1、PAS 61:2006 Determination of priority pollutants in surface water using passive sampling ICS 13.060.45 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW PUBLICLY AVAILABLE SPECIFICATIONPublishing and copyright information The BSI copyright notice displayed in this document indic
2、ates when the document was last issued. BSI 2006 ISBN 0 580 48149 2 Publication history First edition, May 2006 Amendments issued since publication Amd. no. Date Text affected PAS 61:2006 BSI 2006 i PAS 61:2006 Contents Foreword ii Introduction 1 1 Scope 3 2 Normative references 3 3 Terms and defini
3、tions 3 4 Principle 4 5 Handling sampling devices 5 5.1 General 5 5.2 Organics sampling devices 5 5.3 Metals sampling devices 5 6 Estimation of appropriate field deployment time 5 7 Sampling device preparation and assembly 6 7.1 Sampling device preparation 6 7.2 Sampling device assembly 6 7.3 Sampli
4、ng device storage 6 8 Quality assurance 6 8.1 General 6 8.2 Replicate quality control sampling devices 7 8.3 Sampling device controls 7 9 Selection of sampling site and safety precautions 9 9.1 Selection of sampling site 9 9.2 General safety precautions 9 10 Sampling device deployment and retrieval
5、10 10.1 Materials and apparatus 10 10.2 Deployment procedure 10 10.3 Retrieval procedure 11 11 Extraction of analytes from sampling devices and preparation for analysis 12 12 Analysis 12 13 Calculation 13 14 Test report 14 Bibliography 18 Annexes Annex A (informative) Relevant analytical methods (Eu
6、ropean and international standards) 15 Annex B (informative) Quality control measures 16 B.1 Recovery 16 B.2 Method detection limits (LoD) 17 B.3 Precision 17 List of figures Figure 1 Schematic representation of a passive sampling device 2 Figure 2 Quality control samples involved in passive samplin
7、g 7 List of tables Table 1 Sampling device control requirements 8 Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, pages 1 to 19 and a back cover.PAS 61:2006 ii BSI 2006 Foreword This Publicly Available Specification (PAS) was sponsored by the University
8、 of Portsmouth, UK, with financial support from the European Commissions Fifth Framework Programme, STAMPS, Contract No. EVK1-CT-2002-00119. It has been developed through the British Standards Institution (BSI). Acknowledgement is given to the following organizations that were consulted in the devel
9、opment of this PAS: AlControl (Sweden) AlControl (UK) Aquateam Norwegian Water Technology Centre Central Finland Regional Environmental Centre Chalmers University of Technology Consejo Superior de Investigaciones Cientificas D G T R e s e a r c h L t d Environmental Chemistry, Ume University, Sweden
10、 Environmental Monitoring Unit Ltd Exposmeter AB, Ume, Sweden L G C The Procter organophosphorus compounds; organotin compounds; substances and preparations, or the breakdown products of such, which have been proved to possess carcinogenic or mutagenic properties or properties which may affect stero
11、idogenic, thyroid, reproduction or other endocrine-related functions in or via the aquatic environment; persistent and bioaccumable and toxic (PBT) and very Persistent and very Bioaccumulating substances (vPvB); cyanides; metals and their compounds; arsenic and its compounds; biocides and plant prot
12、ection products; materials in suspension; substances that contribute to eutrophication (in particular, nitrates and phosphates); substances that have an unfavourable influence on the oxygen balance (and can be measured using parameters such as BOD (biochemical oxygen demand), COD (chemical oxygen de
13、mand), etc. Pollutant levels in surface water have traditionally been monitored by spot sampling (also known as bottle or grab sampling). Such sampling gives a snapshot of pollutant levels at a particular time. But pollutant levels in surface water have a tendency to fluctuate and so it is desirable
14、 to monitor pollutant levels over time. This may be achieved by repeated spot sampling, continuous monitoring, biomonitoring or passive sampling. Passive sampling involves the deployment of a calibrated device that uses a diffusion gradient to collect pollutants over a period of days to weeks, follo
15、wed by extraction and analysis of the pollutants in a laboratory. This provides a measure of time-weighted average concentrations of pollutants to which the sampling device was exposed. Passive sampling devices used in surface water typically consist of a receiving phase (typically a solvent or sorb
16、ent) that acts as a sink for compounds of interest, which may be held behind or surrounded by a membrane through which the target substances can permeate. A schematic representation of such a sampling device is shown in Figure 1. In its simplest form a passive sampling device is comprised solely of
17、a membrane, or fibre, or bulk sorbent which acts as a receiving phase.PAS 61:2006 2 BSI 2006 Figure 1 Schematic representation of a passive sampling device Key 1 Receiving phase 4 Membrane 2 Water 5 Pollutants 3 Housing NOTE In some sampling device designs, the housing is replaced by a membrane that
18、 completely encloses the receiving phase. For more information on individual types of passive sampling devices, refer to the Bibliography. 1 2 3 4 5 BSI 2006 3 PAS 61:2006 1 Scope This PAS describes a method for the determination of time-weighted average concentrations of priority pollutants in surf
19、ace water by passive sampling, followed by analysis. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (includin
20、g any amendments) applies. BS 6068-1.2, ISO 6107-2, Water quality Glossary Part 2: Additional terms relating to types of water, and treatment and storage of water and waste water, and terms used in sampling and analysis of water BS 6068-6.4, ISO 5667-4, Water quality Sampling Part 4: Guidance on sam
21、pling from lakes, natural and man made BS 6068-6.14, ISO 5667-14, Water quality Sampling Part 14: Guidance on quality assurance of environmental water-sampling and handling BS EN 25667-1, BS 6068-6.1, ISO 5667-1, Water quality Sampling Part 1: Guidance on the design of sampling programmes BS EN ISO
22、5667-3:2003, BS 6068-6.3:2003, Water quality Sampling Part 3: Guidance on the preservation and handling of water samples BS ISO 5667-6, Water quality Sampling Part 6: Guidance on sampling of rivers and streams 3 Terms and definitions For the purposes of this PAS, the terms and definitions given in B
23、S 6068-1.2 (ISO 6107-2) and the following apply. 3.1 analytical recovery standard compound added to sampling device receiving phase prior to analysis and whose recovery levels during analysis are used to provide information about recovery efficiency 3.2 fabrication control quality control sampling d
24、evice to record contamination from the manufacturing process, sampling device components, laboratory storage, processing and analytical procedures 3.3 field control quality control sampling device to record any chemical accumulated in sampling devices during transportation, deployment and retrieval
25、3.4 passive sampling collection of chemical compounds without provision of energy from an external sourcePAS 61:2006 4 BSI 2006 3.5 priority pollutant substance which is a potential source of water pollution NOTE A list of priority pollutants is given in the EU Water Framework Directive 2. 3.6 perfo
26、rmance reference compound (PRC) compound that has moderate to high fugacity from the sampling device, which does not interfere with the sampling and analytical processes and which is added to the device receiving phase prior to deployment NOTE 1 The off-loading (elimination) rates of the PRCs are us
27、ed to provide information about in situ uptake kinetics. NOTE 2 Currently there are no PRCs available for metals sampling devices. 3.7 reagent control retained aliquot of reagent used in preparation and analysis of sampling devices which is analysed with the samples in order to diagnose any contamin
28、ation from the reagents used 3.8 recovery spike quality control sampling device, pre-spiked with known mass of compounds of interest, used to determine the recovery levels of target compounds from processed sampling devices to establish control limits for the analytical process 3.9 sampling device c
29、lass class of target analytes which a sampling device is designed to accumulate NOTE Sampling device classes include the following: polar organic compounds; non-polar organic compounds; and inorganic compounds, including metals. 3.10 shipping control (optional) quality control sampling device to rec
30、ord any contamination or changes during transportation and storage of sampling devices on their way to and from the manufacturer to the user and from the user to the laboratory that performs the preparation of sampling devices for analysis 4 Principle Target priority pollutants accumulate in the rec
31、eiving phase of a passive sampling device over a defined time period of exposure to surface water. The pollutants are extracted from the sampling devices in the laboratory and the amount of each pollutant accumulated is determined by chemical analysis. Provided that mass transfer of the pollutant to
32、 the sampling device varies linearly with concentration, the time weighted average concentration of pollutants to which the sampling device was exposed over the deployment period can be calculated. The process is illustrated in a flow chart in Figure 2 in Clause 8. BSI 2006 5 PAS 61:2006 5 Handling
33、sampling devices 5.1 General 5.1.1 Ensure safety precautions are in place for handling all chemicals. 5.1.2 Because of the high sensitivity of the method, minimize physical contact with the receiving phase or membrane of the sampling devices. Where handling is necessary, use only new, powder free vi
34、nyl or latex gloves. Do not re-use gloves. 5.1.3 For some devices minimize exposure to airborne contaminants during manipulation in order to minimize vapour phase contamination. NOTE The use of a clean room conforming to BS EN ISO 14644-1, or laminar flow hood is recommended when preparing some samp
35、ling devices. 5.1.4 Store sampling devices and extracts away from other chemicals, particularly those of a volatile nature. 5.1.5 Use new suitable pipette tips for the addition of reagents to extracts. 5.2 Organics sampling devices 5.2.1 Minimize contact of organics sampling devices with plastic mat
36、erials. 5.2.2 Clean all equipment that comes into contact with sampling devices. 5.3 Metals sampling devices 5.3.1 Acid wash all equipment that comes in contact with the sample, other than the passive sampling devices, in accordance with BS EN ISO 5667-3:2003, 3.2.2.4. 5.3.2 Use suprapure acid for a
37、ddition to samples or for digestion. 6 Estimation of appropriate field deployment time Prior to deployment, estimate the exposure time for the class of sampling device on the basis of pollutant uptake rate and capacity of the receiving phase for the analytes of interest. NOTE 1 The exposure time sho
38、uld not extend to the non-linear uptake phase (see also Clause 4). NOTE 2 Where available, exposure time advised by the manufacturer should be used.PAS 61:2006 6 BSI 2006 7 Sampling device preparation and assembly 7.1 Sampling device preparation Where appropriate, prepare performance reference compo
39、unds solutions for each class of sampling device. Use these to spike the receiving phase of selected sampling devices prior to assembly, in the interests of quality assurance. Use fresh materials and state the use by date for the loaded passive sampling devices. NOTE The receiving phase should be ho
40、mogeneously spiked. In some cases, spiking can be carried out during manufacture. 7.2 Sampling device assembly 7.2.1 Assemble sampling devices in an environmentally controlled room equipped to remove atmospheric contaminants. 7.2.2 Label each sampling device in accordance with BS EN ISO 5667-3:2003,
41、 Clause 5. NOTE 1 Use of a clean room conforming to BS EN ISO 14644-1, or a laminar flow hood is recommended when preparing some sampling devices. NOTE 2 The addition of a suitable label for each sampling device by the manufacturer will aid sampling device identification during deployment and recove
42、ry and after recovery. 7.3 Sampling device storage Store prepared sampling devices in vapour-tight containers at controlled temperatures selected in accordance with manufacturers instructions. 8 Quality assurance 8.1 General Implement quality assurance measures throughout the fabrication, sampling a
43、nd handling processes in accordance with BS 6068-6.14 (ISO 5667-14). Compare results of analysis of sampling devices deployed together (as specified in 8.2), and of sampling devices with sampling device controls (as specified in 8.3), in order to calculate uncertainty of the sampling (see Clause 13)
44、. NOTE 1 Figure 2 illustrates how the quality assurance steps fit into the passive sampling process. NOTE 2 Guidance for analytical quality control is given in DD ENV ISO 13530. BSI 2006 7 PAS 61:2006 8.2 Replicate quality control sampling devices Prepare multiple sampling devices (e.g. 3 to 5 per s
45、ampling site) for each sampling device class: polar organics, non-polar organics and inorganics including metals. 8.3 Sampling device controls For each sampling device set (group of sampling devices deployed together), prepare sampling device controls in accordance with Table 1. The number and type
46、of controls is determined by the end user and is dependent upon the required level of confidence. NOTE For monitoring the concentration of chemicals near their limit of detection, more controls may be required. Figure 2 Quality control samples involved in passive sampling Preparation Storage Transpo
47、rt Deployment Exposure Retrieval Storage Transport Processing Analysis Fabrication controls Field controls Field controls Fabrication controls Reagent controls Recovery spikes Performance reference compounds Preparation Storage Transport Deployment Exposure Retrieval Storage Transport Processing Analysis Preparation Storage Transport Deployment Exposure Retrieval Storage Transport Storage Transport Processing Analysis Fabrication controls Field controls Field controls Fabrication controls Reagent controls Recovery spikes Performance reference compounds
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