| ILM04.0/05.0 | Method 200.7 | Method 6010B | Brief definition of function according to ILM04.0/05.0 |
|---|---|---|---|
| Analytical Sample | Sample - this method does not clearly indicate counting rules | Sample - this method does not clearly indicate counting rules | Everything other than the ICV, ICB, CCV, CCB, calibration standards and calibration blank. |
| Sample Delivery Group (SDG) | Group of 20 samples | Not clearly stated | A unit within a sample case that is used to identify a group of samples for delivery. An SDG is a group of 20 or fewer real samples within a case. Note that since sample deliveries will not include Preparation Blanks, ICSA and ICSAB and other solutions that are counted as Analytical Samples, the number of Analytical Samples for an SDG may be higher than 20. |
| Contract Required Detection Limit (CRDL) | No equivalent | Estimated IDLs are provided but not mandated. | The detection limits for each of the 22 elements that must be met to comply with the Statement of Work or Method. |
| Instrument Detection Limit (IDL) | Method detection limits (MDL) - 7 replicates of fortified reagent water at 2-3 x instrument detection limit | Method detection limits (MDL) - at 3-5 times anticipated detection limits - 7 replicates on 3 non-consecutive days 'for additional confirmation'. | The detection limit calculated by multiplying by 3 the average of the standard deviations obtained on 3 nonconsecutive days from a standard solution at a concentration of 3-5 times the instrument manufacturers suggested IDL. Seven consecutive measurements are taken to define the standard deviation under the same conditions as the proposed analytical method. |
| Initial Calibration Verification (ICV) | See IPC below. | ICV | Used to initially verify the validity of the calibration by measuring the recovery of analytes in this standard immediately after calibration. A second source standard. |
| Initial Calibration Blank (ICB) | Calibration blank | Calibration blank | A “calibration blank” that immediately follows the ICV. Usually compared to the Instrument Detection Limit (IDL). |
| Continuing Calibration Verification (CCV) | Initial performance check (IPC) standard - combines both ICV and CCV - first time limits are + 5% | CCV - accompanied by calibration blank - can use ICV instead - ± 10% limits plus < 5 %RSD | Used to verify the validity of the calibration on an on-going basis. This standard is measured at a frequency of every 10 'analytical samples'. Recovery limits + 10% |
| Continuing Calibration Blank (CCB) | Calibration blank | Calibration blank | A 'calibration blank' that immediately follows the CCV. Usually compared to the Instrument Detection Limit (IDL). |
| Contract Required Detection Limit Test for ICP (CRI) | No equivalent | No equivalent | A standard containing the analytes at 2 times the CRDL or IDL whichever is greater. No control limits yet applicable. Not required for Al, Ba, Ca, Fe, Mg, Na and K. Analyzed at the beginning and end of the SDG. |
| Interference Check Solution (ICSA) | Spectral interference check (SIC) solutions - up to 17 interferent solutions tested - test for 10% error in baseline | Interference check sample - analytes at 0.5-1.0 mg/L - interferents at 100 mg/L of Al, Ca, Cr, Cu, Fe, Mg, Mn, Ni, Ti and V are shown in Table 2 of the method. - test for 20% error in baseline | Used to check the effect of interferents on the determination of the analytes. ICSA is the interferents only solution and contains Al, Ca and Mg at 500 mg/L and Fe at 200 mg/L. Analytes should be within 0 ± 2 x CRDL. Analyzed at the beginning and end of the SDG. Note the 20% error limit in the 6010B method probably refers to ± 10% since otherwise the method is exactly the same as 200.7. |
| Interference Check Solution (ICSAB) | See above. | See above. | Used to check the effect of interferents on the determination of the analytes. ICSAB contains both interferents and 16 selected analytes. Analytes must be recovered within ± 20%. Analyzed at the beginning and end of the SDG. |
| Preparation Blank (Prep Blk) | Lab reagent blank (LRB) | Method blank | Also known as a Reagent Blank. A volume of deionized distilled water processed through the sample preparation procedure. Analytes are then monitored versus the CRDL. In ILM04.0/05.0, no preparationblank correctionof samples is done. One per SDG. |
| No equivalent | Lab fortified blank (LFB) - an aliquot of LRB which has been spiked with analytes - one per SDG | No equivalent | |
| Lab Control Sample (LCS) | Quality control sample (QCS) - 3 analyses to within + 5% recovery | No equivalent | A control standard sourced from the EPA or another independent source. The LCS is put through the sample preparation process and then the recovery of the analyes is calculated and compared to ± 20% limits. One per SDG. |
| Duplicate (Dup) | Laboratory duplicates (LD1 and LD2) | Matrix spiked duplicate Samples - measure 2 duplicates of a spiked sample - RPD to 20% - and spike recovery to ± 25% | A duplicate aliquot of a sample, put through the sample preparation procedure. Acts as a monitor for contamination and losses during sample preparation. The Relative Percent Difference between the duplicate and the sample is calculated and compared to ± 20% limits or CRDL limits. One per SDG. Note the Matrix Spiked Duplicate of 6010B tries to combine both the Matrix Spike and Duplicate tests into one but most ICP software is currently not designed to handle this combination. |
| Serial Dilution (Ser) | Dilution test | Dilution test - do for new or unusual matrices | Conduct a five fold dilution on one sample from each SDG. The calculated result after correction for dilution must agree within ± 10% of the undiluted sample result. |
| Spiked Sample Analysis (SSA) or Matrix Spike (MS) | Lab fortified matrix (LFM) - spike every 10 % of samples - recover to ± 30% | No equivalent (see PDSA) | A spike is added to a sample prior to the digestion or sample preparation procedures. The recovery of the spike is calculated and compared to ± 25% limits. A matrix spike is required for each SDG. |
| Linear Range Analysis (LRA) | Linear dynamic range (LDR) - verified annually - top standard recovered to - 10% limit - dilute all samples that are more than 90% of the LDR | LDR - as per 200.7 | A standard which is analyzed quarterly to confirm the linearity of analytical calibrations. A high level standard must be recovered within 5% of the true value. This defines the upper limit of the linear dynamic range. |
| Post Digestion Spike - only required if the SSA fails | Analyte addition test - spike at 20-100 times the MDL - recover to ± 15% limits | Post digestion spike addition (PDSA) - do for new or unusual matrices - spike at 10-100 times the MDL - recover to ± 25% limits | Post digestion spikes are often used to assess whether the Method of Standard Additions is required. This is done separately from pre-digestion spikes because the pre¬digestion spike might be indicative of contamination picked up during the sample preparation procedure. |
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