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Standards and Standard Methods Review on Sampling, Determination and Quantifying the PCBs

Authors: dr. Felicia Precup , phd. ph.. Sanda Cotescu , phd. eng. Paul Pencioiu 1) SC ICPE SA-Bucuresti

1) 1) 1)

Abstract: This paper aimes to review the international and national standards and standard methods used to sample, determine and quantify the PCB from a wide range of matrices: indoor/outdoor air, drinking/waste water, soil, waste, petroleum products, used oils, food and animal feeding stuff.

Key words: standard, standard method

Introduction. Used on a large scale in the past for their interesting and useful properties which made them suitable for a wide range of industrial applications the PCBs represent now a n environmental and health challenge. Their production and use is now prohibited in most country, but they continue to be widely spread in the environment: air, water, soil, waste and living organisms. Their source are now either uncontrolled burning processes (incinerators) or `historical' electrical, construction, printing waste which were not properly disposed off. Because they accumulate in the food chain and have a toxic effect on humans it is very important to identify them and determine their concentration in all the matrices. International and national standardization organization developed a large number of standards and standard methods on this issue in order to promote environmental protection and public safety. In order to comply with the European environmental requirements Romania adopted some of these standards (EN or ISO) to replace old ones or to meet the newly appeared environmental demands. As the standards are periodically reviewd and new standards are approved annual or monthly, it's important to keep up with the changes and a periodical review is very useful. Chapter 1. ISO standards. ISO (International Organization for Standardization), a non-governmental organization, is the world's largest developer and publisher of International Standards and consists of a network of the national standards institutes of 157 countries, one member per country, with a Central Secretariat in Geneva, Switzerland, that coordinates the system. Matrix ISO 16000-1:2004; Indoor air-- Part 1: General aspects of sampling strategy ISO 16000-12:2008; Indoor air -- Part 12: Sampling strategy for polychlorinated biphenyls (PCBs), polychlorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs) and polycyclic aromatic hydrocarbons (PAHs) ISO/FDIS 16000-13; Indoor air -- Part 13: Determination of total (gas and particle-phase) polychlorinated dioxin-like biphenyls (PCBs) and polychlorinated dibenzo-p-dioxins/dibenzofurans (PCDDs/PCDFs)-Collection on sorbent-backed filters ISO/FDIS 16000-14; Indoor air -- Part 14: Determination of total (gas and particle-phase) polychlorinated dioxin-like biphenyls (PCBs) and polychlorinated dibenzo-p-dioxins/dibenzofurans (PCDDs/ PCDFs)-Extraction, clean-up and analysis by high-resolution gas chromatography /mass spectrometry ISO 5667-1:2006; Water quality -- Sampling -- Part 1: Guidance on the design of sampling programmes and sampling techniques ISO 5667-3:2003; Water quality -- Sampling -- Part 3: Guidance on the preservation and handling of water samples ISO 5667-10:1992; Water quality -- Sampling -- Part 10: Guidance on sampling of waste waters published, stage; 90.60 published, stage 60.60

Standard Outdoor air

Notes/standard status

Indoor air

TC 146

under development, stage 50.20

under development, stage 50.00 published, stage 60.60 published, stage: 60.60 published, stage 90.93

Water

TC 147

ISO 5667-11:1993; Water quality -- Sampling -- Part 11: Guidance on sampling of groundwaters ISO/DIS 5667-11; Water quality -- Sampling -- Part 11: Guidance on sampling of groundwaters ISO 5667-13:1997; Water quality -- Sampling -- Part 13: Guidance on sampling of sludges from sewage and water treatment works ISO/WD 5667-13; Water quality -- Sampling -- Part 13: Guidance on sampling of sludges from sewage and water treatment works ISO 5667-15:1999; Water quality -- Sampling -- Part 15: Guidance on preservation and handling of sludge and sediment samples ISO/DIS 5667-15; Water quality- Sampling - Part 15: Guidance on preservation and handling of sludge and sediment samples ISO 5667-18:2001; Water quality -- Sampling -- Part 18: Guidance on sampling of groundwater at contaminated site ISO 17858:2007; Water quality -- Determination of dioxin-like polychlorinated biphenyls -- Method using gas chromatography/ mass spectrometry ISO 6468:199 ; Water quality -- Determination of certain organo chlorine insecticides, polychlorinated biphenyls and chlorobenzenes -- Gas chromatographic method after liquid-liquid extraction. ISO 10381-1:2002; Soil quality - Sampling-- Part 1: Guidance on the design of sampling programme ISO 10381-2:2002;Soil quality - Sampling - Part 2: Guidance on sampling techniques ISO 10381-4:2003; Soil quality - Sampling - Part 4: Guidance on the procedure for investigation of natural, near-natural and cultivated sites. ISO 10381-5:2005; Soil quality -- Sampling -- Part 5: Guidance on the procedure for the investigation of urban and industrial sites with regard to soil contamination ISO 10382:2002; Soil quality - Determination of organochlorine pesticides and polychlorinated biphenyls -- Gas-chromatographic method with electron capture detection

published, stage 90.92 to be revised under development, stage 40.60 published, stage 90.92 to be revised under development, stage 20.99 published, stage 90.92 under development, stage 40.60 published, stag: 90.92 published, stage 60.60 published, stage 90.93 published, stage 90.60 published, stage 90.60 published, stage 60.60 published, stage 60.60 published, stage 90.60

TC 190

Soil

Waste Petroleum products and used oils Insulating liquids Food Animal feeding stuff

Pulp, paper and board

ISO 15318:1999; Pulp, paper and board -- Determination of 7 specified polychlorinated biphenyls (PCB) published, stage 90.93

Standards stag code: 20.99 WD (working draft) approved for registration as CD (committtee draft) 40.60 Close of voting 50.00 FDIS (final draft international standard) registered for formal approval 60.00 International Standard under publication 60.60 International Standard published 90.60 Close of review 90.92 International Standard to be revised 90.93 International Standard confirmed

Chapter 2. Romanian standards International standards adopted by the Standardization Association from Romania (ASRO)the Romanian National Standards Institute or referred to in the Romanian legislation: Matrix Outdoor air Standard

SR EN 1948-1:2006 A CT 53 Stationary source emissions - Determination of the mass concentration of PCDDs/PCDFs and dioxin-like PCBs - Part 1: Sampling of PCDDs/PCDFs SR EN 1948-2:2006 A CT 53 Stationary source emissions - Determination of the mass concentration of PCDDs/PCDFs and dioxin-like PCBs - Part 2: Extraction and clean-up of PCDDs/PCDFs

Notes/standa rd status

Replaces: SR EN 1948-1:2003 Replaces: SR EN 1948-2:2003

SR EN 1948-3:2006 A CT 53 Stationary source emissions - Determination of the mass concentration of PCDDs/PCDFs and dioxin-like PCBs - Part 3: Identification and quantification of PCDDs/PCDFs

Replaces: SR EN 1948-3:2003

Indoor air

SR EN ISO 6468:2000 Water quality - Determination of certain organochlorine insecticides, polychlorinated biphenyls and chlorobenzenes - Gas chromatographic method after liquid-liquid extraction SR ISO 5667-10:1994 Water quality - Sampling - Part 10: Guidance on sampling of waste waters SR ISO 5667-12:2001 Water quality. Sampling. Part 12: Guidance on sampling of bottom sediments SR ISO 5667-11:2000 Water quality. Sampling. Part 11: Guidance on sampling of groundwaters SR ISO 5667-4:2000 Water quality. Sampling. Part 4: Water quality. Sampling. Part 4: Guidance on sampling from lakes, natural and man made SR ISO 5667-6:1997 Water quality.Sampling. Part 6: Water quality. Sampling. Part 6: Guidance on sampling of rivers and streams SR ISO 10382:2007 T: Soil quality - Determination of organochlorine pesticides and polychlorinated biphenyls -- Gas-chromatographic method with electron capture detection

Soil

CT 285

Water

Waste

SR EN 12766-2:2002: Petroleum products and used oils - Determination of PCBs and related products - Part 2: Calculation of polychlorinated biphenyl (PCB) content SR EN 12766-1: 2003: Petroleum products and used oils - Determination of PCBs and related products - Part 1: Separation and determination of selected PCB congeners by gas chromatography (GC) using an electron capture detector (ECD) SR EN 12766-3:2005: Petroleum products and used oils - Determination of PCBs and related products - Part 3: Determination and quantification of polychlorinated terphenyls (PCT) and polychlorinated benzyl toluenes (PCBT) content by gas chromatography (GC) using an electron capture detector (ECD) SR EN 12766-3:2005/AC:2007) Petroleum products and used oils - Determination of PCBs and related products Part 3: Determination and quantification of polychlorinated terphenyls (PCT) and polychlorinated benzyl toluenes (PCBT) content by gas chromatography (GC) using an electron capture detector (ECD)

Petroleum products and used oils

Insulating liquids

SR EN 1528-1:2004 Fatty food - Determination of pesticides and polychlorinated biphenyls (PCBs) - Part 1: General SR EN 1528-2:2003 Fatty food - Determination of pesticides and polychlorinated biphenyls (PCBs) - Part 2: Extraction of fat, pesticides and PCBs, and determination of fat content SR EN 1528-3:2004: Fatty food - Determination of pesticides and polychlorinated biphenyls (PCBs) - Part 3: Clean-up methods SR EN 1528-4:2004: Fatty food - Determination of pesticides and polychlorinated biphenyls (PCBs) ­ Part 4: Determination, confirmatory tests, miscellaneous prEN 15741 Animal feeding stuffs - Determination of OC-pesticides and PCB's by GC/MS prEN 15742 Animal feeding stuffs - Determination of OC-pesticides and PCB's by GC/ECD

Food

phase 3099 phase 3099

Animal feeding stuff CT 95

Pulp, paper and board -

Chapter 3. EN Standards

CEN is the European Committee for Standardization founded by the national standards bodies in the European Economic Community and EFTA countries.

Matrix

Standard

EN 1948-1:2006 Stationary source emissions - Determination of the mass concentration of PCDDs/PCDFs and dioxin-like PCBs - Part 1: Sampling of PCDDs/PCDFs EN 1948-2:2006 Stationary source emissions - Determination of the mass concentration of PCDDs/PCDFs and dioxin-like PCBs - Part 2: Extraction and clean-up of PCDDs/PCDFs, EN 1948-3:2006 Stationary source emissions - Determination of the mass concentration of PCDDs/PCDFs and dioxin-like PCBs - Part 3: Identification and quantification of PCDDs/PCDFs CEN/TS 1948-4:2007 Stationary source emissions - Determination of the mass concentration of PCDDs/PCDFs and dioxin-like PCBs - Part 4: Sampling and analysis of dioxin-like PCBs EN ISO 16000-1:2006 sampling strategy Indoor air - Part 1: General aspects of

Notes/standard status

89/429/EEC, 94/67/EC, 89/369/EEC 89/429/EEC, 94/67/EC 89/429/EEC, 94/67/EC, 89/369/EEC Under development 2010-05 ISO 16000-1:2004 89/106/EEC 89/106/EEC Approved 2008-08

Indoor air

Outdoor air

EN ISO 16000-12 Indoor air - Part 12: Sampling strategy for polychlorinated biphenyls (PCBs), polychlorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs) and polycyclic aromatic hydrocarbons (PAHs) EN ISO 6468:1996 Water quality - Determination of certain organochlorine insecticides, polychlorinated biphenyls and chlorobenzenes - Gas chromatographic method after liquid-liquid extraction EN ISO 5667-1:2006 Water quality - Sampling - Part 1: Guidance on the design of sampling programmes and sampling techniques EN ISO 5667-3:2003 Water quality - Sampling - Part 3: Guidance on the preservation and handling of water samples EN ISO 5667-3:2003/AC:2007 Water quality - Sampling - Part 3: Guidance on the preservation and handling of water samples

ISO 6468:1996 76/464/EEC ISO 5667-1:2006 ISO 5667-3:2003 ISO 5667-3:2003

Water

Soil

EN 15308:2008 Characterization of waste - Determination of selected polychlorinated biphenyls (PCB) in solid waste by using capillary gas chromatography with electron capture or mass spectrometric detection CEN/TR 15310-1:2006 Characterization of waste - Sampling of waste materials - Part 1: Guidance on selection and application of criteria for sampling under various conditions CEN/TR 15310-2:2006 Characterization of waste - Sampling of waste materials - Part 2: Guidance on sampling techniques CEN/TR 15310-3:2006 Characterization of waste - Sampling of waste materials - Part 3: Guidance on procedures for sub-sampling in the field. CEN/TR 15310-4:2006 Characterization of waste - Sampling of waste materials - Part 4: Guidance on procedures for sample packaging, storage, preservation, transport and delivery CEN/TR 15310-5:2006 Characterization of waste - Sampling of waste materials - Part 5: Guidance on the process of defining the sampling plan 99/31/EC EN 12766-1:2000 Petroleum products and used oils - Determination of PCBs and related products - Part 1: Separation and determination of selected PCB congeners by gas chromatography (GC) using an electron capture detector (ECD) EN 12766-2:2001 Petroleum products and used oils - Determination of PCBs and related products - Part 2: Calculation of polychlorinated biphenyl (PCB) content EN 12766-3:2004 Petroleum products and used oils - Determination of PCBs and related products - Part 3: Determination and quantification of polychlorinated terphenyls (PCT) and polychlorinated benzyl toluenes (PCBT) content by gas chromatography (GC) using an electron capture detector (ECD) EN 12766-3:2004/AC:2007 Petroleum products and used oils Determination of PCBs and related products - Part 3: Determination and quantification of polychlorinated terphenyls (PCT) and polychlorinated benzyl toluenes (PCBT) content by gas chromatography (GC) using an electron capture detector (ECD)

99/31/EC

Waste

99/31/EC 99/31/EC 99/31/EC

Petroleum products and used oils

TC 19

Insulating liquids

EN/C275-Food analysis

EN 1528-1:1996 Fatty food - Determination of pesticides and polychlorinated biphenyls (PCBs) - Part 1: General

EN 1528-2:1996 Fatty food - Determination of pesticides and polychlorinated biphenyls (PCBs) - Part 2: Extraction of fat, pesticides and PCBs, and determination of fat content EN 1528-3:1996 Fatty food - Determination of pesticides and polychlorinated biphenyls (PCBs) - Part 3: Clean-up methods EN 1528-4:1996 Fatty food - Determination of pesticides and polychlorinated biphenyls (PCBs) - Determination, confirmatory tests, miscellaneous No

Food

Animal feeding stuff Pulp, paper and board

TC 172 EN ISO 15318:1999 Pulp, paper and board - Determination of 7 specified polychlorinated biphenyls (PCB) SO 15318:1999

Chapter 4. ASTM Standards. ASTM International, originally known as the American Society for Testing and Materials (ASTM), is one of the largest voluntary standards development organizations in the world Matrix Outdoor air Indoor air Standard

ASTM D 4861-05 Standard Practice for Sampling and Selection of Analytical Techniques for Pesticides and Polychlorinated Biphenyls in Air ASTM D 5157-97. Small scale environmental chamber. Determination of Organic Emissions from Indoor Materials/products

Notes/standard status

Water Soil Waste Insulating liquids

ASTM D6160-98(2003)e1 Standard Test Method for Determination of Polychlorinated Biphenyls (PCBs) in Waste Materials by Gas Chromatography

Petroleum products and used oils

ASTM D 4059 Standard Test Method for Analysis of Polychlorinated Biphenyls in Insulating Liquids by Gas Chromatography

Food Animal feeding stuff Pulp, paper and board Chapter 5. DIN Standards. These standards are published by the German Institute for Standardization (Deutsches Institut für Normung). NOTES/STANDARD STATUS

German version EN 19481:2006 German version EN 19482:2006 German version EN 19483:2006 German version CEN/TS 1948-4:2007

MATRIX

STANDARD

DIN EN 1948- Stationary source emissions - Determination of the mass concentration of PCDDs/PCDFs and dioxin-like PCBs - Part 1: Sampling of PCDDs/PCDFs; DIN EN 1948-2:-Stationary source emissions - Determination of the mass concentration of PCDDs/PCDFs and dioxin-like PCBs - Part 2: Extraction and clean-up of PCDDs/PCDFs; DIN EN 1948-3: Stationary source emissions - Determination of the mass concentration of PCDDs/PCDFs and dioxin-like PCBs - Part 3: Identification and quantification of PCDDs/PCDFs DIN EN 1948-4:-Stationary source emissions - Determination of the mass concentration of PCDDs/PCDFs and dioxin-like PCBs - Part 4: Sampling and analysis of dioxin-like PCBs;

Outdoor air

DIN EN ISO 16000-12-Indoor air - Part 12: Sampling strategy for polychlorinated biphenyls (PCBs), polychlorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs) and polycyclic aromatic hydrocarbons (PAHs) DIN ISO 16000-13 Indoor air - Part 13: Determination of total (gas and particle-phase) polychlorinated dioxin-like biphenyls and polychlorinated dibenzo-p-dioxins/dibenzofurans - Collection on sorbent-backed filters DIN ISO 16000-14 Indoor air - Part 14: Determination of total (gas and particle-phase) polychlorinated dioxin-like biphenyls (PCBs) and polychlorinated dibenzo-p-dioxins/dibenzofurans (PCDDs/PCDFs) Extraction, clean-up and analysis by high-resolution gas chromatography VDI 2464 Part 1 Ambient air measurement - Indoor air measurement - Measurement of polychlorinated biphynyls (PCBs); GC/MS method for PCB 28, 52, 101,138, 153, 180 VDI 2464 Part 2 Ambient air measurement - Indoor air measurement - Measurement of polychlorinated biphenyls (PCBs); HR-GC/HR-MS method for coplanar PCBs VDI 4300 Part 2 Indoor-air pollution measurement - Measurement strategy for polycyclic aromatic hydrocarbons (PAHs), polychlorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs) and polychlorinated bibhenyle (PCBs) DIN 38407-3 German standard methods for the determination of water, waste water and sludge - Jointly determinable substances (group F) - Part 3: Determination of polychlorinated biphenyls (F 3) DIN 38414-20 German standard methods for the examination of water, waste water and sludge - Sludge and sediments (group S) - Part 20: Determination of 6 polychlorinated biphenyls (PCB) (S 20) DIN 38407-37 German standard methods for the examination of water, waste water and sludge - Jointly determinable substances (group F) Part 37: Determination of organochlorine pesticides, polychlorinated biphenyls and chlorobenzene in water - Method using gas chromatography (GC) and mass spectrometric detection (MS) after liquid-liquid extraction (F 37) Soil DIN EN 15308 Characterization of waste - Determination of selected polychlorinated biphenyls (PCB) in solid waste by using capillary gas chromatography with electron capture or mass spectrometric detection;

German version EN ISO 16000-12:2008

ISO/DIS 16000-13:2006

Indoor air

German

Water

German

German Under development

Waste

German version of EN 15308:2008

Petroleum products and used oils Insulating liquids Food Animal feeding stuff Pulp, paper and board VDI is the Association of German Engineer, the largest engineering association in Western Europe. Conclusions. Due to their toxicity the identification of PCBs in different matrices (air, water, waste, soil, food, human liquids) is very important. Standards provide specific vocabulary, good conditions for interoperability and enhence knowledge transfer and so they prove to be very useful to improve environmental protection and to reduce human exposure to hazardous substances. Bibliography: [1] http://www.iso.org [2] http://www.magazin.asro.ro [3] http://www.din.de [4] http://www.cen.eu [5] http://www.astm.org [6] http://www.vdi.de

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