2010 Email:info@gls.co.jp 2 OK 3 4
5 6 HCl 80 PP, PPDigiTUBE HNO3 80 120 PP, 80 110PPDigiTUBE H2SO4 230 HF 95 PP HCl/HNO3 95110 PP H2SO4/HNO3 1 st 200 2 nd 80120 HNO3/HClO4 145 200 7 p213, (5) 2006, SCP SCIENCE Application Guide, SII Nanotechnology 8
450 HF 450 HF PPDigiTUBE 130 PFA,PTFE,TFM 250 1000 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 9 45 90 120 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
13 14 1 Temp 105 = 120 105 PP 110 3 rd Step 65 2 nd Step 45 OK Time 45 60 70 120 15 16 1 st Step
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 95 2 17 n=3 100% 18 DigiPREPJr DigiPREP Jr PP <DigiTUBEs> 0.5 g 10 ml DigiPREP Jr 95 65 H 2 O 2 0.5 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
DigiPREPJr 30 % 2 ml 60 % 2 ml 2 ml DigiTUBEs DigiPREP Jr + Touch Screen Controller 95 70 10 ml 21 20 40 60 90 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 0.055% 0.005 0.056% 0.005 K 0.127% 0.001 0.127% 0.0008 25 26 DigiPREP100mL JIS 100 ml 30 160 20g DigiSET 50 ml Jr 24MS48 100 ml Jr 12MS30 27
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 29 30 10 20g 20g 20 30 30 420 50 110 110 2025 ml 50 0.5 ml 0.5 ml (25) 145mL 20 50 80 30 ml 0.5 ml 0.5 ml 320 440 485 min. 31 32
20g DigiTube 100 L 100 ml (20 g) 100 ml Cd:40ppb/20g DigiPREP Jr 1 50 2030 100 ml 1.0 m 2 50 110 30110 30mL 110 24015 0.5 ml 20 ml 10 ml DigiTUBEs 50 ml ICP/MS Cd:1.6 ppb/ml 25 33 34 PTFE 380 10 350 65mL 115mL 100 V 350 DigiPREP HT 250 10 Position 35 36
MetaPREP AT-1 JIS K0102 AsSe 37 38 PC MW 0.1-0.5g 0.3g 39 40
1. 2. 3. NaKCaMg 4. DigiPREP Jr. 41 42 RhPt CuFe 43 44
Chelating Cartridge SPE Manifold DigiTUBEs Rack 45 PTFE Drain Rack PP Drain Rack 46 SPE HF 47 48
NaKClCaMg CrIII)CrVI AsIIIAsV) PbCd PbCd Pb 49 50 3M 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 100 50 5 10 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 www.gls.co.jp 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.85-92 52
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.127-133 Vol. 58 (2009), No. 7, pp.623-631 53 - - - - - 1970 54 - - - - - 1970 55 56
L47mm 100mL M 100mL/10g M Cd MetaSEPCH11Kg/Bottle, http://www.gls.co.jp/product/catalog/02/611.html 57 58 NaKCaMg ICPMS 6mL InertSEPME1GL InertSEPICMEGL NOBIASCHELATEPA1 NOBIASCHELATEPB1 Cd,Pb Na 100004ppm500 ppm99 % K 3804ppm 500 ppm99 % Ca 400ppm4 90 % Mg 1300ppm4 90 % Cl 190004ppm500 ppm99.5 % SO 2 4 26004ppm500 ppm95 % 0.8m0.1MHNO 3 BCR505IRMM XSTC760ASPEX ICP Agilent7500cx He 59 60
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 0.006gL1 0.005gL1 204311:1512:45ICP-MS 62 62 (n=4) (n=4) (n=4) (n=4) (n=2) Zn 93.8 4.9 93.5 2.8 86.5 3.0 99.0 1.1 94.5 1.3 Cd 94.3 5.3 95.0 3.3 92.0 1.5 96.4 2.7 95.2 0.4 Pb 93.4 6.1 95.1 2.4 94.0 1.7 94.6 3.1 92.5 0.6 Mo 15.7 9.6 87.0 3.0 27.7 2.0 68.4 4.0 98.7 1.1 63 63 64
InertSep ME-1 250 mg/6 ml or InetSep mini ME-1 280 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) 65 66 HfTa 2M IrPtAu 10 ml MetaSEPAnaLig PM 500mg /3mL 2M ICP-MSICP-AES 67 20 68
Cr Fe1000ppm Cr Ni Ni1000ppm 69 70 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
MetaSEPAnaLigPM08 Pt BT: WH E-1 / E-22 / E-33 / E-44 M 0.3M /0.1 M 73 74 MRTSPEPb MetaSEP AnaLig Pb-02 500 3 L 5 L 0.03M EDTA 5 L 10-15 ml M 5 L L M 5 L 10 ml.03medta 2.5mLx2 100 90 80 70 60 50 40 30 20 10 M 2M HNO3 Matrix H2O Matrix 75 0 Pb Al Ba Cd Co Cu Fe Mn Ni Ti Zn Ca Mg 76
NiCuPb MetaSEP Cr-02 Cr(VI) Sample NonSPE Cu.() AfterSPE Cu(ppm) CuRemoval % PbRecovery MetaSEP AnaLig Cr-02 250 mg/3ml OriginalCuSolution MRTAnaLigPb01 MRTAnaLigPb02 Sample OriginalNiSolution MRTAnaLigPb02 NonSPE Ni(ppm) 1361 1361 1361 1000 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 0.03 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 (%)" 87 95 88 77 Sample 10 ml ph 0~10.5 0.51 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 78 79 80