1065.190 PM-stabilization and weighing environments for gravimetric analysis.§ 1065.190 PM-stabilization and weighing environments for gravimetric analysis.
(a) This section describes the two environments required to stabilize and weigh PM for gravimetric analysis: the PM stabilization environment, where filters are stored before weighing; and the weighing environment, where the balance is located. The two environments may share a common space. These volumes may be one or more rooms, or they may be much smaller, such as a glove box or an automated weighing system consisting of one or more countertop-sized environments.
(b) We recommend that you keep both the stabilization and the weighing environments free of ambient contaminants, such as dust, aerosols, or semi-volatile material that could contaminate PM samples. We recommend that these environments conform with an “as-built” Class Six clean room specification according to ISO 14644-1 (incorporated by reference in § 1065.1010); however, we also recommend that you deviate from ISO 14644-1 as necessary to minimize air motion that might affect weighing. We recommend maximum air-supply and air-return velocities of 0.05 m/s in the weighing environment.
(c) Verify the cleanliness of the PM-stabilization environment using reference filters, as described in § 1065.390(d).
(d) Maintain the following ambient conditions within the two environments during all stabilization and weighing:
(1) Ambient temperature and tolerances. Maintain the weighing environment at a tolerance of (22 ±1) °C. If the two environments share a common space, maintain both environments at a tolerance of (22 ±1) °C. If they are separate, maintain the stabilization environment at a tolerance of (22 ±3) °C.
(2) Dewpoint. Maintain a dewpoint of 9.5 °C in both environments. This dewpoint will control the amount of water associated with sulfuric acid (H2SO4) PM, such that 1.2216 grams of water will be associated with each gram of H2SO4.
(3) Dewpoint tolerances. If the expected fraction of sulfuric acid in PM is unknown, we recommend controlling dewpoint at within ±1 °C tolerance. This would limit any dewpoint-related change in PM to less than ±2%, even for PM that is 50% sulfuric acid. If you know your expected fraction of sulfuric acid in PM, we recommend that you select an appropriate dewpoint tolerance for showing compliance with emission standards using the following table as a guide:
Table 1 of § 1065.190 - Dewpoint Tolerance as a Function of % PM Change and % Sulfuric Acid PM
|Expected sulfuric acid fraction of PM||±0.5% PM mass change||±1% PM mass change||±2% PM mass change|
|5%||±3 °C||±6 °C||±12 °C|
|50%||±0.3 °C||±0.6 °C||±1.2 °C|
|100%||±0.15 °C||±0.3 °C||±0.6 °C|
(e) Verify the following ambient conditions using measurement instruments that meet the specifications in subpart C of this part:
(1) Continuously measure dewpoint and ambient temperature. Use these values to determine if the stabilization and weighing environments have remained within the tolerances specified in paragraph (d) of this section for at least 60 min. before weighing sample media (e.g., filters). We recommend that you use an interlock that automatically prevents the balance from reporting values if either of the environments have not been within the applicable tolerances for the past 60 min.
(2) Continuously measure atmospheric pressure within the weighing environment. An acceptable alternative is to use a barometer that measures atmospheric pressure outside the weighing environment, as long as you can ensure that atmospheric pressure at the balance is always within ±100 Pa of that outside environment during weighing operations. Record atmospheric pressure as you weigh filters, and use these pressure values to perform the buoyancy correction in § 1065.690.
(f) We recommend that you install a balance as follows:
(1) Install the balance on a vibration-isolation platform to isolate it from external noise and vibration.
(2) Shield the balance from convective airflow with a static-dissipating draft shield that is electrically grounded.
(3) Follow the balance manufacturer's specifications for all preventive maintenance.
(4) Operate the balance manually or as part of an automated weighing system.
(g) Minimize static electric charge in the balance environment, as follows:
(1) Electrically ground the balance.
(2) Use 300 series stainless steel tweezers if PM sample media (e.g., filters) must be handled manually.
(3) Ground tweezers with a grounding strap, or provide a grounding strap for the operator such that the grounding strap shares a common ground with the balance. Make sure grounding straps have an appropriate resistor to protect operators from accidental shock.
(4) Provide a static-electricity neutralizer that is electrically grounded in common with the balance to remove static charge from PM sample media (e.g., filters), as follows:
(i) You may use radioactive neutralizers such as a Polonium ( 210Po) source. Replace radioactive sources at the intervals recommended by the neutralizer manufacturer.
(ii) You may use other neutralizers, such as corona-discharge ionizers. If you use a corona-discharge ionizer, we recommend that you monitor it for neutral net charge according to the ionizer manufacturer's recommendations.
(5) We recommend that you use a device to monitor the static charge of PM sample media (e.g., filter) surface.
(6) We recommend that you neutralize PM sample media (e.g., filters) to within ±2.0 V of neutral. Measure static voltages as follows:
(i) Measure static voltage of PM sample media (e.g., filters) according to the electrostatic voltmeter manufacturer's instructions.
(ii) Measure static voltage of PM sample media (e.g., filters) while the media is at least 15 cm away from any grounded surfaces to avoid mirror image charge interference.[70 FR 40516, July 13, 2005, as amended at 73 FR 37299, June 30, 2008; 73 FR 59323, Oct. 8, 2008; 76 FR 57440, Sept. 15, 2011]