2. Measurement Process Characterization
2.3. Calibration
2.3.6. Instrument calibration over a regime

## What can go wrong with the calibration procedure

Calibration procedure may fail to eliminate bias There are several circumstances where the calibration curve will not reduce or eliminate bias as intended. Some are discussed on this page. A critical exploratory analysis of the calibration data should expose such problems.
Lack of precision Poor instrument precision or unsuspected day-to-day effects may result in standard deviations that are large enough to jeopardize the calibration. There is nothing intrinsic to the calibration procedure that will improve precision, and the best strategy, before committing to a particular instrument, is to estimate the instrument's precision in the environment of interest to decide if it is good enough for the precision required.
Outliers in the calibration data Outliers in the calibration data can seriously distort the calibration curve, particularly if they lie near one of the endpoints of the calibration interval.
• Isolated outliers (single points) should be deleted from the calibration data.
• An entire day's results which are inconsistent with the other data should be examined and rectified before proceeding with the analysis.
Systematic differences among operators It is possible for different operators to produce measurements with biases that differ in sign and magnitude. This is not usually a problem for automated instrumentation, but for instruments that depend on line of sight, results may differ significantly by operator. To diagnose this problem, measurements by different operators on the same artifacts are plotted and compared. Small differences among operators can be accepted as part of the imprecision of the measurement process, but large systematic differences among operators require resolution. Possible solutions are to retrain the operators or maintain separate calibration curves by operator.
Lack of system control The calibration procedure, once established, relies on the instrument continuing to respond in the same way over time. If the system drifts or takes unpredictable excursions, the calibrated values may not be properly corrected for bias, and depending on the direction of change, the calibration may further degrade the accuracy of the measurements. To assure that future measurements are properly corrected for bias, the calibration procedure should be coupled with a statistical control procedure for the instrument.
Example of differences among repetitions in the calibration data An important point, but one that is rarely considered, is that there can be differences in responses from repetition to repetition that will invalidate the analysis. A plot of the aggregate of the calibration data may not identify changes in the instrument response from day-to-day. What is needed is a plot of the fine structure of the data that exposes any day to day differences in the calibration data.
Warning - calibration can fail because of day-to-day changes A straight-line fit to the aggregate data will produce a 'calibration curve'. However, if straight lines fit separately to each day's measurements show very disparate responses, the instrument, at best, will require calibration on a daily basis and, at worst, may be sufficiently lacking in control to be usable.