Section Four

Good Laboratory Practice:

Quality Assurance of Analytical
Measurements
 What is Good Laboratory
Practice (GLP)?
• The goal of GLP is to certify that every step
of the analysis is valid.
• Standard Operating Procedures (SOP)
• Quality Assurance Unit (QAU)
 Validation of Analytical Methods
Defintion Example
Technique Scientific principle gives Spectrophotometry
compositional information
Method Distinct adaptation of Pararosaniline
technique selected method to
measurement purpose determine SO2
Procedure Written directions to use a ASTM D2914
method Sulfur Dioxide
Protocol Set of definitive directions EPA Reference
that must be followed, Method Determine
SO2 Atmosphere
without exception
Validation
Validationinvolves
involves
determining:
determining:
•selectivity
•selectivity
•linearity
•linearity
•accuracy
•accuracy
•precision
•precision
•sensitivity
•sensitivity
•range
•range
•limit
•limitof
ofdetection
detection
•limit
•limitof
ofquantitation
quantitation
•ruggedness/robustness
•ruggedness/robustness

Standard
Standardreference
reference
materials
materials(SRMs)
(SRMs)best
bestfor
for
determining accuracy.
determining accuracy.

Fig. 4.1. General process for evaluation/validation of methodology.

©Gary Christian, Analytical Chemistry, 6th Ed. (Wiley)
 RF
RF==(signal
(signal––yyintercept)/(concentration).
intercept)/(concentration).
AAzero
zeroslope
slopeindicates
indicateslinear
linearresponse
responseover
overthe
theconcentration
concentrationrange
rangeselected.
selected.

©Gary Christian,
Analytical Chemistry,
6th Ed. (Wiley)

Fig. 4.2. Response factor plot for Figure 3.8. (p. 104)
The
Theprecision
precisionbecomes
becomespoorer
pooreratatlow
lowconcentrations.
concentrations.
(Also
(Alsosometimes
sometimesatathigh
highconcentrations,
concentrations,asasin
inspectrophotometric
spectrophotometricmeasurements
measurements ––
see
seespectrometric
spectrometricerror,
error,Fig.
Fig.16.27.)
16.27.)

Fig. 4.3. Dependence of relative standard deviation on concentration.

©Gary Christian, Analytical Chemistry, 6th Ed. (Wiley)
ZZ==(X
(Xi-X)/s = (mean conc. of lab – accepted conc.)/(S.D. accepted conc.)
i-X)/s = (mean conc. of lab – accepted conc.)/(S.D. accepted conc.)

AAz-value
z-valueof
of22means
meansaalab
labisistwo
twoS.D.
S.D.away
awayfrom
fromthe
theaccepted
acceptedvalue
value
(95%
(95%chance
chanceofofsystematic
systematicerror).
error).

Fig. 4.4. Representative z-value distributions for ©Gary Christian,

Analytical Chemistry,

proficiency tests with a series of laboratories. 6th Ed. (Wiley)