無機分析前処理三種の神器_2010jaima

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2 5 6 HCl 80 PP, PPDigiTUBE HNO PP, PPDigiTUBE H2SO4 230 HF 95 PP HCl/HNO PP H2SO4/HNO3 1 st nd HNO3/HClO p213, (5) 2006, SCP SCIENCE Application Guide, SII Nanotechnology 8

450 HF 450 HF PPDigiTUBE 130 PFA,PTFE,TFM 250 1000

PTFE :DigiTUBEs MetaTUBE PTFE 50 ml 100 ml

3 450 HF 450 HF PPDigiTUBE 130 PFA,PTFE,TFM Temp 95 Step 2: ph10 Si,Na,K,B ph10 Si S Pt 65 Step 1: 70 p213, (5) 2006, SCP SCIENCE Application Guide, SII Nanotechnology Time 10 PP PTFE :DigiTUBEs MetaTUBE PTFE 50 ml 100 ml DigiTUBEs 100 ml 125 ml MetaTUBE PTFE 100 ml 100 ml 11 NaB 12

4 Temp 105 = PP rd Step 65 2 nd Step 45 OK Time st Step

Pb, Se 2 ppm 5 ml EPH-1 CRM SCPSCIENCE 500 L

24 ICPAES 50 ml 95 2 17 n=3 100% 18 DigiPREPJr

5 DigiPREPJr. DigiTUBEs DigiPREP Jr As, Cd, Cr, Cu, Fe, Mn, Pb, Se 2 ppm 5 ml EPH-1 CRM SCPSCIENCE 500 L 50mL 5 ml DigiPREP Jr. 24 ICPAES 50 ml n=3 100% 18 DigiPREPJr DigiPREP Jr PP <DigiTUBEs> 0.5 g 10 ml DigiPREP Jr H 2 O g 60 % H 2 O 2 30 % HNO 3 70% 5 ml Plasma Pure H 2 O 2 30% 1 ml DigiPREP Jr 24 DigiTUBEs PP Watch Glass PP 0.5h 1.5h 3h 4h 19 20

6 DigiPREPJr 30 % 2 ml 60 % 2 ml 2 ml DigiTUBEs DigiPREP Jr + Touch Screen Controller ml min 22 CRMDigiPREP DigiPREPJr. 0.5 g 10 ml DigiTUBEs 23 24

Cd NISTCRM 1568a Mn 20.5 0.64 20.0 1.6 Fe 6.9 0.40 7.4 0.9 Cd 0.021 0.007 0.022 0.002 Cu 2.67 0.20 2.4 0.5 NIST CRM 1568a Zn 18.9 0.22 19.4 0.5 Mg 0.

7 Cd NISTCRM 1568a Mn Fe Cd Cu NIST CRM 1568a Zn Mg 0.055% % K 0.127% % DigiPREP100mL JIS 100 ml g DigiSET 50 ml Jr 24MS ml Jr 12MS30 27

8 DigiPREP Jr.50 ml100 L DigiProbe DigiTUBEPP100 ml PP 60 % H 2 O 2 30 % MilliQ NMIJ CRM 7501-a NMIJ CRM 7502-a DigiPREP Jr 100 ml Type DigiTUBE 100 ml g 20g ml ml 0.5 ml (25) 145mL ml 0.5 ml 0.5 ml min

9 20g DigiTube 100 L 100 ml (20 g) 100 ml Cd:40ppb/20g DigiPREP Jr ml 1.0 m mL ml 20 ml 10 ml DigiTUBEs 50 ml ICP/MS Cd:1.6 ppb/ml PTFE mL 115mL 100 V 350 DigiPREP HT Position 35 36

10 MetaPREP AT-1 JIS K0102 AsSe PC MW g 0.3g 39 40

11 NaKCaMg 4. DigiPREP Jr RhPt CuFe 43 44

12 Chelating Cartridge SPE Manifold DigiTUBEs Rack 45 PTFE Drain Rack PP Drain Rack 46 SPE HF 47 48

13 NaKClCaMg CrIII)CrVI AsIIIAsV) PbCd PbCd Pb M EmporeDisk ph H He 3M SDB GLS InertSEP ME-1 CH2 CH CH2 CH CH2 R R R CH CH2 C CH2 R R R -[CH-CH 2 ] n - C O R O R: C CH2 OH CH 2 N CH2 OH C O Li Na K Rb Cs Fr Be Mg Ca Sr Ba Ra Sc Y La Ac Ti V Cr III Zr Hf Retention Efficiency (%) H ph Nb Ta Mo VI W VI V Cu Mn Fe Co Tc Re Ru Os Rh Ir Ni Pd Pt M Cu Ag Au Zn Cd Hg B Al Ga In Tl C Si Ge Sn Pb N P As Sb Bi Sample Load0.025mg/L, 200ml O S Se Te Po F Cl Br I At Ne Ar Kr Xe Rn GLS MetaSEP IC-ME -[CH-CH 2 ] [CH-CH 2 ][CH-CH 2 ]- La Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu R CO-CH 2 -R CO-CH 2 -R N + 3 WEB Ac Th Pa U Np Pu Am Cm Bk Cf Es Fm Md No Lr,, 9347 (1999),, Vol. 31 (2004), pp.37-45,, Vol. 58 (2004), No. 1, pp

MetaSEP ICME I A II A III B IV B V B VI B VII B VIII VIII VIII I B II B III A IV A V A VI A VII A VIII A 1 H He 2 Li Be B C N O F Ne 3 Na Mg Al Si P S Cl Ar 4 K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge

14 MetaSEP ICME I A II A III B IV B V B VI B VII B VIII VIII VIII I B II B III A IV A V A VI A VII A VIII A 1 H He 2 Li Be B C N O F Ne 3 Na Mg Al Si P S Cl Ar 4 K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br Kr 5 Rb Sr Y Zr Nb Mo Tc Ru Rh Pd Ag Cd In Sn Sb Te I Xe 6 Cs Ba La-Lu Hf Ta W Re Os Ir Pt Au Hg Tl Pb Bi Po At Rn 7 Fr Ra Ac-Lr Rf Db Sg Bh Hs Mt Uun Uuu Uub Uuq Uuh Uuo Fr Ra La Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu MetaSEP IC-ME Ac Th Pa U Np Pu Am Cm Bk Cf Es Fm Md No Lr,,,,,,,,,, Vol. 58 (2009), No. 3, pp Vol. 58 (2009), No. 7, pp

ppm99 % Ca 400ppm4 90 % Mg 1300ppm4 90 % Cl

15 L47mm 100mL M 100mL/10g M Cd MetaSEPCH11Kg/Bottle, NaKCaMg ICPMS 6mL InertSEPME1GL InertSEPICMEGL NOBIASCHELATEPA1 NOBIASCHELATEPB1 Cd,Pb Na ppm500 ppm99 % K 3804ppm 500 ppm99 % Ca 400ppm4 90 % Mg 1300ppm4 90 % Cl ppm500 ppm99.5 % SO ppm500 ppm95 % 0.8m0.1MHNO 3 BCR505IRMM XSTC760ASPEX ICP Agilent7500cx He 59 60

16 ICPMS 40mL 0.5M10mL 50mL ph:56 a)me1,icme, b)pa1,pb1 10mLmin1 a)2mhno325ml b)10ml,3mhno325ml 10mL2 0.1M5mL S 100mgL1 10 S S 5mgL1 ICME,PA1 S S 0.1mgL1 ME1, S Zn Zn Zn 0.5gL1 0.1gL1 0.03gL1 510mLmin1 10mLmin1 0.51mlmin1 ICPMS 0.1M 5mL 10mL2 a)2mhno32ml3,3ml b)3mhno32ml3,3ml 1mL Be100ngml1,Y,In,Tl 10ng ml1) 10mL 61 Mo 15gL1 ICME Mo Mo 5gL1 ME1 Mo 2010 Cd Cd 0.006gL gL :1512:45ICP-MS (n=4) (n=4) (n=4) (n=4) (n=2) Zn Cd Pb Mo

17 InertSep ME mg/6 ml or InetSep mini ME mg MW 0.5 g 20 ml 5 L 35 ml M10 ml M 5 ml 10 ml 0.5 M 5 L 50 ml 0.5 M 5 ml 5 ml M L ICPAAS : Vol. 57, p.969 (2008) HfTa 2M IrPtAu 10 ml MetaSEPAnaLig PM 500mg /3mL 2M ICP-MSICP-AES

Cr Fe1000ppm Cr Ni Ni1000ppm 69 70 MetaSEPAnaLigPM08 Hf MetaSEPAnaLigPM08 Cu BT: WH E-1

18 Cr Fe1000ppm Cr Ni Ni1000ppm MetaSEPAnaLigPM08 Hf MetaSEPAnaLigPM08 Cu BT: WH E-1 / E-22 / E-33 / E-44 BT: WH E-1 / E-22 / E-33 / E-44 M 0.3 M /0.1 M M 0.3 M/0.1 M 71 72

19 MetaSEPAnaLigPM08 Pt BT: WH E-1 / E-22 / E-33 / E-44 M 0.3M /0.1 M MRTSPEPb MetaSEP AnaLig Pb L 5 L 0.03M EDTA 5 L ml M 5 L L M 5 L 10 ml.03medta 2.5mLx M 2M HNO3 Matrix H2O Matrix 75 0 Pb Al Ba Cd Co Cu Fe Mn Ni Ti Zn Ca Mg 76

1000 AfterSPE Ni(ppm) 0.38 0.01 0.046 NiRemoval % 99.97 100.00 99.99 PbRecovery 4 ml of 100 ppb Pb in 1000 ppm Matrix Solution was loaded into MRT-SPE cartridge. Pb was eluted by 0.

20 NiCuPb MetaSEP Cr-02 Cr(VI) Sample NonSPE Cu.() AfterSPE Cu(ppm) CuRemoval % PbRecovery MetaSEP AnaLig Cr mg/3ml OriginalCuSolution MRTAnaLigPb01 MRTAnaLigPb02 Sample OriginalNiSolution MRTAnaLigPb02 NonSPE Ni(ppm) AfterSPE Ni(ppm) NiRemoval % PbRecovery 4 ml of 100 ppb Pb in 1000 ppm Matrix Solution was loaded into MRT-SPE cartridge. Pb was eluted by 0.03 M EDTA-NH4 Solution (2mL x 4 times = 8mL). Pb concentration after MRT-SPE must be 50 ppb in elution solution. Recovery Rate is calibrated "Avagage Pb ppb / 50 ppb x 100 (%)" Sample 10 ml ph 0~ ml /min 12 ml /min Sample Loading Elute 3 M HCl/Et-OH 3ml2 Water 20 ml +Phosphate Buffer 5 ml 510 ml /min Rinse Phosphate Buffer 3 ml 510 ml /min 4 M NaCl UV 540 nm Diphenyl-carbazide colourimetric assay Analysis

試料分解と目的元素精製法_2010日本分析化学会

試料分解と目的元素精製法_2010日本分析化学会 H2007T(10:3011:00) ICPAES,ICPMS 22416 http://www.caa.go.jp/safety/pdf/100419kouhyou_1.pdf http://www.caa.go.jp/safety/pdf/100419kouhyou_1.pdf 2010-07-28 Cd0.4 ppm232 * CODEX STAN 193-1995, Rev.3-2007 Web