Methanol Specifications

Results of Proficiency Test
Methanol
September 2008
Organised by:
Institute for Interlaboratory Studies

Spijkenisse, the Netherlands
Authors: ing. R.J. Starink

Correctors: dr. R.G. Visser and ing. S. Lagendijk
Report: iis08C06X
November 2008
Spijkenisse, November 2008
CONTENTS
1
INTRODUCTION ..................................................................................................................................... 3
SET UP .................................................................................................................................................... 3
2.1
ACCREDITATION ................................................................................................................................... 3
2.2
PROTOCOL............................................................................................................................................. 3
2.3
CONFIDENTIALITY STATEMENT ......................................................................................................... 4
2.4
SAMPLES ................................................................................................................................................ 4
2.5
STABILITY OF THE SAMPLES .............................................................................................................. 5
2.6
ANALYSES .............................................................................................................................................. 5
RESULTS................................................................................................................................................. 5
3.1
STATISTICS ............................................................................................................................................ 6
3.2
GRAPHICS .............................................................................................................................................. 6
3.3
Z-SCORES .............................................................................................................................................. 6
EVALUATION .......................................................................................................................................... 7
4.1
EVALUATION PER TEST ....................................................................................................................... 7
4.2
PERFORMANCE EVALUATION FOR THE GROUP OF LABORATORIES ...................................... 11
4.3
COMPARISON OF THE PROFICIENCY TEST OF SEPTEMBER 2008 WITH PREVIOUS PTS.... 13
Appendices:
1.
Data and statistical results ................................................................................................................. 15
2.
List of number of participants per country ......................................................................................... 68
3.
Abbreviations and literature ............................................................................................................... 69
page 2 of 69
Methanol: iis08C06X
INTRODUCTION
Since 1996, a proficiency test for Methanol was organised every year by The Institute for
Interlaboratory Studies. During the annual proficiency testing program 2008/2009, it was decided
to continue the round robin for the analysis of Methanol in accordance with the latest applicable
version of the IMPCA specification and ASTM E346:03. In the latest IMPCA specification of
January 2008, the Sulphur determination ASTM D3961:98 as test method is mentioned. As
ASTM D3961:98 was withdrawn in 2004 with no replacement, it was decided by the IMPCA
group to prepare a new IMPCA method for the determination of Sulphur based on ASTM D3961.
The draft version of this IMPCA005:08 was sent along with the samples.
In this international interlaboratory study 64 laboratories in 31 different countries have
participated. See appendix 2 for a list of participants in alphabetical country order. In this report
the results of the proficiency test are presented and discussed.
SET UP
The Institute for Interlaboratory studies (i.i.s.) in Spijkenisse, The Netherlands, was the organiser
of this proficiency test. To get maximum information from this study it was decided to send 2
different samples (1*1 L labelled #0844 and 1*0.25 L labelled #0845).
Sample #0844 was spiked with Dibenzothiophene (1.23 mg/kg) especially for the determination
of Sulphur. A hardcopy of draft test method IMPCA005:08 was enclosed with the samples.
Sample #0845 was spiked with Sodium Chloride (0.52 mg Cl/kg) and Benzene (10 mg/kg).
The participants were requested to report rounded and unrounded results. The unrounded results
were preferably used for statistical evaluations.
2.1
ACCREDITATION
The Institute for Interlaboratory Studies in Spijkenisse, the Netherlands, is accredited in
accordance with ISO guide 43 and ILAC-G13:2000, (R007), since January 2000, by the Dutch
Accreditation Council (Raad voor Accreditatie). This ensures 100% confidentially of participants
data. Feedback from the participants on the reported data is encouraged and customers
satisfaction is measured on regular basis by sending out questionnaires.
2.2
PROTOCOL
The protocol followed in the organisation of this proficiency test was the one as described for
proficiency testing in the report iis Interlaboratory Studies: Protocol for the Organisation,
Statistics and Evaluation of November 2008 (iis-protocol, version 3.1).
Methanol: iis08C06X
page 3 of 69
2.3
CONFIDENTIALITY STATEMENT
All data present in this report must be regarded as confidential and for use by the participating
companies only. Disclosure of the information in this report is only allowed by means of the entire
report. Use of the contents of this report for third parties is only allowed by written permission of
the Institute of Interlaboratory Studies. Disclosure of the identity of one or more of the
participating companies will be done only after receipt of a written agreement of the companies
involved.
2.4
SAMPLES
The necessary 100 litre bulk material was provided by a large Methanol producer. The bulk
material was divided in two parts. Approx. 75 litre bulk material was after spiking with 70 mL of a
1.014 mg/L Dibenzothiophene solution, homogenised in a pre-cleaned metal drum and divided
over 72 brown glass bottles of 1 L and labelled #0844. The other 25 litre bulk material in a precleaned can was, after spiking with 200.1 mg Benzene and 16.40 mg Sodium Chloride,
homogenised and divided over 95 brown glass bottles of 0.25 L and labelled #0845.
The homogeneity of the subsamples #0844 was checked by determination of Density in
accordance with ASTM D4052:02, Water content in accordance with ASTM E203:01 and Sulphur
content in accordance with ASTM D3961:03 on 4 stratified random selected samples. The
homogeneity of the subsamples #0845 was checked by determination of Chloride in accordance
with IMPCA 002:1998 and UV absorbance at 250nm according IMPCA004:06 on 5 stratified
random selected samples.
Density at 20C
in kg/L
Water
in mg/kg
Sulphur
in mg/kg
sample #0844-1
0.79144
190
1.03
sample #0844-2
0.79144
200
1.11
sample #0844-3
0.79143
190
0.91
sample #0844-4
0.79144
200
1.05
Table 1: homogeneity test of subsample #0844
UV absorbance
at 250 nm
Chloride
in mg/kg
sample #0845-1
0.275
0.58
sample #0845-2
0.272
0.55
sample #0845-3
0.271
0.59
sample #0845-4
0.271
0.58
sample #0845-5
0.269
0.59
Table 2: homogeneity test of subsample #0845
From the results in table 1 and 2, the repeatabilities of the results were calculated by
multiplication of the standard deviations by 2.8:
page 4 of 69
Methanol: iis08C06X
Density at 15C
in kg/L
Water
in mg/kg
Sulphur
in mg/kg
Chloride
in mg/kg
UV-absorbance
at 250nm
r (sample #0844)
0.00001
16.2
0.23
--
--
r (sample #0845)
--
--
--
0.03
0.006
Horwitz
IMPCA 002:98
IMPCA 004:06
0.22
0.03
0.010
reference test
r (reference test)
ASTM D4052:02 ASTM E203:01

0.00010
80.0
Table 3: repeatabilities of subsamples #0844 and #0845
The repeatabilities of Density, Water and Sulphur for sample #0844 were in agreement with the
respective methods and the estimated repeatability calculated using the Horwitz equation. The
repeatabilities of Chloride and UV absorbance at 250nm for sample #0845 were in agreement
with IMPCA 002:98 and IMPCA 004:06. Therefore homogeneity of the subsamples #0844 and
#0845 was assumed.
Two samples of Methanol (1 * 1 L sample of #0844 and 1 * 0.25 L sample of #0845) were sent to
the participating laboratories on August 27, 2008.
2.5
STABILITY OF THE SAMPLES

The stability of Methanol, packed in the brown glass bottles, was checked. The material was
found sufficiently stable for the period of the proficiency test.
2.6
ANALYSES
The participants were asked to determine Acidity, Anorganic Chloride, Appearance, Carbonisable
Substances Pt/Co, Colour Pt/Co, Density @ 20 oC, Distillation (IBP & DP), Acetone, Ethanol,
Water Miscibility, Nonvolatile Matter, Purity (on dry basis), Permanganate Time Test, Specific
Gravity 20/20 C/C, Apparent Specific Gravity 20/20 C/C, Sulphur, Total Iron, Trimethylamine
and Water (coulometric and titrimetric) on sample #0844. On sample #0845 was requested to
analyze: Anorganic Chloride, Acetone, Benzene, Ethanol, Sulphur and UV absorbance at 300,
268.5, 250 and 220 nm.
To get comparable results, a detailed report form on which the units and the preferred test
methods were printed, was sent together with each set of samples. Also a letter of instructions, a
MSDS and a draft method IMPCA006:08 were added to the package.
RESULTS
During four weeks after sample despatch the results of the individual laboratories were gathered.
The original data are tabulated per determination in appendix 1 of this report. The laboratories
are represented by their code numbers.
Directly after the deadline, a reminder fax was sent to the laboratories that had not reported
results at that moment. Shortly after the deadline the available results were screened for suspect
data. A result was called suspect in case the Huber Elimination Rule (a robust outlier test) found
Methanol: iis08C06X
page 5 of 69
it to be an outlier. The laboratories that produced these suspect data were asked to check the
results. Additional or corrected results are used for data analysis and original results are placed
under 'Remarks' in the result tables in appendix 1.
3.1
STATISTICS
Statistical calculations were performed as described in the report i.i.s. Interlaboratory Studies:
Protocol for the Organisation, Statistics and Evaluation of November 2003 (iis-protocol, version
3.0).
For the statistical evaluation the unrounded (when available) figures were used instead of the
rounded results. Results reported as '<' or '>' were not used in the statistical evaluation.
First the normality of the distribution of the various data sets per determination was checked by
means of the Lilliefors-test. After removal of outliers this check was repeated. In case a data set
does not have a normal distribution, the (results of the) statistical evaluation should be used with
due care.
In accordance to ISO 5725 (1986 and 1994) the original results per determination were submitted
subsequently to Dixon and Grubbs outlier tests. Outliers are marked by
D(0.01) for the Dixon test and by G(0.01) or DG(0.01) for the Grubbs test. Stragglers are marked
by D(0.05) for the Dixon test and by G(0.05) or DG(0.05) for the Grubbs test. Both outliers and
stragglers were not included in the calculations of the averages and the standard deviations.
Finally, the reproducibilities were calculated from the standard deviations by multiplying these
with a factor of 2.8.
3.2
GRAPHICS
In order to visualise the results against the reproducibilities from literature, Gauss plots were made,
using the sorted data for each determination (see appendix 1). On the Y-axis the analytical results
are plotted. The corresponding laboratory numbers are under the X-axis. A straight line presents
the average of the reported data. Two striped lines present the reproducibility limits of the selected
standard, calculated as mean target reproducibility, parallel to the average line. Outliers and
other data, which were excluded from the calculations, are represented as a cross. Accepted data
are represented as a triangle. Furthermore, Kernel Density Graphs were made. This is a method
for producing a smooth density approximation to a set of data that avoids some problems
associated with histograms (see appendix 3; nr.14 and 15)
3.3
Z-SCORES
As it was decided to evaluate the performance of the participants against the literature
requirements, e.g. ASTM reproducibilities, the z-scores were calculated using a target standard
deviation. This target standard deviation was calculated from the literature reproducibility by
division with 2.8. The z-scores were calculated according to:
page 6 of 69
Methanol: iis08C06X
z(target) = (result - average) / target standard deviation

To evaluate the performance of the participating laboratories the z-scores were calculated.
Absolute values for z<2 are very common and absolute values for z>3 are very rare. Therefore
the usual interpretation of z-scores is as follows:
|z|<1
1< |z|<2
2< |z|<3
|z|>3
4
good
satisfactory
questionable
unsatisfactory
EVALUATION
In this proficiency test some major problems were encountered with despatch of the samples to
the laboratories in Mexico, P.R. of China, Poland, Russia, Thailand and Venezuela. Thirteen
participants received the samples near or after the final reporting date. In total, 14 participants
reported after the deadline and 4 participants did not report any result at all. Not all participants
were able to report all requested parameters. Finally, 60 participants did send in 748 numerical
results. Observed were 24 outlying results, which is 3.2 % of the total of numerical results. In
proficiency studies outlier percentages of 3 % - 7.5 % are quite normal.
4.1
EVALUATION PER TEST

In this section the results are discussed per test. Not normal distributions were found for the
following determinations: Acidity, Anorganic Chloride (#0844 and #0845), Carbonisable
Substances, Colour Pt/Co, Density @ 20 oC, IBP (automatic and manual), DP (automatic and
manual), Nonvolatile Matter, Specific Gravity, Apparent Specific Gravity, Total Iron (##0844),
Ethanol (#0844 and #0845) and UV absorbance at 268.5 nm. In these cases the statistical
evaluation should be used with due care. From the Kernel Density graphs, one can see that this
conclusion is not always justified.
Acidity:
No analytical problems were observed. Only one result was outside the
reproducibility limits and the observed reproducibility is, after rejection of the
statistical outlier, in good agreement with the requirements of ASTM D1613:06.
Anorg. Chloride: This determination is somewhat problematic. For both samples, in total four
results were outside the reproducibility limits. The calculated reproducibility of
sample #0844 is, after rejection of the statistical outlier, in good agreement with
the requirements of IMPCA002:98. The calculated reproducibility of sample
#0845 is, after rejection of the statistical outliers, not in agreement with the
requirements of IMPCA002:98. The average recovery of the chloride content
(calculated from the difference between the assigned value for the original
sample #0844 and the spiked sample #0845 and the theoretical increment of
0.52 mg Cl/kg) is good (104%). The individual recoveries vary over a large
Methanol: iis08C06X
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range. The same was found in previous proficiency tests. Experience has
shown that very low levels of chloride are very difficult to determine with
accuracy by means of turbidimetry. The best technique for anorganic chloride
with the highest accuracy is the IMPCA method using dedicated titration
equipment.
Appearance:
No analytical problems were observed. All labs agreed about the appearance of
the sample #0844: bright, clear and free of suspended matter.
Carbonisable Substances: This determination is problematic for one laboratory. Only one
result was outside the reproducibility limits. The observed reproducibility is, after
rejection of the statistical outlier, almost in agreement with the requirements of
ASTM E346:03e1. The rounding of the result is probably the cause that the
spread is relativity large.
Colour:
No analytical problems were observed. No results were found outside the

reproducibility limits. The observed reproducibility is in good agreement with the
requirements of ASTM D1209:05e1.
Density @ 20oC: This determination was problematic only for one laboratory. Only one result was
outside the reproducibility limits and the observed reproducibility is, after
rejection of the statistical outlier, in good agreement with the requirements of
ASTM D4052:02e1.
Distillation:
This determination was problematic for at least one laboratory. For both
samples, in total only one result was outside the reproducibility limits. All
calculated reproducibilities (for IBP and DP, automated and manual mode) are
good in agreement with the requirements for automated and manual modes of
ASTM D1078:05. This remarkable as obviously several participants did not
correct for barometric pressure: the theoretical mid boiling point of 64.5C for
Methanol was not included in the reported IBP-DP range (see table 3 in ASTM
D1078).
Water Miscibility: No analytical problems were observed. All laboratories reported the test as
pass, except one that reported complete. This may be remarkable as the
sample #0844 contained 0.1% Toluene.
NVM:
This determination is problematic for only one laboratory. Only one result was
outside the reproducibility limits. The reproducibility is, after rejection of the
statistical outlier, in good agreement with the requirements of ASTM D1353:03.
PTT:
All participants agreed on a result far above 60 minutes.

As it is unknown whether a Permanganate Time Test of >60 minutes is in the
applicability range, it is therefore difficult to draw any conclusions. Therefore, no
z-scores were calculated.
page 8 of 69
Methanol: iis08C06X
SG 20/20 oC:
No analytical problems were observed. No results were outside the

reproducibility limits and the calculated reproducibility is in good agreement with
the requirements of ASTM D4052:02e1.
The Specific Gravity is defined as: the ratio of the weight in Vacuum of a unit
volume of a material at stated temperature to the weight in Vacuum of an equal
volume of gas-free distilled water at a stated temperature.
SG 20/20 oC = (density material at 20 oC) / (density water at 20 oC).
ASG 20/20 oC: No analytical problems were observed. No results were outside the reproducibility
limits and the calculated reproducibility is in good agreement with the
requirements of ASTM D4052:02e1.
The Apparent Specific Gravity is defined as: the ratio of the weight in air of a
unit volume of a material at stated temperature to the weight in air of equal
density of an equal volume of gas-free distilled water at a stated temperature.
SG Apparent 20/20 oC = (density material at 20 oC 0.00120) / (density water at
20 oC - 0.00120).
SG General:
When the Specific Gravities and Apparent Specific Gravities were calculated
from the reported Densities, it was noticed that the reported results for the
Specific Gravity 20/20 oC and Apparent Specific Gravity 20/20 oC are in line with
the calculated results. Users of method ASTM D891 should be aware that this
method results in Apparent Specific Gravity. To arrive at Specific Gravity or
Density an additional conversion is necessary. The method provides the
calculation formula.
Sulphur:
As ASTM D3961:98 was withdrawn in 2004 with no replacement, it was decided

by the IMPCA group to prepare a new IMPCA method for the determination of
Sulphur based on ASTM D3961. The draft version of this IMPCA005:08 was
sent along with the samples.
To evaluate the applicability of this method, sample #0844 was specially
prepared for this determination: it was spiked with Dibenzothiophene (1.23 mg
Sulphur/kg). Sample #0845 should be used as blank. On the report form it was
requested to determine the Sulphur content according this draft method and
also according the usually used test method.
For sample #0844 the determination of Sulphur according the usually used test
method is problematic. Although all results are within the reproducibility limits,
the calculated reproducibility is not in agreement with the requirements of ASTM
D5453:08b. For sample #0845 no suitable conclusions can be made as the
consensus value found is below or near the detection limit of the method.
The average recovery of the Sulphur (calculated from the difference between
the consensus value for the original sample #0844 and the spiked sample
Methanol: iis08C06X
page 9 of 69
#0845) and the theoretical increment of 1.23 mg S/kg is unsatisfactory (71%).

The individual recoveries vary over a large range.
Regretfully, only six participants reported results for the draft method
IMPCA005:08, of which three less than results. Therefore it was not possible to
draw any significant conclusions, except for the fact that the mean from the
three numerical results for sample #0844 is the same as the amount of Sulphur
spiked to this sample.
Total Iron:
This determination may be problematic. Nine results are outside the

reproducibility limits. The calculated reproducibility is, after rejection of the
statistical outliers not at all in agreement with the requirements of ASTM
E394:04. However, the consensus value is closed to the detection limit of the
determination.
Water (coul.):
This determination is problematic. Seven results were outside the reproducibility

limits. The calculated reproducibility is, even after rejection of the statistical
outliers, not at all in agreement with the strict requirements of ASTM E1064:05.
Water (titr.):
This determination is not problematic. No results were outside the

reproducibility limits. The calculated reproducibility is, after rejection of the
statistical outlier, in agreement with the requirements of ASTM E203:01.
These determinations are very problematic as the group is

Purity as is and on db:
trimodally divided. This phenomenon can be easily explained as many
participants did not detect the presence of Toluene (0.1%) in sample #0844
(group3 in the Kernel Density plot or results above 99.95%M/M). Toluene was
added during the spiking of Sulphur to this sample. The run time of the GC
method IMPCA001 is obviously too short. The run is stopped just before the
elution of toluene. Other participants that did not follow IMPCA001 detected
Toluene (group2 in the Kernel density plot or results around 99.86%M/M). Not
all participants that detected Toluene used the true response factor, thus
resulting in a very low purity (group1 in the Kernel density plot or results around
99.64%M/M).
Benzene:
This determination is somewhat problematic. Although, no results were outside

the reproducibility limits, the calculated reproducibility is not in agreement with
the strict estimated reproducibility limits calculated using the Horwitz equation.
The average recovery of the Benzene and the theoretical increment of 10.4 mg
Benzene/kg may be satisfactory (the actual blank Benzene content is
unknown).
Ethanol:
This determination is problematic. For both samples in total eight results were
outside the estimated reproducibility limits calculated using the Horwitz
equation. Both the calculated reproducibilities are, after rejection of the
statistical outliers, not at all in agreement with the estimated reproducibility
page 10 of 69
Methanol: iis08C06X
limits calculated using the Horwitz equation. The concentrations found for both
samples differ not significantly, which was expected as this component was not
spiked. The fact that the ratio R/r is almost 3, suggests that random and
systematic errors are both equally present.
Acetone:
For both samples, no significant conclusions can be drawn as only resp. eight
and nine numerical results were reported and the averages found are both
below the detection limit of the method.
TMA:
Only four participants reported a numerical result for this determination.

Therefore no meaningful conclusions could be drawn.
UV-Absorbance: For this determination sample #0845 was spiked with 10 mg Benzene/kg to get
a positive result on UV-absorbance. Although it was not requested to report it, it
was noticed that participants used a 10mm or a 50mm cuvet for this
determination, which are both allowed in IMPCA004:05. As the results of the
determinations for 268.5nm, 250nm and 220nm are divided into two groups, the
results per determination were split and evaluated separately.
Almost all UV absorbance determinations were very problematic. Only the
calculated reproducibilities for UV at 300nm and 220nm using a 50mm cuvet
were in agreement with the requirements of IMPCA004:06. All other calculated
reproducibilities were, even after rejection for the statistical outliers, not at all in
agreement with IMPCA004:06.
4.2
PERFORMANCE EVALUATION FOR THE GROUP OF LABORATORIES

A comparison has been made between the reproducibility as declared by the relevant standard
and the reproducibility as found for the group of participating laboratories. The average results
per sample, calculated reproducibilities and reproducibilities derived from literature standards (in
casu ASTM standards) are compared in the next tables.
Methanol: iis08C06X
page 11 of 69
Parameter
unit
average
2.8 * sd
R (lit)
Acidity as acetic acid
mg/kg
51
11.65
8.11
14.00
Anorganic Chloride as Cl, #0844
mg/kg
16
0.09
0.18
0.30
Anorganic Chloride as Cl, #0845
mg/kg
26
0.63
0.36
0.30
Carbonisable Substances
Pt/Co
31
6.9
6.1
5.0
Colour
Pt/Co
36
2.3
4.1
7.0
kg/L
51
0.79133
0.00031
0.00050
Initial Boiling Point (automatic)
24
64.36
0.61
1.00
Dry Point (automatic)
23
64.77
0.56
0.69
Initial Boiling Point (manual)
20
64.37
0.24
0.69
Dry Point (manual)
19
64.84
0.49
0.84
Nonvolatile Matter
mg/100 mL
29
0.51
1.34
2.40
minutes
46
98.6
51.2
unknown
Specific Gravity 20/20 C
44
0.79273
0.00031
0.00050
Apparent Spec.Grav.20/20 C
17
0.79248
0.00028
0.00050
Density @ 20 C
Permanganate Time Test
Sulphur (D5354), #0844
mg/kg
22
1.03
0.71
0.59
Sulphur (IMPCA005), #0844
mg/kg
1.21
0.78
unknown
Total Iron on sample as Fe, #0844
mg/kg
17
0.0133
0.0226
0.0072
Water (coulometric)
mg/kg
39
191.3
53.6
32.7
Water (titrimetric)
mg/kg
29
198.9
94.3
270.0
Purity
%M/M
unknown *)
Purity on dry basis
%M/M
unknown *)
Benzene, #0845
mg/kg
19
9.80
3.82
3.11
Ethanol, #0844
mg/kg
38
11.61
5.30
3.59
Ethanol, #0845
mg/kg
37
11.65
5.88
3.61
UV absorbance at 300 nm (50 mm cuvet)
17
0.0076
0.0097
0.0114
UV absorbance at 268.5 nm (50 mm cuvet)
15
0.0329
0.0135
0.0089
16
0.1640
0.0403
0.0166
17
1.1532
0.2218
0.3310
10
0.0015
0.0034
0.0023
UV absorbance at 268.5 nm (10 mm cuvet)
11
0.0059
0.0091
0.0016
11
0.0300
0.0163
0.0030
11
0.2337
0.0463
0.0671
table 5: Reproducibilities for sample #0844 and #0845

*) No reproducibility limits be determined, as results are trimodally divided
Without further statistical calculations it can be concluded that for many tests there is a good
compliance of the group of participating laboratories with the relevant standards. The tests that
are problematic have been discussed in paragraph 4.1.
page 12 of 69
Methanol: iis08C06X
4.3
COMPARISON OF THE PROFICIENCY TEST OF SEPTEMBER 2008 WITH PREVIOUS PTS

September
2008
September
2007
September
2006
September
2005
Number of reporting labs
60
48
45
43
Number of results reported
748
619
685
593
Statistical outliers
24
28
40
36
Percentage outliers
3.2 %
4.5 %
5.8 %
6.1 %
table 6: comparison with previous proficiency tests.
In proficiency tests, outlier percentages of 3% - 7.5% are quite normal.

The performance of the determinations of the proficiency tests was compared against the
requirements of the respective standards. The conclusions are given the following table:
Determination
September
2008
September
2007
September
2006
September
2005
++
++
++
++
Acidity as acetic acid

Chloride as Cl
++
++
++
++
Carbonisable Substances
--
--
+/-
--
Colour
++
++
++
++
Density @ 20 C
++
++
++
++
Distillation (automatic)
++
++
++
++
Distillation (manual)
++
++
++
++
Nonvolatile Matter
++
++
++
++
Permanganate Time Test
n.e.
n.e.
--
--
Specific Gravity 20/20 C
++
++
++
++
Sulphur
--
n.e.
n.e.
--
Total Iron
--
++
--
Water (coulometric)
--
--
--
--
Water (titrimetric)
++
++
++
++
Benzene
--
n.d.
n.d.
n.d.
--
n.e.
--
Acetone
n.e.
n.e.
n.e.
--
--
Ethanol
--
--
--
UV absorbance 300nm
--
n.e.
n.e.
n.e.
UV absorbance 268.5 nm
--
--
n.e.
n.e.
n.e.
UV absorbance 250 nm
--
--
n.e.
n.e.
n.e.
UV absorbance 220 nm
++
++
n.e.
n.e.
n.e.
--
++
table 7: comparison determinations against the standard requirements
The performance of the determinations against the requirements of the respective standards is
listed in the above table. The following performance categories were used:
++:
group performed much better than the standard
+ :
group performed better than the standard
+/-:
group performance equals the standard
- :
group performed worse than the standard
-- :
group performed much worse than the standard
n.e.: not evaluated
Methanol: iis08C06X
page 13 of 69
-- empty page --
page 14 of 69
Methanol: iis08C06X
APPENDIX 1
Determination of Appearance on sample #0844;
lab
52
150
153
171
174
273
311
319
323
332
333
334
342
343
345
346
347
357
372
395
443
444
445
446
468
494
528
529
608
609
646
657
663
786
823
824
825
857
858
859
862
864
867
902
963
971
974
1004
1007
1009
1010
1016
1029
1041
1102
1108
1149
1204
1510
1615
1712
1728
1905
1931
method
IMPCA003
visual
IMPCA003
IMPCA003
visual
IMPCA003
IMPCA003
IMPCA003
visual
IMPCA003
visual
IMPCA003
IMPCA003
IMPCA003
IMPCA003
IMPCA003
visual
IMPCA003
visual
IMPCA003
visual
visual
visual
visual
IMPCA003
IMPCA003
IMPCA003
visual
IMPCA003
IMPCA003
IMPCA003
IMPCA003
IMPCA003
IMPCA003
IMPCA003
IMPCA003
IMPCA003
IMPCA003
IMPCA003
IMPCA003
in house
IMPCA003
IMPCA003
visual
IMPCA003
IMPCA003
IMPCA003
visual
IMPCA003
visual
in house
normality
n
outliers
mean (n)
st.dev. (n)
R(calc.)
R(IMPCA003:98)
Methanol: iis08C06X
value
mark
CFSM
B&C
----C&F
C&F
B&C
C&F
CFSM
CFFMS
------------CFFSM
----CFSM
----CFSM
CFSM
CFSM
CFSM
CFSM
pass
B&C
pass
CFFMIS
B&C
CFSM
CFSM
CFSM
CFSM
CFFSM
CFSM
B&C
----CFSM
CFSM
CFSM
CFFSM
CFFSM
CFFSM
CFFSM
CFFSM
CFSM
----CFFSM
CFSM
CFFSM
clear
pass
CFSM
CFSM
----clear
CFSM
CFSM
--------CSF
CBFFSM
C&C
----clear
NOSMS
----n.a
51
0
n.a.
n.a.
n.a.
n.a.
z(targ) remarks
----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------Abbreviations:
CFSM
B&C/C&F/C&C
CFFMS/SM/MIS
CBFFSM
CSF
NOSMS
Clear Free of Suspended Matter

Bright&Clear / Clear&Free / Clear&Colourless
Clear Free From Suspended Matter
Clear Bright Free From Suspended Matter
Clear with Suspended Fiber
No Opalescence, Suspended Matter
page 15 of 69
Determination of Acidity as Acetic Acid on sample #0844; results in mg/kg

lab
52
150
153
171
174
273
311
319
323
332
333
334
342
343
345
346
347
357
372
395
443
444
445
446
468
494
528
529
608
609
646
657
663
786
823
824
825
857
858
859
862
864
867
902
963
971
974
1004
1007
1009
1010
1016
1029
1041
1102
1108
1149
1204
1510
1615
1712
1728
1905
1931
method
D1613
D1613
D1613
D1613
D1613
D1613
D1613
D1613
D1613
D1613
D1613
D1613
D1613
D1613
D1613
D1613
value
15
9.1
27
11.3
10.9
12
12
9
14
------------13.7
----16
----10.1
9
12
10.6
----12.2
----13
12.13
5
15.1677
16.679
10.25
9.09
13.6
15
12.11
----11
11
12
11
11
10.6
11
11.6
8.8
----8.02
----17.98
12
12
17
9
12.49
8.3
11
9.85
--------8.713
8
7.50
15
20
11.9
8.4
normality
n
outliers
mean (n)
st.dev. (n)
R(calc.)
R(D1613:06)
not OK
51
1
11.65
2.898
8.11
14.00
D1613
D1613
D1613
D1613
D1613
D1613
D1613
E346
D1613
D1613
D1613
D1613
D1613
D1613
D1613
D1613
D1613
D1613
D1613
D1613
D1613
D1613
D1613
D1613
D1613
D1613
D1613
D1613
D1613
in house
D1613
D1613
D1613
D1613
D1613
D1613
page 16 of 69
mark
z(targ)
0.67
-0.51
U,G(0.01)
3.07
-0.07
-0.15
0.07
0.07
-0.53
0.47
------------0.41
----0.87
-----0.31
-0.53
0.07
-0.21
----0.11
----0.27
0.10
-1.33
0.70
1.01
-0.28
-0.51
0.39
C
0.67
0.09
-----0.13
-0.13
C
0.07
-0.13
-0.13
-0.21
-0.13
-0.01
-0.57
-----0.73
----1.27
0.07
0.07
1.07
-0.53
0.17
-0.67
-0.13
-0.36
---------0.59
-0.73
-0.83
U
0.67
1.67
0.05
-0.65
remarks
Reported 0.0027
First reported 19
First reported 21
Reported 0.0015
Methanol: iis08C06X
494
0
10
Methanol: iis08C06X
0.16
20
30
0.14
Kernel Density
0.12
0.1
0.08
0.06
0.04
0.02
0
40
page 17 of 69
153
1728
974
1009
529
345
528
1712
52
657
323
342
646
446
1016
444
468
663
372
825
1004
1007
311
273
1905
864
171
1041
857
858
824
823
862
174
395
859
608
347
1102
150
609
319
1010
357
867
1204
1931
1029
963
1510
1615

30
25
20
15
10
Determination of Anorganic Chloride as Cl on sample #0844 and sample #0845; results in mg/kg
lab
52
150
153
171
174
273
311
319
323
332
333
334
342
343
345
346
347
357
372
395
443
444
445
446
468
494
528
529
608
609
646
657
663
786
823
824
825
857
858
859
862
864
867
902
963
971
974
1004
1007
1009
1010
1016
1029
1041
1102
1108
1149
1204
1510
1615
1712
1728
1905
1931
method
IMPCA002
IMPCA002
IMPCA002
IMPCA002
IMPCA002
IMPCA002
IMPCA002
IMPCA002
IMPCA002
IMPCA002
IMPCA002
in house
IMPCA002
IMPCA002
IMPCA002
in house
Turbidimetric
IMPCA002
IMPCA002
inh-005
IMPCA002
IMPCA002
Turbidity meter
IMPCA002
IMPCA002
IMPCA002
IMPCA002
IMPCA002
IMPCA002
in house
in house
in house
Turbidity meter
IMPCA002
IMPCA002
IMPCA002
in house
normality
n
outliers
mean (n)
st.dev. (n)
R(calc.)
R(IMPCA002:98)
page 18 of 69
#0844
0.2
<0.3
----<0.1
0.11
----<0.25
0.07
<0.25
--------0.14
----0.26
------------<0.25
<0.25
0.05
<0.20
<0.1
------------<0.25
0.031677
----<0.1
<0.1
0.14
<1
<0.25
----<0.25
0.1
<0.1
0.06
----0.05
0.06
<0.25
<0.25
----------------0.009
0.05
0.069
<0.25
----<0.10
----0.06
----------------n.d.
----0.468
--------not OK
16
1
0.09
0.066
0.18
0.30
mark
C
G(0.01)
z(targ)
1.02
------------0.18
---------0.20
------------0.46
----1.58
---------------------0.38
-------------------------0.56
------------0.46
----------------0.08
-----0.29
-----0.38
-0.29
-------------------------0.77
-0.38
-0.21
-----------------0.29
------------------------3.52
---------
#0845
0.9
0.6
----0.88
0.89
----0.64
0.69
1.0
----------------0.76
------------0.6
0.65
0.49
----0.58
------------0.60
--------0.57
0.544
0.64
<1
--------0.61
----0.68
0.58
----0.61
0.62
0.64
0.655
--------------------0.11
0.62
>0.25
----0.5723
------------------------0.408
----0.320
--------not OK
26
2
0.63
0.129
0.36
0.30
mark
G(0.05)
G(0.05)
Spike
0.52
z(targ) Recov % remarks

2.53
156 First reported 0.4
-0.27
98
----2.34
152
2.44
154
----0.10
106
0.57
115
3.46
----------------1.22
129
-------------0.27
98
0.20
108
-1.30
77
-----0.46
94
-------------0.27
98
---------0.55
92
-0.79
0.10
106
<3.46
---------0.18
100
----0.48
113
-0.46
94
-----0.18
100
-0.08
102
0.10
106
0.24
109
---------------------4.84
4
-0.08
102
---------0.53
93
-------------------------2.06
61
-----2.88
<0
---------
(0.63-0.09) / 0.52 * 100 = 104%
Methanol: iis08C06X
0.5
Anorganic Chloride as Cl on #0844
0.45
0.4
0.35
0.3
0.25
0.2
0.15
0.1
0.05
1.2
1728
343
52
646
334
174
824
319
1009
1102
857
862
1007
859
395
1004
528
Anorganic Chloride as Cl on #0845
0.8
0.6
0.4
0.2
323
52
174
171
343
319
825
Kernel Density
#0845
867
372
311
864
646
1009
862
859
3.5
Kernel Density
#0844
823
357
150
494
444
857
1029
608
609
395
1615
1728
1007
2.5
4
1.5
0.5
1
0
-0.2
Methanol: iis08C06X
0.2
0.4
0.6
0.8
0
-0.5
0.5
1.5
page 19 of 69
Determination of Carbonisable Substances Pt/Co on sample #0844;

lab
52
150
153
171
174
273
311
319
323
332
333
334
342
343
345
346
347
357
372
395
443
444
445
446
468
494
528
529
608
609
646
657
663
786
823
824
825
857
858
859
862
864
867
902
963
971
974
1004
1007
1009
1010
1016
1029
1041
1102
1108
1149
1204
1510
1615
1712
1728
1905
1931
method
E346
E346
E346
E346
E346
E346
E346
E346
E346
E346
E346
E346
E346
E346
E346
E346
E346
E346
E346
E346
E346
E346
E346
E346
E346
E346
E346
E346
E346
in house
E346
E346
E346
E346
E346
E346
E346
E346
normality
n
outliers
mean (n)
st.dev. (n)
R(calc.)
R(E346:03e1)
page 20 of 69
value
10
8
5
5
5.5
----5
<5
5
----10
------------------------5
7
10
----10
----10
----<0.1
20
----<5
6.6
7
10
--------5
5
----5
5
7
6
<10
5
----------------<5
10
<30
5
----10
5
------------5
----10
----5
7.5
-----
mark
G(0.01)
z(targ) remarks
1.72
0.60
-1.08
-1.08
-0.80
-----1.08
<-1.08
-1.08
----1.72
-------------------------1.08
0.04
1.72
----1.72
----1.72
--------- Deviating unit reported??
7.32
----<-1.08
-0.18
0.04
1.72
---------1.08
-1.08
-----1.08
-1.08
0.04
-0.52
<1.72
-1.08
----------------<-1.08
1.72
-----1.08
----1.72
-1.08
-------------1.08
----1.72 First reported 1
-----1.08
0.32
-----
not OK
31
1
6.9
2.17
6.1
5.0
Methanol: iis08C06X
25
20
15
10
0.18
528
395
1007
444
657
446
1615
52
333
1029
150
646
1905
372
859
609
862
174
311
323
153
1204
1728
171
1041
857
824
823
858
357
1010
867
Kernel Density
0.16
0.14
0.12
0.1
0.08
0.06
0.04
0.02
0
0
Methanol: iis08C06X
10
20
30
page 21 of 69
Determination of Colour as Pt/Co on sample #0844;

lab
52
150
153
171
174
273
311
319
323
332
333
334
342
343
345
346
347
357
372
395
443
444
445
446
468
494
528
529
608
609
646
657
663
786
823
824
825
857
858
859
862
864
867
902
963
971
974
1004
1007
1009
1010
1016
1029
1041
1102
1108
1149
1204
1510
1615
1712
1728
1905
1931
method
D1209
D1209
D1209
D1209
D1209
D1209
D1209
D1209
D1209
D1209
D1209
D1209
value
<5
1
<2
1
1.1
5
<5
2
<5
--------1
3
----<5
----2
<5
2
<5
<5
2
<5
<5
<5
0
1.5
1.5
<5
2.0
3
5
0
----<3
1
3
5
2
2
2
<5
3
----4
----<5
5
5
<5
<5
3.35
1
<5
----4
----1
1
1
----2
2.5
1
normality
n
outliers
mean (n)
st.dev. (n)
R(calc.)
R(D1209:05e1)
not OK
36
0
2.3
1.46
4.1
7.0
D1209
D1209
D1209
D1209
D1209
D1209
D1209
D1209
D5386
D1209
D1209
D1209
D1209
D1209
D1209
D1209
D1209
D1209
D1209
D1209
D1209
D1209
D1209
D1209
D1209
D1209
D1209
D1209
D1209
D1209
D1209
D1209
in house
D1209
D1209
D1209
D1209
ISO6271
D1209
D1209
D1209
D1209
page 22 of 69
mark
z(targ) Remarks
-----0.51
-----0.51
-0.47
1.09
-----0.11
-------------0.51
0.29
-------------0.11
-----0.11
---------0.11
-------------0.91
-0.31
-0.31
-----0.11
0.29
1.09
-0.91
---------0.51
0.29
1.09
-0.11
-0.11
-0.11
----0.29
----0.69
--------1.09
1.09
--------0.43
-0.51
--------0.69
-----0.51
-0.51
-0.51
-----0.11
0.09
-0.51
Methanol: iis08C06X
20
18
16
14
12
10
8
6
4
2
0.35
1004
273
1007
857
657
963
1108
867
1016
342
825
646
372
1905
609
444
347
862
319
859
858
529
1728
528
174
150
334
171
1510
1204
1931
824
1615
1029
494
663
Kernel Density
0.3
0.25
0.2
0.15
0.1
0.05
0
-4
-2
Methanol: iis08C06X
page 23 of 69
Determination of Density at 20 oC on sample #0844; results in kg/L

lab
52
150
153
171
174
273
311
319
323
332
333
334
342
343
345
346
347
357
372
395
443
444
445
446
468
494
528
529
608
609
646
657
663
786
823
824
825
857
858
859
862
864
867
902
963
971
974
1004
1007
1009
1010
1016
1029
1041
1102
1108
1149
1204
1510
1615
1712
1728
1905
1931
method
D4052
D4052
D4052
D4052
D4052
D4052
D4052
D4052
IP365
D4052
D4052
D4052
D4052
D4052
value
0.7914
0.7911
0.7955
0.7913
0.7914
0.7915
0.7914
----0.7913
----0.7914
0.7916
0.7911
--------0.7913
0.7913
0.7912
0.7913
0.7913
----0.7914
0.7913
0.7913
0.7913
0.791
0.79131
0.7914
0.79133
0.79128
----0.7914
0.7914
----0.7914
0.7914
0.7913
0.79134
0.79132
0.79132
0.7913
0.79131
0.79138
----0.7913
0.7913
0.7913
----0.79139
----0.7912
----0.79126
0.79132
0.7912
0.79133
----0.7914
0.7915
0.79124
0.79133
0.7913
0.79128
0.7917
normality
n
outliers
mean (n)
st.dev. (n)
R(calc.)
R(D4052:02e1)
not OK
51
1
0.79133
0.000112
0.00031
0.00050
D4052
D4052
D4052
D4052
D1298
D4052
D4052
D4052
D4052
D4052
D4052
D4052
D4052
D4052
D4052
D4052
D4052
D4052
D4052
D4052
D4052
D4052
D4052
D4052
D4052
D4052
D4052
D4052
D4052
D4052
D4052
D4052
in house
D4052
D4052
D4052
D4052
D4052
page 24 of 69
mark
G(0.01)
z(targ) remarks
0.40
-1.28
23.36
-0.16
0.40
0.96
0.40
-----0.16
----0.40
1.52
-1.28
---------0.16
-0.16
-0.72
-0.16
-0.16
----0.40
-0.16
-0.16
-0.16
-1.84
-0.10
0.40
0.01
-0.27
----0.40
0.40
----0.40
0.40
-0.16
0.07
-0.05
-0.05
-0.16
-0.10
0.29
-----0.16
-0.16
-0.16
----0.35
-----0.72
-----0.38
-0.05
-0.72
0.01
----0.40
0.96
-0.49
0.01 Reported 791.33
-0.16
-0.27
2.08
Methanol: iis08C06X
0.793
0.7925
0.792
0.7915
0.791
0.7905
6000
Kernel Density
5000
4000
3000
2000
1000
0
0.7905
0.791
Methanol: iis08C06X
0.7915
0.792
0.7925
0.793
page 25 of 69
153
334
1931
273
1510
824
529
657
823
663
52
174
311
444
333
1204
867
1007
857
1712
608
1108
859
1041
858
864
528
372
395
347
171
346
1728
323
445
974
825
862
963
446
468
971
609
1905
1029
357
1615
1102
150
1010
342
494
0.79
Determination of IBP and DP (automated) @ 760 mmHg on sample #0844; results in C

lab
52
150
153
171
174
273
311
319
323
332
333
334
342
343
345
346
347
357
372
395
443
444
445
446
468
494
528
529
608
609
646
657
663
786
823
824
825
857
858
859
862
864
867
902
963
971
974
1004
1007
1009
1010
1016
1029
1041
1102
1108
1149
1204
1510
1615
1712
1728
1905
1931
method
D1078
D1078
D1078
D1078
D1078
D1078
D1078
D1078
D1078
D1078
D1078
D1078
D1078
D1078
D1078
in house
D1078
D1078
D1078
D1078
D1078
D1078
D1078
D1078
normality
n
outliers
mean (n)
st.dev. (n)
R(calc.)
R(D1078:05-A)
page 26 of 69
IBP
64.3
64.4
----------------64.5
------------64.6
64.5
--------64.5
----64.4
64.5
64.4
----------------64.5
64.3
63.8
--------------------------------64.4
64.5
64.4
--------------------------------------------64.7
64.2
64.5
----64.4
----64.4
63.8
--------64.4
64.1
--------64.2
----not OK
24
0
64.36
0.216
0.61
1.00
mark
z(targ)
-0.17
0.10
----------------0.38
------------0.66
0.38
--------0.38
----0.10
0.38
0.10
----------------0.38
-0.17
-1.57
--------------------------------0.10
0.38
0.10
--------------------------------------------0.94
-0.45
0.38
----0.10
----0.10
-1.57
--------0.10
-0.73
---------0.45
-----
DP
64.6
64.8
----------------64.7
------------64.8
64.1
--------64.8
----64.8
64.8
64.8
----------------64.9
64.8
64.3
--------------------------------64.8
65.0
65.0
--------------------------------------------65.3
64.6
64.8
----64.8
----64.8
64.4
--------64.7
64.6
--------64.9
-----
mark
ex
z(targ)
-0.70
0.11
-----------------0.30
------------0.11
-2.72
--------0.11
----0.11
0.11
0.11
----------------0.51
0.11
-1.91
--------------------------------0.11
0.91
0.91
--------------------------------------------2.13
-0.70
0.11
----0.11
----0.11
-1.51
---------0.30
-0.70
--------0.51
-----
remarks
See paragraph 4.1

Result DP excluded as DP < IBP
See paragraph 4.1
See paragraph 4.1
See paragraph 4.1
not OK
23
0
64.77
0.200
0.56
0.69
Methanol: iis08C06X
65.5
Initial Boiling Point

65
64.5
64
63.5
372
347
150
345
311
334
357
347
357
345
333
150
372
468
1007
1029
1010
1007
1102
1029
333
1510
1102
825
825
823
1010
823
311
824
52
1510
824
468
1615
446
1905
1009
446
1009
52
1905
1615
1108
1108
494
63
66
65.5
Dry Point
65
64.5
64
63.5
494
334
63
3.5
Kernel Density
IBP
2.5
Kernel Density
DP
3
2.5
2
1.5
1.5
1
0.5
0
63.5
0.5
64
Methanol: iis08C06X
64.5
65
65.5
66
0
63.5
64
64.5
65
65.5
66
page 27 of 69
Determination of IBP and DP (manual) @ 760 mmHg on sample #0844; results in C

lab
52
150
153
171
174
273
311
319
323
332
333
334
342
343
345
346
347
357
372
395
443
444
445
446
468
494
528
529
608
609
646
657
663
786
823
824
825
857
858
859
862
864
867
902
963
971
974
1004
1007
1009
1010
1016
1029
1041
1102
1108
1149
1204
1510
1615
1712
1728
1905
1931
method
D1078
D1078
D1078
D1078
D1078
D1078
D1078
D1078
D1078
D1078
D1078
D1078
D1078
D1078
D1078
D1078
D1078
D1078
D1078
D1078
D1078
normality
n
outliers
mean (n)
st.dev. (n)
R(calc.)
R(D1078:05-M)
page 28 of 69
IBP
--------------------64.3
----64.6
----------------64.4
------------------------64.4
----64.3
64.4
------------64.4
--------64.4
64.38
64.2
--------------------64.3
64.3
64.4
64.4
64.4
64.3
----64.3
----54.4
64.3
------------------------------------64.39
------------64.5
--------not OK
20
1
64.37
0.086
0.24
0.69
mark
z(targ)
---------------------0.28
----0.94
----------------0.13
------------------------0.13
-----0.28
0.13
------------0.13
--------0.13
0.05
-0.69
---------------------0.28
-0.28
0.13
0.13
0.13
-0.28
-----0.28
----C,G(0.01) -40.53
-0.28
------------------------------------0.09
------------0.53
---------
DP
--------------------65.0
----65.0
----------------64.8
------------------------64.8
----64.6
64.8
------------65.2
--------64.9
64.57
64.8
--------------------64.7
64.7
64.8
64.7
64.8
64.8
----65.6
----65.6
64.8
------------------------------------65.22
------------65.0
---------
mark
z(targ)
--------------------0.53
----0.53
-----------------0.14
-------------------------0.14
-----0.80
-0.14
------------1.19
--------0.19
-0.90
-0.14
---------------------0.47
-0.47
-0.14
-0.47
-0.14
-0.14
----DG(0.01)
2.52
----C,DG(0.01)
2.52
-0.14
------------------------------------C
1.26
------------0.53
---------
remarks
See paragraph 4.1
First reported 63.8 and 70.0
First reported 65.89
not OK
19
2
64.84
0.176
0.49
0.84
Methanol: iis08C06X
65.5
Initial Boiling Point

65
64.5
64
63.5
319
963
609
319
1728
528
1728
974
342
609
859
395
657
1204
864
445
862
1204
395
528
646
867
445
444
1004
273
273
963
859
864
1004
858
867
857
862
342
858
857
657
974
63
66
Dry Point
65.5
65
64.5
64
63.5
444
646
63
2.5
Kernel Density
IBP
Kernel Density
DP
4
1.5
3
1
2
0.5
1
0
63.5
64
Methanol: iis08C06X
64.5
65
65.5
66
0
63.5
64
64.5
65
65.5
66
page 29 of 69
-- empty page --
page 30 of 69
Methanol: iis08C06X
Determination of Water Miscibility on sample #0844;

lab
52
150
153
171
174
273
311
319
323
332
333
334
342
343
345
346
347
357
372
395
443
444
445
446
468
494
528
529
608
609
646
657
663
786
823
824
825
857
858
859
862
864
867
902
963
971
974
1004
1007
1009
1010
1016
1029
1041
1102
1108
1149
1204
1510
1615
1712
1728
1905
1931
method
D1722
D1722
D1722
D1722
D1722
D1722
D1722
D1722
D1722
D1722
D1722
D1722
D1722
D1722
D1722
D1722
D1722
D1722
D1722
E346
D1722
D1722
D1722
D1722
D1722
D1722
D1722
D1722
D1722
D1722
D1722
D1722
D1722
D1722
D1722
D1722
D1722
D1722
D1722
in house
D1722
D1722
D1722
D1722
D1722
D1722
D1722
D1722
D1722
D1722
normality
n
outliers
mean (n)
st.dev. (n)
R(calc.)
R(D1722:04)
Methanol: iis08C06X
value
pass
pass
pass
pass
pass
pass
pass
--------------------pass
----pass
----pass
pass
pass
pass
pass
pass
pass
pass
pass
pass
pass
pass
pass
pass
pass
pass
pass
----pass
pass
pass
pass
pass
pass
pass
pass
pass
----pass
pass
pass
pass
pass
pass
pass
pass
pass
pass
------------pass
pass
pass
----complete
pass
-----
mark
z(targ) remarks
-----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
n.a.
50
0
n.a.
n.a.
n.a.
n.a.
page 31 of 69
Determination of Nonvolatile Matter on sample #0844; results in mg/100 mL

lab
52
150
153
171
174
273
311
319
323
332
333
334
342
343
345
346
347
357
372
395
443
444
445
446
468
494
528
529
608
609
646
657
663
786
823
824
825
857
858
859
862
864
867
902
963
971
974
1004
1007
1009
1010
1016
1029
1041
1102
1108
1149
1204
1510
1615
1712
1728
1905
1931
method
D1353
D1353
D1353
D1353
D1353
D1353
D1353
D1353
D1353
D1353
D1353
D1353
D1353
D1353
D1353
D1353
D1353
D1353
D1353
D1353
D1353
D1353
D1353
D1353
D1353
D1353
D1353
D1353
D1353
in house
D1353
D1353
D1353
D1353
D1353
D1353
D1353
D1353
D1353
D1353
normality
n
outliers
mean (n)
st.dev. (n)
R(calc.)
R(D1353:03)
page 32 of 69
value
0
0.2
0.000
0.2
0.32
<1
<1
1.43
--------0.7
--------2.0
1.1
--------<1
0.3
0.2
----0.97
----<1
0.2
----5
--------0.2
1
0.2
----------------0.2
0.4
0.3
0.4
0.3
0.3
0.3
----------------1.5
0.1
<1
<0.8
<1
0.2
<1
------------0.10
0.33
0.6
----0.2
0.55
-----
mark
ex
z(targ)
-0.60
-0.36
ex
-0.60
-0.36
-0.22
--------1.07
--------C
0.22
--------C
1.74
0.69
-------------0.25
-0.36
----0.54
----C
-----0.36
----U,G(0.01)
5.24
---------0.36
0.57
-0.36
-----------------0.36
-0.13
-0.25
-0.13
-0.25
-0.25
-0.25
----------------1.15
-0.48
--------U
-----0.36
-----------------0.48
-0.21
0.10
-----0.36
0.05
-----
remarks
Not a real result
Not a real result
First reported 9
First reported 2.7
First reported <0.001

Reported 0.005, probably different unit (%wt instead of mg/100mL)
Reported <0.001, probably different unit (%wt instead of mg/100mL)
not OK
29
3
0.51
0.478
1.34
2.40
Methanol: iis08C06X
1.6
528
343
1004
319
345
646
444
333
1615
1905
857
859
1510
174
867
372
864
862
858
150
171
1728
657
825
1029
468
395
609
1007
1204
52
153
Kernel Density
1.4
1.2
1
0.8
0.6
0.4
0.2
0
-2
Methanol: iis08C06X
page 33 of 69
Determination of Permanganate Time Test @ 15C on sample #0844; results in minutes

lab
52
150
153
171
174
273
311
319
323
332
333
334
342
343
345
346
347
357
372
395
443
444
445
446
468
494
528
529
608
609
646
657
663
786
823
824
825
857
858
859
862
864
867
902
963
971
974
1004
1007
1009
1010
1016
1029
1041
1102
1108
1149
1204
1510
1615
1712
1728
1905
1931
method
D1363
D1363
D1363
D1363
D1363
D1363
D1363
D1363mod.
D1363
D1363
D1363
D1363
D1363
D1363
D1363
D1363
D1363
D1363
D1363
D1363
D1363
D1363
D1363
D1363
D1363
D1363
D1363
D1363
D1363
D1363
D1363
D1363
D1363
D1363
D1363
D1363
in house
D1363
D1363
D1363
D1363
D1363
D1363
D1363
D1363
D1363
D1363
normality
n
outliers
mean (n)
st.dev. (n)
R(calc.)
R(D1363:06)
page 34 of 69
value
67
125
----120
122
102
105
150
>100
------------94
----90
86
96
100
100
102
81
90
125
--------75
135
116
79
80
107
90
------------92
70
100
100
105
102
105
107
----75.0
----110
105
90
98
100
----100
127
60
--------104
----68
90
100
92
----OK
46
0
98.6
18.27
51.2
unknown
mark
z(targ) remarks
------------------------------------------------------------------------------------- First reported 61
----------------------------------------------------------------------------------------------------------------------------------------------------------------- First reported 135
-------------
Compare R(iis07C08) = 39.5 at a mean of 104.9
Methanol: iis08C06X
170
150
130
110
90
70
0.035
319
528
150
1041
445
174
171
529
974
867
646
864
859
311
1004
273
1204
395
862
357
372
1010
1029
857
1728
858
347
1009
342
824
1905
1007
657
1712
345
444
346
443
609
608
494
963
825
52
1615
1102
50
Kernel Density
0.03
0.025
0.02
0.015
0.01
0.005
0
0
50
Methanol: iis08C06X
100
150
200
page 35 of 69
Determination of Specific Gravity 20/20 C/C on sample #0844;

lab
52
150
153
171
174
273
311
319
323
332
333
334
342
343
345
346
347
357
372
395
443
444
445
446
468
494
528
529
608
609
646
657
663
786
823
824
825
857
858
859
862
864
867
902
963
971
974
1004
1007
1009
1010
1016
1029
1041
1102
1108
1149
1204
1510
1615
1712
1728
1905
1931
method
D4052
value
----0.7926
----0.7927
0.7928
0.7929
0.7928
0.79275
--------0.7928
----0.7925
----0.7924
----0.7927
0.7926
0.7927
0.7927
----0.7928
--------0.7927
0.7927
0.7927
0.7928
0.7927
0.7927
----0.7928
0.7928
----0.7928
0.7928
0.7928
0.7927
0.7927
0.7927
0.7927
0.79274
0.79281
----0.79272
0.7927
0.7927
0.7925
0.7928
0.7928
0.7927
----0.79269
----0.79263
--------0.7928
----0.7927
----0.79270
----0.7931
normality
n
outliers
mean (n)
st.dev. (n)
R(calc.)
R(D4052:02e1)
not OK
44
0
0.79273
0.000109
0.00031
0.00050
D4052
D4052
D4052
calc.
in house
D4052
in house
D4052
D4052
D4052
D4052
D4052
D4052
in house
in house
in house
D4052
D4052
D4052
D4052
D4052
D4052
D4052
D4052
D4052
in house
in house
D4052
D4052
D4052 calc.
D4052
D4052
in house
D4052
D891
in house
D4052
D4052
D4052
in house
D4052
in house
in house
page 36 of 69
mark
z(targ) remarks
-----0.71
-----0.15
0.41
0.97
0.41
0.13
--------0.41
-----1.27
-----1.83
-----0.15
-0.71
-0.15
-0.15
----0.41
---------0.15
-0.15
-0.15
0.41
-0.15
-0.15
----0.41
0.41
----0.41 First reported 0.17928
0.41
0.41
-0.15
-0.15
-0.15
-0.15
0.08
0.47
-----0.03
-0.15
-0.15
-1.27
0.41
0.41
-0.15
-----0.20
-----0.54
--------0.41
-----0.15
-----0.15
----2.09
Methanol: iis08C06X
0.7934
0.7932
0.793
0.7928
0.7926
0.7924
0.7922
5000
273
1931
867
823
663
825
824
657
311
174
333
529
444
1009
1204
319
1007
864
963
494
468
395
171
1728
372
1615
347
528
859
862
974
858
857
971
609
608
1010
1029
357
1102
150
342
1004
345
0.792
Kernel Density
4500
4000
3500
3000
2500
2000
1500
1000
500
0
0.792
0.7925
Methanol: iis08C06X
0.793
0.7935
page 37 of 69
Determination of Specific Gravity, Apparent 20/20 C/C on sample #0844;

lab
52
150
153
171
174
273
311
319
323
332
333
334
342
343
345
346
347
357
372
395
443
444
445
446
468
494
528
529
608
609
646
657
663
786
823
824
825
857
858
859
862
864
867
902
963
971
974
1004
1007
1009
1010
1016
1029
1041
1102
1108
1149
1204
1510
1615
1712
1728
1905
1931
method
in house
D4052
D4052
D4052
ih-960
D4052/891
D4052
D891
D4052
in house
in house
D891
D891
D4052 calc.
D4052
in house
in house
normality
n
outliers
mean (n)
st.dev. (n)
R(calc.)
R(D4052:02e1)
page 38 of 69
value
0.7925
--------0.79248
0.7926
----------------------------0.7923
----------------0.7925
0.7925
----------------------------0.79248
------------0.7922
0.7926
--------------------0.79245
0.79246
0.79246
0.7925
0.79249
0.79256
--------------------0.7926
------------------------------------------------0.79247
---------
mark
z(targ) remarks
0.12
--------0.00
0.68
-----------------------------1.00
----------------0.12
0.12
----------------------------0.00
-------------1.56
0.68
---------------------0.16
-0.11
-0.11
0.12
0.06
0.45
--------------------0.68
-------------------------------------------------0.05
---------
not OK
17
0
0.79248
0.000101
0.00028
0.00050
Methanol: iis08C06X
0.7931
0.7929
0.7927
0.7925
0.7923
0.7921
0.7919
0.7917
4500
657
174
1007
867
52
357
372
862
864
528
171
1728
858
859
857
342
646
0.7915
Kernel Density
4000
3500
3000
2500
2000
1500
1000
500
0
0.7918 0.792 0.7922 0.7924 0.7926 0.7928 0.793
Methanol: iis08C06X
page 39 of 69
Determination of Sulphur on sample #0844 and #0845; results in mg/kg

lab
52
150
153
171
174
273
311
319
323
332
333
334
342
343
345
346
347
357
372
395
443
444
445
446
468
494
528
529
608
609
646
657
663
786
823
824
825
857
858
859
862
864
867
902
963
971
974
1004
1007
1009
1010
1016
1029
1041
1102
1108
1149
1204
1510
1615
1712
1728
1905
1931
method
D5453
D5453
D5453
#0844
1.0
1
----1.4
--------1.1
----1.3
----1.3
1.3
----------------0.63
0.8
1.0
--------1.18
------------1.2
------------<0.5
----1.2
------------0.9
----------------1.1
----1.1
----------------------------<0.5
1.35
0.49
0.76
1.13
0.8
----------------<0.1
0.65
----<1.0
normality
n
outliers
mean (n)
st.dev. (n)
R(calc.)
R(D5453:08b)
OK
22
0
1.03
0.254
0.71
0.59
D5453
D5453
D5453
D5453
D5453
D5453
D5453
D5453
D5453
D5453
D3961
D5453
D5453
D5453
D5453
in house
ISO20846
D3961
D6212
D5453
D5453
in house
D5453
page 40 of 69
mark
Spike:
1.23
z(targ)
-0.15
-0.15
----1.74
--------0.32
----1.27
----1.27
1.27
-----------------1.90
-1.09
-0.15
--------0.70
------------0.80
------------<-2.52
----0.80
-------------0.62
----------------0.32
----0.32
----------------------------<-2.52
1.51
-2.56
-1.28
0.47
-1.09
----------------<-4.41
-1.80
----<-0.15
#0845
<1
0.1
----<1
--------<1
----<1
--------0.9
----------------<0.5
0.2
<0.5
--------0.23
------------<1
--------------------<1
------------<0.1
----------------<1
----<1
----------------------------<0.5
----0.04
<0.2
0.12
0.3
--------------------0.1
----<1.0
n.a.
7
1
0.16
n.a.
n.a.
unknown
mark
z(targ) Recovery %
----68
----68
--------101
------------76
--------93
--------93
G(0.01)
----93
--------------------38
----52
----68
------------83
----------------85
----------------<28
--------85
----------------60
--------------------76
--------76
--------------------------------<28
----97
----27
----49
----79
----52
--------------------<1
----40
--------<68
remarks
First reported 1.7
False negative
False negative
False negative
(1.03 0.16) / 1.23 * 100 = 71 %
Methanol: iis08C06X
1.8
1.6
1.4
1.2
1
0.8
0.6
0.4
0.2
1.6
171
1016
334
323
333
494
657
444
1102
311
867
862
150
52
372
824
1108
357
1041
1728
347
1029
Kernel Density
#0844
1.4
1.2
1
0.8
0.6
0.4
0.2
0
0
0.5
Methanol: iis08C06X
1.5
page 41 of 69
-- empty page --
page 42 of 69
Methanol: iis08C06X
Determination of Sulphur (IMPCA005) on sample #0844 and #0845; results in mg/kg

lab
52
150
153
171
174
273
311
319
323
332
333
334
342
343
345
346
347
357
372
395
443
444
445
446
468
494
528
529
608
609
646
657
663
786
823
824
825
857
858
859
862
864
867
902
963
971
974
1004
1007
1009
1010
1016
1029
1041
1102
1108
1149
1204
1510
1615
1712
1728
1905
1931
method
IMPCA005
IMPCA005
IMPCA005
D3961
IMPCA005
IMPCA005 mod.
normality
n
outliers
mean (n)
st.dev. (n)
R(calc.)
R(lit.)
Methanol: iis08C06X
#0844
------------------------1.2
--------------------------------------------------------------------------------------------0.94
<1
--------------------<1
----1.5
----------------------------<0.01
----------------------------------------------------------------n.a.
3
0
1.21
0.280.
0.78
unknown
mark
Spike:
1.23
z(targ)
-----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
#0845
------------------------<0.5
--------------------------------------------------------------------------------------------<0.2
<1
--------------------<1
----<0.5
----------------------------<0.01
-----------------------------------------------------------------
mark
z(targ) remarks
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------- False negative
-----------------------------------------------------------------
n.a.
0
0
n.a.
n.a.
n.a.
unknown
page 43 of 69
Determination of Total Iron as Fe on sample #0844; results in mg/kg

lab
52
150
153
171
174
273
311
319
323
332
333
334
342
343
345
346
347
357
372
395
443
444
445
446
468
494
528
529
608
609
646
657
663
786
823
824
825
857
858
859
862
864
867
902
963
971
974
1004
1007
1009
1010
1016
1029
1041
1102
1108
1149
1204
1510
1615
1712
1728
1905
1931
method
E394
E394
E394
E394
E394
E394
E394
E394
E394
E394
E394
E394
E394
E394
E394
E394
E394
E394
E394
E394
E394
E394
in house
in house
E394
E394
E394
E394
E394
E394
E394
E394
E394
normality
n
outliers
mean (n)
st.dev. (n)
R(calc.)
R(E394:04)
page 44 of 69
value
<0.02
<0.01
----<0.01
0.01
----<0.01
0.025
------------------------0.01
--------<0.01
0.013
<0.01
------------------------0.0064
--------0.01
<0.05
0.07
--------<0.1
0.03
----0.02
0.01
0.024
0.01
<0.1
0.002
----------------<0.01
0.02
0.007
<0.1
----<0.10
----0.006
--------0.0044
<0.1
1.8959
----0.053
0.018
-----
mark
G(0.05)
G(0.01)
G(0.01)
z(targ) remarks
-----------------1.28
--------4.58
-------------------------1.28
-------------0.11
-----------------------------2.69
---------1.28
----22.16
------------6.53
----2.62
-1.28
4.19
-1.28
-----4.41
--------------------2.62
-2.45
-----------------2.85
---------3.47
----735.48 False positive
----15.52
1.84
-----
not OK
17
3
0.0133
0.00808
0.0226
0.0072
Methanol: iis08C06X
0.12
0.1
0.08
0.06
0.04
0.02
1615
657
1728
824
319
859
857
1007
1905
372
174
609
345
862
858
1009
528
1102
1204
867
35
Kernel Density
30
25
20
15
10
5
0
-0.05
Methanol: iis08C06X
0.05
0.1
0.15
page 45 of 69
Determination of Water content (coulometric) on sample #0844; results in mg/kg

lab
52
150
153
171
174
273
311
319
323
332
333
334
342
343
345
346
347
357
372
395
443
444
445
446
468
494
528
529
608
609
646
657
663
786
823
824
825
857
858
859
862
864
867
902
963
971
974
1004
1007
1009
1010
1016
1029
1041
1102
1108
1149
1204
1510
1615
1712
1728
1905
1931
method
E1064
E1064
E1064
E1064
E1064
E1064
E1064
E1064
E1064
E1064
E1064
E1064
E1064
E346
E1064
E1064
E1064
E1064
E1064
E1064
E1064
E1064
E1064
E1064
E1064
E1064
E1064
E1064
E1064
E1064
E1064
in house
E1064
E1064
E1064
E1064
E1064
E1064
E1064
E1064
E1064
E1064
normality
n
outliers
mean (n)
st.dev. (n)
R(calc.)
R(E1064:05)
page 46 of 69
value
177
174
------------158
----187.8
206
----260
----189
193
----183.6
178
200
169
179.9
159.2
----190
----227
218
--------183
210
200
190
--------182
--------200
220
214
209
193
210
----224
----204
270
35
153
180.85
----196
173
190.7
206
----211
175
153.381
--------192
-----
mark
G(0.05)
G(0.05)
G(0.01)
U
z(targ)
-1.22
-1.48
-------------2.85
-----0.30
1.26
----5.88
-----0.19
0.15
-----0.66
-1.14
0.75
-1.91
-0.97
-2.75
-----0.11
----3.06
2.29
---------0.71
1.60
0.75
-0.11
---------0.79
--------0.75
2.46
1.95
1.52
0.15
1.60
----2.80
----1.09
6.74
-13.38
-3.28
-0.89
----0.41
-1.56
-0.05
1.26
----1.69
-1.39
-3.24
--------0.06
-----
remarks
Reported 0.01592
Reported 0.021
Reported 0.018085
OK
39
3
191.27
19.155
53.63
32.71
Methanol: iis08C06X
300
250
200
150
100
50
0.018
333
1004
468
963
858
494
859
609
1204
867
862
323
974
1108
357
857
646
343
1029
864
1905
445
1102
657
342
319
346
608
823
395
1010
52
347
150
1510
372
1041
443
273
1615
1009
1007
Kernel Density
0.016
0.014
0.012
0.01
0.008
0.006
0.004
0.002
0
0
100
Methanol: iis08C06X
200
300
400
page 47 of 69
Determination of Water content (titrimetric) on sample #0844; results in mg/kg

lab
52
150
153
171
174
273
311
319
323
332
333
334
342
343
345
346
347
357
372
395
443
444
445
446
468
494
528
529
608
609
646
657
663
786
823
824
825
857
858
859
862
864
867
902
963
971
974
1004
1007
1009
1010
1016
1029
1041
1102
1108
1149
1204
1510
1615
1712
1728
1905
1931
method
E203
E203
E203
value
----177
414
174
188
170
207
----201
--------------------206
--------190
177
--------238
----213
--------115.3
202.04
------------180
--------204
230
257
210
230
222
214
------------189
----274
----------------140
--------------------212
----145
----170
214
219
normality
n
outliers
mean (n)
st.dev. (n)
R(calc.)
R(E203:01)
OK
29
1
198.9
33.69
94.3
270.0
E203
E203
E203
E203
E203
E203
E203
D1364
E203
E203
E203
E203
E203
E203
E203
E203
E203
E203
E203
E203
E203
E203
E203
E203
D1364
E203
E203
page 48 of 69
mark
z(targ)
-----0.23
U,G(0.01)
2.23
-0.26
-0.11
-0.30
0.08
----0.02
--------------------0.07
---------0.09
-0.23
--------0.41
----C
0.15
---------0.87
0.03
-------------0.20
--------0.05
0.32
0.60
0.12
0.32
0.24
0.16
-------------0.10
----0.78
-----------------0.61
--------------------0.14
----C
-0.56
-----0.30
0.16
0.21
remarks
Reported 0.0414, probably different unit (Wt% instead of mg/kg)
Methanol: iis08C06X
500
450
400
350
300
250
200
150
100
50
0.014
153
974
825
444
858
824
859
1931
862
1905
446
1204
857
311
345
823
529
323
357
963
174
657
372
150
171
273
1728
1615
1016
528
Kernel Density
0.012
0.01
0.008
0.006
0.004
0.002
0
0
100
Methanol: iis08C06X
200
300
400
500
page 49 of 69
Determination of Purity as is on sample #0844; results in %M/M

lab
52
150
153
171
174
273
311
319
323
332
333
334
342
343
345
346
347
357
372
395
443
444
445
446
468
494
528
529
608
609
646
657
663
786
823
824
825
857
858
859
862
864
867
902
963
971
974
1004
1007
1009
1010
1016
1029
1041
1102
1108
1149
1204
1510
1615
1712
1728
1905
1931
method
IMPCA001
in house
IMPCA001
IMPCA001
ih-064
in house
IMPCA001
in house
calc.
in house
in house
in house
in house
IMPCA001
in house
in house
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
in house
in house
calc.
in house
in house
in house
normality
n
outliers
mean (n)
st.dev. (n)
R(calc.)
R(lit.)
page 50 of 69
value
----99.880
99.9
99.882
99.879
------------99.88
----------------99.62
--------99.782
99.67
------------99.8594
--------99.815
99.87
99.968
--------99.82
----99.817
--------99.64
99.64
99.65
99.867
99.872
99.880
99.88
99.870
99.63
----99.8476
----99.8656
----99.88
--------------------------------99.9761
99.988
99.9853
--------99.978
----Group 1
OK
6
0
99.64
0.017
0.05
unknown
mark
C
C
C
C
C
z(targ)
----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------Group 2
Not OK
19
0
99.86
0.030
0.08
unknown
remarks


Group 3
OK
5
0
99.98
0.008
0.02
unknown
Methanol: iis08C06X
100.1
100
99.9
99.8
99.7
99.6
12
1510
1615
1905
1204
528
153
171
859
323
862
150
1007
174
858
494
864
857
974
444
963
609
657
468
347
357
825
824
823
867
343
99.5
Kernel Density
Group 2
10
8
6
4
Group 1
Group 3
2
0
99.4
99.6
Methanol: iis08C06X
99.8
100
100.2
page 51 of 69
Determination of Purity on dry basis on sample #0844; results in %M/M

lab
52
150
153
171
174
273
311
319
323
332
333
334
342
343
345
346
347
357
372
395
443
444
445
446
468
494
528
529
608
609
646
657
663
786
823
824
825
857
858
859
862
864
867
902
963
971
974
1004
1007
1009
1010
1016
1029
1041
1102
1108
1149
1204
1510
1615
1712
1728
1905
1931
method
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
in house
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
in house
IMPCA001
in house
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
in house
normality
n
outliers
mean (n)
st.dev. (n)
R(calc.)
R(lit.)
page 52 of 69
value
99.56
99.898
----99.898
99.898
----99.893
99.91
99.90
--------99.91
----99.64
99.7456
----99.798
99.69
----99.995
----99.8832
----99.59
99.795
99.89
99.991
--------99.85
<99.999
99.836
99.9947
----99.65
99.65
99.66
99.887
99.894
99.901
99.90
99.889
99.652
----99.8683
----99.8860
99.97
----99.99
>99.85
----99.9988
99.91168
99.9987
----------------99.99851
--------99.997
----Group 1:
OK
9
0
99.649
0.0532
0.149
unknown
mark
C
C
C
C
C
C
C
C
C
C
z(targ)
----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------Group 2:
not OK
21
0
99.881
0.0336
0.094
unknown
Remarks



First reported >99.99
Group 3:
not OK
9
0
99.993
0.0091
0.025
unknown
Methanol: iis08C06X
100.1
100
99.9
99.8
99.7
99.6
99.5
1029
1102
1615
395
1905
663
528
1009
1004
319
1041
334
859
323
862
174
150
171
858
311
494
864
857
974
444
963
609
657
347
468
345
357
825
867
824
823
343
52
446
99.4
Kernel Density
group 2
6
5
4
3
group 3
group1
2
1
0
99.4
99.6
Methanol: iis08C06X
99.8
100
100.2
page 53 of 69
Determination of Benzene content on sample #0845; results in mg/kg

lab
52
150
153
171
174
273
311
319
323
332
333
334
342
343
345
346
347
357
372
395
443
444
445
446
468
494
528
529
608
609
646
657
663
786
823
824
825
857
858
859
862
864
867
902
963
971
974
1004
1007
1009
1010
1016
1029
1041
1102
1108
1149
1204
1510
1615
1712
1728
1905
1931
method
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
in house
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
inh-043
IMPCA001
IMPCA001
normality
n
outliers
mean (n)
st.dev. (n)
R(calc.)
R(Horwitz)
page 54 of 69
value
----10.2
----10
9.3
----10.4
10.1
------------------------------------8.9
present
<10
----10.5
------------10
--------------------8.9
--------8
----10
10.9
7.3
12
12
10.8
9.4
----6.9
--------------------------------10.53
----------------------------------------OK
19
0
9.80
1.366
3.82
3.11
mark
z(targ) remarks
----0.36
----0.18
-0.45
----0.54
0.27
-------------------------------------0.81
------------0.63
------------0.18
---------------------0.81
---------1.62
----0.18
0.99
-2.25
1.98
1.98
0.90
-0.36
-----2.61
--------------------------------0.66
-----------------------------------------
Spike:
10.4
Methanol: iis08C06X
14
12
10
862
859
857
864
1041
444
311
150
319
494
825
171
867
174
657
357
823
858
963
0.35
Kernel Density
0.3
0.25
0.2
0.15
0.1
0.05
0
0
Methanol: iis08C06X
10
15
page 55 of 69
Determination of Ethanol content on sample #0844 and #0845; results in mg/kg

lab
52
150
153
171
174
273
311
319
323
332
333
334
342
343
345
346
347
357
372
395
443
444
445
446
468
494
528
529
608
609
646
657
663
786
823
824
825
857
858
859
862
864
867
902
963
971
974
1004
1007
1009
1010
1016
1029
1041
1102
1108
1149
1204
1510
1615
1712
1728
1905
1931
method
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
E346
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
in house
IMPCA001
in house
in house
IMPCA001
IMPCA001
IMPCA001
IMPCA001
E346
IMPCA001
IMPCA001
in house
normality
n
outliers
mean (n)
st.dev. (n)
R(calc.)
R(Horwitz)
page 56 of 69
#0844
10
12.0
----12
11
----13
8.6
11
----------------11.8
10.5
----12.6
11
11
<5
----9.4
--------12
12
182.18
--------15
<5
11.3
--------12
13
11
11.0
11.5
12
12
12.3
11.4
----9.2
----9.52
17.2
11
12.8
11
----11.12
11.075
11.54
--------6.76
<30
16.68
--------12.7
----not OK
38
1
11.61
1.893
5.30
3.59
mark
G(0.01)
C
z(targ)
-1.25
0.31
----0.31
-0.47
----1.09
-2.34
-0.47
----------------0.15
-0.86
----0.78
-0.47
-0.47
---------1.72
--------0.31
0.31
133.04
--------2.65
-----0.24
--------0.31
1.09
-0.47
-0.47
-0.08
0.31
0.31
0.54
-0.16
-----1.88
-----1.63
4.36
-0.47
0.93
-0.47
-----0.38
-0.41
-0.05
---------3.78
----3.96
--------0.85
-----
#0845
10
11.8
----13.8
14.1
----12.6
9.1
11
----------------11.2
10.0
----11.7
12
10
16.26
----9.2
------------12
----------------<5
10
--------12
13
11
10.6
11.7
11
12
12.2
11.5
----9.2
----9.44
17.2
10
12.6
11
----13.05
11.55
10.97
--------7.37
----17.19
--------12.1
-----
mark
z(targ)
-1.29
0.11
----1.66
1.89
----0.73
-1.99
-0.51
-----------------0.36
-1.29
----0.03
0.26
-1.29
3.57
-----1.91
------------0.26
---------------------1.29
--------0.26
1.04
-0.51
-0.82
0.03
-0.51
0.26
0.42
-0.12
-----1.91
-----1.72
4.30
-1.29
0.73
-0.51
----1.08
-0.09
-0.54
---------3.33
----4.29
--------0.34
-----
Remarks
False negative

False negative
First reported 21.11 and 21.759
not OK
37
0
11.66
2.100
5.88
3.61
Methanol: iis08C06X
30
Ethanol on #0844
25
20
15
10
1004
528
1615
1004
609
1615
311
824
1009
347
1905
864
862
823
494
859
171
150
343
858
468
858
1102
347
867
1041
657
867
1029
343
1041
323
1010
174
357
1007
825
857
372
52
345
974
444
963
1204
319
30
Ethanol on #0845
25
20
15
10
0.4
395
174
171
824
1029
311
1009
864
1905
862
357
494
823
0.25
Kernel Density
#0844
0.35
150
323
859
1010
825
1102
857
657
1007
52
372
345
974
444
963
1204
319
Kernel Density
#0845
0.2
0.3
0.25
0.15
0.2
0.1
0.15
0.1
0.05
0.05
0
0
0
10
15
20
25
10
15
20
25
19
#0845
17
15
13
11
9
7
#0844
5
5
10
Methanol: iis08C06X
15
20
normality
n
outliers
mean (n)
st.dev. (n)
r(calc.)
R(calc)
OK
33
3
11.31
1.111
1.188
3.193
page 57 of 69
Determination of Acetone content on sample #0844 and #0845; results in mg/kg

lab
52
150
153
171
174
273
311
319
323
332
333
334
342
343
345
346
347
357
372
395
443
444
445
446
468
494
528
529
608
609
646
657
663
786
823
824
825
857
858
859
862
864
867
902
963
971
974
1004
1007
1009
1010
1016
1029
1041
1102
1108
1149
1204
1510
1615
1712
1728
1905
1931
method
IMPCA001mod.
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
E346
IMPCA001
D1612
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
IMPCA001
in house
IMPCA001
in house
D1612
IMPCA001
IMPCA001
IMPCA001
IMPCA001
D1612
IMPCA001
IMPCA001
D1612
in house
normality
n
outliers
mean (n)
st.dev. (n)
R(calc.)
R(lit.)
page 58 of 69
#0844
<10
<5
----<1
<1
----<5
<10
<10
----------------<5
<1
----<5
<10
<10
<10
----<1
----<0.003
----<5
>0.003
------------<10
<5
--------<5
<1
<10
1.8
<10
<1
2
<10
<5
----<10
----<1
1.1
<2
3.5
<10
----0.659
0.756
1.09
--------<30
<30
0.0127
----<30
<20
----n.a.
8
0
<5
n.a.
n.a.
unknown
mark
z(targ)
-----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
#0845
<10
<5
----<1
<1
----0
0.0
<10
----------------<5
<1
----<5
<10
<10
<10
----0.9
------------<5
----------------<10
<5
--------<5
<1
<10
0.6
<10
1
1
<10
<5
----<10
----<1
1.2
<2
3.5
<10
----0.877
0.86
1.16
--------<30
----nd
----<30
---------
mark
z(targ) remarks
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------- First reported 0.0127
-----------------
n.a.
9
0
<5
n.a.
n.a.
unknown
Methanol: iis08C06X
Determination of Trimethylamine on sample #0844; results in g/kg

lab
52
150
153
171
174
273
311
319
323
332
333
334
342
343
345
346
347
357
372
395
443
444
445
446
468
494
528
529
608
609
646
657
663
786
823
824
825
857
858
859
862
864
867
902
963
971
974
1004
1007
1009
1010
1016
1029
1041
1102
1108
1149
1204
1510
1615
1712
1728
1905
1931
method
E346
E346
in house
E346
in house
E346
E346
normality
n
outliers
mean (n)
st.dev. (n)
R(calc.)
R(lit)
Methanol: iis08C06X
value
----------------------------------------------------------------------------------------------------------------------------------------------------------------6
------------------------<5
15
<10
--------14.102
<100
--------------------N.D.
-----------------
mark
z(targ) remarks
-----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
n.a.
4
0
n.a.
n.a.
n.a.
unknown
page 59 of 69
Determination of UV Absorbance at 300nm (50 mm and 10 mm cuvet) on sample #0845;

lab
52
150
153
171
174
273
311
319
323
332
333
334
342
343
345
346
347
357
372
395
443
444
445
446
468
494
528
529
608
609
646
657
663
786
823
824
825
857
858
859
862
864
867
902
963
971
974
1004
1007
1009
1010
1016
1029
1041
1102
1108
1149
1204
1510
1615
1712
1728
1905
1931
method
IMPCA004
IMPCA004
IMPCA004
50 mm
0.014
--------------------0.008
0.010
------------0.0023
0.010
------------0.010
----0.00494
0.007
----0.013
------------------------------------0.001
--------0.006
--------0.010
0.009
0.006
0.008
----0.005
------------------------0.068
----------------0.0053
-------------------------------------
normality
n
outliers
mean (n)
st.dev. (n)
R(calc.)
R(IMPCA004:06)
OK
17
1
0.0076
0.00346
0.0097
0.0114
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
in house
in house
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
in house
IMPCA004
IMPCA004
IMPCA004
IMPCA004
page 60 of 69
mark
G(0.01)
ex
z(targ)
1.56
--------------------0.09
0.58
-------------1.30
0.58
------------0.58
-----0.66
-0.15
----1.32
-------------------------------------1.62
---------0.40
--------0.58
0.34
-0.40
0.09
-----0.64
------------------------14.79
-----------------0.57
-------------------------------------
10 mm
------------0.002
0.0000
<0.001
------------------------------------0.001
----0.002
-----------------0.0096
------------------------------------------------0.0005
----------------------------------------0.001
0.0036
0
-----------------0.027
--------------------0.003
--------0.002
-----
mark
G(0.05)
G(0.01)
z(targ) remarks
------------0.61
-1.87
-----------------------------------------0.63
----0.61
-----------------13.73
-------------------------------------------------1.25
-----------------------------------------0.63
2.58
-1.87
-----------------35.24
--------------------1.84
--------0.61
----- Reported 100
OK
10
2
0.0015
0.00122
0.0034
0.0023
Methanol: iis08C06X
0.08
0.07
50 mm cuvet
0.06
0.05
0.04
0.03
0.02
0.01
1009
52
444
319
342
347
857
858
862
311
395
859
823
1102
867
372
334
657
0.015
0.01
10 mm cuvet
0.005
-0.005
120
Kernel Density
50 m cuvet
100
250
1004
1615
357
1905
171
974
346
824
174
1007
1041
445
-0.01
Kernel Density
10 m cuvet
200
80
150
60
100
40
50
20
0
-0.02
Methanol: iis08C06X
0.02
0.04
0.06
0.08
0
-0.04
-0.03
-0.02
-0.01
0.01
page 61 of 69
Determination of UV Absorbance at 268.5nm (50 mm and 10 mm cuvet) on sample #0845;

lab
52
150
153
171
174
273
311
319
323
332
333
334
342
343
345
346
347
357
372
395
443
444
445
446
468
494
528
529
608
609
646
657
663
786
823
824
825
857
858
859
862
864
867
902
963
971
974
1004
1007
1009
1010
1016
1029
1041
1102
1108
1149
1204
1510
1615
1712
1728
1905
1931
method
IMPCA004
IMPCA004
IMPCA004
50 nm
0.075
--------------------0.0327
0.035
------------0.0237
0.034
------------0.040
----0.03030
0.045
----0.032
------------------------------------<0.001
--------0.032
--------0.033
0.033
0.033
0.032
----0.030
------------------------0.100
----------------0.0283
-------------------------------------
normality
n
outliers
mean (n)
st.dev. (n)
R(calc.)
R(IMPCA004:06)
not OK
15
2
0.0329
0.00482
0.0135
0.0089
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
in house
in house
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
in house
IMPCA004
IMPCA004
IMPCA004
IMPCA004
page 62 of 69
mark
G(0.05)
G(0.01)
ex
z(targ)
13.20
---------------------0.07
0.65
-------------2.90
0.33
------------2.22
-----0.83
3.79
-----0.29
-------------------------------------------------0.29
--------0.02
0.02
0.02
-0.29
-----0.92
------------------------21.04
-----------------1.45
-------------------------------------
10 nm
------------0.007
0.0031
0.002
------------------------------------0.0065
----0.007
-----------------0.0055
------------------------------------------------0.0042
----------------------------------------0.005
0.0105
0.001
-----------------0.003
--------------------0.008
--------0.011
-----
mark
G(0.05)
G(0.05)
z(targ) remarks
------------1.85
-4.94
-6.85
------------------------------------0.98
----1.85
-----------------19.90
-------------------------------------------------3.02
-----------------------------------------1.63
7.94
-8.59
-----------------15.55
--------------------3.59
--------8.81
----- Reported 99
OK
11
2
0.0059
0.00324
0.0091
0.0016
Methanol: iis08C06X
0.12
50 mm cuvet
0.1
0.08
0.06
0.04
0.02
1009
52
395
347
319
342
857
859
858
311
823
862
444
372
867
1102
334
0.015
0.01
10 mm cuvet
0.005
-0.005
1905
1004
1615
357
171
346
974
824
174
273
1007
1041
445
-0.01
90
100
Kernel Density
50 m cuvet
90
80
Kernel Density
10 m cuvet
80
70
70
60
60
50
50
40
40
30
30
20
20
10
10
0
0
0.05
Methanol: iis08C06X
0.1
0.15
0
-0.02
-0.01
0.01
0.02
page 63 of 69

lab
52
150
153
171
174
273
311
319
323
332
333
334
342
343
345
346
347
357
372
395
443
444
445
446
468
494
528
529
608
609
646
657
663
786
823
824
825
857
858
859
862
864
867
902
963
971
974
1004
1007
1009
1010
1016
1029
1041
1102
1108
1149
1204
1510
1615
1712
1728
1905
1931
method
IMPCA004
IMPCA004
IMPCA004
50 nm
0.192
--------------------0.1615
0.153
------------0.1651
0.181
------------0.155
----0.18161
0.173
----0.186
------------------------------------0.087
--------0.159
--------0.156
0.153
0.146
0.159
----0.145
------------------------0.217
----------------0.1584
-------------------------------------
normality
n
outliers
mean (n)
st.dev. (n)
R(calc.)
R(IMPCA004:06)
OK
16
2
0.1640
0.01440
0.0403
0.0166
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
in house
in house
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
in house
IMPCA004
IMPCA004
IMPCA004
IMPCA004
page 64 of 69
mark
G(0.05)
G(0.05)
ex
z(targ)
4.73
---------------------0.43
-1.87
------------0.18
2.87
-------------1.53
----2.97
1.51
----3.71
-------------------------------------13.02
---------0.85
---------1.36
-1.87
-3.05
-0.85
-----3.22
------------------------8.95
-----------------0.95
-------------------------------------
10 nm
------------0.032
0.0287
0.022
------------------------------------0.037
----0.032
----------------0.0180
------------------------------------------------0.0284
----------------------------------------0.030
0.0366
0.03
----------------0.114
--------------------0.035
--------0.053
-----
mark
G(0.01)
G(0.05)
z(targ) remarks
------------1.88
-1.18
-7.37
------------------------------------6.50
----1.88
-----------------11.07
-------------------------------------------------1.45
----------------------------------------0.03
6.13
0.03
----------------77.72
--------------------4.65
--------21.30
----- Reported 96
OK
11
2
0.0300
0.00581
0.0163
0.0030
Methanol: iis08C06X
0.25
0.2
50 mm cuvet
0.15
0.1
0.05
1009
52
444
372
342
395
334
311
862
823
1102
857
347
319
858
859
867
657
0.12
0.1
10 mm cuvet
0.08
0.06
0.04
0.02
25
1041
1905
346
1004
1615
171
357
1007
974
174
824
273
445
70
Kernel Density
50 m cuvet
Kernel Density
10 m cuvet
60
20
50
15
40
30
10
20
5
10
0
0
0
Methanol: iis08C06X
0.1
0.2
0.3
0.05
0.1
0.15
page 65 of 69

lab
52
150
153
171
174
273
311
319
323
332
333
334
342
343
345
346
347
357
372
395
443
444
445
446
468
494
528
529
608
609
646
657
663
786
823
824
825
857
858
859
862
864
867
902
963
971
974
1004
1007
1009
1010
1016
1029
1041
1102
1108
1149
1204
1510
1615
1712
1728
1905
1931
method
IMPCA004
IMPCA004
IMPCA004
50 nm
1.451
--------------------1.208
1.09
------------1.2188
1.185
------------1.200
----1.23052
1.222
----1.158
------------------------------------1.111
--------1.140
--------1.050
1.065
1.100
1.081
----1.010
------------------------1.26
----------------1.2750
-------------------------------------
normality
n
outliers
mean (n)
st.dev. (n)
R(calc.)
R(IMPCA004:06)
OK
17
1
1.1532
0.07922
0.2218
0.3310
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
in house
in house
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
IMPCA004
in house
IMPCA004
IMPCA004
IMPCA004
IMPCA004
page 66 of 69
mark
G(0.05)
ex
z(targ)
2.52
--------------------0.46
-0.53
------------0.56
0.27
------------0.40
----0.65
0.58
----0.04
-------------------------------------0.36
---------0.11
---------0.87
-0.75
-0.45
-0.61
-----1.21
------------------------0.90
----------------1.03
-------------------------------------
10 nm
------------0.227
0.2285
0.220
------------------------------------0.233
----0.237
----------------0.2241
------------------------------------------------0.2246
----------------------------------------0.215
0.2326
0.26
----------------1.095
--------------------2.498
--------0.269
-----
mark
G(0.01)
G(0.05)
z(targ) remarks
-------------0.28
-0.22
-0.57
-------------------------------------0.03
----0.14
-----------------0.40
-------------------------------------------------0.38
-----------------------------------------0.78
-0.05
1.10
----------------35.95
--------------------94.52
--------1.47
----- Reported 83
OK
11
2
0.2337
0.01654
0.0463
0.0671
Methanol: iis08C06X
1.6
1.4
50 mm cuvet
1.2
1
0.8
0.6
0.4
0.2
52
1102
1009
372
395
334
311
347
342
444
823
657
859
319
862
858
857
867
2.5
10 mm cuvet
1.5
0.5
1615
1041
1905
1007
357
346
1004
174
171
824
445
273
974
18
Kernel Density
50 m cuvet
3.5
Kernel Density
10 m cuvet
16
14
12
2.5
10
2
8
1.5
0.5
0
0
0.5
Methanol: iis08C06X
1.5
page 67 of 69
APPENDIX 2
List of number of participants per country
Number of laboratories
1 laboratory in
1 laboratory in
1 laboratory in
1 laboratory in
1 laboratory in
3 laboratories in
3 laboratories in
1 laboratory in
1 laboratory in
3 laboratories in
4 laboratories in
2 laboratories in
2 laboratories in
1 laboratory in
7 laboratories in
1 laboratory in
1 laboratory in
1 laboratory in
1 laboratory in
2 laboratories in
1 laboratory in
5 laboratories in
1 laboratory in
2 laboratories in
3 laboratories in
1 laboratory in
1 laboratory in
2 laboratories in
4 laboratories in
5 laboratories in
1 laboratory in
page 68 of 69
Country
BELGIUM
CANADA
CHILE
ESTONIA
FINLAND
FRANCE
GERMANY
GREECE
ITALY
KOREA
MALAYSIA
MEXICO
NEW ZEALAND
NORWAY
P.R. of CHINA
POLAND
ROMANIA
RUSSIA
SAUDI ARABIA
SINGAPORE
SOUTH AFRICA
SPAIN
SWEDEN
THAILAND
THE NETHERLANDS
TRINIDAD and TOBAGO W.I.
TURKEY
U.A.E.
U.S.A.
UNITED KINGDOM
VENEZUELA
Methanol: iis08C06X
APPENDIX 3
Abbreviations:
C
= final result after checking of first reported suspect result
D(0.01)
= outlier in Dixons outlier test
D(0.05)
= straggler in Dixons outlier test
G(0.01)
= outlier in Grubbs outlier test
G(0.05)
= straggler in Grubbs outlier test
DG(0.01)
= outlier in Double Grubbs outlier test
DG(0.05)
= straggler in Double Grubbs outlier test
= error in calculations
= reported in different unit
Ex
= excluded from calculations
n.a.
= not applicable
W.
= result withdrawn on request of participant
Literature:
1
iis Interlaboratory Studies, Protocol for the Organisation, Statistics & Evaluation, November 2008
ASTM E178-02
ASTM E1301-03
ISO 5725-86
ISO 5725, parts 1-6, 1994
M. Thompson and R. Wood, J. AOAC Int, 76, 926, (1993)
W.J. Youden and E.H. Steiner, Statistical Manual of the AOAC, (1975)
IP 367/96
DIN 38402 T41/42
10
P.L. Davies, Fr. Z. Anal. Chem, 331, 513, (1988)
11
J.N. Miller, Analyst, 118, 455, (1993)
12
IMPCA Methanol Reference Specifications, IMPCA, Brussels, January 2008.
13
ASTM E346-03e1
14
Analytical Methods Committee Technical brief, No4 January 2001.
15
The Royal Society of Chemistry 2002, Analyst 2002, 127 page 1359-1364, P.J. Lowthian and
M. Thompson (see http://www.rsc.org/suppdata/an/b2/b205600n/).
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Results of Proficiency Test

Institute for Interlaboratory Studies

Authors: ing. R.J. Starink

Spijkenisse, November 2008

Institute for Interlaboratory Studies

CONFIDENTIALITY STATEMENT ......................................................................................................... 4

STABILITY OF THE SAMPLES .............................................................................................................. 5

EVALUATION PER TEST ....................................................................................................................... 7

PERFORMANCE EVALUATION FOR THE GROUP OF LABORATORIES ...................................... 11

COMPARISON OF THE PROFICIENCY TEST OF SEPTEMBER 2008 WITH PREVIOUS PTS.... 13

Data and statistical results ................................................................................................................. 15

List of number of participants per country ......................................................................................... 68

Abbreviations and literature ............................................................................................................... 69

Institute for Interlaboratory Studies

Spijkenisse, November 2008

Spijkenisse, November 2008

Institute for Interlaboratory Studies

Table 1: homogeneity test of subsample #0844

Table 2: homogeneity test of subsample #0845

Institute for Interlaboratory Studies

Spijkenisse, November 2008

ASTM D4052:02 ASTM E203:01

Table 3: repeatabilities of subsamples #0844 and #0845

STABILITY OF THE SAMPLES

Spijkenisse, November 2008

Institute for Interlaboratory Studies

Institute for Interlaboratory Studies

Spijkenisse, November 2008

z(target) = (result - average) / target standard deviation

EVALUATION PER TEST

Spijkenisse, November 2008

Institute for Interlaboratory Studies

No analytical problems were observed. No results were found outside the

All participants agreed on a result far above 60 minutes.

Institute for Interlaboratory Studies

Spijkenisse, November 2008

No analytical problems were observed. No results were outside the

As ASTM D3961:98 was withdrawn in 2004 with no replacement, it was decided

Spijkenisse, November 2008

Institute for Interlaboratory Studies

#0845) and the theoretical increment of 1.23 mg S/kg is unsatisfactory (71%).

This determination may be problematic. Nine results are outside the

This determination is problematic. Seven results were outside the reproducibility

This determination is not problematic. No results were outside the

These determinations are very problematic as the group is

This determination is somewhat problematic. Although, no results were outside

Institute for Interlaboratory Studies

Spijkenisse, November 2008

Only four participants reported a numerical result for this determination.

PERFORMANCE EVALUATION FOR THE GROUP OF LABORATORIES

Spijkenisse, November 2008

Institute for Interlaboratory Studies

Acidity as acetic acid

Anorganic Chloride as Cl, #0844

Anorganic Chloride as Cl, #0845

Initial Boiling Point (automatic)

Dry Point (automatic)

Initial Boiling Point (manual)

Dry Point (manual)

Specific Gravity 20/20 C

Permanganate Time Test

Sulphur (D5354), #0844

Sulphur (IMPCA005), #0844

Total Iron on sample as Fe, #0844