WP5 TEST REPORT. Test Report WP Methodology Study 08, CROATIA

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1 IST IST Vapour Detection - area reduction in demining WP5 TEST REPORT Report WP Methodology Study 08, CROATIA Report Version: 1.0 Report Preparation Date: 8 March 2004 Classification: Contract Start Date: 01 January 2001 Duration: 36 months Project Co-ordinator: Partners: Swedish Rescue Services Agency Biosensor Applications AB, Sweden GTD Ingeniería de Sistemas y Software Industrial S.A., Spain [Withdrew from project 9 April 2001] Norwegian People s Aid, Norway Swedish Rescue Services Agency, Sweden Weizmann Institute of Science, Israel Project funded by the European Community under the Information Society Technologies Programme ( ) The copyright of this document is the property of partners. No part may be reproduced, transmitted in any form or by any means electronic, mechanical, photo copying, recording or otherwise, transferred to other documents, disclosed to a third party or used for any other purpose except in accordance with the provisions of European Commission Contract No. IST Biosens_WP5.2.1_Methodology_Study_Croatia_08 Report_SRSA_rev2.0

2 Report, WP Methodology Study 08, CROATIA SUMMARY: This report comprises the test results from the WP Methodology Study 08, Croatia. During week 336 and 337, September 2003 a team of 4 SRSA personnel has been performing tests at the Site in Croatia. In the test results from Methodology Study 01, FOI, indicated the ground to be free from explosive substances or explosive related substances before the plantation of mines took place. The main objectives with WP Methodology Study 08 in Croatia were : Sampling of air in the boxes above planted mines. Collection of soil samples in the boxes above planted mines after air sampling Sampling of air and soil above the planted Mines. Verify the logistical chain; from sampling of filters inclusive of analyses in the laboratory for confirmation of its functionality in a sufficient way. (Reference s). Comparison in yield between Biosensor System and Mine Detection Dogs. The results shows the control filters and control filters left behind in Sweden to have a false alarm rate of 0%, none samples positive of 20 in total. No positive alarms were expected. These results indicates the positive responses for TNT/DNT presence in the material from Methodology Study 08, Croatia to be generated from TNT/DNT present in the mine. The positive results of reference tests indicates the logistical chain from sampling of filters inclusive of analyses in the laboratory to be functional in a sufficient way. These results can be used for evaluation and fulfilment of the objectives for Methodology study 08. The number of tests are not large enough to have a statistically significant material. Sampling in the 16 boxes took place day 2, 3, 4, 5 and 6. The yield day 2 was 1 sample positive for TNT of 3 in total. The yield day 3 was none of 4 in total. The yield day 4 was none sample positive for TNT of 8 in total. The yield day 5 was 5 samples possible positive for TNT of 8 in total. The filters used day 5 were without support ring resulting in a LOD of 50 pg (TNT/DNT). If the results were to be evaluated according to a LOD of 100 pg the yield day 5 will be reduced to 3 samples positive instead of 5. The yield for day 6 was 1 sample positive for TNT/DNT of 5 in total. Severe weather conditions with rain and wind day 2 and 3. The results shows the positive and possible positive results regarding presence of TNT/DNT in boxes to be 7 of 28 in total, approximately 25%. If the evaluation is made with a LOD on 100 pg (TNT/DNT) for all filters the yield will be 5 of 28 in total, approximately 18%. The results shows Sampling between boxes 5 sample positive ( + ) for TNT of 23 in total, approximately 21%. The ratio positive results above mine to positive results between mines is 1:1. The major part of all the positive results were sampled day 5. Sampling of Fresh air at mine shows 2 sample positive for TNT of 22 in ii/ ix

3 Report, WP Methodology Study 08, CROATIA total, approximately 9%.. Positive results regarding presence of TNT/DNT during Methodology Study 08, Croatia were predominantly taken place on day 5. This indicates the weather conditions to be more favourably on day 5 compared to the other test days. Severe weather conditions with rain day 2 in combination with wind might be one explanation for absence of positive results day 2. The rain day 2 might have washed away the accumulated compounds of TNT/DNT from the soil surface. The positive results day 5 indicates the levels of TNT/DNT concentration in the soil surface to be large enough for passing the threshold as a positive response with the available LOD for these test procedures. One explanation for the somewhat randomised pattern regarding presence of TNT/DNT in and between boxes might be caused by the wind. Improvements to the LOD better than 100 pg is desirable. Two Mine Detection Dogs were used during Methodology Study 08. The dogs were searching the box areas before the sampling of air took place. The dogs successfully pinpointed all the 16 planted test mines without any false alarms. ing in a yield of 100%. This successful performance was repeated the working day after. The fact that the MDD were able to pinpoint all the planted mines despite the rain indicates the dogs sensitivities for TNT/DNT detection to be extremely high. The dogs might not need the TNT/DNT to be accumulated on the soil top surfaces for their detection. It might be sufficient for the dogs to smell the continuously leakage of TNT/DNT vapour from the planted mines. On the other hand it might also indicate that the dogs use one or several other substance/substances than TNT/DNT (or in combination with TNT/DNT) as a marker for their assessment of the smelling patterns originated from mines. The soil samples however seem to not have been influenced by the rain. Instead quite high levels of concentrations of TNT/DNT in ng /g TS have been found. One difference between sampling procedures for air and soil samples is that collection of soil samples are made on the soil surface and a few centimetres below while the air samples are collected on the top of the soil surface. The rain on the 2 nd of September refer to Appendix 3 might have washed away the accumulated compounds of TNT/DNT from the top of the soil surface. Note that it seem to be TNT deposit also between the boxes. Records of Change Revision Date File Reference Reason of change Rev /January/2004 First Edition Rev /March/2004 Updates after review iii/ ix

4 Report, WP Methodology Study 08, CROATIA CONTENT ABBREVIATIONS...VIII DEFINITIONS...IX 1 WP METHODOLOGY STUDY 08, CROATIA, SHORT INTRODUCTION WP METHODOLOGY STUDY 08, CROATIA, TEST WP METHODOLOGY 08 CROATIA, RESULTS TEST RESULTS WP METHODOLOGY STUDY 08, CROATIA DAY Comments to results WP Methodology Study 08, Croatia, day Chronological order for sampling of filters s fresh air at mine s realated to box (air samples) s from sampling between boxes Reference s TEST RESULTS WP METHODOLOGY STUDY 08 CROATIA DAY Comments to results WP5.2.1 Methodology Study 08, Croatia day Chronological order for sampling of filters s related to samling of fresh air at hotel premises s related to samling of fresh air at mine s from sampling of Personnel s realated to box (air samples) s from sampling between boxes Reference s TEST RESULTS WP METHODOLOGY STUDY 08 CROATIA DAY Comments to results WP5.2.1 Methodology Study 08, Croatia day Chronological order for sampling of filters s related to samling of fresh air at mine s realated to box (air samples) s from sampling between boxes s from sampling of new line (air) s from sampling of new line (soil) s related to line (air) s related to line (soil) Reference s TEST RESULTS WP METHODOLOGY STUDY 08 CROATIA DAY Comments to results WP5.2.1 Methodology Study 08, Croatia day Chronological order for sampling of filters s realted to sampling of fresh air at mine s realated to box (air samples) s from sampling between boxes s related to line (air samples)...28 iv/ ix

5 Report, WP Methodology Study 08, CROATIA s related to line (soil samples) Reference s TEST RESULTS WP METHODOLOGY STUDY 08 CROATIA DAY Comments to results WP5.2.1 Methodology Study 08, Croatia day Chronological order for sampling of filters s realted to sampling of fresh air at mine s realated to box (air samples) s from sampling between boxes s related to box (soil samples) Reference s Control filters left behind in Sweden WEATHER CONDITIONS COMPARISON WITH MINE DETECTION DOGS DISCUSSION AND CONCLUSIONS REFERENCE DOCUMENTS v/ ix

6 Report, WP Methodology Study 08, CROATIA FIGURES TABLES Table 1 Summary activities day by day, WP Methodology Study 08 Croatia. Table 2 Summary Controls, WP Methodology Study 08 Croatia. Table 3 results WP5.2.1 Methodology Study 08 Croatia day 1-2. Table 4 results WP5.2.1 Methodology Study 08, Croatia day 2. Chronological order for sampling of filters. Table 5 results WP5.2.1 Methodology Study 08, Croatia day 2, results related to sampling fresh air at mine. Table 6 results WP5.2.1 Methodology Study 08, Croatia day 2, results related to box. Table 7 results WP5.2.1 Methodology Study 08, Croatia day 2. results related to sampling between boxes. Table 8 results WP5.2.1 Methodology Study 08, Croatia day 3. Table 9 results WP5.2.1 Methodology Study 08, Croatia day 3. Chronological order for sampling of filters. Table 10 Table 11 Table 12 results WP5.2.1 Methodology Study 08, Croatia day 3 s related to sampling of fresh air at hotel premises (outdoor). results WP5.2.1 Methodology Study 08, Croatia day 3. s related to sampling of fresh air at mine. results WP5.2.1 Methodology Study 08. Croatia day 3. of test personnel. Table 13 results WP5.2.1 Methodology Study 08. Croatia day 3. s related to box (air samples). Table 14 results WP Methodology Study 08. Croatia day 3. s related to sampling between boxes (air samples). Table 15 results WP5.2.1 Methodology Study 08. Croatia day 4. Table 16 results WP5.2.1 Methodology Study 08. Croatia day 4. Chronological order for sampling of filters. Table 17 results WP5.2.1 Methodology Study 08. Croatia day 4. s related to sampling of fresh air at mine. Table 18 results WP5.2.1 Methodology Study 08. Croatia day 4. s related to box (air samples). Table 19 results WP5.2.1 Methodology Study 07. Croatia day 4. s related to sampling between boxes (air samples). Table 20 results WP5.2.1 Methodology Study 08. Croatia day 4. s related from sampling of new line (air samples). vi/ ix

7 Report, WP Methodology Study 08, CROATIA Table 21 results WP Methodology Study 08. Croatia day 4. s related to sampling of new line (soil samples). Table 22 results WP5.2.1 Methodology Study 08. Croatia day 4. s related to line (air samples). Table 23 results WP5.2.1 Methodology Study 08. Croatia day 4. s related to line (soil samples). Table 24 results WP5.2.1 Methodology Study 08. Croatia day 5. Table 25 results WP5.2.1 Methodology Study 08. Croatia day 5. Chronological order for sampling of filters. Table 26 results WP5.2.1 Methodology Study 08. Croatia day 5. s related to sampling of fresh air at mine. Table 27 results WP5.2.1 Methodology Study 08. Croatia day 5. s related to box (air samples). Table 28 results WP5.2.1 Methodology Study 08. Croatia day 5. s related to sampling between boxes (air samples). Table 29 results WP5.2.1 Methodology Study 08. Croatia day 5. s related to line (air samples). Table 30 results WP5.2.1 Methodology Study 08. Croatia day 5. s related to line (soil samples). Table 31 results WP5.2.1 Methodology Study 08. Croatia day 6. Table 32 results WP5.2.1 Methodology Study 08. Croatia day 6. Chronological order for sampling of filters. Table 33 results WP5.2.1 Methodology Study 08. Croatia day 6. Sampling of fresh air at mine. Table 34 results WP5.2.1 Methodology Study 08. Croatia day 6. s related to box (air samples). Table 35 results WP5.2.1 Methodology Study 08. s from sampling between boxes. Table 36 results WP5.2.1 Methodology Study 08. Croatia day 6. s related to sampling in boxes (soil samples). Table 37 results WP5.2.1 Methodology Study 08. Croatia day 6. Reference tests. Table 38 results WP5.2.1 Methodology Study 08. Control filters left behind in Sweden. Table 39 results WP5.2.1 Methodology Study 08. s sampling in boxes (air samples) Appendix 1 Appendix 2 Appendix 3 Mine Portfolio Weather Data APPENDICES vii/ ix

8 Report, WP Methodology Study 08, CROATIA Abbreviations Abbreviation BAAB DNT ERC FOI LOD NPA R&D SOP SRSA Tetryl TNT TS UN Definition Biosensor Applications AB Dinitrotoluene Exploded Related Compounds Swedish Defence Research Agency Limit of Detection Norwegian Peoples Aid Research and Development Standard Operation Procedures Swedish Rescue Service Agency Trinitrophenylmetylnitramine (military high explosive) Trinitrotoluene (military high explosive) Torr Substans (Swedish for Dry Substance) United Nations viii/ ix

9 Report, WP Methodology Study 08, CROATIA Definitions Environmental Phase Period Programme Protocol Report G N Reference Sampling of Personnel in box before plant of mine, (air sample) in box before plant of mine, (soil sample) Up-wind Sampling of one filter during certain conditions. A test sampled upwards the direction of wind outside the test area. A number of The calendar time at the Site A document that describes which that shall be performed. A pamphlet for test in a certain Programme Evaluation of results from the Period Older type of filter Newer type of filter with objective to control the Logistic Chain. with objective to establish samples from test personnel and test personnel clothing to avoid false alarms due to contamination. with objective to establish a chromatogram (based on air samples from box) for the actual box before plant of mine. with objective to establish a chromatogram (based on soil samples from box) for the actual box before plant of mine. For example at Nordic wind, meaning the wind blows from the north, up-wind is defined as north direction. ix/ ix

10 Report WP Methodology Study 08, CROATIA 1 WP METHODOLOGY STUDY 08, CROATIA, SHORT INTRODUCTION This document comprises the Report from the tests conducted under the WP Methodology Study 08 in Croatia during week 336 and 337 in September WP is a part of the WP 5, and Evaluation, within the EU Project Biosens IST Refer to EU document Annex 1, Description of Work, 05/12/2000-IST (). Plantation of test mines in the 16 boxes and in the permanent test line number 4 were performed during week 215( April 2002) in accordance to Methodology Study 01. The main objectives with WP Methodology Study 08 in Croatia were : Sampling of air in the boxes above planted mines. Collection of soil samples in the boxes above planted mines after air sampling Sampling of air and soil above the planted Mines. Verify the logistical chain; from sampling of filters inclusive of analyses in the laboratory for confirmation of its functionality in a sufficient way. (Reference s). Comparison in yield between Biosensor System and Mine Detection Dogs. The submitted instructions from Biosensor Applications AB concerning Handling and Operation of Equipment and Storage and Transportation of filters have been applied during the tests. For Handling and Operation of Equipment refer to Operational Manual and System Description from Biosensor Applications AB, see paragraph 5. For Storage and Transportation of filters refer to instructions from Biosensor Applications AB, see paragraph 5. For conduction of test, refer to Protocol Methodology study 08, paragraph 5. All filters were transported for analyses with gas chromatograph to Biosensor Applications AB s premises in Stockholm. All classification of test results from analyses in gas chromatograph were performed by Biosensor Applications AB personnel. See paragraph 5. The submitted instructions from FOI concerning Handling, Storage and Transportation of soil samples have been applied, refer to paragraph 5. All soil samples were transported from the test site to FOI s premises in Stockholm. All classification of test results were performed by FOI personnel. 1/ 43

11 Report WP Methodology Study 08, CROATIA 2 WP METHODOLOGY STUDY 08, CROATIA, TEST The number of samples during WP Methodology Study 08 in Croatia were 148 samples in total (120N and 28S). According to the Programme 220 samples were planned to be collected (192N and 28S). The Period was carried out during 6 working days at the SRSA Croatian Site. The type of mines are presented in appendix 2. For information about the test site refer to paragraph 5. In the test site specially prepared boxes of 10 times 10 meter are marked out. One mine is planted in each box. The types of mine planted are presented in appendix 1, box by box. In table 1 a summary of the activities performed day by day plus results during WP Methodology Study 08 in Croatia is presented: Day Denomination* Control filter (Left behind in Sweden) Filters estimated no./ Yield Filter No.** 10N/10N 08N5, 08N12, 08N17, 08N44, 08N102, 08N128, 08N153, 08N163, 08N168, 08N200 Discarded filter Numbers Yield*** Explosive Related Compounds (ERC) TNT/DNT Preparations Cleaning of Personnel Control filters 10N/10N 08N30, 08N48, 08N50, 08N63, 08N83, 08N100, 08N126, 08N130, 08N146, 08N164 See paragraph Sampling of fresh air at mine Sampling in boxes (air) above planted permanent Mine Sampling between boxes 16N/2N 08N198, 08N134 Severe weather conditions 16N/3N 08N77, 08N68, 08N158 Severe weather conditions + 08N158 13N/2N 08N18, 08N154 Severe weather conditions + 08N Sampling of fresh air at hotel 2N/2N 08N75, 08N Sampling of 6N/6N 08N175, 08N152, + 2/ 43

12 Report WP Methodology Study 08, CROATIA Day Denomination* Filters estimated no./ Yield Filter No.** Discarded filter Numbers Yield*** Explosive Related Compounds (ERC) TNT/DNT personnel and hotel premises 08N91, 08N188, 08N173, 08N103 08N Sampling of fresh air at mine 16N/4N 08N93, 08N7, 08N23, 08N Sampling in boxes (air) above planted permanent Mine 16N/4N 08N70, 08N190, 08N182, 08N Sampling between boxes 12N/3N 08N49, 08N150, 08N Sampling in boxes (air) above planted permanent Mine 16N/8N 08N45, 08N39, 08N25, 08N3, 08N27, 08N119, 08N120, 08N Sampling between boxes 13N/6N 08N111, 08N196, 08N174, 08N113, 08N74, 08N Sampling of fresh air at mine 16N/8N 08N1, 08N76, 08N97, 08N129, 08N123, 08N194, 08N88, 08N of new line (air samples) 4N/4N 08N52, 08N19, 08N78, 08N Sampling above permanent test mine (air samples) 4N/4N 08N170, 08N199, 08N189, 08N of new line (soil samples) 4S/4S 08S1, 08S2, 08S3, 08S4 + 08S1, 08S2, 08S3, 08S Sampling above permanent test mine (soil samples) 4S/4S 08S5, 08S6, 08S7, 08S8 + 08S5, 08S6, 08S7, 08S Sampling of fresh air at mine 4N/3N 08N59, 08N57, 08N69 Without support ring 08N69 with support ring + 08N57*, 08N59* Sampling in boxes (air) above none/8n 08N34, 08N179, 08N184, 08N131, Without support ring + 3/ 43

13 Report WP Methodology Study 08, CROATIA Day Denomination* Filters estimated no./ Yield Filter No.** Discarded filter Numbers Yield*** Explosive Related Compounds (ERC) TNT/DNT planted permanent Mine 08N32, 08N35, 08N109, 08N118 08N32, 08N34, 08N35, 08N109*, 08N118* Sampling between boxes none/6n 08N40, 08115, 08N180, 08N42, 08N65, 08N54 Without support ring + 08N42*, 08N54, 08N65*, 08N Sampling above newly planted test mine (air) 4N/4N 08N60, 08N86, 08N162, 08N N Sampling above newly planted test mine (soil) 4S/4S 08S9, 08S10, 08S11, 08S S9, 08S10, 08S11, 08S Sampling in boxes (air) above planted permanent Mine Sampling of fresh air at mine Sampling between boxes Sampling in boxes (soil) above planted permanent Mine none/5n 08N177, 08N36, 08N110, 08N104, 08N107 2N/5N 08N151, 08N61, 08N142, 08N185, 08N176 none/5n 08N9, 08N167, 08N4, 08N89, 08N55 16S/16S 08S13, 08S14, 08S21, 08S20, 08S15, 08S16, 08S17, 08S18, 08S19, 08S23, 08S22, 08S25, 08S26, 08S24, 08S27, 08S Reference tests 8N/8N 08N37, 08N136, 08N157, 08N92, 08N121, 08N192, 08N147, 08N191 Total no. of filter: 148 pct (220 pct.) 120N (192N) +28S (28S) 4/ N S13, 08S14, 08S21, 08S20, 08S15, 08S16, 08S17, 08S18, 08S19, 08S22, 08S25, 08S26, 08S24, 08S27, 08S N37, 08N136, 08N157, 08N92, 08N121, 08N192, 08N147, 08N191 Table 1 Summary activities day by day, WP Methodology Study 08 Croatia. Parenthesis shows amount of samples originally planned. In the planned number 192 N within brackets 4 environmental test are included. These test were not executed according to the Programme due to severe weather conditions. * For definitions of test procedures refer to Biosens WP5.2.1 Methodology 08, CROATIA Programme, SRSA rev1, dated 22/August/2003. For samples marked with * in column yield these samples had not been positive for a LOD of 100 pg (TNT/DNT).

14 Report WP Methodology Study 08, CROATIA ** N= New type of filter, S= Soil Sample, see paragraph 5. ***The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This AB s personnel. (For filters without support ring the LOD was for DNT= 50 [pg] and TNT= 50 [pg]). ***The evaluation of the test results (soil samples) are based on FOI instructions regarding LOD ( Limit of Detection) for DNT= 10 [pg/g TS], TNT= 10[pg/g TS]. This evaluation is performed by LC-MS. All evaluations of the test results (soil samples) were performed by FOI personnel. Note: Due to severe weather conditions the test programme had to be rescheduled. The number of test according to the Programme were reduced with 72 filters. No Environmental test were performed during this test occasion. 3 WP METHODOLOGY 08 CROATIA, RESULTS In the table 2 below a summary of Controls is presented: Denomination No. of filters + No. of filters? No. of filters - Total No. of filters Planned No. of filters Reference s Environmental s Samples between boxes Control Samples, prepared at the hotel Fresh air samples, at hotel premises Fresh air samples, in mine of new line before plantation Control Samples, left behind in Sweden Σ Table 2 Summary Controls regarding TNT/DNT presence, WP Methodology Study 08 Croatia. The results above shows a rate for the Reference tests to 100% positive for TNT and DNT alarm as expected, 8 samples positive of 8 in total. The results also shows the control filters and control filters left behind in Sweden to have a false alarm rate of 0%, no samples positive of 20 in total. No positive alarms were expected. Sampling between boxes shows 5 samples positive ( + ) for TNT or DNT of 23 in total, approximately 22%. Sampling of Fresh air at mine shows 2 samples positive for TNT or DNT of 22 in total, approximately 9%. 5/ 43

15 Report WP Methodology Study 08, CROATIA The test results have carefully been analysed. The points listed below have especially been studied : 1. Chronological order for sampling of filters 2. s related to box 3. s related to line 4. s from sampling of Personnel 5. s related from Sampling of fresh air 6. Reference s and Control filters In the following paragraph the results from the tests are presented. Explanations to colour coding for samples: Positive Alarm,TNT(Alarm Expected) Negative False Alarm,TNT (Alarm Expected) Positive Alarm, only DNT (Alarm Expected) No Alarm as Expected (Alarm not Expected) Positive Alarm TNT/DNT (No Alarm Expected) 6/ 43

16 Report WP Methodology Study 08, CROATIA 3.1 s WP Methodology Study 08, Croatia day 1-2 The table below presents the test results from day 1-2: Day 1-2 Denomination Sample / Control filter, prepared at hotel 08N164 Prepared at Jan s hotel room Control filter, prepared at hotel 08N Control filter, prepared at hotel 08N Control filter, prepared at hotel 08N Control filter, prepared at hotel 08N Control filter, prepared at hotel 08N Control filter, prepared at hotel 08N Control filter, prepared at hotel 08N Control filter, prepared at hotel 08N Control filter, prepared at hotel 08N Sampling of fresh air at mine 08N198 06: Sampling of fresh air at mine 08N134 06: Sampling in boxes (air) above permanent test mine 08N : Sampling between boxes 08N18 07: Sampling in boxes (air) above permanent test mine 08N : Sampling between boxes 08N : Sampling in boxes (air) above permanent test mine Table 3 results WP5.2.1 Methodology Study 08, Croatia day N :34 Rain *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This 7/ 43

17 Report WP Methodology Study 08, CROATIA Comments to results WP Methodology Study 08, Croatia, day 1-2 The comments are divided according to the points listed in paragraph Chronological order for sampling of filters Day 2 Denomination Sample / Sampling of fresh air at mine 08N198 06: Sampling of fresh air at mine 08N134 06: Sampling in boxes (air) above permanent test mine 08N : Sampling between boxes 08N : Sampling in boxes (air) above permanent test mine 08N : Sampling between boxes 08N154 07: Sampling in boxes (air) above permanent test mine 08N :34 Rain Table 4 results WP5.2.1 Methodology Study 08, Croatia day 1-2. Chronological order for sampling of filters. Control filters are excluded. *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This Due to severe weather conditions day 2 the test programme had to be rescheduled s fresh air at mine The results related to sampling of fresh air at the hotel are presented in the table below: Day 2 Denomination Sample / Sampling of fresh air at mine 08N198 06: Sampling of fresh air at mine 08N134 06:50 Table 5 results WP5.2.1 Methodology Study 08, Croatia day 2, results related to sampling fresh air at mine. *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This 8/ 43

18 Report WP Methodology Study 08, CROATIA s realated to box (air samples) The results from sampling of Personnel are presented in the table below: Day 2 Denomination Sample / Sampling in boxes (air) above 08N :10 permanent test mine Sampling in boxes (air) above 08N :20 permanent test mine Sampling in boxes (air) above permanent test mine 08N :34 Table 6 results WP5.2.1 Methodology Study 08, Croatia day 2, results related to box *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This s from sampling between boxes Day 2 Denomination Sample / Sampling between boxes 08N : Sampling between boxes 08N154 07:25 Table 7 results WP5.2.1 Methodology Study 08, Croatia day 2, results related to sampling between boxes. *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This Reference s No Reference s were performed on day 1. 9/ 43

19 Report WP Methodology Study 08, CROATIA 3.2 s WP Methodology Study 08 Croatia day 3 The table below presents the test results from day 3: Day 3 Denomination Sample / Sampling of fresh air at hotel 08N75 15:29 Samp Sampling of fresh air at hotel 08N171 15:45 Samp Sampling of Personnel 08N175 16:00 Max Samp Sampling of Personnel 08N152 16:12 Peter Samp Sampling of Personnel 08N :33 Max s Vehicle Samp Sampling of Personnel 08N188 16:48 SRSA Vehicle Samp Sampling of Personnel 08N173 17:00 Steve s room Samp Sampling of Personnel 08N103 17:18 Storage room Samp Sampling of fresh air at mine 08N93 18:45 Samp Sampling of fresh air at mine 08N7 18:45 Samp Sampling in boxes (air) above permanent test mine 08N :05 Samp Sampling between boxes 08N49 19:10 Samp 1 3 and Sampling in boxes (air) above permanent test mine 08N :20 Samp Sampling between boxes 08N150 19:20 Samp 1 4 and Sampling in boxes (air) above permanent test mine 08N :28 Samp Sampling between boxes 08N6 19:32 Samp 1 9 and Sampling in boxes (air) above permanent test mine 08N :40 Samp Sampling of fresh air at mine 08N23 19:41 Samp Sampling of fresh air at mine 08N81 19:45 Samp 2 Table 8 results WP5.2.1 Methodology Study 08, Croatia day 3 10/ 43

20 Report WP Methodology Study 08, CROATIA *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This Comments to results WP5.2.1 Methodology Study 08, Croatia day 3 The comments are divided according to the points listed in paragraph Chronological order for sampling of filters Day 3 Denomination Sample / Sampling of fresh air at hotel 08N75 15:29 Samp Sampling of fresh air at hotel 08N171 15:45 Samp Sampling of Personnel 08N175 16:00 Max Samp Sampling of Personnel 08N152 16:12 Peter Samp Sampling of Personnel 08N :33 Max s Vehicle Samp Sampling of Personnel 08N188 16:48 SRSA Vehicle Samp Sampling of Personnel 08N173 17:00 Steve s room Samp Sampling of Personnel 08N103 17:18 Storage room Samp Sampling of fresh air at mine 08N93 18:45 Samp Sampling of fresh air at mine 08N7 18:45 Samp Sampling in boxes (air) above permanent test mine 08N :05 Samp Sampling between boxes 08N49 19:10 Samp 1 3 and Sampling in boxes (air) above permanent test mine 08N :20 Samp Sampling between boxes 08N150 19:20 Samp 1 4 and Sampling in boxes (air) above permanent test mine 08N :28 Samp Sampling between boxes 08N6 19:32 Samp 1 9 and Sampling in boxes (air) above permanent test mine 08N :40 Samp 2 11/ 43

21 Report WP Methodology Study 08, CROATIA Day 3 Denomination Sample / Sampling of fresh air at mine 08N23 19:41 Samp Sampling of fresh air at mine 08N81 19:45 Samp 2 Table 9 results WP5.2.1 Methodology Study 08, Croatia day 3. Chronological order for sampling of filters. *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This AB s personnel. + =positive TNT/DNT response, - =negative TNT/DNT response s related to samling of fresh air at hotel premises Day 3 Denomination Sample / Sampling of fresh air at hotel 08N75 15:29 Samp Sampling of fresh air at hotel 08N171 15:45 Samp 1 Table 10 results WP5.2.1 Methodology Study 08, Croatia day 3. s related to sampling of fresh air at hotel premises (outdoor). *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This s related to samling of fresh air at mine Day 3 Denomination Sample / Sampling of fresh air at mine 08N93 18:45 Samp Sampling of fresh air at mine 08N7 18:45 Samp Sampling of fresh air at mine 08N23 19:41 Samp Sampling of fresh air at mine 08N81 19:45 Samp 2 Table 11 results WP5.2.1 Methodology Study 08, Croatia day 3. s related to sampling of fresh air at mine. *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This 12/ 43

22 Report WP Methodology Study 08, CROATIA s from sampling of Personnel Day 3 Denomination Sample / Sampling of Personnel 08N175 16:00 Max Samp Sampling of Personnel 08N152 16:12 Peter Samp Sampling of Personnel 08N :33 Max s Vehicle Samp Sampling of Personnel 08N188 16:48 SRSA Vehicle Samp Sampling of Personnel 08N173 17:00 Steve s room Samp Sampling of Personnel 08N103 17:18 Storage room Samp 1 Table 12 results WP5.2.1 Methodology Study 08, Croatia day 3. of Personnel *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This s realated to box (air samples) Day 3 Denomination Sample / Sampling in boxes (air) above 08N :05 Samp 2 permanent test mine Sampling in boxes (air) above 08N :20 Samp 2 permanent test mine Sampling in boxes (air) above 08N :28 Samp 2 permanent test mine Sampling in boxes (air) above permanent test mine 08N :40 Samp 2 Table 13 results WP5.2.1 Methodology Study 08, Croatia day 3. s related to box (air samples). *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This 13/ 43

23 Report WP Methodology Study 08, CROATIA s from sampling between boxes Day 3 Denomination Sample / Sampling between boxes 08N49 Samp 1 3 and Sampling between boxes 08N150 19:20 Samp 1 4 and Sampling between boxes 08N6 19:32 Samp 1 9 and 10 Table 14 results WP5.2.1 Methodology Study 08, Croatia day 3. s related to sampling between boxes (air samples). *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This Reference s No Reference s were performed on day 3. 14/ 43

24 Report WP Methodology Study 08, CROATIA 3.3 s WP Methodology study 08 Croatia day 4 The table below presents the test results from day 4: Day 4 Denomination Sample / Sampling of fresh air at mine Sampling of fresh air at mine 08N1 09:10 Samp 1 08N76 09:10 Samp Sampling between boxes 08N111 09:35 Samp 2 16 and Sampling in boxes (air) 08N :43 Samp Sampling between boxes 08N196 09:50 Samp 2 14 and Sampling in boxes (air) Sampling in boxes (air) 08N :00 Samp 1 08N :05 Samp Sampling of fresh air at mine Sampling of fresh air at mine Sampling of fresh air at mine Sampling of fresh air at mine Sampling in boxes (air) 08N97 10:20 Samp 2 South of box 16 08N129 10:20 Samp 1 South of box 16 08N123 10:35 Samp 2 South of box 13 08N194 10:35 Samp 1 South of box 13 08N :45 Samp Sampling between boxes 08N174 11:45 Samp 2 12 and Sampling between boxes 08N113 12:05 Samp 2 12 and Sampling in boxes (air) 08N :08 Samp 1 15/ 43

25 Report WP Methodology Study 08, CROATIA Day 4 Denomination Sample / Sampling between boxes 08N74 12:17 Samp 2 7 and Sampling between boxes 08N31 12:30 Samp 2 6 and Sampling in boxes (air) Sampling in boxes (air) Sampling in boxes (air) Sampling of fresh air at mine Sampling of fresh air at mine 08N :35 Samp 1 08N :46 Samp 2 08N :00 Samp 2 08N88 13:00 Samp 1 08N73 13:00 Samp of new line (air) 08N52 2:1 15:55 Samp of new line (air) 08N19 2:2 15:55 Samp of new line (air) 08N78 2:3 16:15 Samp of new line (air) 08N85 2:4 16:15 Samp of new line (soil) 08S1 2: of new line (soil) 08S2 2: of new line (soil) 08S3 2: of new line (soil) 08S4 2: Sampling above planted permanent test mine (air) Sampling above planted permanent test mine (air) Sampling above planted permanent test mine (air) Sampling above planted permanent test mine (air) Sampling above planted permanent test mine (soil) Sampling above planted permanent test mine (soil) Sampling above planted permanent test mine (soil) Sampling above planted permanent test mine (soil) 08N170 4:1 16:45 Samp 1 08N199 4:2 16:45 Samp 2 08N189 4:3 17:00 Samp 1 08N84 4:4 17:00 Samp 2 08S5 4:1 66 1,7 08S6 4: S7 4: S8 4:4 111 Table 15 results WP5.2.1 Methodology Study 08, Croatia day 4. Level for soil samples are given in ng/ g TS. 16/ 43

26 Report WP Methodology Study 08, CROATIA *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This ***The evaluation of the test results (soil samples) are based on FOI instructions regarding LOD ( Limit of Detection) for DNT= 10 [pg/g TS], TNT= 10[pg/g TS]. This evaluation is performed by LC-MS. All evaluations of the test results (soil samples) were performed by FOI personnel Comments to results WP5.2.1 Methodology Study 08, Croatia day 4 The comments are divided according to the points listed in paragraph Chronological order for sampling of filters Day 4 Denomination Sample / Sampling of fresh air at mine Sampling of fresh air at mine 08N1 09:10 Samp 1 08N76 09:10 Samp Sampling between boxes 08N111 09:35 Samp 2 16 and Sampling in boxes (air) 08N :43 Samp Sampling between boxes 08N196 09:50 Samp 2 14 and Sampling in boxes (air) Sampling in boxes (air) 08N :00 Samp 1 08N :05 Samp Sampling of fresh air at mine Sampling of fresh air at mine Sampling of fresh air at mine Sampling of fresh air at mine 08N97 10:20 Samp 2 South of box 16 08N129 10:20 Samp 1 South of box 16 08N123 10:35 Samp 2 South of box 13 08N194 10:35 Samp 1 South of box 13 17/ 43

27 Report WP Methodology Study 08, CROATIA Day 4 Denomination Sample / Sampling in boxes (air) 08N :45 Samp Sampling between boxes 08N174 11:45 Samp 2 12 and Sampling between boxes 08N113 12:05 Samp 2 12 and Sampling in boxes (air) 08N :08 Samp Sampling between boxes 08N74 12:17 Samp 2 7 and Sampling between boxes 08N31 12:30 Samp 2 6 and Sampling in boxes (air) Sampling in boxes (air) Sampling in boxes (air) Sampling of fresh air at mine Sampling of fresh air at mine 08N :35 Samp 1 08N :46 Samp 2 08N :00 Samp 2 08N88 13:00 Samp 1 08N73 13:00 Samp of new line (air) 08N52 2:1 15:55 Samp of new line (air) 08N19 2:2 15:55 Samp of new line (air) 08N78 2:3 16:15 Samp of new line (air) 08N85 2:4 16:15 Samp Sampling above planted permanent test mine (air) Sampling above planted permanent test mine (air) Sampling above planted permanent test mine (air) Sampling above planted permanent test mine (air) 08N170 4:1 16:45 Samp 1 08N199 4:2 16:45 Samp 2 08N189 4:3 17:00 Samp 1 08N84 4:4 17:00 Samp 2 Table 16 results WP5.2.1 Methodology Study 08, Croatia day 4. Chronological order for sampling of filters. *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This 18/ 43

28 Report WP Methodology Study 08, CROATIA *The evaluation of the tests results (soil samples) are based on FOI instructions regarding LOD (Limit of Detection) for DNT= 10 [pg/g TS], TNT= 10 [pg/g TS]. This evaluation is performed by LC-MS. All evaluations of the test results (soil samples) were performed by FOI personnel s related to samling of fresh air at mine Day 4 Denomination Sample / Sampling of fresh air at mine Sampling of fresh air at mine Sampling of fresh air at mine Sampling of fresh air at mine Sampling of fresh air at mine Sampling of fresh air at mine Sampling of fresh air at mine Sampling of fresh air at mine 08N1 09:10 Samp 1 08N76 09:10 Samp 2 08N97 10:20 Samp 2 South of box 16 08N129 10:20 Samp 1 South of box 16 08N123 10:35 Samp 2 South of box 13 08N194 10:35 Samp 1 South of box 13 08N88 13:00 Samp 1 08N73 13:00 Samp 2 Table 17 results WP5.2.1 Methodology Study 08, Croatia day 4. Sampling of fresh air at mine. *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This s realated to box (air samples) Day 4 Denomination Sample / Sampling in boxes (air) Sampling in boxes (air) Sampling in boxes (air) 08N :43 Samp 1 08N :00 Samp 1 08N :05 Samp 2 19/ 43

29 Report WP Methodology Study 08, CROATIA Day 4 Denomination Sample / Sampling in boxes (air) 08N :45 Samp Sampling in boxes (air) Sampling in boxes (air) Sampling in boxes (air) Sampling in boxes (air) 08N :08 Samp 1 08N :35 Samp 1 08N :46 Samp 2 08N :00 Samp 2 Table 18 results WP5.2.1 Methodology Study 08, Croatia day 4. s related to box (air samples). *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This s from sampling between boxes Day 4 Denomination Sample / 20/ Sampling between boxes 08N111 09:35 Samp 2 16 and Sampling between boxes 08N196 09:50 Samp 2 14 and Sampling between boxes 08N174 11:45 Samp 2 12 and Sampling between boxes 08N113 12:05 Samp 2 12 and Sampling between boxes 08N74 12:17 Samp 2 7 and Sampling between boxes 08N31 12:30 Samp 2 6 and 1 Table 19 results WP5.2.1 Methodology Study 08, Croatia day 4. s related to sampling between boxes (air samples).

30 Report WP Methodology Study 08, CROATIA *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This s from sampling of new line (air) Day 4 Denomination Sample / of new line (air) 08N52 2:1 15:55 Samp of new line (air) 08N19 2:2 15:55 Samp of new line (air) 08N78 2:3 16:15 Samp of new line (air) 08N85 2:4 16:15 Samp 2 Table 20 results WP5.2.1 Methodology Study 08, Croatia day 4. s from sampling of new line (air samples). *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This s from sampling of new line (soil) Day 4 Denomination Sample / of new line (soil) 08S1 2: of new line (soil) 08S2 2: of new line (soil) 08S3 2: of new line (soil) 08S4 2:4 50 Table 21 results WP5.2.1 Methodology Study 08, Croatia day 4. s from sampling of new line (soil samples). The levels are given in ng/ g TS. ***The evaluation of the test results (soil samples) are based on FOI instructions regarding LOD ( Limit of Detection) for DNT= 10 [pg/g TS], TNT= 10[pg/g TS]. This evaluation is performed by LC-MS. All evaluations of the test results (soil samples) were performed by FOI personnel. 21/ 43

31 Report WP Methodology Study 08, CROATIA s related to line (air) Day 4 Denomination Sample / Sampling above planted permanent test mine (air) Sampling above planted permanent test mine (air) Sampling above planted permanent test mine (air) Sampling above planted permanent test mine (air) 08N170 4:1 16:45 Samp 1 08N199 4:2 16:45 Samp 2 08N189 4:3 17:00 Samp 1 08N84 4:4 17:00 Samp 2 Table 22 results WP5.2.1 Methodology Study 08, Croatia day 4. s related to line (air samples). *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This s related to line (soil) Day 4 Denomination Sample / Sampling above planted permanent test mine (soil) Sampling above planted permanent test mine (soil) Sampling above planted permanent test mine (soil) Sampling above planted permanent test mine (soil) 08S5 4:1 66 1,7 08S6 4: S7 4: S8 4:4 111 Table 23 results WP5.2.1 Methodology Study 08, Croatia day 4. s related to line (soil samples). The levels are given in ng/ g TS. *The evaluation of the test results (soil samples) are based on FOI instructions regarding LOD ( Limit of Detection) for DNT= 10 [pg/g TS], TNT= 10[pg/g TS]. This evaluation is performed by LC-MS. All evaluations of the test results (soil samples) were performed by FOI personnel Reference s No Reference s were performed on day 4. 22/ 43

32 Report WP Methodology Study 08, CROATIA 3.4 s WP Methodology study 08 Croatia day 5 The table below presents the test results from day 5: Day 5 Denomination Sample / Sampling of fresh air at mine Sampling in boxes (air) 08N59 (+) 09:15 Samp 2 08N :45 Samp Sampling between boxes 08N40 10:00 Samp 2 16 and Sampling of fresh air at mine Sampling in boxes (air) Sampling above newly planted test mine (air) Sampling above newly planted test mine (air) 08N69 10:04 Samp 1 08N :04 Samp 2 08N60 10:14 Samp 1 08N86 10:22 Samp Sampling between boxes 08N115 10:30 Samp 2 14 and Sampling above newly planted test mine (air) Sampling above newly planted test mine (air) Sampling in boxes (air) Sampling of fresh air at mine Sampling in boxes (air) 08N :31 Samp 1 08N71 10:40 Samp 1 08N :40 Samp 2 08N57 (+) + 10:45 Samp 2 08N :00 Samp Sampling between boxes 08N180 (+) + 11:13 Samp 2 13 and Sampling in boxes (air) 08N :25 Samp Sampling between boxes 08N42 (+) 11:37 Samp 2 12 and Sampling in boxes (air) 08N35 7 (+) + 11:50 Samp Sampling between boxes 08N65 (+) 12:04 Samp 2 7 and 6 23/ 43

33 Report WP Methodology Study 08, CROATIA Day 5 Denomination Sample / Sampling in boxes (air) 08N109 6 (+) 12:15 Samp Sampling between boxes 08N :27 Samp 2 6 and Sampling in boxes (air) Sampling above newly planted test mine (soil) Sampling above newly planted test mine (soil) Sampling above newly planted test mine (soil) Sampling above newly planted test mine (soil) 08N118 1 (+) 12:40 Samp 2 08S S ,9 08S S Table 24 results WP5.2.1 Methodology Study 08, Croatia day 5. The levels for soil samples are given in ng/ g TS. *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This (+) represents a LOD between pg. *The evaluation of the test results (soil samples) are based on FOI instructions regarding LOD ( Limit of Detection) for DNT= 10 [pg/g TS], TNT= 10[pg/g TS]. This evaluation is performed by LC-MS. All evaluations of the test results (soil samples) were performed by FOI personnel Comments to results WP5.2.1 Methodology Study 08, Croatia day 5 The comments are divided according to the points listed in paragraph Chronological order for sampling of filters Day 5 Denomination Sample / Sampling of fresh air at mine Sampling in boxes (air) 24/ 43 08N59 (+) 09:15 Samp 2 08N :45 Samp Sampling between boxes 08N40 10:00 Samp 2 16 and Sampling of fresh air at mine 08N69 10:04 Samp 1

34 Report WP Methodology Study 08, CROATIA Day 5 Denomination Sample / Sampling in boxes (air) Sampling above newly planted test mine (air) Sampling above newly planted test mine (air) 08N :04 Samp 2 08N60 10:14 Samp 1 08N86 10:22 Samp Sampling between boxes 08N115 10:30 Samp 2 14 and Sampling above newly planted test mine (air) Sampling above newly planted test mine (air) Sampling in boxes (air) Sampling of fresh air at mine Sampling in boxes (air) 08N :31 Samp 1 08N71 10:40 Samp 1 08N :40 Samp 2 08N57 (+) + 10:45 Samp 2 08N :00 Samp Sampling between boxes 08N180 (+) + 11:13 Samp 2 13 and Sampling in boxes (air) 08N :25 Samp Sampling between boxes 08N42 (+) 11:37 Samp 2 12 and Sampling in boxes (air) 08N35 7 (+) + 11:50 Samp Sampling between boxes 08N65 (+) 12:04 Samp 2 7 and Sampling in boxes (air) 08N109 6 (+) 12:15 Samp Sampling between boxes 08N :27 Samp 2 6 and Sampling in boxes (air) 08N118 1 (+) 12:40 Samp 2 Table 25 results WP5.2.1 Methodology Study 08, Croatia day 5. Chronological order for sampling of filters. *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This (+) represents a LOD between pg. 25/ 43

35 Report WP Methodology Study 08, CROATIA *The evaluation of the test results (soil samples) are based on FOI instructions regarding LOD ( Limit of Detection) for DNT= 10 [pg/g TS], TNT= 10[pg/g TS]. This evaluation is performed by LC-MS. All evaluations of the test results (soil samples) were performed by FOI personnel s realted to sampling of fresh air at mine Day 5 Denomination Sample / Sampling of fresh air at mine Sampling of fresh air at mine Sampling of fresh air at mine 08N59 (+) 09:15 Samp 2 08N69 10:04 Samp 1 08N57 (+) + 10:45 Samp 2 Table 26 results WP5.2.1 Methodology Study 08, Croatia day 5. s related to sampling of fresh air at mine. *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This (+) represents a LOD between pg s realated to box (air samples) Day 5 Denomination Sample / Sampling in boxes (air) Sampling in boxes (air) Sampling in boxes (air) Sampling in boxes (air) Sampling in boxes (air) Sampling in boxes (air) Sampling in boxes (air) Sampling in boxes (air) 26/ 43 08N :45 Samp 08N :04 Samp 2 08N :40 Samp 2 08N :00 Samp 2 08N :25 Samp 2 08N35 7 (+) + 11:50 Samp 2 08N109 6 (+) 12:15 Samp 2 08N118 1 (+) 12:40 Samp 2 Table 27 results WP5.2.1 Methodology Study 08, Croatia day 5. s related to box (air samples). (+) represents a LOD between pg.

36 Report WP Methodology Study 08, CROATIA *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This s from sampling between boxes Day 5 Denomination Sample / Sampling between boxes 08N40 10:00 Samp 2 16 and Sampling between boxes 08N115 10:30 Samp 2 14 and Sampling between boxes 08N180 (+) + 11:13 Samp 2 13 and Sampling between boxes 08N42 (+) 11:37 Samp 2 12 and Sampling between boxes 08N65 (+) 12:04 Samp 2 7 and Sampling between boxes 08N :27 Samp 2 6 and 1 Table 28 results WP5.2.1 Methodology Study 08, Croatia day 5. s related to sampling between boxes (air samples). *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This (+) represents a LOD between pg. 27/ 43

37 Report WP Methodology Study 08, CROATIA s related to line (air samples) Day 5 Denomination Sample / Sampling above newly planted test mine (air) Sampling above newly planted test mine (air) Sampling above newly planted test mine (air) Sampling above newly planted test mine (air) 08N60 10:14 Samp 1 08N86 10:22 Samp 1 08N :31 Samp 1 08N71 10:40 Samp 1 Table 29 results WP5.2.1 Methodology Study 08, Croatia day 5. s related to line (air samples). Newly planted mines. *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This s related to line (soil samples) Day 5 Denomination Sample / Sampling above newly planted test mine (soil) Sampling above newly planted test mine (soil) Sampling above newly planted test mine (soil) Sampling above newly planted test mine (soil) 08S S ,9 08S S Table 30 results WP5.2.1 Methodology Study 08, Croatia day 5. s related to line (soil samples). Newly planted mines. The levels are given in ng/ g TS. ***The evaluation of the test results (soil samples) are based on FOI instructions regarding LOD ( Limit of Detection) for DNT= 10 [pg/g TS], TNT= 10[pg/g TS]. This evaluation is performed by LC-MS. All evaluations of the test results (soil samples) were performed by FOI personnel Reference s No Reference s were performed on day 5. 28/ 43

38 Report WP Methodology Study 08, CROATIA 3.5 s WP Methodology study 08 Croatia day 6 The table below presents the test results from day 6: Day 6 Denomination Sample / Sampling of fresh air at mine Sampling of fresh air at mine 08N151 09:30 Samp 1 08N61 09:30 Samp Sampling between boxes 08N9 09:45 Samp 2 between box 2 and Sampling in boxes (air) 08N :50 Samp Sampling between boxes 08N167 09:55 Samp 2 between box 5 and Sampling in boxes (air) Sampling of fresh air at mine Sampling in boxes (air) Sampling of fresh air at mine Sampling of fresh air at mine 08N :00 Samp 1 08N142 10:08 Samp 2 between box 8 and 11 08N :15 Samp 1 08N185 10:25 Samp 2 08N176 10:30 Samp 1 between box 8 and Sampling between boxes 08N4 10:35 Samp 2 between box 10 and Sampling in boxes (air) 08N :40 Samp Sampling between boxes 08N89 10:45 Samp 2 between box 10 and Sampling in boxes (air) 08N :54 Samp Sampling between boxes 08N55 11:04 Samp 1 between box 10 and Reference 08N :15 Samp Reference 08N :22 Samp Reference 08N :26 Samp Reference 08N :32 Samp Reference 08N :37 Samp 1 29/ 43

39 Report WP Methodology Study 08, CROATIA Day 6 Denomination Sample / Reference 08N :42 Samp Reference 08N :47 Samp Reference 08N :52 Samp 2 08S :12 08S ,6 13:15 08S :16 08S :18 08S :21 08S :22 08S :24 08S :24 08S :25 08S :25 08S :25 08S :30 08S :30 08S :30 08S :32 08S :33 Table 31 results WP5.2.1 Methodology Study 08, Croatia day 6. *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This ***The evaluation of the test results (soil samples) are based on FOI instructions regarding LOD ( Limit of Detection) for DNT= 10 [pg/g TS], TNT= 10[pg/g TS]. This evaluation is performed by LC-MS. All evaluations of the test results (soil samples) were performed by FOI personnel. 30/ 43

40 Report WP Methodology Study 08, CROATIA Comments to results WP5.2.1 Methodology Study 08, Croatia day 6 The comments are divided according to the points listed in paragraph Chronological order for sampling of filters Day 6 Denomination Sample / Sampling of fresh air at mine Sampling of fresh air at mine 08N151 09:30 Samp 1 08N61 09:30 Samp Sampling between boxes 08N9 09:45 Samp 2 between box 2 and Sampling in boxes (air) 08N :50 Samp Sampling between boxes 08N167 09:55 Samp 2 between box 5 and Sampling in boxes (air) Sampling of fresh air at mine Sampling in boxes (air) Sampling of fresh air at mine Sampling of fresh air at mine 08N :00 Samp 1 08N142 10:08 Samp 2 between box 8 and 11 08N :15 Samp 1 08N185 10:25 Samp 2 08N176 10:30 Samp 1 between box 8 and Sampling between boxes 08N4 10:35 Samp 2 between box 10 and Sampling in boxes (air) 08N :40 Samp Sampling between boxes 08N89 10:45 Samp 2 between box 10 and Sampling in boxes (air) 08N :54 Samp Sampling between boxes 08N55 11:04 Samp 1 between box 10 and Reference 08N :15 Samp 1 31/ 43

41 Report WP Methodology Study 08, CROATIA Day 6 Denomination Sample / Reference 08N :22 Samp Reference 08N :26 Samp Reference 08N :32 Samp Reference 08N :37 Samp Reference 08N :42 Samp Reference 08N :47 Samp Reference 08N :52 Samp 2 08S :12 08S ,6 13:15 08S :16 08S :18 08S :21 08S :22 08S :24 08S :24 08S :25 08S :25 08S :25 08S :30 08S :30 08S :30 08S :32 08S :33 Table 32 results WP5.2.1 Methodology Study 08, Croatia day 6. Chronological order for sampling of filters. The levels for soil samples are given in ng/ g TS. 32/ 43

42 Report WP Methodology Study 08, CROATIA *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This ***The evaluation of the test results (soil samples) are based on FOI instructions regarding LOD ( Limit of Detection) for DNT= 10 [pg/g TS], TNT= 10[pg/g TS]. This evaluation is performed by LC-MS. All evaluations of the test results (soil samples) were performed by FOI personnel s realted to sampling of fresh air at mine Day 6 Denomination Sample / Sampling of fresh air at mine Sampling of fresh air at mine Sampling of fresh air at mine Sampling of fresh air at mine Sampling of fresh air at mine 08N151 09:30 Samp 1 08N61 09:30 Samp 2 08N142 10:08 Samp 2 between box 8 and 11 08N185 10:25 Samp 2 08N176 10:30 Samp 1 between box 8 and 11 Table 33 results WP5.2.1 Methodology Study 08, Croatia day 6. Sampling of fresh air at mine. *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This s realated to box (air samples) Day 6 Denomination Sample / Sampling in boxes (air) Sampling in boxes (air) Sampling in boxes (air) Sampling in boxes (air) Sampling in boxes (air) 08N :50 Samp 1 08N :00 Samp 1 08N :15 Samp 1 08N :40 Samp 1 08N :54 Samp 1 Table 34 results WP5.2.1 Methodology Study 08, Croatia day 6. s related to box (air samples). *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This 33/ 43

43 Report WP Methodology Study 08, CROATIA s from sampling between boxes Day 6 Denomination Sample / Sampling between boxes 08N9 09:45 Samp 2 between box 2 and Sampling between boxes 08N167 09:55 Samp 2 between box 5 and Sampling between boxes 08N4 10:35 Samp 2 between box 10 and Sampling between boxes 08N89 10:45 Samp 2 between box 10 and Sampling between boxes 08N55 11:04 Samp 1 between box 10 and 15 Table 35 results WP5.2.1 Methodology Study 08, Croatia day 6. s from sampling between boxes. *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This s related to box (soil samples) Day 6 Denomination Sample / 08S :12 08S ,6 13:15 08S :16 08S :18 08S :21 08S :22 08S :24 08S :24 08S :25 34/ 43

44 Report WP Methodology Study 08, CROATIA Day 6 Denomination Sample / 08S :25 08S :25 08S :30 08S :30 08S :30 08S :32 08S :33 Table 36 results WP5.2.1 Methodology Study 08, Croatia day 6. s related to box (soil samples). The levels are given in ng/ g TS. *The evaluation of the test results (soil samples) are based on FOI instructions regarding LOD ( Limit of Detection) for DNT= 10 [pg/g TS], TNT= 10[pg/g TS]. This evaluation is performed by LC-MS. All evaluations of the test results (soil samples) were performed by FOI personnel Reference s Day 6 Denomination Sample / Reference 08N :15 Samp Reference 08N :22 Samp Reference 08N :26 Samp Reference 08N :32 Samp Reference 08N :37 Samp Reference 08N :42 Samp Reference 08N :47 Samp Reference 08N :52 Samp 2 Table 37 results WP5.2.1 Methodology Study 08, Croatia day 6. Reference test. *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This 35/ 43

45 Report WP Methodology Study 08, CROATIA 3.6 Control filters left behind in Sweden The table below presents the test results from blank filters left behind in Sweden: Denomination Sample Control filter (Left behind in Sweden) Control filter (Left behind in Sweden) Control filter (Left behind in Sweden) Control filter (Left behind in Sweden) Control filter (Left behind in Sweden) Control filter (Left behind in Sweden) Control filter (Left behind in Sweden) Control filter (Left behind in Sweden) Control filter (Left behind in Sweden) Control filter (Left behind in Sweden) 08N102 08N44 08N163 08N17 08N153 08N128 08N12 08N5 08N200 08N168 Table 38 results WP5.2.1 Methodology Study 08. Control filters left behind in Sweden. *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This All control filters left behind in Sweden were negative for both TNT and DNT as expected. 36/ 43

46 Report WP Methodology Study 08, CROATIA 3.8 Weather Conditions The weather conditions during the whole test period was: temperature in air 10-26ºC precipitation day 2 (Tuesday 02/September/2003) wind velocity 0-5 m/s Severe weather conditions day 2. Comparable weather conditions day 2, 4, 5 and 6. Refer to Appendix 3. For more metrological data refer to test protocol. 3.9 Comparison with Mine Detection Dogs Two Mine Detection Dogs were used during Methodology Study 08. The dogs were searching the box areas before the sampling of air took place. The dogs successfully pinpointed all the 16 planted test mines without any false alarms. ing in a yield of 100%. This successful performance was repeated the working day after. The fact that the MDD were able to pinpoint all the planted mines despite the rain indicates the dogs sensitivities for TNT/DNT detection to be extremely high. The dogs might not need the TNT/DNT to be accumulated on the soil top surfaces for their detection. It might be sufficient for the dogs to smell the continuously leakage of TNT/DNT vapour from the planted mines. On the other hand it might also indicate that the dogs use one or several other substance/substances than TNT/DNT (or in combination with TNT/DNT) as a marker for their assessment of the smelling patterns originated from mines. 37/ 43

47 Report WP Methodology Study 08, CROATIA 4 DISCUSSION AND CONCLUSIONS The results in Table 37, paragraph 3 shows a rate for the Reference tests to 100% positive TNT/DNT, 8 of 8 in total. Control filters left behind in Sweden showed no presence of TNT or DNT of 10 filters in total. Control filters prepared at hotel premises showed no presence of TNT or DNT of 10 filters in total. These results indicates the positive responses for TNT/DNT presence in the material to be generated from TNT/DNT present in the mine. These results also indicates the logistical chain from sampling of filters inclusive of analyses in the laboratory to be functional in a sufficient way. Thus results can be used for evaluation and fulfilment of the objectives for Methodology Study 08. The number of tests are not large enough to have a statistically significant material. Sampling of air in the boxes above planted mines and Sampling of air and soil above the planted Mines. es air samples Sampling in the 16 boxes took place day 2, 3, 4, 5 and 6. The yield day 2 was 1 sample positive for TNT of 3 in total. The yield day 3 was none of 4 in total. The yield day 4 was none sample positive for TNT of 8 in total The yield day 5 was 5 samples possible positive for TNT of 8 in total if the results are evaluated with a LOD of 50 pg. Otherwise 3 samples possible positive for TNT of 8 in total. Severe weather conditions day 2. The weather conditions were comparable day 3, 4, 5 and 6. Date of test day Filters estimated no. Yield Explosive Related Compounds (ERC) TNT/DNT None N 1N 1 + and N and N and N 5N (3N)** 5(3) + and 3(5) N 1N 1 + and 5 - Table 39 results WP5.2.1 Methodology Study 08. s sampling in boxes (air samples). *The evaluation of the tests results are based on LOD (Limit of Detection) for DNT= 100 [pg], TNT= 100 [pg]. This The table above shows the positive results regarding presence of TNT/DNT in boxes to be 7(5) of 28 in total, approximately 25%(11%). ** Day 5 was sampled with filters without support ring. Filters without support ring can be evaluated with a LOD of 50 pg. If the LOD is set to 100 pg for all filters the results presented within the brackets is achieved. 38/ 43

48 Report WP Methodology Study 08, CROATIA es soil samples The results regarding soil samples in boxes were 15 samples positive for TNT of 16 in total. Of these 15 soil samples in boxes were 3 samples also positive for DNT. s air samples Sampling s in line 4 took place day 4. The results were neither positive for TNT nor DNT. Sampling above new line (line 2) before plantation of mines took place day 4 and resulted in none (of 4 in total) positive response for TNT. Sampling above newly planted mines took place day 5 and resulted in 1 positive response for TNT. s soil samples Soil samples were collected in the new line (line 2) before plantation on day 4. The results show 4 samples positive for presence of TNT in 4 samples in total. Soil samples collected in the permanent test line (line 4) on day 4 show 4 samples positive for presence of TNT in 4 samples in total. One of those samples was also positive for DNT. Positive results regarding presence of TNT/DNT during Methodology Study 08, Croatia were predominantly taken place on day 5. This indicates the weather conditions to be more favourably on day 5 compared to the other test days. Severe weather conditions with rain day 2 in combination with wind might be one explanation for absence of positive results day 2. The rain day 2 might have washed away the accumulated compounds of TNT/DNT from the soil surface. The positive results day 5 indicates the levels of TNT/DNT concentration in the soil surface to be large enough for passing the threshold as a positive response with the available LOD for these test procedures. One explanation for the somewhat randomised pattern regarding presence of TNT/DNT in and between boxes might be caused by the wind. Improvements to the LOD better than 100 pg is desirable. The soil samples however seem to not have been influenced by the rain. Instead quite high levels of concentrations of TNT/DNT in ng /g TS have been found. Note that it seem to be TNT deposit also between the boxes. Comparison with Mine Detection Dogs Two Mine Detection Dogs were used during Methodology Study 08. The dogs were searching the box areas before the sampling of air took place. The dogs successfully pinpointed all the 16 planted test mines without any false alarms. ing in a yield of 100%. This successful performance was repeated the working day after. The fact that the MDD were able to pinpoint all the planted mines despite the rain indicates the dogs sensitivities for TNT/DNT detection to be extremely high. The dogs might not need the TNT/DNT to be accumulated on the soil top surfaces for their detection. It might be sufficient for the dogs to smell the continuously leakage of TNT/DNT vapour from the planted mines. On the other hand it might also indicate that the dogs use one or several other substance/substances than TNT/DNT (or in combination with TNT/DNT) as a marker for their assessment of the smelling patterns originated from mines. This last conclusion is supported by the test results from air sampling were the Biosensor System has detected TNT/DNT in spots between the planted mines (sampling between boxes). 39/ 43

49 Report WP Methodology Study 08, CROATIA 5 REFERENCE DOCUMENTS Handhavande av BAAB s insugningsutrustning K1020 N, (New filter version), 1AXNP Provprotokoll SRSA, Jan Gustafsson Cleaning of Personnel, SRSA Jan Gustafsson se instruktion för plantering av minor. Mine Equivalence, BAAB Handling, Storage and Transportation of soil samples, FOI se instruktion för jordprovstagning Recommended Sampling Data for new filter version, BAAB ( 3 minuter enligt muntlig överenskommelse ) Instruktion för plantering av minor, SRSA Jan Gustafsson, BI-M rev 1 Instruktion för jordprovstagning, SRSA Jan Gustafsson, BI-M rev 1 WP5.2.1 Methodology 08, CROATIA Programme, SRSA rev1, dated 22/August/2003. Resluts, air samples. dated 22/October/2003/, Lars Eng, BAAB. Resluts, soil samples.foi dated 01/October/2003, Lena Sarholm, FOI. 40/ 43

50 Report WP Methodology Study 08, CROATIA APPENDIX 1 Content SRSA Mine type 1 TMA-5 2 TMA-5 3 TMA-5 4 TMA-5 5 PMA-1 6 PMA-1 7 PMA-1 8 PMA-1 9 TMA-5 10 TMA-5 11 PMA-1 12 PMA-1 13 PMA-2 14 PMA-2 15 PMA-2 16 PMA-2 41/ 43

51 Report WP Methodology Study 08, CROATIA APPENDIX 2 Mine Portfolio Mine Model Type Explosive charge PROM-1 AP 423 g TNT PMR-2 AP 100 g TNT PMA-1 AP 200 g TNT PMA-2 AP 70 g TNT+30 g RDX PMA-3* AP 35 g VS-50 AP 43 g RDX TMA-5 AT 6,65 kg TNT TMA-2 AT 6,5 kg TNT Note: It has come to our knowledge that the Technical Annex, Description of Work 05/12/2000-IST () page 87 falsely states that PMA-3 contains 35g of TNT explosives. According to FOI and UN Mine Records, PMA-3 contains Tetryl and not TNT. 42/ 43

52 Report WP Methodology Study 08, CROATIA APPENDIX 3 Weather Data 43/ 43