Contents

7. Procedures

Effective Date: 07/2008
Point of Contact: Quality Engineer for Regulatory Programs

Technical Procedures

Laboratory activities shall be directed and controlled by internally approved procedures using techniques appropriate for the identified purpose. Many recognized, well-established methods and procedures already exist that may be incorporated into technical procedures to meet the client needs (e.g., consensus methods). However, since complex matrices usually require variation from published procedures, a flexible approach must be available to allow development, modification, and enhancement of a procedure on a real-time basis. This section describes the basic requirements for the development, qualification, change control, and routine review of procedures.

Procedure Development

Step 1 If a procedure exists that meets the project needs, no procedure development is required.

If a procedure does not exist that meets the project needs, develop a test plan that documents the approach.
Note: The Definitions/Acronyms exhibit defines these terms.

Step 2 Ensure that the requirements in the Procedures, Permits, and Other Work Instructions subject area are met for procedures and test plans.

Step 3 Include the following in all procedures and test plans:

Include the following as appropriate to the scope and complexity of the procedure or test plan:

Step 4 If a published, well-established method (e.g., ASTM, EPA) already exists and is to be used, complete one of the following actions:

Step 5 The client shall agree on the procedures/test plans used according to one of the following:

Procedure Qualification

Technical procedures used for the first time in the laboratory must be qualified before reporting results to any client. Test plans are qualified during execution of the work. Qualification includes the selection of appropriate QC checks to permit the evaluation of data quality and includes the following steps.

Step 1 Determine the need for qualification:

Determine what test materials will be used to conduct the qualification:

Determine how the qualification will be performed based on the data quality required by the project:

Step 2 Use a suitable number of replicate determinations to provide a measure of statistical control. Generally accepted standards dictate using a minimum of four replicates for each test case. Whenever possible, seven replicates should be used. This data is used to establish statistical control on an advisory basis until sufficient data are acquired, typically considered to be 30 data sets.

Step 3 Evaluate the procedure/test plan for its overall effectiveness in the areas of sensitivity, (method detection level) selectivity, linear range limitations, matrix or analytical precision and accuracy and counting statistics (minimum detectable activity and counter performance for radiochemistry), as applicable to the technique and/or analyte and depending on whether the technique is preparative, analytical, or encompasses both. This requires that testing include blank evaluation, precision and accuracy determination, efficiency, uncertainty, and determination of interferences as appropriate to the technique (i.e., preparative versus determinative).

Step 4 Make all qualification data traceable to the technical procedures(s) or test plan(s) it supports and retain it on file to enable retrospective examination should the need arise.

Procedure Change Control

It is recognized that no technical procedure can be expected to be applicable, as written, to every type of sample the laboratory may receive. The primary concern when deviating from or changing a procedure must be whether or not the change has a negative impact on the client's data quality requirements. The following describes the types of changes, which may occur during the execution of work and the specific action required. Note: The suggested guidelines within the Technical and Operating Procedures subject area will not be used.

Immediate Actions: If personnel hazard or equipment damage is imminent, take immediate action to make the situation safe, as described below:

Substitutions: Staff members make an adjustment in a procedure that a reasonable, technically competent person would be expected to consider equivalent. The substitution must have no significant effect on the final analytical results (e.g., substituting a different column with equivalent performance characteristics, using glassware other than that specified when it has no effect on analytical processes) and must not change the existing environmental, safety and health conditions.

Because substitution does not impact the method performed or the final analytical data, no documentation of change is required other than that necessary to allow reproduction of results.

Deviations: Deviation is divergence from the original procedure that does not adversely impact the analyst's ability to meet the precision, accuracy, detection limit, selectivity, and QC criteria of the procedure (e.g., use of packed versus capillary columns). Therefore, the decision to deviate shall be based on published literature (e.g., alternate methods) and/or known sample chemistry.

Deviation requires documenting the changes made to a procedure. Documentation of deviations made shall be included in the final report narrative. Justification of the deviation should be evident in the acceptable performance associated with the final results and should also be discussed. Acceptable performance shall be demonstrated by the analyst's ability to meet or exceed the original method's precision, accuracy, detection limit, selectivity, and QC criteria. When a deviation is used routinely, it shall be incorporated into the procedure.

  1. Pre-Planned Deviations
    Pre-planned deviations are those changes that are known before a procedure is applied. In this case the deviation(s) shall be documented, approval of the project manager shall be obtained, and the project manager shall notify the client for acceptance prior to sample analysis. The deviation shall be documented in the project record, and summarized in the final report to the client. A test plan may be used to document the deviation to the procedure. The notification and acceptance may be by an electronic mail message, DSI, memo or other written documentation.
  2. Real-Time Deviations
    Real-time deviations are those changes that become necessary during the application of a procedure. As long as the deviation does not negatively impact the client's data quality requirements, an explanation in the final report is sufficient documentation. Also, the client shall be notified as soon as possible after the deviation occurs. The project is responsible for ensuring client notification.

Modifications: Modification changes the character of a procedure, and thereby, potentially limits a procedure's ability to meet the originally stated precision, accuracy, detection limit, selectivity, and QC criteria (e.g., microwave versus beaker digestion). Because the impact of such a modification cannot be ascertained before implementation, it must be demonstrated by application. Modifications shall not be performed real-time.

Modification requires the procedure to be qualified, documented, approved, and agreed upon with the client before work. Justification of the modification should be evident in the QC data associated with the final results and should also be discussed. A modification with long-term applicability should be developed into a new procedure that is issued with a new title and code.

Note: Method modification is not permitted when a regulatory method must be used for client work due to regulation. The only exception to this rule is when DOE-RL has first been notified and has approved use of the modified method or for 1831 work agreement is reached with the client working in conjunction with the regulator. Method qualification is required prior to approval.

Interim Change Notices: Project staff use the Interim Change Notice (ICN) form for the purpose of making an editorial correction or simple change to a document. The ICN provides for identifying, approving, and issuing the change within a short period of time. The ICN receives the same level of review and approval as the original document if the change is technical in nature. Since multiple ICNs can make a document difficult to implement, it is policy that a document be revised when a change is extensive or there are already three ICNs applied to the document. Note: ICNs shall not be used for modifications.

Administrative Procedures

Laboratory-specific administrative activities shall be directed and controlled by internally approved procedures. Ensure that the requirements in the Procedures, Permits, and Other Work Instructions subject area are met.

Each administrative procedure, at a minimum, shall include:

Routine Review of Procedures

The responsible manager ensures that:

Suggested Guidelines

The following are examples of procedure review activities that could take place:

References

Procedures, Permits, and Other Work Instructions subject area

Stopping and Restarting Work (Safety Rights and Responsibility) subject area