FINAL
BEST DEMONSTRATED AVAILABLE TECHNOLOGY (BOAT)
BACKGROUND DOCUMENT ADDENDUM FOR
F002 (1,1,2-TRICHLOROETHANE)
AND
F005 (BENZENE, 2-ETHOXYETHANOL, AND
2-NITROPROPANE)
Larry Rosengrant, Chief
Treatment Technology Division
Jose Labiosa
Project Manager
U.S. Environmental Protection Agency
Office of Solid Waste
401 M Street, S.W.
Washington, DC 20460
May 1990
NOTE: This Background Document is an amendment to the November 1986 Final Best
Demonstrated Available Technology (BOAT) Background Document for F001-F005
Spent Solvents (EPA/530-SW-86-056, 3 volumes)
-------
ACKNOWLEDGMENTS
This document was prepared for the U.S. Environmental Protection
Agency, Office of Solid Waste, by Versar Inc. under Contract No.
68-W9-0068. Mr. Larry Rosengrant, Chief, Treatment Technology Section,
Waste Treatment Branch, served as the EPA Program Manager during the
preparation of this document and the development of treatment standards
for F002/F005 wastewaters and nonwastewaters. The technical project
officer for the waste was Ms. Monica Chatmon-McEaddy. Mr. Jose Labiosa
served as work assignment manager. Mr. Steven Silverman served as legal
advisor.
Versar personnel involved in the preparation of this document
included Mr. Jerome Strauss, Program Manager; Mr. Stephen Schwartz,
Assistant Program Manager; Ms. Christel Ackerman and Ms. Josefina
Castellanos, Principal Investigators and Authors; Ms. Justine Alchowiak,
Quality Assurance Officer; Ms. Martha Martin, Technical Editor; and
Ms. Sally Gravely, Program Secretary.
3057g
-------
TABLE OF CONTENTS
Section Paee No.
1. INTRODUCTION AND SUMMARY 1-1
2. INDUSTRIES AFFECTED AND WASTE CHARACTERIZATION 2-1
2.1 Industries Affected 2-1
2.2 Waste Characterization 2-2
3. APPLICABLE AND DEMONSTRATED TREATMENT TECHNOLOGIES 3-1
4. PERFORMANCE DATA 4-1
5. DETERMINATION OF BEST DEMONSTRATED AVAILABLE TECHNOLOGY
(BDAT) 5-1
5.1 Nonwastewaters 5-1
5.2 Wastewaters 5-1
6. CALCULATION OF TREATMENT STANDARDS 6-1
6.1 Benzene 6-1
6.1.1 Wastewaters 6-1
6.1.2 Nonwastewaters 6-2
6.2 1,1,2-Trichloroethane 6-3
6.2.1 Wastewaters 6-3
6.2.2 Nonwastewaters 6-5
6.3 2-Nitropropane 6-7
6.3.1 Wastewaters 6-7
6.3.2 Nonwastewaters 6-12
6.4 2-Ethoxyethanol 6-12
6.4.1 Wastewaters 6-12
6.4.2 Nonwastewaters 6-13
7. REFERENCES 7-1
APPENDICES
Appendix A - Performance Data for Treatment of Benzene -
Containing Wastewaters A-l
Appendix B - Analytical Methods for 2-Nitropropane
and 2-Ethoxyethanol B-l
ii
-------
LIST OF TABLES
Pane No.
Table 1-1 BOAT Treatment Standard for 1,1,2-Trichloroethane
(F002) and Benzene (F005) Wastewaters 1-6
Table 1-2 BOAT Treatment Standard for 1,1,2-Trichloroethane
(F002) and Benzene (F005) Nonwastewaters 1-6
Table 1-3 BOAT Treatment Standards for 2-Ethoxyethanol and
2-Nitropropane Nonwastewaters 1-7
Table 1-4 BDAT Treatment Standards for 2-Ethoxyethenol and
2-Nitropropane Wastewaters 1 7
Table 2-1 Characterization Data for Benzene, 2-Ethoxyethanol,
and 1,1,2-Trichloroethane 2-3
Table 2-2 Summary of Industries for Which Spent Solvent Waste
Characterization Data Are Available 2-5
Table 4-1 Data Set Summary 4-2
Table 4-2 BAT Performance Data for the Biological Treatment
of Benzene 4-3
Table 4-3 Incineration Data for Benzene-Containing
Nonwastewaters 4-8
Table 4-4 Performance Data for the Biological Treatment of
1,1,2-Trichloroethane 4-9
Table 4-5 Performance Data for Steam Stripping of Wastewaters
Containing 1,1,2-Trichloroethane 4-11
Table 4-6 Incineration Data for 1,1,1-Trichloroethane
Nonwastewaters 4-12
Table 4-7 Performance Data for the Steam Stripping of
Wastewaters Containing 2-Nitropropane 4-13
Table 4-8 Performance Data for the Biological Treatment of
Wastewaters Containing 2-Ethoxyethanol 4-14
Table 4-9 Wastewater Treatment Performance Data for n-Butyl
Alcohol 4-16
iii
-------
LIST OF TABLES
(CONTINUED)
Page No.
Table 6-1 Physical Properties of 2-Nitropropane and
Nitrobenzene 6-8
Table 6-2 Performance Data for Treatment of Wastewaters
Containing Nitrobenzene by Steam Stripping Followed
by Carbon Adsorption 6-11
Table 6-3 Physical and Structural Properties of 2-Ethoxyethanol
and n-Butyl Alcohol 6-14
Table 6-4 Wastewater Treatment Performance Data for n-Butyl
Alcohol 6-15
Table A-l Performance Data for Steam Stripping of Benzene -
Containing Wastewaters A-l
Table A-2 Performance Data for Liquid-Liquid Extraction
Followed by Steam Stripping Followed by Activated
Carbon Adsorption of Benzene-Containing Wastewaters .. A-2
Table B-l Gas Chromatograph Conditions for 2E Analysis B-2
Table B-2 Validation Data for 2E Analytical Method B-2
IV
-------
1. INTRODUCTION AND SUMMARY
This background document presents the data and rationale for the
development of treatment standards for 1,1,2-trichloroethane (F002),
benzene (F005), 2-ethoxyethanol (F005), and 2-nitropropane (F005). This
document is issued as an addendum to the November 1986 background
document for F001-F005 spent solvents (USEPA 1986).
F002 and F005 are listed as hazardous wastes from nonspecific sources
as identified in 40 CFR 261.31:
F002 - The following spent halogenated solvents: tetrachloroethy-
lene, methylene chloride, trichloroethylene, 1,1,1-trichloro-
ethane, chlorobenzene, 1,1,2-trichloro-1,2,2-trifluorethane,
orthodichlorobenzene, trichlorofluoromethane, and
1,1,2-trichloroethane; all spent solvent mixtures/blends
containing, before use, a total of 10 percent or more (by
volume) of one or more of the above halogenated solvents or
those listed in F001, F004, or F005; and still bottoms from
the recovery of these spent solvents and spent solvent
mixtures.
F005 - The following spent nonhalogenated solvents: toluene, methyl
ethyl ketone, carbon disulfide, isobutanol, pyridine,
benzene, 2-ethoxyethanol, and 2-nitropropane; all spent
solvent mixtures/blends containing, before use, a total of
10 percent or more (by volume) of one or more of the above
nonhalogenated solvents or those solvents listed in F001,
F002, or F004; and still bottoms from the recovery of these
spent solvents and spent solvent mixtures.
The Environmental Protection Agency (EPA) promulgated treatment
standards for F002 and F005 as part of the final "Solvents and Dioxins
Rule" (51 FR 40572, November 7, 1986). However, treatment standards for
1,1,2-trichloroethane (F002) and for benzene (F005), 2-ethoxyethanol
(F005), and 2-nitropropane (F005) were not included in the final
"Solvents and Dioxins Rule" because these solvents were added too late
for the Agency to gather data to characterize and evaluate them. The
1-1
3057g
-------
final rule adding 1,1,2-trichloroethane to F002 and adding benzene,
2-ethoxyethanol, and 2-nitropropane to F005 was promulgated on
February 25, 1986 (51 FR 6737).
Although the Hazardous and Solid Waste Amendments (HSWA) directed the
Agency to restrict the disposal of these new constituents 6 months after
they were listed, EPA was unable to propose or promulgate treatment
standards because there were no SW-846 analytical methods that could
satisfactorily analyze 2-ethoxyethanol and 2-nitropropane in complex
waste matrices. Therefore, the Agency has been unable to propose
treatment standards for these constituents until today's proposal.
Further, since the final "Solvents and Dioxins Rule" was promulgated,
the Agency has obtained additional data and performed further evaluations
of these wastes and thus has enough information to establish numerical
treatment standards for 1,1,2-trichloroethane (F002) and benzene (F005)
and require methods of treatment for 2-ethoxyethanol (F005) and 2-nitro-
propane (F005).
The final treatment standards for 1,1,2-trichloroethane (F002) and
benzene (F005) wastewaters and nonwastewaters are presented in Tables 1-1
and 1-2 at the end of this section. These standards are based on the
total concentration of the constituents in the waste for both wastewaters
and nonwastewaters.
The Agency is modifying the proposed treatment standards in the
November 22, 1989, 54 FR 48461 for 2-ethoxyethanol and 2-nitropropane.
These revisions are in response to comments. EPA determined that there
is not sufficient information to develop a concentration-based standard
for wastewaters and nonwastewaters containing 2-ethoxyethanol and
2-nitropropane (see Sections 6.3 and 6.4). EPA is instead promulgating
methods of treatment for these two F005 constituents.
1-2
3057g
-------
For the purpose of determining the applicability of the treatment
standards, wastewaters are defined as wastes containing less than 1
percent (weight basis) total suspended solids* and less than 1 percent
(weight basis) total organic carbon (TOC).
At this time, EPA is withdrawing the alternative method of treatment,
steam stripping followed by carbon adsorption, for F005 wastewaters
containing 2-nitropropane. This revision to the proposed regulatory
approach follows EPA's determination that the adoption of steam stripping
followed by carbon adsorption as BDAT should require minimum operating
conditions to ensure that 2-nitropropane wastewaters do not go untreated
through this treatment technology. EPA based its determination on the
azeotrophic behavior of 2-nitropropane in F006 wastewaters and the fact
that steam stripping of azeotropes would require a combination of more
than one distillation unit. EPA lacks sufficient information to
incorporate such requirements in the BDAT standard. However, EPA has
determined that wet air oxidation followed by carbon adsorption as well
as chemical oxidation followed by carbon adsorption represent BDAT for
2-nitropropane based on the treatment of wastewaters containing
nitrobenzene. The Agency is promulgating these last two treatment
technologies as an alternative treatment standard for F005 wastewaters
and nonwastewaters containing 2-nitropropane. Wastewater effluents from
the carbon adsorption unit can be land disposed. Nonwastewater residues
from these two alternative treatment technologies must meet the
nonwastewater treatment standards for F005 nonwastewaters containing
2-nitropropane, as a pre-requisite for land disposal.
* The term "total suspended solids" (TSS) clarifies EPA's previously used
terminology of "total solids" and "filterable solids." Specifically,
total suspended solids is measured by method 209C (Total Suspended
Solids Dried at 103-105°C) in Standard Methods for the Examination
of Water and Wastewater, 16th edition.
1-3
3057g
-------
Note that at the time treatment standards were originally promulgated
for F001-F005 (51 FR 40572), useful data were not available on total
constituent concentrations in nonwastewater residuals; hence, TCLP was,
at that time, considered to be the best available measure of performance
for solvents in nonwastewaters. Since that time EPA has consistently
promulgated total concentration standards for organic constituents in
nonwastewater residuals and will do so for the four solvents for which
standards are being promulgated here.
In developing the promulgated treatment standards for 1,1,2-trichloro-
ethane and benzene solvent wastes, EPA is using the same methodology that
it is using for U and P waste codes in this Third Third rulemaking. This
somewhat modifies the methodology used in the First Third and Second
Third rulemakings (USEPA 1989a). In the current rulemaking for U and P
regulatory standards, the Agency considered all of the treated waste
performance data where the constituent was treated to the detection limit
in all cases. Then the Agency determined which of the detection limits
were the most representative of the specific U and P wastes. To account
for the anticipated variability in waste characteristics of untreated U
and P wastes, the Agency typically selected the highest detection limits
for the constituent that corresponded to the chemical represented by the
U or P code. Thus, the Agency believes the resultant treatment standards
should be achievable on a routine basis for the majority of U and P
wastes. Because of the diversity of solvent wastes, the Agency believes
this same methodology should apply to two of the four solvents for which
standards are being promulgated here: 1,1,2-trichloroethene (F002) and
benzene (F005). The 2-ethoxyethanol and 2-nitropropane treatment
standards are being promulgated as methods of treatment.
The technologies used as the basis for BOAT are presented in
Section 3, and the treatment data used to develop specific performance
levels are presented in Section 4. In Section 5, BDAT is selected for
1-4
3057g
-------
each solvent. Section 6 contains the calculation of treatment standards
for each solvent.
Compliance with these treatment standards is a prerequisite for
placement of these wastes in facilities designated as land disposal
treatment units according to 40 CFR Part 268. The BDAT treatment
standards for 1,1,2-trichloroethene and benzene wastewaters and
nonwastewaters are presented in Tables 1-1 and 1-2. Tables 1-3 and 1-4
present the BDAT treatment standards for 2-ethoxyethanol and
2-nitropropane.
1-5
3057g
-------
Table 1-1 BOAT Treatment Standards for 1,1,2-Trichloroethane
(F002) and Benzene (F005) Wastewaters
Constituent
Maximum (composite sample)
Total concentration (mg/1)
1,1,2-Trichloroethane
Benzene
0.03
0.07
Table 1-2 BDAT Treatment Standards for 1,1,2-Trichloroethane
(F002) and Benzene (F005) Nonwastewaters
Constituent
Maximum (single grab)
Total concentration (mg/kg)
1,1,2-Trichloroethane
Benzene
7.6
3.7
1-6
3057g
-------
Table 1-3 BDAT Treatment Standards for 2-Ethoxyethanol and
2-Nitropropane Nonwastewaters
INCINERATION3 AS A METHOD OF TREATMENT
alnclneration must be conducted in accordance with the technical
requirements of 40 CFR Part 264 or Part 265, Subpart 0.
Table 1-4 BDAT Treatment Standards for 2-Ethoxyethanol and
2-Nitropropane Wastewaters
Constituent Treatment Standard
2-Ethoxyethanol Incineration3 or
Biological Treatment
2-Nitropropane Incineration;3 or
Wet Air Oxidation followed by
Carbon Adsorption; or Chemical
Oxidation followed by Carbon
Adsorption
alncineration must be conducted in accordance with the technical
requirements of 40 CFR Part 264 or Part 265, Subpart 0.
1-7
3057g
-------
2. INDUSTRIES AFFECTED AND WASTE CHARACTERIZATION
2.1 Industries Affected
A background document was produced to support the proposed listing
(50 FR 20908, July 30, 1985) of 1,1,2-trichloroethane, benzene,
2-ethoxyethanol, and 2-nitropropanol as constituents of F002 and F005.
This background document was revised slightly for the final rule (51 FR
6537) listing the four solvents as part of F002 and F005. The background
documents for both the proposed rule and the final rule are contained in
their respective public dockets. The listing background document for the
final rule is also contained in the public docket for this rulemaking.
Information in the listing background documents indicates that the
principal uses of these four solvents as solvents are as follows:
1,1,2-Trichloroethane Manufacture and use of paints and coatings;
organic synthesis and miscellaneous
processing.
Benzene Organic synthesis and miscellaneous
processing.
2-Ethoxyethanol Manufacture and use of paints, coatings, and
inks; organic synthesis and miscellaneous
processing.
2-Nitropropane Manufacture and use of paints, coatings, and
inks; organic synthesis and miscellaneous
processing.
Since promulgation of the final rule listing the four solvents as
part of F002 and F005. the Agency has contacted potential generators of
the four solvents. The contacted facilities confirmed the types of
industries affected, as cited in the final listing background document
(Cain Chemical 1988, Eastman Kodak 1988, Safety-Kleen 1988, Sinclair and
Valentine 1988, Versar 1988). However, at least two printing ink
2-1
3057R
-------
manufacturers expressed the opinion that 2-ethoxyethanol and
2-nitropropane are used very sparingly, if at all, in printing inks.
2.2 Waste Characterization
Since promulgation of the final rule listing the four solvents, the
Agency has received additional characterization data for three of the
four solvents from a facility that incinerates them (Eastman Kodak
1988). These data are presented in Table 2-1.
As with most F001-F005 spent solvent wastes, the four solvents are
expected to be found mixed with other wastes. Table 2-2 lists industries
for which characterization data were available to the Agency for the
development of BDAT standards for F001-F005 spent solvents (USEPA 1986).
2-2
3057g
-------
Table 2-1 Characterization Data for Benzene, 2-Ethoxyethanol,
and 1,1,2-Trichloroethane3
Solvent
Benzene
Benzene
Benzene
Approx .
Cone.
95%
80%
10%
Generating
Process
Chemical
manufacturing
Chemical
manufacturing
Laboratory use
Quantity
Generated
270 gal /day
30 gal /day
2400 gal/yr
Physical
Characteristic
Liquid
Liquid
Liquid
Other
Constituents
Water 5%
Miscellaneous organics 20%
Miscellaneous solvents 20%
2-Ethoxyethanol
2-Ethoxyethanol
2-Ethoxyethanol
1,1,2-Trichloroethane
1,1,2-Tr ichloroethane
10%
10%
Dispersion coating
300 Ib
Liquid with
some sediment
Parts painting
55 gal
Sludge
Trace
5%
15%
Dispersion
Testing
Cleaning
100 Ib/yr
165 gal/yr
800 gal/yr
Solid
Liquid
Liquid
Carbon tetrachloride 10%
Carbon disulfide 10%
Water 10%, DMSO 10%
Chloroform 15%
Acetonitrile 15%
Methyl ethyl ketone 25%
Iron oxide 25%
Amyl acetate 20%
Lindol 10%
Cellulose nitrate 10%
Xylene 10%
Paint solids 64%
Tin 4%
Butyl cellosolve 12%
Hexyl cellosolve 10%
Filters and dispersion 99.9%
Dichloromethane 95%
Dichloromethane 50%
Toluene 20%
Ethanol 15%
-------
3379g
Table 2-1 (continued)
Solvent
Approx.
Cone.
Generating
Process
Quantity
Generated
Physical
Characteristic
Other
Constituents
1.1,2-Trichloroethane Trace Solvent coating
1,1,2-Trichloroethane Trace Solvent coating
1,1,2-Trichloroethane 50%
1,1,2-Trichloroethane 10%
1,1,2-Trichloroethane
98%
Solvent .coating
Research
Chemical
manufacturing
68700 Ib/yr
3300 Ib/yr
3000 gal/yr
1000 gal/yr
800 gal/yr
Solid
Solid
Liquid
Liquid with
some sludge
Liquid
Waste filters, rags, poly
containers, and other solid
refuse 98%
Miscellaneous organics 2%
Waste filters,
polyethylene bags,
rags, etc. 99%
Miscellaneous solvents 1%
Methyl acetate 1%
Dichloromethane 49%
Dichloromethane 62%
2-Butanone 9%
Miscellaneous organics 3.3%
Acetone 1%
Methanol 5%
Tetrahydrofuran 1%
Ethanol 1%
Ethyl acetate 1%
Methyl acetate 1%
Toluene 1.7%
Acetonitrile 4%
Residual Organics 2%
al)nlike other waste streams, which were incinerated after being mixed with other wastes, this waste was incinerated separately.
Source: Eastman Kodak 1988
-------
Table 2-2 Summary of Industries for Which Spent Solvent
Waste Characterization Data Are Available
Industry
Description of spent solvent waste
Furniture manufacturing
Plastics and resins
manufacturing
Fiber manufacturing
Pharmaceutical manufacturing
Paint manufacturing
Dyes and pigments
manufac tur ing
Organic chemicals
manufac tur ing
Agricultural chemicals
manufac tur ing
Printing industry
Can coating industry
Membrane production industry
Spent thinner and solvent
Still bottoms and caustic
Epoxy resin waste
Phenolic and polyester/alkyd resin waste
Solvent recovery bottoms, laboratory sol-
vents , and chrome plating solution
Solvent recovery bottoms
Paint tank wash
Spent thinner
Dyes and pigments waste
Still bottoms and caustic
Isocyanates manufacturing wastes
Alkenes manufacturing waste
Aldehyde furan manufacturing wastes
Pesticide manufacturing waste
Spent recovery bottoms
Spent ink wash
Spent can coating residue
Spent solvents and organics
30578
2-5
-------
3. APPLICABLE AND DEMONSTRATED TREATMENT TECHNOLOGIES
The background document for F001-F005 spent solvents (USEPA 1986)
identified applicable and demonstrated technologies for treating
F002/F005 wastes containing the four new solvents. The Agency has
identified a new emerging technology that may be applicable to the
treatment of at least two of the four solvents. This technology,
catalytic hydrodehalogenation (IITRI 1989), has been tested at bench
scale on 1,1,2-trichloroethane and benzene. Hydrodehalogenation is a
gaseous phase chemical reaction involving a chlorinated solvent and
hydrogen gas in the presence of a noble metal catalyst, such as
platinum. Products of the reaction are hydrogen chloride and the
dehalogenated solvent. To the best of the Agency's knowledge, however,
no commercial-scale plants use this technology. Therefore, the
technology cannot be considered demonstrated.
Technologies considered to be applicable and demonstrated for spent
solvents are described fully in the background document for F001-F005
spent solvents (USEPA 1986). Based on the 1986 information, EPA
conversations with generators and treaters of these newly listed wastes
and the multi-source leachates (see Section 4), EPA has identified
several applicable waste management practices for the newly listed
solvents, EPA has determined that incineration and wet air oxidation
followed by carbon adsorption are applicable and demonstrated for
1,1, 2-trichloroethane , benzene, 2-.ethoxyethanol, and 2-nitropropane in
F002 and F005 spent solvents for nonwastewaters; and distillation
(including air or steam stripping), biological treatment, and carbon
adsorption are applicable and demonstrated for wastewaters. Some of
these treatment technologies allow for the recovery of the spent
solvents. For example, an F005 waste containing 2-ethoxyethanol could be
treated by distillation to recover 2-ethoxyethanol. However, these
recovery technologies may leave behind residuals that may require further
treatment prior to disposal.
3-1
3057g
-------
4. PERFORMANCE DATA
This section presents the data available on the performance of
demonstrated technologies in treating the listed wastes. These data are
used later in this document for determining which technologies represent
the best demonstrated available technology (BDAT) and for developing
treatment standards.
EPA lacks performance data for the treatment of F002 and F005 wastes
containing 1,1,2-trichloroethane, benzene, 2-ethoxyethanol, and 2-nitro-
propane. Instead, EPA has performance data from the treatment of other
wastes that contain these or similar constituents. EPA believes that
those constituents identified as similar constituents are at least as
difficult to treat as those for which EPA currently lacks performance
data. In addition, the Agency believes, based on its contacts with
facilities managing these wastes, that none of the constituents in F002
and F005 are likely to interfere with, or reduce the treatment of,
1,1, 2-trichloroethane, benzene, 2-ethoxyethanol, and 2-nitropropane. The
characterization data presented in Table 2-1 for incineration of solvent
wastes support this belief.
Treatment data from several sources were examined by the Agency to
develop the proposed treatment standards (USEPA 1987, 1988a, 1988b,
1989b; Accurex 1986; University of Cincinnati 1989a, 1989b). A summary
of the performance data used to establish standards for the solvents is
presented in Table 4-1. The individual data sets are presented in
Tables 4-2 through 4-8. Each of the data sets shown in Tables 4-2
through 4-8 is presented in its unedited version. However, the data were
eventually edited, as noted on each table, when standards were calculated
based on the data. Data editing was performed consistent with the EPA
methodology for BDAT rulemaking (USEPA 1989a) .
4-1
3057g
-------
Table 4-1 Data Set Stmmary
Table Ho.
Title
Source
4-2
4-3
Biological treatment of benzene
USEPA 1987b.
Incineration data for benzene-containing Acurex 1986, USEPA 1989b, and
nonwastewaters USEPA 1988a.
4-4
Biological treatment of 1,1,2-trichloro- USEPA 1987b.
ethane
4-5 Steam stripping of wastewaters containing USEPA 1987b.
1,1.2-trichloroethane
4-6
Incineration data for 1,1,1-trichloro-
ethane nomrastewaters
Acurez 1986, USEPA 1989b, and
USEPA 1988b.
4-7 Steam stripping of wastewaters
containing 2-nitropropane
University of Cincinnati 1989a.
4-8 Biological treatment of wastewaters
containing 2-ethoxyethanol
University of Cincinnati 1988b.
4-9 Hastewater treatment performance
data for n-butyl alcohol
USEPA 1989c
3057g
4-2
-------
Table 4-2 BAT Performance Data for the Biological Treatment of Benzene
Plant
no.
12F
296V
306V
384T
444V
695V
851V
Sampling
date
5/12/81
5/19/81
5/26/81
6/2/81
6/9/81
6/15/81
6/16/81
2/20/79
2/27/79
2/28/79
3/1/79
11/27/83
11/28/83
11/29/83
11/30/83
12/1/83
12/4/83
12/5/83
12/6/83
12/7/83
12/8/83
12/11/83
12/12/83
12/13/83
12/14/83
12/15/83
11/14/78
11/15/78
11/16/78
12/4/78
12/5/89
12/6/78
3/6/79
3/7/79
3/8/79
Concentration of
benzene
in influent (ppb)
1543
737
1024
444
738
877
607
<19,900
278,300
280,000
380,000
40,039
34,692
33,642
90,757
36,508
58,191
62,675
25,554
30,637
31,970
24,891
21,165
24,600
30,285
18,744
957
1,500
879
<10
<10
<10
36,640
36,150
41,290
Recovery-corrected
Concentration of concentration of
benzene benzene
in effluent (ppb) in effluent (ppb)8 Hotes
<10 19.6
<10 19 . 6
<10 19.6
<10 19.6
<10 19.6
<10 19.6
<10 19.6
<10 13.9
<10 18.5
38 70.4
11 20.4
<10 10
<10 10
<10 10
<10 10
<10 10
<10 10
<10 10
<10 10
<10 10
<10 10
<10 10
<10 10
<10 10
<10 10
<10 10
<10 10
<10 10
<10 10
<10 12.6 T
<10 12.6 T
<10 12.6 T
<10 10
<10 10
<10 10
3057g
4-3
-------
Table 4-2 (continued)
Concentration of
Plant Sampling benzene
no. date in influent (ppb)
948F 6/18/80
6/19/80
6/20/80
6/23/80
6/24/80
6/25/80
6/26/80
6/27/89
7/7/80
7/8/80
7/9/80
7/10/89
7/11/80
948F 7/14/80
7/15/80
7/16/80
7/17/80
7/18/80
7/21/80
7/22/80
7/23/80
7/24/80
7/25/89
7/28/80
7/29/80
7/30/89
7/31/89
8/1/80
8/4/80
8/5/80
8/6/80
8/7/80
8/8/80
250
IBS
74
640
130
670
110
450
1,400
271
220
1,200
330
66
19
<1Q
-------
Table 4-2 (continued)
Plant
no.
1293T
1609V
1650F
1650V
2430V
24817
Concentration of
Sampling benzene
date in influent (ppb)
2/19/84
2/20/84
2/21/84
2/22/84
2/23/84
2/26/84
2/27/84
2/28/84
2/29/84
3/1/84
3/4/84
3/5/84
3/6/84
3/7/84
3/8/84
9/11/78
9/2/78
9/13/78
2/17/83
2/23/83
3/2/83
3/14/83
5/22/79
1/9/79
1/10/79
1/11/79
10/11/80
10/12/80
10/13/80
10/14/80
10/15/80
10/16/80
10/17/80
10/18/80
10/19/80
10/20/80
569
445
360
<10
417
209
510
668
821
705
712
1,127
1,185
983
1,105
160
157
365
1,150
-------
Table 4-2 (continued)
Plant Sampling
no. date
24B1F (cont.) 10/21/80
10/24/80
10/25/80
10/26/80
10/27/80
10/28/89
10/29/80
10/30/80
10/31/89
11/1/80
11/2/80
11/3/80
11/4/80
11/5/80
11/6/80
11/7/89
11/8/80
11/9/80
11/10/80
11/11/60
Z631F 6/2/80
6/3/89
6/4/80
6/5/80
6/9/80
6/10/80
6/11/80
6/12/80
6/16/89
6/17/80
6/18/80
6/19/80
6/23/80
6/24/80
6/25/80
6/26/80
Concentration of
benzene
in influent (ppb)
<10
59
57
36
168
247
52
60
59
61
106
69
43
27
32
38
34
40
60
<10
2,000
2,190
1,913
2,565
6,985
5,213
3,079
2,398
9,524
5,925
2,825
5,575
4,880
3,557
4,497
5,363
Recovery-corrected
Concentration of concentration of
benzene benzene
in effluent (ppb) in effluent (ppb)° Rotes
<10 19.6
15 29.4
<10 19.6
<10 19.6
<10 19.6
<10 19.1
<10 19.6
<10 19.6
<10 19.6
<10 19.6
<10 19.6
<10 19.6
<10 19.6
<10 19.6
<10 19.6
<10 19.6
<10 19.6
<10 19.6
<10 19.6
<10 19.6 T
<10 19.6
<10 19.6
<10 19.6
<10 78.4
11 21.6
<10 19.6
<10 19.6
<10 19.6
<10 19.6
<10 19.6
<10 19.6
<10 19.6
<10 19.6
<10 19.6
<10 19.6
<10 19.6
3057g
4-6
-------
Table 4-2 (continued)
Concentration of
Concentration of
Recovery-corrected
concentration of
Plant
no.
263 IF (cont.)
4051V
Sampling
date
6/30/89
7/1/80
7/2/80
7/3/80
7/7/80
7/8/80
7/9/80
7/10/80
1/16/79
1/17/79
1/18/79
4/23/79
4/24/79
benzene
in influent (ppb)
10,800
7,683
9,200
4,030
11,000
7,893
11,800
7,508
3,783
3,300
3,200
190
62
benzene benzene
in effluent (ppb) in effluent (ppb)a Rotes
<10 19.6
<10 19.6
<10 19.6
<10 78.4
17 33.3
<10 19.6
<10 19.6
<10 19.6
23 23
20 20
<10 10
<10 19.6
<10 19.6
Motes:
1 Data not used. Influent benzene concentration was less than detection limit; thus,
treatment may not have been substantial.
Y Data not used; improper QA/QC or no QA/QC used.
* Recovery-corrected concentration of benzene in effluent was calculated by dividing the
concentration of benzene in the effluent by a recovery factor. Recovery factors were
obtained from laboratory matrix spike or surrogate spike data. They are percent recoveries
divided by 100. Plants with a T suffix are not adjusted for recovery because of the
analytical method used. Plants with a V suffix have the following recovery factors: 296V,
0.72; 306V, 0.54; 444V, 1.0; 695V, 0.79; 851V, 1.0; 1609V, 1.0; 1650V, 0.91; 2430V, 0.97;
and 4051V, 0.51. Recovery data were not available for plants with an F suffix, so the
lowest recovery factor from the V plants (0.51) was used. Recovery factors greater than
1.0 were set to 1.0.
Source:
USEPA 1987b.
4-7
3057g
-------
Table 4-3 Incineration Data for Benzene-Containing Nonwastewaters
Plant
no.
Site 1
Site 2
Site 3
Site 4
Site 5
Site 6
Site 7
Site 8
Site 9
Site 10
#1
*2
*3
#4
#5
*6
Sample 1
Sample 2
Sample 3
Sample 4
Sample S
Honwastewater
concentration
93 mg/kg
<0.1 g/kg
HD
HD
HO
<0.1 g/kg
<0.1 g/kg
<0.1 g/kg
HD
6700 mg/1
57 Bg/kg
61 mg/kg
48 mg/kg
59 as/kg
55 mg/kg
HD
17 mg/kg
19 mg/kg
5.6 mg/kg
212 mg/kg
170 mg/kg
Scrubber
effluent
<5 mg/1
<50 MS/1
HD
HD
HD
<50 MS/1
<50 MS/1
<50 MS/1
HD
<0.5 mg/1
<0.01 mg/1
<0.01 mg/1
HD
<0.01 mg/1
<0.01 Bg/1
HD
HD
HD
HD
HD
HD
Kiln
ash
<1 mg/kg
<0.1 g/kg
HD
HD
HD
<0.1 g/kg
<0.1 g/kg
<0.1 g/kg
HD
HD
<0.01 mg/kg
<0.01 mg/kg
HD
<0.01 Bg/1
<0.01 Bg/1
HD
<0.025
<0.025
<0.025
<0.025
<0.025
TCLP
(kiln ash)
2 MS/1
3 MB/1
HD
HD
HD
10 MS/1
3 MB/I
3 MB/1
HD
HD
HD
HD
HD
HD
HD
HD
HD
HD
HD
HD
HD
Ash
recovery-
corrected
cone . Rotes
1.33 Bg/kg R
T
T
T
T
0.57 ng/l" R, HD
0.01 mg/kg R
0.01 Bg/kg R
0.01 Bg/kg R
0.01 mg/kg R
0.03
0.03
0.03
0.03
0.03
Rotes:
HD - Ho data, not analyzed, or data not used.
R - Recovery-corrected concentration is based on recovery of surrogates
1.2-dichloroetbane, toluene, and p-bromofluorobenzene (751 recovery for Site 1; 1411
recovery-rounded to lOOZ-for fl, fZ, ft, and f5).
T - Data not used; influent concentration below detection limits.
"Scrubb
>er wastewater recovery-corrected concentration.
Source for Sites 1-9: Acurex 1986.
Source for *l-*6: USEPA 1989b.
Source for Samples 1-5: USEPA 1988a.
4-8
3057g
-------
Table 4-4 Performance Data for the Biological Treatment
of 1,1,2-Trichloroethane
Plant
Concentration of
1.1.2-trichloro-
Sampline ethane
date in influent (ppb)
Concentration of
1,1. 2-tr ichloro-
etbane
in effluent (ppb)
Recovery-corrected
concentration of
1,1,2-trichloro-
e thane
in effluent (ppb) Hates
415T 11/29/83 <10
11/30/83 <10
12/1/83 <10
12/2/83 <10
12/3/83 <10
12/4/83 <10
12/5/83 <10
12/6/83 <10
12/7/83 <10
12/8/83 <10
12/11/83 <10
12/12/83 <10
12/13/83 <10
12/14/83 <10
12/15/83 <10
263 IF 6/2/80 23
6/3/80 <10
6/4/80 <10
6/5/80 <10
6/9/80 <10
6/10/80 <10
6/11/80 <10
6/12/80 <10
6/16/80 <10
6/17/80 <10
6/18/80 <10
6/19/80 <10
6/23/80 24
6/24/BO 28
6/25/80 11
6/26/80 11
6/30/80 <10
7/1/80 <10
7/2/80 12
7/3/BO 12
7/7/80 <10
<10 T
<10 T
<10 T
<10 T
<10 T
<10 T
<10 T
<10 T
<10 T
<10 T
<10 T
<10 T
<10 T
<10 I
<10 T
<10 10.2
<10 T
<10 T
<10 T
<10 T
<10 T
<10 T
<10 T
<10 T
<10 T
<10 T
<10 T
<10 10.2
<10 10.2
<10 10.2
<10 10.2
<10 T
<10 T
<10 10.2
<10 10.2
<10 T
3057g
4-9
-------
Table 4-4 (continued)
Concentration of
1,1,2-trichloro-
Concentration of
1,1,2-trichloro-
Eecovery-corrected
concentration of
1,1,2-trichloro-
Plant
no.
2631F (cant)
2631V
Sampling
date
7/8/80
7/9/80
7/10/80
1/16/79
1/17/79
1/18/79
ethane ethane
in influent (ppb) in effluent (ppb)
<10 <10
12 <10
<10 <10
523 33
680 <10
690 11
ethane
in effluent (ppb)
10.2
33.7
10.2
11.2
Hotes
T
T
Rotes:
T - Data not used. Influent concentration was less than detection limit; thus,
treatment may not be substantial.
Recovery Recovery factor for Plant Ho. 2631V = 98Z.
Recovery factor for Plant Ho. 263IF was not available; therefore, 98Z was used.
Source:
USEPA 1987b.
4-10
3057s
-------
Table 4-5 Performance Data for Steam Stripping of
Hastewaters Containing 1,1,2-Tricbloroetbane
Recovery-corrected
Concentration of Concentration of concentration of
1,1,2-trichloro- 1,1,2-trichloro- 1,1,2-trichloro-
Plant
no.
4 1ST
913F
Rotes :
T -
Sampling
date
11/29/83
11/30/83
12/1/83
12/2/83
12/3/83
12/4/83
12/5/83
12/6/83
12/7/83
12/8/83
12/11/83
12/12/83
12/13/83
12/14/83
12/15/83
8/12/85
8/13/85
8/14/85
8/19/85
8/20/85
8/29/85
8/30/85
9/16/85
9/17/85
9/18/85
9/19/85
9/20/85
9/25/85
10/9/89
Data not used.
ethane in ethane
untreated use (ppb) in effluent (ppb) in
8,900 <10
3,900 <10
<10 <10
<10 <10
<10 <10
870 <10
<10 <10
12,900 <10
13,500 <10
11,200 <10
220 <10
<10 10
<10 <10
<10 <10
2,000 <10
<10 <10
<10 <10
-------
Table 4-6 Incineration Data for 1,1,1-Trichloroethane Honwastewaters
Plant
no.
Site 1
Site 2
Site 3
Site 4
Site 5
Site 6
Site 7
Site B
Site 9
Site 10
#1
#2
#3
#4
#5
#6
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sample 5
Dotes :
T - Data
Nonwastewater
untreated
concentration
8,800 mg/1
HD
29,000 mg/1
HD
HD
HD
1,900 mg/1
10,000 mg/1
17,500 mg/1*
6,700 mg/1
0.045 mg/kg
0.026 mg/kg
0.029 mg/kg
0.02 mg/kg
0.032 mg/kg
HD
81,000 mg/kg
33,000 mg/kg
34,000 mg/kg
44,000 mg/kg
45,000 mg/kg
44,000 mg/kg
not used. Influent
Treated
kiln ash
(mg/kg)
<1
HD
<.5
3.7
HD
HD
<100
<1 ug/kg
<500 ug/kg
<1
<0.01
<0.01
HD
<0.01
<0.01
HD
<2
<2
<2
<2
<2
<2
concentrations
Ash recovery-
corrected
concentration
(mg/kg)
1.33
0.7
183. 3
0.002
0.7
1.33b
0.01
0.01
0.01
0.01
2.13
2.13
2.13
2.13
2.13
2.13
were less than dc
Hotes
HD
T
HD
HD
Y
HD
HD
HD
itection
limit; therefore, treatment may not be substantial.
7 - Detection limit so high as to make data meaningless. Data not
used.
HD - Data not used, no data, or data not analyzed.
Recovery 751 for Sites 1-10, 1001 for #l-#6; 941 for Sample Sets 1-6.
rlow-based composite of two feed streams.
Concentration of constituent in APCE effluent.
Source for Sites 1-10: Acurez 1986.
Source for #l-#6: USEFA 1989b.
Source for Samples 1-6: USEFA 1988b.
4-12
3057g
-------
Table 4*7 Performance Data for the Steam Stripping of
Hastewaters Containing 2-Hitropropane
Concentration of
Plant Sampling 2-nitropropane
no. date in influent (ppm)
University of 9/1/88 3,480
Cincinnati 1,314
9/1/88 2,560
303
9/1/88 977
405
9/1/88 1,120
743
9/1/88 701
737
9/1/88 646
775
Recovery-corrected
Concentration of concentration of
2-nitropropane 2-nitropropane
in effluent (ppm) in effluent (ppm)
0 . 114 0 . 126
0.141 0.156
0.456 0.504
0.398 0.440
0.319 0.353
0.348 0.385
Hotes: Sample holding times were exceeded for effluent samples.
Duplicate samples were taken of the influent. Corresponding effluent duplicates
were not taken.
Information on the analytical method used to generate these data is presented in
Appendix A.
Recovery - Data were recovery-corrected by applying the formula R - X/.745, where R is the
recovery-corrected value, X is the as-reported value, and 0.904 is the percent
recovery divided by 100.
Source: University of Cincinnati 1989a.
3057g
4-13
-------
Table 4-8 Performance Data for the Biological Treatment
of Hastewaters Containing 2-Ethoiyethanol
Concentration of
plant Sampling 2-ethoxyethanol
no. date in influent (ppm)
University of 4/6/89 412
Cincinnati 2020
4/11/89 414
1760
4/14/89 386
1250
4/18/89 466
2105
4/21/89 441
2270
4/25/89 500
2600
4/27/89 954
2640
5/2/89 894
2586
5/4/89 837
2532
5/9/89 442
3070
5/12/89 HD
HD
5/17/89 793
2675
Recovery-corrected
Concentration of concentration of
2-ethoxyethanol 2-ethoxyethanol
in effluent (ppm) in effluent (ppm) Rotes
<10 17.0
<10 17.0
<10 17.0
<10 17.0
<10 17.0
<10 17.0
<10 17.0
<10 17.0
<10 17.0
<10 17.0
<10 17.0
<10 17.0
<10 17.0
<10 17.0
39 66.2
<10 17.0
24 40.7
<10 17.0
22.5 51.3
<10 17.0
23.5 I
<10 y
125 212.2 X
<10 17.0
5/16/89
5/19/89
2070
2720
17.0
17.0
3057g
4-14
-------
Table 4-8 (continued)
Concentration of
Plant Sampling 2-ethoxyethanol
no. date in influent (ppm)
5/20/89
5/23/89
6/27/89
7/4/89
7/11/89
7/18/89
7/25/89
8/1/89
8/2/89
8/3/89
8/4/89
850
2690
797
3340
455
2650
480
3110
480
2690
455
2460
500
2630
532
505
505
438
Recovery-corrected
Concentration of concentration of
2-ethoxyethanol 2-ethoxyethanol
in effluent (ppm) in effluent (ppm) Hotes
296 502.0
<10 17.0
226 384
<10 17.0
<10 17.0
623 1060
30.3 51.4
589 1000
18.1 30.7
782 1330
18.5 31.4
27.8 47.2
63.6 108
576 978
117 199
88.4 ISO
89.2 151
HD
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
Rotes: Two parallel experiments were run, one in which the influent value was always
approximately 500 mg/1 and one in which the influent value was always approximately
2,500 os/1.
Information on the analytical method used to generate these data is presented in
Appendix A.
T Data not used since no 2-ethoxyethanol was detected in Influent.
HD - Hot detected.
X Data not used because system was in upset condition (temperature allowed to get too
high).
Source: University of Cincinnati 1989b.
4-15
3057g
-------
Table 4-9 Hastewater Treatment Performance Data for n-Butyl Alcohol
Rouse
Influent
Technology Concentration
Technology Size Facility
Average
Effluent
Concentration
Removal
(Z) Reference
AS Full 1168E 10000-100000
40.000
99.79 HERL
Source: DSEPA 1989c.
4-16
3057g
-------
5. DETERMINATION OF BEST DEMONSTRATED AVAILABLE
TECHNOLOGY (BOAT)
The Agency has reviewed several data sets relating to the performance
of treatment technologies for wastewaters and nonwastewaters containing
benzene, 1,1,2-trichloroethane, 2-nitropropane, and 2-ethoxyethanol in
F002/F005 solvents.
5.1 Nonwastevaters
For nonwastewaters, EPA has treatment data from a well-designed and
well-operated incinerator treating wastes containing benzene. Thus, BDAT
for benzene-containing nonwastewaters is incineration. For the remaining
wastes, BDAT treatment of nonwastewaters is determined based on transfer
by comparing the parameters that affect treatment of the specific wastes
with parameters of other similar wastes for which demonstrated treatments
are known. Further, the contacted facilities have reported that they
routinely treat these wastes by incineration prior to land disposal. As
a result, the Agency believes that the constituents in the subject wastes
can be treated to the same performance levels as those observed in other
wastes for which the Agency has treatment data. The Agency believes that
none of the constituents in F002 and F005 are likely to interfere with,
or reduce, treatability of the four solvents. This belief is based on
characterization data received from facilities currently incinerating
these wastes. Therefore, BDAT for 1,1,2-trichloroethane, 2-nitropropane,
and 2-ethoxyethanol is incineration by transfer from 1,1,1-trichloro-
ethane, nitrobenzene, and methyl ethyl ketone, respectively, for specific
reasons discussed in Section 6.
5.2 Wastevaters
Performance data sets are available for the treatment of wastewaters
containing benzene, 2-nitropropane, 1,1,2-trichloroethane, and
5-1
30578
-------
2-ethoxyethanol. For benzene, data sets for three technologies are
available: (1) steam stripping, (2) liquid-liquid extraction followed by
steam stripping followed by activated carbon adsorption, and
(3) biological treatment. Biological treatment performance data are
presented in Table 4-2; performance data for steam stripping and liquid-
liquid extraction followed by steam stripping and activated carbon
adsorption are presented in Appendix A. Each of these technologies is
demonstrated and available. A review of the data sets for each
technology indicates that biological treatment achieves the greatest
reduction of the constituent in the effluent. For some of the facilities
for which biological treatment data are available, the treatment
technology includes such additional treatment steps as steam stripping,
ion exchange, solvent extraction, carbon adsorption, and gravity
separation. In those cases where additional treatment steps are present,
however, biological treatment is the principal removal step. Thus,
biological treatment is considered BDAT for benzene-containing
wastewaters.
Both biological and steam stripping treatment data (see Tables 4-4
and 4-5, respectively) are available for 1,1,2-trichloroethane. The
Agency has reviewed these data sets and has concluded that both tech-
nologies significantly reduce the constituent in the treated effluent and
that these treatment levels are comparable. The data sets were compared
using the statistical "analysis of variance" (ANOVA) technique described
in the methodology document (USEPA 1989a). In this analysis the calculat-
ed "F value" is less than the "critical value." Statistically, this
indicates that the mean effluent concentration values of the two treatment
systems are not significantly different (i.e., they are homogeneous);
thus, both technologies are considered to be "best demonstrated."
Therefore, BDAT for 1,1,2-trichloroethane-containing wastewaters is
either biological treatment or steam stripping.
5-2
3057g
-------
For 2-nitropropane, the only treatment performance data available for
wastewater treatment are for steam stripping; however, these data are
flawed (see Section 6.3.1). For a similar compound, nitrobenzene, there
are data for steam stripping followed by carbon adsorption. Nitrobenzene
is believed to be harder to treat by these technologies than 2-nitropro-
pane. Although the treated nitrobenzene data appear to indicate that
this constituent is amenable to steam stripping, the data show flaws in
the design of the steam stripper and the detection of isotropic behavior
of the wastes (see Section 6.3.1). Therefore, BDAT for 2-nitropropane-
containing wastewaters is incineration, or wet air oxidation or chemical
oxidation followed by carbon adsorption.
For 2-ethoxyethanol, the only treatment performance data available to
the Agency are for biological treatment of wastewaters. However, EPA is
not using these data because of system upsets and missed holding times
(see Section 6.A.I). Therefore, BDAT for 2-ethoxyethanol-containing
wastewaters is biological treatment (e.g., activated sludge) based on
transfer of treatment technology from n-butyl alcohol.
5-3
3057g
-------
6. CALCULATION OF TREATMENT STANDARDS
The specific data used in the development of the treatment standards
and the approach used by the Agency to develop these standards are
discussed below for each of the four solvents.
6.1 Benzene
Data from well-designed and well-operated demonstrated treatment
facilities were available to establish the treatment standards for
benzene-'containing wastewaters and nonwastewaters.
6.1.1 Wastewaters
For wastewaters, the Agency is basing the standard on performance
data received from 16 facilities employing biological treatment. These
data are presented in Table 4-2. Data from plants with the V suffix were
recovery corrected by applying actual benzene spike recovery values as
reported in the Summary of Analytical Data to Support BAT Guidelines.
Data from plants with the T suffix do not require recovery correction
because analytical method 1625 was used. (This method automatically
incorporates a recovery-correction factor.) Data from plants with the F
suffix were recovery corrected by applying the formula R •= X/0.51, where
R is the recovery-corrected value, X is the as-reported value, and the
constant 0.51 is the lowest recovery value reported by the V-suffix
facilities.
The mean recovery-corrected concentration of the 133 data points used
in the analysis is 25.0 /ig/1. The statistically determined variability
factor value of 2.88 multiplied by the mean recovery-corrected concentra-
tion results in a treatment standard for benzene wastewaters of 72.0 Mg/1
(rounded to 0.07 mg/1).
6-1
3057g
-------
6.1.2 Nonwastewaters
For nonwastewaters, the Agency has reviewed three data sets on the
performance of incineration systems to treat benzene-containing wastes
(see Table 4-3). The data sets are the Acurex data set (Acurex 1986),
the K011/K013/K014 data set (USEPA 1989b), and the K087 data set (USEPA
1988a). Only one of the ten data points in the Acurex data set (site 1)
was used in determining the standard. (The reported detection limit is
1 mg/kg.) For eight of the remaining Acurex data points either there was
no analysis for benzene in the feed or the untreated waste benzene
concentrations were below detection limits, suggesting that treatment may
not have been substantial. A ninth Acurex data point showed benzene in
the untreated and treated wastes, but the treated waste sample had
benzene concentration data only for the scrubber water and not for the
kiln ash (nonwastewater). Four data points from the BOAT K011/K013/K014
background document were used. (The reported detection limit is
0.01 mg/kg.) Although two other data points were available in this data
set, they lacked data on benzene levels in the treated residuals and thus
were not used in establishing the standard.
The Agency notes the difference in the benzene detection limits of
the three data sets. The Agency also notes that a benzene concentration
below the BOAT K011/K013/K014 background document detection limit of
0.01 mg/kg would also be below the benzene detection limit of 0.025 mg/kg
presented in the K087 background document and the detection limit of
1.0 mg/kg used by Acurex. Therefore, for the purpose of establishing the
standard for benzene, a detection limit of 1.0 mg/kg is assumed for all
benzene incineration ash data. In this way, EPA has reasonable assurance
that all analytical laboratories can measure compliance. Further,
choosing the highest detection limit is consistent with the Third Third
methodology for U and P wastes, as discussed in Section 1 of this
document.
6-2
3057g
-------
The reported benzene recovery factor presented in the K087 background
document data is 98 percent. For the other two data sets, mixtures of
1,2-dichloroethane, toluene, and p-bromofluorobenzene were spiked into
ash samples prior to analysis for volatile organics. The lowest percent
recovery for the Acurex data was 75 percent; for the BDAT K011/K013/K014
background document data, the lowest recovery value was 141 percent. The
75 percent recovery rate is used to set the standard.
To determine the standard, the average of all recovery-corrected
performance data is multiplied by a variability factor. The Agency has
determined that the variability factor of 2.8 should be used when all
performance data are below detection limits, as explained in the
methodology document (USEPA 1989a). Therefore, the standard for benzene
nonwastewaters is 1.0 mg/kg x (1/0.75) x 2.8 - 3.72 mg/kg benzene.
6.2 1.1.2-Trichloroethane
6.2.1 Wastewaters
Data sets for both biological treatment and steam stripping treatment
of 1,1,2-trichloroethane-containing wastewaters were used by the Agency
to establish the treatment standard. As described in Section 5.2, the
ANOVA analyses showed no statistical difference in the treatment
performance of the two technologies.
Biological treatment data are presented in Table 4-4; steam stripping
treatment data are presented in Table 4-5. Biological treatment
performance data consisted of data sets from two facilities. Constituent
levels in the influent waste stream from Plant No. 415 were all below the
detection limit of the constituent; therefore, these data were not used
in establishing the standard because evidence of substantial treatment
cannot be demonstrated. Eleven data points from Plant No. 2631 were used
6-3
3057g
-------
to establish the standard. The reported recovery-correction factor is
98 percent. Data from this plant also included data points with influent
concentrations below detection limits; these data points were not included
in the analysis. The mean recovery-corrected effluent concentration of
the 11 data points used in the analysis is 12.4 Mg/1 • The
statistically determined variability factor of 2.13 multiplied by the
mean recovery- corrected concentration results in a treatment standard for
biologically treated 1 , 1, 2-trichloroethane- containing wastewaters of 26.4
(rounded to 0.03 mg/1) .
Steam stripping treatment data are presented in Table 4-5. While
steam stripping is considered by the Agency to be a fully demonstrated
and available treatment technology, only one of the two data sets is
considered to be from a well-designed and well-operated system (i.e.,
Plant No. 415T) . The second data set, from Plant No. 913, was a public
data submittal, and the Agency is unable to verify whether quality
assurance/quality control procedures for sampling and laboratory analysis
were completely satisfactory or whether the treatment system was well
operated on the days of sampling. For comparison purposes, however,
these data do indicate treatment results similar to those achieved by
Plant No. 415T.
Data from plants with the T suffix do not require recovery correction
because analytical method 1625 was used.
All data on the treated effluent were below the method detection
limit of 10.0 /ig/1. The Agency notes that 1, 1, 2-trichloroethane
concentrations in many of the untreated waste samples were also below
detection limits. Since all treated waste data were also below the
limit, the mean concentration of 1, 1, 2-trichloroethane used in developing
the standard is 10.0 Mg/1- In the instance in which all performance
data for a constituent are nondetects, the Agency uses a variability
6-4
3057g
-------
factor of 2.8 to determine the standard, as explained in the methodology
document (USEPA 1989a). Thus, the calculated standard for 1,1,2-tri-
chloroethane in wastewaters using the steam stripping treatment data is
10.0 /ig/1 x 2.8 = 28.0 /ig/1 (rounded to 0.03 mg/1) , which, by
comparison, is the same value calculated by using the biological
treatment data. Thus, the BDAT standard for 1,1,2-trichloroethane-
containing wastewaters is 0.03 mg/1.
6.2.2 Nonwastewaters
The Agency has no performance data for the treatment of
1,1,2-trichloroethane-containing nonwastewaters. Therefore, the Agency
is setting the standard for 1,1,2-trichloroethane by transferring data
from the treatment of a similar constituent, 1,1,1-trichloroethane, which
the Agency believes should behave similarly to 1,1,2-trichloroethane
when incinerated because of their similarities in structure and
physical/chemical properties.
The Agency has reviewed three data sets on the performance of
incineration systems to treat 1:,1,1-trichloroethane-containing wastes
(see Table 4-6). The data sets are the Acurex data set (Acurex 1986),
the K011/K013/K014 data set (USEPA 1989b), and data from the Final Best
Demonstrated Available Technology Background Document for K016, K018,
K019, K020, and K030 Wastes (USEPA 1988b). Five of the ten data points
in the Acurex data were used in determining the standard. Of the
remaining five data points, four had constituent levels in the feed
reported below the detection limit (thus presenting the possibility that
treatment may not have been substantial) or the constituent had not been
analyzed for, and one data point had 1,1,1-trichloroethane-treated values
only for the air pollution control equipment effluent and not for the ash
or bottoms residue. Four of six data points were used from the BDAT
K011/K013/K014 background document. The remaining two data points
6-5
3057g
-------
did not have the constituent analysis results reported for the treated
residuals. Six data points were used from the BDAT K016/K018/K019/K020/
K030 background document (USEPA 1988b).
The Agency notes the difference in the 1,1,1-trichloroethane
detection limits of the three data sets. Detection values for the Sites
1 through 10 data (Acurex 1986) ranged from 1 /*g/kg for Site 8 to
100 mg/kg for Site 7. A detection limit of 1 MgAg for 1,1,1-
trichloroethane analysis is considered to be suspect by the Agency.
Similar detection limits for volatiles in the wastewater matrix are
achievable, but they are not likely to be achieved in the analysis of
solids. Similarly, a detection limit of 100 mg/kg is so high as to make
the data useless; therefore, data from this site are not being considered
in the analysis. The reported detection limits for 1,1,1-trichloroethane
in the two background documents cited above are 0.01 mg/kg and 2.0 mg/kg.
The Agency uses a logic similar to that presented for determining the
detection limit for the benzene nonwastewater standard; that is, the
highest reported value in the data sets considered in the analysis is
used to establish the standard. Therefore, for 1,1,1-trichloroethane, a
detection of 2.0 mg/kg is assumed for all constituent incineration ash
data. As previously stated, this assumption allows the Agency reasonable
assurance that all analytical laboratories can measure for compliance.
Therefore, since all data used in the analysis were presented as being
below detection limits, 2.0 mg/kg is considered to be the uncorrected
basis for the standard.
The reported constituent recovery factors for the Acurex, BDAT
K011/K013/K014, and BDAT K016/K018/K019/K020/K030 data sets are 75, 100,
and 94 percent, respectively. Each data point used in the analysis has
been corrected by the recovery factor specific to that data set. The
75 percent recovery rate is used to calculate the recovery-corrected
concentration, or 2.0 rag/kg x I/.15 - 2.7 mgAg- The recovery-corrected
6-6
3057g
-------
concentration is multiplied by a variability factor in order to determine
the standard. The Agency notes that the variability factor is 2.8 when
performance data are below detection limits, as explained in the
methodology document (USEPA 1989a). Therefore, the standard for
1,1,2-trichloroethane, which is transferred from 1,1,1-trichloroethane,
is 2.7 mg/kg x 2.8 = 7.6 mg/kg.
6.3 2-Nitropropane
6.3.1 Wastewaters
Data from well-designed and well-operated commercial-scale treatment
facilities are not available to the Agency for 2-nitropropane-containing
wastewaters.
Two data sets were received by the Agency. The first data set was a
pilot-scale study of 2-nitropropane treated by steam stripping at the
University of Cincinnati (University of Cincinnati 1988). However, this
data contained analyses of samples whose holding times were exceeded.
Thus, the development of a treatment standard for 2-nitropropane-
containing wastewaters cannot be based on these data.
A second set of data was reviewed that presented performance data for
treatment of wastewaters containing nitrobenzene by liquid-liquid
extraction, followed by steam stripping and carbon adsorption.
Nitrobenzene should be more difficult to treat using steam stripping and
carbon adsorption than 2-nitropropane, based on a comparison of the
physical properties of both compounds. Table 6-1 presents a comparison
of the physical properties of 2-nitropropane and nitrobenzene. The data
indicate similar solubilities of the two compounds in water. Further,
the lower boiling point and higher vapor pressure of 2-nitropropane
indicate that it should be less difficult to treat than nitrobenzene
6-7
30578
-------
Table 6-1 Physical Properties of 2-Nitropropane and Nitrobenzene
Property
Molecular weight
Boiling point (°C)
Density at 20 °C (g/cm )
Solubility at 20°C (percent)
Vapor pressure at 28.2°C (mmHg)
2-Nitropropane
89.09
129.25
0.99
1.7
22
Nitrobenzene
123.0
210.9
1.19
1.9
<1.0
6-8
3057g
-------
using steam stripping. Carbon adsorption is expected to treat residual
2-nitropropane from the steam stripper to the nondetect level as it did
for nitrobenzene because less nitropropane should be contained in the
steam stripper treated effluent. Performance data for treatment of
wastewaters containing nitrobenzene by steam stripping followed by carbon
adsorption is presented in Table 6-2. Although the treated nitrobenzene
data appear to indicate that this constituent is amenable to stream
stripping, the data show flaws in the design of the steam stripper and
detection of azeotropic behavior of the wastes.
At this time, EPA is withdrawing the alternative method of treatment,
steam stripping followed by carbon adsorption, for F005 wastewaters
containing 2-nitropropane. This revision to the proposed regulatory
approach follows EPA's determination that the adoption of steam stripping
followed by carbon adsorption technology as BDAT should require minimum
operating conditions to ensure that 2-nitropropane wastewaters to not go
untreated through this treatment technology. EPA based its determination
on the azeotropic behavior of 2-nitropropane in F005 wastewaters and the
fact that steam stripping of azeotropes could require a combination of
more than one distillation unit. EPA lacks sufficient information to
incorporate such requirements in the BDAT standard. EPA, however, has
determined that wet air oxidation followed by carbon adsorption as well
as chemical oxidation followed by carbon adsorption, represent BDAT for
2-nitropropane based on the treatment of wastewater containing nitro-
benzene. EPA is promulgating these last two treatment technologies as an
alternative treatment standard for F005 wastewaters and nonwastewaters
containing 2-nitropropane. Wastewater effluents from the carbon
adsorption unit can be land disposed. Nonwastewater residues from these
two alternative treatment technologeis must meet the nonwastewater
treatment standards for F005 nonwastewaters containing 2-nitropropane, as
a pre-requisite for land disposal.
6-9
3057g
-------
Several commenters have expressed concern over the proposal of
different treatment technologies for the same waste constituent. The
Agency realizes the burden of treating constituents for which different
wastewater criteria for the same listed waste have been promulgated.
However, these problems are academic since the Agency is promulgating
incineration or wet air oxidation followed by carbon adsorption, or
chemical oxidation followed by carbon adsorption as a method of treatment
for wastewater forms of 2-nitropropane.
EPA believes that the promulgated treatment standard option of
oxidation, chemical or wet-air, followed by activated carbon is superior
to steam stripping because steam stripping is considered a technology
that treats the waste, whereas oxidation technologies destroy the waste.
Oxidation followed by carbon adsorption is also superior because
oxidation is more rugged than biotreatment: an oxidation system is less
easily disabled by a refractory influent stream and more easily restored
to working order than a biological treatment unit. As discussed in the
proposed rule, wet-air oxidation is most appropriate for those
wastewaters near the wastewater cutoff level (i.e., 1 percent TOC), while
chemical oxidation effectively treats those wastes with lower percentages
of TOC. EPA's decision to require activated carbon following the
oxidation step ensures a backup system to compensate for the uncertainty
about final effluent concentrations of these U and P wastes inherent in
any process treating unquantifiable wastes. Most importantly, however,
since spent activated carbon from treating these wastewaters becomes a
nonwastewater form of these wastes (54 FR 48384) and thus must be
incinerated according to the promulgated nonwastewater standard,
requiring activated carbon treatment ensures that both wastewater and
nonwastewater forms of these wastes go to incineration, a method
demonstrated to successfully treat a wide variety of organic wastes.
6-10
3057g
-------
Table 6-2 Performance Data for Treatment of Wastewaters Containing
Nitrobenzene by Steam Stripping Followed by Carbon Adsorption
Untreated waste (mg/1) Treated waste (mg/1)
K103 K104
<1500
<1500
<3000
<3000
<3000
2700
2200
2300
2900
3900
<0.03
<0.03
<0.15
<0.03
<0.03
Source: USEPA 1988c. Data obtained from Onsite Engineering Report for
E.I. Du Pont de Nemours, Inc., Beaumont, Texas.
6-11
3057g
-------
6.3.2 Nonwastewaters
The Agency has no performance data for the treatment of 2-nitropro-
pane-containing nonwastewaters. In addition, the Agency has determined
that concentration-based treatment standards cannot be promulgated for
nonwastewater forms of this constituent because not enough data are
available to support the proposed standard. As a result, the Agency is
promulgating treatment standards for this constituent expressed as
methods of treatment. The method of treatment for nonwastewater forms of
2-nitropropane is incineration.
6.4 2-Ethoxvethanol
6.4.1 Wastewaters
Data from well-designed and well-operated commercial-scale treatment
facilities are not available to the Agency for 2-ethoxyethanol
contaminated wastewaters. A data set consisting of 41 data points is
available from pilot-scale studies conducted at the University of
Cincinnati (University of Cincinnati 1989b), where synthetic wastewaters
containing 2-ethoxyethanol were treated by biological treatment and
removal efficiencies greater than 99 percent were achieved (see
Table 4-8). The analytical method used to analyze 2-ethoxyethanol is
described in Appendix B. The studies included results from two
systems--one using a concentration of 500 mg/1 of the constituent in the
feed and the other using 2,500 mg/1. The Agency notes that according to
information reported by the source, the pilot data indicate several plant
upsets. One upset resulted from high ambient temperatures in the test
area from the end of June through early July; the other resulted from
sludge recycle problems in the 500-mg/1 system in May.
6-12
3057g
-------
The analytical data for biological treatment also included analysis
of samples whose holding times were exceeded prior to analysis;
therefore, EPA is not using these data. Further, EPA is attempting to
develop a more precise analytical test for 2-ethoxyethanol. A copy of
the procedure is attached as Appendix B. However, in view of the
experimental status of this method, EPA at this time is not setting any
concentration-based treatment standards but is instead promulgating a
method of treatment.
EPA does, however, have data for biological treatment (e.g.,
activated sludge) of n-butyl alcohol. n-Butyl alcohol is a very similar
compound based on a comparison of the physical and structural properties
of 2-ethoxyethanol and n-butyl alcohol. This comparison indicates
similar structures, molecular weights, and boiling points (see
Table 6-3). The data for n-butyl alcohol indicate that an influent
concentration of up to 100 ppm can be treated to a concentration of
0.04 ppm. These performance data are presented in Table 6-4. The Agency
believes 2-ethoxyethanol can also be treated to these levels based on
similarities in physical ad structural properties to n-butyl alcohol.
Therefore, the Agency is promulgating biological treatment (e.g.,
activated sludge) as a method of treatment for 2-ethoxyethanol based on
transfer from n-butyl alcohol.
6.4.2 Nonwastewaters
The Agency does not have performance data for the treatment of
2-ethoxyethanol nonwastewaters. In addition, the Agency has determined
that concentration-based treatment standards cannot be promulgated for
nonwastewater forms of this constituent because not enough data are
available to support the proposed standard. As a result, the Agency is
promulgating treatment standards for this constituent expressed as
methods of treatment.
6-13
3057g
-------
Table 6-3 Physical and Structural Properties of
2-Ethoxyethanol and n-Butyl Alcohol
Property 2-Ethoxyethanol n-Butyl Alcohol
Empirical formula ^4^10^2 C^H^O
Molecular weight 90.12 74.12
Boiling point (°C) 135 118
Molecular formula HOCH2CH2OC2Hij CH3CH2CH2CH2OH
6-14
3057g
-------
Table 6-4 Hastewater Treatment Performance Data for n-Butyl Alcohol
Range
Influent
Technology Concentration
Technology Size Facility (PF*>)
Average
Effluent
Concentration
Removal
(Z) Reference
AS Full 1168E 10000-100000
40.000
99.78 HERL
Source: USEPA 1989c.
6-15
3057g
-------
However, EPA does have data for incineration of nonwastewater forms
of methyl isobutyl ketone (MIBK). Because of its similarity in
structure, boiling point, vapor pressure, and heat of combustion,
2-ethoxyethanol should behave similarly to MIBK when incinerated. Based
on an examination of data from numerous facilities that incinerate
MIBK-containing nonwastewaters, the Agency expects that MIBK will be
completely destroyed in incineration systems that are well designed and
well operated. Therefore, the Agency is promulgating incineration as the
method of treatment for nonwastewaters containing 2-ethoxyethanol.
6-16
3057g
-------
7. REFERENCES
This reference list contains only those references that were not
included in the F001-F005 spent solvent background document (USEPA 1986)
Acurex. 1986. Characterization of hazardous waste incineration
residuals. Acurex final report FR-86-102/EE. Acurex Corporation,
Mountain View, California.
Cain Chemical. 1988. Telefax dated October 31, 1988, from R. Orpeneck
(Cain Chemical) to J. Vorbach (U.S. Environmental Protection Agency).
Eastman Kodak. 1988. Letter dated August 23, 1988, from B. Klauderman
(Eastman Kodak) to J. Vorbach (U.S. Environmental Protection Agency).
IITRI. 1989. IIT Research Institute. Jody, B.J., andR.J. Dihu. In
proceedings of the 6th National Conference on Hazardous Wastes and
Hazardous Materials, April 12-14, 1989, New Orleans, pp. 559-562.
Safety-Kleen. 1988. Letter dated November 28, 1988, from S. Walczyuski
(Safety-Kleen) to J. Vorbach (U.S. Environmental Protection Agency).
Sinclair and Valentine. 1988. Letter dated October 11, 1988, from
S. Barker (Sinclair and Valentine) to J. Vorbach (U.S. Environmental
Protection Agency).
University of Cincinnati. 1989a. Hazardous waste treatment technology
assessments. Volume II. Organics treatment - physical separation.
Cincinnati, Ohio: University of Cincinnati, Department of Civil and
Environmental Engineering.
University of Cincinnati. 1989b. Hazardous waste treatment technology
Assessment, Volume III. Organics treatment - biological processes.
Cincinnati, Ohio: University of Cincinnati, Department of Civil and
Environmental Engineering.
USEPA. 1983. U.S. Environmental Protection Agency, Office of Water.
Summary of analytical data to support BAT guidelines. Washington, D.C.
U.S. Environmental Protection Agency.
USEPA. 1986. U.S. Environmental Protection Agency, Office of Solid
Waste. Final best demonstrated available technology (BOAT) background
document for F001-F005 spent solvents. 3 vols. EPA/530-SW-86-056.
Washington, D.C.: U.S. Environmental Protection Agency.
7-1
3057R
-------
USEPA. 1987a. U.S. Environmental Protection Agency, Office of Water.
Final development document for effluent limitations guidelines and
standards for the organic chemicals, plastics and synthetic fibers
point source category. EPA 440/1-87/009. Washington, D.C: U.S.
Environmental Protection Agency.
USEPA. 1987b. U.S. Environmental Protection Agency. Administrative
record accompanying the final rule for the effluent limitations
guidelines for the organic chemicals, plastics and synthetic fibers
data base. (52 FR 42522-42584). BAT subcategory one and two final
edited data base listings. Sorted by pollutant number.
USEPA. 1988a. U.S. Environmental Protection Agency, Office of Solid
Waste. Final best demonstrated available technology background
document for K087 wastes. Washington, D.C. U.S. Environmental
Protection Agency.
USEPA. 1988b. U.S. Environmental Protection Agency, Office of Solid
Waste. Final best demonstrated available technology background
document for K016, K018, K019, K020, and K030 wastes.
EPA/530-SW-88-031B. Washington, D.C.: U.S. Environmental Protection
Agency.
USEPA. 1988c. U.S. Environmental Protection Agency, Office of Solid
Waste. Final best demonstrated available technology background
document for K103 and K104 wastes. Washington, D.C.: U.S.
Environmental Protection Agency.
USEPA. 1989a. U.S. Environmental Protection Agency, Office of Solid
Waste. Methodology for developing best demonstrated available
technology (BDAT) treatment standards. Washington, D.C.: U.S.
Environmental Protection Agency.
USEPA. 1989b. U.S. Environmental Protection Agency, Office of Solid
Waste. Final best demonstrated available technology (BDAT) background
document for K011, K013, and K014 wastes. Washington, D.C.: U.S.
Environmental Protection Agency.
USEPA. 1989c. Office of Research and Development. Computer printout:
Data on wastewater treatment from the WERL treatability database.
Retrieved 02/89. Cincinnati, OH: U.S. Environmental Protection Agency
Versar. 1988. Notes of telephone calls to potential generators of
F002/F005 containing the four solvents in question.
7-2
3057g
-------
APPENDIX A
PERFORMANCE DATA FOR TREATMENT OF
BENZENE-CONTAINING WASTEWATERS
-------
Plant
Table A-l Performance Data for Steam Stripping of
Benzene-Containing Wastewaters
Date
Influent concentration
(ppb)
Recovery-corrected
effluent concentration
(ppb)
415P 1/31/85
2/1/85
2/11/85
2/11/85
12/4/85
12/5/85
12/6/85
1494T 1/22/84
1/25/84
2/5/84
2/6/84
2/7/84
2/8/84
2/9/84
2/10/84
2/12/84
2/13/84
2/14/84
2/15/84
2/16/84
2680T 3/25/84
3/26/84
3/27/84
3/28/84
3/29/84
4/1/84
4/2/84
4/3/84
4/4/84
4/5/84
ND
ND
22,300
48,100
412,000
279,000
274,000
1,242,040
1,076,150
289,500
372,910
1,068,840
1,551,220
1,591,810
166,040
ND
137,303
198,146
269,360
1,506,800
94,893
147,212
34,693
61,172
61,110
83,329
54,921
129,069
127,658
127,530
80 a
55 a
<10 a
<10 a
329 a
138 a
134 a
171
57
<10
95
76
38
32
53
<10
<10
<10
<10
<10
<10
<10
<10
<10
<10
<10
<10
<10
<10
<10
aData not used; improper QA/QC or no QA/QC used.
Source: USEPA 1987b.
A-l
30578
-------
Table A-2 Performance Data for Liquid-Liquid Extraction
Followed by Steam Stripping Followed by Activated
Carbon Adsorption of Benzene-Containing Wastewaters
Parameter
Influent concentration (ppb)
K103 K104
Recovery-collected
effluent concentration (ppb)
Benzene
81,000
73,000
65,000
55,000
32,000
240,000
320,000
70,000
11,000
4,500
55
7
22 a
25
12
aData not used; system not well operated.
Source: EPA-collected data presented in USEPA 1988c.
A-2
3057g
-------
APPENDIX B
ANALYTICAL METHODS
FOR
2-NITROPROPANE AND
2-ETHOXYETHANOL
-------
Analytical Method for 2-Nitropropane
Samples were prepared for measurement of 2-nitropropane and other
BDAT parameters in accordance with SW-846 Method 8030. Options included
SW-846 Method 5030 (purge and trap) and instrument calibration by an
external standard.
Analytical Method for 2-Ethoxyethanol (2E)
The Federal Register (40 CFR Chapter 1, Part 261, App. Ill)
recommends SW-846 Methods 8030 and 8240 for the detection of 2E. Initial
analytical efforts established that the usual cleanup methods, purge and
trap or heated purge and trap (SW-846 Method 5030), resulted in very poor
recoveries because of the low purging efficiency of 2E. Direct injection
was identified as the only choice. However, direct injection of aqueous
samples significantly deteriorates the performance of GC/MSs, rendering
Method 8240 impractical for routine analysis of samples. Validation was
attempted for Method 8030 with direct injection. Reliable data could not
be obtained for 2E, but methylene chloride and toluene recoveries from
the same samples were excellent, leading the analyst at EER Technologies
Corporation and the project staff to believe that the GC column and not
the technique was at fault. An adaptation of this method utilizing a
different GC column was tested.
This adapted method utilized a packed gas chromatograph column
containing 3 percent SP1500 on 80/120 mesh Carbopack B and the run
conditions found in Table B-l. The chosen column was tested at the
specified conditions on spiked sample matrices. The project staff
developed a scheme of injections to formalize the process of determining
the validity of the results. EER Technologies Corporation analyzed the
samples and reported the data in Table B-2 as well as the information
summarized below:
In analyzing standards to develop a calibration curve, the resulting
curve yielded a fairly linear response (r2 - 0.9760, y - 2.056x -
19.64). The surrogate responses gave mean peak height responses of 21.5
for methylene chloride and 104 for toluene, with standard deviations of
2.55 and 1.72, respectively. Injections to obtain the MDL and MQL were
carried out as outlined in SW-846, and the appropriate calculations were
made. Based on this testing, the MDL and MQL were calculated to be 1.15
and 1.91, respectively, but EER felt that a more realistic value for the
MQL would be 5.0 mg/1 since injections at the 2.0-mg/l level did not
exhibit a measurable peak.
B-l
3057g
-------
Table B-l Gas Chromatograph Conditions for 2E Analysis
Parameter
Value
GC column
Column packing
Injection temperature
Column temperature
Detector temperature
Detector type
Carrier gas
Injection volume
Temperature program
6' x 1/8" stainless steel
80/120 mesh Carbopack B w/32 SP1500
250°C
220°C
300°C
FID at 128 x
Nitrogen at 20 ml/min
2 ftl
4 min at 50°C then to 220°C
at 32°C/min and hold
10•10 AFS
Table B-2 Validation Data for 2E Analytical Method
Sample Matrix
Unpreserved feed
Unpreserved
effluent
Preserved feed
Preserved effluent
Run 1
Run 2
Avg
XRR
Run 1
Run 2
Avg
& RR
Run 1
Avg
Run 1
Run 2
Avg
% RR
Matrix
Spike
(% Rec.)
96.0
105.0
101.0
8.96
87.4
92.9
90.2
6.10
93.2
93.2
88.2
99.3
93.8
11.8
Matrix
Spike
Dup.
(% Rec.)
100.0
106.0
103.0
5.82
98.5
92.9
95.7
5.85
102.0
102.0
102.0
92.8
97.4
9.40
% Relative
Range
4.08
0.95
2.46
11.9
0.00
5.97
9.02
9.02
14.5
6.77
3.82
NOTE: The Method Detection Limit (MDL) was determined to be 1.15 mg/1
and the Method Quantitation Limit (MQL) was determined to be
1.91 mg/1. These limits were determined via methods outlined in
SW-846. The spiking concentration used was 5 times the MQL,
which was 10.0 mg/1. Seven blanks were also run, and the average
background "noise" was 5.14 mg/1 with a standard deviation of
0.06 mg/1.
B-2
3057s
-------
As testing with the column continued, it showed decreased
sensitivity. It is not unusual for a GC system to vary by this amount,
especially using direct injection and an FID detector. Also, the
variation may have been the result of short shelf-life of the stock
standard. Recalibration was done with freshly prepared stock standard,
and the results were acceptable. Since the sensitivity of the column
resulted in poor results as testing continued, a new column was
installed, but the original sensitivity was never reproduced. The MQL
was then increased to 10 mg/1.
Source: University of Cincinnati 1989b.
B-3
3057g
------- |