Methanol Specifications

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Results of Proficiency TestMethanol

September 2008

Organised by: Institute for Interlaboratory StudiesSpijkenisse, the Netherlands

Authors: ing. R.J. StarinkCorrectors: dr. R.G. Visser and ing. S. LagendijkReport: iis08C06X

November 2008



Spijkenisse, November 2008 Institute for Interlaboratory Studies

page 2 of 69 Methanol: iis08C06X

CONTENTS

1 INTRODUCTION ..................................................................................................................................... 3

2 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

3 RESULTS................................................................................................................................................. 5

3.1 STATISTICS ............................................................................................................................................ 6

3.2 GRAPHICS .............................................................................................................................................. 6

3.3 Z-SCORES .............................................................................................................................................. 6

4 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 PT’S.... 13

Appendices:

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

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

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



Institute for Interlaboratory Studies Spijkenisse, November 2008

Methanol: iis08C06X page 3 of 69

1 INTRODUCTION

Since 1996, a proficiency test for Methanol was organised every year by The Institute forInterlaboratory Studies. During the annual proficiency testing program 2008/2009, it was decidedto continue the round robin for the analysis of Methanol in accordance with the latest applicableversion of the IMPCA specification and ASTM E346:03. In the latest IMPCA specification ofJanuary 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 IMPCAgroup 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 haveparticipated. See appendix 2 for a list of participants in alphabetical country order. In this reportthe results of the proficiency test are presented and discussed.

2 S ET UP

The Institute for Interlaboratory studies (i.i.s.) in Spijkenisse, The Netherlands, was the organiserof this proficiency test. To get maximum information from this study it was decided to send 2different 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 determinationof 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 resultswere preferably used for statistical evaluations.

2.1 A CCREDITATION

The Institute for Interlaboratory Studies in Spijkenisse, the Netherlands, is accredited inaccordance 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 participant’sdata. Feedback from the participants on the reported data is encouraged and customer’ssatisfaction is measured on regular basis by sending out questionnaires.

2.2 P ROTOCOL

The protocol followed in the organisation of this proficiency test was the one as described forproficiency testing in the report ‘iis Interlaboratory Studies: Protocol for the Organisation,Statistics and Evaluation’ of November 2008 (iis-protocol, version 3.1).





2.3 C ONFIDENTIALITY S TATEMENT

All data present in this report must be regarded as confidential and for use by the participatingcompanies only. Disclosure of the information in this report is only allowed by means of the entirereport. Use of the contents of this report for third parties is only allowed by written permission ofthe Institute of Interlaboratory Studies. Disclosure of the identity of one or more of theparticipating companies will be done only after receipt of a written agreement of the companiesinvolved.

2.4 S AMPLES

The necessary 100 litre bulk material was provided by a large Methanol producer. The bulkmaterial was divided in two parts. Approx. 75 litre bulk material was after spiking with 70 mL of a1.014 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 pre-cleaned 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 inaccordance with ASTM D4052:02, Water content in accordance with ASTM E203:01 and Sulphurcontent in accordance with ASTM D3961:03 on 4 stratified random selected samples. Thehomogeneity of the subsamples #0845 was checked by determination of Chloride in accordancewith IMPCA 002:1998 and UV absorbance at 250nm according IMPCA004:06 on 5 stratifiedrandom selected samples.

Density at 20ºCin kg/L

Waterin mg/kg

Sulphurin 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 absorbanceat 250 nm

Chloridein 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 bymultiplication of the standard deviations by 2.8:





Density at 15ºCin kg/L

Waterin mg/kg

Sulphurin mg/kg

Chloridein mg/kg

UV-absorbanceat 250nm

r (sample #0844) 0.00001 16.2 0.23 -- --

r (sample #0845) -- -- -- 0.03 0.006

reference test ASTM D4052:02 ASTM E203:01 Horwitz IMPCA 002:98 IMPCA 004:06

r (reference test) 0.00010 80.0 0.22 0.03 0.010

Table 3: repeatabilities of subsamples #0844 and #0845

The repeatabilities of Density, Water and Sulphur for sample #0844 were in agreement with therespective methods and the estimated repeatability calculated using the Horwitz equation. Therepeatabilities of Chloride and UV absorbance at 250nm for sample #0845 were in agreementwith 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 tothe participating laboratories on August 27, 2008.

2.5 S TABILITY OF THE SAMPLES

The stability of Methanol, packed in the brown glass bottles, was checked. The material wasfound sufficiently stable for the period of the proficiency test.

2.6 A NALYSES

The participants were asked to determine Acidity, Anorganic Chloride, Appearance, CarbonisableSubstances Pt/Co, Colour Pt/Co, Density @ 20 oC, Distillation (IBP & DP), Acetone, Ethanol,Water Miscibility, Nonvolatile Matter, Purity (on dry basis), Permanganate Time Test, SpecificGravity 20/20 ºC/ºC, Apparent Specific Gravity 20/20 ºC/ºC, Sulphur, Total Iron, Trimethylamineand Water (coulometric and titrimetric) on sample #0844. On sample #0845 was requested toanalyze: 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, aMSDS and a draft method IMPCA006:08 were added to the package.

3 R ESULTS

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 laboratoriesare represented by their code numbers.

Directly after the deadline, a reminder fax was sent to the laboratories that had not reportedresults at that moment. Shortly after the deadline the available results were screened for suspectdata. A result was called suspect in case the Huber Elimination Rule (a robust outlier test) found





it to be an outlier. The laboratories that produced these suspect data were asked to check theresults. Additional or corrected results are used for data analysis and original results are placedunder 'Remarks' in the result tables in appendix 1.

3.1 S TATISTICS

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, version3.0).

For the statistical evaluation the unrounded (when available) figures were used instead of therounded 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 setdoes not have a normal distribution, the (results of the) statistical evaluation should be used withdue care.In accordance to ISO 5725 (1986 and 1994) the original results per determination were submittedsubsequently to Dixon and Grubbs outlier tests. Outliers are marked byD(0.01) for the Dixon test and by G(0.01) or DG(0.01) for the Grubbs test. Stragglers are markedby D(0.05) for the Dixon test and by G(0.05) or DG(0.05) for the Grubbs test. Both outliers andstragglers were not included in the calculations of the averages and the standard deviations.

Finally, the reproducibilities were calculated from the standard deviations by multiplying thesewith a factor of 2.8.

3.2 G RAPHICS

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 resultsare plotted. The corresponding laboratory numbers are under the X-axis. A straight line presentsthe average of the reported data. Two striped lines present the reproducibility limits of the selectedstandard, 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 dataare represented as a triangle. Furthermore, Kernel Density Graphs were made. This is a methodfor producing a smooth density approximation to a set of data that avoids some problemsassociated 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 literaturerequirements, e.g. ASTM reproducibilities, the z-scores were calculated using a target standarddeviation. This target standard deviation was calculated from the literature reproducibility bydivision with 2.8. The z-scores were calculated according to:





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. Thereforethe usual interpretation of z-scores is as follows:

| z | < 1 good1 < | z | < 2 satisfactory2 < | z | < 3 questionable

| z | > 3 unsatisfactory

4 E VALUATION

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. Thirteenparticipants received the samples near or after the final reporting date. In total, 14 participantsreported after the deadline and 4 participants did not report any result at all. Not all participantswere able to report all requested parameters. Finally, 60 participants did send in 748 numericalresults. Observed were 24 outlying results, which is 3.2 % of the total of numerical results. Inproficiency studies outlier percentages of 3 % - 7.5 % are quite normal.

4.1 E VALUATION PER TEST

In this section the results are discussed per test. Not normal distributions were found for thefollowing determinations: Acidity, Anorganic Chloride (#0844 and #0845), CarbonisableSubstances, Colour Pt/Co, Density @ 20 oC, IBP (automatic and manual), DP (automatic andmanual), 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 statisticalevaluation should be used with due care. From the Kernel Density graphs, one can see that thisconclusion is not always justified.

Acidity: No analytical problems were observed. Only one result was outside thereproducibility 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 fourresults were outside the reproducibility limits. The calculated reproducibility ofsample #0844 is, after rejection of the statistical outlier, in good agreement withthe requirements of IMPCA002:98. The calculated reproducibility of sample#0845 is, after rejection of the statistical outliers, not in agreement with therequirements of IMPCA002:98. The average recovery of the chloride content(calculated from the difference between the assigned value for the originalsample #0844 and the spiked sample #0845 and the theoretical increment of0.52 mg Cl/kg) is good (104%). The individual recoveries vary over a large





range. The same was found in previous proficiency tests. Experience hasshown that very low levels of chloride are very difficult to determine withaccuracy by means of turbidimetry. The best technique for anorganic chloridewith the highest accuracy is the IMPCA method using dedicated titrationequipment.

Appearance: No analytical problems were observed. All labs agreed about the appearance ofthe sample #0844: bright, clear and free of suspended matter.

Carbonisable Substances: This determination is problematic for one laboratory. Only oneresult was outside the reproducibility limits. The observed reproducibility is, afterrejection of the statistical outlier, almost in agreement with the requirements of

ASTM E346:03e1. The rounding of the result is probably the cause that thespread is relativity large.

Colour: No analytical problems were observed. No results were found outside thereproducibility limits. The observed reproducibility is in good agreement with therequirements of ASTM D1209:05e1.

Density @ 20 oC: This determination was problematic only for one laboratory. Only one result wasoutside the reproducibility limits and the observed reproducibility is, afterrejection 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 bothsamples, in total only one result was outside the reproducibility limits. Allcalculated reproducibilities (for IBP and DP, automated and manual mode) aregood in agreement with the requirements for automated and manual modes of

ASTM D1078:05. This remarkable as obviously several participants did notcorrect for barometric pressure: the theoretical mid boiling point of 64.5ºC forMethanol was not included in the reported IBP-DP range (see table 3 in ASTMD1078).

Water Miscibility: No analytical problems were observed. All laboratories reported the test as“pass”, except one that reported “complete”. This may be remarkable as thesample #0844 contained 0.1% Toluene.

NVM: This determination is problematic for only one laboratory. Only one result wasoutside the reproducibility limits. The reproducibility is, after rejection of thestatistical 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 theapplicability range, it is therefore difficult to draw any conclusions. Therefore, noz-scores were calculated.





SG 20/20 oC: No analytical problems were observed. No results were outside thereproducibility limits and the calculated reproducibility is in good agreement withthe requirements of ASTM D4052:02e1.The Specific Gravity is defined as: “ the ratio of the weight in Vacuum of a unitvolume of a material at stated temperature to the weight in Vacuum of an equalvolume 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 reproducibilitylimits and the calculated reproducibility is in good agreement with therequirements 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 equaldensity 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 at20 oC - 0.00120).

SG General: When the Specific Gravities and Apparent Specific Gravities were calculatedfrom the reported Densities, it was noticed that the reported results for theSpecific Gravity 20/20 oC and Apparent Specific Gravity 20/20 oC are in line withthe calculated results. Users of method ASTM D891 should be aware that thismethod results in Apparent Specific Gravity. To arrive at Specific Gravity orDensity an additional conversion is necessary. The method provides thecalculation formula.

Sulphur: As ASTM D3961:98 was withdrawn in 2004 with no replacement, it was decidedby the IMPCA group to prepare a new IMPCA method for the determination ofSulphur based on ASTM D3961. The draft version of this IMPCA005:08 wassent 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 mgSulphur/kg). Sample #0845 should be used as blank. On the report form it wasrequested to determine the Sulphur content according this draft method andalso according the usually used test method.For sample #0844 the determination of Sulphur according the usually used testmethod is problematic. Although all results are within the reproducibility limits,the calculated reproducibility is not in agreement with the requirements of ASTMD5453:08b. For sample #0845 no suitable conclusions can be made as theconsensus value found is below or near the detection limit of the method.The average recovery of the Sulphur (calculated from the difference betweenthe consensus value for the original sample #0844 and the spiked sample





#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 methodIMPCA005:08, of which three ‘less than’ results. Therefore it was not possible todraw any significant conclusions, except for the fact that the mean from thethree numerical results for sample #0844 is the same as the amount of Sulphurspiked to this sample.

Total Iron: This determination may be problematic. Nine results are outside thereproducibility limits. The calculated reproducibility is, after rejection of thestatistical outliers not at all in agreement with the requirements of ASTME394:04. However, the consensus value is closed to the detection limit of thedetermination.

Water (coul.): This determination is problematic. Seven results were outside the reproducibilitylimits. The calculated reproducibility is, even after rejection of the statisticaloutliers, not at all in agreement with the strict requirements of ASTM E1064:05.

Water (titr.): This determination is not problematic. No results were outside thereproducibility limits. The calculated reproducibility is, after rejection of thestatistical outlier, in agreement with the requirements of ASTM E203:01.

Purity “as is” and “on db”: These determinations are very problematic as the group istrimodally divided. This phenomenon can be easily explained as manyparticipants 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 wasadded during the spiking of Sulphur to this sample. The run time of the GCmethod IMPCA001 is obviously too short. The run is stopped just before theelution of toluene. Other participants that did not follow IMPCA001 detectedToluene (group2 in the Kernel density plot or results around 99.86%M/M). Notall participants that detected Toluene used the true response factor, thusresulting in a very low purity (group1 in the Kernel density plot or results around99.64%M/M).

Benzene: This determination is somewhat problematic. Although, no results were outsidethe reproducibility limits, the calculated reproducibility is not in agreement withthe strict estimated reproducibility limits calculated using the Horwitz equation.The average recovery of the Benzene and the theoretical increment of 10.4 mgBenzene/kg may be satisfactory (the actual blank Benzene content isunknown).

Ethanol: This determination is problematic. For both samples in total eight results wereoutside the estimated reproducibility limits calculated using the Horwitzequation. Both the calculated reproducibilities are, after rejection of thestatistical outliers, not at all in agreement with the estimated reproducibility





limits calculated using the Horwitz equation. The concentrations found for bothsamples differ not significantly, which was expected as this component was notspiked. The fact that the ratio R/r is almost 3, suggests that random andsystematic errors are both equally present.

Acetone: For both samples, no significant conclusions can be drawn as only resp. eightand nine numerical results were reported and the averages found are bothbelow 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 geta 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 thisdetermination, which are both allowed in IMPCA004:05. As the results of thedeterminations for 268.5nm, 250nm and 220nm are divided into two groups, theresults per determination were split and evaluated separately.

Almost all UV absorbance determinations were very problematic. Only thecalculated reproducibilities for UV at 300nm and 220nm using a 50mm cuvetwere in agreement with the requirements of IMPCA004:06. All other calculatedreproducibilities were, even after rejection for the statistical outliers, not at all inagreement with IMPCA004:06.

4.2 P ERFORMANCE EVALUATION FOR THE GROUP OF LABORATORIES

A comparison has been made between the reproducibility as declared by the relevant standardand the reproducibility as found for the group of participating laboratories. The average resultsper sample, calculated reproducibilities and reproducibilities derived from literature standards (incasu ASTM standards) are compared in the next tables.





Parameter unit n 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 0.30Carbonisable Substances Pt/Co 31 6.9 6.1 5.0

Colour Pt/Co 36 2.3 4.1 7.0

Density @ 20 oC kg/L 51 0.79133 0.00031 0.00050

Initial Boiling Point (automatic) °C 24 64.36 0.61 1.00

Dry Point (automatic) °C 23 64.77 0.56 0.69

Initial Boiling Point (manual) °C 20 64.37 0.24 0.69

Dry Point (manual) °C 19 64.84 0.49 0.84

Nonvolatile Matter mg/100 mL 29 0.51 1.34 2.40

Permanganate Time Test minutes 46 98.6 51.2 unknownSpecific Gravity 20/20 °C 44 0.79273 0.00031 0.00050

Apparent Spec.Grav.20/20 °C 17 0.79248 0.00028 0.00050

Sulphur (D5354), #0844 mg/kg 22 1.03 0.71 0.59

Sulphur (IMPCA005), #0844 mg/kg 3 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




UV absorbance at 268.5 nm (10 mm cuvet) 11 0.0059 0.0091 0.0016UV absorbance at 250 nm (10 mm cuvet) 11 0.0300 0.0163 0.0030

UV absorbance at 220 nm (10 mm cuvet) 11 0.2337 0.0463 0.0671table 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 goodcompliance of the group of participating laboratories with the relevant standards. The tests thatare problematic have been discussed in paragraph 4.1.





4.3 C OMPARISON OF THE PROFICIENCY TEST OF S EPTEMBER 2008 WITH PREVIOUS PT ’S

September2008

September2007

September2006

September2005

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 therequirements 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 oC ++ ++ ++ ++

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 -- n.e. -- ++ --

Water (coulometric) -- -- -- --

Water (titrimetric) ++ ++ ++ ++

Benzene -- n.d. n.d. n.d.

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 islisted 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 standardn.e.: not evaluated





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APPENDIX 1 Determination of Appearance on sample #0844 ;

lab method value mark z(targ) remarks52 IMPCA003 CFSM -----

150 visual B&C -----153 ----- -----171 IMPCA003 C&F -----174 IMPCA003 C&F -----273 visual B&C -----311 IMPCA003 C&F -----319 IMPCA003 CFSM -----323 IMPCA003 CFFMS -----332 ----- -----333 ----- -----334 ----- -----342 visual CFFSM -----343 ----- -----345 IMPCA003 CFSM -----346 ----- -----347 visual CFSM -----357 IMPCA003 CFSM -----372 IMPCA003 CFSM -----395 IMPCA003 CFSM -----

443 IMPCA003 CFSM -----444 IMPCA003 pass -----445 visual B&C -----446 IMPCA003 pass -----468 visual CFFMIS -----494 IMPCA003 B&C -----528 visual CFSM -----529 visual CFSM -----608 visual CFSM -----609 visual CFSM -----646 IMPCA003 CFFSM -----657 IMPCA003 CFSM -----663 IMPCA003 B&C -----786 ----- -----823 visual CFSM -----824 IMPCA003 CFSM -----

825 IMPCA003 CFSM -----857 IMPCA003 CFFSM -----858 IMPCA003 CFFSM -----859 IMPCA003 CFFSM -----862 IMPCA003 CFFSM -----864 IMPCA003 CFFSM -----867 IMPCA003 CFSM -----902 ----- -----963 IMPCA003 CFFSM -----971 IMPCA003 CFSM -----974 IMPCA003 CFFSM -----

1004 IMPCA003 clear -----1007 in house pass -----1009 IMPCA003 CFSM -----1010 IMPCA003 CFSM -----1016 ----- -----

1029 visual clear -----1041 IMPCA003 CFSM -----1102 IMPCA003 CFSM -----1108 ----- -----1149 ----- -----1204 IMPCA003 CSF -----1510 visual CBFFSM -----1615 IMPCA003 C&C -----1712 ----- -----1728 visual clear -----1905 in house NOSMS -----1931 ----- -----

Abbreviations:normality n.a CFSM Clear Free of Suspended Mattern 51 B&C/C&F/C&C Bright&Clear / Clear&Free / Clear&Colourlessoutliers 0 CFFMS/SM/MIS Clear Free From Suspended Mattermean (n) n.a. CBFFSM Clear Bright Free From Suspended Matterst.dev. (n) n.a. CSF Clear with Suspended FiberR(calc.) n.a. NOSMS No Opalescence, Suspended MatterR(IMPCA003:98) n.a.





Determination of Acidity as Acetic Acid on sample #0844; results in mg/kglab method value mark z(targ) remarks52 D1613 15 0.67

150 D1613 9.1 -0.51153 D1613 27 U,G(0.01) 3.07 Reported 0.0027171 D1613 11.3 -0.07174 D1613 10.9 -0.15

273 D1613 12 0.07311 D1613 12 0.07319 D1613 9 -0.53323 D1613 14 0.47332 ----- -----333 ----- -----334 ----- -----342 D1613 13.7 0.41343 ----- -----345 D1613 16 0.87346 ----- -----347 D1613 10.1 -0.31357 D1613 9 -0.53372 D1613 12 0.07395 D1613 10.6 -0.21443 ----- -----444 D1613 12.2 0.11445 ----- -----446 E346 13 0.27468 D1613 12.13 0.10494 D1613 5 -1.33528 D1613 15.1677 0.70529 D1613 16.679 1.01608 D1613 10.25 -0.28609 D1613 9.09 -0.51646 D1613 13.6 0.39657 D1613 15 C 0.67 First reported 19663 D1613 12.11 0.09786 ----- -----823 D1613 11 -0.13824 D1613 11 -0.13825 D1613 12 C 0.07 First reported 21857 D1613 11 -0.13858 D1613 11 -0.13859 D1613 10.6 -0.21862 D1613 11 -0.13864 D1613 11.6 -0.01867 D1613 8.8 -0.57902 ----- -----963 D1613 8.02 -0.73971 ----- -----974 D1613 17.98 1.27

1004 D1613 12 0.071007 in house 12 0.071009 D1613 17 1.071010 D1613 9 -0.531016 D1613 12.49 0.171029 D1613 8.3 -0.671041 D1613 11 -0.131102 D1613 9.85 -0.361108 ----- -----1149 ----- -----1204 D1613 8.713 -0.591510 D1613 8 -0.731615 D1613 7.50 -0.831712 D1613 15 U 0.67 Reported 0.00151728 D1613 20 1.671905 D1613 11.9 0.051931 D1613 8.4 -0.65

normality not OKn 51outliers 1mean (n) 11.65st.dev. (n) 2.898

R(calc.) 8.11R(D1613:06) 14.00





Kernel Density

0

0.02

0.04

0.06

0.08

0.1

0.12

0.14

0.16

0 10 20 30 40

0

5

10

15

20

25

30

4 9 4

1 6 1 5

1 5 1 0

9 6 3

1 0 2 9

1 9 3 1

1 2 0 4

8 6 7

3 5 7

1 0 1 0

3 1 9

6 0 9

1 5 0

1 1 0 2

3 4 7

6 0 8

8 5 9

3 9 5

1 7 4

8 6 2

8 2 3

8 2 4

8 5 8

8 5 7

1 0 4 1

1 7 1

8 6 4

1 9 0 5

2 7 3

3 1 1

1 0 0 7

1 0 0 4

8 2 5

3 7 2

6 6 3

4 6 8

4 4 4

1 0 1 6

4 4 6

6 4 6

3 4 2

3 2 3

6 5 7

5 2

1 7 1 2

5 2 8

3 4 5

5 2 9

1 0 0 9

9 7 4

1 7 2 8

1 5 3





Determination of Anorganic Chloride as Cl on sample #0844 and sample #0845; results in mg/kglab method #0844 mark z(targ) #0845 mark z(targ) Recov % remarks52 IMPCA002 0 .2 C 1.02 0.9 2.53 156 Firs t repor ted 0.4

150 IMPCA002 <0.3 ----- 0.6 -0.27 98153 ----- ----- ----- -----171 IMPCA002 <0.1 ----- 0.88 2.34 152174 IMPCA002 0.11 0.18 0.89 2.44 154

273 ----- ----- ----- -----311 IMPCA002 <0.25 ----- 0.64 0.10 106319 IMPCA002 0.07 -0.20 0.69 0.57 115323 IMPCA002 <0.25 C ----- 1.0 G(0.05) 3.46 175 First reported 0.5332 ----- ----- ----- -----333 ----- ----- ----- -----334 IMPCA002 0.14 0.46 ----- -----342 ----- ----- ----- -----343 IMPCA002 0.26 1.58 0.76 1.22 129345 ----- ----- ----- -----346 ----- ----- ----- -----347 ----- ----- ----- -----357 IMPCA002 <0.25 ----- 0.6 -0.27 98372 IMPCA002 <0.25 ----- 0.65 0.20 108395 in house 0.05 -0.38 0.49 -1.30 77443 IMPCA002 <0.20 ----- ----- -----444 IMPCA002 <0.1 ----- 0.58 -0.46 94445 ----- ----- ----- -----446 ----- ----- ----- -----468 ----- ----- ----- -----494 IMPCA002 <0.25 ----- 0.60 -0.27 98528 in house 0.031677 -0.56 ----- -----529 ----- ----- ----- -----608 Turbidimetric <0.1 ----- 0.57 -0.55 92609 IMPCA002 <0.1 C - ---- 0.544 -0.79 87 Firs t repor ted 0.506646 IMPCA002 0.14 0.46 0.64 0.10 106657 inh-005 <1 ----- <1 <3.46663 IMPCA002 <0.25 ----- ----- -----786 ----- ----- ----- -----823 IMPCA002 <0.25 ----- 0.61 -0.18 100824 Turbidity meter 0.1 0.08 ----- -----825 IMPCA002 <0.1 ----- 0.68 0.48 113857 IMPCA002 0.06 -0.29 0.58 -0.46 94858 ----- ----- ----- -----859 IMPCA002 0.05 -0.38 0.61 -0.18 100862 IMPCA002 0.06 -0.29 0.62 -0.08 102864 IMPCA002 <0.25 ----- 0.64 0.10 106867 IMPCA002 <0.25 ----- 0.655 0.24 109902 ----- ----- ----- -----963 ----- ----- ----- -----971 ----- ----- ----- -----974 ----- ----- ----- -----

1004 in house 0.009 -0.77 ----- -----1007 in house 0.05 -0.38 0.11 G(0.05) -4.84 41009 in house 0.069 -0.21 0.62 -0.08 1021010 Turbidity meter <0.25 ----- >0.25 -----1016 ----- ----- ----- -----1029 IMPCA002 <0.10 ----- 0.5723 -0.53 931041 ----- ----- ----- -----1102 IMPCA002 0.06 -0.29 ----- -----1108 ----- ----- ----- -----1149 ----- ----- ----- -----1204 ----- ----- ----- -----1510 ----- ----- ----- -----1615 IMPCA002 n.d. ----- 0.408 -2.06 611712 ----- ----- ----- -----1728 in house 0.468 G(0.01) 3.52 0.320 -2.88 <01905 ----- ----- ----- -----1931 ----- ----- ----- -----

normality not OK not OKn 16 26outliers 1 2 Spikemean (n) 0.09 0.63 0.52 (0.63-0.09) / 0.52 * 100 = 104%st.dev. (n) 0.066 0.129

R(calc.) 0.18 0.36R(IMPCA002:98) 0.30 0.30





Kernel Density#0844

0

1

2

3

4

5

6

7

8

-0.2 0 0.2 0.4 0.6 0.8

Kernel Density#0845

0

0.5

1

1.5

2

2.5

3

3.5

-0.5 0 0.5 1 1.5

0

0. 05

0. 1

0. 15

0. 2

0. 25

0. 3

0. 35

0. 4

0. 45

0. 5

1 0 0 4

5 2 8

3 9 5

8 5 9

1 0 0 7

8 6 2

8 5 7

1 1 0 2

1 0 0 9

3 1 9

8 2 4

1 7 4

3 3 4

6 4 6

5 2

3 4 3

1 7 2 8

Anorganic Chloride as Cl on #0844

0

0.2

0.4

0.6

0.8

1

1.2

1 0 0 7

1 7 2 8

1 6 1 5

3 9 5

6 0 9

6 0 8

1 0 2 9

8 5 7

4 4 4

4 9 4

1 5 0

3 5 7

8 2 3

8 5 9

8 6 2

1 0 0 9

6 4 6

8 6 4

3 1 1

3 7 2

8 6 7

8 2 5

3 1 9

3 4 3

1 7 1

1 7 4

5 2

3 2 3

Anorganic Chloride as Cl on #0845





Determination of Carbonisable Substances Pt/Co on sample #0844;lab method value mark z(targ) remarks52 E346 10 1.72

150 E346 8 0.60153 E346 5 -1.08171 E346 5 -1.08174 E346 5.5 -0.80

273 ----- -----311 E346 5 -1.08319 E346 <5 <-1.08323 E346 5 -1.08332 ----- -----333 E346 10 1.72334 ----- -----342 ----- -----343 ----- -----345 ----- -----346 ----- -----347 ----- -----357 E346 5 -1.08372 E346 7 0.04395 E346 10 1.72443 ----- -----444 E346 10 1.72445 ----- -----446 E346 10 1.72468 ----- -----494 E346 <0.1 ----- Deviating unit reported??528 E346 20 G(0.01) 7.32529 ----- -----608 E346 <5 <-1.08609 E346 6.6 -0.18646 E346 7 0.04657 E346 10 1.72663 ----- -----786 ----- -----823 E346 5 -1.08824 E346 5 -1.08825 ----- -----857 E346 5 -1.08858 E346 5 -1.08859 E346 7 0.04862 E346 6 -0.52864 E346 <10 <1.72867 E346 5 -1.08902 ----- -----963 ----- -----971 ----- -----974 ----- -----

1004 E346 <5 <-1.081007 in house 10 1.721009 E346 <30 -----1010 E346 5 -1.081016 ----- -----1029 E346 10 1.721041 E346 5 -1.081102 ----- -----1108 ----- -----1149 ----- -----1204 E346 5 -1.081510 ----- -----1615 E346 10 C 1.72 First reported 11712 ----- -----1728 E346 5 -1.081905 E346 7.5 0.321931 ----- -----


R(calc.) 6.1R(E346:03e1) 5.0





Kernel Density

0

0.02

0.04

0.06

0.08

0.1

0.12

0.14

0.16

0.18

0 10 20 30

0

5

10

15

20

25

8 6 7

1 0 1 0

3 5 7

8 5 8

8 2 3

8 2 4

8 5 7

1 0 4 1

1 7 1

1 7 2 8

1 2 0 4

1 5 3

3 2 3

3 1 1

1 7 4

8 6 2

6 0 9

8 5 9

3 7 2

6 4 6

1 9 0 5

1 5 0

1 0 2 9

3 3 3

5 2

1 6 1 5

4 4 6

6 5 7

4 4 4

1 0 0 7

3 9 5

5 2 8





Determination of Colour as Pt/Co on sample #0844;lab method value mark z(targ) Remarks52 D1209 <5 -----

150 D1209 1 -0.51153 D1209 <2 -----171 D1209 1 -0.51174 D1209 1.1 -0.47

273 D1209 5 1.09311 D1209 <5 -----319 D1209 2 -0.11323 D1209 <5 -----332 ----- -----333 ----- -----334 D1209 1 -0.51342 D1209 3 0.29343 ----- -----345 D1209 <5 -----346 ----- -----347 D1209 2 -0.11357 D1209 <5 -----372 D1209 2 -0.11395 D1209 <5 -----443 D1209 <5 -----444 D5386 2 -0.11445 D1209 <5 -----446 D1209 <5 -----468 D1209 <5 -----494 D1209 0 -0.91528 D1209 1.5 -0.31529 D1209 1.5 -0.31608 D1209 <5 -----609 D1209 2.0 -0.11646 D1209 3 0.29657 D1209 5 1.09663 D1209 0 -0.91786 ----- -----823 D1209 <3 -----824 D1209 1 -0.51825 D1209 3 0.29857 D1209 5 1.09858 D1209 2 -0.11859 D1209 2 -0.11862 D1209 2 -0.11864 D1209 <5 -----867 D1209 3 0.29902 ----- -----963 D1209 4 0.69971 ----- -----974 D1209 <5 -----

1004 D1209 5 1.091007 in house 5 1.091009 D1209 <5 -----1010 D1209 <5 -----1016 D1209 3.35 0.431029 D1209 1 -0.511041 ISO6271 <5 -----1102 ----- -----1108 D1209 4 0.691149 ----- -----1204 D1209 1 -0.511510 D1209 1 -0.511615 D1209 1 -0.511712 ----- -----1728 D1209 2 -0.111905 D1209 2.5 0.091931 D1209 1 -0.51


R(calc.) 4.1R(D1209:05e1) 7.0





Kernel Density

0

0.05

0.1

0.15

0.2

0.25

0.3

0.35

-4 -2 0 2 4 6 8

0

2

4

6

8

10

12

14

16

18

20

6 6 3

4 9 4

1 0 2 9

8 2 4

1 6 1 5

1 9 3 1

1 2 0 4

1 5 1 0

1 7 1

3 3 4

1 5 0

1 7 4

5 2 8

5 2 9

1 7 2 8

8 5 8

8 5 9

3 1 9

8 6 2

3 4 7

4 4 4

6 0 9

3 7 2

1 9 0 5

6 4 6

8 2 5

3 4 2

8 6 7

1 0 1 6

9 6 3

1 1 0 8

6 5 7

8 5 7

2 7 3

1 0 0 7

1 0 0 4





Determination of Density at 20 oC on sample #0844; results in kg/Llab method value mark z(targ) remarks52 D4052 0.7914 0.40

150 D4052 0.7911 -1.28153 D4052 0.7955 G(0.01) 23.36171 D4052 0.7913 -0.16174 D4052 0.7914 0.40

273 D4052 0.7915 0.96311 D4052 0.7914 0.40319 ----- -----323 D4052 0.7913 -0.16332 ----- -----333 D4052 0.7914 0.40334 D4052 0.7916 1.52342 D4052 0.7911 -1.28343 ----- -----345 ----- -----346 D1298 0.7913 -0.16347 D4052 0.7913 -0.16357 D4052 0.7912 -0.72372 D4052 0.7913 -0.16395 D4052 0.7913 -0.16443 ----- -----444 D4052 0.7914 0.40445 D4052 0.7913 -0.16446 D4052 0.7913 -0.16468 D4052 0.7913 -0.16494 D4052 0.791 -1.84528 D4052 0.79131 -0.10529 D4052 0.7914 0.40608 D4052 0.79133 0.01609 D4052 0.79128 -0.27646 ----- -----657 D4052 0.7914 0.40663 D4052 0.7914 0.40786 ----- -----823 D4052 0.7914 0.40824 D4052 0.7914 0.40825 D4052 0.7913 -0.16857 D4052 0.79134 0.07858 D4052 0.79132 -0.05859 D4052 0.79132 -0.05862 D4052 0.7913 -0.16864 D4052 0.79131 -0.10867 D4052 0.79138 0.29902 ----- -----963 D4052 0.7913 -0.16971 D4052 0.7913 -0.16974 D4052 0.7913 -0.16

1004 ----- -----1007 in house 0.79139 0.351009 ----- -----1010 D4052 0.7912 -0.721016 ----- -----1029 D4052 0.79126 -0.381041 D4052 0.79132 -0.051102 D4052 0.7912 -0.721108 D4052 0.79133 0.011149 ----- -----1204 D4052 0.7914 0.401510 IP365 0.7915 0.961615 D4052 0.79124 -0.491712 D4052 0.79133 U 0.01 Reported 791.331728 D4052 0.7913 -0.161905 D4052 0.79128 -0.271931 D4052 0.7917 2.08


R(calc.) 0.00031R(D4052:02e1) 0.00050





Kernel Density

0

1000

2000

3000

4000

5000

6000

0.7905 0.791 0.7915 0.792 0.7925 0.793

0.79

0. 7905

0. 791

0. 7915

0. 792

0. 7925

0. 793

4 9 4

3 4 2

1 5 0

1 0 1 0

1 1 0 2

3 5 7

1 6 1 5

1 0 2 9

6 0 9

1 9 0 5

9 7 1

4 6 8

4 4 6

9 6 3

8 6 2

8 2 5

9 7 4

4 4 5

3 2 3

3 4 6

1 7 2 8

1 7 1

3 4 7

3 9 5

3 7 2

5 2 8

8 6 4

8 5 8

8 5 9

1 0 4 1

6 0 8

1 1 0 8

1 7 1 2

8 5 7

8 6 7

1 0 0 7

1 2 0 4

3 3 3

4 4 4

3 1 1

5 2

1 7 4

6 6 3

8 2 3

6 5 7

5 2 9

8 2 4

2 7 3

1 5 1 0

3 3 4

1 9 3 1

1 5 3





Determination of IBP and DP (automated) @ 760 mmHg on sample #0844; results in °C lab method IBP mark z(targ) DP mark z(targ) remarks52 D1078 64.3 -0.17 64.6 -0.70

150 D1078 64.4 0.10 64.8 0.11153 ----- ----- ----- -----171 ----- ----- ----- -----174 ----- ----- ----- -----

273 ----- ----- ----- -----311 D1078 64.5 0.38 64.7 -0.30319 ----- ----- ----- -----323 ----- ----- ----- -----332 ----- ----- ----- -----333 D1078 64.6 0.66 64.8 0.11 See paragraph 4.1334 D1078 64.5 0.38 64.1 ex -2.72 Result DP excluded as DP < IBP342 ----- ----- ----- -----343 ----- ----- ----- -----345 D1078 64.5 0.38 64.8 0.11346 ----- ----- ----- -----347 D1078 64.4 0.10 64.8 0.11357 D1078 64.5 0.38 64.8 0.11372 D1078 64.4 0.10 64.8 0.11395 ----- ----- ----- -----443 ----- ----- ----- -----444 ----- ----- ----- -----445 ----- ----- ----- -----446 D1078 64.5 0.38 64.9 0.51468 D1078 64.3 -0.17 64.8 0.11494 D1078 63.8 -1.57 64.3 -1.91 See paragraph 4.1528 ----- ----- ----- -----529 ----- ----- ----- -----608 ----- ----- ----- -----609 ----- ----- ----- -----646 ----- ----- ----- -----657 ----- ----- ----- -----663 ----- ----- ----- -----786 ----- ----- ----- -----823 D1078 64.4 0.10 64.8 0.11824 D1078 64.5 0.38 65.0 0.91825 D1078 64.4 0.10 65.0 0.91857 ----- ----- ----- -----858 ----- ----- ----- -----859 ----- ----- ----- -----862 ----- ----- ----- -----864 ----- ----- ----- -----867 ----- ----- ----- -----902 ----- ----- ----- -----963 ----- ----- ----- -----971 ----- ----- ----- -----974 ----- ----- ----- -----

1004 ----- ----- ----- -----1007 in house 64.7 0.94 65.3 2.13 See paragraph 4.11009 D1078 64.2 -0.45 64.6 -0.701010 D1078 64.5 0.38 64.8 0.111016 ----- ----- ----- -----1029 D1078 64.4 0.10 64.8 0.111041 ----- ----- ----- -----1102 D1078 64.4 0.10 64.8 0.111108 D1078 63.8 -1.57 64.4 -1.51 See paragraph 4.11149 ----- ----- ----- -----1204 ----- ----- ----- -----1510 D1078 64.4 0.10 64.7 -0.301615 D1078 64.1 -0.73 64.6 -0.701712 ----- ----- ----- -----1728 ----- ----- ----- -----1905 D1078 64.2 -0.45 64.9 0.511931 ----- ----- ----- -----

normality not OK not OKn 24 23outliers 0 0mean (n) 64.36 64.77st.dev. (n) 0.216 0.200

R(calc.) 0.61 0.56R(D1078:05-A) 1.00 0.69





Kernel DensityIBP

0

0.5

1

1.5

2

2.5

3

63.5 64 64.5 65 65.5 66

Kernel DensityDP

0

0.5

1

1.5

2

2.5

3

3.5

63.5 64 64.5 65 65.5 66

63

63. 5

64

64. 5

65

65. 5

4 9 4

1 1 0 8

1 6 1 5

1 0 0 9

1 9 0 5

4 6 8

5 2

8 2 3

8 2 5

1 5 1 0

1 1 0 2

1 0 2 9

3 7 2

3 4 7

1 5 0

3 4 5

3 1 1

3 3 4

3 5 7

4 4 6

8 2 4

1 0 1 0

3 3 3

1 0 0 7

Initial Boiling Point

63

63. 5

64

64. 5

65

65. 5

66

3 3 4

4 9 4

1 1 0 8

5 2

1 0 0 9

1 6 1 5

1 5 1 0

3 1 1

8 2 3

1 1 0 2

1 0 2 9

1 0 1 0

3 4 7

3 5 7

3 4 5

3 3 3

1 5 0

3 7 2

4 6 8

1 9 0 5

4 4 6

8 2 4

8 2 5

1 0 0 7

Dry Point





Determination of IBP and DP (manual) @ 760 mmHg on sample #0844; results in °Clab method IBP mark z(targ) DP mark z(targ) remarks52 ----- ----- ----- -----

150 ----- ----- ----- -----153 ----- ----- ----- -----171 ----- ----- ----- -----174 ----- ----- ----- -----

273 D1078 64.3 -0.28 65.0 0.53311 ----- ----- ----- -----319 D1078 64.6 0.94 65.0 0.53 See paragraph 4.1323 ----- ----- ----- -----332 ----- ----- ----- -----333 ----- ----- ----- -----334 ----- ----- ----- -----342 D1078 64.4 0.13 64.8 -0.14343 ----- ----- ----- -----345 ----- ----- ----- -----346 ----- ----- ----- -----347 ----- ----- ----- -----357 ----- ----- ----- -----372 ----- ----- ----- -----395 D1078 64.4 0.13 64.8 -0.14443 ----- ----- ----- -----444 D1078 64.3 -0.28 64.6 -0.80445 D1078 64.4 0.13 64.8 -0.14446 ----- ----- ----- -----468 ----- ----- ----- -----494 ----- ----- ----- -----528 D1078 64.4 0.13 65.2 1.19529 ----- ----- ----- -----608 ----- ----- ----- -----609 D1078 64.4 0.13 64.9 0.19646 D1078 64.38 0.05 64.57 -0.90657 D1078 64.2 -0.69 64.8 -0.14663 ----- ----- ----- -----786 ----- ----- ----- -----823 ----- ----- ----- -----824 ----- ----- ----- -----825 ----- ----- ----- -----857 D1078 64.3 -0.28 64.7 -0.47858 D1078 64.3 -0.28 64.7 -0.47859 D1078 64.4 0.13 64.8 -0.14862 D1078 64.4 0.13 64.7 -0.47864 D1078 64.4 0.13 64.8 -0.14867 D1078 64.3 -0.28 64.8 -0.14902 ----- ----- ----- -----963 D1078 64.3 -0.28 65.6 DG(0.01) 2.52971 ----- ----- ----- -----974 D1078 54.4 C,G(0.01) -40.53 65.6 C,DG(0.01) 2.52 First reported 63.8 and 70.0

1004 D1078 64.3 -0.28 64.8 -0.141007 ----- ----- ----- -----1009 ----- ----- ----- -----1010 ----- ----- ----- -----1016 ----- ----- ----- -----1029 ----- ----- ----- -----1041 ----- ----- ----- -----1102 ----- ----- ----- -----1108 ----- ----- ----- -----1149 ----- ----- ----- -----1204 D1078 64.39 0.09 65.22 C 1.26 First reported 65.891510 ----- ----- ----- -----1615 ----- ----- ----- -----1712 ----- ----- ----- -----1728 D1078 64.5 0.53 65.0 0.531905 ----- ----- ----- -----1931 ----- ----- ----- -----


R(calc.) 0.24 0.49R(D1078:05-M) 0.69 0.84





Kernel DensityIBP

0

1

2

3

4

5

6

63.5 64 64.5 65 65.5 66

63

63. 5

64

64. 5

65

65. 5

66

6 4 6

4 4 4

8 5 7

8 6 2

8 5 8

8 5 9

3 4 2

8 6 4

1 0 0 4

8 6 7

3 9 5

4 4 5

6 5 7

6 0 9

1 7 2 8

3 1 9

2 7 3

5 2 8

1 2 0 4

9 7 4

9 6 3

Dry Point

63

63. 5

64

64. 5

65

65. 5

9 7 4

6 5 7

8 5 8

8 5 7

1 0 0 4

9 6 3

8 6 7

2 7 3

4 4 4

6 4 6

1 2 0 4

8 6 4

3 9 5

3 4 2

5 2 8

6 0 9

4 4 5

8 6 2

8 5 9

1 7 2 8

3 1 9

Initial Boiling Point

Kernel DensityDP

0

0.5

1

1.5

2

2.5

63.5 64 64.5 65 65.5 66





-- empty page --





Determination of Water Miscibility on sample #0844;lab method value mark z(targ) remarks52 D1722 pass -----

150 D1722 pass -----153 D1722 pass -----171 D1722 pass -----174 D1722 pass -----

273 D1722 pass -----311 D1722 pass -----319 ----- -----323 ----- -----332 ----- -----333 ----- -----334 ----- -----342 D1722 pass -----343 ----- -----345 D1722 pass -----346 ----- -----347 D1722 pass -----357 D1722 pass -----372 D1722 pass -----395 D1722 pass -----443 D1722 pass -----444 D1722 pass -----445 D1722 pass -----446 D1722 pass -----468 D1722 pass -----494 D1722 pass -----528 E346 pass -----529 D1722 pass -----608 D1722 pass -----609 D1722 pass -----646 D1722 pass -----657 D1722 pass -----663 D1722 pass -----786 ----- -----823 D1722 pass -----824 D1722 pass -----825 D1722 pass -----857 D1722 pass -----858 D1722 pass -----859 D1722 pass -----862 D1722 pass -----864 D1722 pass -----867 D1722 pass -----902 ----- -----963 D1722 pass -----971 D1722 pass -----974 D1722 pass -----

1004 D1722 pass -----1007 in house pass -----1009 D1722 pass -----1010 D1722 pass -----1016 D1722 pass -----1029 D1722 pass -----1041 D1722 pass -----1102 ----- -----1108 ----- -----1149 ----- -----1204 D1722 pass -----1510 D1722 pass -----1615 D1722 pass -----1712 ----- -----1728 D1722 complete -----1905 D1722 pass -----1931 ----- -----

normality n.a.n 50outliers 0mean (n) n.a.st.dev. (n) n.a.

R(calc.) n.a.R(D1722:04) n.a.





Determination of Nonvolatile Matter on sample #0844; results in mg/100 mLlab method value mark z(targ) remarks52 D1353 0 ex -0.60 Not a real result

150 D1353 0.2 -0.36153 D1353 0.000 ex -0.60 Not a real result171 D1353 0.2 -0.36174 D1353 0.32 -0.22

273 D1353 <1 -----311 D1353 <1 -----319 D1353 1.43 1.07323 ----- -----332 ----- -----333 D1353 0.7 C 0.22 First reported 9334 ----- -----342 ----- -----343 D1353 2.0 C 1.74 First reported 2.7345 D1353 1.1 0.69346 ----- -----347 ----- -----357 D1353 <1 -----372 D1353 0.3 -0.25395 D1353 0.2 -0.36443 ----- -----444 D1353 0.97 0.54445 ----- -----446 D1353 <1 C ----- First reported <0.001468 D1353 0.2 -0.36494 ----- -----528 D1353 5 U,G(0.01) 5.24 Reported 0.005, probably different unit (%wt instead of mg/100mL)529 ----- -----608 ----- -----609 D1353 0.2 -0.36646 D1353 1 0.57657 D1353 0.2 -0.36663 ----- -----786 ----- -----823 ----- -----824 ----- -----825 D1353 0.2 -0.36857 D1353 0.4 -0.13858 D1353 0.3 -0.25859 D1353 0.4 -0.13862 D1353 0.3 -0.25864 D1353 0.3 -0.25867 D1353 0.3 -0.25902 ----- -----963 ----- -----971 ----- -----974 ----- -----

1004 D1353 1.5 1.151007 in house 0.1 -0.481009 D1353 <1 -----1010 D1353 <0.8 -----1016 D1353 <1 U ----- Reported <0.001, probably different unit (%wt instead of mg/100mL)1029 D1353 0.2 -0.361041 D1353 <1 -----1102 ----- -----1108 ----- -----1149 ----- -----1204 D1353 0.10 -0.481510 D1353 0.33 -0.211615 D1353 0.6 0.101712 ----- -----1728 D1353 0.2 -0.361905 D1353 0.55 0.051931 ----- -----


R(calc.) 1.34R(D1353:03) 2.40





Kernel Density

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Determination of Permanganate Time Test @ 15°C on sample #0844; results in minuteslab method value mark z(targ) remarks52 D1363 67 -----

150 D1363 125 -----153 ----- -----171 D1363 120 -----174 D1363 122 -----

273 D1363 102 -----311 D1363 105 -----319 D1363 150 -----323 D1363mod. >100 -----332 ----- -----333 ----- -----334 ----- -----342 D1363 94 -----343 ----- -----345 D1363 90 -----346 D1363 86 -----347 D1363 96 -----357 D1363 100 -----372 D1363 100 -----395 D1363 102 -----443 D1363 81 C ----- First reported 61444 D1363 90 -----445 D1363 125 -----446 ----- -----468 ----- -----494 D1363 75 -----528 D1363 135 -----529 D1363 116 -----608 D1363 79 -----609 D1363 80 -----646 D1363 107 -----657 D1363 90 -----663 ----- -----786 ----- -----823 ----- -----824 D1363 92 -----825 D1363 70 -----857 D1363 100 -----858 D1363 100 -----859 D1363 105 -----862 D1363 102 -----864 D1363 105 -----867 D1363 107 -----902 ----- -----963 D1363 75.0 -----971 ----- -----974 D1363 110 -----

1004 D1363 105 -----1007 in house 90 -----1009 D1363 98 -----1010 D1363 100 -----1016 ----- -----1029 D1363 100 -----1041 D1363 127 -----1102 D1363 60 -----1108 ----- -----1149 ----- -----1204 D1363 104 -----1510 ----- -----1615 D1363 68 -----1712 D1363 90 C ----- First reported 1351728 D1363 100 -----1905 D1363 92 -----1931 ----- -----

normality OKn 46outliers 0mean (n) 98.6st.dev. (n) 18.27

R(calc.) 51.2R(D1363:06) unknown Compare R(iis07C08) = 39.5 at a mean of 104.9





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0.792 0.7925 0.793 0.7935

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Determination of Specific Gravity, Apparent 20/20 °C/°C on sample #0844;lab method value mark z(targ) remarks52 in house 0.7925 0.12

150 ----- -----153 ----- -----171 D4052 0.79248 0.00174 D4052 0.7926 0.68

273 ----- -----311 ----- -----319 ----- -----323 ----- -----332 ----- -----333 ----- -----334 ----- -----342 D4052 0.7923 -1.00343 ----- -----345 ----- -----346 ----- -----347 ----- -----357 ih-960 0.7925 0.12372 D4052/891 0.7925 0.12395 ----- -----443 ----- -----444 ----- -----445 ----- -----446 ----- -----468 ----- -----494 ----- -----528 D4052 0.79248 0.00529 ----- -----608 ----- -----609 ----- -----646 D891 0.7922 -1.56657 D4052 0.7926 0.68663 ----- -----786 ----- -----823 ----- -----824 ----- -----825 ----- -----857 in house 0.79245 -0.16858 in house 0.79246 -0.11859 D891 0.79246 -0.11862 D891 0.7925 0.12864 D4052 calc. 0.79249 0.06867 D4052 0.79256 0.45902 ----- -----963 ----- -----971 ----- -----974 ----- -----

1004 ----- -----1007 in house 0.7926 0.681009 ----- -----1010 ----- -----1016 ----- -----1029 ----- -----1041 ----- -----1102 ----- -----1108 ----- -----1149 ----- -----1204 ----- -----1510 ----- -----1615 ----- -----1712 ----- -----1728 in house 0.79247 -0.051905 ----- -----1931 ----- -----


R(calc.) 0.00028R(D4052:02e1) 0.00050





Kernel Density

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0.7918 0.792 0.7922 0.7924 0.7926 0.7928 0.793

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Determination of Sulphur on sample #0844 and #0845; results in mg/kglab method #0844 mark z(targ) #0845 mark z(targ) Recovery % remarks52 D5453 1.0 -0.15 <1 ----- 68

150 D5453 1 -0.15 0.1 ----- 68153 ----- ----- ----- -----171 D5453 1.4 1.74 <1 ----- 101174 ----- ----- ----- -----

273 ----- ----- ----- -----311 D5453 1.1 0.32 <1 ----- 76319 ----- ----- ----- -----323 D5453 1.3 C 1.27 <1 ----- 93 First reported 1.7332 ----- ----- ----- -----333 D5453 1.3 1.27 ----- ----- 93334 D5453 1.3 1.27 0.9 G(0.01) ----- 93342 ----- ----- ----- -----343 ----- ----- ----- -----345 ----- ----- ----- -----346 ----- ----- ----- -----347 D5453 0.63 -1.90 <0.5 ----- 38357 D5453 0.8 -1.09 0.2 ----- 52372 D5453 1.0 -0.15 <0.5 ----- 68395 ----- ----- ----- -----443 ----- ----- ----- -----444 D5453 1.18 0.70 0.23 ----- 83445 ----- ----- ----- -----446 ----- ----- ----- -----468 ----- ----- ----- -----494 D5453 1.2 0.80 <1 ----- 85528 ----- ----- ----- -----529 ----- ----- ----- -----608 ----- ----- ----- -----609 D3961 <0.5 <-2.52 ----- ----- <28 False negative646 ----- ----- ----- -----657 D5453 1.2 0.80 <1 ----- 85663 ----- ----- ----- -----786 ----- ----- ----- -----823 ----- ----- ----- -----824 D5453 0.9 -0.62 <0.1 ----- 60825 ----- ----- ----- -----857 ----- ----- ----- -----858 ----- ----- ----- -----859 ----- ----- ----- -----862 D5453 1.1 0.32 <1 ----- 76864 ----- ----- ----- -----867 D5453 1.1 0.32 <1 ----- 76902 ----- ----- ----- -----963 ----- ----- ----- -----971 ----- ----- ----- -----974 ----- ----- ----- -----

1004 ----- ----- ----- -----1007 ----- ----- ----- -----1009 ----- ----- ----- -----1010 in house <0.5 <-2.52 <0.5 ----- <28 False negative1016 ISO20846 1.35 1.51 ----- ----- 971029 D3961 0.49 -2.56 0.04 ----- 271041 D6212 0.76 -1.28 <0.2 ----- 491102 D5453 1.13 0.47 0.12 ----- 791108 D5453 0.8 -1.09 0.3 ----- 521149 ----- ----- ----- -----1204 ----- ----- ----- -----1510 ----- ----- ----- -----1615 ----- ----- ----- -----1712 in house <0.1 <-4.41 ----- ----- <1 False negative1728 D5453 0.65 -1.80 0.1 ----- 401905 ----- ----- ----- -----1931 D5453 <1.0 <-0.15 <1.0 ----- <68

normality OK n.a.n 22 7outliers 0 Spike: 1mean (n) 1.03 1.23 0.16 (1.03 – 0.16) / 1.23 * 100 = 71 %st.dev. (n) 0.254 n.a.

R(calc.) 0.71 n.a.R(D5453:08b) 0.59 unknown





Kernel Density#0844

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-- empty page --





Determination of Sulphur (IMPCA005) on sample #0844 and #0845; results in mg/kglab method #0844 mark z(targ) #0845 mark z(targ) remarks52 ----- ----- ----- -----

150 ----- ----- ----- -----153 ----- ----- ----- -----171 ----- ----- ----- -----174 ----- ----- ----- -----

273 ----- ----- ----- -----311 IMPCA005 1.2 ----- <0.5 -----319 ----- ----- ----- -----323 ----- ----- ----- -----332 ----- ----- ----- -----333 ----- ----- ----- -----334 ----- ----- ----- -----342 ----- ----- ----- -----343 ----- ----- ----- -----345 ----- ----- ----- -----346 ----- ----- ----- -----347 ----- ----- ----- -----357 ----- ----- ----- -----372 ----- ----- ----- -----395 ----- ----- ----- -----443 ----- ----- ----- -----444 ----- ----- ----- -----445 ----- ----- ----- -----446 ----- ----- ----- -----468 ----- ----- ----- -----494 ----- ----- ----- -----528 ----- ----- ----- -----529 ----- ----- ----- -----608 ----- ----- ----- -----609 ----- ----- ----- -----646 IMPCA005 0.94 ----- <0.2 -----657 IMPCA005 <1 ----- <1 -----663 ----- ----- ----- -----786 ----- ----- ----- -----823 ----- ----- ----- -----824 ----- ----- ----- -----825 ----- ----- ----- -----857 D3961 <1 ----- <1 -----858 ----- ----- ----- -----859 IMPCA005 1.5 ----- <0.5 -----862 ----- ----- ----- -----864 ----- ----- ----- -----867 ----- ----- ----- -----902 ----- ----- ----- -----963 ----- ----- ----- -----971 ----- ----- ----- -----974 ----- ----- ----- -----

1004 IMPCA005 mod. <0.01 ----- <0.01 ----- False negative1007 ----- ----- ----- -----1009 ----- ----- ----- -----1010 ----- ----- ----- -----1016 ----- ----- ----- -----1029 ----- ----- ----- -----1041 ----- ----- ----- -----1102 ----- ----- ----- -----1108 ----- ----- ----- -----1149 ----- ----- ----- -----1204 ----- ----- ----- -----1510 ----- ----- ----- -----1615 ----- ----- ----- -----1712 ----- ----- ----- -----1728 ----- ----- ----- -----1905 ----- ----- ----- -----1931 ----- ----- ----- -----

normality n.a. n.a.n 3 0outliers 0 Spike: 0mean (n) 1.21 1.23 n.a.st.dev. (n) 0.280. n.a.

R(calc.) 0.78 n.a.R(lit.) unknown unknown





Determination of Total Iron as Fe on sample #0844; results in mg/kglab method value mark z(targ) remarks52 E394 <0.02 -----

150 E394 <0.01 -----153 ----- -----171 E394 <0.01 -----174 E394 0.01 -1.28

273 ----- -----311 E394 <0.01 -----319 E394 0.025 4.58323 ----- -----332 ----- -----333 ----- -----334 ----- -----342 ----- -----343 ----- -----345 E394 0.01 -1.28346 ----- -----347 ----- -----357 E394 <0.01 -----372 E394 0.013 -0.11395 E394 <0.01 -----443 ----- -----444 ----- -----445 ----- -----446 ----- -----468 ----- -----494 ----- -----528 E394 0.0064 -2.69529 ----- -----608 ----- -----609 E394 0.01 -1.28646 E394 <0.05 -----657 E394 0.07 G(0.05) 22.16663 ----- -----786 ----- -----823 E394 <0.1 -----824 E394 0.03 6.53825 ----- -----857 E394 0.02 2.62858 E394 0.01 -1.28859 E394 0.024 4.19862 E394 0.01 -1.28864 E394 <0.1 -----867 E394 0.002 -4.41902 ----- -----963 ----- -----971 ----- -----974 ----- -----

1004 in house <0.01 -----1007 in house 0.02 2.621009 E394 0.007 -2.451010 E394 <0.1 -----1016 ----- -----1029 E394 <0.10 -----1041 ----- -----1102 E394 0.006 -2.851108 ----- -----1149 ----- -----1204 E394 0.0044 -3.471510 E394 <0.1 -----1615 E394 1.8959 G(0.01) 735.48 False positive1712 ----- -----1728 E394 0.053 G(0.01) 15.521905 E394 0.018 1.841931 ----- -----


R(calc.) 0.0226R(E394:04) 0.0072





Kernel Density

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Determination of Water content (coulometric) on sample #0844; results in mg/kglab method value mark z(targ) remarks52 E1064 177 -1.22

150 E1064 174 -1.48153 ----- -----171 ----- -----174 ----- -----

273 E1064 158 -2.85311 ----- -----319 E1064 187.8 -0.30323 E1064 206 1.26332 ----- -----333 E1064 260 G(0.05) 5.88334 ----- -----342 E1064 189 -0.19343 E1064 193 0.15345 ----- -----346 E1064 183.6 -0.66347 E1064 178 -1.14357 E1064 200 0.75372 E1064 169 -1.91395 E1064 179.9 -0.97443 E346 159.2 U -2.75 Reported 0.01592444 ----- -----445 E1064 190 -0.11446 ----- -----468 E1064 227 3.06494 E1064 218 2.29528 ----- -----529 ----- -----608 E1064 183 -0.71609 E1064 210 1.60646 E1064 200 0.75657 E1064 190 -0.11663 ----- -----786 ----- -----823 E1064 182 -0.79824 ----- -----825 ----- -----857 E1064 200 0.75858 E1064 220 2.46859 E1064 214 1.95862 E1064 209 1.52864 E1064 193 0.15867 E1064 210 U 1.60 Reported 0.021902 ----- -----963 E1064 224 2.80971 ----- -----974 E1064 204 1.09

1004 E1064 270 G(0.05) 6.741007 in house 35 G(0.01) -13.381009 E1064 153 -3.281010 E1064 180.85 U -0.89 Reported 0.0180851016 ----- -----1029 E1064 196 0.411041 E1064 173 -1.561102 E1064 190.7 -0.051108 E1064 206 1.261149 ----- -----1204 E1064 211 1.691510 E1064 175 -1.391615 E1064 153.381 -3.241712 ----- -----1728 ----- -----1905 E1064 192 0.061931 ----- -----


R(calc.) 53.63R(E1064:05) 32.71





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Determination of Water content (titrimetric) on sample #0844; results in mg/kglab method value mark z(targ) remarks52 ----- -----

150 E203 177 -0.23153 E203 414 U,G(0.01) 2.23 Reported 0.0414, probably different unit (Wt% instead of mg/kg)171 E203 174 -0.26174 E203 188 -0.11

273 E203 170 -0.30311 E203 207 0.08319 ----- -----323 E203 201 0.02332 ----- -----333 ----- -----334 ----- -----342 ----- -----343 ----- -----345 D1364 206 0.07346 ----- -----347 ----- -----357 E203 190 -0.09372 E203 177 -0.23395 ----- -----443 ----- -----444 E203 238 0.41445 ----- -----446 E203 213 C 0.15 First reported 0.021468 ----- -----494 ----- -----528 E203 115.3 -0.87529 E203 202.04 0.03608 ----- -----609 ----- -----646 ----- -----657 E203 180 -0.20663 ----- -----786 ----- -----823 E203 204 0.05824 E203 230 0.32825 E203 257 0.60857 E203 210 0.12858 E203 230 0.32859 E203 222 0.24862 E203 214 0.16864 ----- -----867 ----- -----902 ----- -----963 E203 189 -0.10971 ----- -----974 E203 274 0.78

1004 ----- -----1007 ----- -----1009 ----- -----1010 ----- -----1016 D1364 140 -0.611029 ----- -----1041 ----- -----1102 ----- -----1108 ----- -----1149 ----- -----1204 E203 212 0.141510 ----- -----1615 E203 145 C -0.56 First reported 111.921712 ----- -----1728 E203 170 -0.301905 E203 214 0.161931 E203 219 0.21


R(calc.) 94.3R(E203:01) 270.0





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Determination of Purity “as is” on sample #0844; results in %M/Mlab method value mark z(targ) remarks52 ----- -----

150 IMPCA001 99.880 -----153 in house 99.9 -----171 IMPCA001 99.882 -----174 IMPCA001 99.879 -----

273 ----- -----311 ----- -----319 ----- -----323 ih-064 99.88 -----332 ----- -----333 ----- -----334 ----- -----342 ----- -----343 in house 99.62 C ----- First reported 99.979345 ----- -----346 ----- -----347 IMPCA001 99.782 C ----- First reported 99.982357 in house 99.67 -----372 ----- -----395 ----- -----443 ----- -----444 calc. 99.8594 -----445 ----- -----446 ----- -----468 in house 99.815 -----494 in house 99.87 -----528 in house 99.968 -----529 ----- -----608 ----- -----609 in house 99.82 C ----- First reported 99.9822646 ----- -----657 IMPCA001 99.817 -----663 ----- -----786 ----- -----823 in house 99.64 C ----- First reported 99.98 824 in house 99.64 C ----- First reported 99.99 825 IMPCA001 99.65 C ----- First reported 99.97 857 IMPCA001 99.867 -----858 IMPCA001 99.872 -----859 IMPCA001 99.880 -----862 IMPCA001 99.88 -----864 IMPCA001 99.870 -----867 IMPCA001 99.63 -----902 ----- -----963 IMPCA001 99.8476 -----971 ----- -----974 in house 99.8656 -----

1004 ----- -----1007 in house 99.88 -----1009 ----- -----1010 ----- -----1016 ----- -----1029 ----- -----1041 ----- -----1102 ----- -----1108 ----- -----1149 ----- -----1204 calc. 99.9761 -----1510 in house 99.988 -----1615 in house 99.9853 C ----- First reported 99.98471712 ----- -----1728 ----- -----1905 in house 99.978 -----1931 ----- -----

Group 1 Group 2 Group 3normality OK Not OK OKn 6 19 5outliers 0 0 0mean (n) 99.64 99.86 99.98st.dev. (n) 0.017 0.030 0.008

R(calc.) 0.05 0.08 0.02R(lit.) unknown unknown unknown





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Determination of Purity on dry basis on sample #0844; results in %M/Mlab method value mark z(targ) Remarks52 IMPCA001 99.56 -----

150 IMPCA001 99.898 -----153 ----- -----171 IMPCA001 99.898 -----174 IMPCA001 99.898 -----

273 ----- -----311 IMPCA001 99.893 C ----- First reported 99.998319 IMPCA001 99.91 -----323 IMPCA001 99.90 -----332 ----- -----333 ----- -----334 IMPCA001 99.91 -----342 ----- -----343 IMPCA001 99.64 C ----- First reported 99.999 345 IMPCA001 99.7456 C ----- First reported 99.9976 346 ----- -----347 IMPCA001 99.798 C ----- First reported 99.998357 IMPCA001 99.69 -----372 ----- -----395 IMPCA001 99.995 -----443 ----- -----444 IMPCA001 99.8832 -----445 ----- -----446 IMPCA001 99.59 -----468 IMPCA001 99.795 -----494 IMPCA001 99.89 -----528 in house 99.991 -----529 ----- -----608 ----- -----609 IMPCA001 99.85 C ----- First reported 99.9952646 IMPCA001 <99.999 -----657 IMPCA001 99.836 -----663 IMPCA001 99.9947 C ----- First reported 99.99786 ----- -----823 IMPCA001 99.65 C ----- First reported 99.99 824 IMPCA001 99.65 C ----- First reported 99.99 825 IMPCA001 99.66 C ----- First reported 99.99 857 IMPCA001 99.887 -----858 IMPCA001 99.894 -----859 IMPCA001 99.901 -----862 IMPCA001 99.90 -----864 IMPCA001 99.889 -----867 IMPCA001 99.652 -----902 ----- -----963 IMPCA001 99.8683 -----971 ----- -----974 in house 99.8860 -----

1004 IMPCA001 99.97 -----1007 ----- -----1009 in house 99.99 C ----- First reported 99.999 1010 IMPCA001 >99.85 C ----- First reported >99.99 1016 ----- -----1029 IMPCA001 99.9988 -----1041 IMPCA001 99.91168 -----1102 IMPCA001 99.9987 -----1108 ----- -----1149 ----- -----1204 ----- -----1510 ----- -----1615 IMPCA001 99.99851 C ----- First reported 99.99791712 ----- -----1728 ----- -----1905 in house 99.997 -----1931 ----- -----

Group 1: Group 2: Group 3:normality OK not OK not OKn 9 21 9outliers 0 0 0mean (n) 99.649 99.881 99.993st.dev. (n) 0.0532 0.0336 0.0091

R(calc.) 0.149 0.094 0.025R(lit.) unknown unknown unknown





99. 4

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Kernel Density

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Determination of Benzene content on sample #0845; results in mg/kglab method value mark z(targ) remarks52 ----- -----

150 IMPCA001 10.2 0.36153 ----- -----171 IMPCA001 10 0.18174 IMPCA001 9.3 -0.45

273 ----- -----311 IMPCA001 10.4 0.54319 IMPCA001 10.1 0.27323 ----- -----332 ----- -----333 ----- -----334 ----- -----342 ----- -----343 ----- -----345 ----- -----346 ----- -----347 ----- -----357 IMPCA001 8.9 -0.81372 in house present -----395 IMPCA001 <10 -----443 ----- -----444 IMPCA001 10.5 0.63445 ----- -----446 ----- -----468 ----- -----494 IMPCA001 10 0.18528 ----- -----529 ----- -----608 ----- -----609 ----- -----646 ----- -----657 IMPCA001 8.9 -0.81663 ----- -----786 ----- -----823 IMPCA001 8 -1.62824 ----- -----825 IMPCA001 10 0.18857 IMPCA001 10.9 0.99858 IMPCA001 7.3 -2.25859 IMPCA001 12 1.98862 IMPCA001 12 1.98864 IMPCA001 10.8 0.90867 inh-043 9.4 -0.36902 ----- -----963 IMPCA001 6.9 -2.61971 ----- -----974 ----- -----

1004 ----- -----1007 ----- -----1009 ----- -----1010 ----- -----1016 ----- -----1029 ----- -----1041 IMPCA001 10.53 0.661102 ----- -----1108 ----- -----1149 ----- -----1204 ----- -----1510 ----- -----1615 ----- -----1712 ----- -----1728 ----- -----1905 ----- -----1931 ----- -----

normality OKn 19outliers 0 Spike:mean (n) 9.80 10.4st.dev. (n) 1.366

R(calc.) 3.82R(Horwitz) 3.11





Kernel Density

0

0.05

0.1

0.15

0.2

0.25

0.3

0.35

0 5 10 15

0

2

4

6

8

10

12

14

9 6 3

8 5 8

8 2 3

3 5 7

6 5 7

1 7 4

8 6 7

1 7 1

8 2 5

4 9 4

3 1 9

1 5 0

3 1 1

4 4 4

1 0 4 1

8 6 4

8 5 7

8 5 9

8 6 2





Determination of Ethanol content on sample #0844 and #0845; results in mg/kglab method #0844 mark z(targ) #0845 mark z(targ) Remarks52 IMPCA001 10 -1.25 10 -1.29

150 IMPCA001 12.0 0.31 11.8 0.11153 ----- ----- ----- -----171 IMPCA001 12 0.31 13.8 1.66174 IMPCA001 11 -0.47 14.1 1.89

273 ----- ----- ----- -----311 IMPCA001 13 1.09 12.6 0.73319 IMPCA001 8.6 -2.34 9.1 -1.99323 IMPCA001 11 -0.47 11 -0.51332 ----- ----- ----- -----333 ----- ----- ----- -----334 ----- ----- ----- -----342 ----- ----- ----- -----343 IMPCA001 11.8 0.15 11.2 -0.36345 IMPCA001 10.5 -0.86 10.0 -1.29346 ----- ----- ----- -----347 IMPCA001 12.6 0.78 11.7 0.03357 IMPCA001 11 -0.47 12 0.26372 IMPCA001 11 -0.47 10 -1.29395 IMPCA001 <5 ----- 16.26 3.57 False negative443 ----- ----- ----- -----444 IMPCA001 9.4 -1.72 9.2 -1.91445 ----- ----- ----- -----446 ----- ----- ----- -----468 IMPCA001 12 0.31 ----- -----494 IMPCA001 12 0.31 12 0.26528 E346 182.18 G(0.01) 133.04 ----- -----529 ----- ----- ----- -----608 ----- ----- ----- -----609 IMPCA001 15 C 2.65 ----- ----- First reported 2.514646 IMPCA001 <5 ----- <5 ----- False negative657 IMPCA001 11.3 -0.24 10 -1.29663 ----- ----- ----- -----786 ----- ----- ----- -----823 IMPCA001 12 0.31 12 0.26824 IMPCA001 13 1.09 13 1.04825 IMPCA001 11 -0.47 11 -0.51857 IMPCA001 11.0 -0.47 10.6 -0.82858 IMPCA001 11.5 -0.08 11.7 0.03859 IMPCA001 12 0.31 11 -0.51862 IMPCA001 12 0.31 12 0.26864 IMPCA001 12.3 0.54 12.2 0.42867 IMPCA001 11.4 -0.16 11.5 -0.12902 ----- ----- ----- -----963 IMPCA001 9.2 -1.88 9.2 -1.91971 ----- ----- ----- -----974 in house 9.52 -1.63 9.44 -1.72

1004 IMPCA001 17.2 4.36 17.2 4.301007 in house 11 -0.47 10 -1.291009 in house 12.8 0.93 12.6 0.731010 IMPCA001 11 -0.47 11 -0.511016 ----- ----- ----- -----1029 IMPCA001 11.12 -0.38 13.05 1.081041 IMPCA001 11.075 -0.41 11.55 -0.091102 IMPCA001 11.54 -0.05 10.97 -0.541108 ----- ----- ----- -----1149 ----- ----- ----- -----1204 E346 6.76 -3.78 7.37 -3.331510 IMPCA001 <30 ----- ----- -----1615 IMPCA001 16.68 C 3.96 17.19 C 4.29 First reported 21.11 and 21.7591712 ----- ----- ----- -----1728 ----- ----- ----- -----1905 in house 12.7 0.85 12.1 0.341931 ----- ----- ----- -----


R(calc.) 5.30 5.88R(Horwitz) 3.59 3.61





Kernel Density#0844

0

0.05

0.1

0.15

0.2

0.25

0.3

0.35

0.4

0 5 10 15 20 25

Kernel Density#0845

0

0.05

0.1

0.15

0.2

0.25

0 5 10 15 20 25

normality OKn 33outliers 3mean (n) 11.31st.dev. (n) 1.111r(calc.) 1.188R(calc) 3.193

0

5

10

15

20

25

30

1 2 0 4

3 1 9

9 6 3

4 4 4

9 7 4

5 2

3 4 5

3 7 2

8 5 7

8 2 5

3 5 7

1 0 0 7

1 7 4

3 2 3

1 0 1 0

1 0 4 1

1 0 2 9

6 5 7

8 6 7

8 5 8

1 1 0 2

3 4 3

4 6 8

1 5 0

1 7 1

8 5 9

4 9 4

8 2 3

8 6 2

8 6 4

3 4 7

1 9 0 5

1 0 0 9

8 2 4

3 1 1

6 0 9

1 6 1 5

1 0 0 4

5 2 8

Ethanol on #0844

0

5

10

15

20

25

30

1 2 0 4

3 1 9

9 6 3

4 4 4

9 7 4

3 4 5

5 2

3 7 2

1 0 0 7

6 5 7

8 5 7

1 1 0 2

8 2 5

1 0 1 0

8 5 9

3 2 3

3 4 3

8 6 7

1 0 4 1

3 4 7

8 5 8

1 5 0

8 2 3

4 9 4

3 5 7

8 6 2

1 9 0 5

8 6 4

1 0 0 9

3 1 1

8 2 4

1 0 2 9

1 7 1

1 7 4

3 9 5

1 6 1 5

1 0 0 4

Ethanol on #0845

5

7

9

11

13

15

17

19

5 10 15 20

#0844

#0845





Determination of Acetone content on sample #0844 and #0845; results in mg/kglab method #0844 mark z(targ) #0845 mark z(targ) remarks52 IMPCA001mod. <10 ----- <10 -----

150 IMPCA001 <5 ----- <5 -----153 ----- ----- ----- -----171 IMPCA001 <1 ----- <1 -----174 IMPCA001 <1 ----- <1 -----

273 ----- ----- ----- -----311 IMPCA001 <5 ----- 0 -----319 IMPCA001 <10 ----- 0.0 -----323 IMPCA001 <10 ----- <10 -----332 ----- ----- ----- -----333 ----- ----- ----- -----334 ----- ----- ----- -----342 ----- ----- ----- -----343 IMPCA001 <5 ----- <5 -----345 IMPCA001 <1 ----- <1 -----346 ----- ----- ----- -----347 IMPCA001 <5 ----- <5 -----357 IMPCA001 <10 ----- <10 -----372 IMPCA001 <10 ----- <10 -----395 IMPCA001 <10 ----- <10 -----443 ----- ----- ----- -----444 IMPCA001 <1 ----- 0.9 -----445 ----- ----- ----- -----446 E346 <0.003 ----- ----- -----468 ----- ----- ----- -----494 IMPCA001 <5 ----- <5 -----528 D1612 >0.003 ----- ----- -----529 ----- ----- ----- -----608 ----- ----- ----- -----609 ----- ----- ----- -----646 IMPCA001 <10 ----- <10 -----657 IMPCA001 <5 ----- <5 -----663 ----- ----- ----- -----786 ----- ----- ----- -----823 IMPCA001 <5 ----- <5 -----824 IMPCA001 <1 ----- <1 -----825 IMPCA001 <10 ----- <10 -----857 IMPCA001 1.8 ----- 0.6 -----858 IMPCA001 <10 ----- <10 -----859 IMPCA001 <1 ----- 1 -----862 IMPCA001 2 ----- 1 -----864 IMPCA001 <10 ----- <10 -----867 IMPCA001 <5 ----- <5 -----902 ----- ----- ----- -----963 IMPCA001 <10 ----- <10 -----971 ----- ----- ----- -----974 in house <1 ----- <1 -----

1004 IMPCA001 1.1 ----- 1.2 -----1007 in house <2 ----- <2 -----1009 D1612 3.5 ----- 3.5 -----1010 IMPCA001 <10 ----- <10 -----1016 ----- ----- ----- -----1029 IMPCA001 0.659 ----- 0.877 -----1041 IMPCA001 0.756 ----- 0.86 -----1102 IMPCA001 1.09 ----- 1.16 -----1108 ----- ----- ----- -----1149 ----- ----- ----- -----1204 D1612 <30 ----- <30 -----1510 IMPCA001 <30 ----- ----- -----1615 IMPCA001 0.0127 ----- nd C ----- First reported 0.01271712 ----- ----- ----- -----1728 D1612 <30 ----- <30 -----1905 in house <20 ----- ----- -----1931 ----- ----- ----- -----

normality n.a. n.a.n 8 9outliers 0 0mean (n) <5 <5st.dev. (n) n.a. n.a.

R(calc.) n.a. n.a.R(lit.) unknown unknown





Determination of Trimethylamine on sample #0844; results in μ g/kglab method value mark z(targ) remarks52 ----- -----

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 E346 6 -----864 ----- -----867 ----- -----902 ----- -----963 ----- -----971 ----- -----974 ----- -----

1004 E346 <5 -----1007 in house 15 -----1009 E346 <10 -----1010 ----- -----1016 ----- -----1029 in house 14.102 -----1041 E346 <100 -----1102 ----- -----1108 ----- -----1149 ----- -----1204 ----- -----1510 ----- -----1615 E346 N.D. -----1712 ----- -----1728 ----- -----1905 ----- -----1931 ----- -----

normality n.a.n 4outliers 0mean (n) n.a.st.dev. (n) n.a.

R(calc.) n.a.R(lit) unknown





Determination of UV Absorbance at 300nm (50 mm and 10 mm cuvet) on sample #0845;lab method 50 mm mark z(targ) 10 mm mark z(targ) remarks52 IMPCA004 0.014 1.56 ----- -----

150 ----- ----- ----- -----153 ----- ----- ----- -----171 IMPCA004 ----- ----- 0.002 0.61174 IMPCA004 ----- ----- 0.0000 -1.87

273 IMPCA004 ----- ----- <0.001 -----311 IMPCA004 0.008 0.09 ----- -----319 IMPCA004 0.010 0.58 ----- -----323 ----- ----- ----- -----332 ----- ----- ----- -----333 ----- ----- ----- -----334 IMPCA004 0.0023 -1.30 ----- -----342 in house 0.010 0.58 ----- -----343 ----- ----- ----- -----345 ----- ----- ----- -----346 in house ----- ----- 0.001 -0.63347 IMPCA004 0.010 0.58 ----- -----357 IMPCA004 ----- ----- 0.002 0.61372 IMPCA004 0.00494 -0.66 ----- -----395 IMPCA004 0.007 -0.15 ----- -----443 ----- ----- ----- -----444 IMPCA004 0.013 1.32 ----- -----445 IMPCA004 ----- ----- -0.0096 G(0.05) -13.73446 ----- ----- ----- -----468 ----- ----- ----- -----494 ----- ----- ----- -----528 ----- ----- ----- -----529 ----- ----- ----- -----608 ----- ----- ----- -----609 ----- ----- ----- -----646 ----- ----- ----- -----657 IMPCA004 0.001 -1.62 ----- -----663 ----- ----- ----- -----786 ----- ----- ----- -----823 IMPCA004 0.006 -0.40 ----- -----824 IMPCA004 ----- ----- 0.0005 -1.25825 ----- ----- ----- -----857 IMPCA004 0.010 0.58 ----- -----858 IMPCA004 0.009 0.34 ----- -----859 IMPCA004 0.006 -0.40 ----- -----862 IMPCA004 0.008 0.09 ----- -----864 ----- ----- ----- -----867 IMPCA004 0.005 -0.64 ----- -----902 ----- ----- ----- -----963 ----- ----- ----- -----971 ----- ----- ----- -----974 IMPCA004 ----- ----- 0.001 -0.63

1004 IMPCA004 ----- ----- 0.0036 2.581007 in house ----- ----- 0 -1.871009 IMPCA004 0.068 G(0.01) 14.79 ----- -----1010 ----- ----- ----- -----1016 ----- ----- ----- -----1029 ----- ----- ----- -----1041 IMPCA004 ----- ----- -0.027 G(0.01) -35.241102 IMPCA004 0.0053 -0.57 ----- -----1108 ----- ----- ----- -----1149 ----- ----- ----- -----1204 ----- ----- ----- -----1510 ----- ----- ----- -----1615 IMPCA004 ----- ----- 0.003 1.841712 ----- ----- ----- -----1728 ----- ----- ----- -----1905 IMPCA004 ----- ----- 0.002 0.611931 IMPCA004 ----- ex ----- ----- ----- Reported 100

normality OK OKn 17 10outliers 1 2mean (n) 0.0076 0.0015st.dev. (n) 0.00346 0.00122

R(calc.) 0.0097 0.0034R(IMPCA004:06) 0.0114 0.0023





0

0.01

0.02

0.03

0.04

0.05

0.06

0.07

0.08

6 5 7

3 3 4

3 7 2

8 6 7

1 1 0 2

8 2 3

8 5 9

3 9 5

3 1 1

8 6 2

8 5 8

8 5 7

3 4 7

3 4 2

3 1 9

4 4 4

5 2

1 0 0 9

50 mm cuvet

-0.01

- 0.005

0

0. 005

0.01

0. 015

1 0 4 1

4 4 5

1 0 0 7

1 7 4

8 2 4

3 4 6

9 7 4

1 7 1

1 9 0 5

3 5 7

1 6 1 5

1 0 0 4

10 mm cuvet

Kernel Density50 m cuvet

0

20

40

60

80

100

120

-0.02 0 0.02 0.04 0.06 0.08


0

50

100

150

200

250

-0.04 -0.03 -0.02 -0.01 0 0.01





Determination of UV Absorbance at 268.5nm (50 mm and 10 mm cuvet) on sample #0845; lab method 50 nm mark z(targ) 10 nm mark z(targ) remarks52 IMPCA004 0.075 G(0.05) 13.20 ----- -----

150 ----- ----- ----- -----153 ----- ----- ----- -----171 IMPCA004 ----- ----- 0.007 1.85174 IMPCA004 ----- ----- 0.0031 -4.94

273 IMPCA004 ----- ----- 0.002 -6.85311 IMPCA004 0.0327 -0.07 ----- -----319 IMPCA004 0.035 0.65 ----- -----323 ----- ----- ----- -----332 ----- ----- ----- -----333 ----- ----- ----- -----334 IMPCA004 0.0237 -2.90 ----- -----342 in house 0.034 0.33 ----- -----343 ----- ----- ----- -----345 ----- ----- ----- -----346 in house ----- ----- 0.0065 0.98347 IMPCA004 0.040 2.22 ----- -----357 IMPCA004 ----- ----- 0.007 1.85372 IMPCA004 0.03030 -0.83 ----- -----395 IMPCA004 0.045 3.79 ----- -----443 ----- ----- ----- -----444 IMPCA004 0.032 -0.29 ----- -----445 IMPCA004 ----- ----- -0.0055 G(0.05) -19.90446 ----- ----- ----- -----468 ----- ----- ----- -----494 ----- ----- ----- -----528 ----- ----- ----- -----529 ----- ----- ----- -----608 ----- ----- ----- -----609 ----- ----- ----- -----646 ----- ----- ----- -----657 IMPCA004 <0.001 ----- ----- -----663 ----- ----- ----- -----786 ----- ----- ----- -----823 IMPCA004 0.032 -0.29 ----- -----824 IMPCA004 ----- ----- 0.0042 -3.02825 ----- ----- ----- -----857 IMPCA004 0.033 0.02 ----- -----858 IMPCA004 0.033 0.02 ----- -----859 IMPCA004 0.033 0.02 ----- -----862 IMPCA004 0.032 -0.29 ----- -----864 ----- ----- ----- -----867 IMPCA004 0.030 -0.92 ----- -----902 ----- ----- ----- -----963 ----- ----- ----- -----971 ----- ----- ----- -----974 IMPCA004 ----- ----- 0.005 -1.63

1004 IMPCA004 ----- ----- 0.0105 7.941007 in house ----- ----- 0.001 -8.591009 IMPCA004 0.100 G(0.01) 21.04 ----- -----1010 ----- ----- ----- -----1016 ----- ----- ----- -----1029 ----- ----- ----- -----1041 IMPCA004 ----- ----- -0.003 G(0.05) -15.551102 IMPCA004 0.0283 -1.45 ----- -----1108 ----- ----- ----- -----1149 ----- ----- ----- -----1204 ----- ----- ----- -----1510 ----- ----- ----- -----1615 IMPCA004 ----- ----- 0.008 3.591712 ----- ----- ----- -----1728 ----- ----- ----- -----1905 IMPCA004 ----- ----- 0.011 8.811931 IMPCA004 ----- ex ----- ----- ----- Reported 99

normality not OK OKn 15 11outliers 2 2mean (n) 0.0329 0.0059st.dev. (n) 0.00482 0.00324

R(calc.) 0.0135 0.0091R(IMPCA004:06) 0.0089 0.0016





0

0.02

0.04

0.06

0.08

0.1

0.12

3 3 4

1 1 0 2

8 6 7

3 7 2

4 4 4

8 6 2

8 2 3

3 1 1

8 5 8

8 5 9

8 5 7

3 4 2

3 1 9

3 4 7

3 9 5

5 2

1 0 0 9

50 mm cuvet


0

10

20

30

40

50

60

70

80

90

100

0 0.05 0.1 0.15

-0.01

- 0.005

0

0. 005

0.01

0. 015

4 4 5

1 0 4 1

1 0 0 7

2 7 3

1 7 4

8 2 4

9 7 4

3 4 6

1 7 1

3 5 7

1 6 1 5

1 0 0 4

1 9 0 5

10 mm cuvet


0

10

20

30

40

50

60

70

80

90

-0.02 -0.01 0 0.01 0.02





Determination of UV Absorbance at 250nm (50 mm and 10 mm cuvet) on sample #0845; lab method 50 nm mark z(targ) 10 nm mark z(targ) remarks52 IMPCA004 0.192 4.73 ----- -----

150 ----- ----- ----- -----153 ----- ----- ----- -----171 IMPCA004 ----- ----- 0.032 1.88174 IMPCA004 ----- ----- 0.0287 -1.18

273 IMPCA004 ----- ----- 0.022 -7.37311 IMPCA004 0.1615 -0.43 ----- -----319 IMPCA004 0.153 -1.87 ----- -----323 ----- ----- ----- -----332 ----- ----- ----- -----333 ----- ----- ----- -----334 IMPCA004 0.1651 0.18 ----- -----342 in house 0.181 2.87 ----- -----343 ----- ----- ----- -----345 ----- ----- ----- -----346 in house ----- ----- 0.037 6.50347 IMPCA004 0.155 -1.53 ----- -----357 IMPCA004 ----- ----- 0.032 1.88372 IMPCA004 0.18161 2.97 ----- -----395 IMPCA004 0.173 1.51 ----- -----443 ----- ----- ----- -----444 IMPCA004 0.186 3.71 ----- -----445 IMPCA004 ----- ----- 0.0180 -11.07446 ----- ----- ----- -----468 ----- ----- ----- -----494 ----- ----- ----- -----528 ----- ----- ----- -----529 ----- ----- ----- -----608 ----- ----- ----- -----609 ----- ----- ----- -----646 ----- ----- ----- -----657 IMPCA004 0.087 G(0.05) -13.02 ----- -----663 ----- ----- ----- -----786 ----- ----- ----- -----823 IMPCA004 0.159 -0.85 ----- -----824 IMPCA004 ----- ----- 0.0284 -1.45825 ----- ----- ----- -----857 IMPCA004 0.156 -1.36 ----- -----858 IMPCA004 0.153 -1.87 ----- -----859 IMPCA004 0.146 -3.05 ----- -----862 IMPCA004 0.159 -0.85 ----- -----864 ----- ----- ----- -----867 IMPCA004 0.145 -3.22 ----- -----902 ----- ----- ----- -----963 ----- ----- ----- -----971 ----- ----- ----- -----974 IMPCA004 ----- ----- 0.030 0.03

1004 IMPCA004 ----- ----- 0.0366 6.131007 in house ----- ----- 0.03 0.031009 IMPCA004 0.217 G(0.05) 8.95 ----- -----1010 ----- ----- ----- -----1016 ----- ----- ----- -----1029 ----- ----- ----- -----1041 IMPCA004 ----- ----- 0.114 G(0.01) 77.721102 IMPCA004 0.1584 -0.95 ----- -----1108 ----- ----- ----- -----1149 ----- ----- ----- -----1204 ----- ----- ----- -----1510 ----- ----- ----- -----1615 IMPCA004 ----- ----- 0.035 4.651712 ----- ----- ----- -----1728 ----- ----- ----- -----1905 IMPCA004 ----- ----- 0.053 G(0.05) 21.301931 IMPCA004 ----- ex ----- ----- ----- Reported 96


R(calc.) 0.0403 0.0163R(IMPCA004:06) 0.0166 0.0030





0

0.05

0.1

0.15

0.2

0.25

6 5 7

8 6 7

8 5 9

8 5 8

3 1 9

3 4 7

8 5 7

1 1 0 2

8 2 3

8 6 2

3 1 1

3 3 4

3 9 5

3 4 2

3 7 2

4 4 4

5 2

1 0 0 9

50 mm cuvet


0

5

10

15

20

25

0 0.1 0.2 0.3

0

0.02

0.04

0.06

0.08

0.1

0.12

4 4 5

2 7 3

8 2 4

1 7 4

9 7 4

1 0 0 7

3 5 7

1 7 1

1 6 1 5

1 0 0 4

3 4 6

1 9 0 5

1 0 4 1

10 mm cuvet


0

10

20

30

40

50

60

70

0 0.05 0.1 0.15





Determination of UV Absorbance at 220nm (50 mm and 10 mm cuvet) on sample #0845; lab method 50 nm mark z(targ) 10 nm mark z(targ) remarks52 IMPCA004 1.451 G(0.05) 2.52 ----- -----

150 ----- ----- ----- -----153 ----- ----- ----- -----171 IMPCA004 ----- ----- 0.227 -0.28174 IMPCA004 ----- ----- 0.2285 -0.22

273 IMPCA004 ----- ----- 0.220 -0.57311 IMPCA004 1.208 0.46 ----- -----319 IMPCA004 1.09 -0.53 ----- -----323 ----- ----- ----- -----332 ----- ----- ----- -----333 ----- ----- ----- -----334 IMPCA004 1.2188 0.56 ----- -----342 in house 1.185 0.27 ----- -----343 ----- ----- ----- -----345 ----- ----- ----- -----346 in house ----- ----- 0.233 -0.03347 IMPCA004 1.200 0.40 ----- -----357 IMPCA004 ----- ----- 0.237 0.14372 IMPCA004 1.23052 0.65 ----- -----395 IMPCA004 1.222 0.58 ----- -----443 ----- ----- ----- -----444 IMPCA004 1.158 0.04 ----- -----445 IMPCA004 ----- ----- 0.2241 -0.40446 ----- ----- ----- -----468 ----- ----- ----- -----494 ----- ----- ----- -----528 ----- ----- ----- -----529 ----- ----- ----- -----608 ----- ----- ----- -----609 ----- ----- ----- -----646 ----- ----- ----- -----657 IMPCA004 1.111 -0.36 ----- -----663 ----- ----- ----- -----786 ----- ----- ----- -----823 IMPCA004 1.140 -0.11 ----- -----824 IMPCA004 ----- ----- 0.2246 -0.38825 ----- ----- ----- -----857 IMPCA004 1.050 -0.87 ----- -----858 IMPCA004 1.065 -0.75 ----- -----859 IMPCA004 1.100 -0.45 ----- -----862 IMPCA004 1.081 -0.61 ----- -----864 ----- ----- ----- -----867 IMPCA004 1.010 -1.21 ----- -----902 ----- ----- ----- -----963 ----- ----- ----- -----971 ----- ----- ----- -----974 IMPCA004 ----- ----- 0.215 -0.78

1004 IMPCA004 ----- ----- 0.2326 -0.051007 in house ----- ----- 0.26 1.101009 IMPCA004 1.26 0.90 ----- -----1010 ----- ----- ----- -----1016 ----- ----- ----- -----1029 ----- ----- ----- -----1041 IMPCA004 ----- ----- 1.095 G(0.01) 35.951102 IMPCA004 1.2750 1.03 ----- -----1108 ----- ----- ----- -----1149 ----- ----- ----- -----1204 ----- ----- ----- -----1510 ----- ----- ----- -----1615 IMPCA004 ----- ----- 2.498 G(0.05) 94.521712 ----- ----- ----- -----1728 ----- ----- ----- -----1905 IMPCA004 ----- ----- 0.269 1.471931 IMPCA004 ----- ex ----- ----- ----- Reported 83


R(calc.) 0.2218 0.0463R(IMPCA004:06) 0.3310 0.0671





0

0.2

0.4

0.6

0.8

1

1.2

1.4

1.6

8 6 7

8 5 7

8 5 8

8 6 2

3 1 9

8 5 9

6 5 7

8 2 3

4 4 4

3 4 2

3 4 7

3 1 1

3 3 4

3 9 5

3 7 2

1 0 0 9

1 1 0 2

5 2

50 mm cuvet

0

0.5

1

1.5

2

2.5

3

9 7 4

2 7 3

4 4 5

8 2 4

1 7 1

1 7 4

1 0 0 4

3 4 6

3 5 7

1 0 0 7

1 9 0 5

1 0 4 1

1 6 1 5

10 mm cuvet


0

2

4

6

8

10

12

14

16

18

0 1 2 3


0

0.5

1

1.5

2

2.5

3

3.5

4

0 0.5 1 1.5 2





APPENDIX 2

List of number of participants per country

Number of laboratories Country1 laboratory in BELGIUM

1 laboratory in CANADA1 laboratory in CHILE1 laboratory in ESTONIA1 laboratory in FINLAND3 laboratories in FRANCE3 laboratories in GERMANY1 laboratory in GREECE1 laboratory in ITALY3 laboratories in KOREA4 laboratories in MALAYSIA2 laboratories in MEXICO2 laboratories in NEW ZEALAND1 laboratory in NORWAY7 laboratories in P.R. of CHINA1 laboratory in POLAND1 laboratory in ROMANIA

1 laboratory in RUSSIA1 laboratory in SAUDI ARABIA2 laboratories in SINGAPORE1 laboratory in SOUTH AFRICA5 laboratories in SPAIN1 laboratory in SWEDEN2 laboratories in THAILAND3 laboratories in THE NETHERLANDS1 laboratory in TRINIDAD and TOBAGO W.I.1 laboratory in TURKEY2 laboratories in U.A.E.4 laboratories in U.S.A.5 laboratories in UNITED KINGDOM1 laboratory in VENEZUELA




APPENDIX 3

Abbreviations :

C = final result after checking of first reported suspect result

D(0.01) = outlier in Dixon’s outlier test

D(0.05) = straggler in Dixon’s 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

E = error in calculations

U = reported in different unit

Ex = excluded from calculations

n.a. = not applicableW. = result withdrawn on request of participant

Literature :

1 iis Interlaboratory Studies, Protocol for the Organisation, Statistics & Evaluation, November 2008

2 ASTM E178-02

3 ASTM E1301-03

4 ISO 5725-865 ISO 5725, parts 1-6, 1994

6 M. Thompson and R. Wood, J. AOAC Int, 76, 926, (1993)

7 W.J. Youden and E.H. Steiner, Statistical Manual of the AOAC, (1975)

8 IP 367/96

9 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/).

Documents

Methanol Specifications