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A gas dilution system can provide known values of calibration gases through controlled dilution of high-level calibration gases with an appropriate dilution gas. The instrumental test methods in 40 CFR Part 60 -- e.g., Methods 3A, 6C, 7E, 10, 15, 16, 20, 25A and 25B -- require on-site, multi-point calibration using gases of known concentrations. A gas dilution system that produces known low-level calibration gases from high-level calibration gases, with a degree of confidence similar to that for Protocol1 gases, may be used for compliance tests in lieu of multiple calibration gases when the gas dilution system is demonstrated to meet the requirements of this method. The Administrator may also use a gas dilution system in order to produce a wide range of Cylinder Gas Audit concentrations when conducting performance specifications according to Appendix F, 40 CFR Part 60. As long as the acceptance criteria of this method are met, this method is applicable to gas dilution systems using any type of dilution technology, not solely the ones mentioned in this method.
The gas dilution system shall be evaluated on one analyzer once during each field test. A precalibrated analyzer is chosen, at the discretion of the source owner or operator, to demonstrate that the gas dilution system produces predictable gas concentrations spanning a range of concentrations. After meeting the requirements of this method, the remaining analyzers may be calibrated with the dilution system in accordance to the requirements of the applicable method for the duration of the field test. In Methods 15 and 16, 40 CFR Part 60, Appendix A, reactive compounds may be lost in the gas dilution system. Also, in Methods 25A and 25B, 40 CFR Part 60, Appendix A, calibration with target compounds other than propane is allowed. In these cases, a laboratory evaluation is required once per year in order to assure the Administrator that the system will dilute these reactive gases without significant loss. Note: The laboratory evaluation is required only if the source owner or operator plans to utilize the dilution system to prepare gases mentioned above as being reactive.
The gas dilution system shall produce calibration gases whose measured values are within +2 percent of the predicted values. The predicted values are calculated based on the certified concentration of the supply gas (Protocol gases, when available, are recommended for their accuracy) and the gas flow rates (or dilution ratios) through the gas dilution system.
2.1.1 The gas dilution system shall be recalibrated once per calendar year using NIST-traceable primary flow standards with an uncertainty <0.25 percent. A label shall be affixed at all times to the gas dilution system listing the date of the most recent calibration, the due date for the next calibration, and the person or manufacturer who carried out the calibration. Follow the manufacturer's instructions for the operation and use of the gas dilution system. A copy of the manufacturer's instructions for the operation of the instrument, as well as the most recent recalibration documentation shall be made available for the Administrator's inspection upon request.
2.1.2 Some manufacturers of mass flow controllers recommend that flow rates below 10 percent of flow controller capacity be avoided; check for this recommendation and follow the manufacturer's instructions. One study has indicated that silicone oil from a positive displacement pump produces an interference in SO2 analyzers utilizing ultraviolet fluorescence; follow laboratory procedures similar to those outlined in Section 3.1 in order to demonstrate the significance of any resulting effect on instrument performance.
An EPA Protocol calibration gas is recommended, due to its accuracy, as the high-level supply gas.
An EPA Protocol gas shall be used as an independent check of the dilution system. The concentration of the mid-level supply gas shall be within 10 percent of one of the dilution levels tested in Section 3.2.
If the gas dilution system is to be used to formulate calibration gases with reactive compounds (Test Methods 15, 16, and 25A/25B (only if using a calibration gas other than propane during the field test) in 40 CFR Part 60, Appendix A), a laboratory certification must be conducted once per calendar year for each reactive compound to be diluted. In the laboratory, carry out the procedures in Section 3.2 on the analyzer required in each respective test method to be laboratory certified (15, 16, or 25A and 25B for compounds other than propane). For each compound in which the gas dilution system meets the requirements in Section 3.2, the source must provide the laboratory certification data for the field test and in the test report.
The gas dilution system shall be evaluated at the test site with an analyzer or monitor chosen by the source owner or operator. It is recommended that the source owner or operator choose a precalibrated instrument with a high level of precision and accuracy for the purposes of this test. This method is not meant to replace the calibration requirements of test methods. In addition to the requirements in this method, all the calibration requirements of the applicable test method must also be met.
3.2.1 Prepare the gas dilution system according to the manufacturer's instructions. Using the high-level supply gas, prepare, at a minimum, two dilutions within the range of each dilution device utilized in the dilution system (unless, as in critical orifice systems, each dilution device is used to make only one dilution; in that case, prepare one dilution for each dilution device). Dilution device in this method refers to each mass flow controller, critical orifice, capillary tube, positive displacement pump, or any other device which is used to achieve gas dilution.
3.2.2 Calculate the predicted concentration for each of the dilutions based on the flow rates through the gas dilution system (or the dilution ratios) and the certified concentration of the high-level supply gas.
3.2.3 Introduce each of the dilutions from Section 3.2.1 into the analyzer or monitor one at a time and determine the instrument response for each of the dilutions.
3.2.4 Repeat the procedure in Section 3.2.3 two times, i.e., until three injections are made at each dilution level. Calculate the average instrument response for each triplicate injection at each dilution level. No single injection shall differ by more than +2 percent from the average instrument response for that dilution.
3.2.5 For each level of dilution, calculate the difference between the average concentration output recorded by the analyzer and the predicted concentration calculated in Section 3.2.2. The average concentration output from the analyzer shall be within +2 percent of the predicted value.
3.2.6 Introduce the mid-level supply gas directly into the analyzer, bypassing the gas dilution system. Repeat the procedure twice more, for a total of three mid-level supply gas injections. Calculate the average analyzer output concentration for the mid-level supply gas. The difference between the certified concentration of the mid-level supply gas and the average instrument response shall be within +2 percent.
3.3 If the gas dilution system meets the criteria listed in Section 3.2, the gas dilution system may be used throughout that field test. If the gas dilution system fails any of the criteria listed in Section 3.2, and the tester corrects the problem with the gas dilution system, the procedure in Section 3.2 must be repeated in its entirety and all the criteria in Section 3.2 must be met in order for the gas dilution system to be utilized in the test.
1. "EPA Traceability Protocol for Assay and Certification of Gaseous calibration Standards," EPA-600/R93/224, Revised September 1993.