Method 5B 1/14/2019 While we have taken steps to ensure the accuracy of this Internet version of the document, it is not the official version. To see a complete version including any recent edits, visit: https://www. ecfr.gov/cgi- bin/ECFR ?yage=browse and search under Title 40, Protection of Environment METHOD 5B—DETERMINATION OF NONSULFURIC ACID PARTICULATE MATTER EMISSIONS FROM STATIONARY SOURCES Note: This method does not include all of the specifications (e.g., equipment and supplies) and procedures (e.g., sampling and analytical) essential to its performance. Some material is incorporated by reference from other methods in this part. Therefore, to obtain reliable results, persons using this method should have a thorough knowledge of at least the following additional test methods: Method 1, Method 2, Method 3, Method 5. 1.0 Scope and Application 1.1 Analyte. Nonsulfuric acid particulate matter. No CAS number assigned. 1.2 Applicability. This method is determining applicable for the determination of nonsulfuric acid particulate matter from stationary sources, only where specified by an applicable subpart of the regulations or where approved by the Administrator for a particular application. 1.3 Data Quality Objectives. Adherence to the requirements of this method will enhance the quality of the data obtained from air pollutant sampling methods. 2.0 Summary of Method Particulate matter is withdrawn isokinetically from the source and collected on a glass fiber filter maintained at a temperature of 160 ±14 °C (320 ±25 °F). The collected sample is then heated in an oven at 160 °C (320 °F) for 6 hours to volatilize any condensed sulfuric acid that may have been collected, and the nonsulfuric acid particulate mass is determined gravimetrically. 3.0 Definitions [Reserved] 4.0 Interferences [Reserved] 5.0 Safety 5.1 Disclaimer. This method may involve hazardous materials, operations, and equipment. This test method may not address all of the safety problems associated with its use. It is the responsibility of the user of this test method to establish appropriate safety and health practices and to determine the applicability of regulatory limitations prior to performing this test method. 6.0 Equipment and Supplies Same as Method 5, section 6.0, with the following addition and exceptions: ------- Method 5B 1/14/2019 6.1 Sample Collection. The probe liner heating system and filter heating system must be capable of maintaining a sample gas temperature of 160 ±14 °C (320 ±25 °F). 6.2 Sample Preparation. An oven is required for drying the sample. 7.0 Reagents and Standards Same as Method 5, section 7.0. 8.0 Sample Collection, Preservation, Storage, and Transport. Same as Method 5, with the exception of the following: 8.1 Initial Filter Tare. Oven dry the filter at 160 ±5 °C (320 ±10 °F) for 2 to 3 hours, cool in a desiccator for 2 hours, and weigh. Desiccate to constant weight to obtain the initial tare weight. Use the applicable specifications and techniques of section 8.1.3 of Method 5 for this determination. 8.2 Probe and Filter Temperatures. Maintain the probe outlet and filter temperatures at 160 ±14 °C (320 ±25 °F). 9.0 Quality Control Same as Method 5, section 9.0. 10.0 Calibration and Standardization Same as Method 5, section 10.0. 11.0 Analytical Procedure 11.1 Record and report the data required on a sheet such as the one shown in Figure 5B-1. 11.2 Handle each sample container as follows: 11.2.1 Container No. 1. Leave the contents in the shipping container or transfer the filter and any loose PM from the sample container to a tared non-reactive oven-proof container. Oven dry the filter sample at a temperature of 160 ±5 °C (320 ±9 °F) for 6 hours. Cool in a desiccator for 2 hours, and weigh to constant weight. Report the results to the nearest 0.1 mg. For the purposes of this section, the term "constant weight" means a difference of no more than 0.5 mg or 1 percent of total weight less tare weight, whichever is greater, between two consecutive weighings, with no less than 6 hours of desiccation time between weighings. 11.2.2 Container No. 2. Note the level of liquid in the container, and confirm on the analysis sheet whether leakage occurred during transport. If a noticeable amount of leakage has occurred, either void the sample or use methods, subject to the approval of the Administrator, to correct the ------- Method 5B 1/14/2019 final results. Measure the liquid in this container either volumetrically to ±1 ml or gravimetrically to ±0.5 g. Transfer the contents to a tared 250 ml beaker, and evaporate to dryness at ambient temperature and pressure. Then oven dry the probe sample at a temperature of 160 ±5 °C (320 ±9 °F) for 6 hours. Cool in a desiccator for 2 hours, and weigh to constant weight. Report the results to the nearest 0.1 mg. 11.2.3 Container No. 3. Weigh the spent silica gel (or silica gel plus impinger) to the nearest 0.5 g using a balance. This step may be conducted in the field. 11.2.4 Acetone Blank Container. Measure the acetone in this container either volumetrically or gravimetrically. Transfer the acetone to a tared 250 ml beaker, and evaporate to dryness at ambient temperature and pressure. Desiccate for 24 hours, and weigh to a constant weight. Report the results to the nearest 0.1 mg. Note: The contents of Container No. 2 as well as the acetone blank container may be evaporated at temperatures higher than ambient. If evaporation is done at an elevated temperature, the temperature must be below the boiling point of the solvent; also, to prevent "bumping," the evaporation process must be closely supervised, and the contents of the beaker must be swirled occasionally to maintain an even temperature. Use extreme care, as acetone is highly flammable and has a low flash point. 12.0 Data Analysis and Calculations Same as in Method 5, section 12.0. 13.0 Method Performance [Reserved] 14.0 Pollution Prevention [Reserved] 15.0 Waste Management [Reserved] 16.0 References Same as Method 5, section 17.0. ------- Method 5B 17.0 Tables, Diagrams, Flowcharts, and Validation Data 1/14/2019 Container number Weight of particulate collectet ,mg Final weight Tare weight Weight gain 1. 2. Total: Less acetone blank Weight of particulate matter Volume of liquid water collected Impinger volume, Silica gel weight, ml g Final Initial Liquid collected Total volume collected g* ml *Convert weight of water to volume by dividing total weight increase by density of water (1 g/ml). Figure 5B-1. Analytical Data Sheet ------- |