STANDARD OPERATING PROCEDURE

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STANDARD OPERATING PROCEDURE Powered By Docstoc
					STANDARD OPERATING PROCEDURE
Gravimetric Analysis of Particulate Collected with R&P Partisol
Samplers and MetOne SASS Samplers

                                                          DEQ03-LAB-0027-SOP
                                                      Version 2.0 June 27, 2003


                                                                                       Laboratory Division
                                                                                       1712 SW 11th Avenue
                                                                                       Portland, OR 97201
                                                                                       Phone: (503) 229-5983
                                                                                       Fax: (503) 229-6924
                                                                                       www.deq.state.or.us




Prepared by: Sarah Bennie and Ben Jones ________________ Date: _____________________

Reviewed by: _______________________________________ Date: _____________________
Technical Director

Approved by: _______________________________________ Date: _____________________           June 2003
Quality Assurance Officer
This page left intentionally blank.
Department of Environmental Quality
Gravimetric Analysis of Particulate Collected with R&P Partisol Samplers and MetOne SASS
Samplers                                                                 Date: June 27, 2003
Revision: 2.0                                                                                                                        Page 3 of 25


                                                   Table of Contents

Table of Contents ............................................................................................................................ 3
1.      Test Method ............................................................................................................................ 4
2.      Applicable Matrices................................................................................................................. 4
3.      Detection Limits ...................................................................................................................... 4
4.      Scope and Application ............................................................................................................ 4
5.      Summary................................................................................................................................. 4
6.      Definitions ............................................................................................................................... 4
7.      Interferences ........................................................................................................................... 6
8.      Safety ...................................................................................................................................... 8
9.      Equipment and Supplies ......................................................................................................... 8
10.          Reagents ............................................................................................................................ 9
11.          Standards ........................................................................................................................... 9
12.          Sample Collection, Preservation, Shipment, and Storage ................................................. 9
13.          Calibration and Standardization ......................................................................................... 9
14.          Quality Control .................................................................................................................. 10
     14.1.       Data Assessment and QC Acceptance Criteria ........................................................... 10
     14.2.       Corrective Actions for Out-of-control Data ................................................................... 10
     14.3.       Contingencies for Handling Out-of-control Data .......................................................... 11
15.          Procedure ......................................................................................................................... 12
     15.1.       Pre-sampling conditioning:........................................................................................... 12
     15.2.       Pre-sampling weighing:................................................................................................ 12
     15.3.       Post-sampling conditioning: ......................................................................................... 14
     15.4.       Post-sampling weighing: .............................................................................................. 14
16.          Calculations ...................................................................................................................... 15
17.          Method Performance ........................................................................................................ 16
18.          Maintenance ..................................................................................................................... 17
19.          Pollution Prevention.......................................................................................................... 19
20.          Waste Management ......................................................................................................... 19
21.          References ....................................................................................................................... 19
Appendix A: Calibration of Working Mass Standards.................................................................... 20
Appendix B: Criteria Tables for PM2.5 FRM Sampling ................................................................ 23
   Department of Environmental Quality
   Gravimetric Analysis of Particulate Collected with R&P Partisol Samplers and MetOne SASS
   Samplers                                                                 Date: June 27, 2003
   Revision: 2.0                                                                             Page 4 of 25



1. Test Method
   Gravimetric Analysis of Particulate Collected with R&P Partisol Samplers and MetOne SASS
   Samplers


2. Applicable Matrices
   This method applies to the analysis of ambient air particulate collected on 47mm diameter Teflon
   filters.


3. Detection Limits
   Based on the Partisol field blanks statistics, we have estimated the method detection limit at 0.6
   µg/M3, assuming a volume of 24M3 per sample We are also using 0.6 µg/M3 as our method
   reporting limit.
   Because EPA has requested that the results of speciation sampling be uncensored, we have not
   applied a reporting limit to the SASS results. If we use the Partisol field blanks statistics for the
   SASS sampler, the MDL would be 2.1 ug/M3 , assuming a volume of 9.7M3 per sample.


4. Scope and Application
   This method describes the gravimetric analysis of ambient air particulate samples collected on
   47mm Teflon filters. This method is specifically applicable to samples collected using either an
   R&P Partisol sampler or a MetOne SASS sampler. The R&P Partisol sampler has been used as
   the Federal Reference Method (FRM) sampler for the PM2.5 program, although it can also be
   used for PM10 sampling.. The MetOne SASS sampler has been used for the Speciation program
   within the PM2.5 program.
   This procedure also describes the calculation of the particulate mass per volume of sampled air,
   using both the laboratory gravimetric data and the field sampling data.
   Although the sampling SOPs are described else where, the laboratory personnel must be familiar
   with the sampling requirements.
   The method complies with the national ambient air quality standards referred to as PM2.5, as
   described in Appendix L of 40 CFR, Part 50.


5. Summary
   An electrically powered air sampler draws ambient air at a constant volumetric flow rate into
   specially designed inertial particle-size separator (e.g, cyclones or impactors) where the
   suspended particulate matter in the PM2.5 or PM10 size ranges is separated for collection on a
   polytetrafluoroethylene (PTFE) filter over a specified sampling period. Each filter is weighed
   before and after sample collection to determine the net gain due to the particulate matter. The
   mass concentration in the ambient air is computed as the total mass of collected particles in the
   PM2.5 or the PM10 size ranges divided by the actual volume of air sampled, and is expressed in
   µg/m3 at LTP (local temperature and pressure)


6. Definitions
   Batch: environmental samples that are prepared and/or analyzed together with the same process
   and personnel, using the same lot(s) of reagents.
Department of Environmental Quality
Gravimetric Analysis of Particulate Collected with R&P Partisol Samplers and MetOne SASS
Samplers                                                                 Date: June 27, 2003
Revision: 2.0                                                                               Page 5 of 25

         Analytical batch is composed of prepared environmental samples (extracts, digestates
         or concentrates) which are analyzed together as a group. An analytical batch can include
         prepared samples originating from various environmental matrices.
Blank: a sample that has not been exposed to the analyzed sample stream in order to monitor
contamination during sampling, transport, storage or analysis. The blank is subjected to the usual
analytical and measurement process to establish a zero baseline or background value and is
sometimes used to adjust or correct routine analytical results.
         Lab Blanks: These are filters that are conditioned, pre-sample weighed, stored in
         labeled Petri dishes in the laboratory, reconditioned, and then reweighed along with post-
         sample filters. They are weighed with the similarly numbered post-sample (or loaded)
         filters at regular intervals (rather than all at one time).
         Field Blanks: These are filters that are treated in all ways as a normal sample (including
         installation on the samplers in the field) except that no air is sampled onto them. (Field
         blanks, as defined in this SOP, are referred to as “transfer blanks” in LIMS.)
Calibration: to determine, by measurement or comparison with a standard, the correct value of
each scale reading on a meter, instrument, or other device. The levels of the applied calibration
standard should bracket the range of planned or expected sample measurements.
Continuing Calibration Blank (CCB): a “zero” standard analyzed along with the CCV standard.
The CCB verifies that the lower end of the calibration curve remains valid during the analysis of
the batch of samples. A CCB is analyzed at the beginning of each batch, at the end of a batch,
and at least every 10 samples during a batch. For this SOP, the CCB is the balance reading
when nothing is placed on the balance pan.
Continuing Calibration Verification Standard (CCV): a standard analyzed after the initial
calibration to verify that the instrument calibration remains valid. A CCV is analyzed at the
beginning of each batch, at the end of a batch, and at least every 10 samples during a batch. For
this SOP, the CCV is the 200 mg working standard.
Control filter: A control filter is weighed at the beginning of each weighing session. One filter is
chosen at random at the beginning of every new filter lot. The filter is weighed, it is placed in an
air-permeable Petri dish that is stored in the weighing room. The Petri dish is labeled with the
filter’s weight, the filter’s ID, the date, and the lot number. The control filter is used to monitor any
significant changes in the control room’s environment that may affect the filters.
Holding Times (Maximum Allowable Holding Times): the maximum times that samples may
be held prior to analysis and still be considered valid or not compromised.
Laboratory Control Sample (LCS): a sample matrix, free from the analytes of interest, spiked
with verified known amounts of analytes or a material containing known and verified amounts of
analytes. It is generally used to establish intra-laboratory or analyst specific precision and bias or
to assess the performance of all or a portion of the measurement system. For this SOP, the LCS
is equivalent to the QCS.
Laboratory Duplicate: aliquots of a sample taken from the same container under laboratory
conditions and processed and analyzed independently. For this SOP, aliquots cannot be taken
from a single filter. As an alternative, we reweigh 1 out of 10 filters and refer to it as a laboratory
duplicate, a reweigh duplicate, or a reweigh.
Laboratory Information Management System (LIMS): a comprehensive computerized
database system that a laboratory uses for sample tracking and data management, from sample
receipt to reporting and archiving.
Matrix (Quality System): the component or substrate that contains the analyte of interest.
   Department of Environmental Quality
   Gravimetric Analysis of Particulate Collected with R&P Partisol Samplers and MetOne SASS
   Samplers                                                                 Date: June 27, 2003
   Revision: 2.0                                                                              Page 6 of 25

            For this analysis, the matrix is ambient air particulate, which is really neither “air and
            emissions” or “solids”, the most relevant NELAC matrices. For the purposes of batch and
            QC requirement determinations, this is the only matrix (although particulate size can
            affect the results in some cases).
   Matrix Spike (spiked sample or fortified sample): a sample prepared by adding a known mass
   of target analyte to a specified amount of matrix sample for which an independent estimate of
   target analyte concentration is available. Matrix spikes are used, for example, to determine the
   effect of the matrix on a method's recovery efficiency. For this SOP, we have no reliable method
   of spiking the samples.
   Method Detection Limit (MDL): the minimum concentration of an analyte that can be identified,
   measured, and reported with 99% confidence that the analyte concentration is greater than zero.
   Particulate matter: A generic term for a broad class of chemically and physically diverse
   substances that exist in the air as discrete particles (liquid droplets or solids) over a wide range of
   sizes.
   Quality Control Sample (QCS): an uncontaminated sample matrix spiked with known amounts
   of analytes from a source independent from the calibration standards. It is generally used to
   establish intra-laboratory or analyst specific precision and bias or to assess the performance of all
   or a portion of the measurement system. For this SOP, the 100 mg mass standard acts as the
   QCS.
   Quantitation Limits: levels, concentrations, or quantities of a target variable (e.g., target analyte)
   that can be reported at a specified degree of confidence.
   Replicate Analyses: the measurements of the variable of interest performed identically on two or
   more sub-samples of the same sample within a short time interval. For this SOP, replicate
   analysis is performed on samples (also referred to as field duplicates) collected at the same site
   and the same time, using the same model of sampling equipment. The duplicate samples are
   collected with either a collocated sampler (MV or Partisol sampler) or another channel of the
   same sampler (SASS Speciation sampler).
   Standardized Reference Material (SRM): a certified reference material produced by the U.S.
   National Institute of Standards and Technology or other equivalent organization and
   characterized for absolute content, independent of analytical method. For this method, our
   primary mass standards masses are NIST traceable.


7. Interferences
   Because these filters may be analyzed to determine the particulate’s chemical composition,
   interferences are not limited to interferences that have a significant effect on the mass. Any
   contamination or material loss will have a greater effect on some chemical species than it will
   have on the mass. Analysts should keep this in mind during all processes involving the filters.
   The following are specific interference that may affect mass, sample composition, or both:
   1) Both the filter material and the loaded particulate can absorb moisture. Teflon filters gain less
      than 4 µg of weight with every 10% increase in relative humidity. Depending on the weight
      and composition of the particulate, the absorbed moisture on the particulate may be much
      greater than the absorbed moisture on the filter membrane. High moisture may also affect
      chemical reactions leading to volatilization of inorganic salts. To correct for humidity
      differences, a controlled environment with the RH at 32.5% +/- 2% is used for equilibrating (≥
      24 hours) and weighing all of the filters.
   2) Temperature variations in the weighing room can result in balance instability as the balance is
      sensitive to temperature and air density changes. The particulate itself is also sensitive to
Department of Environmental Quality
Gravimetric Analysis of Particulate Collected with R&P Partisol Samplers and MetOne SASS
Samplers                                                                 Date: June 27, 2003
Revision: 2.0                                                                                Page 7 of 25

   temperature as volatilization can occur at different rates at different temperatures. Maintaining
   the temperature at 21.5° C +/- 0.5° C is sufficient to minimize adverse temperature effects.
3) Vibrations may result in balance readout instability. The use of a balance table of high mass
   with vibration-isolating pads reduces the effects of building or room vibrations. Vibration
   producing instruments, such as fans or audio speakers, should not be in contact with the
   balance table. Infrequently, machinery or construction in or outside the building may lead to
   episodes of balance instability.
4) Static electricity can interfere in two ways:
         a) If static has built-up on the filters or nearby objects, it can cause balance inaccuracies.
         The balance may be slow to reach a stable weight and lab duplicates (and field
         duplicates) may be out of control.
         b) Static electricity that is present on filters or their containers may cause transfer of
         particulate from and/or to the filter surface.
   The buildup of static charge can be reduced by grounding conductive materials, applying anti-
   static solutions to non-conductive surfaces (i.e., inside of balance chamber), avoiding air
   currents blowing directly onto plastic surfaces, wearing low-static clothing, and using a
   grounding pad for the operator to touch prior to and during filter weighing. The most important
   measure taken in this method is the use of Staticmaster strips to reduce static on the filters
   both before and during weighing. Exposure to the Staticmaster strips for 30 seconds prior to
   weighing is sufficient to reduce the charge on the filters under normal circumstances. A
   Staticmaster strip is also placed in the weighing chamber. The Staticmaster strips have a
   limited lifetime (due to the 138 day half-life of Polonium 210) and are replaced every 6 to 9
   months.
5) Touching the mass standards, filters, and filter handling equipment can contaminate them with
   oils, perspiration, and cosmetic products. Handling filters only with the appropriate forceps
   can eliminate contaminants.
6) The cassettes that hold the filters during sampling can add to the weight of the filters. The
   originally supplied white cassettes off-gassed or exuded organic compounds that increased
   the mass of the filters. We have found that thorough cleaning (including hot water, detergent,
   and sonic treatment) can reduce this contamination. This does not seem to be a problem with
   the newer blue cassettes, although an initial thorough cleaning of them is still necessary.
7) Dust can contaminate filters at any stage of handling. Cleaning the work area and keeping
   filters in protective containers help reduce dust contamination. All items used in the weighing
   room (e.g. furniture, paper, trays, cleaning equipment) should be considered to be sources of
   dust and efforts should be made to reduce their contribution. The controlled room air supply is
   filtered to reduce particulate circulation in the room. New analysts are encouraged to weigh
   dust, sand and small fibers to get a sense for how much these contaminants weigh.
8) Chemical vapors can change the weight and composition of the collected particulate in several
   ways. Particulate can absorb organic vapors, including plant generated volatiles (i.e.,
   terpenes), combustion products (i.e., vehicle fumes), or laboratory reagents (e.g. solvents).
   Air particulate can also react with gases, particularly ammonia (which is present in human
   breath and laboratory reagents).
9) Power supply or grounding fluctuations and equipment operations inside or outside of the
   building can also cause possible balance instability. We have not found this to be a problem
   at our current facility.
  Department of Environmental Quality
  Gravimetric Analysis of Particulate Collected with R&P Partisol Samplers and MetOne SASS
  Samplers                                                                 Date: June 27, 2003
  Revision: 2.0                                                                            Page 8 of 25

8. Safety
  For general laboratory safety procedures, consult the DEQ Laboratory Safety Manual (Chemical
  Hygiene Plan).
  Refer to the Job Hazard Assessment for this procedure (Particulate Matter Weighing) and
  conduct analysis in accordance with the safety precautions specified.
  Material Safety Data Sheets (MSDS) are available in the laboratory library.


9. Equipment and Supplies
  • AQLIMS database and associated VB programs for capturing weights from balance and
    performing calculations.
  • Cassette opening tool
  • Computer. The computer is configured to capture the weights from the balance and store
    them in a database table used by AQLIMS.
  • Filter cassettes, consisting of three parts: a top, bottom, and screen, as supplied by R & P.
    These cassettes meet the requirements as stated in section 7.3.5 of Appendix L to 40 CFR
    Part 50, except they have beveled edges as required for the R&P Partisol samplers.
  • Filter labels, vinyl, pre-numbered, that fit in the groove on the edge of the cassettes
  • Forceps, non-magnetic, stainless steel, non-serrated
  • Forceps, plastic-tipped
  • In-line filter installed on the line attached to the building compressed air, Balson Filter Tube,
    Grade BQ
  • Kimwipes
  • Light box used to examine filters for pin holes.
  • Lighted magnifier used for examining the filters for damage or contamination.
  • Mass standards: Primary standards are 100 and 200 mg ASTM class 1 weights that are
    NVLAP certified annually. Working standards are 100 and 200 mg weights that are compared
    to the Primary standards quarterly.
  • Microbalance, ATI-Cahn C44. The autozero and self-calibration features should be disabled.
  • Petri dishes, polystyrene, 50x9 mm, Falcon.
  • Post-sampling conditioning trays, fabricated by staff
  • Protective boxes for shipping and temporary storage of filters while they are in the filters
    cassettes, 2 5/8'”square by 5/8" high molded, hinged clear styrene
  • Refrigerator maintained at <4°C.
  • Slide trays, Leica 4G002 (Pro Photo Supply by special order).
  • Static dissipating pad surrounding the balance.
  • Staticmaster anti-static strip (1U400) installed in the weighing chamber of the balance.
  • Staticmaster anti-static strips (2U500) mounted the top and bottom of plastic stand.
  • Teflon filters, 46.2 mm, as supplied by EPA. These filters meet the requirements as stated in
    section 6.0 of Appendix L to 40 CFR Part 50. These have a nominal pore size of 2 um (based
    on water filtering) but collect greater than 99.7% of the 0.3 um particles based on air filtering.
  • Temperature and relative humidity sensor and controller, Humiscan (General Eastern) with
    accuracies of ±0.2°C, and ±1% RH. Associated with this device is a data logger and software
    to download the logged data.
  • Temperature and relative humidity sensor and recorder, Dickson THDx with accuracies of
    ±1°C, and ±2% RH.
  • Ultrasonic bath. Sonicore Model 211 TH, or similar.
  • Weighing room, controlled for temperature and RH using a Honeywell Digital Controller (UDC
    3300), a Munters desiccant wheel dehumidifier (HC-300-EA), the building steam supply, and a
    Copco installed furnace/air-conditioner unit. The temperature and relative humidity of the room
   Department of Environmental Quality
   Gravimetric Analysis of Particulate Collected with R&P Partisol Samplers and MetOne SASS
   Samplers                                                                 Date: June 27, 2003
   Revision: 2.0                                                                            Page 9 of 25

     is recorded continuously. Either a chart paper record (from the Dickson THdx meter) or a data
     file (from the Humiscan datalogger) is retained as a record of the room’s conditions.
   • Weighing table, 3 point Gibraltar stone table.
   • Working mass standards, 100 and 200 mg weights that are compared to the primary standards
     quarterly.

10. Reagents
    • Micro detergent


11. Standards
   The balance is calibrated using an internal mass standard. This calibration is confirmed daily
   using the “working” 100 and 200 mg working standards, which are calibrated to the primary
   standards every three months (See “Appendix A”).


12. Sample Collection, Preservation, Shipment, and Storage
   There are slight differences in the handling procedures for SASS Speciation samples and for
   Partisol samples. It is primarily the Partisol procedures that are described below. See the
   Speciation Sampling Canister Processing SOP to learn the differences for the SASS Speciation
   samples.
   Clear, polystyrene plastic protective cases are used for sample retrieval, shipment, and storage of
   the Partisol sampler samples. These hold individual filters within their sampling cassettes and
   are taped shut prior to sampling.
   Samples are collected from the samplers by field staff, at which time they are stored in either a
   cooler or an on-site refrigerator. Samples are retrieved from the samplers within 177 hours of the
   end of sampling for Partisol FRM PM2.5 samples (48 hours for SASS Speciation samples). Any
   abnormalities that are observed on the filters, the sampler, or the nearby environment are noted
   on the appropriate field sheet. During shipping or transport, the samples are kept at <4˚C. Upon
   return to the laboratory, the samples are placed in a refrigerator maintained at ≤ 4˚C.
   To equilibrate the filters, they are taken to the weighing room, removed from their protective
   cases and equilibrated in their cassettes for a minimum of 24 hours before post-sampling
   weighing.
   The holding time for pre-sampling (tared) filters is 30 days, although the results are not
   downgraded if this holding time is exceeded. The holding time for post-sampling (loaded) filters is
   10 days, unless they are maintained ≤ 4˚C during the entire time between retrieval and the start
   of conditioning, in which case the time period cannot be more than 30 days. (The latter option
   was modified by EPA slightly by memo dated March 1, 2002 stating that the holding time can be
   calculated at 34 days minus the average temperature—degrees C—during transport and post-
   sampling storage—but not more than 30 days.)
   After post-sampling (loaded) weighing, filters are stored in labeled Petri dishes and cataloged in
   closed cardboard boxes. They are stored in either a refrigerator or freezer for an archiving period
   of at least one year.


13. Calibration and Standardization
   Calibration of the balance prior to weighing is covered under “Section 15, Procedure”.
   Calibration of the working mass standards occurs every three months, and is covered in
   “Appendix A”.
   Department of Environmental Quality
   Gravimetric Analysis of Particulate Collected with R&P Partisol Samplers and MetOne SASS
   Samplers                                                                 Date: June 27, 2003
   Revision: 2.0                                                                                   Page 10 of 25

14. Quality Control

   14.1.      Data Assessment and QC Acceptance Criteria
   Data assessment and QC acceptance criteria are of primary importance in assessing the quality
   of data resulting from an analytical batch. Both negative and positive biases are a concern. The
   following data assessment and QC data are required for all analyses:

   Listing of required Quality Control (QC) elements, including frequency and acceptance limits.

   Quality Control Element               Frequency                              Acceptance Limits
   Quality control sample                1 at the beginning of each             ± 3µg
   (QCS)—100mg working                   batch
   mass standard

   Continuing Calibration                1 per 10 samples                       ± 3µg
   Blank (or CCB)—empty
   balance pan
   Continuing Calibration                1 per 10 samples.                      ± 3µg
   Verification (CCV)—200mg
   working mass standard
   Field blanks                          All sites, at a frequency of           Between -10µg to +20µg
                                         approximately 5%
   Lab blanks                            At least 1 per 20 samples, or          ≤ ±10µg/filter
                                         one every batch.
   Laboratory duplicates--               1 in every 10 samples                  ≤ ±7µg/filter.
   reweighs
   Control filter                        1 at beginning of batch                ≤ ± 5µg/filter change from the
                                                                                last weighing session.
   Weighing room temperature             Check record for the 24 hours          21.5°C ± 0.5°C
                                         prior to weighing
   Weighing room relative                Check record for the 24 hours          32.5% ± 2%.
   humidity                              prior to weighing


   14.2. Corrective Actions for Out-of-control Data

       It is at the analyst’s discretion on how to handle out-of-control or unacceptable data. Quality
       control measures and corrective actions are as follows:


       1) QCS: If the initial weighing of the 100 mg mass standard is out-of-control, re-tare and re-
          calibrate the instrument and weigh the 100 mg mass again. If it is still out of control,
          inform the senior chemist. Together, the analyst and the senior chemist may investigate
          by checking for balance stability, confirming the weight of the standard relative to the
          primary standards, performing a balance corner-check (see appendix A) or contacting a
          balance technician to make repairs.
Department of Environmental Quality
Gravimetric Analysis of Particulate Collected with R&P Partisol Samplers and MetOne SASS
Samplers                                                                 Date: June 27, 2003
Revision: 2.0                                                                               Page 11 of 25

    2) CCB: If the CCB is out of control, the balance can be retared (which will automatically
       bring the CCB in-control) after investigating that the balance pan is clean. If the CCV is
       then in-control, then the filters weighed since the last in-control CCB should be
       reweighed. The CCB can be checked frequently during the weighing session, and if it is
       in-control but off slightly, the balance can be retared. If the CCB is out of control more
       than once during a weighing session, discuss and investigate the instability with the
       senior chemist.
    3) CCV: If the CCV is out of control, the balance can be retared and recalibrated. If the
       CCV is still out of control, the same actions should be taken as stated under the QCS.
       Whenever the CCV is found to be out of control, all filters weighed after the last in-control
       CCV should be reweighed.
    4) Field blanks: If any field blank has a weight change that falls outside the control limits,
       investigate the weighing process by repeating the post-sampling weighing and verifying
       that the pre-weighing data in the database is correct. If the field blank data is still out of
       control, inform the senior chemist. Further investigation may include investigating the
       contribution to the blank in the various steps of sample collection, transport, and
       processing.
    5) Lab blanks: Investigate by reweighing both the lab blank in question and any additional
       lab blanks within the session, and by checking the calibration of the balance. If the post-
       sampling weighing is out of control for only the one lab blank, inform the senior chemist,
       but continue weighing the post-sampling filters. If the investigation concludes that the out
       of control condition is more widespread, the problem must be resolved before weighing
       may continue.
    6) Laboratory duplicates or reweighs: If a replicate weighing exceeds the established control
       limit, investigate the source of the poor precision. Gently clean the weighing pan with a
       photographer’s brush that is located near the balance. Re-weigh the other nine filters
       from the duplicate’s original set. Inform the senior chemist if the problem cannot be
       resolved.
    7) Control filter: If the control filter’s weight is significantly different from previous weighings,
       investigate and correct the problem before proceeding. Needed corrections may include
       cleaning the balance pan, re-zeroing and recalibrating the instrument, checking for
       sources of balance instability, and examining the filter for contamination. If a solution
       cannot be found, inform the senior chemist and investigate further, including the
       confirmation that the room did not become out-of-control since the previous weighing
       session.
    8) Weighing room temperature and humidity control: Inform the senior chemist if the room is
       out-of-control, and investigate the reason for the room’s instability. (The PM2.5 rule
       actually only requires that the room be controlled to between of mean relative humidity of
       between 30% and 40% with a variability of not more than 5% within 24 hours, and a
       mean temperature of between 20°C and 23°C with a variability of not more than 2°C
       within 24 hours. If these less stringent measures are the met, the senior chemist may
       judge that the conditions are in-control, and weighing may continue.) The accuracy of the
       system sensors may need to be investigated. Shut down and restart the room’s systems
       according to the chart on the door. HVAC professionals may be employed to improve the
       operation of the environmental controls.


14.3.     Contingencies for Handling Out-of-control Data
    If none of the corrective actions brings the QC elements under control, the data may be
    reported as estimates or not reported at all, as decided by the analyst and the section
  Department of Environmental Quality
  Gravimetric Analysis of Particulate Collected with R&P Partisol Samplers and MetOne SASS
  Samplers                                                                 Date: June 27, 2003
  Revision: 2.0                                                                           Page 12 of 25

      manager.


15. Procedure

  15.1. Pre-sampling conditioning:
       1) Inspect the filters for flaws using EPA’s guidelines. Use the non-serrated stainless steel
          forceps (as in all filter handling) and a lightbox for backlighting. Filters are inspected and
          conditioned by box number. Perform these inspections in the conditioning room.
          Record approximate percentages of faults and discard rejected filters. Inform the EPA if
          the number of rejects is excessive compared to their testing results.
              The list of EPA defined flaws include:
              • Pinholes
              • Separation of ring
              • Chaff or flashing (extra attached residual material on the ring which would prevent
                airtight sealing in the cassette.)
              • Loose material
              • Discoloration
              • Filter non-uniformity
              • Other imperfections

       2) Place the filters in slide trays, maintaining all ring IDs facing left.
       3) Gently blow the filters clean using the compressed air line with the in-line grade BQ filter
          (in room U51). This step removes loose pieces of filter membrane or filter rings that
          may have contaminated the filters during manufacturing.
       4) Immediately return the filters to the weighing room and condition them for a minimum of
          one week. (If it is determined that a lot requires more than a week for initial
          equilibration, this period of time should be extended.) Label each tray with the lot
          number, box number, analyst’s initials, and the date that conditioning began. Place the
          loaded slide trays into their holding boxes, leaving the box doors open.


  15.2. Pre-sampling weighing:
  This describes the process for Partisol sampler filters. The MetOne sampler filters are processed
  similarly but they are loaded in the canisters prior to being taken to the field. See the Speciation
  Sampling Canister Processing SOP to learn the differences for the SASS Speciation samples.
  Note: Upon initially opening the weighing program, several choices and inputs are required. The
  analyst must be trained on using this software, but each computer input will not be discussed
  here.
       1) Record in a blue book and in the LIMS system the following data: analyst’s initials, date,
          time, balance ID, relative humidity, and temperature. At the start of a new slide tray,
          tape the label with the conditioning information in the blue book.


       2) Determine whether the temperature and relative humidity in the conditioning room has
          been 21.5°± 0.5°C and 32.5%± 2.0%, respectively, for the previous 24 hours. This may
          involve visually reviewing the chart or it may mean performing calculations based on
          data files stored in the computer. If the requirements are met, continue weighing. If not,
          investigate why and take corrective action according to the quality control methods
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          described in “Section 14, Quality Control”. In addition, during the weighing session,
          confirm every ten filters that the room remains under the controlled conditions.
     3) Open the door to the balance chamber momentarily, and then close it. Tare the
        instrument after the reading becomes steady, then perform a balance calibration (i.e.
        push the calibration button). Check the balance’s tare again. If the tare is 0.000 µg,
        continue. If it is ≤ ±0.002 µg, re-tare and continue. If it is > ±0.002 µg, re-tare and
        recalibrate. If the balance needs to be recalibrated more than once at this point, it is not
        stable enough to continue weighing, and the source of the instability needs to be
        investigated.
     4) Weigh the 100 mg and 200 mg working mass standards, using the plastic forceps to
        handle them. If they are not within ± 3 µg, investigate and take corrective action (see
        “Section 14, Quality Control”). Record these weights in the blue book.
     5) Weigh the control filter (see “Section 14, Quality Control”). If the weight change from the
        previous weighing exceeds ± 5 µg, check the balance tare, the mass standards, and
        recalibrate if necessary.
     6) Visually inspect the filter for any defects or signs of contamination. Discard the filter if
        defects are noted. If a single particle or fiber is noted as a contaminated, gently remove
        it from the filter by gently tapping the back of the filter against the edge of the
        Staticmaster assembly.
     7) Place the filter on the Staticmaster strip outside the balance. The filter should remain on
        the strip for at least 30 seconds.
     8) Enter the filter ID number in the computer and in the logbook.
     9) Move the filter from the Staticmaster strip to the balance pan. Close the door and allow
        the readout to become stable (remain unchanged for 20 seconds). Capture the weight
        in the LIMS program and record the weight in the blue book. Occasionally, the last digit
        of the display will alternate between 2 numbers. If this continues for 30 seconds or
        more, it is because the filter mass is approximately midpoint between the two displayed
        values. Accept the last value displayed at ~30 seconds.
     10) Place the filter in a clean cassette and press the top half into the bottom half at several
         points along the edge to securely close the cassette. (Filters must always be placed in
         the cassettes with the ring ID facing up, away from the screen. This allows us to know
         which side is loaded with particulate even if the loading is very light.) Attempt to rotate
         the two portions of the ring. If the portions rotate, reassemble the cassette using a
         different set of rings. (Note, with age, the cassette rings may crack. If cassette rings
         snap together too loosely, look for cracks in the bottom ring. Discard any cracked rings.)
     11) Place the filter ID number label on the edge of the cassette. The label may need to be
         trimmed with scissors to allow the label to fit in the recess on the edge of the cassette. If
         trimming is required, ensure that the number is still legible. (The label may cause
         jamming in the sampler if the label’s edges protrude beyond the recessed groove on the
         cassette’s edge.)
     12) Place the cassette in a clean, individual shipping case.
     13) Repeat the weighing process with additional filters.
     14) After weighing 5 filters, check the balance’s tare. This is the continuing calibration blank
         (CCB). See “Section 6, Definitions” for a definition and “Section 14, Quality Control” for
         control limits and corrective actions.
     15) After weighing 10 filters, record the temperature and relative humidity of the conditioning
         room. Check the balance’s tare (CCB). Perform the necessary control actions and then
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          check the 200 mg mass standard. This is the continuing calibration verification (CCV).
          See “Section 6, Definitions” for a definition and “Section 14, Quality Control” for control
          limits and corrective actions.
     16) Randomly select one of the previously weighed ten filters, remove it from the cassette,
         and reweigh. This is the lab duplicate or “reweigh”. See “Section 6, Definitions” for a
         definition and “Section 14, Quality Control” for control limits and corrective actions.
     17) During each weighing session, place at least one per 20 (but no fewer than 1) of the
         weighed filters directly into a Petri dish and set it aside to be used as a laboratory blank
         (see sections 6 and 14). A corresponding filter ID label should be placed on the lab
         blank container and the Petri dish marked with the date, the term “Lab Blank”, and the
         analyst’s initials.
     18) At the end of each weighing session, record the balance’s tare, the time, the
         temperature, the relative humidity, and the 200 mg working standard weight.
     19) Following weighing, the filter shipping boxes should be labeled with the filter expiration
         date (30 days from the initial weighing), and taped shut with masking tape. Place filters
         that are ready for sampling in the designated area in the laboratory. The laboratory staff
         is responsible for ensuring that an appropriate number of filters are available for the
         monitoring staff. Extra filters (relative to the number of filters that will be used within the
         next few weeks) should not be weighed. This will minimize the number of filters that are
         discarded because they are not used before their expiration date.
     20) Print out a report of the weights captured during the weighing session and check the
         entries against the records in the blue book. If any errors were made, investigate further
         and have the senior chemist correct any erroneous records. The printed reports should
         be stored as a backup record of the weights captured by the database.


15.3.    Post-sampling conditioning:
Because filters “expire” after being sampled, and because some filters will be returned to the
laboratory close to their expiration date, the check-in refrigerator must be checked at least twice a
week (preferably Monday AM and Thursday AM) so that filters can be transferred to the control
room and weighed
     1) Retrieve the filters that the monitoring staff have checked-in and placed in the
        refrigerator. In the conditioning room, remove the cassettes from the shipping cases
        and place the cassettes in the conditioning trays in numerical order. Mark each tray with
        the date and time that the conditioning began.
     2) At the same time, open a Petri dish of one lab blank for every 20 filters (or at least one
        per weighing session for smaller batches), and arrange it in numerical order with the
        samples. Condition the lab blank(s) alongside the post-sampling filters. Condition all
        filters for at least 24 hours with the room conditions in-control.


15.4. Post-sampling weighing:
    For the post-sampling weighing, follow the same steps as the pre-sampling weighing except:
         1) Weigh the post-sampling filters as soon as possible after the 24 hour conditioning
            period.
         2) After weighing the mass standards, weigh the lab blank(s) and capture the weight
            normally. See Section 14 for the control limits and the corrective actions.
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            3) When removing the filters from the cassettes, use the specially designed tool to
               separate the rings of the cassettes.
            4) Immediately before post-sampling weighing, inspect each filter for damage or any
               unusual appearance. This may include tears in the filter, unevenness of the loading
               pattern, pin holes, inappropriate sized particulate, and liquid droplets. Make a
               comment in both LIMS and in the blue book of any damage or unusual appearance.
               If large particles--such as insect body parts--are present, carefully remove and add a
               comment in LIMS and in the blue book. When damage appears to have originated in
               the field, include a description of the damage in the LIMS and bluebook but also ask
               the senior chemist to communicate the problem to the monitoring staff.
            5) After each filter is weighed, place it in a Petri dish onto which the corresponding ID
               label has been transferred.
            6) One filter from each set of 10 is set aside and reweighed as a lab duplicate or
               reweigh. See Section 14 for control limits and corrective actions.
            7) At the end of each weighing session, immediately transfer all post-weighed filters to
               the archiving refrigerator.


16. Calculations
   LIMS will perform the calculations based on the data from the monitoring staff and the inorganic
   staff. The equation is:
                                         1000(Mpost – Mpre)
                            C µg/m3 =    ------------------------
                                                  Va
       where
       Cµg/m3 = ambient particulate concentration in µg/m3
       Mpost = post-sampling filter weight in mg
       Mpre = pre-sampling filter weight in mg
       Va = sampled air volume in ambient m3

   If the sampling period is less than 1380 minutes, the concentration may need to be calculated as
   stated in Section 3.3 of Appendix L to Part 50:
    “ . . . However, when a sample period is less than 1,380 minutes, the measured concentration
   (as determined by the collected PM2.5 mass divided by the actual sampled air volume), multiplied
   by the actual number of minutes in the sample period and divided by 1,440 minutes may be used
   as if it were a valid concentration measurement for the specific purpose of determining a violation
   of the NAAQS....”
   To perform these calculations, both the field data and filter weights must be recorded in the
   appropriate database tables. The filter weights are captured directly from the balance as
   described in the Procedure section of this SOP. Recording the field data in the data base
   includes both importing data files from the samplers and hand entering information that is
   recorded on the field sheets. Both the monitoring staff and the lab staff are involved in populating
   the field data tables and in evaluating the validity of the results.
   The results are reported with “grades” that convey the validity of the results. Validation criteria
   are defined in a series of tables (see Appendix B: Criteria Tables for PM2.5 FRM Sampling.) The
   grades are as follows:
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           A = Valid (“A+” if valid results were generated by DEQ Laboratory)
           B = Estimate, with comments
           C = Invalid, with comments
           D = No sample, with comments
  The data reports also need to include any appropriate EPA flags that should be associated with
  the data in the AIRS (or AQS) system. Because we transfer only “A” data to EPA, only valid
  quality data needs to have EPA flags, when appropriate. These flags can be extracted from the
  descriptive comments associated with each results, but our best means of communicating these
  flags is to include in the analysis comment the statement: “EPA flags: xx, yy”. The following are
  some of the flags that we have used in the past:
           Y = Short sample still yielding violation of NAAQS.
           W = Sampling flow rate was off the set point by >5% for >5 minutes.
           X = The filter temperature during sampling was different than the ambient temperature by
           >5° C for >30 minutes.
           DST = For speciation samples, the shipping temperature was out of specifications
           (>4°C).
           E = Forest fires in the area impacted the results.
           6 = Data based on sampling or analysis prior to QAPP approval.
  Additional flags may be utilized as appropriate (see memo from R. Scheffe, on June 15, 2000).
  Besides the reports that organize the particulate matter results, several additional reports are
  generated to describe quality control information. For example, once a month the monitoring staff
  gives the lab staff a list of the previous month’s field blanks. The filter IDs are entered into
  AQLIMS, and a monthly field blank report is generated. The filter IDs of all lab blanks are also
  entered into AQLIMS, and a monthly lab blank report is generated.


17. Method Performance
  Based on the 2002 data, the average change (loaded weighing – tare weighing) in lab blanks’
  weights is +0.0002 mg, with a standard deviation of 0.0029 mg.
  Based on the 2002 data, the average change (loaded weighing – tare weighing) in field blanks’
  weights (Partisol samples only) is +0.0030 mg, with a standard deviation of 0.0039 mg.
  We have only participated in one round robin study for particulate matter gravimetric analysis. In
  that 1999 round robin study, several filters were weighed by 6 different laboratories. This
  involved repeatedly shipping filters between laboratories, and repeatedly weighing--at different
  laboratories--the same filters. This round robin study format created some biases due to the
  study process itself (i.e. the filters gained weight with time and continued handling.) Because of
  this bias, the round robin study may lead us to judge the method to be less precise than it actually
  is. Disregarding this limitation, one conclusion that can be drawn from the round robin report was
  that the “average” standard deviation of the results from all laboratories for any one filter is
  0.0046 mg. Oregon DEQ results were biased 0.0024mg per filter lower than the overall
  averages, with a standard deviation of bias equal to 0.0014 mg per filter. Therefore, Oregon DEQ
  results were well within the acceptable range, although the fact that Oregon DEQ received the
  filters in the middle of the study (4th out of 7) probably helped our apparent performance in the
  study.
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18. Maintenance
  1) Weekly cleaning of area and equipment:
           The balance chamber is cleaned weekly with a fine brush. In addition, the pan is cleaned
           whenever particles are visible or a sudden change in the instrument tare occurs.
           Staticmasters are cleaned every week at the same time as the balance chamber. They
           can be cleaned with a puff of canned, pressurized air.
           The tables, floor, and all dust-catching surfaces in the room are cleaned weekly with a
           moist towel. This should occur when the room will not be used for several hours (for
           example, on Friday afternoon.)
           Vacuuming the room should also be avoided, unless a HEPA filter vacuum is used.
  2) Preventative actions to reduce dust contamination of equipment and weighing area:
           To reduce dust contamination in the balance chamber, the door is kept closed except
           when the balance is in use.
           Inspect the HVAC filters (FARR 30) annually. Replace if they are heavily loaded. One
           filter is located behind the return air vent on the east wall of room, near the floor. The
           other is located under the refrigerant unit in the utility closet.
           Keep the room door closed, and limit the traffic into the room.
           Minimize the amount of paper, supplies, and equipment that are brought into the room
           (and keep work spaces uncluttered to make cleaning easier.) In general, sources of dust
           and fibers should not be brought into the weighing room unless necessary.
  3) Filter cassette cleaning:
           Filter cassettes and screens are cleaned when they are first purchased and subsequently
           after each use. (See “Section 7, Interferences” for a discussion of their initial cleaning.)
           The plastic rings of the cassettes are cleaned by washing them in a dishwasher at 60° C
           with a final rinse of RO water (all while in a mesh bag). Note: limit the number of rings
           per bag so that wash and rinse water reaches all rings in the batch.
           If the rings remain sticky (probably due to glue from the labels) after this cleaning, they
           can be cleaned with Scotch Brite scrubbers, Goo-Gone, or sharp scrapping tools. After
           this intensive cleaning, they need to be dishwasher washed again.
           The metal screens can easily capture fibers, so they are not exposed to fibrous material
           during cleaning or drying. They are placed in slide trays, soaked in hot water with a small
           amount of micro and then thoroughly rinsed with tap water followed by DI water.
           Rings should only be handled on outside edges (where they will not touch the filters) and
           the screens should only be handled with stainless steel forceps.
           After cleaning, the cassette parts are dried in the weighing room. Once dry, they should
           be stored in closed plastic boxes to keep them clean.
  4) Shipping container cleaning:
           After each use, remove all tape from the used shipping boxes, and clean them with a
           Kimwipe that is moistened with DI water. The cases should be kept closed as much as
           possible so that they remain clean. When the containers become cracked, heavily
           scratched, or have excessive tape on their surfaces, they should be discarded.
  5) Staticmaster strips replacement:
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         Staticmasters are replaced every six to nine months. The date of manufacture is
         stamped on each strip. ODEQ’s working expiration date for strips is 9 months to a year
         from the date of manufacture. Old strips are returned to the manufacturer.
6) Mass reference standards maintenance:
         The mass standards must be handled only with plastic forceps reserved for this purpose.
         The tips of the forceps are cleaned with alcohol and a lint-free wipe.
         The mass standards are stored in closed boxes. The working standards are kept next to
         the balance. The primary standards are stored in a dessicator cabinet.
         Primary mass standards are NVLAP certified once a year and the working standards are
         checked against the primary standards every three months (see Appendix A: Calibration
         of Working Mass Standards). The comparison consists of performing at least five
         weighing of each working and primary standard, with balance re-zeroing and recalibration
         between each set. If the standard deviation of any of the mass standards is greater than
         2µg, the weighings are repeated. The updated working weights for the working mass
         standards are then assigned based on these comparisons.
         The mass standard storage boxes are labeled with the date of the last certification (for
         primary standards) or calibration (for working standards).
7) Balance settings:
         Once the balance features are setup correctly, do not change the settings. The balance
         can be programmed to control a variety of features. Most features are set to the defaults
         except the following:
                 Allow handshaking with computer:           code 5-4-1
                 Print continuously on stability:           code 6-1-5
                 Very unstable conditions:                  code 1-1-4
                 Stability at 0.25 digits:                  code 1-3-1
                 Long delay:                                code 1-4-3
                 Auto-zero off:                             code 1-6-2
                 Auto-calibration off:                      code 1-15-1
         Any changes to these settings should be discussed with the senior chemist. Access to
         the balance programming is locked to prevent any accidental changes from occurring.
8) Dehumidifier maintenance:
         Two filters in the Munters HC300 dehumidifier require cleaning annually or more
         frequently if any dusting operations occur in the storeroom where it is installed. See the
         operation manual for the filter locations. Clean the filters in the dishwasher or by rinsing
         with water.
         The dehumidifier should have additional preventive maintenance performed annually, as
         described in the operation manual. The maintenance includes checking the desiccant
         wheel, checking the air seals, and checking the outlet air temperature (120°F). Note:
         Past experience has been that when an acrid smell develops in the room, it is likely due
         to the desiccant wheel no longer rotating. A burned out motor or worn lower gasket could
         cause the desiccant wheel to stop rotating.
9) Temperature and Relative Humidity sensors maintenance:
         To maintain a record of the room conditions, the chart paper on the Dickson unit is
         replaced weekly and the Humiscan data logger file is downloaded to the shared directory
         approximately 3 times a week.
         The temperature and relative humidity sensors are calibrated or verified once a year.
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19. Pollution Prevention
   There is no specific pollution prevention associated with this method.


20. Waste Management
   There is no specific waste management associated with this method.


21. References
       1) Manuals for:
             Cahn C44 Microbalance.
             DicksonTHDx Temperature and Humidity Recorder.
             General Eastern Humiscan Industrial Humidity Transmitter.
             Honeywell UDC 3300 Universal Digital Controller.
             Munters Dehumidifier Model HC-300-EA.
       2) US EPA (1997a) National Ambient Air Quality Standards for Particulate Matter-Final
          Rule; 40 CFR Part 50. Federal Register, 62(138):38651-38760; July 18, 1997.
       3) US EPA (1997b) Revised Requirements for Designation of Reference and Equivalent
          Methods for PM2.5 and Ambient Air Quality Surveillance for Particulate Matter-Final Rule;
          40 CFR Parts 53 & 58. Federal Register, 62(138):38763-38854; July 18, 1997.
       4) US EPA Memo, David Mobley, on 1/19/2000 regarding filter cassette transport. Note:
          There are typos on the last page include the equation D=34●Tave, which should be D=34-
          Tave. (See http://www.epa.gov/ttn/amtic/files/ambient/pm25/pm25caset.pdf )
       5) US EPA Memo, Richard D. Scheffe, on 6/15/2000regarding use of AIRS flags. (See
          http://www.epa.gov/ttn/amtic/files/ambient/pm25/datamang/regions.pdf )
       6) US EPA Memo, David Mobley, on 3/1/2002 regarding PM2.5 filter retrieval from
          samplers. (See http://www.epa.gov/ttn/amtic/files/ambient/pm25/filtere.pdf )
       7) US EPA Quality Assurance Guidance Document 2.12: Monitoring PM2.5 in Ambient Air;
          Using Designated Reference or Class I Equivalent Methods; March, 1998.
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Appendix A: Calibration of Working Mass Standards
    Scope and Application
    This method provides a procedure for calibrating working mass standards against primary
    mass standards to ensure that the working standards are assigned an accurate weight. This
    method is applicable to use on the Cahn C44 microbalance, located in the temperature and
    relative humidity room. The EPA Quality Assurance Handbook for PM2.5 suggests the
    recalibration of working mass standards every three to six months.
    Principle
    The calibration routine is completed using a double-substitution procedure in which a primary
    standard and the working standard are inter-compared to determine the average difference
    between the two weights. Errors that are introduced from internal calibration of the balance
    or in the balance indications are eliminated through the use of the balance alone as the
    source of mass comparison and by calibrating the balance over the range of use for the
    measurement. This procedure was developed from the Quality Assurance Guidance
    Document, Method Compendium PM2.5 Mass Weight Laboratory Standard Operating
    Procedures for the Performance Evaluation Program issued by the EPA in October 1998,
    which is turn was based on a version of SOP #4 in the NIST Handbook #145.
    Calibration weights
         Two primary mass standards (100 and 200 mg) are Troemner UltraClass weights that are
         NVLAP certified once a year:
            Nominal         Serial        Conventional Mass        Uncertainty       Tolerance
             Mass          Number               (mg)                 (mg)              (mg)
             200            16289             200.0021              0.0015            0.0050
             100            16290             100.0012              0.0017            0.0050

         The primary standards are stored in a closed desiccator, and are used only for calibrating
         the working standards or checking the accuracy of the balance.

         Working standards are used for routine filter weighing controls. These working standards
         are recalibrated against the primary standards on a three to six month schedule to
         identify any changes in weight due to regular handling. Below is a list of the working
         standards as of 02/03/99, but these are subject to change over time:
                       Standard Filter        Observed Mass          Standard Deviation
          Mass             Usage                  (mg)                     (mg)
          100B              FRM                  99.9793                  0.0008
           T2               FRM                 199.9762                  0.0004
           LE                MV                 199.9903                  0.0004
          200JE            None                 200.0140                  0.0006

         The working standards are stored adjacent to the balance for which they are primarily
         utilized.
         The mass standards are calibrated to the nearest microgram, therefore contamination of
         the weights and/or microbalance pan can affect the success of the calibration procedure.
         It is recommended that all potential sources of contamination be reduced or eliminated
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         prior to initiation of this procedure. Although the FRM room is designed to minimize
         sources of dust or other contamination, the analyst must utilize the utmost caution to
         minimize contamination of the standards or the microbalance. Oils from the skin will
         contaminate the standards if they were touched.
         If the standards are dropped, they should be cleaned with a brush and/or can-pressurized
         air, inspected under the stereoscope, and then recalibrated.
         The mass standards are always handled with the designated plastic or plastic tipped
         forceps. Metal forceps may scratch the mass standards.

    Procedure
    1) Preliminary procedure
         Prior to conducting the mass calibration, inspect the mass standards using a low power
         stereoscope, record any defects (scratches, contamination) and, if needed, clean the
         standards with a brush, canned air, alcohol, or lint-free wipe. Clean the working area
         around the balance. Place the primary and working standards in the controlled weighing
         room near the balance. Allow the standards to attain thermal equilibrium with the room
         (i.e. wait at least 2 hours).
         Perform a balance corner check:
                 A corner check is performed by placing a 5 gm working standard in the center of
                 the balance pan and taring the balance after a stable reading is obtained. The
                 mass is then placed at the approximate midpoint between the edge and center of
                 the balance pan (a “corner”), and the weight is recorded after a stable reading is
                 obtained. The mass is moved to the other three corners, and the weights are
                 recorded. If the weight at any corner is greater than ±7µg, the balance is in need
                 of service. Furthermore, the weights recorded at opposite corners should be
                 equal, but opposite in sign. If the weights at opposite corners of the pan are of
                 the same sign, this indicates that significant damage has occurred and
                 substantial repairs to the balance may be required. If the corner checks indicate
                 needed repairs, the senior particulate chemist is informed and further weighing is
                 suspended until corrective action is taken. Corner checks are recorded in a
                 laboratory blue book.
    2) Balance Calibration
         Prior to initiating the mass calibration sequence, open the draft shield on the balance.
         Close the draft shield and tare the balance after it has stabilized. Then, calibrate the
         balance using the internal calibrations function (F1 key on the control unit). When the
         balance has finished calibrating, it will beep and display the current tare weight. If the
         tare weight is not 0.000 mg, tare the balance.
         The balance should be exercised prior to starting the mass calibration routine. Exercising
         involves completing a weighing series and verifying that the balance is operating
         properly. To exercise the balance, weigh each of the six mass standards in succession
         by opening the draft shield, placing the mass on the pan, and closing the draft shield.
         The weights should be placed in the weighing chamber using the standard non-metallic
         forceps. Place weights in the center of the pan. Record the observed mass after
         stabilization and verify that the balance stabilizes within approximately 20 seconds. The
         stabilization time for the mass standards is significantly less than that of the filters. The
         balance reading typically does not change after displaying “mg”. Following the weighing
         of the last mass, record the balance tare. If the tare has drifted more than ± 0.001 mg,
         recalibrate the balance, reweigh the sequence, and verify the drift. If the drift is still
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           greater than ± 0.001 mg, troubleshoot the balance. If the balance seems unsteady after
           the “balance exercising”, the mass standards calibration should be postponed until
           another day.
    3) Mass Calibration Routine
           Tare and calibrate the balance. Weigh each of the masses in succession starting with
           the first mass and ending with the sixth mass in the sequence. Record each result in the
           blue book after the balance has stabilized. At the end of the sequence, check and
           record the balance tare. Zero the balance (even if the tare value is 0.000 mg), and
           calibrate the balance using the internal calibration routine (F1 on the control unit). After
           calibration, begin the second set of weighings in succession, starting with the sixth mass
           and ending with the first mass. After the completion of the second weighing, check the
           tare, zero the balance, and recalibrate. Continue this process until each mass has been
           weighed six times. The first mass weighed in each set should be incremented so that
           any instrument drift is normalized over the six sets of weighings. Check the results of the
           mass calibrations (see “calculations” below). If the calibration has been successfully
           completed, return the standards to their proper locations.
    4) Calculations
           Transfer the calibration data from the laboratory blue book into an Excel worksheet.
           Calculate the mean and standard deviation for each of the weights. If the average test
           results for the primary mass standards do not indicate acceptable agreement (± 5µg) of
           the certified value, perform the following checks: repeat the process, check the primary
           standards for visible signs of contamination or damage, clean the balance pan, and
           externally calibrate using a 5g mass standard. If agreement is still not achieved, have the
           primary standards checked against an independent, certified weight of the same or
           greater confidence level of accuracy. If agreement is still not achieved, a technician
           should service the balance and the mass calibration should be repeated. For working
           mass standards, the assigned “true mass” equals the average mass of the six
           determinations. See the example of a calibration data worksheet below:
                     100       200                    200          200                                Weighing    Starting
      Rep           16290     16289     100 100B       T2          LE       200 200JE    Tare Drift   Direction    Mass
       1           100.001   199.999     99.967     199.961      199.992     200.016       0.001          →        16290
       2           100.000   199.998     99.966     199.959      199.991     200.014       -0.001         →        16289
       3           100.002   200.001     99.967     199.961      199.993     200.017       0.002          →        100B
       4           100.000   199.999     99.968     199.959      199.991     200.015       0.002          →         T2
       5           100.001   199.999     99.967     199.960      199.992     200.016       0.001          →         LE
       6           100.000   199.999     99.967     199.959      199.993     200.014       0.000          →        200JE
   Average        100.0007   199.9992   99.9670     199.9598    199.9920     200.0153      0.0008
    Std Dev        0.0008     0.0010     0.0006      0.0010      0.0009       0.0012       0.0012
 Assigned                               99.967 199.960 199.992 200.015
   Cert. Mass     100.0012   200.0021
  Uncertainty      0.0017     0.0015
   Difference      -0.0005    -0.0029
Department of Environmental Quality
Gravimetric Analysis of Particulate Collected with R&P Partisol Samplers and MetOne SASS
Samplers                                                                 Date: June 27, 2003
Revision: 2.0                                                                                                                                                                                                                            Page 23 of 25



Appendix B: Criteria Tables for PM2.5 FRM Sampling
                    Critical Criteria must be met for result to be valid (unless there are compelling reasons and justification to not do so)
             Criteria                  Instrument              EPA                         Range                    Internal   EPA Current Documentation                Checked          Current                   Future       Comment if results are qualified
                                          Flags                Table          (and frequency if not every sample)    Class     class                                      By             Tracking                 Tracking
Filter Holding Times (see Operational table for pre-sampling holding time criteria)
  Sample recovery time from                 N/A                critical                  <= 4 days                    A         valid filter check-in log , FRM data  AQM         AQM, to LAB, to LIMS, AQM to LIMS to          Sample recovered >96 hours
   sampler after sampling                                                                                                              record, field sheets                       to report             LASAR
                                                                                   >4 days, <= 8 days                 B        invalid
                                                                                        > 8 days                      C        invalid
      Filter holding times:                 N/A                critical     (<= 10 days and T <=25º C) or             A         valid Post-sampling holding time     AQM and      Time tracked by         Time: LIMS to LASAR   Post-sampling holding time or
          post-sampling                                                        (<= 30 days and T <=4º C)                               is documented in LIMS. Post-    LAB        database outside LIMS,                        temperature exceeded
                                                                           Additional guidance: For samples                            sampling temperature is                    to report. Temperature                               OR
                                                                            not weighed within 10 days, the                            documented on thermograph                  tracked by AQM, to                            Post-sampling holding time or
                                                                           temperature is maintained below                             charts and field sheets.                   LAB, to LIMS, to report                       temperature exceeded, but sample not
                                                                              25C and the filter is weighed                                                                                                                     invalidated
                                                                           before a deadline (days) equal to:
                                                                             34 minus ( estimated average
                                                                           temperature since removed from
                                                                                       sampler).

                                                                                 Not within above limits.              B       invalid                                                                   Temperature: AQM to
                                                                                                                                                                                                         LIMS to LASAR


Sampling period
   Sampling period duration          P - sequential            critical            1380 -1500 minutes                  A       valid     FRM data record, field sheet    AQM      Instrument, to AQM, to Instrument to LIMS to Sampling duration > 25 hours
                                      E - manual                           (Note: if sampling period is <1380                                                                     LAB, to report         LASAR                       OR
                                                                              minutes and the concentration                                                                                                                    Sampling duration < 23 hours
                                                                           calculated based on 1440 minutes                                                                                                                          OR
                                                                           is a violation of the daily standard,                                                                                                               Sampling duration < 23 hours but still
                                                                             then this sample is valid for the                                                                                                                 a NAAQS violation (required AIRS
                                                                           purpose of determining a violation                                                                                                                  flag)
                                                                                      of the NAAQS)

                                                                                1080 - 1379 minutes                    B       invalid
                                                                               or 1501 - 1800 minutes
                                                                           sample period < 18 hours or > 30            C       invalid
                                                                                        hours
           Start Time                        no               critical?           Midnight ± 1 hour                    A        valid                                                                                           Start time not at midnight ±1 hour
                                                                                 Midnight ± 12 hour                    B       invalid
Sampling Instrument (see Operational table for additional non-critical sampler criteria)
      Average Flow Rate                      no                critical       avg within 5% of 16.67 lpm               A       valid     FRM data record, field sheet    AQM      Instrument, to AQM, to Instrument to LIMS to Average flow not 16.67 lpm ± 5%
                                                                                  (15.84 to 17.50 lpm)                                                                            LAB, to report         LASAR
                                                                           avg differs from 16.67 lpm by 5%            B       invalid
                                                                                         to 20%.
                                                                             avg differs from 16.67 lpm by             C       invalid
                                                                                   greater than 20%
         Flow Variability            O - sequential            critical                CV <= 2%                        A       valid     FRM data record, field sheet    AQM      Instrument, to AQM, to Instrument to LIMS to Flow variability CV >2%
                                      C - manual                                                                                                                                  LAB, to report         LASAR
                                                                                      2% < CV <=4%                     B       invalid
                                     note :instrument will                              CV >4%                         C       invalid
                                    stop sampling if flow
                                       varies by > 10%
                                      from 16.67 for > 1
                                     min, as indicated by
                                    flags: S - Seq and X -
                                             Man


Filter
     Filter Defect or Damage                N/A                critical                  no defects                    A       valid     Post weighing lab book and     AQM and   AQM, to LAB, to LIMS, AQM or LAB to LIMS      Filter damaged
(visible any time after sampling)                                                                                                        field sheet                      LAB     to report             to LASAR

                                                                              defect or damage judged to               B       invalid
                                                                               affect loading by <= 5%.
                                                                              defect or damage judged to               C       invalid
                                                                               affect loading by > 10%.
      Filter Conditioning                   N/A                critical                 >=24 hrs                       A        valid Weighing log books and             LAB      LAB, to LIMS, to report LIMS to LASAR         Filter not conditioned properly
   (Pre and Post Sampling)                                                                                                             control room log book
                                                                                <24 hours and > 2 hours                B       invalid
                                                                                       < 2 hours                       C       invalid
      Filter Conditioning:                  N/A                critical      20º C <=(24 hr mean)<= 23º C              A        valid Weighing log books, control        LAB      LAB, to LIMS, to report LIMS to LASAR         Filter not conditioned properly
     Temperature Range                                                                                                                 room log book, chart
   (Pre and Post Sampling)                                                                                                             recorder output
                                                                                  24 hr mean >23º C                    B       invalid
                                                                               and <=25º C, or < 20º C
                                                                                  24 hr mean >25º C                    C       invalid
                                                                                 (Post sampling only)
      Filter Conditioning:                  N/A                critical       SD is <= ± 2º C over 24 hr               A       valid     Weighing log books, control     LAB      LAB, to LIMS, to report LIMS to LASAR         Filter not conditioned properly
     Temperature Control                                                                                                                 room log book, chart
   (Pre and Post Sampling)                                                                                                               recorder output
                                                                             SD is > ± 2º C and <= ± 4º C              B       invalid
                                                                                       over 24 hr
                                                                              SD is > ± 4º C over 24 hr                C       invalid
      Filter Conditioning:                  N/A                critical     24 hr mean prior to weighing is            A        valid Weighing log books, control        LAB      LAB, to LIMS, to report LIMS to report        Filter not conditioned properly
       Humidity Range                                                                   30-40%                                         room log book, chart
   (Pre and Post Sampling)                                                  Note: humidity can be between                              recorder output
                                                                             20% and 30% if <= ± 5% of
                                                                                     sampling RH.
                                                                                   < 30 % or >40 %                     B       invalid
                                                                                     <1% or >80%                       C       invalid
      Filter Conditioning:                  N/A                critical       SD over 24 hr is <= +/- 5%               A        valid Weighing log books, control        LAB      LAB, to LIMS, to report LIMS to LASAR         Filter not conditioned properly
       Humidity Control                                                                                                                room log book, chart
   (Pre and Post Sampling)                                                                                                             recorder output
                                                                                   SD over 24 hours is                 B       invalid
                                                                                     > 5% and <20%
                                                                                   SD over 24 hours is                 C       invalid
                                                                                          >20%
      Filter Conditioning:                  N/A                critical       difference in 24 hr means is:            A       valid     Weighing log books, control     LAB      LAB, to LIMS, to report LIMS to LASAR         Filter not conditioned properly
 Humidity Control Comparison                                                            <= ± 5%                                          room log book, chart
  of Pre and Post Sampling                                                                                                               recorder output
           Conditions
                                                                              difference in 24 hr means is:            B       invalid
                                                                                  > ± 5% and <= ± 20%
                                                                              difference in 24 hr means is:            C       invalid
                                                                                           > ± 20%
         Balance location                   N/A                critical         in filter conditioning room            A       valid     Balance maintenance             LAB      comment in LIMS        same                   Balance not in conditioning room
                                                                                                                                         logbook
                                                                             not in filter conditioning room           B       invalid
Calibration/Verification (see Operational table for additional calibration/verification criteria)
   Flow Rate Verification of                NA               operational       <= ± 4% of audit standard               A       valid     Monthly audit sheets            AQM      Internal review of audit same                 Flow rate verification failed
          Sampler                                                                      1/month                                                                                    sheets
                                                                           > 4% but <= 10% of audit standard           B       invalid

                                                                                 >10% of audit standard                C       invalid
Department of Environmental Quality
Gravimetric Analysis of Particulate Collected with R&P Partisol Samplers and MetOne SASS
Samplers                                                                 Date: June 27, 2003
Revision: 2.0                                                                                                                                                                                                          Page 24 of 25

                                                    Operational criteria are used to maintain and evaluate the quality of the results.
                                             Operational criteria would only downgrade results if the criteria (or multiple criteria) indicates >10% (3 ug/M3 minimum) error for "B" class,
                                                                                             or >20% (6ug/M3 minimum ) error for "C".
                                                                              Both "B" and "C" classed samples are invalid for EPA reporting purposes.

            Criteria                Instrument        EPA                         Range                    Currrent Documentation        Checked               Current                    Future         Comment if data is qualified
                                       Flags          Table          (and frequency if not every sample)                                   By                  Tracking                  Tracking
Precision
Precision: Collocated Samples           NA          operational   CV <=10% for samples > 6 ug/m3 Duplicate site sampler                  AQM and       Lab review during          LASAR report?          Primary versus duplicate results CV >10%
                                                                   checked at 25% of sites every 6 comparison report,                      LAB         report validation                                 for >6 ug/m3 samples: verified
                                                                                days               generated monthly

Accuracy
 Sampler Temperature Audit             NA           operational                <= ±2º C                    QA section documentation         QA         QA to AQM                  LASAR report?          NA
   (filter T and ambient T)                                            checked each sampler
                                                                           4 times per year
   Sampler Pressure Audit              NA           operational            <= ±10 mm Hg                    QA section documentation         QA         QA to AQM                  LASAR report?          NA
                                                                       checked each sampler
                                                                           4 times per year
   Sampler Flow Rate Audit             NA           operational       <= ± 4% of audit standard            QA section documentation         QA         QA to AQM                  LASAR report?          NA
                                                                     <= ± 5% of design flow rate
                                                                                4/year
        Balance Audit                  NA           operational      manufacture's specifications          Yearly balance                 Contracted   Label on balance and       same                   NA
                                                                           1 time per year                 maintenance/service           Maintenance   notice from service
                                                                                                                                           Service
                                                                                                                                                       company
Calibration and Check Standards
 Audit Thermometer (QA and             NA           operational       ± 0.1º C resolution, ± 0.5º C        Manufacturer specs,          AQM and QA To be developed                To be developed        NA
           AQM)                                                                 accuracy,                  comparison to traceable
                                                                     check once per month (AQM)            thermometer
  Audit Barometer (QA and              NA           operational          ± 1 mm Hg resolution,             Manufacturer specs,          AQM and QA To be developed                To be developed        NA
           AQM)                                                           ± 5 mm Hg accuracy,              comparison to traceable
                                                                     check once per month (AQM)            barometer
 Audit Orifice (QA and AQM)                         systematic           ± 0.08 Lpm resolution,            Manufacturer specs,          AQM and QA To be developed                To be developed        NA
                                                                           ± ?? Lpm accuracy,              comparison to traceable flow
                                                                     calibrated to primary standard        measurement device
                                                                         every 6 months (AQM)
  Working Mass standards -             NA           operational     ± 0.025 mg from nominal value          Weighing log book                Lab        Label on mass              Label on mass          NA
           Check                                                           checked 1/3 month                                                           standard containers        standard containers
Monitor Maintenance
Sampler Impactor Maintenance           NA           operational           cleaned/changed                  Field sheets                    AQM         Check-in log book          Same                   Sampler impactor was not maintained
                                                                       every 5 sampling events
   Sampler Inlet/downtube              NA           operational           cleaned, monthly                 Monthly audit sheets            AQM         Internal review of audit   same                   NA
         Cleaning                                                                                                                                      sheets
   Sampler filter chamber              NA           operational             cleaned, monthly               Monthly audit sheets            AQM         Internal review of audit   same                   NA
         Cleaning                                                                                                                                      sheets
 Sampler Fan Filter Cleaning           NA           operational       cleaned/changed, monthly             Monthly audit sheets            AQM         Internal review of audit   same                   NA
                                                                                                                                                       sheets
Sampler: Other Manufacturer            NA           operational           Manufacturer's SOP               Monthly audit sheets            AQM         Internal review of audit   same                   NA
  Recommended Cleaning                                                                                                                                 sheets
Filter Checks
        Lot Filter Blank               NA           operational      <= ±15 ug change between        Weighing log book                      Lab        Prior to use of any lot    Results of LOT blank   NA
                                                                  weighings at least 24 hours apart;                                                                              in LIMS?
                                                                              3 per lot

  Unexposed Filter Defects             NA           operational   Pin holes, support ring separation, Log of filter examination             Lab        Do not use defective      same                    NA
                                                                  unevenness, contaminant material;                                                    filters. Report to EPA if
                                                                    all filters examine prior to pre-                                                  number of defects
                                                                          sampling conditioning                                                        seem excessive.

 Filter Integrity or appearance        NA           operational    Any unusual appearance of filter Field sheets and weighing            AQM and       Recorded in log book Recorded on paper            Unusual filter loading appearance
          after exposure                                          after sampling which do not affect log book                              LAB         or field sheet,        work, transferred to
                                                                  mass (see "critical" filter defect or                                                transferred to LIMS,   LIMS, easily include
                                                                        damage criteria above)                                                         comment used in report comment in report

Filter Holding Times (see Critical table for additional filter holding times criteria)
 Pre-sampling holding times            NA           operational     <30 days between pre-sample            LIMS                             Lab        LIMS and AQM to          LIMS and AQM to          Presampling filter holding time > 30 days
                                                                    weighing and use in sampling                                                       separate report to final LASAR
                                                                                                                                                       report
Lab QC Checks
       Lab Filter Blank                NA           operational           <= ±15 ug change,         Lab report                              Lab        Quarterly report from      LIMS report            Weighing QC results not within control
                                                                  at least one per weighing session                                                    separate database                                 limits

        Balance Check                  NA           operational   <= 3 ug; beginning, end, and every Weighing log book                      Lab        Weighing not continued Weighing not               Weighing QC results not within control
                                                                              10th filter                                                              if unacceptable        continued if not           limits
                                                                                                                                                                              acceptable, notify by
                                                                                                                                                                              LIMS if attempt is
                                                                                                                                                                              made to continue
                                                                                                                                                                              weighing
   Duplicate Filter Weighing           NA           operational   <= ±15ug per filter (or established Weighing log book                     Lab        Quarterly report from  LIMS report                Weighing QC results not within control
                                                                      historical 2xSD, if better);                                                     separate database                                 limits
                                                                   duplicate weighings performed on
                                                                  10% of filters at both pre and post
                                                                    weighings sessions, reweighed
                                                                               same day

Sampling Instrument (see Critical table for additional sampler excursion criteria)
   Sampling Flow Rate:            F - seq. & man.   operational   No excursions > ± 5% for > 5 min FRM data record, field sheet            AQM         AQM to LAB to report       LIMS to LASAR          Sampling flow rate off set point by > ±5%
    5 minute intervals                                                                                                                                                                                   for > 5 minutes--Required EPA flag
 Sampler Filter Temperature       R - Sequential    operational      No excursions >5º C for >30           FRM data record                 AQM         Instrument flag           Download from           Sampler filter temperature excursion >5º C
          Sensor                   T - Manual                                 minutes                                                                  investigated , results to instrument to LIMS,     for >30 minutes--Required EPA flag
                                                                                                                                                       Lab, to LIMS, to report investigate and
                                                                                                                                                                                 confirm, modify LIMS
Calibration/Verification (see Critical table for flow rate verification criteria)
     External Leak check               NA           operational             <80 ml/min            Field sheets, audit sheets,              AQM         Check-in log book          Same                   Sampler failed leak test
                                                                  checked every 5 sampling events sampler log book

      Internal leak check              NA           operational              <80 ml/min                    Field sheets, audit sheets,     AQM         Check-in log book          Same                   Sampler failed leak test
                                                                    Only performed if fails external       sampler log book
                                                                              leak check
  Temperature calibration of           NA           operational                <= ± 2º C                   Calibration sheet               AQM         Sticker on instrument      Same                   NA
         sampler                                                       on installation, then 1/yr                                                      and Maintenance
                                                                                                                                                       schedule spreadsheet
One point Temperature check            NA           operational               <= ± 4º C                    Audit sheet, sampler log        AQM         Internal review of audit   same                   Sampler failed temperature verification
          of sampler                                                          1/4 weeks                    book                                        sheets
Pressure calibration of sampler        NA           operational            <= ± 10 mm Hg                   Calibration sheet               AQM         Sticker on instrument      Same                   NA
                                                                       on installation, then 1/yr                                                      and Maintenance
                                                                                                                                                       schedule spreadsheet
   Pressure verification of            NA           operational            <= ± 10 mm Hg                   Audit sheet, sampler log        AQM         Internal review of audit   same                   Sampler failed pressure verification
          sampler                                                             1/4 weeks                    book                                        sheets
   Flow Rate calibration of            NA           operational                <= ± 2%                     Calibration sheet               AQM         Sticker on instrument      Same                   NA
          sampler                                                      on installation, then 1/yr                                                      and Maintenance
                                                                                                                                                       schedule spreadsheet
   Clock/Timer Verification            NA           systematic             1 min/month,                    Audit sheets                    AQM         To be developed            same                   Sampler failed clock/timer verification
                                                                     checked once per 4 weeks
   Microbalance calibration            NA           operational    per manufacture's specification         Service records                  Lab        Label on balance           Same                   NA
                                                                               1/yr
 Lab temperature verification          NA           operational              <= ± 2º C                     Control room lab book            Lab        Label on room temp         Same                   NA
                                                                            1/6 month                                                                  display
   Lab humidity verification           NA           operational              <= ± 2%                       Control room lab book            Lab        Label on room temp         Same                   NA
                                                                            1/6 month                                                                  display
Department of Environmental Quality
Gravimetric Analysis of Particulate Collected with R&P Partisol Samplers and MetOne SASS
Samplers                                                                 Date: June 27, 2003
Revision: 2.0                                                                                                                                                                                            Page 25 of 25

                         Systematic Criteria may affect interpretation of the results but do not usually impact the validity of the results.
                                           Systematic criteria would only downgrade results if the criteria indicates >10% (3 ug/M3 minimum) error for "B" class,
                                                     or >20% (6ug/M3 minimum ) error for "C" class. Both "B" and "C" samples are invalid for EPA reporting purposes

           Criteria              Instrument     EPA                          Range                    Documented                     Checked          Current                 Future        Comment if results are qualified
                                    Flags       Table           (and frequency if not every sample)                                    By             Tracking               Tracking
Data Reporting Criteria
     Data Completeness              NA        systematic         >= 75% of quarterly data             Reports, comparison to         Lab/HQ    HQ reports             LIMS/LASAR reports    NA
                                                                       from each site                 scheduled sampling
       Reporting Units              NA        systematic      ug/m3 at ambient temp/pressure          Reports                        Lab/HQ    Lab review of           Manual calculation of NA
                                                                                                                                               calculations, HQ review different (rotating
                                                                                                                                               of reported results     monthly) sites results,
                                                                                                                                                                       at a frequency of 2 per
                                                                                                                                                                       site at 2 sites per
                                                                                                                                                                       month.

Results Rounding - annual 3 yr      NA        systematic              nearest 0.1 ug/m3               Reports submitted to EPA         HQ      HQ methods             LIMS/LASAR should     NA
                                                                    (>= 0.05 rounded up)                                                                              generate similar
                                                                                                                                                                      reports
Results Rounding - 24 hr, 3 yr      NA        systematic               nearest 1 ug/m3                Reports submitted to EPA         HQ      HQ methods             LIMS/LASAR should     NA
                                                                     (>= 0.5 rounded up)                                                                              generate similar
                                                                                                                                                                      reports
Reporting Limits
PM2.5 Detection Limit: Lower        NA        systematic                  <= 2 ug/M3                  standard deviation of field      Lab     To be developed        To be developed       NA
                                                                                                      blanks <(24 x 2) ug, (I.e.,
                                                                                                      <48ug per filter ?
PM2.5 Detection Limit: Upper        NA        systematic                 >=200 ug/M3                  Sampling downgraded due to     AQM and   To be developed        To be developed       NA
                                                                                                      effects of high loading          LAB
Primary Standards Recertifications
 Flow Rate Primary Standard         NA        systematic     ± 2% of NIST-traceable standard,      Certification documents            AQM      Documents posted with same                   NA
                                                               recertified once every 2 years                                                  instrument
     Primary Reference              NA        systematic   ± 0.1º C resolution, ± 0.5º C accuracy, Certification documents            AQM      Documentation on file same                   NA
        Thermometer                                        ASTM certified Hg in glass, permament
                                                                         certification

Primary Reference Barometer         NA        systematic            ± 1 mm Hg resolution,             Certification documents         AQM      To be developed        same                  NA
                                                                    ± 5 mm Hg accuracy,
                                                                 ?frequency of certification?
     Primary Mass Stds              NA        systematic       ± 0.025 mg from nominal value          NVLAP certification              Lab     Label on mass          Label on mass         NA
                                                                                                      documents, lab book                      standard containers    standard containers
Microbalance
  Microbalance Readability          NA        systematic                  1 ug,                       Manufacturer specs               Lab     LIMS records balance   LIMS records balance NA
                                                               checked at balance purchase                                                     used for weighing      used for weighing

 Microbalance Repeatability         NA        systematic 1 ug, checked at annual maintenance Yearly balance check/service              Lab     Label placed on        Label placed on       NA
                                                                                                                                               balance                balance
Precision (determined by an independent organization? QA or EPA?)
 Single Analyzer Precision ?        NA        systematic                  CV <= 10%                   Report generated by EPA?        EPA?     EPA reports?           EPA reports?          NA
                                                                          1/3 month
 Single Analyzer Precision ?        NA        systematic                  CV <= 10%                   Report generated by EPA?        EPA?     EPA reports?           EPA reports?          NA
                                                                            1/year
   Reporting Organization           NA        systematic                  CV <= 10%                   Report generated by EPA?        EPA?     EPA reports?           EPA reports?          NA
        Precision ?                                                       1/3 month
Bias (determined by an independent organization? QA or EPA?)
 FRM Performance Evalution          NA        systematic                 ±10%,                        EPA report/QA section report   EPA/QA    EPA report             QA section report     NA
                                                              checked at 25% of sites 4/year          compared to LIMS report                                         included in
                                                            (AQM and Lab not directly involved)                                                                       LIMS/LASAR