硫化水素発生-紫外吸収法による鋼中微量硫黄の定量

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A new chemical method for determination of micro amounts of sulfur in steel has been developed. It is found that H_2S is easily evolved during sample dissolution with strong H_3PO_4 containing Fe(II) ions, and the solution absorbing H_2S shows the characteristic absorption at 232nm in ultraviolet region. The developed apparatus is mainly consisted of reaction vessel for sample dissolution and H_2S evolution, scrubbing vessel for removal of evolved water vapour and iron phosphite mist, absorption vessel for H_2S and constant flowrate pump for transferring the absorbing solution to flowcell of U.V. meter. The analytical procedure is performed as follows : 0.500g of sample and 20ml of strong H_3PO_4 containing Fe (II) ions are put into the reaction vessel. The sample is dissolved by heating in N_2 stream. H_2S is evolved in the reaction vessel, scrubbed with 6N HCl in the scrubbing vessel and absorbed with 5.00ml of 0.05N NaOH. The absorbing solution is circulated through flowcell of U.V. meter by the pump. Absorbance is continuously measured at 232nm until it becomes constant. Above 0.5ppm of micro amounts of sulfur can be easily determined with high accuracy. The time required for analysis of one sample is less than 10min. The analytical results of steel samples are in good agreement with those obtained by the conventional method. Moreover, the proposed method has been improved for the higher sensitivity by concentration of sulfide ion with the anion exchange resin.
社団法人日本鉄鋼協会の論文
1982-02-01

硫化水素発生-紫外吸収法による鋼中微量硫黄の定量

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