Scribd
Upload
62 views

Quality in Analytical Laboratory: Chem 725 Redel L. Gutierrez Chem. Dept, Cas, Clsu

This document discusses key concepts in quality control and quality assurance for analytical laboratories. It defines terms like quality assurance, quality control, accuracy, precision, systematic and random errors. It also describes various quality control measures laboratories employ, such as standards and calibration, blanks, recovery studies, precision and accuracy studies, method detection limits, and regulatory requirements. The goal is to ensure quality data and reliable analytical results.

Uploaded by

Nora Buan
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PPTX, PDF, TXT or read online on Scribd
62 views

Quality in Analytical Laboratory: Chem 725 Redel L. Gutierrez Chem. Dept, Cas, Clsu

This document discusses key concepts in quality control and quality assurance for analytical laboratories. It defines terms like quality assurance, quality control, accuracy, precision, systematic and random errors. It also describes various quality control measures laboratories employ, such as standards and calibration, blanks, recovery studies, precision and accuracy studies, method detection limits, and regulatory requirements. The goal is to ensure quality data and reliable analytical results.

Uploaded by

Nora Buan
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PPTX, PDF, TXT or read online on Scribd
You are on page 1/ 32

Quality in

Analytical
Laboratory
Chem 725
Redel L.
Gutierrez
Chem. Dept,
CAS, CLSU
Quality is a Lousy Idea-

If it’s Only an Idea


Quality Assurance vs.
Quality Control
Quality Quality Control
Assurance QA is QC is a system of
a management technical activities
system that to control data
ensures QC is quality (blanks
working as and spikes)
intended (The “tools”)
(The
True Value vs. Measured
Value
True Value Measured Value
The known, The result of an
accepted value of individual’s
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 other
value
Accuracy vs. Precision
Systematic vs.
Random
Systematic Errors
Error Random Errors
Avoidable error Unavoidable errors
due 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
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 concentration of the analyte


and
• The analytical signal
Calibration Curve for
500 DDT
400
y = 9.3005x +
Peak area x

300 4.3313

200
R2 = 0.9989
106

100

0
0 10 20 30 40 50 60

Parts per trillion DDT


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
• 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
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

You might also like

pFad - Phonifier reborn

Pfad - The Proxy pFad of © 2024 Garber Painting. All rights reserved.

Note: This service is not intended for secure transactions such as banking, social media, email, or purchasing. Use at your own risk. We assume no liability whatsoever for broken pages.


Alternative Proxies:

Alternative Proxy

pFad Proxy

pFad v3 Proxy

pFad v4 Proxy