B B1 6) B1 ê 4 /°BèC C$Bé-Ù pNi 231.604 0.913 1.77 5.26 0.084 0.424 0.254 mg/kg Cu 324.752...
16
ICPͲAES, ICPͲMSಽᨆ䈱䈢䉄䈱ᢱಽ⸃䈫⋡⊛ర⚛♖ᴺ 䌾 㘩ຠਛ㊀㊄ዻಽᨆ䉕䈋䈢ዉ䈱⚫ 䌾 䉳䊷䉣䊦䉰䉟䉣䊮䉴ᩣᑼળ␠ ᢱ೨ಣℂ䊒䊨䉻䉪䊃 ᧄ⾗ᢱ䈱䈍䈇ว䈞వ 㪜㫄㪸㫀㫃 㪑 㫀㫅㪽㫆㪗㪾㫃㫊㪅㪺㫆㪅㫁㫇 㪉㪇㪈㪇㪄㪇㪐 ╙㪎㪈࿁ ᣣᧄಽᨆൻቇળ ᐕળ ᧲ർᄢቇ H2007T(10:30䌾11:00) 䊁䉪䊉䊧䊎䊠䊷 ㄭᐕ䈮䈍䈔䉎䉮䊜䇮ფ䇮᳓ਛ䌃䌤ಽᨆ㔛ⷐ䈱⢛᥊ 㑑ᐭ㘩ຠᆔຬળ ᐔᚑ22ᐕ416ᣣ㐿 䇸㘩ຠਛ䉦䊄䊚䉡䊛ኻ╷䈮㑐䈜䉎ᓟ䈱ㅪ៤䈮䈧䈇䈩䇹 http://www.caa.go.jp/safety/pdf/100419kouhyou_1.pdf ᐔᚑ㪉㪉ᐕ㪋㪈ᣣ䋺䇸᳓⾰ၮḰ䈮㑐䈜䉎⋭䇹䋨ᐔᚑ㪈㪌ᐕෘ↢ഭ⋭╙㪈㪇㪈ภ䋩䈱৻ㇱ䈏ᡷᱜ 㑑ᐭ㘩ຠᆔຬળ䈱㘩ຠஜᐽᓇ㗀⹏ଔ䈫䈚䈩䇮⠴↪ㅳ㑆៨ข㊂䉕㪎 㱘㪾㪆㫂㪾 ㊀㪆ㅳ 䈫䈘䉏䈢䈖䈫䉕〯䉁 䈋䉦䊄䊚䉡䊛䈍䉋䈶䈠䈱ൻว‛䈱ၮḰ୯䈏 㪇㪅㪇㪈 㫄㪾㪆㪣 એਅ䈎䉌 㪇㪅㪇㪇㪊 㫄㪾㪆㪣 એਅ䈮ᒝൻ ☨CdၮḰ୯䋨0.4 ppm䋺ᐔᚑ23ᐕ2䋩ၮḰ୯ᡷᱜ 㑑ᐭ㘩ຠᆔຬળ 䇸㘩ຠਛ䉦䊄䊚䉡䊛ኻ╷䈮㑐䈜䉎ᓟ䈱ㅪ៤䈮䈧䈇䈩䇹 http://www.caa.go.jp/safety/pdf/100419kouhyou_1.pdf 䇮䉝䉪䉶䉴2010-07-28 㘩ຠ ၮḰ୯ ☨䋨₵☨䋩 㪇㪅㪋 㫄㪾㪆㫂㪾ᧂḩ ᶭ㘶ᢱ᳓㪁䋨ේ᳓䋩 㪇㪅㪇㪈 㫄㪾㪆㪣એਅ ᶭ㘶ᢱ᳓㪁䋨ຠ䋩 ᬌ䈚䈩䈲䈭䉌䈭䈇 ☳ᧃᶭ㘶ᢱ ᬌ䈚䈩䈲䈭䉌䈭䈇 * 䊚䊈䊤䊦䉡䉤䊷䉺䊷㘃䉕䉃 䋼㘩ຠਛ䈱䉦䊄䊚䉡䊛䈱ၮḰ୯䋾 ၮḰ୯ 㩿㫄㪾㪆㫂㪾㪀 ዊ㤈䇮☨䉕㒰䈒 䈸䈜䉁䇮⢦⧘䉕㒰䈒 ዊ㤈 㪇㪅㪉 䈳䉏䈇䈚䉊 㪇㪅㪈 ⊹䉕䈇䈢䉅䈱 ⼺㘃 㪇㪅㪈 ᄢ⼺䋨῎䈚䈢䉅䈱䋩䉕㒰䈒 ᩮ⩿䇮⨍⩿ 㪇㪅㪈 䉶䊨䊥䉝䉾䉪䇮䈳䉏䈇䈚䉊䉕㒰䈒 ⪲⩿ 㪇㪅㪉 䈠䈱䈱㊁⩿ 㪇㪅㪇㪌 㘩↪䉨䊉䉮䋬䊃䊙䊃䉕㒰䈒 ♖☨ 㪇㪅㪋 ᶏ↥ᨎ⽴ 㪉 䉦䉨䇮䊖䉺䊁䉕㒰䈒 㗡⿷㘃䋨䉟䉦䈶䉺䉮䋩 㪉 ⤳䉕㒰䈚䈢䉅䈱 㘩ຠ⟲ ⠨ Ⓝ㘃䋨䈠䈳䉕㒰䈒䋩 㪇㪅㪈 ᒁ↪䋺ෘ↢ഭ⋭Web Site 䇸㘩ຠ䈮䉁䉏䉎䉦䊄䊚䉡䊛䇹䈮㑐䈜䉎䌑䋧䌁 http://www.mhlw.go.jp/houdou/2003/12/h1209-1c.html 䈠䈱㘩ຠਛ䈱ᳪᨴ‛⾰䋨䌃䌤䋩ⷙᩰ CODEX STAN 193-1995, Rev.3-2007 㘩ຠ ၮḰ୯ 㘩ຠⷙᩰ 㪚㫆㪻㪼㫏 㪥㫆㪅 䊅䉼䊠䊤䊦䊚䊈䊤䊦䉡䉤䊷䉺䊷 㪇㪅㪇㪇㪊 㩿㫄㪾㪆㫃㪀 㪚㪦㪛㪜㪯 㪪㪫㪘㪥 㪈㪇㪏㪄㪈㪐㪏㪈 㘩Ⴎ 㪇㪅㪌 㩿㫄㪾㪆㫂㪾㪀 㪚㪦㪛㪜㪯 㪪㪫㪘㪥 㪈㪌㪇㪄㪈㪐㪏㪌
Transcript of B B1 6) B1 ê 4 /°BèC C$Bé-Ù pNi 231.604 0.913 1.77 5.26 0.084 0.424 0.254 mg/kg Cu 324.752...
ICP AES, ICP MS
H2007T(10:30 11:00)
22 4 16
http://www.caa.go.jp/safety/pdf/100419kouhyou_1.pdf
Cd 0.4 ppm 23 2
http://www.caa.go.jp/safety/pdf/100419kouhyou_1.pdf 2010-07-28
*Web Site
http://www.mhlw.go.jp/houdou/2003/12/h1209-1c.html
CODEX STAN 193-1995, Rev.3-2007
•–
–
––––
–––
––
OK
1
DigiTube 100 L
100 mL
DigiPREP Jr
50 20 301
2 50 110 30 110
110 240 150.5 mL
20 g
20 mL
100 mL (20 g)
1.0 m
100 mL
ICP/MS
10 mL
50 mL
Cd:40 ppb/20 g
Cd:1.6 ppb/mL25
30 mL
Time
Temp
45 60 12070
105
65
451st Step
2nd Step
3rd Step
OK
= 120
105
PP 110
•
•
•
• CRM
• CRM
• CRM
CRM
NIST1549 Milk Powder[ng/mL]
Digiprep BL NIST1549 1 NIST1549 2 NIST1549 1 NIST1549 2
Na 589.592 18.8 51752 52858 5102 5150 0.513 0.497 0.01 %
Mg 280.271 13.6 11320 11399 1115 1110 0.111 0.12 0.003 %
Al 396.153 160 210 186 4.95 2.59 3.77 2 mg/kg
Si 288.158 7.97 38.2 67.8 2.98 5.83 4.40 <50 mg/kg
P 214.914 21.8 111260 111676 10970 10882 1.09 1.06 0.02 %
S 181.975 44.6 32626 32604 3213 3173 0.319 0.351 0.005 %
K 766.490 39.0 125955 130362 12418 12702 1.26 mg/kg
Ca 317.933 355 117112 117933 11514 11460 1.15 1.3 0.05 %
Ti 337.279 1.67 3.41 1.86 0.171 0.018 0.095 mg/kg
Mn 257.610 0.952 4.09 3.69 0.309 0.267 0.288 0.26 0.06 mg/kg
Fe 259.939 26.6 54.2 52.3 2.73 2.51 2.62 1.78 0.1 mg/kg
Ni 231.604 0.913 1.77 5.26 0.084 0.424 0.254 mg/kg
Cu 324.752 0.205 5.87 4.18 0.559 0.388 0.473 0.7 0.1 mg/kg
Zn 206.200 0.453 442 440 43.6 42.8 43.2 46.1 2.2 mg/kg
Sr 421.552 2.56 38.8 38.4 3.57 3.49 3.53 mg/kg
Zr 343.823 0.303 0.42 0.99 0.012 0.066 0.039 mg/kg
Mo 202.031 0.124 8.34 10.5 0.810 1.01 0.910 mg/kg
Ba 455.403 6.06 14.2 14.1 0.799 0.781 0.790 mg/kg
ICP < PerkinElmer 7300DV >
JIS 100mL
30
•
•
• DigiSET
•
160
50 mL Jr 24 MS 48
100 mL Jr 12 MS 30
DigiPREP Jr. DigiPREP MSJIS K 0102 ,
PP : DigiTUBEsPTFE MetaTUBE PTFE
DigiTUBEs 100 mL
125 mL
MetaTUBE PTFE 100 mL
100 mL
10 20 g
20g
min.
110
320 485
(25)
50
20 50
50
110
20
30
30
420
0.5mL
145mL80
0.5mL
0.5mL
0.5mL
440
30ml
20 25 mL
DigiTube 100 L
100mL
DigiPREP Jr
50 20 301
2 50 110 30 110
110 240 150.5ml
20g
20mL
100mL (20g)
1.0 m
100mL
ICP/MS
10mL
DigiTUBEs50mL
Cd:40ppb/20g
Cd:1.6 ppb/mL25
30mL
PTFE 380
10
DigiPREP HT 250 10 Position
•
• 350
• 65mL
• 115mL
•
•100V 350
MetaPREP AT-1 JIS K0102 As Se
PC
0.1-0.5g 0.3g
MW
DigiPREP Jr.
1.
2.
3. Na K Ca Mg
4.
Rh Pt Cu Fe
HF
Na K Cl Ca Mg
Cr III) Cr VI
As III As V)
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.jp
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
•
•
•
•
•
•
• L 47mm
•
• 100mL
• M
•100mL/10g
• M
Cd
• MetaSEP CH 1 1Kg/Bottle,
• http://www.gls.co.jp/product/catalog/02/61 1.html––
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 ppm 90 %
Mg 1300ppm 4 ppm 90 %
Cl 19000 4 ppm 500ppm 99.5 %
SO42 2600 4 ppm 500ppm 95 %
• 6mL– InertSEP ME 1 GL– InertSEP IC ME GL–– NOBIAS CHELATE PA1– NOBIAS CHELATE PB1
•–– 0.8 m 0.1MHNO3– BCR 505 IRMM
•– XSTC 760A SPEX
• ICP– Agilent 7500cx
a) ME 1, IC ME,b) PA1, PB1
a) 2M HNO3 25mLb) 10mL, 3M HNO3 25mL
10mL 2
0.1M 5mL
40mL
0.5M 10mL
0.1M 5mL10mL 2
a)2M HNO3 2mL 3 , 3mLb)3M HNO3 2mL 3 , 3mL
10mL min 1
5 10 mL min 1
0.5 1 ml min 1
10mL min 1
50mL
1mLBe 100ng ml 1, Y, In, Tl 10ng ml 1)
10mL
pH: 5 6
ICP MS
46
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
47
(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
InertSep ME-1 250mg/6mL or InetSep mini ME-1 280mg
MW
0.5g 20mLL
35mLM 10mL
M 5mL10mL
0.5M L
0.5M 5mL
5mL
M L
ICP AAS
50mL
: Vol. 57, p.969 (2008)
Cd CRMISO Q 0034 ISO GUIDE 34)
Cd Cd B B Al AlCr CrMn MnFe FeNi NiCu CuZn ZnAs AsSe SeMo MoSb SbPb PbU U
Na NaMg MgS SK K
Ca Ca
NMIJ CRN 7502-aNo.41 1/50
NMIJ CRN 7501-aNo.41
DigiPREP Jr.
120 min
210 min180 min
150 min
DigiPREP Jr. 50 mL
5 g 7 g 10 g5
100 mL DigiTUBE, PTFE
10 g 20 g
10g
10g
20 50 mL
20 gDigiPREPCRM
NMIJ CRN 7501 a No.41 NMIJ CRN 7502 a No.41
Cd 0.0470 0.0517 0.0024 0.509 0.548 0.02
Mn
Fe
Ni
Cu
Zn
Mo
Na
Mg
Cd
(N=4)
(N=5)
DigiTube 50 L
10mL
DigiPREP Jr
50 20 301
2 50 110 30 110
110 180 150.5ml
(1g)Cd 50ppb,500ppb
50ml
1ml
2M 5mL
IC-ME 250mg
2M
0.1M
25mL 5mL 10mL ICP/MS
Cd:1ppb 10ppb/mL50
m
H
5%8ml 0.5M 10mlpH8-9
Cd
InertSep ME-1 250mg/6mL
pH Cd2M ICP-MS
ME-1 Cd Mo ICP/MSNa K InertSep ME-1, MetaSEP IC-ME
