Analysis of high-purity acids using inductive coupled plasma mass spectrometry

V.M. Retivov; D.V. Kotov; P.A. Volkov; A.V. Lobanova; L.A. Lebedeva; V.Z. Krasilschik; K.K. Bulatitsky; R.A. Sandu

Analysis of high-purity acids using inductive coupled plasma mass spectrometry

V.M. Retivov¹, D.V. Kotov², P.A. Volkov³, A.V. Lobanova⁴, L.A. Lebedeva⁵, V.Z. Krasilschik⁶, K.K. Bulatitsky⁷, R.A. Sandu⁸

research article Pages: 67-73

¹ директор ЦКП «Исследовательский научно-аналитический центр ФГУП «ИРЕА» (Москва)
^2,4 мл. науч. сотрудник, Аналитический испытательный центр ФГУП «ИРЕА» (Москва)
³ зам. директора ЦКП «Исследовательский научно-аналитический центр ФГУП «ИРЕА» (Москва)
⁵ ст. науч. сотрудник, Аналитический испытательный центр ФГУП «ИРЕА» (Москва)
⁶ к.х.н., зам. зав. Аналитическим испытательным центром ФГУП «ИРЕА» (Москва)
⁷ к.х.н., главный метролог, зав. Аналитическим испытательным центром ФГУП «ИРЕА» (Москва)
⁸ д.т.н., директор ФГУП «ИРЕА» (Москва)

Keywords: elemental analysis high-purity acids method of inductive coupled plasma mass spectrometry ICP-MS matrix effects spectral effects

Abstract

It was shown that the nature of the acid and its concentration have significant influence on the intensity of impurities analytical signals. This can be primarily explained by the effect of matrix suppression of the signal, as well as by molecular ions formation that can be registered at the masses of the elements being analyzed. Analytical characteristics were determined for both methods of high-purity acids analysis. For each of the acids, impurity elements were identified on which the matrix has the biggest influence. Second analysis method consists of evaporating the acid and washing off impurities on the evaporating dish walls with concentrated nitric acid followed by dilution of the sample with HNO₃ solution with concentration of 1 to 5%mass. This method can also be used for analysis of the other liquid-phase objects such as Н₂О₂, organic solvents, etc. Two methods were developed for analysis of high-purity acids using mass-spectrometry. The first one is express analysis consisting of diluting the acid being analyzed with high-purity water to the concentration of 10%mass followed by its direct analysis with a mass-spectrometer. This method has some restrictions due to the spectral effects of the matrix that are very hard to avoid and to the solvent purity. An internal standard was used to correlate the matrix effects. The objective of this work was to investigate the effect of the nature of different inorganic acids (HNO₃, HC_l, H₂SO₄, HF, H₃PO₄) on analytic characteristics of the ICP-MS method and to use this information to develop impurity determination methods for these compounds.

How to cite

Ретивов В.М., Котов Д.В., Волков П.А., Лобанова А.В., Лебедева Л.А., Красильщик В.З., Булатицкий К.К., Санду Р.А. Анализ кислот высокой чистоты методом масс-спектрометрии с индуктивно-связанной плазмой // Наукоемкие технологии. 2013. № 3. С. 67–73.

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[1] EHpov V.N. Skhema analiza bajjkalskojj vody metodom mass-spektrometrii s induktivno-svjazannojj plazmojj // Analitika i kontrol. 1999. T. 3. № 4. S. 37-43.

[2] Evans E.H., Giglio J.J. Interferences in inductively coupled plasma mass spectrometry. A review // Journal of Analytical Atomic Spectrometry. 1993. V. 8. P. 1-18

[3] Stewart I., Ollsik J. Steady state acid effects in ICP-MS // Journal of Analytical Atomic Spectrometry. 1998. V. 13. P. 1313-1320

[4] Burton L.L., Horlick G. MS Interview: An elemental mass spectrometry spectral interference data base // Spectrochimica Acta Part B: Atomic Spectroscopy. 1992. V.47. I. 14. P. 1621-1627.

[5] May T., Wiedmeyer R. A table of polyatomic interferences in ICP-MS // Atomic Spectroscopy, 1998. V. 19. P. 150-155.

[6] Todoli J., Mermet J. Acid interferences in atomic spectrometry: analyte signal effects and subsequent reduction // Spectrochimica Acta Part B: Atomic Spectroscopy. 1999. V.54. P. 895-929.

[7] Yman H, Hu S., at all. Preparation of ultra-pure water and acids and investigation of background of an ICP-MS laboratory // Talanta. 2000. V.52 P. 971-981.

[8] Paulsen P., Beaty E., at all. Inductively coupled plasma mass spectrometric analysis of ultrapure acids // Analytical Chemistry. 1988. V. 60. P. 971-979.

[9] Paulsen P., Beary E., at all. Analysis of ultrapure reagents from a large sub-boiling still made of Teflon PFA // Analytical Chemistry. 1989. V. 61. P. 827-830.

[10] Kishi Y., Kawabata K. DRC-ICP-MS analysis of various chemicals used in the semiconductor industry // Atomic Spectroscopy. 2003. V. 24. I. 2. P. 66-72.

[11] Meng Y., Lin H., Huang Z. Determination of trace metal in nitric acid of highly pruity by ICP-MS // Fenxi Shiyanshi. 2001. V. 20.
I. 6. P. 67-69.

[12] Heo Y., Gill J., Lim H. Analysis of Ultra Pure Sulfuric Acid for Semiconductor Using High Resolution ICP-MS // Analytical Science & Technology. 1998. V. 11. I. 4. P. 311-315.

[13] Chanrasia S.C., Sabayam A.C., at all. Combined isopiestic and sub-boiling distillation method for the purification of hydrofluoric acid used for ICP-MS elemental Analysis // Atomic Spectroscopy, 2006. V. 27. I. 4. P. 134-137.

[14] Bonyssier B., Ordonez Y. Determination of mercury in organic solvents and gas condensates by μflow-injection - inductively coupled plasma mass spectrometry using a modified total consumption micronebulizer fitted with single pass spray chamber // Spectrochimica Acta Part B. 2006. V. 61. B (9). P. 1063-1068.

[15] Denoyer E., Bruechner P. Determination of trace impurities in semiconductor-grade hydrofluoric acid and hydrogene peroxide by ICP-MS // Atomic Spectroscopy. 1995. V. 16. I. 1. P. 12-15.

[16] Kawabata K., Kishi Y., Thomas R. The Benefits of dynamic reaction cell ICP-MS technology to determine ultra trace metal contamination levels in high purity phpsphoric and sulfuric acid // Atomic Spectroscopy. 2003. V. 24. I. 2. P. 57-68.