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o
United States
Environmental Protection
Agency
Office of Water
(WH-552)
EPA-821-R-93-014
September 1993
wEPA Oil and Grease Workshop
Norfolk, Virginia
May 4,1993
Printed on Recycled Paper
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DISCLAIMER
This report has been reviewed by the Analytical Methods Staff of the EPA Office of Water. It is in-
tended to inform the public about EPA's efforts to replace Freon-113 in Agency analytical methods.
Mention of company names, trade names or commercial products does not constitute endorsement or
recommendation for use.
Questions or comments regarding this report should be addressed to:
William A. Telliard, Chief
Analytical Methods Staff
Engineering and Analysis Division (WH-552)
Office of Science and Technology
Office of Water
401 M Street, S.W.
Washington, D.C. 20460
ACKNOWLEDGEMENTS
This report was prepared under the direction of William A. Telliard with assistance from the Environ-
mental Services Division of DynCorp Viar, Inc. (under EPA contract no. 68-C9-0019).
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MEETING SUMMARY
OIL AND GREASE WORKSHOP
NORFOLK, VIRGINIA
MAY 4, 1993
ANALYTICAL METHODS STAFF
ENGINEERING AND ANALYSIS DIVISION
OFFICE OF SCIENCE AND TECHNOLOGY
OFFICE OF WATER ,
U.S. ENVIRONMENTAL PROTECTION AGENCY
WASHINGTON, D.C. 20460
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Introduction
The Analytical Methods Staff of the Office of Science and Technology's Engineering and Analysis
Division (within the U.S. EPA Office of Water), held a public workshop on the subject of the Oil and
Grease Freon Replacement Study in conjunction with the 16th Annual Symposium on the Analysis of
Pollutants in the Environment.
The "Oil and Grease Workshop" was held on May 4, 1993 at the Norfolk Marriott Waterside
Hotel in Norfolk, Virginia. The workshop was intended to inform the public about EPA's efforts to find
a replacement for Freon 113 in its analytical methods for oil and grease and to provide a forum for public
comment. The date, time, place and purpose of the workshop were advertised in the Federal Register
on April 19, 1993.
The Freon Replacement Study, is more fully described in a report entitled Preliminary Report of
EPA Efforts to Replace Freon For The Determination of Oil and Grease, EPA-821-R-93-009, June 1993.
Briefly, EPA is seeking a replacement solvent for Freon 113 in three Agency methods for "total
recoverable oil and grease" because production and sale of Freon 113 and other Class I ozone depleting
substances will be banned by January 1, 1996 under both the Clean Air Act Amendments of 1990 and
the Montreal Protocol on Substances That Deplete the Ozone Layer. The Freon Replacement Method
Study is a cooperative effort among the EPA Offices of Water, Solid Waste, and Air and Radiation, with
the voluntary participation of a number of private companies. The first phase study involved exploration
of the use of five alternative solvents and two alternative techniques, tested on a suite of actual industrial
and commercial aqueous and solid waste samples. The preliminary results of EPA's statistical analysis
of the Phase I study data and information about alternative techniques were presented at the workshop.
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Meeting Summary
This document summarizes the information presented at the workshop by EPA and invited
speakers, as well as questions and comments from the audience. The workshop agenda is attached as
Appendix A. The speakers' visual aids are presented as Appendices B through I.
Freon Replacement Study, Phase I Study Results:
and Technology
William A. Tettiard, U.S. EPA Office of Science
The first speaker was William A. Telliard, Chief of the Analytical Methods Staff, within the
Office of Water's Engineering and Analysis Division. Mr. Telliard is also responsible for direction of
the Freon Replacement Study discussed at the workshop.
Mr. Telliard reviewed the regulatory history of chlorofluorocarbons, including the 1990 Clean
Air Act Amendments (CAAA) and the Montreal Protocol on Substances that Deplete the Ozone Layer.
He noted that Freon 113, the solvent used in the oil and grease measurement, is regulated by the CAAA
and the Montreal Protocol, and will be phased out of use by 1996.
He then described Phase I of the Freon Replacement Study. The purpose of Phase I was to
continue the Agency's investigation of replacement solvents to identify a solvent that yields results
equivalent to Freon 113, or failing that, to select a solvent(s) or alternative technique(s) for further study.
The five alternative solvents evaluated in Phase I were w-hexane, n-hexane/methyl tertiary-butyl ewer
(80:20), methylene chloride, perchloroethylene, and DuPont 123 (2,2-dichloro-I,l,l-trifluoroethane.)
Mr. Telliard noted that oil and grease is a "method-defined" parameter, that is, the result obtained
depends on the solvent used.
Mr. Telliard indicated the scope of the problem that EPA faces in changing the oil and grease
method by pointing out that oil and grease is a regulated parameter in approximately 10,500 National
Pollutant Discharge Elimination System (NPDES) permits, and in effluent guidelines for 25 industries.
He stated that in order to obtain realistic results, Phase I of the study tested "real world" samples from
39 plants in 24 industrial categories, including approximately 41 aqueous wastes and-30 solid'wastes.
These samples represented oil and grease of animal, vegetable and mineral (petroleum) origin. He noted
mat all of die industrial plants that had been visited and sampled were effectively removing oil and grease
from their effluents with the treatment equipment they had installed.
He then discussed the preliminary results of the statistical analysis of the study data. He began
by noting that the alternative techniques tested were solid phase extraction (SPE) cartridges, SPE disks,
and infrared methods. He emphasized that the samples tested with each of the alternative solvents and
methods were taken from the same set collected from the 39 plants. Mr. Telliard then reviewed the
statistical evaluation of oil and grease measurements made with the five alternative solvents, using
separatory funnel extraction for aqueous samples and Soxhlet and sonication extraction for solid samples.
He presented nine sets of results:
1. Separatory Funnel Extraction
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la. All aqueous samples
Ib. Petroleum-contaminated aqueous samples
Ic. Non-petroleum (animal fat or vegetable oil) contaminated aqueous samples
2. Soxhlet extraction
2a. All solid samples
2b. Petroleum-contaminated samples
2c. Non-petroleum-contaminated samples
3. Sonication Extraction
3a. All solid samples
3b. Petroleum-contaminated samples
3c. Non-petroleum-contaminated samples.
In reviewing the preliminary statistical evaluation of the data, Mr. Teliiard noted that no solvent
was equivalent to Freon 113 for all aqueous samples (la) or for petroleum-based aqueous samples (Ib),
but that both n-hexane and perchloroethylene had yielded results equivalent to Freon 113 for non-
petroleum-based aqueous samples (Ic). He further stated that no solvent was equivalent to Freon 113
using Soxhlet extraction when all samples were considered (2a), nor when only non-petroleum samples
were considered (2c). However, both n-hexane and the 80:20 mixture of n-hexane and MTBE were
equivalent to Freon 113 when only petroleum samples were tested (2b.) Lastly, he reviewed the
statistical results for the sonication extraction, which is being considered as an alternative to Soxhlet
extraction. The results for the five solvents using sonication were compared to the results of Soxhlet
extraction using Freon 113. The results showed that perchloroethylene was equivalent to Freon 113 for
all solid samples (3a) and that perchloroethylene, DuPont 123 and Freon 113 itself were equivalent to
Freon 113 using Soxhlet extraction for petroleum-contaminated solid samples (3b.) No solvents were
equivalent to Freon 113 using Soxhlet for the non-petroleum samples (3c.) Mr. Teliiard's presentation
materials may be found in Appendix B.
Mr. Teliiard then introduced the next speaker, Joseph Slayton of EPA Region III, Central
Regional Laboratory. Mr. Slayton was the first of four speakers who presented information on the use
of solid phase extraction (SPE) as a substitute for the separatory funnel extraction specified for aqueous
samples in the current EPA methods.
Oil and Grease Analysis Using Solid Phase Extraction Columns: Joseph Slayton, U.S. EPA, Region
HI, Central Regional Laboratory
Mr. Slayton described work performed on eight samples with an early version of the SPE
cartridges marketed by Varian Sample Preparation Products. He began with a summary of the SPE
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method used by Region III for the study. He then compared the boiling points of the six solvents used
in the Phase 1 study, and noted that the high water bath temperature needed for perchloroethylene (90 °C)
makes it an unlikely substitute for Freon 113, due to the losses of volatile materials. Mr. Slayton then
presented the experimental set-up originally used by Varian, that was derived from EPA Method 1652.
He described some difficulties with this apparatus, mainly a large amount of surface area in glassware
and tubing, with the attendant potential for analyte losses. He then described an experimental set-up
taken from EPA Method 525 that also was not satisfactory due to the need to transfer the sample from
the original container to a separatory funnel. Mr. Slayton described an improvement to the Method 525
SPE apparatus, developed by Varian, that involved an "adapter cap" that replaces the original sample
bottle cap and fits directly into the SPE cartridge. This was the apparatus that Region III used for the
Phase I study.
He then turned to a description of Region Ill's SPE feasibility study, and listed the
accomplishments, which included improvements in the SPE apparatus, but provided little data for Phase
I of the Freon Replacement Study. He described experiments conducted with corn oil spiked into one-
liter samples of water, which yielded acceptable results. This experiment also produced data that
suggested that 2 mg/L would be a reasonable limit for blanks. He then presented data on weekly 50
mg/L spikes that showed improved results over time, demonstrating the technique-dependency of the
method.
Mr. Slayton next presented the results for eight samples from the Phase I study. The Region III
laboratory was unable to analyze four of the eight samples they attempted due to high (> 60 mg/L) solids
contents, which tended to clog the SPE cartridges. He then described problems encountered in the study
and potential solutions. Problems included false positives, false negatives and the cartridge clogging
problem. Finally, he made a number of suggestions to improve the present EPA oil and grease method
(413.1), including blank contamination limits, quantitation limits, specifications for handling negative
results and blanks, multiple weighings to constant weight, use of "S" class weights, reporting
requirements, instructions on how to take a grab sample, and additional laboratory QC (initial
demonstration of capability, duplicates and spikes.) Mr. Slayton's presentation materials may be found
in Appendix C.
Evaluation of Solid Phase Extraction Columns for Analysis of Oil and Grease in Aqueous Samples:
Rex Hawley, Varian Sample Preparation Products
The second speaker on SPE was Rex Hawley of Varian Sample Preparation Products. He
described work done with SPE cartridges that were improved on the basis of Region Ill's work. Mr.
Hawley stressed simplicity, error reduction and low cost, as well as reduced solvent usage as advantages
of using SPE. Mr. Hawley presented the apparatus used in Varian's work, including both common
laboratory apparatus and specialized components. He outlined the basic procedure used to prepare the
equipment and analyze a sample. He discussed an evaluation of filter materials and a technique to remove
water from the eluent without using sodium sulfate (an Aquasep filter.) He presented the results of tests
run on synthetic standard samples (Mazzola oil in deionized water) versus the results obtained by the EPA
separatory funnel method, and indicated that good agreement was obtained. Comparable results were also
obtained for samples collected by the Los Angeles County Water District. Mr. Hawley then discussed
the results of analyses of samples provided by EPA. Some of these samples were difficult to analyze
because of high solids contents which caused long elution times. This problem was circumvented by the
use of several SPE columns per sample. He then discussed the solvents used, their polarity and elution
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properties, and pointed out that of the three tested, n-hexane yielded results closest to Freon 113.
Finally, Mr. Hawley discussed the distinction between extraction solvents in liquid/liquid extraction and
elution solvents in SPE. Mr. Hawley's presentation materials may be found in Appendix D.
'* Question and Answer Period
Question: Mr. Jack Cochran of the Hazardous Waste Center asked how results in the range of 500
mg/L could be obtained if the capacity of an SPE cartridge is about 1 % (SO mg)?
Answer: Mr. Hawley replied that 10% was a more realistic estimate of cartridge capacity, and that
the experimental set-up he had used, which introduces the eluting solvent into the sample
bottle itself, was the reason for the recoveries seen.
Question: Mr. Cochran then asked if any problems with drying of the filter due to phase separation
caused less efficient extraction.
Answer: Mr. Slayton replied that brief periods of dryness did not seem to have any effect. Mr.
Hawley added that with the three-dimensional or "depth-filter" approach, drying was not
a problem. Mr. Slayton also observed, in response to Mr. Cochran's earlier question,
that 500 mg was a reasonable result since Mr. Hawley had used multiple cartridges for
some samples.
Question: Mr. Dave Schreiner, with City of Phoenix Wastewater, asked if differences in the
performance of the CIS filter had been observed with petroleum, as opposed to non-
petroleum, contaminated samples.
Answer: Mr. Hawley replied that that would depend on the solvent used.
Mr. Telliard then introduced the next speaker, Craig Mark el I.
Oil and Grease Analysis in Wastewater Using Solid Phase Extraction Disks: Craig MarkeU, The 3M
Corporation
The third speaker on SPE was Craig MarkeU of the 3M Corporation, who discussed work done
with their 47mm and 90mm SPE disks. He began by reviewing the principles of solid phase extraction,
in comparison to liquid/liquid extraction. He then outlined the method used with the SPE disks,
emphasizing the filter aid and the drying step using sodium sulfate. Sodium sulfate was eliminated from
the sample using a syringe-end filter. He presented a diagram of an SPE disk in its holder with the filter
aid material on top. Mr. Marked discussed the capacity of SPE devices, which a member of the audience
had asked about during the Q&A period, and noted that the capacity increases with increasing compound
hydrophobicity. He stated that the capacity of a SPE disk could be up to 20% of its weight. Turning
to selectivity, he noted that different factors are at work for separatory funnel and SPE techniques. He
presented results for five solvents on three different samples, showing that generally higher results were
obtained with more polar solvents. Mr. MarkeU then presented results of the analysis of some of the
Phase I study samples, showing general correlations for two groups of high and low concentration
samples. He presented precision data for the SPE disk method, which ranged from 0 to 23% difference.
He concluded by saying that, while nothing will duplicate Method 413.1 (the EPA oil and grease method
using Freon 113 and a separatory funnel) exactly, SPE disks do work for oil and grease. Mr. Markell
mentioned some preliminary work on alternative techniques such as Oilsorb fibrous mats. Mr. MarkeU's
presentation materials may be found in Appendix E.
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Oil and Grease Analysis Using Solid Phase Extraction Disks and Alternative Solvents: Miriam
Roman, Waste Management Environmental Monitoring Laboratories
Ms. Roman presented results of research carried out at WMX Laboratories using EMPORE disks
to extract oil and grease. Wesson oil was spiked into water using either methanol or acetone as a carrier
solvent. Methanol was tried first, as it is used to treat EMPORE disks, but it did not work well.
Acetone provided a good dispersion of the oil in water. Six one-liter water samples were spiked with
oil at 20 mg/L, acidified, drawn through the EMPORE disks with a vacuum, then eluted with ethyl
acetate. Recoveries of the oil were good in these experiments. However, evaporation in the steam bath
was slow because ethyl acetate has a boiling point of 66 °C, and the bath was kept at 70 °C.
Acetone was used as the eluting solvent next, since in solid phase extraction the eluting solvent
need not be insoluble in water. Extra precautions were taken to ensure that the acetone eluent was free
of water to avoid carry-over of water or sulfuric acid. After elution, the acetone was dried with sodium
sulfate. Results of experiments with acetone yielded good results, with a standard deviation smaller than
that obtained with ethyl acetate.
Evaluation of Oil and Grease Samples using NDIR and Flon S-316: Jim Vance, Horiba Instruments,
Inc.
Mr. Vance made a presentation on the operation of the Horiba OCMA 220 nondispersive infrared
analyzer, including a step-by-step summary of the method used. The method is based on EPA method
413.2, the infrared technique for oil and grease, and it is completely automated within the instrument.
A proprietary chlorofluorocarbon solvent, Flon S-316, is used.
He then showed results of analyses for Phase 1 study samples. First, he described difficulties with
the extraction of some of the more challenging samples. These samples were not amenable to the
instrument's internal extraction mechanism due to the formation of emulsions. Sonication was tried, but
did not work because it emulsified the oil in the water. Emulsion-free extractions were obtained by
shaking samples with solvent in 40 mL VOA vials.
Results for 38 samples showed that 17 results were higher than those obtained with the Freon 113
separatory funnel procedure, 17 were lower, and 4 were below 5 mg/L by both methods. Using the
Horiba instrument, results down to as low as 0.2 mg/L were obtained. Mr. Vance then compared the
precision of results obtained with the two techniques: 3 samples were within 20 mg/L, 7 were within
10 mg/L, and 11 were within 5 mg/L. He concluded that about half of the results were comparable to
the Freon 113 separatory funnel data. He added that extraction efficiency was measured on one sample
that had a result of about 400 mg/L, and was found to be 98.2%.
Mr. Vance then described the benefits of using the Horiba NDIR analyzer. These included low
cost, wider range of materials measured, portability, shorter analysis time, ability to react to changing
water systems quickly, reproducibility of data, low solvent use and the ability to reclaim solvent. He
concluded that this method is viable for the measurement of oil and grease. Mr. Vance's presentation
materials may be found in Appendix F.
Question and Answer Period.
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Question: Mr. Dan Caudle, of Conoco, asked if the IS mL figure mentioned for solvent usage per
sample includes the amount used to clean the instrument between measurements.
Answer: Mr. Vance replied that, due to the cost of solvent, the instrument is only cleaned if an
off-scale reading is obtained. Otherwise, three aliquots of each sample are measured, and
the third one is used as the reading. The zero is checked periodically.
Mr. Telliard then introduced the next speaker, Gerald DeMenna of Chem Chek Consulting/Buck
Scientific. .
Determination of Oil and Grease by Evaporation of Solvent in a Quartz Cell in an Infra-red
Spectrophotometer: Gerald DeMenna, Chem-Chek Consulting/Buck Scientific
Mr. DeMenna described a procedure developed in his laboratory that is designed to yield results
similar to the EPA gravimetric method now in use. The new method uses the same sampling and
extraction methodology as before, but uses a different technique to make the final determination. In the
proposed procedure, a smaller amount of sample (100 mL) and solvent (lOmL) are run through a paint
mixer to extract oil and grease. A 250 uL portion of the extract is pipetted into a quartz plate with a 300
uL cavity. The solvent is evaporated away at 15+1-2 °C, and the absorbance of oil and grease measured
at 3.4 microns (2950 wave numbers) in an infrared spectrophotometer.
Mr. DeMenna presented the results from three environmental samples taken in New Jersey,
comparing EPA Method 413.1, the new quartz plate/evaporation method and an IR method using a 10
mL quartz cell, similar to EPA Method 413.2 (all techniques were performed with Freon 113.) His
results showed that his new quartz plate/evaporation method gave results slightly higher than EPA Method
413.1, and slightly lower than the quartz cell/IR method (Method 413.2). Precision was comparable for
the three methods, and spike recoveries were good.
Mr. DeMenna then presented some data comparing results obtained with Freon 1 13 to methylene
chloride. The latter solvent gave somewhat higher results. He then presented performance specifications
on the new method, including sensitivity, detection limit and linearity. He concluded by saying that the
new technique is adaptable to all IR photometers with an open sample compartment, and that additional
studies with other solvents and a variety of samples are underway in his laboratory. Mr. DeMenna 's
presentation materials may be found in Appendix G.
Question and Answer Period
Question: Mr. Jack Cochran of the Hazardous Waste Center asked Mr. DeMenna if the more
volatile constituents of oil and grease might be lost during the evaporation step in the
proposed procedure.
Answer: Mr. DeMenna acknowledged that this might happen.
Question: Ms. Kay Gamble of McGinnes Laboratories asked if Mr. DeMenna had tried his new
procedure on samples with oil and grease at close to minimum detectable levels.
Answer: Mr. DeMenna stated that he had not yet done so, but that based on the results obtained
so far, he would be conducting further studies of method specifications and alternative
solvents.
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Question: Mr. Schreiner asked if the new method could be used for a waste stream containing fatty
acids.
Answer: Mr. DeMenna answered that it could be used for any kind of hydrocarbon material with
an IR absorbance between 2925 and 2960 wave numbers.
Question: Mr. Schreiner then asked what Mr. DeMenna used to spike his samples in the studies
shown. ,!
Answer: Mr. DeMenna answered that he used the "EPA mixture" of isooctane, hexadecane and
chlorobenzene.
Strategy Options for Regulating Oil and Grease: William A. Tettiard, U.S. EPA Office of Science
and Technology
Mr. Telliard then discussed the policy options being considered at EPA to resolve the problem
of Freon 113 use in the Agency's oil and grease methods.
The first option he presented was to stop monitoring oil and grease, since 1) it may already be
regulated by other measurements, and 2) it may not be needed at the present since the problems it was
originally designed to detect (such as problems with Imhof tanks) no longer exist.
The second option he presented was to obtain a waiver under the Clean Air Act Amendments of
1990 to allow continued use of Freon 113 for this purpose. He noted, however, mat with the
approaching ban and the high cost of Freon 113, this might not be a viable option.
The third option he presented was to develop a correction factor to correct results for an
alternative solvent to what would have been obtained using Freon 113. He stated that this could take the
form of demonstrating the performance of a given solvent and then reverting to that solvent at the time
of permit renewal. He mentioned that this approach would be in line with the current concept of
"performance-based" methods.
Hie fourth option was for EPA to select one solvent or extraction technique that produces results
closest to Freon 113. At this point, the likely choice would be n-hexane.
The fifth option he presented was to give further consideration to alternative techniques, such as
solid phase extraction, that use less solvent. He noted that such techniques are in line with the Agency's
push for pollution prevention and would lower solvent disposal costs.
Mr. Telliard then discussed modernizing the present EPA oil and grease methods along the lines
of Mr. Slayton's suggestions. This would include performance specifications similar to those in the EPA
600 series methods. Finally, he raised to the issue of cost in doing the measurement by other procedures,
noting that many NPDES permit holders may have difficulty with the expense of sophisticated equipment.
Mr. Telliard's presentation materials may be found in Appendix H.
»*
Mr. Telliard then opened the floor for questions and discussion.
Question and Answer Period
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Question: Mr. Dan Caudle of Conoco asked for clarification of the issues raised at the workshop.
He identified three issues that had been raised: if oil and grease continues to be
measured, what solvent to use, how to minimize use of that solvent, and what analytical
finish to use. He asked for a discussion of how these issues fit together.
Answer: Mr. Telliard answered that oil and grease would continue to be measured, and that the
solvent of choice at this point would be n-hexane. He said that the next choice would
be the n-hexane/MTBE mixture, but that he was concerned with the safety issue of using
ether in the laboratory. He noted that the results obtained in the Phase I study with n-
hexane were consistently lower than those obtained with Freon 113, so that such a
solvent substitution would be unlikely to cause any permit holder to be driven out of
compliance. Addressing the analytical finish issue, he stated that it would still be
gravimetric, but that infrared would be considered. He also stated that under a
"performance-based" methodology scenario, any of the techniques discussed at the
workshop would be allowed if the method specifications could be met. He qualified this
by saying that such an approach would be problematic from an enforcement standpoint,
so that the use of n-hexane was most likely.
Question: Mr. George Stanko of Shell Development Company recalled Mr. Telliard's statement in
his earlier talk that oil and grease levels were very low at all of the sampled facilities,
and suggested that the oil and grease measurement no longer served any purpose and
should be abandoned.
Answer: Mr. Telliard replied that he proposed elimination of the method. EPA believes,
however, that monitoring of oil and grease is what keeps the effluents clean, and that
therefore the monitoring would have to continue.
Question: Mr. Steve Naughton of Coyne Textiles commented that he would be submitting data to
EPA to show that the reproducibility of results obtained by different commercial
laboratories on identical split samples was poor. He suggested that a rigorous evaluation
of sources of variability in the oil and grease method was necessary. His second
comment was that from an engineering viewpoint, the fact that the oil and grease method
does not measure any specific substance, but just what is soluble in the solvent used,
makes achieving compliance extremely problematic.
Answer: Mr. Telliard thanked him and stated that if he did submit the data he mentioned, it would
be included hi the report of the meeting. (Mr. Naughton's submission is included as
Appendix I of this report.)
Question: Mr. Dave Clampitt of the Institute of Industrial Launderers commented that he would like
to see a methodology for taking composite samples, rather than grab samples, since that
would be more representative of his industry's effluents.
Answer: Mr. Telliard replied by explaining the historical reason for using grab samples
(prevention of losses of analyte on glass surfaces). He noted that composite sampling
would be worthwhile and probably cost-effective, and said that it might be evaluated in
Phase II of the study.
Question: Mr. Tom Randolph, of Randolph Consulting, asked about EPA's schedule for making
a decision.
Answer: Mr. Telliard answered that, due to the urgency of the approaching Freon 113 ban a
decision would be made by late summer or fall 1993.
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Question: Mr. Caudle noted that many of the problems with the current method stem from the fact
that it measures different substances in different effluents, and that some of what is
measured is not amenable to treatment. He suggested that a better definition of oil and
grease might be needed, and that several methods, rather than one, might therefore be
needed.
Answer: Mr. Tel Hard replied that the oil and grease method does need modernizing, and that a
better understanding of the present method would facilitate study of alternatives.
Question: Mr. Nathan Heldenbran, of Coke Refining, asked what correction factor should be used
for an effluent that has been "non-detect" for several years.
Answer: Mr. Tel Hard thanked him for this observation.
Question: Mr. Stanko asked to be reminded why oil and grease samples need to be preserved to pH
2 or less in the field, when no effluent is discharged at such a low pH.
Answer: Mr. Hawley replied that the purpose is to avoid formation of emulsions and formation
of soaps at basic pH. Mr. Telliard added that the specification for preservation may be
changed to pH 2, rather than 2 or less, to avoid having to ship samples as hazardous
substances.
Question: Mr. Cochran asked if any consideration had been given to the fact that /i-hexane floats
on water, which makes separatory runnel extraction more time consuming.
Answer: Mr. Telliard replied that some thought had been given to this issue, but that there was
no way to avoid this difficulty.
Question: Mr. Keith Smith, of Analytical Services, Inc., Atlanta, Georgia, suggested using pentane
rather than n-bexane since its boiling point is closer to that of Freon 113.
Answer: Mr. Telliard thanked him for this observation.
Question: Mr. Cochran asked that relative standard deviations be included in the next version of the
study report.
Answer: Mr. Telliard promised to do so.
Mr. Telliard closed the workshop by thanking the attendees for coming, and asked for any other
comments or information they might have to share before the anticipated time of the decision on the oil
and grease method.
10
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Appendix A
Workshop Agenda
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OIL AND GREASE WORKSHOP
TUESDAY, MAY 4, 1993
Agenda
Chairman: William A. Telliard
1:30 - 2:00 Freon Replacement Study, Phase I Study Results
William A. Telliard, U.S. EPA Office of Science and Technology
2:00 - 2:15 Oil and Grease Analysis Using Solid Phase Extraction Columns
Joseph Slayton, U.S. EPA, Region III, Central Regional Laboratory
2:15 - 2:30 Evaluation of Solid Phase Extraction Columns for Analysis of Oil and
Grease in Aqueous Samples
Rex Hawley, Varian Sample Preparation Products
2:30 - 2:45 Oil and Grease Analysis in Wastewater Using Solid Phase Extraction
Disks
Craig Markell, The 3M Corporation
2:45 - 3:00 Oil and Grease Analysis Using Solid Phase Extraction Disks and
Alternate Solvents
Miriam Roman, Frank Dias, Barbara Hill, Waste Management
Environmental Monitoring Laboratories
3:00 - 3:15 Evaluation of Oil and Grease Samples using NDIR and Flon S-316
Jim Vance, Horiba Instruments, Inc.
3:15 - 3:30 Determination of Oil and Grease by Evaporation of Solvent in a Quartz
Cell in an Infra-red Spectrophotometer
Jerry DiMenna, Buck Scientific
3:30 - 4:30 Strategy Options for Regulating Oil and Grease
William A. Telliard, U.S. EPA Office of Science and Technology
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Appendix B
Presentation Materials
"Freon Replacement Study, Phase I Study Results"
William A. Telliard, U.S. EPA Office of Water
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Appendix C
Presentation Materials
"Oil and Grease Analysis Using Solid Phase Extraction Columns"
Joseph Slayton, U.S. EPA Region in
-------
-------
Oil and Grease Workshop
Solid Phase Extraction
Joseph Slayton
US EPA ORL Region III
Jennifer Molnar
Environmental Assistance Team
Lockheed (LESAT)
Scott Dillon
University of Maryland
-------
Summary of SPE Method:
* Sample Acidified in Field (pH < 2 ).
* Add 10 mL Isopropyl Alcohol.
* SPE Column Conditioned/Activated (ispropyl/De-i)
* Sample Extracted thru SPE Cartridge
EnvirElut (Varian SPP):
- Bonded C18 Silica Cartridge.
= 5gms.
= 3/4" I.D. (2 cm).
= 4" Length (10 cm).
- Extracts (Fats, Oils, Greases, etc).
- Removes/Filters Suspended Solids.
* SPE Cartridge Fluted (10-15 mL Organic Solvent)
* Solvent Collected in Pre-Weighed Vessel.
* Solvent Evaporated using A/2 Blow Down (N-EVAP).
* Residue Weighed.
* O & G mg/L = (Residue mg - Blk mg)
Sample Vol. L
-------
O&G SPE Feasibility Study:
8 Samples * In Triplicate (3) * Testing 6 Solvents = 144
Solvent
Boiling Pt Water Bath
Freon 113
1, 1 ,2-Trichloro-
1 ,2,2-Trifluoro- •
Ethane
CI2FCCCIF2
n-Hexane
C6H14
80/20
n-Hexane/M7BE
Methy TertButyl
Ether
C5H12O
Dupont 123
2,2-Dichloro-1,1,1-
TriFluoro Ethane
CI2CHCF3
Methytene Chloride
CH2CI2
Perchloroethytene
Tetrachloroethylene
CI2CCC12
48 C
68 C
68/55
99
* *
28 C
40 C
121 C
40 C
40 C
40 C
40 C
40 C
90 C
-------
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L,
1
*
I
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2 Liter
separator/
funnel
125ml
solvent
reservoir
ground glass T 14/35
LSE cartridge
rubber stopper
No. 18-20luer-lok
syringe needle
1 liter
vacuum flask
A. Extraction apparatus
-------
One Uter Sampling Bottle
(Wide Mouth—70 mm)
Adapter Cap (70 mm)
Adapter Cap
damping Shodder
EnvrBut Cartridge
rubber stopper
No. 18-2O luer-lok
syringe needle
1 liter
vacuum flask
A. Extraction apparatus
-------
This SPE Feasibility Study:
* Provided Improvements for Existing SPE Techniques.
= Draft EPA 1652 (Oil and Grease).
= EPA 525.1 (Organics in Drinking Water).
= Manufacturer's Instructions for EnvirElut
Tested "Adapter Cap"
Developed by
Varian Sample Preparation Products
= Replaces Original Sample Container Cap.
= Allows Use of Sample Container as Ext. Vessel.
Provided Little Data for Comparability of Alternate
Solvents for SPE O&G
-------
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Problems
O&G SPE Feasibility Study:
"False Positives": &18 Bonded! Silica bonds additional
mater/a/, e.g., dyesf "semivolatile organics".
999 999
* m 9 t * m
CIS Bonded Siflca
frtts.
??? Production QC ???
??? Additional SPE Pre-rinses ???
"False Negatives": "Difficulty iff extracting sample container:
(DOES 1 % ISOPROPYL ALCOHOL (pH <2)
ExtALL TYPES OF OIL AND GREASE ?)
??? Acetone &/or hydrophobic
membranes ???
Must extract two, "caps" (sample & adapter).
??? New Adapter Cap ???
"Unable to Analyze": Cartridges ClOQ with suspended
solids (> 60 mg/L).
??? Larger (Diameter) Cartridges ???
??? Extraction Disks ???
-------
Problems with 413.1 [ While we are at it ]
Issues Not Addressed:
* Max. allowable blank (2 mg residue ?).
* Quantitation Limits (5mg/L ?).
* Negative Results (blanks exceed samples).
* Negative Blanks (final < inital wt.).
* Necessity for multiple weighings, as with TSS
and how long must a reading remain constant.
* Necessity for Class "S" weights.
* Reporting:
= 7ess than values" (" < "in "MonthlyAve.?")
= number of significant figures.
* HOW TO TAKE A GRAB SAMPLE FOR O&G.
* Additional QC: "Initial Demonstration of Capability"
with performance specifications.
On-going:
Duplicates
Spikes
-------
-------
Appendix D
Presentation Materials
"Evaluation of Solid Phase Extraction Columns for Analysis
of Oil and Grease in Aqueous Samples"
Rex Hawley, Varian Sample Preparation Products
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Appendix E
Presentation Materials
"Oil and Grease Analysis in Wastewater Using
Solid Phase Extraction Disks"
Craig Markell, The 3M Corporation
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-------
-------
Appendix F
Presentation Materials
"Evaluation of Oil and Grease Samples Using NDIR
and Flon S-316"
Jim Vance, Horiba Instruments, Inc.
-------
-------
HORIBA
HORIBA INSTRUMENTS INCORPORATED
17671 Armstrong Avenue. Irvine, Cafifornia 92714
Phone: 1 (800) 4 HORIBA, FAX (714) 250-092'
In California phone (714) 250-4811
COMPARISON OF INFRARED ANALYSIS METHOD AND SOLVENT
FLON S-316 TO FREON-113
A total of 38 samples analyses were made with the Horiba OCMA-220
Infrared Analyzer and solvent Flon S-316. Comparing the data to the
Liq/Liq (A) Freon data we found the following:
17 samples (44.7%) were lower than the corresponding Freon measurement,
17 samples (44.7%) were higher than Freon
4 samples (10.5%) were measured as less than 5 mg/ L by both solvents,
The measured value was +/-
20 mg/L or less on 3 samples (7.8% of 38 samples)
10 mg/L or less on 7 samples (18.4%)
5 mg/L or less on 11 samples (28.9%)
A solvent extraction efficiency test was made using sample #23459.
The solvent extraction efficiency was calculated at greater than 98.2%
based on serial extractions of the sample.
-------
HORIBA
HORIBA INSTRUMENTS INCORPORATED Phone: 1 (800} 4 HORIBA, FAX (714) 250-
17671 Armstrong Avenue, Irvine. California 92714 In California phone (714) 250-4811
BENEFITS OF INFRARED SPECTROPHOTOMETRIC ANALYSIS
\
Cost per test: $0.28 per 15 ml solvent.
Wider range of hydrocarbons measured: 1 ppm to several percent,
Portability of analyzer: Compact & light weight
Shortened analysis time: 4 to 20 samples/ hour.
Ability to react to changing water system quickly: May be used
in the field to test on
site.
Reproducibility: Typically +/- 2 ppm
Amount of solvent required: 15 ml for most samples.
Solvent reclaimed directly: Put used solvent in Horit
solvent reclaimer.
-------
HORIBA
HORIBA INSTRUMENTS INCORPORATED
17671 Armstrong Avenue, Irvine, California 92714
SOLVENT
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
FLON S-316
EPISODE SAMPLE LAB- ID
4364
4366
4367
4368
4369
4370
4371
4372
4373
4374
4398
4400
4401
4402
4420
4421
4423
4422
4424
4425
4441
4442
4443
4444
4445
4445
4446
4447
4449
4450
4451
4452
4476
4476
22221 HORIBA
22223 HORIBA
22224 HORIBA
22225 HORIBA
22229 HORIBA
22231 HORIBA
22232 HORIBA
22233 HORIBA
22234 HORIBA
22236 HORIBA
22239 HORIBA
22241 HORIBA
22243 HORIBA
23106 HORIBA
23110 HORIBA
23111 HORIBA
23113 HORIBA
23116 HORIBA
23120 HORIBA
23121 HORIBA
23124 HORIBA
23457 HORIBA
23459 HORIBA
23461 HORIBA
23463 HORIBA
23466 HORIBA
23468 HORIBA
23470 HORIBA
23472 HORIBA
23473 HORIBA
23475 HORIBA
23477 HORIBA
23479 HORIBA
23480 HORIBA
23481 HORIBA
23482 HORIBA
23484 HORIBA
23485 HORIBA
BOTTLE
2120
2344
2444
2535
2944
3127
3228
3328
3430
3626
.3943
4143
4341
643
1027
1125
1327
1624
12055
12156
12457
45757
45957
46158
46358
46658
46858
47058
47258
47358
47558
47758
47958
48058
48158
48258
48458
48558
Phone: 1 (800) 4 HORIBA, FAX (714) 250-09
In California phone (714) 250-4811
MG/L#1 MG/L#2 MG/L#3
2.5
14.5
13.2
203
6.4
149
113
8.9
292
37
4.6
46
7.1
0
1
10.2
2
0
3.2
39.6
86.7
376
398
230
591
3.2
23.5
293
8.3
149
114
4
5.1
190
256
202
23
15
2.4
14.8
13.5
233
6.4
156
114
9.9
289
30
4.5
45
6.1
0
1
10.3
2
0
3.3
33
87.8
384
380
228
565
2.9
26.6
282
8.8
141
106
4
4.3
194
283
221
24
13
229
153
36.5
390
568
2.6
286
8.5
144
128
195
279
-------
-------
Appendix G
Presentation Materials
"Determination of Oil and Grease by Evaporation of Solvent
in a Quartz Cell in an Infra-red Spectrophotometer"
Gerald DeMenna, Chem-Chek Laboratories
-------
-------
MftY-2B-'93 12:25 ID:BUCK SCIENTIFIC TB_ N0:2038530569 tt!36 P01
Scientific
BUCK Scientific, Inc.
58 Port Point Street • East Norwalk, Connecticut 068S5 • (203) 8S3—9444
Hs. Lynn Riddick
EPA
Material from Oil & Grease lecture in Norfolk, VA
i
EMVIRONMEOTAL OIL £ GREASE
AMALYBIBt An Overview
2k NOVEL Technique for using LESS Freon
and non-Treon" solvents
[Using existing IR Photometers]
Gerald J. DeMenna, Chero-Chek Consulting
44 stelton Road, Piscataway, NJ 08854
[908] 752-7793
xeth. Annual EPA Meeting // 4 May 1993
Norfolk, Virginia
CURRENT METHODOLOGIES!
[l] Extraction and Gravimetric Isolation
of TPH materials
[2] Extraction and Liquid Cell IR Filter
Photometry of TPH (C-H) Absorptions
[3] Gas Chromatographic Separation
with FID Detection for TPH
PROPOSED PROCEDURES
For use with existing Infra-Red filter Photometers
optimized for the 3.4 micron / 2950 cm-l absorption
bands found in ALL hydrocarbon materials
without using large volumes of FREON or
using non-FREON type solvents (Methylene Chloride)
FAX No. 203453-0569 TELEX No. 643589 BUCK Sd ENUC
-------
J38Y-20-'93 12:26 IDiBUCK SCIENTIFIC
TEL NO:2038530569
8136 P0
PROPOSED PROCEDURES
[1] Prepare the sample and perform the
extraction per standard protocols
(SW-S46 / #9070-9071)
[2] Downscale the Volume or Weight of
FREON used for the extraction by
a factor of 2 to 10
[dependant on sample matrix]
[13 "Cast" a film of TPH material from
the FREON on a IR-Quartz "cavity" cell
INSTRUMENTATIONt
Model HC-404 Total Petroleum Hydrocarbon
analyzer
[Filter IR Photometer w/ 20 cm-i bandpass
at 3.42 microns]
Normal Analyses w/ 10mm. IR-Quartz
Liquid Cell using Freon-113
Purchased from BUCK Scientific, Inc.,
E. Norwalk, CT
PRINCIPLES:
Like the existing gravimetric
procedure, the "evaporation method"
will allow the Freon solvent to volatilize
and leave the TPH materials as a film
residue in a XR-transparent Quartz plate.
Standards and spikes carried through the
procedure are used for calibration
and recovery calculations.
-------
MPY-2&--93 12:26 ID: BUCK SCIENTIFIC TEL NO:2038530569 8136 PB3
BENEFITS of MS* PROCEDUREI
[1] Allows use of significantly lower
volumes of regulated solvents.
[2] Allows use of other suitable
solvents with similar partitioning
coefficients
[nethylene chloride for this study]
Evaluation of Method Correlation!
Tact three (3) varied types of
samples for TPH by:
[1] Gravimetric Technique
[2] IR Photometer v/lOmm. Liquid Cell
[3] IR Photometer w/ "cavity cell"
* MOTE - All extractions done with
Freon-113
sample #11 polymer Fabrication Plant,
Elisabeth, NJ / discharge line
Data from triplicate preps w/ statistics
with 5 PPM spike for recovery study
[1] GRAY [2] IR-LIQ [3) IR-EVAP
25 PPM 31 PPM 28 PPM
(5.5% RSD) (3.7% RSD) (4.2% RSD)
31 PPM 36 PPM 33 PPM
[spike recovery 99+% overall]
-------
MftY-20-'93 12:27 IDtBUCK SCIENTIFIC
TEL NO:2038530569
sample #2* Pharmaeutioal Xaufacturar,
Wilmington, DB / pond sludge
Data from triplicate preps v/ statistics,
with 50 PPM spike for recovery study
[1] GRAV
140 PPH
(3.9% USD)
[2] IR-LIQ [3] IR-EVAP
155 PPM
(2.4% RSD)
150 PPM
(3.2% RSD)
195 PPM 202 PPM 201 PPM
[epiXe recovery 97+% overall]
Sample fax Commeraial Development Site*
Westonester, NY / mixed soil corings
Data from triplicate preps w/ statistics,
with 10 PPM spike for recovery study
[1] GRAV
52 PPM
(4.1% RSD)
[2] IR-LIQ [3] IR-EVAP
55 PPM
(3.4% RSD)
S3 PPM
(3.0% RSD)
61 PPM 65 PPM 64 PPM
(spike recovery 98+% overall]
PRELIMINARY COMPARATIVE STUDYt
Freon-113 vs. Methylene Chloride
on the "cavity cell"
Sample: Machinery Shop effluent
Freon-113 CH2C12
87 PPM
(3.3% RSD)
91 PPM
(3.5% RSD)
-------
MflY-20-'93 12:27 ID:BUCK SCIENTIFIC
TEL NO:2038538569
8136 PBS
Performance Specification*
[based on 250uL aliquot in 5mm x 4mm
cavity in IR-Quartz plate]
Sensitivity: 1.5 PPM gives 0.004A signal
Detection Limit: 4 PPH gives 10% reproducibility
at approx. O.OIA
Linearity: Correlation of 0.96 up to 250 PPM
CONCLUSIONSS
This technique is adaptable to all
IK Photometric units with an open sample
compartment to allow use of the "cavity cell"
evaporation plate.
Additional studies with other solvents
and a variety of sample matrices
is required to fully develop the
potential usefullness of the method.
-------
-------
Appendix H
Presentation Materials
"Strategy Options for Regulation Oil and Grease"
William A. Tefflard, U.S. EPA Office of Water
J
-------
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-------
-------
Appendix I
Commercial Laboratory Oil and Grease Data
*
Steve Naughton, Coyne Textile Services
-------
-------
COYNE INTERNATIONAL
ENTERPRISES CORP
EXECUTIVE OFFICES:
P.O. Box 4854
uo Contend Avenue
Syracuse, New Vbrk 13221
(315)475-1626
BALTIMORE. MD
BECKLEY, WV
BETSY LAYNE. KY
BRISTOL. TN
BUFFALO. NY
BURLINGTON. VT
CHARLESTON, WV
CLEVELAND. OH
DU BOIS, PA
ERIE. PA
FAIRMONT. WV
HAZLETON, PA
HUNTINGTON, WV
JOLIET, IL
LEWISTON. ME
LONDON, KY
LONG ISLAND. NY
NEWARK, NJ
NEW BEDFORD. MA
PHILADELPHIA. PA
PITTSBURGH. PA
RICHMOND, VA
SCHENECTADY, NY
SEAFORD, DE
SMtTHBORO. NY
SYRACUSE, NY
TOLEDO, OH
WATERBURY, CT
WINCHESTER, VA
WORCESTER, MA
YORK, PA
COYNE TEXTILE SERVICES
June 29, 1993
Mr. William Telliard
Analytical Methods Staff
United States Environmental Protection Agency
Office of Water
Office of Science and Technology
Engineering and Analysis Division
Washington, DC 20460
Re: SPLIT SAMPLES
Dear Mr. Telliard:
As you may recall, we ran Standard Methods 413.1, 418.1 and
5520F on the split samples collected by your contractor at a CIS
facility as part of your on-going oil/grease evaluation, data is
attached.
Also as you are aware, CTS, our industry, and many others in
the regulated community, including municipalities find the 413.1
method very problematic, especially when the method is used as an
enforcement tool for all industrial discharges without regard to
its applicability. If regulatory enforcement with all the
consequences of bad public relations, fines, loss of customer
base, etc., was not so aggressive, we could better understand
continued use of the method as a general indicator.
Unfortunately, enforcement is very real, fines are being levied,
customers are being lost, not because of any enhanced protection
of the environment, but because of administrative considerations
with regard to the use of this method. The use of historical
local limits of 100 mg/1 based on this method and grab samples
causes significant design problems with wastewater treatment
systems. This is especially true when the method may be
measuring non-oil and grease materials that are soluble and
biodegradable.
Also, for your information attached is a recent
correspondence sent to Onondaga County, New York. As indicated,
data reported by three different commercial laboratories on
identical samples had an unacceptable variance.
140 CORTLAND AVENUE • P.O. BOX 4854 • SYRACUSE, NEW YORK 13221 • 315-475-1626 • FAX 315-475-2140
-------
Mr* William Telliard
June 29, 1993
Page Two
We look forward to discussing this in greater detail at your
Boston, Massachusetts conference.
Very tru
Stepfien PT'Naughton
Environmental Manager
SPN/sle
cc: David Poisson, IIL
Mark Liner, EPA
Barbara Elkus, EPA
John Contney, TRSA
Tom Fieldsend, EPA
-------
EPA SPLITS
METHOD
413.1
5520F
418.1
EPA DATA
180
LAB A
165
106
165
LAB B
146.4
93.6
125
% OF DIFFERENCE
-------
COYNE INTERNATIONAL
ENTERPRISES CORP
COYNE TEXTILE SERVICES
EXECUTIVE OFFICES.
P.O. Box 4894
140 Contend Avenue
Syracuse. New Mxk 1322t
(3)5)475-1626
BALTIMORE. MO
BECKLEY.WV
BETSY LAYNE, KY
BRISTOL, TN
BUFFALO. NY
BURLINGTON. VT
CHARLESTON. WV
CLEVELAND. OH
OU BOIS. PA
ERIE. PA
FAIRMONT, wv
4JETON.PA
MUNTINGTON. WV
JOUET.IL
LEWISTON. ME
LONDON. KY
LONG tSLANO. NY
NEWARK. HI
NEW BEDFORD. MA
PHILADELPHIA. PA
PITTSBURGH. PA
RICHMOND. VA
SCHENECTADY. NY
SEAFORO.DE
SMITHBORO. NY
SYRACUSE, NY
TOLEDO. OH
WATERBURY.CT
WINCHESTER. VA
WORCESTER. MA
YORK. PA
June 10, 19993
Mr. Joseph J. Mastriano
Program Manager
County of Onondaga
Department of Drainage and Sanitation
650 Hiawatha Boulevard, West
Syracuse, New York 13204-1194
0
$
RE: ANALYTICAL INFORMATION
Dear Joe:
As you are aware, we have discussed the complications we are
having with the oil and grease method 413.1 on our wastewater
matrix. We recently had three independent commerical
laboratories run the 413.1 method on identical samples. The data
is attached in Table 1.
As indicated, there is a wide varence in concentrations
reported. We are submitting this for your information to keep
you apprised about the on-going difficulties with establishing an
appropriate database.
Very truly yours,
f>
/jkw-
Stephen P. Naughton
Environmental Manager
SPK:dms
Attachment
cc: Betsy Stevens, Esq., Dept. of Drainage & Sanitation
Dan Ramer, Dept. of Drainage & Sanitation
140 CORTLAND AVENUE • P.O. BOX 4854 • SYRACUSE, NEW YORK 13221 * 315^75-1626 • FAX 315-475-2140
-------
TABLE II
COYNE TEXTILE SERVICES
OIL/GREASE DATA (METHOD 413.1)
DATE
COLLECTED
05/24/93
05/25/93
05/25/93
05/25/93
05/25/93
TIME
COLLECTED
N/A .
12:30 pa
1:30 pm
2:30 pm
4:30 pm
OIL & GREASE 413.1 METHOD
ETS UPSTATE ENV. LABS
933 ppm
927 ppm
328 ppm
140 ppm
227 ppm
455 ppm
280 ppm
17 ppm
6 ppm
83 ppm
140 ppm
497 ppm
397 ppm
277 ppm
543 ppm
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