Results of Proficiency Test - Institute for ... · Results of Proficiency Test Jet Fuel A1 . September 2015 . ... (in %M/M and %V/V), ... JFTOT, Kinematic Viscosity at -20°C, Mercaptan

Results of Proficiency Test Jet Fuel A1 September 2015 Organised by: Institute for Interlaboratory Studies Spijkenisse, the Netherlands Author: ing. A.S. Noordman-de Neef Correctors: dr. R.G. Visser & ing. L. Sweere Report: iis15J02 November 2015

Institute for Interlaboratory Studies Spijkenisse, November 2015

page 2 of 75 Jet Fuel A1: iis15J02

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 .............................................................................................................. 7 2.6 ANALYSES .............................................................................................................................................. 7 3 RESULTS ................................................................................................................................................. 7 3.1 STATISTICS ............................................................................................................................................ 7 3.2 GRAPHICS .............................................................................................................................................. 8 3.3 Z-SCORES ............................................................................................................................................... 8 4 EVALUATION .......................................................................................................................................... 9 4.1 EVALUATION PER TEST ....................................................................................................................... 9 4.2 PERFORMANCE EVALUATION FOR THE GROUP OF LABORATORIES....................................... 15 4.3 COMPARISON OF THE PROFICIENCY TEST OF SEPTEMBER 2015 WITH PREVIOUS PTS ..... 16 Appendices: 1. Data, statistical results and graphic results ........................................................................................... 18 2. Number of participants per country ....................................................................................................... 74 3. Abbreviations and literature ................................................................................................................... 75

Spijkenisse, November 2015 Institute for Interlaboratory Studies

Jet Fuel A1: iis15J02 page 3 of 75

1 INTRODUCTION

Since 1995, the Institute for Interlaboratory Studies organises every year proficiency tests (PT) for Jet Fuel A1. The interlaboratory study on Jet Fuel was extended with PTs for the determination of Particle Size Distribution, FAME and BOCLE. In the annual proficiency testing program of 2015/2016, it was decided to continue the 4 PTs on Jet Fuel A1 in accordance with the latest applicable version of the "Aviation Fuel Quality Requirements for Jointly Operated Systems (AFQRJOS)”, sometimes referred to as the "Joint Fuelling System Check List for Jet A-1”. Overall 142 laboratories in 63 different countries have participated in PT for Jet Fuel A1. This means that; 137 laboratories in 63 different countries have participated in the main part (iis15J02), 45 laboratories in 20 different countries participated in the FAME determination (iis15J02FAME), 20 laboratories in 14 different countries in the BOCLE determination (iis15J02BOCLE) and 57 laboratories in 28 different countries participated in the PT for the Particle Size distribution (iis15J02PS). See appendix 2 for the number of participants per country. In this report, the results of the proficiency test are presented and discussed. This report is also electronically available through the iis internet site www.iisnl.com.

2 SET UP

The Institute for Interlaboratory Studies (iis) in Spijkenisse, the Netherlands, was the organiser of this proficiency test (PT). Sample analyses for fit-for-use and homogeneity testing were subcontracted to an accredited lab. For the main Jet Fuel PT, it was decided to send 2*1 liter bottles of sample labelled #15170 for the analyses according to the "Joint Fuelling System Check List for Jet A-1”. Depending on the registration also was sent; 1*0.1 liter bottle of sample labelled #15171 for the BOCLE PT, 1*0.5 liter bottle of sample labelled #15172 for the Particle Size Distribution PT and/or 1*0.1 liter bottle of sample labelled #15173 and 1*0.1 liter bottle of sample labelled #15174, both for the determination of FAME in Jet Fuel. The participants were requested to report the analytical results using the indicated units and 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/IEC 17043:2010 (R007), since January 2000, by the Dutch Accreditation Council (Raad voor Accreditatie). This PT iis15J02 falls under the accredited scope. It ensures strict adherence to protocols for sample preparation and statistical evaluation and 100% confidentially of participant’s data. Feedback from the participants on the reported data is encouraged and customer’s satisfaction is measured on regular basis by sending out questionnaires.

2.2 PROTOCOL



The protocol followed in the organisation of this proficiency test was the one as described for proficiency testing in the report ‘iis Interlaboratory Studies: ‘Protocol for the Organisation, Statistics and Evaluation of April 2014’ (iis-protocol, version 3.3). This protocol can be downloaded from the iis website http://www.iisnl.com, from the FAQ page.

2.3 CONFIDENTIALITY STATEMENT

All data presented 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 for 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

2.4.1 JET FUEL A1 (MAIN SAMPLE)

The necessary Jet fuel bulk material was obtained from a local supplier. Approximately 400 liter bulk material (JF-150311-UK-iis-1+2) was homogenised in a mixing vessel. From this batch 330 amber glass bottles of one liter were filled, closed with inner and outer caps and labelled #15170. The homogeneity of the subsamples #15170 was checked by the determination of Density in accordance with ASTM D4052 on 10 stratified randomly selected samples, see table 1.

Density at 15°C in kg/m3

Sample #15170-1 798.70 Sample #15170-2 798.70 Sample #15170-3 798.70 Sample #15170-4 798.71 Sample #15170-5 798.71 Sample #15170-6 798.70 Sample #15170-7 798.70 Sample #15170-8 798.71 Sample #15170-9 798.70 Sample #15170-10 798.71

Table 1: homogeneity test results of sub samples #15170

From the above test results, the repeatability was calculated and compared with 0.3 times the reproducibility of the reference method in agreement with the procedure of ISO13528, Annex B2 in the next table:


r (observed) 0.10 reference method D4052:11 0.3 x R (ref. method) 0.15

Table 2: evaluation of repeatability of subsamples #15170



The calculated repeatability is less than 0.3 times the reproducibility of the reference method. Therefore, homogeneity of the subsamples of #15170 was assumed.

2.4.2 JET FUEL A1 – SAMPLE FOR BOCLE (BALL-ON-CYLINDER LUBRICITY EVALUATOR) DETERMINATION

Approximately 1.8 liter hydrocracked Jet fuel bulk material (JF-130620-EXM-iis-1), obtained from a local supplier, was mixed with 1.6 liter of hydrocracked Jet fuel sample of previous PT (#14171) for the BOCLE determination. This mix of approximately 3.4 liter bulk material was homogenized. From this batch 34 amber glass bottles of 0.1 liter were filled, closed with inner and outer caps and labelled #15171. The homogeneity of the subsamples #15171 was checked by the determination of Density in accordance with ASTM D4052 on 8 stratified randomly selected samples, see table 3. Density at 15°C in kg/m3

Sample #15171-1 812.46 Sample #15171-2 812.47 Sample #15171-3 812.48 Sample #15171-4 812.49 Sample #15171-5 812.51 Sample #15171-6 812.51 Sample #15171-7 812.50 Sample #15171-8 812.51

Table 3: homogeneity test results of sub samples #15171

From the above test results, the repeatability was calculated and compared with 0.3 times the reproducibility of the reference method in agreement with the procedure of ISO13528, Annex B2 in the next table:


r (observed) 0.05 reference method D4052:11 0.3 x R (ref. method) 0.15

Table 4: evaluation of repeatability of subsamples #15171 The calculated repeatability is less than 0.3 times the reproducibility of the reference method. Therefore, homogeneity of the subsamples #15171 was assumed.

2.4.3 JET FUEL A1 – SAMPLE FOR PARTICLE SIZE (PS) DISTRIBUTION DETERMINATION The Jet fuel bulk material (JF-140110-iis-iis-MV-1) was obtained from an earlier PT for particle size determination. Approximately 120 liter bulk material was homogenized. From this batch 80 amber glass bottles of 0.5 liter were filled, closed with inner and outer caps and labelled #15172. The homogeneity of the subsamples #15172 was checked by the determination of Particle Size Distribution in accordance with IP564 on eight stratified randomly selected samples. For the particle size ≥4 µm the values ranged from 2345 to 3464 parts/ml. The variation between the test results for homogeneity of the subsamples #15172 were all within the repeatability (r (IP565:13)) and therefore the homogeneity of the subsamples #15172 was assumed.



2.4.4 JET FUEL A1 – SAMPLE FOR FATTY ACID METHYL ESTER (FAME) DETERMINATION It was decided to prepare two samples for FAME determination in Jet fuel with low and high level of FAME. Approximately 11.5 liter Jet fuel bulk material obtained from a local supplier was spiked with 0.065 gram Biodiesel B100 and homogenised. From this batch 58 amber glass bottles of 0.1 liter were filled, closed with inner and outer caps and labelled #15173. The amount left over of the batch used for #15173 (5.9 liter) was spiked with 0.211 gram Biodiesel B100 and homegenised. From this batch 58 amber glass bottles of 0.1 liter were filled, closed with inner and outer caps and labelled #15174. The homogeneity of the subsamples #15173 and #15174 were checked by the determination of FAME in accordance with method IP585 on 8 stratified randomly selected samples, see table 5.

FAME in mg/kg of #15173

FAME in mg/kg of #15174

Sample #15173/4-1 12 49 Sample #15173/4-2 13 47 Sample #15173/4-3 12 49 Sample #15173/4-4 13 47 Sample #15173/4-5 14 47 Sample #15173/4-6 14 48 Sample #15173/4-7 13 48 Sample #15173/4-8 14 46

Table 5: homogeneity test results of sub samples #15173 and #15174

From the above test results, the repeatability was calculated and compared with the corresponding repeatability of the reference method in agreement with the procedure of ISO 13528, Annex B2 in the next table: FAME in mg/kg

of #15173 FAME in mg/kg

of #15174 r (observed) 2.0 2.6 reference method IP585:10 IP585:10 r (ref. method) 2.7 8.2

Table 6: evaluation of repeatabilities of subsamples #15173 and #15174

The calculated repeatability is less than the repeatability of the reference method. Therefore, homogeneity of the subsamples of #15173 and #15174 was assumed. Depending on the registration of each individual participant the following samples were dispatched on August 26, 2015: 2 bottles Jet Fuel A1 (2*1 liter, labelled #15170), 1 bottle especially prepared for the BOCLE determination (1*0.1L, labelled #15171), 1 bottle especially prepared for the Particle Size Distribution determination (1*0.5L, labelled #15172) and 2 bottles especially prepared for the FAME determination (1*0.1 L, labelled #15173 + 1*0.1 L, labelled #15174).



2.5 STABILITY OF THE SAMPLES The stability of Jet Fuel A1, packed in the brown glass bottles was checked in the past. The type of bottle was chosen in accordance with ASTM D4306:13. The material has been found sufficiently stable for the period of the proficiency test.

2.6 ANALYSIS The participants were requested to determine on sample #15170: Acidity total, Aromatics by FIA, Aromatics by HPLC (in %M/M and %V/V), Colour Saybolt (ASTM D156 and ASTM 6045), Density at 15°C, Distillation (IBP, 10%, 50%, 90% recovered, FBP), Existent Gum, Flash Point, Freezing Point, JFTOT, Kinematic Viscosity at -20°C, Mercaptan Sulphur, MSEP, Naphthalenes, Smoke Point, Specific Energy,Total Sulphur. The participants were requested to determine BOCLE on sample #15171, Particle Size Distribution on sample #15172 and Fatty Acid Methyl Ester (FAME) on samples #15173 and #15174. The analyses should be performed according to the "Aviation Fuel Quality Requirements for Jointly Operated Systems (AFQRJOS)", also referred to as the "Joint Fuelling System Check List” or simply “Check List”. To get comparable results a detailed report form, on which the units were prescribed as well as the required standards and a letter of instructions were prepared and made available on the data entry portal www.kpmd.co.uk/sgs-iis/. A SDS and a form for sample receipt were added to the samples. After closure of the data entry portal a detailed report form was made available for download on the iis website www.iisnl.com for participants who were too late with reporting.

3 RESULTS

During four weeks after sample dispatch, the results of the individual laboratories were gathered via the data entry portal. 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 Organisation, Statistics and Evaluation of April 2014’ (iis-protocol, version 3.3). 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 a variant of the Kolmogorov-Smirnov test and by the calculation of skewness and kurtosis. Evaluation of the three normality indicators in combination with the visual evaluation of the graphic Kernel density plot, lead to judgement of the normality being either ‘unknown’, ‘OK’, ‘suspect’ or ‘not OK’. After removal of outliers, this check was repeated. Not all data sets proved to have a normal distribution, in which cases the statistical evaluation of the results should be used with due care. In accordance to ISO 5725 (1986 and 1994) the original results per determination were submitted subsequently to Dixon and Grubbs outlier tests for n<20 and to Rosner General ESD outlier test for n>19. Outliers are marked by D(0.01) or D(1) for the Dixon test, by G(0.01), G(1), DG(0.01) or DG(1) for the Grubbs test and by R(0.01) or R(1) for the Rosner test. Stragglers are marked by D(0.05) or D(5) for the Dixon test, by G(0.05), G(5), DG(0.05) or DG(5) for the Grubbs test and by R(0.05) or R(5) for the Rosner test. Both outliers and stragglers were not included in the calculations of the averages and the standard deviations.

For each assigned value, the uncertainty was determined in accordance with ISO13528. Subsequently the calculated uncertainty was evaluated against the respective requirement based on the target reproducibility in accordance with ISO13528. When the uncertainty passed the evaluation, no remarks are made in the report. However, when the uncertainty failed the evaluation it is mentioned in the report and it will have consequences for the evaluation of the test results. 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 analysis results are plotted. The corresponding laboratory numbers are under the X-axis. The straight horizontal line presents the consensus value (a trimmed mean). The four striped lines, parallel to the consensus value line, are the +3s, +2s, -2s and -3s target reproducibility limits of the selected standard. 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. Also a normal Gauss curve was projected over the Kernel Density Graph for reference.

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. ASTM reproducibilities, the z-scores were calculated using a target standard deviation. This results in an evaluation independent of the variation of this



interlaboratory study. The target standard deviation was calculated from the literature reproducibility by division with 2.8.

When a laboratory did use a test method with a reproducibility that is significantly different from the reproducibility of the reference test method used in this report, it is strongly advised to recalculate the z-score, while using the reproducibility of the actual test method used, this in order to evaluate whether the reported test result is fit-for-use. The z-scores were calculated in accordance with: 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 maybe as follows: |z| < 1 good 1 < |z| < 2 satisfactory 2 < |z| < 3 questionable 3 < |z| unsatisfactory

4 EVALUATION

In this proficiency test problems were encountered with the dispatch of the samples. Several laboratories in Egypt, Kenya, Mauritius, Mozambique, Nigeria, Saudi Arabia and Turkmenistan received the samples late or not at all. For the main Jet Fuel A1 PT, 11 participants reported the results after the final reporting date and another 8 participants did not report any result at all. For the BOCLE, Particle Size Distribution and FAME PTs, respectively 2, 4 and 4 participants reported the results after the final reporting date and respectively 3, 11 and 11 participants did not report any result at all. In total, 129 participants of the main PT, 17 participants of the BOCLE PT, 46 participants of the Particle Size Distribution PT and 33 participants of the FAME PT reported in total 2695 numerical results. Observed were 74 outlying results, which is 2.7% of the reported numerical results. In proficiency studies, outlier percentages of 3% - 7.5% are quite normal.

4.1 EVALUATION PER TEST

In this section, the results are discussed per sample and per test. The methods, which are used by the various laboratories, are taken into account for explaining the observed differences where possible and applicable. These methods are also summarized in the tables together with the reported data. The abbreviations, used in these tables, are listed in appendix 3. In the iis PT reports, ASTM methods are referred to with a number (e.g. D2086) and an added designation for the year that the method was adopted or revised (e.g. D2086:08). If applicable, a



designation in parentheses is added to designate the year of reapproval (e.g. D2086:08 (2013)). In the results tables of Appendix 1 only the method number and year of adoption or revision will be used. Not all original data sets proved to have a normal Gaussian distribution. These are referred to as “not OK” or “suspect”. The statistical evaluation of these data sets should be used with due care, see also paragraph 3.1. Since the checklist is continuously updated, the users are advised to monitor the updates. The latest version at the time of this PT for the AFQRJOS is “DEF STAN 91-91/Issue 7 Amendment 3, dated: February 2015” and ASTM D1655:15. One must keep in mind that ISO-methods are not mentioned in the “Checklist” (AFQRJOS issue 28, March 2015). For Jet Fuel sample #15170

Acidity total: This determination was problematic at the low level 0.0021 mg KOH/g. Three statistical outliers were observerd. The calculated reproducibility after

rejection of the statistical outliers is not in agreement with the requirements of ASTM D3242:11.

Aromatics by: This determination was not problematic. No statistical outliers were FIA (D1319): observed. The calculated reproducibility is in good agreement with ASTM

D1319:14. Aromatics by: The %M/M determination was not problematic. Two statistical outliers were HPLC (D6379) observed. The calculated reproducibility, after rejection of the statistical outliers,

is in agreement with ASTM D6379:11. The %V/V determination may also not be problematic. Three statistical outliers

were observed. Regretfully, no precision data for the determination in %V/V is mentioned in ASTM D6379:11. However, the observed reproducibility, after rejection of the statistical outliers, was similar to the determination in %M/M.

Colour Saybolt: The determination was problematic for the automatic test method ASTM D6045.

One statistical outlier was observed. The calculated reproducibility, after rejection of the statistical outlier, is not in agreement with the requirements of ASTM D6045:12. Some of the variation may be caused by the fact that the majority of the laboratories reported to have used a different cell than the suggested 100 mm cell in ASTM D6045. The calculated reproducibility over the reported results of nine participants who have indeed used a 100 mm cell is quite in line with the requirements of ASTM D6045:12. The manual test method ASTM D156 was very problematic. Only one statistical outlier was observed. However, the calculated reproducibility, after rejection of the statistical outlier, is not at all in agreement with the requirements of ASTM D156:15.



When de average result of the automatic test method ASTM D6045 is compared to the average result of the manual test method ASTM D156 a bias between both methods is observed. This is not obeserved in the two PTs of last year.

Density: This determination was not problematic. One statistical outlier was observed. The

calculated reproducibility, after rejection of the statistical outlier, is in good agreement with the requirements of ASTM D4052:11.

Distillation: This determination was not problematic. In total for the five distillation parameters

seven statistical outliers were observed. The calculated reproducibilities for IBP, 10% rec, 50% rec, 90% rec and FBP, after rejection of the statistical outliers, are all in agreement with the automated mode requirements of ASTM D86:12.

Existent Gum: This determination was not problematic. One statistical outlier was observed. The calculated reproducibility, after rejection of the statistical outlier, is in good agreement with ASTM D381:12.

Flash Point: This determination was not problematic. Three statistical outliers were observed. However, the calculated reproducibility, after rejection of the statistical outliers, is in good agreement with IP170:14.

In the Joint Fuelling System Checklist both IP170/ISO13736 and ASTM D56 or ASTM D3828 are mentioned as test methods. Still some participants (eleven in total) report methods which are not equivalent, like D93 and ISO2719.

Freezing Point: This determination was not problematic. Two statistical outliers were observed.

The calculated reproducibility, after rejection of the statistical outliers, is in agreement with the requirements of ASTM D2386:15e1.

JFTOT: The test results for tube rating are reported as <1 or 1. One participant reported

0. No statistical analysis can be done on this parameter as this is a qualitative parameter.

The reported Delta P test results vary from 0 to 5 of which the majority of the participants reported a value ≤1mmHg. Three statistical outliers were observed. Regretfully, no precision data for the Delta P is mentioned in ASTM D3241:15.

Kin. Viscosity at -20°C: This determination was not problematic. Three statistical outliers were

observed. However, the calculated reproducibility after rejection of the statistical outliers is in agreement with the requirements of ASTM D445:15.

Mercaptan Sulphur:This determination was not problematic. Two statistical outliers were observed. However, the calculated reproducibility, after rejection of the statistical outliers, is in agreement with the requirements of ASTM D3227:13.

MSEP: This determination was not problematic. One statistical outlier was observed. The

calculated reproducibility, after rejection of the statistical outlier, is in agreement with the requirements of ASTM D3948:14.



Naphthalenes: This determination was problematic for a number of laboratories. Eight statistical

outliers were observed. However, the calculated reproducibility, after rejection of the statistical outliers, is in agreement with the requirements of ASTM D1840:07(2013)-B, but not with ASTM D1840:07(2013)-A. When the results from the reported procedures A and B are evaluated separately, the calculated reproducibility, after rejection of the statistical outliers, are respectively not in agreement with the requirements of ASTM D1840:07(2013)-A and B. The overall calculated reproducibility is in agreement with D1840:07(2013)-B due to the smaller variation in reported values of method A participants.

Smoke Point: This determination was not problematic. One statistical outlier was observed.

The calculated reproducibility, after rejection of the statistical outlier, is in full agreement with the requirements of ASTM D1322:15e1-M.

Two participants reported to use method IP57, please note that method IP57 is not longer part of the Joint Fuelling System Checklist.

Specific Energy: This determination was problematic. No statistical outliers were observed.

However, the calculated reproducibility is not in agreement with the requirements of ASTM D3338:09e2 (2014).

Total Sulphur: This determination was problematic for a number of laboratories. Eight statistical

outliers were observed. However, the calculated reproducibility, after rejection of the statistical outliers, is in agreement with the requirements of ASTM D5453:12.

For Jet Fuel BOCLE sample #15171

BOCLE: This determination was problematic. No statistical outliers were observed. The calculated reproducibility is not in agreement with the requirements of the ASTM D5001:10 (2014) semi-automatic nor with the ASTM D5001:10 (2014) full-automatic determination.



For Jet Fuel PS sample #15172

Particle Size Distribution: The average results from test methods IP564 and IP565 differed significantly in earlier PTs. Therefore both methods are evaluated separately in this PT.

The determination according to IP564 was very problematic. In total eleven statistical outliers were observed for the six particle size categories. The test results of one laboratory (code 1299) were all excluded, because this participant reported to use method IP577. The test results of two laboratories (codes 1049 and 1316) were excluded because there were respectively 4 and 3 outliers in 6 related measurements of the particle size distribution. The calculated reproducibilities, after rejection of the outliers and the suspected data, are only in agreement with the requirements of IP564:13 for the less relevant ≥25µm and ≥30µm particle size categories. The test results varied over a large range, especially at lower particle size categories.

The determination according to IP565 was problematic for the determinations ≥4

and ≥6µm. In total eight statistical outliers were observed for the six particle size categories. The test results of two laboratories (codes 1064 and 1585) were excluded because there were 3 outliers in 6 related measurements of the particle size distribution. The calculated reproducibilities, after rejection of the outliers and the suspected data, are in agreement with the requirements of IP565:13, except for the more relevant ≥4µm and ≥6µm particle size categories.

For Jet Fuel FAME sample #15173

FAME: This determination was problematic. Three statistical outliers were observed. The test results of three laboratories (codes 369, 851 and 1065) were excluded, because these participants reported to use method IP583. The average level of FAME reported over all participants is below detection limit of method IP583 (limit of detection = 20 mg/kg).

The calculated reproducibility, after rejection of the suspect data, is not in agreement with the requirements of IP585:10. The average recovery of FAME (theoretical increment of 7.0 mg FAME/kg) is satisfactory: “less than 160%” (the actual blank FAME content is unknown).

For Jet Fuel FAME sample #15174

FAME: This determination was problematic. Only one statistical outlier was observed. However, the calculated reproducibility, after rejection of the statistical outlier, is not in agreement with the requirements of IP585:10. When the results IP583, IP585 and IP590 were evaluated separately, only the calculated reproducibility of the IP583 data is in agreement with the respective requirements. The average recovery of FAME (theoretical increment of 52.0 mg FAME/kg) is good: “less than 95%” (the actual blank FAME content is unknown).



When the values of the FAME determination of both samples (#15173 and #15174) are compared per lab it is shown that the systematical error is bigger than the random error, see Figure 1 below. When the three methods IP583, IP585 and IP590, all three mentioned in the Joint Fuelling System Checklist, are compared, it is clearly shown that the reported results of IP583 have a bias compared to IP585 or IP590, especially at lower FAME levels. Unfortunately, the calculated reproducibility of IP585, the method used by the majority of the participants, is not very much improved when the reproducibility is calculated only over the reported values of IP585.

Figure 1: Comparison FAME determination in mg/kg of samples #15173&#15174 per lab



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 laboratories that participated. The reproducibilities derived from literature standards (in casu ASTM standards) and the calculated reproducibilities of samples #15170, #15171, #15172, #15173 and #15174 are compared in the next tables.

Parameter unit n Average 2.8 * sd R (lit) Acidity total mg KOH/g 82 0.0021 0.0036 0.0018 Aromatics by FIA %V/V 71 17.7 2.1 3.0 Aromatics by HPLC %M/M 24 20.9 1.9 2.1 Aromatics by HPLC %V/V 25 18.8 1.6 n.a. Colour Saybolt (ASTM D6045) automated 50 21.5 1.9 1.2 Colour Saybolt (ASTM D156) manual 71 20.1 3.5 2.0 Density at 15°C kg/m3 125 798.6 0.3 0.5 Initial Boiling Point °C 126 149.5 6.3 8.2 10% recovered °C 124 169.4 2.6 3.7 50% recovered °C 124 197.1 2.3 3.0 90% recovered °C 125 241.0 3.9 3.6 Final Boiling Point °C 123 267.8 3.8 7.1 Existent Gum mg/100mL 72 0.75 1.08 3.15 Flash Point °C 120 41.9 2.8 3.2 Freezing Point °C 112 -54.1 2.2 2.5 JFTOT – Tube Rating 77 ≤ 1 n.a. n.a. JFTOT – Delta P mmHg 62 0.2 1.0 n.a. Kinematic Viscosity at -20°C cSt 83 3.851 0.066 0.073 Mercaptan Sulphur %M/M 75 0.0005 0.0002 0.0003 MSEP rating 90 89.9 11.9 11.8 Naphthalenes %V/V 64 0.56 0.06 0.07 Smoke Point mm 93 23.5 3.5 3.7 Specific Energy MJ/kg 66 43.279 0.059 0.046 Total Sulphur mg/kg 96 704.7 63.5 89.3

Table 7: comparison of the observed and target reproducibilities of sample #15170

Parameter Unit n Average 2.8 * sd R (lit) Wear Scar Diameter (BOCLE) mm 17 0.67 0.07 0.06

Table 8: comparison of the observed and target reproducibility of sample #15171



Parameter Unit n Average 2.8 * sd R (lit) Particle Size > 4 µm (IP564) parts/ml 18 4020 3556 898 Particle Size > 6 µm (IP564) parts/ml 19 918 801 350 Particle Size >14 µm (IP564) parts/ml 19 33 38 26 Particle Size >21 µm (IP564) parts/ml 18 8.0 10.8 10.1 Particle Size >25 µm (IP564) parts/ml 18 3.6 4.7 4.8 Particle Size >30 µm (IP564) parts/ml 18 1.3 1.8 2.2 Particle Size > 4 µm (IP565) parts/ml 21 7204 2721 917 Particle Size > 6 µm (IP565) parts/ml 22 1601 729 419 Particle Size >14 µm (IP565) parts/ml 21 48 32 40 Particle Size >21 µm (IP565) parts/ml 22 10.3 10.1 11.1 Particle Size >25 µm (IP565) parts/ml 22 4.6 6.2 6.0 Particle Size >30 µm (IP565) parts/ml 22 1.9 3.2 3.1

Table 9: comparison of the observed and target reproducibilities of sample #15172

Parameter Unit n Average 2.8 * sd R (lit) FAME Sample #15173 mg/kg 27 11.2 4.6 3.6 FAME Sample #15174 mg/kg 30 49 19 13

Table 10: comparison of the observed and target reproducibility of samples #15173 and sample #15174 Without further statistical calculations, it can be concluded that for many tests there is a good compliance of the group of participants with the relevant standards. The tests that are problematic have been discussed in paragraph 4.1.

4.3 COMPARISON OF THE PROFICIENCY TEST OF SEPTEMBER 2015 WITH PREVIOUS PTS

September 2015

March 2015

September 2014

March 2014

September 2013

March 2013

Number of reporting labs 129 102 132 100 136 92 Number of results reported 2695 1803 2729 1741 2538 1705 Statistical outliers 74 44 62 29 69 45 Percentage outliers 2.7% 2.4% 2.3% 1.6% 2.7% 2.6%

Table 11: 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:



Parameter

September 2015

March 2015

September 2014

March 2014

September 2013

March 2013

Acidity total -- - -- -- - - Aromatics by FIA ++ + ++ + + ++ Aromatics by HPLC + +/- - - ++ +/- Colour Saybolt -- -- -- -- -- -- Density at 15°C ++ ++ ++ ++ ++ ++ Distillation + + + + n.e. n.e. Existent Gum ++ ++ ++ ++ ++ +/- Flash Point + + + + + + Freezing Point + + + - + +/- Kinematic Viscosity @ -20°C +/- - +/- - + - Mercaptan Sulphur + +/- ++ + +/- -- MSEP +/- + + + +/- - Naphthalenes - +/- + + + + Smoke Point +/- + + +/- + ++ Specific Energy - - - - + - Total Sulphur ++ ++ + +/- + + BOCLE - n.e. + n.e. +/- n.e. Particle Size Distribution n.e. n.e. n.e. n.e. -- -- Particle Size Distribution IP564 -- -- - - n.e. n.e. Particle Size Distribution IP565 - - -- -- n.e. n.e. FAME - n.e. -- n.e. -- n.e.

Table 12: comparison determinations against the standard requirements The performance of the determinations against the requirements of the respective standards is listed in the above table. The following performance categories were used:

++: group performed much better than the standard

+ : group performed better than the standard +/-: group performance equals the standard - : group performed worse than the standard -- : group performed much worse than the standard

n.e.: not evaluated



APPENDIX 1 Determination of Acidity, Total on sample #15170; results in mg KOH/g

lab method value mark z(targ) lab method value mark z(targ) 52 D3242 0.001 -1.64 974 D3242 0.0041 3.04 62 D3242 0.0050 C 4.40 994 D3242 0.0020 -0.13 120 D3242 0.004 2.89 995 D3242 0.0022 0.17 131 ----- ----- 996 ----- ----- 132 D3242 0.0012 -1.34 997 D3242 0.0022 0.17 140 D3242 0.0028 1.08 998 ----- ----- 150 D3242 0.001 -1.64 1011 D3242 <0.002 ----- 159 D3242 0.0008 -1.94 1016 D3242 0.0012 -1.34 169 D3242 0.0008 -1.94 1026 D3242 0.001 -1.64 171 D3242 0.002 -0.13 1039 D3242 0.008 R(0.01) 8.93 175 D3242 0.001 -1.64 1049 D3242 0.00236 0.41 177 D3242 0.0019 -0.28 1059 D3242 0.0009 -1.79 194 ----- ----- 1062 D3242 0.003 1.38 216 ----- ----- 1064 D3242 0.0012 -1.34 221 ----- ----- 1065 D3242 0.0042 3.19 224 D974 0.00185 -0.36 1079 D3242 0.0050 C 4.40 225 D3242 0.002 -0.13 1081 D3242 0.002 -0.13 228 ----- ----- 1082 D3242 0.00115 -1.41 230 ----- ----- 1097 D3242 0.0037 2.43 237 ----- ----- 1109 D3242 0.00404 2.95 238 ----- ----- 1121 0.005 4.40 252 ----- ----- 1126 ----- ----- 253 ----- ----- 1134 ----- ----- 254 ----- ----- 1146 ----- ----- 256 ----- ----- 1150 ----- ----- 258 ----- ----- 1161 D664 0.00182 -0.40 273 D974 0.0020 -0.13 1182 ----- ----- 311 D3242 0.001 -1.64 1191 D3242 0.002 -0.13 317 ----- ----- 1203 ----- W ----- 323 D3242 0.005 4.40 1205 ----- ----- 333 D3242 0.001 -1.64 1279 D3242 0.001 -1.64 334 D3242 0.001 -1.64 1297 ----- ----- 335 D3242 0.001 -1.64 1299 D3242 0.008 R(0.01) 8.93 336 ----- ----- 1316 D3242 0.00733 R(0.01) 7.91 340 D3242 0.0031 1.53 1318 D3242 0.0045 3.64 353 ----- ----- 1347 D3242 0.0041 3.04 369 D3242 0.0010 -1.64 1348 D3242 0.0054 5.00 370 D3242 0.0018 -0.43 1372 ----- ----- 371 D3242 0.0015 -0.89 1395 ----- ----- 372 D3242 0.0013 -1.19 1397 D3242 0.001 -1.64 402 ----- ----- 1417 ----- ----- 440 D3242 0.003 C 1.38 1428 ----- ----- 445 IP354 0.001 -1.64 1429 ----- ----- 447 D3242 0.003 1.38 1496 D3242 0.0027 0.92 448 D3242 0.00318 C 1.65 1498 ----- ----- 453 IP354 0.001 -1.64 1528 D3242 0.0047 3.94 463 D3242 0.00203 -0.09 1543 ----- ----- 468 ----- ----- 1585 D3242 0.0023 0.32 473 ----- ----- 1587 ----- ----- 485 ----- ----- 1610 IP354 0.002 -0.13 496 D3242 0.0009 -1.79 1616 D3242 0.0027 0.92 601 ----- ----- 1634 ----- ----- 606 ----- ----- 1650 D3242 0.0008 -1.94 608 ----- ----- 1715 ----- ----- 631 D3242 0.0018 -0.43 1720 D3242 0.002 -0.13 634 ----- ----- 1724 D3242 0.0009 -1.79 657 D3242 0.0022 0.17 1776 D3242 0.00189 -0.30 663 ----- ----- 1784 D3242 0.0021 0.02 671 D3242 0.001 -1.64 1798 ----- ----- 732 ----- ----- 1811 D3242 0.00216 0.11 823 D3242 0.0016 -0.74 1813 D3242 0.0015 -0.89 824 ----- ----- 1833 D3242 0.0015 -0.89 851 D3242 0.0004 -2.55 1842 IP354 0.003 1.38 854 D3242 0.001 -1.64 1883 ----- ----- 862 D3242 0.0012 -1.34 1913 D3242 0.0010 -1.64 869 D3242 0.0006 -2.25 2129 D3242 0.00138 -1.07 922 ----- ----- 2130 IP354 0.0003 -2.70 962 ----- ----- 9090 D3242 0.0008 -1.94 963 D3242 0.0034 1.98



normality OK n 82 outliers 3 mean (n) 0.00209 st.dev. (n) 0.001285 R(calc.) 0.00360 R(D3242:11) 0.00185

Lab 62 first reported 0.0066 Lab 440 first reported 0.006 Lab 448 first reported 0.0096 Lab 1079 first reported 0.0142 Lab 1203 first reported 0.034



Determination of Aromatics by FIA on sample #15170; results in %V/V lab method value mark z(targ) lab method value mark z(targ) 52 D1319 18.0 0.30 974 D1319 16.8 -0.84 62 D1319 17.85 0.15 994 ----- ----- 120 D1319 17.8 0.11 995 ----- ----- 131

----- ----- 996 ----- -----

132 D1319 17.75 0.06 997 ----- ----- 140 D1319 17.0 C -0.65 998 ----- ----- 150 D1319 16.5 -1.13 1011 D1319 18.1 0.39 159 D1319 18.9 1.15 1016 ----- ----- 169 D1319 18.812 1.07 1026 ----- ----- 171 D1319 18.8 1.06 1039 ----- ----- 175 D1319 17.8 0.11 1049 ----- ----- 177 D1319 17.2 -0.46 1059 D1319 16.8 -0.84 194

----- ----- 1062 D1319 18.0 0.30

216

----- ----- 1064 D1319 17.94 0.24 221

----- ----- 1065 D1319 17.5 -0.18

224

----- ----- 1079 D1319 16.895 -0.75 225 D1319 17.4 -0.27 1081 ----- ----- 228

----- ----- 1082 ----- -----

230 D1319 17.69 0.00 1097 D1319 17.22 -0.44 237

----- ----- 1109 D1319 17.77 0.08

238

----- ----- 1121 ----- ----- 252 D1319 18.45 0.72 1126 ----- ----- 253 D1319 18.14 0.43 1134 ----- ----- 254 D1319 18.6 0.87 1146 ----- ----- 256 D1319 18.7 0.96 1150 ----- ----- 258

----- ----- 1161 ----- -----

273 D1319 16 -1.60 1182 ----- ----- 311 D1319 18.1 0.39 1191 ----- ----- 317

----- ----- 1203 EN15553 17.1 -0.56

323 D1319 16.1 -1.51 1205 ----- ----- 333

----- ----- 1279 ----- -----

334 D1319 17.6 -0.08 1297 ----- ----- 335 D1319 17.6 -0.08 1299 D1319 15.7 -1.89 336

----- ----- 1316 ----- -----

340 D1319 18.4 0.68 1318 ----- ----- 353

----- ----- 1347 D1319 18.96 1.21

369 D1319 17.70 0.01 1348 D1319 18.2 0.49 370 D1319 16.79 -0.85 1372 ----- ----- 371

----- ----- 1395 ----- -----

372 D1319 18.07 0.36 1397 D1319 17.9 0.20 402 D1319 17.42 -0.25 1417 ----- ----- 440 D1319 18.065 0.36 1428 D1319 17.5 -0.18 445 D1319 17.9 0.20 1429 ----- ----- 447 D1319 16.7 -0.94 1496 D1319 17.85 0.15 448 D1319 18.47 0.74 1498 ----- ----- 453 IP156 18.3 0.58 1528 EN15553 17.98 0.28 463 D1319 16.2 -1.41 1543 ----- ----- 468

----- ----- 1585 ----- -----

473

----- ----- 1587 ----- ----- 485

----- ----- 1610 IP156 18.6 0.87

496 D1319 18.00 0.30 1616 D1319 18.0 0.30 601

----- ----- 1634 ----- -----

606

----- ----- 1650 D1319 17.48 -0.20 608

----- ----- 1715 ----- -----

631 D1319 17.08 -0.58 1720 ----- ----- 634

----- ----- 1724 D1319 18.0 0.30

657 D1319 18.0 0.30 1776 ----- ----- 663

----- ----- 1784 D1319 16.5 -1.13

671

----- ----- 1798 ----- ----- 732

----- ----- 1811 D1319 16.61 -1.02

823 D1319 16.89 -0.76 1813 D1319 18.1507 0.44 824 D1319 18.2 0.49 1833 D1319 18.32 0.60 851

----- ----- 1842 ----- -----

854 D1319 18.6 0.87 1883 ----- ----- 862 D1319 18.20 0.49 1913 D1319 17.90 0.20 869 D1319 16.74 -0.90 2129 D1319 18.7 0.96 922 D1319 17.63 -0.05 2130 IP156 17.9 0.20 962

----- ----- 9090 ----- -----

963 D1319 17.30 -0.37




Lab 140 first reported 20.6



Determination of Aromatics by HPLC on sample #15170; results in %M/M lab method value mark z(targ) lab method value mark z(targ) 52

----- ----- 974 ----- -----

62

----- ----- 994 ----- ----- 120

----- ----- 995 ----- -----

131

----- ----- 996 ----- ----- 132

----- ----- 997 ----- -----

140

----- ----- 998 ----- ----- 150

----- ----- 1011 ----- -----

159

----- ----- 1016 ----- ----- 169

----- ----- 1026 ----- -----

171 D6379 27.6 C,R(0.01) 8.84 1039 ----- ----- 175

----- ----- 1049 D6379 20.602 -0.43

177

----- ----- 1059 EN12916 21.8 1.16 194

----- ----- 1062 ----- -----

216

----- ----- 1064 ----- ----- 221

----- ----- 1065 ----- -----

224

----- ----- 1079 ----- ----- 225

----- ----- 1081 ----- -----

228

----- ----- 1082 ----- ----- 230

----- ----- 1097 ----- -----

237

----- ----- 1109 D6591 21.52 0.79 238

----- ----- 1121 ----- -----

252

----- ----- 1126 ----- ----- 253

----- ----- 1134 ----- -----

254

----- ----- 1146 ----- ----- 256

----- ----- 1150 ----- -----

258

----- ----- 1161 ISO12916 20.8 -0.17 273

----- ----- 1182 ----- -----

311

----- ----- 1191 ----- ----- 317

----- ----- 1203 ----- -----

323

----- ----- 1205 ----- ----- 333

----- ----- 1279 ----- -----

334

----- ----- 1297 EN12916 21.00 0.10 335

----- ----- 1299 IP436 23.5 R(0.05) 3.41

336

----- ----- 1316 ----- ----- 340

----- ----- 1318 D6379 21.349 0.56

353

----- ----- 1347 ----- ----- 369 D6379 20.70 -0.30 1348 ----- ----- 370 D6379 19.83 -1.45 1372 ----- ----- 371

----- ----- 1395 ----- -----

372 D6379 21.09 0.22 1397 ----- ----- 402

----- ----- 1417 ----- -----

440

----- ----- 1428 ----- ----- 445

----- ----- 1429 ----- -----

447

----- ----- 1496 ----- ----- 448

----- ----- 1498 ----- -----

453

----- ----- 1528 D6379 21.3080 0.50 463 D6379 20.94 0.02 1543 ----- ----- 468

----- ----- 1585 IP436 20.42 -0.67

473

----- ----- 1587 ----- ----- 485

----- ----- 1610 ----- -----

496 D6379 21.44 0.68 1616 D6379 20.67 -0.34 601

----- ----- 1634 ----- -----

606

----- ----- 1650 ----- ----- 608

----- ----- 1715 ----- -----

631

----- ----- 1720 ----- ----- 634

----- ----- 1724 ----- -----

657 IP436 21.2 0.36 1776 ----- ----- 663

----- ----- 1784 ----- -----

671

----- ----- 1798 ----- ----- 732

----- ----- 1811 D6379 21.64 0.94

823 D6379 20.019 -1.20 1813 ----- ----- 824 D6379 21.4 0.63 1833 D6379 19.21 -2.28 851 D6379 20.53 C -0.53 1842 IP436 20.5 -0.57 854

----- ----- 1883 ----- -----

862 D6379 21.37 0.59 1913 ----- ----- 869

----- ----- 2129 D6379 22.32 1.85

922

----- ----- 2130 ----- ----- 962

----- ----- 9090 ----- -----

963 D6379 20.6 -0.43




Lab 171 first reported 17.5 Lab 851 first reported 18.94



Determination of Aromatics by HPLC on sample #15170; results in %V/V lab method value mark z(targ) lab method value mark z(targ) 52

----- ----- 974 ----- -----

62

----- ----- 994 ----- ----- 120

----- ----- 995 ----- -----

131

----- ----- 996 ----- ----- 132

----- ----- 997 ----- -----

140

----- ----- 998 ----- ----- 150

----- ----- 1011 ----- -----

159

----- ----- 1016 IP436 18.1 ----- 169

----- ----- 1026 IP436 20.2 -----

171 D6379 25.0 R(0.01) ----- 1039 D6379 19.0 ----- 175

----- ----- 1049 D6379 18.75528 -----

177

----- ----- 1059 ----- ----- 194

----- ----- 1062 ----- -----

216

----- ----- 1064 ----- ----- 221

----- ----- 1065 ----- -----

224

----- ----- 1079 ----- ----- 225

----- ----- 1081 D6379 17.8 -----

228

----- ----- 1082 ----- ----- 230

----- ----- 1097 ----- -----

237

----- ----- 1109 ----- ----- 238

----- ----- 1121 ----- -----

252

----- ----- 1126 ----- ----- 253

----- ----- 1134 ----- -----

254

----- ----- 1146 ----- ----- 256

----- ----- 1150 ----- -----

258

----- ----- 1161 EN12916 18.5 ----- 273

----- ----- 1182 ----- -----

311

----- ----- 1191 D6379 18.052 ----- 317

----- ----- 1203 ----- -----

323

----- ----- 1205 ----- ----- 333 D6379 18.7 ----- 1279 ----- ----- 334

----- ----- 1297 ----- -----

335

----- ----- 1299 IP436 20.9 R(0.05) ----- 336

----- ----- 1316 IP391 18.9 -----

340

----- ----- 1318 D6379 19.300 ----- 353

----- ----- 1347 ----- -----

369 D6379 18.70 ----- 1348 ----- ----- 370 D6379 18.03 ----- 1372 ----- ----- 371

----- ----- 1395 ----- -----

372 D6379 18.98 ----- 1397 D6379 19.9 ----- 402

----- ----- 1417 ----- -----

440

----- ----- 1428 ----- ----- 445

----- ----- 1429 ----- -----

447

----- ----- 1496 ----- ----- 448

----- ----- 1498 ----- -----

453 IP436 19.0 ----- 1528 D6379 19.1294 ----- 463 D6379 18.82 ----- 1543 ----- ----- 468

----- ----- 1585 IP436 18.45 -----

473

----- ----- 1587 ----- ----- 485

----- ----- 1610 ----- -----

496 D6379 19.39 ----- 1616 D6379 18.65 ----- 601

----- ----- 1634 ----- -----

606

----- ----- 1650 ----- ----- 608

----- ----- 1715 ----- -----

631

----- ----- 1720 ----- ----- 634

----- ----- 1724 D6379 18.71 -----

657 IP436 19.1 ----- 1776 D6379 17.068 R(0.05) ----- 663

----- ----- 1784 ----- -----

671

----- ----- 1798 ----- ----- 732

----- ----- 1811 ----- -----

823

----- ----- 1813 ----- ----- 824 D6379 19.0 ----- 1833 ----- ----- 851 D6379 18.57 C ----- 1842 ----- ----- 854

----- ----- 1883 ----- -----

862

----- ----- 1913 ----- ----- 869

----- ----- 2129 D6379 19.53 -----

922

----- ----- 2130 ----- ----- 962

----- ----- 9090 ----- -----

963

----- -----



normality OK n 25 outliers 3 mean (n) 18.85 st.dev. (n) 0.561 R(calc.) 1.57 Compare to R(calc) from iis14J02= 2.78 R(lit) unknown

Lab 851 first reported 17.13



Determination of Colour Saybolt (Automated) on sample #15170, cell size in mm; lab method Cell value mark z(targ) lab method Cell value mark z(targ) 52 D6045 ----- 20 -3.41 974 ----- ----- ----- 62

----- ----- ----- 994 ----- ----- -----

120 D6045 ----- 22 1.10 995 ----- ----- ----- 131

----- ----- ----- 996 ----- ----- -----

132

----- ----- ----- 997 ----- ----- ----- 140

----- ----- ----- 998 ----- ----- -----

150 D6045 ----- 21 -1.15 1011 ----- ----- ----- 159 D6045 100 22 1.10 1016 D6045 ----- 22 C 1.10 169 D6045 50 19.76 -3.95 1026 ----- ----- ----- 171 D6045 ----- 20 -3.41 1039 ----- ----- ----- 175

----- ----- ----- 1049 D6045 50 22 1.10

177

----- ----- ----- 1059 ----- ----- ----- 194

----- ----- ----- 1062 ----- ----- -----

216

----- ----- ----- 1064 D6045 50 22 1.10 221

----- ----- ----- 1065 ----- ----- -----

224

----- ----- ----- 1079 D6045 100 22 1.10 225 D6045 50 21 C -1.15 1081 D6045 ----- 22 1.10 228

----- ----- ----- 1082 D6045 ----- 22 1.10

230

----- ----- ----- 1097 ----- ----- ----- 237

----- ----- ----- 1109 D6045 100 22 1.10

238

----- ----- ----- 1121 ----- ----- ----- 252

----- ----- ----- 1126 ----- ----- -----

253

----- ----- ----- 1134 ----- ----- ----- 254

----- ----- ----- 1146 ----- ----- -----

256

----- ----- ----- 1150 ----- ----- ----- 258

----- ----- ----- 1161 D6045 ----- 22 1.10

273

----- ----- ----- 1182 D6045 ----- 21 -1.15 311 D6045 ----- 21.5 -0.03 1191 D6045 ----- 21 -1.15 317

----- ----- ----- 1203 ----- ----- -----

323

----- 22 1.10 1205 ----- ----- ----- 333 D6045 ----- 22 1.10 1279 D6045 ----- 21 -1.15 334

----- ----- ----- 1297 ----- ----- -----

335 D6045 50 21 -1.15 1299 D6045 ----- 18 R(0.01) -7.93 336

----- ----- ----- 1316 ----- ----- -----

340

----- ----- ----- 1318 D6045 100 22 1.10 353 D6045 50 22 1.10 1347 ----- ----- ----- 369 D6045 50 21 -1.15 1348 ----- ----- ----- 370

----- ----- ----- 1372 ----- ----- -----

371 D6045 ----- 22 1.10 1395 ----- ----- ----- 372 D6045 50 22 1.10 1397 ----- ----- ----- 402 D6045 ----- 22.0 1.10 1417 D6045 33 21 -1.15 440

----- ----- ----- 1428 D6045 ----- 21 -1.15

445 D6045 50 21 -1.15 1429 D6045 50 22 1.10 447 D6045 100 21 -1.15 1496 ----- ----- ----- 448

----- ----- ----- 1498 ----- ----- -----

453 D6045 50 22 1.10 1528 D6045 50 21 -1.15 463

----- ----- ----- 1543 ----- ----- -----

468

----- ----- ----- 1585 ----- ----- ----- 473

----- ----- ----- 1587 D6045 50 23.0 3.36

485

----- ----- ----- 1610 ----- ----- ----- 496

----- ----- ----- 1616 D6045 50 22 1.10

601

----- ----- ----- 1634 ----- ----- ----- 606

----- ----- ----- 1650 ----- ----- -----

608

----- ----- ----- 1715 D6045 100 21.3 -0.48 631 D6045 50 22 1.10 1720 ----- ----- ----- 634

----- ----- ----- 1724 ----- ----- -----

657

----- ----- ----- 1776 ----- ----- ----- 663

----- ----- ----- 1784 D6045 ----- 21 -1.15

671

----- ----- ----- 1798 ----- ----- ----- 732

----- ----- ----- 1811 D6045 ----- 22.0 1.10

823 D6045 100 22 1.10 1813 D6045 100 21 -1.15 824 D6045 50 22 1.10 1833 ----- ----- ----- 851

----- ----- ----- 1842 ----- ----- -----

854

----- ----- ----- 1883 ----- ----- ----- 862 D6045 50 20 C -3.41 1913 D6045 50 21 -1.15 869 D6045 50 21 -1.15 2129 D6045 50 22 1.10 922

----- ----- ----- 2130 D6045 50 22 1.10

962

----- ----- ----- 9090 D6045 100 22 1.10 963

----- ----- -----



Cell 100 mm only

normality OK OK n 50 9 outliers 1 0 mean (n) 21.51 21.70 st.dev. (n) 0.682 0.458 R(calc.) 1.91 1.28 R(D6045:12) 1.24 1.24

Lab 225 first reported 19 Lab 862 first reported 19 Lab 1016 first reported 16

17

18

19

20

21

22

23

24

1299 169 52 171

862

335

150

225

447

445

369

869

1182

1191

1279

1417

1428

1528

1784

1813

1913

1715 311

120

323

371

402

159

372

453

631

823

824

333

353

1016

1049

1064

1079

1081

1082

1109

1161

1318

1429

1616

1811

2129

2130

9090

1587



Determination of Colour Saybolt (Manual) on sample #15170; lab method value mark z(targ) lab method value mark z(targ) 52

----- ----- 974 D156 20 -0.08

62 D156 21 1.32 994 D156 20 -0.08 120

----- ----- 995 D156 20 -0.08

131

----- ----- 996 D156 20 -0.08 132 D156 20 -0.08 997 D156 18 -2.88 140 D156 21 1.32 998 D156 21 1.32 150

----- ----- 1011 D156 19 -1.48

159

----- ----- 1016 ----- ----- 169

----- ----- 1026 D156 22 2.72

171 D156 20 -0.08 1039 D156 21 1.32 175

----- ----- 1049 ----- -----

177 D156 19 -1.48 1059 D156 19 -1.48 194 D156 22 2.72 1062 D156 20 -0.08 216

----- ----- 1064 D156 21 1.32

221

----- ----- 1065 ----- ----- 224

----- ----- 1079 ----- -----

225

----- ----- 1081 ----- ----- 228

----- ----- 1082 ----- -----

230 D156 20 -0.08 1097 INH-003 20 -0.08 237

----- ----- 1109 D156 21 1.32

238

----- ----- 1121 D156 18 -2.88 252 D156 20 -0.08 1126 ----- ----- 253 D156 20 -0.08 1134 ----- ----- 254 D156 18 -2.88 1146 ----- ----- 256 D156 19 -1.48 1150 ----- ----- 258 D156 19 -1.48 1161 ----- ----- 273 D156 19 -1.48 1182 ----- ----- 311

----- ----- 1191 ----- -----

317 D156 19 -1.48 1203 D156 21 1.32 323 D156 20 -0.08 1205 ----- ----- 333

----- ----- 1279 D156 21 1.32

334 D156 20 -0.08 1297 ----- ----- 335

----- ----- 1299 ----- -----

336 D156 20 -0.08 1316 ----- ----- 340 D156 21 1.32 1318 ----- ----- 353

----- ----- 1347 D156 21 C 1.32

369 D156 21 1.32 1348 D156 21 1.32 370 D156 21 1.32 1372 ----- ----- 371

----- ----- 1395 ----- -----

372 D156 22 2.72 1397 ----- ----- 402 D156 21.0 1.32 1417 ----- ----- 440 D156 19 -1.48 1428 ----- ----- 445 D156 18 -2.88 1429 ----- ----- 447 D156 21 1.32 1496 D156 19 -1.48 448 D156 20 -0.08 1498 ----- ----- 453

----- ----- 1528 D156 21 1.32

463

----- ----- 1543 D156 21 1.32 468 D156 19.0 -1.48 1585 D156 18 -2.88 473 D156 22 2.72 1587 ----- ----- 485

----- ----- 1610 D156 17 -4.28

496

----- ----- 1616 ----- ----- 601

----- ----- 1634 D156 18 -2.88

606

----- ----- 1650 D156 20 -0.08 608 D156 22 2.72 1715 ----- ----- 631

----- ----- 1720 ----- -----

634 D156 19 -1.48 1724 ----- ----- 657 D156 22 2.72 1776 D156 19 -1.48 663 D156 17 -4.28 1784 ----- ----- 671 D156 21 1.32 1798 ----- ----- 732

----- ----- 1811 ----- -----

823 D156 22 2.72 1813 ----- ----- 824

----- ----- 1833 D156 21 1.32

851 D156 20 -0.08 1842 D156 21 1.32 854 D156 20 -0.08 1883 D156 18 -2.88 862 D156 19 -1.48 1913 D156 20 -0.08 869 D156 21 1.32 2129 D156 20 -0.08 922 D156 26 R(0.01) 8.32 2130 ----- ----- 962

----- ----- 9090 ----- -----

963 D156 22 2.72




Lab 1347 first reported 26



Determination of Density at 15°C on sample #15170; results in kg/m3 lab method value mark z(targ) lab method value mark z(targ) 52 D4052 798.7 0.31 974 D4052 798.6 -0.25 62 D4052 798.65 0.03 994 D4052 798.5 -0.81 120 D4052 798.6 -0.25 995 D4052 798.5 -0.81 131 D4052 798.8 0.87 996 D1298 798.5 -0.81 132 D4052 798.67 0.15 997 D4052 798.61 -0.19 140 D4052 798.6 -0.25 998 D4052 798.6 -0.25 150 D4052 798.8 0.87 1011 D4052 798.7 0.31 159 D4052 798.8 0.87 1016 ----- ----- 169 D4052 798.8 0.87 1026 D4052 798.6 -0.25 171 D4052 798.4 -1.37 1039 D4052 798.7 0.31 175 D4052 798.6 -0.25 1049 D4052 798.54 -0.58 177 D4052 798.7 0.31 1059 D4052 798.7 0.31 194 D4052 798.6 -0.25 1062 D4052 798.7 0.31 216 D1298 798.6 -0.25 1064 D4052 798.55 -0.53 221 D4052 798.7 0.31 1065 D4052 798.55 -0.53 224 D1298 798.60 -0.25 1079 D4052 798.64 -0.02 225 D4052 798.7 0.31 1081 D4052 798.65 C 0.03 228

----- ----- 1082 D4052 798.7 0.31

230 D4052 798.7 0.31 1097 ISO12185 798.65 0.03 237

----- ----- 1109 D4052 798.7 0.31

238

----- ----- 1121 IP365 798.7 0.31 252 D1298 798.6 -0.25 1126 D4052 798.65 0.03 253 D4052 798.5 -0.81 1134 ----- ----- 254 D4052 798.6 -0.25 1146 D4052 798.59 -0.30 256 D4052 798.6 -0.25 1150 ISO12185 798.5 -0.81 258 D1298 798.6 -0.25 1161 ISO12185 798.6 -0.25 273 D4052 798.6 -0.25 1182 ISO12185 798.661 0.10 311 D4052 798.7 0.31 1191 D4052 798.6 -0.25 317 D4052 798.8 0.87 1203 ISO12185 798.99 1.94 323 D4052 798.6 -0.25 1205 ISO12185 798.65 0.03 333 D4052 798.6 -0.25 1279 D4052 798.6 -0.25 334 D4052 798.7 0.31 1297 D4052 798.87 1.27 335 D4052 798.4 -1.37 1299 D4052 798.6 -0.25 336 D4052 798.4 -1.37 1316 D4052 798.6 -0.25 340 D4052 798.82 0.99 1318 D4052 798.64 -0.02 353 IP365 798.7 0.31 1347 D4052 798.70 0.31 369 D4052 798.6 -0.25 1348 D4052 798.9 1.43 370 D4052 798.7 0.31 1372 ----- ----- 371 D4052 798.6 -0.25 1395 ----- ----- 372 D4052 798.7 0.31 1397 ----- ----- 402 D4052 798.65 0.03 1417 IP365 798.6 -0.25 440 D4052 798.9 1.43 1428 D4052 798.6 -0.25 445 D4052 798.8 0.87 1429 D4052 798.7 0.31 447 D4052 798.6 -0.25 1496 D1298 798.8 0.87 448 D4052 798.6 C -0.25 1498 D1298 798.6 C -0.25 453 IP365 798.6 -0.25 1528 D1298 798.5 -0.81 463 D4052 798.69 0.26 1543 D4052 798.7 0.31 468 D4052 798.7 0.31 1585 D4052 799.1 R(0.01) 2.55 473 D4052 798.5 -0.81 1587 D4052 798.71 0.37 485 D4052 798.6 -0.25 1610 IP365 798.6 -0.25 496 D4052 798.65 0.03 1616 D4052 798.6 -0.25 601 D1298 798.7 0.31 1634 D4052 798.638 -0.03 606 D1298 798.6 -0.25 1650 D4052 798.67 0.15 608 D4052 798.7 0.31 1715 ISO12185 798.6 -0.25 631 D4052 798.86 1.21 1720 D4052 798.4 -1.37 634 D4052 798.7 0.31 1724 D4052 798.69 0.26 657 D4052 798.8 0.87 1776 D4052 798.65 0.03 663 D4052 798.70 0.31 1784 D4052 798.4 -1.37 671 D4052 798.8 0.87 1798 ----- ----- 732 D4052 798.5 -0.81 1811 D4052 798.63 -0.08 823 D4052 798.64 -0.02 1813 D4052 798.7 0.31 824 D4052 798.7 0.31 1833 D4052 798.7 0.31 851 D4052 798.6 -0.25 1842 ----- ----- 854 D4052 798.6 -0.25 1883 D1298 798.35 C -1.65 862 D4052 798.62 -0.13 1913 D4052 798.6 -0.25 869 D4052 798.60 -0.25 2129 D4052 798.6 -0.25 922 D4052 798.59 -0.30 2130 D4052 798.6 -0.25 962

----- ----- 9090 D4052 798.62 -0.13

963 D4052 798.8 0.87



normality suspect n 125 outliers 1 mean (n) 798.644 st.dev. (n) 0.1057 R(calc.) 0.296 R(D4052:11) 0.500

Lab 448 first reported 0.7986 kg/m3 Lab 1081 first reported 789.65 Lab 1498 first reported 797.6 Lab 1883 first reported 797.5



Determination of Distillation ASTM D86 on sample #15170; results in °C lab method mode IBP mark 10% mark 50% mark 90% mark FBP mark 52 D86 Automated 146.9 168.7 197.3 242.1 268.9 62 D86 Automated 149.0 170.0 197.6 240.5 268.9 120 D86 Automated 150.9 169.4 196.8 240.1 267.0 131 D86 Automated 148.6 169.1 196.9 242.0 265.7 132 D86 Automated 149.2 169.8 197.6 241.3 268.1 140 D86 Automated 146.3 169.7 196.9 241.2 268.1 150 D86 Automated 145.9 170.0 197.1 239.9 267.2 159 D86 Automated 151.3 171.0 198.1 241.0 267.7 169 D86 Automated 148.9 169.5 197.6 240.9 268.0 171 D86 Automated 148.4 169.7 197.2 241.5 267.5 175 D86 Automated 147.8 168.9 197.5 242.9 267.9 177 D86 Automated 148.1 168.4 196.0 238.8 266.0 194 D86 Automated 146.9 169.6 196.8 239.8 267.4 216 D86 Automated 144.5 170.0 196.9 240.3 247.4 R(0.01) 221 D86 Manual 146.0 169.0 197.0 240.0 267.0 224 D86 Manual 152.02 170.52 197.53 240.53 266.60 225 D86 Manual 148.0 168.0 195.0 240.0 C 265.5 228 ----- ----- ----- ----- ----- ----- 230 D86 Automated 146.6 167.5 195.0 240.0 265.7 237 ----- ----- ----- ----- ----- ----- 238 ----- ----- ----- ----- ----- ----- 252 D86 Manual 150.0 170.0 197.0 240.0 267.0 253 D86 Manual 148.0 169.0 196.5 240.0 266.5 254 D86 Manual 152.0 170.0 198.0 242.0 267.0 256 D86 Manual 151.0 170.0 197.0 241.0 267.0 258 D86 Automated 153.5 170.6 198.6 244.8 267.5 273 D86 Automated 148.1 167.4 196.4 241.8 267.7 311 D86 Automated 149.9 169.5 196.7 240.8 268.7 317 D86 Automated 151.6 170.0 197.7 241.2 267.4 323 D86 Automated 148.5 169.5 197.7 240.6 266.2 333 D86 Automated 148.5 169.2 196.7 239.1 268.1 334 D86 Automated 152.7 168.8 196.8 241.0 268.0 335 D86 Automated 152.4 170.1 197.3 241.5 268.5 336 D86 Automated 151.7 169.5 197.5 240.7 266.5 340 D86 Automated 148.9 168.1 197.4 244.3 265.1 353 D86 Automated 152.0 169.1 198.0 243.9 269.2 369 D86 Automated 151.3 168.2 197.0 242.3 268.7 370 D86 Automated 150.7 170.0 197.6 241.3 268.8 371 D86 Automated 151.5 168.9 197.5 240.8 269.2 372 D86 Automated 149.0 169.6 197.2 241.3 268.6 402 ----- ----- ----- ----- ----- ----- 440 IP123 Automated 151.5 169.1 196.9 240.2 269.3 445 IP123 Automated 145.3 168.6 197.0 240.7 268.0 447 D86 Automated 147.0 169.8 197.7 243.3 269.7 448 D86 Automated 149.7 169.7 197.6 241.9 270.0 453 IP123 Automated 151.2 170.2 197.6 242.1 270.1 463 D86 ----- 153.7 170.8 197.9 241.9 269.3 468 D86 Automated 147.6 170.0 197.0 241.1 266.9 473 D86 ----- 152.2 169.6 197.7 242.5 269.4 485 D86 Automated 148.25 169.8 197.05 240.0 267.3 496 D86 Automated 149.3 169.3 196.8 240.4 269.8 601 ----- ----- ----- ----- ----- ----- 606 D86 Automated 149.7 170.5 198.1 241.4 268.9 608 D86 Automated 148.0 169.5 197.2 240.5 266.3 631 D86 Automated 151.2 168.5 196.7 241.2 266.5 634 D86 Manual 150.41 169.41 197.41 244.52 273.52 R(0.01) 657 D86 Automated 150.9 169.2 197.6 241.8 268.1 663 D86 Automated 148.30 170.70 197.70 242.35 269.25 671 D86 Automated 151.7 170.6 198.4 243.5 265.0 732 D86 Manual 150.5 169.0 196.0 239.5 268.0 823 D86 Automated 152.5 170.8 198.5 240.9 269.2 824 D86 Automated 150.6 169.9 197.7 241.7 269.6 851 D86 Automated 151.0 170.0 196.7 241.8 266.6 854 D86 Automated 150.6 170.0 197.7 241.3 268.3 862 D86 Automated 146.7 168.7 196.4 239.8 267.8 869 D86 Manual 150.5 168.5 197.5 241.5 268.5 922 D86 Manual 147.0 168.0 194.0 R(0.05) 239.0 266.0 962 ----- ----- ----- ----- ----- ----- 963 D86 Automated 143.9 170.2 196.4 239.2 265.7 974 D86 Automated 150.2 168.8 196.3 241.5 266.6 994 D86 Manual 149.0 168.5 195.0 239.5 267.0 995 D86 Manual 149.5 168.0 196.0 239.5 267.5 996 D86 Manual 148.5 168.0 196.0 239.5 267.5 997 D86 ----- 148.5 167.5 195.5 238 267



lab method mode IBP mark 10% mark 50% mark 90% mark FBP mark 998 D86 Manual 148.0 168.0 195.5 238.5 268.5 1011 D86 Automated 147.8 169.0 196.8 238.8 268.2 1016 ----- ----- ----- ----- ----- ----- 1026 ISO3405 Automated 150.4 169.7 197.3 239.7 269.4 1039 ISO3405 Automated 145.8 167.2 196.4 239.1 268.6 1049 D86 Automated 149.1 170.1 197.5 240.5 268.1 1059 D86 Automated 149.2 169.9 196.8 240.5 268.9 1062 D86 Automated 151.6 170.3 198.1 241.4 268.6 1064 D86 Automated 148.2 170.2 198.2 243.2 270.0 1065 D86 Automated 152.3 168.6 196.6 240.6 266.6 1079 D86 Automated 150.5 169.4 198.5 242.0 268.5 1081 D86 Automated 149.3 170.5 197.4 240.4 268.8 1082 D86 Automated 149.3 169.7 197.0 241.8 269.3 1097 ISO3405 Automated 151.0 171.1 198.1 242.6 268.9 1109 D86 Automated 152.0 170.7 198.1 242.4 268.5 1121 IP123 Manual 146.1 165.1 R(0.01) 196.6 240.1 263.1 1126 in house Automated 152.2 171.2 196.1 241.4 268.0 1134 ----- ----- ----- ----- ----- ----- 1146 D86 ----- 150.7 169.1 196.9 240.5 267.5 1150 ISO3405 Automated 152.1 169.6 197.1 241.9 267.2 1161 ISO3405 ----- 148.8 168.4 196.8 239.6 269.7 1182 D86 Automated 151.5 169.5 197.7 242.2 269.3 1191 D86 Automated 146.7 170.4 197.5 241.9 269.0 1203 ISO3405 Automated 153.1 ----- 198.2 243.6 268.7 1205 D86 Automated 152.6 170.4 198.0 240.8 268.6 1279 D86 Automated 150.4 170.6 197.4 239.9 262.0 R(0.01) 1297 D86 Automated 147.1 168.9 197.1 240.3 266.1 1299 D86 Automated 148.7 169.8 197.9 242.8 268.5 1316 D86 Automated 148.3 169.3 197.7 242.2 267.7 1318 D86 Automated 145.4 169.5 196.3 239.9 266.2 1347 D86 Manual 150 169 198 241 269 1348 D86 Automated 150.1 167.1 C 198.3 240.8 265.3 1372 ----- ----- ----- ----- ----- ----- 1395 ----- ----- ----- ----- ----- ----- 1397 D86 ----- 152.2 170.5 196.9 239.2 267.7 1417 IP123 Automated 149.9 170.6 199.4 245.2 268.1 1428 D86 Automated 149.4 168.8 196.8 239.7 267.4 1429 D86 Automated 148.1 168.8 196.1 239.4 267.3 1496 D86 Automated 148.4 170.4 197.3 241.5 268.3 1498 D86 ----- 149.0 170.3 197.7 241.5 268.4 1528 D86 Automated 152.1 170.2 197.7 242.2 268.5 1543 D86 Manual 150 170 194 R(0.05) 235 R(0.01) 269 1585 D86 Automated 152.2 170.5 197.2 239.6 268.2 1587 D86 Automated 147.4 169.7 197.4 240.2 266.4 1610 D86 Automated 151.7 170.4 196.3 241.3 267.3 1616 D86 Manual 147.0 169.0 196.0 239.0 265.0 1634 D86 Automated 143.7 170.3 197.9 242.0 269.1 1650 D86 Automated 148.9 167.6 196.0 242.0 270.1 1715 D86 Automated 153.3 169.7 196.9 240.6 267.4 1720 D86 Automated 149.2 170.2 197.3 240.2 271.4 1724 D86 Automated 150.0 169.9 198.0 241.2 268.5 1776 D86 Automated 144.4 168.0 196.6 241.3 266.3 1784 D86 Automated 152.6 170.0 197.9 244.6 267.1 1798 ----- ----- ----- ----- ----- ----- 1811 D86 Automated 149.4 167.5 195.1 238.9 266.3 1813 D86 Automated 146.24 169.74 196.81 239.93 267.58 1833 D86 Automated 148.8 168.8 196.7 239.3 267.4 1842 D86 Automated 148.3 169.3 198.1 243.2 269.6 1883 D86 Manual 155 168 195 241 265 1913 D86 Automated 151.9 170.3 197.9 239.8 265.3 2129 D86 Automated 145.8 168.7 196.3 239.3 266.8 2130 D86 Automated 151.1 170.6 197.2 240.7 266.9 9090 D86 Automated 149.1 169.3 197.5 242.6 267.8

normality Autom./Man./ Unknown OK OK OK OK OK

n 99/ 20/ 7 126 124 124 125 123 outliers 0 1 2 1 3 mean (n) 149.48 169.45 197.14 241.03 267.78 st.dev. (n) 2.261 0.918 0.813 1.401 1.362 R(calc.) 6.33 2.57 2.28 3.92 3.81 R(D86:12) 8.22 3.73 2.97 3.62 7.10



Lab 225 first reported 236.0 for 90% recovery Lab 1348 first reported 161.7 for 10% recovery Initial Boiling Point/°C Temp. at 10% recovery/°C Temp. at 50% recovery/°C Temp. at 90% recovery/°C Final Boiling Point/°C



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z-scores Distillation ASTM D86 on sample #15170 lab method mode IBP 10% 50% 90% FBP 52 D86 Automated -0.88 -0.56 0.15 0.83 0.44 62 D86 Automated -0.16 0.41 0.43 -0.41 0.44 120 D86 Automated 0.48 -0.04 -0.32 -0.72 -0.31 131 D86 Automated -0.30 -0.26 -0.23 0.75 -0.82 132 D86 Automated -0.10 0.26 0.43 0.21 0.13 140 D86 Automated -1.08 0.19 -0.23 0.13 0.13 150 D86 Automated -1.22 0.41 -0.04 -0.88 -0.23 159 D86 Automated 0.62 1.16 0.90 -0.03 -0.03 169 D86 Automated -0.20 0.04 0.43 -0.10 0.09 171 D86 Automated -0.37 0.19 0.06 0.36 -0.11 175 D86 Automated -0.57 -0.41 0.34 1.45 0.05 177 D86 Automated -0.47 -0.79 -1.07 -1.73 -0.70 194 D86 Automated -0.88 0.11 -0.32 -0.95 -0.15 216 D86 Automated -1.70 0.41 -0.23 -0.57 -8.04 221 D86 Manual -1.19 -0.34 -0.13 -0.80 -0.31 224 D86 Manual 0.86 0.80 0.37 -0.39 -0.47 225 D86 Manual -0.51 -1.09 -2.02 -0.80 -0.90 228 ----- ----- ----- ----- ----- ----- 230 D86 Automated -0.98 -1.47 -2.02 -0.80 -0.82 237 ----- ----- ----- ----- ----- ----- 238 ----- ----- ----- ----- ----- ----- 252 D86 Manual 0.18 0.41 -0.13 -0.80 -0.31 253 D86 Manual -0.51 -0.34 -0.60 -0.80 -0.51 254 D86 Manual 0.86 0.41 0.81 0.75 -0.31 256 D86 Manual 0.52 0.41 -0.13 -0.03 -0.31 258 D86 Automated 1.37 0.86 1.38 2.92 -0.11 273 D86 Automated -0.47 -1.54 -0.70 0.59 -0.03 311 D86 Automated 0.14 0.04 -0.42 -0.18 0.36 317 D86 Automated 0.72 0.41 0.53 0.13 -0.15 323 D86 Automated -0.34 0.04 0.53 -0.34 -0.62 333 D86 Automated -0.34 -0.19 -0.42 -1.50 0.13 334 D86 Automated 1.10 -0.49 -0.32 -0.03 0.09 335 D86 Automated 0.99 0.49 0.15 0.36 0.28 336 D86 Automated 0.75 0.04 0.34 -0.26 -0.51 340 D86 Automated -0.20 -1.01 0.24 2.53 -1.06 353 D86 Automated 0.86 -0.26 0.81 2.22 0.56 369 D86 Automated 0.62 -0.94 -0.13 0.98 0.36 370 D86 Automated 0.41 0.41 0.43 0.21 0.40 371 D86 Automated 0.69 -0.41 0.34 -0.18 0.56 372 D86 Automated -0.16 0.11 0.06 0.21 0.32 402 ----- ----- ----- ----- ----- ----- 440 IP123 Automated 0.69 -0.26 -0.23 -0.65 0.60 445 IP123 Automated -1.43 -0.64 -0.13 -0.26 0.09 447 D86 Automated -0.85 0.26 0.53 1.76 0.76 448 D86 Automated 0.07 0.19 0.43 0.67 0.88 453 IP123 Automated 0.58 0.56 0.43 0.83 0.91 463 D86 ----- 1.44 1.01 0.72 0.67 0.60 468 D86 Automated -0.64 0.41 -0.13 0.05 -0.35 473 D86 ----- 0.92 0.11 0.53 1.14 0.64 485 D86 Automated -0.42 0.26 -0.09 -0.80 -0.19 496 D86 Automated -0.06 -0.11 -0.32 -0.49 0.80 601 ----- ----- ----- ----- ----- ----- 606 D86 Automated 0.07 0.79 0.90 0.28 0.44 608 D86 Automated -0.51 0.04 0.06 -0.41 -0.58 631 D86 Automated 0.58 -0.71 -0.42 0.13 -0.51 634 D86 Manual 0.32 -0.03 0.25 2.70 2.26 657 D86 Automated 0.48 -0.19 0.43 0.59 0.13 663 D86 Automated -0.40 0.94 0.53 1.02 0.58 671 D86 Automated 0.75 0.86 1.19 1.91 -1.10 732 D86 Manual 0.35 -0.34 -1.07 -1.19 0.09 823 D86 Automated 1.03 1.01 1.28 -0.10 0.56 824 D86 Automated 0.38 0.34 0.53 0.52 0.72 851 D86 Automated 0.52 0.41 -0.42 0.59 -0.47 854 D86 Automated 0.38 0.41 0.53 0.21 0.20 862 D86 Automated -0.95 -0.56 -0.70 -0.95 0.01 869 D86 Manual 0.35 -0.71 0.34 0.36 0.28 922 D86 Manual -0.85 -1.09 -2.96 -1.57 -0.70 962 ----- ----- ----- ----- ----- ----- 963 D86 Automated -1.90 0.56 -0.70 -1.42 -0.82 974 D86 Automated 0.24 -0.49 -0.79 0.36 -0.47 994 D86 Manual -0.16 -0.71 -2.02 -1.19 -0.31 995 D86 Manual 0.01 -1.09 -1.07 -1.19 -0.11 996 D86 Manual -0.34 -1.09 -1.07 -1.19 -0.11 997 D86 ----- -0.34 -1.47 -1.55 -2.35 -0.31



lab method mode IBP 10% 50% 90% FBP 998 D86 Manual -0.51 -1.09 -1.55 -1.96 0.28 1011 D86 Automated -0.57 -0.34 -0.32 -1.73 0.17 1016 ----- ----- ----- ----- ----- ----- 1026 ISO3405 Automated 0.31 0.19 0.15 -1.03 0.64 1039 ISO3405 Automated -1.25 -1.69 -0.70 -1.50 0.32 1049 D86 Automated -0.13 0.49 0.34 -0.41 0.13 1059 D86 Automated -0.10 0.34 -0.32 -0.41 0.44 1062 D86 Automated 0.72 0.64 0.90 0.28 0.32 1064 D86 Automated -0.44 0.56 1.00 1.68 0.88 1065 D86 Automated 0.96 -0.64 -0.51 -0.34 -0.47 1079 D86 Automated 0.35 -0.04 1.28 0.75 0.28 1081 D86 Automated -0.06 0.79 0.24 -0.49 0.40 1082 D86 Automated -0.06 0.19 -0.13 0.59 0.60 1097 ISO3405 Automated 0.52 1.24 0.90 1.21 0.44 1109 D86 Automated 0.86 0.94 0.90 1.06 0.28 1121 IP123 Manual -1.15 -3.27 -0.51 -0.72 -1.85 1126 in house Automated 0.92 1.31 -0.98 0.28 0.09 1134 ----- ----- ----- ----- ----- ----- 1146 D86 ----- 0.41 -0.26 -0.23 -0.41 -0.11 1150 ISO3405 Automated 0.89 0.11 -0.04 0.67 -0.23 1161 ISO3405 ----- -0.23 -0.79 -0.32 -1.11 0.76 1182 D86 Automated 0.69 0.04 0.53 0.90 0.60 1191 D86 Automated -0.95 0.71 0.34 0.67 0.48 1203 ISO3405 Automated 1.23 ----- 1.00 1.99 0.36 1205 D86 Automated 1.06 0.71 0.81 -0.18 0.32 1279 D86 Automated 0.31 0.86 0.24 -0.88 -2.28 1297 D86 Automated -0.81 -0.41 -0.04 -0.57 -0.66 1299 D86 Automated -0.27 0.26 0.72 1.37 0.28 1316 D86 Automated -0.40 -0.11 0.53 0.90 -0.03 1318 D86 Automated -1.39 0.04 -0.79 -0.88 -0.62 1347 D86 Manual 0.18 -0.34 0.81 -0.03 0.48 1348 D86 Automated 0.21 -1.77 1.09 -0.18 -0.98 1372 ----- ----- ----- ----- ----- ----- 1395 ----- ----- ----- ----- ----- ----- 1397 D86 ----- 0.92 0.79 -0.23 -1.42 -0.03 1417 IP123 Automated 0.14 0.86 2.13 3.23 0.13 1428 D86 Automated -0.03 -0.49 -0.32 -1.03 -0.15 1429 D86 Automated -0.47 -0.49 -0.98 -1.26 -0.19 1496 D86 Automated -0.37 0.71 0.15 0.36 0.20 1498 D86 ----- -0.16 0.64 0.53 0.36 0.24 1528 D86 Automated 0.89 0.56 0.53 0.90 0.28 1543 D86 Manual 0.18 0.41 -2.96 -4.67 0.48 1585 D86 Automated 0.92 0.79 0.06 -1.11 0.17 1587 D86 Automated -0.71 0.19 0.24 -0.65 -0.54 1610 D86 Automated 0.75 0.71 -0.79 0.21 -0.19 1616 D86 Manual -0.85 -0.34 -1.07 -1.57 -1.10 1634 D86 Automated -1.97 0.64 0.72 0.75 0.52 1650 D86 Automated -0.20 -1.39 -1.07 0.75 0.91 1715 D86 Automated 1.30 0.19 -0.23 -0.34 -0.15 1720 D86 Automated -0.10 0.56 0.15 -0.65 1.43 1724 D86 Automated 0.18 0.34 0.81 0.13 0.28 1776 D86 Automated -1.73 -1.09 -0.51 0.21 -0.58 1784 D86 Automated 1.06 0.41 0.72 2.76 -0.27 1798 ----- ----- ----- ----- ----- ----- 1811 D86 Automated -0.03 -1.47 -1.92 -1.65 -0.58 1813 D86 Automated -1.10 0.22 -0.31 -0.85 -0.08 1833 D86 Automated -0.23 -0.49 -0.42 -1.34 -0.15 1842 D86 Automated -0.40 -0.11 0.90 1.68 0.72 1883 D86 Manual 1.88 -1.09 -2.02 -0.03 -1.10 1913 D86 Automated 0.82 0.64 0.72 -0.95 -0.98 2129 D86 Automated -1.25 -0.56 -0.79 -1.34 -0.39 2130 D86 Automated 0.55 0.86 0.06 -0.26 -0.35 9090 D86 Automated -0.13 -0.11 0.34 1.21 0.01



Determination of Existent Gum on sample #15170; results in mg/100 mL Lab method value mark z(targ) lab method value mark z(targ) 52

----- ----- 974 D381 0.8 0.04

62 D381 0.8 0.04 994 ----- ----- 120 D381 <0.5 ----- 995 ----- ----- 131

----- ----- 996 ----- -----

132 D381 1.6 0.76 997 ----- ----- 140 D381 0.00 -0.67 998 ----- ----- 150 D381 1 0.22 1011 D381 < 1 ----- 159 D381 0.6 -0.13 1016 ----- ----- 169 D381 0 -0.67 1026 ----- ----- 171 D381 <1 ----- 1039 IP540 <1 ----- 175 D381 <1 ----- 1049 D381 1.2 0.40 177 D381 0.6 -0.13 1059 D381Mod. 0.6 -0.13 194 D381 3.8 R(0.01) 2.71 1062 D381 0.6 -0.13 216 D381 1.2 0.40 1064 D381 0.0 -0.67 221

----- ----- 1065 ----- -----

224

----- ----- 1079 D381 1.1 0.31 225 0.4 -0.31 1081 D381 0.4 -0.31 228

----- ----- 1082 D381 0.47 -0.25

230 IP540 0.8 0.04 1097 IP540 0.3 -0.40 237

----- ----- 1109 D381 <1 -----

238

----- ----- 1121 ----- ----- 252 D381 1.0 0.22 1126 ----- ----- 253 D381 1.0 0.22 1134 ----- ----- 254

----- ----- 1146 ----- -----

256 D381 1.0 0.22 1150 1.0 0.22 258 D381 1.1 0.31 1161 ----- ----- 273 D381 <0.5 ----- 1182 ----- ----- 311 IP540 2 1.11 1191 D381 1.34 0.52 317 D381 <1 ----- 1203 ISO6246 0.6 -0.13 323 D381 1 0.22 1205 ----- ----- 333

----- ----- 1279 ----- -----

334 D381 1 0.22 1297 ----- ----- 335 D381 1 0.22 1299 D381 1 0.22 336

----- ----- 1316 D381 0.0 -0.67

340 D381 <1 ----- 1318 IP540 0.3 -0.40 353 IP540 0.6 -0.13 1347 D381 0.6 -0.13 369 IP540 <1 ----- 1348 D381 0.6 -0.13 370 IP540 0.7 -0.04 1372 ----- ----- 371

----- ----- 1395 ----- -----

372 D381 1 0.22 1397 ----- ----- 402 D381 0.60 -0.13 1417 IP540 1 0.22 440 D381 1 0.22 1428 D381 1.1 0.31 445 IP540 <1 ----- 1429 ----- ----- 447 IP540 1 0.22 1496 D381 0.1 -0.58 448 IP540 1.0 0.22 1498 ----- ----- 453 IP540 <1 ----- 1528 IP540 0.6 -0.13 463 D381 1.2 0.40 1543 ----- ----- 468 IP540 0.8 0.04 1585 ----- ----- 473 D381 <1 ----- 1587 IP540 0.8 0.04 485

----- ----- 1610 IP540 < 1 -----

496 D381 0.1 -0.58 1616 IP540 0.5 -0.22 601

----- ----- 1634 D381 0.5 -0.22

606 IP540 0.2 -0.49 1650 ----- ----- 608 D381 <1 ----- 1715 ----- ----- 631 IP540 0.55 -0.18 1720 ----- ----- 634

----- ----- 1724 <1,0 -----

657 D381 1 0.22 1776 D381 0.4 -0.31 663 D381 0.9 0.13 1784 D381 0.5 -0.22 671 D381 <0.5 ----- 1798 ----- ----- 732

----- ----- 1811 D381 0.30 -0.40

823 D381 1.2 0.40 1813 IP540 0.4000 -0.31 824

----- ----- 1833 1 0.22

851 IP540 0.5 -0.22 1842 ----- ----- 854

1 0.22 1883 D381 0.8 0.04

862 D381 0.4 -0.31 1913 D381 1.00 0.22 869 D381 0.6 -0.13 2129 D381 0.4 -0.31 922

----- ----- 2130 D381 1 0.22

962

----- ----- 9090 IP540 1.2 0.40 963 D381 1.0 0.22






Determination of Flash Point on sample #15170; results in °C lab method value mark z(targ) lab method value mark z(targ) 52 D56 41.5 -0.34 974 IP170 42.5 0.54 62 D56 41.5 -0.34 994 D93 42.5 0.54 120 D56 42.2 0.27 995 IP170 42.0 0.10 131 D56 40 -1.65 996 D93 42.5 0.54 132 D56 42.5 0.54 997 IP170 42.5 0.54 140 IP170 41.9 0.01 998 D93 43.0 0.97 150 D56 41.5 -0.34 1011 IP170 41.5 -0.34 159 D56 42.2 0.27 1016 IP170 41.5 -0.34 169 D56 40.5 -1.21 1026 IP170 43.5 1.41 171 D56 41.0 -0.78 1039 IP170 42.0 0.10 175 D56 42.5 0.54 1049 ISO13736 41.5 -0.34 177 D56 40 -1.65 1059 IP170 42.5 0.54 194 D56 44.5 2.29 1062 IP170 40.5 -1.21 216 D56 39.0 -2.53 1064 IP170 41.0 -0.78 221 D3828 38.0 R(0.05) -3.40 1065 ----- ----- 224 IP170 41.28 -0.53 1079 IP170 42.5 0.54 225 IP170 41.0 -0.78 1081 IP170 42.1 0.19 228

----- ----- 1082 D56 41.5 -0.34

230 IP170 42.5 0.54 1097 ISO13736 42.0 0.10 237

----- ----- 1109 IP170 42.0 0.10

238

----- ----- 1121 IP170 40.0 -1.65 252 IP170 42.0 0.10 1126 D93 46 R(0.05) 3.60 253 IP170 42.0 0.10 1134 ----- ----- 254 IP170 42.0 0.10 1146 ----- ----- 256 IP170 42.0 0.10 1150 D56 40.0 -1.65 258 IP170 41.5 -0.34 1161 ISO2719 46.5 C,R(0.01) 4.04 273 IP170 42.5 0.54 1182 D93 44 1.85 311 IP170 43.0 0.97 1191 IP170 42.0 0.10 317 IP170 42.5 0.54 1203 ISO2719 44.5 2.29 323 IP170 43.5 1.41 1205 D93 43.0 0.97 333 IP170 41.5 -0.34 1279 D56 43.5 1.41 334 IP170 41.5 -0.34 1297 D93 42 0.10 335 IP170 41 -0.78 1299 IP170 42.5 0.54 336

----- ----- 1316 IP170 42.0 0.10

340 IP170 41.0 -0.78 1318 IP170 41.5 -0.34 353 IP170 41.5 -0.34 1347 IP170 42.0 0.10 369 IP170 42.0 0.10 1348 IP170 42.0 0.10 370 IP170 42.0 0.10 1372 ----- ----- 371 IP170 41.0 -0.78 1395 ----- ----- 372 IP170 42.0 0.10 1397 D56 42.5 0.54 402 D56 42.5 0.54 1417 IP170 42.0 0.10 440 IP170 41.77 -0.10 1428 ----- ----- 445 IP170 41.5 -0.34 1429 D56 40.1 -1.56 447 IP170 41.9 0.01 1496 IP170 41.1 -0.69 448 IP170 42.6 0.62 1498 D56 43.5 1.41 453 IP170 40.5 -1.21 1528 D56 43.5 1.41 463 IP170 41.5 -0.34 1543 D93 41.0 -0.78 468 IP170 41.0 -0.78 1585 IP170 41.5 -0.34 473 IP170 42.5 0.54 1587 IP170 42.0 0.10 485 D56 41.0 -0.78 1610 IP170 44.0 1.85 496 ISO13736 42.5 0.54 1616 IP170 41.0 -0.78 601 IP170 41.5 -0.34 1634 IP170 41.2 -0.60 606 IP170 43.5 1.41 1650 IP170 42.5 0.54 608 IP170 42.0 0.10 1715 D56 42.5 0.54 631 IP170 44.5 2.29 1720 D3828 42.0 0.10 634 D56 39.1 -2.44 1724 IP170 42.0 0.10 657 IP170 41.5 -0.34 1776 IP170 41.5 -0.34 663

----- ----- 1784 D3828 41 -0.78

671 IP170 41.0 -0.78 1798 ----- ----- 732 D93 43.5 1.41 1811 D56 42 C 0.10 823 IP170 41.0 -0.78 1813 IP170 42.0 0.10 824 IP170 41.0 -0.78 1833 IP170 42 0.10 851 IP170 40.45 -1.26 1842 ----- ----- 854 IP170 41.0 -0.78 1883 D56 43 0.97 862 IP170 41.5 -0.34 1913 IP170 43.2 1.15 869 IP170 41.0 -0.78 2129 IP170 41.5 -0.34 922 IP170 42.0 0.10 2130 IP170 42.0 0.10 962

----- ----- 9090 IP170 43 0.97

963 IP170 41.0 -0.78



normality OK n 120 outliers 3 mean (n) 41.89 st.dev. (n) 1.015 R(calc.) 2.84 R(IP170:14) 3.20

Lab 1161 first reported 47.5 Lab 1811 first reported 45.5



Determination of Freezing Point on sample #15170; results in °C lab method value mark z(targ) lab method value mark z(targ) 52 D5972 -55.4 -1.49 974 D2386 -55.0 -1.04 62 D5972 -55.0 -1.04 994 D2386 -53.5 0.64 120 D2386 -54 0.08 995 D2386 -53.0 C 1.20 131

----- ----- 996 D2386 -53.5 0.64

132 D2386 -54.5 -0.48 997 D2386 -53.5 0.64 140 D5972 -54.6 -0.60 998 D2386 -54.0 0.08 150 D5972 -54.4 -0.37 1011 D5972 -55.2 -1.27 159 D2386 -55.39 -1.48 1016 D5972 -54.4 -0.37 169 D2386 -55.0 -1.04 1026 D5972 -55.1 -1.16 171 D2386 -56.0 -2.16 1039 IP529 -54.1 -0.04 175 D2386 -53.5 0.64 1049 D7153 -54.1 -0.04 177 D2386 -54 0.08 1059 D2386 -54.5 -0.48 194 D2386 -52.0 2.32 1062 D7153 -54.0 0.08 216 D2386 -54.0 0.08 1064 D7153 -53.75 0.36 221 D2386 -53 1.20 1065 D7153 -54.0 0.08 224

----- ----- 1079 D5972 -54.5 -0.48

225 D2386 -55.0 -1.04 1081 D7153 -53.9 0.19 228

----- ----- 1082 IP529 -53.9 0.19

230 D2386 -54.25 -0.20 1097 IP529 -53.7 0.41 237

----- ----- 1109 D5972 -55.3 -1.38

238

----- ----- 1121 IP16 -54.0 0.08 252 D2386 -53.0 1.20 1126 ----- ----- 253 D2386 -54.5 -0.48 1134 ----- ----- 254

----- ----- 1146 ----- -----

256 D2386 -53 1.20 1150 D2386 -54.0 0.08 258 D2386 -53.0 1.20 1161 ----- ----- 273 D2386 -56 -2.16 1182 D5972 -53.6 0.52 311 D2386 -54.0 0.08 1191 IP529 -54.1 -0.04 317 D5972 -54.6 -0.60 1203 D2386 -56 -2.16 323 D2386 -54.0 0.08 1205 ----- ----- 333 IP529 -53.9 0.19 1279 D2386 -53.5 0.64 334 D7153 -53.4 0.75 1297 D5972 -54.3 -0.26 335 IP529 -53.7 0.41 1299 D2386 -54.0 0.08 336

----- ----- 1316 D2386 -53.8 0.30

340 D2386 -54 0.08 1318 D7153 -53.6 0.52 353 IP16 -54.0 0.08 1347 D2386 -54 0.08 369 D2386 -54.0 0.08 1348 D2386 -53.0 1.20 370 D2386 -53.5 0.64 1372 ----- ----- 371 D2386 -54.0 0.08 1395 ----- ----- 372 D2386 -53.5 0.64 1397 D2386 -52.7 1.53 402 D2386 -53.5 0.64 1417 ----- ----- 440 IP16 -55 -1.04 1428 ----- ----- 445 IP529 -54.1 -0.04 1429 ----- ----- 447 IP529 -53.6 0.52 1496 D5972 -53.6 0.52 448 IP529 -54.1 -0.04 1498 ----- ----- 453 D5972 -55.2 -1.27 1528 D7153 -53.7 0.41 463 D2386 -54 0.08 1543 D2386 -57 R(0.05) -3.28 468

----- ----- 1585 D2386 -55 -1.04

473 D2386 -53.5 0.64 1587 IP529 -54.0 0.08 485

----- ----- 1610 D5972 -55.3 -1.38

496 D2386 -53.5 0.64 1616 D7153 -53.9 0.19 601 D2386 -53.0 1.20 1634 D2386 -54.0 0.08 606 D2386 -52.5 1.76 1650 D2386 -53.5 0.64 608 D2386 -54.5 -0.48 1715 D5972 -54.2 -0.15 631 D2386 -56.0 -2.16 1720 D7153 -54.4 -0.37 634 D2386 -55.2 -1.27 1724 D2386 -53.0 1.20 657 D2386 -54.0 0.08 1776 D2386 -53.8 0.30 663 D2386 -55.5 -1.60 1784 D2386 -54.5 -0.48 671 D2386 -53.0 1.20 1798 ----- ----- 732

----- ----- 1811 D2386 -53.5 0.64

823 D2386 -54.5 -0.48 1813 D5972 -54.5 -0.48 824 D2386 -54.0 0.08 1833 D5972 -53 1.20 851 D2386 -53.57 0.56 1842 D2386 -55.0 -1.04 854 D2386 -54.0 0.08 1883 D2386 -57 R(0.05) -3.28 862 D2386 -53.15 1.03 1913 D5972 -54.2 -0.15 869 D2386 -53.65 0.47 2129 D2386 -53.0 1.20 922 D2386 -54.5 -0.48 2130 IP16 -54.0 0.08 962

----- ----- 9090 D5972 -54.7 -0.71

963 D2386 -53.5 0.64



normality OK n 112 outliers 2 mean (n) -54.07 st.dev. (n) 0.774 R(calc.) 2.17 R(D2386:15e1) 2.50

Lab 447 also reported: Freezing point manual acc. to IP16: -53.0 Lab 995 first reported: 54.5



Determination of JFTOT; Tube Rating, Delta P in mmHg on sample #15170; lab method tube

rating mark Delta P mark lab method tube rating mark Delta P mark

52 D3241 <1 1 974 D3241 <1 0 62

----- ----- 994 ----- -----

120 D3241 1 0 995 ----- ----- 131

----- ----- 996 ----- -----

132 D3241 <1 0.1 997 ----- ----- 140 D3241 <1 0 998 ----- ----- 150 D3241 <1 1 1011 D3241 1 0 159 D3241 1 0 1016 D3241 <1 <1 169 D3241 1 1 1026 D3241 <1 1.0 171 D3241 <1 0 1039 D3241 <1 0.1 175 D3241 <1 0 1049 D3241 1 0.0 177 D3241 1 1 1059 ----- ----- 194

----- ----- 1062 D3241 1 0.1

216

----- ----- 1064 D3241 1 0 221

----- ----- 1065 ----- -----

224

----- ----- 1079 D3241 <1 0.1 225 D3241 <1 0.0 1081 D3241 <1 0 228

-----

----- 1082 D3241 1 1

230 D3241 <1 <1 1097 D3241 1 0 237

----- ----- 1109 D3241 <1 0

238

----- ----- 1121 ----- ----- 252 D3241 <1 0 1126 ----- ----- 253 D3241 <1 0 1134 ----- ----- 254

----- ----- 1146 D3241 1 0.0

256

----- ----- 1150 ----- ----- 258 D3241 <1.0 0.4 1161 ----- ----- 273

----- ----- 1182 ----- -----

311 D3241 1 3 C,R(0.01) 1191 D3241 1 1 317

----- ----- 1203 ----- -----

323 D3241 <1 C <1 1205 ----- ----- 333

----- ----- 1279 D3241 1 0.0

334 D3241 <1 0 1297 ----- ----- 335 D3241 0 0 1299 D3241 1 0 336

----- ----- 1316 D3241 <1 0

340 D3241 1 <1 1318 D3241 <1 0.0 353

----- ----- 1347 D3241 1 0

369 D3241 1 <1 1348 D3241 1 0 370 D3241 1 <3 1372 ----- ----- 371

----- ----- 1395 ----- -----

372 D3241 1 0 1397 ----- ----- 402 D3241 <1 0 1417 IP323 <1 0 440 IP323 <1 0 1428 D3241 1 0 445 D3241 1 <1 1429 ----- ----- 447 D3241 1 <1 1496 ----- ----- 448 D3241 1 <1 1498 ----- ----- 453 IP323 1 <1 1528 D3241 1 1 463

----- ----- 1543 D3241 1 0

468

----- ----- 1585 ----- ----- 473

----- ----- 1587 D3241 <1 0.1

485

----- ----- 1610 IP323 <1 2.5 R(0.01) 496

----- ----- 1616 D3241 1 0

601

----- ----- 1634 D3241 1 0.0 606

----- ----- 1650 D3241 1 0

608

----- ----- 1715 ----- ----- 631 D3241 <1 <1.0 1720 D3241 1.0 5 R(0.01) 634

----- ----- 1724 D3241 1 0

657 D3241 1 <1 1776 ----- ----- 663

----- ----- 1784 D3241 1 1

671 D3241 1 0.3 1798 ----- ----- 732

----- ----- 1811 ----- -----

823 D3241 1 0 1813 D3241 1 0 824 D3241 1 0.1 1833 D3241 <1 0.2 851 D3241 <1 0.1 1842 IP323 1 <1 854 D3241 <1 0.2 1883 ----- ----- 862 D3241 <1 0 1913 D3241 <1 0.0 869 D3241 <1 0 2129 D3241 1 0 922

----- ----- 2130 D3241 <1 0

962

----- ----- 9090 ----- ----- 963 D3241 <1 0.9



Tube Rating Delta P

normality not OK normality not OK n 77 n 62

41 reported 1 outliers 3

1 reported 0 mean (n) 0.19

36 reported <1 st.dev. (n) 0.362

R(calc.) 1.01

R(lit) unknown

Lab 311 first reported for the Delta P 4 Lab 323 first reported for the tube rating 3 Lab 974 reported <1/NA or NP Delta Pressure



Determination of Kinematic Viscosity at -20°C on sample #15170; results in cSt lab method value mark z(targ) lab method value mark z(targ) 52 D445 3.842 -0.34 974 D445 3.799 -1.99 62 D445 3.806 -1.72 994 ----- ----- 120 D445 3.834 -0.65 995 D445 3.868 0.65 131

----- ----- 996 ----- -----

132 D445 3.8111 -1.52 997 ----- ----- 140 D445 3.839 -0.46 998 ----- ----- 150 D445 3.880 1.11 1011 D445 3.873 0.84 159 D445 3.8495 -0.05 1016 D445 3.8553 0.17 169 D445 3.8517 0.03 1026 ISO3104 3.861 0.39 171 D445 3.864 0.50 1039 D445 3.827 -0.92 175 D445 3.847 -0.15 1049 D445 3.855 0.16 177 D445 3.872 0.81 1059 D445 3.839 -0.46 194 D445 5.9145 C, R(0.01) 78.97 1062 D445 3.838 -0.49 216

----- ----- 1064 D445 3.8460 -0.19

221

----- ----- 1065 ----- ----- 224

----- ----- 1079 D445 3.86688 0.61

225 D445 3.872 0.81 1081 D445 3.854 0.12 228

----- ----- 1082 D445 3.8289 -0.84

230 D445 3.8736 0.87 1097 ISO3104 3.8508 0.00 237

----- ----- 1109 D445 3.8590 0.31

238

----- ----- 1121 ----- ----- 252

----- ----- 1126 ----- -----

253 D445 3.820 -1.18 1134 ----- ----- 254

----- ----- 1146 ----- -----

256 D445 3.850 -0.04 1150 ISO3104 3.8864 C 1.36 258

----- ----- 1161 ----- -----

273

----- ----- 1182 ----- ----- 311 D445 3.848 -0.11 1191 D445 3.894 1.65 317

----- ----- 1203 ISO3104 4.001 R(0.01) 5.74

323 D445 3.877 1.00 1205 ----- ----- 333 D445 3.851 0.00 1279 ----- ----- 334 D445 3.851 0.00 1297 ----- ----- 335 D445 3.828 -0.88 1299 D445 3.866 C 0.58 336

----- ----- 1316 D445 3.853 0.08

340 D445 3.8525 0.06 1318 D7042 3.8417 -0.35 353

----- ----- 1347 D445 3.8314 -0.75

369 D445 3.845 -0.23 1348 D445 3.893 1.61 370 D445 3.8560 0.19 1372 ----- ----- 371

----- ----- 1395 ----- -----

372 D445 3.847 -0.15 1397 D7042 3.846 -0.19 402 D445 3.8391 -0.45 1417 D445 3.8577 0.26 440 D445 3.8712506 0.78 1428 D445 3.825 -0.99 445 IP71 3.851 0.00 1429 ----- ----- 447 D445 3.855 0.16 1496 D445 3.875 0.92 448 D445 3.853 0.08 1498 ----- ----- 453 IP71 3.8689 0.69 1528 D445 3.8901 1.50 463

----- ----- 1543 ----- -----

468

----- ----- 1585 D445 3.8441 -0.26 473

----- ----- 1587 D445 3.84306 -0.30

485

----- ----- 1610 IP71 3.686 R(0.01) -6.31 496 D445 3.853 0.08 1616 D445 3.899 1.84 601

----- ----- 1634 ----- -----

606

----- ----- 1650 D445 3.8479 -0.12 608

----- ----- 1715 ----- -----

631 D445 3.8788 1.07 1720 D445 3.870 0.73 634

----- ----- 1724 D445 3.787 -2.45

657 D445 3.881 1.15 1776 D445 3.8615 0.40 663 D445 3.8456 -0.20 1784 D445 3.828 -0.88 671

----- ----- 1798 ----- -----

732

----- ----- 1811 D445 3.8340 -0.65 823 D445 3.857 C 0.23 1813 D445 3.8490 -0.07 824 D445 3.859 C 0.31 1833 D445 3.773 -2.98 851 D445 3.859 0.31 1842 ----- ----- 854 D445 3.875 0.92 1883 ----- ----- 862 D445 3.8651 C 0.54 1913 D445 3.838 -0.49 869 D445 3.8664 0.59 2129 D445 3.7812 -2.67 922

----- ----- 2130 D445 3.833 -0.69

962

----- ----- 9090 D445 3.871 0.77 963 D445 3.841 -0.38




Lab 194 first reported 4.016 Lab 823 first reported 4.149 Lab 824 first reported 3.743 Lab 862 first reported 4.2304 Lab 1150 first reported 3.9364 Lab 1299 first reported 3.346



Determination of Mercaptan Sulphur on sample #15170; results in % M/M lab method value mark z(targ) lab method value mark z(targ) 52 D3227 0.0004 -0.75 974 D3227 0.0007 1.79 62 D3227 0.0005 0.09 994 UOP163 0.00045 -0.33 120 D3227 0.0004 -0.75 995 D3227 0.00046 -0.25 131

----- ----- 996 D3227 0.0005 0.09

132 D3227 0.0003 -1.60 997 ----- ----- 140 D3227 0.0005 0.09 998 ----- ----- 150 D3227 0.00054 0.43 1011 D3227 0.00043 C -0.50 159 D3227 0.0005 0.09 1016 D3227 0.00046 -0.25 169

----- ----- 1026 D3227 < 1 -----

171 D3227 0.0005 0.09 1039 D3227 0.0005 0.09 175 D3227 0.0005 0.09 1049 D3227 0.000458 -0.26 177 D3227 0.000492 0.03 1059 D3227 0.00059 0.86 194

----- ----- 1062 D3227 0.0005 0.09

216

----- ----- 1064 D3227 0.00046 -0.25 221

----- ----- 1065 ----- -----

224

----- ----- 1079 UOP163 0.00062 C 1.11 225

----- ----- 1081 D3227 0.0005 0.09

228

----- ----- 1082 ----- ----- 230 D3227 0.00059 0.86 1097 ISO3012 0.00042 -0.58 237

----- ----- 1109 D3227 0.00044 -0.41

238

----- ----- 1121 ----- ----- 252

----- ----- 1126 ----- -----

253 D3227 0.0005 0.09 1134 ----- ----- 254

----- ----- 1146 ----- -----

256

----- ----- 1150 ----- ----- 258

----- ----- 1161 D3227 0.00057 0.69

273 D3227 0.0005 0.09 1182 ----- ----- 311 D3227 0.0004 -0.75 1191 ----- ----- 317 UOP163 0.00042 -0.58 1203 ----- ----- 323 D3227 0.0005 0.09 1205 ----- ----- 333

----- ----- 1279 ----- -----

334 D3227 0.0004 -0.75 1297 D3227 0.00065 1.36 335 D3227 0.0005 0.09 1299 D3227 0.0007 1.79 336

----- ----- 1316 D3227 0.0005 0.09

340 D3227 0.00041 -0.67 1318 ----- ----- 353

----- ----- 1347 IP342 0.00058 0.77

369 D3227 0.00043 -0.50 1348 IP342 0.00057 0.69 370 D3227 0.00053 0.35 1372 ----- ----- 371 D3227 0.00051 0.18 1395 ----- ----- 372 D3227 0.0005 0.09 1397 D3227 0.0005 0.09 402 D3227 0.00075 2.21 1417 ----- ----- 440 D3227 0.0003 -1.60 1428 D3227 0.0006 0.94 445 IP342 0.0005 0.09 1429 ----- ----- 447 D3227 0.0005 0.09 1496 D3227 0.00046 -0.25 448 D3227 0.0005 0.09 1498 ----- ----- 453 IP342 0.0004 -0.75 1528 D3227 0.00054 0.43 463

----- ----- 1543 ----- -----

468

----- ----- 1585 D3227 0.0005 0.09 473

----- ----- 1587 ----- -----

485

----- ----- 1610 IP342 0.0005 0.09 496 D3227 0.00037 -1.01 1616 D3227 0.00043 -0.50 601

----- ----- 1634 ----- -----

606

----- ----- 1650 D3227 0.0004 -0.75 608

----- ----- 1715 ----- -----

631

----- ----- 1720 ----- ----- 634

----- ----- 1724 D3227 0.00045 -0.33

657 D3227 0.0003 -1.60 1776 UOP163 0.000420 -0.58 663

----- ----- 1784 D3227 0.0005 0.09

671

----- ----- 1798 ----- ----- 732 D3227 0.00047 -0.16 1811 D3227 0.000623 1.14 823 D3227 0.0008 R(0.05) 2.63 1813 D3227 0.00002 R(0.01) -3.97 824 D3227 0.0004 -0.75 1833 D3227 0.0005 0.09 851 D3227 0.0004 -0.75 1842 IP342 0.0006 0.94 854 D3227 0.00048 -0.08 1883 ----- ----- 862 D3227 0.00054 0.43 1913 ----- W ----- 869 D3227 0.00046 -0.25 2129 D3227 0.0005 0.09 922 D3227 <0.0003 ----- 2130 D3227 0.0005 0.09 962

----- ----- 9090 ----- -----

963 D3227 0.0004 -0.75




Lab 1011 first reported 0.0043 Lab 1079 first reported 0.000925 Lab 1913 first reported 0.00083; with drawn result and reported re-use of sample due to sample shortage



Determination of MSEP on sample #15170; results in MSEP rating lab method value mark z(targ) lab method value mark z(targ) 52 D3948 93 0.73 974 ----- ----- 62 D3948 92 0.49 994 ----- ----- 120 D3948 80 -2.35 995 ----- ----- 131

----- ----- 996 ----- -----

132 D3948 90 0.02 997 ----- ----- 140 D3948 84 -1.40 998 ----- ----- 150 D3948 92 0.49 1011 D3948 87 -0.69 159 D3948 87 -0.69 1016 D3948 86 -0.93 169 D3948 88 -0.45 1026 ----- ----- 171 D3948 84 -1.40 1039 D3948 83 -1.64 175 D3948 85 -1.16 1049 D3948 85 -1.16 177 D3948 91 0.25 1059 D3948 89 -0.22 194

----- ----- 1062 D3948 97 1.67

216

----- ----- 1064 D3948 83 -1.64 221

----- ----- 1065 ----- -----

224

----- ----- 1079 D3948 87 -0.69 225 D3948 84 -1.40 1081 D3948 62 R(0.01) -6.60 228

----- ----- 1082 D3948 89 -0.22

230 D3948 91 0.25 1097 D3948 89 -0.22 237

----- ----- 1109 D3948 91 0.25

238

----- ----- 1121 D3948 95 1.20 252 D3948 94 0.96 1126 ----- ----- 253 D3948 93 0.73 1134 ----- ----- 254 D3948 92 0.49 1146 ----- ----- 256 D3948 94 0.96 1150 D3948 88 C -0.45 258 D3948 93 0.73 1161 ----- ----- 273

----- ----- 1182 ----- -----

311 D3948 85 -1.16 1191 D3948 85 -1.16 317 D3948 91 0.25 1203 ----- ----- 323

----- ----- 1205 ----- -----

333 D3948 91 0.25 1279 D3948 92 0.49 334 D3948 82 -1.87 1297 ----- ----- 335 D3948 92 0.49 1299 D3948 97 1.67 336 D3948 90 0.02 1316 D3948 87 -0.69 340 D3948 85 -1.16 1318 D3948 96 1.44 353 D3948 87 -0.69 1347 D3948 94 0.96 369 D3948 91 0.25 1348 D3948 95 1.20 370 D3948 90 0.02 1372 ----- ----- 371

----- ----- 1395 ----- -----

372 D3948 93 0.73 1397 D3948 89 -0.22 402 D3948 90.0 0.02 1417 ----- ----- 440 D3948 89 -0.22 1428 ----- ----- 445 D3948 92 0.49 1429 ----- ----- 447 D3948 78 -2.82 1496 D3948 88 -0.45 448 D3948 89 -0.22 1498 ----- ----- 453 D3948 93 0.73 1528 D3948 85 -1.16 463 D3948 85 -1.16 1543 ----- ----- 468

----- ----- 1585 D3948 89 -0.22

473 D3948 91 0.25 1587 D3948 88 -0.45 485

----- ----- 1610 D3948 93 0.73

496

----- ----- 1616 D3948 85 -1.16 601 D3948 94 0.96 1634 D3948 87 -0.69 606 D3948 91 0.25 1650 D3948 91 0.25 608 D3948 99 2.15 1715 ----- ----- 631 D3948 98 1.91 1720 D3948 94 0.96 634

----- ----- 1724 D3948 91 0.25

657 D3948 92 0.49 1776 D3948 86 -0.93 663

----- ----- 1784 D3948 87 -0.69

671 D3948 93 0.73 1798 ----- ----- 732

----- ----- 1811 D3948 90.0 0.02

823 D3948 89 -0.22 1813 D3948 95 1.20 824

----- ----- 1833 D3948 90 0.02

851 D3948 95 1.20 1842 ----- ----- 854 D3948 95 1.20 1883 D3948 91 0.25 862 D3948 96 1.44 1913 D3948 94 0.96 869 D3948 97 1.67 2129 D3948 90 0.02 922

----- ----- 2130 D3948 94 0.96

962

----- ----- 9090 D3948 82 -1.87 963 D3948 89 -0.22




Lab 1150 first reported 38 Lab 1650 reported “at 24°C”



Determination of Naphthalenes on sample #15170; results in %V/V lab method value mark z(targ) lab method value mark z(targ) 52 D1840 - meth.B 0.56 0.04 974 D1840 - meth.A 0.573 0.59 62 D1840 - meth.A 0.558 C -0.04 994 ----- ----- 120 D1840 - meth.B 0.65 R(0.01) 3.84 995 ----- ----- 131

----- ----- 996 ----- -----

132 D1840 - meth.B 0.565 0.25 997 ----- ----- 140 D1840 - meth.A 0.54 -0.80 998 ----- ----- 150 D1840 - meth.A 0.58 0.89 1011 D1840 - meth.A 0.56 0.04 159 D1840 - meth.A 0.56 0.04 1016 D1840 - meth.B 0.58 0.89 169 D1840 - meth.B 0.545 -0.59 1026 ----- ----- 171

----- ----- 1039 D1840 - meth.A 0.57 0.46

175 D1840 - meth.B 0.567 0.34 1049 D1840 - meth.A 0.558 -0.04 177 D1840 - meth.A 0.62 2.57 1059 D1840 - meth.B 0.55 -0.38 194

----- ----- 1062 D1840 - meth.A 0.57 0.46

216

----- ----- 1064 D1840 - meth.A 0.552 -0.30 221

----- ----- 1065 ----- -----

224

----- ----- 1079 D1840 - meth.A 0.565 0.25 225

----- ----- 1081 D1840 - meth.A 0.51 -2.07

228

----- ----- 1082 ----- ----- 230 D1840 - meth.B 1.02 R(0.01) 19.47 1097 D1840 - meth.A 0.548 -0.47 237

----- ----- 1109 D1840 - meth.A 0.570 0.46

238

----- ----- 1121 ----- ----- 252

----- ----- 1126 ----- -----

253 D1840 - meth.B 0.57 0.46 1134 ----- ----- 254

----- ----- 1146 ----- -----

256

----- ----- 1150 ----- ----- 258

----- ----- 1161 ----- -----

273 D1840 - meth.B 0.55 -0.38 1182 ----- ----- 311 D1840 - meth.B 0.54 -0.80 1191 D1840 - meth.A 0.538 -0.89 317

----- ----- 1203 D1840 - meth.A 0.55 -0.38

323 D1840 - meth.A 0.56 0.04 1205 ----- ----- 333 D1840 - meth.B 0.56 0.04 1279 ----- ----- 334 D1840 - meth.A 0.55 -0.38 1297 ----- ----- 335 D1840 - meth.A 0.65 R(0.01) 3.84 1299 D1840 - meth.A 0.56 0.04 336

----- ----- 1316 D1840 - meth.B 0.5708 0.50

340 D1840 - meth.B 0.565 0.25 1318 D1840 - meth.B 0.60 1.73 353

----- ----- 1347 D1840 - meth.B 0.462 R(0.01) -4.10

369 D1840 - meth.B 0.53 -1.23 1348 D1840 - meth.B 0.96 R(0.01) 16.93 370 D1840 - meth.A 0.553 -0.25 1372 ----- ----- 371 D1840 - meth.B 0.537 -0.93 1395 ----- ----- 372 D1840 - meth.B 0.55 -0.38 1397 0.83 R(0.01) 11.44 402 D1840 - meth.B 0.552 -0.30 1417 ----- ----- 440 D1840 - meth.B 0.616795 2.44 1428 ----- ----- 445 D1840 - meth.B 0.55 -0.38 1429 ----- ----- 447 D1840 - meth.B 0.56 0.04 1496 D1840 - meth.B 0.5573 -0.07 448 D1840 - meth.B 0.682 C,R(0.01) 5.19 1498 ----- ----- 453 D1840 - meth.B 0.54 -0.80 1528 ----- ----- 463

----- ----- 1543 ----- -----

468

----- ----- 1585 D1840 - meth.A 0.58 0.89 473

----- ----- 1587 ----- -----

485

----- ----- 1610 D1840 - meth.B 0.52 -1.65 496 D1840 - meth.B 0.564 0.21 1616 D1840 - meth.B 0.57 0.46 601

----- ----- 1634 D1840 - meth.B 0.57 0.46

606

----- ----- 1650 ----- ----- 608

----- ----- 1715 ----- -----

631 D1840 - meth.A 0.565 0.25 1720 D1840 - meth.B 0.56 C 0.04 634

----- ----- 1724 ----- -----

657 D1840 - meth.A 0.52 -1.65 1776 D1840 - meth.A 0.67 R(0.01) 4.69 663 D1840 - meth.A 0.599 1.69 1784 D1840 - meth.A 0.59 1.31 671

----- ----- 1798 ----- -----

732

----- ----- 1811 D1840 - meth.A 0.5504 -0.36 823 D1840 - meth.B 0.53 -1.23 1813 D1840 - meth.A 0.547 -0.51 824

----- ----- 1833 ----- -----

851 D1840 - meth.A 0.55 -0.38 1842 D1840 - meth.A 0.56 0.04 854 D1840 - meth.A 0.57 0.46 1883 ----- ----- 862 D1840 - meth.B 0.556 -0.13 1913 D1840 - meth.B 0.589 1.27 869 D1840 - meth.A 0.566 0.29 2129 D1840 - meth.B 0.509 -2.11 922

----- ----- 2130 ----- -----

962

----- ----- 9090 ----- ----- 963 D1840 - meth.B 0.551 -0.34



D1840-method A D1840-method B

normality suspect Not OK Not OK n 64 32 33 outliers 8 2 4 mean (n) 0.559 0.561 0.560 st.dev. (n) 0.0211 0.0207 0.0267 R(calc.) 0.059 0.058 0.075 R(D1840:07-B) 0.066 R(D1840:07-A): 0.047 0.047 0.066

Lab 62 first reported 0.285 Lab 448 first reported 1.15 Lab 1720 first reported 0.68

0.4

0.5

0.6

0.7

0.8

0.9

1

1.1

1347

2129

1081 657

1610 369

823

371

1191 453

140

311

169

1813

1097 273

334

445

372

851

1059

1203

1811 963

402

1064 370

862

1496 62

1049 159

323 52 447

333

1011

1299

1720

1842 496

340

132

631

1079 869

175

854

253

1039

1062

1109

1616

1634

1316 974

150

1016

1585

1913

1784 663

1318 440

177

335

120

1776 448

1397

1348 230



Determination of Smoke Point on sample #15170; results in mm. lab method value mark z(targ) lab method value mark z(targ) 52 D1322 23.5 0.01 974 D1322 24.0 0.39 62 D1322 22 -1.12 994 D1322 23.5 0.01 120 D1322 22 -1.12 995 D1322 24.45 0.73 131

----- ----- 996 D1322 23.5 0.01

132 D1322 23.7 0.16 997 ----- ----- 140 D1322 22 -1.12 998 ----- ----- 150 D1322 24.0 0.39 1011 D1322 23.6 0.09 159 D1322 21.5 -1.50 1016 IP598 24.3 0.62 169 D1322 25.0 1.15 1026 D1322 22 -1.12 171 D1322 25.0 1.15 1039 D1322 22.0 -1.12 175 D1322 22.8 -0.52 1049 D1322 24.2 0.54 177 D1322 23 -0.37 1059 D1322 24.8 1.00 194 D1322 23.0 -0.37 1062 D1322 23.0 -0.37 216

----- ----- 1064 D1322 22.15 -1.01

221

----- ----- 1065 ----- ----- 224

----- ----- 1079 D1322 24.1 0.47

225

----- ----- 1081 D1322 22.7 -0.59 228

----- ----- 1082 ----- -----

230 D1322 27.9 R(0.05) 3.35 1097 D1322 24.33 0.64 237

----- ----- 1109 D1322 24.24 0.57

238

----- ----- 1121 IP57 22.8 -0.52 252 D1322 24.0 0.39 1126 ----- ----- 253 D1322 25 1.15 1134 ----- ----- 254 D1322 24.26 0.59 1146 ----- ----- 256 D1322 23.76 0.21 1150 ----- ----- 258 D1322 24.0 0.39 1161 ISO3014 24 0.39 273 D1322 24 0.39 1182 ----- ----- 311 D1322 25.0 1.15 1191 D1322 23.2 -0.21 317 D1322 21.5 -1.50 1203 D1322 26 1.91 323 D1322 23.0 -0.37 1205 ----- ----- 333 IP57 23.3 -0.14 1279 ----- ----- 334 D1322 23.3 -0.14 1297 D1322 23.5 0.01 335 D1322 23.7 0.16 1299 D1322 23.2 -0.21 336

----- ----- 1316 D1322 24.5 0.77

340 D1322 24.0 0.39 1318 D1322 24.922 1.09 353

----- ----- 1347 D1322 25.0 1.15

369 D1322 22.8 -0.52 1348 D1322 23.0 -0.37 370 D1322 24.0 0.39 1372 ----- ----- 371

----- ----- 1395 ----- -----

372 D1322 23.0 -0.37 1397 D1322 23 -0.37 402

----- ----- 1417 ----- -----

440 D1322 20 -2.64 1428 ----- ----- 445 IP598 23.0 -0.37 1429 ----- ----- 447 D1322 25.0 1.15 1496 D1322 21.2 -1.73 448 D1322 20 -2.64 1498 ----- ----- 453 D1322 23.2 -0.21 1528 D1322 24.5 0.77 463 D1322 23.59 0.08 1543 D1322 20.6 -2.18 468 D1322 23.5 0.01 1585 D1322 24.5 0.77 473

----- ----- 1587 D1322 24.0 0.39

485

----- ----- 1610 IP598 23.5 0.01 496 D1322 23.7 0.16 1616 D1322 24 0.39 601

----- ----- 1634 ----- -----

606

----- ----- 1650 D1322 25.4 1.45 608

----- ----- 1715 D1322 24.5 0.77

631 D1322 23.6 0.09 1720 ----- ----- 634

----- ----- 1724 D1322 26.0 1.91

657 D1322 24.5 0.77 1776 D1322 23.7 0.16 663

----- ----- 1784 D1322 22.1 -1.05

671

----- ----- 1798 ----- ----- 732

----- ----- 1811 D1322 23.40 -0.06

823 D1322 23.2 -0.21 1813 D1322 23.0 -0.37 824 D1322 23.5 0.01 1833 D1322 26 1.91 851 D1322 20.44 -2.30 1842 D1322 24.0 0.39 854 D1322 22.0 -1.12 1883 ----- ----- 862 D1322 25.0 1.15 1913 D1322 23.8 0.24 869 D1322 21.0 -1.88 2129 D1322 22.8 -0.52 922 D1322 25.0 1.15 2130 IP598 23.0 -0.37 962

----- ----- 9090 D1322 23.5 0.01

963 D1322 24.0 0.39



normality OK n 93 outliers 1 mean (n) 23.48 st.dev. (n) 1.239 R(calc.) 3.47 R(D1322:15e1-M) 3.70



Determination of Specific Energy on sample #15170; results in MJ/kg lab method value mark z(targ) lab method value mark z(targ) 52

----- ----- 974 D3338 43.303 1.46

62 D3338 43.287 0.49 994 ----- ----- 120 D3338 43.286 0.43 995 ----- ----- 131

----- ----- 996 ----- -----

132 D3338 43.289 C 0.61 997 ----- ----- 140 D3338 43.243 -2.19 998 ----- ----- 150 D3338 43.307 1.71 1011 D3338 43.253 C -1.58 159 D3338 43.273 -0.36 1016 ----- ----- 169

----- ----- 1026 ----- -----

171 D3338 43.276 -0.18 1039 D3338 43.254 -1.52 175

----- ----- 1049 D3338 43.29193818 0.79

177 D3338 43.289 0.61 1059 D3338 43.281 0.13 194

----- ----- 1062 D3338 43.26 -1.15

216

----- ----- 1064 D3338 43.2933 0.87 221

----- ----- 1065 ----- -----

224

----- ----- 1079 D3338 43.283 0.25 225

----- ----- 1081 ----- -----

228

----- ----- 1082 ----- ----- 230 D3338 43.281 0.13 1097 D3338 43.281 0.13 237

----- ----- 1109 D3338 43.27 -0.54

238

----- ----- 1121 ----- ----- 252

----- ----- 1126 ----- -----

253 D3338 43.2807 0.11 1134 ----- ----- 254

----- ----- 1146 ----- -----

256

----- ----- 1150 ----- ----- 258

----- ----- 1161 D3338 43.242 -2.25

273

----- ----- 1182 ----- ----- 311 D3338 43.28 0.06 1191 D3338 43.2643 -0.89 317

----- ----- 1203 D3338 43.28 0.06

323 D3338 43.32 C 2.50 1205 ----- ----- 333

----- ----- 1279 ----- -----

334

----- ----- 1297 ----- ----- 335

----- ----- 1299 D3338 43.24 -2.37

336

----- ----- 1316 D3338 43.250 -1.76 340 D3338 43.257 -1.34 1318 D3338 43.236 -2.61 353

----- ----- 1347 D3338 43.243 -2.19

369 D3338 43.267 -0.73 1348 D3338 43.28 0.06 370 D3338 43.3061 1.65 1372 ----- ----- 371

----- ----- 1395 ----- -----

372 D3338 43.283 0.25 1397 D3338 43.25 -1.76 402

----- ----- 1417 ----- -----

440 D3338 43.337 3.53 1428 ----- ----- 445 D3338 43.259 -1.21 1429 ----- ----- 447 D3338 43.312 2.01 1496 D3338 43.2888 0.60 448 D3338 43.281 0.13 1498 ----- ----- 453 D3338 43.261 -1.09 1528 D3338 43.2897 0.66 463 D3338 43.32 2.50 1543 ----- ----- 468

----- ----- 1585 D3338 43.290 0.67

473

----- ----- 1587 ----- ----- 485

----- ----- 1610 D3338 43.276 -0.18

496 D3338 43.282 0.19 1616 D3338 43.279 0.00 601

----- ----- 1634 ----- -----

606

----- ----- 1650 D3338 43.265 -0.85 608

----- ----- 1715 ----- -----

631 D3338 43.2948 0.97 1720 ----- ----- 634

----- ----- 1724 D3338 43.287 0.49

657 D3338 43.285 0.37 1776 ----- ----- 663

----- ----- 1784 D3338 43.296 1.04

671

----- ----- 1798 ----- ----- 732

----- ----- 1811 D3338 43.2982 1.17

823 D3338 43.308 1.77 1813 D3338 43.26 -1.15 824 D3338 43.284 C 0.31 1833 D3338 43.257 -1.34 851 D3338 43.291 0.73 1842 ----- ----- 854 D3338 43.278 -0.06 1883 ----- ----- 862 D3338 43.254 -1.52 1913 D3338 43.26 -1.15 869 D3338 43.3058 1.64 2129 D3338 43.268 -0.67 922 D3338 43.281 0.13 2130 D3338 43.289 0.61 962

----- ----- 9090 ----- -----

963 D3338 43.292 0.80



normality OK n 66 outliers 0 mean (n) 43.2789 st.dev. (n) 0.02095 R(calc.) 0.0586 R(D3338:09e2) 0.0460

Lab 132 first reported 42.743 Lab 323 first reported 45.77 Lab 824 first reported 43.129 Lab 1011 first reported 43.55



Determination of Sulphur on sample #15170; results in mg/kg lab method value mark z(targ) lab method value mark z(targ) 52

----- ----- 974 D4294 703 -0.05

62 D5453 705 C 0.01 994 D4294 721 0.51 120 D4294 673.2 -0.99 995 D5453 690.7 -0.44 131

----- ----- 996 D5453 693.4 -0.35

132 D2622 693.3 -0.36 997 D4294 717 0.39 140 D2622 760.5 1.75 998 D4294 701 -0.11 150 D2622 709 C 0.14 1011 D4294 740 1.11 159 D4294 714.6 0.31 1016 ----- ----- 169

----- ----- 1026 ISO20884 700 -0.15

171 D5453 696 -0.27 1039 D2622 698.0 -0.21 175 D4294 663 -1.31 1049 D5453 636.824 C -2.13 177 D4294 712 C 0.23 1059 ISO14506Mod. 680 -0.77 194 D4294 862 R(0.01) 4.93 1062 D5453 717 0.39 216

----- ----- 1064 D5453 710.1 0.17

221

----- ----- 1065 IP336 794.9 R(0.05) 2.83 224 D4294 706.0 0.04 1079 D2622 726 0.67 225

----- ----- 1081 D4294 704.8 0.00

228

----- ----- 1082 D4294 703 -0.05 230 D4294 713 0.26 1097 D5453 710.17 0.17 237

----- ----- 1109 D4294 732 0.86

238

----- ----- 1121 D4294 710 C 0.17 252

----- ----- 1126 ISO20846 733.6 0.91

253 D4294 693 -0.37 1134 ----- ----- 254 D4294 756 1.61 1146 ----- ----- 256

----- ----- 1150 ----- -----

258

----- ----- 1161 ISO20846 685 -0.62 273 D5453 698 -0.21 1182 D4294 709 0.14 311 D2622 694 -0.33 1191 D4294 716 0.36 317 D2622 680 -0.77 1203 ISO20884 690 -0.46 323 D5453 694 -0.33 1205 ISO20846 703.57 -0.03 333 D4294 713 0.26 1279 ----- ----- 334 D5453 686 -0.59 1297 D4294 701.5 -0.10 335

----- ----- 1299 D2622 590 R(0.01) -3.60

336 ISO8754 682 -0.71 1316 D4294 710 C 0.17 340 D4294 697 -0.24 1318 D5453 737.5 1.03 353

----- ----- 1347 D4294 745 1.27

369 D2622 701 -0.11 1348 D4294 820 R(0.01) 3.62 370 IP336 709 0.14 1372 ----- ----- 371 D4294 704.7 0.00 1395 ----- ----- 372 D5453 699 -0.18 1397 D2622 691.6 -0.41 402 D5453 710.2 0.17 1417 IP336 703 -0.05 440 D5453 642.61 -1.95 1428 ISO8754 704 -0.02 445 D5453 691.57 -0.41 1429 ISO20846 769.7 2.04 447 IP336 680 -0.77 1496 D4294 726.6 0.69 448 IP336 661 C -1.37 1498 D5453 464.2 C,R(0.01) -7.54 453 IP336 706 0.04 1528 D2622 706.3 0.05 463 D4294 711.7 0.22 1543 D4294 6460 R(0.01) 180.50 468

----- ----- 1585 D4294 731.3 0.84

473

----- ----- 1587 D4294 692.8 -0.37 485

----- ----- 1610 IP336 837 R(0.01) 4.15

496 D2622 686.2 -0.58 1616 D4294 714 0.29 601

----- ----- 1634 D5453 743 1.20

606

----- ----- 1650 D4294 737 1.01 608

----- ----- 1715 ----- -----

631 D4294 706.5 0.06 1720 D5453 653.0 -1.62 634

----- ----- 1724 IP336 710 C 0.17

657 D5453 692 -0.40 1776 ISO8754 686.2 -0.58 663 D5453 675.9 -0.90 1784 ISO8754 720 0.48 671 D5453 707.73 0.10 1798 ----- ----- 732 D4294 695 -0.30 1811 D5453 731.61 0.85 823 D5453 741.1 1.14 1813 D2622 701 -0.11 824 D5453 718 0.42 1833 D4294 745 1.27 851 D2622 713.60 0.28 1842 D5453 690 -0.46 854 D5453 690 -0.46 1883 ----- ----- 862 D2622 700.1 -0.14 1913 D4294 701 -0.11 869 D4294 707.3 0.08 2129 D5453 681.2 -0.74 922 D5453 692.0 -0.40 2130 IP336 830 R(0.01) 3.93 962

----- ----- 9090 ----- -----

963 D4294 703 -0.05




Lab 62 first reported 0.0705 mg/kg Lab 150 first reported 0.0709 mg/kg Lab 177 probably unit error, reported 0.0712 mg/kg Lab 447 measured as 0.068% by equipment, reported in mg/kg Lab 448 first reported 0.0661 mg/kg Lab 1049 first reported 0.0636824 Lab 1121 first reported 0.071 mg/kg Lab 1316 first reported 0.071 mg/kg Lab 1498 first reported 415.1 Lab 1724 first reported 0.071 mg/kg

550

600

650

700

750

800

850

900

1498

1049

1720 175

663

317

2129

1161 496

854

1842 445

657

1587 132

311

732

340

1039

1026 369

1813

1297 963

1417

1428

1081 224

1528 869

150

1182

1316

1064 402

177

333

1616

1191

1062

1784

1079

1585

1109

1650

1011

1634

1833 140

1065

2130 194



Determination of BOCLE on sample #15171; results in mm lab method value mark z(targ) remarks 150 D5001 0.62 -2.17 171 D5001 0.68

0.53

237

----- ----- 334 D5001 0.64 -1.27 496 D5001 0.711 1.92 963 D5001 0.647 -0.96 1016 D5001 0.671 0.12 1064 D5001 0.700 1.43 1081 D5001 0.6585 -0.44 1082 D5001 0.662 -0.28 1191

----- -----

1264 D5001 0.65 -0.82 1316 D5001 0.72 2.32 1318 D5001 0.68 0.53 1395

----- -----

1616 D5001 0.66 -0.37 1724 D5001 0.67 0.08 1833 D5001 0.67 0.08 1913 D5001 0.655 -0.60 9090 D5001 0.667 -0.06

normality OK

n 17

outliers 0

mean (n) 0.668

st.dev. (n) 0.0251

R(calc.) 0.070

R(D5001:10 0.062

R(D5001:10 (full automatic)) : 0.036

(semi-automatic))

0.5

0.55

0.6

0.65

0.7

0.75

150

334

963

1264

1913

1081

1616

1082

9090

1724

1833

1016 171

1318

1064 496

1316



--- empty page ---



Determination of Particle Size Distribution on sample #15172 acc. to IP564; results in parts/mL

Lab 1299 excluded, used method IP577 Labs 1049&1316 are excluded, see paragraph 4.1 for more details

lab ≥4 µm mark ≥6

µm mark ≥14 µm mark ≥21


µm mark

140 ----- ----- ----- ----- ----- ----- 150 2418.0 645.4 44.0 9.3 3.9 1.4 171 ----- ----- ----- ----- ----- ----- 230 4688.4 929.4 23.4 6.4 3.3 1.4 237 ----- ----- ----- ----- ----- ----- 253 3647.6 960.7 48.4 16.4 6.0 2.3 311 ----- ----- ----- ----- ----- ----- 323 ----- ----- ----- ----- ----- ----- 333 ----- ----- ----- ----- ----- ----- 334 ----- ----- ----- ----- ----- ----- 335 ----- ----- ----- ----- ----- ----- 369 2928.7 682.4 22.6 6.4 3.1 1.4 372 4128 955 29 5.6 2.6 0.9 445 ----- ----- ----- ----- ----- ----- 447 4623.4 1025.6 38.3 8.7 3.5 1.1 453 4460.6 915.3 33.7 10.0 4.2 1.2 496 3570.7 649.3 17.7 3.3 1.5 0.7 657 ----- ----- ----- ----- ----- ----- 823 ----- ----- ----- ----- ----- ----- 824 ----- ----- ----- ----- ----- ----- 851 ----- ----- ----- ----- ----- ----- 922 ----- ----- ----- ----- ----- ----- 963 7193.4 1589.3 54.9 11.4 5.3 2.0 974 4963 1142 56 22 D(5) 16 G(1) 8 D(1) 1011 ----- ----- ----- ----- ----- ----- 1016 ----- ----- ----- ----- ----- ----- 1026 ----- ----- ----- ----- ----- ----- 1039 ----- ----- ----- ----- ----- ----- 1049 2837.3 ex 559.0 ex 160.2 D(1) 156.6 D(1) 156.3 D(1) 155.8 D(1) 1062 ----- ----- ----- ----- ----- ----- 1064 ----- ----- ----- ----- ----- ----- 1065 7952.7 D(5) 1467.1 46.8 9.9 4.0 1.4 1079 ----- ----- ----- ----- ----- ----- 1081 3824 784 14 1.6 0.8 0.4 1082 ----- ----- ----- ----- ----- ----- 1097 4363.8 883.0 25.7 5.5 2.5 0.8 1109 ----- ----- ----- ----- ----- ----- 1191 1379 352 5 0.4 0.2 0 1200 ----- ----- ----- ----- ----- ----- 1201 ----- ----- ----- ----- ----- ----- 1299 11315.9 ex 2714.7 ex 128.4 ex 36.0 ex 24.2 ex 13.3 ex 1316 9071 ex 2095 G(5) 118 G(1) 34 G(1) 22 ex 11 ex 1395 ----- ----- ----- ----- ----- ----- 1402 ----- ----- ----- ----- ----- ----- 1585 ----- ----- ----- ----- ----- ----- 1587 2302.6 621.7 29.9 7.1 2.9 0.7 1610 ----- ----- ----- ----- ----- ----- 1616 5040.9 1068.4 39.5 10.5 5.0 1.9 1634 ----- ----- ----- ----- ----- ----- 1724 ----- ----- ----- ----- ----- ----- 1776 4403.8 966.5 37.4 10.5 5.1 1.9 1811 ----- ----- ----- ----- ----- ----- 1813 ----- ----- ----- ----- ----- ----- 1833 ----- ----- ----- ----- ----- ----- 1913 4188.6 887.1 34.8 9.9 6.0 2.1 2130 4237.0 920.4 34.2 10.2 5.0 2.0 9090 ----- ----- ----- ----- ----- -----

normality suspect suspect OK OK OK OK n 18 19 19 18 18 18 outliers 1+3ex 1+2ex 2+1ex 3+1ex 2+2ex 2+2 mean (n) 4020.08 918.14 33.44 7.95 3.60 1.311 st.dev. (n) 1270.022 286.018 13.554 3.847 1.681 0.6443 R(calc.) 3556.06 800.85 37.95 10.77 4.71 1.804 R(IP564:13) 897.59 350.46 26.32 10.08 4.83 2.170



Particle size ≥ 4 µm Particle size ≥ 6 µm Particle size ≥ 14 µm Particle size ≥ 21 µm Particle size ≥ 25 µm Particle size ≥ 30 µm

0

2000

4000

6000

8000

10000

12000

1191

1587 150

1049 369

496

253

1081 372

1913

2130

1097

1776 453

447

230

974

1616 963

1065

1316

1299

0

500

1000

1500

2000

2500

3000

1191

1049

1587 150

496

369

1081

1097

1913 453

2130 230

372

253

1776 447

1616 974

1065 963

1316

1299

0

20

40

60

80

100

120

140

160

180

1191

1081 496

369

230

1097 372

1587 453

2130

1913

1776 447

1616 150

1065 253

963

974

1316

1299

1049

0

10

20

30

40

50

60

1191

1081 496

1097 372

230

369

1587 447

150

1065

1913 453

2130

1616

1776 963

253

974

1316

1299

1049

0

5

10

15

20

25

30

1191

1081 496

1097 372

1587 369

230

447

150

1065 453

1616

2130

1776 963

253

1913 974

1316

1299

1049

0

2

4

6

8

10

12

14

16

18

20

1191

1081 496

1587

1097 372

447

453

369

150

230

1065

1616

1776 963

2130

1913 253

974

1316

1299

1049



z-scores of Particle Size Distribution on sample #15172 acc. to IP564; results in parts/mL

lab ≥4 µm ≥6 µm ≥14 µm ≥21 µm ≥25 µm ≥30 µm 140 ----- ----- ----- ----- ----- ----- 150 -5.00 -2.18 1.12 0.37 0.17 0.11 171 ----- ----- ----- ----- ----- ----- 230 2.08 0.09 -1.07 -0.43 -0.18 0.11 237 ----- ----- ----- ----- ----- ----- 253 -1.16 0.34 1.59 2.35 1.39 1.28 311 ----- ----- ----- ----- ----- ----- 323 ----- ----- ----- ----- ----- ----- 333 ----- ----- ----- ----- ----- ----- 334 ----- ----- ----- ----- ----- ----- 335 ----- ----- ----- ----- ----- ----- 369 -3.40 -1.88 -1.15 -0.43 -0.29 0.11 372 0.34 0.29 -0.47 -0.65 -0.58 -0.53 445 ----- ----- ----- ----- ----- ----- 447 1.88 0.86 0.52 0.21 -0.06 -0.27 453 1.37 -0.02 0.03 0.57 0.34 -0.14 496 -1.40 -2.15 -1.67 -1.29 -1.22 -0.79 657 ----- ----- ----- ----- ----- ----- 823 ----- ----- ----- ----- ----- ----- 824 ----- ----- ----- ----- ----- ----- 851 ----- ----- ----- ----- ----- ----- 922 ----- ----- ----- ----- ----- ----- 963 9.90 5.36 2.28 0.96 0.98 0.89 974 2.94 1.79 2.40 3.90 7.19 8.63 1011 ----- ----- ----- ----- ----- ----- 1016 ----- ----- ----- ----- ----- ----- 1026 ----- ----- ----- ----- ----- ----- 1039 ----- ----- ----- ----- ----- ----- 1049 -3.69 -2.87 13.48 41.29 88.56 199.35 1062 ----- ----- ----- ----- ----- ----- 1064 ----- ----- ----- ----- ----- ----- 1065 12.27 4.39 1.42 0.54 0.23 0.11 1079 ----- ----- ----- ----- ----- ----- 1081 -0.61 -1.07 -2.07 -1.76 -1.63 -1.18 1082 ----- ----- ----- ----- ----- ----- 1097 1.07 -0.28 -0.82 -0.68 -0.64 -0.66 1109 ----- ----- ----- ----- ----- ----- 1191 -8.24 -4.52 -3.02 -2.10 -1.98 -1.69 1200 ----- ----- ----- ----- ----- ----- 1201 ----- ----- ----- ----- ----- ----- 1299 22.76 14.35 10.10 7.79 11.94 15.47 1316 15.76 9.40 8.99 7.24 10.67 12.50 1395 ----- ----- ----- ----- ----- ----- 1402 ----- ----- ----- ----- ----- ----- 1585 ----- ----- ----- ----- ----- ----- 1587 -5.36 -2.37 -0.38 -0.24 -0.41 -0.79 1610 ----- ----- ----- ----- ----- ----- 1616 3.18 1.20 0.64 0.71 0.81 0.76 1634 ----- ----- ----- ----- ----- ----- 1724 ----- ----- ----- ----- ----- ----- 1776 1.20 0.39 0.42 0.71 0.87 0.76 1811 ----- ----- ----- ----- ----- ----- 1813 ----- ----- ----- ----- ----- ----- 1833 ----- ----- ----- ----- ----- ----- 1913 0.53 -0.25 0.14 0.54 1.39 1.02 2130 0.68 0.02 0.08 0.62 0.81 0.89 9090 ----- ----- ----- ----- ----- -----



--- empty page ---



Determination of Particle Size Distribution on sample #15172 acc. to IP565; results in parts/mL

Lab 1724 first reported 7801.1; 1864.2; 107,4; 28.1;13.5; 4.6 for ≥4 µm; ≥6 µm; ≥14 µm; ≥21 µm; ≥25 µm; ≥30 µm respectively Lab 1811 first reported 442.8; 60.4; 3.7;0.7 for ≥4 µm; ≥6 µm; ≥14 µm; ≥21 µm respectively Lab 372 gave remark: “RR sample visually inspected and contained different kinds of impurities. This can influence the reproducibility” Lab 1081 gave remark: “for our analysis we need 800ml, but we got 500ml. This can influence the precision” Labs 1064&1585 are excluded; see paragraph 4.1 for more details

lab ≥4 µm mark ≥6



µm mark

140 ----- ----- ----- ----- ----- ----- 150 ----- ----- ----- ----- ----- ----- 171 7878 1854 51 9 4 1 230 ----- ----- ----- ----- ----- ----- 237 ----- ----- ----- ----- ----- ----- 253 ----- ----- ----- ----- ----- ----- 311 7549 1836 68 14 7 3 323 ----- ----- ----- ----- ----- ----- 333 7041 1587 44 11 6 3 334 7735 1685 40 8 4 1 335 7043 1362 43 13 6 3 369 ----- ----- ----- ----- ----- ----- 372 ----- ----- ----- ----- ----- ----- 445 4693.9 936.3 38.6 12.4 6.3 2.3 447 ----- ----- ----- ----- ----- ----- 453 ----- ----- ----- ----- ----- ----- 496 ----- ----- ----- ----- ----- ----- 657 ----- ----- ----- ----- ----- ----- 823 8012.8 1876.3 62.1 11.1 5.5 2.7 824 ----- ----- ----- ----- ----- ----- 851 ----- ----- ----- ----- ----- ----- 922 7219.0 1689.7 26.7 4.6 1.9 0.7 963 ----- ----- ----- ----- ----- ----- 974 ----- ----- ----- ----- ----- ----- 1011 6086.8 1335.6 51.5 10.6 4.8 2.0 1016 7327.6 1643.9 45.5 9.8 4.0 1.6 1026 7752 1739.8 49 9 4 2 1039 5878 1386 38 6 2 1 1049 ----- ----- ----- ----- ----- ----- 1062 6808 1430 31.0 4.3 1.7 0.7 1064 5347.1 ex 1045.8 ex 57.7 ex 45.0 R(1) 44.3 R(1) 43.9 R(1) 1065 ----- ----- ----- ----- ----- ----- 1079 8303.4 1633.5 53.4 14.2 8.3 4.6 1081 ----- ----- ----- ----- ----- ----- 1082 ----- ----- ----- ----- ----- ----- 1097 ----- ----- ----- ----- ----- ----- 1109 7239.8 1882.2 56.4 11.3 5.1 2.0 1191 ----- ----- ----- ----- ----- ----- 1200 3641.8 R(5) 1220.4 27.7 4.0 1.3 0.5 1201 7926.0 1533.3 46.6 9.0 3.4 0.9 1299 ----- ----- ----- ----- ----- ----- 1316 ----- ----- ----- ----- ----- ----- 1395 ----- ----- ----- ----- ----- ----- 1402 ----- ----- ----- ----- ----- ----- 1585 7269.9 ex 1648.6 ex 82.0 ex 24.4 R(5) 13.5 R(5) 8.1 R(1) 1587 ----- ----- ----- ----- ----- ----- 1610 8914.6 2071.0 89.8 R(5) 19.0 8.8 2.8 1616 ----- ----- ----- ----- ----- ----- 1634 ----- ----- ----- ----- ----- ----- 1724 ----- W ----- W ----- W ----- W ----- W ----- W 1776 ----- ----- ----- ----- ----- ----- 1811 7523 C 1830 C 56 C 9.3 C 0.2 0.1 1813 5586.7 1402.4 64.9 14.3 6.4 3.7 1833 7139.3 1638.4 58.2 11.3 4.8 1.8 1913 ----- ----- ----- ----- ----- ----- 2130 ----- ----- ----- ----- ----- ----- 9090 7617.9 1645.6 51.7 10.6 5 1.6

normality suspect OK OK OK OK OK n 21 22 21 22 22 22 outliers 1+2ex 0+2ex 1+2ex 2 2 2 mean (n) 7203.6 1600.8 47.78 10.26 4.568 1.909 st.dev. (n) 971.90 260.20 11.497 3.611 2.2255 1.1443 R(calc.) 2721.3 728.6 32.19 10.11 6.231 3.204 R(IP565:13) 916.6 418.7 40.09 11.10 5.974 3.079



Particle size ≥ 4 µm Particle size ≥ 6 µm

Particle size ≥ 14 µm Particle size ≥ 21 µm Particle size ≥ 25 µm Particle size ≥ 30 µm

0

5

10

15

20

25

30

35

40

45

50

1200

1062 922

1039 334

171

1026

1201

1811

1016

1011

9090 333

823

1109

1833 445

335

311

1079

1813

1610

1585

1064

0

2

4

6

8

10

12

14

1811

1200

1062 922

1039

1201 171

334

1026

1016

1011

1833

9090

1109 823

335

333

445

1813 311

1079

1610

1585

1064

0

2

4

6

8

10

12

14

1811

1200 922

1062

1201 171

1039 334

1016

9090

1833

1026

1011

1109 445

823

1610 311

335

333

1813

1079

1585

1064

0

1000

2000

3000

4000

5000

6000

7000

8000

9000

10000

1200 445

1064

1813

1039

1011

1062 333

335

1833 922

1109

1585

1016

1811 311

9090 334

1026 171

1201 823

1079

1610

0

500

1000

1500

2000

2500

445

1064

1200

1011 335

1039

1813

1062

1201 333

1079

1833

1016

9090

1585 334

922

1026

1811 311

171

823

1109

1610

0

10

20

30

40

50

60

70

80

90

100

922

1200

1062

1039 445

334

335

333

1016

1201

1026 171

1011

9090

1079

1811

1109

1064

1833 823

1813 311

1585

1610



z-scores of Particle Size Distribution on sample #15172 acc. to IP565; results in parts/mL

lab ≥4 µm ≥6 µm ≥14 µm ≥21 µm ≥25 µm ≥30 µm 140 ----- ----- ----- ----- ----- ----- 150 ----- ----- ----- ----- ----- ----- 171 2.06 1.69 0.23 -0.32 -0.27 -0.83 230 ----- ----- ----- ----- ----- ----- 237 ----- ----- ----- ----- ----- ----- 253 ----- ----- ----- ----- ----- ----- 311 1.06 1.57 1.41 0.94 1.14 0.99 323 ----- ----- ----- ----- ----- ----- 333 -0.50 -0.09 -0.26 0.19 0.67 0.99 334 1.62 0.56 -0.54 -0.57 -0.27 -0.83 335 -0.49 -1.60 -0.33 0.69 0.67 0.99 369 ----- ----- ----- ----- ----- ----- 372 ----- ----- ----- ----- ----- ----- 445 -7.67 -4.44 -0.64 0.54 0.81 0.36 447 ----- ----- ----- ----- ----- ----- 453 ----- ----- ----- ----- ----- ----- 496 ----- ----- ----- ----- ----- ----- 657 ----- ----- ----- ----- ----- ----- 823 2.47 1.84 1.00 0.21 0.44 0.72 824 ----- ----- ----- ----- ----- ----- 851 ----- ----- ----- ----- ----- ----- 922 0.05 0.59 -1.47 -1.43 -1.25 -1.10 963 ----- ----- ----- ----- ----- ----- 974 ----- ----- ----- ----- ----- ----- 1011 -3.41 -1.77 0.26 0.08 0.11 0.08 1016 0.38 0.29 -0.16 -0.12 -0.27 -0.28 1026 1.68 0.93 0.09 -0.32 -0.27 0.08 1039 -4.05 -1.44 -0.68 -1.08 -1.20 -0.83 1049 ----- ----- ----- ----- ----- ----- 1062 -1.21 -1.14 -1.17 -1.50 -1.34 -1.10 1064 -5.67 -3.71 0.69 8.76 18.62 38.19 1065 ----- ----- ----- ----- ----- ----- 1079 3.36 0.22 0.39 0.99 1.75 2.45 1081 ----- ----- ----- ----- ----- ----- 1082 ----- ----- ----- ----- ----- ----- 1097 ----- ----- ----- ----- ----- ----- 1109 0.11 1.88 0.60 0.26 0.25 0.08 1191 ----- ----- ----- ----- ----- ----- 1200 -10.88 -2.54 -1.40 -1.58 -1.53 -1.28 1201 2.21 -0.45 -0.08 -0.32 -0.55 -0.92 1299 ----- ----- ----- ----- ----- ----- 1316 ----- ----- ----- ----- ----- ----- 1395 ----- ----- ----- ----- ----- ----- 1402 ----- ----- ----- ----- ----- ----- 1585 0.20 0.32 2.39 3.57 4.19 5.63 1587 ----- ----- ----- ----- ----- ----- 1610 5.23 3.14 2.94 2.20 1.98 0.81 1616 ----- ----- ----- ----- ----- ----- 1634 ----- ----- ----- ----- ----- ----- 1724 ----- ----- ----- ----- ----- ----- 1776 ----- ----- ----- ----- ----- ----- 1811 0.98 1.53 0.57 -0.24 -2.05 -1.65 1813 -4.94 -1.33 1.20 1.02 0.86 1.63 1833 -0.20 0.25 0.73 0.26 0.11 -0.10 1913 ----- ----- ----- ----- ----- ----- 2130 ----- ----- ----- ----- ----- ----- 9090 1.27 0.30 0.27 0.08 0.20 -0.28



--- empty page ---



Determination of FAME on sample #15173; results in mg/kg lab method value mark z(targ) remarks 140

----- -----

171 IP585 11.4 0.18 230 IP585 10.97 -0.15 237

----- -----

311 IP585 14 2.17 317 IP585 12.0 0.63 323 IP585 10.0 -0.90 333 IP585 9.9 -0.97 334 IP585 11.5 0.25 335 IP585 10.2 -0.74 336 IP585 8.7 -1.89 369 IP583 16 ex 3.70 see paragraph 4.1 445

----- -----

447 IP585 7.257 -3.00 448 IP585 12.289 C 0.86 first reported 38.664 453 IP590 9.95 -0.94 473 IP585 17.87 R(0.05) 5.13 496 IP585 11.11 -0.05 657 IP585 12.2 0.79 823 IP585 12.0 0.63 824

----- -----

851 IP583 18.44 ex 5.57 see paragraph 4.1 1011

----- -----

1016 IP585 12.67 1.15 1062 in house 2.00 R(0.05) -7.03 1064 IP585 10.7 -0.36 1065 IP583/D7797 19.50 ex 6.38 see paragraph 4.1 1081 IP585 12.3 0.86 1082 IP585 11.395 0.17 1095 IP585 9.9 -0.97 1109

----- -----

1161

----- ----- 1191

----- -----

1201 IP585 8.3 -2.20 1299 IP585 11.3 0.10 1316 IP585 17.6 R(0.05) 4.92 1318 IP585 13.05 1.44 1402

----- -----

1610 IP590 < 3 ----- false negative 1634 IP585 12.98 1.39 1724

----- -----

1833 IP590 10.92 -0.19 1842

----- -----

2129 IP590 14.44 2.50 2130 IP590 10.2 -0.74

IP585 only IP590 only

normality OK

OK not applicable

n 27

23 4

outliers 3+3ex Spike

2 0

mean (n) 11.17 7.0

Recovery <160% 11.14 11.38

st.dev. (n) 1.651

1.619 2.083

R(calc.) 4.62

4.53 5.83

R(IP585:10) 3.65

3.65 2.96 (IP590:10)



All data Method IP585 only Method IP590 only

0

5

10

15

20

25

1062 447

1201 336

333

1095 453

323

335

2130

1064

1833 230

496

1299

1082 171

334

317

823

657

448

1081

1016

1634

1318 311

2129 369

1316 473

851

1065

0

5

10

15

20

25

1062 447

1201 336

333

1095 453

323

335

2130

1064

1833 230

496

1299

1082 171

334

317

823

657

448

1081

1016

1634

1318 311

2129 369

1316 473

851

1065

0

5

10

15

20

25

1062 447

1201 336

333

1095 453

323

335

2130

1064

1833 230

496

1299

1082 171

334

317

823

657

448

1081

1016

1634

1318 311

2129 369

1316 473

851

1065



Determination of FAME on sample #15174; results in mg/kg lab method value mark z(targ) remarks 140

----- -----

171 IP585 46.9 -0.48 230 IP585 44.27 -1.03 237

----- -----

311 IP585 55 1.21 317 IP585 50.8 0.33 323 IP585 36.7 -2.60 333 IP585 43.2 -1.25 334 IP585 48.7 -0.11 335 IP585 47 -0.46 336 IP585 42.9 -1.31 369 IP583 57.3 1.68 445

----- -----

447

----- ----- 448 IP585 56.023 C 1.42 first reported 25.868 453 IP590 31.5 -3.68 473 IP585 57.44 1.71 496 IP585 91.11 C,R(0.01) 8.71 first reported 86.1 657 IP585 47.5 -0.35 823 IP585 41.3 -1.64 824

----- -----

851 IP583 56.23 1.46 1011

----- -----

1016 IP585 47.30 -0.40 1062 in house 44.00 -1.08 1064 IP585 52.7 0.73 1065 IP583/D7797 54.10 1.02 1081 IP585 54.4 1.08 1082 IP585 48.82 -0.08 1095 IP585 44.0 -1.08 IP585 only 1109

----- ----- OK

1161

----- ----- 23 1191

----- ----- 1

1201 IP585 49.8 0.12 49.07 1299 IP585 45.8 -0.71 5.807 1316 IP585 54.3 1.06 16.26 1318 IP585 52.74 0.74 13.43 1402

----- -----

1610

----- ----- 1634 IP585 61.00 2.45 1724

----- -----

1833

----- ----- 1842

----- -----

2129 IP590 57.03 1.63 2130 IP590 47.4 C -0.38 first reported 16.3

IP585 only IP583 only IP590 only

normality OK

OK not applicable not applicable

n 30

23 3 3

outliers 1 Spike

1 0 0

mean (n) 49.20 52.0 Receovery <95% 49.07 55.88 45.31

st.dev. (n) 6.660

5.807 1.629 12.893

R(calc.) 18.65

16.26 4.56 36.10

R(IP585:10) 13.46

13.43 4.50 (IP583:10) 10.48 (IP590:10)



All methods Method IP585 only Method IP583 only Method IP590 only

0

10

20

30

40

50

60

70

80

90

100

453

323

823

336

333

1062

1095

230

1299

171

335

1016

2130

657

334

1082

1201

317

1064

1318

1065

1316

1081

311

448

851

2129

369

473

1634

496

0

10

20

30

40

50

60

70

80

90

100

453

323

823

336

333

1062

1095

230

1299

171

335

1016

2130

657

334

1082

1201

317

1064

1318

1065

1316

1081

311

448

851

2129

369

473

1634

496

0

10

20

30

40

50

60

70

80

90

100

453

323

823

336

333

1062

1095

230

1299

171

335

1016

2130

657

334

1082

1201

317

1064

1318

1065

1316

1081

311

448

851

2129

369

473

1634

496

0

10

20

30

40

50

60

70

80

90

100

453

323

823

336

333

1062

1095

230

1299

171

335

1016

2130

657

334

1082

1201

317

1064

1318

1065

1316

1081

311

448

851

2129

369

473

1634

496



APPENDIX 2: Number of participants per country

1 lab in AFGHANISTAN 3 labs in MALAYSIA 2 labs in AUSTRALIA 1 lab in MAURITIUS 1 lab in AZERBAIJAN 1 lab in MOZAMBIQUE

5 labs in BELGIUM 10 labs in NETHERLANDS 1 lab in BULGARIA 2 labs in NIGERIA

2 labs in CANADA 2 labs in NORWAY 1 lab in CHILE 1 lab in PAKISTAN

6 labs in CHINA, People's Republic 2 labs in PHILIPPINES 1 lab in COTE D'IVOIRE 1 lab in POLAND 1 lab in CROATIA 3 labs in PORTUGAL 1 lab in CYPRUS 2 labs in QATAR 1 lab in CZECH REPUBLIC 2 labs in ROMANIA 1 lab in DJIBOUTI 1 lab in RUSSIAN FEDERATION 1 lab in EGYPT 3 labs in SAUDI ARABIA 1 lab in ESTONIA 1 lab in SENEGAL

2 labs in FINLAND 1 lab in SINGAPORE 6 labs in FRANCE 1 lab in SLOVENIA 2 labs in GEORGIA 1 lab in SOUTH AFRICA 2 labs in GERMANY 2 labs in SOUTH KOREA 2 labs in GREECE 2 labs in SPAIN 1 lab in GUAM 2 labs in SUDAN 1 lab in GUINEA REPUBLIC 5 labs in SWEDEN 1 lab in HONG KONG 1 lab in TANZANIA

2 labs in HUNGARY 1 lab in THAILAND 1 lab in IRELAND 1 lab in TOGO 1 lab in ISRAEL 1 lab in TUNISIA 1 lab in KAZAKHSTAN 4 labs in TURKEY

2 labs in KENYA 1 lab in TURKMENISTAN 2 labs in LATVIA 2 labs in UNITED ARAB EMIRATES 3 labs in LEBANON 14 labs in UNITED KINGDOM 1 lab in LITHUANIA 11 labs in UNITED STATES OF AMERICA 1 lab in MACEDONIA



APPENDIX 4 Abbreviations D(0.01) or D(1) = outlier in Dixon’s outlier test D(0.05) or D(5) = straggler in Dixon’s outlier test G(0.01) or G(1) = outlier in Grubbs’ outlier test G(0.05) or G(5) = straggler in Grubbs’ outlier test DG(0.01) or DG(1) = outlier in Double Grubbs’ outlier test DG(0.05) or DG(5) = straggler in Double Grubbs’ outlier test R(0.01) or R(1) = outlier in Rosner outlier test R(0.05) or R(5) = straggler in Rosner outlier test ex = excluded from calculations n.a. = not applicable n.e. = not evaluated C = final result after checking of first reported suspect result W = withdrawn on request participant SDS = Safety Data Sheet Literature 1 iis Interlaboratory Studies, Protocol for the Organisation, Statistics & Evaluation, April 2014 2 Defence Standard 91-91, Issue 7 Amendment 3, Publication date 02 February 2015 3 Aviation Fuel Quality Requirements for Jointly Operated Systems (AFQRJOS), Issue 28 March 2015,

Bulletin No. 76. 4 ASTM E178-02 5 ASTM E1301-03 6 ISO 13528-05 7 ISO 5725, parts 1-6, 1994 8 M. Thompson and R. Wood, J. AOAC Int, 76, 926, (1993) 9 W.J. Youden and E.H. Steiner, Statistical Manual of the AOAC, (1975) 10 IP 367/84 11 DIN 38402 T41/42 12 P.L. Davies, Fr. Z. Anal. Chem, 331, 513, (1988) 13 J.N. Miller, Analyst, 118, 455, (1993) 14 Analytical Methods Committee Technical Brief, No. 4 January 2001 15 The Royal Society of Chemistry 2002, Analyst 2002, 127, p. 1359-1364, P.J. Lowthian and M.

Thompson. (see http://www.rsc.org/suppdata/an/b2/b205600n/) 16 Bernard Rosner, Percentage Points for a Generalized ESD Many-Outlier Procedure,Technometrics,

25(2), pp. 165-172, (1983).

Documents

Results of Proficiency Test - Institute for ... · Results of Proficiency Test Jet Fuel A1 . September 2015 . ... (in %M/M and %V/V), ... JFTOT, Kinematic Viscosity at -20°C, Mercaptan