Beruflich Dokumente
Kultur Dokumente
Standard Test
Section:
Procedures Manual
Subject:
1.
SCOPE
1.1.
Description of Test
An interlaboratory testing program is used to evaluate the consistency of test results
obtained from a well defined test procedure by different laboratories testing the same
controlled material. An interlaboratory testing program removes the material and
sampling variability and provides information about the equipment and test procedure
variability that can be expected between laboratories or within a laboratory. The test
results obtained from an interlaboratory testing program on a specific test procedure can
be used to develop a precision statement for that test procedure.
This standard test procedure defines a process that can be used to design, coordinate and
analyze an interlaboratory testing program on a specific test procedure.
This standard test procedure is used to determine precision statements for the testing
procedures involved in the interlaboratory testing program.
1.2.
Application of Test
This standard test procedure is used to design, coordinate and analyze an interlaboratory
testing program. It can be used to determine precision statements for the test procedures
used in the interlaboratory testing program when six or more laboratories are involved.
1.3.
Definitions
1
Page: 1 of 331
STP 304-3
STATISTICAL QUALITY
CONTROL PRINCIPLES
Subject:
INTERLABORATORY TESTING
PROGRAMS
Page: 2 of 331
Date: 1996 04 12
STP 304-3
STATISTICAL QUALITY
CONTROL PRINCIPLES
Subject:
INTERLABORATORY TESTING
PROGRAMS
obtained according to this standard test procedure can be used to estimate the bias
1
of a specific test procedure.
1
Summary of Practice
This standard test procedure consists of four basic steps:
The analysis uses tabular, graphical and statistical diagnostic tools for evaluating the
consistency of the data so that unusual values can be identified and investigated. It also
includes calculations of numerical measures of precision for the standard test procedures
within-laboratory repeatability and between-laboratory reproducibility.
2.
Test Procedures
All testing performed in the interlaboratory testing program will be done in accordance
with Saskatchewan Highways and Transportation Standard Test Procedure(s) unless
otherwise noted. The Interlaboratory Testing Program Coordinator will identify the
appropriate Standard Test Procedure(s) that are to be used in the interlaboratory study.
2.2.
Laboratories
Acceptable test results from a minimum of three laboratories are required to complete an
interlaboratory testing program. Acceptable test results from at least six laboratories are
required to develop a precision statement for a test procedure.
Date: 1996 04 12
Page: 3 of 331
STP 304-3
STATISTICAL QUALITY
CONTROL PRINCIPLES
Subject:
INTERLABORATORY TESTING
PROGRAMS
Any laboratory that is qualified to complete the test described in the specific Standard
Test Procedure may participate in the interlaboratory testing program. Qualified
1
implies :
It is very important that the operators in the participating laboratories are familiar with the
test procedure. If the operators are not familiar with the test procedure, they should be
given the opportunity to familiarize themselves with the test procedure and practice its
application before the interlaboratory testing program starts.
2.3.
Materials
Material designates anything with a property that can be measured. Different materials
having the same property may be expected to have different property levels, meaning
1
higher or lower values of the same property. For example, an asphalt concrete mix is a
material that has properties, such as asphalt content, that can be measured. Different
asphalt concrete mixes can have the same property, asphalt content, at different levels,
low asphalt content or high asphalt content.
An interlaboratory testing program should include at least three materials representing
different levels of the property being measured by the standard test procedure. For the
development of broadly applicable precision statements at least six materials should be
1
included in the program.
The materials involved in the interlaboratory testing program should differ primarily only
in the level of the property being measured by the test procedure. If it is known or
suspected that different classes of materials will exhibit different levels of precision when
tested by the test procedure, consideration should be given to conducting a separate
1
interlaboratory testing program for each class of material.
Material homogeneity is required to remove any potential material variability so that each
laboratory is essentially testing an identical material. Thus, each material used in an
interlaboratory testing program should be produced to be or selected to be as homogenous
as possible before it is subdivided into test units. If the randomization and distribution of
individual test specimens (rather than test units) does not conflict with the procedure for
preparing the sample for testing, as specified in the test method, greater homogeneity
between test units can be achieved by randomizing test specimens. In this case, each test
1
unit would be composed of the required number of randomized test specimens.
Page: 4 of 331
Date: 1996 04 12
STP 304-3
2.4.
STATISTICAL QUALITY
CONTROL PRINCIPLES
Subject:
INTERLABORATORY TESTING
PROGRAMS
3.
PROCEDURE
3.1.
Date: 1996 04 12
Page: 5 of 331
STP 304-3
STATISTICAL QUALITY
CONTROL PRINCIPLES
Subject:
INTERLABORATORY TESTING
PROGRAMS
The Interlaboratory Testing Program Coordinator must specify the required care, handling
and conditioning of the materials. The coding system used in identifying the materials
and the distinction between test units and test specimens must be explained to the
participating laboratories.
Data sheets to record raw observations for each material should be supplied. Instructions
should be given on the number of significant digits that are to be recorded when obtaining
the raw observations. Test result sheets on which test results can be calculated and
reported should also be supplied. In most cases it may be possible to combine the result
sheet with the raw data sheet. The number of significant digits to be used in reporting the
test results should also be identified. The participating laboratories should be instructed
to return the raw data and test result sheets as soon as testing is completed, and at least
weekly if testing will continue over several weeks.
Each laboratory should be instructed to keep a record of any special events that arise
during any part of the testing. This record should be returned to the Interlaboratory
Testing Program Coordinator. It may be useful in dealing with unusual data and in
revising the Standard Test Procedure being studied.
The laboratories should be instructed to notify the Interlaboratory Testing Program
Coordinator whenever an error occurs while following (or in following) the test
procedure. A decision must be made as to whether a new set of test units should be sent
to the laboratory for a complete retest of the material.
A questionnaire should be included with the information given to the participating
laboratories. It should be designed to obtain information on specific aspects of the
apparatus, reagents, calibration, and procedure. It should capture any other information
that might assist in dealing with data inconsistencies. The questionnaire can be used to
ensure that the laboratory complied with the requirements of the test method.
3.2.
Trial Run
It may be useful, especially with new test procedures, to conduct a trial run of the
interlaboratory test program with only one or two materials to determine if the standard
test procedure(s) is clear. This can also serve to familiarize laboratories that have little
experience using the standard test procedure(s).
Even though it is just a test run, the entire process that is to be followed in the full scale
test program should be carried out.
3.3.
Page: 6 of 331
Date: 1996 04 12
STP 304-3
STATISTICAL QUALITY
CONTROL PRINCIPLES
Subject:
INTERLABORATORY TESTING
PROGRAMS
If ten laboratories were to each complete 2 tests, the test units would be labeled from B1
to B30, 10 extra samples (50% more) are required for retesting, lost samples, etc.
The specified number of test units per material should be randomly distributed to the all
of the labs. A random number table or a software program using a random number
generator should be used to ensure that the samples are distributed at random.
The test units must be packaged properly to arrive in the desired condition. When the
material is sensitive to the conditions to which it is exposed (light, heat, humidity, etc.)
place special directions for opening the package on the outside of the package. Clearly
indicate the name of the person who has been designated as the contact person for that
laboratory on the address of each package. Once the test units have been shipped, the
Interlaboratory Testing Program Coordinator should call each laboratory to confirm that
all of the test units have arrived safely.
As the interlaboratory testing program progresses, a laboratory may discover that the
standard test procedure was not used properly on some test units. The affected laboratory
must discuss this with the Interlaboratory Testing Program Coordinator who may use his
discretion to decide whether to send a replacement set of test units or leave the results as
they were obtained.
From time to time, at intervals appropriate to the magnitude of the interlaboratory testing
program, the Coordinator should contact each laboratory to determine how the testing is
progressing. By comparing the progress of all laboratories, the Coordinator can
determine whether some laboratories are lagging considerably behind the others and
advise them accordingly.
The completed data sheets should be examined by the Coordinator as soon as they are
received in order to detect unusual values or other deficiencies that should be questioned.
Replacement sets of test units may be issued when there is missing or obviously
erroneous data. The Coordinator will decide whether or not the additional data should be
used in the estimation of the Standard Test Procedures precision.
4.
CALCULATIONS
4.1.
Statistical Calculations
The analysis and treatment of the interlaboratory testing program data has three purposes:
Date: 1996 04 12
to determine whether the collected data are consistent enough to form the basis
for a test procedure precision statement,
to investigate and act on any data that is considered to be inconsistent,
to obtain the precision statistics on which the precision statement can be based.
Page: 7 of 331
STP 304-3
Section:
INTERLABORATORY TESTING
PROGRAMS
Subject:
The statistical analysis of the data is a one way analysis of variance (within and between
1
laboratories) carried out separately for each property level. This type of analysis can be
severely affected by severe outliers. Therefore, it is necessary to examine the data
consistency first. This will be explained through the use of an example.
4.2.
Calculations
4.2.1. Sample Data
The calculations required will be illustrated through the use of an example. For
the purpose of the calculations, assume that 50 Blow Hand Compacted Marshall
Density tests are conducted on three different materials in six different
laboratories. Each laboratory completed three tests on each material. The test
results were recorded in Table 1:
Table 1:
Test
Laboratory Laboratory Laboratory Laboratory Laboratory Laboratory
Number
1
2
3
4
5
6
1.0
2,359.0
2,375.0
2,352.0
2,361.0
2,334.0
2,357.0
2.0
2,359.0
2,360.0
2,365.0
2,368.0
2,336.0
2,360.0
3.0
2,368.0
2,363.0
2,356.0
2,361.0
2,336.0
2,360.0
1.0
2,356.0
2,370.0
2,353.0
2,388.0
2,357.0
2,339.0
2.0
2,352.0
2,368.0
2,365.0
2,380.0
2,358.0
2,348.0
3.0
2,354.0
2,379.0
2,363.0
2,375.0
2,358.0
2,353.0
1.0
2,350.0
2,358.0
2,339.0
2,347.0
2,350.0
2,344.0
2.0
2,352.0
2,356.0
2,348.0
2,353.0
2,351.0
2,349.0
2,350.0
2,354.0
2,351.0
2,347.0
3.0
2,346.0
2,349.0
Material
A
Laboratory
Test Results, x
2,362.0000
5.1962
27.0005
4.7778
22.8274
0.43
1.02
2,363.0
2,366.0000
7.9373
63.0007
8.7778
77.0498
0.79
1.56
2,365.0
2,356.0
2,357.6667
6.6583
44.3330
0.4444
0.1975
0.04
1.31
2,361.0
2,368.0
2,361.0
2,363.3333
4.0415
16.3337
6.1111
37.3455
0.55
0.80
2,334.0
2,336.0
2,336.0
2,335.3333
1.1547
1.3333
-21.8889
479.1239
-1.97
0.23
2,357.0
2,360.0
2,360.0
2,359.0000
1.7321
3.0002
1.7778
3.1606
0.16
0.34
Number
2,359.0
2,359.0
2,368.0
2,375.0
2,360.0
2,352.0
4
5
6
Page: 8 of 331
14,143.3333 s =
155.0014 d =
619.7047
Date: 1996 04 12
STP 304-3
STATISTICAL QUALITY
CONTROL PRINCIPLES
Table 3:
INTERLABORATORY TESTING
PROGRAMS
Subject:
Laboratory
Test Results, x
2,354.0000
2.0000
4.0000
-8.0000
64.0000
-0.64
0.37
2,379.0
2,372.3333
5.8595
34.3337
10.3333
106.7771
0.82
1.09
2,365.0
2,363.0
2,360.3333
6.4291
41.3333
-1.6667
2.7779
-0.13
1.20
2,388.0
2,380.0
2,375.0
2,381.0000
6.5574
42.9995
19.0000
361.0000
1.51
1.22
2,357.0
2,358.0
2,358.0
2,357.6667
0.5774
0.3334
-4.3333
18.7775
-0.35
0.11
2,339.0
2,348.0
2,353.0
2,346.6667
7.0946
50.3333
-15.3333
235.1101
-1.22
1.32
Number
2,356.0
2,352.0
2,354.0
2,370.0
2,368.0
2,353.0
Table 4:
14,172.0000 s2=
173.3333 d2=
788.4426
Laboratory
2,349.3333
3.0551
9.3336
-0.3333
2,349.0
2,354.3333
4.7258
22.3332
2,348.0
2,350.0
2,345.6667
5.8595
2,353.0
2,354.0
2,351.3333
3.7859
2,350.0
2,351.0
2,351.0
2,350.6667
2,344.0
2,349.0
2,347.0
2,346.6667
Number
2,350.0
2,352.0
2,346.0
2,358.0
2,356.0
2,339.0
2,347.0
5
6
0.1111
-0.10
0.80
4.6667
21.7781
1.47
1.24
34.3337
-4.0000
16.0000
-1.26
1.54
14.3330
1.6667
2.7779
0.52
0.99
0.5774
0.3334
1.0000
1.0000
0.31
0.15
2.5166
6.3333
-3.0000
9.0000
-0.94
0.66
14,098.0000 s =
87.0003
50.6671
x=
x
1
Where:
x = the average of the test results for a material for each laboratory,
x = individual test result for a material in each laboratory,
n = the number of test results for a material in each laboratory.
Date: 1996 04 12
Page: 9 of 331
STP 304-3
STATISTICAL QUALITY
CONTROL PRINCIPLES
Subject:
INTERLABORATORY TESTING
PROGRAMS
n
x
(2,359.0 + 2,359.0 + 2,368.0)
x= 1 =
= 2,362.0000
n
3
4.2.3.(ii)
s=
Where:
s = the laboratory standard deviation for a material,
x = the average of the test results for a material for each laboratory,
x = individual test result for a material in each laboratory,
n = the number of test results for a material in each laboratory.
s=
n
2
( x x)
1
=
( n 1)
= 5.1962
x& =
x
1
Where:
x& = the average of the laboratory averages for one material,
x = the average of the test results for a material for each laboratory,
p = the number of laboratories involved in the interlaboratory testing
program.
For Material A:
Page: 10 of 331
Date: 1996 04 12
STP 304-3
STATISTICAL QUALITY
CONTROL PRINCIPLES
Subject:
INTERLABORATORY TESTING
PROGRAMS
p
x
(2,362.0000 + 2,366.0000 + 2,357.6667 + 2,363.3333 + 2,335.3333 + 2,359.0000)
x& = 1 =
= 2,357.2222
p
6
4.2.4.(ii)
Laboratory Deviation, d
Calculate each laboratories deviation by subtracting the laboratory
average from the average of the laboratory averages using the
following equation:
d = x x&
Where:
d = the deviation for each laboratory from the average of laboratory
averages for one material,
x& = the average of the laboratory averages for one material,
x = the average of the test results for a material for each laboratory.
p
d2
sx = 1
( p 1)
Where:
sx = the standard deviation of the laboratory averages for one material,
d = the deviation for each laboratory from the average of laboratory
averages for one material,
p = the number of laboratories involved in the interlaboratory testing
program.
For Material A:
sx =
p 2
d
1
=
( p 1)
Date: 1996 04 12
= 11.1329
(6 1)
Page: 11 of 331
STP 304-3
STATISTICAL QUALITY
CONTROL PRINCIPLES
Subject:
INTERLABORATORY TESTING
PROGRAMS
sr =
s2
1
Where:
sr = the repeatability standard deviation for each material,
s = the laboratory standard deviation for each material,
p = the number of laboratories involved in the interlaboratory testing
program.
For Material A:
sr =
p
s2
1
=
p
4.2.5.(ii)
Page: 12 of 331
Date: 1996 04 12
STP 304-3
STATISTICAL QUALITY
CONTROL PRINCIPLES
Subject:
INTERLABORATORY TESTING
PROGRAMS
( sx )
2
sr ) ( n 1)
(
+
For Material A:
sR * =
2
sr ) ( n 1)
(
(5.0827)2 (3 1)
2
= (11.1329) +
= 11.8812
( sx ) + n
3
2
Page: 13 of 331
STP 304-3
STATISTICAL QUALITY
CONTROL PRINCIPLES
Subject:
INTERLABORATORY TESTING
PROGRAMS
h consistency statistic and the k consistency statistic are computed for each
laboratory for each material..
4.2.6.(i)
d
sx
Where:
h = the between laboratory consistency statistic,
d = the deviation for each laboratory from the average of laboratory
averages for one material,
sx = the standard deviation of the laboratory averages for one material.
4.2.6.(ii)
d
4.7778
=
= 0.43
sx 11.1329
( p 1) t
p( t 2 + p 2)
Where:
hcrit = the critical between laboratory consistency statistic,
p = the number of laboratories involved in the interlaboratory testing
program,
t = Students t value. Determined from Table 9 for a 0.5% two-tailed
level of significance and degrees of freedom.
= degrees of freedom = p - 2
Date: 1996 04 12
STP 304-3
STATISTICAL QUALITY
CONTROL PRINCIPLES
Subject:
INTERLABORATORY TESTING
PROGRAMS
( p 1) t
p t2 + p 2
(6 1) 5.5975
2
6 (5.5975) + 6 2
27.9875
= 1.92
211.9920
Date: 1996 04 12
Page: 15 of 331
STP 304-3
STATISTICAL QUALITY
CONTROL PRINCIPLES
Subject:
k=
INTERLABORATORY TESTING
PROGRAMS
s
sr
Where:
k = the within laboratory consistency statistic,
s = the laboratory standard deviation for each material,
sr = the repeatability standard deviation for each material.
s 5.1962
=
= 1.02
sr 5.0827
kcrit =
( p 1)
1 +
Where:
kcrit = the critical within laboratory consistency statistic,
p = the number of laboratories involved in the interlaboratory testing
program,
F = Value for the F-ratio. Determined from Table 10 for a 0.5% level
of significance with 1 and 2 degrees of freedom,
1 = degrees of freedom 1 = n - 1
2 = degrees of freedom 2 = (p - 1)(n - 1)
n = the number of test results for a material in each laboratory.
Date: 1996 04 12
STP 304-3
STATISTICAL QUALITY
CONTROL PRINCIPLES
Subject:
INTERLABORATORY TESTING
PROGRAMS
1 = n - 1 = 3 - 1 = 2
2 = (p - 1)(n - 1) = (6 - 1)(3 - 1) = 10
For 1 = 2 and 2 = 10 and a 0.5% level of significance from Table 10:
F = 9.4269
Then kcrit can be found by:
kcrit =
4.3.
( p 1)
1 +
6
= 1.98
( 6 1)
1 + 9.4269
Analyzing Results
4.3.1. Tabular and Graphical Display of Statistics
The data from the interlaboratory testing program can be arranged into tables and
graphs so that it is easier to interpret.
4.3.1.(i)
Tables
The h and k consistency statistics from Table 2, Table 3 and Table 4
should be tabulated into separate tables for the h and k consistency
statistics as shown in Table 5 and Table 6. It is best to arrange the
materials in increasing value of property level, as indicated by x& , from
left to right. The laboratories should be arranged in order of laboratory
code number.
4.3.1.(ii)
Date: 1996 04 12
h crit
1.92
1.92
1.92
1.92
1.92
1.92
k crit
1.98
1.98
1.98
1.98
1.98
1.98
Graphs
Bar graphs for the h and k statistics should be prepared in two ways.
The materials should be grouped by laboratories as shown in Figure 1
and Figure 2 and the laboratories should be grouped by materials as
shown in Figure 3 and Figure 4. The laboratories and materials within
Page: 17 of 331
STP 304-3
STATISTICAL QUALITY
CONTROL PRINCIPLES
Subject:
INTERLABORATORY TESTING
PROGRAMS
h Statistic
Material C
Material A
Material B
hcrit
Laboratory
k Statistic
Material C
Material A
Material B
kcrit
Page: 18 of 331
3
4
Laboratory
Date: 1996 04 12
STP 304-3
STATISTICAL QUALITY
CONTROL PRINCIPLES
Subject:
INTERLABORATORY TESTING
PROGRAMS
h Statistic
2.00
1.50
1.00
0.50
0.00
-0.50
-1.00
-1.50
-2.00
Laboratory 1
Laboratory 2
Laboratory 3
Laboratory 4
Laboratory 5
Laboratory 6
hcrit
C
Material
k Statistic
2.25
2.00
1.75
1.50
1.25
1.00
0.75
0.50
0.25
0.00
Laboratory 1
Laboratory 2
Laboratory 3
Laboratory 4
Laboratory 5
Laboratory 6
kcrit
C
Material
Page: 19 of 331
STP 304-3
STATISTICAL QUALITY
CONTROL PRINCIPLES
Subject:
INTERLABORATORY TESTING
PROGRAMS
p, and the number of test results per laboratory per material, n. The
0.5% level of significance was chosen on the basis that too many
laboratories are flagged at the 1.0% level of significance and not
1
enough laboratories are flagged at the 0.1% level of significance. At
the 0.5% level of significance there is a 0.5% chance (1 time in 200)
that a laboratory will be identified as having different test results from
the other labs (some type of testing problem) when in fact its test
results are the same as the other labs (there is no testing problem).
After the critical h and k values are calculated, examine the h and k
statistics reported in Table 5 and Table 6. Underline any values that
exceed the critical values and circle any values that approach the
critical values. A horizontal line representing the critical value should
be drawn on each of the graphs. There will be one line for the k
statistic graphs and two lines (critical values can be either positive or
negative) on the h statistic graphs. Any bars that exceed or approach
the critical values should be investigated.
In this example, the testing done by Laboratory 5 on Material A should
be investigated because the h value exceeds the hcrit value..
4.3.2.(ii)
Date: 1996 04 12
STP 304-3
STATISTICAL QUALITY
CONTROL PRINCIPLES
Subject:
INTERLABORATORY TESTING
PROGRAMS
Page: 21 of 331
STP 304-3
STATISTICAL QUALITY
CONTROL PRINCIPLES
Subject:
INTERLABORATORY TESTING
PROGRAMS
lower than the other laboratories for each material. This laboratory
should be investigated.
5.
Investigation of Errors
5.1.1. Clerical and Sampling Errors
Examine the laboratory report for each flagged h or k value. Attempt to determine
where each test result begins to deviate from the others. Is it in the original
observations? Are the data rounded prematurely? Are the calculations correct?
Look for signs of mislabeling test units to see if the test results for one material
were reported as belonging to another material. These errors should be checked
with the laboratories involved.
5.1.2. Procedural Errors
The laboratory records should be studied to identify any deviations from either the
standard testing procedure or the protocol established for the interlaboratory
testing program. For example, variations in the number of significant digits
reported in the test results may be a sign of incorrect rounding or that equipment
in one laboratory is different from the rest. The event log should be studied for
any special comments relating to the flagged h or k consistency statistics.
5.1.3. Dealing with Errors
If the investigation disclosed no clerical, sampling or procedural errors, the
unusual data should be retained and the precision statistics based on them should
be published.
If the laboratory clearly and seriously deviated from the standard test procedure,
the test results for that laboratory must be removed from the calculations for the
interlaboratory testing program. It may be appropriate to ask the laboratory to
retest one or more materials following the correct standard test procedure. There
is a danger that the laboratory may apply the standard test procedure in the same
manner the second time. If the laboratory is allowed to retest, the data will change
and it will be necessary to recalculate all the h and k consistency statistics and
reexamine the data for inconsistent results.
If the investigation can not determine a reason for some unusual test results for a
particular laboratory and material, it may be appropriate to delete the test results
for that laboratory and material. This will change the data, so it will be necessary
to recalculate all the h and k consistency statistics for the affected materials and
reexamine the data for inconsistent results. It should be noted that data should
only be deleted when there is a large number of laboratories involved in the
Page: 22 of 331
Date: 1996 04 12
STP 304-3
STATISTICAL QUALITY
CONTROL PRINCIPLES
Subject:
INTERLABORATORY TESTING
PROGRAMS
These problems can be the basis for a revising the standard test procedure.
5.2.
Date: 1996 04 12
Page: 23 of 331
STP 304-3
STATISTICAL QUALITY
CONTROL PRINCIPLES
INTERLABORATORY TESTING
PROGRAMS
Subject:
The 1.96 multiplier assumes that the test results being compared are normally
distributed. For methods in which the average of several test results is reported as
a single test result the assumption of normality is usually valid. When normality
cannot be assumed, it is usually acceptable to use the 1.96 multiplier recognizing
2
that the actual probability level may differ slightly from the nominal 95% limit.
The use of the 1.96 multiplier requires that the sample standard deviation (s) be
equal to the population standard deviation (). No within or between laboratory
study will yield a sample standard deviation (s) equal to the population standard
deviation () unless there are at least 30 laboratories included in the study. The
use of the t multiplier, from a students t distribution, does not solve this problem.
In order to resolve this problem, a range of probabilities around 95% must be
accepted as defining the 95% limit. It has been shown that 1.96 is the best
multiplier for achieving the desired (but approximate) 95% coverage. The
multiplier is independent of the number of laboratories in the testing program or
the number of test results obtained by each laboratory. However, a within or
between laboratory testing program must be of reasonably large size in order to
2
provide reliable information on which to base precision statements.
For the testing done on Material A:
rA = 2.8 sr = 2.8 5.083 = 14.2
RA = 2.8 sR = 2.8 11.881 = 33.3
5.2.2. Bias
5.2.2.(i)
Page: 24 of 331
Date: 1996 04 12
STP 304-3
STATISTICAL QUALITY
CONTROL PRINCIPLES
Subject:
INTERLABORATORY TESTING
PROGRAMS
2,362.0 2,357.2
100 = 0.20%
2,357.2
Material B
Material C
Bias A
Bias B
Bias C
Laboratory 1
2,362.0
0.20%
2,354.0
-0.34%
2,349.3
-0.01%
Laboratory 2
2,366.0
0.37%
2,372.3
0.44%
2,354.3
0.20%
Laboratory 3
2,357.7
0.02%
2,360.3
-0.07%
2,345.7
-0.17%
Laboratory 4
2,363.3
0.26%
2,381.0
0.80%
2,351.3
0.07%
Laboratory 5
2,335.3
-0.93%
2,357.7
-0.18%
2,350.7
0.04%
Laboratory 6
2,359.0
0.08%
2,346.7
-0.65%
2,346.7
-0.13%
x&
2,357.2
x&
= 2,362.0
x&
= 2,349.7
Date: 1996 04 12
Page: 25 of 331
STP 304-3
STATISTICAL QUALITY
CONTROL PRINCIPLES
Subject:
INTERLABORATORY TESTING
PROGRAMS
Page: 26 of 331
Date: 1996 04 12
STP 304-3
STATISTICAL QUALITY
CONTROL PRINCIPLES
Subject:
INTERLABORATORY TESTING
PROGRAMS
Material B
Material C
2,357.2 kg/m3
2,362.0 kg/m3
2,349.7 kg/m3
14.2 kg/m3
15.0 kg/m3
12.5 kg/m3
33.3 kg/m3
37.2 kg/m3
12.5 kg/m3
The respective standard deviations among test results may be obtained by dividing
the above limit values by 2.8. More detailed precision statistics are shown in
Table 8.
Table 8: 50 Blow Hand Compaction Marshall Density Precision Statistics (kg/m3)
Material
x&
sr
sR
2,357.2
11.1
5.1
11.9
14.2
33.3
2,362.0
12.6
5.4
13.3
15.0
37.2
2,349.7
4.4
4.4
4.4
12.5
12.5
Page: 27 of 331
STP 304-3
STATISTICAL QUALITY
CONTROL PRINCIPLES
Subject:
INTERLABORATORY TESTING
PROGRAMS
For materials with the property level found in Material C, approximately 95% of
all pairs of test results from within a laboratory similar to that in the study can
be expected to differ in absolute value by less than 12.5 kg/m3. For materials with
the property level of Material C, two test results from the same laboratory would
be considered suspect if they differed in absolute value by more than 12.5 kg/m3.
For materials with the property levels found in Materials A and B, approximately
95% of all pairs of test results from between laboratories similar to those in the
study, can be expected to differ in absolute value by less than 37 kg/m3. For
materials with the property level of Material A or B, two test results from different
laboratories would be considered suspect if they differed in absolute value by
more than 37 kg/m3.
For materials with the property level found in Material C, approximately 95% of
all pairs of test results from between laboratories similar to those in the study
can be expected to differ in absolute value by less than 12.5 kg/m3. For materials
with the property level of Material C, two test results from different laboratories
would be considered suspect if they differed in absolute value by more than 12.5
kg/m3.
6.
ADDED INFORMATION
6.1.
Limitations
The precision statistics obtained by an interlaboratory testing program, such as the one
described in this Standard Test Procedure, must not be treated as exact mathematical
quantities which are applicable to all circumstances and uses. The small number of
laboratories and materials used in the typical interlaboratory testing program guarantees
that there will be times when differences greater than that predicted by the interlaboratory
testing program will arise. This can occur with considerably greater or smaller frequency
than the 95% probability level would imply. The repeatability and reproducibility limit
should be considered as general guides and the associated 95% probability as only a
rough indicator of what can be expected. If more precise information is needed in a
specific case, the laboratories directly involved in the material comparison must conduct
1
interlaboratory studies specifically aimed at the material being studied.
6.2.
References
This test procedure is similar to ASTM E 691-92 Standard Practice for Conducting an
Interlaboratory Study to Determine the Precision of a Test Method. It also incorporates
components of ASTM E 177 -90a Standard Practice for the Use of the Terms Precision
and Bias in ASTM Test Methods.
Page: 28 of 331
Date: 1996 04 12
STP 304-3
STATISTICAL QUALITY
CONTROL PRINCIPLES
Subject:
INTERLABORATORY TESTING
PROGRAMS
C:\WINDOWS\WINWORK\QUALITY\LABCORR\STP304-3.DOC
Date: 1996 04 12
Page: 29 of 331
STP 304-3
STATISTICAL QUALITY
CONTROL PRINCIPLES
Subject:
INTERLABORATORY TESTING
PROGRAMS
0.1%
0.5%
1.0%
1.5%
2.0%
Degrees of
Freedom ()
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
35
40
45
50
10,000,000
Page: 30 of 331
2.5%
3.0%
3.5%
4.0%
4.5%
5.0%
10.0%
18.1707
5.2039
3.6700
3.1355
2.8699
2.7123
2.6083
2.5347
2.4798
2.4375
2.4037
2.3763
2.3535
2.3342
2.3178
2.3036
2.2911
2.2802
2.2705
2.2619
2.2541
2.2470
2.2406
2.2348
2.2295
2.2246
2.2201
2.2159
2.2120
2.2084
2.1936
2.1825
2.1741
2.1673
2.1084
15.8945
4.8487
3.4819
2.9985
2.7565
2.6122
2.5168
2.4490
2.3984
2.3593
2.3281
2.3027
2.2816
2.2638
2.2485
2.2354
2.2238
2.2137
2.2047
2.1967
2.1894
2.1829
2.1770
2.1715
2.1666
2.1620
2.1578
2.1539
2.1503
2.1470
2.1332
2.1229
2.1150
2.1087
2.0537
14.1235
4.5534
3.3216
2.8803
2.6579
2.5247
2.4363
2.3735
2.3266
2.2902
2.2612
2.2375
2.2178
2.2012
2.1870
2.1747
2.1639
2.1544
2.1460
2.1385
2.1318
2.1256
2.1201
2.1150
2.1104
2.1061
2.1022
2.0986
2.0952
2.0920
2.0791
2.0695
2.0621
2.0562
2.0047
12.7062
4.3027
3.1824
2.7765
2.5706
2.4469
2.3646
2.3060
2.2622
2.2281
2.2010
2.1788
2.1604
2.1448
2.1315
2.1199
2.1098
2.1009
2.0930
2.0860
2.0796
2.0739
2.0687
2.0639
2.0595
2.0555
2.0518
2.0484
2.0452
2.0423
2.0301
2.0211
2.0141
2.0086
1.9600
6.3137
2.9200
2.3534
2.1318
2.0150
1.9432
1.8946
1.8595
1.8331
1.8125
1.7959
1.7823
1.7709
1.7613
1.7531
1.7459
1.7396
1.7341
1.7291
1.7247
1.7207
1.7171
1.7139
1.7109
1.7081
1.7056
1.7033
1.7011
1.6991
1.6973
1.6896
1.6839
1.6794
1.6759
1.6449
Values of t
636.5776 127.3211
31.5998 14.0892
12.9244
7.4532
8.6101
5.5975
6.8685
4.7733
5.9587
4.3168
5.4081
4.0294
5.0414
3.8325
4.7809
3.6896
4.5868
3.5814
4.4369
3.4966
4.3178
3.4284
4.2209
3.3725
4.1403
3.3257
4.0728
3.2860
4.0149
3.2520
3.9651
3.2224
3.9217
3.1966
3.8833
3.1737
3.8496
3.1534
3.8193
3.1352
3.7922
3.1188
3.7676
3.1040
3.7454
3.0905
3.7251
3.0782
3.7067
3.0669
3.6895
3.0565
3.6739
3.0470
3.6595
3.0380
3.6460
3.0298
3.5911
2.9961
3.5510
2.9712
3.5203
2.9521
3.4960
2.9370
3.2905
2.8070
63.6559
9.9250
5.8408
4.6041
4.0321
3.7074
3.4995
3.3554
3.2498
3.1693
3.1058
3.0545
3.0123
2.9768
2.9467
2.9208
2.8982
2.8784
2.8609
2.8453
2.8314
2.8188
2.8073
2.7970
2.7874
2.7787
2.7707
2.7633
2.7564
2.7500
2.7238
2.7045
2.6896
2.6778
2.5758
42.4334
8.0728
5.0473
4.0880
3.6338
3.3723
3.2031
3.0851
2.9982
2.9316
2.8789
2.8363
2.8010
2.7714
2.7462
2.7245
2.7056
2.6889
2.6742
2.6611
2.6493
2.6387
2.6290
2.6203
2.6123
2.6049
2.5981
2.5918
2.5860
2.5806
2.5584
2.5420
2.5294
2.5193
2.4324
31.8210
6.9645
4.5407
3.7469
3.3649
3.1427
2.9979
2.8965
2.8214
2.7638
2.7181
2.6810
2.6503
2.6245
2.6025
2.5835
2.5669
2.5524
2.5395
2.5280
2.5176
2.5083
2.4999
2.4922
2.4851
2.4786
2.4727
2.4671
2.4620
2.4573
2.4377
2.4233
2.4121
2.4033
2.3264
25.4519
6.2054
4.1765
3.4954
3.1634
2.9687
2.8412
2.7515
2.6850
2.6338
2.5931
2.5600
2.5326
2.5096
2.4899
2.4729
2.4581
2.4450
2.4334
2.4231
2.4138
2.4055
2.3979
2.3910
2.3846
2.3788
2.3734
2.3685
2.3638
2.3596
2.3420
2.3289
2.3189
2.3109
2.2414
21.2051
5.6428
3.8961
3.2976
3.0029
2.8289
2.7146
2.6338
2.5738
2.5275
2.4907
2.4607
2.4358
2.4149
2.3970
2.3815
2.3681
2.3562
2.3457
2.3362
2.3278
2.3202
2.3132
2.3069
2.3011
2.2958
2.2909
2.2864
2.2822
2.2783
2.2622
2.2503
2.2411
2.2338
2.1701
Date: 1996 04 12
STP 304-3
STATISTICAL QUALITY
CONTROL PRINCIPLES
INTERLABORATORY TESTING
PROGRAMS
Subject:
0.50%
1.00%
Degrees of Freedom
2 (2)
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
35
40
45
50
60
80
100
120
140
150
10,000,000
5.00%
5,403.5336
99.1640
29.4567
16.6942
12.0599
9.7796
8.4513
7.5910
6.9920
6.5523
6.2167
5.9525
5.7394
5.5639
5.4170
5.2922
5.1850
5.0919
5.0103
4.9382
4.8740
4.8166
4.7648
4.7181
4.6755
4.6365
4.6009
4.5681
4.5378
4.5097
4.3958
4.3126
4.2492
4.1994
4.1259
4.0363
3.9837
3.9491
3.9246
3.9149
3.7816
161.4462
18.5128
10.1280
7.7086
6.6079
5.9874
5.5915
5.3176
5.1174
4.9646
4.8443
4.7472
4.6672
4.6001
4.5431
4.4940
4.4513
4.4139
4.3808
4.3513
4.3248
4.3009
4.2793
4.2597
4.2417
4.2252
4.2100
4.1960
4.1830
4.1709
4.1213
4.0847
4.0566
4.0343
4.0012
3.9604
3.9362
3.9201
3.9087
3.9042
3.8414
199.4995
19.0000
9.5521
6.9443
5.7861
5.1432
4.7374
4.4590
4.2565
4.1028
3.9823
3.8853
3.8056
3.7389
3.6823
3.6337
3.5915
3.5546
3.5219
3.4928
3.4668
3.4434
3.4221
3.4028
3.3852
3.3690
3.3541
3.3404
3.3277
3.3158
3.2674
3.2317
3.2043
3.1826
3.1504
3.1108
3.0873
3.0718
3.0608
3.0564
2.9957
215.7067
19.1642
9.2766
6.5914
5.4094
4.7571
4.3468
4.0662
3.8625
3.7083
3.5874
3.4903
3.4105
3.3439
3.2874
3.2389
3.1968
3.1599
3.1274
3.0984
3.0725
3.0491
3.0280
3.0088
2.9912
2.9752
2.9603
2.9467
2.9340
2.9223
2.8742
2.8387
2.8115
2.7900
2.7581
2.7188
2.6955
2.6802
2.6693
2.6649
2.6049
Values of F
16,212.4634 19,997.3583 21,614.1343
198.5027
199.0120
199.1575
55.5519
49.8003
47.4683
31.3321
26.2844
24.2599
22.7847
18.3136
16.5301
18.6346
14.5442
12.9166
16.2354
12.4037
10.8826
14.6883
11.0426
9.5965
13.6138
10.1068
8.7171
12.8266
9.4269
8.0809
12.2263
8.9121
7.6004
11.7543
8.5097
7.2257
11.3737
8.1864
6.9258
11.0604
7.9217
6.6804
10.7980
7.7007
6.4761
10.5756
7.5138
6.3034
10.3842
7.3537
6.1557
10.2182
7.2148
6.0278
10.0727
7.0934
5.9160
9.9440
6.9865
5.8177
9.8294
6.8915
5.7304
9.7270
6.8064
5.6524
9.6347
6.7300
5.5823
9.5513
6.6609
5.5190
9.4753
6.5982
5.4615
9.4060
6.5410
5.4091
9.3423
6.4886
5.3611
9.2837
6.4404
5.3170
9.2298
6.3958
5.2764
9.1798
6.3546
5.2388
8.9763
6.1879
5.0865
8.8278
6.0664
4.9758
8.7148
5.9741
4.8918
8.6256
5.9016
4.8259
8.4947
5.7950
4.7290
8.3346
5.6652
4.6113
8.2407
5.5892
4.5424
8.1789
5.5393
4.4972
8.1350
5.5040
4.4652
8.1177
5.4899
4.4525
7.8794
5.2983
4.2794
4,052.1845
98.5019
34.1161
21.1976
16.2581
13.7452
12.2463
11.2586
10.5615
10.0442
9.6461
9.3303
9.0738
8.8617
8.6832
8.5309
8.3998
8.2855
8.1850
8.0960
8.0166
7.9453
7.8811
7.8229
7.7698
7.7213
7.6767
7.6357
7.5977
7.5624
7.4191
7.3142
7.2339
7.1706
7.0771
6.9626
6.8953
6.8509
6.8194
6.8069
6.6349
4,999.3396
99.0003
30.8164
17.9998
13.2741
10.9249
9.5465
8.6491
8.0215
7.5595
7.2057
6.9266
6.7009
6.5149
6.3588
6.2263
6.1121
6.0129
5.9259
5.8490
5.7804
5.7190
5.6637
5.6136
5.5680
5.5263
5.4881
5.4529
5.4205
5.3903
5.2679
5.1785
5.1103
5.0566
4.9774
4.8807
4.8239
4.7865
4.7600
4.7495
4.6052
_______________________________________________________________________
1
ASTM E691-92 Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method, ASTM
Standards on Precision and Bias for Various Application: Fourth Edition, ASTM, Philadelphia, PA, 1992.
2
ASTM E177-90a Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods, ASTM Standards on
Precision and Bias for Various Application: Fourth Edition, ASTM, Philadelphia, PA, 1992.
Date: 1996 04 12
Page: 31 of 331