ASTM E2143-01(2021)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation:E2143 −01 (Reapproved 2021)
Standard Test Method for
Using Field-Portable Fiber Optics Synchronous
Fluorescence Spectrometer for Quantification of Field
Samples for Aromatic and Polycyclic Aromatic
Hydrocarbons
This standard is issued under the fixed designation E2143; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
1.1 Thistestmethodcoversarapidmethodforthescreening 2.1 ASTM Standards:
of environmental samples for aromatic hydrocarbons (AHs) D1129 Terminology Relating to Water
and polycyclic aromatic hydrocarbons (PAHs). The screening D4489 Practices for Sampling of Waterborne Oils
takes place in the field and provides immediate feedback on D5412 Test Method for Quantification of Complex Polycy-
limits of contamination by substances containing AHs and clicAromatic Hydrocarbon Mixtures or Petroleum Oils in
PAHs. Quantification is obtained by the use of appropriately Water
characterized, site-specific calibration curves. Remote sensing E131 Terminology Relating to Molecular Spectroscopy
by use of optical fibers is useful for accessing difficult to reach E388 Test Method for Wavelength Accuracy and Spectral
areas or potentially dangerous materials or situations. When Bandwidth of Fluorescence Spectrometers
contamination of field personnel by dangerous materials is a E578 Test Method for Linearity of Fluorescence Measuring
possibility, use of remote sensors may minimize or eliminate Systems
the likelihood of such contamination taking place. E579 Test Method for Limit of Detection of Fluorescence of
Quinine Sulfate in Solution
1.2 This test method is applicable toAHs and PAHs present
in samples extracted from soils or in water. This test method is
3. Terminology
applicable for field screening or, with an appropriate
calibration, quantification of total AHs and PAHs. 3.1 For definitions of terms used in this test method refer to
Terminology D1129 and E131.
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
4. Summary of Test Method
standard.
4.1 This test method consists of extracting the AHs and
1.4 This standard does not purport to address all of the
PAHs from soil samples or preparation of water samples
safety concerns, if any, associated with its use. It is the
followed by synchronous fluorescence analysis with a field-
responsibility of the user of this standard to establish appro-
portable instrument. The samples require serial dilutions of
priate safety, health, and environmental practices and deter-
samplestoestablishalinearresponse.Thesemeasurementsare
mine the applicability of regulatory limitations prior to use.
made using standard fluorescence cuvettes. While some opti-
1.5 This international standard was developed in accor-
mization of selectivity can be accomplished by varying the
dance with internationally recognized principles on standard-
wavelength difference between excitation and emission
ization established in the Decision on Principles for the
monochromators, generally spectra generated from petroleum
Development of International Standards, Guides and Recom-
contaminants with a wavelength difference such as 6 nm or 18
mendations issued by the World Trade Organization Technical
nm provide good results and no preliminary spectra are
Barriers to Trade (TBT) Committee.
required (see Test Method D5412).
This test method is under the jurisdiction of ASTM Committee E13 on
Molecular Spectroscopy and Separation Science and is the direct responsibility of
Subcommittee E13.09 on Fiber Optics, Waveguides, and Optical Sensors. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Sept. 1, 2021. Published September 2021. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 2001. Last previous edition approved in 2013 as E2143 – 01 (2013). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/E2143-01R21. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E2143−01 (2021)
4.2 Different soils have varying partition coefficients. 6.5 Certain optical fibers may generate a fluorescence back-
Therefore, representative samples of a subset of the extracts or ground. These should be avoided whenever possible. If they
the water samples should be analyzed by gas chromatography must be used, a background spectrum should be generated and
(GC) or other appropriate methods. The purpose is to establish subtracted from any samples measured.
a site-specific calibration curve to be used for quantification of
7. Apparatus
total AHs and PAHs in the environmental samples of interest.
4.3 When desirable, determination of AHs and PAHs may 7.1 Fluorescence Spectrometer—An instrument recording
in the spectral range of at least 250 nm to 650 nm is required
be made remotely using an optical fiber.
for both excitation and emission spectrum measurements and
capable of scanning both monochromators at a constant speed
5. Significance and Use
with a constant wavelength offset between them for synchro-
5.1 This technique is designed for on-site rapid screening
nous scanning. The bandwidth of the monochromators should
and characterization of environmental soil and water samples
be less than one half the wavelength offset between the
resulting in significant cost savings for environmental reme-
monochromators or smaller. The spectrometer should be ca-
diation projects. Remote analysis can be made with optical
pable of remote sensing via optic fiber. The detector should be
fibers when situations warrant or demand use of this option.
a photomultiplier tube or a device with similar sensitivity and
5.2 Quantification of total AHs and PAHs in these environ-
response time. Occasionally field work requires the spectrom-
mental samples is accomplished by having a subset of the
eter to be battery powered. The instrument should meet the
samples analyzed by an alternate technique and generating a
specifications in Table 1.
site-specific calibration curve.
7.2 Excitation Source—A pulsed (9.9 W) Xenon lamp or
5.3 Synchronous fluorescence provides sufficient spectral
other source having sufficient intensity throughout the ultra-
information to characterize the AHs and PAHs present as
violet and visible regions can be used.
benzene, toluene, ethylbenzene and xylene(s) (BTEX), the
7.3 Cuvette Sample Holder—Sample holders should be
aromatic portion of total petroleum hydrocarbons (TPH), or
fabricated to hold commercially available, fluorescence-free,
large aromatic ring systems up to at least seven fused rings,
fused silica cuvettes.
such as might be found in creosote.
7.4 Optical Fiber Holder—A stage that allows correct
positioning of the optical fiber with respect to the emission and
6. Interferences
excitation monochromators. The device may also be used to
6.1 Thesynchronousfluorescencespectrumcanbedistorted
optically match each fiber and the respective monochromator.
or quantification may be affected if there is a contaminant
7.5 Computer System—The instrument should be interfaced
present that produces a synchronous peak in the same vicinity
to a computer system that is compatible with the instrument
as the material of interest. Often spectroquality solvents
and has suitable software for spectral data manipulation.
contain impurities that produce background signals. Solvent
blanks should be used to verify a low fluorescence background
7.6 Cuvette—A standard 12 mm by 12 mm by 31 mm
so the background can be subtracted from the sample’s
fluorescence-free fused silica cuvette. Four sides of the cuvette
spectrum.
should be polished.
6.2 There are naturally occurring compounds that fluoresce,
7.7 Optical Fiber—Fused silica fiber (preferably a high
which may interfere with the detection of petroleum
hydroxide) is required for transmission of the ultraviolet
compounds, present in the sample. Humic acid from leaf mold
wavelengths required for accurate spectroscopic analysis. In
is an example of such a compound. Its strongest emission
general, this material has good thermal characteristics, can be
occurs in the near ultraviolet range.
obtained with low fluorescence background, and is readily
available commercially.
6.3 Absorption of the exciting light by the sample itself
(self-filtering effect) produces erroneous results. Analysis of
serial dilutions of the sample detects this effect and ensures an
accurate analysis is made. Once linearity is established, then
TABLE 1 Desirable Performance Standards of a Field Portable
integration of the spectrum produces accurate results.
Fluorescence Spectrometer
Characteristic Desirable Range Typical
6.4 Certain solvents used for extraction of the soil samples
Monochromator
could quench or absorb the fluorescence and raise the limit of
Bandwidth 1 nm–5 nm 3 nm
detection. Care should be taken to avoid halogenated solvents
Wavelength accuracy ±0.5nm–2 nm ±1.0 nm
or solvents containing other quenchers. The user of this test
Reproducibility ±0.1 %–1 % ±0.2 %
method should bear this in mind when selecting an appropriate
Interface
solvent.
Data collection computerized laptop PC
Instrument control control and data
NOTE 1—Storage of samples in improper containers, such as plastics
other than polytetrafluoroethylene (or TFE-fluorocarbon), may result in
Source
contamination.
Broad band 200 nm–1000 nm Xenon lamp
NOTE2—Thistestmethodisnormallyusedwithoutaninternalstandard Low-power consumption 5 W–75 W 10 W
due to possible interference by the internal standard.
E2143−01 (2021)
7.8 Glassware—A 10 mL and 2 mL disposable pipet, both 9.2.5 If the quality check in 13.6 indicates a need for
marked with 0.1 mL gradations. A glass disposable test tube, additional extraction, then the additional extraction will be
capable of holding volumes of liquid greater than 15 mL. The performed at this time.
testtubecapsshouldbepolytetrafluoroethylenelinedtoreduce
potential contamination.
10. Preparation of Apparatus
7.9 Scale—Aportablescalecapableofmeasuring 2g of soil 10.1 Prior to mobilization for field use, set up and calibrate
to the nearest 0.1 g. the fluorescence spectrometer according to the manufacturer’s
instructions and Test Methods E388, E578, and E579. Once in
7.10 Centrifuge—A portable centrifuge, capable of holding
the field, include in the calibration procedures, a check of the
the test tubes described in 7.8.
wavelength accuracy of the instrument using an appropriate
7.11 Shaker—A portable shaker, capable of mixing the soil
line-source such as a mercury lamp or xenon lamp. In addition,
and solvent in the test tubes described in 7.8. check the baseline of the instrument by analyzing a solvent
blank. Other options for calibration may include the use of
7.12 Filter Apparatus—A syringe with disposable 100 µm
plastic standards, sealed solutions of anthracene or other
glass detachable filters.
commercially available standards.
8. Reagents and Materials
11. Procedure
8.1 Purity of Reagents—Spectroquality grade reagents
11.1 Water Samples—Analyze the water sample over an
should be used in all instances unless otherwise stated.
appropriate wavelength region using a synchronous scan with
8.2 Purity of Water—ASTM Grade 3 or Grade 4 water
a wavelength offset between the monochromators of 18 nm.
should be used.
Other wavelength offset between the monochromators values
may be used when appropriate.
8.3 Solvents—High purity solvents should be used. Solvents
11.1.1 Subtract the spectrum of a distilled water blank from
should be of sufficient purity so as to not generate a back-
the spectrum of the water sample.
ground fluorescence spectrum when analyzed as a blank.
11.1.2 Integrate the area under the spectrum of the sample
Solvents such as hexane, cyclohexane and methylcyclohexan
...