ICP-AES, AA ppb - 1% ICP-MS ppt - 100ppm SEM-EDX 0.1% - 100% B - U XRF 0.01% - 100% Na - U EMIA ppm - 100% C, S EMGA EMIA : EMGA ppm - 100% O, N, H
Carbon Sulfur Nitrigen Oxygen ISO ISO/TC 17/SC ISO 9556 ('89) ISO TR10719 ('94) ISO 4935 ('89) ISO 13902 ('97) ISO 10720 ('97) WGr. JIS : Japan Industrial Standards Committee ISO : International Standardization Organization JIS JIS G 1201 ('01) JIS G 1211 '11 JIS G1215 ('99 JIS G 1228 ('06) JIS Z 2613('92)* JIS Z 2614('90)
O 2
O 2 3 L/min NDIR H 2 O CO 2 CO SO 2 H 2 O CO 2 CO SO 2
EMIA-920V 140 ~
W Sn + + CO,CO 2 SO 2 &
CO 2 L CO 2 H SO 2 CO
NIST Chemistry WebBook ( http://webbook.nist.gov/chemistry)
NIST Chemistry WebBook ( http://webbook.nist.gov/chemistry)
NIST Chemistry WebBook ( http://webbook.nist.gov/chemistry)
S W Reaction formula MCO2MO2 CO2 CO MSO2 MO2 SO2 MxCyO 2 x MO 2 y CO 2 MxCO 3 x MO 2 CO 2 MxSyO 2 x MO 2 y SO 2 CxHySzO 2 x CO 2 y H 2 OSO 2 of formation W + O2 W O KJ mol W + O2 WO KJ mol Sn + O2 SnO2 KJ mol Fe O2 Fe2O KJ mol Cu O2 CuO KJ mol
ΔHf (kj/mol) μ 10 3 (Pa.s) W W 3 O 8 / WO 3 2274 / 842 6.7, Sn SnO 2 580 Cu CuO 155 Fe Fe 2 O 3 821 0.8 3.2 5.6 W
(W), (Sn), (Cu), (Fe) (Al 2 O 3 ) (Sn) 0.3g (W) 1.5g 1.0g (Sn) 0.3g (W) 3g (Fe) 0.5g 0.1g
O 2 O 2 CO (HC) O 2 O 2 99.5% 700 : Pt HC H 2 O + CO 2 CO CO 2 ( NaOH ) : CO 2 2NaOH+ CO 2 Na 2 CO 3 +H 2 O : H 2 O Mg(ClO 4 ) 2 + 6H 2 O Mg(H 2 O) 6 (ClO 4 ) 2
O 2 : : O 2 : : O 2 : : : W1.5g + Sn0.3g
W1.5g+Sn0.3g 1 1.20 5.75 15.39 2 0.85 6.02 12.42 3 1.32 7.05 16.65 4 0.61 7.46 18.51 5 1.22 5.11 13.40 1.04 6.28 15.27 0.30 0.96 2.45
+ + Ni x x< >CO x x O- CO x x C C + Ni x< > 2 x 2 + Ni x x (CO
EMGA-930 400 ml min He CO N2 H2 H 2 O CO CO 2 (N 2 ) CO2 N2 H2O CO 2 H 2 O TCD N2 H2O N2
CO H 2 N 2 CO 2 H 2 O N 2 H 2 O N 2 N 2 CO 2 H 2 O T C D CuO 450 CO CuO Cu CO 2 H 2 O H 2 2NaOH CO 2 Na 2 CO 3 H 2 O 2KOH CO 2 K 2 CO 3 H 2 O (Mg(ClO 4 ) 2 ) Mg ClO4 2 6H 2 O Mg(H 2 O) 6 ((ClO 4 ) 2 )
14mm 20mm 2 ( ) 1 ( ) 14mm ~ 0 ~ 7kW 32mm
CO H 2 O CO 2
H NIST Chemistry WebBook ( http://webbook.nist.gov/chemistry)
Thermal Conductivity Detecter TCD /10-4 -1-1 H 1649 2 294 201 2 2033 k : 350K 55
- -- -
20s w 7.00 5.00 3s OUT GAS 5s 3s 5s A.Z.wait 50s Drop Time 45s ANALYZE 75s OUT GAS 1 OUT GAS 2 OUT GAS 3 OUT GAS 4 ANANYSE 1 DROP TIME A.Z.WAIT INT.TIME COMP.LEVEL WAIT TIME A.Z.WAIT INT.TIME COMP.LEVEL WAIT TIME A.Z.WAIT INT.TIME COMP.LEVEL WAIT TIME Wait.Time Int.Time
1 1 <1mm 50m
1. 2. Ni 3. 4. 5. 1001000 6.
// / /
1
2 1. 2 / 3
3 1 Al 2 O 3 SiC BN 2 3 X
4 1 2 3 Cu Al 4 5
1. 0.0052 2. W Fe Cu Sn 3. 4., 5. / 1. 2. 3. 4. 5.
: : 0.2g : W 3.0g + Sn 0.3g Fe 0.5g + W 3.0g + Sn 0.3g W+Sn Fe+W+Sn : W3g+ Sn0.3g :Fe0.5g+W3g+Sn0.3g W:3.0g + Sn:0.3g C (massppm) 1 87 2 76 3 86 AVERAGE 83 + Fe0.5g Fe:0.5g+ W:3g + Sn:0.3g C (massppm) 1 138 2 127 3 133 AVERAGE 132
: Sb, :1.0g, : Cu1.5g + Fe1g 0.7mm 0.7mm 0.7mm 0.7mm C (mass ppm) 1 306 2 358 3 393 4 294 5 327 336 : 0.7mm C (mass ppm) 1 81 2 88 3 84 4 82 5 91 85
1. 0.1mm 2. 1 3. W 1. 2. 1. 2. 1 3. 1 4.
(mass ppm)
Al O
1. 1 2. W 3. 1+1 4. 5. 6.
Cu
1. 2. 3. 4. 5. 6. 7. 8.
(mass ppm)
1. 0.5mm 2. 3. 3 1+8) 1+23 46.5%) 30ml+H 2 O 2 30% 500 +H 2 O 60ml
15!! 920 mm 450 mm 1 3604054 1/2 1/6 1/10
massppm 90 6 1.01±0.07 1.04±0.07 1.08±0.12 1.03±0.16 0.98±0.07 1.08±0.08 1.02±0.11 1.03±0.08 1.28±0.14 1.41±0.25 1.58±0.17 1.92±0.12-5.15±1.78
Mg ClO4 2 +
1. 2. 3. 4. 5. 6. 7. 8. 9. 10.
n=5 mass% mass% 4.75 31.96 25.70 20.71 5.00 41.50 13.50 14.43 5.25 49.00 2.31 3.10 5.50 48.91 5.94 6.76 5.75 50.25 0.26 0.34 6.00 49.77 0.39 0.53 6.25 49.18 0.43 0.55 6.50 48.42 2.15 2.59 0.3g+0.5g kw
n=5 mass% mass% 20 47.92 8.97 10.59 30 51.51 0.33 0.43 40 51.32 0.43 0.54 50 51.94 0.11 0.15 60 51.41 0.17 0.22 80 51.34 0.50 0.61 0.3g+0.5g
n=5 mass% mass% 10 49.99 2.44 3.00 20 51.40 0.51 0.67 25 51.76 0.12 0.16 30 51.80 0.30 0.35 40 51.20 3.10 3.85 0.3g+0.5g
n=5 (mass% (g) (%) 0.0 0.3 0.5 0.8 0.0 42.49 47.83 47.97 50.80 7.71 6.92 4.90 0.48 0.5 45.27 51.52 51.34 50.86 (g) 7.90 0.62 0.18 0.57 1.0 50.36 51.52 50.69 51.30 2.23 0.22 0.34 0.78 0.5g+0.5g 0.3g+1.0g
+ 2 Y 2 O 3 + + + 0 0.5 0.3 20.88 21.63 0.45 0.35 0.5 20.82 21.84* 0.28 0.22 1.0 21.75* 0.14 0 0.5 0.3 22.09 21.91 0.14 0.08 0.5 21.97 22.09 0.15 0.09 1.0 21.96 22.17 0.14 0.04 *
55sec 55sec 55sec 50sec 50sec 75sec 50sec He 120sec 50sec He 120sec 30sec
Sn 2g
Si
: X : σ n-1 X σn-1 R : = ( 2.5 3 ) σ n-1 10 C ( or RSD Relative Standard Deviation ) : C.V.(%) = σ n-1 / X 100
/
Y 100ppm 1g 0.1mg 100ppm 0.5g 0.05mg 70ppm 1g 0.07mg (mg) (mg) X
C : 0.0002 4mass%, S : 0.0002 0.34mass%) T.C 30mass%, F.C : 0.3 1.6mass% C : 99.99 % S : 99.99 % WC C 6.15 % C 12 H 22 O 11 C 42.1 % CaCO 3 C 12.0 % K 2 SO 4 S 18.4 %