EPA-ORD / EPA-OST: IO-3.3: Metals in Ambient Particulate Matter Using X-Ray Fluorescence (XRF) Spectroscopy

Summary
Analytes
Revision
Data and Sites

Official Method Name

Compendium Method IO-3.3. Determination of Metals in Ambient Particulate Matter Using X-Ray Fluorescence (XRF) Spectroscopy

Current Revision

Revison 0, June 1999

Media

AIR

Instrumentation

X-Ray Fluoresence

Method Subcategory

Inorganic

Method Source

EPA-ORD / EPA-OST

Citation

EPA, 1999, Compendium Method IO-3.3, DETERMINATION OF METALS IN AMBIENT PARTICULATE MATTER USING X-RAY FLUORESCENCE (XRF) SPECTROSCOPY. EPA/625/R-96/010a.

Brief Method Summary

The method described is x-ray fluorescence applied to PM10, fine (<2.5 um) and coarse (2.5-10 um) aerosols particles captured on membrane filters. The samplers which collect these particles are designed to separate particles on their inertial flow characteristics producing size ranges which simplify x-ray analysis. The instrument is a energy dispersive x-ray spectrometer which utilizes secondary excitation from selectable targets or fluorescers and is calibrated with thin metal foils and salts for over 40 chemical elements.

Scope and Application

Over 40 elements are measured on thin filters used during sampling of ambient air according to careful sampling procedures.

Applicable Concentration Range

Element and filter dependent. Range is roughly 1 ng/cm² to 1000 ng/cm² based on a 100 cm² filter. The volume of air sampled will determine the ultimate air-based concentration range.

Interferences

Interference corrections arises from overlaps that are not deconvoluted by the least squares algorithm. Techniques for interference correction are cited in the method.

Quality Control Requirements

Run-time quality control gives an indication of instrument performance at the time of data acquisition by measurements on stable qualitative standards. The analysis results of Standard Reference Materials SRM1833 and SRM1832 is also used as a quality control measure.

Sample Handling

Samples are collected on specialized filters using cited sampling methods.

Maximum Holding Time

None included.

Relative Cost

$51 to $200

Sample Preparation Methods

Filters are inspected prior to XRF analy

This method has 44 analytes associated with it.

Analyte	Detection Level	Bias	Precision
Aluminum(7429-90-5) Al Aluminium Aluminum Aluminum (fume or dust) Aluminum powder	17.600 ng/cm2	N/A	N/A
Antimony(7440-36-0) Antimony Sb Stibium	31.400 ng/cm2	N/A	N/A
Arsenic(7440-38-2) Arsenic As	0.800 ng/cm2	N/A	N/A
Barium(7440-39-3) Ba Barium	51.800 ng/cm2	N/A	N/A
Bromine(7726-95-6) Br2 Bromine	0.600 ng/cm2	N/A	N/A
Cadmium(7440-43-9) Cadmium Cd	22.000 ng/cm2	N/A	N/A
Calcium(7440-70-2) Ca Calcium	9.000 ng/cm2	N/A	N/A
Cesium(7440-46-2) Caesium Cesium Cs EINECS 231-155-4 HSDB 7040	48.900 ng/cm2	N/A	N/A
Chlorine(7782-50-5) Chlorine Chlorine Cl2	4.800 ng/cm2	N/A	N/A
Chromium(7440-47-3) Chromium Cr	3.000 ng/cm2	N/A	N/A
Cobalt(7440-48-4) Co Cobalt	0.400 ng/cm2	N/A	N/A
Copper(7440-50-8) Copper Copper (metallic) Cu	0.700 ng/cm2	N/A	N/A
Gallium(7440-55-3) EINECS 231-163-8 Gallium HSDB 6956	1.600 ng/cm2	N/A	N/A
Germanium(7440-56-4) EINESC 231-164-3 Germanium Germanium element HSDB 2118	1.100 ng/cm2	N/A	N/A
Gold(7440-57-5) Au Gold	1.700 ng/cm2	N/A	N/A
Iodine(7553-56-2) AI3-08544 Caswell No. 501 EPA Pesticide Chemical Code 046905 Iodine Iodine Tincture USP Iodine crystals NSC 42355	35.500 ng/cm2	N/A	N/A
Iron(7439-89-6) Fe Iron	0.700 ng/cm2	N/A	N/A
Lanthanum(7439-91-0) EINECS 231-099-0 Lanthanum UNII-6I3K30563S	70.600 ng/cm2	N/A	N/A
Lead(7439-92-1) Lead Lead and compounds (inorganic) Lead and lead compounds Pb	1.500 ng/cm2	N/A	N/A
Magnesium(7439-95-4) Magnesium Mg	3.200 ng/cm2	N/A	N/A
Manganese(7439-96-5) Manganese Mn	0.800 ng/cm2	N/A	N/A
Mercury(7439-97-6) Hg Hydrargyrum Liquid silver Mercury Mercury (inorganic) Quicksilver	1.500 ng/cm2	N/A	N/A
Molybdenum(7439-98-7) Amperit 105.054 Amperit 106.2 EINECS 231-107-2 HSDB 5032 MChVL Metco 63 Mo Molybdenum Molybdenum, metallic TsM1	1.600 ng/cm2	N/A	N/A
Nickel(7440-02-0) Ni Nickel Nickel, soluble salts Raney Nickel (R)	0.600 ng/cm2	N/A	N/A
Palladium(7440-05-3) Palladium Pd	22.900 ng/cm2	N/A	N/A
Phosphorus(7723-14-0) Black phosphorus P Phosphorous, Red Phosphorus Phosphorus (yellow or white) Red phosphorus Violet phosphorus White phosphorus Yellow phosphorus	2.600 ng/cm2	N/A	N/A
Potassium(7440-09-7) K Potassium	6.300 ng/cm2	N/A	N/A
Rhodium(7440-16-6) Rh Rhodium Rhodium-103	25.900 ng/cm2	N/A	N/A
Rubidium(7440-17-7) EINESC 231-126-6 Rubidium	0.700 ng/cm2	N/A	N/A
Scandium(7440-20-2) Scandium	1.500 ng/cm2	N/A	N/A
Selenium(7782-49-2) Se Selenium Selenium and Compounds	0.700 ng/cm2	N/A	N/A
Silicon(7440-21-3) Silicon Silicon metal	8.000 ng/cm2	N/A	N/A
Silver(7440-22-4) Ag Silver	20.200 ng/cm2	N/A	N/A
Sodium(7440-23-5) Na Natrium Sodium	5.300 ng/cm2	N/A	N/A
Strontium(7440-24-6) Sr Strontium	1.100 ng/cm2	N/A	N/A
Tellurium(13494-80-9) Aurum paradoxum EINECS 236-813-4 HSDB 2532 Metallum problematum NCI-C60117 Telloy Tellurium Tellurium element Tellurium metallic	26.300 ng/cm2	N/A	N/A
Tin(7440-31-5) Sn Tin	30.500 ng/cm2	N/A	N/A
Titanium(7440-32-6) Ti Titanium	16.900 ng/cm2	N/A	N/A
Tungsten(7440-33-7) Tungsten	3.400 ng/cm2	N/A	N/A
Vanadium(7440-62-2) V Vanadium Vanadium (fume or dust)	5.300 ng/cm2	N/A	N/A
Yttrium(7440-65-5) EINESC 231-174-8 HSDB 7405 Yttrium Yttrium-89	1.200 ng/cm2	N/A	N/A
Zinc(7440-66-6) Zinc Zinc (fume or dust) Zinc and Compounds Zn	1.000 ng/cm2	N/A	N/A
Zirconium(7440-67-7) EINECS 231-176-9 HSDB 2528 Zircat Zirconium Zirconium metal	1.200 ng/cm2	N/A	N/A
sulfur(7704-34-9) sulfur	2.600 ng/cm2	N/A	N/A

Precision Descriptor Notes:	Precision varies with the element and concentration. At high concentrations (greater than 1 ug/cm²) a precision of 7.1 percent can be expected for elements analyzed by one fluorescer and 5.0 percent can be expected for those analyzed by two.
Detection Level Note:	Determined using a Teflon blank for fine particles at the 68 percent confidence level.

Revision	PDF/Link
Revison 0, June 1999

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EPA-ORD / EPA-OST: IO-3.3: Metals in Ambient Particulate Matter Using X-Ray Fluorescence (XRF) Spectroscopy

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