Ch 5 Quality Assurance and Calibration Methods Flashcards
Quality assurance
what we do to get the right answer for our purpose
Raw data
individual measurements, such as peak areas from a chromatogram or volumes from a buret
Treated data
concentrations or amounts found by applying a calibration procedure to the raw data
Results
quantities reported after statistical analysis of treated data
such as mean, standard deviation, and confidence internal
Use objective
states purpose for which results will be used
prevent misuse of data and results
Specifications might include (9)
- sampling requirements
- accuracy and precision
- rate of false results
- selectivity
- sensitivity
- acceptable blank values
- recovery of fortification
- calibration checks
- quality control samples
Sensitivity
the capability of responding reliably and measurably to changes in analyte concentration
p.s. a method must have a detection limit lower than the concentrations to be measured
= slope of the calibration curve
= (change in signal)/(change in analyte concentration)
Specifications
stating how good the numbers need to be and what precautions are required in the analytical procedure
Quality assurance begins with sampling
- choose representative samples
- analyte must be reserved after the sample is collected
Why samples of trace metal analysis are usually collected in plastic or Teflon containers, instead of glass?
Metal ions found on glass surfaces leach out into the sample over time
Why samples for organic analysis are usually collected in glass containers - not plastic?
Organic plasticizers leached from plastic containers -> contaminate the sample
p.s samples are often stored in the dark in a refrigerator to minimize the degradation of organic analytes.
False-positive
says that the concentration exceeds the legal limit when, in fact, the concentration is below the limit
False-negative
says the concentration is below the limit when it is actually above the limit
Selectivity (aka specificity)
ability to distinguish analyte from other species in the sample (avoiding interference)
Specification could include
required accuracy and precision, reagent purity, tolerances for apparatus, the use of standard reference materials, and acceptable values for blanks
Standard reference materials
contain certified levels of analyte in realistic materials that you might be analyzing, such as blood or coal or metal alloys
method blank
a sample containing all components except analyte, and it is taken through all steps of the analytical procedure
p.s. subtract the response of the blank from eh response of a real sample prior to calculating the quantity of analyte in the sample
reagent blank
similar to method blank, but it has not been subjected to all sample preparation procedures
field blank
similar to a method blank, but it has been exposed to the site of sampling
matrix
everything else in the sample other than analyte
spike (aka fortification)
a known quantity of analyte added to a sample to test whether the response to the spike is the same as that expected from a calibration curve
p.s. analyze same as unknown