QA Course Total

Quality is a Lousy Idea-
If its Only an Idea

Quality Assurance vs.
Quality Control
Quality Assurance Quality Control
An overall A series of
management plan to analytical
guarantee the measurements used
integrity of data to assess the
(The system) quality of the
analytical data
(The tools)
True Value vs. Measured
Value
True Value Measured Value
The known, The result of an
accepted value of individuals
a quantifiable measurement of a
property quantifiable
property
Accuracy vs. Precision
Accuracy Precision
How well a How well a series
measurement of measurements
agrees with an agree with each
accepted value other
Accuracy vs. Precision
Systematic vs.
Random Errors
Systematic Error Random Errors
Avoidable error due Unavoidable errors
to controllable that are always
variables in a present in any
measurement. measurement.
Impossible to
eliminate
Quality Control Measures
Standards and Calibration
Blanks
Recovery Studies
Precision and Accuracy Studies
Method Detection Limits
NJQLs
Prepared vs. Purchased Standard
Signals: Peak Area, Beers Law
Calibration Curves
Continuing Calibration Checks
Internal Standards
Performance Testing.
Calibration Curves
Graphical representation of the
relationship between:
The concentration of the analyte

and
The analytical signal
Calibration Curve for DDT
500
Peak area x 10 6
400
y = 9.3005x + 4.3313
300
200 2
R = 0.9989
100
0
0 10 20 30 40 50 60
Parts per trillion DDT

Continuing Calibration
Verification
Many methods dont 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
Analyte spiked into reagent water
Subjected to all sample prep and
analytical procedures
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
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
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 (Students t- value)
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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Quality is a Lousy Idea-

If its Only an Idea

The concentration of the analyte

Parts per trillion DDT

Labs must periodically ?

Field Reagent Blanks

Opened at the sampling site,

Not always required in EPA methods

Laboratory Control Samples

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