QAQC MANUAL FOR FRCACC by olliegoblue27

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									QUALITY ASSURANCE MANUAL College of Forest Resources Chemical Analysis Cost Center January 1, 2007 I. Organization/Responsibilities The College of Forest Resources Chemical Analysis Cost Center (CFRCACC) provides analytical chemistry support primarily for the College of Forest Resources and, to a lesser extent, the University of Washington. The CFRCACC is run by a manager and employee(s) in conjunction with College faculty, staff and students. The manager is responsible for establishing quality assurance/quality control (QA/QC) policies and ensuring those policies are followed. The manager is also the primary laboratory analyst and is responsible for performing sample and QC analysis, training and supervision of employees and students in QA/QC procedures, record keeping, reviewing and reporting results and is the sample custodian. In the absence or under the direct supervision of the manager, trained employees and students may also perform sample and QC analysis and record results. College faculty are also responsible for training and supervision of students and in their areas of expertise act as advisors to the manager. II. Quality Assurance/Quality Control Policy A. The principle objective for operating the CFRCACC is to provide high quality analytical chemistry support and training for the programs and research performed by College faculty and students. Emphasis is placed on consistent production of complete analytical data which accurately represents sample analysis. B. All analytical procedures will be performed according to approved methods including QA/QC parameters required by those methods (methods are specified in paragraph IV of this manual). The initial data quality objective (DQO) for each method is to achieve precision and accuracy levels comparable or better than those stated in the cited methods. Once control charts, Appendix A, have been established for a given method, the statistics used for the chart become the DQOs for the specific test, provided they are better than the initial DQOs. C. No sample data will be recorded without including results for any QC samples associated with the data. D. Data will be entered on printed work sheets or accumulated by data collection and analysis software. All data will be reviewed prior to release from the CFRCACC laboratory. E. Initial training for new employees and students for analytical methods and QA/QC requirements and procedures will be conducted as needed. Additional training will be implemented as required to maintain competence in analytical skills. F. Copies of methods, this QA manual and the University of Washington Environmental Health and Safety (EH&S) Laboratory Safety Manual will be located in the laboratory(s). III. Sample Management A. Samples collected by CFRCACC personnel will be taken according to the schedule in Table 1. All sample analysis will follow preservation techniques and maximum holding times listed in Table 1. Information in Table 1 is excerpted from "EPA Regulations On Test Procedures For The Analysis Of Pollutants", 40 CFR 136.

Table 1.- Required Containers, Preservation Techniques And Holding Times # Parameter Name Container* Time 1 Coliform, fecal and total P, G 2 Chloride P, G 3 Nitrate P, G 4 Nitrite P, G 5 Orthophosphate P, G 6 Sulfate P, G 7 Ammonia(Kjeldahl) P, G 8 pH P, G 9 Total Phosphorus P, G 10 Biochemical Oxygen Demand P,G 11 Total Suspended Solids P, G * Polyethylene (P) or Glass (G) B. Customers of the laboratory will request sample analysis by filling out a Sample Analysis Request form, Appendix B. The completed Sample Analysis Request form and samples will be given to the manager, or in the absence of the manager, a trained employee who will log the samples into the sample log book, fill out a Chain-of-Custody record, Appendix C, and properly store the samples. The Chain-of-Custody record will accompany the samples at all times until the analysis is complete. Samples are retained for a period of one year unless, otherwise specified by the client, and are then disposed of according to EH&S standards. C. The manager as sample custodian ensures, (1) samples are logged and stored properly and handled by a minimum number of people, (2) the lab is secured at all times when not in use, (3) only authorized personnel are allowed in the lab, (4) samples are logged on a permanent Chainof-Custody record, (5) samples are distributed to the proper analyst. IV. Methods A. Anions - The method used for anion analysis (chloride, nitrate, nitrite, orthophosphate and sulfate) is EPA 300.0, Aug. 1991, Appendix D. This method is generally used without modification, however, if a specific sample batch requires method modification(s), the modification(s) will be documented in the analysts lab notebook and noted and explained in the analysis report. B. Fecal Coliforms - The methods used for fecal Coliforms analysis are the MF and MPN procedures from Standard Methods for the Examination of Water and Wastewater (referred to as Standard Methods in this QC manual), 17th Edition, 1989, Methods 9221 and 9222, Appendix E. These methods are generally used without modification, however, if a specific sample batch requires method modification(s), it will be documented in the analysts lab notebook and noted and explained in the analysis report. Preservation Cool, 4C, 0.008% Na2SO4 None Required Cool, 4C Cool, 4C Filter Immediately, Cool, 4C Cool, 4C Cool, 4C H2SO4 pH<2 Cool, 4C Cool, 4C H2SO4 pH<2 Cool, 4C Cool, 4C Max. 6 Hours 28 Days 48 Hours 48 Hours 48 Hours 28 Days 28 Days 6 28 48 48 Holding

Hours Days Hours Hours

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C. Total Kjeldahl Nitrogen - The methods used for total nitrogen analysis (Ammonia) are EPA 351.1 (Kjeldahl Digest) and EPA 350.1 (Determination of Ammonia), Methods for Chemical Analysis of Water and Wastes, March 1983. The digestion solutions in EPA method 351.1 is modified to contain H2O2, Selenium powder, Li2SO4.H2O, and H2SO4. Any other modification(s) will be documented in the analysts lab notebook and noted and explained in the analysis report. D. pH Determination - The method used for pH determination is (pH Method - Electrometric) EPA 150.1 without modification. E. Total Phosphorus, All Forms - The method used for total phosphorus analysis is EPA 365.1 (Colorimetric, Automated, Ascorbic Acid) without modification. F. Biochemical Oxygen Demand - The method used for the determination of five day biochemical oxygen demand is from Standard Methods for the Examination of Water and Wastewater (referred to as Standard Methods in this QC manual), 17th Edition, 1989, Method 5210 B. This method is generally used without modification, however if a specific sample batch requires method modification(s), it will be documented in the analysts lab notebook and noted and explained in the analysis report. G. Total Suspended Solids - The method used for the determination of total suspended solids is from Standard Methods for the Examination of Water and Wastewater (referred to as Standard Methods in this QC manual), 17th Edition, 1989, Method 2540 D. This method is generally used without modification, however if a specific sample batch requires method modification(s), it will be documented in the analysts lab notebook and noted and explained in the analysis report. V. Calibration and Quality Control Procedures A. Lab Facility The lab is kept clean and orderly at all times. B. Equipment/Supplies 1. Method required equipment will generally be used. Changes from requirements will be documented in the method Standard Operating Procedure (SOP). method

2. Method required analytical grade reagents will be used. If these are not available, only reagents of a better grade may be substituted. Labels on all chemical reagents are marked with date received, date opened and, if applicable, date of expiration. Chemicals are stored out of direct sunlight. Those requiring cold storage are kept in a refrigerator, separate from sample storage. Acids and bases are stored separately in specially designated areas. Care is taken to prevent cross contamination of reagents and samples. Contaminated reagents and outdated chemical solutions are disposed of according to EH&S hazardous materials disposal guidelines. For reagents prepared in the lab, shelf life recommendations provided in the analytical method are followed and bottles are marked with the date prepared and the analyst's initials. Standard solutions are stored separately and safeguarded to prevent contamination. 3. Water used for reagent and standard preparation, sample dilution and final glassware rinsing will be Type II, <1 micromho/cm. Water purification is achieved by passing distilled water through ion exchange beds and monitoring the conductance of the resulting water with a suitable conductivity meter. The conductivity measurements will be monitored frequently and recorded on a weekly basis. Water used for microbiological analyses will be further treated by autoclaving.

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C. Labware Cleaning After each use, glassware is washed with detergent, rinsed with tap water, rinsed with Type II water, allowed to dry and stored in a cabinet. Sample bottles and equipment for microbiological analyses are sterilized in accordance with Standard Methods 9040, 17th ed., 1989, Appendix F. D. General Quality Control 1. Calibration Instruments are calibrated daily prior to sample analysis. This calibration is referred to as the initial calibration. Specific calibration requirements are discussed in Section E, Method Specific Quality Control. 2. QC Sample A quality control sample containing the analyte(s) of interest at known concentrations obtained from an outside source will be run with each sample batch. The QC Sample is analyzed to help verify that the standard curve for the analysis is valid. 3. Check Standards An analytical standard containing the analyte(s) of interest will be run every 10-20 samples, depending on the stability of the particular instrument response. At least one check standard will be run with each sample batch. A check standard will be the last sample analyzed. The check standard is used to determined the integrity of the instrument calibration parameters has through out the analysis. If the check standard is not in agreement within 10% of the known value, a new calibration is performed. The check standard is then reanalyzed and if its value is within 10% of the known value, the sample analysis can continue. All samples prior to the out of range check standard back to the last in range check standard must be reanalyzed. If the check standard remains out of range, the analysis is stopped and the reason for the discrepancy is investigated and corrected. 4. Method Blank Each sample batch will contain a reagent blank. The reagent blank will be carried through the entire analytical procedure. If any reagents are changed, e.g. opening a new bottle, during the analysis of a sample batch, a new reagent blank must be prepared and samples using the new reagents must be identified. 5. Performance Evaluation (PE) Samples A blind sample (i.e., true values are not released until the lab has completed the analyses and submitted the results) obtained from a Department of Ecology (DOE) approved source must be analyzed every six months for available parameters. The results of PE sample analyses will be kept in a PE sample analysis log. 6. Blind Samples Periodically samples of unknown concentration are given to the analyst to be analyzed. Whenever possible, blind samples are added to the analytical process in such a manner that the analyst is unaware a blind sample is being analyzed. Appropriate measures are taken when analysis of a blind sample is inconsistent with past results. 7. Duplicates The duplicates from samples split in the lab will be analyzed every 20 samples. At least one duplicate must be run with each sample batch. 8. Matrix Spike A matrix spike will be analyzed with every 20 samples, generally on the sample that has been analyzed in duplicate. The sample will be spiked with the analytes of interest as specified in Section E, Method Specific Quality Control. At least one matrix spike will be run with every sample batch. 9. Method Detection Limit Study An initial method detection limit (MDL) study is performed prior to sample analysis to determine values for the MDL and the practical limit of quantitation (PQL). The MDL and PQL are evaluated following Standard Methods 1030 E, 17th Ed., 1989, Appendix G. Results below the MDL are reported as not detected (ND), results

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between the MDL and the PQL are reported as trace (TR) and results above the PQL are reported as values. MDL and PQL values are reported with all final results. 10. Evaluating Accuracy The ability of the lab to perform accurate analyses is evaluated by analyzing QA/QC samples. There are several types of QA/QC samples analyzed by the lab. Sections V.B.2, 3 and 5 describe QC Samples, Check Standards and PE samples and their use in evaluating the accuracy of an analysis. Other QA/QA samples are available such as certified reference materials (CRMs) and National Institute for Standards and Technology Standard Reference Material (SRM). The use of these or other QA/QC samples will be detailed in Section E, Method Specific Quality Control. 11. Evaluating Precision Analysis precision is evaluated by maintaining control charts for the procedures used in the lab. Appendix A, Control Charts1, describes the use of control charts to evaluate laboratory precision. Control charts based on the analysis of standard solutions, the analysis of duplicate solutions and spike recoveries are in use in the lab. Appendices H, I and J, SOPs from DOE Manchester Laboratory, detail the preparation and use of control charts for these purposes. For example, once the control chart for the analysis of standard solutions has been constructed, all subsequent determinations of the same standard will be plotted on the control chart. As long as the values are within the action limits, values for samples analyzed in conjunction with the standard may be reported. If values exceed either action limit, if more than three consecutive values exceed one warning limit, or if more than seven consecutive values are on one side or the other of the central line, the lab is out of control for that analysis. Analysis for that parameter must cease until the situation is investigated, the cause found and corrective action taken. E. Method Specific Quality Control 1. Anions by Ion Chromatography a. Preparation of Calibration Curves Within batch calibration curves for the anions chloride, nitrite-nitrogen, nitrate-nitrogen, orthophosphate-phosphorus and sulfate-sulfur are prepared from 8 standards over a range of concentrations from 0.02 mg/L to 5.00 mg/L. A stock standard solution containing chloride, nitrate, orthophosphate and sulfate is diluted appropriately to make the working standards. The stock standard solution is stored in a refrigerator and has been found to be stable, by comparison to QC samples, for several months. Nitrite standards are made up daily. Concentration is plotted on the y-axis and peak area is plotted on the x-axis. Two calibration curves are prepared for each anion, one from 0.02 mg/L to 1.00 mg/L, the other from 1.00 mg/L to 5.00 mg/L. Preparing two curves in this manner increases the accuracy of low level analysis. A linear function using the method of least squares and the correlation coefficient are determined for each curve. The correlation coefficient must be greater than 0.9980 for the calibration curve to be valid. Concentrations for subsequent analyses are calculated from the linear function. b. Matrix Spike Levels Two matrix spike levels are used, a low level spike and a high level spike. Low level spike levels are at two times the PQL. High level spike levels are at 1 mg/l. c. Method Detection Limits Method detection limits are determined for each anion and checked every six months. Table 2 gives the MDL and PQL for chloride, nitrite-nitrogen, nitrate-nitrogen, orthophosphate-phosphorus and sulfate-sulfur.

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Procedural Manual for the Environmental Laboratory Accreditation Program, Feb. 1991, DOE

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Table 2. MDL and PQL for Anions Chloride Nitrite-Nitrogen Nitrate-Nitrogen Orthophosphate-Phosphorus Sulfate-Sulfur MDL, mg/L 0.01 0.003 0.003 0.01 0.006 PQL, mg/L 0.05 0.015 0.015 0.05 0.03

2. Fecal Coliforms - There are no instruments requiring calibration for fecal Coliforms determinations nor are there requirements for analyzing check or PE samples. A blank is run with each batch of samples. The filter in the blank determination is rinsed with buffer solution to make sure the buffer is not contaminated. Duplicates are run one in every ten samples. The usual method for determination of fecal Coliforms is the membrane filter (MF) technique. The lab is also capable of determinations using the multiple tube (MPN) technique. As a QC check on the MF method, once each quarter the lab will analyze five fecal Coliforms samples by both the MF and MPN procedures. If 80% agreement between the two methods is not achieved, causes will be sought and remedied, where possible, and the comparative process repeated. Quarterly, the lab will exchange two samples with METRO labs as an inter-lab check on the accuracy of fecal Coliform tests. 3. Total Kjeldahl Nitrogen a. Preparation of Calibration Curves Within batch calibration curves for the Nitrogen Ammonia is prepared from 6 standards over a range of concentrations from 0.10 mg/L to 0.50 mg/L. A stock standard solution containing ammonia is diluted appropriately to make the working standards. The stock standard solution is stored in a refrigerator and has been found to be stable, by comparison to QC samples, for several months. A linear function using the method of least squares and the correlation coefficient are determined for the calibration curve. The correlation coefficient must be greater than 0.9970 for the calibration curve to be valid. Concentrations for subsequent analyses are calculated from the linear function. The ammonia QC sample sets are obtained through an outside source. QC samples contain both inorganic (Ammonium Chloride) and Organic (Glycine) bound nitrogen forms. These QC samples will determine the efficiency of the digestion and its accuracy. b. Matrix Spike Levels Two matrix spike levels are used, a low level spike and a high level spike. Low level spike levels are at two times the PQL. High level spike levels are at 1 mg/l. c. Method Detection Limits Method detection limit is determined for ammonia and checked every six months. The MDL and PQL for ammonia nitrogen are 0.01 and 0.05 mg/L respectively. 4. Total Phosphorus a. Preparation of Calibration Curves Within batch calibration curves for the Phosphorus is prepared from 6 standards over a range of concentrations from 1.0 mg/L to 5.0 mg/L. A stock standard solution containing ammonia is diluted appropriately to make the working standards. The stock standard solution is stored in a refrigerator and has been found to be stable, by comparison to QC samples, for several months. A linear function using the method of least squares and the correlation coefficient are determined for the calibration curve. The correlation coefficient must be greater than 0.9970 for the calibration curve to be valid. Concentrations for subsequent analyses are calculated from the linear function. The Phosphorus QC sample sets are obtained through an outside source. QC samples contain both inorganic (Potassium Phosphate) and Organic (Sodium B-Glycero Phosphate) bound phosphorus forms. These QC samples will determine the efficiency of the digestion and its accuracy.

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b. Matrix Spike Levels Two matrix spike levels are used, a low level spike and a high level spike. Low level spike levels are at two times the PQL. High level spike levels are at 1 mg/l. c. Method Detection Limits Method detection limit is determined for Phosphorus and checked every six months. The MDL and PQL for ammonia nitrogen are 0.03 and 0.10 mg/L respectively. 5. pH Determination The pH of a sample is determined electromertically using a glass electrode in combination with a reference potential electrode. The pH meter is calibrated before use with buffer solutions at pH of 4.0, 7.0, and 10.0. 6. Biochemical Oxygen Demand (BOD5) There are no instruments requiring calibration for BOD5. However, there are provisions within the method for checking the quality of dilution water and determining control limits. A glucoseglutamic acid check is used to determine if contaminants in the laboratory dilution water are inhibiting the growth of an otherwise viable seed or if the seed population itself is inactive. Low results from this check invariably reflect toxicity or low seed viability. This check will be run with each batch of samples. A blank is run with each batch of samples. The blank determination is run with deionized water to make sure there is no contamination associated with the laboratory equipment or method. Duplicates are run one in every ten samples. Samples are inoculated with a buffered nutrient solution and a seed population of viable oxidizing microbes obtained from domestic wastewater sources on the U.W. campus. Dissolved oxygen measurements using the azide modification titration method (Standard Method 4500-O C) are made initially and after five days of incubation. The BOD of a particular solution is computed from the difference in dissolved oxygen levels. 7. Total Suspended Solids There are no instruments requiring calibration for total suspended solids nor are there requirements for analyzing check or PE samples. A blank is run with each batch of samples. The filter in the blank determination is rinsed with deionized water to make sure there is no contamination associated with the laboratory equipment or method. Duplicates are run one in every ten samples. The method for determination of total suspended solids is by vacuum filtration of a well mixed, known volume of water followed by drying the filter at a temperature of 103 to 105oC for one hour. Samples are then cooled in a dessicator and weighed to the nearest tenth of a milligram. Sample drying will be repeated until dry weights are within 0.5 mg for successive weighings. Quarterly, the lab will exchange two samples with Metro labs as an interlab check on the accuracy of total suspended solids tests. F. Equipment Maintenance All lab equipment is maintained so as to keep it in proper working order at all times. Routine maintenance and simple repairs may be made by lab personnel; qualified service representatives will perform more extensive repairs. Preventative maintenance, breakdowns and repair procedures will be noted in the maintenance log for each piece of equipment. The analytical balance is checked monthly or more often using standard weights, class S, and serviced by professional service representatives as required or, at a minimum, annually. The sample refrigerator is maintained at a temperature between 1 and 4.4C. VI. Data Management All records required by this QC manual and the methods referenced here are retained by the CFRCACC laboratory for a period of at least three years. Raw data is retained in the form

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generated, e.g., lab notebook entries, bench sheets, chart recordings and computer disk. A hard copy is also retained of data collected by computer software. Data stored on computer hard disk drives are periodically backed up to floppy disks. All raw data, calculations and reports are reviewed for accuracy and signed by the manager acting as the quality assurance officer. All data is recorded in ink and corrections are initialed. A list of initials identifying the person to whom they belong is kept as a permanent laboratory record. VII. Audits/Reports Two types of audits are used to evaluate CFRCACC lab operations. A system audit is conducted periodically by the Department of Ecology. Performance audits are conducted every six months for accredited parameters, except fecal Coliforms, as part of the EPA Water Pollution Study. Additionally, blind samples are periodically added to the sample stream as an audit of individual analyst performance. Audit and QA/QC reports are prepared yearly and are available in the CFRCACC lab. APPENDICES: A - Control Charts, DOE-QAS Attachment 1 - Analytical Control Charting, Cliff J. Kirchmer. DOE-QAS Attachment 2 - Glossary of QA/QC Terms, DOE-QAS B - Sample Analysis Request Form C - Sample Collection and Chain of Custody Record Form D - EPA Method 300.0, The Determination of Inorganic Anions in Water by Ion Chromatography, August, 1991 E - MPN and MF Fecal Coliforms Methods, Standard Methods, Methods 9221 and 9222, 17th Ed., 1989 F - Washing and Sterilization, Standard Methods, Method 9040, 17th Ed., 1989 G - Method Detection Limit, Standard Methods, Method 1030 E, 17th Ed., 1989 Attachment 1 - Glossary, Standard Methods, Method 1010 C, 17th Ed., 1989 H - DOE Manchester Laboratory SOP #2, Preparation and Use of Precision Analytical Control Charts Based on the Analyses of Standard Solutions I - DOE Manchester Laboratory SOP #3, Preparation and Use of Precision Analytical Control Charts Based on the Analyses of Duplicate Samples J - DOE Manchester Laboratory SOP #4, Preparation and Use of Spike Recovery Control Charts K - EPA Method 350.1 Ammonia Nitrogen (Colorimetric, Automated Phenate), March 1983. L - EPA Method 351.1 Total Kjeldahl Nitrogen (Colorimetric, Automated Phenate), March 1983. M- EPA Method 365.1 Phosphorus, All Forms(Colorimetric, Automated, Ascorbic Acid), 1971. N- EPA Method 150.1 pH (Electrometric), 1971 O- Five Day Biochemical Oxygen Demand, Standard Methods 5210 B 17th Ed., 1989. P- Total Suspended Solids, Standard Methods 2540 D 17th Ed. 1989.

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Appendix A Control Charts Attachment 1 - Analytical Control Charting Attachment 2 - Glossary of QA/QC Terms

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Appendix B Sample Analysis Request Form

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Appendix C Sample Collection and Chain of Custody Record Form

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Appendix D EPA Method 300.0, The Determination of Inorganic Anions in Water by Ion Chromatography, August, 1991

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Appendix E MPN and MF Fecal Coliforms Methods, Standard Methods, Methods 9221 and 9222, 17th Ed., 1989

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Appendix F Washing and Sterilization, Standard Methods, Method 9040, 17th Ed., 1989

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Appendix G Method Detection Limit, Standard Methods, Method 1030 E, 17th Ed., 1989 Attachment 1 - Glossary, Standard Methods, Method 1010 C, 17th Ed., 1989

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Appendix H DOE Manchester Laboratory SOP #2 Preparation and Use of Precision Analytical Control Charts Based on the Analyses of Standard Solutions

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Appendix I DOE Manchester Laboratory SOP #3 Preparation and Use of Precision Analytical Control Charts Based on the Analyses of Duplicate Samples

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Appendix J DOE Manchester Laboratory SOP #4 Preparation and Use of Spike Recovery Control Charts

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