Laboratory Quality Assurance And Quality Control .

TermDefinitionGroundwater ProtectionCriteriaDefined in Remediation Standard Regulations, Section 22a-133k-1(a) of theRegulations of Connecticut State Agencies.Holding TimeThe maximum amount of time a sample may be stored between collection and analysisis referred to as the holding time. Samples analyzed past the holding time arecompromised and may be considered invalid, depending on the intended use of thedata.Industrial CommercialDirect Exposure CriteriaSee Remediation Standard Regulations, Section 22a-133k-1(a) of the Regulations ofConnecticut State Agencies.Initial Demonstration ofCapabilityThe analysis of a set of known concentration samples or standards used to documentan analyst's ability to perform an analytical procedure correctly. The results of theanalyses must meet the precision and accuracy criteria of the method.Instrument BlankAn instrument blank is analyte free media that is introduced into the analyticalinstrumentation to verify the instrumentation is not contaminated. Typicallyinstrument blanks for gas chromatography are pure solvent, while those for metals orwet chemistry techniques are reagent water or acidified reagent water.Internal StandardsInternal standards are compounds that are added, prior to analysis, at a knownconcentration to every standard, blank, sample, and quality control sample at a knownconcentration. Internal standards are used to calibrate the analytical system by plottingthe response of the internal standards versus the compound(s) of interest. Internalstandards should closely match the chemical behavior of the compound(s) of interestand be known not to be present in the sample.Laboratory Control SampleA laboratory control sample (LCS) is a purchased reference standard or reagent wateror clean soil spiked by the laboratory with compound(s) representative of the targetanalytes. The LCS is analyzed in an identical manner as a sample and is used todocument laboratory performance. The results of the LCS are used to documentaccuracy, and precision of the analytical methodology. LCSs are sometimes called alaboratory fortified blank.Laboratory Fortified BlankSee Laboratory Control SampleLaboratory FortifiedSample MatrixSee Matrix SpikeLaboratory Reagent BlankSee Method BlankMatrix DuplicateA matrix duplicate refers to the replicate analysis of a sample prepared in thelaboratory. Duplicates are used to evaluate precision, sample homogeneity, and fieldsample collection activities.vii

TermDefinitionMatrix EffectsThe overall effect of the sample matrix on the analytical results. Severe matrix effectsare usually called matrix interference and can significantly affect the accuracy of ananalytical measurement. For example, some matrices including silt, clay, coal, ash,and peat effectively bind analytes leading to low biased results for certain extractionprocedures.Matrix InterferenceSee Matrix EffectsMatrixThe component or substrate (e.g. surface water, drinking water, soil) that may, or maynot, contain an analyte of interest.Matrix SpikeAn aliquot of an environmental sample to which known quantities of analytes areadded in the laboratory. The matrix spike is analyzed in an identical manner as asample. The purpose of a matrix spike sample is to determine whether the samplematrix contributes bias to the analytical results.Matrix Spike DuplicateAn intra-laboratory split sample, with both aliquots spiked with identicalconcentrations of method analytes. The spiking occurs prior to sample preparationand analysis. The results are used to document the precision and bias of a method in agiven sample matrix. See also “matrix spike.”MediaSee MatrixMethod BlankAn analyte-free matrix to which all reagents are added in the same proportions as usedin sample processing. The method blank should be carried through the entire samplepreparation and analytical procedure. It is used to determine if method analytes orother analytes are present in the laboratory environment, the reagents, or the apparatus.Non-conformanceAn occurrence during the processing or analysis of a sample that is not in conformancewith the quality control criteria of the analytical method. Examples of nonconformances include, but are not limited to: missed holding times, temperatureexcursions, recoveries of surrogates or matrix spikes outside of criteria, initial orcontinuing calibration failures, et cetera.Performance EvaluationSampleSee Proficiency Test SamplePetroleumUsed in this document as the term is defined in Section 22a-449a of the ConnecticutGeneral Statutesviii

TermPrecisionDefinitionThe agreement among a set of replicate measurements without assumption ofknowledge of the true value. Precision is estimated by means of duplicate/replicateanalyses and illustrates the reproducibility of a laboratory’s analysis. Field duplicatesare used to assess precision for the entire measurement system including sampling,handling, shipping, storage, preparation and analysis. Laboratory data precisionanalysis is evaluated through the use of matrix spike/matrix spike duplicate sampleresults. The precision of data is measured by the calculation of the relative percentdifference (RPD) by the following equation:RPD A-B ((A B)/2)x 100Where:A Analytical results from first duplicate measurementB Analytical results from the second duplicate measurementProficiency Test SampleA reference sample provided to a laboratory for the purpose of demonstrating that thelaboratory and the individual analyst performing the test can successfully analyze thesample within acceptable limits. The true value of the sample is unknown by thelaboratory.Proficiency TestingA program in which performance evaluation samples are used to evaluate theanalytical performance of the laboratory.Quality Assurance PlanAn orderly assemblage of detailed procedures designed to produce data of sufficientquality to meet the data quality objectives for a specific data collection activity.Quality Assurance/QualityControlQuality Assurance (QA) involves planning, implementation, assessment, reporting,and quality improvement to establish the reliability of laboratory data. QualityControl (QC) procedures are the specific tools that are used to achieve this reliability.QC procedures measure the performance of an analytical method in relation to the QCcriteria specified in the analytical method. QC information documents the quality ofthe analytical data.Reagent waterReagent water is generally, water that has been generated by any method, which wouldachieve the performance specifications for American Society for Testing MaterialsType II water. For organic analyses, reagent water is free from contamination of theanalytes of interest.Reasonable ConfidenceWhen “Reasonable Confidence” is achieved for a particular data set, theenvironmental professional will have “Reasonable Confidence” that the laboratory hasfollowed the Reasonable Confidence Protocols, has described non-conformances, ifany, and has adequate information to make judgments regarding data quality.Reasonable ConfidenceProtocolsThe Reasonable Confidence Protocols are analytical methods that include specificlaboratory quality assurance and quality control (QA/QC) criteria that produceanalytical data of known and documented quality. The Reasonable ConfidenceProtocols methods are published on the CTDEP web site athttp://www.ct.gov/dep/remediation.ix

TermDefinitionReleaseDefined in Remediation Standard Regulations, Section 22a-133k-1(a) of theRegulations of Connecticut State Agencies and the State of Connecticut, Departmentof Environmental Protection, Site Characterization Guidance Document, effectiveSeptember, 2007, page vi.Release AreaDefined in Remediation Standard Regulations, Section 22a-133k-1(a) of the RCSAand the State of Connecticut, Department of Environmental Protection, SiteCharacterization Guidance Document, effective September 2007, page vi.Remediation StandardRegulation 15 MetalsAntimony, arsenic, barium, beryllium, cadmium, chromium, copper, lead, mercury,nickel, selenium, silver, thallium, vanadium, and zincReporting LimitReporting limit means the concentration of the lowest calibration standard of acalibration curve used for analysis of a given sample by a specific method, correctedfor specific sample weight or volume, dilutions, and for soil and sediment samplesmoisture content. This term is further defined in the Remediation StandardRegulations, Section 22a-133k-1(a) of the Regulations of Connecticut State Agencies.Residential DirectExposure CriteriaDefined in Remediation Standard Regulations, Section 22a-133k-1(a) of theRegulations of Connecticut State Agencies.SensitivitySensitivity refers to the ability of an analytical procedure to detect and quantify ananalyte at a given concentration.Significant Data GapDefined in State of Connecticut, Department of Environmental Protection, SiteCharacterization Guidance Document, effective September 2007, page vi.SpikeTo spike a sample is to fortify a sample in the laboratory with known concentrations ofanalytes.Split SampleAliquots of sample taken from the same container and analyzed independently. Splitsamples are usually taken after mixing or compositing and are used to document intraor inter-laboratory precision.Standard of CareDefined in State of Connecticut, Department of Environmental Protection, SiteCharacterization Guidance Document, effective September 2007, page vi.StandardsStandards are solutions that contain known concentration of target analytes. Examplesinclude stock standards, calibration standards, et cetera.SubstanceDefined in Remediation Standard Regulations, Section 22a-133k-1(a) of theRegulations of Connecticut State Agencies.x

TermDefinitionSurface Water ProtectionCriteriaDefined in Remediation Standard Regulations, Section 22a-133k-1(a) of theRegulations of Connecticut State Agencies.Surrogate AnalyteAn organic compound, which is similar to the target analyte(s) in chemicalcomposition and behavior in the analytical process, but is not normally found inenvironmental samples. The surrogate concentration is measured using the sameprocedures used to measure other analytes in the sample. Surrogate recoveries are usedto evaluate the performance of the analysis.Target AnalytesTarget analytes are the compounds included on the list of analytes for an analyticalmethod.Tentatively IdentifiedCompoundsTentatively identified compounds are unknown compounds for which a possibleidentification was made by comparing the mass spectra of the unknown to a library ofknown mass spectra. Concentrations may also be estimated by assuming a responsefactor.Trip BlankTrip blanks originate within the laboratory. Trip blanks are sample containers thathave been filled with analyte-free reagent water, or soil and carried with other samplecontainers out to the field, and back to the lab without being exposed to samplingprocedures. Trip blanks are used to ascertain if sample containers may have beencontaminated during transportation and storage.Turn-Around TimeThe amount of time it takes for the laboratory to report the analytical results to thecustomer following the submittal of the samples to the laboratory.xi

1.INTRODUCTIONThe Reasonable Confidence Protocols (RCPs) are analytical methods that were developed to standardizethe minimum Quality Assurance/Quality Control (QA/QC) and reporting documentation expected foranalytical laboratory data used by environmental professionals.This document provides general information and guidance regarding the RCPs.The RCPs are acollection of analytical methodologies that are based on analytical methods published by the United StatesEnvironmental Protection Agency (EPA) and others. RCPs have been developed for the most commonlyused analytical methods, and RCPs may be developed for other methods in the future. The RCP methodsare published on the CTDEP web site at http://www.ct.gov/dep/remediation.The primary function of the RCPs is to describe specific quality assurance and quality control proceduresthat will be performed by the laboratory to provide analytical data of known and documented quality.Other components of this guidance include a RCP Laboratory Analysis QA/QC Certification Form thatthe laboratory uses to certify whether the data meets the guidelines for “Reasonable Confidence,” and anarrative that describes QA/QC non-conformances. When “Reasonable Confidence” is achieved for aparticular data set, the environmental professional will have confidence that the laboratory has followedthe RCPs, has described non-conformances, if any, and has adequate information to make judgmentsregarding data quality. When the RCP methods are followed, the environmental professional can haveconfidence that the data are of known and documented quality. This will enable the environmentalprofessional to subsequently evaluate whether the quality of the data is sufficient for its intended purpose.A basic premise of the RCPs is that good communication and the exchange of information between theenvironmental professional and the laboratory will increase the likelihood that the quality of the analyticaldata will meet project-specific Data Quality Objectives (DQOs), and therefore, be suitable for theintended purpose. To this end, an example laboratory communication form was developed to provideguidance regarding the specific information that the laboratory should have prior to analyzing theassociated samples.1-1

The process of obtaining analytical data that is of sufficient quality for the intended purpose andevaluating the quality of analytical data in relation to project-specific DQOs occurs throughout the courseof a project. This process includes: Development of project-specific DQOs in accordance with the CTDEP’s Site CharacterizationGuidance Document effective September 2007 (SCGD). Communication with the laboratory regarding project-specific DQOs and the selection ofappropriate analytical methods in accordance with section 4.2.3 of the CTDEP’s (SCGD). Performance of quality assurance and quality control activities during the analysis of the samplesand reporting of QC results by the laboratory. Performance of a data quality assessment (DQA) of the laboratory quality control data, andlaboratory narrative by the environmental professional to identify QC non-conformances. Performance of a data usability evaluation (DUE) by the environmental professional to determineif the analytical data is of sufficient quality for the intended purpose. The DUE uses the results ofthe DQA and evaluates the quality of the analytical data in relation to the project-specific DQOs.Additional information concerning DQAs and DUEs is presented in CTDEP’s Laboratory QualityAssurance and Quality Control Guidance Data Quality and Usability Evaluations, which is presented assupplemental guidance to the SCGD.1-2

2.BACKGROUNDSection 19a-29a of the Connecticut General Statutes requires that all environmental laboratories becertified by the Connecticut Department of Public Health (CTDPH).CTDPH currently offerscertification in three broad matrices (drinking water, non-potable water/wastewater, and soil/solid waste)for a variety of analytes. Parties who procure laboratory services must verify that the laboratory isapproved by the CTDPH for the specific analytes in the specific matrices for which analysis is requested.Connecticut Regulations require laboratories that analyze samples in Connecticut be approved by theCTDPH.The Environmental Laboratory Certification Program (ELCP) certifies laboratories that meet theminimum requirements of the Connecticut General Statutes, the Regulations of the Connecticut StateAgencies, and the EPA. The ELCP evaluates laboratories based upon the qualifications of the laboratorypersonnel, the results of triennial on-site inspections, facilities, equipment, methods employed, annualproficiency test samples, and QA/QC practices. Certification alone cannot guarantee the validity of dataproduced by a laboratory.The RCPs are based upon the latest promulgated methods appearing in Test Methods for Evaluating SolidWastes, SW-846 (SW-846) published by the United States Environmental Protection Agency (EPA),which provides recommended test procedures and guidance. As such, the QA/QC requirements in SW846 are guidelines. When SW-846 methods were developed, it was anticipated that most projects utilizingthese methods would have an associated Quality Assurance Project Plan (QAPP), which would documentthe specific QA/QC requirements for the project. However, in practice most projects do not have aQAPP, and SW-846 methods are routinely used by the environmental laboratories, each with its owninterpretation of the QA/QC requirements of SW-846.In contrast, the RCPs provide a minimum set of QA/QC criteria. If the laboratory follows the RCPmethods, the associated data set is given a “Reasonable Confidence” status. Environmental professionalsmust understand that the “Reasonable Confidence” status does not mean that data will automatically meettheir needs. “Reasonable Confidence” only means the laboratory followed the recommendations in theRCPs.The environmental professional must evaluate the associated laboratory report to ascertainwhether the data is of sufficient quality to meet the project-specific DQOs and support the environmentaldecisions to be made.2-1

3.REASONABLE CONFIDENCE PROTOCOL STRUCTUREEach RCP method is written using the same general format. Each method contains a list of holding times,containers, preservatives, target analytes, QC criteria, and required report deliverables. Environmentalprofessionals should note that the RCPs do not list laboratory reporting limits, with the exception of RCPMethod 8260, low-level volatile organics. It is the responsibility of the environmental professional torequest the reporting limits that the laboratory should meet for each data set. The following sub-sectionsdescribe several important aspects of the RCPs.3.1Holding Times, Containers, and Preservati

3.4 Quality Control/Quality Control Criteria 3-2 3.5 Report Deliverables 3-2 3.6 Modification of the Reasonable Confidence Protocol Method 8260 to Meet the Groundwater Protection Criteria 3-3 3.7 Project-Specific Laboratory Quality Assurance/Quality Control 3