20 SPEX XSTC : Cd, Se, Pb, As, Cr, B, Zn, Al, Fe, Cu, 5 : Ba, Bi, Ag, Li, Sr 1. Elix3-UV NEW MilliQ - Advantage

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1 BUNSEKI KAGAKU Vol. 60, No. 5, pp The Japan Society for Analytical Chemistry Ba Bi Ag Mo ICP/MS 40 Ar 16 O 40 Ca 16 O 40 Ar 35 Cl 9 Fe m/z 56 As m/z 75 DRC-ICP/MS 18 Li Sr Cd Se Pb As Cr B Zn Al 1 : Fe Cu Mn 3 Sb U Ni 4 Ba, Bi, Ag, Mo Li, Sr 20 SPEX XSTC : Cd, Se, Pb, As, Cr, B, Zn, Al, Fe, Cu, Mn, Sb, U, Ni, Mo 1000 mg L 1 5 : Ba, Bi, Ag, Li, Sr 1 Be Co Ga Y In Tl 1000 mg L 1 Ultrapur Elix3-UV NEW MilliQ - Advantage 2 2 ICP/MS ELAN DRC-e ICP/MS Table 1 Table PTFE 10 ml 0.1 ml AS-ONE EB ml Table 1 Operating conditions for ICP/MS Instrument DRC-e (Perkin Elmer co.) RF Power 1500 W Plasma gas flow rate 15.0 L min 1 Auxiliary gas flow rate 1.20 L min 1 Nebulizer gas flow rate 1.0 L min 1 Cell gas Methane Sample flow rate 1.0 ml min 1 Dwell Time 50 ms u 1

2 434 B U N S E K I K A G A K U Vol Table 2 Analyte mass, cell gas flow rate, and internal standard for each element m/z Cell gas flow rate/ ml min 1 Internal standard Raw water Receiving well Rapid mixing tank 1 Sodium hydroxide (NaOH) Aluminum sulfate (Al 2 (SO 4 ) 3 ) Li Be B 11 0 Al 27 0 Cr Mn Fe Ni Cu Zn As Se Ga Sr 88 0 Mo 98 0 Ag Cd In Sb Ba Chemical sedimentation basin 2 Ozone contact basin 3 Activated carbon treatment facility 4 Flush mixing tank Rapid filter 5 Treated water reservoir Tap water Sodium hypochlorite (NaClO) Aluminum sulfate (Al 2 (SO 4 ) 3 ) 6 Sodium hypochlorite (NaClO) Pb Bi Tl U ml ICP/ MS ml min 1 1 JSAC JSAC μg L 1 1 μg L BEC JSAC JSAC 0302 Fig. 1 Sampling points in water treatment processes at advanced water treatment facility : Raw water ; : Coagulation-sedimentation water ; : Ozone contacted water ; : Activated carbon treated water ; : Rapid filtered water ; : Tap water 5 Li Sr Sb Ag Bi Li Sr : 25 μg L 1 Sb : 0.5 μg L 1 Ag Bi : 0.05 μg L S 6 Fig ICP/ MS Fe m/z Ar 16 O 40 Ca 16 O As m/z Ar 35 Cl 9 DRC-ICP/MS As

3 : DRC-ICP/MS Fig. 2 Optimum flow rate of cell gas for measuring arsenic [Left panel] Relationship between flow rate of cell gas and the ratio of the measured values to the certified values. [Right panel] Relationship between flow rate of cell gas and background equivalent concentration (BEC) Fig. 3 Optimum flow rate of cell gas for measuring iron [Left panel] Relationship between flow rate of cell gas and the ratio of the measured values to the certified values. [Right panel] Relationship between flow rate of cell gas and background equivalent concentration (BEC) Fig. 2 Fe Fig. 3 Fig. BEC As ml min 1 BEC 0.3 ml min ml min 1 Fe ml min 1 BEC 0.6 ml min ml min 1 As 0.3 ml min 1 7 Cr Mn Fe Ni Cu Zn Se 0.6 ml min 1 Table Be m/z 9 Co m/z 59 Ga m/z 71 Y m/z 89 In m/z 115 Tl m/z Be Ga In Tl 5 μg L 1 Co Y 53 ng L ng L 1 5 ng L ng L 1 5 μg L Co Co 0 10 μg L 1 1 Co As 75 Co 5 μg L 1 As 0.15 μg L 1 SIMAA6000 Co As Co 5 μg L 1 As μg L 1 ICP/MS As CoO : As Co

4 436 B U N S E K I K A G A K U Vol Table 3 Determination limits and regulated values for tap water Determination limit/μg L 1 Standard value/ μg L 1 Target value/ μg L 1 Li B Al Cr Mn Fe Ni Cu Zn As Se Sr Mo Ag (100) a) Cd Sb Ba Pb Bi U a) Standard of national secondary drinking water regulations in US EPA As Co Y Be Ga In Tl 4 Be 5 25 μg L Table 3 Bi Ag 1/100 Ag US EPA 0.10 mg L 1 1/50000 Ag Bi 8 1/ Al Cd JSAC JSAC JSAC CV 10 Table 4 5 Li Sr Sb Ag Bi Li Sr : 25 μg L 1 Sb : 0.5 μg L 1 Ag Bi : 0.05 μg L 1 Li Sr Sb Ag Bi /10 Table 5 Sr Fe Al B Ba S Table 6 0 Al μg L 1 Ag μg L μg L μg L 1 Al Sr μg L 1 Sr B Fe Mn Ba Li 1 10 μg L 1 Zn Cu Mo As μg L 1 Ni Cr Pb Sb U μg L 1 Se Cd μg L 1 Ag Bi Al : 200 μg L 1 Mn : 50 μg L 1 Mn 10 μg L 1 4 Ba Mo Bi Ag Ba 700 μg L 1 1/20 Mo 70 μg L 1 1/40 Bi Ag Ag US EPA 0.10 mg L 1

5 : DRC-ICP/MS Table 4 Analytical results for 20 elements in river water reference materials (JSAC and 0302) (n 3) m/z Certified value/ μg L 1 JSAC River water Analytical value/μg L 1 Recovery/ CV/ Certified value/ μg L 1 JSAC 0302 River water Analytical value/μg L 1 Recovery/ CV/ Li 7 Not certified b) Not certified b) B Al Cr Mn Fe Ni 58 Not certified b) Cu Zn As Se 78 (0.11) a) Sr 88 Not certified b) Not certified b) Mo Ag 107 Not certified b) Not certified b) Cd Sb 121 Not certified b) Not certified b) Ba Pb 208 (0.005) a) Bi 209 Not certified b) Not certified b) U a) Reference value b) Certified value or reference value is not shown Table 5 m/z Recoveries of elements in purified water and tap water (n 3) Added/ Purified Water Tap Water μg L 1 Recovery/ CV/ Recovery/ CV/ Li B Al Cr Mn Fe Ni Cu Zn As Se Sr Mo Ag Cd Sb Ba Pb Bi U / Fig Mn U Fe Bi Ag Al 20 Se Li Sb Ba B Mo Sr Pb As Cu Cr Ni Zn Cd Sr Ba Ba 17 Mn U Fe Al Ni Sb B Pb Ni Zn

6 438 B U N S E K I K A G A K U Vol Bi Ag Bi 95 Ag 93 Mn As Fe Al Fig. 1 : Rapid mixing tank ph Fig. 5 Al Cu M(OH) 2 M(OH) 3 : M Table 6 Concentration levels for 20 elements in raw Fe(OH) waters As Concentration/μg L 1 Min. Max. Ave. a) 7 Al Mn Sr B MnO 2 Fe Fe Mn Ba Li Zn Cu Mo Mn As Ni Mn Cr Mn Pb Sb U Se b) Cd b) Mn 4 Bi b) 7 18 Ag b) Al Cu a) Ave. ; value of average (n 6). b) The value of the concentration that was less than the limit of determination was considered as 0, when deriving the average Fig. 4 Removal ratio of 20 elements in advanced water treatment processes Removal ratio ( ); (1- Tap water concentration/raw water concentration) 100. : average of six samples ; upper bar : Maximum value of six samples ; under bar : Minimum value of six samples

7 : DRC-ICP/MS Fig. 5 Changes in concentration of 20 elements in advanced water treatment processes (Measured in December 2006) : Raw water ; : Coagulation - sedimentation water ; : Ozone contacted water ; : Activated carbon treated water ; : Rapid filtered water ; : Tap water 4 DRC-ICP/MS 20 Cd, Se, Pb, As, Cr, B, Zn, Al, Fe, Cu, Mn, Sb, U, Ni, Ba, Bi, Ag, Mo Li, Sr ng L 1 μg L Mn U Fe Bi Ag Al 80 Se Li Sb Ba B Mo Sr 20 Bi Ag 2 Al Cu Mn

8 440 B U N S E K I K A G A K U Vol ) 261 (2003). 2) : 68, 2, 23 (1999). 3) : 22, 43 (2002). 4) : 38, 44 (2008). 5) : 566, 61 (1981). 6) C. Rosin, M. Morlot, P. Hartemann, J. C. Boeglin : Tech. Sci, Methodes, 86, 3, 147 (1991). 7) : 64, 8, 47 (1995). 8) : 59, 279 (2008). 9) H. Yuan, S. Hu, J. Tong, L. Zhao, S. Lin, S. Gao : Talanta, 52, 971 (2000). 10) ( GLP) : ( 2005). 11) K. Jitmanee, N. Teshima, T. Sakai, K. Grudpan : Talanta, 73, 352 (2007). 12) : p. 155 (2007), ( ). 13) : (2004). 14) : (2003). 15) : 3, 73 (2003). 16) K. H. Lee, M. Oshima, T. Takayanagi, S. Motomizu : Anal. Sci., 16, 731 (2000). 17) : 40, 1, 205 (1995). 18) 2000, p ) : 567, 35 (1981). Development of a Highly Sensitive and Simultaneous Analytical Method for 20 s in Raw and Tap Waters Using DRC-ICP/MS and Removal Characteristics of These s in the Process of Water Treatment Miho YANO 1 and Tatsuhiko KAWAMOTO 1 1 Hyogo Prefectural Institute of Public Health and Consumer Sciences, , Arata-cho, Hyogo-ku, Kobe-shi, Hyogo (Received 22 October 2010, Accepted 21 December 2010) A simultaneous multi-component analytical method for 20 types of elements in raw and tapwater samples (Cd, Se, Pb, As, Cr, B, Zn, Al, Fe, Cu, Mn, Sb, U, Ni, Ba, Bi, Ag and Mo, as listed in the Water Works Law, and Li and Sr, which are not-listed but are frequently detected) was studied using DRC-ICP/MS. The investigation revealed 1) that the optimum cell-gas flow rates to control plasma-based interferences was 0.3 ml min 1 for As and 0.6 ml min 1 for the other elements (Cr, Mn, Fe, Ni, Cu, Zn and Se), and 2) that Be, Ga, In and Tl are the most appropriate elements for the internal standards, except in the cases of Co and Y, which are influenced by their concentration level in raw water. Under these analytical conditions, verification by spiked recovery tests exhibited that the recovery rate is , and that the variation coefficient is below 10. The levels of the determination limits for each element were ng L 1 μg L 1, which demonstrates the possibility of measurements for low-concentration samples. From all of these results, this analytical method has been confirmed to be both highly sensitive and accurate. Furthermore, studies of the removal performance for 20 different elements from raw to tap water in an advanced water-purification facility showed that Mn, U, Fe, Bi, Ag and Al can be easily removed (removal ratio of over 80 ). On the other hand, Se, Li, Sb, Ba, B, Mo and Sr can hardly be removed (removal ratio of below 20 ). Keywords : elements ; highly sensitive and simultaneous analytical method ; Dynamic Reaction Cell - Inductively Coupled Plasma/Mass Spectrometry ; raw and tap water ; water treatment process.