Drinking Water Quality

Kennebec Water District - Laboratory Quality Assurance Plan Effective Date: August 31, 2016 Page 1 of 27

Kennebec Water District Filtration Plant

LABORATORY

QUALITY ASSURANCE PLAN

Table of Contents

1. INTRODUCTION

2. QUALITY ASSURANCE MANAGEMENT

3. LABORATORY PRACTICES

4. CALIBRATION METHODS

5. PREVENTIVE MAINTENANCE PROCEDURES

6. STANDARD OPERATING PROCEDURES

7. ACCURACY, PRECISION, AND REPORTING LIMITS

8. QUALITY CONTROL SAMPLES

9. MICROBIOLOGICAL QC TESTING

10. ACTION RESPONSE TO LABORATORY RESULTS

11. RECORD RETENTION & STORAGE

APPENDIX A) STANDARD OPERATING PROCEDURES

APPENDIX B) PREVENTIVE MAINTENANCE SCHEDULES

APPENDIX C) QUALITY ASSURANCE FORMS

APPENDIX D) TRAINING RECORDS

1.0 INTRODUCTION Page 2 Kennebec Water District - Laboratory Quality Assurance Plan Effective Date: August 31, 2016 Page 3 of 27

1.1 Quality Assurance and Quality Control Statement

The purpose of KWD’s Quality Assurance Plan and program is to continually review all aspects of the quality control program and make adjustments— or initiate corrective action— as needed to achieve the laboratory’s data quality goals and needs. An appropriate series of corrective actions, in this scenario, is to:

 review quality control limit calculations for obvious errors,  review matrix spike preparation procedures to determine if any errors were made,

The Kennebec Water District (KWD) is committed to providing analyses of known quality within specific limits of precision and accuracy. The laboratory's primary goal is producing unbiased, documented data on a timely basis.

The laboratory maintains an ongoing Quality Assurance (QA) program designed to maintain and document a uniform set of procedures for the analysis of inorganic and microbiological parameters. This program includes documentation of analytical methodologies, reduction and reporting of data, and instrument and methods performance evaluation.

The Quality Assurance program ensures that the production of complete and acceptable data of known quality is given priority above all other considerations except health and safety.

1.2 Quality Assurance Documents

1.2.1 Quality Assurance Plan

The KWD laboratory Quality Assurance Plan (QA Plan) documents the quality assurance/ quality control policies and procedures used to produce data of known quality. It provides documented guidelines for laboratory personnel to produce and evaluate quality data. All employees are required to adhere read, understand, and sign off on to all procedures described in the document.

The following documents have been utilized in developing the QA Plan:

1) ”Standard Methods for the Examination of Water and Wastewater” 22nd Edition, (STM) APHA, AWWA, WEF, 2012

2) “Manual for the Certification of Laboratories Analyzing Drinking Water” 5th Edition, (MCLADW) USEPA Office of Ground & Drinking Water, 2005

3) “Chapter 263, Maine Comprehensive and Limited Environmental Laboratory Certification Rules” (Chap. 263) Maine Department of Human Services, 2000

1.2.2 Standard Operating Procedures

Routine analytical procedures are documented in a written format known as a Standard Operating Procedure (SOP). The SOP describes in outline form the specific steps of all methodology including sample preparation, analysis and data reduction. SOPs must be reviewed by the KWD Lab QA Coordinator and approved by the Laboratory Director prior to inclusion in the appropriate SOP manual. All SOP revisions must be signed and dated until submitted to the lab QA Coordinator for approval. All pertinent employees must formally review each SOP revision. All SOP’s should be reviewed by all laboratory staff.

1.2.3 Laboratory Certification Documents

Laboratory certification documents issued by the State of Maine or other regulatory authority that authorize the laboratory to conduct and report specific analytical parameters are posted in the laboratory for public inspection.

1.2.4 Quality Assurance and Performance Evaluation Reports

All data and report forms generated during performance evaluation and quality assurance testing conducted for laboratory certification are bound in binders and kept in the laboratory office.

1.2.5 Laboratory Training and Proficiency Testing

All laboratory training and proficiency testing will be performed through the Laboratory Director and recorded in the Laboratory Log Book.

2.0 QUALITY ASSURANCE MANAGEMENT

2.1 Quality Assurance Management Organizational Chart

LABORATORY DIRECTOR Matt Zetterman

QUALITY ASSURANCE COORDINATOR Emile Nicol

ANALYSTS James Epstein Darrell Field Jared Bragdon

2.2 Internal Laboratory Organization

2.2.1 It is the responsibility of each employee to adhere to all quality control procedures specified by this manual and each specific SOP.

2.2.2 Analysts are to report complete quality control data as required by the specific SOP for any given test. Quality control data that is considered out of control is reported to the Laboratory Director or Quality Assurance Coordinator for evaluation and subsequent corrective action.

2.2.3 The Laboratory Director is responsible for the technical and scientific oversight of all laboratory activities. The laboratory technical director must certify that personnel with appropriate education and technical background perform all tests for which the laboratory is certified. Each laboratory will be certified only after presentation of documentation to the department regarding education and work experience.

2.2.4 Quality Assurance Coordinator must review laboratory quality control data, conduct annual internal laboratory audits, and notify management of deficiencies found in the laboratory’s quality system. The QAC must be free from internal and external influences when evaluating data and conducting audits. The QAC must have documented training and/or experience in quality assurance/quality control procedures and must have knowledge of the approved analytical methods and quality system requirements. The QAC must maintain the laboratory’s quality assurance documents up to date. The QAC duties and responsibilities may also be carried out by the laboratory technical director when staffing is limited.

2.4 Reporting Lab Director Change

2.24.51The Laboratory Certification Program must be notified in writing within 30 days of a change in Laboratory Director. Contact information including name and telephone number must be provided.

2.35 Demonstration of Capability and Proficiency Evaluation Programs

2.35.1 Demonstration of Capability

The laboratory must confirm that it can properly operate all methods before introducing the environmental tests. If there are any changes to the method, the confirmation must be repeated.

2.35.1.1 Prior to acceptance and institution of any method, satisfactory demonstration of capability (“DOC”) is required. In general, this demonstration does not test the performance of the method in real world samples, but in the applicable and available clean quality system matrix sample (a quality system matrix in which no target analytes or interferences are present at concentrations that impact the results of a specific test method), e.g., drinking water. In addition, for analytes which do not lend themselves to spiking, the demonstration of capability may be performed using quality control samples.

(a) All demonstrations must be documented. All data applicable to the demonstration must be retained and available.

(b) When an analyte that is not currently found on the laboratory’s list of certified analytes is then added to an existing certified test method, an initial evaluation must be performed for that analyte.

(c) It is the responsibility of the laboratory to document that other approaches to DOC are adequate. The documentation must be within the laboratory’s Quality Manual, e.g., for Bacteriology.

2.35.1.2 Procedure for Demonstration of Capability

(a) A quality control sample must be obtained from an outside source. If not available, the QC sample may be prepared by the laboratory using stock standards that are prepared independently from those used in instrument calibration.

(b) The analyte(s) must be diluted in a volume of clean quality system matrix sufficient to prepare four aliquots at the concentration specified, or if unspecified, to a concentration of one to four times the reporting limit.

(c) At least four aliquots must be prepared and analyzed according to the test method either concurrently or over a period of days.

(d) Using all of the results, the laboratory must calculate the mean recovery in the appropriate reporting units and the standard deviations of the population sample (n-1) (in the same units) for each parameter of interest. When it is not possible to determine mean and standard deviations, such as for presence/absence and logarithmic values, the laboratory must assess performance against established and documented criteria.

2.35.1.3 Thereafter, the laboratory is required to continue demonstrating method performance through the quality control requirements (such as laboratory control samples).

2.5.1.4 In cases where a laboratory analyzes samples using a method in use by the laboratory before the effective date of this rule, and no significant changes in instrument type, personnel or method has occurred, then the continuing demonstration of method performance and the analyst’s documentation of continued proficiency will be acceptable. The laboratory must have records on file to demonstrate that a demonstration of capability is not required.

2. 3 5.1.45 An initial demonstration of capability must be completed each time there is a change in instrument type, personnel, or method.

2.46 Proficiency Testing

2.46.1 The laboratory participates at least twice annually in a Performance Evaluation (P.T.) Testing Program, utilizing blind sample(s) supplied through a T.N.I accredited provider. Results are to be sent directly to the Maine Laboratory Certification Program by October 31 st .

2.46.1.1 The laboratory's management and all analysts must ensure that all PT samples are managed, analyzed, reported, and otherwise handled in the same manner as routine samples, including utilizing the same staff, procedures, equipment, facilities, and frequency of analysis as used for routine analysis for that field of testing.

2.46.1.2 When analyzing a PT sample, the laboratory must employ the same calibration, quality control, acceptance criteria, sequence of analytical steps, number of replicates, and other standard operating procedures as used when analyzing routine samples. The laboratory must follow sample preparation steps for the PT sample as instructed by the approved PT provider for which the PT sample was obtained.

2.46.1.3 The laboratory may not send any PT sample or any portion of a PT sample to another laboratory for any analysis.

2.7 Internal Audits

Laboratory management must audit every part of its management system including its testing and/or calibration activities at least once every twelve months. The audit will cover everything from sampling through reporting.

During the management-system audit, laboratory management must look at the way the laboratory actually operates, and compare this to the laboratory operations as described in its management system documentation. The system described in the documents, and the system as it operates in the real world, must be in accordance.

For example: Suppose the management system documents say that the laboratory maintains records on the qualifications, training, skills, and experience of technical personnel. During the internal audit, check to see that such records are actually being maintained. If they are not, then the audit has detected a problem that must be remedied. Or, say that according to the laboratory’s management system, every piece of test or measuring equipment must, in some way, have its calibration status indicated. During the audit, randomly sample several pieces of equipment to see if their calibration status is identified. If it is not, then your audit has detected another problem that requires further investigation and correction.

It is absolutely essential that internal auditors keep written records of the audit. The laboratory must also keep written records of any actions taken to remedy problems uncovered during the audit. Follow up audits are to be conducted to verify the effectiveness of corrective actions.

A complete record will consist of the following documents, and is considered the minimum level of required documentation:

• Agenda for the Internal Audit • Internal Audit Report identifying Corrective Action Requests or CARs • Root cause analysis for each CAR • Resolution of the CAR • Documentation identifying responsible authority for the generated CAR

3.0 STANDARD LABORATORY PRACTICES

3.1 Training and Safety

3.1.1 The Laboratory Director is responsible for ensuring that each analyst is completely trained in a specific procedure prior to the analyst conducting the procedure without supervision.

3.1.2 The analyst will be continually supervised during training in a new procedure.

3.1.3 Analysts are trained in all aspects of safety prior to training in a new procedure. The analyst has access to all Safety Data Sheets (SDS) pertinent to the procedure. All SDS are compiled into an SDS binder located in the employee break room at the filtration plant, which is accessible at all times.

3.1.4 All employees must initially and annually review the laboratory safety section of the KWD safety manual. Upon completion employees will date and sign the log sheet in the QAP manual.

3.2 Security and Sample Custody

3.2.1 Building Security

The Laboratory/Filtration building exterior doors and windows are locked whenever the building is unoccupied. Only laboratory employees are allowed unescorted access to the laboratory. All supplies and samples to be tested are delivered into the laboratory under authorized laboratory personnel supervision.

3.2.2 Restricted Work Areas

Signs are posted restricting access to the laboratory work areas to authorized employees only. All visitors are directed to a reception area and are allowed in the laboratory only under the direct supervision of authorized laboratory personnel.

3.2.3 Sample Receipt, Sample Receipt Form, and Chain-of-Custody (COC)

Samples are received in the laboratory by designated personnel and are checked immediately for analytical requests, appropriate sample container use, holding time and shipping conditions, preservation , temperature, sample identification, and chain of custody records. A Chain-of-Custody (C-O-C) form (see Appendix C for an example of a typical form) is used to document the data quality objectives for each sample; the sample conditions when obtained, during delivery, and upon arrival at the lab; and is filled out by the person sampling and delivering the sample to the lab. (“Manual for the Certification of Laboratories Analyzing Drinking Water” 5th Edition, (MCLADW) USEPA Office of Ground & Drinking Water, 2005) Drinking water compliance samples will be rejected, or reports for these samples flagged appropriately, if holding times, preservatives, or shipping conditions do not meet ME DHS requirements. If other problems are found, they are documented on the C-O-C , and the sampler is notified with specific details of the problem.

Incoming samples must satisfy KWD’s sample acceptance criteria before being analyzed. Sample acceptance is based on proper protocols for sample collection. This includes complete documentation, sufficient volume, proper chemical preservation, sample container sealing and labeling. No samples will be accepted if holding times have been exceeded or will be exceeded before analysis. Sample acceptance criterion includes proper custody and sample labeling documentation. Proper custody documentation includes an entry for all physical samples delivered to the laboratory with an identification code that matches the sample bottle and a date and signature of the individual who collected the sample and delivered them to the laboratory. The lab will reject samples that show any signs of damage, contamination, inadequate preservation, or loss of integrity. Samples are collected in accordance with the parameters outlined in Section 3.3.

The district’s sample acceptance policy is to be posted in laboratory so acceptance procedures are clear to everyone dropping off samples and to laboratory personnel.

3.2.4 Sample Identification

Each sample is given a unique laboratory identification description. The sample description, date, sample type, sample container, total number of samples, and test(s) requested are recorded on the C-O-C or analysis recording form (See appendix C). Additional information regarding recipients of completed reports and/or invoice is documented. Specific instructions on preservation, preparation, test method(s) and requested analytes are documented on the C-O-C. and on sample containers where appropriate. Unidentified samples will be rejected, or flagged for identification at sample receipt.

Samples for weekly distribution sampling will be numbered as follows:

SiteNumber-YYYYMMDD – for example a sample taken on January 1, 2016 from site number 5 would be 5-20160101.

Operations and Maintenance samples will be numbered as follows:

HHMM-YYYYMMDD with the time being in military time– for example a sample taken at 1:51pm on January 1, 2016 would be 1351-20160101.

3.2.5 Subcontracted Laboratory Samples

The KWD routinely subcontracts with other laboratories for analyses not performed by KWD in-house. Drinking water samples that are sent to other laboratories for analysis, unless handled independently through prior

arrangement, are first processed following the steps outlined in sections 3.2.3 and 3.2.4 above. Drinking water samples must only be sent to laboratories certified to conduct the drinking water analyses desired, and are identified for analysis by drinking water methods. Samples delivered to subcontract laboratories are to be preserved and stored appropriately (see table below) until shipped, and may be shipped using KWD staff or via a commercial delivery service or the USPS. Samples must be handled in a timely fashion so as to not exceed holding time(s) for analytes requested.

Whether KWD acts solely as an intermediate agent handling a sample between a third party and a contract laboratory, or in cases where the sample(s) are part of a larger group of samples from which some of the analyses are performed at the KWD, the original Chain-of-Custody (COC) is retained at the KWD, and a new COC is generated (with specific annotations for contract laboratories) that lists only the samples to be sent for contract laboratory analyses. KWD personnel sign the contract laboratory COC at the time of packing the samples for shipment or relinquishing the samples to the contract lab.

3.3 Sample Preservation and Holding Times

Samples received by the laboratory for analyses are preservedative using the techniques listed in Table 3.3.1 and are analyzed within the holding times listed in Table 3.3.1. Unpreserved samples that are received by the lab immediately after sampling are appropriately preserved immediately upon lab receipt.

Table 3.3.1: Recommended Preservation, Holding Times, Sample Sizes, and Container Material Types for the following Analytes

Sample Suggested Type of Analyte/Test Preservative Holding Time Sample Size Container Alkalinity 4C 14 days 100 ml P or G Chlorophyll-a Freeze after .45 micron 28 days after filtration & 500 ml P, then filtration freezing aluminum foil when frozen Color 4C 48 hours 100 ml P or G Chlorine Residual None Immediately 100 ml P or G Conductivity 4C 28 days 100 ml P or G

E. coli 0.008% Na2S203; 4C 28 days 100 ml P or G Fluoride 4C 28 days 100 ml P or G

Total Coliform 0.008% Na2S203; 4C 30 hours 100 ml P or G Hardness – Total, HN03 to pH <2 after lab 6 Months 100 ml P or G Ca, or Mg receipt

Metals, Total HN03 to pH <2 after lab 6 months 100 ml P or G (except Hg) receipt Nitrate, 4C 48 hours 100 ml P or G unchlorinated Nitrate, chlorinated 4C 14 days 100 ml P or G Page 11 Kennebec Water District - Laboratory Quality Assurance Plan Effective Date: August 31, 2016 Page 12 of 27

Nitrite 4C 48 hours 100 ml P or G Orthophosphate Filter within 15 minutes, 48 hours 50 ml P or G 4C Total P 1 ppb D.L. H2SO4 - pH < 2, 4C (– 30 28 days 50 ml P or G or frozen) pH None Immediately 50 ml P or G Sulfate 4C 28 days 100 ml P or G Total Dissolved 4C 7 days 100 ml P or G Solids (TDS) Turbidity 4C 24 hours 100 ml P or G

3.4 Analytical Methodology

All analytical procedures are written as Standard Operating Procedures and have been reviewed by the Laboratory Director. All personnel performing any given analyses must follow the SOP exactly for that analytical procedure. All revisions must be read by, understood, followed, and signed off on by all laboratory personnel. The following documents are the primary references for analytical SOPs:

1) ” Standard Methods for the Examination of Water and Wastewater” 22nd Edition, (STM) APHA, AWWA, WEF, 2012 2) “Manual for the Certification of Laboratories Analyzing Drinking Water” 5th Edition, (MCLADW) USEPA Office of Ground & Drinking Water, 2005 3) “Maine Comprehensive and Limited Environmental Laboratory Certification Rules” Maine Department of Human Services, 2000 4) “United States Code of Federal Regulations” (CFRs) - to present.

Table 3.4.1 Method References

Parameter Method Number Aluminum 3500 Al B Iron SM 3500 Fe B Total Hardness ( Ca & Mg Hardness) SM 2340 C Alkalinity SM 2320 B Conductivity SM 2510 B Residual Chlorine (Free & Total DPD) SM 4500 Cl G SM 9223 Fluoride SM 4500 F C Total Coliform Bacteria SM 9223B SM 9222 B PH SM 4500 H B Orthophosphate SM 4500 P E Temperature SM 2550 B Total Dissolved Solids SM 2510 B Turbidity SM 2130 B

3.5 Data Reduction and Reporting

3.5.1 Reduction and Verification Page 12 Kennebec Water District - Laboratory Quality Assurance Plan Effective Date: August 31, 2016 Page 13 of 27

The analyst must record all analytical data directly by ink into bound laboratory notebooks unless electronically generated by analytical equipment. It is the analyst’s responsibility to provide all calculations, charts and related graphs for review by the Laboratory Manager or Quality Assurance Coordinator.

3.5.1.1 All data, analyses, calculations, charts and graphs must be entered in ink with date of analysis, and signed by the analyst.

3.5.1.2 Errors must be corrected by drawing a single line through the data entry. The corrected entry should be written as close as possible to the original data, and initialed by the analyst making the correction.

3.5.1.3 Errors must not be erased or corrected using a masking fluid.

3.5.1.4 Data is verified by the primary data processing technician or a second analyst prior to entry into any summary spreadsheet, database, or ME DHS report forms DHHS Monthly Operating Reports (MOR’s).

3.5.2 Data Reporting

Once data from laboratory notebooks has been transcribed to report forms, spreadsheets, or databases, the data is proofread for transcription or data entry errors by the Laboratory Manager or Quality Assurance Coordinator.

3.5.2.1 Reports must include the date the sample was obtained, and the date the sample was received by the laboratory.

3.5.2.2 Reports must include methodology references and dates of analysis.

3.5.2.3 Drinking water non-compliant microbiology test results are reported within 24 hours immediately to the ME DHHS by e-mail in DHHS reporting format, in addition to standard internal KWD reporting.

3.6 Data Validation

3.6.1 All analytical data must be reviewed and approved by the Laboratory Manager Director or Quality Assurance Coordinator (data validator) prior to final reporting.

3.6.2 The Lab Manager or Quality Assurance Coordinator must review data check a minimum of 10% of all calculations prior to approval. If errors are encountered, all calculations on related test batches must be checked.

3.6.3 All chain of custody forms and analysis request forms are reviewed to ensure data is reported in formats, units, and with the proper level of QC data requested for the project. The data validator compares sample I.D. numbers, sample descriptions, matrices, etc. in the final report with those listed on the C-O-C for the sample evaluated. Any discrepancies are investigated, and proper resolutions are incorporated in the final report. Any qualification of the data is verified & documented in the final report by the validator.

3.6.4 The Quality Assurance Coordinator, Laboratory Director, or Alternate Lab Director is responsible for final report approval. All report data and related quality control data is reviewed and the final report is checked for completeness and reporting accuracy.

3.6.5 Upon approval, the Alternate Laboratory Director, or Laboratory Director or Quality Assurance Coordinator must sign the final lab report prior to release.

3.7 Data Quality Assessment and Corrective Action

3.7.1 All data generated must be assessed in terms of accuracy and precision prior to approval or distribution.

3.7.2 Quality control data is assessed by evaluation of laboratory control samples, duplicate samples, spiked samples, and method blanks. The Laboratory Director, Quality Assurance Coordinator, or the Alternate Laboratory Director may request additional quality control measures.

3.7.3 The Laboratory Director or Quality Assurance Coordinator must confirm that any problem requiring corrective action has been resolved and steps have been implemented to eliminate future problems.

3.7.4 All samples related to the problem must be re-analyzed for those analytes requiring corrective action. All data requiring corrective action will not be released as a final report until the analytical problem is resolved and documented in the analyte specific QC logbook.

3.7.5 The final report may be approved and released for distribution after the reanalyzed samples have been successfully assessed for quality control.

3.8 Laboratory Reagents

Laboratory reagents used in conducting analyses are certified “Analytical Reagent Grade” purity (American Chemical Society - ACS) or higher purity, unless otherwise specified by the SOP for that method. SDS sheets for all laboratory reagents and supplies are maintained on file in the laboratory office and are reviewed by all laboratory personnel who use the reagents. All laboratory

personnel must strictly adhere to all safety, storage, and disposal guidelines for any given reagent.

3.9 Laboratory Reagent Water

3.9.1 General Use Reagent Water

Several sources of laboratory reagent (distilled-deionized) water are used for general purpose cleaning and/or reagent preparation.

Conductivity values of laboratory reagent water must be <2 µS/cm at 25C. Any Lot of water that exceeds 2µS/cm at 25C is not used for reagent preparation. A new Lot of reagent water is obtained and any corrective action documented in the Quality Assurance logbook.

3.9.2 Microbiological Reagent Water

Reagent water used for microbiology testing must be tested at the frequencies listed in table 3.9.3. Results of this testing must meet the criteria listed in table 3.9.3. Data obtained from testing microbiological reagent water is recorded in the Microbiological Testing Logbook. If a given lot of microbiology reagent water fails to meet the criteria in 3.9.3, a new lot is obtained and corrective action is recorded in the Microbiological Testing Logbook.

Table 3.9.3 Microbiological Reagent Water Quality Requirements

Test Monitoring Maximum Frequency Acceptable Limit Conductivity Continuously or >0.5 megohms with each use Each resistance or Batch <2 umhos/cm at 25oC pH With each use 5.5-7.5 S.U. Total organic carbon Monthly <1.0 mg/L Heavy metals, single Annually * <0.05 mg/L (Cd, Cr, Cu, Ni, Pb, and Zn) Heavy metals, total Annually * <0.10 mg/L Ammonia/organic nitrogen Monthly <0.10 mg/L Total chlorine residual Monthly or <0.01 mg/L <0.1 with each use mg/L Heterotrophic plate count Monthly <1,000 CFU/mL

* Or more frequently if there is a problem.

3.10 Dishwashing

Clean glassware at the laboratory sink or in laboratory dishwashers. Use hot water, if available, and soap or other detergent approved for laboratory use. If necessary, use a mild scouring powder. Wear appropriate gloves that have been checked to ensure that no holes are present. Use brushes of suitable stiffness and size. Avoid accumulating too many articles in the cleanup area. Usually, work space around a sink is limited; piling up dirty or cleaned glassware can lead to breakage. Remember that the turbid water in a sink may hide a jagged edge on a piece of broken glassware that was intact when put into the water. Drain out the standing water. Then use a pair of heavy gloves to remove broken glass. Avoid use of strong cleaning agents such as nitric acid, chromic acid, sulfuric acid or other strong oxidizers unless specifically instructed to use them.

3.11 Customer Complaints

Complaints may be lodged by various means in writing, electronically through e- mail, by telephone, web application, and in person. Complaints can result from internal customers which include other KWD staff members and external customers such as ratepayers.

Staff who receive a complaint should document the complaint including: the affiliation of the person and organization who lodged the complaint, the date the complaint was received, and the nature of the complaint.

If the person receiving the complaint can determine the cause and the corrective action, they should take the corrective measures, complete the complaint form and forward it to the identified supervisor.

If the cause and corrective action cannot be determined by the person receiving the complaint, submission of the complaint is made to laboratory management.

A corrective action report is generated and the laboratory’s corrective action process initiated. This process involves the determination and investigation of adverse impact on operations and quality.

When the corrective action has been completed, the complaint is closed. All documentation of the event should be submitted to laboratory management and is reviewed for completeness and files the forms.

Complaints are reviewed in the internal audit and management review to ensure any changes from a complaint were proper, effective, timely and successful.

4.0 ANALYTICAL CALIBRATION AND VERIFICATION

4.1 Calibration Standards

4.1.1 All calibration standards (including calibration verification (CV) and continuing calibration verification (CCV standards) must be prepared using chemical reagents of at least "Analytical Reagent Grade" unless approved method permits otherwise. Alternately, commercially available stock standards with a certified value may be used to prepare calibration standards. Calibration standards are verified against a quality control standard prepared or purchased from a source different from the calibration standards. Calibration standards and/or the quality control standard are replaced when the deviation from the QC standard actual value exceeds control limits. (Chap. 263 pg. 20)

4.1.2 Analytical volumetric glassware used for the preparation of calibration standards must be of "Class A" accuracy. All glassware must be cleaned following specific procedures designed to minimize sample contamination.

4.1.3 Calibration solutions must be prepared according to the written SOP for the specific analyte. Preparation must be documented in the QA log or on the standard solution container each time the standard is prepared. The calibration documentation must include; date of preparation, analyte, solvent, concentration prepared, preservation and the name of the analyst who prepared the solution. (Chap. 263, pg. 17)

4.1.4 Calibration solutions are also obtained commercially; the label on these containers include the information listed above.

4.1.5 A minimum of three calibration standards that bracket the expected sample concentration range are used to calibrate instrumentation. The midrange standard should correspond to the midrange concentration of the samples or the middle of the dynamic range for the instrument as appropriate.

4.1.6 Instruments with pre-programmed calibration curves must have the calibration verified using at least one calibration verification (CV) standard in the middle of the dynamic range. (Chap. 263, pg. 19 & 23)

4.2 Calibration Curve

4.2.1 The calibration curve for each instrument is created or verified at the beginning of each analytical run.

4.2.1.1 A calibration curve consists of one reagent blank and a minimum of three calibration standards in graduated concentrations that bracket the expected sample concentration range or otherwise reflect the dynamic analysis range for the instrument.

4.2.1.2 All calibration curve data generated must be recorded directly in the analyte specific laboratory notebook.

4.2.2 If an analytical test result is higher than the highest calibration standard, the sample will be serially diluted with proper matrix matching until analysis results in a value bracketed by the calibration curve. Alternatively, an additional calibration verification standard bracketing the sample absorbance must be run within acceptable QC limits.

4.2.3 Instrument Calibration and Verification Sequence:

A. Calibration blank B. Low level calibration standard C. Mid level calibration standard D. High level calibration standard E. Initial calibration verification standard If out of control, repeat steps A-E F. Method blank G. Continuing calibration verification

4.3 Initial Calibration Verification

4.3.1 The calibration curve for each instrument used, (pre-existing or generated each run) is verified at the beginning of each analytical run by measurement of an initial calibration verification standard. The results of the measurement (% standard recovery) must fall within the upper and lower control chart limits established for the analytical system. If the measurement exceeds the control chart limits, corrective action must be taken until the problem is corrected. The instrument must be recalibrated and the initial calibration verification standard reanalyzed until the results fall within the control limits. (Chap. 263, pg 16)

4.3.1.1 Initial calibration verification data must be recorded in laboratory notebooks.

4.3.1.2 The upper control chart limit is defined at the 95% confidence level as: the mean plus three times the standard deviation.

4.3.1.3 The lower control chart limit is defined at the 95% confidence level as: the mean minus three times the standard deviation.

4.3.1.4 The upper warning limit is defined at the 99% confidence level as: the mean plus two times the standard deviation.

4.3.1.5 The lower warning limit is defined at the 99% confidence level as: the mean minus two times the standard deviation. (MCLADW, pg. IV-6)

4.3.2 The initial calibration verification standard is prepared from a different stock standard lot from the stock standards used to prepare the calibration curve standards.

4.4 Continuing Calibration Verification

4.4.1 A continuing calibration standard at approximately midpoint of the calibration curve should be analyzed at a minimum after every 10 samples or once per hour whichever is more frequent.

4.4.2 The continuing calibration standard must be prepared from a different stock standard lot from the stock standards used to prepare the calibration curve standards.

4.4.3 The percent recovery value from the analysis of a continuing calibration standard must fall within the calculated control limits for that analyte:

4.4.3.1 If values are not within this range recalibration is necessary and the continuing calibration standard must be reanalyzed.

4.4.3.2 Recalibration data must be recorded directly in the laboratory notebook.

4.4.3.3 Samples between the last acceptable calibration verification and a required recalibration are re-analyzed after acceptable recalibration verification. (Region 1 Lab inspector’s checklist)

4.5 Analytical Balance Calibration

4.5.1 The analytical balance weighs to a resolution of 0.0001g; and is calibrated under a service contract annually using ASTM Type 1, weights.

4.5.2 Each analytical balance is calibrated by lab staff on a monthly basis using three ASTM Type “3” weights and recorded in the Laboratory QC Log.

4.5.3 Correction values for applicable ranges are noted on the analytical balance and corrections are applied when the balance is used.

4.5 pH / ISE Meter Calibration

4.5.1 The pH meter is calibrated each day or every four hours of use with fresh pH buffers separated by 3 pH units, bracketing the tested sample pH. The accuracy of the calibration curve is checked daily by testng an

independent pH 6.00 S.U. buffer. Calibration, Q.C., maintenance, and corrective action data is recorded in the pH calibration logbook.

4.5.2 The ISE (Ion Selective Electrode) meter is calibrated each run using three calibration standards bracketing the expected measurement range. Ionic strength buffers are used to minimize interferences. Calibration is checked daily by testing a standard obtained from a different source than the calibration standards.

4.6 Spectrophotometer

4.6.1 Spectrophotometer Description

KWD utilizes a HACH DR 3000 visible light spectrophotometer with a diffraction grating monochromator capable of generating wave-lengths from 340 to 1000 nanometers (nm). The DR 3000 is microprocessor- operated and provides direct readings for absorbance, percent transmittance or concentration.

The DR 3000 contains both pre- programmed calibration curves and accepts user- defined calibration curves as well.

4.6.2 Spectrophotometer Calibration

User defined calibration curves are generated prior to analysis and follow the guidelines outlined in sections 4.1 through 4.4 above. These internal calibration curves used are verified daily or each time a specific program is utilized. (chap.263 pg.16)

This verification of the calibration curve will include the analysis of at least a reagent blank and one standard in the expected range of the samples analyzed. This verification must be within 15% of the certified value of the standard (NELAC), until adequate determinations are performed to calculate control charts for the analyte (see section 4.4). If the verification standard falls outside the acceptance range, the system must be investigated, maintained & recalibrated until acceptable results are obtained. (chap.263 pg.20)

Calibration data, quality control data, maintenance records and corrective action must be recorded directly in the appropriate laboratory logbook.

The spectrophotometer monochromator is checked semi-annually against external standards. (chap. 263 pg. 21)

4.7 Thermometer Calibration and Temperature Monitoring

4.7.1 Thermometer Calibration Page 20 Kennebec Water District - Laboratory Quality Assurance Plan Effective Date: August 31, 2016 Page 21 of 27

4.7.1.1 The thermometers in the laboratory are checked annually against a N.I.S.T. reference thermometer; the calibrating technician, date of calibration, and correction factors are recorded in the laboratory QA logbook. Each thermometer is identified with a label to indicate any temperature correction to be applied to that thermometer’s reading. Any thermometer requiring a correction has that correction applied to all readings entered in laboratory logbooks. (MCLADW sec. 3.2.3)

4.7.1.2 If the calibration deviation exceeds control limits set at 10x the lowest readable increment, i.e. if the correction applied to a thermometer with a readability of 0.1C is +/- 1C, the thermometer must be replaced. Corrective action must be documented in the laboratory notebook.

4.7.1.3 All thermometer calibration corrections should be rounded to the nearest ½ of the smallest measurable increment for that thermometer.

4.8.2 Temperature Monitoring

All incubators and refrigerators in use have their temperature monitored and documented using thermometers immersed in liquid, and are calibrated annually against an N.I.S.T. certified thermometer (See Section 4.8.1). All temperature measurements are recorded on the Laboratory Temperature Monitoring Log Sheet with the date and time of measurement, and the calibration correction (if any) applied to the recorded reading. Temperatures are monitored according to the following schedule:

4.8.2.1 Refrigerator temperatures are recorded on a daily basis directly on the monthly temperature log sheet. The allowable temperature range is 1C to 5C for each shelf in sample storage refrigerators. (chap. 263 page 16)

4.8.2.2 Microbiological incubator temperatures (35 +/-0.5C) are monitored at least twice daily when in use, with readings separated by four hours minimum. Readings are recorded on the monthly temperature log sheet.

4.8.2.3 If the temperature of a measured device exceeds acceptable limits, the device is adjusted and the temperature rechecked. Corrective action is documented directly on the temperature monitoring forms.

4.9 Turbidity Calibration

4.9.1 Daily Calibration

Work in Progress Page 21 Kennebec Water District - Laboratory Quality Assurance Plan Effective Date: August 31, 2016 Page 22 of 27

5.0 PREVENTIVE MAINTENANCE PROCEDURES AND SCHEDULES

Analytical instrumentation and equipment is maintained in accordance with the manufacturer's instructions and good laboratory practice1.

All maintenance and required monitoring of instruments is documented - work performed, date and initials of technician performing the work are recorded on the appropriate Preventive Maintenance (PM) forms which are stored in_the Plant Operators Office.

See Appendix A for Preventive Maintenance Procedures and Schedules.

6.0 STANDARD OPERATING PROCEDURES

Copies of KWD's Standard Operating Procedures for certified analyte testing are attached as Appendix B.

7.0 PROCEDURES FOR DETERMINING ACCURACY, PRECISION AND METHOD DETECTION LIMITS

7.1 Accuracy

Accuracy is determined at least annually for all analytes, and is calculated from % recovery data obtained from testing reagent water spiked with analytical standards. (Chap 263 pg. 16) 1

7.2 Precision

Precision is evaluated at least annually and is calculated using Relative Percent Difference (RPD) data from replicate analyses. Precision is expressed in units of percent deviation. (Chap 263 pg. 17) 1

1Maine Comprehensive Environmental Laboratory Certification Rules; Chapter 263. Page 22 Kennebec Water District - Laboratory Quality Assurance Plan Effective Date: August 31, 2016 Page 23 of 27

7.3 Method Detection Limits

The Method Detection Limit (MDL) is the minimum concentration of an analyte that can be measured and reported with 99 % confidence that the analyte concentration is greater than zero. Method detection Limits for each certified inorganic chemistry analyte are determined annually in accordance with 40 CFR, Part 136, Appendix A. (Chapter 263 pg. 17 & MCLADW pg. H-4)

The MDL and for analytes are listed in the QA Logbook for that Analyte.

8.0 QUALITY CONTROL SAMPLES (Analytical Systems Control)

8.1 Blanks

8.1.1 Blank Types

Blanks are samples designed to assess sample contamination or to calibrate measurement systems. A universal blank matrix does not exist for all sample matrices, therefore each method will specify what solution is used as the initial blank matrix (distilled water, tested water without reagent, etc.).

8.1.1.1 Calibration blanks must contain all matrix modifiers used in preparation of the calibration standards.

8.1.1.2 Reagent blanks must contain the exact concentration of all reagents used for sample preparation and analysis. Reagent blanks must be evaluated whenever a new reagent lot is used for analysis. Reagent blank data must be recorded with the analytical data for that run.

8.1.1.3 Method blanks must contain the exact concentration of every reagent used in an analytical procedure, and must be taken through the entire sample preparation procedure. Data must be recorded in the laboratory notebook.

8.1.2 Frequency and Acceptability

Each analytical batch requires at least one method (or reagent) blank, analyzed at the beginning of the batch after calibration.

8.1.2.1 If the blank concentration is less than or equal to the method detection limit, no corrective action is required.

8.1.2.2 If the concentration of the blank is above the method detection limit, all samples analyzed with the blank and having concentrations less than ten times the blank level either a) may not be reported with an MDL lower than the measured blank concentration, or b) must be re-tested along with another method blank after the contamination is found and the problem corrected. (MCLADW sec. 7.2.5 & 7.2.8 & App. H sec. 2.5.4)

8.1.2.3 The sample value is not corrected for the method blank value.

8.1.2.4 Data for blanks including corrective actions must be recorded directly in the analysis log.

8.2 Duplicate Samples

8.2.1. Testing of duplicate samples provides information on testing precision and homogeneity of the sample. A field duplicate sample is a sample collected, homogenized, and split into two identical aliquots upon collection in the field, prior to receipt by the laboratory. Field duplicates are treated and processed as independent samples by the laboratory, and are considered ‘blind’ duplicates if the laboratory is not aware which sample(s) has been duplicated. For the purposes of internal laboratory performance, duplicate samples may be replicate aliquots of one sample, processed and analyzed in the same batch.

8.2.2 Each analytical batch requires one duplicate sample test per testing run at a minimum of 10% of samples tested. (MCLADW App. H sec. 2.3.1 pg. H-5)

8.2.3 Precision of testing is evaluated by calculating Relative Percent Difference (RPD) with duplicate testing results. The RPD is calculated as follows:

RPD = [(S - D) / ((S + D) /2)] X 100

Where S is the sample value and D is the duplicate value.

8.2.4 A control limit of +/-10% RPD is used for sample value greater than 5 times the MDL, and +/-MDL for less values less than 5 times the MDL.

Duplicate sample data with a value(s) outside the control limits is either flagged with a "d" for the analyte or otherwise annotated in the laboratory report as such.

8.3 Spiked Samples

8.3.1 The objective of testing spiked samples (a Laboratory Fortified Sample Matrix) is to determine the extent of interferences by evaluating the percent recovery of a known amount of added analyte.

8.3.2 The amount of analyte added to the sample should result in a concentration approximately mid-point in the calibration range.

8.3.3 At least one spike per analyte is required per batch of a similar matrix type or at a frequency of one spike per ten samples, whichever is greater. (MCLADW sec. 7.2.6 pg. IV-5)

8.3.4 The percent recovery (%R) of the spike is calculated as follows:

%R = [(SSR - SR) / SA] X 100

Where SSR is the spiked sample result, SR is the sample result, and SA is the spike added. When the sample concentration is less than the detection limit, SR equals zero for purposes of calculating percent recovery.

8.3.5 If the spike recovery data is outside the control limits specified in Sec. 8.4.3, and the test performance is in control, (see next section) the report for this matrix must be flagged to suggest possible matrix interference.

8.4 Quality Control Standards (Laboratory Fortified Blanks)

8.4.1 (See Sections 4.3 and 4.4 Initial and Continuing Calibration Verification) Reference standards are used to insure that instrumentation is properly calibrated in regard to accuracy. The matrix of the reference standard conforms to the type of sample and standard being analyzed, whenever possible.

8.4.1.1 The tested value of the quality control standard must be determined by the same method as the samples.

8.4.1.2 The percent recovery of quality control standards is calculated by: % Recovery = (Observed Value/Certified Value) X 100

8.4.2 Frequency: At least one quality control standard (Lab Fortified Blank) must be performed per batch of a similar matrix type or a frequency of one quality control standard per ten samples, whichever is greater. (MCLADW sec. 7.2.12 pg IV-7) (Chap 263 pg. 20)

8.4.2.1 Aqueous control standards must be certified from their source for a certain value, or may be produced from ACS grade source chemical.

8.4.3 Data for quality control standards should fall between the control limits specified for each analyte. Control charts are plotted with warning (2 X standard deviation) and control (3 X standard deviation) limits. If a quality control standard test result is above or below the applicable limit, all analysis of samples associated with the analytical batch must be repeated.

8.4.4 Data for quality control standards must be recorded directly on the laboratory analysis report pages.

9.0 MICROBIOLOGICAL (MICRO) QC PROCEDURES

9.1 Equipment and Materials

9.1.1 Platinum or Nickel needles or loops are used to inoculate media.

9.1.2 Clear plastic funnels are used to measure water volumes tested in the membrane filtration procedure. The accuracy of the graduations is checked initially with a standard graduated cylinder, and the results (acceptable within 2.5%+or-) are recorded in the micro QC logbook. Funnels are re-calibrated (marked at the 100 mL level if received beyond the 2.5% tolerance.

9.1.3 A glassware inhibitory residue test (Standard Methods 9020B) is performed initially, and each time a alternative washing compound or procedure is used. (MCLADW sec. V pg. 7)

9.1.4 Filter funnels and bacteriological sampling containers are spot checked annually for pH reaction (Standard Methods 9020B) to ensure that labware is at a non-toxic pH value.

9.1.5 Lot numbers and expiration dates for Colisure Media and Sterile Bottles are logged in the micro QC logbook with receipt date. The pH of each lot of media is verified to ensure use within method specifications and recorded in the micro QC logbook.

9.1.6 For sterility purposes, disposable plastic culture dishes are used for micro incubation, and opened packages of dishes are sealed between uses.

9.1.7 Commercially prepared culture tubes with media used for Coliform confirmation testing are made of borosilicate glass and have screw caps with non-toxic liners.

9.5 Colisure ® method QC Procedures

9.5.1. Each lot of media is tested before compliance Total Coliform testing with species specific positive and negative culture control tests. Results are recorded in the micro QC logbook. (MCLADW sec. V pg. 8) Refer to S.O.P.

9.5.2. Each lot of media is checked for auto-fluorescence using a 366nm UV Light and recorded in the Q.C. logbook

9.5.3. Each lot of sterile bacteria test bottles is checked for auto- fluorescence using a 366nm UV light and recorded in the Q.C. logbook

10.0 ACTION RESPONSE TO LABORATORY RESULTS

10.1 In order to comply with provisions of the Total Coliform Rule, the KWD laboratory tests all total coliform-positive cultures for the presence of Escherica Coliform bacteria.

11.0 RECORD RETENTION & STORAGE

11.1 Analytical records from compliance sample testing (including raw data, calculations, and quality control data) are retained at the KWD Filtration Plant office for a period of ten years.

11.2 Analytical records for the past five years are stored in easily retrieved format for certification review.

Kennebec Water District - Laboratory Quality Assurance Plan APPENDIX A

STANDARD OPERATING PROCEDURES Kennebec Water District - Laboratory Quality Assurance Plan APPENDIX B

PREVENTATIVE MAINTENANCE SCHEDULES Kennebec Water District - Laboratory Quality Assurance Plan APPENDIX C

QUALITY ASSURANCE FORMS Kennebec Water District - Laboratory Quality Assurance Plan APPENDIX D

TRAINING RECORDS