EN713方法确认.docx
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EN713方法确认
Linearity(线性)(ForICP-OES)(AN-0160)
1Scope(目的)
ThepurposeofthisvalidationistoestimatethelinearityofSolubleelementsforEN71-3(ISO8124/ASTMF963-2003)withICP-OES.
本实验目的是来确认用ICP测定可迁移元素的线性。
2Procedure(过程)
2.1Prepareaseriesofstandardsolutionsasbelow:
0.1mg/L,0.2mg/L,0.4mg/L,1.0mg/L,2.0mg/LforAs,Hg,Sb,Se
0.5mg/L,1.0mg/L,2.0mg/L,5.0mg/L,10.0mg/LforBa,Pb,Cd,Cr
配制一系列的标准溶液如下:
砷,汞,锑,硒为0.1mg/L,0.2mg/L,0.4mg/L,1.0mg/L,2.0mg/L
钡,铅,铬,镉为0.5mg/L,1.0mg/L,2.0mg/L,5.0mg/L,10.0mg/L
2.2AnalyzethesolutionsassampleswithICP-OES.
用ICP来分析上述溶液。
2.3Calculatethecorrelationcoefficient(R)withminimumrequirementofR>0.995.
检验其标准曲线的相关系数(R)达到最低要求:
R>0.995。
3Results(结果)
ThelinearityofAs,Hg,Sb,Se,Ba,Pb,Cd,Crin0.07NHCL
As,Hg,Sb,Se,Ba,Pb,Cd,Cr在0.07NHCL中的线性范围
ConcentrationofAsstandardworkingsolutions(ppm)
Intensity(c/s)
ConcentrationofBastandardworkingsolutions(ppm)
Intensity(c/s)
0.1
163.832
0.5
62173
0.2
304.492
1
120378
0.4
611.61
2
243331
1
1470.58
5
583033
2
2960.14
10
1155306
ConcentrationofCdstandardworkingsolutions(ppm)
Intensity(c/s)
ConcentrationofCrstandardworkingsolutions(ppm)
Intensity(c/s)
0.5
38905.7
0.5
35531.2
1
75553.9
1
70354.2
2
152807
2
141176
5
374995
5
347859
10
723010
10
650584
ConcentrationofPbstandardworkingsolutions(ppm)
Intensity(c/s)
ConcentrationofHgstandardworkingsolutions(ppm)
Intensity(c/s)
0.5
2264.64
0.1
454.521
1
4415.19
0.2
887.705
2
8858.63
0.4
1738.74
5
21858.9
1
4421.65
10
43296.3
2
8757.17
ConcentrationofSbstandardworkingsolutions(ppm)
Intensity(c/s)
ConcentrationofSestandardworkingsolutions(ppm)
Intensity(c/s)
0.1
255.79
0.1
154.019
0.2
462.193
0.2
281.501
0.4
879.191
0.4
564.169
1
2138.65
1
1407.66
2
4254.23
2
2868.31
4Conclusion(结论).
ThecalibrationcurveislinearwithR>0.995forBa,Pb,Cd,Crfrom0.5ppmto5ppm;As,Hg,Sb,Sefrom0.1ppmto2.0ppm.
最终确认在0.07N盐酸中的砷,汞,锑,硒其线性范围0.1ppm到5ppm,钡,铅,铬,镉其线性范围0.05ppm到10ppm均达到R>0.995。
注:
根据CPSD-AN-00003-MTHD要求,现行使用砷,汞,锑,硒0.2ppm,0.4ppm,1.0ppm和钡,铅,铬,镉1.0ppm,2.0ppm,5.0ppm作为校准工作曲线。
Instrumentdetectionlimit(仪器检出限)
1Scope(目的)
Thepurposeofthisvalidationistodeterminetheinstrumentdetectionlimit(IDL)ofsolubleelementsforEN71-3(ISO8124/ASTMF963-2003)withICP-OES.
做仪器检出限的目的是来确认仪器对可迁移元素元素的检出限.
2Procedure(过程)
2.1PlacethereagentblanktotheICP
将试剂空白打入ICP中。
2.2Takeaseriesofsevenreplicatemeasurementsforsolubleelements
重复读7次试剂空白,记录可迁移元素的强度。
2.3AnalyzethesevenreplicatesandcalculatetheIDLas1.645×standarddeviation.
分析这七次重复测量值并计算理论仪器检出限(等于1.645×标准偏差)。
2.4VerifythecalculatedIDLuntilthesignaltonoiseratioreaches3:
1.
校验仪器检出限直到信背比为3:
1。
3Results(结果)
TheIDLofSolubleelementsin0.07NHCl
可溶出元素在0.07N盐酸中的仪器检出限
Trial
Measured
As(mg/L)
Measured
Ba(mg/L)
Measured
Cd(mg/L)
Measured
Cr(mg/L)
Measured
Hg(mg/L)
Measured
Pb(mg/L)
Measured
Sb(mg/L)
Measured
Se(mg/L)
1
-0.0019
0.0000
-0.0001
-0.0004
-0.0013
0.0000
0.0060
0.0052
2
0.0013
0.0000
-0.0002
-0.0003
-0.0013
-0.0019
0.0003
0.0039
3
-0.0022
-0.0001
-0.0001
-0.0002
-0.0002
-0.0007
0.0020
-0.0019
4
-0.0024
-0.0001
-0.0002
-0.0003
-0.0011
-0.0015
0.0044
0.0055
5
-0.0020
0.0000
-0.0002
-0.0002
-0.0008
-0.0008
0.0017
0.0007
6
-0.0021
-0.0002
-0.0001
-0.0002
-0.0005
-0.0010
-0.0001
-0.0078
7
-0.0093
0.0000
-0.0001
-0.0003
-0.0009
-0.0014
0.0035
-0.0058
StandardDerivation
0.0032
0.0001
0.0001
0.0001
0.000414
0.0006
0.0022
0.005358
InstrumentalDetectionLimit(1.645×SD)
0.0053
0.0001
0.0001
0.0001
0.0007
0.0011
0.0036
0.008813
VerifiedIDL
0.0300
0.0008
0.0008
0.0008
0.0100
0.0200
0.0500
0.0400
VerifiedIDLofAs,Hg,Sb,Se,Ba,Pb,Cd,Crin0.07NHCL
As,Hg,Sb,Se,Ba,Pb,Cd,C在0.07NHCL中的校验仪器检出限
Trail
Count
Blank
Pb0.0200mg/L
SignaltoNoiseRatio
1
30.7716
127.262
4.14
2
22.1958
127.262
5.73
3
27.7183
127.262
4.59
4
24.0611
127.262
5.29
5
24.0826
127.262
5.28
6
26.1864
127.262
4.86
7
24.7588
127.262
5.14
VerifiedIDLofPb
0.0200mg/L
Trail
Count
Blank
As0.0300mg/L
SignaltoNoiseRatio
1
13.7240
64.0326
4.67
2
18.2396
64.0326
3.51
3
13.2481
64.0326
4.83
4
12.9732
64.0326
4.94
5
13.5238
64.0326
4.73
6
13.4412
64.0326
4.76
7
15.0662
64.0326
4.25
VerifiedIDLofAs
0.0300mg/L
Trail
Count
Blank
Ba0.0008mg/L
SignaltoNoiseRatio
1
47.6875
152.871
3.21
2
39.5933
152.871
3.86
3
30.4613
152.871
5.02
4
34.1127
152.871
4.48
5
44.3013
152.871
3.45
6
22.7092
152.871
6.73
7
43.0437
152.871
3.55
VerifiedIDLofBa
0.0008mg/L
Trail
Count
Blank
Cd0.0008mg/L
SignaltoNoiseRatio
1
29.3847
91.4211
3.11
2
18.0108
91.4211
5.08
3
22.8931
91.4211
3.99
4
21.7983
91.4211
4.19
5
22.3136
91.4211
4.10
6
29.5695
91.4211
3.09
7
28.7477
91.4211
3.18
VerifiedIDLofCd
0.0008mg/L
Trail
Count
Blank
Cr0.0008mg/L
SignaltoNoiseRatio
1
18.2995
95.7543
5.23
2
21.5417
95.7543
4.45
3
27.6204
95.7543
3.47
4
25.2868
95.7543
3.79
5
28.1169
95.7543
3.41
6
26.5177
95.7543
3.61
7
23.0814
95.7543
4.15
VerifiedIDLofCr
0.0008mg/L
Trail
Count
Blank
Hg0.01mg/L
SignaltoNoiseRatio
1
12.7314
60.2842
4.74
2
12.7385
60.2842
4.73
3
17.6735
60.2842
3.41
4
13.6835
60.2842
4.41
5
14.9606
60.2842
4.03
6
16.2640
60.2842
3.71
7
14.6059
60.2842
4.13
VerifiedIDLofHg
0.01mg/L
Trail
Count
Blank
Sb0.05mg/L
SignaltoNoiseRatio
1
25.3820
77.2350
3.04
2
13.5101
77.2350
5.72
3
16.9009
77.2350
4.57
4
21.9270
77.2350
3.52
5
16.3218
77.2350
4.73
6
12.5923
77.2350
6.13
7
20.1290
77.2350
3.84
VerifiedIDLofSb
0.05mg/L
Trail
Count
Blank
Se0.04mg/L
SignaltoNoiseRatio
1
19.2417
68.8310
3.58
2
17.4998
68.8310
3.93
3
9.46298
68.8310
7.27
4
19.6852
68.8310
3.50
5
13.0459
68.8310
5.28
6
1.40121
68.8310
49.12
7
4.11653
68.8310
16.72
VerifiedIDLofSe
0.04mg/L
(Criteria:
signaltonoiseratio>3:
1)
4Conclusion(结论)
TheclaimedIDLofsolubleelementsforEN71-3(ISO8124/ASTMF963-2003)isasbelow,As0.03mg/L,Ba0.0008mg/L,Cd0.0008mg/L,Cr0.0008mg/L,Hg0.01mg/L,Pb0.02mg/L,Sb0.05mg/L,Se0.04mg/L.
EN71-3(ISO8124/ASTMF963-2003)方法最终确认的仪器检出限为:
As0.03mg/L,Ba0.0008mg/L,Cd0.0008mg/L,Cr0.0008mg/L,Hg0.01mg/L,Pb0.02mg/L,Sb0.05mg/L,Se0.04mg/L.
Methoddetectionlimit(方法检出限)
1Scope(目的)
Thepurposeofthisvalidationistodeterminethemethoddetectionlimit(MDL)ofPb,As,Cr,Cd,Ba,Sb,Se,HgformaterialsusingICP-OES(AN-0160).
确认ICP-OES对铅,砷,铬,镉,钡,锑,硒,汞的方法检出限。
2Procedure(过程)
2.1Forextractable/solubletest,MDLisestimatedfromverifiedIDLx5.Theest.MDLisspikeintoextractionsolutionwithoutgothroughsamplepreparation.(AccordingtoCPSD-AN-TSOPMethodValidationProcedure-Ver3)根据CPSD-AN-TSOPMethodValidationProcedure-Ver3,萃取测试的方法检出限相当于仪器检出限的5倍。
通过在已经过处理的空白样品溶液中加标准溶液制备。
2.2VerifytheMDLuntilthesignaltonoiseisgreaterthanthree.Recoveriesshallbebetween50%and150%,RSDshallbe20%)
校验仪器检出限直到信背比为3:
1;回收率在±50%间;相对标准偏差不大于20%
3Results(结果)
CalculatedMDLofPb,As,Cr,Cd,Ba,Sb,Se,Hgin0.07NHCL
Pb,As,Cr,Cd,Ba,Sb,Se,Hg在0.07N盐酸中的理论方法检出限
Trial
Measured
Pb
Measured
As
Measured
Cd
Measured
Ba
(mg/L)
Recovery(%)
(mg/L)
Recovery(%)
(mg/L)
Recovery(%)
(mg/L)
Recovery(%)
SpikeConcentration
0.1000
--
0.1500
--
0.0040
--
0.0040
--
1
0.107
107
0.151
101
0.0036
90.2
0.0033
82.5
2
0.100
99.6
0.150
99.9
0.0036
90.7
0.0036
90.0
3
0.101
101
0.149
99.4
0.0036
91.2
0.0033
82.5
4
0.101
101
0.150
100
0.0036
90.5
0.0033
82.5
5
0.100
99.8
0.151
101
0.0035
88.4
0.0034
85.0
6
0.103
103
0.149
99.6
0.0036
91.1
0.0035
87.5
7
0.102
102
0.151
101
0.0036
90.2
0.0036
90.0
Mean
0.102
102
0.150
100
0.0036
90.3
0.0034
85.7
StandardDerivation(SD)
0.0027
--
0.0007
--
0.00004
--
0.0001
--
%RSD
2.65
0.47
1.11
2.94
VerifiedMDL
0.1000mg/L
0.1500mg/L
0.0040mg/L
0.0040mg/L
(Criteria:
Recovery=100±50%,RSD≤20%)
Trial
Measured
Cr
Measured
Hg
Measured
Sb
Measured
Se
(mg/L)
Recovery(%)
(mg/L)
Recovery(%)
(mg/L)
Recovery(%)
(mg/L)
Recovery(%)
SpikeConcentration
0.0040
--
0.0500
--
0.2500
--
0.2000
--
1
0.0039
97.1
0.0463
92.6
0.2523
101
0.1980
99
2
0.0040
99.7
0.0483
96.6
0.2573
103
0.2067
103
3
0.0039
98.3
0.0461
92.2
0.2537
101
0.2060
103
4
0.0038
94.1
0.0472
94.4
0.2544
102
0.1990
100
5
0.0036
90.6
0.0472
94.4
0.2561
102
0.2038
102
6
0.0037
93.0
0.0471
94.2
0.2532
101
0.2077
104
7
0.0038
95.9
0.0500
100
0.2572
103
0.2048
102
Mean
0.0038
95.5
0.0475
94.9
0.2549
102
0.2037
102
StandardDerivation(SD)
0.0001
--
0.0013
--
0.0020
--
0.0038
--
%RSD
2.63
2.74
0.78
1.87
VerifiedMDL
0.0040mg/L
0.0500mg/L
0.2500mg/L
0.2000mg/L
(Criteria:
Recovery=100±50%,RSD≤20%)
VerifiedMDLofPb,As,Cr,Cd,Ba,Sb,Se,Hgin0.07NHCL
Pb,As,Cr,Cd,Ba,Sb,Se,Hg在0.07N盐酸中的校验方法检出限
Trail
Count
Blank
Pb0.100mg/L
SignaltoNoiseRatio
1
37.22
572
15.37
2
37.22
533
14.32
3
37.22
539
14.48
VerifiedMDLofPb
0.100ppm
Trail
Count
Blank
As0.0150mg/L
SignaltoNoiseRatio
1
23.80
258
10.84
2
23.80
270
11.34
3
23.80
262
11.01
VerifiedMDLofAs
0.0150ppm
Count
Blank
Cr0.0040mg/L
SignaltoNoiseRatio
1
63.11
381
6.04
2
63.1