1 1 R 1. Department of Applied Chemistry, Faculty of Science and Engineering, Chuo University, , Kasuga, Bunkyo-ku, Tokyo
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1 BUNSEKI KAGAKU Vol. 52, No. 8, pp. 575 _ The Japan Society for Analytical Chemistry 1 1 R 1 Determination of rare earth elements in river water by fully automated on-line column inductively coupled plasma mass spectrometry using iminodiacetate chelate resin as a column Seiya MITO 1, Masaki OHATA 1 and Naoki FURUTA 1 1 Department of Applied Chemistry, Faculty of Science and Engineering, Chuo University, , Kasuga, Bunkyo-ku, Tokyo (Received 24 March 2003, Accepted 17 June 2003) In order to determine ultra-trace levels of rare earth elements (REEs) in river water, fully automated on-line column inductively coupled plasma mass spectrometry (ICP-MS) using iminodiacetate chelate resin as a column was developed in this study. The determination of REEs in a river-water reference material (SLRS-3) was conducted by using the developed method. The obtained results were in good agreement with the recommended values. This developed method was applied to the determination of REEs in Kanda River, which flows through the center of Tokyo, and the distribution patterns of REEs were evaluated. As a result, the positive anormalies of Gd in REEs patterns were found for both river water filtered with a 0.45 µm membrane filter and that filtered and heated with nitric acid. It is considered that the positive anormaly of Gd can be attributed to the outflow of Gd compounds, which are used for MRI (magnetic resonance imaging) contrast medium. Keywords : river water ; on-line column ; ICP-MS ; iminodiacetate resin ; Gd anormaly. 1 1) 2) 7) 1 : ) 9) 7)10) 8-11) 12) Chelex-100 Muromac A-1
2 576 BUNSEKI KAGAKU Vol Chelex Muromac A-1 Muromac A-1 Muromac A-1 ISIS ICP-MS ICP-MS La 140 Ce 141 Pr 146 Nd 147 Sm 151 Eu 157 Gd 159 Tb 163 Dy 165 Ho 166 Er 169 Tm 172 Yb 175 Lu Gd ASX500 Cetac ISIS Yokogawa Analytical Systems ICP-MS HP4500 Yokogawa Analytical Systems 0.5 mmφ ICP-MS Fig. 1 ISIS ISIS 2 pump I II I II I 0.25 ml pump 2 Fig. 1 a Fig. 1 b ICP-MS HEPA PURE SPACE PS-100 class-100 Fig. 1 Schematic diagram of ISIS (a) step 1 ; adsorption and (b) step 2 ; elution 2 2 Muromac A mesh sodium form Muromac A-1 2 Muromac A g 1.5 mm 50 mm 1000 µg ml 1 TAMAPURE-AA Milli-Q Element 1.5 M HNO 3 ph 0.7 M 30 TAMAPURE-AA TAMAPURE-AA-100 ph Flow chart Fig µm filter A river water A 99 g 1g g heated river water 500 ml A 0.45 µm filter particles
3 : ICP-MS µm filter A ph 3 2 4, Table M HNO M ph 3 4 ph M ml 1.5 M HNO 3 ICP-MS Table 2 Ba Table 2 lsotope Monoxide and hydroxide interferences for REEs Interferences 139 La 140 Ce 141 Pr 146 Nd 130 Ba 16 O 147 Sm 130 Ba 16 O 1 H 151 Eu 135 Ba 16 O 134 Ba 16 O 1 H 157 Gd 141 Pr 16 O 140 Ce 16 O 1 H 159 Tb 143 Nd 16 O 142 Nd 16 O 1 H 142 Ce 16 O 1 H 163 Dy 147 Sm 16 O 146 Nd 16 O 1 H 165 Ho 149 Sm 16 O 148 Sm 16 O 1 H 148 Nd 16 O 1 H 166 Er 150 Sm 16 O 150 Nd 16 O 149 Sm 16 O 1 H 169 Tm 153 Eu 16 O 152 Gd 16 O 1 H 152 Sm 16 O 1 H Fig. 2 water Flow chart for sample preparation of river 172 Yb 175 Lu 156 Gd 16 O 159 Tb 16 O 156 Dy 16 O 158 Dy 16 O 1 H 155 Gd 16 O 1 H 158 Gd 16 O 1 H Table 1 Operating sequences of ISIS for matrix separations, REEs preconcentration and elution for the detrmination of REEs in river water by automated on-1ine column ICP-MS ISIS Flow rate/ Time/ Step Solution (see Fig. 1) ml min 1 s a M nitric acid Water Ammonium acetate buffer solution (ph 3) Sample (ph 3) Ammonium acetate buffer solution (ph 3) Water b M nitric acid
4 578 BUNSEKI KAGAKU Vol Table 3 Formation-yield of monoxide and hydroxide Interfering Formation-yield, Interfering Formation-yield, monoxide hydroxide BaO BaOH LaO LaOH CeO CeOH PrO PrOH NdO NdOH SmO SmOH EuO EuOH GdO GdOH TbO TbOH DyO DyOH HoO HoOH ErO ErOH TmO TmOH YbO YbOH LuO LuOH Table 4 Element Analytical results for the concentration of REEs in SLRS-3 and the detection limits obtained by automated on-1ine column ICP- MS DL/ Found/ Reference value 3) / pg g 1 pg g 1 pg g 1 La Ce Pr Nd Sm Eu Gd Tb Dy Ho Er Tm Yb Lu pg g 1 Table 2 Table 3 14 Ba 100 ng g 1 m/z m/z SLRS-3 National Research Council of Canada Table 4 SLRS-3 3) Ce 5 Ce 4) Ce 249 9pgg 1 5 Na : 1500 µg g 1 Mg : 200 µg g 1 K: 100 µg g 1 Ca : 100 µg g 1 10 pg g Fig. 3 Sampling points at Kanda river
5 : ICP-MS Fig. 3 7 Table 5 a A river water C1 13) Fig. 4 a Gd Gd Table 5 b heated river water Fig. 4 b heated river water Table 5 a Fig. 4 a river water Gd river water 1.5 Gd Fig. 4 a Fig. 4 b Table 5 c 0.45 µm Fig. 4 c river water heated river water heated river water µm Gd 2) 5) Gd magnetic resonance imaging MRI 14) Gd-DTPA Gd diethylenetriaminepentaacetic acid Gd-DOTA Gd 1,4,7,10-tetra(carboxymethyl)-1,4,7,10-tetraazacyclododecane MRI MRI Gd Gd 4 SLRS µm A Gd Gd Gd MRI Gd 1) :, p. 34 (1999), ( ). 2) M. Bau, P. Dulski : Earth Planet. Sci. Lett., 143, 245 (1996). 3) D. B. Peart, R. C. Antweiler, H. E. Taylor, D. A. Roth, T. I. Brinton : Analyst, 123, 455 (1998). 4) X. P. Yan, R. Kerrich, M. J. Hendry : J. Anal. At. Spectrom., 14, 215 (1999). 5) Y. Nozaki, D. Lerche, D. S. Alibo, M. Tsutsumi : Geochim. Cosmochim. Acta, 64, 3975 (2000). 6),,,, B : (Bunseki Kagaku), 50, 419 (2001). 7) S. Hirata, T. Kajiya, M. Aihara, K. Honda, O. Shikino : Talanta, 58, 1185 (2002). 8) E. Vassileva, N. Furuta : Fresenius J. Anal. Chem., 370, 52 (2001). 9) K. Akatsuka, T. Suzuki, N. Nobuyama, S. Hoshi, K. Haraguchi, K. Nakagawa, T. Ogata, T. Kato : J. Anal. At. Spectrom., 13, 271 (1998). 10) L. Ebdon, A. S. Fisher, P. J. Worsfold, H. Crews, M. Baxter : J. Anal. At. Spectrom., 8, 691 (1993). 11) J. W. McLaren, J. W. H. Lam, S. S. Berman, K. Akatsuka, M. A. Azeredo : J. Anal. At. Spectrom., 8, 279 (1993). 12) M. R. Plantz, J. S. Fritz, F. G. Smith, R. S. Houk : Anal. Chem., 61, 149 (1989). 13) :, p. 626 (2003), ( ). 14) :, p. 843 (1999), ( ).
6 580 BUNSEKI KAGAKU Vol Table 5 (a) Analytical results for the concentration of REEs for river water (pg g 1 ) Element Inogashira Zenpukuzi Wada Shin-edogawa Suidobashi Asakusabashi Sumida Park Park Park River La Ce N.D. N.D Pr Nd Sm Eu Gd Tb Dy Ho Er Tm Yb Lu Table 5 (b) Analytical results for the concentration of REEs for heated river water (pg g 1 ) Element Inogashira Zenpukuzi Wada Shin-edogawa Suidobashi Asakusabashi Sumida Park Park Park River La Ce Pr Nd Sm Eu Gd Tb Dy Ho Er Tm Yb Lu Table 5 (c) Analytical results for the concentration of REEs for particles 0.45 µm (pg g 1 ) Element Inogashira Zenpukuzi Wada Shin-edogawa Suidobashi Asakusabashi Sumida Park Park Park River La Ce Pr Nd Sm Eu 71 N.D Gd Tb 20 N.D Dy Ho 21 N.D Er Tm N.D. N.D Yb N.D. N.D Lu N.D. N.D. N.D. N.D. N.D. N.D. 210
7 : ICP-MS 581 Fig. 4 Chondrite-normalized distribution patterns of REEs for river water, (b) heated river water and (c) particles 0.45 µm
8 582 BUNSEKI KAGAKU Vol SLRS µm A 0.45 µm A Gd Gd MRI Gd
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