CORUS R, D and T, Swinden Technology Centre, Rotherham, UK S60 3AR. HALL ANALYTICAL LABORATORIES, Manchester, UK M23 9YJ

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1 THE SUPELCO DIOXIN PREP SYSTEM - FLORISIL VERSION : A MULTI-LAYER SILICA GEL COLUMN CONNECTED IN SERIES TO AN ACTIVATED FLORISIL MICRO-COLUMN FOR RAPID DETERMINATIONS OF PCDD/Fs AND PCBs IN ENVIRONMENTAL SAMPLES Eric Aries 1, David R. Anderson 1, Nicholas Ordsmith 2, Lisa Fitzpatrick 3 and Fiona Barclay 3 1 CORUS R, D and T, Swinden Technology Centre, Rotherham, UK S60 3AR 2 HALL ANALYTICAL LABORATORIES, Manchester, UK M23 9YJ 3 SIGMA ALDRICH COMPANY Ltd., Poole, Dorset, UK BH12 4QH 1 POPs Workshop_30March2006

2 Overview Brief review on standard analytical procedures for PCDD/Fs and PCB analyses Collaboration between Corus / Hall Analytical / Supelco on the Dioxin Prep Systems Supelco Dioxin Prep Systems Dual Carbon Column Version Florisil Version Validation data Sample throughput Acknowledgements 2

3 Standard analytical procedures for PCB and PCDD/F analyses Method US EPA 1613 B : PCDD/Fs in solids, waste waters and sediments Method US EPA 23 : PCDD/Fs in stack emissions Method EN1948 : European method for PCDD/Fs and PCBs in stack emissions Method 1668A : PCBs in water, soil sediment and tissue ISOTOPE DILUTION : 13 C 12 PCDD/F and PCB internal standards High Resolution Gas Chromatography / High Resolution Mass Spectrometry HRGC / HRMS SEVERAL DAYS OF SAMPLE PREPARATION Extraction (Soxhlet, Dionex ASE) Solvent concentration Successive clean-up steps (Silica, Florisil, Alumina, Activated Carbon) Data processing 3

4 Supelco Dioxin Prep System Collaboration Corus / Hall Analytical / Supelco 2002 : Development and validation of the Dioxin Prep System Dual Carbon Column Version in Japan for fast determinations of PCDD/Fs. (Japan Quality Assurance Organisation and Kawajyu Techno Service) 2003 : Evaluation of the Dioxin Prep System Dual Carbon Column Version by Corus and Hall Analytical prior to its UK commercial launch : A collaboration agreement is signed by Corus, Hall and Supelco to develop and validate an enhanced version of the Dioxin Prep System : Development and validation of the Supelco Dioxin Prep System - Florisil Version by Corus and Hall Analytical Laboratories. 4

5 Testing Laboratories Trace Organic Analysis Laboratory (Corus R, D and T) Hall Analytical Laboratories Hall Analytical Laboratories Manchester, UK Contract laboratory UKAS (ISO 17025) accreditation for PCDD/F and PCB analyses 2 HRGC HRMS instruments Corus R, D & T Swinden Technology Centre, Rotherham, UK Researches into the emissions and the formation of PCDD/Fs and PCBs from UK steel plants (iron ore sintering, EAF steel-making) UKAS (ISO 17025) accreditation for PCDD/F and PCB analyses Micromass Autospec Ultima HRGC - HRMS 5

6 Corus and Hall Analytical standard procedures for determination of PCDD/Fs and PCBs in environmental samples EMISSION OR DUST SAMPLES Addition of 13 C 12 PCBs & 2,3,7,8-PCDD/Fs EXTRACTION (ASE 200) MULTI-LAYERED SILICA CHROMATOGRAPHY PCBs Saturated hydrocarbons FLORISIL CHROMATOGRAPHY PCDD/Fs HRGC / HRMS US EPA 23 or 1613B EN-1948 BASIC ALUMINA CHROMATOGRAPHY Saturated hydrocarbons PCBs HRGC / HRMS Method 6 US EPA 1668 A

7 Sample throughput at Trace Organic Analysis Laboratory (Corus) using standard analytical methods 1 fully trained technician / 8 samples Extraction and concentration (ASE 200) = 1 to 2 days Multi-layer silica clean-up = 1 day Florisil step = 1 day Basic Alumina step = 1 day PCBs Analysis overnight Data processing = 1 day PCDD/Fs Analysis overnight Data processing = 1 day PCDD/Fs : 4 to 5 working days PCBs : 5 to 6 working days Additional Tasks : Packing and activation of columns 7

8 SUPELCO DIOXIN PREP SYSTEMS The dual-carbon column version Description Analytical methods Validation data The Florisil version Description Analytical methods Validation data Sample throughput using Supelco Dioxin Prep system - Florisil Version 8

9 Supelco Dioxin Prep System - Dual Carbon Column Version Carboxen 1016 (75 m 2 / g) Carboxen 1000 (1200 m 2 / g) Multi-layer Silica gel column Dual carbon reversible tube Silica gel layer Silica gel layer Vacuum manifold 9

10 Analytical procedure Dioxin Prep System Dual Carbon Column Version ENVIRONMENTAL SAMPLES EXTRACTION (ASE 200) Addition of 13 C 12 2,3,7,8-PCDD/Fs and WHO-12 PCBs Toluene 100 ml CLEAN - UP Dual - carbon column fitted to an empty silica column Back elution of dual-carbon column WASTE 200 ml n-hexane PCDD/F FRACTION HRGC / HRMS 10

11 Analysis of a waste sinter dust (QC material) for PCDD/Fs using the Dioxin Prep System- Dual Carbon Column Version Corus data using standard US EPA 23 analytical method (N = 59) Corus data using Dioxin Prep system (N = 2) Hall Analytical data using Dioxin Prep system (N = 3) ng / kg ,3,7,8-TCDD 1,2,3,7,8-PeCDD 1,2,3,4,7,8-HxCDD 1,2,3,6,7,8-HxCDD 1,2,3,7,8,9-HxCDD 1,2,3,4,6,7,8-HpCDD OCDD 2,3,7,8-TCDF 1,2,3,7,8-PeCDF 2,3,4,7,8-PeCDF 1,2,3,4,7,8-HxCDF 1,2,3,6,7,8-HxCDF 2,3,4,6,7,8-HxCDF 1,2,3,7,8,9-HxCDF 1,2,3,4,6,7,8-HpCDF 1,2,3,4,7,8,9-HpCDF OCDF Total I-TEQ (ng/kg)

12 Supelco Dioxin Prep System - Florisil Version Schematic 250 ml solvent reservoir (28449-U) 24/24mm PP Connector (21216-U) Multi-layered silica tube (28397-U) 6.35/10 mm Reducing union (28398-U) Florisil micro-column 6.35/10 mm Reducing union (28398-U) Vacuum Manifold (28403-U) 12

13 Supelco Dioxin Prep System - Florisil Version Multi-layer silica and activated Florisil MULTI - LAYER SILICA Designed to meet requirements of Japanese Industrial Standard Methods K / K Silica gel 0.9 g Glass filter Multi-layer Silica AgNO 3 (10%) 3g H 2 SO 4 (22%) 6g H 2 SO 4 (44%) 4.5g KOH(2%) 3g ACTIVATED FLORISIL Empty Florisil tubes and connectors. Flame sealed ampoules containing 1g activated Florisil (60/100 mesh) 13

14 Analytical procedure Dioxin Prep System - Florisil Version ENVIRONMENTAL SAMPLES EXTRACTION Addition of 13 C 12 labelled internal standards PCDD/Fs ELUTION 50 ml DCM CLEAN-UP Multi-layer silica Florisil micro-column WASTE + PCBs 175 ml n-hexane WASTE + PCBs 25 ml Hexane/DCM (98 / 2, v/v) PCDD/Fs WASTE (Mainly saturated hydrocarbons) ALUMINA CLEAN - UP PCBs HRGC / HRMS 14

15 PeCDFs HxCDFs HpCDFs Determination of PCDD/Fs in DX-3 certified reference sediment using the Dioxin Prep System Florisil Version ng / kg Certified values (ng / kg) DX-3 Replicate 1 (ng / kg) DX-3 Replicate 2 (ng / kg) DX-3 Replicate 3 (ng / kg) DX-3 Replicate 4 (ng / kg) ,3,7,8-TCDD 1,2,3,7,8-PeCDD 1,2,3,4,7,8-HxCDD 1,2,3,6,7,8-HxCDD 1,2,3,7,8,9-HxCDD 1,2,3,4,6,7,8-HpCDD OCDD 2,3,7,8-TCDF 1,2,3,7,8-PeCDF 2,3,4,7,8-PeCDF 1,2,3,4,7,8-HxCDF 1,2,3,6,7,8-HxCDF 2,3,4,6,7,8-HxCDF 1,2,3,7,8,9-HxCDF 1,2,3,4,6,7,8-HpCDF 1,2,3,4,7,8,9-HpCDF OCDF TeCDDs PeCDDs HxCDDs HpCDDs TeCDFs

16 Determination of WHO-12 PCBs in DX-3 certified reference sediment using the Dioxin Prep System Florisil Version ng / g Certified values (ng / g) DX-3 Replicate 1 (ng / g) DX-3 Replicate 2 (ng / g) DX-3 Replicate 3 (ng / g) DX-3 Replicate 4 (ng / g) PeCB 105 PeCB 114 PeCB 118 PeCB 123 HxCB 156 HxCB 157 HxCB 167 HpCB 189 TeCB 77 TeCB 81 PeCB 126 HxCB

17 Determination of non dioxin-like PCBs in DX-3 certified reference sediment using the Dioxin Prep System - Florisil Version ng / g Information values (ng/g) DX-3 concentrations (ng/g) [Replicate 1] DX-3 concentrations (ng/g) [Replicate 2] DX-3 concentrations (ng/g) [Replicate 3] DX-3 concentrations (ng/g) [Replicate 4] TrCB 28 TePCB 52 PeCB 101 HxCB 153 HxCB 138 HpCB 180 HxCB 149 OcCB 194 OcCB 202 OcCB 205 NoCB 206 NoCB 208 DeCB

18 13C-PeCB 81 13C-PeCB C-PeCB 169 Typical recoveries of 13 C 12 labelled PCDD/Fs and PCBs using the Dioxin Prep System - Florisil Version C-PeCB 77 % DX-3 Replicate 1 (%) DX-3 Replicate 2 (%) DX-3 Replicate 3 (%) DX-3 Replicate 4 (%) 13C-2,3,7,8-TCDD 13C-1,2,3,7,8-PeCDD 13C-1,2,3,6,7,8-HxCDD 13C-1,2,3,4,6,7,8-HpCDD 13C-OCDD 13C-2,3,7,8-TCDF 13C-1,2,3,7,8-PeCDF 13C-1,2,3,6,7,8-HxCDF 13C-1,2,3,4,6,7,8-HpCDF 13C-PeCB C-PeCB C-PeCB C-PeCB C-PeCB C-PeCB C-PeCB C-PeCB 189

19 Fish tissue (WMF-01, Wellington Laboratories) and sandy soil (CRM 529, Supelco) Validation data using the Dioxin Prep System - Florisil Version ng / kg ng / kg ,3,7,8-TCDD 1,2,3,7,8- PeCDD 1,2,3,6,7,8- HxCDD 2,3,4,7,8- PeCDF PeCB 105 PeCB 114 PeCB 118 PeCB 123 HxCB 156 HxCB 157 HxCB 167 HpCB 189 TeCB 77 TeCB 81 PeCB 126 HxCB 169 WMF-01 Fish Tissue - PCDD/F data WMF-01 Fish Tissue - PCB data Certified values (ng / kg) WMF-01 Replicate 1 (ng / kg) WMF-01 Replicate 2 (ng / kg) WMF-01 Replicate 3 (ng / kg) WMF-01 Replicate 4 (ng / kg) Soil CRM PCDD/F data ng / kg Certified values (ng / kg) CRM529 Replicate 1 (ng / kg) CRM529 Replicate 2 (ng / kg) CRM529 Replicate 3 (ng / kg) CRM529 Replicate 4 (ng / kg) ,3,7,8-TCDD 1,2,3,7,8-PeCDD 1,2,3,4,7,8-HxCDD 1,2,3,6,7,8-HxCDD 1,2,3,7,8,9-HxCDD 2,3,7,8-TCDF 1,2,3,7,8-PeCDF 2,3,4,7,8-PeCDF 1,2,3,4,7,8-HxCDF 1,2,3,6,7,8-HxCDF 2,3,4,6,7,8-HxCDF 1,2,3,7,8,9-HxCDF

20 Sample throughput at Trace Organic Analysis Laboratory (Corus) using the Supelco Dioxin Prep System Florisil Version 1 fully trained technician / 9 samples Extraction and concentration (ASE 200) = 1 to 2 days Multi-layer silica clean-up + Florisil = 1 day Basic Alumina step = 1 day PCBs Analysis overnight Data processing = 1 day PCDD/Fs Analysis overnight Data processing = 1 day PCDD/Fs : 3 to 4 working days PCBs : 4 to 5 working days No additional tasks (column packing and activation) 20

21 Acknowledgements Shelley Richardson Corus R, D & T Laurent Ragava, Florian Mure University of Aix-Marseille III, France Rasika Fernando University of Sheffield Sue and Katie Hall Analytical Laboratories 21

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