Académique Documents
Professionnel Documents
Culture Documents
(representative list - may not be all inclusive for all types of analyses)
(QC sample types in this list are typical of those utilized in AIHA-LAP, LLC laboratories)
additional tabbed sheets for examples
Representative
and Applicable
QC Data
Contributors to Uncertainty
Transportation/Storage/Handling:
NA / (FS)
NA / (LCS, FS)
NA / LCS, FB
Laboratory Subsampling
blending techniques
DUP
DUP
sample size
DUP
sample nonhomogeneity
Sample Preparation:
volumetric glassware
dispensing device
balance
temperature
sample extraction
extractant background
LCS, DUP
LCS, DUP
LCS, DUP
LCS, DUP
LCS, DUP
LCS, DUP, MB
LCS, DUP
LCS, DUP
Analysts:
analyst training level and experience
LCS, DUP
LCS, DUP
LCS, DUP
different analysts
Measuring Instruments:
instrument stability
LCS, DUP
LCS, DUP
LCS
LCS
Calibration Standards/Reference
Materials:
calibration stock material uncertainty
LCS
CERTIFICATE
CERTIFICATE
preparation variances
LCS
LCS
LCS
LCS
Data Manipulation:
sampling media/blank correction
instrument blank correction
accuracy of calculations
LCS, MB
LCS
LCS
NA
Where:
DUP = Duplicate, resulting from sub-sampling of a bulk (NOTE: NOT LCS/LCSD duplicate spiked sampling media)
FB = Field Blank
FS = Field Spike - Not typically conducted unless part of sampling method validation. Should be considered only when labora
is responsible for field sampling.
LCS = Laboratory Control Standard, matrix matched and typically taken through the entire analytical process with each sample
batch
MB = Method or Matrix Blank
NA = Not Applicable
ive list - may not be all inclusive for all types of analyses)
al of those utilized in AIHA-LAP, LLC laboratories)
additional tabbed sheets for examples
See
NOTE: This is not part of analytical uncertainty, but must be considered by labs
providing sampling and when providing guidance regarding sample packaging and
shipping. Usually no impact if recommended shipping conditions and holding times in
referenced methods are maintained. Improper packing materials, bulks shipped w/samples,
etc. may adversely affect data. Field blanks, field spiked samples or duplicate field samples
shipped with samples or included in method validation studies may reflect these contributors.
Field variability (FS/DUP) is only considered when lab is responsible for sampling.
Usually no impact if recommended storage conditions and holding times in reference
methods are maintained. Impact is monitored per sample batch only if LCS samples are
prepared on receipt and stored with field samples. Field spiked samples or stability study
samples included in some method validation studies may also reflect these contributors. Field
variability (FS/DUP) is only considered when lab is responsible for sampling.
Usually no impact if recommended storage conditions and holding times in reference
methods are maintained. Improper storage such as sorbent tubes stored with bulk solvent
samples or near solvent sources may adversely affect data. Impact is monitored only if LCS is
prepared on receipt & stored with field samples. Field blank can be used to assess
contamination from collection, transport, and storage.
NOTE: This primarily applies to bulk/solid samples which requires use of laboratory duplicate
sample data to determine impact on uncertainty. It is not applicable for LCS/LCSD media
spike duplicates.
Sample composition, etc.
Stirring, sieving, grinding, etc.
Large enough to allow adequate subsampling.
NA for Class A; applies for graduated tubes or cylinders, etc.
Pipettes, and other types of dispensers that are not Class A.
Balance error is often insignificant compared to other MU sources.
Hot plate or ashing temperatures.
Applies to LCS or DUP if it goes throughthe entire sample preparation process.
Analyte or interferant is present in acids, solvents, etc.
Room temp during bulk asbestos, gravimetry, etc. processes.
Gravimetry involving hydroscopic media, etc.
Must use inter-analyst instead of intra-analyst repeat data, where applicable.
Must use inter-analyst instead of intra-analyst repeat data, where applicable.
Chromatographic peak ID, interference corrections, etc. Must use inter-analyst instead of
intra-analyst repeat data, where applicable.
Baseline drift, repeatability of averaged readings, lab environmental stability, etc.
Impact of high samples on following sample readings; can be monitored by proper use of
CCBs.
Variation in instrument response and calibration process
Due to matrix, inter-element effects, co-eluting GC peaks, etc.
d unless part of sampling method validation. Should be considered only when laboratory
ix matched and typically taken through the entire analytical process with each sample
Contributors to Uncertainty
Transportation/Storage/Handling
NA
NA
Usually no impact if recommended storage conditions and hold times are maintained. LCS
samples are representative if prepared on receipt & stored with field samples - usually no
impact if recommended storage conditions and holding times are maintained. Field spiked
samples or stability study samples included in some method validation studies may also reflect
these contributors.
NA
Usually no impact if appropriate storage conditions are maintained. Field blank can be used to
assess contamination from collection, transport, and storage
Laboratory Subsampling
sample nonhomogeneity
blending techniques
sample size
NA
NA
NA
Sample Preparation:
volumetric glassware
dispensing device
balance
temperature
sample extraction
extractant background
LCS
LCS
NA
NA
LCS
LCS, MB
LCS
NA
LCS
LCS
LCS results reflect variability due to different analysts, as applicable, on different days
LCS
LCS results reflect variability due to different analysts, as applicable, on different days
LCS
LCS
LCS
interferences
LCS
temperature variance
humidity variance
Analysts:
different analysts
LCS results reflect variability due to different analysts, as applicable, on different days
Measuring Instruments:
instrument stability
LCS
CERTIFICATE
CERTIFICATE
Use if customer sample data corrected for desorption efficiency. Obtain from certificate or
estimate.
preparation variances
LCS
LCS
LCS
LCS
LCS
LCS
LCS
Data Manipulation:
sampling media blank correction
instrument blank correction
Accuracy of calculations
LCS = Laboratory Control Standard, typically taken through the entire analytical process with each sample batch
MB = Method or matrix blank
NA = Not Applicable
Examples of Analytical Measurement Uncertainty for Analysis of Organic Solvents on Charcoal Tubes
mg Toluene on Charcoal Tube using CS2
Desorption per NIOSH 1501
LCS/LCSD = 0.0867 mg toluene spike/tube
LCS mg
LCSD
%Rec
LCS mg
LCS %Rec
LCSD mg
LCSD %Rec
0.0876
101.0
0.0884
102.0
0.0862
106.4
0.0832
96.0
0.0824
95.0
0.0850
98.0
0.0799
98.6
0.0812
93.7
0.0867
100.0
0.0858
99.0
0.0839
103.6
0.0825
95.2
0.0832
0.0789
0.0798
0.0850
0.0824
0.0858
0.0850
0.0876
0.0832
0.0884
0.0867
0.0902
0.0850
0.0876
0.0834
0.0819
0.0797
96.0
91.0
92.0
98.0
95.0
99.0
98.0
101.0
96.0
102.0
100.0
104.0
98.0
101.0
96.2
94.5
91.9
0.0841
0.0789
0.0806
0.0850
0.0867
0.0867
0.0850
0.0858
0.0884
0.0919
0.0893
0.0884
0.0876
0.0902
0.0892
0.0812
0.0784
97.0
91.0
93.0
98.0
100.0
100.0
98.0
99.0
102.0
106.0
103.0
102.0
101.0
104.0
102.9
93.7
90.4
0.0923
0.0847
0.0702
0.0632
0.0933
0.1005
0.0987
0.0826
0.0913
0.0770
0.0910
0.0832
0.0984
0.0872
0.0809
0.0926
0.0979
114.0
104.6
86.7
78.0
115.2
124.1
121.9
102.0
112.7
95.1
112.3
102.7
121.5
107.7
99.9
114.3
120.9
0.0874
0.0819
0.0907
0.0676
0.0870
0.0924
0.0933
0.0919
0.0756
0.0920
0.0960
0.0928
0.0884
0.0861
0.0655
0.0956
0.0889
100.8
94.5
104.6
78.0
100.3
106.6
107.6
106.0
87.2
106.1
110.7
107.0
102.0
99.3
75.5
110.3
102.5
98.2
103.1
4.0
4.05%
11.5
11.2%
Example of reporting for 0.085 mg n=butanol: 0.085 mg nbutanol with an analytical uncertainty of +/- 0.019 mg at the
95% confidence level with probable bias of 0.003 mg
Contributors to Uncertainty
Transportation/Storage/Handling
NA
NA
NA
Laboratory Subsampling
sample nonhomogeneity
blending techniques
sample size
DUP
DUP
DUP
Sample Preparation:
volumetric glassware
dispensing device
balance
temperature
sample extraction
extractant background
LCS, DUP
LCS, DUP
LCS, DUP
LCS, DUP
LCS, DUP
LCS, DUP, MB
NA
NA
Analysts:
different analysts
analyst training level & experience
data interpretation by analyst
LCS, DUP
LCS, DUP
LCS, DUP
Measuring Instruments:
instrument stability
carry over effects
day to day calibration differences
interferences
LCS
LCS, DUP
LCS
DUP, MS
LCS, DUP
CERTIFICATE
NA
LCS
LCS
LCS
NA
Data Manipulation:
NA
LCS
Accuracy of calculations
LCS
DUP = Duplicate, resulting from sub-sampling of a bulk (NOTE: NOT LCS/LCSD duplicate spiked sampling media)
FB = Field Blank
FS = Field Spike
LCS = Laboratory Control Standard, matrix matched and typically taken through the entire analytical process, with each
sample batch
MB = Method or matrix blank
NA = Not Applicable
ement Uncertainty
Examples of Analytic
LCS
mg/Kg
195.4
189.6
4157
4186
184
184
4641
4831
179
177
4539
4858
198
207
4458
4514
True
value
mg/Kg
208.8
208.8
4490
4490
208.8
208.8
4490
4490
208.8
208.8
4490
4490
208.8
208.8
4490
4490
184
187
4551
4580
179
186
208.8
208.8
4490
4490
208.8
208.8
4245
4302
4490
4490
188
202
4217
4300
203
190
208.8
208.8
4490
4490
208.8
208.8
matched and typically taken through the entire analytical process, with each
Example of reporting fo
4400 mg/Kg Pb in paint
confidence level and a
LCS % Rec
93.6
90.8
92.6
93.2
88.1
88.1
103.4
107.6
85.7
84.8
101.1
108.2
94.8
99.1
99.3
100.5
mg/Kg
Sample
1604
511
9470
161
1683
956
23470
625
723
23000
14190
10350
5702
109
7079
196
mg/Kg
Sple Dup
1502
602
8794
93
1411
830
26570
730
472
22000
13900
9142
5854
122
6427
186
Std Dev
(S)
72.12
64.35
478.00
48.08
192.33
89.10
2192.03
74.25
177.48
707.11
205.06
854.18
107.48
9.19
461.03
7.07
CV
0.0464
0.1156
0.0523
0.3786
0.1243
0.0998
0.0876
0.1096
0.2970
0.0314
0.0146
0.0876
0.0186
0.0796
0.0683
0.0370
CV2
0.0022
0.0134
0.0027
0.1433
0.0155
0.0100
0.0077
0.0120
0.0882
0.0010
0.0002
0.0077
0.0003
0.0063
0.0047
0.0014
88.1
89.6
101.4
102.0
85.7
89.1
14510
15710
1187
9265
4240
1979
14300
17150
1192
9246
3918
1574
148.49
1018.23
3.54
13.44
227.69
286.38
0.0103
0.0620
0.0030
0.0015
0.0558
0.1612
0.0001
0.0038
0.0000
0.0000
0.0031
0.0260
94.5
95.8
2357
2254
3068
3062
502.75
571.34
0.1853
0.2150
0.0344
0.0462
90.0
96.7
93.9
95.8
97.2
91.0
53160
24810
22860
1133
151
7774
44300
23000
22930
1125
96
4366
6264.97
1279.86
49.50
5.66
38.89
2409.82
0.1286
0.0535
0.0022
0.0050
0.3149
0.3970
0.0165
0.0029
0.0000
0.0000
0.0992
0.1576
94.7
6.3
6.7%
CV2
CV pooled = (CV2/30) =
0.7064
0.1534
15.3%
33.4%
RSD