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TRANSCRIPT
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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
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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
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13 14
15
1
16
Time
Temp
45 60 12070
105
65
451st Step
2nd Step
3rd Step
OK
= 120
105
PP 110
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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
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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
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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
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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
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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
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37
MetaPREP AT-1 JIS K0102 As Se
38
39
PC
0.1-0.5g 0.3g40
MW
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41
DigiPREP Jr.
42
1.
2.
3. Na K Ca Mg
4.
43 44
Rh Pt Cu Fe
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45 46
Chelating Cartridge
SPE Manifold
PP Drain RackPTFE Drain Rack
DigiTUBEs Rack
47
SPE
48
HF
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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
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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
•
•
•
•
•
•
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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
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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
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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
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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
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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
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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