United States
Environmental Protection
Agency
Environmental Monitoring
Systems Laboratory
Las Vegas NV 89114
Research and Development
EPA/600/S4-86/021 July 1986
Project Summary
Performance of RCRA
Method 8280 for the Analysis
of Dibenzo-p-Dioxins and
Dibenzofurans in Hazardous
Waste Samples
J. M. Ballard, T. L. Vonnahme, N. J. Nunn,
D. R. Youngman, and Stephen Billets
Further evaluation of RCRA Method
8280 for the analysis of chlorinated
dibenzo-p-dioxins and dibenzof urans, has
been performed. The Method has been
modified to enable the quantitation of total
tetra- through octa-chlorinated dibenzo-p-
dioxins and dibenzofurans, and has been
applied to six different sample matrices
derived from industrial polychlorophenol
sources and also from fly-ash, still-bottom,
and Missouri soil samples. An interlabora-
tory validation of the Method has been
conducted in two phases: Phase I required
the analysis of spiked and unspiked clay
and sludge samples for certain specified
analytes, and Phase II required the analysis
of 10 samples of soil, sludge, fly-ash and
still-bottom for total tetra- through octa-
chlorinated dioxins and dibenzofurans.
Method detection limits of 13 C12-labeled
polychlorinated dioxins and dibenzofurans
in seven matrices have been determined.
In addition, a comparison was made of the
Contract Laboratory Program carbon col-
umn cleanup (without backflush) with the
corresponding backflush procedure used
in the proposed RCRA Method.
This Project Summary was developed
by EPA's Environmental Monitoring Sys-
tems Laboratory, Las Vegas, NV, to an-
nounce key findings of the research pro-
ject that is fully documented in a separate
report of the same title (see Project Report
ordering information at back).
Introduction
On a molecular basis, 2,3,7,8-tetrachlor-
odibenzo-p-dioxin (2,3,7,8-TCDD) is one of
the most poisonous synthetic chemicals
known. The compound has been shown
in animals to possess teratogenic, embryo-
toxic, carcinogenic, and co-carcinogenic
properties in addition to acute toxicity.
Because of its chemical stability, lipophilic
character, and extreme toxicity, it presents
potentially severe health hazards to the
human population. Although 2,3,7,8-TCDD
is the most toxic of the 75 chlorinated
dibenzo-p-dioxins (PCDD's), many of the
others (and also of the 135 chlorinated
dibenzofurans [PCDF's] which have similar
genesis, structures, and properties) are
known to possess relatively high toxicity
to humans and animals. For this reason,
the entire class of PCDD's and PCDF's is
of environmental concern.
The first synthesis of 2,3,7,8-TCDD was
reported in 1872, and only sporadic re-
ports of the preparation of PCDD's, con-
taining two, four, or eight chlorine atoms,
appeared in the literature during the years
1941-1965. Particular interest in 2,3,7,8-
TCDD, and in the PCDD's and PCDF's in
general, increased markedly with the dis-
covery in the early 1970's of the same ter-
atogenic and toxic effects with certain
commonly used herbicides, e.g., 2,4,5-tri-
chlorophenoxyacetic acid (2,4,5-T), as
were observed with 2,3,7,8-TCDD. Analysis
of 116 samples of 11 different pesticides
-------
produced during the period 1950-1970 re-
vealed the presence of PCDD contamina-
tion (tetra- through octa-chlorinated) in 42
percent of the samples. Consideration of
the chemistry of pesticide manufacture in-
dicated that PCDD's could be formed in
competing side-reactions of the polychlor-
ophenol precursors. The domestic use of
2,4,5-T was subsequently banned, and the
military use of Agent Orange (1:1 mixture
of 2,4,5-T and 2,4-dichlorophenoxyacetic
acid) as a defoliant in Vietnam was discon-
tinued, both in the early 1970's. Because
of the widespread usage of pesticides
potentially contaminated with PCDD's, a
Dioxin Monitoring Program was set up by
the EPA in 1973 to develop an analytical
method capable of detecting 2,3,7,8-TCDD
in environmental samples at the part per
trillion (ppt) level. This effort formed the
basis of the National Dioxin Strategy of
the Agency.
Although the most ubiquitous routes of
non-occupational exposure of the general
population to dioxins have probably been
via the use of contaminated pesticides and
from the emissions of municipal waste in-
cinerators, the most concentrated waste
sources of 2,3,7,8-TCDD are the tars and
sludges resulting from the commercial pre-
paration of 2,4,5-trichlorophenol (2,4,5-
TCP). This latter fact was highlighted dur-
ing an investigation in 1975-1977 of unex-
plained animal deaths at various horse
arenas in Missouri. It was discovered that
the sites had been sprayed with a mixture
of waste oil and distillation residues from
the manufacture of 2,4,5-TCP which were
contaminated with 2,3,7,8-TCDD. Subse-
quent investigation of chemical waste
dump-sites in New York State (Hyde Park;
love Canal), where wastes from the man-
ufacture of 2,4,5-TCP had been buried,
also revealed the presence of substantial
amounts of 2,3,7,8-TCDD.
As a result of this experience, it was
concluded by the EPA that samples con-
taining tetra-, penta-, and hexa-CDD's and
CDF's are likely to exhibit increased toxi-
city (40 CFR 261:1978, January 14, 1985),
and a method to analyze hazardous wastes
for the relevant PCDD's and PCDF's was
included in the Resource Conservation and
Recovery Act (RCRA) requirements for
hazardous waste monitoring as published
in the Federal Register (40 CFR 65:14514,
April 4, 1983). A single-laboratory evalua-
tion of the RCRA Method 8280 for the
analysis of PCDD's and PCDF's in hazar-
dous waste has been the subject of a pre-
vious report prepared for the Office of
Solid Waste (EPA-600/4-85/082). That
report presented results obtained with
sample matrices including pottery clay, a
Missouri soil, a fly-ash, a still-bottom from
a chlorophenol-based herbicide production
process, and an industrial process sludge.
Major revisions to the Method as first
published in 1983 were necessary to ac-
commodate the analysis of complex sam-
ples such as sludge and still-bottom.
The revised Method 8280 has subse-
quently undergone a period of continual
development, and this summary presents
results obtained during the further evolu-
tion of the Method.
Study Design
Changes made to the proposed Method
since publication of the previous report are
summarized as follows: in order to improve
the accuracy of quantitation of the hepta-
and octa-CDD's and CDF's, a second in-
ternal standard (13C12-OCDD) is added to-
gether with 13Cl2-2,3,7,8-TCDD prior to
sample workup. Some of the ions specified
in the multiple ion detection (MID) descrip-
tors have been changed so as to increase
sensitivity by monitoring the most intense
ion in the isotopic cluster. To ensure that
co-eluting polychlorinated diphenyl ethers
(PCDE's) are not contributing to the signal
response due to PCDF's, the molecular ion
of the appropriate PCDE was included in
each MID descriptor. In addition, the cri-
teria for the positive identification of PCDD
and PCDF isomers were made more ex-
plicit. Instrument tune criteria employing
perfluorotri-/7-butylamine (FC-43) were
substituted for those based on the use of
decafluorotriphenylphosphine (DFTPP).
The section on the calculation of concen-
trations of analytes was expanded to in-
clude a procedure for measuring unknown
PCDD and PCDF isomers.
The performance of the Method was in-
itially examined by its application to the
analysis of a variety of wastes derived
from the use of polychlorophenols in the
wood-preserving industry. As an additional
test of Method performance, an interlab-
oratory validation study was conducted in
two parts. A two-part study was used be-
cause the Method had been extensively
improved since its publication in the
Federal Register, and it was felt that par-
ticipating laboratories would be unfamiliar
with some of the revised procedures. The
first phase was intended to allow the par-
ticipants to acquire familiarization with the
Method by analyzing relatively simple mat-
rices for a few specified analytes which
had been spiked into the samples. The se-
cond phase required the total quantitation
of tetra- through octa-CDD's and CDF's in
complex samples containing the analytes
at both low and extremely high levels; no
spiking was used for these samples. A
method detection limit study using a
available 13C12-labeled PCDD and PCD
isomers spiked into seven different sarr
pie matrices was also performed. A corr
parison of the EPA Contract Laborator
Program (CLP) carbon column cleanu]
without and with a backflush elution pro
cedure was conducted to test the ade
quacy of the CLP method for the deter
mination of total PCDD's and PCDF's.
Results
The single-laboratory application of thi
Method to the determination of PCDD':
and PCDF's in complex environmenta
samples (e.g., fly-ash, still-bottom, am
wastes from the industrial use of penta
and tri-chlorophenol) has routinely yield
ed excellent recoveries (60 to 85 percent
of the spiked internal standard 13Cl2-2,3
7,8-TCDD (see Tables 1 and 2). This indi
cates that the extraction and cleanup pro
cedures are able to accommodate sample!
ranging from those with a high aqueous
content to viscous oils and chemical slud
ges. It can be assumed that endogenous
PCDD's and PCDF's are extracted witr
equal success if matrix effects are not ir
effect.
In the absence of a full range of stan
dard reference materials, the accuracy o
the Method is rather difficult to assess
However, data obtained from Phase I o
the interlaboratory study indicate that the
Method is biased high and that the bia:
appears to decrease as the concentrations
of the analytes increase (see Table 3). Date
from the method detection limit (MDL
study can be used as an indicator of intra
laboratory precision. For seven replicate
determinations of a TCDF and a PeCDD ir
fly-ash, with each at a measured concen
tration of 2.6 times their final calculatec
MDL's, the relative standard deviations
(RSD's) were 12.3 percent and 12.2 per-
cent, respectively. Similar determinations
for a PeCDF and a TCDD which were mea-
sured at a level 6.0 and 4.4 times their
MDL's gave RSD's of 5.2 percent and 7.2
percent, respectively.
Encouraging results were obtained from
Phase I of the interlaboratory study in
which specific analytes spiked into clay
and sludge samples were quantitated.
The mean value for 114 determinations
of 11 analytes spiked into clay at the 5 ppb
level was 6.02 ± 2.78 ppb.
The mean value for 16 determinations
of two analytes spiked into clay at the 2.5
ppb level was 3.56 ± 2.35 ppb.
The mean value for 57 determinations
of six analytes spiked into sludge at the
125 ppb level was 126.4 ± 57.9 ppb.
The good overall recovery (greater than
-------
Table 1. Analysis3 of POP Process Samples Using Method 8280
PCCD/
PCDF
TCDD
PeCDD
HxCDD
HpCDD
OCDD
TCDF
PeCDF
HxCDF
HpCDF
OCDF
13r
°72"
2,3,7,8-
TCDD per-
cent recovery
Sludge
B-6d
(ppb)
/VDb
ND
2150
51520°
72300°
ND
ND
68
343
4100°
66.8
Fuel
oil
B-7b
(ppb)
ND
ND
2186
67176°
154000°
ND
154
2933
1342
7500°
69.0
Sludge
B-8b
(ppb)
ND
ND
ND
2166°
2670°
ND
ND
ND
ND
ND
64.3
Sludge
B-12h
(ppb)
ND
ND
ND
978°
2550°
ND
ND
ND
ND
76
67.8
Fuel oil
A-2g
(ppb)
ND
ND
2079
38195°
59100°
ND
246
2852
1913
447
69.2
Alcohol
fuel oil
A-3g
(ppb)
ND
ND
762
17956°
24500°
ND
ND
76
1118
741
60.0
Sludge
A-4g
(ppb)
ND
ND
726
59600°
106000°
ND
ND
1568
1948
3200°
62.9
Soil
A-5g
(ppb)
ND
ND
283
12945°
16500°
ND
ND
65
533
900°
77.0
Soil
A-6.1g
(ppb)
ND
27
730
24700°
26300°
ND
61
252
1695
3080°
75.4
Soil
A-6.2g
(ppb)
ND
ND
396
12300°
15000°
ND
ND
56
434
1690°
74.8
aMean of duplicates; concentrations shown are for the total of all isomers within a given homologous series.
bND is below detection limit for the sample matrix. Detection limits are estimated as 5 ppb for the tetra- through hexa-isomers and as 10 ppb
for the hepta- and octa-isomers.
0 Due to the extremely high levels of HpCDD, OCDD, and OCDF detected in the GC/MS analysis, the extracts were diluted after normal quan-
t/tat/on of the tetra-, penta-, hexa-CDD/CDF and hepta-CDF. HpCDD, OCDD, and OCDF were then quantitated versus 13C12-1,2,3,4-TCDD
which was added after dilution; the values are corrected for 13C12-2>3,7,8-TCDD recovery.
Table 2.
PCCD/
PCDF
TCDD
PeCDD
HxCDD
HpCDD
OCDD
TCDF
PeCDF
HxCDF
HpCDF
OCDF
13r
°/2~
2,3,7,8-
TCDD
percent
recovery
Analysis3 of PCP Process Sample (B-5) and 10 TCP Process Samples Using Method
Water
B-5
(ppb)
/VD6
ND
0.072
2.5C
1.25°
0.024
ND
0.017
0.136
0.029
67.3
Sawdust
H-3
(ppb)
ND
385
268C?
2314°
1250°
3593d
1903d
11903d
1374d
94°
95.2s
Soil
H-7a
(ppb)
ND
ND
ND
ND
5.5
ND
ND
ND
ND
ND
71.2
Soil
H-7b
(ppb)
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
76.4
Soil
H-7c
(ppb)
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
72.3
Water
1-1
(ppb)
ND
ND
11Cf
1677°
345°
3.9*
ND
233d
108°
16°
__f
Sludge
1-2
(ppbl
ND
30
241 O*
42134°
14658°
207
429
5496d
2768°
239°
77.1
8280
Sludge
1-11
(ppb)
ND
ND
399
4404°
4080°
68
23
626
622°
151°
75.6
Soil
1-1 2c
(ppbl
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
84.9
Soil
l-14a
(ppb)
ND
ND
ND
37
20
ND
ND
ND
ND
ND
78.7
So/7
l-14b
(ppb)
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
84.1
aMean of duplicates except for samples B-5 and 1-1 which are the result of single determinations. Concentrations shown are for the total of all
isomers within a given homologous series.
bND is below detection limit for the sample matrix. Detection limits are 5 ppb for soil, sawdust, sludge, and are 0.01 ppb for water.
°'dDue to the very high levels of some hexa-, hepta-, or octa-CDD/CDF isomers, some samples were diluted, and the PCDD's and PCDF's noted
were quantified versus '3C12-OCDD° or '3C12-1,2,3,4-TCDDd; the values are corrected for 13C12-2,3,7,8-TCDD recovery.
eSome interference at the quantitation ion was noted.
Gross interference at the quantitation ion was noted.
-------
Table 3. Interlaboratory Test of Method 8280, Phase I:
Accuracy and Bias of Results
Sample Spike Level Number of Accuracy
Type (ppb) Determinations (Percent)
Bias
(Percent)
± SO of
Bias Estimate
Clay
Clay
Sludge
2.5
5.0
J25
16
114
57
142.4
120.4
101.1
+ 42.4
+ 20.4
+ 1.12
± 11.8
± 5.27
± 6.14
50 percent) of the internal standard and
the small differences between the spiked
concentrations and the mean measured
values both indicate that the Method can
provide acceptable data in a multilabora-
tory program. Phase II of the interlabora-
tory study which required the quantitation
of total tetra- through octa-CDD's and
CDF's in 10 aliquots of 4 sample types,
also provided satisfactory results. The in-
ternal standards (13Cl2-2,3,7,8-TCDD and
13C12-OCDD) were recovered in overall ac-
ceptable yields ranging from 51 to 82 per-
cent. However, quantitation of the analy-
tes was less precise than in Phase I. Two
major, probable reasons for this are as
follows:
1. The complex samples themselves
which sometimes contained endog-
enous amounts of the target analytes
at low and at extremely high levels;
this led to a large dilution requirement
which eliminated the value of the iso-
topic dilution method of quantitation.
2. The need for an analysis which re-
quired the identification, confirma-
tion, and quantitation of an unknown
number of peaks for each congener
often without an authentic reference
standard which could be used to
confirm the identification of each
congener.
In general, the Method performed well
when the laboratories followed the pro-
tocol. A visual examination of the data
showed that approximately 85 percent of
the values reported by the 5 laboratories
and used in the statistical analysis were
consistent among the laboratories.
Statistical analysis of the Phase II data
revealed that:
• Recovery of 13Cl2-2,3,7,8-TCDD in-
ternal standard was a function of
sample type, whereas that of 13C12
-OCDD internal standard was not.
• The laboratories were equivalent in
accuracy for all analytes except
OCDD.
• The laboratories were equivalent in
precision for 31 of the 40 possible
matrix/analyte combinations.
Method detection limits of eight 13C12
-labeled PCDD's and PCDF's spiked into
reagent water were found to be in the low
ppt range (less than 10 ppt); 42 of 48 val-
ues determined for 6 environmental sam-
ples were less than 5 ppb (see Table 4).
Several characteristics and trends are
apparent in the data: 13C12-2,3,7,8-TCDD/
TCDF usually had the lowest MDL values
for each sample type, while 13Cl2-HpCDD/
OCDD usually had the highest; as might
be expected, the MDL values for all
analytes generally increased in passing
from the "clean" sample types (reagent
water, fly-ash) to the more complex,
organics-containing matrices (still-bottom,
industrial sludge). The MDL for 13C12-
2,3,7,8-TCDD in reagent water (0.44 ppt)
determined in this study using Method
8280 compares well with the value re-
ported for 2,3,7,8-TCDD in reagent water
Table 4. Method Detection Limits of '3C,2-Labeled PCDD's and PCDF's in Reagent
Water (PPT) and Environmental Samples (PPB)
(2 ppt) and determined using Method 61
(capillary column GC/MS with selected io
monitoring).
An experimental comparison of th
Contract Laboratory Program (CLP) carbo
column cleanup (the backflush procedur
is not used) with the backflush procedur
used in Method 8280 was undertaken be
cause the CLP method should be faste
and should consume much less solven
while it does not require HPLC equipment
Twin open carbon columns were spikei
with a standard solution containing a mix
ture of 11 PCDD's and PCDF's. The firs
column was eluted with a 2-mL and <
5-mL aliquot of toluene; the second co
lumn was eluted similarly in the reverse
flow direction. The four fractions wer<
analyzed separately, and the recoveries
(see Table 5) indicated that although the
CLP cleanup as written is very satisfactory
for the determination of 2,3,7,8-TCDC
(and possibly other tetra- and penta-CDD's
and CDF's) it is not adequate for the deter
mination of hexa-, hepta-, and octa-CDD's
and CDF's. However, the combination o1
an open carbon column with a backflusr
procedure gave an acceptable perform
ance for the tetra- through octa-substi
tuted congeners.
Recommendations
As a result of the experience gained dur-
ing the single- and multi-laboratory testing
of the Method with a variety of environ-
mental samples, several modifications to
the Method and areas of further study are
recommended:
1. The Method should allow for the
use of disposable, open carbon col-
umns as an option to the currently
specified HPLC carbon column
cleanup. This would allow for an in-
crease in the rate of sample through
put and would also reduce solvent
consumption.
13C12-Labeled
Analyte
2,3,7,8-TCDD
1,2,3,7,8-PeCDD
1, 2,3,6,7, 8-HxCDD
1,2,3,4,6, 7,8-HpCDD
OCDD
2,3,7,8-TCDF
1,2,3,7,8-PeCDF
1,2,3,4,7,8-HxCDF
Reagent
Water3
0.44
2.35
6.63
5.45
7.37
0.58
1.50
2.53
Missouri
So//6
0. 13
0.70
1.24
1.60
1.35
0.11
0.33
0.83
Fly-
Ash"
0.07
0.25
0.55
1.41
2.27
0.06
0.06
0.30
Industrial
Sludge0
0.40
1.47
2.26
3.39
7.68
0.36
0.58
1. 15
Still-
Bottomd
1.81
2.46
16.2
4.59
10.1
2.26
1.61
2.27
Fuel
Oif
0.75
2.09
5.02
8.14
23.2
0.48
0.80
2.09
Fuel Oil/
Sawdust*
0.13
0.18
0.25
0.49
1.34
0.04
0.09
0. 17
a Sample size 1,000 mL
b Sample size 10 g.
c Sample size 2 g.
° 'Sample size 1 g.
Note: The final sample-extract volume was 100
for all samples.
-------
Table 5. Percent Recovery3 of PCDD's and PCDF's from CLP Carbon Column
Method as Written (without Backflush)
Analyte
2,3,7,8-TCDF
1,2,3,4-TCDD
2,3,7,8-rCDD
1,2,3,7,8-PeCDF
1,2,3,4,7-PeCDD
1, 2,3,4,7, 8-HxCDF
1, 2,3,4,7, 8-HxCDD
1,2,3,4,6,7,8-HpCDF
1,2, 3,4,6,7, 8-HpCDD
1, 2,3,4,6,7, 8,9-OCDD
1, 2,3,4,6,7,8, 9-OCDF
2 mL
Toluene
Fraction
81.5
80.0
87.6
71.0
80.9
35.9
39.6
7.8
13.4
ND
ND
Additional
5 mL
Toluene
Fraction
ND
ND
ND
14.0
ND
43.0
46.0
52.6
62.0
50.8
36.0
Total
81.5
80.0
87.6
85.0
80.9
78.9
85.6
60.4
75.4
50.8
36.0
Method Modified (with Backflush)
2 mL
Toluene
Fraction
83.0
80.3
87.6
85.4
87.5
74.5
80.3
54.4
57.8
48.2
45.7
Additional
5 mL
Toluene
Fraction
ND
ND
ND
ND
ND
9.8
9.8
25.5
22.6
25.8
26.9
Total
83.0
80.3
87.6
85.4
87.5
84.3
90.1
79.9
80.4
74.0
72.6
aResults of a single determination.
ND = Not detected.
2. The use of stacked acidic/basic
silica gel columns instead of multi-
ple liquid-liquid partitioning in the
extraction/cleanup procedures
should be investigated. This would
eliminate the problems of emulsion
formation currently encountered
and would also greatly reduce the
quantities of corrosive wastes
generated.
3. Gas chromatography (GC) condi-
tions should be modified to improve
the resolution between the internal
standard (13C12-2,3,7,8-TCDD) and
the recovery standard 13C12-1,2,3,4-
TCDD). If this cannot be readily
achieved, then use of an alternative
recovery standard should be
considered.
4. The elution windows (defined by
first and last eluting isomers) of the
tetra- through octa-CDD and CDF
congeners should be established for
the GC conditions used in the
Method.
5. Because of the known elution over-
lap of some tetra-substituted iso-
mers with penta-substituted iso-
mers (and other potential overlaps
between homologous groups), the
multiple ion detection (MID) de-
scriptors should be modified to in-
clude at least one ion for each
overlapping homologue.
6. Method 8280 should be written to
require as many GC/MS analyses as
necessary by using the appropriate
MID descriptors whenever an elu-
tion overlap is noted in a sample.
7. Kovats Indices should be deter-
mined for available PCDD's and
PCDF's. This would aid laboratories
10.
in the identification of isomers not
known or available to them and
would be useful in a GC screening
program.
The need to monitor for polychlorin-
ated diphenyl ethers (PCDE's) in the
final sample extract should be
investigated.
A source of a well-defined GC per-
formance standard should be iden-
tified. Column performance guide-
lines should be established for a
variety of columns.
Sample reanalysis requirements giv-
en the presence of low and of very
high levels of target analytes should
be defined.
ftU.S.Government Printing Office: 1986 — 646-116/40618
5
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J. M. Ballard, T. L. Vonnahme, N. J. Nunn, andD. R. Youngmanare with Lockheed
Engineering and Management Services Company. Inc.. Las Vegas, NV 89114.
Stephen Billets is the EPA Protect Officer (see below).
The complete report, entitled "Performance of RCRA Method 8280 for the
Analysis of Dibenzo-p-Dioxins and Dibenzofurans in Hazardous Waste
Samples, "(Order No. PB 86-193 679/AS; Cost: $11.95, subject to change) will
be available only from:
National Technical Information Service
5285 Port Royal Road
Springfield, VA2216J
Telephone: 703-487-4650
The EPA Project Officer can be contacted at:
Environmental Monitoring Systems Laboratory
U.S. Environmental Protection Agency
P.O. Box 15027
Las Vegas. NV 89114
United States
Environmental Protection
Agency
Center for Environmental Research
Information
Cincinnati OH 45268
^F7>, US.OFFiC!A..i •••"..
" ----" --
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Official Business
Penalty for Private Use $300
EPA/600/S4-86/021
0000329 PS
U S ENVIR PROTECTION AGENCY
REGION 5 LIBRARY
230 S DEARBORN STREET
CHICAGO IL 60604
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