-
11-1480083-000291-01
QA/QC
(QA/QC Handbook for the Environmental Pollutants
Analysis and Sampling Techniques)
2005
-
QA/QC
(QA/QC Handbook for the Environmental Pollutants
Analysis and Sampling Techniques)
2005
-
- i -
,
.
,
.
.
.
, ,
.
.
(WTO, World Trade Organization) WTO/TBT
(Technical Barrier to Trade)
, ,
.
ISO (International Standard Organization)
ISO/IEC Guide 17025:2005
ILAC (International Laboratory Accreditation
Coorperation) .
1983 4 , ,
,
.
-
- ii -
2005 7
,
. ISO/IEC
Guide 17025:2005
.
.
,
.
2005 7
-
- iii -
. QA/QC
1.0 3
1.1 4
1.1.1 4
1.1.2 4
1.2 8
1.2.1 8
1.2.2 12
1.2.3 14
1.2.4 17
1.2.5 18
1.3 19
1.4 19
1.5 , 20
1.6 20
1.7 20
1.8 20
1.9 21
1.10 21
1.11 21
1.12 21
1.13 22
2 .0 22
2.1 22
-
- iv -
2.1.1 22
2.2 23
2.2.1 23
2.2.2 25
2.2.3 25
2.2.4 , 26
2.3 27
2.3.1 UV-VIS 27
2.3.2 29
2.3.3 30
2.3.4 33
2.3.5 34
2.3.6 34
2.3.7 34
2.3.8 - 41
2.3.9 41
2.3.10 41
2.3.11 42
2.3.12 42
2.3.13 pH 42
2.3.14 43
2.3.15 43
2.4 44
3 .0 47
3.1 47
3.1.1 47
3.1.2 49
3.2 52
3.3 52
3.3.1 52
3.3.2 53
3.3.3 59
-
- v -
3.3.4 59
3.3.5 60
3.3.6 60
4 .0 60
4.1 63
4.2 QA/QC 76
4.3 78
4.3.1 79
4.3.2 81
4.3.3 88
4.3.4 93
4.3.5 97
5 .0 97
5.1 97
5.2 98
5.2.1 pH 98
5.2.2 98
5.2.3 , , , 99
5.2.4 100
5.2.5 101
5.2.6 102
5.2.7 - 103
5.3 104
5.3.1 104
5.3.2 104
5.3.3 113
5.4 113
5.4.1 QC 113
5.4.2 114
5.4.3 118
5.4.4 118
-
- vi -
5.4.5 118
5.5 119
5.6 120
. QA/QC
1.0 127
1.1 127
1.1.1 127
1.1.2 127
1.1.3 129
1.1.4 130
1.2 131
1.2.1 131
1.2.2 131
1.2.3 132
1.2.4 132
1.3 135
1.3.1 135
1.3.2 135
1.3.3 136
1.3.4 136
1.4 136
1.4.1 137
1.5 139
1.5.1 143
1.5.2 144
1.6 146
1.6.1 146
1.6.2 147
1.6.3 (suspended metal) 147
1.6.4 VOC 147
-
- vii -
1.6.5 148
1.6.6 , BOD, COD, ,
151
1.6.7 151
1.6.8 , TRPH 151
1.7 , 152
1.7.1 152
1.8 157
1.8.1 157
1.8.2 157
1.9 157
1.9.1 QA/QC 157
1.9.2 QC 158
2 .0 161
2.1 161
2.2 162
2.2.1 () 162
2.2.2 164
2.3 168
2.4 171
2.4.1 171
2.4.2 , 173
2.4.3 174
2.4.4 175
2.4.5 175
3 .0 197
3.1 197
3.2 199
3.2.1 199
3.2.2 206
3.3 207
-
- viii -
3.3.1 207
3.3.2 210
3.4 214
3.4.1 214
3.4.2 216
3.4.3 217
4 .0 222
4.1 222
4.2 223
4.3 224
4.3.1 224
4.3.2 () 225
4.3.3 , 227
4.3.4 229
5 .0 234
5.1 234
5.1.1 234
52 235
5.2.1 235
5.3 235
5.3.1 236
5.3.2 238
5.3.3 238
5.4 238
5.4.1 238
5.4.2 239
5.4.3 239
5.4.4 239
5.4.5 240
5.4.6 240
5.5 240
-
- ix -
5.6 241
5.7 243
5.7.1 243
5.7.2 243
6 .0 245
6.1 245
6.2 245
6.2.1 245
6.2.2 250
6.2.3 253
1 BOD5 259
2 NELAC 297
302
-
- x -
List of Figure
. QA/QC
-1. 11
-2. 12
-3. 12
-4. (Erlenmeyer ) 12
-5 13
-6 Florence 13
-7 13
-8. 13
-9. Mohr 13
-10. - stopcock 13
-11. 13
-12. Bchner 14
-13. Hirsh 14
-14. 15
-15. 16
-16. 17
-17. 17
-18. 24
-19. 24
-20. cut filter 26
-21. 38
-22. 38
-23. 38
-24. 38
-25. 38
-26. 88
-27. 94
-28. (Cu) ICP/MS
Yttrium89
1 (batch) 96
-29. BOD5 (GGA) 96
-
- xi -
. QA/QC
-1. 129
-2. 130
-3. (coverall) 134
-4. (flip-down) 134
-5. VOCs 139
-6. 144
-7. 145
-8. 146
-9. 163
-10. 166
-11. 166
-12. 168
-13. 169
-14. 169
-15. 170
-16. - 171
-17 174
-18. 177
-19. 178
-20 179
-21. 180
-22. 181
-23. 183
-24. 184
-25. 184
-26. 195
-27. (tedlar ) 196
-28. 200
-29. 203
-30. 204
-31. 209
-32. 212
-
- xii -
-33. 212
-34. Peristaltic pump 212
-35. Air-lift Pump 212
-36. Bailer 212
-37. 213
-38. (Auger) 225
-39. 226
-40. Peterson sampler 226
-41. Eckman sampler 227
-42. Ponar sampler 227
-43. 229
-44. 230
-45. 230
-46. 230
-47. 231
-48. 232
-49. 232
-50. 233
-51. Coliwasa 237
-52. Trier 237
-53. Sampling Thief 237
-54. Dipper 237
-55. 241
-56 - 243
-57. 244
-58. 4 244
-59. 247
-60. 2 254
-61. periphytometer 256
-
- xiii -
List of Table
. QA/QC
-1. OIML 6
-2. 6
-3. 6
-4. 7
-5. 7
-6. 8
-7. (plastic ware) 9
-8. 9
-9-(1). - 1 10
-9-(2). -2 10
-10 11
-11. 19
-12. 24
-13. 25
-14. 26
-15. 28
-16. 29
-17. 31
-18. (graphite Furnace) 32
-19. 39
-20. 39
-21. 40
-22. pH 43
-23. 44
-24. 45
-25. 48
-26. 49
-27. , 53
-28 55
-
- xiv -
-29. ( ) 55
-30. 56
-31. 57
-32. 58
-33. 59
-34. 61
-35. QA/QC 77
-36. 78
-37. GC/MS 80
-38. (T-N)
84
-39.
1 , 90
-40 GC/MS 92
-41. ETC (environmental technology centre)
92
-42. 102
-43. mg/L me/L 103
-44. 105
-45. 106
-46. 107
-47. ( ) 108
-48. ( ) 109
-49. ( ) 110
-50. ( ) 111
-51. () 112
. QA/QC
-1. 130
-2. 133
-3. 137
-4. 139
-5. 154
-
- xv -
-6. 154
-7. 155
-8. 155
-9. 156
-10. 156
-11. 167
-12. 167
-13. 172
-14. 177
-15. 185
-16. 187
-17. 202
-18. 203
-19. 205
-20. 206
-21. 216
-22. 223
-23. ASTM 228
-24. 240
-25. 248
-26. 249
-27. 253
-
I. QA/QC
-
. QA/QC 3
I. QA/QC
1.0
, ,
,
(, ) .
, .
.
.
, .
, (, )
(, , ,
)
, ,
(, ) .
, ,
. ,
, ,
.
-
4 QA/QC
1.1
. ,
(analytical balance) 0.000 1 g
. QC
.
. OIML (
, International Organization of Legal Metrology)
5
(, ) .
1.1.1
.
, .
, (
.).
.
.
,
.
.
1.1.2
1.1.2.1
E1, E2 F1
, .
(OIML, international organization of legal
-
. QA/QC 5
metrology)
. OIML IP (1993)
" E1, E2, F1, F2, M1, M2, M3 " , , ,
, , , , OIML IR 33 "
" 20 C 0.001 2 g/cm3
8.0 g/cm3 (conventional mass)
. 8.0 g/cm3
(stainless steel) (gray cast iron) .
E1, E2, F1, F2, M1, M2, M3 (1 mg~50 kg) .
E1 : E2
E2 : F1
(high resolution) (ultra accurate weight)
F1 : F2
F2 : M1
M1 : M2
M2 : M3
OIML -1 .
, -2 -3 .
1.1.2.2
.
-4 , OIML
1-1 .
-
6 QA/QC
-1. OIML ( mg)
E1 E2 F1 F2 M1 M2 M3
500 kg 0.25 0.75 2.5 7.5 25 75 250
200 kg 0.10 0.30 1.0 3.0 10 30 100
100 kg 0.05 0.15 0.5 1.5 5 15 50
50 kg 0.030 0.10 0.30 1.0 3.0 10 30
20 kg 0.025 0.080 0.25 0.8 2.5 8 25
10 kg 0.020 0.060 0.20 0.6 2 6 20
5 kg 0.015 0.050 0.15 0.5 1.5 5 15
2 kg 0.012 0.040 0.12 0.4 1.2 4 12
1 kg 0.010 0.030 0.10 0.3 1.0 3 10
500 mg 0.008 0.025 0.08 0.25 0.8 2.5 -
200 mg 0.006 0.020 0.06 0.20 0.6 2.0 -
100 mg 0.055 0.015 0.05 0.15 0.5 1.5 -
50 mg 0.004 0.012 0.04 0.12 0.4 - -
20 mg 0.003 0.010 0.03 0.10 0.3 - -
10 mg 0.002 0.008 0.025 0.08 0.25 - -
5 mg 0.002 0.006 0.020 0.06 0.20 - -
2 mg 0.002 0.006 0.020 0.06 0.20 - -
1 mg 0.002 0.006 0.020 0.06 0.20 - -
-2.
10-6
1
10
-5
10-4
-3.
1 - : 0.1 C
1 - : 1 % R.H
1 - : 200 Pa
-- ,
-
. QA/QC 7
-4.
(mg) (mg)
,
-5 .
-5.
1. : 2. :
3. : 4. :
5. : 6. :
7.
(g)
1.0 mg
2.0 mg
5.0 mg
10.0 mg
20.0 mg
50.0 mg
100 mg
200 mg
300 mg
500 mg
1.0 g
20.0 g
30.0 g
50.0 g
100 g
200 g
-
8 QA/QC
1.2
1.2.1
,
, , .
.
.
-6~-9 . -10
(tolerance) .
,
(Tefzel, ethylene-tetrafluoroethylene)
.
-6.
,
C
(borosilica
te glass)
200
150 C
: Pyrex (Corning
glass works)
KIMAX
(Qwens-Ilinois)
: Corning
1000
1050 ,
1100 ( )
1400 (
)
: Vycor (Corning)
-
. QA/QC 9
-7. (plastic ware)
C
Polyethylene 115
HF ,
(
, )
Polystyrene 70HF ,
Teflon 250
-8.
(resin code), C
LDPE1)
-100
HDPE2)
-76
PP3) 0
PPCO4)
-40 -
PMP5)
20
FEP6) -270
ETFE7)
-105
PC8)
-135
PS9) 20
PSF10)
-100
1) LDPE : low-density polyethylene, 2) HDPE : high- density
polyethylene
3) PP : polypropylene, 4) PPCO : polypropylene copolymer
5) PMP : polymethylpentene, 6) FEP : teflon (fluorinated
ethylene propylene)
7) ETFE : tefzel (ethylene - tetrafluoroethylene), 8) PC :
polycarbonate
9) PS : polystyrene, 10) PSF : polysulfone
-
10 QA/QC
-9-(1). - 1
/
/
LDPE S S S M S M
HDPE S S S M S M
PP S S S M S M
PPCO S S S M S M
PMP S S M M S M
FEP S S S S S S
ETFE S S S S S S
PC S U U U U U
PS S M S U S U
PSF S M M U M U
S = , M = , U =
-9-(2). -2
/
/
/
LDPE M U U M U
HDPE M M M M M
PP M M M M U
PPCO M M M M U
PMP M M U M M
FEP S S S S S
ETFE S M S M S
PC M U U U U
PS U U U U U
PSF M U U U U
-
. QA/QC 11
-10 (tolerance)
(mL) (mL) (%)
(graduated flask)
25 0.03 0.12
50 0.05 0.10
100 0.08 0.08
200 0.10 0.05
250 0.11 0.044
300 0.12 0.4
500 0.15 0.03
1000 0.30 0.03
2000 0.50 0.025
(transfer pipette)
2 0.006 0.3
5 0.01 0.2
10 0.02 0.2
25 0.025 0.2
30 0.03 0.1
50 0.05 0.1
100 0.08 0.08
200 0.10 0.05
5 0.01 0.2
10 0.02 0.2
30 0.03 0.1
50 0.05 0.1
100 0.10 0.1
.
-1 .
PYREX
USA
KIMAX
USA
STANDARD
TAPER SIZE
TS
16
TS
19
A A
TO
CONTAIN
STOCK NO.
(500 0.20) mL 500 mL
TC 20 C TC 20 C
NO 5680 NO 5680
-1.
-
12 QA/QC
, (reflux)
(ground glass joint)
. standard taper" . TS
.
A"
.
100 mL TC 20 C" , TC to contain
20 C 100.00 mL .
25 mL TD 20 C" , TD to deliver
20 C 25.00 mL .
1.2.2
.
1)
:
(-2)
: (-3)
(erlenmeyer ) :
(-4)
: ,
(NO2, Br ) (-5)
Florence :
(-6)
: ,
(-7)
-2. -3. -4.
-
. QA/QC 13
-5 -6 Florence -7
2)
: (-8)
Mohr : (-9)
- stopcock : ,
(-10)
: (-11)
- :
- :
- dropping : 1~2
-8. -9. Mohr -10. - stopcock
-11. ( , , dropping )
-
14 QA/QC
3)
Bchner - (-12)
Hirsh - (-13)
-12. Bchner
-13. Hirsh
1.2.3
1)
(volumetric pipette) whole
. (meniscus)
.
.
.
3
. .
3 cm
-
. QA/QC 15
(filler) .
.
.
.
( 2~3 cm .)
-14 ,
(meniscus) .
.
. .
15 -15
.
.
-14.
,
.
.
-
16 QA/QC
-15.
2)
.
Geissler
.
.
0 mL .
.
(coke) .
.
. 0.1
mL 1/10 0.01 mL .
-16 .
-17 .
.
(after flow) . 0.5 mL ,
20 mL 40 .
.
.
.
-
. QA/QC 17
-16. -17.
1.2.4
1)
. .
Chromic acid
Na2Cr2O72H2O 92 g 460 mL 800 mL
.
Sodium (Potassium) Alkoxide
NaOH 120 g (KOH 105g) 120 mL 95 % 1 L
. , 15
,
.
trisodiumphosphate (60 g Na3PO4, 30 g , 500 mL
) .
(KMnO4) (MnO2)
30 % NaHSO3 .
2)
.
-
18 QA/QC
.
1.2.5
1)
.
2)
40~50 C.
3)
, .
4)
(90 C )
. , ,
.
.
.
.
.
,
-11 .
-
. QA/QC 19
-11.
()
, ,
()
, ,
, , 20 %
(8 %)/
(17 %) 4
, ,
400 C 1
, , 105 C 1
, , 105 C 1
, ,
, ,
- 160 C
2
- 121 C
15
1.3
1 C ,
ASTM
.
.
1.4
.
-
20 QA/QC
180 C , 2 C
. .
1.5 ,
, ,
. 4 C
, 2 C
. .
1.6 (water bath)
5100 C
.
.
1.7 (, hot plate)
.
100 C , 2 C
.
.
1.8 (PFE, pressured fluid extractor)
, , .
-- , .
,
. .
, .
.
-
. QA/QC 21
.
1.9 (soxhlet extractor)
,
. (support) (thimble)
.
. .
1.10 (rotary evaporator)
.
.
. .
.
1.11 (auto clave)
121 C , -
, .
.
.
1.12 (incubator)
2 C , .
. .
-
22 QA/QC
1.13
.
(membrane filter) .
6
.
.
.
2.0
2.1
2.1.1
,
.
.
.
.
. , (correlation coefficient)
0.9998 .
.
.
.
(CCS, continuing calibration
standard) . 5 % .
(CVS, calibration verification standard) .
.
-
. QA/QC 23
10 % .
,
(LCS, laboratory control standard) . 15
% .
10 CCS .
5 % .
CCS CVS , ,
.
2.2 (spectrophotometer)
2001000 nm (baseline, blank) ,
, .
.
.
12 .
,
1) (stray light) .
2.2.1
1) (line spectrum)
-18
(m) . (m)
t
(zero) .
-12 .
1) ,
-
24 QA/QC
m t
-18.
-12.
(nm)
486.13 656.28
486.00 656.10
253.65 365.01
435.88 546.07
2) (holmium)
. -19 1 nm
. (scan rate)
(peak) .
.
-19.
-
. QA/QC 25
2.2.2
110 C 3 (1 ) N/20
. 0.030 3
g/L .
10.0 mm 25 C 1 nm
.
-13 ,
.
-13. (%) (25 C)
(nm) (%) (nm) (%)
220 0.446 35.8 340 0.316 78.3
230 0.171 67.4 350 0.559 27.6
240 0.295 50.7 360 0.830 14.8
250 0.495 31.9 370 0.987 10.3
260 0.633 23.3 380 0.932 11.7
270 0.745 18.0 390 0.695 20.2
280 0.712 19.4 400 0.396 40.2
290 0.428 37.3 420 0.124 75.1
300 0.149 70.9 440 0.054 88.2
310 0.048 89.5 460 0.018 96.0
320 0.063 86.4 480 0.004 99.1
330 0.049 71.0 500 0.000 100
2.2.3 (stray light)
-14
-20
cut filter .
-
26 QA/QC
-14.
(nm)
200~220 ,
300~330
700~800
-20. cut filter (%)
2.2.4
2.2.4.1
,
,
.
.
2.2.4.2
1)
.
-
. QA/QC 27
2)
,
, .
, .
,
.
.
3)
.
, ,
.
2.3
2.3.1 UV-VIS (UV-VIS spectrophotometer)
.
, . (DI,
didymium) .
UV-VIS .
.
CCS . 5 % .
CVS . 10 % .
, 10 .
.
-
28 QA/QC
2.3.1.1
(DI, didymium) , 500,
505, 515 520 nm ( 22~23
g 1 % HCl 1 L .).
505 515 nm
, . -15 .
-15.
:
:
500 nm 505 nm 510 nm 515 nm 520 nm
2.3.1.2 (linearity check)
50 % 510 nm
.
50 % , 1/2
. -16 .
-
. QA/QC 29
-16.
:
510 nm
50 %
50 %
50 %
50 %
50 %
50 %
50 %
50 %
50 % 1/2 .
2.3.2 (ion chromatograph)
,
,
(suppressor) .
(auto-sampler) ,
.
(IDL, instrument detection limit), ,
.
.
.
-
30 QA/QC
2.3.3 (AAS, atomic absorption spectrophotometer)
, , ,
, 190800 nm
,
.
, , .
.
.
2.2.3.1 (flame and graphite furnace)
AAS .
. (sensitivity check standard) .
-17
. 0.200 10 %,
.
-17-18 .
2.3.3.2
air-acetylene (aspiration) .
.
. , ,
, , , -
.
.
-
. QA/QC 31
-17.
:
,
mg/L
,
mg/L (%)
(Al) 50
(Sb) 25
(Ba) 20
(Be) 1.5
422.7 nm (Ca) 4.0
287.4 nm (Ca) 60
228.8 nm (Cd) 1.5
368.4 nm (Cd) 850
(Co) 7.0
(Cr) 4.0
(Cu) 4.0
(Fe) 5.0
(Pb) 20
(K) 2.0
(Mg) 0.3
(Mn) 2.5
(Mo) 30
(Ni) 7.0
(Si) 100
(Na) 0.5
(Sr) 5.0
(Sn) 150
(Ti) 80
(Tl) 30
(W) 450
(Zn) 1.0
(Zr) 300
: 10 %
-
32 QA/QC
-18. (graphite Furnace)
:
,
mg/L
,
mg/L (%)
(Al) 0.05
(Sb) 0.04
(AS) 0.04
(Ba) 0.03
(Cd) 0.003
(Co) 0.03
(Cr) 0.007
(Cu) 0.01
(Fe) 0.01
(Mn) 0.005
(Mo) 0.025
(Ni) 0.04
283 nm (Pb) 0.025
271 nm (Pb) 0.016
(Se) 0.06
(Si) 0.14
286 nm (Tn) 0.14
224.6 nm (Tn) 0.08
(Ti) 0.21
(V) 0.15
Zn) 0.007
: 10 %
2.3.3.3 AAS
.
, .
100 mg
. 100 mg/L .
1) : 4 mL HNO3 () 0.100 g ,
HNO3 5 mL , 1,000 mL .
2) : CaCO3 0.2497 g 50 % HNO3 .
-
. QA/QC 33
HNO3 10 mL , 1,000 mL .
3) : CrO3 0.1923 g , 10 mL HNO3
1,000 mL .
4) : 2 mL HNO3 0.100 g 10 mL HNO3
, 1,000 mL .
5) : 10 mL 50 % HCl () 3 mL HNO3
0.100 g 5 mL HNO3 1,000 mL
.
6) : HNO3 Pb(NO3)2 0.1598 g , 1,000 mL
.
7) : 50 % HNO3 MgO 0.1658 g , 10 mL HNO3
1,000 mL .
8) : 1 mL HNO3 10 mL HCl 0.100 g
, 1,000 mL .
9) : 10 mL HNO3 0.100 g , ,
1,000 mL .
10) : 0.1907 g KCl , 1,000 mL .
11) : NaCl 0.2542 g 10mL HNO3 ,
1,000 mL .
12) : 100 mL HCl 1.000g , 1,000
mL .
13) : 10 mL 50% HCl 1.000 g , 1,000
mL .
2.3.4 (inductively coupled plasma
atomic emission spectrometer)
, , ,
(peak resolution), 190800 nm
,
.
, , .
-
34 QA/QC
.
.
2.3.5 (inductively coupled plasma mass
spectrometer)
, ,
, ,
,
.
, , .
.
.
2.3.6 (gas chromatograph mass
spectrometer)
0.2 C , ,
, / .
, ,
, (column bleeding) , ,
, .
,
.
, .
.
.
2.3.7 (GC, gas chromatography)
.
-
. QA/QC 35
, .
0.2 C , ,
, / .
, , ,
(column bleeding) ,
. ,
.
, .
.
.
2.3.7.1
, GC
, .
, .
.
. septum bleed
(septum) . (
septum sweep) (carrier
gas) bleed . (column) bleed
(column)
. (column)
. (surface-active agent) GC
(column) .
(ghost peak) (column)
.
.
(column) .
-
36 QA/QC
2.3.7.2
GC .
(ELCD , electrolytic conductivity detector)
- (contactor) - (separator)
. . -
contactor
- .
(electrometer) .
, , (nitroamine)
.
(ECD, electron capture detector) (Pt)
(Ti) - (emitter) ( -63
)
. (emitter)
. 100
- .
(electrophilic sample molecule)
. ,
.
. , ,
, ,
(-21).
(FID, flame ionization detector) (nozzle),
(ion collector) ()
,
, . (column)
(charged intermediate)
. , electrometer
. FID
-
. QA/QC 37
.
FID
, .
(-22).
(PID, photoionization detector)
(effluent) (picogram)
. UV
(photon) .
UV (ionization potential)
. PID , ,
(-23).
(MS, mass spectrophotometer) ,
(fragmentation pattern) . MS
7 eV (beam) .
(quadrupole mass)
.
mass .
(TCD, thermal conductivity detector) ,
(thermistor) (block)
, , ,
. (O2, N2,
H2O, ) .
(100 ppm ) (-24).
(FPD, flame photometric detector)
. (394 nm),
(526 nm) (-25).
-
38 QA/QC
-21. -22.
-23. -24.
-25.
-
. QA/QC 39
-19 , -20
.
-19.
(detection limit)
, ECD 1 10-9
, FID 1 10-6
, PID 100 10-9
, TCD 100 10-6
, FPD P : 500 10-9, S : 500 10-9
- , NPD1
1 10-6
1 nitrogen-phosphorus detector
-20.
TCD ECD FID NPD FPD ELCD PID
He
H2
N2
/ H2
Air
make-up
N2
He
ArCH2
2.3.7.3 (column), ,
1) (column)
(column) 2~7 mm ( (column)
.) ,
.
2)
- (column)
-
40 QA/QC
. , , , ,
.
- (support)
, , , ,
, ,
. ,
, .
-21 .
- (bridge
intermediate) (styrene)
.
3)
(column)
.
(column)
.
.
-21.
, squalane,
, , ,
,
, ,
-
. QA/QC 41
2.3.8 - (purge & trap equipment)
, leak,
. ,
.
,
.
, .
.
.
2.3.9 (high performance liquid chromatograph)
, , , ,
.
, ,
.
, .
,
. ,
.
.
.
2.3.10
(high performance liquid chromatograph mass spectrometer)
, , , ,
.
,
.
, .
-
42 QA/QC
, .
.
.
2.3.11 (auto analyzer)
, ,
.
.
,
. ,
.
.
.
2.3.12
, ,
.
.
,
. ,
.
.
.
2.3.13 pH
,
. ,
. pH -22 .
-
. QA/QC 43
-22. pH
: :
: pH :
ID pH C
pH 7.00
pH 4.00
pH 1.00
QC
QC :
(RPD) : :
(%R) : :
2.3.14
.
,
. ,
.
2.3.15
.
.
formazine .
Formazine (Formazine stock solution)
.
-
44 QA/QC
1 : 1.00 g hydrazine sulfate (NH2)2H2SO4 100 mL
.
2 : 10 g hexamethylene tetramine (CH2)6H4 100 mL
.
6 ,
, .
Formazine 100 mL (volumetric flask) 1
5 mL 2 5 mL 24 , 100
mL . 400 NTU (nephelometric
turbidity unit) . .
, . ,
. -23 .
-23.
:
0.4 NTU 4.0 NTU40
NTU
100
NTU0.2 NTU 2.0 NTU
20
NTU
100
NTU
2.4
.
.
-
. QA/QC 45
-24 .
. ()
.
-24.
pH meter
probe
probe
/
probe
probe
probe
probe
as described
short term()
long term()
probe
Use proper filling
solution and storage
replace light bulb
adjust scale deflection
( )
()
()
UV-VIS
check lamp alignment
( )
replace lamp( )
clean windows( )
clean sample compartment
( )
clean cuvettes after use
( )
()
AA/flame
Clean nebulizer( )
Clean burner head()
Check tubing, pump, and lamp
(, , )
-
46 QA/QC
-24. ()
AA/flame
Clean quartz windows
( )
Check electronics( )
Check optics( )
6 ()
()
AA/ graphite
check graphite tube( )
flush autosampler tubing
( )
,
check electronics()
6 ()
ICP
clean realing torch( )
,
check waterlines, gases torch
compartment
check wavelength calibration
adjust as needs ( )
check interelement interference
standard
6 ()
6 ()
6
TOC analyzer
change catalyst()
inspect combution tube
6
Gas chromatographs
,
GC
(column)
check temperature cal.
()
()
Purge and trap
clean sparger
check purge flow
-
. QA/QC 47
-24. ()
Autoanalyzers
, flush system
spill
sample probe
optics
pump rollers, platens,
colorimeter filter
flow cells, oil ,
()
6 ()
,
Autoclaves
gaskets
sterilization indicator tape
6 ()
3.0
3.1 (reagent-grade water)
3.1.1
(reagent-grade water) .
-
48 QA/QC
, , S/cm
289K0.056 1.0 0.25 5.0
, , Mcm
298K18 1.0 4.0 0.2
298 K pH 1) 1) 1) 5.0~8.0
(TOC),
, g/L50 50 200 no limit
, , g/L 1 5 10 50
, , g/L 1 5 10 50
, , g/L 3 3 500 no limit
- ,
.
A B B
Maximum heterotrophic
10/1000 L 10/100 mL 100/10 mL
(endotoxin),
EU/mL 2)0.03 0.25
(Type ) (Type )
(-25).
-25.
1) , , pH .
pH .
2) EU = endotoxin units
.
. . ,
, .
,
(feedwater) .
.
.
.
-
. QA/QC 49
(pyrogen)/
(endotoxin)
G~E P G E E E
E E P P P P
G P G E E E
P P G~E P P P
P P P E E P
P P G E E E
(UV oxidation)P P G~E P G P
3.1.2
.
. (reverse osmosis), ,
(deionization), (ultrafiltration)/
. -26
.
-26.
1) E= Excellent ( ) G=Good ( )
P= poor ( )
( .). ,
, .
.
(adsorption) .
,
.
Ultrafilter , 185 nm
.
-
50 QA/QC
3.1.2.1 (distillation)
(borosilicate glass), ,
- (laboratory-grade) .
. 15 ,
. soda lime
(Ascarite) .
. , , (bicarbonate)
.
(demineralization) . 25 C 1.0
Mcm , , 10 Mcm.
3.1.2.2
(suspended impurity)
(semipermeable membrane)
(force) . .
(reverse osmosis membrane module)
.
rejection data . spiral-wound hollow fiber configuration
(fouling) . configuration
,
, , .
flushing .
3.1.2.3
(mixed-bed) (deionized
water) . (mixed-bed) (strong anion)
(strong cation) .
, (ion-exchange bed)
(recirculate) . 25 C 10 Mcm .
-
. QA/QC 51
bed
. ,
. bed (bed-sizing)
. bed
(maximum process flow rate) .
optimal face velocity residence time
.
,
. (pre-filtration), ,
.
3.1.2.4 (adsorption)
.
(granular activated carbon) .
, . ,
.
.
face velocity residence time .
. ,
.
polishing . polishing ,
, .
25 C 10 Mcm , 0.2 m
pore membrane (mixed-bed
deionizer) polishing .
, . .
.
g/L
. TOC, SiO2
.
-
52 QA/QC
. 25 C
1 Mcm .
pH .
. .
3.2
-27 , .
3.3
3.3.1
.
-28 -29 .
.
-30 2 .
SOP .
, -30 (1)
. 3 .
. ,
, -30
(2) . 3
.
-
. QA/QC 53
-27. ,
(HCl, H2SO4, HNO3,
)
VOC
,
,
,
, ,
,
.
.
.
,
,
(100~10 ppm)
(
)
pH,
(, , )
3.3.2 (stock solution)
3.3.2.1
, , , , ( ),
, , , (-31).
-
54 QA/QC
-28
, :
:
:
, , :
lot number :
:
:
g mL
: :
: :
-
. QA/QC 55
-29. ( )
MDL (method detection limit)
: :
ID
g
mL
mL
mL
mL
%
wet
mg/kg
dry
mg/kg
QC
QC
QC (ID) :
ID mL :
:
mL : :
RPD :
(% R) :
% R (% R) :
: :
-
56 QA/QC
-30.
, :
:
:
:
:
:
: :
(w1, g)
(w2, g)
(w2 - w1,
g)
(mL)
(N)
(N): N = g 1000 / mL Eqw (1)
(N) : (3 )
:
: : :
mL
mL
(N)
: N = mL N / mL (2)
(N) : (3 )
: :
: :
-
. QA/QC 57
:
:
source :
:
:
:
:
:
:
:
:
:
: :
-31.
3.3.2.2
. , ,
, , , , ,
. , ,
(-32).
-
58 QA/QC
-32.
:
:
:
:
:
source :
:
:
:
:
:
:
: :
: :
3.3.2.3 (CCS, continuing calibration standard)
, ,
, , (
-33).
-
. QA/QC 59
:
:
, :
, mL :
:
:
:
:
: :
: :
-33.
3.3.3
.
. 5 % .
3.3.4
. 100 % 10 %
.
-
60 QA/QC
3.3.5 (LCS, laboratory control
standard)
,
.
.
.
. 100 % 15 %.
3.3.6
.
. -34
.
4.0
.
,
,
.
, ,
.
.
, , ,
, , ,
, , , , ,
, , .
-
. QA/QC 61
-34.
pHpH 4.00, 7.00, 10.00
0.01 M KCl glass stop bottle 6
400 NTU 1
500 mg/L 3
1 000 mg/L 1 .
100 mg/L 3
NH3-N 1 000 mg/L 3
NO3-N 1 000 mg/L
6
NO2-N 250 mg/L
3
PO4-
P 50 mg/L 3
SiO2 10 mg/L
1
SO42- 100 mg/L 6
1 000 mg/L
10~100 mg/L , 0.5 % HNO3
1
COD 500 mg/L
TOC
1 000 mg/L
10~100 mg/L
, 3
3
1 000 mg/L 3
1000 mg/L
10 mg/L 6
-
62 QA/QC
, ,
.
, , ,
,
.
.
.
1) .
2) (, )
.
3)
.
4) ,
.
5) .
6)
(, ).
.
(standard)
(blank)
(spiked sample)
(certified reference material)
.
.
-
. QA/QC 63
.
.
.
,
. , .
4.1
1) , (calibration)
, ,
.
2) (calibration curve)
.
.
3) (CCV, calibration curve verification)
. 1 (batch) 1 .
4) (control chart)
-
64 QA/QC
.
.
5) (IDL, instrument detection limit)
S/N 2-5 ,
3 .
.
6) (internal standard)
, , .
.
.
, .
,
,
.
7) (surrogate)
.
.
8) (surrogate spike)
, ,
. .
-
. QA/QC 65
GC, GC/MS .
, ,
(purging) .
, .
9) (aliquots)
.
10) (matrix)
. , ,
.
11) (matrix spike)
.
. matrix spike sample
matrix ,
.
12) (blank)
. (reagent blank),
(laboratory blank), (equipment rinsate),
(method blank), (field blank), (trip blank)
.
(method blank)
-
66 QA/QC
matrix
,
. method blank
. method blank
, ,
. reagent blank ( )
laboratory blank ( ) .
(field blank)
(field blank)
(, , ) .
(
, ; analyte-free water)
. .
,
.
.
, 5
. 1 .
,
,
.
(preparation blank) (method blank)
.
(equipment blank)
.
.
-
. QA/QC 67
.
.
20 1
.
.
.
.
(rinsate blank)
(rinsate
blank) .
(trip blank)
( ,
, ) .
Trip VOC .
trip VOC ,
VOC .
VOC
, VOC .
,
. .
13) (replicate sample)
, .
,
-
68 QA/QC
. 2 , (duplicate sample)
. . ( )
.
14) (duplicate sample)
.
. (field
duplicate sample), (matrix duplicate sample),
(spike duplicate sample), (quality control duplicate sample)
.
(field duplicate sample)
2
.
( )
.
10 %
.
.
(blind field duplicate)
.
.
15) (dispersion)
.
.
-
. QA/QC 69
16) (split sample)
.
.
. (field split) ,
(lab split) .
,
.
blind .
.
17) (batch)
. (QC) 20
20 .
20
(batch) .
18) (Reagent water spike)
(analyte-free water)
.
. 5 %
. ,
5 .
19) (MDL, method detection limit)
, 0
-
70 QA/QC
, 99 % , matrix type
.
20) (LCS, laboratory control sample)
,
.
.
21) (LFS, laboratory fortified samples)
,
, , ,
.
22) (error)
.
(personal error) :
(verification tolerance, acceptance tolerance) :
( )
(system error) :
. .
(random error) :
.
(instrument error) :
.
(analytical error) : .
23) (completion)
(batch)
-
. QA/QC 71
100 %
.
%= 100
24) (chain of custody)
, , , , .
.
25) (QC, quality control)
.
, , , , , ,
, .
26) (QCS, quality control sample)
,
.
10
, .
27) QC
QC ( )
.
. .
28) (QA, quality assurance)
.
-
72 QA/QC
.
29) (precision)
, .
duplicate/replicate . /
matrix spike .
(RSD, relative standard deviation)
(CV, coefficient of variation) .
30) (cleanups)
GC (florisil, , )
.
.
31) (organic free reagent)
(reagent water)
. free-organic reagent
water , , ,
.
15 1
90 C .
32) (accuracy)
(random error) (systemic error) .
-
. QA/QC 73
. matrix % (% R)
.
% R = measured valuetrue value
100=spiked value-unspiked value
spiked value100
33) (true value)
. ,
. .
.
34) (spiked sample matrix sample)
. ( ) .
.
. , ,
.
10 () 100 () .
3~5
. ,
, , ,
.
.
(%) .
.
C1V1 = C2V2
, C1 = ,
-
74 QA/QC
V1 =
C2 =
V2 =
35) (field spiked sample)
.
(, FSp ) .
(, FSp1, FSp2 ) .
,
.
36) (IDC, initial demonstration of capability, IPR, initial
precision & recovery)
, ,
, ,
.
37) (MLQ, minimum level of quantitation)
710 10
.
(calibration points) (mass spectra)
. (MQL, minimum
quantitation limit), (minimum level), (limit of
quantitation)
.
38) (column QC sample)
-
. QA/QC 75
. .
.
39) (Bias)
, ,
(systematic error) (0)
, .
40) (composite sample)
.
) 6 m3/s 6 L , 4 m
3/s 4 L
(10 L) .
41) (standard operating procedures, SOPs)
(SOP, standard operating
procedure)
.
(
).
.
. ( )
.
. (matrix interference)
. ( )
-
76 QA/QC
. ( , )
. ( )
.
.
.
.
. (outlier)
.
.
. , ,
.
.
,
.
.
1 BOD5 .
4.2 QA/QC
QA/QC , , -35 .
-
. QA/QC 77
-35. QA/QC
X 1n
n
i=1Xi
.
n
S 1n-1
[ n
i=1(Xi-X)
2]
% Dx 1- x 2x 1
100 2
RSD
100
RPD [
(X 1-X 2)
(X 1+X 2)/2]100
% R(Xmeas.Xtrue )100
value of spiked s.-value of unspiked s.value of added spike
100
UCL % R + 3S
+3
LCL % R - 3S
-3
UWL % R + 2S
+2
LWL % R - 2S
-2
R R =max-min
0
-
78 QA/QC
4.3 (quality control)
.
-36 .
-36.
(calibration)
(calibration
verification)
(blank)
(standard)
(CRM)
(MDL)
(accuracy)
(precision)
(reagent spike)
(replicate,
duplicate analysis)
(, , )
,
(, )
(surrogate
spike)
(control chart)
(QCS)
(LCS)
-
. QA/QC 79
(Response) .
(IDC, initial demonstration of capacity)
.
A 0.10 mg/L ,
. , 0.20 mg/L
0.15 mg/L .
. , .
, ,
.
4.3.1
4.3.1.1 (calibration curve)
,
.
QA/QC .
, (batch)
2 , 3 .
.
. 1
7
.
3 .
.
-
80 QA/QC
.
-37 EPA 10 GC.MS
.
-37. GC/MS 1
(RSD)
0 2
2 10
10 25
25
1
3
5
7
1 : Tenth Annual Analytical Symposium, USEPA, 1987
pH,
. ,
.
5
.
4.3.1.2 (calibration verification)
.
, 4.3.1.1
.
.
(, blank, 1 standard).
,
.
(, )
.
.
-
. QA/QC 81
.
, ,
12 , 10 , 1 (batch)
,
.
4.3.1.3 (CCV, calibration curve verification)
. , .
10 20 1 (batch) 8
.
4.3.2 (IDC, initial demonstration of
capability)
, ,
(IDC)
. , ,
.
, .
.
, ,
.
, , .
( )
, / (QA/QC) ,
, (
, )
-
82 QA/QC
.
/
/
. , ,
. ,
, .
4.3.2.1
(EPN) GC/MS ( )
.
1) .
(SPE, solid phase extractor) - (liquid-liquid extraction)
.
2) ,
.
500 mL
5 -
. , ,
K-D ,
.
3) GC/MS
.
GC/MS ,
, , , , ,
, .
, ,
, ,
.
-
. QA/QC 83
4) .
5 GC/MS .
, , 5 .
5) .
5 ,
, GC/MS ,
QA/QC .
.
6) , .
.
.
7) .
4.3.2.2 (MDL, method detection limit)
(MDL)
99 % 0
. , ,
. (
) .
(SOPs)
. / (QA/QC)
SOPs
( , , )
.
3 .
-
84 QA/QC
,
.
, (
) (MDL)
.
6 1
.
.
-38. (T-N)
2)
(mg/L) (absorbance) (mg/L)
0 0.000
1.0 0.084
2.0 0.159
3.0 0.242
4.0 0.330
y = 0.0818x-0.0006, r2 = 0.9993
(0.2 mg/L)
1 0.012 0.154
2 0.014 0.178
3 0.013 0.166
4 0.010 0.130
5 0.009 0.117
6 0.014 0.178
7 0.013 0.166
0.024
(3.707)0.089
(10) 0.239
2) 0.2 mg/L
-
. QA/QC 85
4.3.2.3
1984 (Clean Water Act)
.
(MDL) 7
. n-1 t
(7 98 % 6
3.143 .). (EPA)
7
(batch)
. EPA
(APHA, american public health association),
(AWWA, american water works association),
(WEF, water environment federation) ,
(Standard Method for the Examination of Water and
Wastewater),
(ASTM, american society for testing and materials) ,
.
4.3.2.4
1) .
/ 2.55
3
(,
)
2) 35 7
matrix spike sample .3)
3) 7 .
3) ASTM Type water NIST
SRM (San Joaquin Soil, Montana Soil ) .
-
86 QA/QC
X= 1n
n
i=1Xi
S=1n-1
[ n
i=1(Xi-X) 2]
Xi = x i , X = n x
4) .
MDL= 3.707 S
5) 2) spike level MDL 5
spike .
10 (t
) . (99.7 %, 99 %, 98 %, 95 % )
.4)
4.3.2.5 (MLQ, minimum level of quantitation MQL)
10
.
(ML, minimum level) 1979 EPA method .
(calibration points)
(mass spectra) . 10 EPA
(calibration point)
.
. EPA
. -
4) 3.707 7 99 % n-1, 6 t
98 % t 3.143 .
-
. QA/QC 87
.
1994
,
10
. 7
3.14 , 3.18
.
[] 3.18 10 3.14 7
t-
.
Currie's (ACS, american chemical society's) (LOQ,
limit of quantitation) 10 10
.
4.3.2.6
.
50 %
. 2 ,
.
( ) 23
.
.
,
. QA/QC
,
.
-
88 QA/QC
4.3.3
, ,
. ,
. ,
,
,
.
26 .
4.3.3.1 (blank)
(batch)
.
(MDL) .
(reagent blank sample), ( SEA
SAND
- Fisher Scientific )
, (method blank), (field blank
sample), (trip blank sample) . ,
,
-
. QA/QC 89
, , ,
.
.
, .
. ,
, .
, .
.
4.3.3.2 (LFS, laboratory fortified sample)
1) (matrix spike)
10 % .
. ( )
.
, .
.5)
.
,
,
.
5) , 10 .
-
90 QA/QC
-39. 1
, ( 5
mg/L)
ID
(mg/L)RSD (%)
reagent (lab) blank 0 0
trip blank 0 0
field blank 0 0
LCS-1 (5mg/L) 21100 4.62
QCS-1 (5mg/L) 24325 5.73
sample 1 2310 0.51
sample 1 ( ) 25028 6.36
sample 1 (
)21750 5.91
1.83
= 112.4 %
2) (surrogate standard)
,
. .
, ,
, . ,
, .
, . 4.3.2
.
3) (IS, internal standard)
, ,
(injection losses,
injection contamination), ,
-
. QA/QC 91
,
.
, ,
.
4.3.2 .
4) (LCS, laboratory control sample)
, ,
.
, .
310
.
,
. .
4.3.3.3 / (replicate sample/split sample)
.
.
. ,
1 (batch) 10 %
1 (batch) 2
.
GC/MS
Naphthalene-d8, Chrysene-d12 1
, 2 6) .
-
92 QA/QC
-40 GC/MS
IDpeak
Internal
Standard
IS factor
(mean IS/IS)
(ug/L)
(%)
RSD
(%)
/
2693 1.000 4332 100.0
reagent (lab) blank 0 2763 0.975 0 4214 97.3
LCS-1 (5ug/L) 10136 2688 1.002 4.62
QCS-1 (5ug/L) 12120 2590 1.040 5.73 4903 113.2
sample 1 1028 2594 1.038 0.49 4416 101.9
sample 1 duplicate 1113 2848 0.946 0.48 4200 97.0
sample 1 mean 0.48 0.52
sample 2 5187 2755 0.977 2.31 4495 103.8
sample 2 split 4965 2674 1.007 2.27 4660 107.6
sample 2 mean 2.29 0.44
-41. ETC (environmental technology centre)
pH - 20 1 20 1 -
,
, 20 1 20 1 20 1 -
20 1 20 1 20 1 -
,
, 20 1 20 1 20 1 -
, 20 1 20 1 20 1 -
COD, BOD 20 1 20 1 20 1 -
20 1 20 1 20 1 20 1
20 1 20 1 20 1 20 1
VOCs 20 1 - 20 1 20 1
PAHs 20 1 20 1 20 1 -
PCBs 10 1 10 1 10 1 10 1
10 1 10 1 10 1 10 1
6) 5 ug/L 5
2693, 5 ug/L 5
4332 . (mass abundance)
-
. QA/QC 93
4.3.4
. ,
, /
.
4.3.4.1 (LCS, laboratory fortified sample)
, ,
.
(LCS, laboratory control sample)
.
.
.
.
.
.
(NIST) (SRM, standard reference material)
(CRM, certified reference material)
, 1 (batch) 1
.
4.3.4.2 (control chart)
,
.
2030
.
.
-
94 QA/QC
(B )
(A )
(reagent, field, trip)
(surrogate)
(surrogate)
,
,
(internal standard)
(B )
(A )
(reagent, field, trip)
(surrogate)
(surrogate)
,
,
(internal standard)
-27.
/ (QA/QC)
(QC) (m, mean recovery
%) (S) (LFS) .
(UCL, upper control limit)
(LCL, lower control limit) (UWL, upper warning limit)
(LWL, lower warning limit) .
= m3S, = 2S
= m3S, = 2S
-
. QA/QC 95
1 (batch)
( ) 2 , ,
.
.7)
. ,
.
(upperlower warning line),
(upperlower action line)
.
,
x : , : , n :
.
7) , 20
, 5 15 5
.
-
96 QA/QC
ICP/MS (89-Yttrium) control chart
3100
3700
4300
4900
5500la
b b
lank
field
sta
ndard
sam
ple
1
Duplic
ate
sam
ple
1
MSD
sam
ple
3
sam
ple
5
sam
ple
7
sam
ple
9
QC
-1
-28. (Cu) ICP/MS
Yttrium89
1 (batch) 8)
(control chart)
0.90
0.95
1.00
1.05
1.10
01 30 02 01 02 03 02 05 02 07 02 09 02 11 02 13
-29. BOD5 (GGA) ( 20
)
4.3.4.3 (PE, performance evaluation)/ (PT, proficience
test)
8) = 4300, (+2s) : 4900, (-2s) : 3700,
(mass abundance)
-
. QA/QC 97
,
.
. 2 .
4.3.5 (BTEX, )
.
, , .
.
(peak ratio) .
(, ,
),
.
(59
.).
( ) .
( 59
.) 59 (
) 59 .
(, 20% )
. Aroclos
PCBs, PAHs
.
5.0
5.1
-
98 QA/QC
(raw data) .
,
. ,
. ,
,
.
.
5.2
.
.
5.2.1 pH
pH .
pH .
25 C.
5.2.2
. 25 C
2 % , 25 C 2
% .
.
um/cm at 25 C = /[1+0.019(t-25)]
25 C .
-
. QA/QC 99
5.2.3 , , (ash)
, , mg/L (%) . (TS,
total solid), (SS, suspended solid) (TDS,
total dissolved solid) mg/L,
.
1)
(mg/L) = [(A-B) / (mL)] 106
, A = TS : 105 C (g)
TDS : 180 C (g)
SS : 105 C (g)
B = (g)
(%) = (A-B) 100 / (mL)
% mg/L 10 000 .
(%) = (mg/L) / 10 000
2)
105 C
.
.
(%) = [( (g) - (g)) 100] / (g)
3)
1 000 C (muffle furnace)
.
-
100 QA/QC
.
(%) = (g) 100 / (g)
4) (composition)
105 C .
1 000 C .
. .
.
, , 100 %. 100
% , .
5.2.4
.
mg/L = (mL N Eqw 1 000)/ (mL)
, mL =
N =
Eqw =
.
% = (mL N mEqw 1 000)/ (mL)
mL =
N =
mEqw = (Eqw/1 000)
,
.
-
. QA/QC 101
5.2.5
, mg/kg g/kg
. .
wet base (mg/kg) = C V / M
C = (mg/L)
V = (mL)
M = (g)
dry base (mg/kg) = wet base (mg/kg) /
, 5 g (digest).
100 mL. 0.56 mg/L
, 100 mL 0.056 mg. 5 g 0.056 mg , 1
kg 11.2 mg .
wet base mg/kg = 0.56 100/5 = 11.2 mg/kg
'wet base'
. ,
.
. 12 % ,
88 %.
dry base (mg/kg) = 11.2 /0.88 = 12.72 mg/kg
5.2.6 (TDS, Total Dissolved Solid)
TDS .
TDS = 0.6 () + Na + K + Ca + Mg + Cl + SO4 + SiO3 + (NO3-N) +
F
-
102 QA/QC
mg/L. TDS TDS
. .
. 20
% , .
.
1.0 TDS/ TDS 1.2
TDS (mg/L ) (m/cm) 0.55 0.7
. , TDS
.
5.2.7 -
.
.
% = [( - )/( + )] 100
(-42)
-42.
mEq/L
0~3.0 0.2 mEq/L
3.0~10.0 2 %
20.0~800 (2~5) %
-43 mg/L me/L
.
. mg/L me/L , mg/L
.
-
. QA/QC 103
-43. mg/L me/L
mg/L x
=me/L
me/L x
=mg/L
mg/L x
=me/L
me/L x
=mg/L
Al3+ 0.1112 8.994 BO2- 0.02336 42.81
B3+
0.2775 3.6.3 Br-
0.01257 79.90
Ba2+
0.01456 68.67 Cl-
0.02821 35.45
Ca2+ 0.04990 20.04 CO32- 0.03333 30.00
Cr3+
0.05770 17.33 CrO32-
0.01724 58.00
Cu2+
0.03147 31.77 F-
0.05264 19.0
Fe2+ 0.03581 27.92 HCO3- 0.01639 61.02
Fe3+
0.05372 18.62 H2PO4-
0.02084 47.99
H+
0.9922 1.008 HPO43+
0.01031 69.99
K+ 0.02558 39.10 HS- 0.03024 33.07
Li+
0.1441 6.941 HSO3-
0.01234 81.07
Mg2+
0.08229 12.15 HSO4-
0.01030 97.07
Mn2+ 0.03640 27.47 I- 0.00788 126.9
Mn4+
0.07281 13.73 NO2-
0.02174 46.01
Na+
0.04350 22.29 NO3-
0.01613 62.0
NH4+ 0.05544 18.04 OH- 0.05880 17.01
Pb2+
0.009653 103.6 PO43-
0.03159 31.66
Sr2+
0.02283 43.81 S2-
0.06238 16.03
Zn2+ 0.03059 32.69 SO42- 0.02082 48.03
, 1 22.989 7.
1/22.989 7 = 0.043 49. 2 , 96.063 6
2/96.063 6 = 0.028 2.
me/L mg/L
. Na , 22.989 7/1 = 22.989 7 , 96.063
6/2 = 48.03.
Na 20mg/L me/L , (20 0.043 49) = 0.869 8 me/L,
0.869 8 me/L Na (0.869 8 23 ) = 20 mg/L .
5.3
(boundary form)
, .
-
104 QA/QC
5.3.1
, , (field notebook), (preservative
preparation log) .
(loose-leaf) .
.
. ,
.
, . ,
. ,
. , , ,
.
5.3.2 (work sheet)
. (ID , , ,
), , (MDL, method
detection limit), , QC ,
.
. (pH, , ,
) . pH
-22 , -44~46
, -45~51
.
-
. QA/QC 105
: :
: :
:
C
m/cm
m/cm
25 C
0.01 M KCl
QC
QC :
1) (RPD) : :
2) (% R) : :
1) RPD (relative percent deviation) = (A-B) /(A+B) 200 A B =
2) R (% recovery) = ( 100)/
25 C 0.01 M KCl 1413 m/cm .
: 25 C 2 % , 25 C
, 2 % .
-44.
-
106 QA/QC
: :
: : :
: : :
mg/L mL mL
DO
mg/L
(PRD) : :
RPD (relative percent deviation) = (A-B) /(A+B) 200 A B =
=
mg/L DO = ( mL N 8,000) / mL
N = , 8000 = 1,000
-45.
-
. QA/QC 107
: ( )
(Na2S2O3) :
: :
: :
Cl2
mg/L
mL
mL
Cl2
mg/L
(RPD) : :
RPD (relative percent deviation) = (A-B) /(A+B) 200 A B =
mg/L Cl2 = [(A+/-B) N 35,450] / mL
A = mL
b = mL
N = Na2S2O3 , 35,450 = 1,000
-46.
-
108 QA/QC
-47. ( )
: : :
MDL (method detection limit) :
:
: :
ID
mL
mL
mg/L
QC
QC
QC : (ID) :
ID : mL :
:
mL : :
RPD :
(% R) :
% R :
: :
-
. QA/QC 109
MDL (method detection limit)
: :
:
: :
ID
mL mg/L
1
2
3
4
CCS
CCV
QC
(CCS) % :
(CVS) :
CVS % : ID :
ID : mL :
: :
RPD :
(% R) :
% R (% R) :
: :
-48. ( )
-
110 QA/QC
MDL (method detection limit)
: :
:
: :
ID
g
mL
mL
mg/L
rep wet
mg/kg
rep dry
mg/kg
1
2
3
4
CCS
CVS
QC
(CCS) % :
(CVS) :
CVS % : ID :
ID : mL :
: :
RPD :
(% R) :
% R (% R) :
: :
-49. ( )
-
. QA/QC 111
: :
: : MDL :
: single junction : double junction :
:
: : :
ID
mL
mg/L
mg/L
1ppm
10ppm
QC
CCS
CCS
QC
QC
% CCS :
QC : QC % :
ID : (RPD) :
ID : mL :
: mL :
: (% R) :
: :
-50. ( )
-
112 QA/QC
: :
: : MDL :
: single junction : double junction :
:
: : :
ID
g
mL
mL
mg/L
mg/L %
rep wet
mg/kg
rep dry
mg/kg
1ppm
10ppm
QC
CCS
CCS
QC
QC
% CCS :
QC : QC % :
ID : (RPD) :
ID : mL :
: mL :
: (% R) :
: :
-51. ()
-
. QA/QC 113
5.3.3
, , , ,
.
. (strip chart),
.
.
, ,
QC MDL
,
(, , ,
)
QC
, ,
5.4
5.4.1 QC
QC , ,
. , ,
, . QC ,
. QC ,
, . QC ,
-
114 QA/QC
, QC , QC , ,
, , , , , ,
, QC .
5.4.2
5.4.2.1
, , ,
, , .
(MDL) .
1)
. ,
.
. ,
. .
2)
.
3)
, ,
. .
.
4)
(reagent grade water) .
, ,
. .
5.4.2.2
-
. QA/QC 115
0.9998 .
5 %,
10 % . QC
5 %, 10 %.
1)
, , ,
.
.
2)
.
.
3) QC (CVS)
, CVS
.
4) ,
5) ,
,
. SOP QA/QC
. .
6)
.
.
7)
, .
-
116 QA/QC
5.4.2.3 9)
, .
, , .
,
.
1)
, .
.
2)
. .
3)
,
. ,
.
4)
.
5.4.2.4
(spike
accuracy limit) .
1)
.
. ,
9) , .
.
-
. QA/QC 117
.
2)
, .
3)
. (micro-pipet)
.
5.4.2.5
.
, .
.
.
.
QC 5 % .
QC .
, .
1)
:
:
: , , ,
. ,
. .
:
. .
2)
. ,
.
-
118 QA/QC
3)
, .
4)
.
5)
. ,
.
5.4.3
,
. , .
, .
-
- .
.
-
.
- .
5.4.4
.
. .
5.4.5
.
10.6 mg/L , 10 0.6 0.5 0.7 . 10.6
mg/L 3 .
-
. QA/QC 119
.
0 .
0 . 0.002 5
0.00 ,
2 .
0 0 . , 1.008 4
.
, ,
.
, 4.56 1.4 = 6.38 6.4
( 4.56 1.4 1.4 2).
12.11 + 18.0 + 1.013 = 31.123 31.1
.
,
.
5.5
.
- , , ,
, , QC
- , (MDL), (
, , (performance check), ), (, ),
(, , , ),
QA/QC - , , QC ,
, ,
,
- , , , ,
,
-
120 QA/QC
5.6
(SI, The
International System of Units) ,
.
1964
.
.
() () , () .
, .
) : m (), t ()
: kg, s, K, Pa, kHz
,
. ,
.
) Kg (), kg ()
5 sec. (), 5 sec (), 5 secs (), 5 s ()
600 kPag (), 600 kPa (gauge) ()
() ( 1
) . , (), (), ()
.
-
. QA/QC 121
) 35mm (), 35 mm ()
32C () 320C (), 32 C () C SI
25 23 (), 252327 ()
() .
(
1) .
.
) c = 299 792 458 m/s ( )
1 eV = 1.602 177 33 (49) 10-19
J ( )
t = 28.4 0.1 C (), t = 28.4 C 0.2 C = (28.4 0.2) C ()
(
1) . ,
(meter milli )
.
) Nm N m
mN (millinewton) Nm mN
,
,
.
) ms
, m/s, ms- 1 () J / kgK (), J / (kgK) ()
,
.
.
-
122 QA/QC
) mkg/s2
mol (), (mkg)/(s2
mol) (), mkgs-2
mol-1
()
joules/kg (), joules/kilogram (), Jkg-1
(), joules per kilogram ()
210-6
(), 2 10-6
()
0.1 1 000
. , .
- , , , .
-
0.1 1 000
.
- .
) 12 300 mm () 12.3 m () 0.00123 m () 1.23 nm ()
(hm2), (cm
3)
0.1 1 000 mm
. ,
, kg .
) 1 mm (), 1 nm () kJ/g (), MJ/kg ()
,
.
) 1 cm3 = (10
-2 m)
3 = 10
-6 m
3
M/m3 () 10
6/m
3 ()
ppm, ppb 10-6
, 10-9
. .
) 2 ppm (), 2 10-6
(). 2 ppm 2 mg/L
-
. QA/QC 123
mg/l (), mg/ (), mg/L ()
g/ml (), g/m (), g/mL ()
. % (m/m), % (V/V)
.
) 0.67, 67 %
( g/g, mL/m3
)
.
.
) 3 Newtons (), 3 newtons ()
(hyphen)
. megohm", "kilohm", "hectare"
.
.
) kilo-meter (), kilometer ()
( 1)
.
) (mass fraction) (), (mass fraction) ()
(2) 1 .
) (), m2
()
-
. QA/QC
-
. QA/QC 127
. QA/QC
1.0
. 6 .
(chain-of-custody)
(QA, quality assurance) (QC, quality control)
1.1
1.1.1
. .
1.1.2
(reconnaissance survey),
(intensive survey), (fixed station monitoring),
(network monitoring), (ground water monitoring)
(special survey) .
.
( ,
. )
-
128 QA/QC
(, , , , , )
(, )
(, )
(, )
( )
1)
(grab
sample), (composite sample), (continuous sample)
. .
.
,
.
.
. 15 .
.
.
. ( )
( )
.
(auto-sampler)
.
, VOC (volatile organic compound), , TRPH (total recoverable
petroleum hydrocarbon), ,
-
. QA/QC 129
.
1.1.3
1)
,
. ,
.
. , ,
.
3 . VOC, , , TRPH,
.
-1.
2)
.
.
,
.
-
130 QA/QC
. -2.
1.1.4
(-1).
, , , , ,
, .
, , , , ,
, , , .
, , , ,
, , .
.
-1.
, , , , ,
, , , , ,
, ,
, , , ,
, ,
-
. QA/QC 131
1.2
1.2.1
.
.
1)
2)
3)
4)
5)
6)
7)
8)
9)
1.2.2
.
1) .
2) ,
. .
3) , (bowl) (spatula)
, , ,
.
VOC, TRPH
, , (dissolved metal (
(), ()), , .
-
132 QA/QC
,
. VOC, , , TRPH
.
1.2.3
1) ( )
2) ( )
3) ( , , )
4) ( , )
, .
:
: ,
:
:
:
: UV, (micro~wave),
:
: ,
.
,
1.2.4
(-2).
-
. QA/QC 133
-2.
UV -
-
- (coverall)
( ) -
, PVC
(
)
-
1)
, , (SPF, sun
protection factor : 15) .
.
(coverall) , (
-3).
.
.
2)
.
, .
,
, .
-
134 QA/QC
3)
,
.
4)
,
(flip-down) (-4).
5)
, , ( ,
) .
.
6)
, .
.
.
-3. (coverall) -4. (flip-down)
-
. QA/QC 135
1.3
,
,
. ,
5 % ALCONOX
LIQUINOX
.
ALCONOX , ,
. ALCONOX
LIQUINOX .
LIQUINOX , ,
, , .
(isopropanol) .
1.3.1
, .
, 10~15 % (HNO3) .
, 10~15 % (HCl) .
) .
, .
.
1.3.2
.
,
, .
-
136 QA/QC
.
1.3.3
,
. , .
1.3.4
, .
,
(sonicator) .
, 10~15 %
.
, (methanol)
, .
.
1.4
,
.
, (screw cap)
. (teflon)
.
(septum) (borosilicate)
(vial) .
-3 .
-
. QA/QC 137
-3.
, mL
200 AOX1)
COD, (trihalomethane)
250
500 , DO (dissolved oxygen)
1000 , (lignin) (tannin),
BOD2), , , , PAH, , PCB
100 , , ,
250
, , , , , ,
(6+), , , , , , , ,
, , , , , , ,
, , , , , ,
, , pH, , , , ,
, Kjeldahl nitrogen
1000 BOD, , chlorophyll, ,
375 , , TOC3),
1) AOX (absorbable organic halogen)
2) BOD .
3) TOC (total organic carbon)
1.4.1
.
1)
, LIQUINOX
. ,
. 3~5
.
-
138 QA/QC
2) , BOD, COD
LIQUINOX
. ,
. 50 % , 3~5
.
3)
, ACATIONOX
. ,
. 50 % , 50 %
. 3~5
.
4) (extractable organics)
1 L (narrow mouth glass bottle)
. ALCONOX
,
.
.
.
. 5
10 mL 10 .
5 ,
.
5) VOC
40 mL ,
. ALCONOX ,
.
.
.
, 60 105 C
, , .
-
. QA/QC 139
mL
50 P, G cool, 4 C 48
100 P, G cool, 4 C 28
100 P, G
pH
-
140 QA/QC
-4. ()
mL
1)
200 P, G
(70
%m/V)
pH
-
. QA/QC 141
-4. ()
mL
phosphorus
ortho-P50 P, G cool, 4 C 48
Hydrolyzable 50 P, Gcool, 4 C
pH9
100 P, G
100 P, G cool, 4 C 28
BOD 100 P, G cool, 4 C 48
COD 50 P, G cool, 4 C 28
1000 G onlycool, 4 C
pH
-
142 QA/QC
-4. ()
mL
nitrosamine 1000
G,
cool, 4 C 0.008
% Na2S2O3
.
40
PCB 1000
G,
cool, 4 C
.
40
nitroaromatic
isophorone1000
G,
cool, 4 C
.
40
polynuclear aromatic
hydrocarbon1000
G,
cool, 4 C
.
40
1000
G,
cool, 4 C 0.008
% Na2S2O3
.
40
1000
G,
cool, 4 C
.
40
1000
G,
cool, 4 C
pH 5~9
.
40
, ,
30
G
cool, 4 C
30
G
cool, 4 C
500 p cool, 4 C 6
fish sample 30Al
P
chemical waste 100 P, G
1000 P,
