Results of Proficiency Test Gasoil B5 (5% FAME) … · Results of Proficiency Test Gasoil B5 (5% FAME) April 2009 ... 2.3 CONFIDENTIALITY ... it was decided to continue the round

Results of Proficiency Test Gasoil B5 (5% FAME) April 2009 Organised by: Institute for Interlaboratory Studies Spijkenisse, the Netherlands Authors: Ing. R.J. Starink Correctors: Dr. R.G. Visser & Ing. S. Lagendijk Report: iis09G03X June 2009

Institute for Interlaboratory Studies Spijkenisse, June 2009

page 2 of 46 Gasoil B5 (5% FAME): iis09G03X

CONTENTS 1 INTRODUCTION ..................................................................................................................................... 3 2 SET UP..................................................................................................................................................... 3 2.1 ACCREDITATION.................................................................................................................................... 3 2.2 PROTOCOL............................................................................................................................................. 3 2.3 CONFIDENTIALITY STATEMENT ......................................................................................................... 3 2.4 SAMPLES ................................................................................................................................................ 4 2.5 STABILITY OF THE SAMPLES .............................................................................................................. 4 2.6 ANALYSES .............................................................................................................................................. 4 3 RESULTS................................................................................................................................................. 5 3.1 STATISTICS............................................................................................................................................. 5 3.2 GRAPHICS............................................................................................................................................... 6 3.3 Z-SCORES............................................................................................................................................... 6 4 EVALUATION .......................................................................................................................................... 6 4.1 EVALUATION PER TEST ....................................................................................................................... 7 4.2 PERFORMANCE EVALUATION FOR THE GROUP OF LABORATORIES ...................................... 10 4.3 COMPARISON OF THE PROFICIENY TEST OF APRIL 2009 WITH PREVIOUS PT’S……… …… 11 Appendices: 1. Data, statistical results and graphic results........................................................................................... 12 2. z-Scores of the distillation...................................................................................................................... 44 3. Number of participants........................................................................................................................... 45 4. Abbreviations and literature ................................................................................................................... 46

Spijkenisse, June 2009 Institute for Interlaboratory Studies

Gasoil B5 (5% FAME): iis09G03X page 3 of 46

1 INTRODUCTION

Since 2005, the Institute for Interlaboratory Studies organizes every year a proficiency test for Gasoil B5 (5% FAME) according EN590:2004. In the annual proficiency testing program of 2008/2009, it was decided to continue the round robin for the analysis of Gasoil B5 (5% FAME). In this international interlaboratory study, 71 laboratories from 31 different countries have participated. See appendix 3 for a list of participants in alphabetical country order. In this report, the results of the Gasoil B5 (5% FAME) proficiency test are presented and discussed.

2 SET UP

The Institute for Interlaboratory Studies (i.i.s.) in Spijkenisse, The Netherlands, was the organizer of this proficiency test. It was decided to send two identical bottles of 1 litre with Gasoil B5 (5% FAME). Participants were requested to report rounded and unrounded results. The unrounded results were preferably used for statistical evaluation.

2.1 ACCREDITATION The Institute for Interlaboratory Studies in Spijkenisse, the Netherlands, is accredited in agreement with ISO guide 43 and ILAC-G13:2007, (R007), since January 2000, by the Dutch Accreditation Council (Raad voor Accreditatie). This ensures 100% confidentially of participant’s data. Also customer’s satisfaction is measured on a regular basis by sending questionnaires.

2.2 PROTOCOL The protocol followed in the organization of this proficiency test was the one as described for proficiency testing in the report ‘iis Interlaboratory Studies: Protocol for the Organization, Statistics and Evaluation’ of November 2008 (iis-protocol, version 3.1), which can be downloaded from www.iisnl.com. The participants were asked to report the analytical results using the indicated units on the report form.

2.3 CONFIDENTIALITY STATEMENT All data present in this report must be regarded as confidential and for use by the

participating companies only. Disclosure of the information in this report is only allowed by means of the entire report. Use of the contents of this report for third parties is only allowed by written permission of the Institute of Interlaboratory Studies. Disclosure of the identity of one or more of the participating companies will be done only after receipt of a written agreement of the companies involved.



2.4 SAMPLES The necessary 200 litre bulk material (Gasoil B5 with approx. 5% FAME) was purchased from a local Gasoil producer. After homogenization, 192 subsamples were transferred to 1 litre brown glass bottles and labelled #0935. The homogeneity of the subsamples was checked by determination of Density in accordance with ASTM D4052:02e1 on 8 stratified random selected samples.

Density @ 15 oC (kg/m3)

sample #0935-1 830.48 sample #0935-2 830.51 sample #0935-3 830.52 sample #0935-4 830.52 sample #0935-5 830.51 sample #0935-6 830.50 sample #0935-7 830.50 sample #0935-8 830.50

table 1: homogeneity test of the subsamples #0935

From table 1 the repeatabilities of the results were calculated by multiplication of the standard deviation by 2.8:

Density @15ºC (kg/m3)

r (sample #0935) 0.04 reference test D4052:02e1 r (reference test) 0.10

table 2: repeatabilities of the subsamples #0935

The repeatability of the results was in agreement with the repeatability as required by ASTM D4052:02e1. Therefore, homogeneity of the subsamples was assumed. Two bottles (2*1 litre, labelled #0935) were sent to the participating laboratories on March 25, 2009.

2.5 STABILITY OF THE SAMPLES The stability of Gasoil B5 (5% FAME), packed in the brown glass bottles, was checked. The material was found sufficiently stable for the period of the proficiency test.

2.6 ANALYSIS The participants were asked to determine, according specification EN590: Ash Content, Cetane Index ISO4264, Conradson Carbon Residue on 10% Residue, Cloud Point, Cold Filter Plugging Point, Density @ 15°C, Distillation, Flash Point PMcc, Kinematic Viscosity @40°C, Lubricity by HFRR, Oxidation Stability, Polycyclic Aromatic Hydrocarbons, Sulphur Content, Total Contamination, Water and FAME content.



To get comparable results a detailed report form, on which the units were prescribed as well as some of the required standards, was sent together with each set of samples. Also, a letter of instructions and a SDS were added to the package.

3 RESULTS

During four weeks after sample despatch, the results of the individual laboratories were gathered. The original data are tabulated per determination in the appendix 1 of this report. The laboratories are presented by their code numbers. Directly after deadline, a reminder fax was sent to those laboratories that had not yet reported. 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 it to be an outlier. The laboratories that produced these suspect data were asked to check the (raw data of the) reported results. Additional or corrected results have been used for data analysis and the 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 ‘iis Interlaboratory Studies: Protocol for the Organization, Statistics and Evaluation’ of November 2008 (iis-protocol, version 3.1). 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. Not all data sets proved to have a normal distribution, in which cases the conclusions of statistical evaluation should be used with due care. In accordance with 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, by G(0.01) or DG(0.01) for the Grubbs test. Stragglers are marked by D(0.05) for the Dixon test, by G(0.05) or DG(0.05) for the Grubbs test. Both outliers and stragglers were not included in the calculations of averages and standard deviations. Finally, the reproducibilities were calculated from the standard deviations by multiplying them with a factor of 2.8.



3.2 GRAPHICS In order to visualise the data against the reproducibilities from literature, Gauss plots were made, using the sorted data for one determination (see appendix 1). On the Y-axis, the reported 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 relevant 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 4, nr.12-13).

3.3 Z-SCORES To evaluate the performance of the participating laboratories the z-scores were calculated. As it was decided to evaluate the performance of the participants in this proficiency test (PT) against the literature requirements, e.g. EN reproducibilities, the z-scores were calculated using a target standard deviation. This results in an evaluation independent of the spread of this interlaboratory study. The target standard deviation was calculated from the literature reproducibility by division with 2.8. The z-scores were calculated according to: z(target) = (result - average of PT) / target standard deviation The z(target) scores are listed in the result tables in appendix 1. 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 good 1 < | z | < 2 satisfactory 2 < | z | < 3 questionable 3 < | z | unsatisfactory

4 EVALUATION In this interlaboratory study, no problems with sample despatch were encountered during the execution. Two participants decided not to report any results. In total eleven participants reported results after the final reporting date. Finally, 69 participants reported in total 1059 numerical results. Observed were 54 outlying results, which is 5.1 %. In proficiency studies, outlier percentages of 3 % - 7.5 % are quite normal. Not all original data sets proved to have a normal distribution. For Calculated Cetane Index, Cloud Point, Cold Filter Plugging Point, Density @15ºC, Flash Point and Distillation (5% and 10% recovered) non-Gaussian distributions were found. Therefore, the statistical evaluation for these determinations should be used with care.



4.1 EVALUATION PER TEST

In this section, the results are discussed per test. Ash: No significant conclusions were drawn as the consensus value is below

the application range of the reference method. All participants, except four, agreed that ash is equal or less then 0.001 %M/M.

C.I. ISO4264: Regretfully, no reproducibility limits are mentioned in ISO4264:07. It

should be noted that the ASTM has repeatedly amended the calculations routines in ASTM D4737 to incorporate the various diesel oil specifications mentioned in ASTM D975. The last update of ISO 4264 was in 2007, which is the current version (and technically equivalent to the 1996a version of ASTM D4737). In ISO 4264 only one calculation routine is mentioned and in the latest ASTM D4737 (2004 version) two calculation routines are mentioned. The user should take care to use and report the correct method as required by clients.

Nevertheless, one reported result was excluded as this laboratory used the CI calculation of ASTM D976, which is quite different from ISO4264 and ASTM D4737A.

CCR 10% res.: No significant conclusions were drawn as the consensus value is below

the application range of the reference method. However, all participants, except one, agreed that Carbon Conradson Residue is less then 0.1 %M/M.

Cloud Point: This determination is not problematic. No results were outside the

reproducibility limits and the calculated reproducibility is, after rejection of the statistical outlier, in good agreement with the requirements of EN23015:94.

CFPP: This determination is only problematic for one laboratory. Only one result

was outside the reproducibility limits and the calculated reproducibility is, after rejection of the statistical outlier, in good agreement with the requirements of EN116:98.

Density @15°C: This determination is problematic for four laboratories. Four results were

outside the reproducibility limits. The calculated reproducibility is, after rejection of the statistical outliers, in good agreement with ISO12185:96.

FAME: This determination is problematic for 3 laboratories. Three results were

outside the reproducibility limits and the calculated reproducibility is, after rejection of the statistical outliers, in agreement with the requirements of EN14078:03.



Flash Point: This determination is problematic for six laboratories. Six results were outside the reproducibility limits. The calculated reproducibility is, after rejection of the statistical outliers, in good agreement with the requirements of ISO2719:02. When the results for automatic/manual and ignition were evaluated separately, the calculated reproducibility for automated mode with flame ignition is the smallest.

Kin. Visc. 40°C: This determination is problematic for seven laboratories. Seven results

were outside the reproducibility limits, but the calculated reproducibility is, after rejection of the statistical outliers, in good agreement with ISO3104:94.

Lubricity: This determination is not problematic. Only one result was outside the

reproducibility limits and the calculated reproducibility is, after rejection of the statistical outliers, in good agreement with ISO12156:97.

Oxidation Stability: This determination is not problematic. No results were outside the

reproducibility limits and the calculated reproducibility is in good agreement with ISO12205:95.

PAH: This determination is problematic. Five results were outside the

reproducibility limits. The calculated reproducibility is, after rejection of the statistical outliers, not in agreement with the requirements of EN12916:06.

Note that FAME has been found to interfere with the PAH content. The EN12916:2000 was amended in the 2006 version to incorporate diesel fuel with up to 5% FAME. This was done to minimize the interference of FAME with tri+ - aromatic hydrocarbons. The 2000 version of IP391 is technically equivalent to the 2000 version of EN12916. The latest versions differ considerably from earlier versions by the use of a back flush valve. The user should take care to use and report the correct method as required by clients.

Sulphur: Some individual problems have been observed. Only three results were

outside the reproducibility limits. After rejection of the statistical outliers, the calculated reproducibility is in good agreement with the requirements of ISO20884:04. When the results for ISO20846, ISO20884 and ASTM D5453 were evaluated separately, the calculated reproducibilities of the ISO20884 and ASTM D5453 results are in agreement with the respective standard, while the calculated reproducibility of the ISO20846 results is larger and not in agreement with the more strict requirements of this standard.



Total Contamination: No significant conclusions were drawn as the consensus value is below the application range of the test method. All participants, except five, agreed that Total Contamination is less then 6 mg/kg.

Care must be taken of the proper sample preparation, eg. intake and heating of the sample. The correct filter must be used. Also, the proper drying and weighing of the filter can have large influence on the final result.

Water: No analytical problems have been observed. Only three results were

outside the reproducibility limits and the calculated reproducibility is, after rejection of the statistical outliers, in good agreement with the requirements of ISO12937:00.

Distillation: As only four laboratories reported distillation results determined by

manual distillation, these results are listed and evaluated together with the results determined by automatic distillation.

The manual determination may be somewhat problematic. In total only five results were outside the reproducibility limits. The calculated reproducibilities of Initial Boiling Point, 5, 10, 50 and 90% recovered and Final Boiling Point are, after rejection of the statistical outliers, all in good agreement with the requirements of ISO3405:05 (automated). However, when all the calculated reproducibilities were compared against the requirements of the manual mode, the calculated reproducibilities of 10 and 90% recovered and Initial Boiling Point are not in agreement with the requirements of ISO3405:05 (manual).



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 that participated. The average results of the evaluated parameters, calculated reproducibilities and reproducibilities, derived from literature standards (in casu ASTM, EN or ISO standards) are compared in the next tables.

Parameters unit n average 2.8 * sd R (lit)

Ash content %M/M 21 0.00055 0.00106 (0.00500) * Cetane Index ISO4264 48 55.94 0.97 unknown CCR 10% residue %M/M 27 0.0179 0.0270 (0.0168) * Cloud Point °C 49 -8.12 2.16 4.00 Cold Filter Plugging Point °C 55 -26.61 4.22 5.32 Density @ 15 °C kg/m3 62 830.45 0.27 0.50 Fatty Acid Methyl Ester %V/V 46 6.32 0.97 0.90 Flash Point PMcc °C 55 56.38 3.66 4.00 Kinematic Viscosity @ 40 °C mm2/s 51 2.7441 0.0287 0.0307 Lubricity µm 39 199.8 51.9 102.0 Oxidation Stability g/m3 22 2.45 4.19 7.46 Polycyclic Aromatic Hydrocarbons %M/M 34 2.49 1.05 0.93

Sulphur mg/kg 54 7.53 1.99 2.81 Total Contamination mg/kg 35 4.14 5.41 1.24 Water content mg/kg 52 62.88 34.94 54.53 Initial Boiling Point °C 56 172.13 8.40 8.50 5% recovery °C 55 202.31 4.75 12.98 10% recovery °C 60 215.53 5.13 7.16 50% recovery °C 61 273.16 2.88 8.68 90% recovery °C 61 331.99 4.89 6.24 Final Boiling Point °C 59 356.99 7.36 10.50

Table 4: summary of test results of Gasoil samples #0935

*) consensus value is below application range of the test method

Without further statistical calculations, it can be concluded that for most tests there is a good compliance of the group of participating laboratories with the relevant standards. The problematic tests have been discussed in paragraph 4.1.



4.3 COMPARISON OF THE INTERLABORATORY STUDY OF APRIL 2009 WITH PREVIOUS PT’S.

April 2009 April 2008 April 2007 April 2006

Number of reporting labs 69 75 69 42 Number of results reported 1059 1136 1122 675

Statistical outliers 54 38 34 28 Percentage outliers 5.1 % 3.3 % 3.0 % 4.1 %

table 5: 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:

April 2009 April 2008 April 2007 April 2006

Ash content (++) (++) (++) (++) Cetane Index ISO4264 n.e. n.e. n.e. n.e. CCR 10% residue (--) (--) (--) (--) Cloud Point ++ ++ ++ ++ Cold Filter Plugging Point ++ ++ ++ -- Density @ 15 °C ++ + ++ ++ Fatty Acid Methyl Ester - ++ ++ ++ Flash Point PMcc + ++ ++ - Kinematic Viscosity @ 40 °C + ++ -- - Lubricity ++ ++ ++ + Oxidation Stability ++ + + ++ Polycyclic Aromatic Hydrocarbons - - n.e. -- Sulphur ++ +/- + - Total Contamination -- -- -- -- Water content ++ ++ ++ ++ Distillation ++ +/- ++ ++

table 6: comparison determinations against the standard 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



APPENDIX 1 Determination of Ash on sample #0935; result in %M/M

lab method value mark Z(targ) remarks 150 ISO6245 <0.001 ----- 165 ----- ----- 311 ISO6245 0.001 ----- 312 ----- ----- 323 ISO6245 <0.001 ----- 334 ----- ----- 335 ----- ----- 343 ISO6245 <0.001 ----- 430 ----- ----- 431 ----- ----- 433 ----- ----- 445 IP4 <0.001 ----- 447 ISO6245 0.000 ----- 463 ISO6245 <0.001 ----- 494 ISO6245 0.0003 ----- 495 ISO6245 <0.001 ----- 496 ----- ----- 541 ----- ----- 657 ISO6245 0.002 DG(0.05) ----- 862 D482 0.0002 ----- 1006 ----- ----- 1017 ----- ----- 1033 ----- ----- 1047 ISO6245 0.001 ----- 1059 ISO6245 <0.001 ----- 1065 ----- ----- 1080 ----- ----- 1081 D482 0.0004 ----- 1095 ISO6245 0.001 ----- 1108 ----- ----- 1126 ----- ----- 1140 IP4 <0.0001 ----- 1192 ----- ----- 1194 ----- ----- 1195 INH-23 0.0090 G(0.01) ----- False positive? 1201 ISO6245 <0.005 ----- 1203 ISO6245 0.001 ----- 1205 ----- ----- 1218 ----- ----- 1227 ----- ----- 1300 ISO6245 0.00113 ----- 1402 ISO6245 <0.001 ----- 1406 ----- ----- 1407 ----- ----- 1409 ISO6245 <0.001 ----- 1428 ISO6245 0.0002 ----- 1501 ISO6245 0.0006 ----- 1520 ISO6245 0.0001 ----- 1538 ISO6245 0.0006 ----- 1634 ----- ----- 1636 D482 0.00068 ----- 1650 D482 0.00037 ----- 1656 IP4 <0.001 C ----- First reported <0.01 1706 ----- ----- 1710 ISO6245 0.001 ----- 1724 ISO6245 0.0001 ----- 1807 ISO6245 0.000 ----- 1808 ----- ----- 1810 ----- ----- 1811 ----- ----- 1826 ----- ----- 1829 ISO6245 0.00035 C ----- First reported 0.0035 1833 ISO6245 0.0008 ----- 1834 ----- ----- 1861 ----- ----- 1911 ----- ----- 1931 ----- ----- 1948 ISO6245 0.0018 C,DG(0.05) ----- First reported 0.018 1951 ISO6245 <0.01 ----- 2129 ISO6245 0.0007 ----- 2146 ----- -----



normality OK n 21 outliers 3 mean (n) 0.00055 st.dev. (n) 0.000379 R(calc.) 0.00106 R(ISO6245:01) (0.00500) Application Range : 0.001 – 0.180 %M/M

Kernel Density

0

100

200

300

400

500

600

700

-0.005 0 0.005 0.01 0.015

0

0.001

0.002

0.003

0.004

0.005

0.006

0.007

0.008

0.009

0.01

447

1807

1520

1724

1428

862

494

1829

1650

1081

1501

1538

1636

2129

1833

1095

311

1047

1203

1710

1300

1948

657

1195



Determination of Calculated Cetane Index ISO4264 on sample #0935

lab method value mark Z(targ) remarks 150 ISO4264 56.3 ----- 165 ----- ----- 311 ISO4264 56.5 ----- 312 ISO4264 56.3 ----- 323 ISO4264 56.2 ----- 334 ----- ----- 335 ----- ----- 343 D4737 55.9 ----- 430 ----- ----- 431 ----- ----- 433 ----- ----- 445 ISO4264 55.9 ----- 447 ISO4264 55.9 ----- 463 ISO4264 56.1 ----- 494 ISO4264 55.75 ----- 495 ISO4264 56.17 ----- 496 ISO4264 56.221 ----- 541 ----- ----- 657 ISO4264 56.5 ----- 862 ISO4264 55.8 C ----- First reported 53.4 according ASTM D4734 method B 1006 D976 55.0 ex ----- Reported ASTM D976, which has a different calculation routine 1017 ----- ----- 1033 IP380 56.1 ----- 1047 ISO4264 55.9 ----- 1059 ISO4264 55.9 ----- 1065 ISO4264 55.9 ----- 1080 ISO4264 55.9 ----- 1081 ISO4264 55.9 ----- 1095 ----- ----- 1108 ISO4264 56.0 ----- 1126 ISO4264 54.9 ----- 1140 ----- ----- 1192 ----- ----- 1194 D4737 55.5 ----- 1195 ----- ----- 1201 ISO4264 56.2 ----- 1203 ISO4264 56.6 ----- 1205 ----- ----- 1218 ----- ----- 1227 ----- ----- 1300 ISO4264 55.5 ----- 1402 ISO4264 56.2 ----- 1406 D4737 55.94 ----- 1407 ISO4264 55.85 ----- 1409 ISO4264 55.6 ----- 1428 ----- ----- 1501 ISO4264 55.74 ----- 1520 ISO4264 55.54 ----- 1538 ISO4264 56.0 ----- 1634 ISO4264 55.78 ----- 1636 ISO4264 55.89 ----- 1650 D4737 55.6 ----- 1656 IP380 55.6 C ----- First reported 49.4 1706 ----- ----- 1710 ISO4264 56.1 ----- 1724 ISO4264 55.4 ----- 1807 ISO4264 55.6 ----- 1808 ISO4264 55.1 C ----- First reported 52.8 1810 ISO4264 56 ----- 1811 ISO4264 56.4 ----- 1826 ISO4264 56.0 ----- 1829 ISO4264 56.39 ----- 1833 ISO4264 56.22 ----- 1834 ----- ----- 1861 ----- ----- 1911 ISO4264 56.10 ----- 1931 ----- ----- 1948 ----- ----- 1951 ISO4264 55.9 ----- 2129 ISO4264 56.3 ----- 2146 ----- -----



normality not OK n 48 outliers 1 mean (n) 55.94 st.dev. (n) 0.346 R(calc.) 0.97 R(ISO4264:07) unknown Compare R(iis08G03) = 1.28

Kernel Density

0

0.2

0.4

0.6

0.8

1

1.2

1.4

54 55 56 57 58

53

53.5

54

54.5

55

55.5

56

56.5

57

1126

1006

1808

1724

1300

1194

1520

1807

1650

1409

1656

1501

494

1634

862

1407

1636

1081

1080

343

445

447

1047

1065

1951

1059

1406

1538

1810

1108

1826

463

1911

1033

1710

495

1201

323

1402

1833

496

312

150

2129

1829

1811

657

311

1203



Determination of Carbon Residue on 10% distillation residue on sample #0935; result in %M/M

lab method value mark Z(targ) remarks 150 ISO10370 0.01 ----- 165 ----- ----- 311 ISO10370 <0.10 ----- 312 ----- ----- 323 ----- ----- 334 ----- ----- 335 ----- ----- 343 ISO10370 <0.1 ----- 430 ----- ----- 431 ----- ----- 433 ----- ----- 445 IP398 0.04 ----- 447 IP398 <0.1 ----- 463 ISO10370 <0.01 ----- 494 ISO10370 0.008 ----- 495 ISO10370 <0.01 ----- 496 ISO10370 <0.01 ----- 541 ----- ----- 657 ISO10370 0.006 ----- 862 D4530 0.02 C ----- First reported 0.05 1006 D524 0.6 ex ----- Method is not technically equivalent to ISO10370 1017 ----- ----- 1033 ----- ----- 1047 ISO10370 0.026 ----- 1059 ISO10370 0.02 ----- 1065 ----- ----- 1080 ISO10370 0.01 ----- 1081 ISO10370 0.02 ----- 1095 ----- ----- 1108 ----- ----- 1126 ----- ----- 1140 ----- ----- 1192 ----- ----- 1194 ----- ----- 1195 inh-122 0.0064 ----- 1201 ISO10370 0.01 ----- 1203 ISO10370 0.01 ----- 1205 ----- ----- 1218 ----- ----- 1227 ----- ----- 1300 ISO10370 0.0376 ----- 1402 ISO10370 <0.01 ----- 1406 D4530 0.035 ----- 1407 ----- ----- 1409 ISO10370 <0.01 ----- 1428 ISO10370 0.015 ----- 1501 ISO10370 0.022 ----- 1520 ISO10370 0.016 ----- 1538 ISO10370 0.02 ----- 1634 ----- ----- 1636 D4530 0.0231 ----- 1650 ----- ----- 1656 D4530 <0.1 ----- 1706 ----- ----- 1710 ISO10370 0.02 ----- 1724 ISO10370 0.01 ----- 1807 ISO10370 <0.1 ----- 1808 ----- ----- 1810 ----- ----- 1811 ----- ----- 1826 ----- ----- 1829 ISO10370 0.0016 ----- 1833 ISO10370 0.013 ----- 1834 ----- ----- 1861 ----- ----- 1911 ISO10370 0.021 ----- 1931 ----- ----- 1948 ISO10370 0.0281 ----- 1951 ISO10370 0.019 ----- 2129 ISO10370 0.015 ----- 2146 ----- -----



normality OK n 27 outliers 1 mean (n) 0.0179 st.dev. (n) 0.00963 R(calc.) 0.0270 R(ISO10370:93) (0.0168) Application Range 0.1 – 30.0 %M/M

Kernel Density

0

5

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15

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30

35

40

45

-0.05 0 0.05 0.1 0.15 0.2

0

0.01

0.02

0.03

0.04

0.05

0.06

0.07

0.08

0.09

0.1

1829

657

1195

494

1080

1201

1724

1203

150

1833

2129

1428

1520

1951

1710

1538

862

1081

1059

1911

1501

1636

1047

1948

1406

1300

445

1006



Determination of Cloud Point on sample #0935; result in °C

lab method value mark Z(targ) remarks 150 ----- ----- 165 ----- ----- 311 EN23015 -8 0.08 312 EN23015 -9 -0.62 323 EN23015 -9 -0.62 334 EN23015 -8 0.08 335 ----- ----- 343 D2500 -8 0.08 430 ----- ----- 431 ----- ----- 433 ----- ----- 445 IP219 -8 0.08 447 EN23015 -7 0.78 463 EN23015 -9 -0.62 494 EN23015 -8 0.08 495 EN23015 -8 0.08 496 EN23015 -8 0.08 541 ----- ----- 657 EN23015 -9 -0.62 862 D5771 -6.6 1.06 1006 ----- ----- 1017 ----- ----- 1033 D5772 -7.0 0.78 1047 ISO3015 -8 0.08 1059 EN23015 -9 -0.62 1065 D5771 -8.4 -0.20 1080 EN23015 -9 -0.62 1081 D5772 -8.3 -0.13 1095 EN23015 -8 0.08 1108 D5771 -7 0.78 1126 ----- ----- 1140 IP446 -7.4 0.50 1192 ----- ----- 1194 ----- ----- 1195 D2500 -9.6 -1.04 1201 EN23015 -9 -0.62 1203 EN23015 -7 0.78 1205 ----- ----- 1218 ----- ----- 1227 D2500 -8.7 -0.41 1300 EN23015 -8.5 -0.27 1402 EN23015 -7 0.78 1406 ISO3015 -9 -0.62 1407 ----- ----- 1409 EN23015 -8 0.08 1428 EN23015 -9 -0.62 1501 EN23015 -7 0.78 1520 EN23015 -7 0.78 1538 EN23015 -7 0.78 1634 ----- ----- 1636 D2500 -8 0.08 1650 D2500 -8 0.08 1656 IP219 -8 0.08 1706 ----- ----- 1710 EN23015 -9 -0.62 1724 EN23015 -9 -0.62 1807 EN23015 -8 0.08 1808 EN23015 -11 G(0.05) -2.02 1810 EN23015 -8 0.08 1811 EN23015 -7 0.78 1826 EN23015 -8 0.08 1829 EN23015 -9 -0.62 1833 EN23015 -9 -0.62 1834 ----- ----- 1861 ----- ----- 1911 ISO3015 -8.0 0.08 1931 ----- ----- 1948 EN23015 -8 0.08 1951 IP444 -7.4 0.50 2129 EN23015 -9 -0.62 2146 ----- -----



normality not OK n 49 outliers 1 mean (n) -8.12 st.dev. (n) 0.771 R(calc.) 2.16 R(EN23015:94) 4.00

Kernel Density

0

0.05

0.1

0.15

0.2

0.25

0.3

0.35

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-15 -10 -5 0

-15

-13

-11

-9

-7

-5

-3

-1

1

1808

1195

1829

1201

657

1080

1406

1428

1059

1833

1724

323

312

1710

463

2129

1227

1300

1065

1081

1650

1656

1807

1636

1409

1826

1810

496

343

495

445

494

334

1911

311

1095

1948

1047

1140

1951

1811

1108

1203

447

1033

1520

1538

1402

1501

862



Determination of Cold Filter Plugging Point on sample #0935; result in °C

lab method value mark Z(targ) remarks 150 ----- ----- 165 ----- ----- 311 EN116 -26 0.32 312 EN116 -29 -1.26 323 EN116 -28 -0.73 334 EN116 -26 0.32 335 ----- ----- 343 EN116 -26 0.32 430 ----- ----- 431 EN116 -29.0 -1.26 433 ----- ----- 445 IP309 -27 -0.20 447 EN116 -26 0.32 463 EN116 -26 0.32 494 EN116 -27 -0.20 495 EN116 -28 -0.73 496 EN116 -28 -0.73 541 ----- ----- 657 EN116 -28 -0.73 862 D6371 -28 -0.73 1006 D6371 -24 1.38 1017 EN116 -25 0.85 1033 IP309 -28 -0.73 1047 EN116 -30 -1.78 1059 EN116 -25 0.85 1065 EN116 -25 0.85 1080 EN116 -26 0.32 1081 EN116 -25 0.85 1095 EN116 -29 -1.26 1108 ----- ----- 1126 ----- ----- 1140 IP309 -25 0.85 1192 EN116 -26 0.32 1194 EN116 -25.0 0.85 1195 D6371 -25.25 0.72 1201 EN116 -28 -0.73 1203 EN116 -30 -1.78 1205 ----- ----- 1218 ----- ----- 1227 EN116 -27 -0.20 1300 EN116 -27.5 -0.47 1402 EN116 -25.0 0.85 1406 EN116 -28 -0.73 1407 EN116 -28 -0.73 1409 EN116 -26 0.32 1428 EN116 -26 0.32 1501 EN116 -25 0.85 1520 EN116 -27 -0.20 1538 EN116 -25 0.85 1634 ----- ----- 1636 D6371 -26 0.32 1650 EN116 -29 -1.26 1656 IP309 -27 -0.20 1706 ----- ----- 1710 EN116 -24 1.38 1724 EN116 -27 -0.20 1807 EN116 -26 0.32 1808 EN116 -25.5 0.59 1810 EN116 -25 0.85 1811 EN116 -26 0.32 1826 EN116 -24 1.38 1829 EN116 -28 -0.73 1833 EN116 -26 0.32 1834 EN116 -27 -0.20 1861 ----- ----- 1911 EN116 -27.5 -0.47 1931 ----- ----- 1948 EN116 -10 CG(0.01) 8.75 1951 IP307 -27.0 -0.20 2129 EN116 -26 0.32 2146 ----- -----



normality not OK n 55 outliers 1 mean (n) -26.61 st.dev. (n) 1.507 R(calc.) 4.22 R(EN116:98) 5.32

Kernel Density

0

0.05

0.1

0.15

0.2

0.25

-40 -30 -20 -10 0

-35

-30

-25

-20

-15

-10

-5

0

1203

431

1650

862

1033

1407

657

323

1911

1724

1227

1951

1834

1409

311

2129

1807

1080

463

343

1808

1081

1059

1810

1402

1194

1006

1826



Determination of Density @15 °C on sample #0935; result in kg/m3

lab method value mark Z(targ) remarks 150 ISO12185 830.5 0.30 165 ----- ----- 311 ISO12185 830.5 0.30 312 ISO12185 830.3 -0.82 323 ISO12185 830.3 -0.82 334 ISO12185 830.3 -0.82 335 ----- ----- 343 D4052 830.37 -0.42 430 ----- ----- 431 ISO12185 830.45 0.02 433 ISO12185 830.4 -0.26 445 ISO12185 830.6 0.86 447 ISO12185 830.5 0.30 463 ISO12185 830.5 0.30 494 ISO12185 830.5 0.30 495 ISO12185 830.42 -0.14 496 ISO12185 830.25 -1.10 541 ISO3675 831.2 G(0.01) 4.22 657 ISO12185 830.5 0.30 862 D4052 830.51 0.36

1006 D4052 830.5 0.30 1017 D4052 830.5 0.30 1033 IP365 830.4 -0.26 1047 ISO12185 830.3 -0.82 1059 ISO12185 830.2 -1.38 1065 D4052 830.6 0.86 1080 ISO12185 830.4 -0.26 1081 ISO12185 830.6 0.86 1095 ISO12185 830.3 -0.82 1108 ISO12185 830.4 -0.26 1126 D4052 830.5 0.30 1140 IP365 830.5 0.30 1192 ISO12185 830.48 0.19 1194 D1298 831.7 G(0.01) 7.02 1195 D2320 832.7 G(0.01) 12.62 1201 ISO12185 830.2 -1.38 1203 ISO12185 830.5 0.30 1205 ISO12185 830.39 -0.31 1218 ----- ----- 1227 D4052 830.5 0.30 1300 ISO12185 830.4 -0.26 1402 ISO12185 830.3 -0.82 1406 ISO12185 830.41 -0.20 1407 ISO12185 830.59 0.81 1409 ISO12185 830.5 0.30 1428 ISO12185 830.4 -0.26 1501 ISO12185 830.3 -0.82 1520 ISO12185 830.49 0.25 1538 ISO12185 830.56 0.64 1634 ISO12185 830.4 -0.26 1636 D4052 830.5 0.30 1650 D4052 830.46 0.08 1656 D4052 830.4 C -0.26 First reported 836.5 1706 ISO12185 830.4 -0.26 1710 ISO12185 830.4 -0.26 1724 ISO3675 830.5 C 0.30 First reported 831.0 1807 ISO12185 830.51 0.36 1808 ISO3675 831.0 C,G(0.01) 3.10 First reported 834.63 1810 ISO12185 830.4 -0.26 1811 ISO12185 830.4 -0.26 1826 ISO12185 830.5 0.30 1829 ISO12185 830.44 -0.03 1833 ISO12185 830.5 C 0.30 First reported 829.4 1834 ISO12185 830.49 0.25 1861 ----- ----- 1911 ISO12185 830.50 0.30 1931 D4052 830.5 0.30 1948 ISO12185 830.5 0.30 1951 IP365 830.6 0.86 2129 D4052 830.6 0.86 2146 ISO12185 830.495 0.28



normality not OK n 62 outliers 4 mean (n) 830.45 st.dev. (n) 0.097 R(calc.) 0.27 R(ISO12185:96) 0.50

Kernel Density

0

0.5

1

1.5

2

2.5

3

3.5

4

4.5

5

829 830 831 832 833

829.5

830

830.5

831

831.5

832

832.5

833

1059

496

1095

1501

334

343

1810

1080

1300

1634

1656

433

1406

1829

1650

1520

2146

1724

1833

1931

1409

1126

657

1017

1227

150

463

1807

1407

445

1951

1808

1194



Determination of Fatty Acid Methyl Esters content on sample #0935; result in %V/V

lab method value mark Z(targ) remarks 150 D7371 6.15 -0.54 165 ----- ----- 311 EN14078 6.6 0.86 312 ----- ----- 323 EN14078 5.1 DG(0.05) -3.81 334 EN14079 5.11 DG(0.05) -3.78 335 ----- ----- 343 EN14078 6.75 1.33 430 ----- ----- 431 ----- ----- 433 ----- ----- 445 EN14078 6.27 -0.17 447 EN14078 6.3 -0.07 463 ----- ----- 494 ----- ----- 495 EN14078 6.06 -0.82 496 EN14078 6.26 -0.20 541 ----- ----- 657 EN14078 5.6 -2.25 862 EN14078 6.0 -1.01 1006 EN14078 6.4 0.24 1017 ----- ----- 1033 ----- ----- 1047 EN14078 6.24 -0.26 1059 EN14078 6.4 0.24 1065 EN14078 6.20 -0.38 1080 EN14078 6.5 0.55 1081 ----- ----- 1095 EN14078 5.6 -2.25 1108 EN14078 6.0 -1.01 1126 ----- ----- 1140 in house 7 2.10 1192 EN14078 6.41 0.27 1194 EN14078 5.6 -2.25 1195 EN14078 4.5783 G(0.05) -5.43 1201 EN14078 7.1 2.42 1203 EN14078 6.22 -0.32 1205 EN14078 6.2 -0.38 1218 ----- ----- 1227 ----- ----- 1300 EN14078 6.25 -0.23 1402 EN14078 6.22 -0.32 1406 EN14078 6.753 1.34 1407 EN14078 6.45 0.39 1409 EN14078 6.3 -0.07 1428 EN14078 6.4 0.24 1501 ----- ----- 1520 EN14078 6.53 0.64 1538 EN14078 6.16 -0.51 1634 ----- ----- 1636 EN14078 6.72 1.23 1650 EN14078 6.45 0.39 1656 EN14078 6.0 C -1.01 First reported 0.94 1706 EN14078 6.53 0.64 1710 EN14078 6.7 1.17 1724 EN14078 6.478 0.48 1807 EN14078 6.23 -0.29 1808 EN14078 5.92 -1.26 1810 EN14078 6.3 -0.07 1811 EN14078 6.2 -0.38 1826 EN14078 6.5 0.55 1829 ----- ----- 1833 EN14078 6.83 1.58 1834 ----- ----- 1861 ----- ----- 1911 EN14078 6.30 -0.07 1931 ----- ----- 1948 EN14078 7.0 2.10 1951 EN14078 6.0 -1.01 2129 EN14078 5.80 -1.63 2146 ----- -----



normality OK n 46 outliers 3 mean (n) 6.32 st.dev. (n) 0.346 R(calc.) 0.97 R(EN14078:03) 0.90

Kernel Density

0

0.2

0.4

0.6

0.8

1

1.2

1.4

0 2 4 6 8

2

3

4

5

6

7

8

1195

323

334

1194

1095

657

2129

1808

862

1108

1951

1656

495

150

1538

1205

1811

1065

1203

1402

1807

1047

1300

496

445

1409

1911

1810

447

1006

1428

1059

1192

1650

1407

1724

1080

1826

1520

1706

311

1710

1636

343

1406

1833

1140

1948

1201



Determination of Flash Point PMcc on sample #0935; result in °C

lab method value mark Z(targ) remarks 150 ----- ----- 165 ----- ----- 311 ISO2719-AE 58.0 1.14 312 ISO2719-AF 57.5 0.79 323 ISO2719-AF 60.5 DG(0.05) 2.88 334 ISO2719-AF 61.0 DG(0.05) 3.23 335 ----- ----- 343 D93-AE 57 0.44 430 ----- ----- 431 ISO2719-AF 56.5 0.09 433 D6450 70.0 G(0.01) 9.53 445 IP34-AF 56.0 -0.26 447 D93-AF 56.0 -0.26 463 D93-AE 58.0 1.14 494 ISO2719-AE 55.5 -0.61 495 ISO2719-AF 56.5 0.09 496 ISO2719-AE 54.0 -1.66 541 ----- ----- 657 ISO2719-AF 55.0 -0.96 862 D93-MF 54.2 -1.52 1006 D93-A 57 0.44 1017 D93-AE 56 -0.26 1033 IP34-AF 54.5 -1.31 1047 ISO2719-AE 57.5 0.79 1059 ISO2719-AE 57.0 0.44 1065 D93-AE 57 0.44 1080 ISO2719-AE 56.5 0.09 1081 D93-AE 56 -0.26 1095 ISO2719-AE 60.0 2.53 1108 ISO2719-AE 58.0 1.14 1126 ISO2719-AE 56 -0.26 1140 IP34-AE 55.0 -0.96 1192 ISO2719-MF 54 -1.66 1194 ----- ----- 1195 D92-MF 76.8 G(0.01) 14.29 1201 ISO2719-AE 56.0 -0.26 1203 ISO2719-AF 58.0 1.14 1205 D93-AF 57.5 0.79 1218 ----- ----- 1227 D93-AE 67 G(0.01) 7.43 1300 ISO2719-MF 54.0 -1.66 1402 ISO2719-AE 55.0 -0.96 1406 ISO2719-AE 56.0 -0.26 1407 ISO2719-AE 57.5 0.79 1409 ISO2719-AF 63.0 G(0.01) 4.63 1428 ISO2719-AE 55.5 -0.61 1501 D7094-AE 55.9 -0.33 1520 ISO2719-MF 54.9 -1.03 1538 ISO2719-AE 59.0 1.84 1634 ISO2719-AE 56.0 -0.26 1636 D93-AE 55.5 -0.61 1650 D93-AE 56.0 -0.26 1656 IP34-AF 56 C -0.26 First reported 60.3 1706 ISO2719-AE 56.2 -0.12 1710 ISO2719-AF 57.5 0.79 1724 ISO2719-AE. 57.5 0.79 1807 ISO2719-AE 56.5 0.09 1808 ISO2719-MF 56.5 C 0.09 First reported 63.76 1810 ISO2719-AF 55.5 -0.61 1811 ISO2719-AF 55.5 -0.61 1826 ISO2719-M 58.5 1.49 1829 ISO2719-ME 56 -0.26 1833 ISO2719-AF 56 -0.26 1834 ISO2719-MF 55 -0.96 1861 ----- ----- 1911 ISO2719-AE 56.00 -0.26 1931 ----- ----- 1948 ISO2719-AE 58.0 1.14 1951 IP34-AE 56.0 -0.26 2129 ISO2719-AE 58.5 1.49 2146 ----- -----



Only ISO2719/D93/IP34 – AE data

Only ISO2719/D93/IP34 – AF data

Only ISO2719/D93/IP34 – MF data

normality not OK not OK OK OK n 55 32 14 7 outliers 6 1 3 1 mean (n) 56.38 56.64 56.29 55.30 st.dev. (n) 1.309 1.283 1.032 1.659 R(calc.) 3.66 3.59 2.89 4.65 R(ISO2719:02) 4.00 4.02 4.00 4.00

M = Manual; A = Automated; E = Electric; F = Flame

Kernel Density

0

0.05

0.1

0.15

0.2

0.25

0.3

50 60 70 80 90

50

55

60

65

70

75

80

1300

1192

1033

1402

1834

1810

1811

494

1829

1656

1634

1650

1833

1951

1017

1706

1080

1808

343

1006

312

1047

1407

1948

1108

311

1826

1095

334

1227

1195



Determination of Kinematic Viscosity @ 40°C on sample #0935; result in mm2/s

lab method value mark Z(targ) remarks 150 ISO3104 2.741 -0.28 165 ----- ----- 311 ISO3104 2.737 -0.65 312 ISO3104 2.745 0.08 323 ISO3104 2.747 0.26 334 ISO3104 2.730 -1.29 335 ----- ----- 343 D445 2.746 0.17 430 ----- ----- 431 ISO3104 2.7496 0.50 433 ----- ----- 445 IP71 2.754 0.90 447 D443 2.8184 G(0.05) 6.77 463 ----- ----- 494 ISO3104 2.753 0.81 495 ISO3104 2.7334 -0.98 496 ISO3104 2.753 0.81 541 ISO3104 2.762 1.63 657 ISO3104 2.753 0.81 862 D445 2.7332 -1.00 1006 D445 2.7392 -0.45 1017 ----- ----- 1033 IP71 2.758 1.27 1047 ISO3104 2.742 -0.19 1059 ISO3104 2.742 -0.19 1065 D445 2.721 C -2.11 First reported 2.707 1080 ISO3104 2.740 -0.38 1081 D445 2.743 -0.10 1095 ISO3104 2.738 -0.56 1108 ISO3104 2.658 G(0.01) -7.85 1126 D445 2.779 DG(0.05) 3.18 1140 IP71 2.743 -0.10 1192 ISO3104 2.743 -0.10 1194 ----- ----- 1195 D445 2.7890 G(0.05) 4.09 1201 D445 2.763 1.72 1203 ISO3104 2.744 -0.01 1205 ----- ----- 1218 ----- ----- 1227 ----- ----- 1300 ISO3104 2.7360 -0.74 1402 ISO3104 2.661 G(0.01) -7.58 1406 ISO3104 2.7406 -0.32 1407 ISO3104 2.7318 -1.12 1409 ISO3104 2.748 0.35 1428 ISO3104 2.744 -0.01 1501 D7042 2.7413 -0.26 1520 ISO3104 2.7240 -1.84 1538 ISO3104 2.7369 -0.66 1634 ----- ----- 1636 D445 2.7652 1.92 1650 D445 2.7395 -0.42 1656 IP71 2.55 C,G(0.01) -17.70 First reported 2.7002 1706 ISO3104 2.7423 -0.17 1710 ISO3104 2.749 0.44 1724 ISO3104 2.753 0.81 1807 ISO3104 2.7456 0.13 1808 ISO3104 2.7437 C -0.04 First reported 2.69977 1810 ISO3104 2.761 1.54 1811 ISO3104 2.7635 1.77 1826 ISO3104 2.757 1.17 1829 ISO3104 2.74499 0.08 1833 ISO3104 2.72 -2.20 1834 ISO3104 2.7405 -0.33 1861 ----- ----- 1911 ISO3104 2.74308 -0.10 1931 D445 2.7327 -1.04 1948 ISO3104 2.7514 0.66 1951 IP71 2.7785 DG(0.05) 3.14 2129 ISO3104 2.7418 -0.21 2146 ----- -----



normality OK n 51 outliers 7 mean (n) 2.7441 st.dev. (n) 0.01026 R(calc.) 0.0287 R(ISO3104:94) 0.0307

Kernel Density

0

5

10

15

20

25

30

35

40

2.5 2.6 2.7 2.8 2.9

2.5

2.55

2.6

2.65

2.7

2.75

2.8

2.85

1656

1402

1065

334

1931

495

1538

1095

1650

1834

150

2129

1047

1192

1140

1808

1203

312

343

1409

431

1724

657

445

1033

541

1811

1951

1195



Determination of Lubricity by HFRR on sample #0935; result in μm

lab method value mark Z(targ) remarks 150 ISO12156 200 0.01 165 ----- ----- 311 ISO12156 202 0.06 312 ISO12156 193 -0.19 323 ----- ----- 334 ISO12156 166 -0.93 335 ----- ----- 343 ISO12156 197 -0.08 430 ISO12156 204 0.12 431 ----- ----- 433 ----- ----- 445 ISO12156 175 -0.68 447 ISO12156 173 -0.74 463 ISO12156 193.3 -0.18 494 ISO12156 238 1.05 495 ISO12156 201 0.03 496 ISO12156 212 0.34 541 ----- ----- 657 ISO12156 192 -0.21 862 ISO12156 204 0.12 1006 D6079 203.3 0.10 1017 ----- ----- 1033 ISO12156 172 -0.76 1047 ISO12156 202 0.06 1059 ISO12156 176 -0.65 1065 ----- ----- 1080 ISO12156 198 -0.05 1081 ISO12156 211 0.31 1095 ISO12156 210 C 0.28 First reported 126 1108 ISO12156 212 0.34 1126 ----- ----- 1140 ----- ----- 1192 ----- ----- 1194 ----- ----- 1195 ----- ----- 1201 ISO12156 188 -0.32 1203 ISO12156 193 -0.19 1205 ----- ----- 1218 ----- ----- 1227 ----- ----- 1300 ISO12156 243 1.19 1402 ISO12156 185 -0.41 1406 ISO12156 220.9 0.58 1407 ----- ----- 1409 ISO12156 167 -0.90 1428 ISO12156 215 0.42 1501 ISO12156 225 0.69 1520 ISO12156 278 DG(0.01) 2.15 1538 ISO12156 184 -0.43 1634 ----- ----- 1636 ----- ----- 1650 ISO12156 287 DG(0.01) 2.39 1656 IP450 364 G(0.01) 4.51 1706 ----- ----- 1710 ISO12156 189 -0.30 1724 ISO12156 208 0.23 1807 ----- ----- 1808 ----- ----- 1810 ISO12156 215 0.42 1811 ISO12156 208 0.23 1826 ISO12156 191 -0.24 1829 ----- ----- 1833 ISO12156 184 -0.43 1834 ----- ----- 1861 ----- ----- 1911 ----- ----- 1931 ----- ----- 1948 ISO12156 270.16 G(0.05) 1.93 1951 IP450 236 0.99 2129 ISO12156 205 0.14 2146 ----- -----




Kernel Density

0

0.005

0.01

0.015

0.02

0.025

0 100 200 300 400 500

0

50

100

150

200

250

300

350

400

334

1409

1033

447

445

1059

1833

1538

1402

1201

1710

1826

657

1203

312

463

343

1080

150

495

311

1047

1006

862

430

2129

1724

1811

1095

1081

1108

496

1428

1810

1406

1501

1951

494

1300

1948

1520

1650

1656



Determination of Oxidation Stability on sample #0935; result in g/m3

lab method value mark Z(targ) remarks

150 ----- ----- 165 ----- ----- 311 ----- ----- 312 ----- ----- 323 ----- ----- 334 ----- ----- 335 ----- ----- 343 D2274 2.3 -0.06 430 ----- ----- 431 ----- ----- 433 ----- ----- 445 IP388 4.9 0.92 447 ISO12205 3 0.21 463 ----- ----- 494 ISO12205 <0.1 ----- False negative? 495 ----- ----- 496 ----- ----- 541 ----- ----- 657 ISO12205 4 0.58 862 D2274 0.3 -0.81 1006 D2274 0.6 -0.69 1017 ----- ----- 1033 ----- ----- 1047 ISO12205 5.2 C 1.03 First reported 7 1059 ISO12205 <1 ----- 1065 ----- ----- 1080 ----- ----- 1081 ----- ----- 1095 ISO12205 2 -0.17 1108 ----- ----- 1126 ----- ----- 1140 ----- ----- 1192 ----- ----- 1194 ----- ----- 1195 ----- ----- 1201 ISO12205 5 0.96 1203 ISO12205 2.0 -0.17 1205 ----- ----- 1218 ----- ----- 1227 ----- ----- 1300 ISO12205 1.85705 -0.22 1402 ISO12205 <1 ----- 1406 ----- ----- 1407 ----- ----- 1409 ISO12205 3 0.21 1428 ISO12205 4.5 0.77 1501 ISO12205 3.1 0.25 1520 ISO12205 1.6 -0.32 1538 ISO12205 3 0.21 1634 ----- ----- 1636 ----- ----- 1650 ----- ----- 1656 ----- ----- 1706 ----- ----- 1710 ISO12205 1 -0.54 1724 ISO12205 1.14 -0.49 1807 ISO12205 1.1 -0.51 1808 ----- ----- 1810 ----- ----- 1811 ----- ----- 1826 ----- ----- 1829 ----- ----- 1833 ISO12205 0.85 -0.60 1834 ----- ----- 1861 ----- ----- 1911 ----- ----- 1931 ----- ----- 1948 ISO12205 2.0 -0.17 1951 ----- ----- 2129 ISO12205 1.4 -0.39 2146 ----- -----




Kernel Density

0

0.05

0.1

0.15

0.2

0.25

0.3

-5 0 5 10

0

2

4

6

8

10

12

862

1006

1833

1710

1807

1724

2129

1520

1300

1948

1095

1203

343

1538

447

1409

1501

657

1428

445

1201

1047



Determination of Polycyclic Aromatic Hydrocarbons on sample #0935; result in %M/M

lab method value mark Z(targ) remarks 150 ----- ----- 165 ----- ----- 311 EN12916 2.2 -0.86 312 ----- ----- 323 EN12916 2.6 0.35 334 ----- ----- 335 ----- ----- 343 EN12916 2.4 -0.26 430 ----- ----- 431 ----- ----- 433 ----- ----- 445 IP391 2.80 0.95 447 ----- ----- 463 ----- ----- 494 ----- ----- 495 EN12916 2.58 0.29 496 EN12916 2.54 0.16 541 ----- ----- 657 EN12916 2.3 -0.56 862 EN12916 2.17 -0.96 1006 D6591 3.34 2.59 1017 ----- ----- 1033 ----- ----- 1047 EN12916 2.17 -0.96 1059 EN12916 2.0 -1.47 1065 ----- ----- 1080 EN12916 1.93 -1.68 1081 IP391 1.8 -2.08 1095 EN12916 3.19 2.13 1108 EN12916 2.4 -0.26 1126 ----- ----- 1140 ----- ----- 1192 ----- ----- 1194 D6591 0.85 G(0.05) -4.95 1195 ----- ----- 1201 EN12916 2.2 -0.86 1203 EN12916 2.2 -0.86 1205 ----- ----- 1218 IP391 3.68 DG(0.05) 3.62 1227 EN12916 3.02 1.62 1300 EN12916 2.5138 C 0.09 First reported 3.6415 1402 EN12916 2.7 0.65 1406 EN12916 3.90 DG(0.05) 4.28 1407 ----- ----- 1409 EN12916 3.1 1.86 1428 EN12916 2.4 -0.26 1501 INH-840 2.40 -0.26 1520 EN12916 2.88 C 1.19 First reported 3.6 1538 EN12916 2.4 -0.26 1634 ----- ----- 1636 ----- ----- 1650 ----- ----- 1656 ----- ----- 1706 ----- ----- 1710 EN12916 2.4 -0.26 1724 EN12916 2.90 1.25 1807 ----- ----- 1808 ----- ----- 1810 ----- ----- 1811 EN12916 2.95 1.41 1826 IP391 5.2 G(0.01) 8.22 1829 INHOUSE 2.12 -1.11 1833 EN12916 2.62 C 0.41 First reported 3.93 1834 ----- ----- 1861 EN12916 2.437 -0.15 1911 ----- ----- 1931 ----- ----- 1948 EN12916 2.61 0.38 1951 IP391 4.6 G(0.05) 6.40 2129 EN12916 1.98 -1.53 2146 EN12916 2.262 -0.68



normality OK n 34 outliers 5 mean (n) 2.49 st.dev. (n) 0.374 R(calc.) 1.05 R(EN12916:06) 0.93

Kernel Density

0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

0 2 4 6 8

0

1

2

3

4

5

6

1194

1081

1080

2129

1059

1829

1047

862

311

1201

1203

2146

657

1501

343

1428

1710

1108

1538

1861

1300

496

495

323

1948

1833

1402

445

1520

1724

1811

1227

1409

1095

1006

1218

1406

1951

1826



Determination of Sulphur on sample #0935; result in mg/kg

lab method value mark Z(targ) remarks 150 ISO20846 7.7 0.17 165 ----- ----- 311 ISO20884 7 -0.53 312 ISO20884 6.7 -0.83 323 ISO20884 8.1 0.57 334 ISO20884 6.8 -0.73 335 ----- ----- 343 ISO20846 7.2 -0.33 430 ----- ----- 431 ----- ----- 433 ----- ----- 445 D5453 6.8 -0.73 447 D5453 7.36 -0.17 463 ISO20884 7.1 -0.43 494 ISO20846 7.6 0.07 495 ISO20884 8.3 0.77 496 ISO20846 9.02 1.48 541 ----- ----- 657 ISO20846 6.6 -0.93 862 D5453 7.9 0.37 1006 D5453 7.5 -0.03 1017 ----- ----- 1033 ----- ----- 1047 ISO20846 7.7 0.17 1059 ISO20884 7.6 0.07 1065 D7212 12.9 G(0.01) 5.36 1080 ISO20846 7.7 0.17 1081 ISO20846 6.9 -0.63 1095 ----- ----- 1108 ISO20846 8.1 0.57 1126 ISO20846 7.1 -0.43 1140 D7212 6 -1.53 1192 ISO20884 7.4 -0.13 1194 D7220 22.85 G(0.01) 15.29 1195 ----- ----- 1201 D5453 6.4 -1.13 1203 ISO20884 7.7 0.17 1205 D5453 6.80 -0.73 1218 ISO20884 8.0 0.47 1227 D5453 7.68 0.15 1300 ISO20846 9.554 2.02 1402 IP490 7.2 -0.33 1406 ISO20846 7.70 0.17 1407 ISO20846 7.96 0.43 1409 ISO20884 7.6 0.07 1428 ISO20846 7.0 -0.53 1501 ISO20846 7.74 0.21 1520 ISO20846 7.79 0.26 1538 ISO20884 8.38 0.85 1634 ----- ----- 1636 D5453 7.99 0.46 1650 ----- ----- 1656 D5453 8 0.47 1706 ISO20884 7.9 0.37 1710 ISO20884 7.7 0.17 1724 ISO20846 7.06 -0.47 1807 ISO20884 7.45 -0.08 1808 ----- ----- 1810 ISO20884 7.5 -0.03 1811 ISO20884 7.6 0.07 1826 ----- ----- 1829 ISO20884 8.28 0.75 1833 ISO20884 7.25 -0.28 1834 ISO20846 8.55 1.01 1861 D5453 7.08 -0.45 1911 ISO20846 8.06 0.53 1931 D5453 4.38 G(0.01) -3.15 1948 ISO20884 8.43 0.90 1951 IP490 5.7 -1.83 2129 IP490 6.30 -1.23 2146 ISO20846 8.27 0.74



ISO20846 only: ISO20884 only: D5453 only: normality OK OK OK OK n 54 20 20 10 outliers 3 0 0 1 mean (n) 7.533 7.765 7.640 7.351 st.dev. (n) 0.7097 0.7211 0.5127 0.5624 R(calc.) 1.987 2.019 1.435 1.575 R(ISO20884:04) 2.805 1.990 2.818 2.588

Kernel Density

0

0.1

0.2

0.3

0.4

0.5

0.6

0 5 10 15 20 25

0

5

10

15

20

25

1931

1140

1201

312

334

1081

311

1861

463

1402

447

1807

1810

494

1811

1710

1080

1406

1501

1706

1407

1218

1911

323

1829

1538

1834

1300

1194



Determination of Total Contamination on sample #0935; result in mg/kg

lab method value mark Z(targ) remarks 150 EN12662 3.26 ----- 165 ----- ----- 311 EN12662 6 ----- 312 ----- ----- 323 ----- ----- 334 ----- ----- 335 ----- ----- 343 EN12662 3.7 ----- 430 ----- ----- 431 ----- ----- 433 ----- ----- 445 IP440 5.5 ----- 447 EN12662 0.80 ----- 463 EN12662 1.85 ----- 494 EN12662 4.9 ----- 495 EN12662 3.6 ----- 496 EN12662 2.7 ----- 541 EN12662 5.07 ----- 657 EN12662 3.0 ----- 862 EN12662 3 ----- 1006 EN12662 7.9 ----- 1017 ----- ----- 1033 ----- ----- 1047 ----- ----- 1059 EN12662 2.9 ----- 1065 ----- ----- 1080 ----- ----- 1081 ----- ----- 1095 EN12662 7.6 ----- 1108 EN12662 2.1 ----- 1126 ----- ----- 1140 ----- ----- 1192 ----- ----- 1194 ----- ----- 1195 ----- ----- 1201 EN12662 2 ----- 1203 EN12662 9.2 ----- 1205 ----- ----- 1218 ----- ----- 1227 ----- ----- 1300 EN12662 1.142 ----- 1402 EN12662 4.3 ----- 1406 ----- ----- 1407 ----- ----- 1409 EN12662Mod. 3.8 ----- 1428 EN12662 3.6 ----- 1501 EN12662 3.9 ----- 1520 EN12662 3.29 ----- 1538 EN12662 4.4 ----- 1634 ----- ----- 1636 ----- ----- 1650 EN12662 3.94 ----- 1656 IP440 7 C ----- First reported 3.982 1706 ----- ----- 1710 EN12662 6 ----- 1724 EN12662 3.195 ----- 1807 EN12662 5.82 ----- 1808 ----- ----- 1810 ----- ----- 1811 ----- ----- 1826 EN12662 4 ----- 1829 EN12662 1.2 ----- 1833 EN12662 4.26 ----- 1834 ----- ----- 1861 ----- ----- 1911 ----- ----- 1931 EN12662 5.0 ----- 1948 EN12662 0.0144 ex ----- Probably reported in a deviating unit 1951 IP440 13.8 G(0.01) ----- 2129 EN12662 5.0 C ----- First reported 10.6 2146 ----- -----



normality OK n 35 outliers 1 mean (n) 4.14 st.dev. (n) 1.932 R(calc.) 5.41 R(EN12662:08) (1.24) Application range 6 – 30 mg/kg

Kernel Density

0

0.05

0.1

0.15

0.2

0.25

-5 0 5 10 15 20

0

2

4

6

8

10

12

14

16

1948

447

1300

1829

463

1201

1108

496

1059

862

657

1724

150

1520

495

1428

343

1409

1501

1650

1826

1833

1402

1538

494

1931

2129

541

445

1807

1710

311

1656

1095

1006

1203

1951



Determination of Water on sample #0935; result in mg/kg

lab method value mark Z(targ) remarks 150 ISO12937 61 -0.10 165 ----- ----- 311 ISO12937 56 -0.35 312 ISO12937 70 0.37 323 ISO12937 60 -0.15 334 ISO12937 65 0.11 335 ----- ----- 343 ISO12937 61.4 -0.08 430 ----- ----- 431 ----- ----- 433 ----- ----- 445 IP438 65.1 0.11 447 IP438 64.2 0.07 463 ISO12937 45.5 -0.89 494 ISO12937 52 -0.56 495 ISO12937 76 0.67 496 ISO12937 70 0.37 541 ISO12937 76.6 0.70 657 ISO12937 60 C -0.15 First reported 340 862 D6304 62 -0.05 1006 D6304 74.5 0.60 1017 ISO12937 330 G(0.01) 13.72 1033 IP438 68.3 0.28 1047 ISO12937 61 -0.10 1059 ISO12937 60 -0.15 1065 D6304 83.3 1.05 1080 ISO12937 65 0.11 1081 D6304 43 -1.02 1095 ISO12937 67 0.21 1108 ISO12937 52 -0.56 1126 ----- ----- 1140 IP438 53 -0.51 1192 ISO12937 70.02 C 0.37 First reported 387.86 1194 ----- ----- 1195 ----- ----- 1201 ISO12937 100 1.91 1203 ISO12937 39 -1.23 1205 ----- ----- 1218 ----- ----- 1227 ----- ----- 1300 ISO12937 42.86 -1.03 1402 ISO12937 70 0.37 1406 ISO12937 56.6 -0.32 1407 ISO12937 65.0 0.11 1409 ISO12937 73 0.52 1428 ISO12937 64.7 0.09 1501 ISO12937 62.8 0.00 1520 ISO12937 61.00 -0.10 1538 ISO12937 66 0.16 1634 ----- ----- 1636 D6304 85.2 1.15 1650 IP438 62 -0.05 1656 IP386 121 C,G(0.01) 2.98 First reported 53.39 1706 ----- ----- 1710 ISO12937 59 -0.20 1724 ISO12937 64.6 0.09 1807 ISO12937 50.08 -0.66 1808 ISO12937 17.9 DG(0.05) -2.31 1810 ISO12937 80 0.88 1811 ISO12937 82 0.98 1826 ISO12937 60 -0.15 1829 ISO12937 25.0 DG(0.05) -1.94 1833 ISO12937 54 -0.46 1834 ISO12937 60.56 -0.12 1861 D6304 43.77 -0.98 1911 ISO12937 70.5 0.39 1931 E203 166.19 G(0.01) 5.30 1948 ISO12937 72.6 0.50 1951 IP438 52.6 -0.53 2129 IP439 30 -1.69 2146 ----- -----




Kernel Density

0

0.005

0.01

0.015

0.02

0.025

0.03

0.035

0.04

0 100 200 300 400

0

50

100

150

200

250

300

350

1808

2129

1300

1861

1807

494

1140

311

1710

657

1826

1520

1047

1650

1501

1724

1407

334

1538

1033

1402

1192

1948

1006

541

1811

1636

1656

1017



Determination of Distillation (Automated+Manual) ASTM ISO3405 on sample #0935; result in °C Lab method IBP mark 5% mark 10% mark 50% mark 90% mark FBP mark

150 ISO3405 175.0 203.3 215.7 274.6 331.3 352.4 165 ----- ----- ----- ----- ----- ----- 311 ISO3405 172.7 202.3 215.7 276.1 335.4 361.7 312 ISO3405 173.3 202.7 217.2 273.7 331.4 355.2 323 ISO3405 176.5 202.7 216.6 273.6 332.2 357.0 334 ISO3405 173.3 203.6 215.7 273.4 332.5 358.6 335 ----- ----- ----- ----- ----- ----- 343 D86 183.7 DG(0.05) 203.0 217.1 272.3 327.9 351.6 430 ----- ----- ----- ----- ----- ----- 431 ----- 201.7 216.5 272.1 331.1 ----- 433 ----- ----- ----- ----- ----- ----- 445 ISO3405 174.5 203.4 216.5 273.0 332.2 357.3 447 D86 173.7 201.2 214.7 273.4 331.5 360.1 463 D86 170.6 201.2 217.0 273.4 333.3 359.0 494 ISO3405 169.8 201.3 215.9 272.1 329.7 353.9 495 ISO3405 172.5 203.8 217.7 273.2 331.3 358.0 496 ISO3405 171.3 204.5 216.4 273.7 333.6 356.6 541 ----- ----- ----- ----- ----- ----- 657 ISO3405 169.3 204.9 219.0 274.3 333.1 357.7 862 D86 168.7 202.1 215.6 272.6 332.2 357.5 1006 D86 173.7 201.1 215.0 272.6 334.0 358.1 1017 D86 165.9 202.4 218.5 273.0 331.7 357.3 1033 IP123 175.0 202.1 215.6 273.8 334.0 357.2 1047 ISO3405 170.6 200.4 212.9 273.9 334.1 357.2 1059 ISO3405 172.4 199.9 215.7 272.3 330.3 355.7 1065 D86 176.7 203.4 215.5 273.1 331.9 362.1 1080 ISO3405 170.9 202.1 215.0 273.2 333.7 356.4 1081 D86 174 202.3 215.6 273.4 332.5 353.8 1095 ----- ----- ----- ----- ----- ----- 1108 ISO3405 173.6 202.3 215.6 273.3 333.2 357.7 1126 inhouse 171.4 202.6 214.6 271.8 333.2 364.6 1140 D95 172.1 203.3 216.1 272.8 331.3 357.0 1192 ISO3405 172.7 200.7 212.4 270.7 329.7 353.3 1194 ISO3405 156.65 G(0.01) 194.10 DG(0.05) 208.20 G(0.01) 273.55 332.85 347.70 G(0.05) 1195 ----- ----- ----- ----- ----- ----- 1201 ISO3405 169.0 201.6 215.4 273.9 336.1 356.8 1203 ISO3405 172.2 204.4 217.2 275.8 336.1 356.5 1205 D86 179.1 208.4 G(0.05) 219.8 275.4 334.1 360.1 1218 ----- ----- ----- ----- ----- ----- 1227 D86 169.0 196.0 DG(0.05) 211.8 273.0 331.0 355.6 1300 ISO3405-M 171.0 198.0 213.0 272.0 329.0 356.0 1402 ISO3405 177.4 204.3 216.0 274.4 333.6 361.2 1406 ISO3405 181.4 DG(0.05) 204.2 217.1 272.3 328.4 353.4 1407 ISO3405 185.2 G(0.05) 203.2 216.0 272.8 329.8 353.5 1409 ISO3405 173.0 196.6 213.0 272.6 330.5 356.9 1428 ISO3405 174.7 Fr 163.5 202.4 Fr 198.4 216.5 Fr 210.9 273.2 Fr 270.8 330.1 Fr 329.2 357.4 Fr 354.21501 ISO3405-M 172.4 202.4 214.4 272.3 331.7 359.7 1520 ISO3405 168.0 ----- 212.9 272.4 333.3 356.8 1538 ISO3405-M 172.0 202.4 215.4 273.8 332.4 354.4 1634 ISO3405 174.0 203.9 216.2 271.9 330.3 358.8 1636 D86 166.2 198.8 213.5 273.9 333.7 358.8 1650 D86 168.6 203.4 212.7 272.9 333.3 359.2 1656 IP123 167.5 Fr 167.5 199.8 Fr 192.6 213.2 Fr 201.5 272.5 Fr 257.5 330.5 355.6 Fr 358.01706 ISO3405 173.5 202.0 216.2 273.6 331.7 359.0 1710 ISO3405 168.8 203.2 216.0 273.4 332.0 357.2 1724 ISO3405 167.2 201.4 213.6 272.5 330.0 351.8 1807 ISO3405 167.8 195.9 DG(0.05) 211.7 272.5 330.5 355.0 1808 ISO3405-M 167 194.5 DG(0.05) 211 270 329.5 353 1810 ISO3405 174.4 203.2 215.5 272.8 330.0 354.6 1811 ISO3405 177.0 204.7 218.6 274.0 333.0 356.9 1826 ISO3405 173.5 201.7 216.4 272.8 331.3 356.6 1829 ISO3405 174.1 203.0 217.2 274.5 332.9 360.0 1833 ISO3405 170.3 200.9 215.0 272.4 332.3 359.4 1834 ISO3405 177.3 203.8 215.3 273.4 330.5 353.6 1861 ----- ----- ----- ----- ----- ----- 1911 ISO3405 174.25 203.00 217.00 273.40 332.75 356.20 1931 ----- ----- ----- ----- ----- ----- 1948 ISO3405 172.8 204.3 217.1 272.7 331.4 357.0 1951 IP123 172.2 203.3 215.8 273.3 331.7 360.6 2129 ISO3405 173.1 203.9 217.6 274.3 332.2 358.7 2146 ISO3405 171.6 199.2 214.1 273.1 334.3 355.3



normality OK not OK not OK OK OK OK n 56 55 60 61 61 59 outliers 4 5 1 0 0 1 mean (n) 172.13 202.31 215.53 273.16 331.99 356.99 st.dev. (n) 3.001 1.698 1.832 1.030 1.748 2.629 R(calc.) 8.40 4.75 5.13 2.88 4.89 7.36 R(ISO3405:00-A) 8.50 12.98 7.16 8.68 6.24 10.50 R(ISO3405:00-M) 8.41 7.57 3.89 3.74 4.03 4.15 R (ISO3405:05) IBP: 8.50 (table 10) 5%: 12.98 = 2.0 + 2.53 x C/%V and C/%V = 4.34 automated 10%: 7.16 = 3.0 + 2.64 x C/%V and C/%V = 1.57 50%: 8.68 = 2.9 + 3.97 x C/%V and C/%V = 1.46 90%: 6.24 = 2.0 + 2.53 x C/%V and C/%V = 1.68 FBP: 10.50

150

155

160

165

170

175

180

185

190

1194

1636

1724

1807

1650

1710

1227

494

463

1080

496

2146

1140

1203

1059

1192

1948

2129

312

1706

447

1634

1829

1810

1428

150

1065

1834

1205

343

Initial Boiling Point

200

205

210

215

220

225

1194

1807

1192

1520

1300

1656

1724

1501

447

1006

1834

1201

1065

1108

1081

311

1059

494

1402

1140

1706

1826

1428

323

463

1406

1829

312

495

1811

1205

10% recovered

320

322

324

326

328

330

332

334

336

338

340

343

1300

1192

1407

1724

1059

1834

1807

1227

1140

1826

1948

447

1951

1706

1710

2129

445

1538

334

1194

1811

1108

1520

1650

496

1636

1033

1205

311

1201

90% recovered

330

335

340

345

350

355

360

365

370

1194

1724

1808

1406

1834

494

1810

312

1227

1059

1911

1203

1826

1520

1409

323

1710

1033

445

862

657

1006

2129

1636

1706

1833

1829

1205

1402

1065

Final Boiling Point

Kernel Density

0

0.02

0.04

0.06

0.08

0.1

0.12

0.14

150 160 170 180 190 200

Kernel Density

0

0.05

0.1

0.15

0.2

0.25

0.3

200 205 210 215 220 225

Kernel Density

0

0.05

0.1

0.15

0.2

0.25

300 310 320 330 340 350

Kernel Density

0

0.02

0.04

0.06

0.08

0.1

0.12

0.14

0.16

0.18

340 350 360 370



APPENDIX 2 Z-scores Distillation lab IBP 5% 10% 50% 90% FBP150 0.95 0.21 0.07 0.46 -0.31 -1.22165 ----- ----- ----- ----- ----- -----311 0.19 0.00 0.07 0.95 1.53 1.26312 0.39 0.08 0.65 0.17 -0.26 -0.48323 1.44 0.08 0.42 0.14 0.10 0.00334 0.39 0.28 0.07 0.08 0.23 0.43335 ----- ----- ----- ----- ----- -----343 3.81 0.15 0.61 -0.28 -1.83 -1.44430 ----- ----- ----- ----- ----- -----431 ----- -0.13 0.38 -0.34 -0.40 -----433 ----- ----- ----- ----- ----- -----445 0.78 0.23 0.38 -0.05 0.10 0.08447 0.52 -0.24 -0.33 0.08 -0.22 0.83463 -0.50 -0.24 0.57 0.08 0.59 0.54494 -0.77 -0.22 0.14 -0.34 -1.03 -0.82495 0.12 0.32 0.85 0.01 -0.31 0.27496 -0.27 0.47 0.34 0.17 0.72 -0.10541 ----- ----- ----- ----- ----- -----657 -0.93 0.56 1.36 0.37 0.50 0.19862 -1.13 -0.05 0.03 -0.18 0.10 0.141006 0.52 -0.26 -0.21 -0.18 0.90 0.301017 -2.05 0.02 1.16 -0.05 -0.13 0.081033 0.95 -0.05 0.03 0.21 0.90 0.061047 -0.50 -0.41 -1.03 0.24 0.95 0.061059 0.09 -0.52 0.07 -0.28 -0.76 -0.341065 1.51 0.23 -0.01 -0.02 -0.04 1.361080 -0.40 -0.05 -0.21 0.01 0.77 -0.161081 0.62 0.00 0.03 0.08 0.23 -0.851095 ----- ----- ----- ----- ----- -----1108 0.48 0.00 0.03 0.05 0.54 0.191126 -0.24 0.06 -0.37 -0.44 0.54 2.031140 -0.01 0.21 0.22 -0.12 -0.31 0.001192 0.19 -0.35 -1.23 -0.79 -1.03 -0.981194 -5.10 -1.77 -2.87 0.13 0.39 -2.481195 ----- ----- ----- ----- ----- -----1201 -1.03 -0.15 -0.05 0.24 1.85 -0.051203 0.02 0.45 0.65 0.85 1.85 -0.131205 2.30 1.31 1.67 0.72 0.95 0.831218 ----- ----- ----- ----- ----- -----1227 -1.03 -1.36 -1.46 -0.05 -0.44 -0.371300 -0.37 -0.93 -0.99 -0.37 -1.34 -0.261402 1.74 0.43 0.18 0.40 0.72 1.121406 3.05 0.41 0.61 -0.28 -1.61 -0.961407 4.31 0.19 0.18 -0.12 -0.98 -0.931409 0.29 -1.23 -0.99 -0.18 -0.67 -0.021428 0.85 0.02 0.38 0.01 -0.85 0.111501 0.09 0.02 -0.44 -0.28 -0.13 0.721520 -1.36 ----- -1.03 -0.25 0.59 -0.051538 -0.04 0.02 -0.05 0.21 0.19 -0.691634 0.62 0.34 0.26 -0.41 -0.76 0.481636 -1.95 -0.76 -0.80 0.24 0.77 0.481650 -1.16 0.23 -1.11 -0.08 0.59 0.591656 -1.52 -0.54 -0.91 -0.21 -0.67 -0.371706 0.45 -0.07 0.26 0.14 -0.13 0.541710 -1.10 0.19 0.18 0.08 0.01 0.061724 -1.62 -0.20 -0.76 -0.21 -0.89 -1.381807 -1.43 -1.38 -1.50 -0.21 -0.67 -0.531808 -1.69 -1.69 -1.77 -1.02 -1.11 -1.061810 0.75 0.19 -0.01 -0.12 -0.89 -0.641811 1.60 0.51 1.20 0.27 0.46 -0.021826 0.45 -0.13 0.34 -0.12 -0.31 -0.101829 0.65 0.15 0.65 0.43 0.41 0.801833 -0.60 -0.31 -0.21 -0.25 0.14 0.641834 1.70 0.32 -0.09 0.08 -0.67 -0.901861 ----- ----- ----- ----- ----- -----1911 0.70 0.15 0.57 0.08 0.34 -0.211931 ----- ----- ----- ----- ----- -----1948 0.22 0.43 0.61 -0.15 -0.26 0.001951 0.02 0.21 0.10 0.05 -0.13 0.962129 0.32 0.34 0.81 0.37 0.10 0.462146 -0.17 -0.67 -0.56 -0.02 1.04 -0.45



APPENDIX 3 Number of participants

1 laboratory in ARGENTINA

4 laboratories in AUSTRIA

4 laboratories in BELGIUM

1 laboratory in CYPRUS

2 laboratories in CZECH REPUBLIC

2 laboratories in ESTONIA

1 laboratory in FINLAND

2 laboratories in FRANCE

3 laboratories in GERMANY

4 laboratories in GREECE

4 laboratories in HUNGARY

1 laboratory in IRELAND

1 laboratory in ISRAEL

2 laboratories in LITHUANIA

1 laboratory in P.R. of CHINA

1 laboratory in PHILIPPINES

3 laboratories in POLAND

2 laboratories in PORTUGAL

2 laboratories in REPUBLIC OF MACEDONIA

2 laboratories in ROMANIA

1 laboratory in SINGAPORE

1 laboratory in SLOVENIA

1 laboratory in SOUTH KOREA

2 laboratories in SPAIN

1 laboratory in SWEDEN

1 laboratory in TAIWAN R.O.C.

1 laboratory in THAILAND

6 laboratories in THE NETHERLANDS

4 laboratories in TURKEY

2 laboratories in U.S.A.

8 laboratories in UNITED KINGDOM



APPENDIX 4 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 ex = excluded from calculations E = error in calculations n.a. = not applicable W = result withdrawn SDS = Safety Data Sheet Literature: 1 iis Interlaboratory Studies, Protocol for the Organisation, Statistics & Evaluation, November 2008 2 ASTM E178-02 3 ASTM E1301-03 4 ISO 5725-86 5 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 367/84 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 Analytical Methods Committee Technical Brief, No4 January 2001 13 The Royal Society of Chemistry 2002, Analyst 2002, 127 page1359-1364, P.J. Lowthian and M.

Thompson. (see http://www.rsc.org/suppdata/an/b2/b205600n/)

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