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Development of Proficiency Testing for Detection of Irradiated Food: Project E01068. Results of Second Round PSL and TL Trials, September 2006

By D.C.W. Sanderson, L.A. Carmichael, S. Fisk, P. Key, E.M. Scott, M. Thompson, A. Alberti, M. Baden, S. Barth, N. Baumann, M. Bergman, R. Brockmann, P. Brown, J. Brunner, S. Buranasilp, B. Butz, J. Chan Sheot Harn, R. Das, F. Dittmar, C. Gemperle, J. Jung Heon, M. Iglovari, C. Kay, W. Kruspe, C. Lardner, S. MacFarlane, K. McKay, B. Muller, E. Niemi, M. Nuchter-Frangos, S. Onori, M. O'Sullivan, J. Pfordt, I. Poulima, M. Pugh, N. Sardone, C. Schleich, I-S. Song, I. Straub, S. Todoriki, A. Ward, C. Wiezorek and K. Woo Suk
Topics: GE
Publisher: Scottish Universities Environmental Research Centre
Year: 2007
OAI identifier: oai:eprints.gla.ac.uk:44637
Provided by: Enlighten

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  1. 0.00 maximum at 400°C, like blank
  2. 0.00 Signal starts before the relevant temperature range and rises through it up to 400°C without a distinct peak
  3. 0.00038weak peak at about 300
  4. 0.00110no peaks are visible 4.50 6656.00 0.00068no peaks are visible
  5. 0.00230weak peak at about 300°C 4.32 2703.00 0.00160weak peak at about 300°C
  6. 0.003 rise from 200°CMax at 320°C;very small signal 59028 1.8E+07 0.003 rise from 160°CMax at 340°C;very small signal
  7. 0.00364weak peak at about 300°C 27.70 8778.00 0.00316weak peak at 300°C
  8. 0.00415no peaks are visible 0.26 64.56 0.00397no peaks are visible
  9. 0.006 Max at 320°C 352618 2.9E+07 0.012 first peak at 195°C;new rise with second max at 320°C
  10. 0.008 no peak was observed
  11. 0.008 small shoulder at
  12. 0.01173weak peak at about 200°C 243.30 16973.00 0.01433weak peak at about 200°C
  13. 0.013 no peak was observed doi
  14. 0.01777no peaks are visible 0.25 165.50 0.00153no peaks are visible
  15. (1921). 0.02 breadth peak higher temp.
  16. 0.022 small shoulder at doi
  17. 0.027 Max at 190°C new rise from 280°C to 360°C; very small signals 5086 1148071 0.004 Max at 360°C
  18. 0.02853no peaks are visible 0.21 8.37 0.02557no peaks are visible
  19. 0.035 first peak at 220°C;second peak at 350°C very small signals 17697 1193987 0.015 rise from160°C; shoulder at 200°C;Max at 360°C
  20. 0.036 peak-max. by channel
  21. 0.04 breadth peak higher temp.
  22. 0.04281very weak peak at about 200
  23. 0.13 flat signal with peak at
  24. 0.19438peak at about 200°C 1.10 14.28 0.07675peak at about 200°C
  25. 0.19990peak at about 220°C 797.60 4162.00 0.19164peak at about 220°C
  26. 0.239 Max at 200°C; shoulder at 330°C 8817061 2.7E+07 0.321 Max at 205°C; shoulder at 330°C
  27. 0.96438peak at about 225 °C 13840.00 13907.00 0.99518peak at about 225 °C Table C.91 TL data for
  28. 1 TL reader type TLD 3500 Units for intensity nC
  29. 1.00031peak at about 200°C 1265.00 1707.00 0.74107peak at about 200°C
  30. 1.0E-02 max. at 484 deg. C - - - - -
  31. 1.0E-04 max. at 392 deg.
  32. 1.0E+00 max. at 198 deg. C - - - - -
  33. 1.1652274 dominent positive Table C.94 TL data for TL laboratory 14 C.95 Lab No. 15 TL reader type TL-DA-10 Units for intensity counts
  34. 1.2E-03 max. at 298 deg.
  35. 1.2E-03 max. at 330 deg.
  36. 1.49100peak at about 200°C 35300.00 24330.00 1.45088peak at about 200°C
  37. 1.5E-04 max. at 492 deg.
  38. 1.6E-02 max. at 498 deg. C - - - - -
  39. 1.7E+00 max. at 166 deg. C - - - - -
  40. 110 for the spike. doi
  41. 12.67% B.6 Table B.5 Raw data for homogeneity testing of blended samples - screening
  42. 13 Table D1. Allocation of pots to laboratories for round 2 – 35 sets of materials were prepared although only 30 laboratories returned data D.2
  43. 2.524 Max at 215°C; shoulder at 320°C 46272445 1.9E+07 2.405 Max at shoulder at 330°C
  44. 2.8E-03 max. at 434 deg. C - - - - -
  45. 22.42% Table B.6 Raw data for homogeneity testing of blended samples
  46. 22.60% Table B.7 Reference values for TL Homogeneity Testing based on Glow Ratio Mean SD Ginger U
  47. 3.1E-04 max. at 356 deg.
  48. (2006). 47 Table E.5 PSL measurements during mixing for SP8577
  49. 5.0E-01 max. at 202 deg.
  50. 5.30 very large peak at
  51. 5.9E-01 max. at 208 deg.
  52. (2006). 51 Table E.2 PSL measurements during mixing for SP8535 Chilli Powder Mixing of
  53. 6.4E-04 max. at 360 deg.
  54. 7.75134peak at about 212°C 7341.00 2743.00 2.67627peak at about 229°C
  55. 8.0E-02 max. at 458 deg. C - - - - -
  56. 8.72 Very high signal with distinct peak at 210°C 17550 3203 5.48 V Table C.89 TL data for
  57. (1996). 853513 0.002 very small signal no maximum 3015
  58. 9.4E-01 max. at 212 deg. C 7273061 10125609 7.2E-01 max. at 208 deg. C irradiated Table
  59. C a l i b r a t e d
  60. C a l i b r a t e d P S L c o u n t s
  61. Co sources the data appear to be very similar to the reference set, which was re-irradiated remotely using the Isotron commercial
  62. Comparison of participants’ qualitative percentage with the reference set
  63. data for blended samples Linear Log Mean
  64. Dong quai root
  65. (1996). Establishing Luminescence Detection Metrhods for Irradiated Fruits, Vegetables and Shellfish,
  66. Figure 4.1 Initial vs calibrated PSL for reference materials
  67. Figure 5.1 Distribution of glow 1 peak shapes for 20 aliquots each of 3 blends
  68. Figure 5.11 Participants’ TL z-scores for unirradiated samples by laboratory
  69. Figure 5.12 Participants’ TL z-scores for irradiated samples by laboratory
  70. Figure 5.13 Participants’ TL z-scores for blended samples by laboratory
  71. Figure 5.14 Participants’ TL z-scores for unirradiated samples by sample Sample 1
  72. Figure 5.15 Participants’ TL z-scores for irradiated samples by sample Sample 2
  73. Figure 5.16 Participants’ TL z-scores for blended samples by sample Sample 3
  74. Figure 5.17 Contour plot for participants’ TL data for unirradiated samples
  75. Figure 5.18 Contour plot for participants’ TL data for irradiated samples
  76. Figure 5.19 Contour plot for participants’ TL data for blended samples
  77. Figure 5.2 TL homogeneity testing glow 1 vs glow 2 scatter plot for SP8531 and SP8533
  78. Figure 5.3 TL homogeneity testing glow 1 vs glow 2 scatter plot for SP8535 and SP8539
  79. Figure 5.4 TL homogeneity testing glow 1 vs glow 2 scatter plot for SP8577 and SP8578
  80. Figure 5.5 TL homogeneity testing glow ratio plot for SP8531 and SP8533
  81. Figure 5.6 TL homogeneity testing glow ratio plot for SP8535 and SP8539
  82. Figure 5.7 TL homogeneity testing glow ratio plot for SP8577 and SP8578
  83. Figure 5.8 Participants’ glow ratios for SP8531 and SP8533
  84. Figure 5.9 Participants’ glow ratios for SP8535 and SP8539
  85. first rise to 190°C, shoulder between 240°C and 280°C, rise from 320°C 541249 2.8E+07 0.019 first rise to 190°C-200°C,shoulder between 250°C and 280°C,rise fro
  86. (2006). g of blended material was put into each of 50 tubs as before. Mixing the tarragon The same process was followed on 28
  87. Homogeneity Testing Results EN1788 calls for TL quantification of glow 1 signals, glow 2 signals, the glow ratio and identification of whether or not a peak can be observed in the 150-250°C region. Where glow
  88. hours) they should be re-measured and evaluated. Return these results also using the combination of EXCEL spreadsheet and back-up PSL summary file.
  89. (2006). i 72 43 Table D2. Correspondence between SP number and sample number as presented to participants E.1
  90. irradiated 7572 failed irradiated positiv Table
  91. irradiated Table C.83 TL data for TL laboratory 1 C.84 Lab No. 2.00 TL reader type Harshaw TLD 4000 Units for intensity nC
  92. (2006). It was concluded that the temperature control of the SURRC reader used gave a mean value of 250±1°C for peak V during this phase of the study. In earlier interlaboratory trials, between
  93. lower maximum 209°C, broad peak maximum 391°C
  94. Max at 200°C,shoulder at 320°C 49746066 3.1E+07 1.596 Max at 200°C, shoulder at 320°C Table
  95. max. at 188 deg.
  96. max. at 214 deg.
  97. max. at 224 deg.
  98. Max. in temperatur interval
  99. Max. in temperatur interval I 15 056 059 10 622 814 1.42 Max. in temperatur interval I irradiated Table
  100. maximum 235°C, fronting 3150.55 2151.98 1.46 maximum 248°C, fronting irradiated Table C.84 TL data for
  101. maximum at 221°C, lower peak 393°C
  102. maximum at 245°C with shoulder in front of the peak; lower, broad maximum
  103. maximum at 249°C with shoulder in front of the peak; lower, broad maximum 403°C 122.78 1528.71 0.08 maximum at 242°C with shoulder in front of the peak; lower, broad maximum 374°C irradiated, only a part of a mixture, because o
  104. maximum at 400°C, like blank not enough minerals 5.56 27.33 0.20 sharpe maximum 244°C lower peak 391°C irradiated, only a part of a mixture, because o
  105. Negative Intermediate Positive Selected for investigation
  106. no distinct peak in relevant temperature
  107. no Max. in temperatur interval
  108. no Max. in temperatur interval I 353 843* probably (conclusion from measurement
  109. Non-negative results shaded * zero-crossing error – result negative
  110. numbered samples for PSL analysis, and some petri dishes.
  111. out of 270 possible TL analyses, the remainder of determinations failing to produce sufficient minerals to satisfy EN1788. Of these some 92.6% of the unirradiated samples
  112. participant has identified but not corrected overflows
  113. peak in ROI1 28.47 5.773 4.93 peak in ROI1 irradiated Table C.85 TL data for TL laboratory 3 C.86 Lab No. 4 TL reader type Harshaw TLD-Reader 3500 Units for intensity nano Coulomb (nC)
  114. peaks by channel doi
  115. Percentage 83.33% 6.67% 10% 91.11% 1.11%7.78%53.34% 32.22%14.44% Percentage of results returned 92.59% 7.40% 98.80% 1.20% 62.34% 37.66% Unirradiated Irradiated Blends Product Correct Incorrect Other Correct IncorrectOther Correct IncorrectOther
  116. results from the blended samples by concentration and brightness. 1. Expected PSL signals in photon counts from table 2.4. 2. The numbers which would be selected for further investigation under EN13751, ie the sum of intermediate and positive outcomes.
  117. (2006). Return dates Please return PSL screening results no later than 2nd June; for calibrated PSL by 16 th June, and for TL results no later than 30 th
  118. (2006). Return dates Please return PSL screening results no later than 2nd June; for calibrated PSL by 16th June, and for TL results no later than 30th
  119. round peak maximum at 229°C
  120. Saw palmetto berry doi
  121. signal starts at 140°C and rises from there on up to 400°C. No distinct peak in relevant temperature range 99
  122. signal starts at 90°C°C and rises from there on up to 400°C. No distinct peak in relevant temperature range
  123. signal starts in the relvant temperatur range, but the small peak is at 300°C and therefore not within the relevant temperature range.
  124. Sr or equivalent radiation course to a dose of
  125. (2006). Table E.1 PSL measurements during mixing for SP8578 Green Tea It can be seen that the signals recorded are smaller than predicted, but that the criterion for CV <50% has been met.
  126. (1914). Table E.3 PSL measurements during mixing for SP8531 Ginger 1% Results of 10% mixing were as follows (from cycle 5 onwards a spoon was used to mix the contents of the petri dishes back into the mix):
  127. (1914). Table E.3 PSL measurements during mixing for SP8531 Ginger 1% Results of 10% mixing were as follows (from cycle 5 onwards a spoon was used to mix the contents of the petri dishes back into the mix): C y c l e
  128. (2006). Table E.4 PSL measurements during mixing for SP8531 Ginger 10% After a further 60s mixing, approximately 7g of blended ginger (calculated from the total required for participants and for homogeneity testing) was dispensed into pots.
  129. (2006). the chilli powder and tarragon were potted (8g and 6g per pot respectively).
  130. the importance of identifying the presence of peaks in the 150-250°C region, particularly for blended mixtures, temperature control accuracy and precision remains of concern to TL analysis.
  131. TL Homogeneity For Green
  132. Unirradiated Irradiated Blend Figure 4.2 Initial vs calibrated PSL for laboratories 1, 14
  133. Unirradiated Irradiated Blend Figure 4.3 Initial vs calibrated PSL for laboratories 18, 19
  134. Unirradiated Irradiated Blend Figure 4.4 Initial vs calibrated PSL for laboratories 24, 25
  135. Unirradiated Irradiated Blend Figure 4.5 Initial vs calibrated PSL for laboratories 27, 28 and 35
  136. Whole black pepper doi
  137. wide glow-curve, Max. in temperatur interval
  138. z-score for TL analyses – blended samples. Laboratory numbers are those allocated for TL apart from 18 and 24 which are PSL identifiers (these labs joined later)
  139. z-score for TL analyses – unirradiated samples. Laboratory numbers are those allocated for TL apart from 18 and 24 which are PSL identifiers (these labs joined later)
  140. Zscores for Participants data from blended samples
  141. Zscores for Participants data from irradiated samples Z score -
  142. Zscores for Participants data from irradiated samples Z score -60-55-50-45-40-35-30-25-20-15-10
  143. Zscores for Participants data from unirradiated samples

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