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ULTRA TRACE POPs MEASUREMENTS IN AUSTRALIA

ULTRA TRACE POPs MEASUREMENTS IN AUSTRALIA. 26 August 2012 Gavin Stevenson National Measurement Institute. Introduction. NMI Background Role in Australia Services offered Methods employed Sampling and analysis details used Recent Studies Bird eggs as environmental monitors

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ULTRA TRACE POPs MEASUREMENTS IN AUSTRALIA

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  1. ULTRA TRACE POPs MEASUREMENTS IN AUSTRALIA 26 August 2012 Gavin Stevenson National Measurement Institute

  2. Introduction • NMI Background • Role in Australia • Services offered • Methods employed • Sampling and analysis details used • Recent Studies • Bird eggs as environmental monitors • Sydney Harbour Semi-Permeable Memebrane Devices • Residential Dusts

  3. National Measurement Institute - Australia • Part of Federal Government, Department of Industry, Innovation, Science, Research, and Tertiary Education • Role is to meet national legal obligations and promote and represent Australia’s interests in national and international measurement forums • Only partially funded by Department, relies on external fee for service revenue • Services provided • Trade Measurement – Field staff around Australia • Legal Metrology -define the metrological control infrastructure that is required to assure the accuracy and • reliability of measuring instruments used for trade and regulation • Physical standards – prescribe Australia’s units of measurement; Mass, length, time, temperature • Food testing – Nutrients and pathogens

  4. Chemical Services • Analytical Services • Trace Organics – GCMS, LCMS • Trace Organics – ICPMS • Volatile Organics – Summa canisters and tubes with GCMS • POPs – HRMS and LCMS • Sports Drugs – for Australian Sports Anti-Doping Authority • Forensic Drugs – Customs seizures/Federal and State Police/Profiling to track manufacture processes and origins • Chemical Metrology Services • Certified Reference Materials – Establishing traceability to SI unit • Gas Reference Materials • Reference Methods – International comparisons • Proficiency Testing programs • Bioanalysis – DNA reference materials

  5. POPs methodology used at NMI • Based on international methods, with an emphasis on quality systems • USEPA1613, 1668, 1614 Isotope dilution high resolution mass spectrometry • Emission from industrial sources – Stack emission, industrial process wastes (soilds and liquids) and final products (oils, agrochemicals) • Food – Mainly exporters as very little Australian regulation • Remediation projects – Soil, Sediment, Water, Stack emission, Ambient Air • Drinking and wastewater – Bottled water, biosolids • Environmental monitoring – Biota, Soil, Water, SPMDs, Air • Team • 7 staff, each with at least 4 years POPs experience • Research Projects • Collaborations with Universities • Honors and PhD students in lab

  6. Extraction techniques • Accelerated Solvent Extraction for emission and solid samples (after freeze drying if required) • Soxhlet for Ambient air PUFs • Acid digestion for high lipid foods • DMSO for mineral oils

  7. Purification techniques • Concentrated Sulfuric Acid partition • Gel Permeation Chromatography for high lipid/oil samples • Automated column chromatography • Acid/Basic/Neutral Silica • Alumina • Carbon with back elution

  8. Instrumental technique • High Resolution Gas Chromatography/Mass Spectrometry • Resolution > 10,000 • ZB5 and Dbdioxin 60m columns for Dioxins/PCBs • DB5 10m column for PBDEs • Isotope dilution quantification

  9. POPs in Ibis eggs • Honors Thesis of Camila Ridoutt from Uni of NSW • Australian white ibis (Threskiornis molucca) are scavengers in urban parks and landfills so could be a good ‘indicator’ of pollution levels • Eggs were collected from nests in urban, peri-urban or inland breeding sites that contained at least 3 eggs • 219 eggs collected, 33 analysed (3 from each site) for PCDD/Fs, • dl-PCBs, and PBDEs • Lipids were extracted by acid digestion with hydrochloric acid in combination with a hexane/dichloromethane mixture

  10. POPs in Ibis eggs • For each POPs group there was a consistent trend of reduction in lipid levels from urban > peri-urban > rural • Dioxins were higher than Furans • Dioxin concentrations were higher compared to international levels for similar birds • See Poster B6.9 by Alan Yates Dioxin/Furans PCBs PBDEs

  11. Contaminated site monitoring with SPMDs • Homebush Bay site heavily contaminated with POPs after decades of chemical manufacture with poor environmental control • Region ‘cleaned up’ for Sydney Olympics in 2000, but highly contaminated sites remediated between 2006-11, by thermal treatment of soils and dredged sediments • Monitoring was undertaken to establish if contamination was spread during dredging operations

  12. Contaminated site monitoring with SPMDs See Poster B2.2 by Nino Piro

  13. Contaminated site monitoring with SPMDs

  14. Contaminated site monitoring with SPMDs

  15. WESTERN AUSTRALIA Maternal Exposure study of Residential Dusts • Blood, urine, drinking water, residential dust and soil collected in homes of pregnant woman • Aged ≥ 18 years, non-smokers, not occupationally exposed to POPs • Dust collected in vacuum cleaners analysed for Dioxins/PCBs/PBDEs • 23 Urban and 7 Rural locations • Dust Concentrations found during this study will be presented by Ania Stasinska in session D2. 104, Meeting room 8, Wednesday 10:45am • Qualitative ‘fingerprints’ to indentify if these compounds are widespread background contamination or active localised sources • More information to be presented by Shana Rogic in session C2. 103, Meeting room 3&4, Monday 11:20am

  16. Dust Dioxin Congener fingerprints

  17. PBDEs Congener fingerprints

  18. Relocating NMI Laboratory • In June 2012 several chemical laboratories relocated to a purpose built building approximately 6 km from old location • Ultra Trace Analysis • Trace Organics • Trace Metals • Sports Drugs • Chemical Reference Materials • Proficiency Testing • Chemical Reference Methods • Forensic Drugs

  19. Relocating Ultra Trace Laboratory • 3 x HRMS instruments to be housed in same room • Specialised air conditioning, power backup and cooling water • New building equipped with extending overhead hoist to enable instruments to be lifted directly from flat bed truck into room on first floor so oversize elevators not required • Moving HRMS took 90 minutes door to door • After 4 weeks the instruments have settled down to produce required sensitivity

  20. Thanks for listening, please visit us at stand 28 National Measurement Institute 105 Delhi Road North Ryde NSW 2113 Australia Phone: + 61 2 9449 0140 Email: dioxins@measurement.gov.au

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