and titration with iodate. ARSENIC Standard titrimetric method B.S. 1121: Part 38: 1958. ANTIMONY Photometric rhodamine B method (Kidman and Waite, Metallurgia, 1962, 66, 143). COBALT Standard photometric method B.S. 1121: Part 42: 1961. ALUMINIUM Photometric solochrome cyanine R method (Scholes and Smith, Analyst, 1958, 83, 615). ZIRCONIUM Gravimetric mandelic acid method NIOBIUM Chromatographic method (Hunt and Wells, Analyst, 1954, 79, 351). TANTALUM Photometric pyrogallol method (Kidman and White, Metallurgia, 1961, 64, 153). BORON Photometric dianthrimide method (BISRA Methods of Analysis Committee, J. Iron Steel Inst., 1958, 189, 227). NITROGEN Standard titrimetric method, B.S. 1121: Part 39: 1959.

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