J.4 QA_Manual_Feb2021-2.docx

Quality Assurance Manual of the Chemical Monitoring Research Team Chemical and Biological Monitoring Branch Health Effects Laboratory Division National Institute for Occupational Safety and Health Revised February 2021

APPROVALS

Approved by:

Don Beezhold Director, HELD Sam Glover Branch Chief, CBMB, HELD Robert P. Streicher Team Leader, CMRT, CBMB, HELD Revised by:

Ronnee Andrews Quality Assurance Manager, CBMB, HELD Issued: September 1997 Revised: April 2010 Revised: June 2016 Revised: February 2021

FEBRUARY 2021 REVISIONS

Table of Contents

ABBREVIATIONS

DSI……… Division of Science Integration

SECTION 1—INTRODUCTION

Purpose The purpose of the Quality Assurance Manual is to ensure the integrity of laboratory data that is reported to the client, used in method development research, and published within scientific literature. The quality assurance (QA) program covers all areas of the process, from sampling strategy, to method selection, and to the final review and issuance of reports to our clients [AIHA 1995; Ratliff 1990].

Objectives This Manual covers the Chemical and Biological Monitoring Branch (CBMB), Health Effects Laboratory Division (HELD), National Institute for Occupational Safety and Health (NIOSH) laboratories located at the Alice Hamilton building in Cincinnati, Ohio. These laboratories are the primary industrial hygiene laboratories for the Institute. The objectives of the QA program described in this Manual are to assure that the analytical results reported by the CBMB laboratories conform to the highest standards of competence and quality for industrial hygiene testing laboratories [AIHA 2020; ISO 2017].

The quality of the work performed by the laboratory must be known and controlled at all times. The previous history and circumstances of the samples submitted to this laboratory may not always be known to the laboratory personnel or individual analyst. However, prior to sample collection, laboratory personnel provide consultation to clients requesting analytical services on the appropriate procedures for sampling, handling, storing, and shipment of samples. Once the sample has been accepted by the laboratory, the care with which the sample was collected and handled before receipt by the laboratory must be assumed to be of the highest quality. Therefore, laboratory personnel must always be aware of the accuracy and precision of their work and must be prepared to support their results and conclusions at a later date. The various techniques presented herein will help to assure that data produced by the laboratory meet the highest standards of quality and can be supported by written records.

Policies It is essential that the QA policies of this laboratory are clearly defined in a formal, written plan and are reviewed and updated, if needed, at least annually by the QA coordinator. The written plan will be distributed to all laboratory personnel and an electronic copy will be posted on the CBMB local area network (LAN). It is essential that the plan be understood by all laboratory personnel and the policies be followed by all. All standard operating procedures (SOPs) are located in the HELD SOP database for use by all personnel. A link to this database is located on the HELD intranet (https://held.cdc.gov) and the LIMS. The procedures for the preparation, revision, and approval of SOPs are contained in HELD SOP BB-00004 and the SOPs are to be reviewed at least biennially by the QA coordinator. Revisions to the Quality Assurance Manual and SOPs are considered approved by management when posted on the LIMS.

Impartiality and Integrity of Operations Statement The NIOSH/HELD/CBMB laboratory abides by the requirements for impartiality and integrity prescribed by the parent agency, the Centers for Disease Control and Prevention (CDC). All laboratories in the CDC, including medical, environmental and industrial hygiene, are subject to the CDC Laboratory Quality Assurance and Standardization Programs and fulfill the requirements given in ISO 17025:2017, Section 4.1.

Content This Manual describes the procedures to be followed from the receipt of samples to the reporting of results. Emphasis is focused in four general areas:

These procedures and protocols may change as necessary to address new problems, changes in technologies, and to provide more efficient service.

Responsibilities This Manual has been prepared, reviewed, and approved by the individuals whose signatures appear on the title page. These signatures indicate that the procedures and policies contained herein have received the endorsement of the laboratory management and are to be followed by all laboratory personnel. It is the responsibility of each laboratory employee to review the Manual, become familiar with the procedures relevant to each individual’s work, and adhere to them.

Adherence to documented administrative procedures contributes to the efficient handling of sample analysis requests and reduces the likelihood of misunderstandings and outright mistakes in analysis. This Manual is designed to delineate the QA responsibilities of all laboratory personnel (i.e., technician, scientist, clerical, and management).

Proper record keeping must include not only the data needs of the requestor and analyst, but also the data needs of others who, because of administrative or other responsibilities, must have ready access to accumulated data and records. Also, the records must provide a means for others, (e.g., other analysts, QA personnel, and auditors) to reconstruct the procedures and analysis performed by the original analyst.

A system that monitors and documents the performance of analyses completed in the laboratory can help assure that reported results are within acceptable statistical limits of accuracy and precision and that future questions regarding the quality of analytical results can be addressed. The proper function of this system depends upon efforts of all laboratory personnel, including management, the QA coordinator, and the individual analysts.

Definition Quality assurance is the overall activity of providing, to all concerned, the necessary evidence to establish confidence in the quality (e.g., accuracy and precision) of the laboratory’s data [Inhorn 1978; Juran 1951]. Quality assurance provides accountability of data to prevent sample mix-ups and to provide traceability of data, safeguards against loss or falsification of data, and documentation of quality control (QC) operations [Dux 1986]. The process includes an auditing procedure designed to evaluate all known policies and procedures that can affect the quality of the analytical results [AIHA 1995].

References AIHA [1995]. Quality assurance manual for industrial hygiene chemistry. Akron, OH: American Industrial Hygiene Association.

AIHA [2019]. AIHA LAP, LLC Policy Module 1: Accreditation Overview. [https://aiha-assets.sfo2.digitaloceanspaces.com/AIHA/lap-uploads/LAP-Policies/Policy-Module-1.pdf ]. Date accessed: February 2021.

Dux JP [1986]. Handbook of quality assurance for the analytical chemistry laboratory. New York: Van Nostrand Reinhold, pp. 2–5.

Inhorn SL, ed. [1978]. Quality assurance practices for health laboratories. Washington: American Public Health Association.

ISO [2017]. ISO/IEC 17025: General requirements for the competence of testing and calibration laboratories. 3rd ed. Geneva: International Organization for Standardization.

Juran JM, ed. [1951]. Quality-control handbook. New York: McGraw-Hill, pp. 2.10–2.24.

Ratliff TA Jr. [1990]. The laboratory quality assurance system: a manual of quality procedures with related forms. New York: Van Nostrand Reinhold.

SECTION 2—THE ORGANIZATION

Purpose This section describes the organizational structure of the NIOSH/HELD/CBMB laboratories and provides a description of the positions responsible for the quality of the laboratory analyses. An updated list of the positions and names of staff holding these positions are located on the CBMB intranet at SOP CBM-00361.

Organization/Structure The laboratories of CBMB provide analytical chemistry services to the other Divisions and centers of NIOSH including the Division of Field Studies and Engineering (DFSE); the Respiratory Health Division (RHD); the Division of Safety Research (DSR); the Health Effects Laboratory Division (HELD); the Pittsburgh Mining Research Division (PMRD); the Spokane Mining Research Division (SMRD); the Western States Division (WSD); the Division of Science Integration (DSI); and the regional offices of NIOSH. The procedures for requesting analysis and who may request analyses are given in SOP CBM-00360. Service is delivered either by the in-house staff or by contract laboratories. A list of the current staff in CBMB may be obtained from the Division office.

Administrative Issues Administrative issues not covered elsewhere in the CBMB laboratory SOPs can be found in SOP CBM-00359. This SOP contains the laboratory confidentiality statement, the list of approved contract laboratories, and all proficiency testing program participation.

Personnel The CBMB/CMRT laboratory director has overall responsibility for laboratory operations. The laboratory director has the responsibility for providing the resources and services required consistent with other NIOSH objectives and priorities. The laboratory director has the overall responsibility for determining the scope of analytical service that will be provided in consultation with other NIOSH groups who may also provide support services.

The CBMB quality assurance coordinator (QA coordinator) establishes overall data quality goals for the laboratory and procedures (in consultation with other management staff) to meet these goals. Also, the QA coordinator consults with laboratory analysts to meet these data quality goals, works with other staff to resolve QC problems, provides internal reference samples to the analysts, and maintains appropriate QA records for monitoring analytical method performance. The QA coordinator is responsible for identifying problems in the analysis of samples and complaints from the clients of the laboratory and is responsible for determining a course of action to correct the problem or complaint. A yearly audit will be performed by the QA coordinator or their designee. It will also be the QA coordinator’s responsibility to provide every laboratory analyst and CBMB scientist with a copy of this Manual in electronic format and to ensure that each individual understands that they are responsible for following the procedures provided in this Manual. The QA coordinator shall issue quarterly QA reports which document laboratory activities and QA activities. These quarterly reports shall be posted on the LIMS with a link to archives of all reports. The CBMB QA program shall appoint a deputy quality assurance coordinator to provide continuity during QA coordinator absences and to assist with tasks as assigned.

The CBMB laboratory coordinator is responsible for day-to-day contact with clients requesting analytical services from the CBMB laboratories. After consultation with supervisors, the QA coordinator, and/or other laboratory personnel, the laboratory coordinator will inform the client (requestor) how those analytical services are to be provided (i.e., whether in-house or by contract laboratory). The laboratory coordinator serves as the contact point to assure that appropriate procedures for sampling, storage, and shipping of field samples are known to the field personnel using this analytical service.

The CBMB sample clerk is responsible for receipt and log in of samples received by the laboratory. The sample clerk records the condition of the samples when received in the laboratory, notes whether the samples were shipped in the approved manner, assures that the appropriate paperwork is completed to initiate tracking of the samples in the laboratory, and assures that the samples are stored in an appropriate manner and in a secured sample storage area until analysis. If the sample clerk is absent or unavailable, then an alternate will be designated by the laboratory director.

CBMB team leaders have the responsibility for providing the immediate supervision of laboratory personnel and monitoring performance of individuals in their team. They are responsible for assuring that the samples received are analyzed in an expeditious manner and that the data produced meet the quality requirements of the requester, the QA coordinator, and the QA plan.

Analysts (chemists, physical scientists, or other scientists assigned to the analysis) have the responsibility to assure that the data quality they produce meets the CBMB laboratory QA requirements. Analysts have the responsibility to exercise their professional judgment in completing analysis of samples, to recognize operational problems with laboratory instruments and procedures, and to work with other laboratory personnel to resolve any problems found. Analysts have the responsibility to document their work properly, so that if questions arise or work must be defended, they or others can locate the documentation easily and be able to recreate the analysis on demand.

Field coordinators are designated in each NIOSH Division (e.g., DFSE, HELD, PMRD) that submits samples to the CBMB laboratories for analysis. Their responsibilities include reviewing sampling plans with the client requestor and electronic transmittal of the Request for Analytical Chemistry Services to the laboratory coordinator.

Project officers of laboratory services contracts are responsible for assuring that all contract laboratories meet their contractual requirements for data quality. Project officers are responsible for timely, accurate communications of problems and project requirements that may affect the data quality from contractors to NIOSH personnel. The project officer will work with the QA coordinator to assure that audit samples or proficiency test samples are provided and that the contract laboratory meets the same standards of quality as the CBMB laboratories are required to meet.

SECTION 3—LABORATORY COORDINATION

Laboratory coordination is an administrative system that is designed to manage client requests for analytical chemistry support. Laboratory coordination also reviews all requests, tenders and contracts and purchasing of services and supplies. The client request process begins with the initial request by the field researcher and covers all aspects of laboratory operations through completion of the laboratory report. The following describes the protocol followed by the researcher in need of analytical services and by CBMB staff in providing those services.

Request For Analytical Chemistry Services The researcher requesting laboratory analyses prepares and submits the Request for Analytical Chemistry Services on the LIMS (SOP CBM-00361). It is reviewed by the designated field coordinator and then the laboratory coordinator prior to collection of the samples. This form has several uses, the most important being:

The laboratory coordinator, after reviewing the request form, presents the request at the daily laboratory coordination meeting. At this meeting, which may include team leaders, project officers, field coordinators, and the QA coordinator or Deputy QA coordinator, the request is reviewed to determine whether the request is consistent with established analytical methods or if method development research is warranted. The request is assigned a project sequence number, which is used to track all sample sets collected for the project.

Assignment of Laboratory In general, the more routine samples, i.e., samples for which a method is available in the NIOSH Manual of Analytical Methods (NMAM), are sent to the Comprehensive Analytical chemistry Support Contract (CASC) laboratory for analysis. If the analysis requires specialty analyses or methods development, the samples may be sent to the in-house laboratory or elsewhere.

When the request is considered acceptable and all sample sets have been assigned to a laboratory, the laboratory coordinator approves the request in the LIMS. The procedure for processing the request for analytical services can be found in SOP CBM-00365. The requestor refers to the LIMS for information as to where the collected samples should be sent for analysis.

If special collection media such as specialty sorbent tubes or impinger solutions are to be provided for the sampling procedure, the industrial hygienist/requestor must initiate the request when requesting analytical chemistry services via the LIMS. The laboratory coordinator or the appropriate CBMB team leader is responsible for assuring that these media are provided to the requestor by the required date. Additional information on requesting media and supplies is found in HELD SOP CBM-00362.

In some situations, it may be necessary to amend the initial request for analytical chemistry support. This may be necessary due to significant changes in the number of samples or the addition/deletion of a sample set or special requirements to meet the client’s needs. The Request for Analytical Chemistry Services must be edited in the LIMS with the new information. If the laboratory coordinator edits the request, the appropriate field coordinator will be notified. The amended request will be processed in the same manner as the original request. The original sequence number will be assigned to the amended request.

Quality Assurance The QA coordinator and/or Deputy QA coordinator participates in CASC coordination meetings and is familiar with all laboratory requests and reviews the preliminary QA plans (SOP CBM-00378) developed by the laboratory analyst for the proposed sample sets. If internally generated QC samples are needed, they are scheduled for preparation by the QA coordinator or another laboratory analyst.

SECTION 4—SAMPLE SUBMITTAL, RECEIPT, AND LOGGING

Sample Submittal All sample sets must be sent to the assigned laboratory (as noted on the request form) in approved containers and accompanied by the Sample Submittal Form (CBM-00366). Samples on sorbent tubes must never be shipped with bulk organic compounds. The samples must be clearly and unambiguously labeled, preferably each label includes the assigned sequence number. Whenever possible, the researcher provides a narrative describing the nature of the samples, such as possible matrix effects, conditions in the workplace at the time of sampling, and any special instructions with regard to the analyses being requested.

Detailed instructions for submitting samples in sets according to sample type and for completing the Sample Submittal Form are contained in SOP CBM-00366. The Sample Submittal Form must be completed according to the specifications contained in this SOP and must be included with the sample set. It is the responsibility of the sample submitter to assure that these procedures are followed.

Sample Receipt Policy The sample receipt policy is described in SOP CBM-00371. This policy is applicable to all inhouse and contract laboratories. For samples submitted to the in-house laboratory, it is the responsibility of the sample clerk to assure that this policy is carried out. If there is doubt as to whether some aspect of this policy has been followed in a specific situation, the sample clerk requests the assistance of the appropriate team leader. The number and condition of samples as received are noted on the Sample Submittal Form and must be reported in the analytical report. Any discrepancies that cannot be readily resolved between the actual samples and the Sample Submittal Form must be reported to the submitter as soon as possible. Any sample deemed invalid when examined according to SOP CBM-00367 will not be analyzed and will be placed on Hold until questions about sample validity and integrity are answered, returned to the requestor, or discarded.

Sample Logging Procedures Samples are submitted to the laboratory either by mail or by hand delivery by the requestor. All samples and their corresponding paperwork must be sent or delivered to the laboratory sample clerk. It is the sample clerk’s responsibility to see that all samples are properly identified and listed on the Sample Submittal Forms. The sample clerk will then log the sample set into the LIMS using the sequence number followed by a two-letter identification to identify the sample set for a specific analysis. For each subsequence (sample set), the appropriate information contained on the Sample Submittal Form is entered into the LIMS. The procedure for sample receiving and LIMS login is found in SOP CBM-00370.

All samples must be properly stored in the locked sample security room, i.e., solid sorbents in the refrigerator, organic bulks in the hood, and filters and inorganic bulks in wall cabinets. The sample clerk refers to the LIMS or the Request for Analytical Services form for information on which analyst will be assigned the set. The individual analyst is notified via email that the sample set has been assigned to them. It is the responsibility of the team leader to assure that the analyst understands the requirements for the analysis and that the Sample Submittal Form and other information are provided to the analyst before the start of the analysis.

Request for Priority Analyses It is laboratory policy that sample sets will be analyzed on a “first in/first out” basis. In situations where sample stability is questionable, such samples will go to the beginning of the queue. Also, if sample sets can be combined into one large set, this will be done to improve efficiency. There are situations where there is a valid reason for a sample set to move ahead of all sets in the laboratory. Such situations will be treated on an individual basis and according to SOP CBM-00364, which documents the procedure for requesting priority status. Priority basis will not be given to any sample set unless SOP CBM-00364 is followed. This policy effectively requires approval by both the requestor’s Field Coordinator and Division Director as well as the CBMB Branch Chief or designee.

Sample Set Retention SOP CBM-00368 provides guidance on the retention of field samples submitted to the laboratory. There are often situations where the client may wish to have a reanalysis or a completely new analysis of a sample set. Since most samples require extraction/desorption of the analyte, there are often questions as to the stability of the chemicals extracted or desorbed. SOP CBM-00368 provides general guidance; however, the client must be aware that there are many conflicting problems when attempting to reanalyze or perform another type of analysis on previously prepared samples.

SECTION 5—SUPPLEMENTAL CUSTODY CONTROL PROCEDURES

Supplemental custody control procedures are used when additional tracking and custody control beyond the CBMB Sample Submittal Form is needed. The field investigator (principal investigator) is responsible for determining whether supplemental custody control procedures are necessary for a particular sample set. For those samples where it may be necessary to have strict custody control for the entire lifecycle of the sample set, the procedures are discussed in SOP CBM-00369.

SECTION 6—LABORATORY INFORMATION MANAGEMENT SYSTEM

The laboratory information management system (LIMS) is a computer database management system developed to provide administrative support for laboratory management. The system encompasses three functions: data input, file updating, and report generation (see SOP CBM-00365 and SOP CBM-00370).

Project management and tracking is centered on the sequence number. A unique sequence number is assigned to each request for analytical chemistry services. The coordination part of the database contains a sequence number; the requestor’s name, Branch, and Division; sampling location; a description of the project or survey; information regarding possible interferents that may affect the outcome of the analysis; and sampling media needs.

Each sequence may be composed of several subsequences representing discrete sample sets for specific analysis. The logbook part of the database manages the distinct sample sets of a project or survey (sequence number). The sample clerk or alternate logs in each sample set with a two-letter subsequence and enters date received, sample type, number of samples, sample medium, analysis requested, and analyst assigned. The LIMS is also automatically updated on a daily basis through internet access of the CASC laboratory’s LIMS.

The database can be searched to determine the status of sample sets, numbers of samples analyzed in a given time period, workload of a particular laboratory, etc. The database is updated at several points: (1) when a sample analysis request is approved, (2) when samples are received, and (3) when sample analysis is complete.

The LIMS tracks sample set status for all subsequences. Thus, all researchers in NIOSH have access to the status of all laboratory work.

SECTION 7—SELECTION OF ANALYTICAL METHOD

When a request for analytical services is coordinated by the laboratory coordinator, a tentative method of sampling and analysis is selected. The NMAM is a compendium of methods developed or modified either by NIOSH staff or through a NIOSH contract. Methods published in NMAM undergo a rigorous evaluation and validation process that includes documentation of each method’s analytical performance (e.g., accuracy, precision, specificity, limit of detection (LOD), limit of quantitation (LOQ)). If a suitable analytical method is not contained in the NMAM, team leaders, in conjunction with the laboratory coordinator and other CBMB scientific staff, will determine whether other methods are available (SOP CBM-00363).

Performance information on the selected method must include evidence of the analyte’s identity, separation of the analyte(s) from interfering substances, an estimate of the LOD, intralaboratory precision, and accuracy. In general, methods that have been applied to the matrix of interest are preferred to those that have not. Ideally, the method chosen has been validated by interlaboratory comparison and has been evaluated over the concentration range of interest. Resources also must be considered. Suitable methods that are fast, simple, and of relatively low cost are preferred over more complex and costly methods.

If no method has been published for a particular analyte, the laboratory may need to propose a method. Often, an existing method (e.g., one written for a similar compound, or an Occupational Safety and Health Administration (OSHA) method, such as those contained in the OSHA Occupational Chemical Database) can be modified for use. If preliminary studies are necessary as a check of the proposed method, the assignment of these tasks to the appropriate personnel is made by the laboratory management. Advance planning by the requestor in conjunction with the laboratory coordinator usually leads to a preliminary decision on the analytical method selected, but the final choice of a measurement technique is sometimes not made until after the sample set is received by the laboratory, as specific circumstances of the set may influence this choice.

In some situations, use of a method that is not well established or development of an entirely new method may be required. In these cases, the analyst may consult with other laboratory personnel and ensure that the new method is tested or approach taken in method development is the best alternative available. To this end, the analyst must provide rationale for the choice of a particular method, obtain supporting laboratory data, and thoroughly document research results. Otherwise, the reliability of the method may be questioned. Guidelines for development and evaluation of sampling and analytical methods are discussed in detail elsewhere [Kennedy et al. 1995]. A further discussion of this topic can be found in SOP CBM-00363, Specialty Analyses and Short-Term Methods Development.

References Kennedy ER, Fischbach TJ, Song R, Eller PM, Shulman SA [1995]. Guidelines for air sampling and analytical method development and evaluation. Cincinnati, OH: U.S. Department of Health and Human Services, Public Health Service, Centers for Disease Control and Prevention, National Institute for Occupational Safety and Health, DHHS (NIOSH) Publication No. 95–117. [http://www.cdc.gov/niosh/docs/95-117/pdfs/95-117.pdf]

SECTION 8—LABORATORY QUALITY CONTROL TESTING AND ANALYSIS

Introduction This section describes the various control measures that can be used to ensure that the analyses performed in the CBMB laboratory meet the highest standards of quality.

Control Measures Control measures are performed on laboratory analyses to verify the stability and validity of the samples and the performance of the analytical instrumentation. These control measures will be performed on the samples and instrumentation during the analysis process. Some control measures may be required as part of the routine analyses and are performed by the analyst to determine the performance of the system. These include the use of sample blanks to identify possible interferences and contamination, the use of internal standards to compensate for matrix effects, introduction of spiked samples to measure recovery efficiency, the use of replicate analyses to determine precision, duplicate samples to measure the precision of the sampling and analytical process, and the introduction of reference materials such as National Institute of Standards and Technology (NIST) standard reference materials (SRMs) to determine accuracy.

Quality Assurance Plan Before processing a sample, the analyst must have a QA plan. The QA plan will be developed according to the procedures as outlined in SOP CBM-00378. The analytical request and sample submittal paperwork must be reviewed to determine the purpose of the field study, and, if necessary, the analyst may consult with the laboratory coordinator, team leader, QA coordinator, or individual requesting the analysis to determine precisely what is being requested before the samples are analyzed. If necessary, a joint meeting can be held to ensure that all parties understand the requirements of the analysis. Later, this QA plan may be altered as an analysis proceeds and more information regarding the samples is obtained.

SECTION 9—RECORD KEEPING

Introduction Records are kept in the CBMB office or within the LIMS of all analytical data and final reports, including those of contract laboratories. The records are identified by sequence number and shall identify the people involved in all aspects of the sequence, including sampling, sample preparation, and measurement. The data and descriptions shall be sufficient so that the data can be reproduced if necessary.

Laboratory Notebooks The laboratory notebook is the primary source for documentation for the individual analyst’s activities. Laboratory notebooks are used for recording all experimental and analytical notes and data. The notebooks are the property of the CBMB laboratory and are retained by the CBMB laboratory for the time specified in SOP CBM-00379.

Issuance of Notebooks Notebooks are hardcovered and bound. Notebooks with removable pages (e.g., looseleaf) or loose inserts are not permitted. When a new laboratory notebook is logged out from the Branch office to an analyst, a notebook number is assigned and kept in the Lab Notebook Assignment Record, which is located in the Branch office. This notebook number is written on the cover of the notebook together with the analyst’s name and dates the notebook was issued and completed.

How To Make Entries All entries are to be made in indelible ink. The pages of the notebook shall be numbered and dated. Observations, data, and calculations shall be recorded at the time they are made and shall be identifiable to the specific task. Any entries made by an individual other than the person to whom the book was assigned shall be signed and dated. If a mistake is made, a line must be drawn through it and a corrected entry made immediately following, initialed, and dated. The line drawn must not render the deletion illegible. Recording of data on loose sheets for later reentry into the bound notebook is poor procedure, and because of the possibility of transcription errors, must be avoided. Avoid placing laboratory notebooks where spills are likely to occur. Every entry must be dated and initialed at the foot of the page and preferably at the end of each day. In no case shall an entry be initialed less frequently than each page.

What Must Be Entered The minimum data and description entered in the notebook shall be sufficient to enable another analyst to derive the same results as the original worker, with no other source of unpublished information. The notebook shall contain all information gathered by the analyst pertaining to the sample analysis. Where appropriate, laboratory number, field number, sequence number, and other identifying numbers are noted. Analysis requested, identification of the method, modifications to the method, and the sample originator must be included. A description of the sample (whether bulk material, charcoal tube, etc.) must be included. Data such as blank values, recovery studies, or duplicate determinations must also be included. Formulae used to calculate results and a sample calculation must be shown. Electronic data, such as chromatograms stored electronically are included by reference in the notebook. Changes made to electronic data must include a note explaining the reason for the change and the date of revision. See SOP CBM-00379 for additional information. A table of contents must be included to aid in locating experimental data.

Notebook Audits An analyst’s notebook is subject to inspection by team leaders, the QA coordinator, or laboratory accreditation auditors. Therefore, the notebook must be maintained in a professional manner and contain all pertinent information, regardless of the particular importance of that information to the analyst. The notebook must be maintained in such a manner that it can withstand challenges as to the validity, accuracy, or legibility of its contents. Entries shall be timely and not accumulated for more than one day before date and signature are applied.

Records Management and Retention Limits Official government records are retained in accordance with CDC Records Management requirements. All Quality Assurance records and technical records shall be managed via use of a records management matrix which includes identification, collection, indexing, access, filing, storage, maintenance and disposal of these records. Laboratory notebooks are considered Significant and/or Secondary Research Records and as such are stored for a minimum of 11 years after the completion of study project or when an employee leaves. Laboratory notebooks may be retained for longer periods, but the decision will be made on a case-by-case basis. The final disposition of inactive laboratory notebooks is be decided upon review by the Laboratory Director, CBMB Branch Chief, and the Senior Records Liaison.

Analytical Report Files The primary source of information on the laboratory’s activities is the analytical report file. These records are located in the CBMB File Room (Hamilton 519) for reports up to Seq. 12088 and are under the direct responsibility of the Branch Program Operations Assistant and electronically on the LIMS for subsequent sequences. There is a separate file for each sequence and the file shall contain the Request for Analytical Chemistry Services form and the analytical report for each subsequence. Each analytical report shall be accompanied by the original paperwork submitted with the sample set and the CBMB QC Record Form. Where appropriate, other information regarding the sample set (i.e., additional paperwork or background information submitted by the requestor) must be included. Reports received from contract laboratories are also stored in the analytical report file.

SECTION 10—INSTRUMENT MAINTENANCE AND INSTRUMENT LOGS

Introduction Proper instrument performance is essential to assure the reliability of reported results. An instrument maintenance program must address the following areas:

An instrument logbook will be kept for all major instruments. The logbook will contain a record of the routine maintenance done on the instrument and any repairs made by laboratory personnel or manufacturer service personnel along with the date and name or initials of the person performing the maintenance or repair. The cover of the instrument logbook must be clearly marked with the instrument identification and must be kept near the instrument. The following SOPs are available for use in instrument setup and maintenance: SOP CBM-00398, SOP CBM-00399, SOP CBM-00400, SOP CBM-00401, SOP CBM-00402, SOP CBM-00403, SOP CBM-00404.

Procedure Where available, government credit cards, blanket purchase agreements (BPAs), or service contracts are used to assure timely service for major instrumentation. In general, one person in the Branch serves as a contact person for this and if service is needed from a particular instrument manufacturer, the appropriate contact person will put in the request to the vendor. Manufacturer’s instructions shall be followed for safe handling, transport, storage, use and planned maintenance of measuring equipment to ensure proper functioning and in order to prevent contamination or deterioration.

Often, subtle defects in instrument performance, too minor to be noticed during routine use, can jeopardize the quality of data being produced. Standard methods of checking instrument performance can be useful in detecting defects or drifts in instrument response over time. Each major piece of equipment is assigned to an analyst who is responsible for maintaining the instrument logbook. That analyst is also responsible for assuring that the performance checks for that instrument (if available) are carried out. They must also work with other analysts in developing and improving performance check procedures for that instrument.

The first page of the logbook must contain the following information:

Subsequent pages may contain the following information:

Each entry must be dated and signed/initialed. Instrument manuals received with the instrument must be stored and made available for the operator to use for setup, operation, and maintenance of the instrument.

SECTION 11—CALIBRATION

Introduction Calibration is an essential part of quantitative analysis. Most often, the relationship between instrument response (i.e., signal) and analyte concentration is determined through analysis of a series of standard solutions of the analyte of interest. A plot of the instrument response versus analyte concentration constitutes the analytical “calibration curve.” The signal-to-concentration relationship seen with the standards is assumed to apply to the unknowns. For this reason, the procedure used to prepare the unknown field samples shall be as similar as possible to that used to prepare the standards.

Data Analysis A variety of software is available for analysis of the calibration data. These software programs allow users to obtain a graphical display of the calibration curve, linear regression results (e.g., slope, intercept, regression coefficient), and a plot of the residuals from the linear regression. Polynomial regression and weighted regressions also can be performed. A general discussion of the statistical treatment of calibration data and the software available in this laboratory is presented in SOP CBM-00380. Not all statistical treatments or software programs are right for every sample analysis. A more comprehensive treatment of this topic can be found in statistical texts and elsewhere [Kelly et al. 1992; Kennedy et al. 1995].

Calibration standards and reference materials The laboratory shall have a program and procedure for the calibration of its reference standards. 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. Calibrations shall be repeated at appropriate intervals, the length of which can be dependent on the uncertainty required, the frequency of use and verification, the manner of use, stability of the equipment, and risk of failure considerations. Periodic verifications shall be performed to demonstrate the continued validity of the calibration at specified intervals between calibrations. The frequency of verifications can be dependent on the uncertainty required, the frequency of use, the manner of use, the stability of the equipment and the risk of failure considerations. The laboratory shall have procedures describing their external and internal calibration and verification activities and frequencies and the actions to follow if the equipment is found to be out of acceptable specification. Although the frequency of calibration can be extended, it cannot be eliminated. The procedures shall describe the action(s) that will be taken when recalibrations or verifications fail to meet the established criteria, including the use of the nonconformance and corrective action system to identify the root cause, prevent recurrence, and evaluate the impact to data reported since the last passing calibration or verification, including data recall where appropriate. Handling, transport, storage and use of reference standards and reference materials shall be done as specified by the manufacturer in order to prevent contamination or deterioration and in order to protect their integrity.

References Kelley WD, Ratliff TA Jr., Nenadic C [1992]. Basic statistics for laboratories: a primer for laboratory workers. New York: Van Nostrand Reinhold.

Kennedy ER, Fischbach TJ, Song R, Eller PM, Shulman SA [1995].