86.1312-2007—Filter stabilization and microbalance workstation environmental conditions, microbalance specifications, and particulate matter filter handling and weighing procedures.
(a) Ambient conditions for filter stabilization and weighing—
(1) Temperature and humidity.
The filter stabilization environment shall be maintained at 22 °C ±3 °C and a dewpoint of 9.5 °C ±1 °C. Dewpoint shall be measured with an instrument that exhibits an accuracy of at least ±0.25 °C NIST traceable as stated by the instrument manufacturer. Temperature shall be measured with an instrument that exhibits an accuracy of at least ±0.2 °C or better.
(ii)
The immediate microbalance workstation environment shall be maintained at 22 °C ±1 °C and a dewpoint of 9.5 °C ±1 °C. If the microbalance workstation environment freely circulates with the filter stabilization environment, and this entire environment meets 22 °C ±1 °C and a dewpoint of 9.5 °C ±1 °C , then there is no requirement to measure temperature and dewpoint at the microbalance separate from the filter stabilization location. Otherwise, temperature at the microbalance workstation shall be measured with an instrument that exhibits an accuracy of at least ±0.2 °C or better, and dewpoint shall be measured with an instrument that exhibits an accuracy of at least ±0.25 °C NIST traceable as stated by the instrument manufacturer.
(2) Cleanliness.
(i)
The microbalance and filter stabilization environments shall be free of ambient contaminants (such as dust or other aerosols) that could settle on the particulate filters. It is recommended that these environments be built to conform with the Class 1000 specification (or cleaner) as determined by Federal Standard 209D or 209E for clean room classification (Available from the Institute of Environmental Standards and Technology website at www.iest.org or phone (847) 255-1561). An alternative recommendation would be to equilibrate and/or weigh the filters within a separate, smaller, particle-free, temperature and humidity-controlled chamber (i.e., “glove box”).
(ii)
Reference filters shall be used to monitor for gross particle contamination. It is required that at least two unused reference filters remain in the filter stabilization environment at all times in partially covered glass petri dishes, as in paragraph (c) (1) of this section. These reference filters shall be placed in the filter stabilization environment. The reference filters shall be weighed within 2 hours of, but preferably at the same time as, the sample filters. The reference filters shall be changed at least once a month, but never while any sample filters are between their tare weight (pre-sampling) and gross weight (post-sampling) measurements. The reference filters shall be the same size and material as the sample filters.
(3) Quality control of ambient conditions.
(i)
If, before the start of a weighing session, the temperature or dewpoint of the filter stabilization environment are not within specifications, then filters must remain in the environment for at least 30 minutes after conditions are corrected. If the filter stabilization environment changes during a weighing session such that the specifications are no longer met, the weighing session shall be suspended until the environment has returned to within specifications for at least 30 minutes. Once the environment has returned to within specifications for at least 30 minutes, the reference filters shall be reweighed and the criteria in paragraph (a)(3)(ii) of this section shall apply. Note that temperature and dewpoint shall be sampled once per second, and an unweighted 5-minute moving average of this data shall be calculated once per second. This moving average shall be used to determine the environment temperature and dewpoint for the purpose of determining whether or not the environment is within specifications.
(ii)
If the average change in weight of the reference filters is more than 10 micrograms (after correcting for buoyancy as described in paragraph (c)(3) of this section), then all filters in the process of stabilization shall be discarded and all data collected with respect to the discarded filters shall be considered void. Note that more than 2 reference filters may be used to achieve a more robust average of the change in weight of the reference filters.
(b) Microbalance specifications.
The microbalance used to determine the weights of all filters shall have a precision (standard deviation) of at least ±0.25 micrograms or better for repeated weighing of a calibration weight, a precision of at least ±2.5 micrograms or better for repeated weighing of a clean filter, and a readability equal to or less than 0.1 micrograms. It is recommended that the microbalance be installed on a vibration isolation platform to isolate the microbalance's load cell from external vibration. It is also recommended that the microbalance should be shielded from convective airflow by means of an electrically grounded static dissipative draft shield. Microbalance manufacturer specifications for all preventive maintenance, periodic certification, calibration, and re-zeroing shall be followed. All certification and calibration procedures shall be NIST traceable, or traceable to an equivalent national standard.
(c) Particulate matter filter handling and weighing.
Care should be taken to prevent contamination of the sample filters and to prevent a buildup of static charge on the filters that could interfere with filter weighing. Static neutralizers, such as Po-210 sources, shall be used to neutralize charge on a filter prior to each weighing. A static neutralizer should be replaced at the interval recommended by its manufacturer, or when it is no longer able to reduce static charge on a filter to less than ±2 VDC as measured with an electrostatic monitor at the microbalance workstation. The person weighing filters shall be grounded with respect to the microbalance to prevent imparting a static charge on the filters. This can be accomplished safely by using a grounding strap such as the wrist straps that are commonly used in the microelectronics industry, or by connecting a similar grounding strap to the tweezers. To prevent electrical shock, a 1-megohm resistor should be installed in series between the person weighing filters and ground.
(1)
Within the filter stabilization environment, a pair of clean and electrically conductive tweezers shall be used to place a filter in the lower half of a filter cassette and the cassette shall be placed in a partially open glass petri dish. The petri dish lid should extend over the filter to prevent gross contamination, but it should be left slightly open on one edge to permit stabilization with the environment for at least 30 minutes.
(2)
After at least 30 minutes of stabilization, each filter shall be weighed using the specified microbalance. The process of weighing a filter may be repeated and a statistical mean weight of a single filter may be calculated. Sound engineering judgment shall dictate the use of statistics to discard outliers and the weighting of averages. For a clean filter its single weight or statistical mean weight shall be considered the uncorrected tare weight of the filter.
(3)
All filter weights shall be corrected for filter buoyancy in air. For the uncorrected tare weight of a filter, this calculated value is the corrected tare weight of the filter, and it must be recorded (see § 86.1344(e)(18) ). Barometric pressure of the microbalance environment shall be measured with an instrument that exhibits ±0.01% full-scale accuracy and 0.01% per-year full scale stability, and the full-scale value used for such a specification shall not exceed 200 kPa.
(i)
Buoyancy correction calculation. (A) Calculate vapor pressure of liquid water using the dewpoint temperature in the Magnus formula:
Code of Federal Regulations
Where:
Pw=vapor pressure of liquid water, kPa.
Tdp=dewpoint temperature, °C.
(B)
Calculate air density using the ideal gas relationship and molecular weights of standard air and water:
Code of Federal Regulations
Where:
A=air density, kg/m3.
P=barometric pressure, kPa.
Pw=vapor pressure of liquid water, kPa.
T=temperature, °C.
Code of Federal Regulations
Where:
M=corrected mass in units of the balance display.
R=uncorrected filter weight in units of the balance display.
A=calculated air density, kg/m3.
ρw=density of calibration weight used to calibrate the balance, kg/m3.
ρs=density of filter material used to sample PM emissions, kg/m3.
(ii)
For determining ρs note that PTFE (Teflon TM) and borosilicate glass both have densities in the range of 2,200 to 2,400 kg/m 3. Therefore, for PTFE-coated borosilicate glass fiber filters, an acceptable ρs is 2,300 kg/m 3. Note also that polymethylpentene has a density of 850 kg/m 3. Because Teflon PTFE membrane filters have an integral polymethylpentene support ring that accounts for 95% of the filter mass, an acceptable ρs for these filters is 920 kg/m 3. Other ρs values for other filters may be obtained similarly. Information about “ρs should be available from the calibration weight manufacturer.
(iii)
This paragraph (c)(3)(iii) shows an example of the buoyancy correction. This example assumes the following inputs: Barometric pressure (P)=101.325 kPa, temperature (T)=22.0 °C, dewpoint temperature (Tdp )=9.5 °C, balance display (R)=100.0000 mg, calibration weight density (ρw )=8,000 kg/m 3, and filter material density (ρs )=2,300 kg/m 3. Then:
Code of Federal Regulations
Code of Federal Regulations
M=100.0000 × (1 − (1.191/8000))/(1 − (1.191/2300)) = 100.0369 mg.
(4)
The uncorrected weight, corrected weight, barometric pressure, temperature and humidity, of the filter shall be recorded. Afterward the filter shall be returned to the lower half of the filter cassette, and the upper half of the cassette shall be set in place. The cassette-with filter-shall then be stored in a covered glass petri dish or a sealed (i.e., ends plugged) filter holder assembly, either of which shall remain in the filter stabilization environment until needed for testing. It is recommended that the filter be transported between the filter stabilization environment and the location of the emissions test within a sealed filter holder assembly.
(5)
After the emissions test, the filter cassette shall be removed from the filter holder assembly. If this removal is performed in the filter stabilization environment, the upper half of the cassette shall be removed using a properly designed separator tool, the lower half of the cassette-with filter-shall be placed in a partially covered petri dish, and allowed to stabilize for at least 30 minutes. Otherwise, the cassette and filter shall be placed in a closed petri dish until it can be returned to the filter stabilization environment. Once the closed petri dish is returned to the filter stabilization environment, the petri dish shall be opened, the upper half of the cassette shall be removed using a properly designed separator tool, the lower half of the cassette-with filter-shall be placed in a partially covered petri dish, and allowed to stabilize for at least one hour.
(6)
After at least 30 minutes, but no more than 60 hours of stabilization, each filter may be weighed using the specified microbalance. The process of weighing a filter may be repeated and a statistical mean may be calculated. Sound engineering judgment shall dictate the use of statistics to discard outliers and the weighting of averages. For a used filter, its single weight or statistical mean weight shall be identified as the uncorrected gross weight of the filter. The uncorrected gross weight shall be corrected for filter buoyancy using the procedure in (c)(3) of this section. The uncorrected gross filter weight, corrected gross filter weight, barometric pressure, temperature, and dewpoint shall be recorded.
(7)
The net particulate matter weight (Pf) of each filter shall be equal to the corrected gross filter weight minus the corrected tare filter weight.
(8)
Should the particulate matter on the filters contact the petri dish, tweezers, microbalance or any other surface, the data with respect to that filter is void.