Table of Contents · 2020. 6. 30. · Determination of PM10 Mass by Gravimetric Analysis . 1....

MLD016 Revision 7.0 Approval Date: April 30, 2018

Table of Contents 1. INTRODUCTION ...................................................................................................... 1

2. SUMMARY OF METHOD ......................................................................................... 1

3. ACRONYMS AND DEFINITIONS ............................................................................. 2

4. INTERFERENCES ................................................................................................... 3

5. PERSONNEL QUALIFICATIONS AND TRAINING .................................................. 3

6. SAFETY REQUIREMENTS AND HAZARDOUS WASTE ........................................ 4

7. EQUIPMENT, SUPPLIES, AND CHEMICALS.......................................................... 4

8. PROCEDURES ........................................................................................................ 6

9. QUALITY CONTROL .............................................................................................. 14

10. DATA MANAGEMENT ........................................................................................ 20

11. CALCULATIONS ................................................................................................. 21

12. REVISION HISTORY .......................................................................................... 26

13. REFERENCES .................................................................................................... 28

APPENDIX A ................................................................................................................. 30

1. REJECTION CRITERIA FOR PRE-SAMPLED PM10 FILTERS (UNUSABLE) ...... 30

2. ACCEPTABLE DEFECTS FOR PRE-SAMPLED PM10 FILTERS (USABLE) ........ 31

3. VALIDATION CRITERIA FOR POST-SAMPLED PM10 FILTERS ......................... 32

APPENDIX B ................................................................................................................. 33

1. EXAMPLE U.S. EPA MEMORANDUM (REJECTION CRITERIA) .......................... 33

APPENDIX C ................................................................................................................ 37

1. PROCEDURES TO CALCULATE DAILY BALANCE ROOM CONDITIONS .......... 37

APPENDIX D ................................................................................................................ 40

1. EXAMPLE INITIAL DEMONSTRATION OF CAPABILITY DOCUMENTATION ..... 40

APPENDIX E ................................................................................................................. 42

1. SUMMARY OF ANALYSIS SEQUENCE ................................................................ 42


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Standard Operating Procedure Determination of PM10 Mass by Gravimetric

Analysis 1. INTRODUCTION

This methodology for particulate matter with an aerodynamic diameter less than or equal to a nominal ten micrometers (PM10) is in accordance with Code of Federal Regulations (CFR) Title 40, Chapter 1, Subchapter C, Part 50, Appendix J (40 CFR, Part 50, Appendix J). PM10 concentrations are used for designation of attainment status and maintenance of the National Ambient Air Quality Standard (NAAQS).

PM10 is collected on 8” x 10” high purity quartz microfiber filters (PM10 filters) over a 24 hour period. The sampling of PM10 follows the United States Environmental Protection Agency (U.S. EPA) monitoring schedule. The monitoring schedule is referenced in CFR Title 40, Chapter 1, Part 58, Subpart B.

PM10 mass is determined by gravimetric analysis in an environmentally controlled room. The difference between the pre-weight of a filter and the post weight of the same filter after sampling is used to determine the mass of PM10. PM10 concentrations are calculated in both local and standard conditions using this difference in mass, the measured flowrate, local and standard temperatures and pressures, and duration of PM10 sampling.

2. SUMMARY OF METHOD

Individual quartz microfiber filters are weighed in an environmentally controlled room (i.e. balance room). A National Institute of Standards and Technology (NIST) traceable environmental sensor is used to continuously monitor the temperature and humidity in the balance room.

The balance must be calibrated prior to any pre- or post- sampled weighing. Throughout the weigh session control standards are used to verify the balance is functioning correctly. The balance and weights are both NIST-traceable. PM10 filters are weighed in accordance with quality control protocols. The gravimetric PM10 mass results are converted to aerometric units of micrograms per cubic meter (µg/m3) using volume, duration, and pressure parameters retrieved from the sampler. All data associated with the PM10 filter sample is entered into Northern Laboratory Branch’s (NLB) Laboratory Information Management System (LIMS).


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PM10 mass, quality control data, and documentation detailing pertinent information, is compiled into a data package. Next, the data package is reviewed by the PM10 mass analyst, a second level reviewer (peer reviewer), and finally reviewed and approved by NLB management. PM10 mass data is then submitted to U.S. EPA’s Air Quality System (AQS) database.

PM10 filters are archived for at least five years plus the current year in compliance with U.S. EPA guidelines.

3. ACRONYMS AND DEFINITIONS

g Grams °C Degrees Celsius mg Milligram mm Hg Millimeters mercury µm Micrometer µg Microgram µg/m3 Microgram per cubic meter AQS Air Quality System AQSB Air Quality Surveillance Branch CARB California Air Resources Board ASTM American Society for Testing and Materials CFR Code of Federal Regulations COC Chain of custody IDOC Initial demonstration of capability ILS Inorganic Laboratory Section LCD Liquid crystal display LIMS Laboratory Information Management System: Database containing

sample metadata, raw and reported concentration results, and quality control samples and results.

LIMSLink Software allowing review of raw sample data and quality control results, and transfer of data electronically retrieved from the analytical balance to LIMS.

LIMS Reports

Software allows the analyst to generate data reports (i.e. summary reports, monthly data reports) for review and eventually approval by NLB management.

MFC Mass flow controller MLD Monitoring and Laboratory Division MRS Mass reference standard NAAQS National Ambient Air Quality Standard NIST National Institute of Standards and Technology NLB Northern Laboratory Branch PM10 Particulate matter with an aerodynamic diameter less than or equal to a

nominal ten micrometers


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QA Quality assurance QC Quality control SOP Standard operating procedure TSA Technical system audit U.S. EPA United States Environmental Protection Agency VFC Volumetric flow controller

4. INTERFERENCES

Powder free and anti-static gloves must be worn at all times to prevent contamination from body moisture and oils.

Static electricity can build up on the quartz filters causing erroneous mass results or failure of the balance to stabilize. Antistatic devices, such as polonium antistatic strips, are kept in the balance weighing chamber to dissipate static charge. These devices must be replaced annually in order to maximize effectiveness.

The moisture content of a filter affects its weight. Filters are equilibrated in a temperature and humidity controlled conditioning environment for at least 24 hours prior to any pre- and post-weighing session.

Airborne particulates from dust contamination can lead to inaccurate mass measurements. Dust contamination can be reduced by maintaining clean laboratory benchtops, tidy weighing areas, and application of an adhesive entryway mat.

An anti-vibration table must be used because an unstable surface will adversely affect mass measurements.

Air conditioning ductwork, printers, and frequently opened doorways may create undue air flow. This air flow can adversely affect mass measurements. Appropriate placement of the balance, use of a double door entryway, and not weighing when the fan is blowing can minimize airflow on the instrument.

5. PERSONNEL QUALIFICATIONS AND TRAINING

Prior to performing this method, new personnel must be trained by experienced staff. Personnel must be trained to understand the program’s requirements per any applicable State and federal regulations and guidance, and this SOP. Personnel will also be trained on how to safely and properly operate the equipment needed to perform the


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method, the quality assurance components, and LIMS functionality pertaining to the program.

Personnel should provide an initial demonstration of capability (IDOC) prior to performing this method on real-world samples (i.e. data for record). For additional details, please see Appendix D.

Training will be documented and maintained by the laboratory supervisor.

6. SAFETY REQUIREMENTS AND HAZARDOUS WASTE

All personnel must follow the general health and safety requirements found in NLB’s Chemical Hygiene Plan. Radioactive (alpha particle) Polonium-210 antistatic strips for static charge neutralization are used in the laboratory. Polonium strips release low levels of gamma radiation, therefore tools must be used to indirectly handle polonium strips.

7. EQUIPMENT, SUPPLIES, AND CHEMICALS

Equipment and supplies necessary to meet requirements for PM10 mass analysis are described below.

Environmentally controlled balance room. Specifications are described in Section 9.1.

Two relative humidity/temperature recorders and probes must be placed in the balance room. One recorder is designated as the “primary” and the additional recorder is used as a “secondary” recorder. All recorders must be calibrated and certified annually as NIST traceable, by an outside source. Minimal performance specifications: 20-50% RH, 18-25 degrees Celsius, readable to the nearest 0.5% RH and 0.1 degree Celsius, accurate to within 2% RH and 2 degrees Celsius, and at least a five minute logging interval.

LIMS, LIMSLink, and LIMS reports.

Analytical balance equipped with a balance pan in a glass enclosure. Balance must have a minimum resolution of 0.1 mg and minimum precision of 0.5 mg. Electronic data transfer interfaces with the LIMS database system.

Anti-vibration balance support table.


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Filter weighing rack that’s sized to fit on the balance pan and can hold 8” x 10” filter media. The entire assembly with the filter media should fit on the weighing rack when the balance is closed.

Three 1.0000 g weights categorized by American Society for Testing and Materials (ASTM) as Class 1, non-corroding, and certified as NIST-traceable. Each weight must have an individual serial or identification number.

Three 3.0000 g weights categorized by American Society for Testing and Materials (ASTM) as Class 1, non-corroding, and certified as NIST-traceable. Each weight has a certification document with serial number identification.

Three 5.0000 g weights categorized by American Society for Testing and Materials (ASTM) as Class 1, non-corroding, and certified as NIST-traceable. Each weight has a certification document with serial number identification.

8” x 10” high purity quartz microfiber filters. Filters are supplied annually by U.S. EPA along with a memorandum that provides additional information regarding visual inspections for that specific lot of filters (see Appendix B for an example memorandum). Since the filter acceptance criteria set forth in this memorandum can potentially change for a new lot of filters sent from U.S. EPA, analysts should review and apply any new criteria found in this memorandum in addition to the criteria set forth in Appendix A of this SOP when inspecting filters.

Light board.

Radioactive (alpha particle) Polonium-210 antistatic strips for static charge neutralization. Two strips are needed for each balance.

Antistatic brush.

Non-metallic, plastic, or Teflon tipped forceps.

Timer.

Antistatic and powder free gloves.

PM10 sample chain of custody (COC) forms.

Self-adhesive labels


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U.S. EPA-issued monitoring sampling schedule.

Mail out supplies to include: Manila folders (8 ½” x 11”) Glassine envelopes (8 ¼” x 10 ¼”) Clasp envelopes (10” x 13”).

Adhesive entryway mat or sticky mat.

Utility wipes.

8. PROCEDURES

Pre-Sampled Filter Inspection

U.S. EPA provides the quartz microfiber filters used for PM10 sampling, and each filter has a factory stamped serial number (filter number) that begins with the letter “Q” (for quartz). Staff must carefully inspect filters using criteria set forth in Appendix A of this SOP. Staff should also review the memorandum that accompanied the lot of filters sent from U.S. EPA (example in Appendix B of this SOP) for any potential new inspection criteria for that specific set of filters. Following are the steps to perform filter inspections:

8.1.1. Clean powder free and antistatic gloves must be worn when handling PM10 filters.

8.1.2 Clean the light board and the surrounding inspection area with a disposable laboratory wipe moistened with Nanopure water. Afterwards use a dry wipe to make sure the area is clean and dry.

8.1.3 Place pre-sampled quartz microfiber filter flat on the light board, inspecting both sides for any defects.

8.1.4 Review memorandum that accompanied the lot of filters for any potential changes to filter inspection criteria. Note any criteria changes that deviate from the SOP in the laboratory notebook.

8.1.5 Place the acceptable pre-inspected filter into a manila folder, followed by a glassine enclosure, and a chain of custody form. The chain of custody form differs depending on the type of sampler used by the receiving site. Therefore, the analyst must determine and add the correct forms for each mail out site. These forms vary


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for mass flow controller (MFC), volumetric flow controller (VFC), and Ecotech samplers.

Next, group pre-inspected filters in a set. A set consists of one quarter’s worth of filters for a site. Based on U.S. EPA’s one in six sampling frequency, sets include seventeen filters per quarter for each site. This includes filters for up to fifteen sampling days and two filters for field blanks or make-ups.

Finally, position the sets of pre-inspected filters in an environmentally controlled balance room. Place the manila folders with the open edge facing up so that filter equilibration can occur more readily. Again, filters must equilibrate for at least 24 hours prior to pre-weighing.

Prior to weighing pre-sampled filters, check the temperature and relative humidity sensors to ensure that the environmental conditions of balance room are met. See Section 9.1 for the specifications. Detailed instructions for calculating the balance room conditions are found in the PM10 program procedures binder located in the balance room.

Calibration of Analytical Balance

After the balance room’s environmental conditions have been calculated and shown to be within requirements (refer to section 9.1), the analytical balance must be calibrated before weighing. Both the internal and external calibrations must be performed prior to the first weighing session for each day. All weighing must be performed with the glass enclosure door of the balance chamber closed to minimize airflow. There should be two antistatic strips located inside the balance chamber to dissipate static charge. Analyst must also wear powder free and antistatic gloves when handling weights, forceps, and filter media.

Clean laboratory surfaces around the balance with a laboratory wipe. Next, use an antistatic brush to clean the weighing rack and inside the weighing chamber.

Clean the forceps used for handling the weights with a laboratory wipe.

The analytical balance must be level prior to weighing. If the level located on the balance is off center, refer to the manufacturer’s manual for directions on how to relevel the balance.


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Internal calibration: This calibration is performed with the filter weighing rack off the weighing pan.

8.5.4.1 Press the “Internal Calibration” key on the balance liquid crystal display (LCD). LCD should display “OK” when the balance has finished the internal calibration. Press the “OK” button, now the internal calibration is complete.

8.5.5 External calibration is performed with the filter weighing rack on the weighing pan.

8.5.5.1 Create a worklist that includes the calibration sample to be weighed. Retrieve the temperature and relative humidity of the balance room and record the values in the worksheet. For additional details reference Appendix E.

8.5.5.2 Tare the balance with the weighing rack on the balance pan. Wait for display to read 0.0000 g.

8.5.5.3 Carefully place the 1.0000 g and 3.0000 g working weights onto the filter weighing rack. Reference section 9.3 for detailed working weight information. Close the balance enclosure door and wait until the display stabilizes.

8.5.5.4 The mass must be 4.0000 ± 0.0005 g. If the mass falls outside of this range you will need to recalibrate both internally and externally the balance. If after re-calibration the balance is still outside of this range no weighing may occur. Consult with management to determine corrective actions which may include, but are not limited to: reevaluating the balance level and/or stability, contacting the vendor to recalibrate the balance, verifying that the static strips are up-to-date, reweighing the following day, etc.

8.5.5.5 Finally, the data generated from this calibration must be peer reviewed along with all weighing that occurs in a session to ensure validity.

8.5.5.6 Electronically transfer the external calibration mass, temperature, and relative humidity values to LIMS.


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8.6 Pre-Weighing of Filters

Verify the temperature and relative humidity criteria of the balance room meets the requirements set forth in Section 9.1. Verification is documented, peer reviewed, and stored with weighing summaries.

Quartz microfiber filters should have a mass between 3.7 g to 4.7 g. Any quartz fiber filter pre-weighing outside this acceptable range will be rejected and removed from the set of useable PM10 filters.

Pre-weigh and prepare enough filters to cover three months (one quarter), sampling period for a network mail out.

Clean the balance, forceps, and weighing area before any filter weighing.

Perform all weighing with the glass enclosure door closed.

8.6.1 Complete an internal and external calibration prior to any weighing. See Sections 8.5.4. and 8.5.5. for instructions.

8.6.2 Create a pre-weigh worklist that contains the samples to be weighed and associated quality control. Enter the numerical portion of the filter number (omitting the letter ‘Q’). Typically, filters will be in numerical order. For additional details reference Appendix E.

8.6.3 Although quality controls are automatically inserted into both pre-weight & post-weight worklists, make sure the following are accurate:

8.6.3.1 Control standards are weighed by placing them on the filter weighing rack at the beginning and end of a weigh session using working weights. The lower control mass value is 3.0000 g and the upper control mass value is 5.0000 g. In addition to the control standards at the beginning and end of the weigh session, the lower and upper control standards are also alternately weighed after duplicates. If a control standard mass is out of range by more than ±0.0005 g from the target mass, re-weigh the control, duplicates, and alternating standards and all samples weighed since the last valid control. If the control is still out of range the weigh session is not valid. Restart the weigh session. If the control is again out


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of range, consult with management for further instruction and document the incident in the lab notebook and on the COC. For additional details see section 9.4.

8.6.3.2 Duplicates are performed after every ninth filter. The duplicate mass rate must be greater than or equal to ten percent (> 10%). If the original and duplicate mass values differ by more than ±0.0028 g, re-weigh the filter. If the difference is still not within ±0.0028 g the weigh session is not valid. Restart the entire weigh session. If the control is again out of range, consult with management for further instruction and document the incident in the lab notebook and on the COC. For additional details see section 9.6.

8.6.4 Wear powder free and antistatic gloves when handling weights, components, and filter media.

8.6.5 Use non-metallic forceps to place control standard on the balance rack.

8.6.6 Wait until the mass reading has stabilized on the balance for a minimum of 4 seconds in accordance with the analytical balance operating instructions. Once stabilized, submit the value to the pre-weigh worklist.

8.6.7 Repeat steps 8.6.3 through 8.6.6 as needed to complete the set.

8.6.8 Weighing a quartz microfiber filter

8.6.8.1 Place filter weighing rack (holds the PM10 filter) on the balance pan. Tare the balance with the filter weighing rack before weighing any filter. Close the weighing chamber door when weighing.

8.6.8.2 Place a PM10 filter on the filter weighing rack.

8.6.8.3 Ensure mass is stabilized before submitting the filter weight to the worklist. If the weight value on the


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balance does not fluctuate for 4 seconds, the mass is stable.

8.6.8.4 Record the filter’s identification number, pre-weight

date, analyst’s initials, and the pre-weight mass on the COC. Transcribe only the numerical identification number and omit the letter (Q) at the beginning.

8.6.8.5 Place the pre-weighed filter back into the manila

folder along with the glassine enclosure, and the corresponding COC.

8.6.8.6 Repeat steps 8.6.8 through 8.6.8.5 for subsequent

PM10 filters, and all appropriate QC.

8.6.8.7 End weighing session by weighing the lower and upper control standards.

8.6.9 Analyst will review all data transferred to the LIMSLink worklist for

accuracy prior to transferring data to LIMS.

8.6.10 Next, print a pre-weight summary report from LIMS for peer review. Review the report and COC then transfer to the peer reviewer for their review. Both reviewers must initial and date the report. If any changes are made to the data after it has been transferred to LIMS they must be documented, initialed, and dated on the summary report and corresponding COC. Changes must also be documented in the lab notebook.

8.6.11 Once peer review is complete file the reports in the appropriate

binders.

8.7 Post-Sampled Filter Inspection

Check the physical appearance of the post-sampled filter to ensure there is no contamination or filter damage which could invalidate the filter.

PM10 filter acceptance and rejection criteria are detailed in Appendix A, Section 3, of this SOP.


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8.7.1. Clean powder free antistatic gloves must be worn when inspecting PM10 filters.

8.7.2. The PM10 filter is received in the lab folded in half inside a glassine envelope. Sampled side will be inside the folded PM10 filter. Carefully remove filter from the glassine envelope and unfold the PM10 filter in the manila folder. If the filter is received outside of the glassine envelope, the sample is invalid.

8.7.3. Visually inspect the post-sampled filter for damage, contamination, or other physical defects.

8.7.4. If invalidated, the reason should be documented in the “Comments” section of the COC form at the time of discovery.

8.7.5. Use a red pen to write an asterisk (*) on the tab of the manila folder to indicate the sample is invalid.

8.7.6. Return the inspected sample to its manila folder with the sampled side folded inward.

8.7.7. Place sample folders in an environmentally controlled balance room to equilibrate with the conditions referenced in section 9.1 of this SOP. Note the date and time filter conditioning begins to ensure equilibration time is met. All samples that are not known to be invalid are weighed.

8.8 Post-Weighing of Filters

Verify the temperature and relative humidity of the balance room is in accordance with section 9.1 of this SOP before starting a weighing session. PM10 filter samples must be post-conditioned in the environmentally controlled balance room for at least 24 hours prior to weighing. The balance, forceps, and weighing area must be clean before any filter weighing. All weighing must be performed with the glass enclosure door closed.

8.8.1. Internal and external calibrations, as described in sections 8.5.4 and 8.5.5, must be completed prior to any weighing.

8.8.2. Generate a post-weight worklist. Make sure the samples to be weighed match the worklist. Reference Appendix E. for an example sequence.


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8.8.3. Although quality controls are automatically inserted, by LIMSLink, ensure the following conditions are met by reviewing the LIMS worklist:

8.8.3.1. Control standards are weighed at the beginning and end of a weigh session using working weights. The lower control mass value is 3.0000 g and the upper control mass value is 5.0000 g. These lower and upper control standards are also alternately weighed after duplicates. If a control standard mass is out of range by more than ±0.0005 g from the target mass, re-weigh the control, QC, and all samples weighed since the last valid control. If the control is still out of range the weigh session is not valid. Restart the weigh session. If the control is again out of range, consult with management for further instruction and document the incident in the lab notebook and on the COC. See section 9.4 for additional details.

8.8.3.2. Duplicates are performed after every ninth filter. The duplicate mass rate must be greater than or equal to ten percent (> 10 %). If the original and duplicate mass values differ by more than ±0.0050 g, re-weigh the filter. If the difference is still not within ±0.0050 g the weigh session is not valid. Restart the weigh session. If the control is again out of range, consult with management for further instruction and document the incident in the lab notebook and on the COC. See section 9.6 for additional details.

8.8.3.3. A make-up sample must be collected prior to the next scheduled sampling day. Reference AQSB SOP 408 for more information.

8.8.4. Confirm PM10 samples to be weighed match the PM10 post-weight worklist.

8.8.5. Wear powder free antistatic gloves when handling weights, forceps, and filter media.

8.8.6. Tare the balance with the filter weighing rack on the balance pan.


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8.8.7. Weigh in accordance with the worklist. The first items after calibrating should be the control weights. These can be placed directly on the weighing pan.

8.8.8. Verify the identification of the sample to be weighed.

8.8.8.1. Filter number on the sample media should match the COC form. If these numbers do not match the sample is invalid.

8.8.8.2. Sample barcode should correspond with the COC form and worklist.

8.8.9. Place the folded PM10 filter on the weighing rack.

8.8.10. Wait for the mass to stabilize on the balance before transferring the weight to the LIMSLink worklist. See section 8.6.6 for additional details.

8.8.11. Record the post-weight transferred from the balance to the worklist onto the COC. Initial and date.

8.8.12. Return the post-weighed PM10 filter to its respective manila envelope.

8.8.13. Repeat sections 8.8.9 through 8.8.12 for all subsequent filters and QC.

8.8.14. After all PM10 filters are weighed, the lower (3.0000 g) and upper control standard (5.0000 g) are weighed.

8.8.15. Review the post-weight for accuracy by ensuring values noted on the COC match those transferred to LIMS.

8.8.16. Transfer worklist of PM10 post-weight data to LIMS.

8.8.17. Generate a LIMS PM10 post-weight summary report. Confirm PM10 data and QC have been completed and are within criteria. Initial and date the summary report if QC for calibration, duplicates, and checks are within limits.

9. QUALITY CONTROL

9.1 Environmental Room Criteria for PM10 Filter Conditioning and Weighing:


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Criteria Action if criteria is not met

Temperature: The balance room mean temperature must be between 15°C to 30°C for the previous 24 hours. The previous 24 hour standard deviation must also not exceed ±3°C. See Appendix C for procedures to calculate the balance room’s environmental conditions. ARB laboratory uses more stringent environmental conditions than those required by 40 CFR Part 50, Appendix J.

No weighing may occur. If the criteria begins to drift out during a weighing session, stop weighing filters and weigh the last two standards. Transfer the data to LIMS. Weigh remaining filters when the room conditions are back in range for at least 24 hours.

Relative Humidity (RH): The balance room mean RH must fall within 30% to 40% for the previous 24 hours. The previous 24 hour standard deviation must also not exceed ±5% RH. See Appendix C for procedures to calculate the balance room’s environmental conditions. ARB laboratory uses more stringent environmental conditions than those required by 40 CFR Part 50, Appendix J.

No weighing may occur. If the criteria begins to drift out during a weighing session, stop weighing filters and weigh the last two standards. Transfer the data to LIMS. Weigh remaining filters when the room conditions are back in range for at least 24 hours.

9.2 Temperature and Relative Humidity Sensors

There are two temperature and relative humidity sensors for the Balance Room. Both sensors are annually certified as NIST-traceable. One sensor is labelled as the primary sensor and the other as the secondary sensor. The primary sensor is the reference sensor and the secondary sensor is the working sensor. Documentation and NIST-traceability of both sensors is kept with


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the equipment. The two sensors are compared against each other on a quarterly basis. These records are peer and manager reviewed, stored in the laboratory binder, and hard copies are submitted with data packages.

9.2.1. Quarterly Checks of Temperature and Relative Humidity

9.3 Mass Reference Standards (MRS) should be ASTM Class 1 category, non-corroding, and NIST-traceable. Documentation of NIST-traceability must be kept in balance room where the weights reside. Three sets of weights are needed. One set of primary weights and two sets of workings weights. Three sets allow the balance room to function while the working set of weights is sent

Criteria Action if criteria is not met

Every 2 minutes, record the temperature and the relative humidity (RH) from the primary sensor and the secondary sensor, for a total of 10 readings of temperature and 10 readings of RH on each sensor. Take the average of these readings for each sensor. Compare the average from the primary sensor to the average from the secondary sensor by taking the difference between the two. The formula to compare these sensors is (Average difference = secondary sensor – primary sensor) The average temperature difference between the sensors must be within ± 2°C. The relative humidity difference must be within ± 2%.

If the temperature and relative humidity do not meet these criteria, re-perform the check. If the problem persists, consult with management and contact the balance room maintenance contractor or the sensor manufacturer. A third sensor from ARB’s Quality Assurance Section can be used to help troubleshoot the issue. No weighing may occur if the sensors do not fall within the criteria.


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out for certification. The weights used and certified for PM10 mass procedures have a target value of 1.0000 g, 3.0000 g, and 5.0000g.

9.3.1 The lab uses three sets of weights. A primary MRS set and two sets of working weights. The primary MRS and one working weight set are annually sent out to be recertified by an outside source. The secondary set of working weights remain in the balance room. The secondary working set of weights is also sent out annually for certification. This certification is performed after the initial primary and working set of weights return from certification. The outside certification source must provide a NIST certificate for each certified MRS.

9.3.2 Working weights are used for external calibration of the balances, (See section 8.5). Working weights are also used during each weighing session as controls and CCV.

9.4. Control Standards

9.4.1. Two control standards (3.0000 g and a 5.0000 g), are placed at the beginning and the end of a weighing sequence. In addition, after each duplicate sample, the 3.0000 g and 5.0000 g control standards are alternately weighed.

9.5 Analytical Balance Calibrations

9.5.1 The analytical balance must be calibrated daily, quarterly, and annually following the criteria in the table below.

Criteria Action if criteria is not met A control standard must be less than ± 0.0005 g from its certified mass.

If a control standard mass is out of range by more than ± 0.0005 g from its certified mass, re-weigh the control, QC, and all samples weighed since the last valid control. If the control is still out of range, the weigh session is not valid. Restart the weigh session. If the control is again out of range, alert management and contact the manufacturer to adjust or replace the faulty weight.


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Criteria Action if criteria is not met Daily Calibration: The balance must be calibrated once a day and prior to all weighing sessions. A calibration is performed by following the procedures in section 8.5. The calibration combines the 1.0000 g and 3.0000 g MRS for a total mass of 4.0000 g. A calibration check verification of 3.0000 g and a 5.0000 g is also alternated during a weighing session. The calibration limit is ± 0.0005 g.

If the weights are out of range, reweigh the weight. If rechecked weights are not valid, no weighing may occur until the error is corrected. Alert management and contact the manufacturer to adjust or replace the faulty weight.

Quarterly Calibration: Primary and working weights are weighed five times. The determined mass of the weights is then compared to the NIST traceable verified mass. If the difference between the expected mass, (verified mass), of the weights exceeds ± 0.0005 g they are not valid. Difference from expected mass for each weight = observed mass – expected mass.

If the weights are out of range, reweigh the weight. If rechecked weights are not valid, no weighing may occur until the error is corrected. Alert management and contact the manufacturer to adjust or replace the faulty weight.

Annual Calibration: Balance must be calibrated and certified annually by an outside source. The calibration must be traceable to NIST.

If the balance is determined to be out of calibration, it must be recalibrated according to the manufacturer’s instructions and recertified by an outside source.


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9.6 . Duplicates

9.6.1 Duplicates must be weighed with every set of filters. The duplicate mass rate must be greater than or equal to ten percent (>10 %). Typically a duplicate sample will be weighed on the ninth sample position. However, if a set comprises of nine or less PM10 samples, a duplicate must still be weighed.

Criteria Action if criteria is not met For pre-weights the original and duplicate mass values must not differ by more than ± 0.0028 g.

If the difference is not within ± 0.0028 g, the weighing session is not valid. Restart the weigh session If the duplicate is out again, alert management and contact the manufacturer.

For post-weights the original and duplicate mass values must not differ by more than ± 0.0050 g.

If the difference is not within ± 0.0050 g, the weighing session is not valid. Restart the weigh session If the duplicate is out again, alert management and contact the manufacturer.

9.7. Field Blanks

9.7.1. Field blanks are unexposed quartz filters that are placed on a PM10 sample with no air flow passing through the filter.

Criteria Action if criteria is not met The difference between the pre- and post- weight should be within ± 5mg.

Notify the site manager, site operator, and laboratory manager if the field blank concentration is outside ± 5 µg/m3. Document this difference on the COC. No actionable criteria for samples exceeding these limits.


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10. DATA MANAGEMENT

Data management involves PM10 samples logged into LIMS, transfer and review of PM10 pre- and post- weight data to LIMS, documentation of unusual occurrences and their resolutions, creation of data packages (monthly, amendments, and special projects) for peer review and management approval, storage of balance room conditions to the shared drive, and archiving of PM10 filters and their COCs. Program and maintenance logbooks are to be kept with the instrumentation at all times

10.1 After PM10 samples are weighed and transferred to LIMS they must be peer reviewed to ensure accuracy. The peer reviewer must check the daily calibration to ensure it was performed, the PM10 post/pre weight to LIMS to make sure all records show “complete” under LIMS status, and PM10 post/pre weight summaries to certify all weighed mass values match those on the COC.

10.2 Finally, PM10 sample data packages undergo a multi-level data validation process. This process includes analyst review, peer review, and laboratory management review and approval in line with NLB’s Laboratory Quality Control Manual. Data packages created by analyst must consist of the following:

10.2.1. Documentation of the method and program name, description of standards (re-certification and expiration dates), identifiers of standards used (i.e. serial number), criteria limits, and comments for special projects.

10.2.2. Summary of the data generated for a sample date period. This includes precision (comparison of collocated sites) and blank data.

10.2.3. Summary of QC data, calibration checks, and any additional QC documentation connected to the data of interest.

10.2.4. Documentation of any unusual occurrences and how they were resolved. This includes lab action emails to site operators, analyst notes, as well as a record of involvement by management.

10.3. All PM10 mass exceedances of the National Ambient Air Quality Standard (NAAQS) should be reported to laboratory management. PM10 Mass data clients should be notified by management if a PM10 Mass result


Page 21 of 42

exceeds the NAAQS standard. This information should also be documented in the data package.

10.4. PM10 Mass data must be approved by laboratory management before release to the client.

10.5. A continuous digital data recorder (Secondary sensor) is used to document and store environmental conditions of the balance room.

10.6. PM10 filter samples, their respective COC forms, and any program related reports are archived for five years plus the current year according to our records retention policy. Samples and reports that exceed this time period are no longer required to be stored by the laboratory.

10.7. Laboratory management must approve destruction of any archival data older than five years plus the current year.

11. CALCULATIONS

11.1 PM10 Mass Calculations:

PM10 mass data reported to the Federal database (i.e. AQS) must be reported at standard conditions in standard cubic feet per minute (SCFM.) SCFM is the flowrate referenced to a temperature of 25°C and a pressure of 760 millimeter mercury (mm Hg.) This is considered standard temperature and pressure (STP.) PM10 mass data is also reported in local conditions in actual cubic feet per minute (CFM.) Local temperature and pressure (LTP) conditions are used to determine PM10 mass data in local conditions.

Volumetric flow control (VFC) samplers calculate the average flow rate over the sampling period corrected to U.S. EPA reference conditions as Qstd. However, mass flow control (MFC) samplers do not require Qstd calculations. When the sampler’s flow indicator is calibrated in actual volumetric units (Qa), Qstd is calculated as:

Equation 1:

𝑄𝑄𝑠𝑠𝑠𝑠𝑠𝑠 = 𝑄𝑄𝑎𝑎 �𝑃𝑃𝑎𝑎𝑎𝑎𝑇𝑇𝑎𝑎𝑎𝑎

� �𝑇𝑇𝑠𝑠𝑠𝑠𝑠𝑠𝑃𝑃𝑠𝑠𝑠𝑠𝑠𝑠

�


Page 22 of 42

Equation 2:

𝑄𝑄𝑎𝑎 = �45.379 �𝑃𝑃𝑜𝑜𝑃𝑃𝑎𝑎𝑎𝑎

� − 2.243� + [(𝑇𝑇𝑎𝑎𝑎𝑎 − 25)(0.059)]

Where,

Qstd = average flow rate at U.S. EPA reference conditions, std m3/min;

Qa = average flow rate at ambient conditions, local m3/min;

Pav = average barometric pressure during the sampling period or average barometric pressure for the sampling site, kPa (or mm Hg);

Tav = average ambient temperature during the sampling period or seasonal average ambient temperature for the sampling site, Kelvin (K);

Tstd = standard temperature, defined as 298 K;

Pstd = standard pressure, defined as 101.3 kiloPascal (kPa) (or 760 mm Hg);

𝑃𝑃𝑜𝑜𝑃𝑃𝑎𝑎𝑎𝑎

= pressure ratio, �1 − 𝑃𝑃𝑓𝑓𝑃𝑃𝑎𝑎𝑎𝑎�;

Pf = differential pressure across filter (mm Hg);

Qa equation is referenced from SOP 408 of Air Quality Surveillance Branch for local conditions.

Calculate the total volume of air in both standard and local conditions sampled as:

Equation 3:

𝑉𝑉𝑠𝑠𝑠𝑠𝑠𝑠 = 𝑄𝑄𝑠𝑠𝑠𝑠𝑠𝑠(𝑡𝑡)

Equation 4:

𝑉𝑉𝑎𝑎 = 𝑄𝑄𝑎𝑎(𝑡𝑡)

Where,

Vstd = total air sampled in standard volume units, std m3;

Va = total air sampled in ambient conditions volume units, local m3


Page 23 of 42

t = sampling time, minutes.

Calculate the PM10 concentration in both standard and local conditions as:

Equation 5:

𝑃𝑃𝑃𝑃10 𝑠𝑠𝑠𝑠𝑠𝑠 = ��𝑊𝑊𝑓𝑓 −𝑊𝑊𝑖𝑖�(106)

𝑉𝑉𝑠𝑠𝑠𝑠𝑠𝑠�

Equation 6:

𝑃𝑃𝑃𝑃10 𝑎𝑎 = ��𝑊𝑊𝑓𝑓 −𝑊𝑊𝑖𝑖�(106)

𝑉𝑉𝑎𝑎�

Where,

PM10 std = mass concentration of PM10, µg/std m3;

PM10 a = mass concentration of PM10, µg/local m3;

Wf = final weight of filter collecting PM10 particles, g;

Wi = initial weight of filter collecting PM10 particles, g.

11.2 Balance Room Environmental Conditions Calculations. For detailed instructions to determine the environmental conditions, refer to Appendix C.

11.2.1. Temperature

The balance room mean temperature must be between 15°C to 30°C for the previous 24 hours. The previous 24 hour standard deviation must also not exceed ±3°C.

Equation 7:

𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴 = 1𝑛𝑛�𝐴𝐴𝑖𝑖 =

1𝑛𝑛

(𝐴𝐴1 + 𝐴𝐴2 … 𝐴𝐴𝑛𝑛)𝑛𝑛

𝑖𝑖=1

Where,

n = sample size,

𝐴𝐴𝑖𝑖 = Individual observed values,


Page 24 of 42

Equation 8:

𝑆𝑆𝑡𝑡𝐴𝐴𝑛𝑛𝑆𝑆𝐴𝐴𝐴𝐴𝑆𝑆 𝐷𝐷𝐴𝐴𝐴𝐴𝐷𝐷𝐴𝐴𝑡𝑡𝐷𝐷𝐷𝐷𝑛𝑛 = �1

𝑛𝑛 − 1�(𝑥𝑥𝑖𝑖 − �̅�𝑥)2𝑛𝑛

𝑖𝑖=1

Where,

n = sample size,

𝑥𝑥𝑖𝑖 = observed values,

�̅�𝑥 = mean value of observations,

11.2.2. Relative Humidity

The balance room mean relative humidity must fall within 30% to 40% for the previous 24 hours. The previous 24 hour standard deviation must also not exceed ±5% relative humidity.

Equation 9:

𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴 = 1𝑛𝑛�𝐴𝐴𝑖𝑖 =

1𝑛𝑛

(𝐴𝐴1 + 𝐴𝐴2 … 𝐴𝐴𝑛𝑛)𝑛𝑛

𝑖𝑖=1

Where,

n = sample size,

𝐴𝐴𝑖𝑖 = Individual observed values,

Equation 10:

𝑆𝑆𝑡𝑡𝐴𝐴𝑛𝑛𝑆𝑆𝐴𝐴𝐴𝐴𝑆𝑆 𝐷𝐷𝐴𝐴𝐴𝐴𝐷𝐷𝐴𝐴𝑡𝑡𝐷𝐷𝐷𝐷𝑛𝑛 = �1

𝑛𝑛 − 1�(𝑥𝑥𝑖𝑖 − �̅�𝑥)2𝑛𝑛

𝑖𝑖=1

Where,

n = sample size,


Page 25 of 42

𝑥𝑥𝑖𝑖 = observed values,

�̅�𝑥 = mean value of observations,

11.3 Quarterly Calibration Calculations:

11.3.1. Temperature

The temperature readings from both primary sensor and secondary sensor are compared to each other 10 times using an interval of 2 minutes between each parameter. The formula to compare these sensors is:

Equation 11:

𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴 𝐷𝐷𝐷𝐷𝐷𝐷𝐴𝐴𝐴𝐴𝐴𝐴𝑛𝑛𝐷𝐷𝐴𝐴 = (1𝑛𝑛�𝑆𝑆𝑆𝑆𝑖𝑖 =

1𝑛𝑛

(𝐴𝐴1 + 𝐴𝐴2 … 𝐴𝐴𝑛𝑛)) − ( 1𝑛𝑛�𝑃𝑃𝑆𝑆𝑖𝑖 =

1𝑛𝑛

(𝐴𝐴1 + 𝐴𝐴2 … 𝐴𝐴𝑛𝑛))𝑛𝑛

𝑖𝑖=1

𝑛𝑛

𝑖𝑖=1

Where,

n = sample size,

𝑆𝑆𝑆𝑆𝑖𝑖 = secondary sensor temperature observed values,

𝑃𝑃𝑆𝑆𝑖𝑖 = secondary sensor temperature observed values,

11.3.2. Relative Humidity

The relative humidity readings from both the primary sensor and secondary sensor are compared to each other 10 times using an interval of 2 minutes between each parameter. The formula to compare these sensors is:

Equation 12:

𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴 𝐷𝐷𝐷𝐷𝐷𝐷𝐴𝐴𝐴𝐴𝐴𝐴𝑛𝑛𝐷𝐷𝐴𝐴 = (1𝑛𝑛�𝑆𝑆𝑆𝑆𝑆𝑆𝑖𝑖 =

1𝑛𝑛

(𝐴𝐴1 + 𝐴𝐴2 … 𝐴𝐴𝑛𝑛)) − ( 1𝑛𝑛�𝑃𝑃𝑆𝑆𝑆𝑆𝑖𝑖 =

1𝑛𝑛

(𝐴𝐴1 + 𝐴𝐴2 … 𝐴𝐴𝑛𝑛))𝑛𝑛

𝑖𝑖=1

𝑛𝑛

𝑖𝑖=1

Where,

n = sample size,


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𝑆𝑆𝑆𝑆𝑆𝑆𝑖𝑖 = secondary sensor temperature observed values,

𝑃𝑃𝑆𝑆𝑆𝑆𝑖𝑖 = secondary sensor temperature observed values,

12. REVISION HISTORY

The changes from Revision 6.0 to Revision 7.0 are documented in table below:

Date Updated Revision Original Procedure 1 Description: Environmental conditions February 29, 2012 Filter conditioning environment now

reflects 40 CFR Part 50, Appendix J for PM10 mass analysis:

1. Temperature range is 15°C to 30°C with control ± 3°C

2. Relative humidity range is 20% to 45% with control ± 5% RH

Temperature at 21.3°C ± 3°C (18.3-24.3°C) and RH at 37% ± 5% RH (32-42 % RH) for 24 hour equilibration before any weighing.

2 Description: Content of SOP MLD016 June 17, 2013 Contains only PM10 mass analysis. Subsequent extraction

of PM10 samples and Total Suspended Particulates (TSP) sampling procedures were included in SOP MLD016.

3 Description: Instrument for recording environmental conditions July 1, 2013 A continuous digital data recorder

(Omega sensor) is used to document and store environmental conditions of the balance room. The environmental conditions of the room are stored on the Omega unit and backed up to the shared drive weekly. Data recorder manual is stored in the PM10 references binder which is kept in the balance room.

Honeywell weekly chart was used to check and record data for temperature and percent relative humidity.

4 Description: Field blanks July 1, 2013 One field blank per quarter for each

site implemented per U.S. EPA Technical Systems Audit (TSA) recommendations.

There were no field blanks prior to July 2013.

5 Description: Filter inventory time line


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Date Updated Revision Original Procedure August 22, 2013 Per U.S. EPA recommendations,

filters should not be used if they are more than three years old. A first in/ first out approach should be used by all inventory holders so that filters do not age past this point.

There was no timeline guidance in SOP, but it was a practice to use old filters first for quality control purposes.

6 Description: New analytical balance XP 04 by Mettler Toledo August 23, 2013 New balances were purchased and

installed in 2013. Comparison study has been done with existing Sartorius A200S, and approved by the Quality Management Branch (QMB).

Sartorius A200S balance has been replaced by the Mettler Toledo XP204. Comparison Documentation is located in the balance room.

7 Description: Make-up policy November 20, 2013 A make-up sample must be

collected prior to the next scheduled sampling day. Reference AQSB SOP 408 for more information.

Make-up samples were permitted within a quarter.

8 Description: 24-hour sample report form May 19, 2014 Updated COC form including date

and initials of chemist for post-weighing sample.

There was no area on previous COC to include chemist name or date of post-weighing a sample.

9 Description: Moisture equilibration time April 1, 2015 Note the starting time of

equilibration on the COC for every filter received. This is annotated on the samples received by the laboratory line. If for any reason samples are removed from environmentally conditioned roomed it must be documented on the COC along with the new equilibration start time.

The time mail was opened was written on the top envelope.

10 Description: New PM10 Ecotech High Volume Sampler April 6, 2015 Ecotech samplers use a modified

COC because the sampler does not use a Dickson chart. It provides a calculated LTP volume and standard corrected volume.

All sites had similar PM10 Federal Reference Method (FRM) samplers that required a Dickson


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Date Updated Revision Original Procedure Site operators are now required to send in a printout of the Ecotech data file in place of the Dickson chart to verify sampling duration.

chart for sampling duration verification.

11 Description: Environmental conditions revision July 1, 2015 Effective July 1, 2015 filter

conditioning environment now reflects conditions more stringent than 40 CFR Part 50, Appendix J for PM10 mass analysis:

1. Temperature range is 15°C to 30°C with control ± 3°C

2. Relative humidity range is 30% to 40% with control ± 5%RH

Temperature range was 15°C to 30°C with control ± 3°C Relative humidity range was 20% to 45% with control ± 5%RH

13. REFERENCES

Title 40, Chapter 1, Subchapter C, Part 50, Appendix J, Code of Federal Regulations, “Reference Method for the Determination of Particulate Matter as PM10 in the Atmosphere.” U.S. Environmental Protection Agency, 1997.

Title 40, Chapter 1, Subchapter C, Part 58, Subpart B, Code of Federal Regulations, “Monitoring Network.” U.S. Environmental Protection Agency, March 28, 2016.

Section 2.11, “QA Handbook Reference Method for the Determination of PM10 (High Volume PM10 Sampler) at Standard Temperature and Pressure.” U.S. Environmental Protection Agency, January 1990. http://www3.epa.gov/ttnamti1/files/ambient/qaqc/m211.pdf

Quality Assurance Handbook Volume II. U.S. Environmental Protection Agency, May 2013. http://www3.epa.gov/ttn/amtic/files/ambient/pm25/qa/QA-Handbook-Vol-II.pdf

Quality Assurance Handbook Volume II, Appendix D. U.S. Environmental Protection Agency, July 2014. http://www3.epa.gov/ttn/amtic/files/ambient/pm25/qa/appd_validation_template_amtic.pdf

Compendium Method IO-2.1, “Sampling of Ambient Air Total Suspended Particulate Matter (SPM) and PM10 Using High Volume (HV) Sampler.” Center for Environmental Research Information of Office of Research and Development, U.S.

http://www3.epa.gov/ttnamti1/files/ambient/qaqc/m211.pdfhttp://www3.epa.gov/ttn/amtic/files/ambient/pm25/qa/QA-Handbook-Vol-II.pdfhttp://www3.epa.gov/ttn/amtic/files/ambient/pm25/qa/appd_validation_template_amtic.pdfhttp://www3.epa.gov/ttn/amtic/files/ambient/pm25/qa/appd_validation_template_amtic.pdf


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Environmental Protection Agency, June 1999. www.epa.gov/ttn/amtic/files/ambient/inorganic//mthd-2-1.pdf

Compendium Method IO-3.1, “Selection, Preparation and Extraction of Filter Material.” Center for Environmental Research Information of Office of Research and Development, U.S. Environmental Protection Agency, June 1999. www.epa.gov/ttn/amtic/files/ambient/inorganic/mthd-3-1.pdf

U.S. EPA PM Sampling Schedule, http://www3.epa.gov/ttn/amtic/calendar.html

Quality Control Manual of the Monitoring and Laboratory Division, Northern Laboratory Branch, September 2015.

Final Chemical Hygiene Plan for Northern Laboratory Branch 1927 13th Street, 1900 14th Street, March 2016.

Excellence Plus Analytical Balances Operating Instructions, XP Models – Part 1. http://www.mt.com/dam/P5/labtec/02_Analytical_Balances/03_XP/03_Documentations/03_Operating_Instructions/OI_XP_Analytical_Part_1_EN.pdf

Air Resources Board AQSB SOP 408, December 2014. http://www.arb.ca.gov/airwebmanual/aqsbdocs1/AQSB%20SOP%20408%20(PM10%20VFC)_Final.pdf

http://www.epa.gov/ttn/amtic/files/ambient/inorganic/mthd-2-1.pdfhttp://www.epa.gov/ttn/amtic/files/ambient/inorganic/mthd-3-1.pdfhttp://www3.epa.gov/ttn/amtic/calendar.htmlhttp://www.mt.com/dam/P5/labtec/02_Analytical_Balances/03_XP/03_Documentations/03_Operating_Instructions/OI_XP_Analytical_Part_1_EN.pdfhttp://www.mt.com/dam/P5/labtec/02_Analytical_Balances/03_XP/03_Documentations/03_Operating_Instructions/OI_XP_Analytical_Part_1_EN.pdfhttp://www.arb.ca.gov/airwebmanual/aqsbdocs1/AQSB%20SOP%20408%20(PM10%20VFC)_Final.pdfhttp://www.arb.ca.gov/airwebmanual/aqsbdocs1/AQSB%20SOP%20408%20(PM10%20VFC)_Final.pdf


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APPENDIX A

1. REJECTION CRITERIA FOR PRE-SAMPLED PM10 FILTERS (UNUSABLE)

Observation Definition Pinhole A small hole that can be identified by examining both

the front and back of the filter. A filter with such a defect is considered a reject filter and is unusable.

Dense Spot Viewed from the filter back, this appears as a dark area (approximately 1/8"- 1/4" in diameter) without sharply defined edges. Viewed from the front, an accumulation of filter fibers can be seen. Any filter which contains more than one dense spot or one spot larger than 1/4" shall be considered a reject.

Dark Spot (2 or more)

These spots are distinguished from the dense spots in that such dark spots resemble a fly speck. Their presence results in a defective filter. Any filter containing two or more such dark spots will be considered a reject.

Loose Fiber on Filter Back (Not Re-moveable)

This appears as if a rough object had been moved across the filter back and loosened the filter base. If the number of fibers is small and can be brushed off, the defective filter can be used. If in EPA's judgment, the fibers are too large or too numerous to remove, the filter will be considered a reject.

Quartz Fiber (Detached)

When viewed from the back, this defect resembles a thin spot. The shape can be circular or oval. When rubbed, the quartz may become detached. No evidence of this defect can be seen from the front. If it becomes detached and creates a pinhole, the filter is a reject.

Coloration Yellow, red, or other colored spots. A filter with such coloration is a reject.


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2. ACCEPTABLE DEFECTS FOR PRE-SAMPLED PM10 FILTERS (USABLE)

Observation Definition Line Occasionally a fine line is created by the manufacturing

screen across the filter. A filter with such a defect is considered a defective filter. (A defective filter is considered usable.)

Dense Spot Viewed from the filter back, this appears as a dark area (approximately 1/8"- 1/4" in diameter) without sharply defined edges. Viewed from the front, an accumulation of filter fibers can be seen. If there is only one dense spot per filter, and the area covered is less than l /4" in diameter, the filter will be considered a defective filter.

Thin Spot A small area viewed on the filter that appears to be weak. More light can be seen through this area than through the surrounding area. There can be several spots per filter. A filter with such a defect is considered defective.

Dark Spot (1 or less)

These spots are distinguished from the dense spots in that such dark spots resemble a fly speck. Their presence results in a defective filter. Any filter containing one dark spot results in a defective filter.

Quartz Fiber (Not Detached)

When viewed from the back, this defect resembles a thin spot. The shape can be circular or oval. When rubbed, the quartz may become detached. No evidence of this defect can be seen from the front. If it becomes detached and creates a pinhole, the filter is a reject. Otherwise, it is defective.

Loose Fiber on Filter Back (Re-moveable)

This appears as if a rough object had been moved across the filter back and loosened the filter base. If the number of fibers is small and can be brushed off, the defective filter can be used.

Non-uniformity Any obvious visible non-uniformity of the appearance of the filter when viewed over a light table and might indicate gradations in porosity across the face of the filter is a defect.

Other A filter with any imperfection not described above, such as frayed edges or indentations or the results of other poor workmanship, may be considered defective.


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3. VALIDATION CRITERIA FOR POST-SAMPLED PM10 FILTERS

Observation Definition Filter Contamination

Filters which are dropped or become contaminated by any foreign matter (i.e., dirt, finger marks, ink, liquids, etc.) are invalid.

Damaged or Torn Filters

Filters with tears or pinholes which occurred before or during sampling are invalid. Note: a filter that has a hole or is torn before or during sampling will show evidence of particulate matter collection on both sides of the filter caused by the lack of filter integrity. If a damaged or torn filter is received by the lab, with all pieces included, that does not show evidence of tears or pinholes occurring prior to sampling, and not invalidated by the site operator, the sample should be considered valid

Dickson Recorder Chart (Note: Ecotech samples do not contain a Dickson chart and are exempt from this validation criteria)

A complete 24-hour Dickson recorder chart, documenting the flow rate through the sampler for 24 hours, must be submitted to the laboratory with each filter sample. Filter samples without a complete Dickson recorder chart record are invalid. NOTE: In cases of inking problems where the trace is not complete, if the operator validates the sampler operated properly in the comments section of the report form, the sample will be considered valid.

Report Form The filter is considered invalid if a completed COC is not included with the sample.

Filter Leakage If the filter shows signs of air leakage due to a worn or improperly seated gasket, the sample will be invalidated.

Incomplete or Missing COC

If the COC is missing or incomplete the sample is considered invalid until the missing information is provided to the analyst. If the site operator is able to provide the missing information, the analyst should document all correspondence and validate the sample.

Date Samples are Received in the Laboratory

Samples should be weighed as soon as possible to minimize volatile particle mass loss. Because of this U.S. samples received in the laboratory 30 days or more after they are sampled are invalid. Mexico samples received 30 days after they are sampled are considered valid, however, they are flagged. If they are received more than 45 days after sampling they are invalidated.

Incorrect Filter If the incorrect filter is sampled and the COC does not match the filter number, the sample is invalid.


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APPENDIX B

1. EXAMPLE U.S. EPA MEMORANDUM (REJECTION CRITERIA)


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Page 35 of 42


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APPENDIX C

1. PROCEDURES TO CALCULATE DAILY BALANCE ROOM CONDITIONS

1) The Balance Room conditions should be obtained using the PM10 computer (ARB Barcode 20102775) located in the Balance Room, unless the analyst is familiar with locating network files from an alternate computer.

2) Logon to the PM10 computer. Password = Weighings# (case sensitive).

3) Open the “DicksonOne” program for “DicksonOne - 13th/T” located

at https://www.dicksonone.com/devices/202004449338955284. 4) Login. Note: Analyst must be registered to access DicksonOne.

5) Select the “13th/T Primary” device to retrieve historical READINGS. Wait for the “13th/T Primary” device graph to open.

https://www.dicksonone.com/devices/202004449338955284


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6) Click on the “Export” link on the lower right side of the device graph.

7) Typically, the conditions range should be the 24-hour period immediately before the time of weighing begins. Enter the desired conditions range and click Export .

5) Open the ARB email account registered to receive exported READINGS from DicksonOne devices. Open the DicksonOne export email, which will appear similar to this:

6) Click on the link provided to download the file. Windows Explorer automatically opens.


Page 39 of 42

7) Double-click on the name of the compressed Comma Separated Values (CSV) file. The EXCEL program automatically opens.

In the EXCEL program:

8) All readings from the conditions range indicated will open on a single spreadsheet page.

9) Select the GMT Date and Time columns A and B. Delete these columns.

10) For the columns with “Temperature” and “Relative Humidity” header rows, determine the cell array for the 24-hour period of READINGS before weighing begins.

11) Use EXCEL formulas to calculate the 24-hour Average and Standard Deviation (SD) separately for Temperature (Temp) and Relative Humidity (RH) using the following cell formulas:

• Average formula "=Average(cell start:cell stop)" o Example: =Average(F2:F722)

• SD formula "=STDEV(cell start:cell stop)" o Example: =STDEV(F2:F722)

12) Verify that the calculated results for conditions are valid before starting a weigh session.

Criteria Temp: Valid to weigh when calculated Average is 15 to 30 oC and SD is within +/- 3 oC

Criteria RH: Valid to weigh when calculated Average is 30 to 40% and SD is within +/- 5%

11) The 24-hour conditions file is saved (on the non-weighing Balance Room computer) into "XLSX" format into the "13&T Room Conditions" folder as start-date-year to end-date-year. Example: 01012018 to 01022018.xls.


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APPENDIX D

1. EXAMPLE INITIAL DEMONSTRATION OF CAPABILITY DOCUMENTATION


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APPENDIX E

1. SUMMARY OF ANALYSIS SEQUENCE

SEQUENCE COMMENTS 1.1 Calculate 24-hour conditioning

period of filter samples to be weighed (both pre- and post-)

See Appendix C, Calculate Daily Balance Room Conditions

1.2 Perform the Daily Calibration Check of Balance using 4 g (1 g + 3 g) prior to weighing filter samples

See Section 9. Quality Control

1.3 Confirm the weighing order of filter samples and associated QC samples is set in LIMS-link in prior to the start of each weighing session.

Filter samples must be assigned sample numbers, unique for each sample, using LIMS.

1.4 Analyze filter samples in the following order:

Weigh low mass standard, 3 g Weigh high mass standard, 5 g Weigh first 9 filters

(Sample 1 through Sample 9)

Re-weigh first filter (Sample 1 Duplicate)

See Section 9.6, Duplicates.

Weigh mass standard check, 3 g Alternate 3 g and 5 g mass standards check after subsequent Duplicates.

Weigh next 9 filters (Sample 10 through Sample 18)

Re-weigh Sample 10 (Duplicate) Weigh mass standard check, 5 g Weigh next 9 filters (Sample 19

through Sample 27)

Re-weigh Sample 19 (Duplicate) Continue to weigh next 9 filters,

followed by re-weigh of first of 9 as Duplicate

If less than 9 filters are weighed, a Duplicate re-weigh of the first filter must still be weighed.

Weigh low mass standard, 3 g Weigh high mass standard, 5 g

MLD016Revision 7.0Northern Laboratory BranchMonitoring and Laboratory DivisionTable of Contents1. INTRODUCTION2. SUMMARY OF METHOD3. ACRONYMS AND DEFINITIONS4. INTERFERENCES5. PERSONNEL QUALIFICATIONS AND TRAINING6. SAFETY REQUIREMENTS AND HAZARDOUS WASTE7. EQUIPMENT, SUPPLIES, AND CHEMICALS8. PROCEDURES9. QUALITY CONTROL10. DATA MANAGEMENT11. CALCULATIONS12. REVISION HISTORY13. REFERENCESAPPENDIX A1. REJECTION CRITERIA FOR PRE-SAMPLED PM10 FILTERS (UNUSABLE)2. ACCEPTABLE DEFECTS FOR PRE-SAMPLED PM10 FILTERS (USABLE)3. VALIDATION CRITERIA FOR POST-SAMPLED PM10 FILTERSAPPENDIX B1. EXAMPLE U.S. EPA MEMORANDUM (REJECTION CRITERIA)APPENDIX C1. PROCEDURES TO CALCULATE DAILY BALANCE ROOM CONDITIONSAPPENDIX D1. EXAMPLE INITIAL DEMONSTRATION OF CAPABILITY DOCUMENTATIONAPPENDIX E1. SUMMARY OF ANALYSIS SEQUENCE

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