refrigerator at 1-6 °C; store filtrate in -80oC freezer for up to 30 days until analysis Urban stream/ditch water, collected via grab samples and first flush sampler samples 5-day biochemical oxygen demand plastic 1,000 mL Field: store in cooler at 1-6 °C or at ambient temperature if to be analyzed immediately at lab Lab: store at room temperature and start analysis within six hours of collection or store in refrigerator at 1-6 °C and start analysis within 24 hours Urban stream/ditch water, collected via grab samples and first flush sampler samples Turbidity plastic 100 mL Field: store in cooler at 1-6 °C Urban stream/ditch water, collected via grab samples and first flush sampler samples Total Suspended Solids (TSS) plastic 500 mL Field: store in cooler at 1-6 °C Lab: store in refrigerator at 1-6 °C and start analysis within 7 days Urban stream/ditch water, collected via grab samples and first flush sampler samples Volatile Suspended Solids (VSS) plastic 500 mL (use same water as TSS) Field: store in cooler at 1-6 °C Lab: store in refrigerator at 1-6 °C and start analysis within 7 days Urban stream/ditch water, collected via grab samples and Ammonia-nitrogen (NH3-N) plastic 125 mL Field: store in cooler at 1-6 °C Lab: store in
Table 5. Summary of QC requirements for Enterococci analysis by Enterolert QC Sample or Activity Minimum Frequency Acceptance Criteria Corrective Action Capability demonstration Four (4) prepared samples analyzed prior to any customer sample analyses Criteria for LCS recovery and duplicate precision Repeat until acceptable Media sterility check Prior to use of new lot of Colilert18 and weekly No fluorescence Investigate problem. Eliminate contaminations. Obtain new lot of Enterolert if necessary. Repeat until successful before using Enterolert lot. Media positive check with control culture Prior to use of new lot of Enterolert and weekly Fluorescence Investigate problem. Obtain new lot of Enterolert if necessary. Repeat until successful before using Enterolert lot. Media negative checks with control cultures (gram+ and gram-) Prior to use of new lot of Enterolert No fluorescence Investigate problem. Eliminate contaminations. Obtain new lot of Enterolert if necessary. Repeat until successful before using Enterolert lot. Method blank At least weekly, prior to sample analysis < 20 CFU/100 mL Clean analytical system and repeat MB analysis. Identify and eliminate source of contamination. Sample duplicate or matrix spike duplicate At least one (1) weekly, and one with all large sample batches (~20 samples) RPD < 200% for <150 CFU/100 mL RPD < 100% for > 150 CFU/100 mL Investigate problem. If system precision is in control, qualify results. If system precision is out of control, reanalyze entire batch. Internal PE sample Samples and frequency determined by Lab QA Officer Criteria for LCS recovery and duplicate precision Investigate all unacceptable results. Blind PE sample Samples and frequency determined by accrediting agencies and projects Determined by PE provider Investigate all unacceptable results. LCS = laboratory control sample QC = quality control MB = method blank %R = percent recovery MDL = method detection limit RL = reporting limit PE = performance evaluation RPD = relative percent difference
Table 7. Summary of QC requirements for turbidity analysis by Hach meter QC Sample or Activity Minimum Frequency Acceptance Criteria Corrective Action Capability demonstration Four (4) prepared samples analyzed prior to any customer sample analyses Criteria for duplicate precision RPD < 25% Repeat until acceptable 4-Point calibration plus deionized water blank At least quarterly 90-110% R (measured value of primary standards when analyzed as samples within 10% of expected values) Investigate problem. Correct any obvious problems. Repeat calibration until acceptable. Assign values to permanent transfer standards using formazin primary standards At least quarterly Measurement after acceptable calibration and values within 10% of previous established values Investigate problem. Correct any obvious problems including replacing transfer standards if necessary. Repeat until acceptable. Daily calibration check Immediately prior to and after sample analysis GELEX Secondary Turbidity Standards should read within 10% of assigned values Investigate problem. Correct any obvious problems. If necessary reassignment of GELEX values and reanalyze samples. Repeat calibration check until acceptable. Method blank Daily prior to sample analysis <1.0 NTU (i.e., < RL) Clean analytical system and repeat MB analysis. Identify and eliminate source of contamination. Sample analysis For all sample analyses Direct sample reading within acceptable measurement range (i.e., 1.00 NTU to 4000 NTU) If reading below range report result as < RL. If result above range dilute sample. Sample duplicate One (1) per preparation batch RPD < 25% Investigate problem. If system precision is in control, qualify results. If system precision is out of control, reanalyze entire batch. Internal PE sample Samples and frequency determined by Lab QA Officer 75-125% R RPD < 25% Investigate all unacceptable results. Blind PE sample Samples and frequency determined by accrediting agencies and projects Determined by PE provider Investigate all unacceptable results. LCS = laboratory control sample QC = quality control MB = method blank %R = percent recovery MDL = method detection limit RL = reporting limit MS = matrix spike RPD = relative percent difference PE = performance evaluation point
Table 8. Summary of QC requirements for TSS QC Sample or Activity Minimum Frequency Acceptance Criteria Corrective Action Capability demonstration Four (4) prepared samples analyzed prior to any customer sample analyses 90 – 110% R < 10% RSD Repeat until acceptable Balance Calibration Check Prior to weighing any sample filters Weight of certified 200 mg weight: 0.1998 – 0.2002 g Investigate problem including cleaning weight and balance. If balance is out of calibration attempt recalibration or use another balance until obtain acceptable calibration check. Method Blank At least one (1) per analysis batch of up to 10 samples For 1.0 L blank filtered: < 1.0 mg/L Investigate, identify, and correct the problem. If system accuracy is in control, qualify results. If system accuracy is out of control, correct problem before analyzing samples Sample analysis For all sample analyses Total residue on filter: >2.5 mg to < 200 mg If total residue on filter < 2.5 mg report result as < RL If total residue on filter > 200 mg filter a smaller volume of sample. Laboratory Control Sample At least one (1) per year 90 – 110% R Investigate, identify, and correct problem. If system accuracy is in control, qualify results. If system accuracy is out of control, correct problem before analyzing samples. Sample duplicate One (1) per preparation batch of up to 10 samples RPD ≤ 5% Investigate problem. If system precision is in control, qualify results. If system precision is out of control, reanalyze entire batch. Internal PE sample Samples and frequency determined by Lab QA Officer Criteria for LCS recovery and duplicate precision Investigate all unacceptable results. Blind PE sample Samples and frequency determined by accrediting agencies and projects Determined by PE provider Investigate all unacceptable results. LCS = laboratory control sample QC = quality control MB = method blank %R = percent recovery MDL = method detection limit RL = reporting limit where RL = (2.5 mg /mL filtered) x 1000 mL MS = matrix spike RPD = relative percent difference PE = performance evaluation RSD = relative standard deviation
fluorometer QC Sample or Activity Minimum Frequency Acceptance Criteria Corrective Action Calibration With each run r2 value near 0.999 Investigate problem. Correct any obvious problems. Repeat calibration until acceptable. Method Blank Before any run and between sample sets <RL Rinse cuvette and repeat until criteria is met. Sample Duplicate One (1) per sample set (10 samples) RPD + or - 5% Investigate problem. Report to Laboratory Director if problem is unknown. Matrix Spike One (1) per sample set (10 samples) RPD + or - 25% Investigate problem. Report to Laboratory Director if problem is unknown. Laboratory Control Standard One (1) with calibration and with each calibration check 90-110%R Investigate problem. Correct any obvious problems. Repeat until acceptable. Internal PE sample Samples and frequency determined by Lab QA Officer 75-125% R RPD < 25% Investigate all unacceptable results. Blind PE sample Samples and frequency determined by accrediting agencies and projects Determined by PE provider Investigate all unacceptable results. LCS = laboratory control sample QC = quality control MB = method blank %R = percent recovery MDL = method detection limit RL = reporting limit MS = matrix spike RPD = relative percent difference PE = performance evaluation
Table 12. Summary of QC requirements for water toxicity analysis QC Sample or Activity Minimum Frequency Acceptance Criteria Corrective Action Initial Demonstration of Capability All technician performing test must perform once at end of training prior to actual sample analysis The RPD of four (4) samples utilizing the same matrix must be within of the results obtained by a trained technician reading an independently setup sample Investigate issue. Observe for proper technique. Retrain as indicated. Repeat IDC’s until results within acceptable criteria. Negative Method Control One (1) sets of triplicate per each batch analysis ≥15 fluorescing organisms for each set of three (3) Method Blank cells Investigate issue. Re-run Method Blanks in a known “virgin” testing cell. Repeat until results are within acceptable limits. Positive Method Control One (1) sets of triplicate per each batch analysis ≥4 non-fluorescing organisms for each set of three (3) Method Blank cells Investigate issue. Re-run Method Blanks in a known “virgin” testing cell. Repeat until results are within acceptable limits. Sample Analysis For each sample analyzed Three (3) test chambers filled with six (6) Daphnia magna per each sample analyzed Qualify any results that fail to meet criteria due to sample or testing reagent issues. Laboratory Duplicate One (1) per ten (10) samples analyzed RPD ≤ 25% Investigate issue. If system precision is in control, qualify results. If system precision is out of control, reanalyze entire batch associated with specific QC duplicate. Field Duplicate One (1) per ten (10) samples analyzed RPD ≤ 25% Investigate issue. If system precision is in control, qualify results. If system precision is out of control, reanalyze entire batch associated with specific QC duplicate.
Table 13. Summary of QC requirements for measurements with Hach ruggedized probes QC Sample or Activity Minimum Frequency Acceptance Criteria Corrective Action Capability demonstration Four (4) prepared samples analyzed prior to any customer sample analyses LDO 97-104% of theoretical DO pH ± 0.1 of expected Others RPD < 25% Repeat until acceptable. Calibration stability monitoring Immediately before calibration measure standards Not applicable. Not applicable. Results are used to monitor stability of probes and evaluate need for maintenance. Calibration Daily prior to sample analysis and after every 8 hours After calibration, measure calibration standards (conductivity, pH, DO % saturation of water saturated air) as sample pH ± 0.1 of expected, others 99-101% R Investigate and fix any obvious problems. Repeat until acceptable. Calibration check Immediately following calibration Measurement of calibration standards or LCS (conductivity, pH, DO % saturation of LCS or of water saturated air) Cond. 90-110% R, pH ± 0.1 of expected, DO 97-104% sat **LDO method requires LCS to be read in duplicate with each calib. event** Investigate and fix any obvious problems. Recalibrate and repeat until acceptable. Field duplicate (duplicate sample collected at one of sampling sites One (1) per sampling event RPD < 25% Investigate problem. If system precision is in control, qualify results. If system precision is out of control, reanalyze all sampling sites if possible. Internal PE sample Samples and frequency determined by Lab QA Officer 75-125% R RPD < 25% Investigate all unacceptable results. Blind PE sample Samples and frequency determined by accrediting agencies and projects Determined by PE provider Investigate all unacceptable results.
Table 14. Summary of QC requirements for Oakton pH meter QC Activity Minimum Frequency Acceptance Criteria Corrective Action Standardize using two pH buffers that are within 3 pH units of each other Before each meter use +/- 0.1 pH units of actual buffer value* Recalibrate the meter with new buffer solution. If this doesn’t solve the problem, the electrode should be cleaned, repaired, or replaced. Measure a pH buffer bracketed by the two buffers used for standardization as a post-calibration check Before each meter use +/- 0.1 pH units of actual buffer value* Periodically measure pH of standard buffer solution when measuring pH of samples Every 10 samples +/- 0.1 pH units of actual buffer value* Recalibrate the meter and reanalyze the samples measured after the last acceptable check measurement. Check ATC thermometer against NIST-traceable thermometer Quarterly (4 times/year) +/- 0.05oC of a NIST-traceable thermometer Recalibrate the ATC thermometer to a NIST-traceable thermometer *NOTE: Actual pH standard values are temperature dependent. See 5.6.3. in SOP 422.
Data and associated records from analysis of samples and from support activities in the EQL for this project are identified in Table 22. All laboratory paper records are stored in file cabinets within the secure laboratory facility for a period of one to three years. After that period the records are placed in labeled boxes and transferred to a locked room in a nearby university storage room. Electronic data are stored in the laboratory's desktop computers and on a restricted access (i.e., access restricted to Laboratory Director, Laboratory Master Technician, and Laboratory Technicians) intra-university network. Backup copies of electronic media are prepared at least annually and stored in a secure area off-site. Disposition of Records Records are stored for a nominal period of at least ten years. Records are stored for longer periods if requested or required by the customer or regulatory authority. Requests for Records Access to recent (i.e., within the previous year) laboratory records is restricted to laboratory personnel. Access to archived laboratory records is restricted to the Laboratory Director, Laboratory Master Technician, and Laboratory Technicians. All requests for laboratory records should be directed to one of those individuals. Original documents shall not be taken from the file storage area without permission from one of the listed individuals, and copying and distribution of such documents must also have their authorization. Table 22. Data and records generated by field measurements, sample collection, and laboratory sample analysis Activity Data Generator Data Type Data Format Formsa Referenceb
Field measurements Field measurer Field measurement results Written field log sheets Forms 2000F, 2100, 4500 HCAL SOP 420 Sample collection Sampler Field information Written COC Form 1060 SOP 302 Sample receipt Laboratory Director, Laboratory Technician Receipt custody and temperature Written COC Form 1060 QAM 4.2 Receipt Log Spreadsheet Receipt Log, Form 220 QAM 4.3 Internal custody Laboratory Director, Laboratory Technician, Student Time and location of storage Written Form 217 QAM 4.4 Analysis Laboratory Director, Laboratory Technician, Student Total coliform (TC), E. coli (EC), Enterococcus, Bacteriodes thetaiotamicron (GenBac), Bacteriodes dorei (BacHum), Bacteriodes canine (BacCan), 5-day BOD, Turbidity, Total Suspended Solids (TSS), Volatile Suspended Solids (VSS), Optical brighteners, Toxicity Written log sheets and calculation spreadsheet printouts Forms 9230 CAL (TC & EC), 59230 EAL (Enterococcus), 210 & 5220 (BOD5), 2130 (Turbidity), 2540 D DL (TSS), 2540 E DL (VSS), 602 (Optical brighteners), 8711 (Tox), 2520 (Salinity), NH3-N, SOPs 501, 503, 430, 406, 435, 436, 423, 422, 420, 404, 602, 601, 504, 505, 506, 507, 508, 509, 470, Data review, verification and validation Laboratory Director, Laboratory Technician Analysis results Written log sheets, calculation spreadsheet printouts, and runlog spreadsheet Run Log QAM 7.1 Report Laboratory Director, Laboratory Technician Analysis results Electronic template Excerpt from Run Log Spreadsheet QAM 7.4 a All forms are provided in Appendix A: Forms b Referenced SOPs are provided in Appendix D: Environmental Quality Lab Standard Operating Procedures and QAM = EQL QA Manual Assessment/Oversight Assessments and Response Actions
Data Validation and Usability Data Review, Validation, and Verification Requirements Table 24. Criteria for accepting, rejecting, or flagging data Item Criteria If not met sample is accepted, flagged or rejected? Flag Comments Sample not analyzed within hold time Sample received in the lab within 6 hours of collection and analyzed within 2 hours of receipt appropriate hold time Rejected HT Lost sample Proper COC documentation not followed and sample is misplaced (Unable to analyze) LS Unable to Collect Sample Various circumstances (i.e., weather, lost sampling container) cause sample to not be collected (Unable to analyze) NS Sample not held within required temperature range Temperature blank within cooler indicates temperature above 6° C or proper storage equipment failed to read within range (refrigerator/freezer) Rejected T Temperature blank not placed within cooler during sample transport Unknown receipt temperature Flagged UT Incorrect sampling container used for sample collection Incorrect sampling container used for sample collection Flagged SC Improper preservation Improper preservation (i.e., acidification, filtering) Flagged IP Validation and Verification Methods All processes at EQL (sample receiving and handling, sample analysis, data reduction, data reporting, data review, etc.) are subject to examination to evaluate adherence to project specifications. This examination consists of several layers of technical and QA review. These reviews ensure that all data released by EQL were scrutinized by qualified independent reviewers and are scientifically sound, appropriate to the method, completely