# CHESTER LabNet

12242 SW Garden Place Tigard, OR 97223-8246 USA Telephone 503-624-2183 Fax 503-624-2653 www.chesterlab.net



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Gravimetry (PM10

### )

Gravimetry is accomplished following the PM2.5

### protocols at 40 CFR 50, Appendix L and Section 2.12 of the EPA Quality Assurance Handbook for Air Pollution Measurement Systems. The PM10

### method, 40 CFR 50 appendix J, only refers tohigh volume samples, so the laboratory uses the procedures and more stringent QC in appendix L. Chester LabNet operates two microbalances capable of measuring mass to onemicrogram. The balances are under computer control, and all weighing operations follow a strict QC program. All f ilters are allowed to stabilize for two to three weeks, inspected and equilibrated for at least 24 hours in the controlled temperature and humidity weighroom before weighing. Briefly, the filters are tare weighed in batches of ten or less filters with calibration and zero checks before and after every batch. All tare-weighed filters are equilibrated for a minimum of another 20 hours, and 10% are reweighed to demonstrate constant weight. The 10% reweight procedure is also followed for the gross weighing of exposed filters returned from the field. Gravimetry data are batch imported from the balance computer directly into the LIMS. Filtersare loaded into cassettes in a laminar flow hood to prevent contamination.

Balance QC statistics and calibration and gravimetry QC checks are as follows:

QC Element Frequency QC Criterion balance resolution -- 1 μg balance precision -- ± 1 μg balance calibration Daily -- balance zero 10% -- calibration verification 10% ± 3 μg 24-hour tare reweigh 10% ± 10 μg 24-hour gross reweigh 10% ± 10 μg



### Currently, all filters for the project are weighed on a Sartorius model ME5 microbalance. That balance is calibrated daily using the internal calibration. The calibration is checked before and after each set of ten f ilters or less using a 200 mg weight, serial number 2008014, and a 100 mg weight, serial number 5316. The calibration is alsochecked monthly with a separate set of 200 mg and 100 mg weights, serial number 21386. The calibration certificates for the balances and the weights are attached.

### XRF (metals including Pb)

At Chester LabNet, XRF is accomplished following U.S. EPA Method IO-3.3 in Compendium of Methods for the determination of Inorganic Compounds in Ambient Air (EPA 625/R-96/010a) as modified for use with a Kevex Model 770 spectrometer. Calibration is via commercial, single-element, thin-film, vapor-deposited standards (from MicroMatter, Inc.) and organometallic acetate film standards containing two or more non-interfering elements (from U.S. EPA). Because of the extreme stability of XRF instruments, initial calibration may hold for many months. Calibration verification is accomplished by the analysis of NIST thin film standards SRM 1832 and SRM 1833 for eleven representative elements. The certificates of analysis for the NIST SRMs are attached. Precision is checked by the analysis of six elements on a quality control standard filter and by analysis of a sample replicate. Several elements, including S, K, Ca, Fe, Cu, and Zn are measured under more than one of the several excitation conditions normally used for each sample filter.

The QC elements for the analysis of elements by x-ray fluorescence, their frequency of application and control limits, and corrective actions are as follows:

QC Element Frequency Control Limits Corrective Action calibration as needed -- -- calibration verification weekly within NIST uncertainties recalibrate

instrument precision once per batch of < 15 90 – 110% recovery batch reanalysis

Inter-excitation condition check every sample within analysis uncertainty determine cause - remedy sample replicate precision 10% within analysis uncertainty determine cause - remedy

Also, Chester LabNet (operating then as NEA, Inc.) developed an equivalent method for the determination of lead in ambient air particulates by XRF in 1989. This was before IO-3.3 was published. The acceptance letter for the equivalent method is attached, as well.

# Gravimetric Calibration Certificates

# X-Ray Fluorescence NIST Certificates of Analysis

# X-Ray Fluorescence Equivalent Method DocumentationList ofDesignated Reference and Equivalent Methods, April 8, 2004 Page 20

42-006 Pressure transducer (Model 42 only) 42-007 Ozone particulate filter 42-008 RS-232/485 interface 42-009 Permeation dryer [Federal Register: Vol. 54, page 50820, 12/11/89] Thermo Electron/Thermo Environmental Instruments Model 14 BIE AutomatedReference Method: RFNA-0179-035

"Thermo Electron or Thermo Environmental Instruments, Inc. Model 14 B/E Chemiluminescent NOINOiNO
x Analyzer," operated on the 0-0.5 ppm range, with or without any ofthe following options:

14-001 Teflon Particulate Filter 14-003 Long-Time Signal Integrator 14-005 Sample Flowmeter 14-002 Voltage Divider Card 14-004 Indicating Temperature Controller 14-006 Air Filter [Federal Register: Vol. 44, page 7805, 02/07/79 and Vol.44, page 54545, 09/20/79]

Thermo Electron/Thermo Environmental Instruments Model 14 DIE AutomatedReference Method: RFNA-0279-037

"Thermo Electron or Thermo Environmental Instruments, Inc. Model 14 D/E Chemiluminescent NOIN02 1N0
x Analyzer," operated on the 0-0.5 ppm range, with or without any ofthe following options: 14-001 Teflon Particulate Filter; 14-002 Voltage Divider Card. [Federal Register: Vol. 44, page 10429,02/20/79]

Thermo Environmental Instruments Models 42, 42C NO/N0z/NO
x Analyzer AutomatedReference Method: RFNA-1289-074

"Thermo Environmental Instruments Inc. Model 42 or Model 42C NO-N02-NO
x Analyzer," operated on any measurement range between 0-50 ppb 1 and 0-1000 ppb, with any time average setting from 10 to 300 seconds, with temperature and/or pressure compensation on or off, operated at temperatures between 15 DC and 35 DC, with or without an exhaust ozone scrubber or any ofthe following options: 2

42-002 Rack mounts 42-003 Internal Zero/span and sample valves with remote activation 42-004 Sample/ozone flow meters (Model 42 only) 42-005 4-20 rnA current output

Reference Method for Lead Manual Reference Method: 40 CFR Part 50, Appendix G

Reference Method for the Determination ofLead in Suspended Particulate Matter Collected from Ambient Air. [Federal Register: Vol. 43, page 46258, 10/05/78]

Energy-Dispersive X-Ray Fluorescence Spectrometry (TNRCC) Manual Equivalent Method: EQL-0783-058

"Determination ofLead Concentration in Ambient Particulate Matter by Energy-Dispersive X-Ray Fluorescence Spectrometry (Texas Natural Resource Conservation Commission)" Texas Natural Resource Conservation Commission, P.O. Box 13087, Austin, TX 78711- 3087. [Federal Register: Vol. 48, page 29742,06/28/83]

Energy-Dispersive X-Ray Fluorescence Spectrometry (NEA, Inc.) Manual Equivalent Method: EQL-0589-072

"Determination ofLead Concentration in Ambient Particulate Matter by Energy-Dispersive X-Ray Fluorescence Spectrometry (NEA, Inc.)" Nuclear Environmental Analysis, Inc., Suite 260, 10950 SW 5th Street, Beaverton, OR 97005. [Federal Register: Vol. 54, page 20193,05/10/89]

Flame Atomic Absorption Spectrometry Manual Equivalent Method: EQL-0380-043

"Determination ofLead Concentration in Ambient Particulate Matter by Flame Atomic Absorption Spectrometry Following Ultrasonic Extraction with Heated HN03-HCl" Federal Register: Vol. 45, page 14648,03/06/80]

Flameless Atomic Absorption Spectrometry (EPA/RTP, N.C.) Manual Equivalent Method: EQL-0380-044

"Determination of Lead Concentration in Ambient Particulate Matterby Flameless Atomic Absorption Spectrometry (EPA/RTP, N.C.)" [Federal Register: Vol. 45, page 14648,03/06/80]

Flameless (Graphite Furnace) Atomic Absorption (Houston, Texas) Manual Equivalent Method: EQL-0895-107

"Determination ofLead Concentration in Ambient Particulate Matter by Flameless (Graphite Furnace) Atomic Absorption (City of Houston, Texas)." Health and Human Services Department, Environmental Chemistry Service, 1115 S. Braeswood, Houston, TX 77030. [Federal Register: Vol. 60, page 39383, 08/02/95]

Flameless Atomic Absorption Spectrometry (Omaha) Manual Equivalent Method: EQL-0785-059

"Determination ofLead Concentration in Ambient Particulate Matter by Flameless Atomic Absorption Spectrometry (Omaha-Douglas County Health Department)" Omaha-Douglas County Health Department, 1819 Farnam Street, Omaha, NE 68183. [Federal Register: Vol. 50, page 37909, 09/18/85]

### UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
ATMOSPHERIC RESEARCH AND EXPOSURE ASSESSMENT LABORATORY RESEARCH TRIANGLE PARK

NORTH CAROLINA 27711 

### May 10, 1989

Ms. lisa M. Caldwell NEA, Inc. Su ite 260 10950 S. W. 5th Street Beaverton, Oregon 97005

Re: Request for Equivalent Method Determination

Dear Ms. Caldwell:

Pursuant to Section 53.8 of Title 40, Chapter I, Part 53 of the Code of Federal Regulations (40 CFR 53.8), you are hereby notified that your X-ray Fluorescence Spectrometry method for the determination of lead concentration in suspended particulate matter collected from ambient air has been designated as an equivalent method by the Administrator of the Environmental Protection Agency in accordance with Part 53. The method is identified as: EQl-0589-072, "Oetermination of lead Concentration in Ambient Particulate Matter by Energy Oispersive X-ray Fluorescence Spectrometry (NEA, Inc.l."

Note the "designated method identification number" which has been assigned to the method. This number identifies the method as a designated reference or equivalent method. Any.significant changes to the method must be approved by EPA, 'either as a modification under Section 2.8 of 40 CFR Part 58, Appendix C (Modifications of Methods by Users) or under 40 CFR Part 53 as a modified or new method.

As provided in 40 CFR 53.8, a notice of this designation has been submitted for publication in the Federal Register. Until that notice is pUblished, .this letter will constitute proof of the designation. This newly designated method will also be added to the current list of designated reference and equivalent methods maintained by this office. The updated list will be sent to the EPA Regional Offices and will be available to anyone upon request, either through the Regional Offices or through this office.

As a designated equiva lent method, this method is acceptab**le~** 

### {or us by NEA, Inc. for purposes of 40 CFR Part 58, Ambient Air Quality SurVeillance. For such use, the method must be used in strict accordance with the operational procedures or instruction manua 1 

### associ ated with the method and submitted as part of your request for an equivalent method determination.

### Ms. Lisa M. 

### Caldwell May 10, 1989

It is anticipated that requests for technical information and copies of the method description will be directed to both NEA, Inc. and EPA. We plan to distribute copies of the method description upon request but prefer that technical questions concerning the method be directed to NEA, Inc.

If you should have any questions concerning this action, please contact me by letter or by telephone (919) 541-2665. Sincerely yours,

# ~~A~ef Ambient Methods Standardization Branch Quality Assurance Division (MD-77).



# cc: Barry Towns,**ESD/USEPA~** 

### Region X Jon Schweiss, ESD/USEPA, Region X Stan Sleva, OAQPS/USEPA/RTP

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