scott r. oulton, swgdrug secretariat
DESCRIPTION
Scientific Working Group for the Analysis of Seized Drugs Update. by. Scott R. Oulton, SWGDRUG Secretariat. OVERVIEW. In January 2010, the core committee approved two documents: 1) Supplemental Document SD-3 For Part IVC – Examples of Measurement Uncertainty for Weight Determinations - PowerPoint PPT PresentationTRANSCRIPT
by
Scott R. Oulton, SWGDRUG Secretariat
Scientific Working Group for the Analysis of Seized Drugs Update
OVERVIEW In January 2010, the core committee
approved two documents: 1) Supplemental Document SD-3 For Part IVC –
Examples of Measurement Uncertainty for Weight Determinations
2) SWGDRUG Recommendations 5th Edition (revised/edited current recommendations)
Current work projects and future topics Four active subcommittees (uncertainty, editorial,
education and training and CLIC collaboration) Proposed change to reporting requirements New initiatives
Supplemental Document SD-3 for Part IVC
“Examples of Measurement Uncertainty for Weight Determinations”
SUPPLEMENTAL DOCUMENTSSupplemental Documents
Intended to be a resource for those implementing recommendations
Not all inclusive, many ways to implement recommendations
Purpose is to provide examples to be used in conjunction with SWGDRUG Recommendations
The draft supplemental document was posted for public comment in July 2009
Many comments were received The document was vetted through
professional metrologists and statisticians Supplemental Document SD-3 was adopted
January and posted in July 2010
UNCERTAINTY SUBCOMMITTEE
Type A – statistically determined from repetitive measurements (e.g., control chart)
Type B – everything else (e.g., calibration report) Three examples were developed
Example 1: 1 bag of powder (type B uncertainties) Example 2: 1 bag of powder (type A -B uncertainties) Example 3: 15 bags of powder (type A -B uncertainties)
In Example 1, five significant uncertainty sources were considered. For example 2 & 3, data from a well-established control chart captures three of these factors
SUPPLEMENTAL DOCUMENT SD-3
Multiple approaches exist for estimating uncertainties Elements used contain correlated and uncorrelated
sources The illustrated methods in these examples
represent a conservative approach in which the uncertainty is likely to be overestimated This is done to conservatively account for all
correlations even those that for all practical purposes cannot be determined
SUPPLEMENTAL DOCUMENT SD-3
Readability Repeatability Linearity Buoyancy (insignificant) Sensitivity (insignificant) Uncertainty from balance calibration Number of weighing events Sample loss in transfer: for practical
purposes, this is considered indeterminate and irrelevant
FACTORS CONSIDERED
Determine net weight of a white powder received in a plastic bag using a top loading balance. The following conditions apply: The operator is competent on the use of the
balance The balance is:
o calibrated and certifiedo being used above the established minimum
balance loado performing within manufacturer specificationso located in a temperature-controlled
environment (±5 °C)
EXAMPLE SCENARIO
A weigh vessel is: loaded and tared removed and filled with powder reweighed containing powder
Net weight = 30.03 grams Static weighing – obtaining net weight via two
weighing operations Two weighing events
Dynamic weighing – adding powder directly to tared vessel on balance One weighing event
EXAMPLE SCENARIO
Expanded Uncertainty U = k * uc
Using Coverage Factor (k) = 2 (approx. 95%)U = 2 * 0.0176 g = 0.0352 g
Final Ufinal = U * # weighing eventsUfinal = 0.0352 g * 2 = 0.0704 g
CALCULATION2222 )()()()( calbalulinearurepeatureaduuc
guc 0176.00065.00115.001.000577.0 2222
ResultsNet Weight: 30.03 g ± 0.07 g (k=2)Net Weight: 30.03 g ± 0.11 g (k=3)
RESULTS
Uncertainty estimates associated with quantitative measurements e.g., 82.4% ± 3.2%
Extrapolations of weights Weight determined by statistically
measuring a set amount of sub itemso e.g., 10 out of 500 bricks of cocaine
weighed and extrapolated to calculate total weight of 500 kg. The uncertainty is estimated based on statistical analysis of 10 weighed units
WHAT NEXT?
SWGDRUG Recommendations5th Edition
Goal – Revision of existing SWGDRUG Recommendations to:Harmonize terminologyCorrect grammarAdd referencesLink sectionsCorrect sections in conflictClarify recommendations as appropriateUpdate glossary
EDITORIAL COMMITTEE
§ 2 Education and experience for analysts Before:
oa bachelor’s degree (or equivalent, generally a three to four year post-secondary or tertiary degree) in a natural science or in other sciences relevant to the analysis of seized drugs…
OR oby January 1, 2005, a minimum of five (5)
years practical experience in the area of seized drug analysis…
SIGNIFICANT CHANGES
§ 2 Education and experience for analysts After:
oAll new analysts shall have at least a bachelor’s degree (or equivalent, generally a three to four year post-secondary degree) in a natural/physical science.
SIGNIFICANT CHANGES
§ 3 Continuing professional development Before:
o Contact is defined as face-to-face interaction with an instructor or trainer in a classroom or laboratory setting. It does not include self-paced learning or distance education where the instructor has no active interaction with the student.
After:o 3.4 Training can be either face-to-face interaction
with an instructor, distance learning, self-directed or computer based.
Added: current literature review
SIGNIFICANT CHANGES
§ 11 Analytical method validation and verification Before:
o 11.1 Method validation is required to demonstrate that methods are suitable for their intended purpose.
11.1.1 For qualitative analysis, the parameters that need to be checked are selectivity, limit of detection and reproducibility.
11.1.2 Minimum acceptability criteria should be described along with means for demonstrating compliance.
11.1.3 Validation documentation is required. o 11.2 Laboratories adopting methods validated elsewhere should verify these methods
and establish their own limits of detection and reproducibility. After:
o Method validation is required to demonstrate that methods are suitable for their intended purpose (see PART IV B – Validation).
SIGNIFICANT CHANGES
Added hyperlinks to Uncertainty section throughout document
Added hyperlinks to Validation section throughout document
Added “Shall” in place of “Should” in several locations (conduct, ethics, education, etc.)
SIGNIFICANT CHANGES
Revisions to Glossary: Added definition for “false negative” Updated several definitions as a result of
some ISO terms amended within the last few years
e.g., ISO 3534-2:2006, VIM 2008Category A now includes: X-Ray
Diffractometry
SIGNIFICANT CHANGES
Before§ 3.1 … Use second technique …§ 3.1.2 When sample size allows, the second
technique should be applied on a separate sampling for quality assurance reasons. When sample size is limited, additional measures should be taken to assure that the results correspond to the correct sample.
§ 3.4 In cases where hyphenated techniques are used (e.g. gas chromatography-mass spectrometry, liquid chromatography-diode array ultraviolet spectroscopy), they will be considered as separate techniques provided that the results from each are used.
SIGNIFICANT CHANGES
Problem If two samplings important, why have
different procedure for trace samples? Misinterpretation of 3.4, hyphenated
techniques do not offer second samplingSolution
Revise section to emphasize quality assurance stepo Second samplingo Procedural blanko Witnessing
SIGNIFICANT CHANGES
After The laboratory shall employ quality
assurance measures to ensure the results correspond to the exhibit. Example measures are:o the use of two separate samplings o sample identification procedures such as bar-
coding and witness checkso good laboratory practices (e.g., positive and
negative controls, one sample opened at a time, procedural blanks)
SIGNIFICANT CHANGES
Problem e.g., Is DART a Category A or B?
Solution Techniques for the analysis of drug samples
are classified into three categories based on their maximum potential discriminating power. However, the classification of a technique may be lower, if the sample, analyte or mode of operation diminishes its discriminating power.
SIGNIFICANT CHANGES
Solution Examples of diminished
discriminating power may include:oan infrared spectroscopy
technique applied to a mixture which produces a combined spectrum
oa mass spectrometry technique which only produces molecular weight information
SIGNIFICANT CHANGES
Education and Training Subcommittee
Phase 1 Develop core competencies (outline form) Coordinate efforts with ENFSI Drugs Working
Group Phase 2
Identify existing resources (open source, for purchase, etc.)
Phase 3 Post example training programs on-line
EDUCATION AND TRAINING SUBCOMMITTEE
Proposed Revision toReporting Requirements
Mirror ISO/IEC-17025 LanguageNASTransparency
Why Change Reporting?
9.2 Report writing Reports issued by laboratories shall be accurate, clear, objective, and meet the requirements of the jurisdictions served. Unless the laboratory has reasons for not doing so, these reports shall include the following information:
title of report identity and location of the testing laboratory unique case identifier (on each page) clear identification of the end of the report submitting agency date of receipt date of report descriptive list of submitted evidence identity and signature (or electronic equivalent) of analyst results / conclusions analytical techniques employed sampling uncertainty.
Report Writing
116 Responses For – 38% Against – 62%
Most commons reasons against proposal Analytical Techniques Sampling Uncertainty
Cited reasons Courts would not understand Defense attorneys would have a field day Would have to testify more
Survey Results
Analytical Techniques Presumptive test only, qualitative determination
Sampling Tested 1 unit, report all containing
Uncertainty Enhances confidence through increased
understanding of resultso e.g., Gas pump accuracy for 10 gallons
Gas Station 1: 10 ± 0.03 galGas Station 2: 10 ± 1.35 gal
Near statutory thresholdo Blood alcohol 0.08
Survey Results
SWGDRUG9.2 Report writing Reports issued by laboratories shall be accurate, clear, objective, and meet the requirements of the jurisdictions served. Unless the laboratory has reasons for not doing so, these reports shall include the following information:
ISO 170255.10.2 Each test report or calibration certificate shall include atleast the following information, unless the laboratory has validreasons for not doing so:
Survey Results
New Initiatives
Formal Survey Assess implementation of recommendations
in the forensic science community Using www.surveymonkey.com
MS Database Contains over 1200 compounds Inviting community to participate
Cooperation with CLIC Developing recommendations for analysis of
clandestine laboratory samples Development of uncertainty spreadsheet
New Initiatives
SWGDRUG Core Committee
CORE COMMITTEE• DEA – Scott Oulton (Chair)
• Secretariat – Sandra Rodriguez-Cruz
• FBI - Eileen Waninger• ASCLD – Garth Glassburg• NIST – Susan Ballou• ASTM and NEAFS – Jack Mario
• Educator – Vacant (Eric Person)
• Educator – Dr. Suzanne Bell
CORE COMMITTEE• CAC & NWAFS – Jerry Massetti
• MAFS – Richard Paulas• MAAFS – Linda Jackson• SAFS – Christian Matchett• SWAFS – Scott Vajdos• Toxicology – Dr. Robert Powers
CORE COMMITTEE
• Canada – Richard Laing• Japan – Osamu Ohtsuru• United Kingdom – Dr. Sylvia Burns
• Australia – Catherine Quinn• Germany – Dr. Udo Zerell• ENFSI – Dr. Michael Bovens• UNODC – Dr. Iphigenia Naidis
Visit us at:www.swgdrug.org