chapt11

11.0 CORRECTIVE ACTIONS

Quality controls are used to monitor and assess the effectiveness and validity of a sampling or analysis activity. If a specified quality control measure is determined to be out of a predetermined acceptance range, and the source or reason for the deviation is not identified and corrected, the sample data associated with the quality control measure may not be useful or valid information.

Some quality control criteria (ex. calibration) have a direct effect on the test results. Others (ex. blanks and duplicates) are indicators of improper protocols or contamination.

11.1 QUALITY CONTROL MEASURES AND ACCEPTANCE CRITERIA

Table 11.1 identifies each of the quality control checks that are required by test methods and/or DER acceptance criteria. The acceptance range criteria or the source of the acceptance range has been identified.

11.2 IDENTIFYING AND ASSESSING QC MEASURES

Generally, quality control information is reviewed by several individuals. The responsibility for the initial assessment of a quality control measure lies with the individual who (1) identifies the sample or procedure as a QC measure; and (2) has access to the test results:

11.2.1. The individual responsible for operating the analytical instrument or equipment must be responsible for assessing the following applicable QC Measures:

1. Method, reagent and calibration blanks

2. Calibration integrity: initial and continuing calibration, interference standards, and QC check standards

3. System performance checks

4. Tuning criteria

5. Surrogate and internal samples

6. Titrating solutions

11.2.2. The following checks are normally assessed by a secondary reviewer (supervisor or QA Officer), but may be evaluated by the primary analyst:

1. Standard Reference Material

2. QC Check Samples

3. Spiked samples (matrix and blank)

4. Duplicates

11.2.3. The following must be assessed by the organization or individual(s) responsible for sample collection, but may be reviewed by laboratory personnel if the sample has been identified as:

1. Precleaned and field cleaned equipment blanks

2. Trip blanks

3. Field collected duplicates

4. Split samples

11.3 DETERMINING THE SOURCE OF QC PROBLEMS

Once a problem has been identified, the process (whether analytical or review) should be halted until the reason for the problem has been identified. Finding the source of a QC problem involves identifying probable sources of error, and checking each source to determine if the protocols were properly followed. Common sources of error and expected follow-up protocols are outlined on Table 11-2. Usually, the individual who is responsible for identifying the problem is responsible for determining the cause. However, other personnel and organizations may need to cooperate.

11.4 INITIATING CORRECTIVE ACTION

When the source of a QC error has been identified, appropriate steps must be taken to eliminate or minimize recurrences.

11.4.1. If a QC measure listed in 11.2.1 above is not acceptable, testing cannot continue until the QC check meets specifications. Corrective actions may be initiated:

1. By the individual who is operating the instrument; or

2. By an individual in oversight authority (i.e. supervisor or QA Officer) if a solution is not immediately apparent.

11.4.2. Corrective actions for QC measures in 11.2.2 and 11.2.3 must be initiated by the individual who identifies the problem.

11.5 SPECIFIC CORRECTIVE ACTIONS

A list of expected corrective actions for each QC measure is included on Table 11-2. Since many QC problems have unique solutions, the corrective action protocols are not limited to those listed. Further assessment, based on an individual's experience and knowledge may be warranted.

11.6 DOCUMENTATION AND NOTIFICATION OF AFFECTED PARTIES

If a quality control measures fails to meet acceptance criteria, the QC measure, and the procedures were used to correct the problem must be documented.

Documentation does not imply a formal memo or corrective action form:

1. Corrective actions that are initiated during an on-going analytical run may be documented on the chromatogram, integrator or strip chart recorder records as well as in the instrument, analytical and/or field logs.

2. Corrective actions that require input or intervention of more than one individual must at a minimum be documented in the related logs and records. Corrective action forms for larger organizations are recommended.

3. If more than one organization is involved with identifying a QC problem and the associated corrective actions, formal memos are recommended, although dated and signed phone logs are acceptable. In all cases, a copy of all documentation should be maintained in the project files.

If an identified quality control problem affects more than one set of data or multiple projects, the documentation associated with identifying and resolving the problem must be cross referenced to all associated projects.

11.7 CORRECTIVE ACTIONS FROM EXTERNAL SOURCES

The need to initiate corrective action may be the result of activities or audits from external sources. Sources include systems audits; performance audits; split samples; blind QC samples; and findings from project or data validation review.

IN ALL CASES, DER RECOMMENDED CORRECTIVE ACTIONS MUST BE INITIATED.

Table 11.1

ACCEPTANCE CRITERIA AND CORRECTIVE ACTIONS FOR

QUALITY CONTROL CHECKS

QC CHECK		ACCEPTANCE CRITERIA

BLANKS
	Method blank	<MDL
	Reagent blank
	Calibration blank
	Precleaned Equipment Blanks
	Field Cleaned Equipment Blanks
	Trip Blanks

CALIBRATION
	Initial calibration	a. Method acceptance criteria*
		b. DER SOP acceptance criteria

	QC Check Standard	a. Method acceptance criteria*
		b. +/- 10% of true value
		c. Internally generated control limits

	Continuing calibration	a. Method acceptance criteria calibration*
		b. +/- 20% deviation from initial calibration
		c. Internally generated control limits

	Interference standard	Method acceptance criteria

	Tuning criteria	Method acceptance criteria

SYSTEM PERFORMANCE CHECKS
	Pesticide	Method acceptance criteria

	Standard Reference Materials	Within certified limits

	QC Check Samples	Within specified limits

SPIKES
	Matrix Spike	Within range specified by CompQAP (accuracy acceptance limits)

	Blank Spike	Within method specified criteria

Table 11.1, cont.

ACCEPTANCE CRITERIA AND CORRECTIVE ACTIONS FOR

QUALITY CONTROL CHECKS

QC CHECK		ACCEPTANCE CRITERIA
DUPLICATES
	Laboratory Duplicates	Within range specified by CompQAP(precision acceptance limits)

	Matrix Spike Duplicates	Within range specified by CompQAP (precision acceptance limits)

	Field Duplicates	Within range specified by CompQAP
		(precision acceptance limits)

OTHERS
	Surrogate Standards	Method acceptance criteria

	Internal Standards	Method acceptance criteria

	Split Samples	Meets precision criteria of CompQAP

	Titrating Solutions	a. +/- 10% of expected (lab determined) value
		b. Replicate sample aliquot results are within method specified limits

MICROBIOLOGY
	Monthly parameters	Per Page 305 of EPA-600/8-78-017
	Chlorine Residual
	Conductivity
	Heterotrophic Count

	Annual metals concentration	Per Page 305 of EPA-600/8-78-017

	Distilled water suitability test	Per Table IV-A-3 of EPA-600/8-78-017

	Incubators	35 +/-0.5 C or 44.5 +/-0.2 C

	Duplicates	Within calculated precision criteria

	Morphological and Biochemical Confirmation	Per Table IV-A-5 of EPA-600/8-78-017

	Positive and negative media controls	Per Table IV-A-4 of EPA-600/8-78-017

	MF Blanks	<1

	MPN dilution blanks	<1

	Inhibitory residue	Must meet method criteria

Table 11.1, cont.

ACCEPTANCE CRITERIA AND CORRECTIVE ACTIONS FOR

QUALITY CONTROL CHECKS

QC CHECK		ACCEPTANCE CRITERIA
MICROBIOLOGY, cont.
	Membrane Filter Analysis	Verified colonies must be coliforms

	MPN Analysis	Verified colonies must be coliforms

BIOASSAY
	One set of dilution water controls	Method acceptance criteria

	Reference toxicant	a. Per specified method criteria
		b. Outside historically derived control limits

SPECIES IDENTIFICATION
	Confirmation	98-99% of unidentified species are
		verified by independent expert

2. Environmental Contamination (all sample collection, sample and analysis conditions) - review sampling handling protocols

3. Improper or incomplete laboratory and/or field decontamination/cleaning procedures - review cleaning protocols

1. Review data with respect to reported contamination levels. If sample concentrations are near the reported blanks levels, reprocess (reextract or digest) associated samples or resample. If sample concentrations or the reporting levels are significantly higher than blanks, or contaminants are not detected in the samples, report the sample data and concentrations in blank.

2. Take measures to eliminate future problems: discard reagents, revise protocols, perform preventative maintenance on system, adjust use of interfering chemicals (solvents, fuels, etc.).

1. Improperly prepared or outdated standards - review preparation logs for calculation/dilution errors and use of expired sources.

6. Reanalyze all samples bracketing those from previous ACCEPTABLE QC check through next acceptable QC check.

a. Improper sample preparation or analysis - review all protocols associated with sample preparation and analysis

1. Reanalyze all samples bracketing those from previous ACCEPTABLE QC check through next acceptable QC check

2. Reprocess all samples associated with QC check sample or standard reference material (unless the problem is unique to processing of the check sample)

2. Error in preparing or using spike solutions - review all preparation and/or analytical logs (including sample preparation) for proper dilutions, solvents, buffers, etc.

3. Review preparation, calculation and record keeping to determine if additional training or more stringent protocols are needed

4. If the laboratory has no historical data to show that the sample matrix produces consistently unacceptable (out of control) recoveries, and none of the sources discussed above are responsible for the problem, the sample must be reprocessed and reanalyzed. If reanalysis produces the same result, associated samples should be reported with qualified results. If results are different, all associated samples must be reprocessed for analysis.

1. Non representative sample - review sample collection and/or sample processing protocols

2. Revise sample collection/sample processing protocols to assure a representative sample

2. Error in preparing or using titrant and standard solutions - review all preparation and/or analytical logs (including sample preparation) for proper dilutions, solvents, buffers, etc.

3. Outdated standards and/or - review expiration dates and standard preparation logs

5. Non representative sample - review sample collection and/or sample processing protocols

2. Review preparation, calculation and record keeping to determine if additional training or more stringent protocols are needed

1. Clean, replace cartridges and/or perform other preventative maintenance tasks

1. Counting errors or difficulties in identifying coliform organisms (membrane filter).

1. Recount or re-examination colonies to determine counting error or misidentifications.

2. Examine blanks and samples analyzed to determine possible sources of contamination.

3. If 14.a.2 above is found to be the problem, or the problem has not been identified, data must be invalidated and resampling and retesting must occur.

3. Prepare new batch of media from the same lot to determine media acceptability or discard media if the shelf life has expired.

5. Invalidate all affected data linked to the media that was not functioning acceptability.

3. Use alternate positive and negative control samples to confirm media response and check on original samples.

1. Review sterility checks on the autoclave for rinse/dilution water and other associated equipment.

3. Review testing procedures and test location for other sources of contamination.

1. Review sterility checks on the autoclave for dilution water and other sterilized equipment.

2. Review testing procedures and location for possible sources of contamination.

1. Implement rinsing protocols that produce an acceptable inhibitory residue test.

2. Change detergents to one that produces an acceptable test result under normal rinsing operations.

1. Adjust initial colony count based upon positive verification percentage and report as verified coliform count.

* Method acceptance criteria shall be followed. If none is provided, the DER criteria (b) or internal, historically generated control limits (c) shall be used.