United States Environmental Protection Agency Environmental Monitoring Systems Laboratory Las Vegas NV 89193-3478 Research and Development EPA/600/S8-89/046 Aug. 1989 Project Summary Soil Samp Assurance Second Edition Delbert S. Barth, Benjarr Kenneth W. Brown Use of the first edition Sampling Quality Assur Guide" as a text in a se inars conducted at various U.S. EPA Regional Offices elicited many con- structive comments for improve- ments from seminar attendees. Many of these suggested improvements have been incorporated in this se- cond edition. Specifically, the references have been updated, particula the incorporation of rece guidelines documents. M has been given to ex design, specifically to pr developing data quality The statistical coverag expanding considerably t introduction to applicati nt U.S. EPA re attention perimental cedures for objectives. has been i include an ns of geo- statistics and a discussioih of require- ing Quality User's Guide- n J. Mason, Thomas H. Starks, and of the "Soil nee User's ies of sem- rly through ments for the definition oi support in conjunction with guidance for soil sampling. This report is intended to be a liv- ing document providing state-of-the- art guidance. Accordingly, from time to time revisions will be prepared to maintain harmony with improvements in soil sampling quality assurance methodology. Future revisions will be prepared, and authorship identified, on a chapter-by-chapter basis. This Project Summary was devel- oped by EPA's Environmental Monitor- ing Systems Laboratory, Las Vegas, NV, to announce key findings of the research project that is fully docu- mented in a separate report of the same title (see Project Report ordering Information at back). An adequate quality assurance/quality control (QA/'QC) program requires the identification and quantification of all sources of error associated with each step of a monitoring program so that the resulting data will be known quality. The components of error, or variance, include those associated with sampling, sample preparation, extraction, analysis, and residual error. In the past, maior empha- sis often has been placed on QA/QC aspects of sample analysis and closely associated operations such as sample preparation and extraction. For monitor- ing a relatively inhomogeneous medium such as soil, the sampling component of variance will usually significantly exceed the analysis component Thus, in this case a minimum adequate QA/QC plan must include a section dealing with soil sampling. The purpose of this document is to provide guidance in QA/'QC aspects related to soil sampling Generally soil monitoring is undertaken to carry out the provisions and intent of applicable environmental laws with high priority requirements associated with haz- ardous waste management The objec- tives of soil monitoring programs are often to obtain data on the basis of which to answer one or more of the following questions: • Are the concentrations of specified soil pollutants in a defined study region significantly different from the concen- trations in a control region? ------- • Do the concentrations of specified soil pollutants in a defined region exceed established threshold action levels^ • At the measured concentrations of specified soil pollutants in a defined study region, what is the associated risk of adverse effects to public health, welfare, or the environment? For each of these applications, the QA/QC methods and procedures cannot be specified without giving careful consideration to the consequences of making an error, for example, in a decision to require or not to require cleanup of a contaminated region. It follows in general that to be maximally cost-effective and defensible the QA/QC objectives of a soil monitoring program cannot be separated from the objectives of the soil monitoring program itself. In general, the progression of events leading to the development of an ade- quate Quality Assurance Program Plan (QAPP) follows the outline shown below. 1 State study objectives. 2. Evaluate impacts of mistakes. 3. Define data quality objectives (DQOs). 4. Design study to achieve DQOs. 5. Design QAPP to confirm achievement of DQOs. Often it will not be possible to specify in advance what DQOs are possible to achieve. In such cases DQO goals should be set, a QAPP prepared, and a pilot study conducted to determine the achievability of the goals. Present U.S. EPA guidance for development of DQOs requires that specifications for the following factors must be addressed: precision, accuracy, completeness, representativeness, and comparability. A sixth factor of importance to all of the above is the detection limit of the measurement method used. Other important factors which should be considered in specifying DQOs include: • acceptable probability of a Type I error (judging a clean area to be dirty); • acceptable probability of a Type II error (judging a dirty area to be clean); and • desired minimum detectable relative difference between two different geo- graphical areas. The development of DQOs involves an iterative interaction between management and technical staff. Management ident- ifies the needs and resources available. The technical staff develops guidance for assisting management in making the decisions required to develop the DQOs. The DQO process usually involves a three-stage process as outlined below. 1. Identify decision types. 2. Identify data uses/needs. 3. Design data collection program. The end result is site-specific guidance for evaluating and interpreting sampling data. Control samples are normally as important to a soil monitoring study as are samples taken from the study region. The data from control samples aid in the interpretation of the results from the study region and also help to identify sources and important transport routes for soil pollutants. Accordingly, the same level of effort and degree of QA/QC checks should go into selecting and sam- pling a control region as goes into sam- pling the study region. In sampling of a continuous medium such as soil, it is necessary to put extra emphasis on the definition of a sampling unit. In addition to having a specified lo- cation, each sampling unit of soil has a certain three-dimensional volume, shape, and orientation. These latter three characteristics, when taken together, are called the support of the sample. Changes in support not only change th| means of distribution, they also chang< the variances of concentrations and th< correlations of concentrations betweei sampling units. It is essential that any action level fo soils be defined as a concentration over; particular support and location relative ti the ground surface. In this definition of ai action level, the support is referred to n this document as the action support. Fo example, the action support might bi defined as the top ten cm of soil over square of 100 m2. The following table provides recom mendations, as part of the DQO process for confidence levels, powers, and min mum detectable relative increases ove background for different operation; situations. Both Type I (false positive) and Type (false negative) errors should b considered in hypothesis testing. Table and an equation are provided for use i determining the required number ( samples to achieve defined confidenc levels and powers. The location of sarr pling is also important. Stratification < the sampling region may reduce th variance in cases where the variance considered to be unacceptably largi Compositing of samples is generally m recommended since it allows no estimai of the variance among the samples beir composited. However, some compositir of samples increases the representativi ness of samples and may be justified c that basis. Suggested types of QA/QC sampk include various types of blanks, labo atory control standards calibration cne< standards, triplicate samples (splits), du| licate samples, various kinds of au< samples, etc. How many samples of ea( type would be needed in a specific stu< is a question of considerable important The recommended approach is determine how each type of QA/C sample is to be employed and th< Preliminary Site Investigation Emergency Cleanup Planned Removal and Remedial Response Confidence Level (1 -a) 70 - 80% 80 - 90% 90 - 95% Power (1 -P) 90 - 95% 90 - 95% 90 - 95% Relative Increase ovt Backround lWO(ns VRVupl to be Detectable with a Pr< bability (1 - 0) 10 - 20% 70 - 20% 10 - 20% where a = probability of a Type I error and f - probability of a Type II error. ------- •Determine the number fro that type based n the use. For example, field duplicates are used to estimate the combined variance contribution of several sources of variation. Hence, the number of field duplicates to be obtained in a study should be dictated by how precise one wants that estimate of variance to be. Geostatistics (or kriging) is an ap- plication of classical statistical theory to geological measurements that takes into account the spatial continuities of geo- logical variables in estimating the distri- bution of variables. In many ways, geo- statistics is for measurements taken in 2-, 3-, and 4-dimensional space (the three spatial dimensions and the time dimension), what time series is for measurements taken in one-dimensional space (time). However, a principal use of time series is in forecasting; in geosta- tistics the principal emphasis is on inter- polation. Nevertheless, both statistical procedures emphasize modeling the process to get an insight into the system being investigated. The application of classical statistical procedures to soil measurement data requires that the samples be collected randomly (i.e. not on systematic grids), that the data be independent and identically distributed (with the distri- jution being a normal distribution), and that the measurement error variance (particularly the between-batch error variance) be a very small part of the total variance of the measurements in a sample survey of a region. In man soil sampling studies one or all of the following questions will be of primary interest. • Are there any action supports within the study area that have pollutant concentrations above action level? • Where are the above-action-level action supports located? • What is the spatial distribution of pollutant concentration levels among action supports that have pollutant concentrations above action level? The problem with posing soil sampling methods and objectives in terms of population means is that the mean will depend on the size of the area chosen and the distribution of contamination throughout that area. For example, the mean in a small area may exceed the action level; but if the size of small area is increased by adding a substantial amount of less contaminated soil, the mean in the larger area may not exceed ;e action limit. Decisions on the need r remedial action should not be based on how one chooses the size of the area to be sampled, but rather on whether action supports exist that are above designated action limits. A comparison of means is reasonable in comparing pollu- tant concentrations at a background site with pollutant concentrations of a site down-gradient from a suspected hazard- ous waste source. Also, cleanup areas may be defined so that the average concentration in those units of soil may be compared with a standard. It follows from the above discussion that for most applications, geostatistical procedures for designing soil sampling studies and analyzing resultant data are generally preferred over classical statis- tical procedures. Once objectives have been defined for a soil monitoring study, a total study protocol, including an appropriate QA/QC program must be prepared. Usually not enough is known about the sources and transport properties of the soil pollutants to accomplish this in a cost-effective manner without additional study. The suggested approach is to conduct an exploratory study including both a literature and information search followed by selected field measurements based on an assumed dispersion model. The data resulting from this exploratory study serve as the basis for the more definitive total study protocol. If one is dealing with a situation requiring possible emergency action to protect public health, it is necessary to compress the planning and study design into a short time period and proceed to the definitive study without delay. In either case, the objectives of the monitoring study constitute the driving force for all elements of the study design, including the QA/QC aspects. To develop the exploratory study protocol with its associated QA/QC plan, one needs to combine into an assumed dispersion model, the information obtained prior to any field measurements. On the basis of this model, the standard deviation of the mean for soil samples is estimated. Value judgments are used to define required precision and confidence levels (related to acceptable levels of Type I or Type II error). A control region is selected. The numbers of required samples may then be calculated. Additional samples should be required to validate the assumed model. The locations of the sampling sites should be selected by an appropriate combination of judgmental (use of the assumed model), systematic (to allow for the fact that the model may be wrong), and random (to minimize bias) sampling. Sampling and sample handling must be accomplished according to standardized procedures based on principles designed to achieve data of both adequate quality and maximal cost-effectiveness. Particu- lar attention should be given to factors surrounding the disposition of non-soil material collected with the soil samples. The requirements for QA/QC for the exploratory study need not be a stringent as for the more definitive study in the sense that acceptable precisions and confidence levels may be relaxed some- what. Allowance should be made, however, for the collection of a modest additional number of QA/QC samples over that specified in the QA/QC plan to verify that the QA/'QC study design is adequately achieving its assigned objec- tives. Also, all normal analytical QA/'QC checks should be used. If the exploratory study is conducted well, it will provide some data for achieving the overall objectives of the total monitoring study, it will provide a check of the feasibility and efficacy of all aspects of the monitoring design including the QA/QC plan; it will serve as a training vehicle for all participants; it will pinpoint where additional measurements need to be made; and it will provide a body of information and data which can be incorporated into the final report for the total monitoring study. For the more definitive study, the se- lection of numbers of samples and sam- pling sites, sample collection procedures, and sample handling methods and proce- dures follow and build on the principles discussed and results obtained in the exploratory study. Frequency of sampling is an important aspect of the more definitive study which usually cannot be addressed in the exploratory study because of the relatively short time span over which the exploratory study is conducted. The required frequency of sampling depends on the objectives of the study, the sources of pollution, the pollutants of interest, transport rates, and disappear- ance rates (physical, chemical, or biological transformations as well as dilu- tion or dispersion). Sampling frequency may be related to changes over time, season, or precipitation. An approach that has been used successfully has been to provide intensive sampling early m the life of the study (e.g., monthly for the first year) and then to decrease the frequency as the levels begin to drop. The important principle is that the sampling should be conducted often enough that changes in the concentrations of soil pollutants important to the achievement of the monitoring objectives are not missed. ------- The important questions to be answered in the analyses and interpreta- tion of QA/QC data are: "What is the quality of the data?" and "Could the same objective have been achieved through an improved QA/QC design which may have required fewer re- sources?" It is desirable to provide sum- marized tables of validated QA/QC data in the final report. This approach allows users to verify the reported results as well as begin to build a body of QA/QC experimental data in the literature which allow comparisons to be made among studies. Special emphasis should be placed on how overall levels of precision and confidence were derived from the data. If portions of the study results are ambiguous and supportable conclusions cannot be drawn with regard to the reli- ability of the data, that situation must be clearly stated. The adequacy of all aspects of the QA/QC plan should be examined in detail with emphasis on defining for future studies an appropriate minimum ade- quate plan Some aspects of the QA/QC plan may have been too restrictive; some may not have been restrictive enough. Soil monitoring studies should have checks and balances built into the QA/QC plan which will identify early in the study whether the plan is adequate and, ifrequired, allow for corrective action to be taken before the study continues. This is one of the major advantages of conducting an exploratory study. There is insufficient knowledge dealing with soil monitoring studies to state with confidence which portions of the QA/QC plan will be generally applicable to all soil monitoring studies and which must vary depending on site-specific factors. As experience is gained, it may be possible to provide more adequate guidance on this subject. In the meantime, it is recommended that many important factors of QA/QC plans be considered as site-specific until proven otherwise. Another important aspect of QA/QC is auditing The purpose of an audit is to insure that all aspects of the QA/QC system planned for the project are in place and functioning well. This include all aspects of field, sample bank, and laboratory operations. Whenever a prob- lem is identified, corrective action should be initiated and pursued until corrected. Sample chain-of-custody procedures and raw data are checked as appropriate, and results of blind QA/QC samples routinely inserted into the sample load are re- viewed. Spot checks of sampling methods and techniques, sampling '3nd analysis calculations, and data tran- scription are performed. Checks are Delbert S. Barth, Benjamin J. Mason, and Thomas H. Starks, are with the University of Nevada, Las Vegas, NV 89154; the EPA author Kenneth W. Brown ( also the EPA Protect Officer, see below) is with the Environmental Monitoring Systems Laboratory,Las Vegas, NV 89193-3478. The complete report, entitled "Soil Sampling Quality Assurance User's Guide— Second Edition," (Order No. PB 89-189 8641 AS; Cost: $28.95, subject to change) will be available only from: National Technical Information Service 5285 Port Royal Road Springfield, VA22161 Telephone: 703-487-4650 The EPA Project Officer can be contacted af: Environmental Monitoring Systems Laboratory U.S. Environmental Protection Agency Las Vegas, NV 89193-3478 made to ascertain that required doci mentation has been maintained and in I orderly fashion, that each of the recorde items is properly categorized, and cros: checking can be easily accomplishei Checks are made to insure that the da recording conforms to strict docume control protocols and the program QA/QC plan It is recommended that an audit of tf overall QA/QC plan for sample docume tation, collection, preparation, storag and transfer procedures be perform* just before sampling starts. This is review critically the entire samplir operation to determine the need for ai corrective action early in the program The project leader of a soil monitom project is responsible for ascertaining tr all members of his project team ha adequate training and experience to car out satisfactorily their assigned missio and functions. This is normally acco plished through a combination of requir classroom training, briefings on t specific monitoring project about to implemented, and field training exercis< Special training programs should completed by all personnel prior to th involvement in conducting audits US. OFFICIAL MAIL United States Environmental Protection Agency Center for Environmental Research Information Cincinnati OH 45268 Official Business Penalty for Private Use $300 EPA/600/S8-89/046 000085833 PS AGE1CI ------- |