Calibration Requirements for Organic Analyses
Effective Date: 07/2008
Point of Contact: Quality Engineer for Regulatory Programs
The manufacturer's specifications for tuning the gas chromatograph/mass spectrometer (GC/MS) system must be met before calibration. In the case of GC/MS, the same acquisition parameters for calibration, calibration confirmation and sample analyses as used to tune instrument must be used. The calibration for measurement systems, such as the GC/MS, should meet manufacturer's specifications and establish a working response range using a sufficient number of standards. Accuracy of the calibration and the standards used for calibration must be verified by analyzing an initial calibration verification (ICV) standard. Continuing calibration verification (CCV) must be performed routinely or before running samples. Calibration must be performed upon repeated failure of the continuing calibration verification standard and suitable corrective action. Analytical techniques not addressed in this plan are developed according to the Procedures section with consideration given to the quality control requirements (e.g., tune, surrogates, calibration) presented in the Quality Control section and the following tables:
- Minimum Calibration Requirements for Gas Chromatograph/Mass Spectrometer System
- Minimum Calibration Requirements for Gas Chromatograph System
- Minimum Calibration Requirements for Total Organic Carbon, Total Inorganic Carbon, and Total Carbon Analysis
Minimum Calibration Requirements for Gas Chromatograph/Mass Spectrometer System
| Calibration Requirements | Compounds | Acceptance Criteria | Corrective Action | Frequency |
|---|---|---|---|---|
| Tune | Tuning standard specified by method and/or manufacturer | BFB and DFTPP shall meet minimum regulatory criteria on Minimum Ion Abundance Requirements for Volatile Organic Analysis and Minimum Ion Abundance Requirements for Semivolatile Organic Analysis. Different tune criteria specified by manufacturer or developed according to Procedures section | Re-tune or repair as necessary, Recalibrate as required | 12 hours |
| Calibration | Five concentrations of analytes of interest per CLP or client agreements, includes internal standards and surrogates | Standard curve meets CLP maximum RSD and minimum RRF criteria or according to Procedures section | Repair as necessary, re-tune and recalibrate as required | Upon failure of continuing calibration |
| ICV | Analytes of interest per CLP or client agreements, includes internal standards and surrogates | Standard meets maximum %D of ±25% and minimum RRF of 0.05 or developed according to Procedures section | Investigate the system and initiate corrective action | Performed at calibration |
| CCV | Analytes of interest per CLP or client agreements, includes internal standards and surrogates | Standard meets CLP maximum %D and minimum RRF criteria or developed according to Procedures section | Investigate the system and initiate corrective action | Start of each 12 hour clock but after tune |
| Internal standards | Compounds selected and concentrations used are based on CLP or client agreement. Added to each standard and blank just prior to analysis. (Added to all samples just prior to analysis. See Quality Control section) | Meet criteria of retention times within 0.5 minutes of last continuing calibration check, EICP within -50% to +150% of last calibration (or continuing calibration) standard | Investigate the system or re-run, and re-run any sample with internal standard not meeting criteria | All analyses except tune |
| Surrogates | Compounds selected and concentrations used based on CLP or client agreement. Added to each standard and blank. (Added during preparation to samples and associated PB. See Quality Control section) | Meet CLP criteria for minimum RRF and maximum %RSD or %D (calibration or continuing calibration) or developed according to Procedures section. | See Quality Control section | All analyses except tune |
| Calibration blank (See Quality Control section) | N/A | Before each new analytical run(a) | For dial or slope calibration, analysis of calibration standards must measure within 0.05 pH units of true value A calibration verification standard within 0.1 pH units of true value confirms acceptability of calibration | Investigate. Correct. Recalibrate, as required. |
| ISE Working curve |
Minimum of 3 concentrations, with one near the MDL, to define the working range | Before each new analytical run(a) | A mid-range calibration verification standard within ±10% of true value confirms acceptability of calibration | Investigate. Correct. Recalibrate, as required. |
| ISE Known Addition, etc. | Follow manufacturer's recommendations. | All samples, standards and blanks | Calibration verification within ± 3 standard deviation of the historical mean | Investigate. Correct. Recalibrate, as required. |
| Colorimetric analyses (excluding cyanide) | Blank and a minimum of 3 concentrations, with one near the MDL, to define the working range | Before each new analytical run(a) | A mid-range calibration verification standard within ±10% of true value confirms acceptability of calibration | Investigate. Correct. Recalibrate, as required. |
| Titrimetric | N/A | Analytes of interest < EQL. | Recalibrate | Performed at calibration |
%D = Percent Difference
%R = Percent Recovery
%RSD = Percent Relative Standard Deviation
BFB = Bromofluorobenzene
ICV = Initial calibration verification
CCV = Continuing calibration verification
CLP = Contract Laboratory Program
DFTPP = Decafluorotriphenylphosphine
EICP = Extracted ion current profile
EQL = Estimated Quantitation Limit
PB = Preparation Blank
RCRA = Resource Conservation and Recovery Act.
RRF = Relative Response Factor CLP
Minimum Calibration Requirements for Gas Chromatograph System
| Calibration Requirements | Compounds(a) | Criteria | Corrective Actions | Frequency |
|---|---|---|---|---|
| CLP | Resolution Check, PEM, Aroclor 1016/1260, Aroclor 1221, Aroclor 1232, Aroclor 1242, Aroclor 1248, Aroclor 1254, Toxaphene, Low Point Standard A, Low Point Standard B, Midpoint Standard A, Midpoint Standard B, High Point Standard A, High Point Standard B, Instrument Blank, PEM. | CF and %RSD shall be calculated for each compound %RSD criteria for the CF is used to validate the calibration curve and for average CF calculations | Investigate, correct and re-run if necessaryInvestigate, correct and re-run if necessary | After major maintenance or upon failure of CCV |
| Calibration, Non-CLP Alternate | Minimum three concentrations per each analyte of interest to define the working range with one of the standards near the MDL. Compounds selected and concentrations used based on client agreement. | Calculate mean and %RSD over range. %RSD less than 20 except for any 2 single-component analytes of interest which must be less than 30. Quantitation can then be performed using midpoint CF. | Investigate, correct, and re-run if necessary. Alternatively, construct calibration curve. | After major maintenance or failure of CCV. |
| ICV | Analytes of interest per client agreement. | Standard meets maximum %D of ±25%. | Investigate the system and initiate corrective action | At the time of calibration |
| CCV | For CLP, use instrument blank, PEM, and midpoint standard A and B. For non-CLP use one or more calibration standards periodically to check stability. |
Working calibration curve verified by the measurements of one or more calibration standards CF and retention time evaluated against calibration and all subsequent continuing calibrations. Criteria established through method qualification. | Investigate, correct and re-run as appropriate. All samples since last valid calibration check must be reanalyzed. | For CLP: Blank every 12 hours. PEM every 24 hours, Midpoint standard A and B every 24 hours alternating with PEM. For non-CLP, calibration checked each day samples analyzed. |
CCV = Continuing calibration verification
CF = Calibration factor
CLP = Contract Laboratory Program.
MDL = Method detection limit
PEM = Performance Evaluation Mixture.
RSD = relative standard deviation.
(a) Surrogates shall be included in all standards and blanks (see Quality Control section).
Minimum Calibration Requirements for Total Organic Carbon, Total Inorganic Carbon, and Total Carbon Analysis
| Instrument or Test | Calibration Criteria | Frequency | Acceptance Criteria | Failure Action |
|---|---|---|---|---|
| Combustion-infrared method Persulfate-ultraviolet oxidation Wet oxidation method |
According to manufacturer's recommendation Blank and sufficient standards should be used that encompasses the expected concentration |
Before each new analytical run, or every 15 samples | Follow manufacturer's recommendations | Investigate. Correct if necessary. Recalibrate as required. |
| Coulometric method | Initial calibration performed by manufacturer | Confirm acceptability using performance check | ± 3 standard deviation of the historical mean of the performance check | Investigate. Correct as necessary.. |
aAnalytical run is defined as a sequence of analyses within a continuous time period.