Determination of Trace Amounts of Antimony and Boron in High-Purity Iron and Steel by Isotope Dilution/Inductively Coupled Plasma Mass Spectrometry

Abstract

The highly sensitive and precise determination method for trace amounts of Sb and B in high-purity iron and steel has been established by the isotope dilution/Inductively coupled plasma mass spectrometry. For the determination of Sb, the iron matrix was separated by anion-exchange chromatography using Dowex I-X8 in hydrofluoric acid solution, and the isotope ratio ( 121 Sb/ 123 Sb) of the HNO 3 /H 2 O 2 eluate was measured by ICP-MS. The isobaric interference of 123 Te was corrected by subtracting the intensity of 123 Te obtained by the relative intensity of 123 Te and 125 Te. For the determination of B, after the treatment of sulfuric acid-phosphoric acid fuming for the complete decomposition of boron nitride, B was separated by the anion-exchange chromatography using Amberlite IRA-743 at pH 8. The CyDTA was added to prevent the hydrolysis of iron. The isotope ratio ( 11 B/ 10 B) of the HCl eluate was measured by ICP-MS. By these methods, Sb and B in the range of µg/g to sub-µg/g could be determined with good precision. The limit of detection is 5.8 ng/g for Sb and 16 ng/g for B in steel.

Determination of Ultra-trace Tellurium in Steel by ID-ICP-MS/ MS with Liquid-Liquid Extraction

“…Inductively coupled plasma-mass spectrometry (ICP-MS) is another method to determine ultra-trace Te in steels. ICP-MS is expected to be a precise method for low trace amounts of Te in steels 10,11 . Despite this, there have been few reports on the determination of Te in steels by ICP-MS.…”

Matrix-precipitation for the Determination of Trace Impurities in High-purity Iron

“…Many separation techniques, including sorption, [5][6][7][8][9][10][11][12] liquidliquid extraction, [13][14][15][16][17][18] coprecipitation, [18][19][20][21][22] electrolysis, 14,23,24) and volatilization, 25,26) have been employed to determine impurities at ultratrace levels in iron and steels. However, these techniques are often tedious and time-consuming and they sometimes require volatile, flammable, and ill-smelling organic solvents or corrosive and hazardous acids.…”

Determination of boron in high-temperature alloy steel using non-linear inter-element correction and microwave plasma-atomic emission spectrometry

“…In general, the determination of B in steel is carried out using matrix separation methods prior to analysis. [6][7][8][9][10][11][12][13][14][15][16] Added complications of determining B using atomic emission spectrometry are due to Fe spectral interference on the two most sensitive B emission lines and inadequacy of the conventional inter-element correction (IEC) methods. The conventional IEC is based on determining apparent concentration of analyte (i.e., false-positive concentration of analyte in the presence of an interferent) using a high concentration of interferent and then applying a proportional correction on analyte concentration in the sample based on the interferent concentration in the sample.…”