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Methanol Specifications

This document summarizes the results of a proficiency test for methanol conducted in September 2008. 64 laboratories from 31 countries participated in the test by analyzing two methanol samples for various parameters. The samples were prepared and tested for homogeneity by the Institute for Interlaboratory Studies. Laboratories were asked to report results for parameters like density, water content, chloride content, sulfur content, and purity using standardized test methods. The results were statistically analyzed and laboratories' performance was evaluated against acceptance criteria. Historical comparisons were also made to previous proficiency tests for methanol.

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0% found this document useful (0 votes)

268 views69 pages

Methanol Specifications

Uploaded by

Shreepathi Adiga

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Available Formats

Download as PDF, TXT or read online on Scribd

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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

Institute for Interlaboratory Studies

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

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

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

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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).

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2.3

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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:

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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
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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:

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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
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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.

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SG 20/20 oC:

Spijkenisse, November 2008

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

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#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

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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.

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Parameter

Institute for Interlaboratory Studies

unit

average

2.8 * sd

R (lit)

Acidity as acetic acid

mg/kg

11.65

8.11

14.00

Anorganic Chloride as Cl, #0844

mg/kg

0.09

0.18

0.30

Anorganic Chloride as Cl, #0845

mg/kg

0.63

0.36

0.30

Carbonisable Substances

Pt/Co

6.9

6.1

5.0

Colour

Pt/Co

2.3

4.1

7.0

kg/L

0.79133

0.00031

0.00050

Initial Boiling Point (automatic)

64.36

0.61

1.00

Dry Point (automatic)

64.77

0.56

0.69

Initial Boiling Point (manual)

64.37

0.24

0.69

Dry Point (manual)

64.84

0.49

0.84

Nonvolatile Matter

mg/100 mL

0.51

1.34

2.40

minutes

98.6

51.2

unknown

Specific Gravity 20/20 C

0.79273

0.00031

0.00050

Apparent Spec.Grav.20/20 C

0.79248

0.00028

0.00050

Density @ 20 C

Permanganate Time Test

Sulphur (D5354), #0844

mg/kg

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

0.0133

0.0226

0.0072

Water (coulometric)

mg/kg

191.3

53.6

32.7

Water (titrimetric)

mg/kg

198.9

94.3

270.0

Purity

%M/M

unknown *)

Purity on dry basis

%M/M

unknown *)

Benzene, #0845

mg/kg

9.80

3.82

3.11

Ethanol, #0844

mg/kg

11.61

5.30

3.59

Ethanol, #0845

mg/kg

11.65

5.88

3.61

UV absorbance at 300 nm (50 mm cuvet)

0.0076

0.0097

0.0114

UV absorbance at 268.5 nm (50 mm cuvet)

0.0329

0.0135

0.0089

UV absorbance at 250 nm (50 mm cuvet)

0.1640

0.0403

0.0166

UV absorbance at 220 nm (50 mm cuvet)

1.1532

0.2218

0.3310

UV absorbance at 300 nm (10 mm cuvet)

0.0015

0.0034

0.0023

UV absorbance at 268.5 nm (10 mm cuvet)

0.0059

0.0091

0.0016

UV absorbance at 250 nm (10 mm cuvet)

0.0300

0.0163

0.0030

UV absorbance at 220 nm (10 mm cuvet)

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.

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4.3

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COMPARISON OF THE PROFICIENCY TEST OF SEPTEMBER 2008 WITH PREVIOUS PTS

September
2008

September
2007

September
2006

September
2005

Number of reporting labs

Number of results reported

748

619

685

593

Statistical outliers

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.

Specific Gravity 20/20 C

Sulphur

n.e.

Total Iron

Water (coulometric)

Water (titrimetric)

Benzene

n.d.

n.d.
--

n.e.

Acetone

n.e.

Ethanol

UV absorbance 300nm

n.e.

UV absorbance 268.5 nm

n.e.

UV absorbance 250 nm

n.e.

UV absorbance 220 nm

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

Spijkenisse, November 2008

Institute for Interlaboratory Studies

-- empty page --

page 14 of 69

Methanol: iis08C06X

Institute for Interlaboratory Studies

Spijkenisse, November 2008

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

Spijkenisse, November 2008

Institute for Interlaboratory Studies

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

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

Institute for Interlaboratory Studies

Spijkenisse, November 2008

Institute for Interlaboratory Studies

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)

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
175 First reported 0.5
----------------1.22
129
-------------0.27
98
0.20
108
-1.30
77
-----0.46
94
-------------0.27
98
---------0.55
92
-0.79
87 First reported 0.506
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

Institute for Interlaboratory Studies

Spijkenisse, November 2008

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

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

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

Spijkenisse, November 2008

Institute for Interlaboratory Studies

Determination of Carbonisable Substances Pt/Co on sample #0844;

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

Institute for Interlaboratory Studies

Spijkenisse, November 2008

0.18

528

395

1007

444

657

446

1615

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

page 21 of 69

Spijkenisse, November 2008

Institute for Interlaboratory Studies

Determination of Colour as Pt/Co on sample #0844;

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

Institute for Interlaboratory Studies

Spijkenisse, November 2008

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

Spijkenisse, November 2008

Institute for Interlaboratory Studies

Determination of Density at 20 oC on sample #0844; results in kg/L

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

Institute for Interlaboratory Studies

Spijkenisse, November 2008

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

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

Spijkenisse, November 2008

Institute for Interlaboratory Studies

Determination of IBP and DP (automated) @ 760 mmHg on sample #0844; results in C

method
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

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

not OK
23
0
64.77
0.200
0.56
0.69

Methanol: iis08C06X

Institute for Interlaboratory Studies

Spijkenisse, November 2008

65.5

Initial Boiling Point

64.5

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

65.5

Dry Point

64.5

63.5

494

334

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

Methanol: iis08C06X

64.5

65.5

0
63.5

64.5

65.5

page 27 of 69

Spijkenisse, November 2008

Institute for Interlaboratory Studies

Determination of IBP and DP (manual) @ 760 mmHg on sample #0844; results in C

method

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

Institute for Interlaboratory Studies

Spijkenisse, November 2008

65.5

Initial Boiling Point

64.5

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

963

859

864

1004

858

867

857

862

342

858

857

657

974

Dry Point
65.5

64.5

63.5

444

646

2.5

Kernel Density
IBP

Kernel Density
DP

4
1.5
3
1
2
0.5

1
0
63.5

Methanol: iis08C06X

64.5

65.5

0
63.5

64.5

65.5

page 29 of 69

Spijkenisse, November 2008

Institute for Interlaboratory Studies

-- empty page --

page 30 of 69

Methanol: iis08C06X

Institute for Interlaboratory Studies

Spijkenisse, November 2008

Determination of Water Miscibility on sample #0844;

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

n.a.
50
0
n.a.
n.a.
n.a.
n.a.

page 31 of 69

Spijkenisse, November 2008

Institute for Interlaboratory Studies

Determination of Nonvolatile Matter on sample #0844; results in mg/100 mL

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

Institute for Interlaboratory Studies

Spijkenisse, November 2008

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

153

Kernel Density

1.4
1.2
1
0.8
0.6
0.4
0.2
0
-2

Methanol: iis08C06X

page 33 of 69

Spijkenisse, November 2008

Institute for Interlaboratory Studies

Determination of Permanganate Time Test @ 15C on sample #0844; results in minutes

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

Institute for Interlaboratory Studies

Spijkenisse, November 2008

170

150

130

110

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

1615

1102

Kernel Density

0.03
0.025
0.02
0.015
0.01
0.005
0
0

Methanol: iis08C06X

100

150

200

page 35 of 69

Spijkenisse, November 2008

Institute for Interlaboratory Studies

Determination of Specific Gravity 20/20 C/C on sample #0844;

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

Institute for Interlaboratory Studies

Spijkenisse, November 2008

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

Spijkenisse, November 2008

Institute for Interlaboratory Studies

Determination of Specific Gravity, Apparent 20/20 C/C on sample #0844;

method
in house
D4052
D4052

D4052

ih-960
D4052/891

D4052

D891
D4052

in house
in house
D891
D891
D4052 calc.
D4052

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

Institute for Interlaboratory Studies

Spijkenisse, November 2008

0.7931
0.7929
0.7927
0.7925
0.7923
0.7921
0.7919
0.7917

4500

657

174

1007

867

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

Spijkenisse, November 2008

Institute for Interlaboratory Studies

Determination of Sulphur on sample #0844 and #0845; results in mg/kg

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

(1.03 0.16) / 1.23 * 100 = 71 %

Methanol: iis08C06X

Institute for Interlaboratory Studies

Spijkenisse, November 2008

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

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

Spijkenisse, November 2008

Institute for Interlaboratory Studies

-- empty page --

page 42 of 69

Methanol: iis08C06X

Institute for Interlaboratory Studies

Spijkenisse, November 2008

Determination of Sulphur (IMPCA005) on sample #0844 and #0845; results in mg/kg

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

Spijkenisse, November 2008

Institute for Interlaboratory Studies

Determination of Total Iron as Fe on sample #0844; results in mg/kg

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

Institute for Interlaboratory Studies

Spijkenisse, November 2008

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

Kernel Density
30
25
20
15
10
5
0
-0.05

Methanol: iis08C06X

0.05

0.1

0.15

page 45 of 69

Spijkenisse, November 2008

Institute for Interlaboratory Studies

Determination of Water content (coulometric) on sample #0844; results in mg/kg

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

Institute for Interlaboratory Studies

Spijkenisse, November 2008

300

250

200

150

100

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

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

Spijkenisse, November 2008

Institute for Interlaboratory Studies

Determination of Water content (titrimetric) on sample #0844; results in mg/kg

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)

First reported 0.021

First reported 111.92

Methanol: iis08C06X

Institute for Interlaboratory Studies

Spijkenisse, November 2008

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

Spijkenisse, November 2008

Institute for Interlaboratory Studies

Determination of Purity as is on sample #0844; results in %M/M

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

remarks

First reported 99.979

First reported 99.982

First reported 99.9822

First reported 99.98

First reported 99.99
First reported 99.97

First reported 99.9847

Group 3
OK
5
0
99.98
0.008
0.02
unknown

Methanol: iis08C06X

Institute for Interlaboratory Studies

Spijkenisse, November 2008

100.1

100

99.9

99.8

99.7

99.6

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

Spijkenisse, November 2008

Institute for Interlaboratory Studies

Determination of Purity on dry basis on sample #0844; results in %M/M

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

Remarks

First reported 99.998

First reported 99.999

First reported 99.9976
First reported 99.998

First reported 99.9952

First reported 99.99
First reported 99.99
First reported 99.99
First reported 99.99

First reported 99.999

First reported >99.99

First reported 99.9979

Group 3:
not OK
9
0
99.993
0.0091
0.025
unknown

Methanol: iis08C06X

Institute for Interlaboratory Studies

Spijkenisse, November 2008

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

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

Spijkenisse, November 2008

Institute for Interlaboratory Studies

Determination of Benzene content on sample #0845; results in mg/kg

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

Institute for Interlaboratory Studies

Spijkenisse, November 2008

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

page 55 of 69

Spijkenisse, November 2008

Institute for Interlaboratory Studies

Determination of Ethanol content on sample #0844 and #0845; results in mg/kg

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

First reported 2.514

False negative

First reported 21.11 and 21.759

not OK
37
0
11.66
2.100
5.88
3.61

Methanol: iis08C06X

Institute for Interlaboratory Studies

Spijkenisse, November 2008

Ethanol on #0844
25

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

345

974

444

963

1204

319

Ethanol on #0845
25

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

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

#0845
17
15

13
11

9
7

#0844

5
5

Methanol: iis08C06X

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

Spijkenisse, November 2008

Institute for Interlaboratory Studies

Determination of Acetone content on sample #0844 and #0845; results in mg/kg

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

#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

n.a.
9
0
<5
n.a.
n.a.
unknown

Methanol: iis08C06X

Institute for Interlaboratory Studies

Spijkenisse, November 2008

Determination of Trimethylamine on sample #0844; results in g/kg

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

n.a.
4
0
n.a.
n.a.
n.a.
unknown

page 59 of 69

Spijkenisse, November 2008

Institute for Interlaboratory Studies

Determination of UV Absorbance at 300nm (50 mm and 10 mm cuvet) on sample #0845;

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)

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

Institute for Interlaboratory Studies

Spijkenisse, November 2008

0.08
0.07

50 mm cuvet

0.06
0.05
0.04
0.03
0.02
0.01

1009

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

Spijkenisse, November 2008

Institute for Interlaboratory Studies

Determination of UV Absorbance at 268.5nm (50 mm and 10 mm cuvet) on sample #0845;

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)

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)

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

Institute for Interlaboratory Studies

Spijkenisse, November 2008

0.12

50 mm cuvet

0.1

0.08

0.06

0.04

0.02

1009

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

100

Kernel Density
50 m cuvet

90
80

Kernel Density
10 m cuvet

80
70

10
0
0

0.05

Methanol: iis08C06X

0.1

0.15

0
-0.02

-0.01

0.01

0.02

page 63 of 69

Spijkenisse, November 2008

Institute for Interlaboratory Studies

Determination of UV Absorbance at 250nm (50 mm and 10 mm cuvet) on sample #0845;

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)

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

Institute for Interlaboratory Studies

Spijkenisse, November 2008

0.25

0.2

50 mm cuvet

0.15

0.1

0.05

1009

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

1041

1905

346

1004

1615

171

357

1007

974

174

824

273

445

Kernel Density
50 m cuvet

Kernel Density
10 m cuvet

50
15

40
30

20
5
10
0

0
0

Methanol: iis08C06X

0.1

0.2

0.3

0.05

0.1

0.15

page 65 of 69

Spijkenisse, November 2008

Institute for Interlaboratory Studies

Determination of UV Absorbance at 220nm (50 mm and 10 mm cuvet) on sample #0845;

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)

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

Institute for Interlaboratory Studies

Spijkenisse, November 2008

1.6
1.4

50 mm cuvet

1.2
1
0.8
0.6
0.4
0.2

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

Kernel Density
50 m cuvet

3.5

Kernel Density
10 m cuvet

16
14

2.5

10
2
8
1.5

0.5

0
0

0.5

Methanol: iis08C06X

1.5

page 67 of 69

Spijkenisse, November 2008

Institute for Interlaboratory Studies

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

Institute for Interlaboratory Studies

Spijkenisse, November 2008

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

= excluded from calculations

n.a.

= not applicable

= 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

P.L. Davies, Fr. Z. Anal. Chem, 331, 513, (1988)

J.N. Miller, Analyst, 118, 455, (1993)

IMPCA Methanol Reference Specifications, IMPCA, Brussels, January 2008.

ASTM E346-03e1

Analytical Methods Committee Technical brief, No4 January 2001.

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/).

Methanol: iis08C06X

page 69 of 69

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