Results of Proficiency Test Jet Fuel A1 March 2008 - iisnl. · PDF fileResults of Proficiency Test Jet Fuel A1 March 2008 ... (20% evaporated), Flash Point, MSEP ... participants reported

Results of Proficiency Test Jet Fuel A1 March 2008 Organised by: Institute for Interlaboratory Studies Spijkenisse, the Netherlands Author: Ing. R.J.Starink Correctors: Dr. R.G. Visser & Ing. S. Lagendijk Report: iis08J01X May 2008

Institute for Interlaboratory Studies Spijkenisse, May 2008

page 2 of 50 Jet Fuel A1: iis08J01X

CONTENTS 1 INTRODUCTION ..................................................................................................................................... 3 2 SET UP..................................................................................................................................................... 3 2.1 ACCREDITATION.................................................................................................................................... 3 2.2 PROTOCOL ............................................................................................................................................. 3 2.3 CONFIDENTIALITY STATEMENT ......................................................................................................... 3 2.4 SAMPLES................................................................................................................................................. 4 2.5 STABILITY OF THE SAMPLES .............................................................................................................. 4 2.6 ANALYSES .............................................................................................................................................. 4 3 RESULTS................................................................................................................................................. 5 3.1 STATISTICS............................................................................................................................................. 5 3.2 GRAPHICS............................................................................................................................................... 6 3.3 Z-SCORES............................................................................................................................................... 6 4 EVALUATION........................................................................................................................................... 6 4.1 EVALUATION PER TEST ....................................................................................................................... 7 4.2 PERFORMANCE EVALUATION FOR THE GROUP OF LABORATORIES ........................................ 9 4.3 COMPARISON WITH RESULTS OF MARCH 2008 WITH PREVIOUS PT’S.................................... 10 Appendices: 1. Data, statistical results and graphic results ........................................................................................... 12 2. Z-scores for manual and automated distillation .................................................................................... 48 3. List of number of participants per country ............................................................................................. 49 4. Abbreviations and literature ................................................................................................................... 50

Spijkenisse, May 2008 Institute for Interlaboratory Studies

Jet Fuel A1: iis08J01X page 3 of 50

1 INTRODUCTION

Since 1995, the Institute for Interlaboratory Studies organises every year proficiency tests for Jet Fuel A1. In the international Interlaboratory study of March 2008, 70 laboratories in 34 different countries have participated. See appendix 3 for a list of participants in alphabetical country order. In this report the results of the proficiency test are presented and discussed.

2 SET UP

The Institute for Interlaboratory Studies (i.i.s.) in Spijkenisse, The Netherlands, was the organiser of this proficiency test. In this round robin it was decided to send 2 identical samples of Jet Fuel (2*1 liter of sample #0816). The samples were meant for the analyses according to the "Aviation Fuel Quality Requirements for Jointly Operated Systems (AFQRSJOS)”, sometimes referred to as the "Joint Fuelling System Check List For Jet A-1”. The participants were requested to report rounded and unrounded results. The unrounded results were preferably used for statistical evaluation.

2.1 ACCREDITATION

The Institute for Interlaboratory Studies in Spijkenisse, the Netherlands, is accredited in agreement with ISO guide 43 and ILAC-G13:2000, (R007), since January 2000, by the Dutch Accreditation Council (Raad voor Accreditatie). This ensures 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 ‘i.i.s. Interlaboratory Studies: Protocol for the Organisation, Statistics and Evaluation’ (i.i.s.-protocol, version 3.0) of November 2003.

2.3 CONFIDENTIALITY STATEMENT

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



2.4 SAMPLES The necessary bulk material was obtained from a German refinery. The approx. 200 litre bulk sample was homogenised and divided over 157 amber glass bottles of one litre with inner and outer caps and labelled #0816. The homogeneity of the subsamples #0816 was checked by the determination of Density in accordance with ASTM D 4052:02e1 on 8 stratified random selected samples.

Sample Density @ 15°C in kg/m3

#0816-1 798.02 #0816-2 798.03 #0816-3 798.02 #0816-4 798.02 #0816-5 798.03 #0816-6 798.03 #0816-7 798.02 #0816-8 798.02

Table 1: homogeneity test of sub samples #0816

From the results in table 1 the repeatability of the results was calculated by multiplication of the standard deviation by 2.8: Density @ 15°C in kg/m3

r (observed) 0.02 reference test D4052:02e1 r (reference test) 0.10

Table 2: repeatability of subsamples #0816

The repeatability of the results for Density was in agreement with the repeatability mentioned in ASTM D4052:02e1. Therefore, homogeneity of the subsamples #0816 was assumed. To each of the participating laboratories 2 bottles (2*1 litre labelled #0816) were sent on February 27, 2008.

2.5 STABILITY OF THE SAMPLES

In order to be sure that the material, which is used in this proficiency test, is stable for the valid period, the stability of the material packed in the amber glass bottles was checked prior to use. The type of bottle was chosen in accordance with ASTM D4306:01.

2.6 ANALYSIS The participants were requested to determine on sample #0816: Aromatics by FIA, Aromatics by HPLC, Colour Saybolt, Density @ 15°C, Distillation (IBP, 10%, 20%, 50%, 90% recovered and FBP), Existent Gum, Flash Point, Freezing Point, JFTOT, Mercaptans, MSEP,



Naphthalenes, Smoke Point, Specific Energy, Total Acidity, Total Sulphur and Viscosity @ -20°C. The analyses should be performed according to the "Aviation Fuel Quality Requirements for Jointly Operated Systems (AFQRSJOS)", 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 some of the required standards, was sent together with each set of samples. Also a letter of instructions and a MSDS were added to the package.

3 RESULTS

During four weeks after sample despatch the results of the individual laboratories were gathered. The original data are tabulated per determination in the appendix of this report. The laboratories are presented by their code numbers. Directly after the deadline, a reminder fax was sent to those laboratories that did not report results at that moment. Shortly after the deadline the available results were screened for suspect data. A result was called suspect in case the Huber Elimination Rule (a robust outlier test) found it to be an outlier. The laboratories that produced these suspect data were asked to check the results. Additional or corrected results are used for data analysis and original results are placed under 'Remarks' in the result tables in appendix 1.

3.1 STATISTICS Statistical calculations were performed as described in the report ‘i.i.s. Interlaboratory Studies: Protocol for the Organisation, Statistics and Evaluation’ (i.i.s.-protocol, version 3.0) of November 2003. For the statistical evaluation the unrounded (when available) figures were used instead of the rounded results. Results reported as '<…' or '>…' were not used in the statistical evaluation First, the normality of the distribution of the various data sets per determination was checked by means of the Lilliefors-test. After removal of outliers this check was repeated. Not all data sets proved to have a normal distribution, in which cases the 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. Outliers are marked by D(0.01) for the Dixon test, by G(0.01) or DG(0.01) for the Grubbs test. Stragglers are marked by D(0.05) for the Dixon test, by G(0.05) or DG(0.05) for the Grubbs test. Both outliers and stragglers were not included in the calculations of averages and standard deviations.



Finally the reproducibilities were calculated from the standard deviations by multiplying them with a factor of 2.8.

3.2 GRAPHICS

In order to visualise the data against the reproducibilities from literature, Gauss plots were made, using the sorted data for one determination (see appendix 1). On the Y-axis the results are plotted. The corresponding laboratory numbers are under the X-axis. A straight line presents the average of the reported data. Two striped lines present the reproducibility limits of the selected standard, calculated as mean ± target reproducibility, parallel to the average line. Outliers and other data, which were excluded from the calculations, are represented as a cross. Accepted data are represented as a triangle. Furthermore, Kernel Density Graphs were made. This is a method for producing a smooth density approximation to a set of data that avoids some problems associated with histograms (see appendix 4; nr.12 and 13)

3.3 Z-SCORES To evaluate the performance of the participating laboratories the z-scores were calculated. As it was decided to evaluate the performance of the participants in this proficiency test (PT) against the literature requirements, e.g. ASTM reproducibilities, the z-scores were calculated using a target standard deviation. This target standard deviation was calculated from the literature reproducibility by division with 2.8. The z-scores were calculated according to: z(target) = (result - average of PT) / target standard deviation The z(target) scores are listed in the result tables in appendix 1. Absolute values for z<2 are very common and absolute values for z>3 are very rare. Therefore the usual interpretation of z-scores is as follows: | z | < 1 good 1 < | z | < 2 satisfactory 2 < | z | < 3 questionable 3 < | z | unsatisfactory

4 EVALUATION In this Interlaboratory study some major problems with customs clearance were encountered during dispatch of the samples to Australia, Croatia, Jordan, Nigeria, Saudi Arabia, Sudan and Tanzania. Of the total of 70 participants, 11 participants did report the results after the deadline for reporting and 4 participants did not report any results at all. The 66 reporting participants sent in 1168 numerical results. Observed were 35 outlying results, which is only 3.0%. In proficiency studies outlier percentages of 3 % - 7.5 % are quite normal.



4.1 EVALUATION PER TEST Not all original data sets proved to have a normal distribution. Abnormal distributions were found for the following determinations on sample #0816: Colour Saybolt, Density, Distillation-automated mode (20% evaporated), Flash Point, MSEP, Naphthalenes, Smoke Point, Specific Energy and Viscosity. Therefore the statistical evaluation for these determinations should be used with care. In this section the results are discussed per test. Since the checklist is continuously updated, the users are advised to monitor the updates. The latest version at the moment is “Issue 22 June 2007”. One must keep in mind that ISO-methods are not mentioned in the “Checklist”. Aromatics by: This determination is not problematic. No results were outside FIA (D1319): the reproducibility limits and the calculated reproducibility is in good

agreement with ASTM D1319:03e1. Aromatics by: Unfortunately, no significant conclusions can be drawn as only four HPLC (D6379): participants reported the results in %V/V as requested in the Checklist

“Issue 22 June 2007”. Three other participants reported the result in %M/M and one participant used ASTM D6591, which is not suitable for this type of Jet Fuel.

Colour Saybolt: This determination is not problematic in this round robin. Obviously this was

an “easy” sample as a large majority of the laboratories reported 30. Only two results were outside the reproducibility limits. The calculated reproducibility is, after rejection of the statistical outliers, in agreement with the requirements of ASTM D156:07a.

Density: This determination is not problematic. Only two results were outside the

reproducibility limits and the calculated reproducibility is, after rejection of the statistical outliers, in good agreement with the requirements of ASTM D4052:02e1.

Distillation: The automated method is not problematic at all. In total only one result was

outside the reproducibility limits. All calculated reproducibilities are in good agreement with the requirements of ASTM D86:07b (automated).

The manual method is somewhat problematic. In total three results were outside the reproducibility limits. None of the calculated reproducibilities is in agreement with the requirements of ASTM D86:07b (manual). The low number of results may partly explain the large spread.

Existent Gum: No analytical problems were observed. No results were outside the

reproducibility limits and the calculated reproducibility is, after rejection of the statistical outlier, in good agreement with ASTM D381:04e1. When the results for air and steam were evaluated separately, the calculated R (air) is larger then the calculated R (steam). However, both calculated



reproducibilities are in good agreement with the requirements of ASTM D381:04e1.

Flash Point: This determination is problematic. Eight results were outside the strict

reproducibility limits of IP170. The calculated reproducibility is, after rejection of the statistical outliers, not at all in agreement with the requirements of IP170:99. When the results for IP170 were evaluated separately, the reproducibility is still not in agreement with the requirements of the standard.

Four laboratories used ASTM D93, a method that is not mentioned in the Joint Fuelling System Checklist and this method gives a much higher Flash Point. These four results were excluded.

When the results for ASTM D56 were evaluated separately, the reproducibility is in good agreement with the requirements of the standard.

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

reproducibility limits and the calculated reproducibility is in good agreement with the requirements of ASTM D2386:06. When the results for ASTM D2386 (manual method), D7153 (automated method) and D5972 (automated method) were evaluated separately, the calculated reproducibilities of the ASTM D7153 and D5972 results are somewhat larger then the more strict requirements of the respective standards. The spread found for the ASTM D2386 results is within the requirments of the standard.

JFTOT: Some analytical problems have been observed. Three laboratories reported

a higher volume than the maximum allowed (450 ± 45 mL may be pumped in a valid test, see ASTM D 3241:06-B table 2). It should be noted that a pumped volume higher than 495 mL or below 405 mL means that the test is not performed correctly and results obtained are suspect.

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

reproducibility limits. The calculated reproducibility is, after rejection of the statistical outlier, in agreement with the requirements of ASTM D3227:04a.

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

reproducibility limits. The calculated reproducibility is, after rejection of the statistical outlier, in agreement with the requirements of ASTM D3948:07.

Naphthalenes: This determination is very problematic at this low level. Nine results were

outside the reproducibility limits. The calculated reproducibility of the group is, after rejection of the statistical outliers, not at all in agreement with the requirements of ASTM D1840:07 (procedure A and B).



Smoke Point: This determination is not problematic. Only two results were outside the reproducibility limits. The calculated reproducibility is, after rejection of the statistical outliers, in full agreement with the requirements of ASTM D1322:02e1.

Specific Energy: This determination is very problematic. Four results were outside the

reproducibility limits. The calculated reproducibility is, after rejection of the statistical outlier, in agreement with the requirements of ASTM D3338:05.

Total Acidity: This determination is problematic. Only two results were outside the

reproducibility limits. However, the calculated reproducibility is, after rejection of the statistical outliers, not in agreement with the reproducibility of ASTM D3242:07. When the data for purged with N2 were evaluated separately, the calculated reproducibility is not different and therefore also not in agreement with the requirements of ASTM D3242:07. Purging with nitrogen and the use of a blank determination on the titration solvent are mandatory to avoid false high results. Note that ISO6618 is not suitable/not intended for Jet Fuel and is therefore excluded.

Total Sulphur: This determination is problematic at the very low level of Sulphur present in

this sample (1.4 mg/kg). Thirteen results were outside the reproducibility limits. The calculated reproducibility is, after rejection of the statistical outliers, not at all in agreement with the requirements of ASTM D5453:08a (application range 1.0 – 8000 mg/kg). When the results for ASTM D 5453 were evaluated separately, the calculated reproducibility is not different and therefore still not meets the requirements of ASTM D5453:08a.

Viscosity: This determination is very problematic. Seven results were outside the reproducibility limits. The calculated reproducibility is, even after rejection of the statistical outliers, not in agreement with the requirements of ASTM D445:06. When the results for ASTM D445 (manual) were evaluated separately, the calculated reproducibility is somewhat smaller but still not in agreement with the limits of the respective standard. As this determination was also problematic in previous Jet Fuel round robins, it is strongly advised to follow the Viscosity @ -20°C determination according ASTM D445 very accurately, especially temperature control and calibration of the viscometer tubes.

4.2 PERFORMANCE EVALUATION FOR THE GROUP OF LABORATORIES

A comparison has been made between the reproducibility as declared by the relevant standard and the reproducibility as found for the group of participating laboratories that participated. The reproducibilities derived from literature standards (in casu ASTM standards) and the calculated reproducibilities of sample #0816 are compared in the next table.



Parameter unit n Average 2.8 * sd R (lit)

Aromatics (D1319) % V/V 45 13.43 2.29 3.70 Aromatics (Total) (D6379) % V/V 8 15.00 6.69 unknown Colour Saybolt 48 29.8 1.5 2.0 Density at 15°C kg/m3 60 798.04 0.29 0.50 Initial Boiling Point (auto) oC 56 158.06 6.87 8.50 10% recovered (auto) oC 55 176.62 2.67 6.16 20% recovered (auto) oC 56 181.99 2.24 4.75 50% recovered (auto) oC 56 195.26 2.12 5.38 90% recovered (auto) oC 55 225.76 3.33 4.62 Final Boiling Point (auto) oC 53 246.81 3.68 10.50 Initial Boiling Point (manual) oC 7 156.25 8.83 4.59 10% recovered (manual) oC 7 175.51 4.98 3.46 20% recovered (manual) oC 7 181.14 4.86 2.42 50% recovered (manual) oC 7 194.18 5.02 2.62 90% recovered (manual) oC 7 224.27 6.19 3.17 Final Boiling Point (manual) oC 7 245.63 10.27 4.00 Existent Gum mg/100mL 32 0.52 0.82 1.49 Flash Point oC 58 45.19 2.46 1.50 Freezing Point oC 56 -57.62 1.70 2.50 Mercaptan Sulphur % M/M 31 0.00014 0.00027 0.00032 MSEP rating 50 96.29 4.87 5.94 Naphthalenes % V/V 32 0.138 0.054 0.034 Smoke Point mm 46 25.43 2.95 3.00 Specific Energy MJ/kg 35 43.3513 0.0670 0.0460 Total Acidity mg KOH/g 38 0.00141 0.00192 0.00153 Total Sulphur mg/kg 32 1.35 2.05 0.73 Viscosity @ -20°C cSt 40 3.8390 0.0801 0.0729

Table 4: comparison of the observed and target reproducibilities

Without further statistical calculations it can be concluded that for some tests there is a not 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 MARCH 2008 WITH PREVIOUS PT’S

March 2008

September 2007

March 2007

September 2006

Number of reporting labs 66 113 62 96 Number of results reported 1168 2102 1180 1703

Statistical outliers 35 74 66 40 Percentage outliers 3.0% 3.5% 5.6% 2.3%

Table 5: Comparison with previous proficiency tests

In proficiency tests outlier percentages of 3 % - 7.5 % are quite normal.



The performance of the determinations of the proficiency tests was compared against the requirements of the respective standards. The conclusions are given the following table: Parameter March

2008 September

2007 March 2007

September 2006

Aromatics (D1319) ++ ++ ++ +/- Aromatics, Total (D6379) n.e. -- -- -- Colour Saybolt ++ + ++ -- Density at 15oC ++ ++ ++ ++ Distillation automated ++ ++ ++ ++ Distillation manual -- -- n.e. -- Existent Gum ++ ++ ++ ++ Flash Point -- -- -- -- Freezing Point ++ + + ++ Mercaptan Sulphur + + + + MSEP + + ++ + Naphthalenes -- - -- + Smoke Point + - -- - Specific Energy -- + ++ -- Total Acidity -- -- -- -- Total Sulphur -- -- -- + Viscosity @ -20°C -- -- -- --

Table 6: 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.d.: not determined n.e.: not evaluated



APPENDIX 1 Determination of Aromatics by FIA (ASTM D 1319) on sample #0816; results in %V/V

lab method value mark z(targ) remarks 140 ----- ----- 171 D1319 11.8 -1.23 177 D1319 12.8 -0.48 192 D1319 15.05 1.23 194 ----- ----- 224 ----- ----- 225 D1319 14.793 1.03 237 ----- ----- 254 D1319 12.82 -0.46 256 ----- ----- 311 D1319 14.5 0.81 312 D1319 13.13 -0.23 317 ----- ----- 323 D1319 13.7 0.21 334 ----- ----- 340 D1319 13.31 -0.09 399 D1319 14.60 0.89 447 D1319 12.6 -0.63 615 D1319 12.37 -0.80 671 D1319 14.7 0.96 851 ----- ----- 1011 D1319 13.15 -0.21 1017 ----- ----- 1021 D1319 13.6 0.13 1026 ----- ----- 1032 D1319 13.28 -0.11 1034 D1319 13.19 -0.18 1038 ----- ----- 1039 ----- ----- 1049 D1319 12.64 -0.60 1059 D1319 13.3 -0.10 1062 D1319 13.5 0.05 1064 D1319 13.65 0.17 1079 D1319 13.37 -0.04 1081 D1319 11.9 -1.16 1082 D1319 13.32 -0.08 1097 D1319 13.14 -0.22 1105 D1319 13.10 -0.25 1108 ----- ----- 1109 D1319 13.00 -0.32 1138 ----- ----- 1140 ----- ----- 1203 D1319 14.3 0.66 1318 ----- ----- 1402 D1319 13.46 0.02 1414 ----- ----- 1428 D1319 13.19 -0.18 1528 D1319 13.82 0.30 1531 ----- ----- 1600 ----- ----- 1610 D1319 11.7 -1.31 1613 D1319 13.93 0.38 1634 ----- ----- 1635 D1319 14.0 C 0.43 First reported 9.0 1636 D1319 13.17 -0.20 1650 D1319 13.7 0.21 1651 ----- ----- 1657 ----- ----- 1715 ----- ----- 1720 D1319 13.7 0.21 1730 ----- ----- 1810 D1319 12.5 -0.70 1811 D1319 12.9 -0.40 1833 D1319 12.9 -0.40 1842 IP156 13.6 0.13 1913 D1319 13.24 -0.14 1939 ----- ----- 2130 IP156 13.7 0.21 2133 D1319 15.17 1.32 2136 D1319 15.00 1.19



normality OK n 45 outliers 0 mean (n) 13.43 st.dev. (n) 0.818 R(calc.) 2.29 R(D1319:03e1) 3.70

Kernel Density

0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

10 12 14 16 18

10

11

12

13

14

15

16

17

18

1610

171

1081

615

1810

447

1049

177

254

1833

1811

1109

1105

312

1097

1011

1636

1428

1034

1913

1032

1059

340

1082

1079

1402

1062

1842

1021

1064

1650

2130

1720

323

1528

1613

1635

1203

311

399

671

225

2136

192

2133



Determination of Aromatics by HPLC (ASTM D6379) on sample #0816; results in %V/V

lab method value mark z(targ) remarks 140 ----- ----- 171 ----- ----- 177 ----- ----- 192 ----- ----- 194 ----- ----- 224 ----- ----- 225 ----- ----- 237 ----- ----- 254 ----- ----- 256 ----- ----- 311 ----- ----- 312 ----- ----- 317 ----- ----- 323 ----- ----- 334 ----- ----- 340 ----- ----- 399 ----- ----- 447 ----- ----- 615 ----- ----- 671 ----- ----- 851 D6379 14.47 ----- Reported in %V/V 1011 ----- ----- 1017 ----- ----- 1021 ----- ----- 1026 IP436 13.3 ----- Reported in %M/M 1032 ----- ----- 1034 ----- ----- 1038 ----- ----- 1039 D6379 14.78 ----- Reported in %V/V 1049 ----- ----- 1059 ----- ----- 1062 ----- ----- 1064 ----- ----- 1079 ----- ----- 1081 ----- ----- 1082 ----- ----- 1097 ----- ----- 1105 ----- ----- 1108 ----- ----- 1109 D6591 17.86 ex ----- Method is not suitable for this type of Jet Fuel 1138 ----- ----- 1140 ----- ----- 1203 D6379 15.8 ----- Reported in %M/M 1318 ----- ----- 1402 ----- ----- 1414 ----- ----- 1428 ----- ----- 1528 D6379 18.7 ----- Reported in %V/V 1531 ----- ----- 1600 ----- ----- 1610 ----- ----- 1613 ----- ----- 1634 ----- ----- 1635 ----- ----- 1636 ----- ----- 1650 ----- ----- 1651 ----- ----- 1657 D6379 11.5 ----- Reported in %V/V 1715 ----- ----- 1720 ----- ----- 1730 ----- ----- 1810 ----- ----- 1811 ----- ----- 1833 D6379 13.6 C ----- First reported 0.6, result is reported in %M/M 1842 ----- ----- 1913 ----- ----- 1939 ----- ----- 2130 ----- ----- 2133 ----- ----- 2136 ----- -----



normality n.a n 8 outliers 0 mean (n) n.a. st.dev. (n) n.a. R(calc.) n.a. R(D6379:04) n.a.



Determination of Colour Saybolt on sample #0816;

lab method value mark z(targ) remarks 140 D156 30 0.26 171 D156 30 0.26 177 D156 30 0.26 192 D156 30 0.26 194 D156 28 -2.54 224 ----- ----- 225 D156 29 -1.14 237 ----- ----- 254 D156 30 0.26 256 ----- ----- 311 D156 30 0.26 312 D156 30 0.26 317 D156 30 0.26 323 ----- ----- 334 D156 28 -2.54 340 D156 30 0.26 399 D156 30 0.26 447 D156 30 0.26 615 D156 30 0.26 671 D156 30 0.26 851 D156 29 -1.14 1011 D156 30 0.26 1017 ----- ----- 1021 ----- ----- 1026 D156 30 0.26 1032 D156 30 0.26 1034 D156 30 0.26 1038 ----- ----- 1039 D156 30 0.26 1049 ----- ----- 1059 D156 30 0.26 1062 D156 30 0.26 1064 D156 30 0.26 1079 D6045 30 0.26 1081 D6045 30 0.26 1082 D6045 30 0.26 1097 INHOUSE 30 0.26 1105 D156 30 0.26 1108 D156 23 G(0.01) -9.54 1109 D156 30 0.26 1138 D156 26 G(0.01) -5.34 1140 ----- ----- 1203 D156 30 C 0.26 First reported 19 1318 D156 30 0.26 1402 D156 >30 ----- 1414 ----- ----- 1428 D156 30 0.26 1528 D156 30 0.26 1531 ----- ----- 1600 D6045 >30 ----- 1610 D156 30 0.26 1613 ----- ----- 1634 ----- ----- 1635 D156 30 0.26 1636 D156 30 0.26 1650 D156 29 -1.14 1651 D156 30 0.26 1657 D156 30 0.26 1715 D6045 30 0.26 1720 D156 30 0.26 1730 ----- ----- 1810 ----- ----- 1811 ----- ----- 1833 D156 28 -2.54 1842 ----- ----- 1913 D156 30 0.26 1939 D156 30 0.26 2130 D156 30 0.26 2133 ----- W ----- Result withdrawn 2136 D156 30 0.26



normality not OK n 48 outliers 2 mean (n) 29.8 st.dev. (n) 0.53 R(calc.) 1.5 R(D156:07a) 2.0

25

26

27

28

29

30

31

32

33

1108

1138

194

334

1833

1650

851

225

1318

1428

1528

1097

1082

1105

1203

1109

1913

1720

1939

2136

2130

1715

1635

1610

1636

1657

1651

317

312

340

447

399

311

171

140

177

254

192

615

1062

1059

1064

1081

1079

1039

1011

671

1026

1034

1032

Kernel Density

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0.05

0.1

0.15

0.2

0.25

0.3

0.35

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0 10 20 30 40



Determination of Density @ 15°C on sample #0816; results in kg/m3

lab method value mark z(targ) remarks 140 D4052 798.2 0.90 171 D4052 798.2 0.90 177 D4052 797.8 C -1.34 First reported 798.5 192 D4052 798.13 0.50 194 D287 796.8 G(0.01) -6.94 224 D1298 798.2 0.90 225 D4052 798.16 0.67 237 ----- ----- 254 D1298 798.1 C 0.34 First reported 797.4 256 ----- ----- 311 D4052 798.1 0.34 312 D4052 797.9 -0.78 317 D4052 798.1 0.34 323 D4052 797.9 -0.78 334 D4052 797.9 -0.78 340 D4052 798.1 0.34 399 D4052 798.0 -0.22 447 D4052 797.9 -0.78 615 D4052 798.18 0.78 671 D4052 798.2 0.90 851 D4052 798.04 0.00 1011 D4052 798.1 0.34 1017 D4052 798.1 0.34 1021 D4052 798.06 0.11 1026 D4052 798.0 -0.22 1032 D4052 798.0 -0.22 1034 D4052 797.9 -0.78 1038 ----- ----- 1039 D4052 798.1 0.34 1049 D4052 797.97 -0.39 1059 D4052 797.8 -1.34 1062 D4052 798.0 -0.22 1064 D4052 798.0 -0.22 1079 D4052 798.0 -0.22 1081 ISO12185 798.1 0.34 1082 ----- ----- 1097 ISO12185 798.0 -0.22 1105 D4052 798.1 0.34 1108 D4052 798.2 0.90 1109 D4052 797.9 -0.78 1138 IP365 798.2 0.90 1140 ----- ----- 1203 ISO12185 798.1 0.34 1318 D4052 798.07 0.17 1402 D4052 798.0 -0.22 1414 ----- ----- 1428 D4052 798.1 0.34 1528 D4052 798.0 -0.22 1531 ----- ----- 1600 D1298 797.3 G(0.01) -4.14 1610 D4052 798.1 0.34 1613 D4052 798.1 0.34 1634 D4052 798.1 0.34 1635 D4052 797.8 -1.34 1636 D4052 798.1 0.34 1650 D4052 798.03 -0.06 1651 D4052 798.1 0.34 1657 D4052 797.6 G(0.01) -2.46 1715 ISO12185 798.0 -0.22 1720 D4052 798.1 C 0.34 First reported 794.9 1730 D4052 798.0 -0.22 1810 D4052 798.0 -0.22 1811 D4052 798.0 -0.22 1833 D4052 798.0 -0.22 1842 IP365 798.0 -0.22 1913 D4052 798.0 -0.22 1939 D4052 798.05 0.06 2130 D4052 798.1 0.34 2133 D4052 797.8 -1.34 2136 D4052 798.10 0.34



normality not OK n 60 outliers 3 mean (n) 798.04 st.dev. (n) 0.104 R(calc.) 0.29 R(D4052:02e1) 0.50

796

796.5

797

797.5

798

798.5

799

194

1657

1635

2133

1109

1034

312

1026

1097

1064

1833

1842

1913

1402

399

1650

1939

1318

1610

2136

1636

1634

1011

254

317

1428

1081

192

615

140

1138

671

Kernel Density

0

0.5

1

1.5

2

2.5

3

3.5

4

796.5 797 797.5 798 798.5



Determination of Distillation ASTM D86 (automated) on sample #0816; results in °C

lab method IBP mark 10% mark 20% mark 50% mark 90% mark FBP mark 140 D86 156.4 176.6 182.0 195.1 225.3 259.8 G(0.01) 171 D86 152.4 177.1 182.0 195.4 225.2 246.3 177 D86 163.2 175.1 180.9 195.6 225.9 248.4 192 D86 158.6 176.9 182.3 195.9 227.6 246.7 194 ----- ----- ----- ----- ----- ----- 224 ----- ----- ----- ----- ----- ----- 225 ----- ----- ----- ----- ----- ----- 237 ----- ----- ----- ----- ----- ----- 254 D86 162.3 177.3 182.2 195.4 227.1 246.6 256 ----- ----- ----- ----- ----- ----- 311 D86 154.1 174.7 181.1 195.5 226.4 248.2 312 D86 157.0 175.3 181.1 195.0 224.3 247.3 317 D86 163.3 180.4 G(0.05) 184.1 197.7 228.3 248.5 323 D86 160.4 176.4 182.5 195.6 226.4 247.7 334 D86 156.2 176.9 182.3 195.8 226.5 252.9 G(0.01) 340 D86 160.9 178.0 183.4 196.5 226.9 248.3 399 D86 159.0 177.0 182.0 195.0 223.0 245.5 447 D86 157.1 176.6 181.9 195.9 227.6 248.8 615 D86 162.1 177.4 183.0 196.8 228.1 250.8 671 D86 158.5 177.2 182.0 195.0 223.4 244.4 851 D86 158.7 177.2 182.4 195.1 226.5 246.5

1011 D86 159.5 177.6 182.3 195.2 226.0 249.1 1017 D86 159.9 175.4 180.7 193.9 224.1 243.7 1021 D86 156.7 176.4 181.7 195.1 225.9 246.7 1026 ISO3405 157.2 176.7 181.4 195.0 225.9 246.4 1032 D86 158.2 176.5 181.7 195.0 225.5 246.5 1034 D86 157.2 177.2 182.0 194.6 224.7 246.1 1038 ----- ----- ----- ----- ----- ----- 1039 D86 157.9 177.0 182.2 195.5 226.7 247.7 1049 D86 156.3 176.8 182.1 195.0 225.1 246.0 1059 ISO3405 157.9 177.2 182.6 195.4 225.6 248.1 1062 D86 156.5 175.2 180.8 194.2 225.5 244.2 1064 D86 157.1 176.7 181.6 194.9 226.5 247.2 1079 D86 156.1 178.7 182.8 195.9 226.3 247.8 1081 D86 157.1 176.1 181.8 195.1 225.7 246.9 1082 ----- ----- ----- ----- ----- ----- 1097 ISO3405 157.8 176.1 181.3 195.0 226.1 244.9 1105 D86 158.4 175.6 181.6 194.7 225.1 245.1 1108 D86 160.4 176.0 181.0 194.1 224.5 247.0 1109 D86 158.7 175.7 182.0 195.6 227.5 247.2 1138 D86 158.4 177.6 182.9 196.0 225.4 247.8 1140 ----- ----- ----- ----- ----- ----- 1203 ISO3405 154.4 176.8 182.8 196.6 227.8 248.1 1318 D86 156.2 176.3 181.6 194.9 225.2 247.5 1402 D86 160.4 176.0 181.1 194.0 224.2 246.2 1414 ----- ----- ----- ----- ----- ----- 1428 ISO3405 155.30 175.50 181.65 195.9 230.2 G(0.05) 254.01 G(0.05) 1528 D86 159.3 178.4 183.5 196.1 227.2 245.5 1531 D86 164.1 177.1 182.9 195.9 226.4 247.9 1600 ----- ----- ----- ----- ----- ----- 1610 D86 157.9 176.4 181.9 195.2 226.0 246.3 1613 D86 157.3 179.1 183.9 196.5 226.5 247.5 1634 D86 161.2 176.9 181.7 194.8 225.5 247.8 1635 ----- ----- ----- ----- ----- ----- 1636 D86 158.1 175.6 180.6 194.3 225.5 245.4 1650 D86 153.6 174.3 179.9 193.7 224.8 247.6 1651 D86 158.75 177.70 182.80 195.45 224.90 245.60 1657 D86 156.3 177.3 182.5 195.4 225.8 247.2 1715 D86 159.80 175.90 181.25 194.20 224.30 246.40 1720 ----- ----- ----- ----- ----- ----- 1730 ----- ----- ----- ----- ----- ----- 1810 D86 159.2 176.9 182.0 195.0 224.5 246.9 1811 D86 160.8 177.2 181.9 194.9 226.1 246.5 1833 D86 157.1 174.9 181.6 195.0 224.7 246.4 1842 D86 158.6 177.0 181.9 195.0 225.7 245.9 1913 ----- ----- ----- ----- ----- ----- 1939 D86 155.8 176.4 182.0 195.7 227.6 245.1 2130 D86 155.9 176.6 181.9 194.8 224.9 246.6 2133 D86 155.6 176.7 181.7 194.2 223.8 246.1 2136 D86 154.3 176.8 182.5 195.6 225.0 246.0



normality OK OK not OK OK OK OK n 56 55 56 56 55 53 outliers 0 1 0 0 1 3 mean (n) 158.06 176.62 181.99 195.26 225.76 246.81 st.dev. (n) 2.452 0.953 0.800 0.757 1.190 1.313 R(calc.) 6.87 2.67 2.24 2.12 3.33 3.68 R(D86:07b) 8.50 6.16 4.75 5.38 4.62 10.50

Automated: R (D 86:05-A tabel10) IBP: 8.50 10%: 6.16 = 3.0 + 2.64 * C/%V and C/%V = 1.20 20%: 4.75 = 2.9 + 3.97 * C/%V and C/%V = 0.47 50%: 5.38 = 2.9 + 3.97 * C/%V and C/%V = 0.63 90%: 4.62 = 2.0 + 2.53 * C/%V and C/%V = 1.03 FBP: 10.50

Initial Boiling Point (automated method)

50% recovered (automated method)

Final Boiling Point (automated method)

145

150

155

160

165

170

171

311

1203

2133

2130

334

1049

140

1021

447

1833

1026

1613

1610

1059

1032

1105

192

1109

1651

1810

1011

1017

1108

1811

1634

254

317

185

187

189

191

193

195

197

199

201

203

1650

1402

2133

1715

1034

2130

1064

1811

671

1097

1810

1032

1026

851

1081

1011

1657

171

311

323

177

1939

1428

447

1531

1528

1613

615

230

235

240

245

250

255

260

265

1017

671

1105

1636

1528

1842

1049

1034

1610

1026

1715

1811

254

1021

1081

1108

1109

312

1613

1039

1634

1138

1059

311

177

447

615

1428



Determination of Distillation ASTM D86 (Manual) on sample #0816; results in °C

lab method IBP mark 10% mark 20% mark 50% mark 90% mark FBP mark 140 ----- ----- ----- ----- ----- ----- 171 ----- ----- ----- ----- ----- ----- 177 ----- ----- ----- ----- ----- ----- 192 ----- ----- ----- ----- ----- ----- 194 D86 153.33 174.44 178.88 192.22 221.11 247.77 224 D86 159.0 177.12 182.87 195.36 226.38 247.16 225 D86 161.0 178.0 183.0 196.0 226.0 251.0 237 ----- ----- ----- ----- ----- ----- 254 ----- ----- ----- ----- ----- ----- 256 ----- ----- ----- ----- ----- ----- 311 ----- ----- ----- ----- ----- ----- 312 ----- ----- ----- ----- ----- ----- 317 ----- ----- ----- ----- ----- ----- 323 ----- ----- ----- ----- ----- ----- 334 ----- ----- ----- ----- ----- ----- 340 ----- ----- ----- ----- ----- ----- 399 ----- ----- ----- ----- ----- ----- 447 ----- ----- ----- ----- ----- ----- 615 ----- ----- ----- ----- ----- ----- 671 ----- ----- ----- ----- ----- ----- 851 ----- ----- ----- ----- ----- -----

1011 ----- ----- ----- ----- ----- ----- 1017 ----- ----- ----- ----- ----- ----- 1021 ----- ----- ----- ----- ----- ----- 1026 ----- ----- ----- ----- ----- ----- 1032 ----- ----- ----- ----- ----- ----- 1034 ----- ----- ----- ----- ----- ----- 1038 ----- ----- ----- ----- ----- ----- 1039 ----- ----- ----- ----- ----- ----- 1049 ----- ----- ----- ----- ----- ----- 1059 ----- ----- ----- ----- ----- ----- 1062 ----- ----- ----- ----- ----- ----- 1064 ----- ----- ----- ----- ----- ----- 1079 ----- ----- ----- ----- ----- ----- 1081 ----- ----- ----- ----- ----- ----- 1082 ----- ----- ----- ----- ----- ----- 1097 ----- ----- ----- ----- ----- ----- 1105 ----- ----- ----- ----- ----- ----- 1108 ----- ----- ----- ----- ----- ----- 1109 ----- ----- ----- ----- ----- ----- 1138 ----- ----- ----- ----- ----- ----- 1140 ----- ----- ----- ----- ----- ----- 1203 ----- ----- ----- ----- ----- ----- 1318 ----- ----- ----- ----- ----- ----- 1402 ----- ----- ----- ----- ----- ----- 1414 ----- ----- ----- ----- ----- ----- 1428 ----- ----- ----- ----- ----- ----- 1528 ----- ----- ----- ----- ----- ----- 1531 ----- ----- ----- ----- ----- ----- 1600 D86 157 176 182 194 225 243 1610 ----- ----- ----- ----- ----- ----- 1613 ----- ----- ----- ----- ----- ----- 1634 ----- ----- ----- ----- ----- ----- 1635 D86 154 173 180 193 224 241 1636 ----- ----- ----- ----- ----- ----- 1650 ----- ----- ----- ----- ----- ----- 1651 ----- ----- ----- ----- ----- ----- 1657 ----- ----- ----- ----- ----- ----- 1715 ----- ----- ----- ----- ----- ----- 1720 D86 157.0 176.0 182.0 196.5 226.0 247.5 1730 ----- ----- ----- ----- ----- ----- 1810 ----- ----- ----- ----- ----- ----- 1811 ----- ----- ----- ----- ----- ----- 1833 ----- ----- ----- ----- ----- ----- 1842 ----- ----- ----- ----- ----- ----- 1913 D86 152.4 174.0 179.2 192.2 221.4 242.0 1939 ----- ----- ----- ----- ----- ----- 2130 ----- ----- ----- ----- ----- ----- 2133 ----- ----- ----- ----- ----- ----- 2136 ----- ----- ----- ----- ----- -----



normality OK OK OK OK OK OK n 7 7 7 7 7 7 outliers 0 0 0 0 0 0 mean (n) 156.25 175.51 181.14 194.18 224.27 245.63 st.dev. (n) 3.153 1.779 1.737 1.792 2.209 3.669 R(calc.) 8.83 4.98 4.86 5.02 6.19 10.27 R(D86:07-M) 4.59 3.46 2.42 2.62 3.17 4.00

Manual: R (D 86:05-B table 9) IBP: 4.59 = 2.8 + 0.93 * C/%V and C/%V = 1.93 10%: 3.46 = 1.8 + 1.33 * C/%V and C/%V = 1.24 20%: 2.42 = 1.8 + 1.33 * C/%V and C/%V = 0.47 50%: 2.62 = 1.8 + 1.33 * C/%V and C/%V = 0.62 90%: 3.17 = 1.8 + 1.33 * C/%V and C/%V = 1.03 FBP: 4.00 = 3.1 + 0.42 * C/%V and C/%V = 2.14

Initial Boiling Point (manual method)

50% recovered (manual method)

Final Boiling Point (manual method)

150

152

154

156

158

160

162

1913

194

1635

1720

1600

224

225

190

191

192

193

194

195

196

197

198

1913

194

1635

1600

224

225

1720

240

242

244

246

248

250

252

1635

1913

1600

224

1720

194

225



Determination of Existent Gum on sample #0816; results in mg/100 mL

lab method value mark z(targ) remarks 140 D381-S <0.5 ----- 171 D381-S 0.4 -0.23 177 D381-S <1 ----- 192 D381-S <1 ----- 194 ----- ----- 224 ----- ----- 225 D381-A 0.8 0.52 237 ----- ----- 254 ----- ----- 256 ----- ----- 311 D381-A <1 ----- 312 D381-A <1 ----- 317 D381-A <1 ----- 323 ----- ----- 334 ----- ----- 340 D381-A 0.3 -0.42 399 D381-A 0.8 0.52 447 ----- ----- 615 D381-A <1 ----- 671 D381-S 1.4 G(0.05) 1.66 851 D381-S <1 ----- 1011 D381-A <1 ----- 1017 ----- ----- 1021 ----- ----- 1026 D381-A 0.5 -0.04 1032 D381-A 0.5 -0.04 1034 D381-S 0.4 -0.23 1038 ----- ----- 1039 D381-A <1 ----- 1049 ----- ----- 1059 ISO6246-A <1 ----- 1062 D381-S 1.0 0.90 1064 D381-S <1 ----- 1079 D381-S 0.4 -0.23 1081 D381-A 1 0.90 1082 ----- ----- 1097 ISO6046A 0.1 -0.79 1105 D381-S 0.60 0.15 1108 D381-A 1.0 0.90 1109 IP540A 0.04 -0.91 1138 ----- ----- 1140 ----- ----- 1203 ISO6246A <0.1 ----- 1318 D381-A 0.3 -0.42 1402 D381-A 0.2 -0.61 1414 ----- ----- 1428 ISO6046A 0.6 0.15 1528 IP540A 0.6 0.15 1531 ----- ----- 1600 ----- ----- 1610 IP540A 0.5 -0.04 1613 D381-S 0.4 -0.23 1634 D381-S 0.5 -0.04 1635 D381-S 0.2 -0.61 1636 D381-A 0.2 -0.61 1650 D381-S 0.8 0.52 1651 IP131S 0.55 0.05 1657 D381-A 1 0.90 1715 ----- ----- 1720 D381-A 1 0.90 1730 ----- ----- 1810 D381-A 0.2 -0.61 1811 ----- ----- 1833 IP540S 0.2 -0.61 1842 IP540A <1 ----- 1913 D381-S 0.20 -0.61 1939 D381-A <1 ----- 2130 D381-A <1 ----- 2133 D381-S 0.8 0.52 2136 D381-S 0.6 0.15



Only Air-used data: Only Steam-used data normality OK OK OK n 32 18 14 outliers 1 0 1 mean (n) 0.52 0.54 0.50 st.dev. (n) 0.293 0.334 0.242 R(calc.) 0.82 0.94 0.68 R(D381:04e1) 1.49 1.51 1.47

0

0.5

1

1.5

2

2.5

1109

1097

1635

1402

1833

1913

1636

1810

1318

340

171

1613

1034

1079

1610

1634

1026

1032

1651

1105

2136

1428

1528

2133

225

399

1650

1062

1081

1108

1720

1657

671

Kernel Density

0

0.2

0.4

0.6

0.8

1

1.2

-1 -0.5 0 0.5 1 1.5 2



Determination of Flash Point on sample #0816; results in °C

lab method value mark z(targ) remarks 140 ----- ----- 171 IP170-E 44.3 -1.66 177 IP170-M 44.0 -2.22 192 ----- ----- 194 D93 47.77 ex 4.82 224 IP170-MF 44.23 -1.79 225 IP170- 45.0 -0.35 237 ----- ----- 254 IP170-MF 45.0 -0.35 256 ----- ----- 311 IP170-E 45.0 -0.35 312 IP170-AE 45.0 -0.35 317 IP170-F 44.0 -2.22 323 IP170-AF 45.5 0.58 334 IP170-AF 44.5 -1.29 340 ISO13736F 45.0 -0.35 399 IP170-FM 45.0 -0.35 447 IP170- 44.5 -1.29 615 IP170- 46.5 2.45 671 IP170-MF 44.0 -2.22 851 IP170-MF 44.0 -2.22 1011 IP170-MF 44.5 -1.29 1017 D93E 45.8 ex 1.14 1021 D56AE 44.83 -0.67 1026 IP170- 47.0 3.38 1032 IP170-AE 46.0 1.51 1034 IP170-AE 45.0 -0.35 1038 ----- ----- 1039 IP170-AE 46.5 2.45 1049 IP170-AE 44.5 -1.29 1059 IP170-E 43.5 -3.15 1062 IP170-E 46.0 1.51 1064 IP170-E 45.5 0.58 1079 IP170-E 45.5 0.58 1081 D56-AE 45.5 0.58 1082 ----- ----- 1097 ISO13736F 44.6 -1.10 1105 IP170-AF 44.7 -0.91 1108 D56AE 44.0 -2.22 1109 IP170-F 44.5 -1.29 1138 IP170- 45.5 0.58 1140 ----- ----- 1203 D56MF 46.0 1.51 1318 IP170-E 45.0 -0.35 1402 IP170-AE 45.0 -0.35 1414 ----- ----- 1428 IP170-AF 45.5 0.58 1528 D53E 46 C 1.51 First reported 48 1531 ----- ----- 1600 D3828MF 46 1.51 1610 IP170-F 45.6 0.77 1613 D56AE 46 1.51 1634 IP170-MF 43.5 -3.15 1635 D56-MF 48 G(0.05) 5.25 1636 D56AE 45.5 0.58 1650 IP170-AE 46.0 1.51 1651 IP170-AE 45.75 1.05 1657 IP170-AE 47.0 3.38 1715 D56E 45.5 0.58 1720 D3828AF 45.0 -0.35 1730 ----- ----- 1810 D93F 46.5 ex 2.45 1811 IP170-F 46.8 3.01 1833 IP170-AF 45 -0.35 1842 IP170-AE 47.0 3.38 1913 IP170-AF 44.35 -1.57 1939 IP170-MF 44 -2.22 2130 IP170-A 45.0 -0.35 2133 D93 45 ex -0.35 2136 D56-AE 45.0 -0.35



normality not OK n 55 outliers 1 mean (n) 45.16 st.dev. (n) 0.880 R(calc.) 2.46 R(IP170:99) 1.50

Only IP170 data Only D56 data normality not OK not OK n 44 10 outliers 1 0 mean (n) 45.10 45.63 st.dev. (n) 0.928 1.042 R(calc.) 2.60 2.92 R(IP170:99) 1.50 4.30

A = Automated AE = Automated / Electric mode AF = Automated / Flame mode M = Manual MF = Manual / Flame mode

Kernel Density

0

0.05

0.1

0.15

0.2

0.25

0.3

0.35

0.4

0.45

40 42 44 46 48 50

40

41

42

43

44

45

46

47

48

49

1634

1939

317

671

224

1913

1109

334

1097

1021

254

2136

1402

1833

2130

1034

312

1428

1079

1081

1138

1651

1528

1032

1613

1650

1039

1811

1842

194



Determination of Freezing Point on sample #0816; results in °C

lab method value mark z(targ) Remarks 140 D5773A -58.2 -0.65 171 D5972A -57.8 -0.20 177 D2386- -57.0 0.69 192 D2386-M -57.0 0.69 194 ----- ----- 224 ----- ----- 225 D2386-M -56.0 1.81 237 ----- ----- 254 D2386-M -58.0 -0.43 256 ----- ----- 311 D2386M -58.5 -0.99 312 ----- ----- 317 D5972A -58.4 -0.88 323 D2386-M -56.5 1.25 334 D7135-A -57.3 0.36 340 D7153A -57.5 0.13 399 D2386-A -57.7 -0.09 447 IP529 -57.2 0.47 615 D5972A -57.65 -0.04 671 D2386-M -58.0 -0.43 851 D2386-M -58.5 -0.99 1011 D2386-M -59.0 -1.55 1017 ----- ----- 1021 D5972A -58.6 -1.10 1026 D2386-A -58.0 -0.43 1032 D7153- -57.2 0.47 1034 D7153-A -57.3 0.36 1038 ----- ----- 1039 IP529A -57.8 -0.20 1049 D7153A -57.5 0.13 1059 D2386-M -58.0 -0.43 1062 D7153-A -57.5 0.13 1064 D7153A -57.4 0.24 1079 D2386-M -58.5 -0.99 1081 D7153-A -57.1 0.58 1082 IP529A -57.4 0.24 1097 ISO3015M -57.5 0.13 1105 D7153A -57.5 0.13 1108 D5972A -57.7 -0.09 1109 D5972A -57.9 -0.32 1138 ----- ----- 1140 ----- ----- 1203 D2386-M <-58 ----- 1318 D2386-M -57.5 0.13 1402 IP529A -57.1 0.58 1414 ----- ----- 1428 D2386-A -57.4 0.24 1528 D2386-A -57.41 0.23 1531 ----- ----- 1600 D2386-M -58.0 -0.43 1610 IP16M -57.5 0.13 1613 D7153A -57.1 0.58 1634 D2386-M -58.0 -0.43 1635 D2386-M -56 C 1.81 First reported -51 1636 D2386-M -58.0 -0.43 1650 D2386-M -57.0 0.69 1651 D2386-A -57.28 0.38 1657 D2386-M -57.0 0.69 1715 D5972A -57.76 -0.16 1720 D5972A -58.3 -0.76 1730 D5901-A -57.38 0.27 1810 D2386-M -58 -0.43 1811 D2386-A -58 -0.43 1833 IP528 -57.3 0.36 1842 D2386-M -59.0 -1.55 1913 D2386-M -57.75 -0.15 1939 ----- ----- 2130 D2386-M -57.0 0.69 2133 ----- ----- 2136 D7153A -57.7 -0.09



Only D2386 data: Only D7153 data: Only D5972 data: normality OK not OK not OK OK n 56 28 16 8 outliers 0 0 0 0 mean (n) -57.62 -57.64 -57.45 -58.01 st.dev. (n) 0.608 0.772 0.371 0.364 R(calc.) 1.70 2.16 1.04 1.02 R(D2386:06) 2.50 2.50 0.90 0.80

-65

-63

-61

-59

-57

-55

-53

-51

-49

1011

1021

311

317

140

1059

1026

671

254

1109

171

1913

399

615

1610

1049

1097

1528

1082

1730

334

1651

1032

1402

2130

1657

1650

1635

Kernel Density

0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

-60 -59 -58 -57 -56 -55



Determination of JFTOT; Tube Rating, Delta P in mmHg, Pumped Vol. in mL, Temp. in oC

lab method tube mark Delta P mark volume mark temp mark remarks 140 D3241 <1 1 450 260 171 D3241 <1 1 450 260 177 D3241 1 0 450 260 192 D3241 <1 0 425 260 194 D3241 1 0 525 ex 260 Volume >495ml 224 ----- ----- ----- ----- 225 D3241 1 1.4 480 260 237 ----- ----- ----- ----- 254 D3241 <1 0 450 260 256 ----- ----- ----- ----- 311 D3241 1 <1 450 260 312 ----- ----- ----- ----- 317 ----- ----- ----- ----- 323 D3241 <1 <1 450 260 334 D3241 0 0 450 260 340 D3241 1 0 450 260 399 D3241 1 0 460 260 447 ----- ----- ----- ----- 615 D3241 <1 1 450 260 671 D3241 <1 0 455 260 851 D3241 <1 0 450 260

1011 D3241 1 0.0 510 ex 260 Volume >495ml 1017 ----- ----- ----- ----- 1021 D3241 0 1 450 260 1026 D3241 <1 <1 ----- 260 1032 D3241 <1 0.2 440 260 1034 D3241 1 0 450 260 1038 ----- ----- ----- ----- 1039 D3241 <2 2.0 460 260 1049 ----- ----- ----- ----- 1059 ----- ----- ----- ----- 1062 D3241 0 1 480 260 1064 D3241 0 0.0 450 260 1079 D3241 1 0 425 260 1081 D3241 <1 0 450 260 1082 ----- ----- ----- ----- 1097 D3241 1 0.1 480 260 1105 D3241 1 0 465 260 1108 ----- ----- ----- ----- 1109 D3241 <1.0 0 450 260 1138 ----- ----- ----- ----- 1140 ----- ----- ----- ----- 1203 D3241 1 0 ----- ----- 1318 D3241 <1 0.0 450 260 1402 ----- ----- ----- ----- 1414 ----- ----- ----- ----- 1428 D3241 <1 0 450 260 1528 D3241 1 0 450 260 1531 ----- ----- ----- ----- 1600 ----- ----- ----- ----- 1610 D3241 <1 <1 460 260 1613 D3241 <1 0.0 450 260 1634 ----- ----- ----- ----- 1635 D3241 1 1 ----- 260 1636 ----- ----- ----- ----- 1650 D3241 1 0.0 450 260 1651 D3241 1 0 450 260 1657 D3241 1 1 450 260 1715 ----- ----- ----- ----- 1720 D3241 1 1 475 260 1730 ----- ----- ----- ----- 1810 ----- ----- ----- ----- 1811 ----- ----- ----- ----- 1833 D3241 <1 0 510 ex 260 Volume >495ml 1842 ----- ----- ----- ----- 1913 D3241 1 0.0 450 260 1939 ----- ----- ----- ----- 2130 D3241 BLUE <1 460 260 2133 D3241 <1 1 475 260 2136 D3241 1 0 450 260



normality n.a. n.a. n.a. n.a. n 24 39 38 43 outliers 0 0 0 0 mean (n) 0.8 0.3 454 260 st.dev. (n) n.a. n.a. n.a. n.a. R(calc.) n.a. n.a. n.a. n.a. R(D3241:08a) n.a. n.a. n.a. n.a.



Determination of Mercaptan Sulphur on sample #0816; results in % M/M

lab method value mark z(targ) remarks 140 D3227 0.002 G(0.01) 16.45 171 D3227 0.0004 2.27 177 ----- ----- 192 ----- ----- 194 ----- ----- 224 ----- ----- 225 ----- ----- 237 ----- ----- 254 D3227 0.0004 2.27 256 ----- ----- 311 D3227 <0.0003 ----- 312 ----- ----- 317 D3227 <0.0003 ----- 323 ----- ----- 334 ----- ----- 340 D3227 0.00006 -0.74 399 D3227 <0.0003 ----- 447 ----- ----- 615 D3227 0.00006 -0.74 671 ----- ----- 851 D3227 <0.0003 ----- 1011 D3227 0.0001 -0.38 1017 ----- ----- 1021 ----- ----- 1026 D3227 <0.0002 ----- 1032 ----- ----- 1034 D3227 0.00017 0.24 1038 ----- ----- 1039 D3227 0.0003 1.39 1049 ----- ----- 1059 D3227 <0.0003 ----- 1062 D3227 0.0002 0.50 1064 D3227 0.000099 -0.39 1079 D3227 0.000075 -0.60 1081 D3227 0 -1.27 1082 ----- ----- 1097 ISO3012 0.000089 -0.48 1105 D3227 0.000101 -0.37 1108 D3227 0.0000 -1.27 1109 D3227 0.00017 0.24 1138 ----- ----- 1140 ----- ----- 1203 UOP163 0.000077 -0.59 1318 ----- ----- 1402 D3227 0.0001 -0.38 1414 ----- ----- 1428 D3227 0.00015 0.06 1528 D3227 0.00012 -0.21 1531 ----- ----- 1600 ----- ----- 1610 D3227 0.00016 0.15 1613 D3227 0.0002 0.50 1634 ----- ----- 1635 D3227 0.0002 0.50 1636 D3227 0.00011 -0.29 1650 D3227 0.00015 0.06 1651 D3227 0.00018 0.33 1657 ----- ----- 1715 ----- ----- 1720 D3227 0.0003 1.39 1730 ----- ----- 1810 ----- ----- 1811 ----- ----- 1833 D3241 0.00009 -0.47 1842 IP342 0.0001 -0.38 1913 D3227 <0.0003 C ----- First reported 0.00056 1939 D3227 <0.0003 ----- 2130 D3227 0.00013 -0.12 2133 D3227 0.0001 -0.38 2136 D3227 0.00005 -0.83



normality OK n 31 outliers 1 mean (n) 0.00014 st.dev. (n) 0.000098 R(calc.) 0.00027 R(D3227:04a) 0.00032

0

0.0005

0.001

0.0015

0.002

0.0025

1081

1108

2136

615

340

1079

1203

1097

1833

1064

1842

2133

1011

1402

1105

1636

1528

2130

1428

1650

1610

1109

1034

1651

1613

1635

1062

1039

1720

171

254

140

Kernel Density

0

1000

2000

3000

4000

5000

6000

-0.001 0 0.001 0.002 0.003



Determination of MSEP on sample #0763;

lab method value mark z(targ) remarks 140 D3948 97 0.33 171 D3948 97 0.33 177 D3948 98 0.81 192 D3948 98.5 1.04 194 D3948 93 -1.55 224 ----- ----- 225 ----- ----- 237 ----- ----- 254 D3948 99 1.28 256 ----- ----- 311 D3948 96 -0.14 312 D3948 96 -0.14 317 D3948 93 C -1.55 First reported 90 323 D3948 95 -0.61 334 ----- ----- 340 D3948 93 -1.55 399 D3948 97 0.33 447 D3948 94 -1.08 615 D3948 98 0.81 671 D3948 98 0.81 851 D3948 97 0.33 1011 D3948 96 -0.14 1017 ----- ----- 1021 D3948 98 0.81 1026 D3948 95 -0.61 1032 D3948 97 0.33 1034 D3948 93 -1.55 1038 ----- ----- 1039 D3948 95 -0.61 1049 D3948 94 -1.08 1059 D3948 94 -1.08 1062 D3948 95 -0.61 1064 D3948 96 -0.14 1079 D3948 96 -0.14 1081 D3948 95 -0.61 1082 ----- ----- 1097 D3948 95 -0.61 1105 D3948 99 1.28 1108 D3948 97 0.33 1109 D3948 97 0.33 1138 ----- ----- 1140 ----- ----- 1203 ----- ----- 1318 D3948 98 0.81 1402 D3948 95 -0.61 1414 ----- ----- 1428 ----- ----- 1528 D3948 98 0.81 1531 ----- ----- 1600 D3948 98 0.81 1610 D3948 98 C 0.81 First reported 88 1613 D3948 98 0.81 1634 ----- ----- 1635 D3948 96 -0.14 1636 ----- ----- 1650 D3948 99 1.28 1651 D3948 97 0.33 1657 D3948 96 -0.14 1715 ----- ----- 1720 D3948 94 C -1.08 First reported 90 1730 ----- ----- 1810 D3948 95 -0.61 1811 D3948 97 0.33 1833 D3948 96 -0.14 1842 D3948 90 G(0.05) -2.96 1913 D3948 99 1.28 1939 ----- ----- 2130 D3948 96 -0.14 2133 D3948 98 0.81 2136 D3948 95 -0.61



normality not OK n 50 outliers 1 mean (n) 96.29 st.dev. (n) 1.738 R(calc.) 4.87 R(D3948:07) 5.94

85

87

89

91

93

95

97

99

101

103

105

1842

317

1034

340

194

1049

1059

447

1720

1097

1026

1081

1062

1402

1039

1810

2136

323

1657

1833

2130

1064

1079

1635

312

311

1011

1811

1109

1651

399

140

851

171

1108

1032

177

2133

1318

615

1021

671

1528

1610

1613

1600

192

1650

254

1913

1105

Kernel Density

0

0.02

0.04

0.06

0.08

0.1

0.12

0.14

0.16

0.18

0.2

85 90 95 100 105



Determination of Naphthalenes on sample #0816; results in %V/V

lab method value mark z(targ) remarks 140 D1840 0.19 4.24 171 D1840 0.19 4.24 177 D1840 0.13 -0.70 192 ----- ----- 194 D1840 6.4117 G(0.01) 516.01 224 ----- ----- 225 ----- ----- 237 ----- ----- 254 ----- ----- 256 ----- ----- 311 D1840 0.12 -1.52 312 ----- ----- 317 D1840 0.13 -0.70 323 ----- ----- 334 ----- ----- 340 D1840 0.14 C 0.13 First reported 0.18 399 ----- ----- 447 D1840 0.12 -1.52 615 D1840 0.114 -2.01 671 ----- ----- 851 D1840 0.152 1.11 1011 D1840 0.14 0.13 1017 ----- ----- 1021 D1840 0.14 0.13 1026 ----- ----- 1032 ----- ----- 1034 D1840 0.145 0.54 1038 ----- ----- 1039 D1840 0.12 -1.52 1049 D1840 0.13 -0.70 1059 ----- ----- 1062 D1840 0.18 3.42 1064 D1840 0.139 0.04 1079 D1840 0.132 -0.53 1081 D1840 0.11 -2.34 1082 ----- ----- 1097 D1840 0.137 -0.12 1105 D1840 0.151 1.03 1108 D1840 0.40 G(0.01) 21.51 1109 D1840 0.0013 CG(0.01) -11.28 First reported 0.013 1138 ----- ----- 1140 ----- ----- 1203 D1840 0.48 CG(0.01) 28.09 First reported 0.6 1318 D1840 0.140 0.13 1402 D1840 0.127 -0.94 1414 ----- ----- 1428 ----- ----- 1528 D1840 0.14 0.13 1531 ----- ----- 1600 ----- ----- 1610 D1840 0.13 -0.70 1613 ----- ----- 1634 ----- ----- 1635 D1840 0.16 1.77 1636 D1840 0.13 -0.70 1650 ----- ----- 1651 ----- ----- 1657 D1840 0.0225 G(0.01) -9.54 1715 ----- ----- 1720 D1840 0.13 -0.70 1730 ----- ----- 1810 D1840 0.12 -1.52 1811 ----- ----- 1833 ----- ----- 1842 D1840 0.14 0.13 1913 D1840 0.132 -0.53 1939 ----- ----- 2130 D1840 0.142 0.29 2133 D1840 1.29 G(0.01) 94.72 2136 D1840 0.13 -0.70



normality not OK n 32 outliers 6 mean (n) 0.138 st.dev. (n) 0.0192 R(calc.) 0.054 R(D1840:07-A) 0.034 Compare (D1840:07-B) = 0.029

Kernel Density

0

5

10

15

20

25

-0.2 0 0.2 0.4 0.6

0

0.05

0.1

0.15

0.2

0.25

0.3

0.35

0.4

0.45

0.5

1109

1657

1081

615

447

1810

1039

311

1402

2136

1049

177

317

1610

1636

1720

1079

1913

1097

1064

1318

1528

340

1011

1842

1021

2130

1034

1105

851

1635

1062

140

171

1108

1203

2133

194



Determination of Smoke Point on sample #0816; results in mm

lab method value mark z(targ) remarks 140 ----- ----- 171 D1322 24 -1.33 177 D1322 25 -0.40 192 D1322 26.0 0.53 194 ----- ----- 224 ----- ----- 225 ----- ----- 237 ----- ----- 254 D1322 24.5 -0.87 256 ----- ----- 311 D1322 23.0 -2.27 312 ----- ----- 317 D1322 24.0 -1.33 323 ----- ----- 334 ----- ----- 340 D1322 26.0 0.53 399 D1322 26 0.53 447 D1322 26.5 1.00 615 D1322 25.99 0.52 671 D1322 25.5 0.07 851 D1322 25.5 0.07 1011 D1322 27.0 1.47 1017 ----- ----- 1021 D1322 28.0 2.40 1026 D1322 26.5 1.00 1032 D1322 25 -0.40 1034 D1322 26.4 0.91 1038 ----- ----- 1039 D1322 27.5 1.93 1049 D1322 24 -1.33 1059 ----- ----- 1062 D1322 25.0 -0.40 1064 D1322 24.93 -0.47 1079 D1322 25 -0.40 1081 D1322 25 -0.40 1082 ----- ----- 1097 D1322 27.2 1.65 1105 D1322 25.17 -0.24 1108 ----- ----- 1109 D1322 27.81 2.22 1138 ----- ----- 1140 ----- ----- 1203 D1322 24.7 -0.68 1318 ----- ----- 1402 D1322 25 -0.40 1414 ----- ----- 1428 D1322 25 -0.40 1528 D1322 25.04 -0.36 1531 ----- ----- 1600 ----- ----- 1610 D1322 26.2 0.72 1613 D1322 25 -0.40 1634 ----- ----- 1635 D1322 25 -0.40 1636 D1322 25.14 -0.27 1650 D1322 25.19 -0.22 1651 D1322 25 -0.40 1657 D1322 21.0 G(0.05) -4.13 1715 D1322 25.37 -0.06 1720 D1322 24.0 -1.33 1730 ----- ----- 1810 D1322 25.3 -0.12 1811 D1322 25.2 -0.21 1833 D1322 26 0.53 1842 D1322 27.0 1.47 1913 D1322 24.8 -0.59 1939 D1322 24.7 C -0.68 First reported 22 2130 D1322 25.0 -0.40 2133 D1322 21.5 G(0.05) -3.67 2136 D1322 24.6 -0.77



normality not OK n 46 outliers 2 mean (n) 25.43 st.dev. (n) 1.053 R(calc.) 2.95 R(D1322:02e1) 3.00

20

21

22

23

24

25

26

27

28

29

1657

2133

311

317

1049

171

1720

254

2136

1203

1939

1913

1064

1079

1081

2130

1635

1651

1613

1402

1428

1032

177

1062

1528

1636

1105

1650

1811

1810

1715

851

671

615

340

1833

192

399

1610

1034

1026

447

1842

1011

1097

1039

1109

1021

Kernel Density

0

0.1

0.2

0.3

0.4

0.5

0.6

0 10 20 30 40



Determination of Specific Energy on sample #0816; results in MJ/kg

lab method value mark z(targ) remarks 140 ----- ----- 171 D3338 43.384 1.99 177 D3338 43.36 0.53 192 D3338 43.3285 -1.39 194 ----- ----- 224 ----- ----- 225 D4529 43.34 -0.69 237 ----- ----- 254 ----- ----- 256 ----- ----- 311 D3338 43.331 C -1.24 First reported 43.135 312 ----- ----- 317 ----- ----- 323 ----- ----- 334 ----- ----- 340 D4529 43.321 -1.85 399 D3338 43.301 -3.06 447 D3338 43.484 G(0.01) 8.08 615 D3338 43.373 1.32 671 ----- ----- 851 D3338 43.34 -0.69 1011 D3338 43.356 0.28 1017 ----- ----- 1021 ----- ----- 1026 ----- ----- 1032 D3338 43.3250 -1.60 1034 D3338 43.3471 -0.26 1038 ----- ----- 1039 D3338 43.344 -0.45 1049 ----- ----- 1059 ----- ----- 1062 D3338 43.346 -0.32 1064 D3338 43.3485 -0.17 1079 D3338 43.36 0.53 1081 D3338 43.375 1.44 1082 ----- ----- 1097 D3338 43.356 0.28 1105 D3338 43.36 0.53 1108 ----- ----- 1109 D3338 43.36 0.53 1138 ----- ----- 1140 ----- ----- 1203 D3338 43.34 C -0.69 First reported 43.71 1318 ----- ----- 1402 D3338 43.345 C -0.38 First reported 43.013 1414 ----- ----- 1428 ----- ----- 1528 D3338 43.35052 -0.05 1531 ----- ----- 1600 ----- ----- 1610 D3338 43.379 1.68 1613 D3338 43.351 -0.02 1634 ----- ----- 1635 D3338 43.417 C 4.00 First reported 43.018 1636 D3338 43.3511 -0.01 1650 ----- ----- 1651 ----- ----- 1657 D3338 43.4 2.96 1715 ----- ----- 1720 D4529 43.39 2.35 1730 ----- ----- 1810 ----- ----- 1811 ----- ----- 1833 D3338 43.357 0.35 1842 D3338 43.348 -0.20 1913 D3338 43.340 C -0.69 First reported 44.340 1939 ----- ----- 2130 D3338 43.3272 -1.47 2133 D3338 43.32 -1.91 2136 D3338 43.324 -1.66



normality not OK n 35 outliers 1 mean (n) 43.3513 st.dev. (n) 0.02394 R(calc.) 0.0670 R(D3338:05) 0.0460

43

43.1

43.2

43.3

43.4

43.5

43.6

399

2133

340

2136

1032

2130

192

311

1203

851

225

1913

1039

1402

1062

1034

1842

1064

1528

1613

1636

1011

1097

1833

1079

1105

1109

177

615

1081

1610

171

1720

1657

1635

447

Kernel Density

0

5

10

15

20

25

43.2 43.3 43.4 43.5 43.6



Determination of Total Acidity on sample #0816; results in mg KOH/g

lab method value mark z(targ) purged remarks 140 ----- ----- 171 D3242 0.0024 1.81 Yes 177 D3242 0.002 1.08 192 D3242 0.0010 -0.76 Yes 194 ----- ----- 224 ----- ----- 225 D3242 0.001 -0.76 237 ----- ----- 254 D3242- 0.00216 1.37 No 256 ----- ----- 311 D3242 0.001 -0.76 Yes 312 ----- ----- 317 D3242 0.001 -0.76 Yes 323 D3242 0.001 -0.76 Yes 334 ----- ----- 340 D3242 0.0012 -0.39 399 D3242 0.0017 0.53 Yes 447 ----- ----- 615 D3242 0.0033 3.46 Yes 671 ----- ----- 851 D3242 0.002 C 1.08 Yes First reported 0.004 1011 D3242 <0.001 ----- Yes 1017 D3242 0.00145 0.07 Yes 1021 ----- ----- 1026 D3242 0.000055 C -2.49 First reported 0.005 1032 D3242 0.0016 0.34 Yes 1034 D3242 0.0015 0.16 Yes 1038 ----- ----- 1039 D3242 0.001 -0.76 Yes 1049 ----- ----- 1059 D3242 <0.001 ----- Yes 1062 D3242 0.0010 -0.76 Yes 1064 D3242 0.0006 -1.49 Yes 1079 D3242 0.0014 -0.02 Yes 1081 D3242 0 ex -2.59 Yes Not a true value 1082 ----- ----- 1097 D3242 0.0027 2.36 Yes 1105 D3242 0.00072 -1.27 Yes 1108 D3242 0.0043 G(0.01) 5.30 No 1109 D3242 0.00038 -1.90 Yes 1138 ----- ----- 1140 ----- ----- 1203 D3242 0.00175 0.62 Yes 1318 ----- ----- 1402 D3242 0.0005 -1.68 Yes 1414 ----- ----- 1428 ----- ----- 1528 D3242 0.0021 1.26 Yes 1531 ----- ----- 1600 ----- ----- 1610 IP354 0.0019 0.89 Yes 1613 D3242 0.0008 -1.12 Yes 1634 ----- ----- 1635 ----- ----- 1636 ----- ----- 1650 ----- ----- 1651 D3242 0.0018 0.71 Yes 1657 D3242 0.001389 -0.04 Yes 1715 ISO6618 0.0015 ex 0.16 No 1720 D3242 0.001 -0.76 Yes 1730 ----- ----- 1810 ----- ----- 1811 ----- ----- 1833 D3242 0.00217 1.39 Yes 1842 IP354 0.001 -0.76 Yes 1913 D3242 0.0016 0.34 Yes 1939 D3242 0.0005 C -1.68 Yes First reported 0.0051 2130 D3242 0.0016 0.34 Yes 2133 D3242 0.0021 1.26 Yes 2136 D3242 0.00124 -0.32 Yes



Only purged data: normality OK not OK n 38 33 outliers 1 0 mean (n) 0.00141 0.00143 st.dev. (n) 0.000685 0.000670 R(calc.) 0.00192 0.00188 R(D3242:07) 0.00153 0.00154

0

0.0005

0.001

0.0015

0.002

0.0025

0.003

0.0035

0.004

0.0045

0.005

1081

1026

1109

1939

1402

1064

1105

1613

1720

311

225

1062

1039

323

192

317

1842

340

2136

1657

1079

1017

1034

1715

1913

1032

2130

399

1203

1651

1610

851

177

1528

2133

254

1833

171

1097

615

1108

Kernel Density

0

100

200

300

400

500

600

-0.002 0 0.002 0.004 0.006



Determination of Total Sulphur on sample #0816; results in mg/kg

lab method value mark z(targ) remarks 140 D5453 1.17 -0.70 171 D5453 3 6.35 177 D5453 0 ex -5.21 Results excluded not a true value 192 ----- ----- 194 D5453 235 G(0.01) 900.51 224 ----- ----- 225 ----- ----- 237 ----- ----- 254 ----- ----- 256 ----- ----- 311 D5453 1.4 0.19 312 D5453 1.57 0.84 317 ISO20884 <5.0 ----- 323 ----- ----- 334 D5453 0.3 -4.05 340 D5453 0.12 -4.75 399 D7212 2.0 2.50 447 ----- ----- 615 D5453 1.1 C -0.97 First reported 11 671 ----- ----- 851 D2622 <5 ----- 1011 ISO8754 <56 ----- 1017 ----- ----- 1021 D2622 <10 ----- 1026 ISO20884 <2 ----- 1032 D4294 <20 ----- 1034 D5453 1.33 -0.08 1038 ----- ----- 1039 D2622 1 -1.35 1049 ----- ----- 1059 ISO14596 <10 ----- 1062 D5453 1.5 0.57 1064 D5453 0.6 U -2.90 Reported wrong unit (%M/M instead of mg/kg) 1079 D5453 3.4 7.90 1081 ISO20846 1.1 U -0.97 Reported wrong unit (%M/M instead of mg/kg) 1082 ----- ----- 1097 ISO20846 1.6 0.96 1105 D5453 1.119 -0.89 1108 D5453 0.6 -2.90 1109 D5453 1.0 -1.35 1138 IP490 2.3 3.66 1140 ----- ----- 1203 ISO14596 1.25 -0.39 1318 ----- ----- 1402 D5453 0.82 -2.05 1414 ----- ----- 1428 ----- ----- 1528 D5453 1.34 -0.04 1531 ----- ----- 1600 ----- ----- 1610 IP336 <0.0003 ----- 1613 D4294 1.0 -1.35 1634 ----- ----- 1635 D5453 1.20 -0.58 1636 D5453 1.46 0.42 1650 ----- ----- 1651 D5453 1.45 0.38 1657 ----- ----- 1715 ----- ----- 1720 D5453 1.8 1.73 1730 ----- ----- 1810 D5453 1.2 -0.58 1811 D5453 1.06 -1.12 1833 D5453 1.9 2.12 1842 D4294 20 G(0.01) 71.87 1913 D4294 <150 ----- 1939 D3120 <3 ----- 2130 IP336 0.048 -5.02 2133 D4294 14.7 G(0.01) 51.45 2136 D2622 2.5 4.43



Only D5453 data: normality OK not OK n 32 23 outliers 3 1 mean (n) 1.35 1.32 st.dev. (n) 0.733 0.736 R(calc.) 2.05 2.06 R(D5453:08a) 0.73 0.72

Kernel Density

0

0.05

0.1

0.15

0.2

0.25

0.3

0.35

0.4

0.45

-10 0 10 20 30

0

5

10

15

20

25

177

2130

340

334

1108

1064

1402

1039

1109

1613

1811

1081

615

1105

140

1635

1810

1203

1034

1528

311

1651

1636

1062

312

1097

1720

1833

399

1138

2136

171

1079

2133

1842

194



Determination of Viscosity @ -20°C on sample #0816; results in cSt

lab method value mark z(targ) remarks 140 D445-M 3.877 1.46 171 D445-M 3.830 -0.34 177 D445- 3.949 G(0.05) 4.22 192 D445-M 3.9592 DG(0.05) 4.62 194 D445- 3.7779 -2.34 224 ----- ----- 225 D445- 3.907 2.61 237 ----- ----- 254 D445-M 3.8139 C -0.96 First reported 3.412 256 ----- ----- 311 D445-M 3.891 2.00 312 ----- ----- 317 ----- ----- 323 ----- ----- 334 ----- ----- 340 D445- 3.843 0.15 399 D445-M 3.841 C 0.08 First reported 4.1330 447 D445- 3.817 -0.84 615 ----- ----- 671 ----- ----- 851 D445-M 3.8250 -0.54 1011 D445-M 3.844 0.19 1017 D445-M 3.8273 -0.45 1021 D445-M 3.8430 0.15 1026 ISO3104M 3.826 -0.50 1032 D445-M 3.8412 0.09 1034 D445-M 3.8431 0.16 1038 ----- ----- 1039 D445-M 3.842 0.12 1049 ----- ----- 1059 ----- ----- 1062 D445-M 3.8362 -0.11 1064 D445-A 3.8461 0.27 1079 D445-M 3.8375 -0.06 1081 D445-M 3.771 -2.61 1082 D445-M 3.7987 -1.55 1097 ISO3104M 3.8328 -0.24 1105 D445-M 3.8379 -0.04 1108 D445-M 3.952 DG(0.05) 4.34 1109 D445-M 3.8708 1.22 1138 ----- ----- 1140 ----- ----- 1203 ISO3104M 3.832 -0.27 1318 ----- ----- 1402 D445-M 3.929 3.46 1414 ----- ----- 1428 D445-A 3.8412 0.09 1528 D445-M 3.83267 -0.24 1531 ----- ----- 1600 ----- ----- 1610 D445-M 3.8431 0.16 1613 D445-A 3.8399 0.04 1634 ----- ----- 1635 D445-M 3.808 -1.19 1636 ----- ----- 1650 ----- ----- 1651 D445-A 3.8332 -0.22 1657 D445-M 3.635 G(0.01) -7.83 1715 ----- ----- 1720 D445-M 3.862 0.88 1730 ----- ----- 1810 D445-M 3.843 0.15 1811 D445-A 3.8239 -0.58 1833 D445-M 3.84 C 0.04 First reported 3.36 1842 IP71M 3.847 0.31 1913 D445-M 3.8245 -0.56 1939 ----- ----- 2130 IP71M 3.6792 G(0.01) -6.13 2133 D445-M 3.566 G(0.01) -10.48 2136 D445-A 3.839 0.00



normality not OK not OK n 40 30 outliers 6 5 mean (n) 3.8390 3.8397 st.dev. (n) 0.02860 0.02799 R(calc.) 0.0801 0.0784 R(D445:06) 0.0729 0.0729

3.4

3.5

3.6

3.7

3.8

3.9

4

2133

1657

2130

1081

194

1082

1635

254

447

1811

1913

851

1026

1017

171

1203

1528

1097

1651

1062

1079

1105

2136

1613

1833

399

1428

1032

1039

340

1810

1021

1034

1610

1011

1064

1842

1720

1109

140

311

225

1402

177

1108

192

Kernel Density

0

5

10

15

20

25

30

3.5 3.6 3.7 3.8 3.9 4



APPENDIX 2 Z-scores of individual participants for distillation (automated (A) and manual (M)) of sample #0816

Lab IBP(A) 10%(A) 20%(A) 50%(A) 90%(A) FBP(A) IBP(M) 10%(M) 20%(M) 50%(M) 90%(M) FBP(M)140 -0.55 -0.01 0.01 -0.08 -0.28 3.46 ----- ----- ----- ----- ----- -----171 -1.86 0.22 0.01 0.07 -0.34 -0.14 ----- ----- ----- ----- ----- -----177 1.69 -0.69 -0.64 0.18 0.08 0.42 ----- ----- ----- ----- ----- -----192 0.18 0.13 0.18 0.33 1.12 -0.03 ----- ----- ----- ----- ----- -----194 ----- ----- ----- ----- ----- ----- -1.78 -0.87 -2.61 -2.10 -2.79 1.50224 ----- ----- ----- ----- ----- ----- 1.68 1.31 2.01 1.26 1.86 1.07225 ----- ----- ----- ----- ----- ----- 2.90 2.02 2.16 1.94 1.53 3.76237 ----- ----- ----- ----- ----- ----- ----- ----- ----- ----- ----- -----254 1.40 0.31 0.13 0.07 0.81 -0.06 ----- ----- ----- ----- ----- -----256 ----- ----- ----- ----- ----- ----- ----- ----- ----- ----- ----- -----311 -1.30 -0.87 -0.52 0.12 0.39 0.37 ----- ----- ----- ----- ----- -----312 -0.35 -0.60 -0.52 -0.14 -0.89 0.13 ----- ----- ----- ----- ----- -----317 1.73 1.72 1.25 1.27 1.54 0.45 ----- ----- ----- ----- ----- -----323 0.77 -0.10 0.30 0.18 0.39 0.24 ----- ----- ----- ----- ----- -----334 -0.61 0.13 0.18 0.28 0.45 1.62 ----- ----- ----- ----- ----- -----340 0.94 0.63 0.83 0.64 0.69 0.40 ----- ----- ----- ----- ----- -----399 0.31 0.17 0.01 -0.14 -1.68 -0.35 ----- ----- ----- ----- ----- -----447 -0.32 -0.01 -0.05 0.33 1.12 0.53 ----- ----- ----- ----- ----- -----615 1.33 0.36 0.60 0.80 1.42 1.06 ----- ----- ----- ----- ----- -----671 0.14 0.26 0.01 -0.14 -1.44 -0.64 ----- ----- ----- ----- ----- -----851 0.21 0.26 0.24 -0.08 0.45 -0.08 ----- ----- ----- ----- ----- -----

1011 0.47 0.45 0.18 -0.03 0.14 0.61 ----- ----- ----- ----- ----- -----1017 0.61 -0.55 -0.76 -0.71 -1.01 -0.83 ----- ----- ----- ----- ----- -----1021 -0.45 -0.10 -0.17 -0.08 0.08 -0.03 ----- ----- ----- ----- ----- -----1026 -0.28 0.04 -0.35 -0.14 0.08 -0.11 ----- ----- ----- ----- ----- -----1032 0.05 -0.05 -0.17 -0.14 -0.16 -0.08 ----- ----- ----- ----- ----- -----1034 -0.28 0.26 0.01 -0.34 -0.65 -0.19 ----- ----- ----- ----- ----- -----1038 ----- ----- ----- ----- ----- ----- ----- ----- ----- ----- ----- -----1039 -0.05 0.17 0.13 0.12 0.57 0.24 ----- ----- ----- ----- ----- -----1049 -0.58 0.08 0.07 -0.14 -0.40 -0.22 ----- ----- ----- ----- ----- -----1059 -0.05 0.26 0.36 0.07 -0.10 0.34 ----- ----- ----- ----- ----- -----1062 -0.51 -0.64 -0.70 -0.55 -0.16 -0.70 ----- ----- ----- ----- ----- -----1064 -0.32 0.04 -0.23 -0.19 0.45 0.10 ----- ----- ----- ----- ----- -----1079 -0.65 0.95 0.48 0.33 0.33 0.26 ----- ----- ----- ----- ----- -----1081 -0.32 -0.24 -0.11 -0.08 -0.04 0.02 ----- ----- ----- ----- ----- -----1082 ----- ----- ----- ----- ----- ----- ----- ----- ----- ----- ----- -----1097 -0.09 -0.24 -0.41 -0.14 0.20 -0.51 ----- ----- ----- ----- ----- -----1105 0.11 -0.46 -0.23 -0.29 -0.40 -0.46 ----- ----- ----- ----- ----- -----1108 0.77 -0.28 -0.58 -0.60 -0.77 0.05 ----- ----- ----- ----- ----- -----1109 0.21 -0.42 0.01 0.18 1.06 0.10 ----- ----- ----- ----- ----- -----1138 0.11 0.45 0.54 0.38 -0.22 0.26 ----- ----- ----- ----- ----- -----1140 ----- ----- ----- ----- ----- ----- ----- ----- ----- ----- ----- -----1203 -1.21 0.08 0.48 0.70 1.24 0.34 ----- ----- ----- ----- ----- -----1318 -0.61 -0.14 -0.23 -0.19 -0.34 0.18 ----- ----- ----- ----- ----- -----1402 0.77 -0.28 -0.52 -0.66 -0.95 -0.16 ----- ----- ----- ----- ----- -----1414 ----- ----- ----- ----- ----- ----- ----- ----- ----- ----- ----- -----1428 -0.91 -0.51 -0.20 0.33 2.70 1.92 ----- ----- ----- ----- ----- -----1528 0.41 0.81 0.89 0.44 0.87 -0.35 ----- ----- ----- ----- ----- -----1531 1.99 0.22 0.54 0.33 0.39 0.29 ----- ----- ----- ----- ----- -----1600 ----- ----- ----- ----- ----- ----- 0.46 0.40 1.00 -0.20 0.65 -1.841610 -0.05 -0.10 -0.05 -0.03 0.14 -0.14 ----- ----- ----- ----- ----- -----1613 -0.25 1.13 1.13 0.64 0.45 0.18 ----- ----- ----- ----- ----- -----1634 1.03 0.13 -0.17 -0.24 -0.16 0.26 ----- ----- ----- ----- ----- -----1635 ----- ----- ----- ----- ----- ----- -1.37 -2.03 -1.31 -1.26 -0.24 -3.251636 0.01 -0.46 -0.82 -0.50 -0.16 -0.38 ----- ----- ----- ----- ----- -----1650 -1.47 -1.05 -1.23 -0.81 -0.59 0.21 ----- ----- ----- ----- ----- -----1651 0.23 0.49 0.48 0.10 -0.52 -0.32 ----- ----- ----- ----- ----- -----1657 -0.58 0.31 0.30 0.07 0.02 0.10 ----- ----- ----- ----- ----- -----1715 0.57 -0.33 -0.43 -0.55 -0.89 -0.11 ----- ----- ----- ----- ----- -----1720 ----- ----- ----- ----- ----- ----- 0.46 0.40 1.00 2.48 1.53 1.311730 ----- ----- ----- ----- ----- ----- ----- ----- ----- ----- ----- -----1810 0.38 0.13 0.01 -0.14 -0.77 0.02 ----- ----- ----- ----- ----- -----1811 0.90 0.26 -0.05 -0.19 0.20 -0.08 ----- ----- ----- ----- ----- -----1833 -0.32 -0.78 -0.23 -0.14 -0.65 -0.11 ----- ----- ----- ----- ----- -----1842 0.18 0.17 -0.05 -0.14 -0.04 -0.24 ----- ----- ----- ----- ----- -----1913 ----- ----- ----- ----- ----- ----- -2.35 -1.22 -2.24 -2.12 -2.54 -2.541939 -0.74 -0.10 0.01 0.23 1.12 -0.46 ----- ----- ----- ----- ----- -----2130 -0.71 -0.01 -0.05 -0.24 -0.52 -0.06 ----- ----- ----- ----- ----- -----2133 -0.81 0.04 -0.17 -0.55 -1.19 -0.19 ----- ----- ----- ----- ----- -----2136 -1.24 0.08 0.30 0.18 -0.46 -0.22 ----- ----- ----- ----- ----- -----



APPENDIX 3 List of number of laboratories per country 2 laboratories in AUSTRALIA

6 laboratories in BELGIUM

2 laboratories in CÔTE D'IVOIRE

1 laboratory in CROATIA

2 laboratories in CZECH REPUBLIC

1 laboratory in DENMARK

1 laboratory in FINLAND

3 laboratories in FRANCE

4 laboratories in GERMANY

3 laboratories in GREECE

1 laboratory in GUAM

1 laboratory in HONG KONG

2 laboratories in HUNGARY

1 laboratory in INDIA

1 laboratory in ITALY

1 laboratory in JORDAN

1 laboratory in KENYA

1 laboratory in MALAYSIA

1 laboratory in NIGERIA

1 laboratory in NORWAY

1 laboratory in P.R. of CHINA

1 laboratory in PAPUA NEW GUINEA

2 laboratories in PORTUGAL

1 laboratory in REPUBLIC OF GUINEE

2 laboratories in REPUBLIC OF MACEDONIA

1 laboratory in ROMANIA

1 laboratory in SAUDI ARABIA

1 laboratory in SLOVENIA

1 laboratory in SUDAN

1 laboratory in TANZANIA

7 laboratories in THE NETHERLANDS

2 laboratories in TURKEY

1 laboratory in U.A.E.

5 laboratories in U.S.A.

7 laboratories in UNITED KINGDOM



APPENDIX 4 Abbreviations: C = final result after checking of first reported suspect result U = reported in wrong unit D(0.01) = outlier in Dixon’s outlier test D(0.05) = straggler in Dixon’s outlier test G(0.01) = outlier in Grubbs’ outlier test G(0.05) = straggler in Grubbs’ outlier test DG(0.01) = outlier in Double Grubbs’ outlier test DG(0.05) = straggler in Double Grubbs’ outlier test ex = excluded from calculations E = error in calculations n.a. = not applicable W = withdrawn on request participant Literature: 1 i.i.s. Interlaboratory Studies, Protocol for the Organisation, Statistics & Evaluation, November 2003 2 Defence Standard 91-91, Issue 5 Publication date 8 September ‘05 + amendment 2 dated 9 March ‘07. 3 Aviation Fuel Quality Requirements for Jointly Operated Systems (AFQRJOS), Issue 22–28 June 2007,

Bulletin No. 21. 4 ASTM E178-02 5 ASTM E1301-03 6 ISO 5725, parts 1-6, 1994 7 M. Thompson and R. Wood, J. AOAC Int, 76, 926, (1993) 8 W.J. Youden and E.H. Steiner, Statistical Manual of the AOAC, (1975) 9 IP 367/84 10 DIN 38402 T41/42 11 P.L. Davies, Fr. Z. Anal. Chem, 331, 513, (1988) 12 J.N. Miller, Analyst, 118, 455, (1993) 13 Analytical Methods Committee Technical Brief, No4 January 2001 14 The Royal Society of Chemistry 2002, Analyst 2002, 127 page1359-1364, P.J. Lowthian and M.

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

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Results of Proficiency Test Jet Fuel A1 March 2008 - iisnl. · PDF fileResults of Proficiency Test Jet Fuel A1 March 2008 ... (20% evaporated), Flash Point, MSEP ... participants reported