TECHNICAL REPORT: OF WATER QUALITY LABORATORIES

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UN/ECE Task Force onLaboratory Quality Management &AccreditationTECHNICAL REPORT:GUIDANCE TO OPERATIONOF WATER QUALITYLABORATORIESSeptember 2002

PREFACEThe “Guidance to Operation of Water Quality Laboratories” was drawn up as part of theactivity of the UN/ECE Task Force on Laboratory Quality Management & Accreditation(UN/ECE TF-LQM&A) under the Convention on the Protection and Use ofTransboundary Watercourses and International Lakes (Helsinki, 1992) by taking intoaccount the requirements of the Guidelines on Water-Quality Monitoring andAssessment of Transboundary Rivers (prepared by RIZA, the Netherlands as leadcountry of the UN-ECE Task Force on Monitoring and Assessment).Before drawing-up the guidance the UN/ECE TF-LQM&A completed a survey on thepresent practices in the laboratories implementing water quality monitoring in thecountries signatory to the Convention. The survey included: (a) information on thesampling and analytical methods used, (b) inventory on the laboratory facilities includinginstrumentation, and (c) the quality control measures and status of accreditation. 27 outof 46 countries responded to a Questionnaire, which had been distributed in English andRussian languages. In addition to the information from this survey, requirements oflaboratory accreditation, guidelines for good laboratory practices, laboratory practices indeveloped countries and related documents (e.g., Handbook for Analytical QualityControl in Water and Wastewater Laboratories, US-EPA) have been taken into accountduring drawing-up the guidelines.The guidance was revised by the members of the Task Force Core Group in December1999, during the first half of 2000 and in the year 2001. It was discussed during the firstand second meeting of Monitoring and Assessment Working Group too.The guidance is addressed to laboratory managers, leaders of field investigations, andother personnel who bear responsibility for generation of water and wastewater data.Information is offered to assist the reader in establishment of water (environmental)laboratories, particularly taking into account the quality control measures needed forprevention and correction of factors leading to breakdowns in the validity of data.

Table of ContentPART I.12345INTRODUCTION.11.1 Objectives and Character of the Guidance. 11.2 Monitoring Cycle and Activities Dealt with in this Guidance. 11.3 Laboratory Quality Management . 21.3.1 Methodologies. 41.3.2 Laboratory Facilities and Personnel. 8QUALITY REQUIREMENTS OF WATER QUALITY MONITORING .92.1 Quality Assurance, Quality Control in Water Laboratories. 92.2 Requirements for Accreditation . 10COLLECTION OF SAMPLES FROM THE AQUATIC ENVIRONMENT.133.1 Sample Collection from Sediments. 163.1.1 Sampling Equipment . 163.1.2 Storage, Transport and Preservation of Sediment Samples . 193.1.3 Selection of Particle Size . 213.1.4 Drying of Sediment. 21PREREQUISITES OF QUALITY WORK IN LABORATORIES .224.1 Laboratory Services. 224.1.1 Distilled-Deionised Water . 224.1.2 Compressed Air. 254.1.3 Electrical Supplies. 254.2 Instrumentation. 264.3 Laboratory Glassware . 274.3.1 Types of Glassware. 284.3.2 Glassware for Volumetric Analyses. 294.3.3 Cleaning of Glass and Porcelain. 304.3.4 Disposable Glassware . 314.3.5 Specialized Glassware. 324.4 Reagents, Solvents and Gases . 324.4.1 Reagent Quality . 324.4.2 General lnorganic Analyses . 334.4.3 Radiological Analyses . 344.4.4 Analyses of Organic Compounds. 344.4.5 Storing and Maintaining Quality of Reagents and Solvents . 354.5 Elimination of Determinate Errors. 364.5.1 Reagent Blank. 364.5.2 Method Blank . 364.5.3 Elimination of Interferences. 364.6 Laboratory supplies . 38SPECIAL REQUIREMENTS FOR TRACE ORGANIC ANALYSIS.395.1 Collection of the Samples. 395.1.1 Discrete BottIed Samples. 395.1.2 Carbon Adsorption Samples . 40

5.2 Glassware. 405.3 Reagents and Chemicals . 405.4 Common Analytical Operations . 416 CONTROL OF ANALYTICAL PERFORMANCE .436.1 Precision and Accuracy . 436.2 Evaluation of Daily Performance . 466.2.1 Quality Control Charts. 477 DATA HANDLING AND REPORTING .497.1 The Analytical Result Value . 497.1.1 Significant Figures . 497.1.2 Rounding-Off Numbers . 507.1.3 Glossary of Terms . 517.2 Report Forms. 527.2.1 Loose Sheets . 527.2.2 Bound Books . 527.2.3 Pre-Printed Report Forms . 537.2.4 Digital Read-out . 548 SKILLS.558.1 Skills . 568.2 Training . 56References, literature.57Annex 1. .58Annex 2. .61Annex 3. .83

Page 1Technical report: Guidance to operation of water quality laboratoriesPART I.1 INTRODUCTION1.1Objectives and Character of the GuidanceThis guidance is intended to assist ECE Governments and joint bodies (e.g. bilateral ormultilateral river commissions) in understanding laboratory quality management andproviding guidance to laboratory managers to design or upgrade water laboratories andto strive for accreditation.The target group comprises decision-makers in ministries with competence onenvironment, water management and human health; environmental, water, health andother competent agencies, and all those who are responsible for managing themonitoring and assessment of transboundary rivers.The character of this guidance is technical rather than strategic as the latter aspects arebeing dealth with in the relevant chapters of the Guidelines on monitoring andassessment of transboundary rivers and transboundary groundwaters (see thedocuments for the forthcoming second meeting of the Parties to the Convention issuedunder symbol MP.WAT/2000/9 and 10).1.2Monitoring Cycle and Activities Dealt with in this GuidanceThe process of monitoring and assessment should principally be seen as a sequence ofrelated activities that starts with the definition of information needs, and ends with theuse of the information product. This cycle of activities is shown in Figure 1.Water managementInformation needsInformation utilisationAssessment and reportingAssessment strategiesData analysisMonitoring programmesData handlingData collectionFigure 1. The monitoring cycle

Page 2Technical report: Guidance to operation of water quality laboratoriesSuccessive activities in this monitoring cycle should be specified and designed basedon the required information product as well as the preceding part of the chain. Indrawing up programmes for the monitoring and assessment of river basins, ripariancountries should jointly consider all stages of the monitoring process.The guidelines on monitoring and assessment are supported with five backgroundreports, which are as follows: Transboundary rivers and international lakesCurrent practices in monitoring and assessment of rivers and lakesBiological assessment methods for watercoursesQuality assuranceState of the art on monitoring and assessment of riversAlthough the guidelines and the background reports deals with some aspects of thelaboratory work, particular the major quality assurance approaches, there is a need forguidance in establishment and upgrading laboratory work in water/environmentallaboratories.The evaluation of the obtained information may lead to new or redefined informationneeds, thus starting a new sequence of activities. In this way, the monitoring processwill be improved.The present guidance on laboratory quality management exclusively deals with theactivity designated in the above figure by “Data collection”. This activity in themonitoring cycle is composed of a number of sub-activities such as collecting samples,ensuring quality work in laboratories and reporting analytical results.The guidance summarised in the present document will address to laboratory managersdesigning or upgrading water laboratories and will help these laboratories in thecountries in transition to be prepared for accreditation.1.3Laboratory Quality ManagementWater quality targets, objectives and standards are set to evaluate the quality of thewater resources, both surface and subsurface water bodies, to characterise ecologicalstatus (for surface waters) and to establish satisfactory condition for intended uses ofthe aquifer(s). The laboratory data define whether that condition is being met, andwhether the water is at acceptable quality to fit for the purpose. If the laboratory resultsindicate a violation of the standard, action is required by the pollution control authorities.The analyst must be aware that his professional competence, the procedures he hasused, and the reported values are reliable and may be used with confidence.Similarly to the monitoring cycle in water management we can draw a measurementcycle for the implementation of the monitoring, starting with the collection of samplesand closing with reporting the analytical results. As the place of the measurement cyclein the monitoring cycle is indicated in Figure 1 as “Data collection”, Figure 2 shows the

Page 3Technical report: Guidance to operation of water quality laboratorieselements of the measurement cycle. It starts with the sampling and closes with reportingthe measurement results.Information needsInformation utilizationMonitoring programmesData handlingQuality AssuranceQuality ControlSampling planMeasurement resultsSample CollectionField measurementsLaboratorymeasurementsFigure 2. The measurement cycle ensuring the quality of the monitoring results.Water quality monitoring rests upon a firm base of laboratory data. The role of theanalytical laboratory is to provide the qualitative and quantitative data to be used fordifferent purposes. The data must accurately describe the characteristics or the sample,or the type and concentration of constituents in the sample analysed in the laboratory. Inmany cases, an approximation or invalidated (incorrect) result is worse than no answerat all, because it will lead to miss interpretations.The progress of research, effectiveness of pollution control will depend upon the validityof the results reported by the laboratory. Therefore, the laboratory data must be backedup by an adequate programme to document the proper control and application of all ofthe factors, which effect the final result.Depending on the information needs of the water management, monitoring datacollection relate to physical, chemical, radiological, hydrobiological, ecotoxicological andmicrobiological measurements. Generation of these data requires representativesampling followed by analytical work in specialised laboratories.

Page 4Technical report: Guidance to operation of water quality laboratoriesThe design of the monitoring programme should describe the targeted water qualityvariables (characteristics, parameters, determinands), the matrices in the aquaticenvironment from where samples should be taken, analytical accuracy targets, includingdetection limits, application ranges and acceptable tolerances. The specialisedlaboratories should apply the appropriate sampling and analytical methods, should havethe necessary rooms, should be properly equipped, having the necessaryinstrumentation. Skills of laboratory personnel must ensure the quality of the work duringthe sampling and the analyses.Compilation of the guidance on laboratory quality management has been based on theexpectation that sampling and laboratory work consider all kinds of measurements,which might be required during implementation of the water quality monitoring, detailedin the monitoring design. The guidance target considerations, which should taken duringdesign and operation of the laboratories to generate reliable, comparable monitoringresults.The laboratory management should plan the work in the laboratory before starting withthe sampling. Sampling and analytical methodologies must be defined as the first step ofthe implementation of the monitoring.1.3.1 MethodologiesIn general, the widespread use of a sampling or analytical method, its appearance ininternational/national methodological standard indicates that it is a reliable means ofsampling or analysis. This fact tends to support the reliability of the results reported. Theuse of an individual method, or a little-known technique forces the data user to questionthe appropriateness and validity of the results.The need for standardisation of methods or using standardised methods within alaboratory is readily apparent. Uniform methods among co-operating laboratories, e.g.,implementing monitoring in international river basins, are also important in order toremove the methodology as a variable in comparison, or joint use of data. Uniformity ofmethods is particularly important when laboratories are providing data to a common databank, or when several laboratories are co-operating in joint field surveys. The lack ofstandardisation of methods raises doubts as to the validity of the results reported. If thesame constituent is measured by different analytical procedures within a singlelaboratory, or in several laboratories, the question is raised as to which procedure issuperior, and why the superior method is not used.Selection of an analytical method should be made by careful considerations. Forexample, physical and chemical methods for monitoring should be selected by thefollowing criteria: The method should measure the desired constituent with precision and accuracysufficient to meet the data needs even in the presence of interferences, whichmight be encountered in the samples. Box 1 and Table 1 show the approachused in the Danube river basin transnational monitoring network.

Page 5Technical report: Guidance to operation of water quality laboratories The procedure should utilise the equipment and skills available in the laboratory. The selected methods should be in use that the methods are properly validated. The method should be sufficient to produce the measurement results within therequired time-frame.Box 1. Determinands: basis for selection of appropriate analytical methodin the Danube river basin Tans-National Monitoring Network (TNMN)The resulting lists of determinands for water and sediments as agreed for the DanubeTNMN are presented in Table 1, together with the levels of interest and analyticalaccuracy targets, which are defined as follows: The minimum likely level of interest is the lowest concentration considered likely to beencountered or important in the TNMN. The principal level of interest is the concentration at which it is anticipated that mostmonitoring will be carried out. The required limit of detection is the target limit of detection (LOD), whichlaboratories are asked to achieve. This has been set, wherever practicable, at onethird of the minimum level of interest. This is intended to ensure that the bestpossible precision is achieved at the principal level of interest and that relatively few"less than results" will be reported for samples at or near the lowest level of interest.Where the performance of current analyses is not likely to meet the criterion of aLOD of one

the sampling. Sampling and analytical methodologies must be defined as the first step of the implementation of the monitoring. 1.3.1 Methodologies In general, the widespread use of a sampling or analytical method, its appearance in international/national methodological standard indic

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