Additional Sample 992027 Tests: 1: Analyst Ballard commenced his analysis of sample 992027, exhibit 162, on the 26/08/1999 when he performed a GCMS test using the Microgram reference, exhibit 158, although at this time he had access to the curator’s standard. The following is a brief excerpt from the transcript: Q: But given that you had the standard, why, if that was the preferable scientific course, did you not adopt it for this testing? A: Because when I performed the GCMS test on 26/08/1999, I only had the results from the colour test, which gave or didn’t indicate any specific type of substance. Therefore I didn’t know it was methcathinone, and I didn’t run a methcathinone standard. I ran it, as per the usual manner, I believe, with a mixed drug standard. Curiously, having stated that he did not know what this substance was, this analyst compared the GCMS test results for sample 992027 with a literature reference for methcathinone. His actions beg the question why not use the curator’s standard? Again he disregarded the AGAL manual in that he failed to run a reagent blank at the start of these GCMS tests, a reagent blank being a run of the solvent and/or solvents used in the standard and sample to be tested. Having failed to run a reagent blank this analyst admitted that he couldn’t exclude that a large amount of methcathinone was present in the solvent. Analyst Ballard agreed: ‘It is, as I said, fundamental to run it.’ This analyst also agreed that he overloaded the machine but added the following: “...Whether the substance is overloaded to some degree or not, I believe the spectral information obtained is still accurately shown.” (Day 59, Pages 3300 - 3304) As well as his disregard for the manual and overloading of the sample this analyst was questioned regarding the ion abundance differences between the Microgram reference, exhibit 158, and the sample, exhibit 162. The chromatogram produced more than 15 peaks distinguished by different retention times with the major peak being severely overloaded. When this sample was compared to the Microgram reference all the major ions were outside the tolerance level of  plus or minus 20%, as per the AGAL manual.- a) The most abundant ion  becomes the yardstick from which the other ions are measured - in this case, in both the literature reference and sample 992027, the 58 ion is the yardstick. b) In sample 992027 the next most abundant ion is the 56 ion having a relative intensity of 42.37% - the Microgram reference a relative intensity of 11%. c) In the literature reference the second most abundant ions were 51 and 77 equally with a relative intensity of 11% - in sample 992027 the 51 ion has a relative intensity of 34.1% and the 77 ion 26.48%. d) The last common major ion is the 42 ion with the literature reference showing a relative intensity of 7.7% and the sample 992027 of 32.3%. Analyst Ballard’s attention was then drawn to the Spectrometric Identification of Organic Compounds table, which became exhibit DDD and this analyst agreed that if the 58 ion as identified in his test results is accurate, then it was inconsistent with the methcathinone molecule - the 58 ion having three nitrogens and ‘methcathinone’ two and is therefore inconsistent with the methcathinone molecule. The following is a brief excerpt from the transcript: Q: You’ve never considered nor thought it necessary to consider which particular fragment the 58 ion might represent from the molecule? A: No, I could calculate it but in my analysis I don’t use these tables. The second example looked at in relation to the spectrogram data was the 77 ion which had only one entry with a resolution at 77.05 which also has three nitrogens. Although this analyst conceded all of the above he still maintained that his conclusion, that the sample 992027 contained methcathinone, was correct. When asked to explain how he could arrive at the conclusion from this GCMS test that sample 992027 matched the Microgram reference despite the differences in ion intensities, this analyst said “... that is observed from reinjection of the very sample.”  The following questions and answers were given: His Honour: I’m just not sure what you mean by the answer: “That is observed from reinjection of the very same sample”. Do you mean the very same sample of methcathinone as shown in those differences? A: The very same sample being 992027. His Honour: You mean if you injected it twice you get the same result? A: Injecting it twice and observing some differences in the relative ion abundances, the overall pattern remaining the same but the numerical values for ion abundances being a little different from one run to another. Defense Counsel: You are referring are you to the next occasion that you injected 2027 which was on 30 August 1999 because you only injected 2027 once on 26 August 1999, that’s so isn’t it? A: That’s right, the 30 August was the other occasion. The total ion chromatogram for this test showed a broad peak having a retention time of 9.375 with a base of over half a minute. A scan from within the peak shows widely different ion intensities from the spectrum for 992027. In obtaining different spectra for the same peak suggests an unreliable test, according to the defense analyst, because the two mass spectra are taken at different retention times and therefore the tests are of no value in making an identification.   2: The following day, 27/08/1999, analyst Ballard conducted an IR test on sample 992027, exhibit 163 and compared it to the Microgram Journal reference, exhibit 155. The test result for the sample 992027 contained a number of peaks marked with specific wave numbers but the literature reference did not and analyst Ballard performed a visual analysis with respect to the peak patterns. He declared sample 992027 to be a match for methcathinone. The defense analyst said there were vast differences between the sample and the literature reference, e.g. - marked differences in the intensities of the absorbance bands and peak shapes. Analyst Ballard agreed that his GCMS tests on this sample indicated that it contained over 15 different compounds and therefore it could not be called practically pure. It was suggested to analyst Ballard that as the sample was a long way from being pure, IR testing was not a relevant test here and therefore a conclusion as to identity could not be reached. This analyst disagreed. The defense analyst testified: “There’s nothing wrong with running infrared testing for use as complementary data, but it’s difficult to make a positive assignment for an unknown substance from an infrared spectrum of an impure mixture.”   3: Also on 27/08/1999 analyst Ballard conducted a TLC test on sample 992027 in which the methcathinone standard was used as part of a mixed drug standard. The methcathinone standard was certified to be 99% pure by the supplier Radiant International and the sample 992027 had been assessed by this analyst as having a purity of 77.4%. Despite the disparity in the levels of purity between standard and sample, both produced the same two spots in the same line in the TLC test, exhibit 164. The following is an extract from the transcript; Q: The whole point of the standard is to produce one spot with one RF, that’s why it’s a standard so you can measure it, so you can compare things against it? A: That’s correct. This produced one main spot with a faint trace of who knows what. As I said I don’t know what the other spot is above it. Q: But it happens to coincide with the faint spots on 992027? A: It appears to coincide with the faint spots on 2027, yes. Analyst Ballard did not agree that he may have contaminated the standard with the sample or vice-versa. None of the other standards contained within the mixed drug standard showed more than one spot. The defense analyst said in TLC testing contamination can be introduced by micro drops, from the solution being spotted onto the plate, falling from the narrow ball glass capillary tube. Secondly if a clean capillary tube for every spot is not used contamination can occur and thirdly that there may be a second compound in the solution. A brief excerpt from the transcript: Q: Now it seems as though the methcathinone standard seems to produce exactly the same spots in exactly the same position on the TLC? A: From where I’ve drawn it from my observations it would appear so. Q: That would indicate on this hypothesis that both the methcathinone standard and 2027 have methcathinone within them and another compound which cannot be distinguished in TLC, correct? A: That’s a possibility, I was only really concerning myself with the main spot. Q: That is that the standard and 2027 are both contaminated with exactly the same compound or at least one is so similar it can’t be distinguished on TLC? A: I don’t know if “contaminated” is a good word. and a little later: Q: Well, now is it then that something which is said to be produced in some clandestine laboratory happens to show exactly the same impurity as something which comes from a pure known source and is purchased for exactly the same purpose that it is an extraordinary coincidence, would it not? A: I couldn’t say what sort of coincidence that would be The AGAL manual refers to Clark’s mobile phase in the amphetamine system and is regarded as a definitive test in analytical chemistry, according to the defense analyst. Analyst Ballard used the solvent system 25 parts ethyl acetate, 10 parts acetone, 1 part ammonia, a solvent system which can be unstable and therefore affect results.   4: This analyst ran another GCMS test on sample 992027, this time using the curator’s standard, the first time it was used for this sample in GCMS testing. However, at the committal hearing and with the benefit of his notes, analyst Ballard failed to mention this GCMS test on sample number 992027. This analyst in evidence said the test results sat on his desk from 30/08/1999, when they were produced, until sometime after the committal hearing of the 23/05/2000 and therefore did not make it into his case file. He also stated that he did not discuss this test with the prosecution until giving his evidence-in-chief. Further, as the AGAL manual demands, this GCMS test was not second read or signed by a senior analyst and therefore the validity of these tests was put into jeopardy. The total ion chromatogram for sample 992027 showed, as did the previous GCMS test on this sample, at least 15 peaks and the five most abundant ions were again outside the acceptance and rejection criteria, as stated in the manual, that being plus or minus 10% as the curator’s standard was used. The following is a brief excerpt from the transcript: Q: So one should expect, there, that they would meet the tolerances which are set down in the manual if indeed they were the same substance, namely, methcathinone? A: If it is written in the manual, yes, I guess you could expect that, but I could show on the same day inspections will fall out side the 10%. Q: In any event, you do concede this much, do you, that the sample 2027 and the standard as shown in exhibit 165 page 1 and reflected in the intensities in exhibit MMM do not match according to the acceptance and rejection criteria of your own manual? A: Looking at those five specific items, that is correct. Both the sample, 992027, and the methcathinone standard were run in methanol. The spectrum for the methcathinone standard produces a ‘curious peak’ because it appeared that the multiplier and detector had shut down which indicates overloading of the detector. In the spectrum for sample 992027 again the major peak has a retention time of 9.3 and the peak has a broad base of over half a minute which indicates that the peak is overloaded and the data produced is not reliable according to the defense analyst.   5 The final pre-trial test on this sample was the Gas Chromatography or GC test conducted 14 September 1999, exhibit 166, together with the methcathinone standard. These tests were run, according to analyst Ballard, for quantitation purposes. Unlike the GC test run on 24/08/1999 for samples 991685 to 991691, this run of tests was run in sequence at 29 minute intervals but as in the earlier GC test, analyst Ballard widened the window for retention time to 0.3. The defense analyst said that a 0.300 window is a plus or minus setting which equates to a window 36 seconds wide and that any peak centred around 9.5 minutes within that 36 second window will be labelled ‘methcathinone’. The retention time of the methcathinone standard on the first run in this series was 9.64 and similarly the second run of the standard was again 9.64. The third run of the standard was 9.65, a negligible difference and the last run was 9.64 which is a reproducible result for the standard of 9.64, a real retention time. Sample 992027 on the first run gives a retention time of 9.4 and the duplicate run of this sample also produced a retention time of 9.4, also a reproducible result and a difference of 0.24 minutes or 14.4 seconds which is significant. This difference in retention time according to analyst Ballard is that sample 992027 was a basic extraction in chloroform and the standard was a hydrochloride salt in methanol. This analyst claimed that retention time differences were the result of his sample preparation, the standard was in the hydrochloride salt form and sample 992027 in free base form. An inspection of this analyst’s GC analyses of 15/09/1999 in which a mixed drug standard was used against sample 991691, little effect on retention time was noted. The mixed drug standard was in methanol and the sample in chloroform - the retention times were 13.168 minutes and 13.225 respectively, a difference of 0.057. With reference to the form of sample or standard on injection, either hydrochloride salt or free base, it must be remembered that the injection port is held at 250 degrees celsius. At this temperature amine salts are rapidly and quantitatively dissociated into the free base form. In effect both standard and sample would enter the chromatography column in free base form. As Dr Kibby noted: “...It is most unfortunate that the test, whereby a basic extract of, for example, sample 992027 was not directly compared to a dissolution of sample 992027 in methanol. That would be the piece of experimental proof we would need to support Mr Ballard’s contention.” The defense analyst said that the difference in retention time of .24 of a minute, 14.4 seconds indicates that sample 992027 is different from the methcathinone standard. NB: At this point in proceedings, during Dr Kibby’s cross examination, the judge sent the jury for lunch and addressed the crown prosecutor: His Honour: Madam Crown, I take it that those who are instructing you understand the significance of all this evidence that is given by this witness? Crown Prosecutor: Yes your Honour. His Honour: And the Crown would want to proceed? Crown Prosecutor: I will consider our position over lunch After the lunch period and in the absence of the jury: Crown Prosecutor: Your Honour, we say a verdict of attempt will be open to the jury.             His Honour: Attempt to do what? Crown Prosecutor: Manufacture prohibited drug methcathinone. That’s why we need time to consider our position. As well as the difference in retention time the peak shape between standard and sample were different. Analyst Ballard gave evidence that although there was a difference in retention time at the apex of the peaks, the base of the column came out of the column at the same time. The defense counsel said that it would be “very difficult to tell that from the compressed time scale of these exhibits. Dr Kibby expanded the time scale and using the retention times and width and heights of the peaks calculated when the peaks came out of the column. He gave the following explanation of this process: “...I find that in fact the standard commences to come off the column some three seconds after the unknown material. But even of more significance is the apices of the respective peaks are separated by 14.4 seconds, and even more interesting is the fact that when the unknown material has finished eluting from the column, the standard material requires another 24 seconds to finish eluting from the column. Now, one would expect for the same compounds giving peaks of the same area is that they should start at the same time, have a retention time at the apex of the peak at the same time and finish eluting from the column at the same time. Instead, these peaks - 3 second difference at the start of the peak, 14 second difference between the apices and 14 second difference by the time they stopped coming off the column. That to me says different compounds.” (Day 60, Pages 3314- 3340) (Day 77, Page 4249 - 4253) On 28 May 2001 and at the completion of Dr Kibby’s evidence and cross examination and, it must be said, with no objection from the Crown, the trial judge gave the jury a Prasad Direction. This directive allowed the jury to stop the trial at this point if they considered that the Crown had not proven their case by bringing in a not guilty verdict. They could not at this time bring in a verdict of guilty. This jury did not take up the direction.   Certificates of Analysis: Analyst Ballard Issued three certificates of analysis, two for samples 991685 - 991691 and one for 992027:- a) On 03/08/1999 analyst Ballard produced a Preliminary Certificate of Analysis on AFDL Nos 991685 - 991691 confirming the presence of methcathinone in each. This analyst did not have access to the methcathinone standard until 05/08/1999. In this certificate analyst Ballard certifies that: “I analysed the items described below which were submitted to the laboratory on the third day of July 1999 by Detective Senior Constable G Ballard of the NSW Police Crime Agencies.” This certificate refers to police reference No C562712 / AFDL Nos 991685 - 991691, the weights for each sample and the conclusion that all were identified as containing methcathinone. Analyst Ballard did not weigh the samples himself and therefore was not in a position to certify to that. Secondly, this analyst’s assertion that the items were delivered to the laboratory by Detective G. Ballard - information analyst Ballard says he gleaned from a sample submission form known as a P37 form - is in direct contrast to the evidence of Detective G. Ballard and analyst Murtagh. b) On 07/09/1999 this analyst issued his final certificate of analysis which included the same information from the preliminary certificate plus the calculated purity levels of methcathinone for each sample. No further testing for qualitative purposes was carried out in support of this certificate - a GC test for purity only was undertaken, this test having retention time difference of 0.23 minutes and the test in which analyst Ballard interacted with the instrument. c) The certificate of analysis for sample 992027 was issued on 17/09/1999 at the completion of testing for this sample.