QUALITY ASSURANCE MANUAL MARION LABORATORY … · The quality assurance (QA) and quality control...

Alloway Document No.: 5001

Revision: 0

Title: Quality Assurance Manual

Revised Date: 2/11/08

Effective Date: 2/11/08

Document Location: shared\lab\adminsops\QAManual_Marion_Feb08.doc of 113 Property of Alloway. Unsigned copies are uncontrolled copies of a time sensitive document and may not be current after 8/26/08.

QUALITY ASSURANCE MANUAL

MARION LABORATORY

Inorganics, Organics, and Microbiology The Alloway Chemistry Quality Assurance Manual is a summary of material available from federal and state agencies and information accumulated and researched by the staff of Alloway during the past twenty years of operation. This manual is designed to outline the routine methods and quality control procedures we utilize to perform analytical determinations in environmental samples and to outline our basic Quality Assurance and Quality Control (QA/QC) Program. This manual provides Alloway personnel and clients with a description of company policy for operating, maintaining, and improving our quality system.

Copyright February 2008, Alloway All rights reserved. No part of this manual may be reproduced or distributed in any form or by any means without the prior written permission of Alloway. The Alloway logo is intended for use by Alloway personnel and may not be used without prior permission from Alloway management.


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1.0 TITLE PAGE

Alloway 1776 Marion-Waldo Road Marion, OH 43302 Phone: (740) 389-5991 Phone: (800) 873-2835 Fax: (740) 389-1481 ________________________________ John R. Hoffman President _____________________________________ Marcy Bolek Vice President Technical Services _____________________________________ Michael J. Herdlick Quality Assurance Officer ______________________________ Todd Brown Laboratory Supervisor ______________________________ Rhonda Morris Laboratory Supervisor 2.0 TABLE OF CONTENTS


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Description/ Page Section Numbers Legal Notice. .............................................................................................1 1. Title Page............................................................................................2 2. Table of Contents ................................................................................3 3. Policies and Objectives................................................................... 4-5 4. Laboratory Organization and Responsibility ............................... 6-10 5. Corrective Actions and Root Cause Analysis ............................. 11-12 6. Quality Assurance Reports to Management ............................... 13-14 7. Quality Document Control.......................................................... 15-17 8. Sample Procurement and Acceptance Policies .......................... 18-25 9. Facilities, Analytical Procedures, Preventative Procedures...... 26-28 10. Laboratory Purchasing Policies and Procedures ..................... 29-30 11. Capital Equipment Expenditures ................................................ 31-32 12. Calibration Procedures and Frequency Checks......................... 33-36 13. Analytical Standards and Traceability of Measurements........... 37-38 14. Data Review, Report Generation, and Recordkeeping............... 39-41 15. Precision and Accuracy Statements............................................ 42-44 16. Performance and System Audits .......................................................45 17. Standard Operating Procedures for Conducting Audits ..................46 18. Statistical Methods...................................................................... 47-49 19. Equations and Definitions .......................................................... 50-57

Appendices 1. Laboratory Equipment List ......................................................... 58-60 2. Laboratory Organizational Chart ............................................. 61-62 3. State Certification Table............................................................. 63-64 4. Internal Audit Checklist .............................................................. 65-97 5. Sample Preservation Table ....................................................... 98-101 6. Example of Quality Control Charts ........................................ 102-103 7. ALLOWAY Sample Request Sheet.......................................... 104-105 8. ALLOWAY Chain of Custody Form..................................... 106-107 9. Data Deliverables Packages................................................... 108-109 10. Laboratory Floor Plan........................................................... 110-111 11. References ............................................................................... 112-113 3.0 POLICIES AND OBJECTIVES


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3.1 Alloway’s goal is to provide the highest quality analytical service to our clients. Our staff, from bench-level analysts/technicians to the President, is committed to operating a quality system which will enhance our client relationships and achieve a positive working environment for our employees. Through the use of this Quality Assurance Program in conjunction with specific methodologies, we strive to deliver a complete quality system from the time a client contacts us for a quotation until the final report is delivered.

3.2 Our commitment is to our clients and to our employees as we constantly strive to provide a valuable

service and maintain a stable source of employment. We, at Alloway, believe that the company has positioned itself to handle the constant changes in the industry as we approach the future.

3.3 This section identifies and describes the organization, objectives, policies and activities of Alloway.

The quality assurance (QA) and quality control (QC) aspects of these laboratory practices are based on the National Environmental Laboratory Accreditation Conference (NELAC) standard (July 2002, effective July 2004 and subsequent standards), the ISO/IEC Guide 17025 Standards, and other regulatory authority documents. In addition, the objectives of Alloway are outlined below.

3.3.1 Determine the accuracy and precision of each analytical method and to document these results on control charts.

3.3.2 Maintain and continuously improve the quality system within all areas of the laboratory. 3.3.3 Demonstrate on-going training of all analysts/technicians through the analysis of Proficiency

Testing Samples and internal blind samples, in addition to conducting internal audits. 3.3.4 Attend various conferences to keep abreast of the regulations at the federal and state levels. 3.3.5 Maintain and improve the quality of data generated in the laboratory. 3.3.6 Maintain and improve recordkeeping, storage and retrieval of data, report writing, and assure

sample integrity. 3.3.7 Maintain controlled documentation of all administrative and technical standard operating

procedures utilized in the laboratory. 3.3.8 Assist the laboratory with any method development. 3.3.9 Ensure that all testing personnel familiarize themselves with the quality documentation as

presented to them by management. 3.3.10 The continued commitment of management to the compliance with the ISO/IEC Guide 17025

Standard through the use of approved test methodologies. 3.3.11 Continued commitment of management to the compliance set forth in the NELAC standards. 3.3.12 Continued commitment of management to the compliance of state and federal regulatory

authority programs.

3.4 INTERNAL LABORATORY OBJECTIVES AND POLICIES

3.4.1 Analyst Pressure Policy 3.4.1.1 If an analyst/technician believes or perceives they are being pressured by a supervisor,

laboratory manager, or administrative personnel to perform their work in a manner that violates either a Standard Operating Procedure, ethics policy, or any other company policy, they may communicate the situation to the next higher level of management up to and including the President or the Quality Assurance Department whichever is more appropriate.

3.4.1.2 If an external source of pressure is perceived by an analyst or employee, then the analyst/employee shall refer the “source of pressure” onto the next level of management up to and including the President or Quality Assurance Department.

3.4.2 Ethics Policy and Data Integrity Agreements

3.4.2.1 The company has established an ethics policy for all analysts involved in the laboratory operations per the guidelines set forth by NELAC and A2LA. The ethics policy is utilized by the management of Alloway to convey the companies' ethical guidelines and expectations for all analysts. The ethics agreement must be signed by each incoming analyst immediately after reading the ethics policy. This document outlines the guidance for analytical decision


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making and ensuring data integrity. The guidelines are intended to assist analysts in generating traceable, legally defensible data, while avoiding making decisions which could be construed as fraudulent use of data. The purpose of the document is also to ensure that all analysts understand that fraudulent practices are not condoned under any circumstances.

3.4.2.2 As part of the new employee's training program, the ethics policy is reviewed with senior management. This policy has been approved by the President of Alloway. The ethical agreements represent the ethics program as part of the overall quality system including, but not limited to, the punishments and penalties for improper, unethical, and illegal actions.

3.4.3 Force Majeure Policy 3.4.3.1 Alloway shall not be responsible or liable for any delay to service if such delay is caused by

any act of God, fire, flood, explosion, war, insurrection, riot, embargo, action, statute, ordinance, regulation or order of any government agency, shortage of labor, material, fuel, supplies or transportation, strike or other labor dispute, or any cause, contingency, or occurrence of any nature, whether or not similar to those herein before specified, beyond the company's control which prevents, hinders, or interferes with the performance of said services.


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4.0 LABORATORY ORGANIZATION AND RESPONSIBILITY

4.1 Alloway operates three analytical laboratories in the United States. This Quality Assurance Manual (QAM) addresses the organization and operations at the Marion Ohio facility. The QAM includes the organics, inorganics, metals and microbiological departments.

4.2 The organizational chart is provided in Appendix 2 of this manual. The technical and

administrative personnel are listed below. The laboratory maintains a staff of approximately twenty individuals. Our employees are trained in a wide variety of disciplines including, but not limited to, the fields of chemistry, biology, business, and mathematics.

4.3 Corporate and Marion Laboratory Responsibility Profile

• John R. Hoffman - President (Deputy: Marcy Bolek) • Marcy Bolek - Vice President Technical Services (Deputy: John Hoffman) • Radek Bolek - Vice President (Deputy: John Hoffman) • Michael J. Herdlick - Quality Assurance Officer (Deputy: Todd Brown) • Ryan Kluth - Technical Director – NELAC (Deputy: Todd Brown) • Todd Brown - Laboratory Supervisor (Deputy: Rhonda Morris) • Rhonda Morris - Laboratory Supervisor (Deputy: Todd Brown) • Kerry Steinberger - Analyst II – Inorganics

4.4 KEY JOB DESCRIPTIONS

4.4.1 The following describes the responsibilities, qualifications and experience requirements for

personnel working at the Marion Laboratory. The company reserves the right to permit exceptions to educational requirements depending on the situation and the experience of an employee.

4.4.1.1 President – Establish direction for the company by developing a strategy and by organizing the company for success. Performs business development plans and provides training to key employees for personnel development. The President delegates responsibility, authority, and accountability for assigned tasks to the management team. Have full responsibility, authority, and accountability for activities within the company, subject to compatibility with the broad policies and objectives of the company. Requirements for this position are decided on a case by case basis by the Board of Directors.

4.4.1.2 Vice President, Technical Services - The Vice President, Technical Services manages plans, organizes, and directs the activities of Alloway’s technical services. He or she establishes priorities for the laboratory in line with the priorities assigned by the President for the company. Has full responsibility for the daily activities associated with the production laboratory including staffing, shipment/receipt of analytical samples, proper sample procurement, verification of equipment operations, review of test data, and generation of final reports. Maintains budgetary control over assigned supervisory units. Oversees capital purchases and outlines protocols for the purchasing procurement of reagents, chemicals, and other supplies used by the laboratory.

4.4.1.2.1 Customer Responsibilities – Provides project management of major projects as deemed necessary to provide support to each laboratory. This includes periodic review of requests, tenders, and contracts from clients. Also responsible for assisting with review of complaints from clients and rectifying technical problems.

4.4.1.2.2 Quality System Responsibilities - Responsible for the laboratory technical compliance of all state regulatory, NELAC, and ISO/IEC 17025 compliance issues. Assists with the implementation and effective management of the quality system. Also assists in


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maintaining the ethics policies and procedures within the laboratory. Helps to ensure that the document control policies are being followed in the laboratory.

4.4.1.2.3 Requirements - This individual shall possess a minimum of a four-year degree from an accredited educational institution in physical, chemical, environmental, biological or engineering science with at least 24 semester hours of college chemistry and at least two years of experience in the analysis of environmental samples for organic and inorganic analytes.

4.4.1.3 Quality Assurance Officer – Reports to the President. The Quality Assurance Officer is responsible to develop, implement and maintain the Quality Assurance System and to be the focal point for resolution of quality issues. He or she maintains the quality assurance manual and controlled documents. He or She monitors quality control activities and informs laboratory management of quality issues. The Quality Assurance Officer assists with the implementation and management of the quality system in conjunction with the Vice President of Operations and is responsible for maintaining certifications, outside audits, and corrective action programs. The QA Officer also performs report review.

4.4.1.3.1 Requirements – This individual shall possess a minimum of a four-year degree in chemistry, engineering, biological sciences or related scientific field that will allow for understanding of activities performed at Alloway.

4.4.1.4 Laboratory Supervisor - Responsible for the day to day direct supervision of specific departments and for secondary review of analytical data. The Laboratory Supervisor is responsible for the oversight of the technical content of the procedures and analytical testing. He or She performs project management duties and prepares and conducts personnel performance evaluations. These individuals shall possess a Bachelor’s Degree in a relevant scientific field or possess an Associate’s Degree with at least two years of analytical experience.

4.4.1.5 Analyst II - This individual reports to the Laboratory Supervisor and performs analyses as assigned including chemical, bacteriological and bioassay. Responsible for daily production of their assigned method(s) as defined in the laboratory documented quality program. He or She is also responsible for completion of quality control assignments and documentation , work independently using laboratory SOP’s, perform data handling, data reduction and calculations, perform equipment maintenance as required or assigned, trouble shoot instrumentation and assist in training and supervision of Analyst I and Laboratory Assistants. An Analyst II must possess a four-year degree in physical, chemical, environmental biological or engineering science and at least 16 hours of college chemistry.

4.4.1.6 Analyst I – This individual reports to the Laboratory Supervisor and performs analyses assigned including chemical, bacteriological and bioassay. This person completes all applicable quality control requirements and documentation, follows SOP’s, prepares solutions and reagents and performs data handling, data reduction and calculations as required. The Analyst I also assists in the preparation of supplies for customers, assists with sample log-in and assists with sampling as needed. An Analyst I must possess a bachelor’s degree in a technical field or a minimum of 6 years experience is required.

4.4.1.7 Laboratory Assistant – This individual reports to the Laboratory Supervisor and works directly with an analyst and assists in preparation of laboratory supplies and equipment. He or She also provides support with field activities and cleans and maintains glassware, composite samplers and other field or laboratory equipment. The requirements for this position a high school diploma or demonstrated work history.

4.4.1.8 Office Manager - This individual performs the daily administrative functions at the laboratory including coordinating reports, answers the telephone and assists customers and routes calls as required. He or She is responsible for making sure that reports go out timely and without typographical errors. The requirement for this position is a high school diploma.


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4.5 LABORATORY PERSONNEL TRAINING POLICES AND PROCEDURES 4.5.1 According to ISO/IEC 17025 Guidelines, NELAC Guidelines, and other regulatory agencies,

the laboratory shall have a policy and procedures for identifying training needs and providing training of personnel. The goal of the policy is to ensure the competence of all who operate specific equipment, perform tests and/or calibrations, evaluate results, and sign off on final reports. Personnel performing specific tasks shall be deemed qualified on the basis of appropriate education, training, experience, and demonstrated skills. The policies and procedures stated here would be applicable for new personnel, current personnel, and contract personnel.

4.5.2 New Personnel-Corporate Documents 4.5.2.1 New laboratory personnel undergo an employee orientation by the management team so that

the employee is familiar with the structure of Alloway. The company maintains a Policy Handbook to facilitate the employee training. The training on this handbook is done by a member of the management team.

4.5.2.2 The new employee is also trained on four other laboratory documents. The Chemical Hygiene Plan, Hazard Communication Manual, and Lockout/Tagout Plan are reviewed to the new employee by the Quality Assurance Officer or by senior level management. At this time, the Ethics Policy is also reviewed with the new employee by senior management. This training shall be accomplished within one month of hiring the new employee.

4.5.3 New Personnel-Laboratory Training 4.5.3.1 Upon hiring, the new employee will be trained by the respective supervisor for those tests,

instruments, and methods that they will be responsible for mastering. The main training document will be the standard operating procedure for a test method. It is the responsibility of the trainer(s) to set up a specific internal schedule for the new employee and keep proper records of the employee's training progress. Copies of the training documents must be routed to the Quality Assurance Officer.

4.5.3.2 With analytical testing, repetition is extremely important for understanding the tests. Supervisors and Analysts work closely with the new employee and will offer guidance for performing analytical testing. Part of the initial training will be to work with a current employee and assist them with their tasks. A new employee will continuously be supervised by the department to monitor their progress. In some cases, an individual may be sent outside of the company to a vendor training class or seminar.

4.5.3.3 The employee will be considered "trained" for a specific test method once the employee has demonstrated competency on the standard operating procedure and sufficient analytical sequences can be generated to produce either an initial demonstration of capability or method detection limit study. Documentation of initial training is completed and forms are given to the QA Department for filing. Information must be presented that the employee has read, understands, and agrees to implement the latest revision of the standard operating procedure. This is normally accomplished with a spreadsheet initialed by the employee.

4.5.3.4 Another training mechanism for a new employee may involve the testing of a proficiency test (PT) sample for a particular analyte. This PT sample will be issued either by the QA Department or the laboratory supervisor. Acceptable scores on a PT sample will not necessarily replace the requirement for conducting a demonstration of capability, but will provide indication on how the employee has progressed with their training program.

4.5.3.5 New employees hired for laboratory positions, but not performing analytical testing, are considered trained for their position after they have completed the necessary training sessions on respective standard operating procedures and have worked with their respective supervisors to the point that constant review of their work is not required. For these employees, training on the standard operating procedures may be accomplished by the supervisor, Quality Assurance Officer or designated representative. All training documents are forwarded to the Quality Assurance Officer for filing.

4.5.4 Current Personnel-Corporate and Laboratory Training


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4.5.4.1 An employee's continued ability to successfully perform various procedures is monitored by the employee's supervisor and management. Personnel training are up to date when the training file includes documentation that the employee has read, understands, and agrees to implement the latest revision of the standard operating procedure. This is normally accomplished with a spreadsheet initialed by the employee.

4.5.4.2 In addition, technical training must be kept current through one of three mechanisms: 4.5.4.2.1 Method Detection Limit Study 4.5.4.2.2 Acceptable Results on a Proficiency Test Sample 4.5.4.2.3 Continued Demonstration of Capability

4.5.4.3 At least one of the above must be completed within the calendar year for each test conducted by the employee to ensure their continued demonstration of success with the methodology. The Quality Assurance Officer and the section supervisors are responsible for completing training documents and ensuring that the training files are kept up to date. Certificates from educational sessions and outside courses and conferences are also placed in the employee training files. Training files for health, safety, ethics, and other miscellaneous programs are also kept for the employee by the President.

4.5.5 Contract Personnel - Contract personnel are normally not hired within the laboratory to perform testing. The laboratory may contract with outside vendors for those tests or programs for which the laboratory does not offer services. In this case, the contractor is not an employee of Alloway.

4.6 CLIENT CONFIDENTIALITY POLICY 4.6.1 The microbiological records must be maintained for five years, lead and copper records must be

maintained for 12 years and all other laboratory data and documents must be maintained for a period of ten years unless a longer term is agreed to by the client and Alloway. This time frame has been established by a variety of regulatory agencies here in Ohio and across the country. All data and documents will be maintained in the laboratory facility for three years. After three years the documents may be moved offsite to a storage location. In the course of everyday business, employees will have access to confidential information about Alloway’s business and about our customers. This information must not be discussed with anyone, either inside or outside of Alloway, except when required in the normal course of business.

4.6.2 Clients who contract services from our organization must be given information only in regard to their respective samples of interest. All chain of custody records, certificates of analysis, electronic media, facsimile transmission and other media must be provided solely to the client of concern and held secure within the laboratory. In addition, phone conversations with clients must strictly be in relation to their respective samples and not to any other samples or projects within the laboratory. Any undue pressure placed upon customer service agents, marketing staff or analysts/assistants, for release of confidential information, must be reported to the management of Alloway.

4.6.3 It is important to note, however, that state and federal authorities, such as the EPA, do have the right to request information concerning clients when the information is for public documentation and record. This type of information is generally transmitted via the respective state reporting form(s). In addition, when an on-site audit is conducted by a regulator, it is the policy of the laboratory for the audit team to review the raw data and documents on-site during the audit. The laboratory may also grant the auditors the right to copy records to be reviewed off site should the need arise. Additional information may also need to be transmitted to the auditors via facsimile or email regarding their respective audit. Depending on the audit proceedings, the laboratory would except that client confidentiality would be respected by the auditors.

4.6.4 The Vice President, Technical Services, the Quality Assurance Officer, or the President must be consulted before releasing any information to the EPA or other third parties. Unless specifically directed by these individuals, personnel are to release information only to the designated clients.


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4.6.5 Client information can only be released to other parties if there is written documentation from the original client and a clear understanding of who is requesting the material and the purpose for the request.

4.6.6 It is the policy of the laboratory to ensure that all documents which are faxed, emailed, written, or even verbally conversed concerning data is intended only for the personal and confidential use of the recipient named.

4.7 ACCREDITATION LOGO AND NAME POLICY

4.7.1 According to ISO/IEC Guide 17025 and the NELAC standards, the laboratory must develop a

policy and procedure for controlling the term “NELAC Accredited." It is the responsibility of the laboratory to communicate the policies and for corporate personnel to ensure that all requirements are met.

4.7.2 Logo Reproduction-Certificates of Analysis - Because the NELAC accreditation is extensive and encompasses various matrices and analytical programs, the laboratory policy does not include a statement on the Certificate of Analysis. The laboratory may reference on the Certificate of Analysis the actual laboratory accreditation number for specific national and state accreditations.

4.8 SUBCONTRACTED TESTS

4.8.1 Should the laboratory be required to subcontract analytical tests to other laboratories due to a

capacity or certification issue, then the contract laboratory's Certificate of Analysis must accompany the original request for analytical services. This ensures that proper credit is granted to the laboratory that performed the actual analytical testing. It is expected that the contract laboratory will provide similar accreditation information on their respective analytical reports.

4.9 CALIBRATION LABELS

4.9.1 Calibration labels containing “NELAC Accredited" is not affixed to equipment that has been

calibrated by an accredited laboratory.

4.10 ADVERTISING AND BUSINESS SOLICITATION

4.10.1 According to the standards, the laboratory may incorporate statements concerning their respective accreditation in publicity and/or advertising materials including brochures, technical literature, business reports, web sites, and quotations or proposals for work. The use of NELAC accreditation information enhances the reputation and value of accreditation for all stakeholders. Thus it is the policy of the laboratory to utilize statements regarding the accreditation of the laboratory through technical literature, facsimiles, web sites, and internet electronic mails. The statements must be accurate and reflective of the laboratory's capabilities and accreditations. For those accrediting authorities that certify the laboratory for numerous parameters, it is the policy of the laboratory to note a blanket certification number or individual state name.


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5.0 CORRECTIVE ACTIONS and ROOT CAUSE ANALYSIS

5.1 The Corrective Action Program is a key element to the quality assurance program at Alloway. Problems, concerns, and recommended operational improvements encountered during operations are documented through the use of corrective action forms. These types of problems are identified and corrected by the appropriate personnel and properly documented. Any problems requiring the attention of the appropriate supervisor or management are corrected in a timely fashion and followed up to ensure the corrective action is effective. The main purpose of the corrective action program is to assess, correct, and prevent situations from occurring by conducting root cause investigation.

5.2 ROOT CAUSE ANALYSIS PROCEDURE

5.2.1 Identify the individuals responsible for assessing each data type. This may include conducting interviews with employees involved with the work;

5.2.2 Identify the individuals responsible for initiating the corrective actions; 5.2.3 Specify the problem, which includes checking log in records, technical procedures, validation of

records, and critical review of the quality control associated with the analytical run. Review all raw data carefully for any transcription or transposition errors. Recheck calculations if necessary.

5.2.4 Perform the corrective action; and 5.2.5 Review the corrective action reports

5.3 The corrective action form is initiated by anyone identifying a deviation from an SOP, sample

handling issue, or unacceptable quality control check. Unacceptable quality control checks would include such examples as a contaminated method blank with results that cannot be qualified, a laboratory control standard with biased low results, or a continuing calibration check with a low bias. Each technical SOP will contain specific language that outlines when samples are to be re-extracted, re-analyzed, or qualified. Situations may vary due to holding time restrictions, volume of sample submitted to the laboratory, or complications with the sample matrix.

5.4 The statement of the problem, date, and person initiating the form is completed. If the projected

completion date and person to be assigned the responsibility for implementing corrective action is known, these items are completed.

5.5 The corrective action procedure may also be utilized for internal audit findings that cast doubt

regarding the validity of test results. Depending upon the investigation, clients may need to be notified regarding these test results. This may require re-issuing Certificates of Analysis, case narratives being written for a project, or additional quality control reports issued to clients. In addition, it is the policy of the laboratory to inform the specific clients either by verbal communication or through a case narrative report when problems are discovered from internal audit concerns or even external audit situations. The Quality Assurance Officer should verify implementation by reviewing the item and ensuring implementation remains in effect. The Quality Assurance Officer signs and dates that the verification is complete.


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5.6 POLICY REGARDING COMPLAINTS

5.6.1 A key part of the Corrective Action Program involves the handling of complaints received from clients or other individuals. Although minor complaints can be rectified quickly and effectively, there are times when situations occur that merit a deeper investigation. The complaints from clients must be rectified through one of three vehicles:

5.6.1.1 Completion of a corrective action form and/or 5.6.1.2 Completion of a complaint form and/or 5.6.1.3 Case narrative and/or footnotes to Certificate of Analysis

5.6.2 A complaint is defined as an external concern issued by another party regarding an event that occurred in the laboratory. Complaints might not be in writing but should be made record by the laboratory. It is important that a complaint which merits investigation by the laboratory be fully documented as part of a root cause investigation. Again, numerous departments within the laboratory may be involved rectifying a complaint.

5.6.3 Any individual employed by the laboratory may take a complaint and may rectify it, but for those complaints that require additional assistance, involve monetary situations, or other management issues, these complaints must be referred to the next level of management.

5.6.4 Finally, part of the complaint investigation will include a brief or possibly extensive audit by a supervisor or member of management. This audit is made part of the corrective action process and is documented as such. It must not replace the separate external audits as noted in the QAM.

5.7 NONCONFORMANCE TESTING PROCEDURES

5.7.1 According to ISO/IEC Guide 17025 and the NELAC standards, the laboratory shall have a policy for control of nonconforming testing. Nonconforming work is defined to be that laboratory testing which does not conform to the standard operating procedures of the laboratory or procedures agreed to by the client.

5.7.2 Specific situations that would be considered as nonconforming testing may include deviation from internal standard operating procedures, method deviations, or client specific requests for internal projects. These deviations could be caused by instrument problems, force majure situations, or calibration reagents and standards that are outside of specifications from the manufacturer. It is the responsibility of the Vice President; Technical Services or designated authority to determine if nonconforming work can be deemed acceptable even after an evaluation of the significance of the nonconforming work has been completed. Clients may need to be contacted by the Vice President, Technical Services or designated authority to determine whether data would need to be qualified or resamples collected.

5.7.3 A root cause investigation may have to be initiated that involves analysts, vendors, instrument manufacturers, or other agencies. As part of the root cause investigation, a corrective action form must be implemented and completed to ensure that root cause investigation is completed.

5.7.4 It is the responsibility of the Quality Assurance Officer and supervisor of the department to determine when the analytical work can be resumed. This resumption of work may only occur once the proper instrument checks, verifications, or quality control samples are deemed acceptable. If it is possible that a nonconformance situation would recur, then the corrective action procedures must be initiated and completed as noted in the above statements.


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6.0 QUALITY ASSURANCE REPORTS TO MANAGEMENT

6.1 The Quality Assurance Department is operated under the Quality Assurance Officer who reports directly to the President. Listed below are example reports that are discussed with senior management regarding the quality assurance program in the laboratory.

6.1.1 Copies of all correspondence relating to laboratory certification or accreditation, 6.1.2 Summary of Corrective Action Reports, 6.1.3 Suggestions for quality program improvements including recommendations for purchase of new

equipment, 6.1.4 Recommendations and status of training of laboratory personnel, 6.1.5 Quality Control items such as control charts or control limits for trends or repeat problems, 6.1.6 Document changes in quality assurance procedures requested by various clients, 6.1.7 Reports on any unusual laboratory events or out of control situations, 6.1.8 Internal audit reports,

6.1.8.1 Audit reports from external sources, or 6.1.8.2 Proficiency Testing Results

MANAGEMENT REVIEW / INTERNAL AUDIT

6.1.9 As required by various state and national accrediting agencies including NELAC and ISO Guide 17025, a Management Review is held annually to review the quality assurance program of the laboratory. The quality system must be evaluated at least annually by the management to ensure its continuing suitability and effectiveness and to introduce any necessary changes or improvements. The Quality Assurance Officer meets with the technical personnel at various times throughout the year. The topics that are discussed include on-site audits, updates to standard operating procedures, method detection limit studies and state certification and accreditation status.

6.2 STANDARD OPERATING PROCEDURE FOR CONDUCTING MANAGEMENT REVIEW

6.2.1 Review of the laboratory is done at least annually by one or more of the following staff members: President of Alloway, Vice President of Technical Services, Quality Assurance Officers, Laboratory Supervisors, and any additional personnel.

6.2.2 Management review will be conducted by the Laboratory Supervisor or designated representative

6.2.3 Tentative agenda will be as follows: 6.2.3.1 Review matters from the previous management review 6.2.3.2 Review reports from third party assessments and other external audits 6.2.3.3 Review the suitability of policies and procedures for the laboratory 6.2.3.4 Review audit reports from clients and other client feedback 6.2.3.5 Review results from internal audits 6.2.3.6 Review results from proficiency testing 6.2.3.7 Review results from in-house quality control checks 6.2.3.8 Review any complaints from clients or personnel 6.2.3.9 Review staff training, equipment, and facility resources 6.2.3.10 Review future plans 6.2.3.11 Review changes in volume and type of work 6.2.3.12 Review corrective and preventative actions

6.2.4 Open discussion of requirements and findings 6.2.5 Close meeting 6.2.6 Document minutes 6.2.7 Implement all necessary changes and recommendations through the use of corrective action

forms.


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7.0 QUALITY DOCUMENT CONTROL

7.1 STANDARD OPERATING PROCEDURES

7.1.1 The purpose of the Standard Operating Procedures (SOPs) is to specifically detail a particular methodology utilized in the laboratory and to prevent any deviations from agreed upon procedures. SOPs are considered either technical or administrative. The administrative SOPs are written to encompass more specific operational functions. The cover sheet of the SOP includes management authorization and the date of implementation of the standard operating procedure. QA will transfer the approved copy to the read only file of the computer network for use in the laboratory. This is the only method of distribution to the laboratory. Any copies printed from this file will indicate that the document may not be current as of the date of printing. The weekly meeting will be used to inform the staff when a new SOP or revision is issued. Employees must check their laboratory department’s controlled copy to ensure that the updated copy is in use. The SOPs are available in electronic form via the read-only directory of the Alloway - Marion server. When SOPs are updated or revised, there may be certain state or regulatory agencies that will require a review of the document before it is implemented as final in the laboratory.

7.2 QUALITY ASSURANCE MANUALS

7.2.1 The Quality Assurance Manual (QAM) is reviewed and updated at least annually. This Manual is the basis for the overall quality system instituted by the laboratory. The QAM is a controlled document. The QAM is available in electronic form via the read-only directory of the Alloway-Marion server. When the QAM is updated or revised, there may be certain state or regulatory agencies that will require a review of the document before it is implemented as final in the laboratory. The complete listing of technical and administrative SOPs is available via the read-only directory of the ALLOWAY-Marion server.


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7.3 NON-STANDARD TESTING and DEPARTURES FROM STANDARD SPECIFICATIONS

7.3.1 If a client desires to employ a test methodology that our laboratory does not normally operate, start-up quality control information must be documented before any samples are analyzed. The start-up quality control that must be accomplished includes a Method Detection Limit Study, a Demonstration of Capability, and the generation of an acceptable calibration curve. A technical SOP must also be written to detail the analytical procedures. There may be occasions when the above documentation could not be generated within a suitable time frame, however, a client's project may dictate that the work is more qualitative in nature and not quantitative.

7.3.2 There may also be situations when the laboratory will have to analyze samples according to a departure from standard specifications. It is the policy of the laboratory for either the laboratory supervisor or designated representative to approve departures from standard operating procedures on a case by case basis. Some examples for departures include: analyzing samples outside of recommended holding times, special preparatory measures for samples, or a deterministic change due to the nature of a particular sample. All information for departures from standard operating procedures must be clearly documented on a Certificate of Analysis or through a separate case narrative.


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7.4 REMOVAL OF DOCUMENTS and REVISION HISTORY

7.4.1 All invalid or obsolete documents are promptly removed from the read only directory on the Alloway server to prevent unintended use. The original signed document is retained for legal or knowledge preservation purposes by the Quality Assurance Department for the minimum time period as documented in section 4.6. These obsolete documents are stamped with the statement "Document Obsolete." A revision history is kept by the Quality Assurance Department for all standard operating procedures that describes new or altered text within the document.

7.5 POLICIES REGARDING NEW WORK

7.5.1 Both ISO Guide 17025 and the NELAC standards state that arrangements must be made for ensuring that the laboratory reviews all new work to ensure that it has the appropriate facilities and resources before commencing such work. This procedure is outlined below and is policy for the laboratory. Please note that new work is defined to be special projects that are above and beyond the normal routine number of samples that arrive in the laboratory.

7.5.2 Review of new work is a continuous process that is carried out by a number of individuals. When a client approaches the laboratory with analytical work the following steps are normally taken to ensure that capacity can be met, turnaround time is obtained, pricing is reasonable, and equipment is functioning properly.

7.5.2.1 Client calls, emails, or faxes Alloway concerning a new project. Call is taken in house by Customer Service, Marketing, or Lab Staff.

7.5.2.2 The individual who spoke with the client must convey the necessary information to either the laboratory supervisor or their respective designate for consideration.

7.5.2.3 It is the responsibility of the laboratory staff to evaluate the project scope including equipment concerns, personnel conflicts, and/or method limitations.

7.5.2.4 If a project cannot be initiated, this information is explained to the client and the reasons for the rejection of analytical work. In some instances, the work may be subcontracted to another laboratory or portions of the work subcontracted to another facility.

7.5.2.5 If the project is acceptable to the laboratory staff, the client is notified of the laboratory's status concerning the project. Guidelines are then established for the project in conjunction with the client such as sample pick-up points, final number of samples, etc.

7.5.2.6 Samples are brought to the laboratory and analyzed according to project specifications and method requirements. Any problems associated with the samples should be conveyed to the client.

7.5.2.7 All analytical data is generated by the laboratory and Certificates of Analysis are issued to the client. Specific quality control reports may be required for the project.

7.5.2.8 Extracts and the physical samples are normally retained by the laboratory for at least 30 days after the testing is completed.

7.5.3 It is important to remember that sample capacity, personnel, and equipment through-put are reviewed constantly within the laboratory to ensure that the laboratory is operating efficiently. The laboratory supervisor meets regularly with their staff in order to have current information regarding samples, turnaround time, and instrument problems.

7.5.4 The Quality Assurance Officer and designated project managers may also offer opinions and guidelines on certain projects if there are questions regarding methodologies, detection limits, or certification issues.

7.6 REVIEW OF REQUESTS, TENDERS, AND CONTRACTS

7.6.1 The review of requests, tenders, and contracts for the laboratory involves a number of departments due to the nature and complexity of specific materials. According to the ISO Guide 17025 and the NELAC requirements, the laboratory should periodically review all contracts according to the following procedures that have been made policy for the laboratory.

7.6.2 Quotation for Analytical Services


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7.6.2.1 Majority of laboratory-client contracts are handled with a formal quotation for analytical services.

7.6.2.2 Quotations are normally valid for one-year, however, the quote may be extended with a renewal through a purchase order.

7.6.2.3 Quotations are reviewed periodically by customer service and senior level management regarding updates to scope of testing, pricing, or methods.

7.6.3 Client Contracts 7.6.3.1 In certain cases, the client may actually require the laboratory to complete a contract

agreement either as a blanket purchase order or as a specific project contract. 7.6.3.2 These contracts are reviewed by the customer service manager, senior management, and

possibly the President of Alloway. 7.6.3.3 If these contracts require signatures, only an officer of Alloway is authorized to be the

signatory. 7.6.4 Comments

7.6.4.1 Analytical contracts or quotations must be acceptable to both client and laboratory personnel. Any significant deviation from the contract by either party should be properly and immediately addressed with Alloway. This would include situations such as change of analytical scope, duration of a project, rental of equipment, or personnel modifications.

7.6.4.2 Due to the nature of environmental testing, it can be expected that certain minor deviations to a quote or contract may occur. This would include such items as the total number of samples and the specific sample matrix.

7.6.4.3 Contracts are reviewed by the laboratory by supervisory staff that will evaluate the incoming work and assign specific analysts, methods, or instruments for particular samples. For review of routine and repetitive samples, the date and initials of the person in the laboratory responsible for carrying out the work is sufficient. For new, complex, and advanced environmental testing, additional review may need to be obtained before the samples are accepted.


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8.0 SAMPLE PROCUREMENT and ACCEPTANCE POLICIES

8.1 This section describes the procedures for collecting and handling samples in the field and the specific sample acceptance policies set forth by the laboratory. The majority of the samples received at Alloway are collected by our clients and shipped via courier or delivered to the laboratory by the client. Because proper sampling techniques are required for the validity of any test, sampling is the most important process in the measurement. It is the responsibility of the client (if client is performing the sample collection) to ensure that the proper sample amounts are provided for the requested analyses.

8.2 The main objective is to collect a small representative sample from an area so that the sample is

transported and subsequently analyzed at the laboratory. Specific sampling protocols and directions are available from the laboratory. Strict adherence must be followed to ensure that all protocols are met for proper sample collection. Once the laboratory receives the samples, all documentation such as facsimiles, memorandums, electronic mail orders, and other communications must be retained by the laboratory as part of the project.

8.3 SAMPLE PRESERVATION REQUIREMENTS

8.3.1 Appendix 5 is provided in a table to summarize the preservation requirements for the methods utilized by the laboratory. The parameters of interest, method reference, minimum sample amount, container, preservation documentation, and holding time information is referenced. Any deviation from this information must be documented by the client and approved by the laboratory representative. All information regarding the sample acceptance deviation is noted on the Chain of Custody.

8.4 PROCEDURE FOR COLLECTING SAMPLES IN THE FIELD

8.4.1 The client must determine the environmental analyses to be accomplished by the laboratory via the scope of the given project.

8.4.2 The client must obtain proper sampling containers from Alloway personnel at the laboratory via direct contact or by courier.

8.4.3 Before taking samples, complete all paperwork and request forms in indelible ink while in the field. Note the time and date the sample was taken.

8.4.3.1 If the samples are a “rush,” check with Laboratory Supervisor to ensure timely completion. Mark the samples “rush” including the date results are needed on the paperwork.

8.4.4 Sampling procedures are identified on the submitted paperwork when required by the client. (Note that proper field records such as temperature, conductivity, free residual chlorine and pH must be analyzed for appropriate sites. These short holding time parameters are the responsibility of the client if the client collects the samples in the field)

8.4.5 For samples which require thermal preservation, the temperature of the container upon receipt at the laboratory is checked. The criteria are either within 2°C of the required temperature or from just above freezing to +2º of the specified temperature. (See exception below). Clients are immediately notified when received samples do not meet the criteria. Affected results are identified by footnoting the Certificate of Analysis.

8.4.6 For samples that are hand delivered to the laboratory, samples are deemed acceptable for receipt if the chilling process has begun and the samples were collected on the same day. The temperature acceptance criteria are waived for these samples. This information must be noted on the chain of custody and other corresponding documentation.

8.4.7 Samples for chemical testing performed by the Marion Laboratory require the following preservation handling

8.4.7.1 Inorganics 8.4.7.1.1 For aqueous samples, fill containers approximately 90 percent full. This provides enough

sample volume for sample mixing and ensures preservatives (if any) are not removed


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during the filling process. The majority of the sample containers are amber liter bottles with Teflon™ lined caps that are pre-preserved with sulfuric acid, sodium hydroxide, or no preservative.

8.4.7.1.2 For soil samples, completely fill the 4 ounce or 8 ounce glass jars. Majority of the samples do not arrive chilled for inorganic parameters however, samples must be stored under thermal preservation. When samples arrive in containers and coolers, it is necessary to ensure that the thermal preservation is documented on the chain of custody.

8.4.7.2 Organics 8.4.7.2.1 For aqueous samples, fill containers completely full for amber quarts and with no

headspace for the measurement of volatile organic compounds. For the 40 mL vials used to collect volatile organic compounds, ensure that no headspace or air bubbles are present in the vials. When samples arrive in the containers and coolers, it is necessary to ensure that the thermal preservation is documented on the chain of custody. For non-aqueous samples, it is recommended that the samples be collected in 4 or 8 ounce glass jars.

8.4.7.3 Metals 8.4.7.3.1 For aqueous samples, fill containers approximately 90 percent full. Do not overfill the

container as nitric acid has been added to the containers. For soil samples, fill containers full in a 4 ounce or 8 ounce glass jar. Aqueous samples to be analyzed for metals do not require thermal preservation and are thus stored at room temperature in the laboratory. Soil samples are maintained under thermal preservation. If the samples do arrive with thermal preservation, then the samples are still considered acceptable for preparation and subsequent analysis.

8.4.7.4 TOX and TOC 8.4.7.4.1 For aqueous samples, fill containers completely full with no headspace. Do not overfill

the container as sulfuric acid has been added to the containers. Samples for TOX are analyzed in the Alloway Lima facility. For TOC soil samples, fill containers full in a 4 ounce or 8 ounce glass jar. Samples must be stored under thermal preservation.

8.4.7.5 Coliform Bacteria 8.4.7.5.1 Samples collected for the analysis of coliform bacteria are analyzed in Alloway Marion

or Alloway Lima. According to the guidelines set forth by the Ohio EPA, it is not necessary that these samples meet any thermal preservation requirement. Samples for testing performed by other Alloway laboratories or subcontract laboratories require preservation, containers and holding times as specified by the designated laboratory quality program. The laboratory assists the client with these preservation, containers and holding time requirements. The individual receiving the samples checks these items upon receipt.

8.5 SAMPLE COLLECTION POLICIES

8.5.1 Grab Sample Policies 8.5.1.2 Grab samples represent the majority of all environmental samples. A grab sample is the

collection of a sample that is a representative aliquot from one specific site location. 8.5.2 Composite Sample Policies

8.5.2.1 Sample compositing is done in the laboratory or field for a variety of matrices. Laboratory compositing is performed only at the client request. The compositing follows the client instructions for sample composition. Depending upon the scope of the project, other samples are composited in the field. Under the Safe Drinking Water Act, up to five drinking water samples may be composited in the laboratory for analysis. Please contact the laboratory for questions regarding composite samples for those states with specific procedures.


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8.6 SUBSAMPLE POLICIES

8.61 A sub-sample is defined to be an aliquot of the sample matrix itself that is utilized for preparation, extraction, or analysis procedures. Each of the technical SOPs details the amount of a sample that must be utilized for a given test. The situation can vary per matrix and container received by the laboratory, but in general, the sample container is obtained by the analyst and an aliquot removed by either pipette, solid extractor, or poured off into a specific sample container. The remainder of the sample is returned to storage for future utilization. Unless otherwise directed by the client or regulatory authority, the laboratory will attempt to subsample a homogenous aliquot of the sample for process. Listed below are the respective procedures per the individual matrices:

8.6.1.2 Drinking Water-for preserved and non-preserved samples, remove a prescribed aliquot

with either a pipettor or by pouring off a specified amount into a test vessel. 8.6.1.3 Non-Potable Water-for preserved and non-preserved samples, remove a prescribed

aliquot with either a pipettor or by pouring off a specified amount into a test vessel. 8.6.1.4 Solid Material-remove a prescribed aliquot with a disposable solid extractor such as a

wooden depressor or plastic pipettor. This solid material would include soils, sediments, sludges, and other matrices with >15% settleable solids.

8.6.1.5 Oil Material-remove a prescribed aliquot with a disposable plastic pipettor or by pouring off a specified amount into a test vessel.

8.6.1.6 Chemical Waste-a product or by-product of an industrial process of which a prescribed aliquot is removed with a disposable plastic pipettor or with a wooden depressor.

8.6.2 Specific sub-sampling glassware is subject to specific laboratory prescribed cleaning procedures whereas the disposable sampling tools are only for one time use and are then discarded. As per the individual technical SOPs, the subsample would then be carried through the standard preparatory and/or analytical procedures for determinative results.

8.7 PROCEDURE FOR SAMPLE HANDLING IN THE LABORATORY (Includes Procedures for Rejecting Analytical Samples)

8.7.1 The following information will serve as acceptance/rejection procedures for analytical samples.

This includes samples for compliance purposes such as from regulated waste water permittees and Public Water Suppliers.

8.7.1.2 Sample Identification - Sample information identified on the sample tags and Chains of Custody include:

8.7.1.2.1 The sample matrix such as drinking water, sludge, etc. 8.7.1.2.2 The name of the client and sample collector 8.7.1.2.3 When the sample was collected (date and time) and the collector information 8.7.1.2.4 Parameters to be analyzed 8.7.1.2.5 A completed Chain of Custody contains all information needed to inform the

laboratory of the requested analyses. 8.7.1.2.6 Samples that arrive in the laboratory are checked by the Sample Custodian to ensure

samples have been properly collected and preserved, and the proper paperwork accompanies each sample. All notations and records must be made in indelible ink where appropriate. The temperature of the sample container is checked with an infrared thermometer and the result is noted on the Chain of Custody. When samples are deemed acceptable to the custodian, the chain of custody or other paperwork is denoted as "samples accepted" with initials and date of login.

8.7.1.2.7 Samples arrive from a variety of clients using a variety of sample submittal forms. All forms accompanying such samples are filed with the client’s file and attached to the file copy of the laboratory reports. Upon completion of the project, the laboratory staff determines the disposition of additional documents or items used for sample


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identification. The original Chain of Custody is returned to the client with the report of the analyses performed. A duplicate copy is attached to the laboratory copy of the analysis report and kept in laboratory files.

8.7.1.3 Sample Preservation - Samples for the Marion laboratory must be evaluated to determine the proper preservatives required for each sample by the Sample Custodian per the sample log-in procedures.

8.7.1.3.1 The pH of all preserved samples, except for those for analysis of volatile compounds, is checked using pH indicator paper. The temperature of all coolers containing samples is monitored upon arrival in the laboratory using an infrared thermometer or a temperature blank. The laboratory records the temperature upon receipt or indicates that the cooling process has begun for samples collected on the same day as receipt.

8.7.1.3.2 If samples are not preserved correctly in the field, then the client must be contacted to discuss options for analysis and sample acceptance. All samples that arrive in the laboratory including samples broken in shipment shall be given a unique laboratory numbers and logged into the LIMS. The client shall be contacted about the breakage of the samples so that it can be determined if re-sampling is required.

8.7.1.4 Sample Receipt Log- LIMS - All sample documentation received in the laboratory is retained by the laboratory in log books. Each sample is assigned a unique laboratory number based on year and sample number. Information retained on these chain of custodies or other legal documentation includes the following:

8.7.1.4.1 Client name and number 8.7.1.4.2 Unique sample identification 8.7.1.4.3 Analyses to be performed 8.7.1.4.4 Date and time sampled 8.7.1.4.5 Date received at the laboratory 8.7.1.4.6 Purchase order number (if known) 8.7.1.4.7 Geographic location of sample (if known) 8.7.1.4.8 Temperature of the cooler or other container 8.7.1.4.9 pH, if preserved with acid or base, and presence or absence of chlorine if necessary 8.7.1.4.10 Matrix 8.7.1.4.11 Relinquish and Receipt signatures 8.7.1.4.12 The laboratory number assigned to the sample is marked on the sample container(s)

with indelible ink. For those sample points requiring multiple containers, the chain of custody and respective container must be marked with an alphabetical system in order to preserve the uniqueness of a container for an individual method. For those samples that must be subcontracted to an outside facility, the laboratory must advise the client and note all relevant information on the Chain of Custody.

8.7.1.4.13 After the paperwork is completed at login, someone other than the person who logged in the sample will review the documentation for completeness

8.7.1.4.14 An analyst logs the following information about each sample into the Laboratory Information Management (LIM) system:

8.7.1.4.15 Date and time the sample was collected 8.7.1.4.16 Location of the sample 8.7.1.4.17 Name of the sample collector 8.7.1.4.18 Client’s name, address, client number and purchase order number 8.7.1.4.19 Information about sample matrix 8.7.1.4.20 Analyses to be performed 8.7.1.4.21 Where to send the report and the invoice 8.7.1.4.22 Any additional information (for example, if the sample is rush) 8.7.1.4.23 The analyst utilizes the LIM system to determine which samples receive which tests

through backlog reports. The analyst then must physically go to the receiving department to locate the particular samples of interest. There is no internal chain of custody or sign out sheet procedure.


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8.7.1.5 Sample Storage - After the sample information is recorded and samples are divided or preserved, the sample or portions of the sample are distributed for analysis. The Analyst places samples requiring thermal preservation for storage in a secure slightly above freezing to 8ºC room. Samples to be analyzed for volatile organic compounds are stored in a separate refrigerator to prevent any cross-contamination. Samples are kept in the appropriate secure rooms until all analyses are complete. Samples are stored for a short period after the analyses are complete in case of a request for re-analysis or additional analysis.

8.7.1.5.1 Sample fractions, extracts, leachates, and other sampling preparatory products shall also be stored at slightly above freezing to 8 oC. Samples and their derivatives should be stored away from all standards, reagents, food, and other potentially contaminating sources.

8.7.1.6 Sample Tracking - A list of analyses to be performed daily is prepared from the LIMS through backlog reports. These backlog reports are available for each section of the laboratory. When all requested analyses are completed, a Certificate of Analysis is submitted to the client.

8.7.1.6.1 Sample holding times are tracked by the LIM system with holding dates monitored on backlog reports. Short holding time parameters defined as less than 48 hours are marked at sample login and immediately taken to the laboratory for analysis. This would include analytes such as pH, BOD, CBOD, turbidity, color, ortho-phosphate, hexavlent chromium, and UV-254. This procedure is done to ensure that short holding time parameters are correctly determined at the login step even before the information is logged into the LIM system.

8.7.1.6.2 For sample preparation and analysis, an aliquot is removed from the sample container and prepared as defined in the laboratory SOP. Depending upon the nature of the test, the analyst loads the samples onto the instrument and programs the instrument to analyze the samples in the order they appear in the instrument sequence and in the instrument logbook. Printed laboratory benchsheets must be utilized for all tests with a space available to enter the signature or initials of the analyst, date of analyses, the laboratory sample identification number, and volume of sample analyzed, value from the measurement system, factor, and final volume to be reported

8.7.1.7 Sample Disposal - After the completion of all analyses requested and a review of all data, the designated representative prepares a Certificate of Analysis to submit to the client. The date reported is noted on each certificate. Routine samples are disposed as defined in the Chemical Hygiene Plan. Non-routine samples are returned to the client when applicable. Non-hazardous samples are disposed of by the laboratory in accordance with all local, state, and federal regulations.

8.7.1.8 Qualified Samples - If the Sample Custodian or analyst discovers improper field preservation or a damaged sample container, the client is contacted so that a determination can be made if a resample is possible. If another sample cannot be secured, the original sample is analyzed but the results reported must be qualified with the identification of the problem encountered during sample receipt. If required by a state drinking water certification program, the laboratory must notify the state laboratory about the unacceptable sample(s).

8.7.1.9 Archiving of Data - According to ISO/IEC Guide 17025 and the NELAC guidelines, the laboratory must establish and maintain procedures for identification, collection, indexing, access, filing, storage, maintenance, and disposal of quality and technical records. All records are to be held secure and in confidence. Technical records are defined to be all documents, forms, and recordings involved sample collection, sample processing, sample analysis, and sample removal. This includes electronic media and hard copy documents. Quality records include reports from internal audits, management reviews, copies of external audits, and records of standard operating procedures, and corrective actions.

8.8 FLOWCHART FOR HARD COPY RECORDS


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8.8.1 Identification: All records must be properly identified according to the section or department of the laboratory where the records were generated. For instance, metals bench sheets would be kept within the metals department.

8.8.2 Collection: Records must be kept in an orderly fashion and collected by the individual analyst or supervisor and placed into liberty boxes for removal out of the laboratory. For those records that are still in service, the liberty boxes are accessible in the laboratory.

8.8.3 Indexing: Liberty boxes are used and marked for the sequence of events, dates of analysis, or laboratory section. Indexing is not necessarily accomplished with a numerical ordering system.

8.8.4 Access: Records less than one year old are kept in the laboratory for ease of retrieval. Those older than a year are normally moved to one of two storage areas within the corporate building. For archived records, access is strictly maintained to prevent any theft, damage, or deterioration to the documents.

8.8.5 Filing: In order to have some type of organizational structure, records should be segregated in the liberty boxes by either the analyst or supervisor.

8.8.6 Storage: Records are maintained in two secure areas where access is limited. Normally the supervisor or designated individual will move the liberty boxes to the proper location.

8.8.7 Maintenance: Records are maintained under strict access and are periodically checked to ensure that the records have not been damaged.

8.8.8 Disposal: The microbiological records must be maintained for five years, lead and copper records must be maintained for 12 years and all other laboratory data and documents must be maintained for a period of ten years unless a longer term is agreed to by the client and Alloway. Once the required time frame has been met the documents may be disposed of by a commercial hauler. Documents are shredded to protect the client confidentiality. The liberty boxes must be properly marked as ready to dispose by the Quality Assurance Officer.

8.9 FLOWCHART FOR ELECTRONIC MEDIA

8.9.1 Identification: All electronic media will be identified either by the software vendor or internally by management Part of the identification process may include writing on the compact disk or tape.

8.9.2 Collection: Records must be kept in an orderly fashion and collected by management.

8.9.3 Indexing: Software is normally indexed by the management and stored in fireproof storage containers.

8.9.4 Access: Records are maintained by the Quality Assurance Officer and access limited to the department and to the Laboratory Supervisor.

8.9.5 Filing: Due to the small size of the electronic media, compact disks and other electronic media are not indexed but simply filed in the fire proof storage devices.

8.9.6 Storage: Records are maintained in two secure areas where access is limited.

8.9.7 Maintenance: No special maintenance of the records is required except for protection against the elements.

8.9.8 Disposal: Records beyond the required time frame may be disposed of by management. The electronic media may be discarded through the trash after deleting the files from the media.


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8.10 Electronic Data Management - Sample logging, tracking and reporting efforts are computerized on each laboratory’s Laboratory Information Management System (LIMS). All database media is transferred to CD-ROM and this information is maintained for a period of five years for microbiological data, twelve years for lead and copper data and ten years for all other data.


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9.0 FACILITIES, ANALYTICAL PROCEDURES, AND PREVENTATIVE ACTION

PROCEDURES

9.1 Alloway’s Marion laboratory is home to the Drinking Water division. With approximately 10,000 square feet of laboratory space (15,000 total) this facility is suitable for a laboratory operation. A complete list of the laboratory equipment is found in Appendix 1.

9.2 GLASSWARE PREPARATION

9.2.1 All materials that come into contact with samples, blanks, and reagents must be scrupulously cleaned to avoid contamination and the generation of inaccurate data. Alloway uses new, pre-cleaned glassware certified by the company supplying the containers. In order to produce the most reliable and accurate results, Class A Volumetric Glassware is utilized for all standard solutions preparation. Specific information regarding glassware cleaning is contained in the technical SOPs for glassware preparation.

9.3 SAMPLE PREPARATION

9.3.1 The type of analysis to be done and the exact sample matrix are used for selecting the sample preparation methods. As specified in the laboratory technical SOP, the samples must first be prepped or prepared before the determinative test is accomplished. Because various parameters may have different preparation procedures, the technical SOPs must be referenced for specific procedures. The sample aliquot for analysis is defined in the laboratory procedure to ensure a representative amount of material is analyzed.

9.4 ANALYTICAL PROCEDURES

9.4.1 Appendix 5 lists all the analyses routinely performed in this laboratory for drinking water, waste water, and hazardous waste samples. All analytical methods used by the laboratory are based on recognized and official methods which are listed in the tables in Appendix 5. Contact the laboratory for the listing of Standard Operating Procedures (SOPs) or the specific SOP used by the laboratory to perform the methods referenced in Appendix 5.

9.5 PREVENTATIVE ACTION PROCEDURES

9.5.1 According to ISO/IEC Guide 17025 and the NELAC standards, the laboratory must maintain a preventive action policy to reduce the likelihood of the occurrence of nonconformances and to take advantage of the opportunities for improvement. This is not to be confused with a corrective action procedure which is an "after the fact" situation and deems a possible root cause investigation.

9.5.2 Preventative Actions are intended to assist the laboratory with possible situations and problems that could arise for future work. The following is a list of categories that would be appropriate as preventative action guidelines including the responsible party for initiating actions and controlling their effectiveness.

9.6 PREVENTIVE ACTION: EQUIPMENT

9.6.1 Each major piece of equipment is the responsibility of the analyst (operator) with the ultimate responsibility belonging to the Laboratory Supervisor. The operator maintains an instrument logbook for that piece of equipment detailing how the instrument was used, the preventive maintenance done on that equipment and any corrective action undertaken by the employee or outside technician to remedy equipment problems. Equipment is taken out of service whenever


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routine maintenance and corrective actions do not correct the problem. Whenever equipment is taken out of service it is labeled with a sign, dated and initialed.

9.6.2 Depending upon the instrument and the technical ability of the analyst(s), a service contract with the vendor who sold the instrument is established when problems arise. Preventive maintenance is designed to ensure that equipment and instrumentation is kept in good working order so that downtime is eliminated or reduced. The goal of maintenance is to increase measurement system reliability and thus ensure sample integrity throughout the analytical process.

9.6.3 Instrument logs must contain a record of the day-to-day repairs required to keep the instrument functioning at the most productive level.

9.6.4 Normal routine preventive maintenance requirements may be defined in the technical SOP for each method with some of these checks outlined below. The majority of these checks are accomplished with each analytical run except for situation when optical cells or source units need to be cleaned extensively.

9.7 FLOWCHART FOR EQUIPMENT CHECKS

9.7.1 ICP Units: routine maintenance includes checking all injector ports, lines, reagents, valves, tubing, sample introduction system, torch assembly, diagnostic checks, and analytical profiling.

9.7.2 ICP-MS Units: routine maintenance includes checking all injector ports, lines, reagents, valves, tubing, sample introduction system, tune checks, flow rates, mass spectrometer source.

9.7.3 Graphite Furnace Units: routine maintenance includes checking all injector ports, lines, reagents, cleaning the furnace heads, checking lamps for proper alignment.

9.7.4 Cold Vapor Hg Unit: routine maintenance includes checking all injector ports, lines, reagents, valves, tubing, and optical cell cleaning.

9.7.5 Ion Chromatography Units: routine maintenance includes verifying sufficient quantity of gas with no worn out or blocked air tubing; checking quantity of reagents and expiration dates; check for leaks from suppresor and/or columns; check background conductivity as proportional to eluent strength; check for abnormal backpressure; and check for miscellaneous supplies.

9.7.6 Colorimetric Units: routine maintenance includes checks for leaks, ensure lamp is turned on, check reagent for quantity and expiration dates; check integrity of bubbles and flowing bubble pattern, and check for miscellaneous supplies.

9.7.7 Gas Chromatographs: routine maintenance includes oven checks, column maintenance, injection port cleaning and service of detectors such as mass spectrometers.

9.7.8 High Performance Liquid Chromatograph: routine maintenance includes detector maintenance, autosampler maintenance, and miscellaneous checks.

9.8 PREVENTIVE ACTION: ANALYTICAL SAMPLES

9.8.1 It is the policy of the laboratory to encourage all clients to submit analytical samples utilizing the laboratory's designated collection containers and preservatives. This helps to minimize problems and situations that could jeopardize the integrity of the sample. Since the laboratory has control over the type, level of quality, and make of the respective containers, this is a preventative step to avoiding sampling pitfalls. Below is a general outline for the preventative action regarding analytical samples: 9.8.1.1 A sample order is placed by the client to the laboratory; 9.8.1.2 The order is forwarded to the Shipping Department; 9.8.1.3 The order is reviewed and completed by the Shipping Department utilizing the

laboratory’s pre-preserved and pre-cleaned analytical containers; 9.8.1.4 The order is sent normally by courier according to the client’s specifications; 9.8.1.5 The paper order is filed for completeness; 9.8.1.6 Once the samples are received back to the laboratory, they are checked into the

laboratory

9.9 PREVENTIVE ACTION: METHOD REVISIONS


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9.9.1 It is the responsibility of the Vice President of Technical Services, Quality Assurance Officers, and the supervisors to keep abreast on changes and updates to the analytical methods used by the laboratory. This process may involve attending conferences, receiving updates from outside auditors, or periodic review of web sites sponsored by federal and state authorities. Below is a general outline for updating method revisions as laboratory procedures: 9.9.1.1 The Quality Assurance Officer determines that a new update to a method or a new

method has been developed by US EPA for environmental testing. 9.9.1.2 A copy of the method is obtained and evaluated by the Quality Assurance Officer in

conjunction with supervisors. 9.9.1.3 The method must be carefully scrutinized to ensure that the method has been

promulgated and approved by US EPA for testing. Further accreditation may be required for specific state requirements.

9.9.1.4 If the method is to be adopted, then a change to the standard operating procedure must be made or a new standard operating procedure written for a new method.

9.9.1.5 All specific quality control start up information including a method detection limit must be generated before analytical samples are analyzed.

9.9.1.6 Once the method has been approved by the Quality Assurance Officer, the method may be implemented into the laboratory.


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10.0 LABORATORY PURCHASING POLICIES AND PROCEDURES 10.1 The laboratory shall have a policy and procedures for the selection and purchasing of services and

supplies it utilizes that affect the quality of the tests and/or calibrations. This is a requirement under the ISO/IEC 17025 Guidelines as well as for NELAC. In addition, it is the laboratory's responsibility to evaluate suppliers of critical consumables, supplies and services which affect the quality of testing and shall maintain records of these evaluations and list those approved. This is managed with a Current Vendors Master List which details the vendors utilized by the laboratory for supplies, equipment, and consumables.

10.2 CONSUMABLES

10.2.1 Standard Operating Procedure for Purchasing Consumables 10.2.1.1 The Marion laboratory standard operating procedure for the purchase, receipt, and

storage of consumables follows: 10.2.1.2 All relevant information regarding consumables to be ordered is gathered from the

analyst(s) most familiar with the procedure. 10.2.1.3 The information is then forwarded to the department head or designated assistant for

ordering. 10.2.1.4 The order is placed to the appropriate vendor. In many cases, a contract will be set

up between Thermo Fisher Scientific and Alloway whenever appropriate. Most consumables are purchased through Thermo Fisher Scientific. A similar contract is set up with Scientific Specialties and Alloway for bottles used in the shipping and receiving department. An account is set up with each vendor from whom supplies are ordered. The specific account number and purchase order number are required.

10.2.1.5 Once orders are placed, the items will be shipped accordingly taking into account any overnight deliveries that must be made.

10.2.1.6 Once items are received, the items are checked for damage and order accuracy. Any problems are relayed immediately to the vendor. The paperwork is signed and dated as acceptable and forwarded to the Marion office for review and processing by accounting.

10.3 ADDITIONAL SUPPLIES

10.3.1 ALLOWAY has developed a Master List of vendors to ensure that purchased supplies meet quality criteria prior to use. The laboratory ensures that purchased equipment and consumable materials are not used until they have been inspected, calibrated or otherwise verified as complying with any standard specifications relevant to the calibrations or tests concerned. This can be based on experience with a vendor, specific pricing charged to the laboratory by a vendor, or the availability of specific supplies.

10.3.2 Standard Operating Procedure for Purchasing Additional Supplies 10.3.3 All relevant information regarding products or equipment is gathered from the

analyst/technician(s) most familiar with the procedure in conjunction with the Vice President, Technical Services.

10.3.4 In some cases, demonstrations are conducted on new supplies prior to purchase. These demonstrations are done on site or at the vendor’s facility.

10.3.5 When purchasing is desired, a contract is completed between the vendor and ALLOWAY. 10.3.6 If training needs to be conducted for the new supplies, the Technical Director or Quality

Assurance Officer arranges for the contracted vendor to train all staff in the necessary areas to operate the instrument(s).

10.3.7 Once orders are placed, the items will be shipped accordingly taking into account any overnight deliveries that must be made.

10.3.8 Once the items are received, the items are checked for damage and order accuracy. Any problems are relayed immediately from Alloway to the vendor. The paperwork is signed and


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dated as acceptable and forwarded to the Marion office for review and processing by accounting.


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11.0 CAPITAL EQUIPMENT EXPENDITURES

11.1 The laboratory shall have a policy and procedures for the selection and purchasing capital equipment. This is a requirement under ISO/IEC Guide 17025 as well as for NELAC. The standard operating procedure for purchasing capital equipment is detailed as follows:

11.2 STANDARD OPERATING PROCEDURE FOR PURCHASING EQUIPMENT

11.2.1 An evaluation is made by the laboratory manager, supervisors, and other personnel regarding

specific instrument or equipment that may need to be purchased. The purchase may be driven by capacity issues or instrument problems.

11.2.2 All relevant information regarding the instrumentation is obtained and evaluated by the Laboratory Supervisor and Technical Director in conjunction with the President of ALLOWAY.

11.2.3 In some cases, demonstrations are conducted on new equipment prior to purchase. There may even be a trial period whereby the instrument will be tested in the laboratory.

11.2.4 When it has been determined that the instrument will meet the laboratory’s production and quality assurance requirements, a contract will be completed between the supplier and ALLOWAY.

11.2.5 When the order for the equipment is placed, the items will be shipped accordingly by the supplier.

11.2.6 Once the equipment has been received by the laboratory, the items are checked for completeness and order accuracy. Any problems are immediately reported to the vendor. The paperwork is signed and dated as acceptable and forwarded to the Lima office for review and processing by accounting.

11.2.7 All start up quality control checks and instrument training must be completed before analytical samples are analyzed by the laboratory.

11.3 CHEMICAL PROCUREMENT AND STORAGE

11.3.1 The laboratory utilizes a wide variety of chemicals and reagents for analytical testing.

Chemicals and reagents used for testing are ACS grade or better and are dated with an expiration date. Gases are purchased with the highest commercial purity required for the test method. Reagents, chemicals, and solvents are purchased through a variety of vendors and stored in areas designated for chemical storage. Please refer to the ALLOWAY Chemical Hygiene Plan for additional information.

11.4 CERTIFICATIONS and SUBCONTRACTING


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11.4.1 The laboratory subcontracts first to other ALLOWAY laboratories with equivalent certifications or accreditations required by the client. When an ALLOWAY laboratory does not have the capability or certification an approved subcontract laboratory is selected. Subcontract laboratories are approved if they are ISO 17025 accredited, NELAC accredited, or have the client-specified certification. Copies of the subcontract laboratories’ scope of accreditation and certification should be obtained and maintained on file by the Quality Assurance Officer. The client should be notified in writing before subcontracting. The documentation is by facsimile or email. At a minimum, verbal client approval must be documented by the laboratory prior to sending samples to another ALLOWAY or outside laboratory.

11.4.2 A current listing of the laboratory's certification status is maintained in Appendix 3 of the Quality Assurance Manual. All of the original licenses, certifications, and accreditations are kept in the Marion, Ohio office. Due to extensive numbers of certifications held by the laboratory, it is important to note that certification status can change from time to time. Clients are encouraged to check with the laboratory personnel to ensure that the certification status of the laboratory remains intact for a specific project.

11.4.3 The laboratory performing the subcontract work shall be indicated in the final report with the respective analyses attached. The laboratory maintains a register of all subcontractors that it utilizes for environmental tests.


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12.0 CALIBRATION PROCEDURES AND FREQUENCY CHECKS

12.1 The laboratory performs the testing based on the reference method cited. Where the reference method does not indicate the quality control or calibration process, the laboratory must adopt at least the calibration and quality control checks defined in this Manual. The laboratory performs routine checks which monitor the method performance for every batch of samples. These checks include the following:

12.1.1 Review to ensure the methods listed are those employed by the laboratory. 12.1.2 Potential interferences from samples are investigated. Samples containing high concentrations of

inorganic or organic materials need to be diluted for proper analysis, which increases the detection limits for compounds in that matrix.

12.1.3 Review of calibration and calibration verification. 12.1.4 Criteria specified in the laboratory SOP for review of method detection limits, reporting limits

and practical quantitation limits (PQLs) and precision and accuracy. 12.1.5 Retesting of retained samples when quality control or matrix effects. 12.1.6 Correlation of analytes with project and other client information.

12.2 Acceptance criteria for method performance include precision and accuracy data from the reference

method as listed in the laboratory SOP. Where reference method criteria is not specified, the laboratory defines default limits for the technology in the laboratory SOP.

12.3 INSTRUMENT CALIBRATION (Initial and Continuing)

12.3.1 All analytical instruments must be calibrated before analyses of samples can begin. This is

accomplished based on the requirements in the technical SOP for a particular method. Most of the analytical methods require the analysis of an initial calibration that is usually consists of multiple calibration points. The initial calibration curve must meet the acceptance criteria specified in the laboratory SOP before reporting of any sample data. Acceptance criteria for the initial calibration curves are expressed as correlation coefficients, relative standard deviation, or other reference defined parameter such as total area counts.

12.3.2 Once the initial calibration curve has been generated, the calibration curve must be verified with a second source check standard, sometimes referred to as a continuing calibration check. These verification standards are utilized to ensure that the calibration remains in range and meets specific method requirements. Each specific technical SOP will note the acceptance criteria for these check standards in terms of a percent recovery or a relative percent difference.

12.3.3 Reported sample results must be bracketed by calibration standard concentrations else a dilution is required to bring the values within the calibration range. Results may be qualified as estimated "J flags" when data is reported below the lowest standard or above the highest standard.

12.4 METHOD BLANKS


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12.4.1 Every analytical method must include a method blank. The method blank is treated like any sample. The method blank for the batch must be a similar matrix to the samples analyzed. The laboratory uses clean soil or reagent water for similar matrices. Method blanks are performed once per batch of twenty. Method blanks must include all reagents, solutions and steps in the process. Distinct method blanks are added to the batch when the reference method specifies or contamination isolation is required.

12.4.2 Instrument blanks are performed at the beginning of an instrument analysis to assure the equipment is not contaminated prior to analyzing samples. Instrument blanks are used at the frequency defined in the technical standard operating procedure.

12.5 QUALITY CONTROL CHECKS

12.5.1 Unless the technical SOP stipulates otherwise, internal quality control checks, laboratory

performance and systems audits and frequency checks include:

Quality Control Check Frequency Method blanks One per batch or method specifications Laboratory control sample (LCS) or LFB One per batch or method specifications Calibration Check Samples One per batch or method specifications Replicate Samples One per batch or method specifications Matrix-spiked Samples One per batch or method specifications

12.6 LABORATORY THERMOMETERS

12.6.1 Laboratory thermometers are calibrated annually against a NIST Certified Thermometer. These values are recorded on a thermometer form and kept at the laboratory. Every five years, the NIST Certified Thermometer(s) are sent to the manufacturer for recalibration and cleaning. The manufacturer must be A2LA or NVLAP accredited. Correction factors are recorded. If the correction factor (or difference in reading from the NIST and laboratory thermometer) is greater than the control criteria for the use, the thermometer is replaced. Correction factors are noted on the thermometer and thermometers are labeled with their expiration date. All laboratory records include the observed value.

12.6.2 Thermometers located in refrigerators and freezers are checked daily, recorded, and initialed. Refrigerators are set at 6 +/- 2 o C and freezer temperatures are to be below 0 o C. Specific criteria for each thermometer are provided with the log sheets. Thermometers located in ovens and water baths are monitored for criteria specified in the laboratory SOP. Any deviation from these criteria requires immediate corrective action. Corrective action includes adjusting the temperature settings. If the next reading does not indicate an acceptable temperature reading, a corrective action form is completed. The Quality Assurance Officer is notified and the situation monitored.

12.7 ANALYTICAL BALANCES AND WEIGHTS

12.7.1 Balance type must be appropriate for the analysis. Balances are checked before use on days utilized by laboratory personnel with Class S-1 certified weights encompassing the normal range


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of weighing. Tolerance levels are noted on the balance bench sheets. Any deviation from these limits requires immediate corrective action. The Quality Assurance Officer is notified, and the balance labeled as out of service. During the down time for a balance, another balance must be utilized.

12.7.2 Weights meeting ASTM Type 1, Class 1 or 2 specifications must be recertified at least every five years; however, it is recommended that a two-year cycle be followed. (Note: Class S and ASTM Type 1, Class 1 or 2 weights are considered equivalent). The weight set must be recalibrated by a NVLAP accredited facility. The weight sets are labeled with the serial number that corresponds to the certificate.

12.8 REAGENT WATER

12.8.1 Laboratory pure-water is generated using an outside contracted purification system. Daily

checks of the water are done to verify the purity of the water. Any problem with the purity of the water requires immediate corrective action. The Quality Assurance Officer is notified and all laboratory staff are notified of an unacceptable reagent water condition. A service call for repair is placed to correct the problem.

12.9 VOLUMETRIC DEVICES

12.9.1 All volumetric pipettors shall be checked for accuracy on at least a quarterly basis. Tolerance limits must be established for the pipettors and noted during the checks. Burettes that are not class A are also checked for accuracy on a quarterly basis.

12.10 UNCERTAINTY MEASUREMENT IN TESTING


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12.10.1 The laboratory maintains a standard operating procedure for polices and procedures for conducting uncertainty of measurement. Uncertainty of measurement is characterized by a level of confidence for a reported result or measurand. The measurement uncertainty for a particular measurand is examined in the laboratory by any of the following methods.

12.10.1.1 Method Quality Control-evaluation of an analytical run with non-matrix defined confidence intervals or levels of acceptance. Includes such checks as reporting limit standards, laboratory control standards, initial calibration curves, continuing calibration checks, and preparatory blanks. Specific limits are associated with each quality control check based on method specific criteria.

12.10.1.2 Control Charts-evaluation of quality control checks that are examined for trend analysis. Utilizes a lower and upper limit for data acceptance if no specific method criteria exist.

12.10.1.3 Precision-also referred to as repeatability. Measured through the use of sample duplicates, matrix spike duplicates, or field replicates. A specific limit is associated with acceptance of these quality control checks; however, the precision measurement is based on real-world sample data where matrix interferences are probable. Normally, an analytical run would not be rejected should the precision measurement on a matrix-related sample be outside acceptance limits. Should this situation occur, it is common to report the data as qualified or estimated.

12.10.1.4 Accuracy-also referred to as bias or recovery testing. The difference between the expectation of the test results and an accepted reference value. Measured by matrix spike analysis. A specific limit is associated with acceptance of this quality control check; however, the accuracy measurement is based on real-world sample data where matrix interferences are probable. Normally, an analytical run would not be rejected should the accuracy measurement on a matrix-related sample be outside acceptance limits. Should this situation occur, it is common to report the data as qualified or estimated.

12.10.1.5 Interlaboratory comparison-laboratory participation in proficiency testing studies with other laboratories to compare means, recoveries, and methods. A specific level of confidence is noted on the Proficiency Testing Results along with a grade of "acceptable" or "not acceptable."

12.11 As noted in the ISO 17025 documentation on measurement uncertainty, commercial testing laboratories generally utilize the above mention checks to evaluate the level of significance or confidence of the data produced. In those cases where a well recognized test method specifies limits to the value of the major sources of uncertainty of measurement and specifies the form of presentation of calculated results, the laboratory is considered to have satisfied this clause by following the test method.

12.12 Uncertainty measurements can also be applied to marginal exceedance values specifically for method blanks, lab control standards and matrix spikes. The values are handled on a case by case basis in the laboratory following the guidelines set forth in Chapter 5 of the NELAC Standards.


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13.0 ANALYTICAL STANDARDS AND TRACEABILITY

13.1 MEASUREMENT TRACEABILITY and ANALYTICAL STANDARDS

13.1.1 Scope and Application 13.1.1.1 Traceability is the property of a measurement result whereby it can be related to

stated references, through an unbroken chain of comparisons, each step in the chain having stated uncertainties. The purpose of requiring traceability is to ensure that measurements are accurate representations of the specific quantity subject to measurement, within the uncertainty of measurement.

13.1.1.2 Traceability is characterized by six essential elements: 13.1.1.2.1 Unbroken chain of comparison-begins with an unbroken chain of

comparisons originating at national, international, or intrinsic standards of measurement and ending with the working reference standards of a given laboratory.

13.1.1.2.2 Measurement uncertainty-for each step in the traceability chain calculated according to defined methods and must be stated at each step of the chain so that an overall uncertainty for the whole chain can be calculated.

13.1.1.2.3 Documentation-each step must be performed according to documented procedures and the results documented in a calibration or test report.

13.1.1.2.4 Competence-the laboratories must supply evidence of technical competence. 13.1.1.2.5 Reference to SI Units-where possible, the national, international, or intrinsic

standards must be primary standards for realization of the SI units. 13.1.1.2.6 Recalibrations-calibrations must be repeated at appropriate intervals in such a

manner that traceability of the standard is preserved. 13.1.2 ALLOWAY Policy for Traceability Measurement-Vendors

13.1.2.1 For the purposes of demonstrating measurement traceability, calibration certificates and certificates for certified reference materials should, wherever applicable, indicate the traceability to national or international standards of measurement and should provide the measurement result and associated uncertainty of measurement.

13.1.2.2 Wherever applicable, a statement of compliance with an identified metrological specification can be accepted instead of measurement results and associated uncertainties. Only calibration certificates or reports endorsed by a recognized accreditation body's logo or which otherwise makes reference to accredited status, are considered to satisfy traceability requirements.

13.1.2.3 Certificates are normally received with the reference materials. Certificates are maintained within the laboratory by the supervisor of the department or their designated authority.

13.1.3 ALLOWAY Policy for Standards and Reagents Documentation 13.1.3.1 Records of the sources of all standards are kept in the Maximum Advantage

Reagent Traceability Software program (MART). This software ensures traceability of all standards used to calibrate tests and instruments and ensures independent check standards or reference materials are traceable. The information recorded in MART is noted below: • ALLOWAY-Sequential Quality Control number • Type of standard or reference material • Where the standard or reference material was purchased • Lot number and vendor information of the standard or reference material • When the standard or reference material was received • When the standard or reference material was opened


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• List of analytes and respective concentrations in the standard or reference material

• Expiration date of the standard or reference material (when the expiration date is not available, the laboratory will assign a shelf life of normally one year).

• When standard (primary and working) was made in the laboratory • Documentation of how the standards were made in the laboratory

13.1.3.2 All calibrations and validations of equipment must be traceable to national

standards whenever possible. Where traceability to national standards of measurement is not applicable, the laboratory must perform its own respective in house checks through the use of interlaboratory comparisons, proficiency testing, or independent analysis. The purity of the chemicals and standards must be appropriate for the necessary tests. The vendors ALLOWAY uses must provide this traceability information on their respective certifications of analysis. If any vendor does not provide the above documentation, the vendor must be contacted. Traceability documents must be filed by individual analysts/technicians in their respective departments. From the neat or primary standards, dilutions are made for working standards to generate calibration curves, etc. Other serial dilutions are required depending upon the scope of linearity for the test involved.

13.1.3.3 ACS grade reagents are used in the laboratory. The majority of the reagents are reagent grade with some analyses requiring specialized grades that are specified in the laboratory methods. Reagent chemicals are stored and handled according to the instructions supplied by the manufacturer and documented in the laboratory SOP for the specific test method.

13.1.3.4 Reagent concentrations are expressed in terms of normality, molarity and additive volumes. Normal solution (N) contains one gram equivalent of solute per liter of solution. Molar solution (m) contains one gram molecular weight of solute per liter of solution. An additive volume (a+b) is where “a” denotes volume of concentrated reagent and “b” refers to volume of distilled water required for dilution.

13.1.3.5 Standard solutions are prepared in Class A volumetric flasks. Primary and secondary dilutions are then made from the stock solutions and are thoroughly mixed. The standards and prepared solutions are stored in refrigerators, freezers or at room temperature depending upon the compounds of interest and the manufacture’s instructions. The laboratory SOP defines the exact solution handling storage and containers. MART Program contains the preparation instructions for all solutions and standards. Other standards/reagents are kept in either glass or plastic containers. All chemical reagents, standards and solutions prepared by the laboratory must be labeled with the solution name, initials of the preparer and dated with the ultimate expiration date per MART Program. In general, most reagents are used very quickly and not kept for extended periods of time. It is common good laboratory practice to only keep the solutions and liquid standards a maximum of one year after preparation or opening or per manufacturers or method requirements, whichever comes first, however, a material may continue to be utilized if its reliability can be verified by the laboratory.

13.1.3.6 The laboratory must retain records for all standards, reagents, certified reference materials, and other quality control standards. This is usually in the form of a certificate of analysis or certification statement or in MART Program.


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14.0 DATA REVIEW, REPORT GENERATION AND RECORDKEEPING

14.1 VALIDATION

14.1.1 Data validation is a formal process whereby analytical data is rejected, accepted or qualified based on an established set of criteria. Review of the data and quality control begins at the bench level. Each analyst has read and understands, based on the technical SOP, the criteria for each test. The analyst has the authority to terminate an analytical run at any time the quality control is out of the acceptance range stated in the technical SOP. The data validation process is emphasized at the bench level with review by senior supervisors, managers, and quality assurance personnel.

14.2 DATA QUALIFIERS

14.2.1 Data qualifiers are normally applied to qualify any data which is either suspect due to matrix interferences, quality control deviations, outside the calibration range or for any data reported below Alloway’s normal PQL or reporting limit. The laboratory must appropriately qualify all data where quality control is out of control. The policy of the laboratory is to alert the client via the Certificate of Analysis or a case narrative when the quality control for a particular test(s) is out of control. Normally, the information contained on the Certificate of Analysis is a notation denoting that the data is being qualified and must be viewed as an estimate due to a matrix effect.

14.3 CASE NARRATIVES

14.3.1 Case narratives are typically written for clarification purposes of any problems or concerns from sample analysis including blank contamination. The Quality Assurance Officer or representative writes these narratives with the assistance of the Laboratory Supervisor/Analyst.

14.4 FINAL REPORTS AND DATA PACKAGES

14.4.1 Because ALLOWAY does not participate in the CLP Program, our data packages and final reports do not follow their specific protocol. See Appendix 9 for a detailed list of final report contents. Typically, a client will receive the following information for a submitted sample: Final Report, Chain-of-Custody, and a sign-off sheet by the Quality Assurance Officer. Other specific high-level analytical data packages are also available to clients and the laboratory has the ability to produce most of the CLP forms. The laboratory reviews the reporting needs of the client and produces the final report and data package based on the client’s needs.

14.4.2 A Certificate of Analysis is printed for each sample submitted. This ensures that each sample has a unique identification number. In many cases, special state or industrial reports must also be completed for our clients. The majority of states that operate a drinking water program require the laboratory to utilize the state’s form for public drinking water suppliers. It is critical that the reports be completed in their entirety according to the specifications of the state authority.

14.4.3 Units of measurement are respective for the matrix involved such as aqueous samples in terms of volume while soils/sludges will be in terms of dry weight.

14.5 SIGNATURES

14.5.1 The Vice President, Technical Services or designee is the person accepting responsibility for the content of the certificate or report. The use of photographic, electronic, and mechanical means of reproduction of signatures or names of signers is acceptable, as long as the user can identify the person taking responsibility for the report and that automated signatures are safeguarded.


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14.5.2 Certain individuals have been granted authority to sign or initial analytical reports for clients. The mechanical stamper is kept safeguarded within the laboratory and is only available to those individuals who are permitted to sign analytical reports. Note that the Laboratory Information Management System controls the individuals who can sign the Certificates of Analysis by assigning that individual’s name to the report.

14.6 ERRONEOUS RESULTS

14.6.1 If the laboratory or client discover any reporting problems or concerns, the problem is investigated and documented through the corrective action process. If the resolution identifies a reporting error, the laboratory reissues the report.

14.6.2 Note that the “date printed” is always placed on the Certificate of Analysis. If results have been archived, the old “date printed” as well as the new “date printed” will appear on the Certificate of Analysis. An entry is made into a book of reprinted reports if a Certificate of Analysis is revised and reissued to the client.

14.7 CONTINGENCY PLAN

14.7.1 Our plan of action, if the laboratory was to go out of business, would be to ensure that all test samples are returned to the client and that all Certificates of Analysis generated would be submitted to the client. This includes any raw data associated with the samples. Depending upon the nature of the close of business, corporate attorneys or other parties of interest would retain all documents in a confidential state in order to protect our clients. If requested by the client(s), all records are transferred to the client(s) and kept under their protection.

14.8 ELECTRONIC DATA

14.8.1 The acquisition data from the instruments is retained on compact disks (CDs) or other media. Routine system back ups are stored in fire proof storage devices in a secure area with restricted access.

14.9 SECURITY OF COMPUTER DATA

14.9.1 Alloway maintains a Laboratory Information Management System, which is a pre-designed software package developed for a commercial laboratory. This is the main system used for log-in procedures, sample reduction, generation of reports, quality control charting and invoicing for the laboratory. The software is stored on a network environment which is backed-up daily.

14.10 RECORD KEEPING

14.10.1 Laboratory data is archived by the individual analyst and transferred to the office area for final archive and storage. The analytical raw data is kept five years for microbiological, at least ten years for chemical and twelve years for lead and copper. Special arrangements can be made to keep data for extended periods of time based on a client contract agreement. Hard copy records are archived and placed in storage areas for retrieval as needed.

14.10.2 Technical personnel record all original observations in laboratory notebooks or worksheets whenever electronic data generation is not performed. Notebooks, worksheet and electronic data printouts are signed and dated by the analyst making the observation. Changes are noted by lining out the entry, entering the correction, initialing and dating the record. Entries are always made with indelible black ink.


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14.11 DATA VALIDATION PROCEDURE: CHEMISTRY SECTION

ALLOWAY HISTORICAL REVIEW OF DATA:

1. Reporting Limit Checks 2. Review of Standard Operating

Procedures 3. Laboratory Control Standard Checks 4. Control Checks for specific quality

control checks 5. Review of Method Detection Limit

Studies

STEP 2: The analyst reviews all of the data from an analytical run, and if the QC is accepted, the data is given to the appropriate supervisor.

STEP 3: The supervisor or designated representative reviews the data and either approves the data or has the sample re-extracted or re-analyzed. Secondary review.

STEP 4: The Vice President, Technical Services or designated representative completes the three tier review with a final sign off on the analytical reports.

Alloway’s QC Criteria for Chemistry: 1. The calibration curve must meet the method criteria. 2. Surrogate recoveries (when surrogates are required in the method) must be within QC limits. 3. The method specific lab fortified blanks, matrix spikes, and duplicates must have been analyzed and be within either method specific criteria or within statistically determined limits. 4. The method blank must be less than the reporting limit for each analyte. (No correction for blanks) 5. All other method specific criteria.

STEP 5: If the data has met all of the appropriate quality control checks, the Certificate of Analysis is issued for that particular sample.

STEP 1: Samples are prepped and then analyzed according to specific method.


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15.0 PRECISION AND ACCURACY STATEMENTS

15.1 The following are descriptions of quality assurance and quality control checks used to determine the accuracy and precision of the analyses performed in our laboratory.

15.2 Alloway follows the quality assurance and quality control principles set forth by the U.S. EPA in

the Handbook for Analytical Quality Control in Water and Wastewater Laboratories (EPA-600/4-79-019), Manual for the Certification of Laboratories Analyzing Drinking Water (EPA 815-B-97-001) and US EPA SW-846 “Test Methods for Evaluating Solid Waste Physical/Chemical Methods” (EPA SW-846, November 1986, plus Updates I, II and III). The laboratory will also reference guidelines from ISO/IEC 17025, A2LA, NELAC, and other EPA publications. In addition, the laboratory will reference subsequent updates for these documents.

15.3 CHEMICAL TESTING


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15.3.1 Inorganics - The system is initially calibrated with a series of standards spanning the normal working range of the samples. The calibration is checked on a daily basis using a standard within the calibration range. A laboratory reagent blank, laboratory control sample, and matrix spike/matrix spike duplicate are analyzed. If insufficient sample is provided for a matrix spike/matrix spike duplicate test, then the laboratory control sample must be analyzed in duplicate as a precision assessment. The technical standard operating procedures address specific quality control requirements.

15.3.2 Metals - The system is initially calibrated with a series of standards spanning the normal working range of the samples. The calibration is checked on a daily basis using a standard near the midpoint. A laboratory reagent blank or method blank, laboratory control sample, and matrix spike/matrix spike duplicate are analyzed. If insufficient sample is provided for a matrix spike/matrix spike duplicate test, then the laboratory control sample must be analyzed in duplicate as a precision assessment. The technical standard operating procedures address specific quality control requirements.

15.3.3 Organics - The system is initially calibrated with a series of standards spanning the normal working range of the samples. The calibration is checked on a daily basis using a standard near the midpoint. A laboratory reagent blank or method blank, laboratory control sample, and a matrix spike/matrix spike duplicate are analyzed. If insufficient sample is provided for a matrix spike/matrix spike duplicate test, then the laboratory control sample must be analyzed in duplicate as a precision assessment. The technical standard operating procedures address specific quality control requirements. For mass spectrometer testing, the daily tune check must pass regulatory requirements before sample analysis can begin.

15.4 DEMONSTRATION OF CAPABILITY

15.4.1 The demonstration of capability (DOC) is required for each analyst per individual methodology. Four spiked samples are prepared using reagent water with a mid-level calibration standard or at a calibration specified in the reference method. The samples are analyzed and the recoveries noted. The average recovery and standard deviation for each compound is determined. The results from the DOC are placed in the training file for each analyst. The reference method specified acceptance limits must be met prior to an analyst performing the analysis. The analyst data is reviewed to determine if the recovery data is within the limits for the analysis.

15.4.2 If the data calculations indicate that the results are within established laboratory or method criteria, then the demonstration of capability is deemed to be valid. Should the analytical data for the demonstration of capability be outside the control limits, then the study must be re-evaluated.

15.4.3 When it is not possible to determine the mean and standard deviation, the laboratory must assess performance against the established criteria in the method. This would be appropriate for such tests as presence/absence or pH.

15.5 METHOD DETECTION LIMITS

15.5.1 Method Detection Limit Studies (MDLs) are done on an annual basis to measure the sensitivity of the instrument and the analytical method. The policy of the laboratory is to conduct an MDL study according to the specific methodology outlined by the US EPA.

15.6 INORGANICS/METALS CONTROL CHARTS

15.6.1 The laboratory generates control charts and limits for each test method. The graphs contained in Appendix 6 illustrate the control charts generated in the inorganics/metals section. Control charts are kept for each instrument or by each EPA method depending upon the analytes of interest and the specific software used to generate the charts. Control charts are updated periodically depending upon the volume of samples analyzed. All control chart data is reviewed


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at least annually to determine if limits require updating. Normal statistical practices are employed for developing the control charts as noted below.

Lower Warning Limit- Avg - 2*std

Upper Warning Limit- Avg + 2*std Lower Control Limit- Avg - 3*std

Upper Control Limit- Avg + 3*std

Where: avg = Average of the sample set std = Standard deviation of the sample set.

15.6.2 The policy of the laboratory is to evaluate the Laboratory Control Standards or Laboratory Fortified Blanks as the key quality control check. These samples are processed through the entire analytical determination to evaluate whether or not the process is in control. Sample specific checks such as matrix spikes and matrix spike duplicates are important in the evaluation of data. However, because the limits established for these checks are not as rigid, these are matrix related and not system related.

15.7 PROFICIENCY TESTING

15.7.1 According to ISO Guide 17025 and the other state guidelines, the laboratory shall perform analyses of periodic performance testing samples for those certified parameters provided that the samples are obtained from an accredited vendor.

15.7.2 In addition to the quality control samples analyzed in-house, ALLOWAY participates in a number of outside quality assurance proficiency testing programs:

• US EPA Federal Water Supply (WS) Studies (twice annually)

• US EPA Federal Water Pollution (WP) Studies-DMRQA

• State of New York Performance Evaluation Samples – (twice annually for each

matrix)

15.7.3 The proficiency testing studies are now being operated by a contract third-party facility. The laboratory uses only a NIST/A2LA approved PT provider for WS and WP samples. Some other programs may require specific vendors to be utilized for the proficiency testing. For scoring systems, some programs are based on a true value and others on a mean. For many analytes, acceptance limits are set as fixed percentages of the true sample concentration. For some analytes, a 95% prediction interval is calculated from available proficiency testing data.

15.7.4 As part of the data reduction and retention policies, the laboratory shall maintain copies of all written bench sheets and chain of custodies related to the analysis of all proficiency testing samples for a minimum of five years for microbiology, ten years for chemical and twelve years for lead and copper. This information also includes such items as raw data and data calculations.


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16.0 PERFORMANCE AND SYSTEM AUDITS

16.1 Alloway is audited approximately quarterly by outside authorities from state agencies and key clients. The information contained in Appendix 3 lists the certifications and accreditations as of the date indicated. For the most current list of certifications, please contact the Quality Assurance Department. The format for external audits is highly varied depending upon the agency or client conducting the audit. The Vice President, Technical Services or Quality Assurance Officer is contacted to arrange an audit date. The labs are examined rigorously both with respect to the data generated and interviews conducted with key personnel.

16.2 INTERNAL AUDITS

16.2.1 The Quality Assurance Officer conducts an internal system audit at least annually or whenever corrective action notifications, or control chart trends indicate an operational concern. System audits are accomplished with the use of checklists. Please refer to Appendix 4 for an example of a typical audit checklist. Performance audits include proficiency testing samples and audits to specific SOPs. SOP auditing is conducted whenever trends or corrective actions indicate a specific concern in an operational activity.

16.2.2 Internal audits are used to verify that the operations of the laboratory continue to comply with the requirements of the laboratory’s quality system. It is the responsibility of the Quality Assurance Officer to organize an internal audit as required by a predetermined schedule and as requested by management. Internal audits must include the examination of data quality, and must determine if procedures are being followed, objectives are being achieved, designated duties are carried out and if there are opportunities for improvement.

16.2.3 The results of internal audits form an integral part of the input to management-review activities. The auditor must be independent, whenever resources permit, of the activities to be audited to ensure that an effective audit will be conducted. Alloway requires that all internal audits be conducted either by senior management personnel or by the Quality Assurance Officer. Internal audits are scheduled on the basis of status and importance of the activity to be audited. Each aspect of the quality system is audited a minimum of once per year.


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17.0 STANDARD OPERATING PROCEDURE FOR CONDUCTING INTERNAL AUDITS

17.1 Identify the area or test method where the internal audit will be conducted. Depending on the situation, this can be done announced or unannounced.

17.2 Utilize a checklist outlining the method procedures for performance audit or use the checklist for a

system audit.

17.3 Begin the internal audit with the necessary personnel present.

17.4 Evaluate the method and/or procedure detailing all findings and recommendations.

17.5 Evaluate quality control checks.

17.6 Evaluate on a confidential basis any evidence of inappropriate actions or vulnerabilities related to data integrity.

17.7 Close the audit by completing the checklist and discussing the audit with management.

17.8 Take timely corrective action on deficiencies found in the audit by completing a corrective action

form.

17.9 Conduct a follow-up audit at a reasonable time to ensure that deficiencies have been addressed. This may be done in steps to ensure that all aspects of the internal audit have been completed.

17.10 The internal auditor has the right to stop work for a particular methodology if it appears that the

problems and/or situations are compromising data quality. Senior management must be notified immediately of this situation and proper steps must be taken to ensure that the quality of data is not compromised. When the problem is rectified, work for the particular methodology is reinstated.


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18.0 STATISTICAL METHODS

18.1 The purpose of this section is to provide a brief description of the many statistical techniques available for evaluating analytical data.

18.2 CONTROL CHARTS

18.2.1 Our most widely used statistical tool is the Shewhart Control Chart (Appendix 6). A control chart is a graphical plot of test results with respect to time with limits drawn within which results are expected to lie when the scheme is in statistical control. These charts provide historical trends in data such as laboratory control samples and surrogates. Control charts are generated on a periodic basis. It has been recommended that at least 20 points be utilized to plot the chart. Information included in the control chart includes method, parameter(s), dates, and upper/lower control limits. Data points that fall outside established limits indicate a possible out-of-control situation and must be met with the laboratory’s corrective action process. Note that in many instances the laboratory will follow the prescribed limits as dictated in the respective analytical methods.

STATISTICAL REQUIREMENTS Arithmetic Mean (Average) Average = Sum of values/ n Where: n = Number of values Geometric Mean (Measure of central tendancy for data points from a skewed distribution) Geometric Mean = [(x1)(x2)…(xn)]1/2

Confidence Limit (95%) 95%CL = average +/- 1.96 s Limits of the range of analytical values within which a single analysis will be included 95% of the time Shifts and Trends The probability is 1:32 that 5 consecutive results will either be above or all below the mean value. When 5 or more consecutive values are in one direction, it is a good indication that the test is moving out of control.

CURVE LINE FITTING (REGRESSION ANALYSIS)

The majority of the analytical methods require the generation of a multi-point calibration curve before sample analysis. One method of evaluating a “goodness of fit” is to use regression analysis. A single straight line that lies closest to all of the points on a scatter plot is known as a regression line. Curves can also be evaluated through the use of correlation coefficients. This technique is used for external standard calibration. The computer software will generate the formulas and equations for verifying calibration curves. 1) Slope – Intercept Form: Y = ax + b Where: y = Instrument response a = Slope x = concentration of calibration standard


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b = intercept 2) Correlation Coefficient (r): – “goodness of fit” • Value of r > 0.990 for SW-846 methods. • Value of r > 0.995 for drinking water methods. If the r value fails, another model must pass to achieve an acceptable calibration curve. 3) Quadratic Model:

y = ax2 + bx + c

4) Coefficient of Determination (Curve fitting):

( )

( )

yy

Yypn1nyy

COD n

1i

2obs

n

1i

2iobs

2n

1iobs

∑

∑∑

=

==

−

−⎟⎟⎠

⎞⎜⎜⎝

⎛−−

−⎟⎠⎞

⎜⎝⎛ −

=

Where: yobs = Observed response (area) for each concentration from each initial calibration standard. _ y = Mean observed response from the initial calibration. Yi = Calculated (or predicted) response at each concentration from the initial calibration(s). n = Total number of calibration points (i.e., 6 for a quadratic model; 7 for a third order model). p = Number of adjustable parameters in the polynomial equation (i.e., 3 for a third order; 2 for a second order polynomial).


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AVERAGE RESPONSE FACTOR When using the internal standard calibration technique the average response factor is evaluated. Method specific criteria are listed in the technical SOP for an acceptable percent relative standard deviation (% RSD) for the average response factor. When this criteria is met, it is assumed the calibration is linear and the data are calculated from the average response factor.

STATISTICAL REQUIREMENTS

Arithmetic Mean (Average) n valuesof sum Average=

Where: n = Number of values Geometric Mean (Measure of central tendency for data points from a skewed distribution)

( )( ) ( )[ ]xxx n21 Mean Geometric 21

K=

Confidence Limit (95%) s 1.96 average 95%CL ±= Limits of the range of analytical values within which a single analysis will be included 95% of the time


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19.0 EQUATIONS AND DEFINITIONS

Note: Most of these calculations are performed by the computer analysis software Relative Percent Difference (Precision) The Relative Percent Difference (RPD) is used to assess the precision of a measurement based upon replicate samples. The value of RPD is obtained from the following equation:

RPD = | (x1 - x2) | * 100 (x1 + x2)/2

Where: x1 and x2 = observed measurements. The actual RPD of all duplicated and replicate samples will be determined and compared to the limits given. Any samples that are outside the acceptance criteria require corrective action and follow-up. Percent Recovery (Accuracy) The percent recovery is used to assess the accuracy of a sampling and analysis procedure through the use of matrix spikes. The value of the percent recovery is obtained from the following equation:

% Recovery = 100 * SSR-SR SA

Where: SSR = Spiked Sample Result SR = Sample Result SA = Spike Added Determination of invalid samples based upon percent recoveries is discussed on a case-by-case basis. Percent Relative Standard Deviation or Coefficient of Variance The percent of relative standard deviation (%RSD) is used to assess the precision of a series of runs in organic analyses. It is determined by:

%RSD = standard deviation * 100 mean


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Standard Deviation (s) The Standard Deviation for a sample group is defined as follows:

s = ( )y y

ni −

−∑ 2

1

Where: s = standard deviation yi = measured values of the ith replicate y = mean of the replicate measurements n = number of replicates Method Detection Limit (MDL) The Method Detection Limit for all measurements is defined as follows:

MDL = t (n-1, 1-α = 0.99) * s Where: MDL = Method Detection Limit s = standard deviation of the replicate analyses t = student’s t-value appropriate to a 99% confidence level and a standard deviation estimate with n-1 degree of freedom (t = 3.143 for 7 replicates) Practical Quantitation Limit (PQL) The Practical Quantitation Limit or Reporting Limit is defined to be the actual limit used to report with confidence of the ability to see a particular analyte at this level. The PQL is at least one to ten times greater than the MDL. The PQL or RL is the lowest concentration of the standard from the calibration curve. Percent Dry Weight % DW = (g of dry sample/g of wet sample) x 100 based on 5-10 g dried overnight at 105° C. Sediment, soil, and sludge samples are reported on a dry weight basis. Dry Weight PQL PQL = Non adjusted PQL/ percent solids For soil samples, the PQL must be adjusted for non-detectable compounds as a true measurement of the soil value. Notation: Based upon the matrix of samples within an analytical run, the comparability of data is evaluated with replicate or duplicate samples. This is a precision measurement. Furthermore, because of the various matrices received by the laboratory for environmental parameters, samples can be batched as a representative matrix such as a sludge, soil, solid, or aqueous.


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Response Factor (RF)

( )( )( )( )CA

CAsis

iss RF =

Where: As = Response for parameter in standard Ais = Response for internal standard in standard Cis = Concentration (µg/L) of internal standard Cs = Concentration (µg/L) of parameter Organic Concentration (µg/L)

( ) ( )( )( )( )( )VA

IAois

ssL

g

RF C =μ

Where: As = Response of parameter in sample Ais = Response of internal standard in sample Is = Amount of internal standard added to each extract (µg) Vi = Initial volume of water extracted (L) Mean Response Factor (RF)

∑= n RF RFi

Where: RFi = individual Response factor (i…n) Soil Concentration (µg/kg) example

( ) ( )( )( )( )( )( )( )( )DRF

CWVA

VIAsiis

tsxkg

g =μ

Where: Ax = Area of compound of interest RF = Response factor Vi = Volume of extract added for purging D = Dilution factor Ws = Weight of sample in grams Vt = Volume of total extract Ais = Area of internal standard Is = Internal standard conc


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Peak Gaussian Factor

( )( )10

1

21

W W 1.83 PGF ×

=

Where: W(1/2) = Peak width at half height W(1/10) = Peak width at tenth height Resolution

wt R =

Where: t = difference in elution times between two peaks w = average peak width at the baseline of two peaks

DEFINITIONS Some common definitions used by the laboratory to determine quality control acceptance criteria include the following: AETS-Alloway Environmental Testing Services Audit – A systematic evaluation to determine the conformance to quantitative and qualitative specification of some operational function or activity. Acceptance Criteria- Specified limits placed on characteristics of an item, process, or service defined in requirement documents. Accreditation- The process by which an agency or organization evaluates and recognizes a laboratory as meeting certain predetermined qualifications or standards, thereby accrediting the laboratory. Accuracy-The degree of agreement between an observed value and an accepted reference value. Accuracy includes a combination of random error (precision) and systematic error (bias) components which are due to sampling and analytical operations; a data quality indicator. Aliquot - A portion of the field sample to be processed through the analytical steps Analytical Batch – Composed of prepared environmental samples (extracts, digestates, or concentrates) which are analyzed together as a group. An analytical batch can include prepared samples originating from various environmental matrices. Bias- Consistent deviation of measured values from the true value. Blind Sample – A sub-sample for analysis with a composition known to the submitter. The analyst/technician/laboratory may know the identity of the sample but not its composition. It is used to test the analyst/technician’s or laboratory’s proficiency in the execution of the measurement process.


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Calibration – To determine, by measurement or comparison with a standard, the correct value of each scale reading on a meter, instrument, or other device. The levels of the applied calibration standard must bracket the range of planned or expected sample measurements. Calibration Curve – The graphical relationship between the known values, such as concentrations, of a series of calibration standards and their instrument response. Calibration Standard – A substance or reference material used to calibrate an instrument. Certified Reference Material - a reference material one or more of whose property values are certified by a technically valid procedure, accompanied by or traceable to a certificate or other documentation issued by a certifying body. Chain of Custody - record that details the possession of the analytical samples from the time of collection to receipt in the laboratory. Continuing Calibration Check - A check standard analyzed periodically to evaluate whether the analytical process remains in control. These results are compared to the initial calibration. Confidence Coefficient - The probability that a measured result will be within a specified confidence interval. Corrective Action – The action taken to eliminate the causes of an existing nonconformity, defect or other undesirable situation in order to prevent recurrence. Data Quality Indicators – Quantitative statistics and qualitative descriptions that are used to interpret the degree of acceptability or utilization of data to the user. Demonstration of Capability – A procedure to establish the ability of the analyst/technician to generate acceptable accuracy. Document Control – The act of ensuring that documents are proposed, reviewed for accuracy, approved for release by authorized personnel, distributed properly and controlled to ensure use of the correct version at the location where the prescribed activity is performed. Duplicate Analyses- The analyses or measurements of the variable of interest performed identically on two sub-samples of the same sample. The results from duplicate analyses are used to evaluate analytical or measurement precision but not the precision of sampling, preservation or storage internal to the laboratory. EDDs – Electronic Deliverables. Field Blank - a reagent blank prepared in the field by filling a clean container with pure deionized water and appropriate preservation. Gas Chromatograph – main instrument for performing organics testing Holding Times (Maximum Allowable Holding Times) – The maximum times that samples are be held prior to analysis and still be considered valid or not compromised. Homogeneous Sample - A sample which has an even distribution of material . Instrument Blank - a clean sample processed through the instrumental steps of the measurement process. Limit of Detection (LOD) – The lowest concentration level that can be determined by a single analysis and with a defined level of confidence to be statistically different from a blank.


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Instrument Detection Limit - The minimum concentration of an analyte that can be measured with 99% confidence that the analyte concentration is greater than zero. Determine the IDL with seven replicates of standard solution at the instrument with no specific analytical preparation. Mass Spectrometer – detector utilized in organics testing coupled with gas chromatography Method Detection Limit - The minimum concentration of an analyte that can be measured with 99% confidence that the analyte concentration is greater than zero. Determine the MDL with seven replicates of standard solution taken through the preparative and analytical procedures. Initial Calibration - A series of standards analyzed to produce a calibration curve in order to develop a linear system. Internal Standard – A known amount of standard added to a test portion of a sample as a reference for evaluating and controlling the precision and bias of the applied analytical method. Laboratory Control Sample – A sample matrix, free from the analytes of interest, spiked with verified known amounts of analytes from a source independent of the calibration standards or a material containing known and verified amounts of analytes. It is generally used to establish intra-laboratory or analyst/technician specific precision and bias or to assess the performance of all or a portion of he measurement system. LIMS – Laboratory Information Management System. Matrix- The component or substrate that contains the analyte of interest. Matrix Spike – A sample prepared by adding a known mass of target analyte to a specified amount of matrix sample for which an independent estimate of target analyte is available. Matrix spikes are used, for example, to determine the effect of the matrix on a method’s recovery efficiency. Matrix Spike Duplicate – A second replicate matrix spike prepared in the laboratory and analyzed to obtain a measure of the precision of the recovery for each analyte. Precision- The degree to which a set of observations or measurements of the same property, obtained under similar condition, conform to themselves; a data quality indicator. Precision is usually expressed as standard deviation, variance or range, in either absolute or relative terms. Preservation – Refrigeration and/or reagents added at the time of sample collection (or later) to maintain the chemical and/or biological integrity of the sample. Proficiency Testing – A means of evaluating a laboratory’s performance under controlled conditions relative to a given set of criteria through analysis of unknown samples provided by an external source. Proficiency Testing Sample - a sample, the composition of which is unknown to the analyst and is provided to test whether the laboratory can produce analytical results within the specified acceptance criteria. Quality Assurance – An integrated system of activities involving planning, quality control, quality assessment, reporting and quality improvement to ensure that a product or service meets defined standards of quality with a stated level of confidence. Quality Assurance Manual – A document stating the management policies, objectives, principles, organizational structure and authority, responsibilities, accountability, and implementation plan of an


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organization for ensuring quality in its work processes, products, and services. The quality system provides the framework for planning, implementing, and assessing work performed by the organization and for carrying out required QA and QC. Quality Assurance Project Plan (QAPP) – A formal document describing the detailed quality control procedures by which the quality requirements defined for the data and decisions pertaining to a specific project are to be achieved. Quality Control – The overall system of technical activities whose purpose is to measure and control the quality of a product or service so that it meets the needs of users. Random Error - A deviation in a step of an analytical procedure that can be treated by statistical technique. Reagent Blank or Method Blank – A sample consisting of reagent(s), without the target analyte or sample matrix, introduced into the analytical procedure at the appropriate point and carried through all subsequent steps to determine the contribution of the reagents and of the involved analytical steps. Reference Method – A method of known and documented accuracy and precision issued by an organization recognized as competent to do so. Reference Standard – A standard, generally of the highest metrological quality available at a given location, from which measurements made at that location are derived. Regulatory Level - A concentration of a contaminant which is cited in federal or state regulations. Reporting Limit - The practical quantitation level for an analyte, greater than the MDL, accounting for dilutions and matrix specific concerns. Reporting Limit Check – A quality control check at the PQL to ensure report validity. Sample Duplicate – Two samples taken from and representative of the same population and carried through all steps of the sampling and analytical procedures in an identical manner. Duplicate samples are used to assess variance of the total method including sampling and analysis. Spike – A known mass of target analyte added to a blank sample or sub-sample; used to determine the recovery efficiency or for other quality control purposes. Standard Operating Procedures (SOPs) – A written document which details the method of an operation, analysis or action whose techniques and procedures are thoroughly prescribed and which is accepted as the method for performing certain routine or repetitive tasks. Systems Audit – A thorough, systematic, qualitative on-site assessment of the facilities, equipment, personnel, training, procedures, record-keeping, data validation, data management, and reporting aspects of a total measurement system. Surrogate – a compound that is similar in chemical nature to a target compound that is utilized to measure extraction and analytical soundness. Traceability – The property of a measurement whereby it can be related to appropriate standards through an unbroken chain of custody. Trip Blank - A sample which is prepared at the laboratory with reagent water and utilized on-site to detect any contamination from the site or from the container in which it is stored.


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Type I Error - Probability of deciding a constituent is present when it actually is absent. Type II Error - Probability of not detecting a constituent when it actually is present. Validation – The process of substantiating specified performance criteria.


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Chemistry Quality Assurance Manual for Chemistry Analyses

Alloway Environmental Laboratories-

Marion Lab

Appendix 1 Laboratory Equipment List


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Marion Lab

Appendix 2 Laboratory Organization Chart


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Marion Lab

Appendix 3 State Certification Table


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Marion Lab

Appendix 4 Internal Audit Report


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ALLOWAY

INTERNAL AUDIT REPORT-Revised February 2008

The following pages present the criteria from ISO/IEC Guide 17025, "General Requirements for the competence of testing and calibration laboratories" in a checklist format. The Internal Audit Report has also been designed to incorporate those items listed under the National Environmental Laboratory Accreditation Conference (NELAC) July 1, 2004 standards. The NELAC standard checklist may also be utilized as the template for the internal audit report. This report may also be utilized for other state/regulatory authorities. As appropriate, comments should be made at the end of the report for specific items such as standard operating procedure revisions and document revisions. Note to auditors: (a) Place a tick mark (*) in the Yes, No, or Not Applicable space for each item. (b) Complete the document reference where applicable. (c) Note any special comments. (d) Attach additional pages if necessary. Auditor's Name _______________________________________ Auditor's Signature _______________________________________ Date of Audit _______________________________________ Date of Audit _______________________________________ Completion


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Compliance Requirement Y N NA

Reference

4.1.1 The laboratory or the organization of which it is part shall be an entity that can be held legally responsible.

4.1.2 It is the responsibility of the laboratory to carry out its testing and calibration activities in such a way as to meet the requirements of this International Standard and to satisfy the needs of the client, the regulatory authorities or organizations providing recognition.

4.1.3 The laboratory management system shall cover work carried out in the laboratory's permanent facilities, at sites away from its permanent facilities, or in associated temporary or mobile facilities.

4.1.4 If the laboratory is part of an organization performing activities other than testing and/or calibration, the responsibilities of key personnel in the organization that have an involvement or influence on the testing and/or calibration activities of the laboratory shall be defined in order to identify potential conflicts of interest.

4.1.5 The laboratory shall

a) have managerial and technical personnel with the authority and resources needed to carry out their duties and to identify the occurrence of departures from the quality system or from the procedures for performing tests and/or calibrations, and to initiate actions to prevent or minimize such departures

b) have arrangements to ensure that its management and personnel are free from any undue internal and external commercial, financial and other pressures and influences that may adversely affect the quality of their work;

c) have policies and procedures to ensure the protection of its clients' confidential information and proprietary rights, including procedures for protecting the electronic storage and transmission of results;

d) have policies and procedures to avoid involvement in any activities that would diminish confidence in its competence, impartiality, judgement or operational integrity;

e) define the organization and management structure of the laboratory, its place in any parent organization, and the relationships between quality management, technical operations and support services;

f) specify the responsibility, authority and interrelationships of all personnel who manage, perform or verify work affecting the quality of the tests and/or calibrations;


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Reference

g) provide adequate supervision of testing and calibration staff, including trainees, by persons familiar with methods and procedures, purpose of each test and/or calibration, and with the assessment of the test or calibration results;

h) have technical management which has overall responsibility for the technical operations and the provision of the resources needed to ensure the required quality of laboratory operations;

i) appoint a member of staff as quality manager (however named) who, irrespective of other duties and responsibilities, shall have defined responsibility and authority for ensuring that the quality system is implemented and followed at all times;

the quality manager shall have direct access to the highest level of management at which decisions are made on laboratory policy or resources;

j) appoint deputies for key managerial personnel

4.2.1 The laboratory shall establish, implement and maintain a quality system appropriate to the scope of its activities. The laboratory shall document its policies, systems, programs, procedures and instructions to the extent necessary to assure the quality of the test and/or calibration results.

The system's documentation shall be communicated to, understood by, available to, and implemented by the appropriate personnel.

4.2.2 The laboratory's quality system policies and objectives shall be defined in a quality manual (however named).

The overall objectives shall be documented in a quality policy statement. The quality policy statement shall be issued under the authority of the chief executive. It shall include at least the following:

a) the laboratory management's commitment to good professional practice and to the quality of its testing and calibration in servicing its clients;

b) the management's statement of the laboratory's standard of service;

c) the objectives of the quality system;

d) a requirement that all personnel concerned with testing and calibration activities within the laboratory familiarize themselves with the quality documentation and implement the policies and procedures in their work; and

e) the laboratory management's commitment to compliance with this International Standard.


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Reference

4.2.3 The quality manual shall include or make reference to the supporting procedures including technical procedures. It shall outline the structure of the documentation used in the quality system.

• QAM shall provide procedures for feedback and corrective action

• Arrangements for exceptionally permitting departures from documented policies and procedures

• Procedures for handling complaints

• Procedures for protecting confidentiality

• Procedures for audits and data review

• Training procedures

• Reference to procedures for reporting analytical results

• Table of contents, references, and appendices

• Data Integrity Training and ethics training


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Reference

4.2.4 The roles and responsibilities of technical management and the quality manager, including their responsibility for ensuring compliance with this International Standard, shall be defined in the quality manual.

The quality manual shall also contain or make reference to another internal document of:

• A quality policy statement including objective and commitments by top management

• Organization and management structure of the lab and its place in any parent organization plus organizational charts

• Relationship between management, technical operations, support services and the quality system

• Procedures to ensure that all records are retained for a minimum of ten years

• Job descriptions of key staff and reference to the job descriptions of other staff

• Identification of the laboratory's approved signatories

• Laboratory's procedures for achieving traceability of measurements

• A list of all test methods under which the laboratory performs its accredited testing

• Mechanisms for ensuring the laboratory reviews all new work

• Reference to the calibration or verification procedures used

4.3.1 General

The laboratory shall establish and maintain procedures to control all documents that form part of its quality system (internally generated or from external sources), such as regulations, standards, other normative documents, test and/or calibration methods, as well as drawings, software, specifications, instructions and manuals.

4.3.2.1 All documents issued to personnel in the laboratory as part of the quality system shall be reviewed and approved for use by authorized personnel prior to issue.

A master list or an equivalent document control procedure identifying the current revision status and distribution of documents in the quality system shall be established and be readily available to preclude the use of invalid and/or obsolete documents.


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4.3.2.2 The procedure adopted shall ensure that:

a) authorized editions of appropriate documents are available at all locations where operations essential to the effective functioning of the laboratory are performed;

b) documents are periodically reviewed and, where necessary, revised to ensure continuing suitability and compliance with applicable requirements;

c) invalid or obsolete documents are promptly removed from all points of issue or use, or otherwise assured against unintended use;

d) obsolete documents retained for either legal or knowledge preservation purposes are suitably marked.

4.3.2.3 Quality system documents generated by the laboratory shall be uniquely identified. Such identification shall include the date of issue and/or revision identification, page numbering, the total number of pages or a mark to signify the end of the document, and the issuing authority(ies).

4.3.3.1 Changes to documents shall be reviewed and approved by the same function that performed the original review unless specifically designated otherwise. The designated personnel shall have access to pertinent background information upon which to base their review and approval.

4.3.3.2 Where practicable, the altered or new text shall be identified in the document or the appropriate attachments.

4.3.3.3 If the laboratory's documentation control system allows for the amendment of documents by hand pending the re-issue of the documents, the procedures and authorities for such amendments shall be defined.

Amendments shall be clearly marked, initialed and dated. A revised document shall be formally re-issued as soon as practicable.

4.3.3.4 Procedures shall be established to describe how changes in documents maintained in computerized systems are made and controlled.


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Compliance Requirement

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4.4.1 The laboratory shall establish and maintain procedures for the review of requests, tenders and contracts. The policies and procedures for these reviews leading to a contract for testing and/or calibration shall ensure that:

a) the requirements, including the methods to be used, are adequately defined, documented and understood (see 5.4.2);

b) the laboratory has the capability and resources to meet the requirements;

c) the appropriate test and/or calibration method is selected and capable of meeting the clients' requirements (see 5.4.2).

Any differences between the request or tender and the contract shall be resolved before any work commences. Each contract shall be acceptable both to the laboratory and the client.

4.4.2 Records of reviews, including any significant changes, shall be maintained. Records shall also be maintained of pertinent discussions with a client relating to the client's requirements or the results of the work during the period of execution of the contract.

4.4.3 The review shall also cover any work that is subcontracted by the laboratory.

4.4.4 The client shall be informed of any deviation from the contract.

4.4.5 If a contract needs to be amended after work has commenced, the same contract review process shall be repeated and any amendments shall be communicated to all affected personnel.


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Compliance Requirement

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4.5.1 When a laboratory subcontracts work whether because of unforeseen reasons (e.g. workload, need for further expertise or temporary incapacity) or on a continuing basis (e.g. through permanent subcontracting, agency or franchising arrangements), this work shall be placed with a competent subcontractor. A competent subcontractor is one that, for example, complies with this International Standard for the work in question.

4.5.2 The laboratory shall advise the client of the arrangement in writing and, when appropriate, gain the approval of the client, preferably in writing.

4.5.3 The laboratory is responsible to the client for the subcontractor's work, except in the case where the client or a regulatory authority specifies which subcontractor is to be used.

4.5.4 The laboratory shall maintain a register of all subcontractors that it uses for tests and/or calibrations and a record of the evidence of compliance with this International Standard for the work in question.

4.6.1 The laboratory shall have a policy and procedure(s) for the selection and purchasing of services and supplies it uses that affect the quality of the tests and/or calibrations.

Procedures shall exist for the purchase, reception and storage of reagents and laboratory consumable materials relevant for the tests and calibrations.

4.6.2 The laboratory shall ensure that purchased supplies and reagents and consumable materials that affect the quality of tests and/or calibrations are not used until they have been inspected or otherwise verified as complying with standard specifications or requirements defined in the methods for the tests and/or calibrations concerned. These services and supplies used shall comply with specified requirements.

Records of actions taken to check compliance shall be maintained.

4.6.3 Purchasing documents for items affecting the quality of laboratory output shall contain data describing the services and supplies ordered. These purchasing documents shall be reviewed and approved for technical content prior to release.

4.6.4 The laboratory shall evaluate suppliers of critical consumables, supplies and services which affect the quality of testing and calibration, and shall maintain records of these evaluations and list those approved.

The laboratory shall afford clients or their representatives cooperation to clarify the client's request and to monitor the laboratory's performance in relation to the work performed, provided that the laboratory ensures confidentiality to other clients.


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The laboratory shall have a policy and procedure for the resolution of complaints received from clients or other parties. Records shall be maintained of all complaints and of the investigations and corrective actions taken by the laboratory (see also 4.10).

4.9.1 The laboratory shall have a policy and procedures that shall be implemented when any aspect of its testing and/or calibration work, or the results of this work, do not conform to its own procedures or the agreed requirements of the client. The policy and procedures shall ensure that:

a) the responsibilities and authorities for the management of nonconforming work are designated and actions (including halting of work and withholding of test reports and calibration certificates, as necessary) are defined and taken when nonconforming work is identified;

b) an evaluation of the significance of the nonconforming work is made;

c) corrective actions are taken immediately by Alloway, together with any decision about the acceptability of the nonconforming work;

d) where necessary, the client is notified and work is recalled;

e) the responsibility for authorizing the resumption of work is defined.

4.9.2 Where the evaluation indicates that the nonconforming work could recur or that there is doubt about the compliance of the laboratory's operations with its own policies and procedures, the corrective action procedures given in 4.10 shall be promptly followed.

4.10.1 General The laboratory shall establish a policy and procedure and shall designate appropriate authorities for implementing corrective action when nonconforming work or departures from the policies and procedures in the quality system or technical operations have been identified.

4.10.2 Cause analysis The procedure for corrective action shall start with an investigation to determine the root cause(s) of the problem.

4.10.3 Selection and implementation of corrective actions Where corrective action is needed, the laboratory shall identify potential corrective actions. It shall select and implement the action(s) most likely to eliminate the problem and to prevent recurrence.

Corrective actions shall be to a degree appropriate to the magnitude and the risk of the problem.


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The laboratory shall document and implement any required changes resulting from corrective action investigations.

4.10.4 Monitoring of corrective actions The laboratory shall monitor the results to ensure that the corrective actions taken have been effective.

4.10.5 Additional audits Where the identification of nonconformances or departures casts doubts on the laboratory's compliance with its own policies and procedures, or on its compliance with this International Standard, the laboratory shall ensure that the appropriate areas of activity are audited in accordance with 4.13 as soon as possible.

4.11.1 Needed improvements and potential sources of nonconformances, either technical or concerning the quality system, shall be identified.

If preventive action is required, action plans shall be developed, implemented and monitored to reduce the likelihood of the occurrence of such nonconformances and to take advantage of the opportunities for improvement.

4.11.2 Procedures for preventive actions shall include the initiation of such actions and application of controls to ensure that they are effective.

4.12.1.1 The laboratory shall establish and maintain procedures for identification, collection, indexing, access, filing, storage, maintenance and disposal of quality and technical records. Quality records shall include reports from internal audits and management reviews as well as records of corrective and preventive actions.

4.12.1.2 All records shall be legible and shall be stored and retained in such a way that they are readily retrievable in facilities that provide a suitable environment to prevent damage or deterioration and to prevent loss.

Retention times of records shall be established.

4.12.1.3 All records shall be held secure and in confidence.

4.12.1.4 The laboratory shall have procedures to protect and back-up records stored electronically and to prevent unauthorized access to or amendment of these records.

4.12.2.1 The laboratory shall retain records of original observations, derived data and sufficient information to establish an audit trail, calibration records, staff records and a copy of each test report or calibration certificate issued, for a defined period.


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The records for each test or calibration shall contain sufficient information to facilitate, if possible, identification of factors affecting the uncertainty and to enable the test or calibration to be repeated under conditions as close as possible to the original.

The records shall include the identity of personnel responsible for the sampling, performance of each test and/or calibration and checking of results.

4.12.2.2 Observations, data and calculations shall be recorded at the time they are made and shall be identifiable to the specific task.

4.12.2.3 When mistakes occur in records, each mistake shall be crossed out, not erased, made illegible or deleted, and the correct value entered alongside. All such alterations to records shall be signed or initialed by the person making the correction.

In the case of records stored electronically, equivalent measures shall be taken to avoid loss or change of original data.

4.13.1 The laboratory shall periodically, and in accordance with a predetermined schedule and procedure, conduct internal audits of its activities to verify that its operations continue to comply with the requirements of the quality system and this International Standard.

The internal audit program shall address all elements of the quality system, including the testing and/or calibration activities.

It is the responsibility of the quality manager to plan and organize audits as required by the schedule and requested by management.

Such audits shall be carried out by trained and qualified personnel who are, wherever resources permit, independent of the activity to be audited.

4.13.2 When audit findings cast doubt on the effectiveness of the operations or on the correctness or validity of the laboratory's test or calibration results, the laboratory shall take timely corrective action, and shall notify clients in writing if investigations show that the laboratory results may have been affected.

4.13.3 The area of activity audited, the audit findings and corrective actions that arise from them shall be recorded.

4.13.4 Follow-up audit activities shall verify and record the implementation and effectiveness of the corrective action taken.

4.14.1 In accordance with a predetermined schedule and procedure, the laboratory's executive management shall periodically conduct a review of the laboratory's quality system and testing and/or calibration activities to ensure their continuing suitability and effectiveness, and to introduce necessary changes or improvements. The review shall take account of:

the suitability of policies and procedures;


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reports from managerial and supervisory personnel;

The outcome of recent internal audits;

corrective and preventive actions;

assessments by external bodies;

the results of interlaboratory comparisons or proficiency tests;

changes in the volume and type of the work;

client feedback;

complaints;

other relevant factors, such as quality control activities, resources and staff training.

4.14.2 Findings from management reviews and the actions that arise from them shall be recorded.

The management shall ensure that those actions are carried out within an appropriate and agreed timescale.

5.1.1 Many factors determine-the correctness and reliability of the-tests and/or calibrations performed by a laboratory. These factors include contributions from:

- human factors (5.2);

- accommodation and environmental conditions (5·3);

- test and calibration methods and method validation (5.4);

- equipment (5.5);

- measurement traceability (5.6);

- sampling (5.7);

- the handling of test and calibration items (5.8).

5.1.2 The extent to which the factors contribute to the total uncertainty of measurement differs considerably between (types of) tests and between (types of) calibrations. The laboratory shall take account of these factors in developing test and calibration methods and procedures, in the training and qualification of personnel, and in the selection and calibration of the equipment it uses.

5.2.1 The laboratory management shall ensure the competence of all who operate specific equipment, perform tests and/or calibrations, evaluate results, and sign test reports and calibration certificates.

When using staff that are undergoing training, appropriate supervision shall be provided.


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Personnel performing specific tasks shall be qualified on the basis of appropriate education, training, experience and/or demonstrated skills, as required.

5.2.2 The management of the laboratory shall formulate the goals with respect to the education, training and skills of the laboratory personnel.

The laboratory shall have a policy and procedures for identifying training needs and providing training of personnel. The training program shall be relevant to the present and anticipated tasks of the laboratory.

5.2.3 The laboratory shall use personnel who are employed by, or under contract to, the laboratory. Where contracted and additional technical and key support personnel are used, the laboratory shall ensure that such personnel are supervised and competent and that they work in accordance with the laboratory's quality system.

5.2.4 The laboratory shall maintain current job descriptions for managerial, technical and key support personnel involved in tests and/or calibrations.

5.2.5 The management shall authorize specific personnel to perform particular types of sampling, test and/or calibration, to issue test reports and calibration certificates, to give opinions and interpretations and to operate particular types of equipment.

The laboratory shall maintain records of the relevant authorization(s), competence, educational and professional qualifications, training, skills and experience of all technical personnel, including contracted personnel. This information shall be readily available and shall include the date on which authorization and/or competence is confirmed.

5.3.1 Laboratory facilities for testing and/or calibration, including but not limited to energy sources, lighting and environmental conditions, shall be such as to facilitate correct performance of the tests and/or calibrations.

The laboratory shall ensure that the environmental conditions do not invalidate the results or adversely affect the required quality of any measurement. Particular care shall be taken when sampling and tests and/or calibrations are undertaken at sites other than a permanent laboratory facility.

The technical requirements for accommodation and environmental conditions that can affect the results of tests and calibrations shall be documented.


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5.3.2 The laboratory shall monitor, control and record environmental conditions as required by the relevant specifications, methods and procedures or where they influence the quality of the results. Due attention shall be paid, for example, to biological sterility, dust, electromagnetic disturbances, radiation, humidity, electrical supply, temperature, and sound and vibration levels, as appropriate to the technical activities concerned.

Tests and calibrations shall be stopped when the environmental conditions jeopardize the results of the tests and/or calibrations.

5.3.3 There shall be effective separation between neighboring areas in which there are incompatible activities. Measures shall be taken to prevent cross-contamination.

5.3.4 Access to and use of areas affecting the quality of the tests and/or calibrations shall be controlled. The laboratory shall determine the extent of control based on its particular circumstances.

5.35 Measures for good housekeeping

5.4.1 General The laboratory shall use appropriate methods and procedures for all tests and/or calibrations within its scope. These include sampling, handling, transport, storage and preparation of items to be tested and/or calibrated, and, where appropriate, an estimation of the measurement uncertainty as well as statistical techniques for analysis of test and/or calibration data.

The laboratory shall have instructions on the use and operation of all relevant equipment, and on the handling and preparation of items for testing and/or calibration, or both, where the absence of such instructions could jeopardize the results of tests and/or calibrations.

All instructions, standards, manuals and reference data relevant to the work of the laboratory shall be kept up to date and shall be made readily available to personnel (see 4.3).

Deviation from test and calibration methods shall occur only if the deviation has been documented, technically justified, authorized, and accepted by the client.

5.4.2 Selection of methods

The laboratory shall use test and/or calibration methods, including methods for sampling, which meet the needs of the client and which are appropriate for the tests and/or calibrations it undertakes. Methods published in international, regional or national standards shall preferably be used.

The laboratory shall ensure that it uses the latest valid edition of a standard unless it is not appropriate or possible to do so. When necessary, the standard shall be supplemented with additional details to ensure consistent application.


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When the client does not specify the method to be used, the laboratory shall select appropriate methods that have been published either in international, regional or national standards, or by reputable technical organizations, or in relevant scientific texts or journals, or as specified by the manufacturer of the equipment. Laboratory-developed methods or methods adopted by the laboratory may also be used if they are appropriate for the intended use and if they are validated.

The client shall be informed as to the method chosen.

The laboratory shall confirm that it can properly operate standard methods before introducing the tests or calibrations. If the standard method changes, the confirmation shall be repeated.

The laboratory shall inform the client when the method proposed by the client is considered to be inappropriate or out of date.

5.4.3 Laboratory-developed methods

The introduction of test and calibration methods developed by the laboratory for its own use shall be a planned activity and shall be assigned to qualified personnel equipped with adequate resources.

Plans shall be updated as development proceeds and effective communication amongst all personnel involved shall be ensured.

5.4.4 Non-standard methods

When it is necessary to use methods not covered by standard methods, these shall be subject to agreement with the client and shall include a clear specification of the client's requirements and the purpose of the test and/or calibration. The method developed shall have been validated appropriately before use.

5.4.5.1 Validation is the confirmation by examination and the provision of objective evidence that the particular requirements for a specific intended use are fulfilled.

5.4.5.2 The laboratory shall validate non-standard methods, laboratory-designed/developed methods, standard methods used outside their intended scope, and amplifications and modifications of standard methods to confirm that the methods are fit for the intended use. The validation shall be as extensive as is necessary to meet the needs of the given application or field of application. The laboratory shall record the results obtained, the procedure used for the validation, and a statement as to whether the method is fit for the intended use.


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5.4.5.3 The range and accuracy of the values obtainable from validated methods (e.g. the uncertainty of the results, detection limit, selectivity of the method, linearity, limit of repeatability and/or reproducibility, robustness against external influences and/or cross-sensitivity against interference from the matrix of the sample/test object), as assessed for the intended use, shall be relevant to the clients' needs.

5.4.6.1 A calibration laboratory, or a testing laboratory performing its own calibrations, shall have and shall apply a procedure to estimate the uncertainty of measurement for all calibrations and types of calibrations.

5.4.6.2 Testing laboratories shall have and shall apply procedures for estimating uncertainty of measurement. In certain cases the nature of the test method may preclude rigorous, metrologically and statistically valid, calculation of uncertainty of measurement. In these cases the laboratory shall at least attempt to identify all the components of uncertainty and make a reasonable estimation, and shall ensure that the form of reporting of the result does not give a wrong impression of the uncertainty. Reasonable estimation shall be based on knowledge of the performance of the method and on the measurement scope and shall make use of, for example, previous experience and validation data.

5.4.6.3 When estimating the uncertainty of measurement, all uncertainty components which are of importance in the given situation shall be taken into account using appropriate methods of analysis.

5.4.7.1 Calculations and data transfers shall be subject to appropriate checks in a systematic manner.

5.4.7.2 When computers or automated equipment are used for the acquisition, processing, recording, reporting, storage or retrieval of test or calibration data, the laboratory shall ensure that:

a) computer software developed by the user is documented in sufficient detail and is suitably validated as being adequate for use;

b) procedures are established and implemented for protecting the data; such procedures shall include, but not be limited to, integrity and confidentiality of data entry or collection, data storage, data transmission and data processing;

c) computers and automated equipment are maintained to ensure proper functioning and are provided with the environmental and operating conditions necessary to maintain the integrity of test and calibration data.


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5.5.1 The laboratory shall be furnished with all items of sampling, measurement and test equipment required for the correct performance of the tests and/or calibrations (including sampling, preparation of test and/or calibration items, processing and analysis of test and/or calibration data).

In those cases where the laboratory needs to use equipment outside its permanent control, it shall ensure that the requirements of this International Standard are met.

5.5.2 Equipment and its software used for testing, calibration and sampling shall be capable of achieving the accuracy required and shall comply with specifications relevant to the tests and/or calibrations concerned.

Calibration programs shall be established for key quantities or values of the instruments where these properties have a significant effect on the results.

Before being placed into service, equipment (including that used for sampling) shall be calibrated or checked to establish that it meets the laboratory's specification requirements and complies with the relevant standard specifications. It shall be checked and/or calibrated before use (see 5.6).

5.5.3 Equipment shall be operated by authorized personnel.

Up-to-date instructions on the use and maintenance of equipment (including any relevant manuals provided by the manufacturer of the equipment) shall be readily available for use by the appropriate laboratory personnel.

5.5.4 Each item of equipment and its software used for testing and calibration and significant to the result shall, when practicable, be uniquely identified.

5.5.5 Records shall be maintained of each item of equipment and its software significant to the tests and/or calibrations performed. The records shall include at least the following:

a) the identity of the item of equipment and its software;

b) the manufacturer's name, type identification, and serial number or other unique identification;

c) checks that equipment complies with the specification (see 5.5.2);

d) the current location, where appropriate;

e) the manufacturer's instructions, if available, or reference to their location;

f) dates, results and copies of reports and certificates of all calibrations, adjustments, acceptance criteria, and the due date of next calibration;


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g) the maintenance plan, where appropriate, and maintenance carried out to date;

h) any damage, malfunction, modification or repair to the equipment.

5.5.6 The laboratory shall have procedures for safe handling, transport, storage, use and planned maintenance of measuring equipment to ensure proper functioning and in order to prevent contamination or deterioration.

5.5.7 Equipment that has been subjected to overloading or mishandling, gives suspect results, or has been shown to be defective or outside specified limits, shall be taken out of service. It shall be isolated to prevent its use or clearly labeled or marked as being out of service until it has been repaired and shown by calibration or test to perform correctly.

The laboratory shall examine the effect of the defect or departure from specified limits on previous tests and/or calibrations and shall institute the “Control of nonconforming work” procedure (see 4.9).

5.5.8 Whenever practicable, all equipment under the control of the laboratory and requiring calibration shall be labeled, coded or otherwise identified to indicate the status of calibration, including the date when last calibrated and the date or expiration criteria when recalibration is due.

5.5.9 When, for whatever reason, equipment goes outside the direct control of the laboratory, the laboratory shall ensure that the function and calibration status of the equipment are checked and shown to be satisfactory before the equipment is returned to service.

5.5.10 When intermediate checks are needed to maintain confidence in the calibration status of the equipment, these checks shall be carried out according to a defined procedure.

5.5.11 Where calibrations give rise to a set of correction factors, the laboratory shall have procedures to ensure that copies (e.g. in computer software) are correctly updated.

5.5.12 Test and calibration equipment, including both hardware and software, shall be safeguarded from adjustments which would invalidate the test and/or calibration results.

5.6.1 General

All equipment used for tests and/or calibrations, including equipment for subsidiary measurements (e.g. for environmental conditions) having a significant effect on the accuracy or validity of the result of the test, calibration or sampling shall be calibrated before being put into service.

The laboratory shall have an established program and procedure for the calibration of its equipment.


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5.6.2.1.1 For calibration laboratories, the program for calibration of equipment shall be designed and operated so as to ensure that calibrations and measurements made by the laboratory are traceable to the International System of Units (SI) (Système international d'unités).

A calibration laboratory establishes traceability of its own measurement standards and measuring instruments to the SI by means of an unbroken chain of calibrations or comparisons linking them to relevant primary standards of the SI units of measurement. The link to SI units may be achieved by reference to national measurement standards. National measurement standards may be primary standards, which are primary realizations of the SI units or agreed representations of SI units based on fundamental physical constants, or they may be secondary standards which are standards calibrated by another national metrology institute.

When using external calibration services, traceability of measurement shall be assured by the use of calibration services from laboratories that can demonstrate competence, measurement capability and traceability.

The calibration certificates issued by these laboratories shall contain the measurement results, including the measurement uncertainty and/or a statement of compliance with an identified metrological specification (see also 5.10.4.2).

5.6.2.1.2 There are certain calibrations that currently cannot be strictly made in SI units. In these cases calibration shall provide confidence in measurements by establishing traceability to appropriate measurement standards such as:

- the use of certified reference materials provided by a competent supplier to give a reliable physical or chemical characterization of a material;

- the use of specified methods and/or consensus standards that are clearly described and agreed by all parties concerned.

Participation in a suitable program of interlaboratory comparisons is required where possible.

5.6.2.2.1 For testing laboratories, the requirements given in 5.6.2.1 apply for measuring and test equipment with measuring functions used, unless it has been established that the associated contribution from the calibration contributes little to the total uncertainty of the test result. When this situation arises, the laboratory shall ensure that the equipment used can provide the uncertainty of measurement needed.


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5.6.2.2.2 Where traceability of measurements to SI units is not possible and/or not relevant, the same requirements for traceability to, for example, certified reference materials, agreed methods and/or consensus standards, are required as for calibration laboratories (see 5.6.2.1.2).

5.6.3.1 Reference standards

The laboratory shall have a program and procedure for the calibration of its reference standards.

Reference standards shall be calibrated by a body that can provide traceability as described in 5.6.2.1.

Such reference standards of measurement held by the laboratory shall be used for calibration only and for no other purpose, unless it can be shown that their performance as reference standards would not be invalidated.

Reference standards shall be calibrated before and after any adjustment.

5.6.3.2 Reference materials

Reference materials shall, where possible, be traceable to SI units of measurement, or to certified reference materials. Internal reference materials shall be checked as far as is technically and economically practicable.

5.6.3.3 Intermediate checks

Checks needed to maintain confidence in the calibration status of reference, primary, transfer or working standards and reference materials shall be carried out according to defined procedures and schedules.

5.6.3.4 Transport and storage

The laboratory shall have procedures for safe handling, transport, storage and use of reference standards and reference materials in order to prevent contamination or deterioration and in order to protect their integrity.

5.7.1 The laboratory shall have a sampling plan and procedures for sampling when it carries out sampling of substances, materials or products for subsequent testing or calibration.

The sampling plan as well as the sampling procedure shall be available at the location where sampling is undertaken.

Sampling plans shall, whenever reasonable, be based on appropriate statistical methods. The sampling process shall address the factors to be controlled to ensure the validity of the test and calibration results.


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5.7.2 Where the client requires deviations, additions or exclusions from the documented sampling procedure, these shall be recorded in detail with the appropriate sampling data and shall be included in all documents containing test and/or calibration results, and shall be communicated to the appropriate personnel.

5.7.3 The laboratory shall have procedures for recording relevant data and operations relating to sampling that forms part of the testing or calibration that is undertaken.

These records shall include the sampling procedure used, the identification of the sampler, environmental conditions (if relevant) and diagrams or other equivalent means to identify the sampling location as necessary and, if appropriate, the statistics the sampling procedures are based upon.

5.8.1 The laboratory shall have procedures for the transportation, receipt, handling, protection, storage, retention and/or disposal of test and/or calibration items, including all provisions necessary to protect the integrity of the test or calibration item, and to protect the interests of the laboratory and the client.

5.8.2 The laboratory shall have a system for identifying test and/or calibration items. The identification shall be retained throughout the life of the item in the laboratory. The system shall be designed and operated so as to ensure that items cannot be confused physically or when referred to in records or other documents. The system shall, if appropriate, accommodate a sub-division of groups of items and the transfer of items within and from the laboratory.

5.8.3 Upon receipt of the test or calibration item, abnormalities or departures from normal or specified conditions, as described in the test or calibration method, shall be recorded.

When there is doubt as to the suitability of an item for test or calibration, or when an item does not conform to the description provided, or the test or calibration required is not specified in sufficient detail, the laboratory shall consult the client for further instructions before proceeding and shall record the discussion.

5.8.4 The laboratory shall have procedures and appropriate facilities for avoiding deterioration, loss or damage to the test or calibration item during storage, handling and preparation. Handling instructions provided with the item shall be followed.

When items have to be stored or conditioned under specified environmental conditions, these conditions shall be maintained, monitored and recorded.

Where a test or calibration item or a portion of an item is to be held secure, the laboratory shall have arrangements for storage and security that protect the condition and integrity of the secured items or portions concerned.


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5.9 Assuring the quality of test and calibration results

The laboratory shall have quality control procedures for monitoring the validity of tests and calibrations undertaken.

The resulting data shall be recorded in such a way that trends are detectable and, where practicable, statistical techniques shall be applied to the reviewing of the results.

This monitoring shall be planned and reviewed and may include, but not be limited to, the following:

a) regular use of certified reference materials and/or internal quality control using secondary reference materials;

b) participation in interlaboratory comparison or proficiency-testing programs;

c) replicate tests or calibrations using the same or different methods;

d) retesting or recalibration of retained items;

e) correlation of results for different characteristics of an item.

5.10.1 General

The results of each test, calibration, or series of tests or calibrations carried out by the laboratory shall be reported accurately, clearly, unambiguously and objectively, and in accordance with any specific instructions in the test or calibration methods.

The results shall be reported, usually in a test report or a calibration certificate (see note 1), and shall include all the information requested by the client and necessary for the interpretation of the test or calibration results and all information required by the method used. This information is normally that required by 5.10.2, and 5.10.3 or 5.10.4.

In the case of tests or calibrations performed for internal clients, or in the case of a written agreement with the client, the results may be reported in a simplified way.

Any information listed in 5.10.2 to 5.10.4 which is not reported to the client shall be readily available in the laboratory which carried out the tests and/or calibrations.

5.10.2 Test reports and calibration certificates

Each test report or calibration certificate shall include at least the following information, unless the laboratory has valid reasons for not doing so:

a) a title (e.g. “Test Report” or “Calibration Certificate”);


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b) the name and address of the laboratory, and the location where the tests and/or calibrations were carried out, if different from the address of the laboratory;

c) unique identification of the test report or calibration certificate (such as the serial number), and on each page an identification in order to ensure that the page is recognized as a part of the test report or calibration certificate, and a clear identification of the end of the test report or calibration certificate;

d) the name and address of the client;

e) identification of the method used;

f) a description of, the condition of, and unambiguous identification of the item(s) tested or calibrated;

g) the date of receipt of the test or calibration item(s) where this is critical to the validity and application of the results, and the date(s) of performance of the test or calibration;

h) reference to the sampling plan and procedures used by the laboratory or other bodies where these are relevant to the validity or application of the results;

i) the test or calibration results with, where appropriate, the units of measurement;

j) the name(s), function(s) and signature(s) or equivalent identification of person(s) authorizing the test report or calibration certificate;

k) where relevant, a statement to the effect that the results relate only to the items tested or calibrated.

5.10.3 Test reports

5.10.3.1 In addition to the requirements listed in 5.10.2, test reports shall, where necessary for the interpretation of the test results, include the following:

a) deviations from, additions to, or exclusions from the test method, and information on specific test conditions, such as environmental conditions;

b) where relevant, a statement of compliance/non-compliance with requirements and/or specifications;

c) where applicable, a statement on the estimated uncertainty of measurement; information on uncertainty is needed in test reports when it is relevant to the validity or application of the test results, when a client's instruction so requires, or when the uncertainty affects compliance to a specification limit;

d) where appropriate and needed, opinions and interpretations (see 5.10.5);


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e) additional information which may be required by specific methods, clients or groups of clients.

5.10.3.2 In addition to the requirements listed in 5.10.2 and 5.10.3.1, test reports containing the results of sampling shall include the following, where necessary for the interpretation of test results:

a) the date of sampling;

b) unambiguous identification of the substance, material or product sampled (including the name of the manufacturer, the model or type of designation and serial numbers as appropriate);

c) the location of sampling, including any diagrams, sketches or photographs;

d) a reference to the sampling plan and procedures used;

e) details of any environmental conditions during sampling that may affect the interpretation of the test results;

f) any standard or other specification for the sampling method or procedure, and deviations, additions to or exclusions from the specification concerned.

5.10.4.1 In addition to the requirements listed in 5.10.2, calibration certificates shall include the following, where necessary for the interpretation of calibration results:

a) the conditions (e.g. environmental) under which the calibrations were made that have an influence on the measurement results;

b) the uncertainty of measurement and/or a statement of compliance with an identified metrological specification or clauses thereof;

c) evidence that the measurements are traceable (see note 2 in 5.6.2.1.1).

5.10.4.2 The calibration certificate shall relate only to quantities and the results of functional tests. If a statement of compliance with a specification is made, this shall identify which clauses of the specification are met or not met.

When a statement of compliance with a specification is made omitting the measurement results and associated uncertainties, the laboratory shall record those results and maintain them for possible future reference.

When statements of compliance are made, the uncertainty of measurement shall be taken into account.

5.10.4.3 When an instrument for calibration has been adjusted or repaired, the calibration results before and after adjustment or repair, if available, shall be reported.


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5.10.4.4 A calibration certificate (or calibration label) shall not contain any recommendation on the calibration interval except where this has been agreed with the client. This requirement may be superseded by legal regulations.

5.10.5 Opinions and interpretations

When opinions and interpretations are included, the laboratory shall document the basis upon which the opinions and interpretations have been made. Opinions and interpretations shall be clearly marked as such in a test report.

5.10.6 Testing and calibration results obtained from subcontractors

When the test report contains results of tests performed by subcontractors, these results shall be clearly identified. The subcontractor shall report the results in writing or electronically.

When a calibration has been subcontracted, the laboratory performing the work shall issue the calibration certificate to the contracting laboratory.

5.10.7 Electronic transmission of results

In the case of transmission of test or calibration results by telephone, telex, facsimile or other electronic or electromagnetic means, the requirements of this International Standard shall be met (see also 5.4.7).

5.10.8 Format of reports and certificates

The format shall be designed to accommodate each type of test or calibration carried out and to minimize the possibility of misunderstanding or misuse.

5.10.9 Amendments to test reports and calibration certificates

Material amendments to a test report or calibration certificate after issue shall be made only in the form of a further document, or data transfer, which includes the statement:

“Supplement to Test Report [or Calibration Certificate], serial number ... [or as otherwise identified]”,

or an equivalent form of wording.

Such amendments shall meet all the requirements of this International Standard.

When it is necessary to issue a complete new test report or calibration certificate, this shall be uniquely identified and shall contain a reference to the original that it replaces.


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Appendix I: NELAC Advertising Policy

Compliance Requirement Y N NA Reference

1.1 The laboratory shall have a policy and procedure for controlling the use of the term "NELAC"

1.2 The “NELAC” logo shall not be used by a laboratory that is not NELAC accredited.

1.3 The “NELAC Accredited” logo shall not be used by applicants for NELAC accreditation.

1.4 The “NELAC Accredited” logo shall be used by an NELAC accredited laboratory only under the name in which it holds NELAC accreditation.

1.5 When promoting or providing proof of accreditation, accredited laboratories shall use the scope(s) of accreditation, as this document details the specific tests or calibrations which are accredited. The certificate shall be used for display purposes and may also accompany the scope.

1.6 It is the responsibility of the laboratory to communicate this Advertising Policy and its requirements to the necessary corporate/marketing representatives to ensure that all requirements are met.

2.1 “NELAC Accredited” logo sheets are sent to all accredited laboratories, and an electronic version is available upon request.

2.2 Where the NELAC name and/or logo is used by accredited laboratories, it shall always be accompanied by at least the word “accredited.”

2.3 While there are no restrictions on the size and color of the “NELAC Accredited” logo reproduction, the logo must maintain its form.

2.4 The “NELAC Accredited” logo may be generated electronically provided that the prescribed formats and forms are retained.

3.1 Where the “NELAC Accredited” logo is used to endorse test or calibration results, it shall always be accompanied by the NELAC certificate number(s).

3.2 The “NELAC Accredited” logo may be displayed on all certificates and reports that contain exclusively results from calibrations and tests that have been carried out within the laboratory's official NELAC Scope of Accreditation.

3.3 The “NELAC Accredited” logo shall not be used on certificates and reports if none of the results presented are from tests or calibrations included on the NELAC Scope(s) of Accreditation.


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3.4 Where both accredited and non-accredited tests/calibrations are included on an endorsed report or certificate, non-accredited results shall be clearly and unambiguously identified as such. This can be done by placing an asterisk after each such result along with a footnote stating: “The test/calibration results are not covered by our current NELAC accreditation”.

3.5 On reports where results are reported within the field where accreditation exists but in a technology that is not included in the scope, they must be so indicated. (For example, if a laboratory is accredited in the Environmental Field for only wet chemistry and metals, any gas chromatographic data reported would need to be identified as non-accredited.)

3.6 If the intent is to ensure that the client meets the requirements of the NELAC Traceability Policy, the calibrations performed by an NELAC accredited calibration laboratory must be included on the calibration laboratory's NELAC Scope of Accreditation, and the calibration certificate issued must contain the “NELAC Accredited” logo (or a reference to NELAC accreditation) and the NELAC certificate number.

3.7 There shall be nothing in the reports, certificates or in any attachments or other materials which implies or may lead any user of the results or any interested party to believe that the work is accredited when it is not.

4.1 An NELAC accredited laboratory may include the results of subcontracted tests or calibrations in its endorsed reports or certificates only if:

4.1.1 The accredited laboratory has informed the client in writing of the proposed subcontracting and has obtained prior approval; and

4.1.2 The subcontractor is itself accredited by NELAC or an NELAC recognized MRA partner for the specific tests or calibrations concerned and the results have been included in the subcontracting laboratory's endorsed calibration or test report(s) submitted to the accredited laboratory. Any non-accredited subcontracted calibrations or tests shall be specified as noted in Section 3.4 of this policy.

4.1.3 The subcontracted calibration or test results shall be clearly and unambiguously identified on the certificate or report.

5.1 Where statements of opinions and interpretations are outside the Scope of Accreditation, the laboratory is required to include a disclaimer such as the following in the certificate or report: “The opinions/interpretations expressed in this report are outside the scope of this laboratory's NELAC accreditation.


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5.2 It is preferable, however, to express opinions and interpretations that are outside the Scope of Accreditation on a separate letter which is not part of the endorsed certificate or report and that does not carry the “NELAC Accredited” logo or other reference to NELAC accreditation.

6.1 Calibration labels containing the “NELAC Accredited” logo may be affixed only to equipment that has been calibrated by the accredited calibration laboratory.

6.2 Calibration labels containing the “NELAC Accredited” logo shall include at least the following information:

6.2.1 The name of the accredited calibration laboratory or its NELAC Certificate number;

6.2.2 The instrument identification;

6.2.3 The date of the current calibration;

6.2.4 Cross reference to the calibration certificate issued with respect to this calibration.

7.1 Accredited laboratories may incorporate statements concerning their accreditation in publicity and/or advertising materials, including brochures and organization publications, technical literature, business reports, web sites and quotations or proposals for work.

7.2 The use of the “NELAC Accredited” logo or other reference to NELAC used to promote accreditation enhances the reputation and value of accreditation for all stakeholders. It is the responsibility of the accredited laboratories to ensure that there is no misrepresentation of the accreditation status and that the accreditation process is not brought into disrepute.

7.3 The accreditation claim shall be related only to the testing or calibration that is covered under the NELAC Scope of Accreditation, and not with any other activities in which the laboratory or its parent organization are involved.

7.4 NELAC accreditation is site specific. The accreditation claim shall be related only to the specific laboratory location that is covered under the NELAC Scope of Accreditation, and not with any other non-accredited locations.

7.5 In proposals or quotations, the accredited laboratory shall distinguish tests or calibrations that are covered under the NELAC Scope of Accreditation from those that are not covered.

7.6 Where the “NELAC Accredited” logo is printed on letterhead or other corporate stationery, such stationery shall not be used for work proposals, quotes, reporting of test or calibration results exclusively outside the NELAC Scope of Accreditation, or certifying a product or other item.


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7.7 The “NELAC Accredited” logo or accreditation claim shall not be affixed to a material, item or product (or related part, including packaging), or used to imply that an item or product has been certified.

7.8 If the “NELAC Accredited” logo is included in literature relating to a product, the logo must appear directly adjacent to the reference to the accredited calibration or testing laboratory and it must be clearly stated that inclusion of the logo does not imply certification/approval of the products calibrated or tested.

7.9 The “NELAC Accredited” logo shall not be displayed on business cards in a manner that might imply personnel certification.

8.1 Every circumstance where the principle of accurate representation applies cannot be anticipated and dealt with in this document. Therefore, it is the responsibility of the accredited and applicant laboratory representatives not to misrepresent their accredited status under any circumstances.

8.2 If there are questions, the laboratory should submit intended uses of the logo, draft advertisements, and/or any other accreditation claims to NELAC Headquarters for advance review.

8.3 Upon suspension or termination of accreditation, a laboratory must immediAlloway cease to issue calibration certificates, test reports, and test certificates displaying the logo and shall cease publishing documents (including advertisements, websites, etc.) containing the logo or reference to NELAC Accreditation.


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Appendix 2: Traceability of Measurement


T1. All calibrations and verifications of measuring and test equipment, reference standards, and reference materials shall be conducted by accredited calibration laboratories (in some instances an accredited testing laboratory may also be able to satisfy traceability requirements) or by a recognized national metrology institute.

T2. Calibrations or verifications must be documented in a calibration certificate or report endorsed by a recognized accreditation body’s logo, or otherwise makes reference to accredited status.

T3. Laboratories shall define their policy for achieving measurement traceability. This policy shall be in compliance with this policy document.

T4. Where uncertainty calculations are applicable, testing and calibration laboratories shall calculate measurement uncertainty in accordance with the ISO “Guide to the Expression of Uncertainty in Measurement.” These uncertainties shall be supported by uncertainty budgets, and they shall be represented as expanded uncertainties typically using a coverage factor of k=2 to approximate the 95% confidence level. (Refer to A2LA's Interim Policy on Measurement Uncertainty for Testing Laboratories, August 2000)

T5. If a calibration certificate or report contains a statement of the measurement result and the associated uncertainty, then the uncertainty statement shall be accompanied by an explanation of the meaning of the uncertainty statement. (For example, “This uncertainty represents an expanded uncertainty expressed at approximately the 95% confidence level using a coverage factor of k=2.)

T6. TURs shall be calculated using the expanded uncertainty of the measurement, not the “collective uncertainty of the measurement standards”.

T7. Implicit uncertainty statements (generally expressed in terms of a TUR) shall be accompanied by words to the effect that the uncertainty ratio was calculated using the expanded measurement uncertainty. In addition the coverage factor and confidence level shall be stated.

T8. Calibration reports and certificates issued by A2LA-accredited calibration laboratories shall contain a traceability statement.

T9. All in-house calibrations shall be supported by the following minimal set of elements:

a) The in-house laboratory shall maintain documented procedures for the in-house calibrations and the in-house calibrations shall be evidenced by a calibration report, certificate, or sticker, or other suitable method, and calibration records shall be retained for an appropriate, prescribed time;

b) The in-house laboratory shall maintain training records for calibration personnel and these records shall demonstrate the technical competence of the personnel performing the calibrations;


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c) The in-house laboratory shall be able to demonstrate traceability to national or international standards of measurement by procuring calibration services from accredited calibration labs or a national metrology institute;

d) The in-house laboratory shall have and apply procedures for evaluating measurement uncertainty. Measurement uncertainty shall be taken into account when statements of compliance with specifications are made;

e) Reference standards shall be recalibrated at appropriate intervals to ensure that the reference value is reliable. Policy and procedures for establishing and changing calibration intervals shall be based on the historical behavior of the reference standard.


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Appendix 3: Manual Integration Review


MI 1. Does the laboratory have a defined standard operating procedure for conducting Manual Integrations in the laboratory?

MI 2. Does the laboratory train its personnel on the SOP on manual integrations to provide clear guidelines into technically sound integrations?

MI 3. Does the laboratory conduct data reviews including the review of manual integrations? Does this include secondary or electronic review?

MI 4. Upon review of manual integrations, has the laboratory established a coding system for when manual integrations occur? Are the samples or standards properly noted with before and after pictures?

MI 5. Does the laboratory have procedures in place for rejection of manual integrations at the bench level?

MI 6. Does the data acquisition system save the original computer generated version of the peak(s)?

MI 7. Does the data acquisition system proper save all the new manual integrations(s)?

MI 8. Does the data reduction system offer an audit trail as part of the software package?


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Inorganics/Metals

Note: If thermal preservation is required in the laboratory, requirements are 0-6 degrees C

Parameter Method Minimum Volume (mL)

Container Preservative and Temperature

Hold Time

Alkalinity SM2320B

100 mL P,G Cool, 4ºC 14 days



Marion Lab

Appendix 5 Sample Preservation Table


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Bromide,Bromate, Chorate,Chlorite

300.0 100 mL P,G Cool, 4ºC With EDA

28 days

Chloride 300.0 100 mL P,G Cool, 4ºC 28 days

Chlorine

SM4500Cl-G 200 mL P,G Cool , 4ºC 24 hours

Color

SM2120B 100 mL P,G Cool, 4ºC 48 hours

Cyanide 335.4/9012 100 mL P,G NaOH to pH>12, 4ºC 14 days

Fluoride SM4500F-C 100 mL P Cool, 4ºC 28 days

Hardness

130.2/SM 2340C

100 mL P,G HNO3 to pH<2 6 months

Hexavalent Chromium

SM4500Cr 100 mL P,G Cool, 4ºC 24 hours

Mercury

245.2/7470 100 mL P,G HNO3 to pH<2 28 days

Metals

Various 100 mL P,G HNO3 to pH<2 6 months

Nitrate-Nitrite 353.2/SM4500NO3-F

100 mL P,G H2SO4 to pH<2 28 days

Nitrite

353.2 100 mL P,G NP, Cool,4ºC 48 hours

Ortho Phosphate

SM4500P-E 100 mL P,G Cool, 4ºC 48 hours

Phosphate SM4500P-E 100 mL P,G

H2SO4 to pH<2, 4ºC 28 days

PH (Corrosivity)

150.1/SM 4500H+

100 mL P,G Cool, 4ºC 24 hours

Total Residue

160.3/ SM 2540B


Non-Suspended Solids

160.1/SM 2540C


Suspended Solids

160.2/SM 2540D


Conductivity

SM 2510B 100 mL P,G Cool, 4ºC 10 days

Turbidity

180.1 100 mL P,G Cool, 4ºC 48 hours

Sulfate 300.0 100 mL P,G Cool, 4ºC 28 days

TKN

351.2 100 mL P,G H2SO4 to pH<2, 4ºC 28 days

Total Organic Carbon

9060/SM 5310B

240 mL G H2SO4 to pH<2, 4ºC 28 days

Ignitability

1020 100 mL P,G Cool, 4ºC 28 days

BOD, CBOD

SM 5210B 100 mL P,G Cool, 4ºC 48 hours

O/G and TPH

1664 1 L G H2SO4 to pH<2, 4ºC 28 days

Parameter Method Minimum Volume (mL)

Container Preservative and Temperature

Hold Time

Cyanide-Amenable

335.4/9012 100 mL or grams P,G NaOH to pH>12, 4ºC 28 days

Sulfide 376.2/9030 100 mL or grams P,G NaOH to pH > 9 Plus zinc acetate

7 days

Sulfite SM 504A 100 mL or grams P,G Cool, 4ºC 24 hours

Lead Dust Wipes 200.7/6010 Wipe Wipe No thermal 6 months


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preservation

Lead Paint Chips 200.7/6010 Paint Chips Paint Chips No thermal preservation

6 months

UV 254

SM 5910 B 100 mL or grams P,G Cool, 4ºC 48 hours

TCLP 1311 4 L 4 L amber glass Not Preserved, 4ºC Various

Ammonia

350.1 100 mL P,G H2SO4 to pH<2, 4ºC 28 days

Organics

Volatile Organic Compounds 524.2 40-mL 3 x 40-mL vials

Na2S2O3 Ascorbic acid or HCl

pH<2 4ºC

14 days

EDB and DBCP 504.1 40-mL 3 x 40-mL vials

Na2S2O3 1:1 HCL, pH < 2

4ºC

14 days

Chlorinated Pesticides 508 1-L 1-L amber glass Na2S2O3 4ºC

7 days before ext. 14 days after ext.

Chlorinated Acids (Herbicides) 515.1 1-L 1-L amber glass Na2S2O3 4ºC


Semi-VOA (Extractable) 525.2 1-L 1-L amber glass

Sodium Sulfite 1:1 HCl pH< 2

4ºC


Flame Retardants 527 1 -L 1-L amber glass 9.4 g Potassium dihydrogen citrate; 0.35 g EDATA acid;

0.1 g Ascorbic Acid

14 days before ext 30 days after ext

Explosives 529 1-L 1-L amber glass 5 g Trizma Pre-Set crystals;

0.5 g copper sulfate pentahydrate

14 days before ext 30 days after ext

N-methyl Carbamates 531.2 50-mL 60-mL vial or 2 x 40-mL vials

0.4 g Potassium dihydrate citrate; and 0.004 g sodium

thiosulfate

28 days

Carbamates and Amide Pesticides 632.2 1-L 1-L amber glass

H2SO4 pH 2-4

4ºC


Glyphosphate 547 50-mL 60-mL vial Na2S2O3 4ºC 14 days

Endothall 548.1 100-mL 240-mL amber glass

Na2S2O3 1:1 HCl pH < 2

4ºC


Diquat and Paraquat 549.2 250-mL 1-L amber Polyethylene

Na2S2O3 H2SO4 pH =2

4ºC


Haloacetic Acids (HAAs) 552.2 40-mL 240-mL amber glass NH4Cl -10ºC dark

14 days before ext. 14 day after ext.

Volatile Organics 624/8260 40-mL 3 x 40-mL vials HCl 4ºC

14 days

Polynuclear Aromatic Hydrocarbons (PAHs) 8270 1-L 1-L amber glass Na2S2O3 (if chlorinated)

4ºC

7 days before ext (water) 40 days after ext. (water) 14 days before ext. (soils) 40 days after ext. (soils)

Semi-Volatiles 625/8270 1-L 1-L amber glass Na2S2O3 (if chlorinated) 4ºC


Pesticides/PCBs 608/8081 1-L 1-L amber glass Na2S2O3 (if chlorinated) 4ºC

7 days before ext (water) 40 days after ext. (water)


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14 days before ext. (soils) 40 days after ext. (soils)

N-P Pesticides 8140/8141 1-L 1-L amber glass Not Preserved

4ºC


Herbicides 615/8150/8151 1-L 1-L amber glass Na2S2O3 (if chlorinated)

4ºC



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Marion Lab

Appendix 6 Example of Quality Control Chart


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Marion Lab

Appendix 7 ALLOWAY-Sample Request Sheet


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Marion Lab

Appendix 8 ALLOWAY Chain of Custody Form


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Marion Lab

Appendix 9 Data Deliverables Packages


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Marion Lab

Appendix 10 Laboratory Floor Plan


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ALLOWAY

LAYOUT PLAN OF MARION LABORATORY


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Marion Lab

Appendix 11 References


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REFERENCES

1. Quality Assurance Principles for Analytical Laboratories, AOAC, 1991 2. Code of Federal Regulations, 40 CFR Parts 100-149, Revised 2007 3. General Requirements for Accreditation of Laboratories, American

Association for Laboratory Accreditation, August 2000 plus updates 4. Environmental Lead Program Requirements, American Association for

Laboratory Accreditation, August 2000 plus updates 5. Manual for the Certification of Laboratories Analyzing Drinking

Water, US EPA Office of Ground Water and Drinking Water, March 1997 and updates

6. Guide to Environmental Analytical Methods, Genium Publishing Corporation, 1992 Present

7. Standard Methods, 20th edition, 1998 8. Standard Methods, 19th edition, 1995 9. Test Methods for Evaluating Solid Waste (SW-846), US EPA,

November 1996, plus subsequent updates 10. The Laboratory Quality Assurance System, Ratliff, 1990 11. Quality Assurance/Quality Control Guidance for Removal Activities,

US EPA, EPA/540/G-90/004, April 1990 12. NELAC Constitution and Bylaws, 2002 plus updates 13. Handbook for Analytical Quality Control in Water and Wastewater

Laboratories, US EPA-600/4-79-019, March 1979 14. ALLOWAY Chemical Hygiene Plan 15. National Function Guidelines for Organic Data Review, US EPA CLP 16. Statistical Techniques for Data Analysis, John Keenan Taylor, 1990 17. Statistical Quality Control, Grant & Leavenworth, 1980 18. Handbook of Quality Assurance for the Analytical Chemistry

Laboratory, Dux, 1986 19. A2LA Guide for the Estimation of Measurement Uncertainty in

Testing, July 2002 20.Stanard Methods 21st Edition, 2006

QUALITY ASSURANCE MANUAL MARION LABORATORY … · The quality assurance (QA) and quality control...

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