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1 * Nutrients analysis and current status relevant standard solutions Chikako Kato NH 4+ NO 3 NO 2 3 PO 4 2 SiO 3 5 1) 4) * 5) ) 0.2 % 1% 2% 6) WOCE (World Vol. 6, No
2 Ocean Circulation Experiment; 3 %1 %1 % 2 %1 %1 %1 % 2 % % % 2 ICES (International Council for the Exploration of the Sea; )3 CSK (Cooperative Study of the Kuroshio and Adjacent Regions; ) 4), 6), 7) 6) VKIWater Quality Institute; VKI 8) 10) µm ph % 8) NRC (National Research Council of Canada) MOOS-1 11) 200 m 0.05 µm MOOS NOAA (National Oceanic and Atmospheric Administration; ) NRC MOOS-1 5), 11) 1MOOS-1 VKI % 5) MOOS-1 5) 5) % ), 13) AIST Bulletin of Metrology Vol. 6, No September 2007
3 MOOS-1 11) 認証値 (µmol/l) RSD NO NO ± % - NO 2 2- SiO 3 3- PO ± % 26.0 ± % 1.56 ± % *k = 2 5) - NO 3 - NO 2 2- SiO 3 3- PO 4 濃度 (µmol/l) RSD % % % % 8 5) 1965ICES ICES ICES2 Part phpart 9 54ICES ICES ICES CSK CSK ICES41988ICES ICES ICES QUASIMEME (Quality Assurance of Information for Marine Environmental Monitoring in Europe) NOAANRC NOAA/NRC intercomparison in NRCMOOS MOOS-1 2NOAA/NRC intercomparison in % Vol. 6, No
4 2003MRI intercomparison in %0.15 % 3.5 %1.7 % CCQMConsultative Committee for Amount of Substance; NRCSMU (Slovak Institute of Metrology)2 CCQM-P89NMIJ NRCSMU 1 CCQM SI 14) (a) (b) 5 15) AIST Bulletin of Metrology Vol. 6, No September 2007
5 JCSS 1000 mg/l0.35 % NIST National Institute of Standards and Technology; Standard Reference Material SRM mg/kg6 mg/kg0.61 %, k = ) KRISSKorea Research Institute of Standards and Science; CRM No NO mg/kg5.0 mg/kg 0.5 % 17) KNO 3 3), 4), 18), 19) NaNO 3 11), 16), 17) ) ) ), 19) NMIJNIST 19) 21) 19) %0.07 % 21) NIST SRM193 21) 0.22 µm 20) 1 L1 ml 3) 6 3), 4) 16) NISTKRISS 0.61 %0.5 % 16), 17) JCSS 1000 mg/l 0.35 % FLUKANIST NaNO 2 3), 4), 18), 19) ) ), 19) 19) %0.09 % 1 L 1 ml 3), 4) 3 3) 18) JCSS 1000 mg/l0.35 % MerckNIST SRM 999a KCl 1000 mg/l2 mg/l0.2 % FLUKANIST Vol. 6, No
6 NH 4 Cl 23) ) JIS K ) JIS K ml 50 ml 0.1 mol/l0.1 mg1.5 g 1 mol/l20 ml 11 mol/l JIS 99.5 % 25) 23) FLUKANIST 26) JCSS 1000 mg/lnistsrm mg/kg3 mg/kg0.3 % 27) KRISS CRM No PO mg/kg0.50 % 28) KH 2 PO 4 3), 4), 29) NaH 2 PO 4 28) ) ) JIS K ) mol/l 1 mol/l 3) 3), 4) 1 L 1 ml 3), 4) 4.5 mol/l2 ml 3) 6 3) JCSS NISTSRM mg/g0.04 mg/g 0.43 % 32) KRISS CRM No SI20.1 % HC mg/l 5.2 mg/l 0.52 % 33) Na 2 SiF 6 Na 2 SiO 3 SiO ), 4) 1 2 3), 4) NISTKRISS 32), 33) 0.1 % ) AIST Bulletin of Metrology Vol. 6, No September 2007
7 ICP-OES 33) JCSS NISTKRISS JCSS 3), 4) Morris (1963) 35) 540 nm 0.02ppm 0.2ppm 36) 3), 4) 3), 4), 35) 3) M(1) + 2+ NO3 + M + 2H NO 2 + M + H 2O (1) NO 2 NO 3), 4) + NO3 + 2H + 2e NO 2 + H 2O (E 0 = 0.94 V) (2) + NO3 + 4H + 3e NO + 2H 2O (E 0 = 0.97 V) (3) (1) ph NO + H O + 2 NO 2 + 2OH 3 2 e (E 0 = V) (4) (4) ph 8.2 3) 220 nm 37) ph Vol. 6, No
8 37) 36) + NH 4 + ClO NH 2Cl + H 2O (5) NH 2Cl + 2C6H 6OH + 2ClO O 6 = C6 H6 = N C6H OH + 3HCl + 2OH (6) 630 nm 36) 0.1 % 2-37), 38) 38) ph ph 0.1ppm 0.5ppm 36) 3) 3 [ PMo O ] 12H O PO MoO H (7) 880 nm 885 nm ) 4) L- 1 4) 0.1ppm 1.2ppm 36) 3), 4) 4 [ SiMo O ] 12H O SiO MoO H (8) 12 AIST Bulletin of Metrology Vol. 6, No September 2007
9 ph 4 ph ppm 10ppm0.1ppm 1ppm 36) 3 % 3) 4) 2(a) 39) * 2(b) 39) 4) 34), 40)-43) Vol. 6, No
10 43) 3 43) 10 µm 200 µm 44) kvkv 44) 4 10 µl 100 µl nmol L -1 mmol L ), 46) Foret 47) 48) 5 AIST Bulletin of Metrology Vol. 6, No September 2007
11 OH H + 48) 49) K + H + K + OH KOH RSD1.4 % 2.0 % 0.7 % 1.4 % 49) 2 50) 62 UV 6 50) ON OFF 0.05 µm 45 µm 4) RSD 1 % 5 % 0.4 % 51) 0.1 µm 51) 0.2 µm 44) 0.53 µm 51) RSD 2.8 %5.5 %2.1 %1.6 % 49) () 0.65 µm 51) 50 nm(rsd 1 %) 51) 0.1 µm10 nm 51) RSD6.7 %0.6 % RSD 0 µm 40 µm 4) RSDWOCE Vol. 6, No
12 3 % 0.1 % 4) RSD 0.05 µm 40 µm0.02 µm 0.25 µm 5) 50) 26 ph 26 ph ), 52) RSD 0.6 µm 53) 0 µm 5.0 µm 4) 52) MOOS-1 -ICP0.06 µm 54) nm RSD 0.46 % 34) 0 µm200 mm 4) RSD1.4 % 2.0 % 0.7 % 1.4 % 49) 52) -MOOS µm 55) 2 µm 130 µm % 1) AIST Bulletin of Metrology Vol. 6, No September 2007
13 3)-5), 34), 36), 44), 51)-53), 55) RSD NO 3 - (µmol/l) NO 2 - (µmol/l) NH 4 + (µmol/l) PO 4 3- (µmol/l) SiO 3 2- (µmol/l) 求める濃度範囲 対応濃度範囲 RSD 対応濃度範囲 RSD 対応濃度範囲対応濃度範囲 RSD 対応濃度範囲 RSD 吸光光度法 % % ( 青 ) ( 黄 ) フローインジェクション分析法 (AAS) % ( 陰イオン交換 ) % - ( 化学発光 ) % % 連続流れ分析法 % % キャピラリーゾーン電気泳動 % % イオンクロマト JIS K 0102 硝酸 亜硝酸の相互分離可能グラフィー排水試験法公定法 IEC-ICP-MS りん酸 けい酸の相互分離可能 MOOS-1の測定に使用 *µmol/l **AAS:IEC-ICP-MS:- 6) NMIJ 1) :, 49-1(2002) ) : 13, ) :, ),,, : (JODC), ) : 2003, 50(2006) ) :, 10(2002) ) A. Alain and K. Roger: Stability and preservation of primary calibration solutions of nutrients, Marine Chemistry 52(1996) ) M. Jill: Reference materials for monitoring nutrients in sea water environment, Fresenius J. Anal. Chem. 352(1995) Vol. 6, No
14 9) Certificate for QC SW4.1 Nutrients in Natural Seawater, VKI. 10) Certificate for QC SW4.2 Nutrients in Natural Seawater, VKI. 11) V. Clancy and S. Willie: Preparation and certification of a reference material for the determination of nutrients in seawater, Anal. Bioanal. Chem. 378(2004) ) :. 13) html 14) M. J. T. Milton and T. J. Quinn: Primary methods for the measurement of amount of substance, Metrologia 38(2001) ) :, 32-8(1993) ) Certificate of Analysis Standard Reference Material 3185, Nitrate Anion Standard Solution, NIST(2005). 17) Certificate of Reference Material No NO2, Nitrate Anion Standard Solution, KRISS(2003). 18),,, :, 85(1990) ) A. Hioki, T. Watanabe, K. Terajima, N. Fudagawa, M. Kubota and A. Kawase: Accuracy in Gravimetric Determination of Nitrate and Nitrite as Nitron Nitrate, Analytical Sciences 6(1990) ) P. A. Liberatore: Automated nitrate analysis of water, Instruments at Work UV-59 (Varian, 1993) ) Certificate of Analysis Standard Reference Material 193, Potassium Nitrate, NIST(1991). 22) NPS Anion Analysis Revision 3, RTI(2005). 23) A. Hioki, M. Kubota and A. Kawase: Accuracy in the precise coulometric titration of ammonia and ammonium ion with electrogenerated hypobromite, Talanta 38(1991) ) JIS K , (2006). 25) : (5), The Chemical Times 200-2(2006) ) C. Kuo, P. Wang and C. Wu: Fluorometric determination of ammonium ion by ion chromatography using postcolumn derivatization with o-phthaldialdehyde, J. Chromatogr. A 1085(2005) ) Certificate of Analysis Standard Reference Material 3186, Phosphate Anion Standard Solution, NIST(2005). 28) Certificate of Reference Material No PO2, Phosphate Anion Standard Solution, KRISS(2003). 29) ph ),,,,, : /, 52(2003) ) JIS K , (1996). 32) Certificate of Analysis Standard Reference Material 3150, Silicon Standard Solution, NIST(2004). 33) Certificate of Reference Material No SI2, Silicon Standard Solution, KRISS(2004) 34) : FIA, 21(2003) ) A.W. Morris and J. P. Riley: The determination of nitrate in sea water, Analytica Chimica Acta 29(1963) ), 5, ), 4, ),, :, 15 ;,,, 74-5(2003) ) : AACS-V. 40) J. Floch, S. Blain, D. Birot and P. Treguer: In situ determination of silicic acid in sea water based on FIA and colorimetric dual-wavelength measurements, Analytica Chimica Acta, 377(1998) ),,,, :, 54(2005) ) K. Fukushi, Y. Nakayama and J. Tsujimoto: Highly sensitive capillary zone electrophoresis with artificial seawater as the background electrolyte and transient isotachophoresis as the on-line concentration procedure for simultaneous determination of nitrite and nitrate in seawater, J. Chromatogr. A 1005(2003) ) :, (1996) AIST Bulletin of Metrology Vol. 6, No September 2007
15 44) :, (1996) ) :, (2006) ),,, :, 52(2003) ) F. Foret, E. Szoko, B. L. Karger: On-column transient and coupled column isotachophoretic preconcentration of protein samples in capillary zone electrophoresis, J. Chromatogr. 608(1992) ) :, (1996) ),,,, :, 53(2004) ) P. Bruno, M. Caselli, G. de Gennaro, B. De Tommaso, G. Lastella and S. Mastrolitti: Determination of nutrients in the presence of high chloride concentrations by column-switching ion chromatography, J. Chromatogr. A 1003(2003) ) M. J. Moorcroft, J. Davis and R. G. Compton: Detection and determination of nitrate and nitrite, Talanta 54(2001) ) :, 55-5(2006) ) J. M. Estela and V. Cerda: Flow analysis techniques for phosphorus, Talanta 66(2005) ) L. Yang, R. E. Sturgeon and J. W. H. Lam: On-line determination of dissolved phosphate in sea-water by ion-exclusion chromatography inductively coupled plasma mass spectrometry, J. Anal. At. Spectrom. 16 (2001) ) A. Hioki, J. W. H. Lam and J. W. McLaren: On-Line Determination of Dissolved Silica in Seawater by Ion Exclusion Chromatography in Combination with Inductively Coupled Plasma Mass Spectrometry, Anal. Chem. 69 (1997) Vol. 6, No
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