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Quality is a Lousy Idea-
If it’s Only an Idea
Quality Assurance vs.
Quality Control
Quality Assurance
An overall
management plan to
guarantee the
integrity of data
(The “system”)
Quality Control
A series of
analytical
measurements used
to assess the
quality of the
analytical data
(The “tools”)
True Value vs. Measured
Value
True Value
The known,
accepted value of
a quantifiable
property
Measured Value
The result of an
individual’s
measurement of a
quantifiable
property
Accuracy vs. Precision
Accuracy
How well a
measurement
agrees with an
accepted value
Precision
How well a series
of measurements
agree with each
other
Accuracy vs. Precision
Systematic vs.
Random Errors
Systematic Error
Avoidable error
due to controllable
variables in a
measurement.
Random Errors
Unavoidable errors
that are always
present in any
measurement.
Impossible to
eliminate
Quality Control Measures
• Standards and Calibration
• Blanks
• Recovery Studies
• Precision and Accuracy Studies
• Method Detection Limits
• NJQLs
Standards and Calibration
• Prepared vs. Purchased Standard
• Signals: Peak Area, Beer’s Law
• Calibration Curves
• Continuing Calibration Checks
• Internal Standards
• Performance Testing.
Calibration Curves
Graphical representation of the
relationship between:
• The analytical signal
• The concentration of the analyte
and
Calibration Curve for DDT
y = 9.3005x + 4.3313
0
100
200
300
400
500
0 10 20 30 40 50 60
Parts per trillion DDT
Peakareax106
R2
= 0.9989
Continuing Calibration
Verification
• Many methods don’t require that
daily calibration curves are
prepared
• A “calibration verification” is
analyzed with each batch of samples
Sample Batch
• 10 - 20 samples (method defined)
or less
• Same matrix
• Same sample prep and analysis
• Contains a full set of
QC samples
Internal Standards
• A compound chemically similar to
the analyte
• Not expected to be present in the
sample
• Cannot interfere in the analysis
• Added to the calibration standards
and to the samples in identical
amounts.
Internal Standards
• Refines the calibration process
• Analytical signals for calibration
standards are compared to those
for internal standards
• Eliminates differences in random
and systematic errors between
samples and standards
Performance Testing
Blind samples submitted to
laboratories
?
?
?Labs must periodically
analyze with acceptable
results in order to maintain
accreditation
Blanks, Blanks, Blanks
• Laboratory Reagent Blanks
• Instrument Blanks
• Field Reagent Blanks
• Trip Blanks
Laboratory Reagent Blanks
• Contains every reagent used in the
analysis
• Is subjected to all analytical
procedures
• Must give signal below detection
limit
• Most methods require one with
every batch
Instrument Blank
• A clean sample (e.g., distilled water)
processed through the instrumental
steps of the measurement process;
used to determine instrument
contamination.
Field Reagent Blanks
• Prepared in the lab, taken to the
field
• Opened at the sampling site,
exposed to sampling equipment,
returned to the lab.
Trip Blanks
• Prepared in the lab, taken to the
field
• Not opened
• Returned to the lab
• Not always required in EPA methods
Recovery Studies
• Matrix Spikes
• Laboratory Control Samples
• Surrogates .
Matrix Spikes
• Sample spiked with a known
amount of analyte
• Subjected to all sample prep and
analytical procedures
• Determines the effect of the matrix
on analyte recovery
• Normally one per batch
Laboratory Control Sample
• Subjected to all sample prep and
analytical procedures
• Analyte spiked into reagent water
Laboratory Control Sample
Also known as:
• Laboratory Fortified Blank (LFB)
• Quality Control Sample (QCS)
Surrogates
• Similar to an internal standard
• Added to all analytical samples,
and to all QC samples to monitor
method performance, usually
during sample prep
• Methods often have specific
surrogate recovery criteria
• Most common in Organic methods
Quality Control Measures
• Standards and Calibration
• Blanks
• Recovery Studies
• Precision and Accuracy Studies
• Method Detection Limits
• NJQLs
Precision and Accuracy
• Required for initial certification
and annually thereafter
• A series of four laboratory control
samples
• Must meet accuracy (recovery) and
precision (standard deviation)
requirements, often in method
Precision and Accuracy
• Required with a change in
instrumentation or personnel
• Specific to the analyst
• Other names include:
P&A, DOC, IDOC
Method Detection Limit
“The minimum concentration of a
substance that can be measured and
reported with 99% confidence that the
analyte concentration is greater than
zero”
N.J.A.C 7:18 - 1.7
Method Detection Limit
• MDLs are determined according to
40 CFR, part 136, Appendix B
• Seven replicate laboratory control
samples, analyzed for precision
• Multiply standard deviation by
3.14 (Student’s t- value)
Method Detection Limit
• Must be performed initially for
certification
• Must meet criteria specified in
method
• Must be performed with change in
instrumentation or test method
• Annually with ELCP
New Jersey
Quantitation Limits
(NJQLs)
• The minimum concentration of an
analyte that can be quantified with
statistical confidence
• 5 x MDL, for the NJ Lab
Certification Program

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Qa course total pot

  • 1. Quality is a Lousy Idea- If it’s Only an Idea
  • 2. Quality Assurance vs. Quality Control Quality Assurance An overall management plan to guarantee the integrity of data (The “system”) Quality Control A series of analytical measurements used to assess the quality of the analytical data (The “tools”)
  • 3. True Value vs. Measured Value True Value The known, accepted value of a quantifiable property Measured Value The result of an individual’s measurement of a quantifiable property
  • 4. Accuracy vs. Precision Accuracy How well a measurement agrees with an accepted value Precision How well a series of measurements agree with each other
  • 6. Systematic vs. Random Errors Systematic Error Avoidable error due to controllable variables in a measurement. Random Errors Unavoidable errors that are always present in any measurement. Impossible to eliminate
  • 7. Quality Control Measures • Standards and Calibration • Blanks • Recovery Studies • Precision and Accuracy Studies • Method Detection Limits • NJQLs
  • 8. Standards and Calibration • Prepared vs. Purchased Standard • Signals: Peak Area, Beer’s Law • Calibration Curves • Continuing Calibration Checks • Internal Standards • Performance Testing.
  • 9. Calibration Curves Graphical representation of the relationship between: • The analytical signal • The concentration of the analyte and
  • 10. Calibration Curve for DDT y = 9.3005x + 4.3313 0 100 200 300 400 500 0 10 20 30 40 50 60 Parts per trillion DDT Peakareax106 R2 = 0.9989
  • 11. Continuing Calibration Verification • Many methods don’t require that daily calibration curves are prepared • A “calibration verification” is analyzed with each batch of samples
  • 12. Sample Batch • 10 - 20 samples (method defined) or less • Same matrix • Same sample prep and analysis • Contains a full set of QC samples
  • 13. Internal Standards • A compound chemically similar to the analyte • Not expected to be present in the sample • Cannot interfere in the analysis • Added to the calibration standards and to the samples in identical amounts.
  • 14. Internal Standards • Refines the calibration process • Analytical signals for calibration standards are compared to those for internal standards • Eliminates differences in random and systematic errors between samples and standards
  • 15. Performance Testing Blind samples submitted to laboratories ? ? ?Labs must periodically analyze with acceptable results in order to maintain accreditation
  • 16. Blanks, Blanks, Blanks • Laboratory Reagent Blanks • Instrument Blanks • Field Reagent Blanks • Trip Blanks
  • 17. Laboratory Reagent Blanks • Contains every reagent used in the analysis • Is subjected to all analytical procedures • Must give signal below detection limit • Most methods require one with every batch
  • 18. Instrument Blank • A clean sample (e.g., distilled water) processed through the instrumental steps of the measurement process; used to determine instrument contamination.
  • 19. Field Reagent Blanks • Prepared in the lab, taken to the field • Opened at the sampling site, exposed to sampling equipment, returned to the lab.
  • 20. Trip Blanks • Prepared in the lab, taken to the field • Not opened • Returned to the lab • Not always required in EPA methods
  • 21. Recovery Studies • Matrix Spikes • Laboratory Control Samples • Surrogates .
  • 22. Matrix Spikes • Sample spiked with a known amount of analyte • Subjected to all sample prep and analytical procedures • Determines the effect of the matrix on analyte recovery • Normally one per batch
  • 23. Laboratory Control Sample • Subjected to all sample prep and analytical procedures • Analyte spiked into reagent water
  • 24. Laboratory Control Sample Also known as: • Laboratory Fortified Blank (LFB) • Quality Control Sample (QCS)
  • 25. Surrogates • Similar to an internal standard • Added to all analytical samples, and to all QC samples to monitor method performance, usually during sample prep • Methods often have specific surrogate recovery criteria • Most common in Organic methods
  • 26. Quality Control Measures • Standards and Calibration • Blanks • Recovery Studies • Precision and Accuracy Studies • Method Detection Limits • NJQLs
  • 27. Precision and Accuracy • Required for initial certification and annually thereafter • A series of four laboratory control samples • Must meet accuracy (recovery) and precision (standard deviation) requirements, often in method
  • 28. Precision and Accuracy • Required with a change in instrumentation or personnel • Specific to the analyst • Other names include: P&A, DOC, IDOC
  • 29. Method Detection Limit “The minimum concentration of a substance that can be measured and reported with 99% confidence that the analyte concentration is greater than zero” N.J.A.C 7:18 - 1.7
  • 30. Method Detection Limit • MDLs are determined according to 40 CFR, part 136, Appendix B • Seven replicate laboratory control samples, analyzed for precision • Multiply standard deviation by 3.14 (Student’s t- value)
  • 31. Method Detection Limit • Must be performed initially for certification • Must meet criteria specified in method • Must be performed with change in instrumentation or test method • Annually with ELCP
  • 32. New Jersey Quantitation Limits (NJQLs) • The minimum concentration of an analyte that can be quantified with statistical confidence • 5 x MDL, for the NJ Lab Certification Program