Reference method for measuring releases of fine particulate matter from stationary sources: method I


Method I: Options

  1. Applicability
  2. Principle
  3. Apparatus
  4. Reagents and Materials
  5. Procedures
  6. Calculations
  7. Nomenclature

1.  Applicability

This method is used to measure the mass concentration and mass emission or release of filterable PM2.5 and condensable particulate matter (CPM) released from stationary sources. The front-half of Method G is combined with the back-half of Method H to form a method for fine particulate matter from stationary sources. The sum of the filterable PM2.5 and the condensable particulate matter will give total PM2.5. This method is subject to the limitations of Methods G and H.

2.  Principle

The principles provided in Methods G and MethodH are applicable to this method.  Three valid tests are required for the determination of total PM2.5. Each test must be a minimum of two hours and collect at least 1.5 (53 ft³) of stack gas on a dry basis at reference conditions.

3.  Apparatus

As per Methods G and MethodH.

4.  Reagents and Materials

The reagents and materials listed in Section 4 of Method H must be utilized when combining Methods G and H.  This includes the use of HPLC grade water used for rinsing both the front- and back-half components.

5.  Procedures

5.1  Taring

As per Method H.

5.2  Sample Collection

Sample Rate Selection. Use the procedures in Section 5.1 and Figure G-9 of Method G to select an appropriate sampling rate for the cyclone such that the criteria for dwell times, cutoff diameter and isokinetics are met. Select a sample run time greater than two hours that results in a sample volume of at least 1.5 m³ (5 ft³) at dry standard conditions.

Sample Train Preparation. Combine the front half of the Method G train with the back half of the Method H train as depicted in Figure I-1. Measure 3 mL of ethanol and make up to 10 mL with HPLC water and add to the condensate trap or stemless impinger. The first impinger contains 100 mL of HPLC water, the second impinger is left empty and the third one must contain 100 to 300 g of silica gel desiccant. Record the weight of the impinger/condensate trap (after the ethanol addition), the condenser and the other three impingers (to the nearest 0.5 g) on the Moisture Analysis Data Sheet (Figure H-2).

Figure I-1 Method I Schematic: Combined Methods G and H

Figure I-1 Method I Schematic: Combined Methods G and H (See long description below)
Description of Figure I-1

Figure I-1 is a schematic depiction of the Method I sampling train, which in essence consists of the front half (cyclone, probe and filter) of Method G, combined with the impinger train of Method H.

 

Sample Train Operation. As per Method G, use Figure G-9 or a similar strategy to determine the orifice setting at each sampling point and a sample time resulting in a total sample volume of at least 1.5 m³ (53 ft³) at dry standard conditions. 

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5.3  Sample Recovery

Carefully disconnect the probe from the sampling train, seal all openings. Seal the openings of the PM2.5 cyclone. Exercise care in moving the train components from the test site to the sample recovery area to minimize the loss of collected particulate matter or contamination.

In the sample recovery area, weigh the components of the sample train. Record the weight (to the nearest 0.5 g) of the condenser, condensate trap and each of the three impingers on the Moisture Analysis Data Sheet (Figure H-2).

Recover the front-half train components as described in Section 5.2 of Method G using HPLC water in place of Type II to avoid accidental use of Type II water in the CPM recovery. Recover the back-half train components as described in Section 5.3 of Method H.  

5.4  Sample Analysis

All analyses shall be completed within two weeks of sampling in a clean laboratory equipped with a fume hood. The relative humidity of the room in which the weighing is performed should be maintained at or below 50%.

In the laboratory, remove the containers from their protecting polyethylene bags and verify that no liquid leaks had taken place. Leaks will invalidate the test results. Note the condition of the samples as received in the laboratory in Figure I-2.

Figure I-2 Description of Received Samples

Figure I-2 Description of Received Samples (See long description below)
Description of Figure I-2

Figure I-2 is a template to document the conditions in which the laboratory receives the samples from each Method I test run. The heading prompts the recording of the following data for each test run:

  • Plant
  • Location
  • Test number
  • Date
  • Test conducted by

The 3 columns of the main section of the table deals with the sample reception conditions: Container/Jar No.; Description; and Observations.

  • Each run produces 11 samples that that may be checked in the corresponding row.
  • The sample descriptions are listed in the second column:
    1. Water and acetone rinses of cyclone and nozzle (combine as per Method G)
    2. Water and acetone rinses of cyclone exit tube, probe liner and front half of the filter holder (combine as per Method G)
    3. Filter;
    4. Condensate, soaks and HPLC water rinses of the back half of the primary filter holder, condenser, condensate trap, and front half of the mist filter;
    5. Dichloromethane (DCM) soaks and rinses of the back half of the primary filter holder, condenser, condensate trap, and front half of the mist filter;
    6. Mist filter;
    7. Front-half HPLC water blank;
    8. Front-half acetone blank;
    9. Back-half HPLC water/ethanol blank;
    10. Dichloromethane blank, and
    11. Mist filter blank.
  • The Observations column elicits answer to questions about leakage during transport, and sample container seal conditions.

 

Sample analysis requires numerous gravimetric determinations of evaporated residues. Follow the procedures in Method G for processing Containers 1, 2, 3, 7 and 8. Follow the procedures in Method H for Containers 4, 5, 6, 9, 10 and 11. Once a constant weight has been determined for all the sample residues use the Particulate Analytical Data Sheet in Figure I-3 to determine the weight of the different particulate fractions.

Figure I-3 Particulate Analytical Data Sheet

Figure I-3 Particulate Analytical Data Sheet (See long description below)
Description of Figure I-3

Figure I-3 is a template to record the gravimetric determinations required for the various forms of particulate matter. The heading prompts the recording of the following data for each test run:

  • Plant
  • Location
  • Test number
  • Date
  • Test conducted by

The 6 columns of the main section of the table have the following titles:

  • Train Component
  • Description
  • Final Weight (mg)
  • Tare Weight (mg)
  • Weight of Particulate (mg)
  • Fraction

Columns 1, 2, and 6 are descriptive. The gravimetric results are entered in columns 3 and 4, and the net values are recorded in column 5.

Finally Figure H-6 includes the formulas to calculate Filterable PM2.5, CPM, Total PM2.5, Filterable PM, and Total PM.

 

Notes:

  • The weight of the blanks must not exceed 2 mg
  • Do not correct for negative blank values
  • No blank corrections are allowed when blank residue is above 2 mg

6.  Calculations

Calculate the stack gas parameters as per Section 6 of Method G. If applicable, calculate the filterable PM, PM2.5 and CPM concentrations and emission rates as per Section 6 of Methods G and MethodH.

The method detection limit for the gravimetric determination of residues from jars is 0.42 mg. The total expanded uncertainty (95% probability) for TPM, that consists of filterable PM (includes +PM2.5 and PM2.5) and condensable particulate matter, is 1.5 mg.

Concentration of TPM or TPM2.5. Calculate the concentration of TPM or TPM2.5 using Equation I-1  

Equation H-1

Equation I-1 (See long description below)
Description of Equation I-1

Concentration of TPM
CTPM equals to the total particulate matter (filterable + condensable) weight collected in the run (W TPM, mg) divided by the dry sample volume at reference conditions (Vm ref, m3).

Concentration of TPM2.5
CTPM2.5 equals to the total PM2.5 (filterable + condensable) collected in the run (W TPM2.5, mg) divided by the dry sample volume at reference conditions (Vm ref, m3).

 

Mass Emission Rate.  Calculate the mass emission or release rate of TPM or TPM2.5 using Equation I-2.

Equation I-2

Equation I-2 (See long description below)
Description of Equation I-2

Mass Emission Rate of TPM
ERTPM (kg/hr) equals to the product of the 10-6 constant, times the concentration of TPM, (CTPM, mg/m3), times the volumetric stack gas flow rate (Qs, m3/h).

Mass Emission Rate of TPM2.5
ERTPM2.5 (kg/hr) equals to the product of the 10-6 constant, times the concentration of TPM2.5, (CTPM2.5, mg/m3), times the volumetric stack gas flow rate (Qs, m3/h).

 

7.  Nomenclature

C TPM2.5
concentration of total PM 2.5 in the stack gas on a dry basis at reference temperature and pressure, mg/m³

C TPM
concentration of total particulate matter in the stack gas on a dry basis at reference temperature and pressure, mg/m³

ER TPM2.5
mass emission rate of total PM 2.5, kg/h

ER TPM
mass emission rate of total particulate matter, kg/h

Q s
volumetric stack gas flow rate on a dry basis at reference temperature and pressure, m³/h

(V m) ref
volume of stack gas sample on a dry basis at reference temperature and pressure, m³

W TPM2.5
weight of total PM 2.5 collected during the test run, mg

W TPM
weight of total particulate collected during the test run, mg

10 -6
conversion, kg/mg

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