Abstract:The experimental conditions for the determination of carbon and sulfur in nickel-based corrosion resistant alloy by high frequency combustion infrared absorption method were discussed by preparing calibration curve using certified reference material of nickel-based alloy with similar content. The effect of flux type, dosage and sampling mass on the determination was mainly investigated. The results showed that the combustion of sample was complete and the infrared absorption peak was symmetrical and smooth under the following conditions: 0.30g of pure copper-0.30g pure iron and 0.40g of pure iron-1.50g of pure tungsten were used as flux for the determination of carbon and sulfur. Meanwhile, the relative standard deviations (RSD) of results were minimal. When (0.300±0.005)g of sample was used for the determination of carbon and sulfur, the sample would not overflow after melting and the RSDs of measurement results were minimal. The results indicated that the correlation coefficient of the calibration curve of carbon content was r=0.9998. The limit of detection was 0.00012% and the limit of quantification was 0.00040%. The correlation coefficient of the calibration curve of sulfur content was r=0.9999. The limit of detection was 0.00011% and the limit of quantification was 0.00036%. The experimental method was applied for the determination of carbon and sulfur in three nickel-based corrosion resistant alloy samples. The found results were in range of 0.0053%-0.156% and 0.0011%-0.0032%, respectively. The RSD (n=6) of determination results was less than 1% and 3%, respectively. The nickel-based corrosion resistant alloy sample was determined according to the experimental method. The spiked recovery tests of carbon and sulfur in sample were conducted by adding different dosages of standard reagents (lithium carbonate and potassium sulfate, respectively). The recoveries for carbon and sulfur were 95%-104% and 96%-105%, respectively.
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