United States EFA-600/7-84H360
Environmental Protection
Agency Ma 1984
£EPA Research and
Development
FEASIBILITY OF USING
SOLID ADSORBENTS
FOR DIOXIN SAMPLING
Prepared for
Office of Environmental Engineering and Technology
Prepared by
Industrial Environmental Research
Laboratory
Research Triangle Park NC 27711
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i
This document is available to the public through the National Technical Informa-
tion Service, Springfield, Virginia 22161. :
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EPA-600/7-84-060
May 1984
FEASIBILITY OF USING SOLID ADSORBENTS
FOR DIOXIN SAMPLING
by
F. L. DeRoos and A. K. Wcnsky
BATTELLE
Columbus Laboratories
Columbus, Ohio 43201
Contract Number 68-02-3628
Work Assignment 008
EPA Project Officer:
Merrill D. Jackson
Industrial Environmental Research Laboratory
U. S. Environmental Protection Agency
Research Triangle Park, NC 27711
Prepared for
Office of Environmental Engineering and Technology
OFFICE OF RESEARCH AND DEVELOPMENT
U. S. ENVIRONMENTAL PROTECTION AGENCY
WASHINGTON, D.C. 20460
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ABSTRACT
The recovery efficiencies from Amberlite* XAD-2 resin and Florisil*
of spiked 2,3,7,8-tetrachlorodibenzo-p-dioxin (2,3,7,8-TCDD) were determined
in order to assess the suitability of these adsorbents for sampling. Two
spiking methods were used: Method A consisted of uniformly depositing 1 mL of
the spiking solution onto the adsorbent, and Method B consisted of covering the
whole adsorbent sample with the spiking solution. No significant difference
in recovery efficiencies was found between the two methods or between the two
adsorbents under study. The overall percent recovery from Amberlite* XAD-2
resin was 92 * 8 and from Florisil*, 95 * 6.
ii
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CONTENTS
Abstract ii
Figures . . iv
Tables iv
1. Introduction 1
2. Conclusions 2
3. Experimental 3
Method A 3
Method B 3
Sample Extraction and Cleanup 3
Instrumental Analysis 6
Quality Control 7
4. Results and Discussion 13
References 16
Appendix A . Quality Assurance Audit Report A-l
ii-i
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FIGURES
Number Page
1 Multilayer silica column for clean-up of extract ........ 5
2A Trace of m/z 320 in standard test mixture (20 pg
2,3,7,8-TCDD and 95 pg of 2,3,7,8-TCDD-l3C12 ......... 8
2B Trace of m/z 322 in standard test mixture (20 pg
2,3,7,8-TCDD and 95 pg of 2,3,7,8-TCDD-13C12 ......... 9
2C , Trace of m/z 332 in standard test mixture (20 pg
2,3,7,8-TCDD and 95 pg of 2,3,7,8-TCDD-13Ci2 ......... 1°
2D Trace of m/z 334 in standard test mixture (20 pg
2,3,7,8-TCDD and 95 pg of 2,3,7,8-TCDD-13C12 ......... 11
TABLES
1 Summary of performed experiments 4
2 Recovery data for spiked native 2,3,7,8-TCDD on XAD-2 resin . . 14
3 Recovery data for spiked native 2,3,7,8-TCDD on Florlsil. ... 15
iv
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SECTION 1
INTRODUCTION
Due Co Che well known coxicicy and ubiquitous nature of polychlorinaced
dibenzo-p-dioxins (PCDDs) chey are Che subject of great interest in deter-
mining their route of entry into the environment. Although PCDDs are known
co be formed during cercain industrial chemical manufacturing processes (e.g.,
polychlorophenols and their derivatives), ic is suspected that combustion
sources may be the major source of environmental loading. In order to deter-
mine Che presence of trace quantities of this class of compounds (in com-
bustion gas screams), 2,3,7,8-cecrachlorodibenzo-p-dioxin (2,3,7,8-TCDD) was
chosen as a test case. Two programs were initiated by the U.S. Environmental
Protection Agency in order Co demonstrate the reliability of the sampling and
analysis procedures.
This program which was aimed at assessing the extraccion efficiency of
2,3,7,8-TCDD from Amberlite* XAD-2 or Florisil*, the adsorbents normally
used in collecting organics emitted from combustion sources in either the
Source Assessment Sampling Syscem (SASS) train or the Modified Method 5 (MM5).
The other program conducted under Task 131, Contract Number 68-02-2686,
focused on determining Che recovery efficiency of a continuous, dynamic
calibration spike of 2,3,7,8-TCDD directly in Che emission of an operacing
combuscion system using either che SASS or MM5 sampling trains.
The data obtained from these two studies demonstrated the efficiency of
dioxin recovery in the sampling system as a whole and in adsorbent material
that constitutes the collection medium of the TCDD in particular.
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SECTION 2
CONCLUSIONS
No significant difference was observed in spike recoveries
whether spiking Method A where 1 ml aliquot of che spike
solution was deposited on the adsorbent or Method B where
25 ml of the spiking solution covered the whole adsorbent
sample was used. However, Method B appears to be slightly
more representative of how TCDO will be distributed and
adsorbed on the surface of the actual sample.
The average percent recovery of spiked 2,3,7,8-TCDD from
XAD-2 at 2.1 ng and 16.5 ng levels was 94 + 6 when Method A
was used and 91 * 10 when Method B was used.
The average percent recovery of spiked 2,3,7,8-TCDD at
2.1 ng and 16.5 ng levels from Plorisil was 102 + 6 when
Method A was used and 89 + 6 when Method B was used.
The overall average percent recovery of 2,3,7,8-TCDD in all
of the experiments performed with XAD-2 was 92 * 8. This
number is comparable with the overall average recovery of
96Z obtained for the whole system as described in Task 131,
Contract Number 68-02-2686.
No significant difference in recovery efficiencies of
2,3,7,8-TCDD from either XAD-2 or Florisil was observed.
However, XAD-2 has the advantage of being a more universal
adsorbent for organics in general.
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SECTION 3
EXPERIMENTAL
The spiking of 2,3,7,8-TCDD into Amberlite® XAD'-Z and Florisil® was
carried out using two Methods, A and B.
METHOD A
This method consisted of uniformly depositing 1 mL of methyLane chloride
containing either 3 ng or 30 ng of 2,3,7,8-TCDD onto the surface of a 15 g
portion of the adsorbent. This method is not expected to result in a uniform
distribution on the adsorbent.
METHOD B
This method consisted of depositing -25 mL of the methytene chloride
spiking solution to cover the whole body of the adsorbent. The spiking,
therefore, was uniform onto the adsorbent. The methyiene chloride was
removed by evaporation at room temperature for both methods.
A summary of Che experiments performed and Che spike levels is given in
Table 1.
SAMPLE EXTRACTION AND CLEANUP
Each of the adsorbent samples, spiked with 2,3,7,8-TCDD using either
Method A or Method B, was Soxhlet extracted for 16 hours with 250 mL of
methylene chloride. The methylene chloride extract was spiked with 2 ng of
2,3,7,8-TCDD-l-'Ci2 co serve as an internal standard for quantification of
native 2,3,7,8-TCDD and to correct for any losses which occurred during Che
clean-up and concentration of the extracts.
The methylene chloride extracts^were quantitatively transferred Co
Kuderna-Oanish (K-0) concentrators using three 10 mL rinses of fresh
methylene chloride and concentrated to approximately 1 mL.
The extracts were cleaned up by passing them through a series of gravity
fed liquid chromatography columns. The first column was a mulcilayered silica
column containing alcernate layers of activated silica, 44Z concentrated
sulfuric acid on silica and 33Z 1M potassium hydroxide on silica. This column
is schematically illustraced in Figure 1. The concentrated methylene chloride
extract was Cransferred Co the column using chree 5 mL rinses of hexane. The
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TABLE 1. SUMMARY OF PERFORMED EXPERIMENTS
Adsorbent
XAD-2
XAD-2
XAD-2
XAD-2
XAD-2
XAD-2
Florisil
Florisil
Florisil
Florisil
Florisil
Florisil
Spiking
Method
A
A
A
B
B
B
A
A
A
B
B
B
Number of
Replicate (s)
1
3
3
1
3
3
1
3
3
1
3
3
2,3,7,8-TCDD
Spike
(ng/15 g)(a>
0
2.1(C)
16.5(c)
0
2,l(c)
16.5(C)
0
2.1(c)
16.5(c)
0
2.1(c)
16.5(c)
2,3,7,8-TCDD
Level
(ng/m3)0>)
0
0.7
5.5
0
0.7
5.5
0
0.7
5.5
0
0.7
5.5
TOTAL NUMBER OF TESTS:
28
(a) 150 g XAD-2 or Florisil is the standard amount used in a SASS
train adsorbent cartridge. This quantity was scaled to
15 gm (10%) in order to minimize the use of 2,3,7,8-TCDD.
(b) Based on 30 m^ total stack gas emissions for a standard SASS
train run.
(c) These are the actual levels obtained when the spiked solutions
targeted at 3 ng and 30 ng were analyzed.
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Activated silica
44Z Sulfuric acid on silica
Activated silica
gm)
33% 1M Potassium Hydroxide on Silica
gm)
Glass wool
Figure 1. Multilayer silica column for clean-up of extract.
column vas eluced with approximately 25 mL of hexane/benzene (1:1) with che
entire eluate being collected. The mulciLayered silica column removed acidic and
basic compounds that might have been co-extracted along with the 2,3,7,8-TCDD as
well as the easily oxidized materials. Although this step is often accomplished
using liquid-liquid washes in a separatory funnel, che mulcilayered silica column
reduces the losses of analyte due to adsorption on glass surfaces and interfacial
losses caused by poor separation of the liquid phases as observed both in
Battelle and Dow Chemical Laboratories.
The eluate from che multilayered silica column.was concentrated using a K-D
concentrator and solvent exchanged into 1-2 mL of hexane and added to a second
chromatographic column containing approximately 5 g of activated basic alumina.
This column was sequentially eluted with 40 mL of hexane, 25 mL of hexane/carbon
cetrachloride (1:1), and 20 mL of hexane/mechylene chloride (1:1). The hexane/
me thy1ene chloride eluate which contained the 2,3,7,3-TCDO was collected and
solvent exchanged into 20 uL of n-detfane. The n-decane concentrate was stored at
0°C until it was analysed.
The solvents used, hexane, benzene, carbon cetrachloride, and methylene
chloride, were Distilled-in-Glass* (Burdick and Jackson Laboratories, Inc.,
Muskegon, MI). Alumina and silica gel were purchased from BioRad Laboratories,
Richmond, CA. These were solvent rinsed and activated immediately prior to
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being used. The 2,3,7,8-tetrachlorodibenzo-p-dioxin-13C12 C2,3,7,8-TCDD-13C12,
was purchased from KOR Isotopes, Cambridge, MA, and the 1,2,3,4-tetrachloro-
dibenzo-p-dioxin (1,2,3,4-TCDD) was purchased from Ultra Scientific, Inc.,
Hope, RI. All analytical glassware was washed with soap and water, rinsed
with reagent grade acetone, and baked at 450 °C for a minimum of 12 hours
prior to use.
The XAD-2 precleaned resin, grade number 2-0279 (Supelco, Inc., Belief onte,
PA) was extracted for 18 hours with methylene chloride and dried with a fluidize
bed technique prior to being used. Test batches of resin were extracted and
blanks checked by glass capillary GC/FID prior to use.
The Florisil was purchased from Sigma Chemical Company, St. Louis, MO,
product number F-9217, 60-100 mesh activated at 677°C (1250°F) . It was
washed with methylene chloride and dried at 400 °C prior to use.
INSTRUMENTAL ANALYSIS
The 2,3,7,8-TCDD was quantified in the extracts using high resolution
gas chromatography/high resolution mass spectrometry (HRGC/HRMS) . The HRGC
system was a Carlo Erba Model 4160 gas chromatograph operated under the
following conditions:
Column: 30m DB-5
Carrier Velocity: 30 cm/sec
Starting Temperature: 120°C
Hold Time at Start: 3 min
Program Rate: 20°C/min
Final Temperature: 260 °C
Hold Time at Maximum: 9 min
Injection: splitless, split closed
for 45 seconds
The HRMS system was a VG Model MM-7070H high resolution mass spectrometer
used under the following conditions:
Electron lonization: 70 eV
Accelerating Voltage: 4000 volts
Electron Emission: 200 ya
Source Temperature: 200 °C
Resolution: ' . 10,000-12,000, M/AM, 10% valley
A VG Model 2035 data system capable of controlling ' le mass spectrometer
under high resolution multiple ion detection CHRMID) conditions was used.
All data were stored on 9-track magnetic tape and will be retained for
five years.
The 2,3,7,8-TCDD levels were quantified by comparing the response of the
2,3,7,8-TCDD with that of the 2,3, 7,8-TCDD-13C12 using the following equation:
2,3,7,8-TCDD (ng) - ^ °J ffi ]% x ng of 2,3,7,8-TCDD-13^
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QUALITY CONTROL
The HRCC was checked at Che scare of each day as well as periodically
during Che course of Che analyses. The checks consisced of injecting known
quantities of both 2,3,7,8-TCDD and mixed TCDD isomer solutions. These
injeccions served to verify Che chromacographic resolution, peak shape,
injector liner status, column adsorption, absolute mass spectrometer
sensitivity, and correct mass focus of the MID unit. From past experience,
variations in these parameters, such as absolute response, can be correlaced
Co specific instrument conditions which need attention.
The HEWS was tuned each day using perfluorokerosene (PFK). The tuning
consisced of optimizing the various lens and focus voltages to provide the
best sensitivity and peak shape. The resolution was adjusted such chat it was
between 10,000 and 12,000 (10Z valley, M/AM definition). The lock mass, for
MID control, was m/z 319 for PFK. Its mass focus was verified by the mass
marker as well as by manual interpretation. During the analyses its intensity
was monitored Co assure that sensitivity changes did not occur. Five ion
masses were monitored during each analysis. They were:
m/z 318.9792 Mass Spectrometer Lock Mass
m/z 319.8965 Native TCDD
m/z 321.8936 Native-TCDD
m/z 331.9368 TCDD-f^C .
rn/z 333.9338 TCDD- C^
The lock mass peak was produced from a low level of PFK which was continuously
introduced into the ion source using the batch inlet. The peak was centroided
by the. data system to provide mass focus correction thus assuring that the
TCDD ion masses were accurately monitored. Two native TCDD ion masses and two
TCDD- C.2 ion masses were monitored to enhance the specificity of Che
analyses. Although one ion mass from each would be sufficient for quantifi-
cation (e.g., m/z 320 and m/z 332 or m/z 322 and m/z 334) by monitoring two
masses, it is possible to include the isotope ratio as one of the criteria for
identifying TCDD.
The criteria used in this program Co identify 2,3,7,8-TCDD were Che
following:
o Retention cime muse agree wich Che internal standard within
± 1 sec
o Ratio of m/z 320 to m/z 322 must be 0.77 ± 0.08 (101) of 77
o Signal to noise ratios for m/z 320 and m/z 322.must be greater
than 3/1.
A cypical analysis of a 2,3,7,8-TCDD test mixture containing 95 pg/uL of
2,3,7,8-TCDD- C12 and 20 pg/yL of 2,3,7,8-TCDD is shown in Figures 2A, 2B,
2C, and 2D.^frora this analysis the chromatographic performance was verified
and the quantitative accuracy of the system was assessed. For each test
mixture that was analyzed the quantity of 2,3,7,8-TCDD present was calculated.
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Figure 2A. Trace of m/z 320 in standard test mixture
(20 pe 2,3,7,8-TCDD and 95 pg of 2,3,7,8-
TCDD-I3C12-
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I.*.
figure 2B. Trace of m/z 322 in standard test mixture
(20 pg 2,3,7,8-TCDD and 95 pg of 2,3,7,8-
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Figure 2C. Trace of m/z 332 in standard test mixture
(20 pg 2,3,7,8-TCDD and 95 pg of 2,3,7,8-
TCDD-13c12.
10
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Figure 2D. Trace of n/z 334 in standard test mixture
(20 pg 2,3,7,8-TCDD and 95 pg of 2,3,7,8-
TODD-13c12.
11
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In addition the ratios of m/z 320/m/z 322 and m/z 332/m/z 334 were also calcu-
lated. The quantity of 2,3,7,3-TCDD determined as well as Che ion ratios are
sensitive to any error in MID mass assignment. Typically the 2,3,7,8-TCDD
will quantify to 20 pg ± 3 pg and the ion ratios will compare within ± 0.07 of
the theoretical value (0.77). ..._.
Method blanks and solvent injections were also analyzed concurrently with
the samples. The method blanks served to verify that TCDOs were present in
the extraction solvent, liquid chromatography packing material, or elution
solvents. The solvent injections were used to determine if any carry over
occurred following the analysis of a sample containing 2,3,7,8-TCDD. Solvent
injections were made periodically, however, they were always made following a
sample which contained relatively high levels of TCDDs as compared to the
average of the group.
At the completion for the work assignment, the Battelle QA Officer,
Mr. Richard E. Heffelfinger reviewed the completed work and checked for
compliance with the QA/QC requirements of the workplan. The results of his
audit are summarized in the Task Quality Assurance (QA) Audit report in
Appendix A.
12
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SECTION 4
RESULTS AND DISCUSSION
The results of Che twenty eight spiking experiments are summarized in
Table 2 for XAD-2 resin and Table 3 for Florisil. The 2.1 ng and 16.5 ng
levels were the actual determined levels in the spiking solution targeted
at 3 ng and 30 ng. The low determined levels are most likely due to
decomposition of the 2,3,7,8-TCDD during the storage period or possibly due
to adsorption on the surface of the container. In general, the overall per-
cent recovery data from either the XAD-2 resin or Florisil were very good and
averaged 92+ 8 and 95 + 6t respectively. The spiking methods used (A and B)
were found to be essentially equivalent with regards to recovery efficiencies.
The average percent recovery from XAD-2 resin was 94+6 when Method A was
used and 91 + 10 when Method B was used. Likewise, the average percent
recovery from Florisil was 102 + 6 when Method A was used and 89+6 when
Method B was used. The data obtained in Task 131 Contract Number~~68-02-2686
gave comparable results or an overall system recovery of 94 percent.
In general, the data indicate that either Florisil or XAD-2 can be used
effectively for sampling, 2,3,7,8-TCDD. However, the recovery results appear
to be more consistent when XAD-2 resin was used as compared to Florisil. In
addition, XAD-2 was shown on many occasions to be a universal adsorber for
organics in general(l»2,3) and would therefore be more useful than Florisil
if several compounds need to be determined including dioxins.
The reproducibillty of the determination as measured by the RSDs_(l-12
percent) as well as the recoveries (89-102 percent) of the spiked 2,3,7,8-
TCDD indicate that the cleanup and detection procedures described earlier are
effective and could be used in sampling and analysis of dioxins.
Methods A and B appear to be equivalent in spiking the dioxin onto,the
resin with a measurable tendency for lower recoveries when Method B was used.
The need for evaporating a larger solvent volume with Method B might ex-
plain the possible loss of a very small amount of the dioxin.
13
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TABLE 2. RECOVERY DATA FOR SPIKED NATIVE 2,3,7,8-TCDD ON XAD-2 RESIN
Native
Spike Level
(ng)
0
2.1
16.5
0
2.1
16.5
Native
Rep. 1
0.08
2.0
17.4
0.010
•
•
1.8
14.2
Determined
(ng)
Rep. 2
ND
1.8
16.3
ND
1.8
14.3
Level
Rep. 3
ND
1.7
15.6
ND
2.2
16.0
Recovery Percent
Rep. 1
ND
95
105
ND
86
86
Rep. 2
ND
86
99
ND
86
87
Rep. 3
ND
81
95
ND
105
97
Avg.
ND
87
100
ND
92
90
92*
RSD
ND
8
5
ND
12
7
8*
'Spiking
Method
A
A
A
B
B
B
RSD = Relative standard deviation (percent)
ND = Not determined
* = Overall recovery
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TABLE 3. RECOVERY DATA FOR SPIKED NATIVE 2,3,7,8-TCDD ON FLORISIL
Native
Spike Level
(ng)
0
2.1
16.5
0
2.1
16.5
Native
Rep. 1
0.017
2.2
17.9
0.034
1.7
16.8
Determined Level
(ng)
Rep. 2
ND
2.0
17.8
ND
1.7
14.9
Rep. 3
ND
1.8
18.0
ND
1.9
15.0
Rep. 1
ND
105
108
ND
81
102
Recovery Percent
Rep. 2
ND
95
108
ND
81
90
Rep. 3
ND
86
109
ND
90
91
Avg.
ND
95
108
ND
84
94
95*
RSD
ND
11
1
ND
6
7
6*
Spiking
Method
A
A
A
B
B
B
RSD = Relative standard deviation (percent)
ND = Not determined
* = Overall recovery
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REFERENCES
1. Selection and Evaluation of Sorbent Resins for Collections of Organic
Compounds, EPA-600/7-77-044 (April 1977).
2. Characterization of Sorbent Resins for Use in Environmental Sampling,
EPA-600/7-78-054 (March 1978).
3. Further Characterization of Sorbents for Environmental Sampling,
EPA-600/7-79-216 (September 1979).
16
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APPENDIX A
TASK QUALITY ASSSURANCE (QA) AUDIT
A-l
-------
TASK QUALITY ASSURANCE (QA) AUDIT
Date Of Audit October 12. 1983
Task No. 008 Contract No. 68-02-3628
Task Title Feasibility of Using Solid Adsorbents for Dioxin Sampling
Task Manager F. L. DeRoos Task Officer M. D. Jackson
Consents:
Applicable Documents: WnrV PI a™ f. QA Plan nat-a,j F,kr.. ,~.
•^•^•^^M^^H^BWM^^«*^^«B«M^«^BWMM^W^BM*^*a^Wn^«^»^W^P*
Laboratory Recor Books 37945 &
Sampling and Sample Tracking: Clearly described - forward tracking excellent.
Analyses—Laboratory Activities: Adequate rgeord of laboracorv activities
Results: prngraTn QA nlang v«>r<» adhgrgd to and oh •igefivps achieved.
Approved by QA Officer:
R. E. Heffelfinger
A-2
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TECHNICAL REPORT DATA
fPlease reed Inunctions on the reverse before completing
5rp.ePORT NO.
A-600/7-84-060
3.
riTUfi AND SU8TITC8
easibility of using Solid Adsorbents for Dioxin
Sampling
3. RECIPIENT'S ACCESSION NO.
5. REPORT OAT8
May 1984
. L. DeRoos and A. K. Wensky
7SRPORMING ORGANIZATION NAM8 AND ADDRESS
attelle- Columbus Laboratories
J505 King Avenue
Columbus. Ohio 43201
J^ m MM ^ MMB^MV • BIMMBMMM ^ • m. _ „ , _ _ _ _ __
jit SPONSORING AGENCY NAME AND ADDRESS
I EPA, Office of Research and Development
jlhdustrial Environmental Research Laboratory
[Research Triangle Park, NC 27711
8. PERFORMING ORGANIZATION CODE
8. PERFORMING ORGANIZATION REPORT NO.
10. PROGRAM SL8MSNT NO.
NO.
68-02-3628. Task 8
13. TYPE OP REPORT AND PERIOD COVERED
Task Final; 4- 12/82 _
14. SPONSORING AGSNCV COO8
EPA/600/13
ITSUPPUSMENTARY NOTES IERL-RTP project officer is "Merrill D. Jackson, Mail Drop 62,
R919/541-2559.
The report gives results of a determination of the recovery efficiencies
Ifrom XAD-2 resin (Amb'erlite) and Florisil of spiked 2, 3,7, 8-tetrachlorodibenzo-p-
Idioxin (2, 3. 7,8-TCDD), in order to assess the suitability of these adsorbents for
Isampling. Two spiking methods were used: Method A consisted of uniformly deposit-
ling 1 mL of the spiking solution onto the adsorbent, and Method B consisted of cover-
ling the whole adsorbent sample with the spiking solution. There was no significant
[difference in recovery efficiencies between the two methods or between the two ad-
Jsorbents. Overall recovery from XAD-2 resin was 92 +/- 8%, and 95 +/- 6% from
inorisil. !
DESCRIPTORS
pollution Analyzing
Jeterocyclic Compounds
Hydrocarbons
Adsorbents — •
Combustion
Sampling
KEY WORDS AND DOCUMENT ANALYSIS
b.ioBNTiPIERS/OPEN ENDED TERMS
Pollution Control
Stationary Sources
Dioxins
T etr achlorodibenzo- p-
dioxin (TCDD)
STATEMENT
'Release to Public
19. SECURITY CLASS (Tim Report)
Unclassified
20. SECURITY CLASS (This paffe>
Unclassified
c. COSATi Meld/Group
T3B"
07 C
11G
21B
14B
21. NO. OF PAGES
23
22. PRICE
, form 2220-1 (*»73)
A-3
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