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KMID : 0385520160290040170
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Analytical Science & Technology
2016 Volume.29 No. 4 p.170 ~ p.178
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A comparison study of 76Se, 77Se and 78Se isotope spikes in isotope dilution method for Se
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Kim Lee-won
Lee Seo-Young
Pak Yong-Nam
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Abstract
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Accuracy and precision of ID methods for different spike isotopes of 76Se, 77Se, and 78Se were compared for the analysis of Selenium using quadrupole ICP/MS equipped with Octopole reaction cell. From the analysis of Se inorganic standard solution, all of three spikes showed less than 1 % error and 1 % RSD for both short-term (a day) and long-term (several months) periods. They showed similar results with each other and 78Se showed was a bit better than 76Se and 77Se. However, different spikes showed different results when NIST SRM 1568a and SRM 2967 were analyzed because of the several interferences on the m/z measured and calculated. Interferences due to the generation of SeH from ORC was considered as well as As and Br in matrix. The results showed similar accuracy and precisions against SRM 1568a, which has a simple background matrix, for all three spikes and the recovery rate was about 80% with steadiness. The %RSD was a bit higher than inorganic standard (1.8 %, 8.6 %, and 6.3 % for 78Se, 76Se and 77Se, respectively) but low
enough to conclude that this experiment is reliable. However, mussel tissue has a complex matrix showed inaccurate results in case of 78Se isotope spike (over 100 % RSD). 76Se and 77Se showd relatively good results of around 98.6 % and 104.2 % recovery rate. The errors were less than 5 % but the precision was a bit higher value of 15 % RSD. This clearly shows that Br interferences are so large that a simple mathematical calibration is not enough for a complex-matrixed sample. In conclusion, all three spikes show similar results when matrix is simple. However, 78Se should be avoided when large amount of Br exists in matrix. Either 76Se or 77Se would provide accurate results.
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KEYWORD
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Se, ID method, Se spikes, ORC ICP/MS, isobaric interference,
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