qaqcgaylord2012 - qa qc.pdf6/8/2012 6 qa/qc the purpose of the laboratory quality assurance program,...

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Operator Training and Certification Unit

Robert Babcock

Renee Arntz

Wastewater

Dan Holmquist

Earl Wuestnick

Bruce Lack

Drinking Water

Laura Chuhran

Matt Tomlinson

Paul Brun Del Re

John Koenigsknecht

�ACTIVATED SLUDGE

�OXIDATION DITCHES

�SEQUENCING BATCH REACTORS

�ATTACHED GROWTH

�WASTE STABILIZATION LAGOONS

�INDUSTRIAL ( I & II)

�ANAEROBIC DIGESTION

�BIOSOLIDS APPLICATION WORKSHOPS

�PHOSPHORUS REMOVAL

�LABORATORY (I, II, III)

�LABORATORY QA/QC

TRAINING

Operator Training and Certification Unit - Wastewater

CERTIFICATIONCLASS

A-1a

OPERATOR

INDUSTRIAL

MUNICIPALA, B, C, D, L1, L2, SC

May Each Year

29 Classifications (By Process)

November Each Year

Storm Water Management*

(Construction and Industrial)

Concentrated Animal Feed Operations*

(CAFO)


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TECHNICAL ASSISTANCE

Plant Operations

Laboratory


OPERATOR TRAINING AND OPERATOR TRAINING AND CERTIFICATION UNITCERTIFICATION UNIT

OPERATOR TRAINING AND OPERATOR TRAINING AND CERTIFICATION UNITCERTIFICATION UNIT

www.michigan.gov/deqoperatortraining

For More InformationTraining Schedules

Certification Schedules

Certification Requirements

Certification Renewal (Applications)

Continuing Education Credits

ETC.

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Why Concerned WithWhy Concerned With

Quality Assurance ?Quality Assurance ?

1. PROVIDE CONFIDENCE

2. SAVES MONEY

3. IT’S THE LAW

Provides Confidence� In ourselves

� In our personnel

� In us, by others

� Governmental Agencies

� Courts

Saves Money� Provides accurate data to optimize plant operations,

� Optimize chemical additions

� Fair assessment of charges on industrial discharges

� Prevent a court case

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It’s The Law� Revisions of EPA methods have QA/QC procedures

built in.

� DEQ is requiring QA/QC support for data on MOR’s.

QA/QC

�The purpose of a laboratory is to provide data to be used in decision making.

�The decisions may be as limited as the adjustment of a single valve, to as far-reaching as whether millions of dollars should be spent to improve the facility.

�These decisions rely on data that is assumed to be accurate.

Purpose of Self Monitiring

�The goal of the NPDES program is to preserve and protect water quality.

�Permits require self-monitoring.

�Data must be scientifically valid and defensible and of known and acceptable precision and accuracy

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Purpose of QA/QCALL ABOUT TRACEABILITY:

�Ability to definitively demonstrate permit compliance?

�Recreate the sampling and analytical activities?

�Documentation should be able to stand on its own merit without explanation.

�Data of known and documented quality.

QA/QCQuality assurance programs have two primary functions in the laboratory:

First, the programs should continually monitor the reliability (accuracy and precision) of the results reported; i.e., they should continually provide answers to the question “How good (accurate and precise) are the results obtained?” This function is the determination of quality.

The second function is the control of quality (to meet the program requirements for reliability). As an example of the distinction between the two functions, the processing of spiked samples may be a determination of measurement quality, but the use of analytical grade reagents is a control measure. ( EPA)

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QA/QC

� The purpose of the Laboratory Quality Assurance program, to provide confidence, or assure, that the data reliably describes the characteristics or the concentration of constituents in the samples submitted to the laboratory.

� This assurance must extend not only to the data being compiled at this time, but also to the data of the past and the data that will be compiled in the future.

� The program then, must be an on-going project that continually monitors and judges the reliability of the results of all analyses, records the checks made, and works to assure that future analyses can and will be done to give reliable results.

QA/QCThe quality assurance program should be developed to meet two primary functions:

� First, the program should act to control the quality of data generated in order to meet the requirements for reliability. To do this, the program must be set up to assure that the analyses used are acceptable and that these analyses are carried out using proper equipment and laboratory techniques.

� The second function is to monitor the reliability or truth of the results reported. This basically amounts to checking to see if the controls developed in the first part of the program are working.

Quality AssuranceQuality AssuranceAn overall

management plan to

guarantee the

integrity of data

(The “system”)

Quality ControlQuality ControlA series of

analytical

measurements used

to assess the

quality of the

analytical data

(The “tools”)

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True Value vs. Measured ValueTrue Value vs. Measured Value

True ValueTrue Value

The known, accepted value of a quantifiable property

Measured ValueMeasured Value

The result of an individual’s measurement of a quantifiable property

Accuracy vs. PrecisionAccuracy vs. Precision

AccuracyAccuracyHow well a measurement agrees with an accepted value

PrecisionPrecisionHow well a series of measurements agree with each other

Imprecise and Inaccurate Precise but Inaccurate

Accurate but Imprecise Precise and Accurate

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Systematic vs. Systematic vs.

Random ErrorsRandom Errors

Systematic ErrorSystematic Error

Avoidable error due to controllable variables in a measurement.

Random ErrorsRandom Errors

Unavoidable errors that are always present in any measurement. Impossible to eliminate

Quality Control MeasuresQuality Control Measures

�Standards and Calibration

�Blanks

�Recovery Studies

�Precision and Accuracy Studies

�Method Detection Limits

Standards and CalibrationStandards and Calibration�Prepared vs. Purchased Standard

�Calibration Curves

�Continuing Calibration Checks

�Internal Standards

�Performance Testing.

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Blanks, Blanks, BlanksBlanks, Blanks, Blanks� Laboratory Reagent Blanks

� Instrument Blanks

� Duplicates

� Standards

� Spike Sample

� Split Samples

� Field Reagent Blanks

� Trip Blanks

Sampling� Collection Analysis Schedule

� Collection Location

� Sample Type ( Grab, Composite, Sampler Instruction)

� Sample Handling:

� Security

� Chain of Custody

� Proper Preservation, Container, Holding Time

� Proper Storage

� Documentation

Quality Assurance Elements

� QUALITY MANUAL

� STANDARD OPERATING PROCEDURES (SOPS)

� TRAINING

� RELIABLE AND WELL- MAINTAINED EQUIPMENT

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Quality Assurance Elements

� INSTRUMENT CALIBRATIONS – (AND VERIFICATIONS)

� TRACEABLE STANDARDS

� REVIEW OF DATA AND QC RESULTS

� CORRECTIVE ACTION PROCESS

Record-Keeping

Records to be Kept:

�Bench Sheets

�Lab Logbook

�Procedures References

�Equipment Maintenance and Repair

�Chemical / Equipment Inventory

Control Samples

Control samples are introduced into the train of actual samples to monitor the performance of the analytical system. These control samples include duplicates, spikes, and reference samples:

�Duplicate analyses are performed to determine precision.

� Spiked and reference samples are used to monitor accuracy

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Internal ControlsInternal Controls

Duplicates

Spikes

Steps of Procedures(Blanks, Dilutions, etc.)

External ControlsExternal ControlsReference Samples

Split Samples

Why IsQA/QC

Necessary?

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TYPES of ERRORSTYPES of ERRORSTYPES of ERRORSTYPES of ERRORS

SYSTEMATIC

Consistent ERRORS that affect the end results

in the same way every time.

RANDOM

Inconsistent ERRORS that affect the end results

unpredictably.

DEFINE THE FOLLOWING:

Random errors:

Consistent ERRORS that affect the end results

in the same way every time.

Inconsistent

Systematic errors:

ERRORS that affect the endresults unpredictably.

ERRORS WORKSHEETERRORS WORKSHEET

LABEL THE FOLLOWING AS

RANDOM OR SYSTEMATIC ERRORS:

Using a pipet with a chipped tip

that always delivers 0.4 mL less

than its calibrated value.

Systematic

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ERRORS WORKSHEETERRORS WORKSHEET

LABEL THE FOLLOWING AS

RANDOM OR SYSTEMATIC ERRORS:

Not calibrating an instrument on

a regular basis.

Random

How can we Determine

the Affects of Errors?

CONTROL CHARTS

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Control Charts

Purpose:

� Organize Data

� Compare Data

� Judge Data

Control Charts

Developed by DEQ-OTCU

� PHOSPHORUS

� CHLORINE RESIDUAL

� SUSPENDED SOLIDS

� BOD

� AMMONIA

� FECAL COLIFORM

Example Control Chart

AVG

51.8451.80

52.00

.90

.10

.20

.30

.40

.50

.70

.60

.50

.40

Sta

nd

ard

Len

gth

, cm

Number of Standard11 12 13 14 15 16 17 18 19 20 21 22 23 24 25

Organizes Data

Compares Data

Judges Reliability???

Control Limits ?

Warning Limits ?

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- 1s + 1s

Bell Curve

Value

Fre

qu

ency

x

68 %

95 %

99 %

95 %

Confidence

Interval

99 %

Confidence

Interval

Warning Limits

Control Limits

Example Control Chart

51.80

AVG

51.84

52.00

.90

.10

.20

.30

.40

.50

.70

.60

.50

.40

UWL

52.03

UCL

52.13

LWL

51.65LCL

51.55

Sta

nd

ard

Len

gth

, cm

Number of Standard11 12 13 14 15 16 17 18 19 20 21 22 23 24 25

Examples of Control Charts� These charts are available for your use.

� e-mail us and we can send you the file.

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Frequency of Testing� After control charts have been developed, analysis of

control samples should be done on a frequency which depends upon several factors.

� These factors include size and complexity of facility, number of samples analyzed, impact on environment, legal liability, and degree of analytical control required.

Test Type & Frequency of TestingSUNDAY MONDAY TUESDAY WEDNESDAY THURSDAY FRIDAY SATURDAY

Coliform Blank

Influent Ammonia

Duplicate

Influent

Phosphorus

Duplicate

Influent

Sus. Solids

Duplicate

Influent

Sus. Solids

Duplicate

Influent

Ammonia Spike

Influent BOD

Duplicate

Effluent

Ammonia

Duplicate

Effluent

Phosphorus

Duplicate

Glucose

Effluent

Sus. Solids

Duplicate

Effluent

Ammonia Spike

Effluent BOD

Duplicate

Influent

Ammonia

Duplicate

Influent

Phosphorus

Spike

Effluent

Sus. Solids

Duplicate

Influent

Sus. Solids

Duplicate

Influent

Ammonia Spike

Influent BOD

Duplicate

Effluent

Ammonia

Duplicate

Effluent

Phosphorus

Spike

Glucose

Coliform Duplicate

Effluent

Sus. Solids

Duplicate

Effluent

Ammonia Spike

Effluent BOD

Duplicate

QUALITY ASSURANCE MONITORING FREQUENCY

B.O.D.lab days/week 1 3 5 7 7

anal./mo. 1-20 21-50 51-100 101-150 >150

DUPS.

SPLITS

GLUCOSE

REFS.

1/mo 2/mo 4/mo 6/mo 8/mo

1/yr 2/yr 2/yr 2/yr 2/yr

4/yr 12/yr 12/yr 12/yr 24/yr


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SUSPENDED SOLIDSlab days/week 1 3 5 7 7

anal./mo. 1-20 21-50 51-100 101-150 >150

DUPS.

SPLITS

REFS.





PHOSPHORUSlab days/week 1 3 5 7 7

anal./mo. 1-20 21-50 51-100 101-150 >150

DUPS.

SPLITS

SPIKES

REFS.






COLIFORMlab days/week 1 3 5 7 7

anal./mo. 1-20 21-50 51-100 101-150 >150

DUPS.

BLANKS


1/mo 2/mo 1/wk 1/wk 1/wk

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CHLORINE RESIDUALlab days/week 1 3 5 7 7

anal./mo. 1-20 21-50 51-100 101-150 >150

DUPS.

REFS.



ISE SLOPE 2/mo 2/mo 2/mo 2/mo 4/mo


pHlab days/week 1 3 5 7 7

anal./mo. 1-20 21-50 51-100 101-150 >150

REFS. 1/yr 1/yr 2/yr 2/yr 2/yr

SLOPE CHECK 2/mo 2/mo 2/mo 2/mo 2/mo


AMMONIA NITROGENlab days/week 1 3 5 7 7

anal./mo. 1-20 21-50 51-100 101-150 >150

DUPS.

SPLITS

SPIKES

REFS.





ISE SLOPE 2/mo 2/mo 2/mo 2/mo 4/mo

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Putting Together a Laboratory QA Program Checklist of Items Needed 1. Program Write-Up 2. Procedures Reference Sheets 3. Schedule of Frequencies for QA Analyses 4. Precision (Duplicate) Data for Appropriate Parameters BOD Suspended Solids Fecal Coliform Phosphorus Ammonia-N 5. Precision Control Charts 6. Accuracy ( Percent Recovery) Data for Appropriate Parameters Phosphorus Ammonia 7. Accuracy Control Charts 8. Temperature Log 9. Samples Split With Another Laboratory 10. Reference Samples Obtained From an Outside Source 11. Electrode Slope Logs pH Ammonia Electrode Chlorine Residual Electrode 12. Glucose / Glutamic Acid Accuracy Check for BOD 13. Equipment Calibration Records Analytical Balance Spectrophotometer 14. Laboratory Maintenance Schedule/Plan 15. Chemical Inventory 16. Equipment Inventory

EPARecommended Elements of a Laboratory

Quality Assurance Plan

� At a minimum, the following items should be included in a lab QA plan.

Laboratory organization and

responsibility� Include a chart or table showing the laboratory organization and lines

of responsibility, including QA managers;

� List the key individuals who are responsible for ensuring the production of valid measurements and the routine assessment of measurement systems for precision and accuracy (e.g., the persons responsible for internal audits and reviews of the implementation of the plan and its requirements);

� Reference (but do not include) the job descriptions of the personnel and describe training to keep personnel updated on regulations and methodology, and document that laboratory personnel have demonstrated proficiency for the methods they perform

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A list of SOPs with the dates of the most recent

revisions

� (An SOP can reference an EPA method but the EPA method itself is not an SOP. An SOP details actual in-house laboratory operating procedures with respect to laboratory analyses, instrument operations, QC procedures, etc.)

� The lab’s QA manager should:

Ensure that current copies of SOPs are in the laboratory and in the QA Manager’s files;

Ensure that SOPs are reviewed annually and revised as changes are made;

Ensure that SOPs have signature pages and dated revisions.

Field sampling procedures

� Describe required preservation, proper containers, correct sample container cleaning procedures, sample holding times from collection to analysis, and sample shipping and storage conditions;

� Provide copies of appropriate custody forms.

� Describe how samples are checked when they arrive at the lab for proper containers, temperature and proper preservation (e.g., pH, chlorine residual).

Laboratory sample handling

procedures

� Use bound laboratory note books, filled out in ink, with entries dated and signed. (A secure, password protected, electronic data base is acceptable).

� Describe how unprocessed and processed samples are stored at the proper temperature, isolated from laboratory contaminants, standards and highly contaminated samples and, sometimes, each other;

� Describe practices to ensure that holding times will not be exceeded;

� Describe how personnel maintain integrity of all samples, (e.g., by tracking samples from receipt by laboratory through analysis to disposal);

� Discuss when Chain-of-Custody procedures are imposed (for samples likely to be the basis for an enforcement action);

� Specify criteria for rejection of samples which do not meet shipping, holding time and/or preservation requirements and procedures for notification of sample originators.

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Calibration procedures for

chemistry

� Specify type of calibration used for each method and frequency of use;

� Describe standards' source, age, storage, labeling;

� Describe use of control charts.

Data reduction, validation, reporting and

verification

� Describe data reduction process;

� Describe data evaluation process;

� Describe reporting procedures, including format;

� Describe procedure for data corrections.

Quality controlDescribe quality control procedures used for all analytical procedures. Parameters for chemistry should include:

• instrument performance check standards;

• frequency of determination of method detection limit (MDL) calculations;

� calibration, internal and surrogate standards;

laboratory reagent blanks;

� laboratory duplicates;

quality control and proficiency testing samples;

� laboratory fortified blanks and laboratory fortified sample matrices;

� initial demonstrations of method capability;

� qualitative identification/confirmation of contaminants.

� .Parameters for microbiology should include:

� positive and negative culture controls;

� sterility controls;

� proficiency testing and other quality control samples.

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Schedule of internal audits

� Show written schedule.

Preventive maintenance

procedures and schedules

� Equipment list & PM schedules

Corrective action contingencies

� Describe response to obtaining unacceptable results from analysis of lab QC checks;

� Name persons responsible for the various corrective actions;

� Describe how the corrective actions taken are documented

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Record keeping procedures� Describe procedures and how they are

documented;

� Describe security policy of electronic databases.

DEQ-OTCU

e-mails

� [email protected]

� [email protected]

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