à v ] - gl s.à v ] • .\ ± ½. b1 n$ – g | ½. aî ( | ½. aî,¢. • »b-2d ½. b1b b_b®b...

2010

Email: info@gls.co.jp

2

•–

•––

•––

•••

•

3 4

OK

5 6

7 8

145 – 200

1st 200

2nd 80 120

95 110

95

230

80 – 120

80

HNO3/HClO4

H2SO4/HNO3

PPHCl/HNO3

PPHF

H2SO4

80 110 PP DigiTUBEPP,HNO3

PP DigiTUBEPP,HCl

p213, (5) 2006, SCP SCIENCE Application Guide, SII Nanotechnology

9

PtSiSi, Na, K, B

pH10pH10

S

HFHF

1000250130450450

PFA, PTFE, TFMPP DigiTUBE

p213, (5) 2006, SCP SCIENCE Application Guide, SII Nanotechnology 10

Time

Temp

65

95

45 12090

Step 1:

Step 2:

70

11

PP : DigiTUBEsPTFE MetaTUBE PTFE

DigiTUBEs 100 mL

125 mL

MetaTUBE PTFE 100 mL

100 mL12

50 mL100 mL

Na B

13 14

15

1

16

Time

Temp

45 60 12070

105

65

451st Step

2nd Step

3rd Step

OK

= 120

105

PP 110

17

DigiPREP JrDigiTUBEs

As, Cd, Cr, Cu, Fe, Mn, Pb, Se 2 ppm 5 mL EPH-1 CRM SCPSCIENCE 500 L

50mL

5 mL

DigiPREP Jr. 24 95 2

50 mL

ICP AES

DigiPREP Jr.

18

n=3

100%

19

0.5 g10 ml

DigiPREP Jr

60 %H2O2 30 %

DigiPREP Jr

20

95

65

4h0.5h 3h

0.5 g

H2O2

HNO3 70% 5 mL Plasma PureH2O2 30% 1 mL

DigiPREP Jr 24DigiTUBEs PPWatch Glass PP

1.5h

PP <DigiTUBEs>

DigiPREP Jr

21

DigiPREP Jr

22

30 % 2 ml60 % 2 ml

2 ml

DigiTUBEsDigiPREP Jr + Touch Screen Controller

10 mL

7095

20 40 60 90 min

23

CRM DigiPREP

0.5 g

10 mL

24

DigiPREP Jr.

DigiTUBEs

25

Cd

NIST CRM 1568a

26

NIST CRM 1568a

19.4 0.518.9 0.22Zn

0.056 % 0.0050.055 % 0.005Mg

0.127 % 0.00080.127 % 0.001K

20.0 1.620.5 0.64Mn

2.4 0.52.67 0.20Cu

0.022 0.0020.021 0.007Cd

7.4 0.96.9 0.40Fe

27

JIS 100 mL

30

•

•

• DigiSET

•

160

50 mL Jr 24 MS 48

100 mL Jr 12 MS 30

DigiPREP 100 mL

20 g

29

60 %H2O2 30 % MilliQ

DigiPREP Jr. 50 mL 100 L

DigiProbeDigiTUBE PP 100 mL

PPDigiPREP Jr 100 mL Type

DigiTUBE 100 mL

NMIJ CRM 7501-a

NMIJ CRM 7502-a

30

31

10 20 g

32

20g

min.

110

320 485

(25)

50

20 50

50

110

20

30

30

420

0.5 mL

145mL80

0.5 mL

0.5 mL

0.5 mL

440

30 mL

20 25 mL

33

DigiTube 100 L

100 mL

DigiPREP Jr

50 20 301

2 50 110 30 110

110 240 150.5 mL

20g

20 mL

100 mL (20 g)

1.0 m

100 mL

ICP/MS

10 mL

DigiTUBEs50 mL

Cd:40ppb/20g

Cd:1.6 ppb/mL25

30mL

34

35

PTFE 380

10

DigiPREP HT 250 10 Position

36

•

• 350

• 65 mL

• 115 mL

•

•100 V 350

37

MetaPREP AT-1 JIS K0102 As Se

38

39

PC

0.1-0.5g 0.3g40

MW

41

DigiPREP Jr.

42

1.

2.

3. Na K Ca Mg

4.

43 44

Rh Pt Cu Fe

45 46

Chelating Cartridge

SPE Manifold

PP Drain RackPTFE Drain Rack

DigiTUBEs Rack

47

SPE

48

HF

49

Na K Cl Ca Mg

Cr III) Cr VI

As III As V)

50

•– Pb Cd

– Pb Cd

•––– Pb

GLS MetaSEP IC-ME

GLS InertSEP ME-1

3M

SDB

R’

CH2 CH CH2 CH CH2

CH2CCH2CH

RR R

R RR

CH2 CH CH2 CH CH2

CH2CCH2CH

RR R

R RR

-[CH-CH2]n-

CO R

-[CH-CH2]

CO-CH2-R

[CH-CH2] [CH-CH2]-

CO-CH2-RN+

3

O

CH N

CH2

CH2

C

C

O

OH

OH

R:

2

O

CH N

CH2

CH2

C

C

O

OH

OH

R:

2

WEB www.gls.co.jp52

3M EmporeDiskpH

Sample LoadSample Load 0.025mg/L, 200ml0.025mg/L, 200ml

Li Be

Mg

Ca

Sr

Ba

Sc

Y

La

Ti V Cr III

VI

Nb Mo

VI

V

Mn Fe Co

Rh

Ni

Pd

Pt

Cu

Au

Zn

Cd

B

Al

Ga

In

Tl

Sn

Pb

Sb

Bi

O

S

Se

Te

At

I

Br

Cl

F

He

Ne

Ar

Kr

Xe

Rn

N

P

C

Si

Po

As

Hg

Ag

Ir

Ru

Os

Tc

ReWTa

AcRaFr

Cs

Rb

K

Na

H

La

Ac

Ce

Th

Pr

Pa

Nd

U

Pm

Np

Sm

Pu

Eu

Am

Gd

Cm

Tb

Bk

Dy

Cf

Ho

Es

Er

Fm

Tm

Md

Yb

No Lr

Lu

H

pH

Retention Efficiency (%)

10050

5 10

Zr

Hf

Ge

Cu M

, , 9 347 (1999)

, , Vol. 31 (2004), pp.37-45

, , Vol. 58 (2004), No. 1, pp.85-92

53

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

Ac Th Pa U Np Pu Am Cm Bk Cf Es Fm Md No Lr

MetaSEP IC ME

, , , , , Vol. 58 (2009), No. 3, pp.127-133

, , , , , Vol. 58 (2009), No. 7, pp.623-631

MetaSEP IC-ME

54

-

-

-

-

-

1970

55

-

-

-

-

-

197056

•

•

•

•

•

•

57

• L 47 mm

•

• 100 mL

• M

•100 mL/10 g

• M

Cd

58

• MetaSEP CH 1 1 Kg/Bottle,

• http://www.gls.co.jp/product/catalog/02/61 1.html––

59

Na K Ca Mg

ICP MS

Cd, Pb

Na 10000 4 ppm 500 ppm 99 %

K 380 4 ppm 500 ppm 99 %

Ca 400ppm 4 90 %

Mg 1300ppm 4 90 %

Cl 19000 4 ppm 500 ppm 99.5 %

SO42 2600 4 ppm 500 ppm 95 %

60

• 6 mL– InertSEP ME 1 GL– InertSEP IC ME GL–– NOBIAS CHELATE PA1– NOBIAS CHELATE PB1

•–– 0.8 m 0.1 M HNO3– BCR 505 IRMM

•– XSTC 760A SPEX

• ICP– Agilent 7500cx

• He

61

a) ME 1, IC ME,b) PA1, PB1

a)2M HNO3 25 mLb) 10mL, 3 M HNO3 25 mL

10 mL 2

0.1M 5mL

40 mL

0.5 M 10 mL

0.1M 5 mL10 mL 2

a) 2M HNO3 2mL 3 , 3 mLb)3 M HNO3 2mL 3 , 3 mL

10mL min 1

5 10 mL min 1

0.5 1 ml min 1

10mL min 1

50 mL

1 mLBe 100ng ml 1, Y, In, Tl 10 ng ml 1)

10 mL

pH: 5 6

ICP MS6262

ICP MS

S 100 mg L 1 10S

Zn 0.5 g L 1

S 5 mg L 1 IC ME, PA1S

Zn 0.1 g L 1

S 0.1 mg L 1 ME 1,S

Zn0.03 g L 1

Mo 15 g L 1 IC MEMo

Cd 0.006 g L 1

Mo 5 g L 1 ME 1Mo

Cd0.005 g L 1

2043 11:15 12:45 ICP-MS

2010

6363

(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

64

65

InertSep ME-1 250 mg/6 mL or Ine tSep mini ME-1 280 mg

MW

0.5 g 20 mL5 L

35 mLM 10 mL

M 5 mL10 mL

0.5 M 5 L

0.5 M 5 mL

5 mL

M L

ICP AAS

50 mL

: Vol. 57, p.969 (2008) 66

67

Hf Ta

Ir Pt Au

ICP-MS ICP-AES

68

10 mL

20

2M

2MMetaSEP AnaLig®PM500 mg / 3 mL

69 70

Fe1000ppm Ni1000ppm

Cr NiCr

71

M 0.3 M /0.1 M

MetaSEP AnaLig PM 08 Hf

BT:

WH

E-1 /

E-2 2 /

E-3 3 /

E-4 4

72

M 0.3 M /0.1 M

MetaSEP AnaLig PM 08 Cu

BT:

WH

E-1 /

E-2 2 /

E-3 3 /

E-4 4

73

M 0.3M /0.1 M

MetaSEP AnaLig PM 08 Pt

BT:

WH

E-1 /

E-2 2 /

E-3 3 /

E-4 4

74

75

MRT SPE Pb

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

.03 M EDTA 2.5 mL x 2

76

0

10

20

30

40

50

60

70

80

90

100

Pb Al Ba Cd Co Cu Fe Mn Ni Ti Zn Ca Mg

2M HNO3 MatrixH2O Matrix

M

77

Ni Cu Pb

95100.000.011361MRT AnaLig Pb 02

8799.970.381361MRT AnaLig Pb 01

1361Original Cu Solution

Pb RecoveryCu Removal%

After SPECu (ppm)

Non SPECu. ( )Sample

8899.990.0461000MRT AnaLig Pb 02

1000Original Ni Solution

Pb RecoveryNi Removal%

After SPENi (ppm)

Non SPENi (ppm)Sample

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 (%)"

78

MetaSEP AnaLig Cr-02 250 mg/3mL

Sample Loading

Elute

Diphenyl-carbazide colourimetric assay Analysis

4 M NaCl

3 M HCl/Et-OH 3ml 2

Water 20 mL+Phosphate Buffer 5 mL

0.5 1 mL /min Rinse

Sample 10 mL

pH 0~10.5

MetaSEP Cr-02 Cr(VI)

Phosphate Buffer 3 mL

1 2 mL /min

5 10 mL /min

UV 540 nm

5 10 mL /min

79 80