ASTM E2143-01(2006)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: E 2143 – 01 (Reapproved 2006)
Standard Practice 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 E 2143; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope D 5412 Test Method for Quantification of Complex Poly-
cyclic Aromatic Hydrocarbon Mixtures or Petroleum Oils
1.1 Thistestmethodcoversarapidmethodforthescreening
in Water
of environmental samples for aromatic hydrocarbons (AHs)
E 131 Terminology Relating to Molecular Spectroscopy
and polycyclic aromatic hydrocarbons (PAHs). The screening
E 388 Test Method for Wavelength Accuracy of Spectral
takes place in the field and provides immediate feedback on
Bandwidth of Fluorescence Spectrometers
limits of contamination by substances containing AHs and
E 578 TestMethodforLinearityofFluorescenceMeasuring
PAHs. Quantification is obtained by the use of appropriately
Systems
characterized, site-specific calibration curves. Remote sensing
E 579 Test Method for Limit of Detection of Fluorescence
by use of optical fibers is useful for accessing difficult to reach
of Quinine Sulfate in Solution
areas or potentially dangerous materials or situations. When
contamination of field personnel by dangerous materials is a
3. Terminology
possibility, use of remote sensors may minimize or eliminate
3.1 For definitions of terms used in this test method refer to
the likelihood of such contamination taking place.
Terminology D 1129 and E 131.
1.2 This test method is applicable toAHs and PAHs present
in samples extracted from soils or in water. This test method is
4. Summary of Test Method
applicable for field screening or, with an appropriate calibra-
4.1 This test method consists of extracting the AHs and
tion, quantification of total AHs and PAHs.
PAHs from soil samples or preparation of water samples
1.3 This standard does not purport to address all of the
followed by synchronous fluorescence analysis with a field-
safety concerns, if any, associated with its use. It is the
portable instrument. The samples require serial dilutions of
responsibility of the user of this standard to establish appro-
samplestoestablishalinearresponse.Thesemeasurementsare
priate safety and health practices and determine the applica-
made using standard fluorescence cuvettes. While some opti-
bility of regulatory limitations prior to use.
mization of selectivity can be accomplished by varying the
2. Referenced Documents wavelength difference between excitation and emission mono-
2 chromators, generally spectra generated from petroleum con-
2.1 ASTM Standards:
taminants with a wavelength difference such as 6 or 18 nm
D 1129 Terminology Relating to Water
provide good results and no preliminary spectra are required
D 4489 Practices for Sampling of Waterborne Oils
(see Test Method D 5412).
4.2 Different soils have varying partition coefficients.
This practice is under the jurisdiction of ASTM Committee E13 on Molecular Therefore, representative samples of a subset of the extracts or
Spectroscopy and is the direct responsibility of Subcommittee E13.09 on Optical
the water samples should be analyzed by gas chromatography
Fibers and Wave Lengths.
(GC) or other appropriate methods. The purpose is to establish
Current edition approved Sept. 1, 2006. Published September 2006. Originally
a site-specific calibration curve to be used for quantification of
approved in 2001. Last previous edition approved in 2001 as E 2143 – 01.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
total AHs and PAHs in the environmental samples of interest.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
4.3 When desirable, determination of AHs and PAHs may
Standards volume information, refer to the standard’s Document Summary page on
be made remotely using an optical fiber.
the ASTM website.
Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959, United States.
E 2143 – 01 (2006)
5. Significance and Use nous scanning. The bandwidth of the monochromators should
be less than one half the wavelength offset between the
5.1 This technique is designed for on-site rapid screening
monochromators or smaller. The spectrometer should be ca-
and characterization of environmental soil and water samples
pable of remote sensing via optic fiber. The detector should be
resulting in significant cost savings for environmental reme-
a photomultiplier tube or a device with similar sensitivity and
diation projects. Remote analysis can be made with optical
response time. Occasionally field work requires the spectrom-
fibers when situations warrant or demand use of this option.
eter to be battery powered. The instrument should meet the
5.2 Quantification of total AHs and PAHs in these environ-
specifications in Table 1.
mental samples is accomplished by having a subset of the
7.2 Excitation Source—A pulsed (9.9 W) Xenon lamp or
samples analyzed by an alternate technique and generating a
other source having sufficient intensity throughout the ultra-
site-specific calibration curve.
violet and visible regions can be used.
5.3 Synchronous fluorescence provides sufficient spectral
7.3 Cuvette Sample Holder—Sample holders should be
information to characterize the AHs and PAHs present as
fabricated to hold commercially available, fluorescence-free,
benzene, toluene, ethylbenzene and xylene(s) (BTEX), the
fused silica cuvettes.
aromatic portion of total petroleum hydrocarbons (TPH), or
7.4 Optical Fiber Holder—A stage that allows correct
large aromatic ring systems up to at least seven fused rings,
such as might be found in creosote. positioning of the optical fiber with respect to the emission and
excitation monochromators. The device may also be used to
6. Interferences optically match each fiber and the respective monochromator.
7.5 ComputerSystem—The instrument should be interfaced
6.1 Thesynchronousfluorescencespectrumcanbedistorted
to a computer system that is compatible with the instrument
or quantification may be affected if there is a contaminant
and has suitable software for spectral data manipulation.
present that produces a synchronous peak in the same vicinity
7.6 Cuvette—A standard 12 by 12 by 31 mm fluorescence-
as the material of interest. Often spectroquality solvents
free fused silica cuvette. Four sides of the cuvette should be
contain impurities that produce background signals. Solvent
polished.
blanks should be used to verify a low fluorescence background
7.7 Optical Fiber—Fused silica fiber (preferably a high
so the background can be subtracted from the sample’s
spectrum. hydroxide) is required for transmission of the ultraviolet
wavelengths required for accurate spectroscopic analysis. In
6.2 There are naturally occurring compounds that fluoresce,
which may interfere with the detection of petroleum com- general, this material has good thermal characteristics, can be
obtained with low fluorescence background, and is readily
pounds,presentinthesample.Humicacidfromleafmoldisan
available commercially.
example of such a compound. Its strongest emission occurs in
the near ultraviolet range. 7.8 Glassware—A 10 mL and 2 mL disposable pipet, both
6.3 Absorption of the exciting light by the sample itself marked with 0.1 mL gradations. A glass disposable test tube,
(self-filtering effect) produces erroneous results. Analysis of capable of holding volumes of liquid greater than 15 mL. The
serial dilutions of the sample detects this effect and ensures an testtubecapsshouldbepolytetrafluoroethylenelinedtoreduce
accurate analysis is made. Once linearity is established, then potential contamination.
integration of the spectrum produces accurate results.
7.9 Scale—Aportablescalecapableofmeasuring2gofsoil
6.4 Certain solvents used for extraction of the soil samples to the nearest 0.1 g.
could quench or absorb the fluorescence and raise the limit of
7.10 Centrifuge—A portable centrifuge, capable of holding
detection. Care should be taken to avoid halogenated solvents
the test tubes described in 7.8.
or solvents containing other quenchers. The user of this test
7.11 Shaker—A portable shaker, capable of mixing the soil
method should bear this in mind when selecting an appropriate
and solvent in the test tubes described in 7.8.
solvent.
7.12 Filter Apparatus—A syringe with disposable 100-µm
glass detachable filters.
NOTE 1—Storage of samples in improper containers, such as plastics
other than polytetrafluoroethylene (or TFE-fluorocarbon), may result in
contamination.
NOTE 2—This test method is normally used without an internal stan-
TABLE 1 Desirable Performance Standards of a Field Portable
dard due to possible interference by the internal standard.
Fluorescence Spectrometer
6.5 Certain optical fibers may generate a fluorescence back-
Characteristic Desirable Range Typical
ground. These should be avoided whenever possible. If they
Monochromator
must be used, a background spectrum should be generated and Bandwidth 1–5 nm 3 nm
Wavelength accuracy 6 0.5–2 nm 6 1.0 nm
subtracted from any samples measured.
Reproducibility 6 0.1– 1% 6 0.2%
7. Apparatus Interface
Data collection computerized laptop PC
7.1 Fluorescence Spectrometer—An instrument recording
Instrument control control and data
in the spectral range of at least 250 to 650 nm is required for
Source
both excitation and emission spectrum measurements and
Broad band 200–1000 nm Xenon lamp
capable of scanning both monochromators at a constant speed
Low-power consumption 5–75 W 10 W
with a constant wavelength offset between them for synchro-
E 2143 – 01 (2006)
8. Reagents and Materials a wavelength offset between the monochromators of 18 nm.
Other wavelength offset between the monochromators values
8.1 Purity of Reagents—Spectroquality grade reagents
may be used when appropriate.
should be used in all instances unless otherwise stated.
11.1.1 Subtract the spectrum of a distilled water blank from
8.2 Purity of Water—ASTM Grade 3 or Grade 4 water
the spectrum of the water sample.
should be used.
11.1.2 Integrate the area under the spectrum of the sample
8.3 Solvents—Highpuritysolventsshouldbeused.Solvents
over the appropriate wavelength region to determine the
should be of sufficient purity so as to not generate a back-
relative value.
ground fluorescence spectrum when analyzed as a blank.
11.1.3 Determine if the sample is in the linear range. The
Solvents such as hexane, cyclohexane and methylcyclohexane,
determination of linear range is done by performing a 1:1
ethanol,methanol,etc.mustnotabsorbinthespectralregionof
dilution. Subtract the spectrum of a distilled water blank from
interest.
the spectrum of the 1:1 dilution. Integrate the area under the
9. Sampling and Sample Preparation
spectrum of the sample over the appropriate wavelength
region. If the integrated value is half of the original value, then
9.1 Water Samples—Collect water samples in accordance
the sample is in the linear range; otherwise, perform subse-
with Practice D 4489, as applicable.
quent dilutions until the linear range is established.
9.1.1 If the water samples contain visible particles, then the
11.2 SoilSamples—Analyzethesoilsampleextractoverthe
samples may be either centrifuged or filtered depending on the
appropriate wavelength region using a synchronous scan with
nature of the particles. Large, dense particles can usually be
a wavelength offset between the monochromators of 18 nm.
centrifuged to the bottom of the sample container, while finer
11.2.1 Subtract the spectrum of a solvent blank from the
particles must be filtered. The water samples should be
spectrum of the soil sample.
centrifuged in the containers in which they are sampled, in
11.2.2 Integrate the area under the spectrum of the sample
order to avoid volatilization of the organic hydrocarbons. The
over the appropriate wavelength region to determine the
water samples should be filtered into the cuvette for analysis.
relative value.
9.1.2 Add approximately 2.5 mL of the water sample into
11.2.3 Determine whether the sample is in the linear range
the cuvette using a disposable pipet and place the cuvette into
according to 11.1.3.
the instrument sample holder.The sample is ready for analysis.
11.3 Quantitative Analysis—After several soil or water
9.2 Soil Samples—Collect the sample using accepted pro-
samples have been analyzed by the instrument, pick several
cedures already established by ASTM Committee D18.
samples representing a range of concentrations (at least three:
9.2.1 Obtain a representative 2-g soil sample from the
high, medium, and low) and include solvent blanks and
samplecontainer.Thesampleshouldbeweigheddirectlyinthe
samples of known composition. These samples should be
test tube.
analyzed by the laboratory using the appropriate method, such
9.2.2 Add 10 mL of the appropriate solvent to the soil
as total petroleum hydrocarbons using the Environmental
sample in the test tube using a disposable pipet.
ProtectionAgency (EPA), gasoline range organics (GRO), and
9.2.3 Shake the sample until greater than 90 % of the
diesel range organics (DRO) methods or total polycyclic
sampleissuspendedinthesolvent.Followthisshakingprocess
aromatic hydrocarbons. Many of the approved EPA methods
bycentrifugingthesampleinordertoseparatethesolventfrom
also include aliphatic hydrocarbons in the analysis. If the
the soil.
relative proportion of aromatic hydrocarbons to aliphatic
9.2.4 Pour the extract into a second test tube. At this point
hydrocarbons remains constant then the correlation graphs
some particles may be present in the extract, thus filtration will
described in 11.3.1 can be developed.
be required to remove them.
11.3.1 For each sample analyzed by the laboratory, plot the
9.2.5 If the quality check in 13.6 indicates a need for
laboratory concentration versus the instrument concentration
additional extraction, then the additional extraction will be
on a scatter plot.Apply a trend line to the data set and perform
performed at this time.
linear regression. The equation of the trend line can be used to
10. Preparation of Apparatus 3
predict the value of future instrument analyses. For further
10.1 Prior to mobilization for field use, set up and calibrate information, see Ref (1)in Appendix X1.
the fluorescence spectrometer according to the manufacturer’s
12. Calculations
instructions and Test Methods E 388, E 578, and E 579. Onc
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