Q. How can I contact the
manufacturer of the Envirol quick test kits?
A. It appears that Envirol is out of business, or bought by another
company. However, information on a number of their kits is now available from
SDI (for example, as "SDI Quick Tests"). A contact at SDI is Karen
Peluso at 315-699-5526 or 315-727-4064 (mobile).
Q. Names of companies providing field XRF services.
A. Information of various XRF vendors already is posted on this web site. Please go to
X-Ray
Fluorescence then "Vendor/Instrument Information."
Q. Do you know why LIF and ROST are less expensive than
MIP? Is it the longevity of the probe itself? It is just hard for me to conceptualize
because the LIF systems are only found on CPT rigs that are much larger and
less mobile than the hammer rigs MIPs are found on.
A. In many or most cases, LIF or ROST is more cost effective than MIP.
However, they both have very different applications and either could be more
cost effective for a particular project. For heavier TPH constituents, PAH
compounds, and NAPLs, the LIF or ROST is the preferred option. In contrast,
MIP can only detect volatile compounds, but is effective for a broader range
of contaminant classes than LIF or ROST. BTEX and halogenated solvents are
important contaminant classes where MIP is effective while LIF/ROST is not.
In addition, whereas LIF and ROST are preferred for detecting NAPLs, MIP is
more effective for detecting lower concentrations of contaminants dispersed
in soil and groundwater.
MIPs are still generally deployed from smaller
direct push rigs (for example, rotary hammer platforms) that have a high
relative level of mobility and are less expsensive to operate. However,
LIF or ROST deployed from a heavier CPT rig would be able to achieve greater
push depths than a rotary hammer MIP and this can provide better coverage
in sites with deep contamination or DNAPLs. Even this generalization may
be too broad as many vendors, like Veronex, are making MIP available on
larger rigs.
In short, whether LIF or MIP is more cost
effective depends on your specific project needs. It is also important to
realize that data generated from LIF/ROST and MIP are semiquantitative and,
therefore, have limitations. Quantitation of individual compounds of concern
usually requires supplemental data (for example, discrete samples submitted
for offsite or on-site analysis using GC or GC/MS).
Q. I am searching for
a field screening technique to determine the presence of arsenic in soils.
Are there any existing technologies/protocols to achieve +/- results in
the field, perhaps colormetric?
A. We are not aware of colorimetric techniques for arsenic that have
achieved wide use, particularly in soil. X-ray fluorescence (XRF) is likely
your best option, without knowing more about your site. Use of XRF on undisturbed,
in-place soil would give you qualitative to semiquantitative data, whereas
actually collecting a sample and homogenizing it (say, in a sandwich bag
or other plastic bag) before analysis may yield semi-quantitative to quantitative
data. Other sample processing steps (for example, sieving, grinding, drying)
could further improve data quality.
Lead is a potential interferent for arsenic analysis by XRF which, if present
at the site, would need to be compensated for in the XRF method--a vendor
can help with this. Also, optimal reporting limits for arsenic by XRF are
in the 40-60 mg/kg range and are very matrix-specific. Actual reporting
limits attained for a given project may be considerably higher. Actual sensitivity,
as well as other aspects of method performance (precision and accuracy),
should be evaluated for a specific project through initial "pilot testing"
of the method and assessed relative to project action levels and data quality
objectives.
Q. I have a site with
lead impacted soils. We have been directed by the MPCA to excavate, stablilize
(when exceedance of TCLP) and haul. My question is, is there a field TCLP
analysis that can be used to facilite the excavation? My concern is that
the 16 hours required for TCLP would slow the whole process down.
A.To the best of our knowledge, there is no way around the TCLP extraction
time. The problem is not from the lead analysis but rather the TCLP extraction
that simulates leaching in acidic conditions. A weak acid (Acetic acid)
is added to a weighed sample and the solid sample is spun for 18 + 2 hours
in an appropriate container (depending on the analyses proposed on the extract).
The 18-hour spin time is crucial to the extraction and can't be avoided.
A question we would pose is why not use x-ray
flourescence (XRF) to guide excavation in near real-time and then segregate
waste piles based on the "20 times rule." The "20 times rule" is a way to
correlate a totals concentration with a worst-case TCLP concentration. A
description is attached. The 20 times rule concentration for lead is 100
mg/kg, where the total lead concentration is 20 times the TCLP limit of
5 mg/L. Use of this could expedite the excavation.
If lead is the only TCLP constituent of concern
and the form is consistent (an oxide, metallic, other) it could be possible
to make a correlation between XRF and a technology such as graphite furnace
atomic absorption (GFAA) spectroscopty or fixed lab analyses. However, under
most circumstances lead comes in many different forms and abundances, and
making a sound correlation between total XRF or fix lab GFAA analyses will
not work. We would suggest that excavation be guided by XRF and then the
material stockpiled on site and segregated to the degree possible based
on concentration. If the total metals concentration does not exceed the
20 times rule (100 mg/kg) then further characterization is not necessary.
If the waste exceeds the 20 times rule by several orders of magnitude (>10,000
mg/kg) then TCLP would once again not be required because TCLP results would
exceed the TCLP limit of 5 mg/L and the soil would be simply disposed of
as a hazardous waste. For the soil with concentrations above the 20 times
rule, but less than two orders of magnitude above the 20 times rule, the
material should be stock piled and a single 5to 10 point composite collected
and analyzed for TCLP lead. You can bring TCLP instrumentation to the field
for lead and it can work effectively, but only if there are not any other
constituents of concern because bringing ICAP to the field is not yet practicable.
To provide you with the best guidance, we
really need more information about conditions at the site. For example,
(1) What is the action level for lead at
the site? We need to know this because if the site action level is 400 ppm
then all excavated soils will likely fail TCLP. If the site action level
is 40 then soil removed will likely have TCLP values that both pass and
fail. In this case we would recommend pile segregation and TCLP analyses.
(2) How is the excavation efficiency being monitored? (for example, using
a fixed laboratory, GFAA or ICAP, Field XRF and so forth). We need to know
what analytical methods are being employed at the site so we can recommend
a comprable approach or at least a method that can be used collaboratively
with existing results.
(3) What are the requirements for disposal of lead? We need to know the
disposal requirments so we can determine the effectiveness of the TCLP 20
times rule discussed above.
Q. On a project I am working
on, a community group has asked me to answer two questions. First, whether
there is a continuous air monitoring system that can speciate VOCs, and whether
there is a continuous air monitoring system for total VOCs. I am hoping that
some one might be able to provide an answer. We have a problem with TCE in
an area, and so far, all of the work is focused on grab samples using SUMMA
canisters. Every so often we get a high reading of TCE. We want to know whether
there's another method for monitoring on a continuous basis. Also, the monitor
has to be pretty sensitive, as the Region IX provisional PRG for TCE is between
1.7 - 0.017 ppbv. If there is any information you have, it would be much appreciated.
Thanks very much.
A. In answer to your first question (speciation of VOCs), Fourier Transform
Infrared Spectoscopy (FTIR) technologies could be used to address the issues
at your site. I have attached a list of potential FTIR technology vendors
and suggest you contact them directly to get specific answers on the perfomance
of the various types of available equipment. FTIR has low reporting limits
in the parts per billion by volume (ppbv) range, and can speciate a broad
range of VOCs. Unfortunately, FTIR is still somewhat challenging and expensive
to apply in the field. In addition, useful information on FTIR and other "open
path" air monitoring technologies can be found at
cluin.org/programs/21m2.
Portable gas chromatographs (GC) may also be useful for VOC speciation at
your site. A number of companies market portable units with air pumps and
pre-concentrators that can be used for continuous ambient air monitoring.
Examples are the Scentograph sold by Inficon and the FM2000 sold by O.I. Analytical.
Their company websites are
www.hapsite.com
and
www.oico.com.
With pre-concentrators and a range of sensitive detectors, these units can
measure a broad range of VOCs and acheive reporting limits in the ppbv range.
In addition, there are some new sensor technologies emerging, but these are
still experimental and not widely available. More information on some of these
technologies is available at
www.sentix.org.
In answer to your second question, a broad range of continuous monitoring
equipment is available that can report concentrations of total VOCs. Examples
include personal health and safety monitors that are based on photoionization
detectors (PIDs) and flame ionization detectors (FIDs); refer to a safety
supply house
for additional information. However, such systems may not be sensitive enough
or respond to a broad enough range of VOCs to meet your needs. For example,
many total VOC meters respond well to hydrocarbons, such as benzene, but less
well to halogenated solvents such as TCE. Thus, the technologies noted above
that can speciate VOCs at low concentrations may also be your best bet to
report total VOC concentrations of concern for your site.
Q. In your training
module: Inorganic Chemical Characterization Techniques ... slide MV-7 you
state "carbon monoxide and sulfur compounds ... pass directly through the
units internal filters ... " Can you provide a reference that will substantiate
this claim? It is contrary to my experience, and I would like to clear this
up.
A. We have contacted several vendors of mercury vapor analyzers (MVA)
regarding the instruments' sensitivity to carbon monoxide and sulfur compounds.
Based on the most current information we collected, it appears that carbon
monoxide has no effect as an interference and gaseous sulfur compounds generally
have no effect. Sulfur dioxide (SO2), aromatic organics, and
other organics such as acetone may cause potential interferences, but must
be present in extremely high concentrations to saturate the instrument before
you can see a noticable effect. Sulfur particulates that can pass through
internal filters (for example, 0.2 microns) can cause interferences by depositing
on internal sample lines and scavenging mercury. Some instruments allow
for the filters to be analyzed and any interferences can be subtracted from
detected mercury concentrations. However, given the types of applications
in the environmental industry (ambient air monitoring), it is highly unlikely
that today's instruments will have problems with interferences. The slide
from which you pulled this information is from training developed in May
2002. Since then, this information has been updated.
Q. What percentage
of metals in dirt and or water constitutes it as a hazardous waste?
A. The percentage of a metal in a soil does not determine
if it is a hazardous waste under the Resource Conservation and Recovery
Act (RCRA). A soil or liquid is classified as a hazardous waste under RCRA
if the concentration measured in a weak acid extract of the soil or water
exceeds the regulatory threshold limit values provided in 40 CFR part 261.24.
US EPA method 1311, which can be downloaded at the following web address
http://www.epa.gov/epaoswer/hazwaste/test/pdfs/1311.pdf
is used to prepare the extract from a soil or water sample. The method is
equally applicable to waters or multiphasic liquids. The regulatory threshold
limit values are provided as a liquid concentrations and can be found at
http://ecfr.gpoaccess.gov/cgi/t/text/text-idx?c=ecfr.
You can calculate a conservative estimate of when a total metals concentratration
for a water or soil is likely to exceed the specified TCLP threshold limit
values by dividing the concentration measured by 20 and comparing that concentration
to the threshold limit values. If the concentration does not exceed the
threshold limit value then doing a TCLP test is not required. If it does
then you may need to do the test to make sure the extract will exceed. The
twenty times rule is just based on complete extraction of all contaminants
and is therefore very conservative, actual leachability will likely be much
lower depending on the mineral species present.
For more information you can download the final TCLP rule by going to www.epa.gov/clariton/clhtml/pubtitle.html
pressing "control F" and searching for document number oswfr89026.
Q. I have been trying
to access the "hot Topic" hotlink to the http://www.frtr.gov;
the federal remediation treatment roundtable matrix. It has not been accessible
for 2 days now- is it no longer supported, or is the site down? Do you know
who a POC for that site would be?
A. I was able to access the FRTR web site; however, I noticed that
I had to type the "www..." portion of the address for the site to load (in
addition to the ...frtr.gov portion of the address).
Q. Do you know of anyone
who is familiar with using a forensic investigation to conduct isotopic
analysis of TCE? The concept is to differentiate between two TCE sources
in ground water based on a "fingerprint" of their isotopes. We have a site
in Minnesota that we are considering using this type of analysis on.
A. The isotopes of chlorine fractionate poorly over a very narrow
range. Carbon, on the other hand, has a good deal of fractionation over
a broader range. End member product isotope ratios will need to be established
to determine if the technique will be viable. There are numerous consulting
firms in addition to EPA's Brownfield Technical Support Center (BrownfieldsTSC.org)
which specialize in forensics. Geomega (Andy Davis, 303-443-9117) http://www.geomega.com/contact.htm
and Ian Kaplan's firm, which is associated with UCLA. Randy Basset, formally
with the U of A. and the staff at the University of Texas. Bruce Darling
with LBG Guyton and associates guytonl@bellsouth.net.
Another useful resource can be found at http://www.zymaxforensics.com/.
Q. Hi, I am interested
to know what would be the accuracy on determination of Ca in cement by XRF
(Philips 2404 WD). We intend to use pressed powder pellets. Is this the
best sample preparation method? What should be done to achieve accurate
results?
A. We have contacted the German laboratory that manufactures the
instrument you will be using to run your analysis, but have not been successful
in connecting with them. Our recommendation is that you continue to attempt
to contact this laboratory concerning their default laboratory precision
and bias numbers for the method and instrument to be used. This is the normal
initial step in identifying the potential limits on accuracy, which can
be expected and the adequacy of the measurement for the intended use. These
default limits are generally based on the analysis of standards or a Compton
scattering calibration. Regardless of the calibration used, the point in
finding out what the initial instrumental performance limits are is to begin
to evaluate if the total uncertainty associated with a measurement is too
great such that the data cannot be reliably used for the intended purpose
or decision.
Total measurement variability (bias and precision
= accuracy) will determine the accuracy of a measurement. To more fully
understand the expected variability in results from the true state, standard
statistical methods should be used to analyze the variability/uncertainty
associated with any set of measurements as the data is collected or early
in the data collection process. A demonstration of methods applicability
should be considered where two comparable methods for analysis are used
to arrive at information, in this case CA concentrations in concrete. Results
can then be compared to further understand or identify any potential bias
created by the sampling process, analytical instrument, or matrix sampled.
Total uncertainty can be evaluated by analyzing a series of additive factors,
which range from sampling uncertainty through analytical uncertainty. Each
of these sources of uncertainty can be measured using specific types of
quality control samples, which can be introduced during the sampling and
analysis process. William Ingersoll's work can help practitioners begin
to learn to quantitate total measurement uncertainties. This type of sophisticated
analysis is generally only needed when low-level concentrations are expected
and decision criteria are close to the method reporting limits.
With respect to your specific problem, the
high concentration of CA can pose some challenges and potential benefits
to the overall accuracy of your measurements. At high concentrations, most
x-ray fluorescence (XRF) units are accurate to within several percent, which
is usually much more than sufficient to support construction materials decision-making.
An 55Fe (iron) source for a radioactive source type XRF unit is preferred
based on the activation coefficient for CA, but this would limit any trace
element capabilities.
Using an X-ray tube instrument, interferences
can arise as a function of concentration when K shell configurations overlap.
The total chemistry of the material being analyzed will control the need
for inter-element corrections and the presence of interferences, an X-ray
tube unit would facilitate this type of analysis and you should contact
a vendor like Niton or Innov-x for more information on x-ray tube instruments
(see table below).
Bottom line, is that you should not have
a problem, in our opinion, but without a better understanding of the instrument
you are planning to use and the chemistry of the concrete in question we
cannot provide any definitive information to you. We suggest you perform
a demonstration of methods applicability using a handful of samples and
perform analyses using both XRF and inductively coupled argon plasma spectroscopy
(ICP) to ensure that the results you are going to obtain will be sufficiently
reliable to support decision making. Even in this regard, without knowledge
of your decision criteria we cannot be sure that any additional work is
required. If default precision and bias are sufficiently low versus expected
concentrations and related tolerances to support decision making no action
other than tracking results statistically using a probability plot, may
be all that is needed (see EPA G-9 for better discussion of the use of probability
plots (http://www.epa.gov/quality/qa_docs.html).
Q. Can you please tell
me what electromagnetic radiation are used in each of the technologies?
e.g gas chromatography- is it infrared?
A. Here are the types of electromagnetic radiation associated with
analyte detection for the analytical technologies we have listed:
- XRF -- X-rays
- Test kits (colorimetric and IA) -- UV
or visible spectrum
- FOCS -- UV or visible spectrum
- LIF -- UV or visible spectrum
- GFAA -- Visible spectrum
- FTIR -- Infrared (IR)
- GC -- although some detectors use electromagnetic
radiation for detection (there are IR and atomic emission detectors, for
example), most GC detectors use some form of current for detection (that
is, they use an ionization process of some type to set up a measurable
electical current). In some cases, however, the ionization source itself
is radioactive (e.g., the Nickel-63 beta source used in electron capture
detectors).
- Mass Spec -- this again generally uses
ionization (along with magnetic fields), as opposed to EM radiation.
Q. Are any innovative
technologies for measuring BTEX, MTBE, TBA contamination in shallow soil
and wheathered shale bedrock to determine hot spots or contaminant gradient?
A. The best technology for measuring BTEX, MTBE, and TBA in the fields
is a gas chromatograph/mass spectrometry (GC/MS) system equipped with a
purge and trap sample sparging unit. Portable GC/MS systems, such as the
Inficon Hapsite system, can be equipped with a head space sample preparation
unit or a purge vessel. The headspace option is less desirable for use because
of the relatively high water solubility of MTBE and TBA. Even when a purge
vessel is used and MTBE or TBA are primary targets, method performance can
be improved by salting the water (usually mixed with soil) before analysis
in a purge vessel. This step is performed to improve extraction efficiency
and the purge vessel is also often heated to 40 degrees centigrade. A gas
chromatographic system can also be used with an optimized extraction system
using a purge vessel equipped with a photo ionization detector (PID) or
a dual detection system with a flame ionization detector (FID). However,
this type of instrument configuration is best used when matrix interferences
are known to be minimal, which is rarely the case for most petroleum sites.
There are no specific test kits that are available for these analytes specifically.
Q. What are the chemical
constituents of diesel fuel? Are PAHs present in diesel or are they products
of combustion.
A. Usually diesel fuels are a complex mixture or unsaturated aliphatic
and aromatic hydrocarbons. Poly nuclear aromatic hydrocarbons (PAH) are
present in most refined hydrocarbon fuels as a result of the cracking process.
They are a product of the combustion process, like that used in refining
or during the burning of petroleum products. Heavier hydrocarbon fuel products
such as jet fuels may have higher contents of PAH as might heavy oils, but
the relative concentration of PAHs is also dependant on the cracking process
used during refining and the nature of the feed crude being processed. In
general, PAHs can make up between 1 and 10 percent of a refined petroleum
product with lighter end products having lower relative percentages than
heavier end products. Spent or burned hydrocarbonsiduals can have even higher
PAH contents.
Q. Trying to locate
companies that provide training services on EPA methods such as 625?
A. Try the following web links www.pacslabs.com
and www.lab-data.com or also contact
a local certified laboratory in your area who has an experienced gas chromatography/mass
spectrometer group, they might be willing to show you their lab and discuss
their procedures with you. Make sure, regardless of the trainer you select
that they depend heavily on the method itself where necessary and do not
suggest method modifications, which are not generally accepted or peer reviewed.
Q. What is the PRG for
total lead in California?
A. The California PRG for lead is 150 ppm for residential receptors.
More information can be obtained at dtsc.ca.gov.
Q. Are there any commercially
available field screening methods available for Pesticides? Can they provide
economical, real time data that can be used to screen out samples for lab
based confirmation?
A. There are numerous commercially available pesticide kits that
can be found through several vendors.
Strategic Diagnostics is one such vendor. Listed below is a table of methods
for which commercially available kits are available.
| Immunoassay |
SW-846 Method |
| PCBs |
4020 |
| Chlordane |
4041 |
| DDT |
4042 |
| Toxaphene |
4040 |
| PCP |
4010 |
Also look at SW-846 on line for more information
at the following website for specific information on methods concerning
specific pesticides. The data collected using these methods can be used
for many purposes including confirmation with or without fixed lab comparative
analyses. The selection of comparative analyses for fixed lab analyses can
certainly be facilitated using field test kits, but the decision is usually
driven by concentration. It is our opinion that lab-based comparative analyses
should be focus in and around decision criteria where there is the highest
degree of uncertainty.
Q. To what extent do
different soils retain water?
A. Clay soils retain the most water. Sandy soils have the coarsest
texture and therefore the largest pore sizes. These large pore sizes are
too large to hold water through its cohesive property. Clay soils have the
finest texture, therefore the smallest pore sizes. Clay soils are able to
hold much more water because of their smaller pore size.
Q. I have a regulatory
group that needs a reference to indicate that results from in-situ field
methods for analysis of volatile organics in soil and soil gas are frequently
higher than those measured from the same media/site in the laboratory. I
realize this is common knowledge that sampling and subsampling cause loss
but I need a good reference to explain this. I have several of Hewitt's
papers.
A. We do not agree that it is necessary common knowledge that in
situ measurements are generally biased high relative to fixed laboratory
methods when analyzing samples for the presence of volatile organics. Test
kits can appear to biased high because they tend to analyze for the presence
of several classes of compounds. If several compounds are present then it
could appear that a result from the test kit [say for chlorinated volatiles]
could appear to be biased high as compared to specific results [for say
chlorobenzene]. In terms of soil gas, the comparison between volatile analyses
in the lab and soil gas will be likely the opposite. Because concentrations
in soil gas are dependant on what can partition from the soil, volatiles
remain in place that are stripped during the application of the analytical
lab method. Allen Hewitt has documented that significant loss of volatile
can be expected in soil samples where the samples are agitated and/or just
exposed to a change in atmospheric pressure, however other methods which
involve the extraction of sample in the field using methanol can be very
effective at minimizing the loss of volatiles during sampling prior to analysis.
A bigger question maybe how representative is the sample that is collected
and how heterogeneous is the sample that can result in observed differences
between volatile analyses regardless of when and where they were performed.
Hewitt’s papers are amongst the best published in terms of looking at the
impact of sampling methods on the loss of volatiles. However, there are
other sources of variance that may also be realized because soil gas is
different from purge and trap or extraction methods. You must be careful,
for example, when using field based analyses that use similar analytical
procedures both in the lab and in the field. If the result obtained in the
field is from a head space analyzer, such is commonly used with potable
GC/MS methods, the relationship expected is similar to that which might
be expected from soil gas (for example, relative to low bias).
Q. Can isotopic methods
be used to identify the parent chemical of VOC daughter products (1,1-DCE
and vinyl chloride) in cases where these daughters could have resulted from
the breakdown of more than one parent (TCE and 1,1,1-TCA)?
A. It is possible to distinguish between isotopes of chlorine in
water if sufficient fractionation exists between various parent sources.
Ablation in surface soil and other geochemical processes can impact chlorine
ratios so we do not suggest attempting soil isotopic analyses. Ratio numbers
between various daughter products and parents can also be helpful. For more
details concerning isotopic methods and other forensic methods we suggest
you go to the following website and journal for more information. http://www.zymaxusa.com/
and http://www.environmentalforensics.org/journal.htm.
Isotopic fractionation of chlorine is limited
in extent even under the best conditions. Chemical fingerprinting and other
intrinsic tracers or surrogate compound analyses may be useful for determining
the potential for linking contamination to source areas. Are there any other
contaminants that might be characteristic of one source area versus the
other? These can sometimes be useful.
Q. I am interested in
recommendations on field screening of sediments for low levels Naphthalene
contamination (~100ppb).
A. There are numerous field screening techniques that can be
used to test for the presence of petroleum hydrocarbons and several with
the capability to semi-quantitatively or quantitatively identify polynuclear
aromatic hydrocarbons in the low part per million (ppm) range in sediment
or soil samples. Usability for these kits diminish as detection limits in
the mid to low ppb range are required.
One such technology is available at http://www.site-lab.com/
and uses ultraviolet fluorescence (UVF) to quantitatively identify total
PAHs. Site lab currently has one UVF detector with the capability to detect
total PAHs at 25 ppb and another can detect total PAHs at 50 ppb. The kits
require a quick extraction procedure followed by analysis using the UVF
detector. Site-specific response factors can be developed based on a preliminary
demonstration of methods applicability (DMA) study and responses may then
be used to estimate naphthalene concentrations in the low ppb range. A consultation
with the manufacturer, completion of a DMA, and development of site specific
limits of detection are recommended before attempting to use this technology
full scale at your site.
Immunoassay kits can detect PAH compounds in the low ppm range and kits
are available from Strategic diagnostics http://www.sdix.com/
can detect carcinogenic PAH compounds in the low ppb range. The naphthalene
concentrations required to elicit a response in these carcinogenic immunoassay
test kits are unfortunately much higher (30,000 ppb). These tests also lack
the specificity to qualitatively identify only naphthalene as they respond
to a variety PAH compounds.
One recommendation for your sampling effort would be to evaluate all potential
chemicals of concern. Are other PAH or TPH compounds expected in sediment
samples? If so, these other indicator compounds can often be used to develop
correlations between field test kit concentrations and fixed laboratory
results. For an example of how that can accomplished see the Cos Cob Case
Study developed by EPA's Brownfield Technical Support Center at http://www.brownfieldstsc.org/pdfs/CosCob-casestudy_Final.pdf.
Specifically, you should review the section discussing the DMA and evaluation
of PAH and TPH field results.
If quantitative and qualitative results for specifically naphthalene in
the low ppb range are truly required for project success then sample analysis
by an appropriate EPA SW-846 may be warranted. Method
8270 operated in the selective ion mode can achieve very low ppb level
detection limits, method 8310 a high pressure liquid chromatography (HPLC)
method designed for analysis of PAH compounds may be suitable to meet project
objectives, and finally method 8260 for volatile organic compounds if effective
for naphthalene in the low ppb range.
Q. Can GC-MS generally
be used to differentiate between types of petroleum based fuel products?
A. In most environmental applications, gas chromatography with
a flame ionization detector (GC/FID) is used to evaluate fuel concentrations
and comparison with standards (diesel, gasoline, kerosene, jet fuel, motor
oil) is used to qualitatively identify the type of petroleum hydrocarbon.
Fuel patterns from the sample are visually matched to standards and can
be used to identify fuel types in the sample.
GC/MS although a more costly method can also be used to qualitatively and
quantitatively evaluate different fuel products see http://www.dpra.com/index.cfm/m/147.
Although this technique is not as commonly used. GC/MS analysis will allow
the user to identify different hydrocarbons in a complex fuel mixture.
One suggestion for the use of GC/MS to identify different petroleum based
fuel products is to evaluate concentrations of polynuclear aromatic hydrocarbons
(PAHs) in the sample. Most fuel types contain varying concentrations and
types of PAHs (naphthalene, benzo (a) pyrene, chrysene ect.) and the ratio
of these PAHs in a fuel sample can be used to distinquish different fuel
types. GC/MS techniques for analysis of PAHs includes EPA
SW-846 method 8270 [operation in the selective ion mode (SIM) allows
the user to achieve lower detection limits and avoid common interferences].
GC/MS analysis of volatile components of fuels can also assist in differentiating
between various fuel types. For example a standard EPA
SW-846 Method 8260 m analysis of a fuel or fuel contaminated sample
would provide critical information for benzene, toluene, ethylbenzene, and
xylene (BTEX) ratios which can be used to identify freshly spilled fuels
vs. older spills. Methyl tert butyl ether (MTBE) if identified in a sample
using this analysis would also indicate a gasoline fuel type manufactured
from the early 1990s to early 2000 (a gasoline additive used during that
time period).
If fingerprinting fuel types to determine potentially responsible parties
is the goal then several forensic chemistry techniques are also available.
See http://www.dpra.com/index.cfm/m/159.
Q. I am trying to measure
vapors that might come off free product fuel oil. Is it better to use Summa
cannisters for this. Is it OK to use Charcoal tubes to measure TVOC's from
this as (#2 fuel oil)?
A. Depending on your data needs both the summa canister and
charcoal tubes are effective techniques for evaluating vapors potentially
resulting from #2 fuel oil. You need to determine whether you want to evaluate
specific volatile compounds or total volatile components and at what concentrations
to better assist in choosing potential analytical techniques.
For example a standard EPA SW-846 Method such as method
8260 analysis of the product would provide qualitative and quantitive
results in the low part per billion (ppb) range for a number of volatile
organic compounds likely found in the fuel. These include benzene, toluene,
ethylbenzene, and xylene (BTEX), methyl tert butyl ether, and substituted
benzenes such as 1,2,4 and 1,3,5-trimethylbenzene. Specifics of the method
can be found at http://www.epa.gov/epaoswer/hazwaste/test/pdfs/8260b.pdf.
An analysis of vapors specifically volatilizing and coming off the fuel
(without the benefit of an inert gas purge of the free product as with SW-846
method 8260) should use a summa canister or other air sample collection
technique such as tedlar bags. The laboratory would still use a modified
SW-846 method 8260 method for analysis such as the TO-14 method performed
by air toxics http://www.airtoxics.com/cinfo/solutions.html#8260b.
There are also numerous commercial analytical laboratories that provide
this type of analysis in your area.
The advantage of the charcoal tubes for analysis is the benefit of real
time results, however these technologies tend to provide results with higher
detection limits (in the ppm range) and specific ranges of detection (for
example 5-15 ppm), provide limited compound specificity (not all compounds
available or provide results for compound classes), and are subject to potential
interferences. Charcoal tubes are available from manufacturers such as Draeger
or distribution companies such as SKC.
In conclusion, charcoal color tubes provide semi-quantitative results in
real or near real time and can be configured to detect specific compounds
or classes of compounds but are subject to limitations. If you require detection
limits in the ppb range and would prefer a definitive method of analysis
then GC/MS/FID techniques such as the TO-14 with SW-846 8260 analysis is
recommended.
Number 2 fuel oil can also be in a pure state and may not contain many of
those compounds detected by the methods noted above. Alternative methods
include simulated distillations of isotopic dilution methods such as EPA
600 Series method 1625, when more accurate forensic information is needed.
Concentration can also limit the utility of canister and tube methods. Careful
testing is needed of any method proposed for use to evaluate the quality
of information produced versus the decision requirements. Wothout further
information it is difficult to make a project specific recommendation concerning
you site unless more is known concerning the decisions you are attempting
to make.
Q. I am looking for
a reliable field test kit for TCE in soil. Unfortunately, Strategic Designs
Inc. no longer carries their soil test kit, only water. Are you aware of
another vendor that carries a similar field test kit?
A. You are correct, after speaking with representatives at Strategic
Diagnostics, it appears they have discontinued the soil application for
the TCE test kit and only produce a kit for TCE in water (See http://www.sdix.com/ProductSpecs.asp?nProductID=22.)
Our search did not identify another vendor producing immunoassay test kits
for TCE in soil, however we did identify another field based analytical
technology. The L2000DX analyzer provided by Dexsil
is capable of providing quantitative analysis or organic chlorine compounds
and specifically TCE. The technology converts organically bound chlorine
in the soil sample to inorganic chloride and the resulting chloride can
be quantified using the L2000DX analyzer. The technology is limited in much
the same way as immunoassay techniques that can be subject to cross-reactivity
of similar organic chlorine compounds. If other chlorinated solvents, PCBs,
or organochlorine pesticides are potentially present in your specific site
matrix, the technology cannot qualitatively identify these compounds and
they are reported as TCE. If the contaminant is unknown the instrument can
be configured to provide a "worst case" scenario for an upper limit concentration
of a target compound.
The LD2000DX analyzer costs $3,675 to purchase and test kit materials are
also required to complete analyses. Dexsil also provides rentals of the
equipment allowing a user to purchase test kit materials only and rent the
more costly analyzer. Method detection limits for TCE in a clean soil matrix
were reported by the manufacturer at 2ppm and the practical quantitation
limit for a similar matrix was reported to be 8 ppm. Actual MDLs and PQLs
for application at your site would likely several times higher. Depending
on the presence or absence of potential interferences and applicable action
levels the technology may provide sufficient sensitivity for application
at your site. We recommend a consultation with technical experts at Dexsil
and that you conduct a demonstration of method applicability (DMA) study
in accordance with the principles of EPA's Triad approach at your site prior
to using the technology full scale. Information concerning design of a DMA
through review of Triad case studies and profiles can be found at http://www.triadcentral.org/.
Q. Why are ionization
interference less severe in ICP than flame emission spectroscopy?
A. Ionization interference is less severe in ICP for several
reasons. The plasma spark used in ICP analysis burns much hotter than a
flame emission system. The temperature of an ICP flame in the analytical
zone is approximately 10,000 degrees C. The higher analysis temperature
allows more interfering analytes to be burned away. ICP also uses a magnetic
coil to hold the sample in place and this magnetism confines metals in the
convection zone (plasma spark) for a longer period of time. The longer resonance
time allows complete ionization of the sample thus limiting interference
when compared to flame emission.
Q. What is the critical
composition of Aromatic compounds (BTEX) in the air to be a main reason
for cancer in human body?
A. The critical (and only) component of BTEX that is defined
by EPA as a known human carcinogen is benzene. Existing data for the remaining
compounds (toluene, ethybenzene, and xylene) do not indicate that these
compounds cause cancer in the human body.
The threshold for daily exposure to benzene via inhalation is 3 x 10-2 mg/m3.
For additional information concerning chemical compounds and their effects
on the human body go to http://www.epa.gov/iris/index.html.
Q. I'd like to know
whether UVF, XVF, VIS/NIR, can be used to measure a soil's fertility?
A.
Although this question extends beyond our expertise in the environmental
characterization and remediation arena we have provided the following suggestions.
Evaluation of soil fertility is complex and involves analysis of a
range of macronutrients (nitrogen, phosphorus, potassium, sulfur, calcium,
magnesium etc.), micronutrients (boron, chlorine, copper, iron, manganese,
molybdenum, zinc) pH, soil composition (sand, silt, clay), cation exchange
capacity, and organic material content to name a few. The evaluation is
also specific to geographical location and the crop being grown.
Ultraviolet fluorescence (UVF) can be used for analysis of compounds such
as nitrogen and sulfur related to soil fertility. See http://www.jyinc.com/usadivisions/Emission/slfauv21.htm.
We could not find any references for XVF technology and assume you are referring
to x-ray fluorescence (XRF). This technology is ideally suited for analysis
of metals in a variety of matrices and specifically soil. Because these
analytes are the main nutrients you would be interested in evaluating for
an estimation of soil fertility this technology would be useful. Today's
XRF analyzers are field portable and can quantitatively and qualitatively
identify elements from sodium to uranium making evaluation of micronutrient
and macronutrient concentrations easy and in real time. Vendors include
Niton, Innov-X,
Oxford
instruments, and Rigaku,
RONTEC, and XCALIBUR
to name a few recently evaluated under EPAs Environmental Technology Verificaiton
(ETV) program. Visible near infrared (VIS/NIR) spectrophotometers can be
used to evaluate some plant and soil characteristics associated with fertility.
Portable units are available from vendors such as analytical
spectral devices (ASD) that can assist in evaluation of organic carbon,
total nitrogen, cation exchange capacity, sand fraction, silt fraction,
clay fraction, copper, zinc, chromium, nickel, cadmium, and manganese.
Q. How can I set up
an experiment for analyzing hyrdocarbons concentration in concrete?
A. The technique recommended is the same as those currently
in use by environmental analytical laboratories. The sample must be physically
ground or crushed to a powder to increase the effectiveness of the solvent
extraction. From there a method such as EPA SW-846 method 8015B or 8440
is recommended.
Q. Can TCE be fingerprinted
to evaluate two different sources when it cannot be done by concentration
measurement or variation in groundwater geochemistry?
A. After ruling out evaluation of sources by concentration and
groundwater geochemistry you are essentially left with isotope fractionation
as the only tool available to potentially differentiate between multiple
TCE sources.
You may be able to differentiate sources using isotope fractionation or
other forensic chemistry techniques. Forensic chemistry techniques are discussed
at http://zymaxusa.com and
http://www.environmentaldatapages.com/bmorrep.htm
.
Variations in manufacturing processes and source materials that affect carbon
and chlorine isotopes have been used to distinguish between different manufacturers.
See http://www.science.uottawa.ca/~eih/ch6/6chloro.htm.
Q. How do you prepare
1-benzyl-5-phenylbarbituric acid for FTIR - KBR pellet or something different?
Can you send me an FTIR scan of this compound?
A. There are hundreds of libraries that can be accessed through
the internet. However many require a membership fee. See http://www.spectroscopynow.com/Spy/basehtml/SpyH/1,1181,3-0-0-0-0-home-0-0,00.html
or http://www.acdlabs.com/products/spec_lab/exp_spectra/spec_libraries/fdm_ir.html#organic.
A good resource for available databases can be found at http://www.lohninger.com/spectroscopy/dball.html
Some spectra may be downloaded for free at http://www.aist.go.jp/RIODB/chem.html.
Q. I'm interested in finding an updated field sampling
technique and analytical method for the quantification of dissolved gases
in groundwater. I'm not sure if something of this nature exists. I am looking
for something that gives good quality results but doesn't cost as much as
traditional analytical costs for these gases. Any ideas?
Thanks for your attention to this matter.
A. There are a variety of traditional
analytical methods available for dissolved gases. Since you have not provided
actual gas names for compounds you are interested in we will assume you would
like traditional gases such as dissolved oxygen and those applicable to monitored
natural attenuation (MNA) projects such as carbon dioxide, methane, ethane,
ethene.
Other compounds of interest
can be fuel breakdown products such as acetylene, iso-butane, n-butane, propane, and propene
or chlorinated solvent daughter products such as trichloroethene,
1,2 dichloroethene, and vinyl chloride.
Dissolved oxygen can be monitored using field analytical
technologies such as a water quality meter provided by YSI www.ysi.com
or Horiba http://www.horiba-water.com/am.html,
and can also be evaluated using colorimetric test kits such as those provided
by Hach http://www.hach.com/.
Currently there are no colorimetric
or other simple field analytical techniques to evaluate dissolved concentrations
of carbon dioxide, methane, ethane, ethene. Field portable gas chromatographs (GC) with
electron capture detectors (ECD), photo-ionization detectors (PID), and flame
ionization detectors (FID) such as those available from Photovac
www.photovac.com
and SRI www.srigc.com are available to provide quantification
of most dissolved gasses for environmental applications.
Q. What would be
the cost effective analytical approach for determining if PAHs
in shallow soil samples at a LUST site are associated with fill material or
are actually the result of either a release or a spill of diesel fuel?
A. We would suggest the use of GC/MS
operated in the selected ion monitoring (SIM) mode to identify the types and
concentrations of polynuclear aromatic hydrocarbons (PAH) in the shallow soil
and samples associated with the diesel spills. Most fuel types contain varying
concentrations and types of PAHs (naphthalene, benzo (a) pyrene, chrysene) and the ratio of these PAHs in a particular sample can be used to distinguish different
fuel types or contaminant sources. GC/MS techniques for analysis of PAHs
includes EPA SW-846 method 8270 http://www.epa.gov/epaoswer/hazwaste/test/8_series.htm
[operation in the selective ion mode (SIM) allows the user to achieve lower
detection limits and avoid common interferences].
If fingerprinting fuel types
to determine potentially responsible parties (PRP) is the goal, then several
forensic chemistry techniques are also available (http://www.dpra.com/index.cfm/m/12).
Analysis of crude oil and petroleum product fractions using GC/MS has been
used by a number of consulting firms and laboratories. The Zymax
website http://zymaxusa.com/
has a lot of useful information concerning GC/MS analysis of crude oils and
petroleum products for forensic chemistry applications. GC/MS, although a
more costly method, can also be used to qualitatively and quantitatively evaluate
different fuel products (see http://www.dpra.com/index.cfm/m/147).
Although this technique is not as commonly used, GC/MS analysis will allow
the user to identify different hydrocarbons in a complex fuel mixture.
A simple weight of evidence
approach can be used to evaluate the likelihood that PAHs in the shallow fill are associated with the diesel release.
A simple procedure outlining this process is as follows.
1) Analyze several shallow
fill samples and several diesel contaminated soil/ product samples from the
site for PAHs.
2) In accordance with EPA
statistical guidance use a proxy value of one half the quantitation limit for any non-detected
values
2) Normalize all results
to benzo (A) pyrene or
another carcinogenic PAH (that is divide the concentration of each PAH compound
in the sample by the concentration of benzo (A)
pyrene in that sample to develop PAH ratios rather
than use absolute values)
3) Develop correlations
for each shallow subsurface sample vs. each diesel sample using all 16 PAH
compounds (normalized to benzo (A) pyrene).
If the correlation coefficients (R2) approach 1 (0.8 or better
show a strong correlation), then the materials likely came from a similar
process or have a common origin. Correlation coefficients approaching 0 indicate
that the materials are very different in composition and it is very unlikely
that they came from a similar process or have a common origin.
4) Finally, you can use
bar charts to evaluate similarities in PAH ratios to compare samples from
the shallow surface and those from the diesel impacted soil. If the materials
are similar in nature then they will have very similar PAH ratio patterns
for each of the 16 individual PAH compounds. For example two materials with
a likely common origin will have naphthalene as the highest concentration,
followed by phenanthrene, followed by acenaphthene, and so on and would also have negligible amounts
of the same compounds such as dibenzo (A,H) anthracene, benzo (B) fluoranthene, and indeno-(1,2,3-CD)
pyrene for example.
5) Any shallow soil samples
with strong correlations to diesel samples and displaying very similar PAH
patterns are likely the result of a diesel release and not that of the fill
material.
Q. Is there a simple
test for lead that can be done in the classroom either colorimetrically
or gravimetrically?
A. There are many colorimetric test
kits for available for lead; however, the matrix (paint, soil, water, tissue)
you are interested in evaluating is unclear. Colorimetric kits that provide
non quantitative results (yes/no lead is present) for paint samples include
http://www.leadinspector.com,
http://www.leadcheck.com/
Colorimetric kits that provide
non quantitative results (yes/no lead is present) for water include http://www.watersafetestkits.com/html/drinkingkits.asp
Examples of quantitative
gravimetric methods for the analysis of lead in classroom teaching applications
can be found at http://chem.lapeer.org/Chem1Docs/LeadAnal.html
and http://www.chem.tamu.edu/class/majors/experimentnotefiles/notes18.htm
Q. Method &
use of Dr/2400 Spectrophotometer, principal of operation
A. The question
concerning Hach’s DR2400 spectrophotometer is unclear.
The DR2400 can be used to provide quantitative analysis for a variety of Hach test kits. We have provided several links below where
you can obtain user information, products specifications, procedures, and
instrument manuals for the DR2400 115VAC and DR2400 230VAC models. Or visit
www.hach.com
for more information.
Hach - DR/2400 Portable Spectrophotometer
Hach - Download Documentation - DR/2400 Portable Spectrophotometer
Manuals