The International Laboratory Accreditation Cooperation (ILAC) has established worldwide recognition of laboratory accreditation bodies through periodic peer evaluations resulting in mutual recognition (aka the ILAC Arrangement). This international, multilateral mutual recognition agreement among accreditation bodies aims to develop a global network of accredited testing, calibration and inspection facilities that can be relied on to provide impartial and accurate data. The fundamental purpose is to provide confidence in the competence of bodies supporting these activities. The speech will highlight the role of ILAC, the challenges facing the present system, the need to update the ISO/IEC 17000 series standards, and the long-standing issues of adequate measurement traceability and the application of measurement uncertainty.
226Ra is an important analyte in drinking water and effluents from mining operations due to its radioactivity and long halflife. 226Ra in mine effluents is regulated under metal mining and effluent regulations in Canada. Standard radiometric methods for the analysis of 226Ra are based on alpha spectroscopy after separation and concentration of the analyte via precipitation and filtration. A novel method employing online preconcentration and analysis via ICP-MS for the measurement of 226Ra in effluents is presented. The method has been successfully implemented at an operating mine site for the analysis of effluent water quality on a daily basis.
Québec City's population experienced a major outbreak of legionellosis during the summer of 2012, with 181 cases and 13 deaths. The Legionella source was an air conditioning cooling tower in the center of the city. At the time, no regulation required owners of cooling towers to manage Legionella levels in water and its associated health risks. Last spring, the Québec provincial government implemented a regulation requiring cooling tower owners to have a maintenance plan. The Québec government also assessed requiring monthly Legionella monitoring in 2014.
This presentation will look back on the 2012 outbreak and explain the actions taken by the Québec government to implement its new regulation. Legionella analysis and laboratory accreditation for Legionella analysis will also be discussed.
Many laboratories around the world perform routine testing on a wide range of samples such as food, water or biological materials. The results may have important public health implications as well as strong economic impact. For these reasons, the implementation of quality systems based on international standards is necessary. These standards provide procedures for the implementation of external and internal quality control for all activities conducted in the laboratory verification of the quality of results and periodic verification of the quality control system. One of the most important tools for quality control is the use of reference materials. A reference material is a substance or material in which one or more of its properties have a value sufficiently homogenous and well established to be used for the calibration of an apparatus, the evaluation of a measurement, or the validation of analytical methods. The NRC Certified Reference Materials (CRMs) program, which is operated by the Measurement Science and Standards portfolio, provides CRMs for analysis of biotoxins and other organic and inorganic contaminants in environmental samples, food and nutritional supplements. Over the years this program has developed in scope and today NRC is internationally recognized as an important producer of CRMs, which are distributed to over 40 countries.
Ruth Perez Calderon
Pinpointing persistent organic pollutants (POPs) among the ~100,000 chemicals used in industry and commerce represents major analytical and logistical challenges. As a consequence of their chemically inert behaviour, POPs are often toxic, resistant to degradation and prone to accumulate in living organisms.
Mass spectrometry (MS), typically hyphenated with (gas or liquid) chromatography, has developed into the most widely used technique for the analysis of POPs. Nowadays, it is relatively straightforward to develop highly sensitive and selective MS based methods for the identification and quantification of suspected POPs. However, such targeted methods are not usually helpful for the analysis of unknown POPs.
Sifting through the enormous data sets generated by current- and next-generation instrumentation is a major obstacle to identifying unknown POPs. One way to overcome this is to classify potential POPs on the basis of their mass defect, i.e., the slight deviation of the exact mass of a molecule from its integer value. It will be shown that an integrated strategy involving sophisticated MS technology, automated data processing software and in vivo toxicology experiments provides an efficient means to identify environmental pollutants in a variety of complex environmental samples.
Laboratories meeting ISO 17025 and other quality standards and Codes have statements describing their quality objectives and quality policies. These statements often fall short in linking quality to Laboratory competitive strategy. A reason for this short fall is that laboratories, in general, tend to view quality as a stand alone function. Laboratories interested in sustained competitive advantage must link their quality function to the overall business performance of the laboratory. This presentation will discuss:
This session will help participants with :
The analysis of polychlorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzo-furans (PCDFs) and dioxin-like polychlorinated biphenyls (dlPCBs), as well as other persistent organic pollutants (POPs) such as polybrominated diphenylethers (PBDEs) and polychlorinated naphthalenes (PCNs) is very challenging. Prior to instrumental analysis, all desired components of a compound group must be extracted from sample matrix. Target compounds must then be separated and purified by removing interferences through a cleanup procedure. Traditional open column cleanup for POPs takes up to three days for a set of ten samples for each of these groups of compounds excluding the time required for glassware cleaning and background contamination checks. Many laboratories analyse the various POPs separately, or combine two of the groups together due to difficulties in collecting the analytes in a single extract. In the past decade, automated extraction and cleanup systems have been adopted for the analysis of these compounds. Automated methods can produce reliable results for all four of the aforementioned groups of compounds, but requires extensive washing of the system between sample batches to minimize carryover and contamination. In this study, the CAPE Technologies cleanup technique was investigated for determination of dioxins and dioxin like compounds in environmental samples. Disposable columns provided by CAPE Technologies were used to analyze PCDD/Fs, dlPCBs, PBDEs and PCNs together in one analytical run for fish tissue and sediment samples. All four groups of compounds were successfully separated into two fractions. The results for compounds in each group were consistent and of high quality. Using disposable columns significantly reduces the cleanup time from three days to one day. Besides, using disposable columns eliminates cross contamination between sample batches. In addition, this technique uses much less solvent and generates much less waste solvent than other methods. The CAPE Technologies cleanup technique is simple, fast, inexpensive and environmentally friendly when compared to traditional and automated methods. It can be used as an effective cleanup method for the simultaneous sample preparation of PCDD/Fs, dlPCBs, PBDEs and PCNs for a variety of environmental matrices
The ISO 17025 standard is an ISO standard that has been in place for about fifteen years and used in Canada and elsewhere, mostly in the developed and developing world to accredit laboratories. It has been adopted by many commercial and public laboratories since its inception in 1999. Interestingly, just before this ISO standard became common, but around the same time, a few serious water quality incidents occurred that help speak to the standards importance.
From 2007 to 2010, in partnership with the University of Guelph, the development of an Ontario Ministry of the Environment laboratory method to assess bioaccumulation of contaminants from field-collected sediments in three freshwater organisms was undertaken. From the very beginning the method was developed with standardization in mind. After a very thorough literature review of current practice in bioaccumulation assessments, meticulous thought went into assessing the impact of key variables on data quality (e.g., loading density, organism size, standardizing sediment total organic carbon). In the end a Ph.D. thesis and "Bioaccumulation of sediment-associated contaminants in freshwater organisms" method were complete. Then came the task of putting this method into practice in a production laboratory for new sediments and new and emerging compounds. The authors will discuss how the process of accrediting and co-ordinating an inter-laboratory assessment of a new method has posed both interesting and frustrating challenges. Along the way the authors will attempt to draw parallel comparisons between chemical and biological method development and highlight the aspects of biological testing that make it unique. In addition, how the strong basis of method validation to the international standard, ISO 17025 has allowed this method to confidently be adapted to answer new and challenging questions will be discussed.
Contaminants of emerging concern (CECs) in the environment are generally described as contaminants that were unknown, unrecognized (not detectable) or unregulated (not routinely monitored) and, represent a diverse group of chemicals that may pose a risk to human health and the environment. CECs can be discovered with either newly available analytical technologies and/or implicated by a prior knowledge of the process details. Due to limited analytical capability (e.g., hardware, software, analytical standards), analysis of CECs has been focused on selected analytes rather than a holistic approach, which includes as many known chemical classes in the analysis as possible. Using water and wastewater treatment plant samples, a new analytical workflow was proposed, applied and evaluated in the quantitative analysis of 58 CECs and qualitative analysis of their treatment by-products.
An ultrahigh performance liquid chromatography (UHPLC) system with Thermo Hypersil Gold® and Betasil® C18 columns, 2.6 , 2.1x100mm to separate acidic and base/neutral compounds was used. Analytes eluted from these two analytical columns were transferred via an electrospray ionization source (ESI) to an Orbitrap mass spectrometer (Orbitrap MS, ThermoFisher Scientific Exactive Plus), analyzed in positive and negative ionization modes at mass resolution setting of 140,000. The UHPLC separations used a flow rate of 0.45 mL/min and 15-min gradient elution. Mobile phases used for positive ionization were 5 mM HCOONH4/0.1% HCOOH in 10:90/CH3OH:H2O (A) and 90:10/CH3OH:H2O (B); and negative ionization used 10:90/CH3CN:H2O with pH adjusted to 6.95±0.3 (A) and CH3CN (B). These parameters and the column used produced chromatographic peaks with full-width-at-half maximum (FWHM) of about eight seconds. The Orbitrap MS was set to collect data from 95 to 950 amu at a scanning speed of about 1.7 scans/sec, resulting in 25-30 data points to precisely define chromatographic peaks. Analytical data were transferred to an offline data processor where data were screened against a database of >400 target compounds (CECs) including phthalates, anesthetics, biocides, corrosion inhibitors, musk fragrances, quaternary ammonium surfactants, sunscreen cosmetics, UV-light stabilizers, hormones, estrogens, veterinary drugs, pesticides, perfluorohydrocarbons, pharmaceuticals and personal care products (PPCPs) and known metabolites, and treatment byproducts of pesticides and PPCPs. Using TraceFinder 3.1 software, identification of these target compounds was performed by UHPLC retention time and accurate mass of quasi molecular ions (i.e., protonated molecule ion or ion formed from a molecular ion by loss of a hydrogen atom) of each target. Taking advantage of the long-term mass axis stability of the Orbitrap MS, a mass extraction window of ±5 ppm was used to do both qualitative and quantitative analysis. Quality control/quality assurance data obtained from routine UHPLC-Orbitrap MS analysis of clean water samples have shown good precision and accuracy for the 58 target compounds analyzed. Quantitative analysis was performed for target compounds with analytical standards while area counts of positively-identified analytes were used to monitor treatment efficiency, occurrence, temporal and seasonal trends. This method eliminates matrix effects observed in UHPLC/tandem mass analysis particular seen in the analysis of ethinylestradiol (EE2), allowing for the unambiguous identification and quantitation of EE2 and other estrogens in environmental samples.
This presentation examines the aggregate performance of accredited and non-accredited laboratories in CALA proficiency testing studies, using summary data reported on the CALA web site (http://www.cala.ca/pt_accred_vs_nonaccred.html). Failure rates of the two groups are tracked for some individual test groups, and for multiple test groups combined, in 19 rounds between October 2003 and January 2013. The results demonstrate improved performances of both groups over the 10-year period, and that for several of the test groups there is at least a 99% level of confidence that the mean failure rate for non-accredited laboratories is greater than that for accredited laboratories.
Lab uncertainty is a quantifiable term related to the analytical method. However,it is a very misleading and almost insignificant term in the analysis of soils where 1-2 g sub-samples are being forced to represent the 100-200 g sample delivered to the lab. The problem is largely being ignored with the result that many soil analyses are statistically meaningless, especially when the soil is coarse-grained and the contaminant levels are low. The real uncertainty in these cases can be several hundred percent and this is creating great confusion for the consultant in the interpretation of the site condition, resulting in needless cleanups in some cases and needless failures to clean up in others. Real life examples will be presented and possible solutions discussed.
Most of the Chemical laboratories designed to support manufacturing operations, are design/built on a conventional casework basis, by architects and engineers with little knowledge of advanced analytical methods and advancements in equipment technology. The presentation will focus on the different design aspects of a chemical lab, with emerging technologies in both lab peripherals and instrumentation. It will look at the modular design concepts and briefly touch on the footprint changes for analytical instruments like XRF, ICP, NMR and other analytical instruments.
Representatives from the Canadian Food Inspection Agency (CFIA), a regional municipality, a representative speaking for provincial regulators as well as a member of the private sector have all been invited to each brief the delegates on what may be on the horizon from the various perspectives of the regulators.
Dr. Corinne Pequignot
Natural – matrix materials such as fish and mussels tissues were used in the NCP III Phase 7 interlaboratory study (ILS) which was conducted to assess the performance of laboratories providing data to Northern Contaminants Program (NCP) and to Arctic Monitoring and Assessment Programme (AMAP). This study is part of the NCP III Quality Assurance/Quality Control (QA/QC) Program. The QA/QC studies focused on performance evaluation of analytical laboratories providing data to the NCP managers. Analysis is performed on contaminants of concern such as trace metals, persistent organic pollutants (POPs) and emerging contaminants. The number of participating laboratories increased from the previous study (42 vs 32 labs) and has doubled since Phase 1 (19 labs in 2005/2006).
Six natural-matrix materials and twelve injection-ready standards were provided to assess levels of organic and inorganic contaminants. Data quality assessments were conducted for dioxins, organochlorine pesticides (OCs), polychlorinated biphenyls (PCBs) and emerging contaminants (polybrominated diphenyl ethers (PBDEs) including brominated flame retardants (BFRs), perfluorinated chemicals (PFCs), polychlorinated naphthalenes (PCNs), chlorinated paraffins (CPs), and trace metals including mercury and methyl mercury. Results were evaluated using “Robust Statistics: a method of coping with outliers”. Compared to the previous rounds, laboratories demonstrated higher performance for certified natural-matrix material for PDBEs/BFRs, OCs, trace metals and higher performance for uncharacterized natural-matrix material for PCDDs/PCDFs/DLPCBs. The increased numbers of participated laboratories helps to expand the database and data comparability of the results. The final NCP III Phase 7 QA/QC report is available upon request. An eighth round in the series of studies is currently being conducted in anticipation of achieving further improvements in the analysis of these contaminants. An overview of the program and results of laboratory analytical performance will be disused.
Section 5.6 of ISO 17025 requires that all equipment used for tests and/or calibrations, including equipment for subsidiary measurements (e.g. for environmental conditions) having a significant effect on the accuracy or validity of the result of the test, calibration or sampling shall be calibrated before being put into service and that the programme for calibration of equipment shall be designed and operated so as to ensure that calibrations and measurements made by the laboratory are traceable to the International System of Units (SI). This presentation will review in detail the many aspects of this section of the standard; discuss various interpretations (such as - what is "a significant effect" and explore how they apply to testing labs using either external calibration providers or in-house calibration methods.
Quantitative Analysis of the Accuracy of the Uncertainty of Measurement Mike Gao, Debra Long and Steve Craik (EPCOR Water Services, Edmonton, AB) Abstract Any measurement has its uncertainty. Uncertainty is considered to be an attribute associated with the measurement result. Uncertainty of measurement (UM) is defined as a parameter that characterizes the dispersion of the values that can reasonably be attributed to the measurand (BIPM, etc., Guide to the Expression of Uncertainty in Measurement, 2008). The estimation of UM is a requirement of ISO/IEC 17025 due to the limitation of the test method, the needs of the customers and the existence of narrow limits on which conformity to a specification are based. Therefore, the accuracy of the estimated uncertainty becomes important. In order to estimate the true value of the measurand, a limited number of repetitive measurements are performed and the mean result is calculated. The mean result is the best estimate of the true value. Similarly, the UM is calculated based on a limited number of repetitive measurements. Therefore, the estimated UM also has its own uncertainty for a defined number of repetitive measurements. The larger number of repetitive measurements used in the estimation, the closer the mean result is to its true value and the closer the estimated UM is to its true uncertainty. This study focuses on the quantitative analysis of the UM. The F-test is used to evaluate the accuracy (or inaccuracy) of the estimated UM and to define the confidence intervals of the UM. The correlation between the uncertainty of the UM and the number of repetitive measurements is also studied. A consideration of applying a safety factor in the reportable UM is discussed. Both the theory and the application are examined. The Monte Carlo technique is used in the simulation of the application. This study will provide meaningful guidance for users when UM, associated with the measurement result, is a significant consideration in decision making. It also helps people to better understand the statistical meaning of quality control limits and to set up scientifically sound quality control statistics that are fit for the purpose of measurement.
The majority of analytical methods using instrumental detection assume a simple linear y = mx + b type relationship between analyte concentration and either instrument response or a mathematical transform of instrument response (e.g. pH, Beer-Lambert law). This assumption ignores commonly encountered second and third order effects that may result in significant departures from the simple linear model and induce significant bias in test results. Examples of higher order effects and calibration algorithms that provide workable solutions will be discussed.
Specific topics covered:
Environment Canada is currently in the process of revising the national Metal Mining Effluent Regulations, and is in consultation with relevant stakeholders on these revisions. Selenium is a metalloid chemical of concern being monitored in the effluents of various mining operations. This presentation will focus on a discussion of various analytical issues pertaining to industrial reporting for regulatory purposes. Specifically, the importance of practical quantitation limits (PQLs) and method detection limits (MDLs), in the context of applying regulatory guidelines and effluent discharge limits, will be evaluated and discussed.
One of the key factors for traceable weighing results is effective calibration and routine testing embedded in the quality management system of an organization. While calibration of weighing instruments is well understood on a metrology level, there are still many ambiguities within the quality department, the laboratory or the shop floor on how to interpret calibration data and proof the validity of weighing results. Especially the concept of minimum weight which is a direct consequence of measurement uncertainty is not established well in the industry despite of the existence of specific balance regulations as e.g. USP General Chapter 41 "Balances".
This session introduces GWP, the global standard for risk-based lifecycle management of weighing equipment. It provides scientific guidance regarding calibration and routine operation of the instruments. GWP takes into consideration the following standards:
GWP provides scientific knowledge about the specific methodology and the frequencies of regular calibration and routine tests required by quality standards, based on the respective process accuracy requirements and the risk of the weighing application. The concept of minimum weight ensures that all measurements come with a controlled measurement uncertainty, meeting the specific accuracy requirements. The risk-based approach, on the other hand, provides a systematic methodology to define calibration and test frequencies. Specifically regarding routine testing there are widespread misconceptions throughout the industries. Proven by experimental data, a scientific strategy is presented that defines appropriate testing to qualify weighing equipment in a cost-effective and efficient manner. What you will take away:
The determination of trace elements As, Se, Cd and Hg by ICP-MS is hampered by spectral interferences. Notably, the overlap from 40Ar35Cl+ and 40Ca35Cl+ on 75As+, 40Ar38Ar+ and 40Ca38Ar+ on 78Se+, 95Mo16O+ and 94Mo16OH+ on 111Cd+, and 184W16OH+ on 111Hg+ are so severe that a high mass resolution of 8,000 to 30,000 is required to resolve all these interferences. If the interfering peak is greater than the analyte peak, a much greater resolution is required. The more contaminated the sample, the worse the interference and more severe the degradation in accuracy and detection capability. At a mass resolution >8,000, over 95% of the analytical signal is lost in conventional sector field systems. Mathematical corrections for such interferences are painstaking, inaccurate, and fraught with uncertainties.
Agilent's latest ICP-MS technology can easily and reliably resolve these interferences, with good sensitivity and detection limits for matrices laden in interferences occurring at different concentrations and proportions. The basic principles of spectral interference control using chemical resolution, mass resolution, relaxation focusing and kinetic energy discrimination will be explained.
The Laboratory Service Branch (LaSB) of the Ministry of the Environment analyzes several hundred water samples for mercury every year in support of the Ministry's various Regulatory and Monitoring Programs. Recently, LaSB had purchased two new instruments capable of analyzing mercury in aqueous levels lower than previously possible with our current instrumentation. The presentation will discuss the process of developing, comparing and validating the new analytical method.
Sampling is typically required for both monitoring and for research purposes. Sampling data may be used to monitor air and water effluents or to characterize various environmental media (air, water, soil, biota) for pollutant levels. It may also be used to comply with regulatory requirements, detect accidental releases, identify trends, or develop an inventory or database of pollutant levels.
The CALA Current Sampling Practices Guide has been developed to provide anyone involved in environmental or many other types of sampling with sufficient information in the form of existing best practice examples, to plan and carry out scientifically defensible sample collection for submission to a laboratory for analysis.
The intent is to show what documentation is currently available on the subject of what happens between the time that a sampler (an individual who does sampling) receives instructions to visit a sampling target and when the sample arrives at the laboratory for testing.
The intent is not to recommend or mandate particular sampling instructions, rather to show what the body of knowledge on the subject is currently.
With this Guide we hope that users of the information can identify areas where: