Quality Control Terminology

QC Parameter Accuracy Precision Extraction efficiency Contamination

Procedures Analysis of reference materials or known standards Analysis of replicate samples Analysis of matrix spikes Analysis of blanks

Procedure in Quality Control

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

True Value vs. Measured Value

True Value The known, accepted value of a quantifiable property Measured Value The result of an individuals measurement of a quantifiable property

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, Beers Law Calibration Curves Continuing Calibration Checks Internal Standards Performance Testing.

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

Calibration Curves
Graphical representation of the relationship between:
The concentration of the analyte and The analytical signal

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

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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.

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

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

Random Error

An error which varies in an unpredictable manner, in magnitude and sign, when a large number of measurements of the same quantity are made under effectively identical conditions. Random errors create a characteristic spread of results for any test method and cannot be accounted for by applying corrections. Random errors are difficult to eliminate but repetition reduces the influences of random errors. Examples of random errors include errors in pipetting and changes in incubation period. Random errors can be minimized by training, supervision and adherence to standard operating procedures.

Random Errors

x x True Value x x x x x x x x x x x

Systematic Error
An error which, in the course of a number of measurements of the same value of a given quantity, remains constant when measurements are made under the same conditions, or varies according to a definite law when conditions change. Systematic errors create a characteristic bias in the test results and can be accounted for by applying a correction. Systematic errors may be induced by factors such as variations in incubation temperature, blockage of plate washer, change in the reagent batch or modifications in testing method.

Systematic Errors

x x True Value x x x x x x x

Process Control Chart

Great practical use in factories First introduced by Walter A. Shewhart Help to reduce variability Monitor performance over time Trends and out-of-control are immediately detected

Shewhart Chart
100 90 80 70 60 50 40 30 20 10 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14

Desired Value

+3 sd +2 sd +1 sd

Target value
-1 sd -2 sd -3 sd

15 16

SQC Run