試料分解と目的元素精製法_2010日本分析化学会

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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.

1 H2007T(10:3011:00) ICPAES,ICPMS Cd0.4 ppm232 * CODEX STAN , Rev Web Site

2 OK

ml 1.0 m 2 50 110 30 110 10 ml 30 ml 110

3 20g 1 DigiTube 100 L 100 ml (20 g) 100 ml Cd:40 ppb/20 g DigiPREP Jr ml 1.0 m ml 30 ml ml 20 ml ICP/MS 50 ml Cd:1.6 ppb/ml 25

Temp 105 65 =120 105 PP110 3 rd Step 2 nd Step CRM CRM 45 1 st Step OK Time CRM CRM 45 60 70 120 NIST1549MilkPowder [ng/ml] DigiprepBL NIST15491 NIST15492 NIST15491 NIST15492 Na589.592 18.

4 Temp = PP110 3 rd Step 2 nd Step CRM CRM 45 1 st Step OK Time CRM CRM NIST1549MilkPowder [ng/ml] DigiprepBL NIST15491 NIST15492 NIST15491 NIST15492 Na % Mg % Al mg/kg Si <50 mg/kg P % S % K mg/kg Ca % Ti mg/kg Mn mg/kg Fe mg/kg Ni mg/kg Cu mg/kg Zn mg/kg Sr mg/kg Zr mg/kg Mo mg/kg Ba mg/kg DigiPREPJr. DigiPREPMS JISK0102, JIS 100mL 30 DigiSET ml Jr 24MS ml Jr 12MS30 ICP < PerkinElmer 7300DV >

5 10 20g PP PTFE :DigiTUBEs MetaTUBE PTFE DigiTUBEs 100 ml 125 ml MetaTUBE PTFE 100 ml 100 ml 20g 20g DigiTube 100L DigiPREP Jr 1 100mL (20g) 100mL Cd:40ppb/20g mL 1.0m mL 0.5mL 2025 ml mL ml 10mL DigiTUBEs 50mL (25) 145mL ml 0.5mL 0.5mL min. 20mL ICP/MS Cd:1.6 ppb/ml 25

6 PTFE DigiPREP HT Position MetaPREP AT-1 JIS K0102 AsSe mL 115mL 100V 350

7 PC g 0.3g MW DigiPREP Jr.

8 NaKCaMg 4. RhPt CuFe

HF CrIII)CrVI AsIIIAsV) NaKClCaMg 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

InertSEP ME-1 R R R -[CH-CH 2 ] n - C O R CH 2 N CH2 OH C O 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

][CH-CH 2 ]- CO-CH 2 -R CO-CH 2 -R N + 3 WEB www.gls.co.

9 HF CrIII)CrVI AsIIIAsV) NaKClCaMg 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 3M SDB CH2 CH CH2 CH CH2 R R R CH CH2 C CH2 O R: C CH2 OH 1 H He 2 Li Be B C N O F Ne MetaSEP IC-ME 3 Na Mg Al Si P S Cl Ar GLS InertSEP ME-1 R R R -[CH-CH 2 ] n - C O R CH 2 N CH2 OH C O 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 GLS MetaSEP IC-ME R -[CH-CH 2 ] [CH-CH 2 ][CH-CH 2 ]- CO-CH 2 -R CO-CH 2 -R N + 3 WEB 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 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

10 L47mm 100mL M 100mL/10g M Cd MetaSEPCH11Kg/Bottle,

NaKCaMg ICPMS Cd,Pb Na 100004ppm500 ppm 99 % K 3804ppm 500 ppm 99 % Ca

5 % SO 2 4 26004ppm500ppm 95 % 6mL InertSEPME1GL InertSEPICMEGL

11 NaKCaMg ICPMS Cd,Pb Na ppm500 ppm 99 % K 3804ppm 500 ppm 99 % Ca 400ppm4 ppm 90 % Mg 1300ppm4 ppm 90 % Cl ppm500ppm 99.5 % SO ppm500ppm 95 % 6mL InertSEPME1GL InertSEPICMEGL NOBIASCHELATEPA1 NOBIASCHELATEPB1 0.8m0.1MHNO3 BCR505IRMM XSTC760ASPEX ICP Agilent7500cx

12 40mL 0.5M10mL ph:56 50mL 510mLmin1 ICPMS 10mLmin1 0.51mlmin1 a)me1,icme, b)pa1,pb1 10mLmin1 a)2mhno325ml b)10ml,3mhno325ml 10mL2 0.1M5mL 0.1M5mL 10mL2 a)2mhno32ml3,3ml b)3mhno32ml3,3ml 1mL Be100ngml1,Y,In,Tl 10ngml1) 10mL ICPMS S 100mgL1 10 Zn 0.5gL1 S S 5mgL1 ICME,PA1 S Zn 0.1gL1 S 0.1mgL1 ME1, S Mo 15gL1 ICME Mo Mo 5gL1 ME1 Mo Zn Cd Cd 0.03gL gL gL :1512:45ICP-MS 46 (n=4) (n=4) (n=4) (n=4) (n=2) Zn Cd Pb Mo

969 (2008) CdCRM ISOQ0034ISOGUIDE34) NMIJ CRN 7501-a NMIJ CRN 7502-a No.41 No.

13 InertSep ME-1 250mg/6mL or InetSep mini ME-1 280mg MW 0.5g 20mL L 35mL M10mL M 5mL 10mL 0.5M L 50mL 0.5M 5mL 5mL M L ICPAAS : Vol. 57, p.969 (2008) CdCRM ISOQ0034ISOGUIDE34) NMIJ CRN 7501-a NMIJ CRN 7502-a No.41 No.41 1/50 Cd Cd B B Al Al Cr Cr Mn Mn Fe Fe Ni Ni Cu Cu Zn Zn As As Se Se Mo Mo Sb Sb Pb Pb U U Na Na Mg Mg S S K K Ca Ca

14 DigiPREPJr. 120 min 150 min 180 min 210 min DigiPREPJr.50mL 10g 20g 10g 10g 5 g 7 g 10 g ml DigiTUBE, PTFE ml

15 20g DigiPREP CRM NMIJCRN7501aNo.41 NMIJCRN7502aNo.41 Cd Mn Fe Ni Cu Zn Mo Na Mg Cd (N=4) (N=5) DigiTube 50L DigiPREP Jr mL ml (1g)Cd 50ppb,500ppb 5%8ml0.5M10ml ph8-9 Cd:1ppb10ppb/mL H 50 25mL m 5mL 10mL ICP/MS 50ml 2M 5mL 1ml IC-ME 250mg 2M 0.1M

16 Cd InertSep ME-1 250mg/6mL phcd 2M ICP-MS ME-1 CdMoICP/MS NaK InertSep ME-1, MetaSEP IC-ME

無機分析前処理三種の神器_2010jaima

無機分析前処理三種の神器_2010jaima 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