GC-MS Tests 18/08/2000 - 28/04/2001 3: On the 18/08/2000 analyst Ballard conducted a second GCMS test on sample 991685, which became exhibit 167, together with the curator’s standard, the first time that the standard was used with any of the seven suspect samples in GCMS testing. Analyst Ballard was testing for signs of decomposition for which if evident he could gain spectra. The following is an excerpt from the testimony: Q: Interestingly enough, you can see there is a difference in the standard one year later, if we look at it personally. If you look at the suspect sample, that hasn’t changed at all. It’s exactly the same 12 months later, isn’t it? A: That’s right. If there was some breakdown, it may have been a small amount of it breaking down. If something is going to be decomposed it doesn’t mean overnight it’s not going to be that substance.   In this analyst’s notes he had marked the whole of the major peak as methcathinone, despite peaks overlapping and hitting the top of the graph and having a very broad base and covering a retention time of about half a minute.  This analyst said that amphetamine-type samples and standards in their hydrochloride form dissolved in methanol and run on GCMS often produce such peaks and added that often it’s a program problem but for the purposes he was using it, it was more than adequate Although he agreed that overlapping peaks prevent accurate measurements, he claimed that only applies to quantitation tests but for identification purposes it was sufficient. Analyst Ballard made the following comment concerning the peak morphology mentioned above: “Ideally, you would like a well resolved, sharp thin peak but you are governed by what the particular compound does on that particular instrument. This particular compound methcathinone hydrochloride in methanol gave that shape of peak. That was the curator standard.” It was pointed out to him that there were at least four peaks shown in the spectrum for the standard which drew this response from the analyst: “Yes, and that is reflected in the sample 991685, an almost identical peak shape and the apex which is the very top of the peak is listed as 9.551 for the methcathinone standard and 9.556 for the sample when they were both prepared in the same way.” Analyst Ballard produced a scan of the methcathinone standard spectrum from this test which showed a different retention time, 9.724. The analyst explained his standard having two retention times as follows: “It is showing what I’d call a split peak for methcathinone and what I believe I’ve shown with page 2 of exhibit 167 and MFI 63, this scan, is that both the main part at 9.551 matches methcathinone and that the part at 9.724 is the same. “ He disagreed that he had overloaded the sample as well as the standard or that producing four peaks for the standard rendered that standard invalid for identification purposes. Thirteen months earlier, 24 August 1999, this analyst ran a GC quantitation test using the same methcathinone standard, that is methcathinone hydrochloride in methanol, which produced needle sharp peaks and a marked difference in retention times for the standard and this sample of 9.78 and 9.55 respectively - the only change in retention time, as shown in this test some thirteen months later, is that of the standard - analyst Ballard added that the two tests were performed on different instruments. He does concede in principle that overloading the column can alter the peak shape but does not concede that he did that in this test. He agreed that he uses 1000 nanograms of standard per microlitre and in this test used a narrow bore column which he maintained is standard practice at AGAL. He further conceded that his methcathinone standard had decomposed a little. The Hewlett Packard manual for High Resolution Chromatography, indicates that for a column of 250 micron internal diameter, the load should be between 10 and 300 nanograms. However, Dr Kibby explained that “the more you load into a column the lower is the efficiency of the resolution of your system.” In the defense analyst’s opinion, ideally up to 100 nanograms should be used and no more than 300. Although analyst Ballard used low resolution chromatography, the column used is a high resolution column and the manual refers to that. (Day 55, Pages 3054 - 3059)  (Day 59, Pages 3267 - 3287)  (Day 77, Pages 4224 - 4337)   Concerning the above tests, the defense analyst gave the following evidence under cross-examination: Crown: Isn’t 167 an example of how, even though you have overloaded the system an experienced analyst has to look at those tests and interpret them in a valid way? A: No, because we know that a year prior to this, when you ran a sample 991685, you got a retention time on 24 August of 9.78 minutes. That’s not been duplicated here, yet it was duplicated in mid September 1999. Where sample 992027, the results of that analysis were virtually identical with those obtained on 24 August. A year later we have got this rubbish, and it purports to have the same retention time and relevant ion pattern. How? That’s a mystery to me. Absolute mystery. Q: Couldn’t the 24 August test, the results in your retention times be explained because of what Mr Ballard told us about the preparation of the sample, as opposed to the methcathinone standard? A: No. It’s my belief Mr Ballard was seriously in error in that explanation. It is inconsistent with organic chemistry. (Day 79, Pages 4290 - 4291) It must be noted that the re-injection of the standard referred to above by Dr Kibby is represented by two scans, one for the standard and one for the sample which coincidently bare the same scan number 812 and which are almost identical.   4: Eleven days before the commencement of the trial, 18/01/1999, analyst Ballard, at the request of Detective Scholtes, performed a GCMS tests on samples 991685 to 991691 to identify caffeine. The mixed drug standard, which included caffeine, was run. All the samples were deemed to contain methcathinone when compared to the electronic literature standard. The chloroform rinse used as a reagent blank produced peaks - the manual dictates that reagent blanks must be free of peaks. This analyst’s TLC tests of 12 July 1999 showed a spot for caffeine in three samples only, namely 991689, 991690 and 991691.   5: There were further GCMS testing of 27 and 28 April 2001 to test this analyst’s solvent theory, namely that retention times differed because of his sample preparation, that is that the difference was due to the use of different solvents, methanol and chloroform. Exhibit LLL was produced as a result of this testing of methylamphetamine and pseudoephedrine. The peaks for methylamphetamine showed a negligible difference in retention time of 0.04 when using either solvent. Dr Kibby testified that that minimal difference in retention times discounted analyst Ballard’s solvent theory for methamphetamine. The defense analyst gave the following testimony: “In fact the simplest Mr Ballard could have done was just take the sample material, inject that as the hydrochloride salt in methanol, do a basic extract on that and show us the difference there. I mean, why wasn’t that done? Why an experiment with methamphetamine and pseudoephedrine?” Concerning the lack of any discernible print out for pseudoephedrine, the defense analyst explained that the injection port is held at 250 degrees celsius and this “temperature is actually critical; no effect on methamphetamine and in fact no effect on pseudoephedrine provided it’s in the base form. But when you inject it into a hot injection block in the acid form, pseudoephedrine will decompose, methamphetamine won’t.” The following is an excerpt from the evidence of Dr Kibby: Q: Your final expert opinion on the tests run by Mr Ballard on GC for qualitative purposes in relation to the methcathinone standard? A: There is one thing that I would like to add; The qualitative tests show the compounds are different and therefore, Mr Ballard’s quantitative estimations on those exhibits Z through to GG are invalid.