United States
Environmental Protection
Agency
Office of Solid Waste and
Emergency Response
Washington, DC 20460
Center for Environmental
Research Information
Cincinnati, OH 45268
Technology Transfer
June 1989
EPA/625/6-89/021
EPA Handbook
Hazardous Waste
Incineration
Measurement Guidance
Manual
Volume III of the
Hazardous Waste
Incineration Guidance
Series
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ERA/625/6-89/021
June 1989
Handbook
Hazardous Waste
Incineration Measurement
Guidance Manual
Volume 111 of the Hazardous Waste
Incineration Guidance Series
Office of Solid Waste and Emergency Response
US. Environmental Protection Agency
Washington, DC 20460
Air and Energy Engineering Research Laboratory
Research Triangle Park, NC 27711
and
Center for Environmental Research Information
Office of Research and Development
US. Environmental Protection Agency
Cincinnati, OH 45268
Printed on Recycled Paper
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Notice
This document has been reviewed in accordance with the U.S. Environmental Protection Agency's peer and administra-
tive review policies and approved for publication. Mention of trade names or commercial products does not constitute
endorsement or recommendation for use.
The guidance document is intended to provide information on how regulatory requirements in 40 CFR Subpart O may
be satisfied in a wide variety of situations. This guidance document is not, in and of itself, a regulatory requirement and
should not be regarded as such. Therefore, although compliance with regulatory requirements is mandatory, compli-
ance with this guidance manual (although useful as a means of satisfying regulatory obligations) is not.
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Abstract
This document provides general guidance to permit writers in reviewing the measurement aspects of incineration
permit applications and trial burn plans. It is oriented to how measurements are made, not what measurements to make.
The guidance deals specifically with commonly required measurement parameters and measurement methods for
process monitoring, sampling and analysis aspects of trial burns and subsequent operation of the incinerator, and
quality assurance/quality control (QA/QC) associated with these activities. As a guidance tool, this document intro-
duces the major elements of incineration measurements via sample checklists, general discussion, and technical
references. -
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Acknowledgements
This guidance document was prepared for the U.S. Environmental Protection Agency's Office of Solid Waste (OSW) and
the Office of Research and Development (ORD) under the direction of Sonya M. Stelmack and Robin M. Anderson of
OSWfe Permits and State Programs Division and Larry D. Johnson of ORD's Air and Energy Engineering Research
Laboratory (now with Atmospheric Research and Exposure Assessment Laboratory). The document was prepared by
Midwest Research Institute (MRI) under subcontract to AT. Kearny, Inc. The principal investigator was Andrew
Trenholm. Major MRI contributors included Gary Kelso, Mitchell Erickson, Scott Klamm, and Dennis Hooten. Additional
contributions and technical review were provided by Clarence Haile, John Coates, Roy Neulicht, Gary Hinshaw, Paul
Gorman, and Bruce Boomer. Drafts of the document were reviewed by the U.S. EPA Incinerator Permit Writers Work
Group.
iv
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Contents
Page
Abstract Hi
Acknowledgements :........ . . . . iv
Contents v
Tables vi
Figures vii
1. Introduction ..... 1
2. Specific Recommendations for Permit Reviewers 3
2.1 Trial burn runs 3
2.2 Trial burn schedule 3
2.3 Monitoring , 3
2.4 Sampling and analysis 3
2.5 Reporting of results . 6
2.6 Continuing analysis and monitoring 8
3. Measurement Methods , ..9
3.1 Specification of method options .9
3.2 Process monitoring 9
3.3 Sample collection 11
3.4 Chemical analysis 15
4. Quality Assurance/Quality Control 25
4.1 Data quality objectives .-.. 25
4.2 General discussion of QA project plan 25
4.3 Guidance for precision and accuracy objectives ...>... 29
5. References 31
Appendices
A. Analysis methods for Appendix VIII hazardous constituents given in EPA-600/8-84-002 and SW-846 33
B. Measurement checklists 41
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Tables
Number Page
1 Example of a trial burn schedule 3
2 Example calculation to determine whether VOST sample size is sufficient to measure 99.99% ORE for
carbon tetrachloride 6
3 Example reporting of volatile POHC emissions 7
4 Sampling methods for stack gases in RCRA trial burns 13
5 EPA reference methods used to test RCRA hazardous waste incinerators 13
6 VOST audit compounds 14
7 Selected problem POHCs 17
8 Sample preparation methods given in EPA-600/8-84-002 18
9 Sample preparation and introduction techniques given in SW-846 18
10 Analytical methods for characteristics of RCRA hazardous waste feed samples 19
11 Analytical methods for principal organic hazardous constituents (POHCs) given in EPA-600/8-84-002 19
12 Analytical methods for principal organic hazardous constituents (POHCs) given in SW-846 .*. 20
13 Analytical methods for inorganics 21
14 Analytical methods for stack gas samples 22
15 Essential elements of a QA project plan 25
16 Summary of precision and accuracy objectives '' -29
VI
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Figures
Number
1 Example daily schedule.
Page
4
VII
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Section 1
Introduction
Subtitle C of the Resource Conservation and Recovery
Act (RCRA) requires the US. Environmental Protection
Agency (EPA) to develop, promulgate, and implement
regulations which control the generation, transportation,
treatment, storage, and disposal (TSD) of hazardous
wastes. An integral part of these activities is reviewing
and issuing permits to hazardous waste incineration
facilities.
Several documents have been or are being prepared as
a Hazardous Waste Incineration Guidance Series pre-
pared by EPA to assist both the applicant and the permit
writer in the RCRA Part B process leading to a final
operating permit for hazardous waste incinerators. This
document on measurement guidance is Volume III of this
series. Below is a list of additional guidance manuals in
the series:
Volume I Guidance Manual of Hazardous Waste Inciner-
ator Permits, Mitre Corporation, SW-966, NTIS
PB84-100577, July 1983 (document scheduled
for revision). This describes the overall
incinera tor permitting process, highlights the
specific guidance pro vided by other manuals,
and addresses permitting issues not covered
in the other manuals such as treatment of data
in lieu of a trial burn. Thus it can be viewed as
a road map and a good summary of all permit-
ting issues.
Volume II Guidance on Setting Permit Conditions and
Reporting Trial Burn Results, Acurex, EPA-625/
6-89-019, 1989. Includes guidance on select-
ing key operating parameters, translating trial
burn data into permit operating conditions,
and reporting trial burn results. Also discusses
planning a trial burn to achieve workable per-
mit limits.
Volume IV Guidance on Metals and Hydrogen Chloride for
Hazardous Waste Incinerators, Versar, 1989
(draft under EPA review). Specific guidance
on limiting metals emissions from incinerators
is provided. In particular, a risk assessment
approach to setting limits on metal compo-
nents in the waste is employed. Guidance
is also provided on doing risk-based checks
on HCI emissions. (Note: Earlier title was
Guidance for Permit Writers for Limiting Metal
and HCI Emissions from Hazardous Waste
Incinerators.)
Volume V Guidance on PIC Controls for Hazardous Waste
Incineration, Midwest Research Institute, 1989
(draft under EPA review). Details the specific
permit requirements for CO and total hydro-
carbon (THC) emissions from hazardous
waste incinerators in the RCRA system. Emis-
sion limits for CO and THC and the rationale
for their selection are discussed. (Note: Earlier
title was: Guidance on Carbon Monoxide Con-
trols for Hazardous Waste Incineration.)
Volume VI Proposed Methods for Measurement of CO, O2,
THC, HCI, and Metals at Hazardous Waste
Incinerators, 1989 (draft under EPA review).
Presents a draft mea surement method for the
above parameters including performance
specifications for continuous CO monitors.
In addition, a document has been prepared to assist
regulatory personnel in observing trial burns: Trial Bum
Observation Guide EPA-530/SW-89-027 March 1989,
Midwest Research Institute, September 1988. Includes
general guidance on preparation, on-site activities, and
reporting aspects of observing a trial burn test.
The Hazardous Waste Incineration Measurement Guid-
ance Manual provides general guidance to permit writers
in reviewing the measurement aspects of incineration
permit applications and trial burn plans. It is oriented to
how measurements are made, not what measurements
to make. The guidance deals specifically with commonly
required measurement parameters and measurement
methods for process monitoring, sampling and analysis
aspects of trial burns and subsequent operation of the
incinerator, and quality assurance/quality control (QA/
QC) associated with these activities.
As a guidance tool, this document introduces the major
elements of incineration measurements via general dis-
cussion and technical references. It is not intended to
specify a complete list of measurements that should be
required in every case, nor does it provide complete
descriptions of all pertinent methods. The references
cited provide additional descriptions of measurement
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methods, and at times, measurement experts may need
to be consulted for judgments in unusual situations. Test-
ing, operating, and permitting hazardous waste incinera-
tors typically involves best engineering and scientific
judgment on a case-by-case basis. No single publication
can answer all of the possible technical and regulatory
questions related to incineration measurements.
The following sections of the report cover recommenda-
tions to permit reviewers, methods, and QA/QC. Sec-
tion 2 provides some specific recommendations to permit
reviewers on various aspects of the trial burn plan and
permit application. Section 3 gives commonly used
methods for measuring the monitoring, sampling, and
analysis parameters. Section 4 discusses the QA/QC
procedures which should be addressed for the measure-
ment methods in the quality assurance plan. Section 5
gives the references used in the report. Appendix A
reproduces guidance for analyses methods given in EPA-
600/8-84-002 and in SW-846. Appendix B provides
checklists to be used by permit writers to help assess the
completeness of measurement information in trial burn
plans and incinerator permit applications. The checklists
include process monitoring parameters, sampling
parameters, analysis of samples, and QA/QC for the pro-
cess monitoring and sampling and analysis parameters.
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Section 2
Specific Recommendations for Permit Reviewers
Many aspects of RCRA incinerator trial burns are not
specifically addressed in the regulations (40 CFR Parts
264 and 270). This can result in different judgments or
decisions made by RCRA permit reviewers as they
review permit applications. Case-by-case judgments are
appropriate at times; however, a more uniform decision-
making process among reviewers is needed. This sec-
tion provides specific recommendations for some
aspects of the trial burn and the reporting of the results to
promote this uniformity.
2.1 Trial Burn Runs
Three replicate runs are recommended for each specific
set of incinerator operating conditions. Sufficient waste
feed must be stockpiled or readily available in order that
the same waste characteristics are used for replicate
runs. All three replicate runs should comply with the
RCRA requirements for destruction and removal effi-
ciency (ORE), particulate emissions, and hydrogen chlo-
ride (HCI) emissions. This provides added assurance
that the incinerator can repeatedly meet the standards. If
the incinerator fails only some of the standards (e.g., only
particulate), measurement of only those standards that
failed can be considered for a retest, provided that the
key operating conditions remain the same and that any
modification to the incinerator would not negatively affect
the unit's ability to comply with the other performance
standards.
2.2 Trial Burn Schedule
Generally, one run per day should be scheduled. This
can vary depending upon the complexity of the spe-
cific trial burn.
A trial burn schedule indicating the overall test sched-
ule and an anticipated daily schedule, similar to the
examples shown in Table 1 and Figure 1, should be
included in the trial burn plan. The daily schedule in
Figure 1 assumes 2 h of actual sample time for the
semivolatile organic sampling train (semi-VOST) and
three volatile organic sampling train (VOST) trap pairs
at a 40-min sampling time per pair, as an example.
2.3 Monitoring
The regulations call for continuous monitoring of com-
bustion temperature, waste feed rate, the indication of
combustion gas velocity, and CO in the stack gas [40
CFR 264-347(a)(1)]. Monitoring of key process param-
eters should be as continuous as feasible. A recom-
mended minimum requirement for selected key
parameters is reading a measurement value at least
every 15 s and recording a value at least every minute.
Strip charts and/or data loggers can be used to record
data. If these minimum requirements cannot be met,
then justification for why less frequent measurement/
recording times are acceptable should be provided by
the applicant. Continuous monitoring with alarms or
automatic shutdown at specified set points, without
permanent data recording, may be appropriate for
some parameters. Volume VI of the Guidance Series
(referenced in Section 1) contains draft performance
specifications for CO monitors.
Table 1. Example of a Trial Burn Schedule
Prior to Incinerator shakedown/site modifications
test "Miniburns"
Monitors) calibration/evaluation
Preparation of special wastes
Pretest meeting(s)
Day 1 Arrive on-site :
Set-up
Sample solid wastes .
Day 2 Complete set-up
Sample solid wastes
Preliminary measurements
Day 3 Run 1
Day 4 Run 2, audits
Day 5 Run 3
Day 6 Pack equipment/leave site
Day 4-8 Samples arrive at lab
Day 35-50 Sample analysis complete
Day 35-60 Preliminary results reported
Day 95 Test report submitted
2.4 Sampling and Analysis
Waste feed samples should be collected every 15 min
over the entire period of stack sampling and then be
composited into one sample per test run for each
waste feed. The applicant may justify less frequent
sampling if data are provided to show that the
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Figure 1. Example dally schedule.
Daily Schedule
Activity
Incinerator Operation
at Test Conditions
Daily Test Equipment
Preparations
Start Test
Method 5, Sample
Semi VOST Sample
Method 3 ORSAT Sample
VOST S/
Waste Feed Samples ^/
(Each Waste Stream)
Solid Waste Samples"/
Scrubber Water Samples
Ash Residue
Auxiliary Fuel
End Test
Lunch
Recover Samples/ORSAT Analysis
Traeeability/Sample Storage
Contingency
Time (hr)
I 2345678
{
a
a
a
J_ a
i
i
i
i
2
n
I
imm
>
3^
i
»!««
9
raw
10 11
^H
12
J2/Traverse 1 -£/Three Trap Pairs
jy Traverse 2 A/Grab Samples, Composite
and Individual VOA Vials (If necessary)
-S/May be necessary to Sample
Previous Day
homogeneity and composition of the waste feed do
not vary.
Each drum burned during the trial burn should be
sampled, unless the applicant can justify why this is
not necessary. Grab samples should be composited
for each waste type.
All other process samples (e.g., scrubber water, ash,
etc.) should be taken every 30 min over the entire
stack sampling period, and then be composited into
one of each sample type per test run. In some cases it
may not be feasible to comply with this recommenda-1
tion for ash sampling.
Sampling should not begin until the incinerator opera-1
tion has reached steady-state on waste feed. A mini-
mum of 30 min of operation feeding waste is
recommended, or for a rotary kiln, the greater of 301
min or the solids residence time.
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Sampling should continue through incinerator operat-
ing abnormalities unless the waste feed cutoff system
shuts the incinerator down. If sampling is stopped
during a trial burn, the test may be completed using
the same sampling trains if the burn is completed on
the same day it was started.
Minimum stack sampling time for each run (actual
sampling time not including time for port changes,
changing VOSTtrap pairs, etc.) should be 1 h for EPA
Method 5 (M5), semi-VOST, and VOST. Data from less
than 1 h of sample collection would be an invalid test
run. Two hours ,of stack sampling time is recom-
mended as optimal. In some cases more than 2 h of
sampling may be required, eg., to achieve required
detection limits. A minimum of three VOST trap pairs
per run is also recommended. A .fourth pair is often
taken in case one pair is broken or lost due to analysis
problems.
All sampling required for a test run in the trial burn
should, whenever possible, be conducted concur-
rently, with only the normal minor differences associ-
ated with different sampling methods (e.g., MM5 and
VOST schedules in Figure 1). However, differences in
sampling period start and finish due to sampling prob-
lems are allowable. Examples are a particulate train
that fails a leak check at port change and sampling
must be restarted with a new train, a VOST trap that
breaks at the end of the sampling period so that
another pair must be run, or sequential sampling
required due to limitations in available sampling ports.
However, all waste feed sampling must be continued
for the entire period, and possibly any water effluent or
ash sampling. Also, the incinerator must continue at
the same process operating conditions with collection
of the operating data for the entire period.
Separate semi-VOST (SW-846 Method 0010), com-
monly called Modified Method 5 (MM5), and Method 5
(M5) should be used for semivolatile and nonvolatile
POHCs and particulates, respectively. This is neces-
sary since drying the particulates collected and probe
rinse prior to weighing may result in loss of semivo-
latile POHCs.
Semi-VOST sampling trains with XAD resin traps
should not be used to collect samples for HCI analysis.
XAD resins may be contaminated with chlorides prior
to sampling or HCI may be retained in the XAD during
sampling.
Condensate collected in impingers after the XAD resin
module in a semi-VOST sampling train should always
be considered part of a semivolatile POHC sample.
The condensate should be extracted and the extract
combined with the extracts from other portions of the
sampling train.
The final leak check for VOST should be run at the
highest vacuum used during the sampling run but not
less than 1 in of mercury vacuum.
A sampling train which develops problems during a
trial burn may be validated on a case-by-case basis if it
can be shown that the results were not significantly
biased. For example, if an M5 train passed the leak
check after sampling in the first port but failed the
confirming leak check before beginning sampling in
the second port due to a probe liner being broken
during port change, the test could be allowed to con-
tinue after replacement of the probe liner and including
rinsing of the broken liner for particulate recovery.
However, if the train failed the leak check after removal
from the first port, the sample would be invalid, even if
it were believed that the probe liner was broken as the
probe was removed from the port (i.e., it is not possible
to know if the probe liner was already broken before
removal from the port).
POHCs which have a boiling point between 100° and
140°C may break through the XAD-2 resin in a semi-
VOST if the sampling time is too long or may be diffi-
cult to purge from a VOST trap. The validity of the
method chosen for these POHCs should be deter-
mined prior to testing (see Section 3.4.5.4). Experts in
analytical chemistry may need to be consulted to
determine the appropriate sampling method for these
POHCs.
Volatile POHCs should be sampled with the VOST
(SW-846 Method 0030), if possible. Samples may be
collected in bags if VOST samples cannot be per-
formed. The bag sample procedure is less desirable
due to potential problems with adsorption in the bag
and loss of sample. Stability of the POHC to be sam-
pled in the bag should be checked prior to sampling, if
this method is used. Field blanks are essential with
bag sampling.
VOST field blanks are required, and VOST trip blanks
and laboratory blanks are highly recommended.
It is recommended that both the front (Tenax) and back
(Tenax/charcoal) trap of all pairs of traps from each run
be analyzed separately. The results of these separate
analyses allow determination of the percent distribu-
tion of the volatile POHCs collected on the front and
back traps. The samples are considered valid (no
breakthrough) if the back trap contains no more than
30% of the quantity collected on the front trap. This
criteria does not apply when the quantity of sample
collected is low (i.e., less than 75 ng on the back trap).
Some latitude in judging the validity of a sample versus
this criteria can be considered based on how closely
the DRE standard was met and how closely the trap
distribution criteria was met. For example, if the DRE
was 99.999% and the distribution was slightly higher
than 30% on the back trap, one could still have confi-
dence a 99.99% DRE was achieved. Use of three
traps in series (Tenax-Tenax-Tenax/charcoal) can be
considered to provide further indication of sample
validity, however, use of thi§; approach should be
reviewed by an expert experieheeclin VOST sampling
and analysis.
The VOST protocol allows multiple pairs of traps from
the same run to be combined for analysis, if increased
analytical sensitivity is required. In rare cases where
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this increased sensitivity is needed, a reasonable
approach is to combine all front traps from a test run
for one analysis and all back traps for a second analy-
sis. This procedure retains information on distribution
of POHCs between the front and back traps while
allowing the greater sensitivity. The same criteria
described above is used to judge the validity of the
samples.
The trial burn plan should show that a sufficient quan-
tity of POHCs is in the waste feed to demonstrate a
destruction and removal efficiency (ORE) of 99.99%,
given the VOST or semi-VOST sample size and lower
detection limits of the analytical instrumentation. An
example calculation based on VOST sampling is
shown in Table 2. Generally, a concentration of 100
ppm in the waste is considered a minimum detectable
level for POHCs.
Traceability procedures must be used for handling all
samples. Full chain-of-custody procedures are typi-
cally much more labor-intensive but may be used at the
applicants option.
2.5 Reporting of Results
The results should be reported in a format which includes
all information and data necessary to calculate final
results, presented in as clear and succinct format as
possible. This will include a description of the operating
system; the operating conditions during the test; the
measured quantities of POHCs, HCI, and paniculate in
all samples; and the calculated results. Example formats
for presentation of these data are presented in the Guid-
ance on Setting Permit Conditions and Reporting Trial
Bum Results.
The results of the analyses for particulate emissions, HCI
emissions and removal efficiency, and ORE should be
reported separately for each run and should not be aver-
aged for the trial runs. This does not preclude averaging
multiple samples taken during each run.
VOST analytical results should be reported as individ-
ual values for each trap as well as an average value for
each run (as total ng/L of sample). The average
amounts to dividing the total quantity (ng) on all traps
by the total sample volume (L) for all traps. An illustra-
tive example is provided in Table 3. In this example, in
run 3, a sample was lost, but the total sampling period
was still > 60 min, so the results are usable. Ordinar-
ily, 120-min sampling is the goal. Note that samples
were collected with four pairs of VOST traps so that the
minimum recommendation of three pairs of traps per
run is still met when data for one pair are lost in run 3.
The permit reviewer should consult the Guidance on
Setting Permit Conditions and Reporting Trial Burn
Results for further guidance on how results should be
reported and the Practical Guide Trial Burn for Haz-
ardous Waste Incinerators1 and other references on
how sampling and analytical data should be converted
into final results. A portion of the Practical Guide is
repeated below to provide practical suggestions
regarding blank correction, significant figures, round-
ing, and handling "less than" and "greater than"
values.
Table 2. Example Calculation to Determine Whether VOST
Sample Size Is Sufficient to Measure 99.99% ORE for
Carbon Tetrachloride
Basis
Waste feed flow rate: 15.2 kg/min (2,000 Ib/h)
POHC: Carbon tetrachloride
Waste feed concentration: 500 ppm (0.50 g/kg feed)
Stack gas flow rate: 4,500 scfm (127.4 rrf'/min)
Lower detection limit: 2 ng per trap
Proposed sampling
VOST: 3 trap pairs at 500 mL/rriin flow rate; 20 L sample/pair
1. POHC input rate
15.2 kg/min x 0.50 g/kg = 7.6 g/min .
2. POHC stack output rate at 99.99% ORE
7.6 g/min (1 0.9999) = 0.00076 g/min
3. POHC concentration in stack gas at 99.99% ORE
0.00076 g/min _ o.0000060g/m3x109ng/gx lO^mVL = 6.0 ng/L
127.4 mVmin !
4. Sample amount collected on one pair of traps
20 Lx 6.0 ng/L = 120 ng
Since the VOST lower detection limit for carbon tetrachloride is 2 ng,
the sample is sufficient to detect carbon tetrachloride to determine a
ORE of 99.99% or lower. A margin of safety above the detection limit
is desirable. :, - .
This calculation assumes both traps in a pair are combined for
analysis. If they are analyzed separately, the distribution of mass on
each trap must be considered.
2.5.1 Blank Correction
Because achievement of 99.99% ORE often results in
stack concentrations that are at or below ambient or
laboratory levels for POHCs, contamination of samples
can be a significant problem. The purpose of blank cor-
rection procedures is to account for any portion of the
sample results that represent contamination, or some-
thing other than the value intended to be measured (e.g.,
stack emissions).
The underlying philosophy of the procedure is based on a
paper prepared by the American Chemical Society Com-
mittee on Environmental Improvement2 and on experi-
ence in conducting and interpreting trial burn data. The
ACS paper assumes that blank values are random sam-
ples that vary because of preparation, handling, and
analysis activities. Under this assumption, blank values
can be treated statistically. The "best estimate" for the
blank for any particular sample is the mean of the avail-
able blanks. The ACS procedure also enables determina-
tion of whether a sample is "different from" the blank. If
the sample value is not significantly different from the
blank value, a sample cannot be blank-corrected.
Even so, the measured sample value does provide an
upper bound for the emission value and may still provide
sufficient information for determining if the required ORE
of 99.99% was met.
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Table 3. Example Reporting of Volatile POHC Emissions
Run no.
1
2
3
Trap pair
1
2
3
4
Total/average"
1
2
3
4
Total/average0 "
1
2?
3
4
Total/average"
Sample
period
(mln)
30
30
30
30
120
30
31
30
30
121
30
29
30
89
Sample
volume*
(L)
20.1
19.8
21.3
19.5
80.7
19.7
22.1
20.8
21.0
83.6
20.4
20.2
19.9
60.5
Average blank value1 (ng)
Standard deviation1 (ng)
POHC concentration0 Stack gas Emission rate*
POHC collected" (ng) (ng/L = ng/Nm») flow rate" (ug/mln)
CCI4
16
19
30 (24)
25 (19)
78
37(31)
21 (15)
28 (22)
31 (25)
93
14
8.6
12
35
5.8
6.9
CCI2CHCI CCI4
71 (60)
180 (170)
45 (34)
105 (94)
360 0.97
220 (210)
180(170)
270 (260)
210(200)
840 1.1
56 (45)
37 (26)
48 (37)
108 0.58
11
2.7
CCI,CHCI (NmVmln) CCI, CCI,CHCI
4.5 181 180 810
10.0 173 190 1700
1.8 190 110 340
Note: Slow VOST results are shown; a similar format would be used for fast VOST or integrated bag sampling for volatiles.
Sample volume is dry standard liters of stack gas.
" If blank corrected, that value shown in parentheses.
c Blank corrected as applicable.
' Stack gas flow rate is dry normal (standard) cubic meters per minute.
Totals for sample period, volume, and amount collected; averages for concentration, flow rate, and emission rate.
1 All blanks (both field blanks and trip blanks) were used for average and standard deviation.
8 Sample lost.
The blank correction procedure applies mainly to stack
emission samples and consists of the following:
a. Assemble data for each POHC from all of the field and
trip blanks. An example of such data for VOST might
be:
Run 1 Run 2 Run 3
POHC A Field blank 0.008 ug < 0.002 ug 0.004 ug
Trip blank 0.005 u,g 0.004 ng 0.003 pig
b. Determine whether or not the field blanks are statisti-
cally differ ent from the trip blanks by using the paired
t-test (consult a statistics text).
If the field blanks are significantly higher than the trip
blanks, use the field blank data only. If the blanks are
not significantly different, use all of the blank values.
Higher field blanks indi cate background due to field
exposure, which trip blanks do not measure.
c. Calculate the average and standard deviation of the
blanks (many calculators have statistics functions
which allow you to do this easily).
d. Determine whether or not each measured sample
value is "different from" the blank value by using the
following test for each sample:
s = sample value (ug)
b = (blank average) + 3 (standard deviation of
blanks)
If s is greater than b, then the sample is "different"
from the blanks.
e. If the measured sample value is different from the
blank value, then the blank correction procedure is
applied:
Blank-corrected emission value (ug) =
measured sample value (ug) - average blank value
f. If measured sample value is not different from blank
value, then the measured sample value is used as an
upper bound emission value, and the emission rate is
considered less than or equal to the measured value.
This results in the reporting of emission concentration
and mass emission rate with a "< " sign. As a conse-
quence, DRE would be reported with a " > " sign.
2.5.2 Significant Figures and DRE
DRE is usually reported with one or two significant fig-
ures depending on the accuracy of the measured values
which go into the calculation of DRE. It is important to
note that a reported DRE of 99.99% or 99.999% has only
one significant figure. The reason for this is that what is
actually being measured is the penetration, which is the
amount of a compound which is not destroyed. That is:
-------
ORE = 100% Penetration
For a ORE of 99.99%, the penetration is 0.01 % (one
significant figure). For a ORE of 99.9916%, the penetra-
tion is 0.0084% (two significant figures).
The ORE is reported with the same number of significant
figures as the least accurately measured value used in
the calculations. The controlling measurement that deter-
mines the number of significant figures is usually the
stack concentration. GC/MS methods can normally only
report concentrations with one or two significant figures.
This will result in a ORE with the same number of signifi-
cant figures as reported concentrations, unless another
measured value (waste feed concentration, waste feed
flow rate, or stack gas flow rate) has fewer significant
figures.
2.5.3 Rounding Off ORE Results
The rules on this are stated in the Guidance Manual for
Hazardous Waste Incineration Permits:3 "... if the ORE
was 99.988%, it could not be rounded off to 99.99%." In
other words, your calculated value, after rounding to the
proper number of significant figures, must equal or
exceed 99.99% to be acceptable. (Note: This same rule
applies to rounding HCI results to 99%.)
2.5.4 Reporting ORE with a " < " or" > " Sign
As mentioned in the section on blank corrections, if the
sample is not "different" from the blank (greater than the
average blank plus three standard deviations), then it
cannot be blank-corrected. As a consequence, the ORE
will be reported with, a ">" sign. This reported ">"
value will also occur when the POHC in the sample is
undetected (below detection limit of the analysis
method). But as long as the ORE is > 99.99%, this is not
a problem.
In cases where both the blanks and samples have high
values, a ORE below 99.99% may be preceded by a " > "
sign (i.e., > 99.96%). Such a number is useless in evalu-
ating achievement of 99.99%. Experience in using the
recommended sampling methods and avoiding contami-
nation is the only way to minimize this possibility.
Occasionally, a sample may saturate the GC/MS with the
POHC in question. This will result in an emission rate
with a ">" sign and a ORE with a "<" sign. If such a
ORE is below 99.99%, the incinerator clearly fails. If it is
above 99.99% (i.e., <99.9964%), the number is use-
less. To avoid such problems, the test protocol should be
chosen based on estimated concentrations. Several fac-
tors to consider include (1) collecting less sample on the
VOST (2) using a sample splitter during analysis so that
only a portion of the sample is directed to the GC/MS, or
(3) using alternative sampling methods (e.g., integrated
bag). If these techniques are being considered, the
Source Methods Standardization Branch, AREAL, EPA
or OSW, EPA should be consulted.
The conclusion of this section is always design the sam-
pling and analysis so that passage/failure of the 99.99%
criterion is determinable. This can best be done by pre-
liminary estimates of POHC concentrations in the stack
(assuming 99.99% ORE) and with selection of sampling
and analysis methods having appropriate upper and
lower limits of detection. Experience in use of these
methods to avoid contamination is also a key factor.
2.6 Continuing Analysis and Monitoring
After the trial burn test is completed and after the permit
is obtained, analysis and monitoring must continue. Each
type of waste feed material must be analyzed at least on
an annual basis according to recent EPA policy. More
frequent analysis is necessary if composition of the
waste feed is highly variable or is expected to change
(e.g., different source, process change, etc.).
The permit will establish the monitoring requirements for
process parameters, air pollution control devices, and
stack gas emissions. The exact parameters to be moni-
tored are established on a case-by-case basis, as
described in the Guidance on Setting Permit Conditions
and Reporting Trial Burn Results. The permit monitoring
requirements and continuing waste feed analyses are
intended to verify continued satisfactory operation of the
incinerator.
-------
Sections
Measurement Methods
Many methods can be used for process monitoring, sam-
pling, and analysis of samples during a trial burn and
subsequent operation of the incinerator. This review
focuses on the most commonly used and recommended
methods for measurement.
3.1 Specification of Method Options
The trial burn plan must present the sampling and analyt-
ical methods in sufficient detail for both review and field
and laboratory implementation. Many of the referenced
methods give several options which may be employed by
the sampler or analyst. The trial burn plan should specify
which options will be used. If selection of an option
depends on the sampling conditions or sample charac-
teristics and cannot be made at the time the plan is
submitted, the decision criteria for subsequent selection
of the options must be presented. Some referenced
methods, especially those presented in the Arthur D.
Little report, Sampling and Analysis Methods for Hazard-
ous Waste Combustion,4 are general descriptions of the
methods and may not provide sufficient detail to specify
the methods. In such cases, the trial burn plan should
give a detailed step-by-step procedure. Often the sam-
pling crew and analytical laboratory will have sets of
standard operating procedures (SOPs) for the common
analyses encountered in hazardous waste incineration.
These SOPs can be appended to the trial burn plan and
cited in the text.
For many trial burns, sampling and analysis of different
analytes will be performed by more than one laboratory.
Few laboratories have the capabilities to do all of the
analyses required. In these cases the applicant should
specifically identify the laboratory who will be doing the
work for each method and should specify the methods
employed in the same level of detail for all laboratories.
The trial burn plan may include this information or it
should specify a time, sufficiently before the trial burn to
allow EPA review, that it will be provided. The laboratory
that conducts the sampling and analysis may not have
been selected when the trial burn plan is submitted.
3.2 Process Monitoring
Two important parameters which must be continuously
monitored during operation of the incinerator are the
waste feed rate and the combustion temperature.
Another important parameter is the combustion chamber
pressure, which is often used as a method of monitoring
fugitive emissions. Methods used to measure these three
parameters are discussed below. CO monitoring will be
covered in Volume VI of the Guidance Series (see Sec-
tion 1.0) being prepared by EPA. Other parameters, e.g.,
combustion gas velocity, are not covered at this time. The
EPA, Office of Solid Waste, may be consulted for addi-
tional guidance.
3.2.1 Waste Feed Rate
The waste feed rate to an incinerator can be monitored in
a variety of ways, depending upon the types of feeds
encountered. The feeds may be solids or sludges, free-
flowing liquids, or gases.
3.2.1.1 Solid-Sludge Feeds
Volumetric methods These include calibrated
augers and pumps, rotary feeders, and belt conveyors.
These systems are not generally available precalibrated
but must be calibrated by the user for each particular
feed material. The accuracy of the method depends upon
steady operation at a given speed and assumes appro-
priate feeders are used to ensure the cavities are always
filled to capacity. Most of these methods can provide
some kind of tachometer signal to indicate speed, which
must be related to feed rate by performing calibration
tests. These methods are generally more appropriate as
secondary indicators of feed rate.
Level indicators These include methods based upon
mechanical, ultrasonic, nuclear, and radio frequency
principles of operation. Nearly all tank level indicators will
perform better with somewhat uniform (free-flowing) par-
ticles. This will aid in distributing the level of material
evenly within the vessel, allowing for more accuracy in
whatever monitoring system is used. Typically, these
methods can monitor tank levels to within ± 1 %.
Since level indicators cannot provide physical character-
istics for the feed material (i.e., density, moisture), care
must be taken when using any of these systems to
account for cross-sectional area of the tank and changes
in composition of the feed.
-------
Stationary weight indicatorsThese methods, which
include weigh hoppers/bins and platform scales, deter-
mine the dead weight of material loaded into a hopper,
bin, or container. After weighing, the contents are then
fed as batches into the process. All of these weigh sys-
tems give fairly accurate monitoring of weight (within
*1%), but one must consider the batch feeding system
operations before a true appraisal of the feed rate moni-
toring can be made.
Conveyor weighing systemsThese methods include
belt weighers, weigh belts/augers, and loss-in-weight
feeders. All conveyor weighing systems are fairly similar
in operation, mainly differing because of placement loca-
tions of the weighing device. In general, the accuracy of
these systems is around ±2% but tends to decrease as
particles become larger and less uniform in size. Sludges
can be monitored with the systems, provided that wet
material does not drain off the conveyor belt. Screw
augers, however, can often be used in such cases to
replace the conventional conveyor belt.
Momentum flowmetersTwo types of these solid flow-
meters are available, based upon either impact or torque.
These devices work fairly well with dry, f lowable materials
but are less accurate if feed particles are very large,
nonuniform, or viscous. Typical accuracies are within
*2%. Sludges are not recommended because of their
viscosity and splashing effects.
Nuclear absorption Methods based upon absorption
of gamma radiation include nuclear level meters, nuclear
belt or auger scales, and a combination of nuclear den-
sity meters and ultrasonic flowmeters. Nuclear absorp-
tion only measures density; therefore, another instrument
must also be used to measure volume, speed, or another
parameter to obtain feed rate. Nuclear instruments can
be used on nearly any material including sludges. Radia-
tion absorption is proportional to the mass present, so
particle size and configuration will not greatly hinder
accuracy. Sludge operations will work best with a nuclear
density detector/ultrasonic flowmeter combination, ena-
bling the process material to be fed through conventional
piping. Accuracies of nuclear devices may not be as high
. as gravimetric systems but may be sufficient on a practi-
cal basis.
3.2.1.2 Liquid Feeds
Typical flowmeters used to monitor the liquid waste feed
rate to incinerators are detailed below.
Rotameter This type of flowmeter is available for a
wide range of liquid viscosities including some light-
weight slurries. It is calibrated through using a fluid of
known density. Reported accuracies are within ±5% of
full-scale.
Orifice meterThis instrument is used with gases and
low viscosity fluids. Typical accuracies are ±1% full-
scale, which is the accuracy of the differential
pressure measuring device used on a clean fluid. When
used with dirty or viscous fluids, both accuracy and life of
the instrument are sacrificed. An accuracy of ±5% may
be more realistic in these cases.
Vortex shedding meter This device is applicable to
low-viscosity fluids and gases under turbulent flow condi-
tions. The accuracy is ±2% under normal operations.
Positive displacement meter This type of flowmeter
is more applicable than other types for use with higher
viscosity fluids. However, accuracy is highest when used
with a clean, moderately viscous fluid. It cannot be used
with multiphase liquids, gases, or slurries of varying
density.
Mass flowmeter This instrument, also known as a
Coriolis flowmeter, applies to liquids of widely varying
viscosity and density and most slurries. It has been
advertised for use with gases, but that application may be
rare. The reported accuracy is within ± 1 %.
3.2.1.3 Gaseous Feeds
The best types of flowmeters for gases are the orifice
meter and the Vortex shedding meter, discussed above
under liquid feeds.
3.2.2 Combustion Temperature
Combustion temperature is usually monitored through
the use of thermocouples, optical pyrometers, or both.
3.2.2.1 Thermocouples
Thermocouples are available in a variety of types, with
each type constructed of specific metals or alloys. The-
temperature ranges and reported accuracy vary by type.
The environment the thermocouple is suited for also var-
ies. A summary of thermocouple types and limitations is
given below.
Type Materials
Upper Thermocouple
Temp. Accuracy
Environment
J
E
K
S
R
B
Iron/constantan
Chromel/constantan
Chromel/Alumel
Pt 10% rhodium/pure Pt
Pt 13% rhodium/pure Pt
Pt 30% rhodium/pure Pt
6% rhodium
1400
1650 !
2300
2650
2650
3100
0.75
0.50
0.75
0.25
0.25
0.50
Reducing, vac-
uum, or inert
Oxidizing or inert
Oxidizing or inert
Oxidizing or inert
(no metal tubes)
Oxidizing or inert
(no metal tubes)
Oxidizing or inert
(no metal tubes)
Source: Complete Temperature Measurement Handbook and Encyclopedia,
Omega Engineering Inc., 1986.5
The accuracies given above do not consider environ-
mental effects. Thermocouple location in the combustion
chamber, for example, greatly affects the accuracy of
temperature readings. Typically, thermocouples are
located at the gas exit from the combustion chamber.
This is generally believed to give the best overall average
10
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combustion chamber temperature. Other factors to con-
sider when examining thermocouple locations are:
Temperature readings will be affected by radiant
pickup or loss if the thermocouple is located close to
and within a direct line of sight of either the flame or
the cold quench chamber.
To improve accuracy and limit wall effects, the thermo-
well should extend 3 to 6 in. beyond the refractory and
should be located where the gas velocity is high and
not in a stagnant corner of the chamber.
The use of two thermocouples in separate wells is recom-
mended to provide a check on continued proper opera-
tion. The difference in the readings between the two
thermocouples should be noted during initial operation;
e.g., one thermocouple will likely give a reading higher
than the other one. The difference between the two read-
ings should then be checked periodically as an indicator
of problems with one of the thermocouples. If the differ-
ence changes by more than 50 °F, both thermocouples
should be checked for proper operation.
Following the above guidelines allows for some degree of
consistency in measuring combustion temperature in an
incinerator. Changes in either the thermocouple type or
location should prompt reconsideration of the accuracy
and representativeness of the measurement.
3.2.2.2 Optical Pyrometers
Optical pyrometers are typically used to measure the
temperature of the furnace wall or an object within the
furnace but can be used to measure the combustion gas
temperature. In cases where the gas temperature is
desired, the pyrometer is normally equipped with a
closed end tube much like a thermocouple well but larger,
and the pyrometer is sighted on the end of this tube. In
this situation, emissivity corrections are not needed, This
configuration is normally used for high temperatures
when contamination or breakage of thermocouples is a
problem and the cost or difficulty of replacement is high.
The pyrometer will normally require calibration but
should, when calibrated, be approximately as accurate
as a thermocouple.
3.2.3 Combustion Chamber Pressure
Monitoring of the combustion chamber pressure is often
used to ensure correct operation of the incinerator and to
prevent fugitive emissions. Many combustion chambers
are operated under draft (less than atmospheric pres-
sure) conditions, which ensures that combustion off
gases do not exit the chamber before passing on to the
scrubber or other air pollution control equipment.
Instruments used to monitor combustion chamber pres-
sure are known as differential pressure gauges, AP
transducers, or draft gauges. Such instruments are com-
posed of a bellows or diaphragm enclosed within a stain-
less steel casing. Deflection of the diaphragm due to
combustion chamber pressure is then measured by mag-
netic pickup coils also mounted within the casing. The
instruments are located on the combustion chamber and
typically measure pressures on the order of several
inches of water.
Accuracy of a differential pressure gauge is within ± 1 %
full-scale, although the combustion chamber environ-
ment severely hinders this performance. Particulate clog-
ging, moisture, corrosion, and other contaminants are
typical problems. A precise measure of combustion
chamber pressure is difficult, but these instruments can
be used to indicate whether the pressure within the com-
bustion chamber is positive or negative. Calibration
against an inclined manometer at least annually is
recommended.
3.3 Sample Collection
Sampling methods for the waste feed, stack gases, auxil-
iary fuel, quench and scrubber water, and ash are given
primarily in four sources: (1) Tesf Methods for Evaluating
Solid Waste Physical/Chemical Methods, SW-8466; (2)
Sampling and Analysis Methods for Hazardous Waste
Combustion*; (3) Code of Federal Regulations, 40 CFR
Part 60, Appendix A7; and (4) The American Society for
Testing and Materials, Annual Book of ASTM Standards.*
EPA-600/8-84-002 should be consulted first as it provides
cross-references to more fully documented sources of
methods (i.e., SW-846 or ASTM). These other sources
should then be consulted. If there is a conflict between
these documents, SW-846 has precedence. The discus-
sion which follows addresses the most commonly used
methods available for sampling these parameters.
3.3.1 Waste Feed
The objective of waste feed sampling is to obtain a repre-
sentative sample of the waste feed. It is important that the
sampling plan be explicit and that it explain the logic
behind the selection of the sample collection scheme.
For many waste feeds, representative sampling is
difficult.
The waste feed for incinerators may be a free-flowing
liquid, slurry, sludge, or a powdered, granular, or large-
grained solid. Various methods are available for sampling
these waste feeds and are described in SW-846,6 EPA-
600/8-84-0024 and the ASTM Standards.8 These meth-
ods are discussed in further detail in the following
subsections.
3.3.1.1 Free-Flowing Liquids
The most common method used for sampling free-
flowing, low-viscosity liquids is tap sampling from the
waste feed line or tank. Other methods that may be used
for sampling from drums, tanks, or ponds include a col-
iwasa (composite liquid waste sampler), weighted bottle,
or dipper. Each of these methods and types of equipment
used are described in the following sources:
11
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SW-846
Sampling Method Chapter 9,
EPA-600/
8-84-002
Method
Old New
ASTM ASTM
Standards Standards
Tip sampling
Cottwasa
Dipper
Weighted bottla
TMof
p. 49-51
p. 50.53
p. 50,52
p. 50,54
S004
S001
S002
S003
S005
D-270-75
D-270-75
E-300-73
D-4057-9.3
D-4057-9.6
D-4057-9.5
D-4057-9.7
Sampling a free-flowing liquid waste feed can be per-
formed by obtaining tap samples from the storage tank or
process feed line(s). The liquid in a storage tank should
be thoroughly agitated and mixed to obtain representa-
tive samples. If the feed contains two immiscible liquid
phases or solids which could stratify in the feed line, a
mixer may need to be inserted in the feed line prior to the
tap to obtain representative samples.
3.3.7.2 Viscous Liquids, Slurries, Sludges, and Solid
Waste Samples
Sampling methods and the equipment required for vis-
cous liquids, slurries, sludges, and solid waste feeds are
described in SW-846, EPA-600/8-84-002, and the ASTM
Standards. These methods are described in SW-846 and
EPA-600/8-84-002 as follows:
Method Name
Type of Waste
Thiol (grain sampler) Dry powder or granules
Trior(corof) Sludge or moist solids
Trowel (scoop) Moist or dry solids
Auger Packed solids
SW-846 ADL
Chapters Method
p. 50,54 S005
p. 50,55 S006
p. 50 S007
p. 50
The sampling protocols given in the ASTM Standards for
the different types of waste feeds are:
Extremely viscous liquids
Crushed or powdered materials
Soil or rock-lite material
SoiWika material
Fly ash-like material
ASTM Standard D140-70
ASTM Standard D346-75
ASTM Standard D420-69
ASTM Standard D1452-65
ASTM Standard D2234-76
Samples of extremely viscous liquids, slurries, and
sludges are usually obtained from their containers by the
methods described above. Samples of solid waste are
usually obtained from the containers, waste piles, or from
the process feed system, such as a conveyor belt or
auger system.
3.3.2 Auxiliary Fuel
Sampling of liquid auxiliary fuel may be appropriate so
that the samples may be analyzed for the POHCs and
higher heating value (for total heat input), although this
measurement is not required by RCRA. The methods for
sampling the fuel are the same as those used for free-
flowing liquid wastes. Tap sampling (S004) is the most
common method used for liquid fuels.
3.3.3 Stack Gases
Stack gases must be sampled for the following parame-
ters during the trial burn; particulates, hydrogen chloride
(HCI), H2O, CO2, CO, and principal organic hazardous
constituent (POHC) emissions. Stack gas flow rate, vol-
ume, and temperature must be measured during the
sample collection. Analyses of these samples are
required by 40 CFR Part 264 (Subpart O) and 40 CFR
Parts 270.19 and 270.62.7 Table 4 summarizes the sam-
pling methods used for stack gases for RCRA trial burns.
Many of these parameters can be sampled using the
standard EPA reference methods shown in Table 5.
Methods for both volatile and nonvolatile metals are
included in Table 4 for completeness, since sampling may
be requested. Additional information on methods for CO,
oxygen, total hydrocarbon (THC), HCI, and metals,
including draft performance specifications for CO and
oxygen, can be found in Volume VI of the Guidance
Series (see Section 1).
An important aspect of obtaining a valid stack gas sam-
ple is the experience and performance of the sampling
personnel. The sampling personnel, especially the
supervisor, must be adequately trained, as evidenced by
either previous experience or documented training.
3.3.3.7 HCI
Hydrochloric acid (HCI) emissions are currently mea-
sured using a CEM or manual methods consisting of a
collection train and/or analytical procedure. Manual col-
lection methods normally extract a gas sample from the
stack and absorb the HCI in an absorbent. The sampling
train consists of a particulate filter, the absorption solu-
tion, and a provision for measuring the sampled gas
volume. The EPA Method 5 train, an EPA Method 5 train
modified for metals, or a specific impinger train have all
been employed. The M5 trains are normally used when
HCI is to be collected in addition to sampling for particu-
lates or metals. If sampling is to be performed for only
HCI, then a specific impinger train is employed. For sam-
pling HCI using the M5 as described in the Federal Regis-
ter, the M5 procedures are followed except that the water
in the impingers is replaced with an absorbing solution. A
draft method for HCI sampling, Determination of HCI
Emissions from Municipal and Hazardous Waste Inciner-
ators, is being prepared by EPA, AREAL, Source Meth-
ods Standardization Branch. This method is undergoing
further revision, e.g., a better filter arrangement than
shown in the current draft will be recommended.
A solution of sodium of potassium hydroxide has fre-
quently been used to absorb the HCI. This approach has
been satisfactory except that the solution also absorbs
the other acid gases contained in the sample including
carbon dioxide (CO.,). The use of the hydroxide solution
therefore may require that a correction be applied to the
sample volume for the gases that were removed before
the gas volume meter in the sampling stream. This cor-
rection may be avoided by substituting other solutions for
12
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Table 4. Sampling Methods for Stack Gases in RCRA Trial Burns
Sampling parameter
Sampling method
Particulates, C\; H2O, nonvola-
tile metals (if present in feed)
Semivolatile and nonvolatile
POHCs
Volatile POHCs
C02,02
CO
Volatile metals (if present in
feed)
M5 train with appropriate solutions in one
or more of the impingers
Semi-VOST (SW-846 Method 0010)
VOST (SW-846 Method 0030) ,
EPA Method 3 Orsat analysis of integrated bag sample
Continuous monitor, proposed performance specifications are being prepared by
EPA3 . .
M5 train with appropriate solutions in the
second impinger
NOTE: POHCs = Principal organic hazardous constituents.
VOST = Volatile organics sampling train.
Table 5. EPA Reference Methods Used to Test RCRA Hazardous Waste Incinerators
Method description
EPA Method 1: Sample and velocity traverses for stationary sources
EPA Method 2: Determination of stack gas velocity and volumetric flow rate (type S pilot tube)
EPA Method 2A: Direct measurement of gas volume through pipes and small ducts , ..
EPA Method 3: Gas analysis for carbon dioxide (CO2), oxygen (O2), excess air, and dry molecular weight (Orsat)
EPA Method 4: Determination of moisture content in stack gases
EPA Method 5: Determination of particulate emissions from stationary sources
NOTE: All of these EPA methods are fully described in 40 CFR Part 60, Appendix A, revised as of July 1,19857
the hydroxide. There is a lack of consensus on the
impinger reagent most appropriate for collection of HCI.
A sodium carbonate solution has been recommended,
since this reagent will not absorb CO2. There is evidence
to suggest that caustic reagent is not necessary and that
HCI is efficiently trapped in any aqueous medium. If this
is true, then distilled water (e.g., ASTM Type II reagent
water) may be the reagent of choice for collection of HCI.
The draft method being prepared by EPA recommends
dilute acid solutions.
3.3.3.2 Volatile Organics
The methods used to sample the POHCs and other
organics depend upon their volatility. Volatile POHCs
(generally those with a boiling point between 30° and
100°C, see Section 3.4.5.4.1) are sampled using a VOST
The VOST and its operation are fully described in the
Protocol for the Collection and Analysis of Volatile POHCs
Using VOST,a the two-volume study Validation of the Vola-
tile Organic Sampling Train (VOST) Protocol,10 the EPA-
600/8-84-002" as Method S012, and Part 111, Chapter 10
of SW-846 as Method 0030.
Several variations on the basic VOST design are avail-
able from vendors or may be constructed by the sampling
organization. The sampling plan should show a sche-
matic of the train actually used and also describe the
exact apparatus and operation. Critical aspects include
the train setup, probe position in the actual stack geome-
try to be tested, leak check procedures, and sample
handling. The latter is particularly important, since the
volatile organics in ambient air as well as other sources of
contamination can affect the accuracy of results. There-
fore, care must be taken to prevent contamination of the
sorbent cartridges before and after the collection of the
stack gas sample.
In planning the VOST sample collection, the sample vol-
ume required to demonstrate the 99.99% ORE should be
calculated as described in Section 2.4 and Table 2. The
volume of the VOST collection can then be scaled
accordingly. If numeric values for POHCs at concentra-
tions much higher than the value needed for the 99.99%
ORE must be reported, a second VOST collection with a
smaller sample volume may be required to prevent satu-
ration of the GC/MS system.
As noted in the documents describing VOST, a variety of
methods are available for generating standards for cali-
bration of the GC/MS. The VOST protocol10 specifies the
injection of a methanolic standard solution onto the car-
tridge followed by flash evaporation of the methanol. This
is workable but presents several practical problems. Very
volatile compounds can evaporate from the methanolic
solution. The residual methanol prevents scanning the
mass spectrometer below about mass 34 (M + 2 of meth-
13
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anol). There is also a possibility that some POHCs may
react with the methanol. Other alternatives listed in the
validation documents10 are gas cylinder standards, per-
meation devices, and static gas bottle standards.
Gas cylinder standards are prepared from outside
sources and certified by the supplier. These cylinders
can be purchased to contain various POHCs at various
gas concentrations.
Permeation tubes and other devices can generate a reli-
able, accurate gas mixture. They are commercially avail-
able or can be prepared for most POHCs. However,
setting up, maintaining, and monitoring a permeation
system is expensive and time-consuming. In addition,
the concentrations of the POHCs in the gas stream are
governed by their permeation rate, so the flexibility to
generate different concentrations is limited.
Static gas bottle standards are generated by evaporating
a known amount of the POHCs in a gas bottle to give a
known gaseous concentration. This is a simple standard
preparation method; however, accuracy can be a prob-
lem if evaporation is incomplete or the POHC adsorbs to
the wall of the vessel.
The EPA also operates a program to develop organic gas
audit materials and provide these audit gas cylinders for
use in VOST performance audits during trial burns. Four
different audit cylinders are available that contain the
volatile organic compounds shown in Table 6. Any fed-
eral, state, or local agency or its contractor planning haz-
ardous waste trial burn tests may request a performance
audit by contacting Mr. Robert Lampe, USEPA, Environ-
mental Monitoring Systems Laboratory, Quality
Assurance Division, Research Triangle Park, North Caro-
lina 27711.
Collection of stack gas samples in Tedlar bags is listed as
an option for sampling volatile organics in Method S011
in EPA-600/8-84-002; however, several problems with the
analysis of bag samples severely limit the utility of this
option. Samples are collected in 30-L Tedlar gas bags
using an integrated gas sampling train. The bags are
then transported to the analytical laboratory, and if the
VOST traps are saturated, a small volume of gas from the
bag is transferred to a clean VOST trap for analysis. This
approach presents some practical problems. Tedlar bag
samples have a relatively short holding time of 1 to 2 days
for some specified compounds according to EPA Method
23.12 Therefore, the use of Tedlar bags is practically lim-
ited to tests where the VOST analysis is being conducted
on-site or within a very short holding time. The bag sam-
ple procedure is less desirable than VOST due to poten-
tial problems with adsorption in the bag and loss of
sample. Stability of the POHC to be sampled in the bag
should be checked prior to sampling, if this method is
used. Field blanks are essential with bag sampling.
3.3.3.3 Semivolatile Organics
Semivolatile POHCs and other organics with boiling
points above 100°C are sampled with a semi-VOST
(sometimes referred to as a Modified Method 5 [MM5]
train). Those organic compounds with boiling points
between 100° and 140°C may also be suitable for sam-
pling with VOST However, experts in analytical chemistry
should be consulted for sampling of compounds in this
boiling point range.
The semi-VOST is an EPA Method 5 train which has
been modified by placing a sorbant module (usually con-
taining XAD-2 resin) before the first impinger. This train is
identified in Part III, Chapter 10 of SW-846 as Method
0010,6 and in EPA-600/8-84-002 as Method S008.4 The
sampling train is fully described in Modified Method 5
and Source Assessment Sampling System Operations
Manual, and in the two-volume report, Laboratory and
Field Evaluation of the Semi-VOST (Semivolatile organic
sampling train) Method." Sampling trains with XAD resin
traps should not be used to collect HCI.
Tables. VOST Audit Compounds*
Group I compounds Group II compounds
Group III compounds
Group IV compounds
Carbon tetrachloride
Chloroform
Perchtoroethylene
Vinyl chloride
Benzene
Group 1 ranges
7to90ppb
90to430ppb
430 to 10.000 ppb
Trichloroethylene
1,2-Dichloroethane
1 ,2-Dibromoethane
Acetonitrile
Trichlorofluoromethane
(F-11)
Dichlorodifluoro-
methane (F-12)
Bromomethane
Methyl ethyl ketone
1,1,1-Trichloroethane
Group II ranges
7 to 90 ppb
90 to 430 ppb
Vinylidene chloride
1,1,2-Trichloro-1,2,2-
trifluoroethane
(F-113)
1,2-Dichloro-1,1,2,2-
tetrafluoroethane
(F-114)
Acetone
1-4 Dioxane
Chlorobenzene
Group III ranges
7 to 90 ppb
90 to 430 ppb
Acrylonitrile
1,3-Butadiene
Ethylene oxide
Methylene chloride
Propylene oxide
Ortho-xylene
Group IV ranges
7 to 90 ppb
430 to 10,000 ppb
Source: "Performance Audit Results for Volatile POHC Measurements," JAPCA, Vol. 38, No. 6, June 1988."
All gas standards are in a balance gas of nitrogen.
14
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Each stack-testing organization uses a slightly different
variation on the basic semi-VOST The sampling plan
should show a schematic of the train actually to be used
and briefly describe the semivolatile collection appa-
ratus, as well as cite the protocol to be followed. Critical
aspects include the train setup and position of the XAD
cartridge. Contamination from grease in the glassware
fittings in the train has caused problems with the subse-
quent analysis. Therefore, most guidance (see, for exam-
ple, Referenced) states that no grease (either
hydrocarbon or silicone) is to be used in the train. This
lack of grease may cause problems with demonstrating a
satisfactory leak check but ensures against gross sample
contamination which can render the samples
unanalyzable.
In recovering the sample from the sampling train and
subsequent analysis, it must be emphasized that all inte-
rior portions of the train prior to and including impingers
that contain cpndensate after the XAD-2 sorbent module
must be considered as part of the semivolatile organics
sample. This includes nozzle and probe rinses, impinger
contents, the filter, the XAD-2, and all glassware rinses. In
addition, it should be noted that the filter from this sample
collection should not be used for the paniculate measure-
ment. Upon heating to constant weight to measure the
paniculate, the filter may lose some or all of the semivo-
latile organic analytes. The contents of the impingers
after the XAD-2 sorbent module should be analyzed for
all POHCs, but is particularly important for very water-
soluble compounds.
3.3.3.4 Metals
When specific metals can be identified as potential emis-
sions, sampling will probably be best addressed by
selecting a specific sampling and analytical approach.
Specific methods which have been developed include
EPA Method 12 for lead, Method 101A for mercury, Meth-
ods 103 and 104 for beryllium, and Method 108 for arse-
nic. In most cases, however, sampling will be required for
multiple metals. For this, the draft metals protocol Meth-
odology for the Determination of Trace Metal Emissions in
Exhaust Gases From Stationary Source Combustion Pro-
cesses (prepared by the EPA, AREAL, Source Methods
Standardization Branch) describes the only system that
has been proposed to collect both the volatile and non-
volatile fraction of the stack gases. This draft protocol will
be incorporated into a methods document under prepa-
ration by EPA, OSW as background for proposed amend-
ments to the RCRA incinerator regulations.9 Sampling for
hexavalent chromium presents several problems. These
problems are the stability of the sample and recovery
efficiencies when separating low level samples. Both oxi-
dizing and reducing materials may affect the stability Of
the samples and produce errors in the determination.
EPA is currently working on a suitable procedure to col-
lect chromium(VI) stack samples. A separate sampling
*rain used only for collection of chromium(VI) is
recommended.
3.3.4 Quench and Scrubber Waters
Samples of quench and scrubber waters (both input and
output) are usually taken by the tap sampling method
(S004) or by dipper (S002). Weighted bottles (S003) can
also be used. The corresponding ASTM and SW-846
methods are listed in Section 3.3.1.
3.3.5 Incinerator Ash (Residue)
The method most commonly used for sampling ash is the
trowel method (S007). The protocols given in the ASTM
Standards or SW-846 methods manual for sampling solid
materials given previously in Section 3.3.1 provide addi-
tional information.
3.3.6 Documentation
The trial burn plan should address documentation of all
sample collection activities. Sample collection times and
conditions must be recorded when the samples are col-
lected. For the VOST and semi-VOST, defined periodic
readings of temperature and flow parameters must be
recorded. Generally, example data recording forms
should be provided in the trial burn plan. Often com-
puters or programmable calculators are used for calcula-
tion of the sampling parameters. These should be
addressed in the plan with sufficient information to docu-
ment how calculations were made.
3.4 Chemical Analysis
The recommended methods for analyzing samples taken
during the trial burn or routine operation of an RCRA
hazardous waste incinerator are found primarily in SW-
846,6 EPA-600/8-84-002,4 40 CFR Part 60, Appendix A,7
and in the ASTM Standards.8 EPA-600/8-84-002 should
be consulted first as it provides cross-references to more
fully documented sources of methods (i.e., SW-846 or
ASTM), These other sources should then be consulted. If
there is a conflict between these documents, SW-846 has
precedence.
The following sections discuss sample shipping, receipt,
and documentation; planning the analysis; general ana-
lytical considerations; analysis of waste feed; analysis of
stack samples; and analysis of other effluent streams.
3.4.1 Sample Shipping, Receipt, Documentation,
and Storage
The trial burn plan must contain provisions for orderly
and welldocumented transfer of the samples from the
incinerator to the laboratory including documentation of
how samples were handled.
The trial burn plan should address:
a. Sample storage requirements on-site and during stor-
age at the labo ratory prior to analysis.
b. Holding times prior to analysis.
15
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c. Sample labeling.
d. Documentation procedures for handling and transfer
of samples.
Sample storage conditions and times should be speci-
fied. Holding times and storage conditions prior to extrac-
tion can be particularly important depending on the type
of sample. Between analysis steps, appropriate storage
conditions must also apply. The holding time and archiv-
ing conditions for samples and extracts after the analysis
also should be specified. If possible, they should be held
long enough to permit reanalysis if requested.
The sample labeling procedures and logging (notebook,
forms, barcode) of the samples should be addressed.
Documentation of sample shipping, receipt, and transfer
must be addressed in the plan. Generally, traceability
forms accompany the samples and are signed and dated
at each event. If formal chain-of-custody is to be used,
additional documentation certifying the unbroken chain
and security of the samples is required.
3.4.2 Planning the Analysis
The analysis must be carefully planned in order to pre-
vent costly mistakes or schedule slippage. The trial burn
plan should address how samples will be transferred to
the appropriate laboratory personnel and how the per-
sonnel will be instructed on the analytical objectives.
Written instructions to the analysts should address the
following: sample numbers, storage location, the analyti-
cal methods to be used, the analysis objective and limit
of detection required if not implicit in the method, analy-
sis sequence, QC requirements (duplicates, spikes,
blanks, etc.), other special instructions, and due date.
The plan should indicate the presence of or have
attached SOPs.
The first step in planning the analysis is to identify the
target analytes. The process for selection of the organic
hazardous constituents to be determined in the waste
feed is described in Section III.B of the EPA-600/8-84-
002* and in Part III, Chapter 13 of SW-846.6 The general
characteristics of the waste feed are determined first by
proximate analysis, then survey analysis, and finally by
directed analysis. Based on these results, a limited num-
ber of organics are selected for recommendation as prin-
cipal organic hazardous constituents (POHCs). This
selection procedure is not discussed in detail in this
report.
One important consideration in selecting the POHCs is to
avoid those which are difficult to analyze. Table 7 shows
a select list of "problem" POHCs, the cause of the prob-
lem, and some possible solutions to the problem.
3.4.3 General Analytical Considerations
3.4.3.7 Glassware Cleaning and Tracking
All glassware used for the analyses must be properly
cleaned. Each laboratory must develop adequate stan-
dard operating procedures for glassware cleaning. Sepa-
rate cleaning procedures are generally required for
organic and inorganic analysis, since different interfer-
ences are of concern.
It is highly advisable to have a glassware tracking system
in place to prevent cross-contamination of glassware.
The analyses described in this document address both
high level (e.g., feed samples at 30% POHC concentra-
tion) and trace analysis (e.g., the same POHC in the
stack gas sample at the nanogram-per-gram level). Thus,
the potential for cross-contamination is great.
A glassware screening system is also advisable to verify
the adequacy of the glassware cleaning.
3.4.3.2 Standards, Reagents, and Solvents
Standards, reagents, and solvents must be of the appro-
priate purity. New lots should be checked for purity. New
standards should also be checked for chemical identity
and their concentration verified.
3.4.3.3 Physical Sample Preparation
Some samples may require homogenization, blending,
aliquoting, or compositing. Basic guidance is given in
Methods P001, P002, and POOS of the EPA-600/8-84-
0024 and in Part III, Chapter 9 of SW-846.6 Specific proce-
dures should be detailed in the trial burn plan.
3.4.4 Analysis of Waste Feed
The waste feed must be sampled and analyzed in
accordance with 40 CFR Parts 270.19, 270.62, and
264.13.7 Specifically, the waste feed must be analyzed for
higher heating value, viscosity (if liquid), and the hazard-
ous organic constituents listed in 40 CFR Part 261,
Appendix VIII.7 Analysis is required for any of the ~ 300
constituents in Appendix VIII, which may be reasonably
expected to be present for waste characterization or for
selected constituents from the list for trial burns. Many
other parameters may be determined to fully characterize
the waste. Various methods and techniques are available
to prepare the field samples for analysis. Table 8 lists the
sample preparation methods described in the EPA-600/
8-84-002. Table 9 lists the sample preparation and intro-
duction techniques described in SW-846.6 Table 10
shows the recommended analytical methods that may be
used to characterize the waste feed.
Physical analyses give information on the physical char-
acteristics and general chemical composition of the
waste including the following:
16
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Table 7. Selected Problem POHCs
Compound
Cause of problem
Possible solution
Acetonitrile
Acetyl chloride
Aflatoxins
Aniline
Benzenearsonic acid
Benzidine
Bis(chloromethyl)ether
2-Butanone peroxide
2-sec-Butyl-4,6-dinitrophenyl
Carbon oxyfluoride
Chloral
Coal tars
Creosote
Cyanogen
Cyanogen bromide
Cyanogen chloride
Cycasin
A/,W-Diethylhydrazine
1,1-Dimethyl.nydrazine
1,2-Dimethylhydrazine
1,4-Dioxane
1,2-Diphenylhydrazine
Diphenylamine
Formaldehyde
Formic acid
Hydrazine
Hydroxydimethylarsine oxide
Iron dextran
Maleic anhydride
Maleic hydrazide
Mustard gas
Nitroglycerin
Phenylmercury acetate
Phosgene
Pyridine
Selenourea
Toluene diisocyanate
Water soluble
Decomposition
High toxicity
Water soluble
Low volatility
Decomposition?
Decomposition
Reactive
Acidic, extracts poorly
Decomposition?
Water soluble
Complex mixture
Complex mixture
Gas
Gas
Gas
Low volatility
Unstable
Unstable
Unstable
Water soluble
Unstable
Basic, extracts poorly
Water soluble
Water soluble
Unstable
Low volatility
High molecular weight
Unstable
Unstable
Highly toxic
Explosive
Low volatility
Highly toxic
Water soluble
Low volatility
Water soluble
Derivatize with HI
Sample with Semi-VOST train
Derivatize to sample
DerivatizewithHI
GPC
Derivatize with HI
Special HPLC column
Heating value
Viscosity (if liquid)
Ash content
Total organic chlorine
« Moisture content
Solid content
Elemental composition (optional)
The heating value and viscosity (for liquids) are required
by RCRA. The ash content is generally required as an
indicator of inorganic loading and other factors which
may affect the amount of paniculate generated. Total
organic chloride is needed to determine the HCI removal
efficiency. The other analyses are not required but may
be of value to the incinerator operator in characterizing
the waste feed and in operating the incinerator.
A method for analysis of total organic chloride in waste is
under development by EPA, AREAL. In certain situations
measurement of total chloride in the waste may be substi-
tuted for total organic chloride. The Source Methods
Standardization Branch, AREAL or OSW, should be con-
sulted on this topic.
3.4.4.7 Analysis of Waste Feed for POHCs
A major objective of the trial burn is to measure the ORE
of selected POHCs. To do this, the sampling and analysis
program must measure both the input and output rates of
the POHCs. Only those organics selected for measure-
ment (i.e., the POHCs) need to be measured in the waste
feed during a trial burn.
The RCRA hazardous compounds are given in 40 CFR
Part 261, Appendix VIII.7 The methods for analyzing vari-
ous matrices for the POHCs are given in EPA-600/8-84-
0024 as Methods A101 to A190 and in SW-8466 as
Methods 8010 and 8310. Table 11 lists the methods given
in EPA-600/8-84-002, and Table 12 lists the methods
given in SW-846.
Specific methods for the Appendix VIII compounds
(including inorganic compounds) given in EPA-600/8-84-
002 and SW-846 are shown in the appendix.
3.4.4.2 Analysis for Inorganics
Inorganic analysis is not addressed in detail in this man-
ual. The applicable analytical methods are cited for com-
pleteness in Table 13. For further information, the reader
is referred to EPA-600/8-84-0024 and SW-846.6
17
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3.4.5 Analysis of Stack Samples
Stack samples are analyzed for POHCs to determine
ORE, hydrogen chloride, and participate as required in 40
CFR 264.34S.7 In addition, other analyses may be
required for specific demonstrations. The recommended
methods for analysis of stack samples are listed in Table
14. This section describes the methods generally used
and discusses some potential problems and solutions.
3.4.5.1 Hydrogen Chloride Analysis
The hydrogen chloride in the stack gas must be mea-
sured to demonstrate an emission rate of less than 4 Ib/hr
or 99% removal before discharge to the atmosphere (40
CFR 264.345). (It may be possible to use data from
analysis of chlorine in the waste to determine compliance
with an uncontrolled HCI emission rate or to determine
control device inlet HCI rates for calculation of efficiency.)
A number of analytical methods have been employed to
analyze the impinger catch for HCI. These methods
include the automated ferricyanide colorimetric Methods
9250 and 9251 and the titrimetric Method 9252 from.SW-
846, ion chromatography ASTM Method D-4327-84 and
Method 300.0 from Chemical Analysis of Water and
Wastes. Ion chromatography is the preferred method.
Because of the greater detail provided, the ASTM
Table 8. Sample Preparation Methods Given in
EPA-600/8-84-002
Sample preparation method
Method
number
Representative aliquots (composites) of field samples
Liquids (aqueous and organic) P001
Sludges POQ2
Solids " P003
Surrogate addition to sample aliquots for organic analysis
Volatile organics P011
Basic extractable organics P012
Acidic extractabla organics P013
Neutral extractable organics P014
Extraction of organic compounds
Aqueous liquids * P021
SemivoIatHes P02la
Vbtatiles P02ib
Sludges (including gels and slurries) P022
Somivolatiles P022a
Volatiles P022b
Organic liquids P023
SolWs . P024
Semh/olatiles by homogenization P024a
Semivolatiles by Soxhiet extraction P024b
Volatiles P024c
Drying and concentrating solvent extracts P031
Digestion procedures for metals P032
Sample cleanup procedures
Ftorfsif column chromatography P041
BioBeadsSX-3 R042
Silica gel chromatography P043
Alumina column chromatography P044
Liquid/liquid extraction P045
Source: Arthur D. Little, Inc., "Sampling and Analysis Methods for
Hazardous Waste Combustion," EPA-600/8-84-002,
PB84-155845; February 1984.4
D-4327-84 procedure is recommended over Method
300.0. The other methods mentioned above may be suit-
able in some circumstances. The draft EPA method
referred to in Section 3.3.3.1 specifies ion chromatogra-
phy and provides details.
3.4.5.2 Particulate Analysis
Particulate must be measured in the stack gas to demon-
strate a maximum particulate emission concentration of
no greater than 180 mg/Nm3, corrected to 7% O2 (50%
excess air) (40 CFR 264.345). The particulate is mea-
sured gravimetrically according to the procedures estab-
lished in EPA Reference Method 5 (40 CFR 60).
Two procedures are available. In the first procedure, the
filter is desiccated and then weighed to a constant
weight. In the alternate procedure, the filter is oven-dried
for 2 to 3 h at 105°C (220°F) and cooled in a desiccator
Table 9. Sample Preparation and Introduction Techniques
Given in SW-846'
Sample preparation and introduction techniques
Method
number
Sample workup techniques '
Inorganics
Acid digestion of waters for total recoverable 3005
or dissolved metals for analysis by FLAA" or ICPC
Acid digestion of aqueous samples and extracts 3010
for total metals analysis by FLAA or ICP
Acid digestion for aqueous samples and extracts 3020
for total metals analysis by GFAA"
Dissolution procedure for oils, greases, or waxes 3040
Acid digestion of sediments, sludges, or waxes 3050
Organics
Organic extraction and sample preparation 3500
Separatory funnel liquid-liquid extraction 3510
Continuous liquid-liquid extraction 3520
Soxhiet extraction 3540
Sonication extraction 3550
Waste dilution 3580
Sample introduction techniques
Purge and trap method 5030
Protocol for analysis of sorbent cartridcjes from 5040
VOST"
Sample cleanup
Cleanup 3600
Alumina column cleanup 3610
Alumina column cleanup and separation of 3611
petroleum wastes
Florisil column cleanup 3620
Silica gel cleanup 3630
Gel-permeation cleanup . 3640
Acid-base partition cleanup , 3650
Sulfur cleanup 3660
Source: U.S. Environmental Protection Agency/Office of Solid
Waste, Washington, DC, "Test Methods for Evaluating Solid
Waste: Physical/Chemical Methods," SW-846, Third
Edition, November 1986.6
" FLAA = flame atomic absorption spectroscopy.
c ICP = inductively coupled plasma spectroscopy.
0 GFAA = graphite furnace atomic absorption spectroscopy.
VOST = volatile organic sampling train.
18
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before the filter is weighed to a constant weight. Note that
the filter used for participate analysis should not also be
used as part of the semivolatile organic analysis, since
the drying-to-constant-weight procedure may lose some
of the semivolatile organics.
The probe rinse is checked for any leakage during trans-
port. The liquid is measured volumetrically or grayimetri-
cally to the nearest ±1 ml_ (±1 g). The contents are
transferred to a tared 250-mL beaker. The probe rinse is
evaporated to dryness at ambient temperature and pres-
sure. The beaker is weighed to a constant weight, and the
results are reported to the nearest 0.1 mg.
Table 10. Analytical Methods for Characteristics of RCRA
Hazardous Waste Feed Samples
Characteristics of hazardous wastes
Analysis
method
Source"
Ignitability: Pensky-Martens closed-cup
method
Ignitability: Setaflash closed-cup method
Corrosivity toward steel
pH electrometric measurement
Reactivity
Extraction procedure "(EP) toxicity
Appendix VIII hazardous constituents
Ultimate analysis (elemental composition)
"Viscosity '" '
'Higher heating value
Chlorides
Ash: Sample drying and ignition
Ash: Thermogravirhetric analysis
Total organic carbon (TOC)
Total organic halides (TOX)b
Total and amenable cyanide
Sulfides
1010
D-93-80
C001
1020
D-3278-78
C001
1110
C002
9040
C002
8.3
COOS
1310
C004
See Appendix
A003
A005 -
D-445-79
A006
D-2015-77
D-3286-77
D-808-81
A001a,b
D-1888-78
A002
D-1888-78
9060
A004
9020
A004
9010
9030
SW-846
ASTM
ADL
SW-846
ASTM
ADL
SW-846
ADL
SW-846
ADL
SW-846
ADL
SW-846
ADL
ADL
ADL
ASTM
ADL
ASTM
ASTM
ASTM
ADL
ASTM
ADL
ASTM
SW-846
ADL
SW-846
ADL
SW-846
SW-846
Note: * Required under RCRA,
Sources:
ADL = Arthur D. Little, Inc., "Sampling and Analysis Methods for
Hazardous Waste Combustion," EPA-600/8-84-002, PB84-155845,
February 1984.'
SW-846 = U.S. Environmental Protection Agency/Office of Solid
Waste, Washington, DC, "Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods," SW-846, Third Edition, November
1986.6
ASTM = American Society for Testing and Materials, "Annual Book
of ASTM Standards," Philadelphia, Pennsylvania.8
0 The methods listed were developed for wastewater and are not
applicable to organic waste. If this analysis is necessary, the Source
Methods Standardization Branch, AREAL, EPA or OSW, EPA
should be consulted.
Weights are reported separately as filter weight and
probe rinse.
3.4.5.3 Oxygen and Carbon Dioxide
Oxygen and carbon dioxide are collected in sample bags
(e.g., Mylar, Tedlar) and analyzed by EPA Reference
Method 3 (see Table 5). The method uses the Orsat
apparatus to measure the volumetric change in liquid
volume with selective absorption of oxygen or CO2. Sam-
ples must be analyzed within 3 h, so the analysis is
almost always conducted on-site.
Integrated bag samples, if required, must be collected
over the entire test period.
3.4.5.4 Analysis for POHCs
The POHCs are divided into two general groups for anal-
ysis volatile and semivolatile organics. Methods for
these groups are discussed below. Analysis for metals
may also be required and is presented briefly below.
Volatile POHCs The volatile POHCs are collected
either on the VOST or in Tedlar gas bags (S011) for the
high concentration volatiles which saturate the
Table 11. Analytical Methods for Principal Organic Hazardous
Constituents (POHCs) Given in EPA-600/8-84-002
Analysis
Description of analysis methods method
Volatiles A101
Purging procedure for the analysis of aqueous liquids A101 a
Purging procedure for the analysis of sludges A101b
Purging procedure for the analysis of solids A101c
Extractables A121
HPLC/UV generalized procedure A122
HPLC/UV generalized procedure . ' A123
Aldehydes derivatization procedures A131
Aldehydes HPLC analysis A132
Carboxylic acids , A133
Alcohols A134
Phosphine A136
Fluorine A137
Gases cyanogens and phosgene A138
Gases mustards A139
Gases A141
Acid chlorides A144
Aflatoxins A145
Brucine A148
Citrus red No. 2 A149
Cycasin A150
Ethylene oxide A156
2-Fluoroacetamide A157
Lasiocarpine , A160
Phenacetin A174
Strychnine A180
Oximes A183
Tris(1-aziridinyl)phosphinesulfide A190
Source: Arthur D. Little, Inc., "Sampling and Analysis Methods for
Hazardous Waste Combustion," EPA-600/8-84-002,
PB84-155845, February 1984.4
19
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VOST, as described in Section 3.3.3.2. The sorbent
tubes from the VOST are analyzed by thermal
desorption/gas chromatography/mass spectrometry as
described in the VOST Method 5040 in SW-846.6 Several
variations on the basic thermal desorption unit design
are available from vendors or may be constructed by the
analytical laboratory. The desorption unit must be
leakand contamination-free, as demonstrated by QC
sample performance. The laboratory must also have the
capability and experience to generate reliable standards
for quantitation.
VOST analyses require not only adequate facilities, but
also experience and good technique. A major potential
problem is the presence of background compounds in
the samples as evidenced by the blank samples. Back-
ground contamination can generally be traced to prob-
lems with the trap cleanup, sample collection, or sample
handling (see Section 3.3.3.3). In addition, care must be
taken that the analysis step does not introduce contami-
nation. Cross contamination from previous high-level
samples can be a problem. Contamination from ambient
air can also be a problem.
The VOST method (5040 in SW-8466) indicates that
VOST is valid for compounds with a boiling point of less
than 100°C (and generally higher than 30°C) and should
be validated prior to use outside this range. There is
Table 12. Analytical Methods for Principal Organic Hazardous
Constituents (POHCs) Given in SW-846
Description of analytical methods
Analysis
method
Gas chromatographlc methods (GC)
Hatogenated volatile organics 8010
Nonhalogenated volatile organics 8015
Aromatic volatile organics , 8020
Acrolein, acrylonitrile, acetbnitrile 8030
Phenols 8040
Phthalate esters 8060
Organochtorine pesticides and PCBs1 8080
Nilroaromatlcs and cyclic ketones 8090
Polynuclear aromatic hydrocarbons 8100
Chlorinated hydrocarbonsd 8120
Organophosphorus pesticides 8140
Chlorinated herbicides 8150
Gas chromatographlc/mass spectroscopy methods (GC/MS)
GC/MS method for volatile organics 8240
GC/MS method for semivolatile organics:
Packed column technique 8250
Capillary column technique 8270
GC/MS method for PCDD/PCDP 8280
H/p/i performance liquid chromatography (HPLC)
HPLC polynuclear aromatic hydrocarbons 8310
Source: US. Environmental Protection Agency/Office of Solid Waste,
Washington, DC, "Test Methods for Evaluating Solid Waste:
PhysicalfChemical Methods," SW-846, Third Edition,
November 1986.«
PCBs = polychforinated biphenyls
PCDD = polychlorinated dibenzo-p-dioxins
PCDF = polychlorinated dibenzofurans
occasionally a need to consider use of VOST for com-
pounds with boiling points in the 100° to 130° range. A
compound with a boiling point in this range may be diffi-
cult to purge from the VOST trap. The validity of the
method for these POHCs should be determined prior to
testing; this can be done by using previous test data or by
validating the method using QA samples. For example,
the VOST protocol provides a QA procedure whereby the
sample traps are spiked with the compound of interest
and analyzed to determine percent sample recovery.
One operational problem with VOST is sample overload
during the analysis. The objective of the VOST analysis is
to demonstrate a ORE of 99.99% or greater. The amount
of a POHC collected on the VOST is dependent on both
the ORE and the amount fed into the incinerator. The
amount of POHC fed should be scaled to yield the POHC
at a concentration near the middle of the GC/MS range,
assuming 99.99% ORE. Thus very low quantities from
the VOST trap indicate far greater than the required ORE,
and very high quantities indicate far less than the
required ORE. High VOST analysis results may be above
the cutoff for the ORE requirement. Depending on the
data-reporting requirements, precise quantitation of high
values may not be necessary if the 99.99% ORE require-
ment is not met. In this case the VOST sample volume
and the calibration range of the analysis can be scaled to
demonstrate the 99.99% ORE with less concern about
quantitation of values much greater or lower than the
regulatory target. The best approach for most trial burns
is to scale the POHC feed rate to match the needed
collection on the VOST. If this is not possible, use a
second sampling method (i.e., bag sample) as a backup
in case the VOST samples saturate the GC/MS.
An option listed in EPA-600/8-84-0024 by which a sample
of stack gas is collected in a Tedlar bag (Method S011)
presents several problems with respect to the short hold-
ing times of these samples, as discussed in Sec-
tion 3.3.2.3. If Tedlar bag samples are used to quantitate
high-level samples, a known volume of gas is pulled
through a clean VOST trap. The gas volume to be col-
lected on the trap is determined from an estimation of the
concentration of the POHC from the saturated peak
obtained in the analysis of the first VOST trap. The trial
burn plan must include appropriate QA measures to dem-
onstrate that field samples are valid for the holding times
and gas matrix actually encountered from the test.
Semivolatile POHCs The semivolatile POHCs are
sampled using a semi-VOST with an XAD-2 sorbent
module, as described in Section 3.3.3.3. Nonvolatile
POHCs (boiling points above 300 °C) are also collected
by the semiVOST sampling train.
The semivolatile and nonvolatile POHCs are generally
analyzed by extraction followed by GC/MS analysis. The
appropriate standard methods are cited in Tables 8,9,11,
and 12, and Appendix A. Tables 8 and 9 list the sample
preparation and introduction techniques. Tables 11 and
20
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Table 13. Analytical Methods for Inorganics
ADL SW-846
method Analysis method Analysis
Inorganics number method* number method*
Aluminum
Antimony
Arsenic
Barium
Beryllium
Boron
Cadmium
Calcium
Cobalt
Chromium
Hexavalent chromium1
Copper
Iron
Lead
!
Magnesium
Manganese
Mercury
Molybdenum
Nickel
Osmium
Phosphorus
Potassium
Selenium
Silicon
Silver
Sodium
.
Strontium
A021
A221
A222
A021
A223
A021
A224
A021
A021
A225
A021
A021
A021
A226
_
AQ21
A021
A021
A227
A021
A021
A228
A021
A021
A229
A021
A230
A021
A021
A231
A021
A021
A232
A021
A021
A233
ICAP
AAS, DAM
AAS, GFM
AAS, GFM
AAS, GH
ICAP
AAS, DAM
AAS, GFM
ICAP
AAS, DAM
AAS, GFM
ICAP
ICAP
AAS, DAM
AAS, GFM
ICAP
ICAP
ICAP
AAS, DAM
AAS, GFM
ICAP
ICAP
ICAP
AAS, DAM
AAS, GFM
ICAP
ICAP
'CV.AAS
ICAP
ICAP
AAS, DAM
AAS, GFM
ICAP
AAS, DAM
AAS, GFM
ICAP
ICAP
AAS, GFM
AAS, GH
ICAP
ICAP
AAS, DAM
AAS, GFM
ICAP
ICAP
AAS, DAM
AAS, GFM
6010
7020
6010
7040
7041
6010
7060
7061
6010
7080
6010
. 7090
7091
6010
6010
7130
7131
6010
7140
6010
7200
7201
6010
7190
7191
7195
7196
7197
7198
6010
7210
6010
7380
6010
7420
7421
6010
. 7450
6010
7460
7470
7471
6010
7480
7481
6010
7520
7550
V1U .
6010
7610
6010
7740
7741
6010
6010
7760
7761
6010
7770
ICAP
AAS, DAM
ICAP
AAS, DAM
AAS, GFM
ICAP
AAS, DAM
AAS.GH
ICAP
AAS, DAM
ICAP
AAS, DAM
AAS, GFM
ICAP
ICAP
AAS, DAM
AAS, GFM
ICAP
AAS, DAM
ICAP
AAS, DAM
AAS, GFM
ICAP
AAS, DAM
AAS, GFM
COPRTN
C
C/E
DPP
ICAP
AAS, DAM
ICAP
AAS, DAM
ICAP
AAS, DAM
AAS, GFM
ICAP
AAS, DAM
ICAP
AAS, DAM
CV.AAS.L
CV,AAS,S
ICAP
AAS, DAM
AAS, GFM
ICAP
AAS, DAM
AAS, DAM
_
ICAP
AAS, DAM
ICAP
AAS, GFM
AAS.GH
ICAP
ICAP
AAS, DAM
AAS, GFM
ICAP
AAS, DAM
Table 13. (continued)
ADL SW-846
method Analysis method Analysis
Inorganics number method* number method*
Thallium
Thorium
Titanium
Vanadium
Zinc
A021
A234
A021
A021
A021
A235
A021
ICAP
AAS, DAM
AAS, GFM
ICAP
ICAP
ICAP
AAS, DAM
AAS, GFM
ICAP
6010
7840
7841
6010
7910
7911
6010
ICAP
AAS, DAM
AAS, GFM
' , '
ICAP
AAS, DAM
AAS, GFM
ICAP
Zirconium
Anions
Total cyanides
Phosphides
Sulfides
A021
A251
A252
ICAP
1C
TC
A253 GC/FPD
9030
7950 AAS, DAM
9010
9012
* ICAP = inductively coupled argon plasma emission
spectroscopy
AAS, DAM = atomic absorption spectroscopy, direct aspiration
method
AAS, GFM = atomic absorption spectroscopy, graphite furnace
method
AAS.GH = atomic absorption spectroscopy, gaseous hydride
method
COPRTN = coprecipitation method
CV, AAS = cold vapor/atomic absorption spectroscopy
CV, AAS, L = cold vapor/atomic absorption spectroscopy, for
liquids.
CV, AAS, S = cold vapor/atomic absorption spectroscopy, for
solids
C = colorimetric method
C/E = chelation/extraction method
T = titration method
1C = ion chromatography .
GC/FPD = gas chromatography/flame photometric detector
DPP = differential pulse polarography
Sources: Arthur D. Little, Inc., "Sampling and Analysis Methods for
Hazardous Waste Combustion," EPA-600/8-84-002,
PB84-155845, February 1984."
US. Environmental Protection Agency/Office of Solid
Waste, Washington, DC, "Test Methods for Evaluating Solid
Waste: Physical/Chemical Methods," SW-846, Third
Edition, November 1986.6
The methods listed for hexavalent chromium were developed for
water samples.
12 list applicable instrumental analysis methods. Appen-
dix A lists all of the analysis methods for the Appen-
dix VIII hazardous constituents by compound or element
in alphabetical order.
Each semi-VOST sample returns to the laboratory in
several fractions which must be treated and ultimately
combined to yield a full sample. Typically the fractions are
(1) filter, (2) sorbent trap, (3) front-half organic rinse, (4)
back-half organic rinse, and (5) cqndensate from and
rinses of impingers. The fractions are spiked with surro-
gates, extracted, combined, cleaned up, and then
analyzed.
Surrogate compounds are generally isotopically labeled
(e.g., deuterated) analogs of the POHCs or similar com-
21
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pounds not found in the waste feed which can be spiked
into the samples to monitor recovery of the native
POHCs. Since several fractions must be extracted using
different techniques, surrogates may be split into groups
to monitor recovery of each extraction.
Table 14. Analytical Methods for Stack Gas Samples
Sample
Analysis
parameter Analysis method
MS train
Filter, probe rinse
Water impingers
Caustic impinger
Multiple metals train
Seml-VOST
Filter, probe rinse
XAD-2
Condensate
VOST
Mylar gas bag
Tedlargasbag
Particulate
CI-(HCI)
CI-(HCI)
Metals
SV-POHCs
SV-POHCs
SV-POHCs
V-POHCs
C02,O2
V-POHCs
EPA Method 5"
Ion chromatography
or EPA 352.2=
Ion chromatography
or EPA 352.2=
See Table 13
See Appendix A
GC/MS
GC/MSperSW-846,
Method 5040
EPA Method 3b
Transfer to Tenax
trap and GC/MS
perSW-846,
Method 5040
1 SV-POHCs = semivolatile and nonvolatile principal organic
hazardous constituents
V-POHCs = volatile principal organic hazardous constituents
Source: 40 CFR Part 60, Appendix A.7
«Reference:" Methods for Chemical Analysis of Water and Wastes,"
EPA-600/4-79-020, March 1979."
The filter and sorbent traps are generally Soxhlet-
extracted with dichloromethane (Method 3540), ben-
zene, hexane, or other organic solvent. The organic rinse
fractions are combined with the filter and sorbent trap
extracts. The aqueous fractions are extracted using
liquid-liquid partition in a separatory funnel (e.g., EPA
Method 3510 using dichloromethane) or by continuous
liquid-liquid extraction (e.g., EPA Method 3520 with dich-
loromethane). A second extraction of aqueous fractions
with methyl-t-butyl ether may be necessary when the
POHC is a water-soluble compound (e.g., pyridine).
The sample extracts are then evaporatively concentrated
to the desired volume. Kuderna-Danish evaporation and
other techniques are described in the appropriate SW-
846 extraction methods.
A variety of adsorbent column and other cleanup meth-
ods are available for cleanup of organic extracts prior to
analysis. Several are listed in SW-846 (Section 4.2.2) and
EPA-600/8-84-002 (P041-P045). The selection of the
sample cleanup technique is dependent on the type and
concentration of the interferences. Prior experience with
the matrix or screening of the samples can help charac-
terize the interferences. For many trial burns with rela-
tively clean stack gases, no cleanup may be required. If
the POHC levels are low enough to require special mass
spectral techniques, such as selected ion monitoring,
cleanup is more likely to be required.
Implementation of the extraction, concentration, and
cleanup methods requires not only the detailed written
methods and appropriate reagents and materials, but
also qualified personnel. Effective execution of these
methods, as measured by surrogate compound recover-
ies and the amount of interferences, comes only after
extensive training in general trace organic laboratory
methods and experience in the specific methods.
Although not specifically required, most laboratories
choose to analyze the extracts for POHCs by GC/MS.
The ability of this technique to quantitate the POHCs
reliably makes it cost-effective relative to the additional
laboratory cleanup required for GC with other detectors.
In addition, there is a much greater chance of obtaining
higher than true values due to interferences with other
detectors, which can result in a reported ORE that is
lower than actual.
The GC/MS data must be interpreted both qualitatively
and quantitatively. Methods 8240,8250,8270, and other
applicable methods give general guidance on data inter-
pretation. Qualitative data interpretation entails matching
the retention time and spectral characteristics of the
sample with the standards. The QA plan must specify
criteria on the retention time and spectral characteristics
(e.g., presence of ions, ion intensity ratios, etc.). The
POHCs are quantitated by the internal standard method.
Specifically, the area of the unknown is ratioed to that of
the internal standard, multiplied by the amount of the
internal standard, and also multiplied by the response
factor for that compound relative to the internal standard.
The details of the quantitation must be specified in the
trial burn plan including number and levels of standards,
analysis sequence, blanks, and repeat injections. In addi-
tion, the trial burn plan should address contingencies for
interferences, high level samples, samples outside the
standard curve, and other anticipated problems.
For many high-efficiency incinerators, the POHCs in the
stack gas will be below the lower limit of quantitation
(LOQ) or even below the limit of detection (LOD). The trial
burn plan should give the criteria for LOQ and LOD and
should also state how samples in these ranges will be
reported. Reporting of low-level numbers can affect the
calculation of the ORE and can also cause confusion in
the trial burn report review process.
Data interpretation not only requires qualified and experi-
enced personnel, but also time. Sufficient time must be
allowed in the analysis and reporting schedule for the
data reduction.
22
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Metals. Analysis of stack gas samples for metals may
be conducted during some trial burns and the applicable
methods are listed in Table 13. The draft protocol for the
multiple metals train discussed in Section 3.3.3.4 con-
tains additional information on analysis. It employs a
hydrofluoric acid/nitric acid digestion in microwave
bombs for the probe rinse and filter samples resulting
from stack sampling. It also offers an option of either a
hydrofluoric acid/nitric acid digestion in microwave
bombs or a nitric acid/hydrogen peroxide digestion on a
hot plate for the impinger contents except the potassium
permanganate impinger, which is analyzed for mercury
only. An aliquot of the other (combined) impinger con-
tents is also reserved for mercury analysis.
3.4.6 Analysis of Other Effluent Streams
In addition to the stack samples, samples from the other
effluent streams must be analyzed. Although not calcu-
lated in the ORE, a quantitative analysis of the scrubber
water, ash residues, and other residues is required by 40
CFR, Part 270.62 for the purpose of estimating the fate of
POHCs. This section addresses analysis of quench and
scrubber water samples and ash samples. Analysis
methods for other effluent streams should be adaptable
from similar waste matrices, as described in Sec-
tion 3.4.4.
General characterization (e.g., proximate analysis) and
inorganic analysis of the water and ash samples can be
conducted using the same methods used for waste feed
samples, as discussed in Section 3.4.4 and summarized
in Table 10.
3.4.6.1 Quench and Scrubber Water
For semivolatile analysis, water samples are extracted
using liquidliquid partition in a separatory funnel (Method
3510 in SW-846 using dichloromethane) or continuous
liquid-liquid extraction (Method 3520 in SW-846 using
dichloromethane). The sample extracts are then evapo-
ratively concentrated to the desired volume. Kuderna-
Danish evaporation and other techniques are described
in the appropriate SW-846 extraction methods. If needed,
a variety of adsorbent column and other cleanups are
available for cleanup of organic extracts prior to analysis.
Several are listed in SW-846 (Section 4.2.2) and EPA-
600/8-84-002 (P041-P045). For many trial burns with rela-
tively clean stack gas and thus clean scrubber water, no
cleanup will be required. Most laboratories choose to
analyze the quench and scrubber water extracts by GC/
MS. Methods 8250, 8270, and other applicable methods
give general guidance on analysis of semivolatiles and
data interpretation. For volatile POHCs, the samples are
prepared for and analyzed by purge and trap using the A.
D. Little A101 series methods or the SW-846 Methods
5030 (preparation) and 8240 (analysis). Section 3.4.5.4.2
addresses the GC/MS analysis in more detail.
3.4.6.2 Ash Samples
To determine semivolatile POHCs in ash samples, the
samples are Soxhletextracted using dichloromethane
(Method 3540 in SW-846), benzene, hexane, or other
organic solvent. The sample extracts are then evapora-
tively concentrated to the desired volume, cleaned up,
and analyzed by GC/MS as described for the water sam-
ples in the preceding section. To determine volatile
POHCs in ash samples, the samples are prepared in a
tetraglyme dispersion (Method 5030 in SW-846, A101C
in EPA-600/8-84-002) and then analyzed by purge and
trap.
23
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Section 4
Quality Assurance/Quality Control
4.1 Data Quality Objectives
The subject of data quality objectives (DQOs) has
recently been addressed by the Quality Assurance Man-
agement Staff (QAMS) of EPA in a publication entitled
Development of Data Quality Objectives: Description of
Stages I and /A16 This document describes an approach
to designing environmental data collection programs
based on the development of DQOs which is intended to
define the quality of the data needed to achieve an
acceptable level of confidence and provide adequate
information to make regulatory decisions and recommen-
dations. The DQO process provides a logical, objective,
and quantitative framework for finding an appropriate
balance between the time and resources that will be
used to collect data and the quality of the data needed to
make the decision.
Data quality objectives are statements of the level of
uncertainty that a decision maker is willing to accept in
results derived from environmental data, when the
results are going to be used in a regulatory or program-
matic decision. These quantitative DQOs must be
accompanied by clear statements of:
The decision to be made.
Why environmental data are needed and how they will
be used.
Time and resource constraints on data collection.
* Descriptions of the environmental data to be
collected.
Specifications regarding the domain of the decision.
The calculations, statistical or otherwise, that will be
performed on the data in order to. arrive at a result.
Once DQOs have been developed and a design for the
data collection activity expected to achieve these objec-
tives has been selected, DQOs are used to define quality
assurance (QA) and quality control (QC) programs that
are specifically tailored to the data collection program
being initiated. A QA Project Plan is prepared document-
ing all of the activities needed to ensure that the data
collection program will produce environmental data, of
the type and quality required to satisfy the DQOs. With-
out first developing DQOs, a QA program can only be
used to document the quality of data obtained, rather
than to ensure that the quality of data obtained will be
sufficient to support an Agency decision. This approach
to DQOs is recommended when planning QA for an
RCRA trial burn.
4.2 General Discussion of QA Project Plan
The quality assurance/quality control (QA/QC) proce-
dures for the process monitoring, sampling, and analyti-
cal activities for a trial burn and the continuing operation
of a hazardous waste incinerator must be included in a
quality assurance (QA) project plan which accompanies
the permit application. The QA plan should be based on
the guidelines document issued by the Office of Monitor-
ing Systems and Quality Assurance of EPA entitled
Interim Guidelines and Specifications for Preparing Qual-
ity Assurance Project P/ans.1? The document has identi-
fied 16 essential elements of a QA plan, which are shown
in Table 15.
Table 15. Essential Elements of a QA Project Plan
1. Title Page
2. Table of Contents
3. Project Description
4. Project Organization and Responsibility
5. QA Objectives
6. Sampling Procedures
7. Sample Custody
8. Calibration Procedures and Frequency
9. Analytical Procedures
10. Data Reduction, Validation, and Reporting
11. Internal Quality Control Checks
12. Performance and Systems Audits
13. Preventative Maintenance
14. Specific Routine Procedures Used to Assess Data Precision,
Accuracy, and Completeness
15. Corrective Action
16. Quality Assurance Reports to Management
Source: U.S. Environmental Protection Agency/Office of Monitoring
Systems and Quality Assurance, Office of Research and
Development, Washington, D.C., "Interim Guidelines and
Specifications for Preparing Quality Assurance Project -
Plans," QAMS-005/80 (December 29,1980)."
25
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A QA plan prepared for a trial burn must contain specific
QA/QC procedures for the process monitoring, sampling,
and analytical activities identified in the trial burn plan
and permit application. The plan should contain suffic-
ient detail to allow the permit writer to assess the ade-
quacy of the QA/QC procedures that will be used.
The discussion that follows first presents a general dis-
cussion of the 16 elements required in a QA plan and
then discusses specific guidance for assessing precision
and accuracy for individual measurement methods.
4.2.1 Title Page
The title page of the QA plan must be signed by approv-
ing personnel. The plan must be approved by the project
leaders immediate supervisor and the quality assurance
manager (QAM). If the QA plan is prepared by a subcon-
tractor to the permit applicant, the title page should also
contain the approving signatures of the subcontractor's
program manager and QAM.
4.2.2 Table of Contents
The table of contents should list the introduction, the 16
essential elements of the QA plan, and any appendices
attached to the plan (such as standard operating proce-
dures, etc.).
4.2.3 Project Description
The project description is presented in detail in the per-
mit application. In the QA plan, a brief summary of the
project description should be provided and reference to
the applicable section(s) of the permit application should
be made. The summary should, however, provide suffic-
ient detail so that the reviewer of the QA plan can under-
stand the important elements of the project plan.
4.2.4 Project Organization and Responsibility
The project organization responsible for all QA/QC activ-
ities should be provided in an organization chart that
gives the names, titles, and line authority of the individ-
uals. The resumes and QA/QC responsibilities for each
individual in the organization should be provided. This
organization should include the following:
Project leader
Quality assurance manager (QAM)
Field sampling task leader
Field sampling quality control coordinator
Analytical task leader
Analytical quality control coordinator
Quality control and data manager
Data analysis task leader
4.2.5 QA Objectives
The primary QA objective for any project is to ensure that
the measurement data collected are precise, accurate,
complete, and representative. This section of the QA plan
should give specific precision, accuracy, and complete-
ness objectives for each process measurement and anal-
ysis performance. Guidance for precision, accuracy, and
completeness objectives for specific measurement
parameters is given in Section 4.3.
The terms precision, accuracy, completeness, and repre-
sentativeness may be defined as follows:
Precision is the degree of agreement between
repeated measurements of one property using the
same method or technique and is usually expressed
as a range percent (R%) for a small number of data
points (2 < n < 8) or as percent relative standard
deviation (%RSD) for a large (n > 8) number of data
points.
Accuracy is the degree of agreement of a measure-
ment (or average of measurements of the same thing),
X, with an accepted reference or true value, T, usually
expressed as percent accuracy (%A) defined as X/T
(X100).
Completeness is a measure of the amount of valid data
obtained from a measurement system compared to
the amount of data collected that was expected, usu-
ally expressed as a percent. |
Representativeness expresses the degree to which
measurement data and samples precisely, accurately,
and completely characterize the process conditions.
4.2.6 Sampling Procedures
The sampling procedures to be used in the trial burn and
continuing operation of the incinerator should be speci-
fied in the trial burn plan and permit application. Sam-
pling procedures should include the sampling methods,
sampling locations, sampling frequencies, sampling
equipment, and datarecording methods. All forms for
recording sampling data should be given.
The QA plan should present any details necessary to
describe the sampling procedures that are not given in
the trial burn plan and permit application. Particular
attention should be given to any anticipated deviations
from referenced sampling methods.
4.2.7 Sample Custody
Two procedures can be used to document sample cus-
tody for a trial burn: traceability and chain-of-custody.
Traceability procedures are acceptable to EPA and
should be used unless litigation is anticipated, in which
.case the applicant may select the more rigorous chain-of-
custody procedures.
The QA plan should describe all of the elements of sam-
ple traceability including sample labeling, preservation,
packing, shipping, and laboratory receiving and storage
procedures. All documentation and record-keeping forms
such as field sampling traceability forms, field logbook,
sample analysis request sheet, laboratory traceability
forms, and laboratory logbook should be described. Stor-
26
-------
age of samples after analysis must also be addressed.
If the chain-of-custody procedure will be used, then a
complete description of the procedure must be given in
the QA plan. Chain-of-custody procedures acceptable to
EPA are fully described in SW-846, Section 1.3.6
4.2.8 Calibration Procedures and Frequency
The calibration procedures for all monitoring and sam-
pling equipment to be calibrated should be specifically
defined. For each piece of equipment, the calibration
technique, reference standard(s), acceptance limits, and
frequency of calibration should be specified.
Calibration of analytical instruments is usually specified
in the reference methods. If the analytical methods do not
specify calibration procedures or deviations from the
methods are anticipated, the calibration procedures must
be fully described. The calibration standards, calibration
curves, average response factors, and/or relative
response factors to be used for each instrument and
analysis should be specified. The methods for recording
and storing calibration data should be given.
4.2.9 Analytical Procedures
The analytical procedures to be used to analyze samples
collected should be specified in the trial burn plan and
permit application. Analytical procedures should include
the analytical methods, instrumentation and equipment,
and data-recording methods. All forms to be used for
recording analytical data should be given.
The QA plan should provide any details necessary to
describe the analytical procedures that are not given in
the trial burn plan and permit application. Particular
attention should be given to any anticipated deviations
from referenced procedures and methods.
4.2.10 Data Reduction, Validation, and Reporting
All procedures for the reduction of monitoring, sampling,
and analytical data collected should be specified. Equa-
tions, calculations, and conversion factors should be
given for determining specific results to be reported, such
as stack emissions, waste feed concentrations, etc.
Methods used to obtain and reduce analytical data, such
as method internal standards, recovery internal stan-
dards, relative response factors, and qualitative and
quantitative peak identification, should be given.
Procedures to validate the integrity and quality of the
data acquired through readings, interpretations, and cal-
culations should be specified. Some examples of data
validation procedures are:
a. Verification by the analytical task leader that all raw
data gen erated have been properly stored.
b. Examination of at least 5% of the raw data (e.g., chro-
matograms) by the analytical task leader and analyti-
cal QCC to verify adequacy of documentation, confirm
peak shape and resolution, ensure computer was
sensing peaks appropriately, etc.
c. Confirmation that raw areas for internal standards and
calibration standards and raw and relative areas for
surrogate compounds are within acceptable limits
around the expected value.
d. Verification that all associated blank, standard, and
QC data are reported along with analytical results.
e. Examination of all field data forms by the field sam-
pling task leader and field sampling QCC.
f. Verification of all calculations for one test run by a
second reviewer.
The test results and operating parameters to be reported
should be specified in a table including the units (e.g., Ib/
h) for each parameter. All documentation (e.g., field data
sheets, calculations, GC/MS printouts, etc.) that will be
delivered with the reported results should be identified*
4.2.11 Internal Quality Control Checks
All internal quality control methods should be described
for monitoring, sampling, and analysis activities. Internal
quality controls serve to document the validity of the data
obtained and to control the quality of the data as it is
being generated.
Items which should be included in the QA plan as internal
quality control checks include the following:
Calibration standards and devices
Zero/span gases
Audit gas cylinders
Blank samples
Field trip blanks
Field equipment blanks
Method blanks ^
Reagent and solvent blanks
« Method internal standards
Recovery internal standards
Spiked blanks
Spiked samples
Replicate analyses
Matrix/spike duplicate analyses
Surrogates
Calibration checks
4.2.12 Performance and Systems Audits
The QA plan should describe the types of performance
and systems audits that will occur and identify the
responsible individuals. Performance of equipment and
personnel should be audited periodically by the project
leader, field sampling leader, analytical task leader, the
27
-------
quality assurance officer, and the quality control coordi-
nators. Systems audits should also be performed periodi-
cally on monitoring systems, sampling, and analytical
systems.
4.2.13 Preventive Maintenance
The frequency and types of scheduled preventive main-
tenance procedures used for process monitoring equip-
ment, sampling equipment, and analytical equipment
and instrumentation should be given in the QA plan. In
addition, any nonscheduled maintenance procedures
which may occur when troubleshooting should be pro-
vided. It is desirable that the preventive maintenance
procedures be described in standard operating proce-
dure (SOP) manuals for the various types of equipment
used.
Logbooks for maintenance performed by field sampling
and laboratory personnel should be maintained. Equip-
ment logbooks should also be kept for maintenance per-
fowned by internal service departments and outside
service departments.
4.2.14 Specific Routine Procedures Used to Assess
Data Precision, Accuracy, and Completeness
The specific procedures that will be used to assess the
precision and accuracy of measurement data on a rou-
tine basis must be given. The procedures should include
equations to calculate precision and accuracy. Examples
are given below.
4.2.14.1 Precision
For data sets with a small number of points (2 < n < 8),
the estimate of precision can be expressed as range
percent (R%):
n-1
For large data sets (n > 8), the estimate of precision can
be expressed as percent relative standard deviation
(%RSD):
Standard deviation (SD) =
0/oRDg - 100°/o_x SD
C
The methods for determining how precision will be deter-
mined for each measurement parameter should be
given.
4.2.14.2 Accuracy
Accuracy can be determined for process monitors and
analyses from performance and audit samples (i.e., stan-
dards supplied as blind audits by the QCC to determine
percent accuracy [A°/o]); for analyses as percent recov-
ery (R%) of native analytes from blanks spiked with
native analytes prior to sample preparation; and for anal-
yses as percent recovery of internal standards (RS%)
spiked prior to sample preparation. Example equations
for accuracy calculations are given below.
For performance samples:
AO/O _ Amount found x 100
True value
For samples spiked with native analyte:
_, n Amount calculated-native amount prior to spiking 100
H°/0 = y _ . X
._ Amount spiked in
Rs% =
where: C, = highest value determined
C2 = lowest value determined
C = mean value of the set
and
_ n C
C=Z n1
i = 1
where: C, = ith determination
*
n = number of determinations
n Amount calculated - amounk of internal standard spiked 100
._ Amount of internal standard spiked i n
4.2.15 Corrective Action
Corrective action procedures thsit will be taken if prob-
lems are detected during system audits, performance
audits, and data collection; if data are lost; or if significant
QA problems develop which must be described in the QA
plan. The individuals responsible for initiating corrective
action procedures should be identified and the methods
for reporting corrective actions should be described.
4.2,16 Quality Assurance Reports to Management
The quality control coordinators, in cooperation with the
project leader, analytical task leader, field sampling task
leader, and data analysis task leader should inspect criti-
cal areas of the project requiring QA/QC activities. The
inspections should include a review, where applicable, of
the following:
28
-------
Staff qualifications
Equipment calibration and maintenance records
Instrument performance
Protocol adherence
Sample custody
Document control
Data entry including error handling, correction, and
additions
Data traceability and completeness
Data calculation and validation
Internal QC data
External QA data
Data accuracy, precision, and completeness
The results of inspections/audits should be reported by
the QAM to the project leader and corporate manage-
ment; summaries should be included in the final report.
The QCCs should independently maintain a QA file for
the project. At the end of the project, the QA project file
should be turned over to the QA manager.
4.3 Guidance for Precision and Accuracy
Objectives
The quality assurance objective of any project is to pro-
vide reliable data for documenting the performance of the
incinerator.
Specific precision and accuracy objectives for general
analytical procedures are given in Table 16. Objectives
for semivolatile POHCs are goals recommended by EPA
in the publication Sampling and Analysis Methods for
Hazardous Waste Combustion.4 Objectives for chlorine
and hydrogen chloride are estimated from past analysis
of similar types of samples.
Quality assurance objectives for completeness and rep-
resentativeness should be determined from the data
quality objectives (DQOs) and should reflect specific
requirements of the project.
Table 16. Summary of Precision and Accuracy Objectives
Accuracy"
Parameter
Semivolatile POHC
Volatile POHC
Chlorine
Hydrogen chloride
Matrix
Stack emissions
XAD-2
Filter
Water
Front-half rinse
Back-half rinse
Aqueous waste
Sludge
Solid waste
Scrubber water
Ash/residual
Organic liquid
VOST traps
(stack emissions)
Aqueous waste
Sludge
Solid waste
Scrubber water
Organic liquid
waste
Aqueous waste
Sludge
Solid waste
Organic liquid
waste
KOH solution
Precision*
(range %
or % RSD)
<30
<30
<30
< 30
<30
< 30
< 30
<50
<30
<30
<30
< 30
<30
< 10
< 10
<10
< 10
15
mean
recovery
(%)
>50
>70
>50
>50
>70
>50
' > 70
50-150%''
NAC
NA
NA
NA
NA
NA
NA
NA
NA
100 * 15
Procedures for assessing precision are presented in Section 4.2.14.
' Procedures for assessing accuracy are presented in Section 4.2.14.
c Not available.
29
-------
-------
Section 5
References
1. Midwest Research Institute, Practical Guide Trial
Burns for Hazardous Waste Incinerators, EPA-600/2-
86/050, NTIS PB86-190246, April 1986.
2. "Guidelines for Data Acquisition and Data Quality
Evaluation in Environmental Chemistry," Analytical
Chemistry, 52(14):2242-2249, December 1980.
3. US. Environmental Protection Agency, Guidance
Manual for Hazardous Waste Incinerator Permits, SW-
966, NTIS PB84-100577, Office of Solid Waste,
Washington, D.C., 1983.
4. Arthur D. Little, Inc., Sampling and Analysis Methods
for Hazardous Waste Combustion, EPA-600/8-84-
002, NTIS PB84-155845, February 1984 (new edition
expected in 1989).
5. Complete Temperature Measurement Handbook and
Encyclopedia, Omega Engineering, Inc., 1986.
6. U.S. Environmental Protection Agency, Test Methods
for Evaluating Solid Waste Physical/Chemical
Methods, SW-846, Third Edition, Office of Solid
Waste and Emergency Response, Washington, D.C.,
November 1986.
7. Code of Federal Regulations, Revised as of July 1,
1985.
8. American Society for Testing Materials, Annual Book
of ASTM Standards, Philadelphia, Pennsylvania,
Annual Series.
9. U.S. Environmental Protection Agency, Protocol for
the Collection and Analysis of Volatile POHCs Using
VOST, EPA-600/8-84-007, NTIS PB84-170042, March
1984.
10. US. Environmental Protection Agency, Validation of
the Volatile Organic Sampling Train (VOST) Protocol,
EPA-600/4-86-014, NTIS PB86-145547 (Vol. 1),
PB86-145554(Vol. 2), Environmental Monitoring Sys-
tems Laboratory, 2 Volumes, January 1986.
11. "Performance Audit Results for Volatile POHC Mea-
surements," JAPCA, Vol. 38, No. 6, June 1988.
12. Federal Register, Volume 45, No. 114, Wednesday,
June 11,1980.
13. US. Environmental Protection Agency, Modified
Method 5 Train and Source Assessment Sampling
System Operator's Manual, EPA-600/8-85-003, NTIS
PB85-169878, February 1985.
14. Radian Corporation, Laboratory and Field Evaluation
of the Semi-VOST (Semi-Volatile Organic Sampling
Train) Method, EPA-600/4-85-075, NTIS PB86-
123551, Environmental Monitoring Systems Labora-
tory, 2 Volumes, November 1985.
15. US. Environmental Protection Agency, Methods for
Chemical Analysis of Water and Wastes, EPA-600/4-
79-020, NTIS PB297686, March 1979.
16. US. Environmental Protection Agency, Development
of Data Quality Objectives: Description of Stages I
and II, Quality Assurance Management Staff, July 16,
1986.
17. US. Environmental Protection Agency, Interim Guide-
lines and Specifications for Preparing Quality
Assurance Project Plans, Office of Monitoring Sys-
tems and Quality Assurance, QAMS-005/80, Decem-
ber 29,1980.
31
-------
-------
Appendix A
Analysis Methods for Appendix Vill Hazardous
Constituents Given in EPA-600/8-84-002 and SW-846
Analysis Methods for Appendix Vill Hazardous Constitutents
EPA-600/8-84-002 SW-846
Compound Method No.* Method No."
Acetonitrile
Acetophenone
3-(a-Acetonylbenzyl)-4-hydroxy-coumarin and salts (Warfarin)
2-Acetylaminofluorene
Acetyl chloride
1-Acetyl-2-thiourea
Arcolein
Acrylamide
Acrylonitrile
Aflatoxins
Aldrin
Allyl alcohol
Aluminum phosphide
4-Aminobiphenyl
6-Amino-l,la,2,8,8a,8b-hexahydro-8-(hydroxymethyl)-8a-
methoxy-5-methylcarbamate azirino[2 ' ,3 ' : 3,4]pyrrolo
[1,2-a]indole-4,7-dione(ester) (Mitomycin C)
5-(Aminomethyl)-3-isoxazolol
Amitrole
Aniline '
Antimony and compounds, N.O.S.
Aramite
Arsenic and compounds, N.O.S.
Arsenic acid
Arsenic pentoxide
Arsenic trioxide
Auramine
Azaserine
Barium and compounds, N.O.S.
Barium cyanide
Benz(c)acridine
Benz(c)anthracene
Benzene
Benzene, 2-amino-1-methyl
Benzene, 4-amino-1-methyl
Benzenearsonio acid
Benzene, dichloromethyl-
Benzenethiol
Benzidine
Benzo(b)fluoranthene
Benzo(j)fluoranthene
Benzo(a)pyrene
p-Benzoquinone
Benzotrichloride
Benzyl chloride
Beryllium and compounds, N.O.S.
A101
A121
A122
A121
A144
A123
A101
A101
A101
A145
A121
A134
A253
A121
A122
A121
A121
A121
A221
A121
A222
A222
A222
A222
A121
A123
A223
A223
A252
A121
A121
A101
A222
A121
A121
A121
A121
A121
A121
A121
A121
A121
A224
8030, 8240
8250
8250
8250
*
8250
8030, 8240
8015, 8240
8030, 8240
8250
8080, 8250
8240
8250
8250
8250
8250
7040, 7041
8250
7060, 7061
7060, 7061
7060, 7061
7060,7061
8250
*
7080, 7081
7080
9010
8250
8100, 8250, 8310
8020, 8240
*
*
7060,7061
8120,8250
8250
8250
8100, 8250, 8310
8100, 8250, 8310
8100, 8250, 8310
8250
8120, 8250
8010, 8120, 8250
Compound
Type'
V
sv
sv
sv;
V
sv
V
V
V
* .
. sv
v
s
sv
sv
sv -
sv
sv
M
sv
M
M
M
M
SV
SV
M
M
CN
SV
SV
V
M
SV
SV
sv
sv
sv
sv
sv
sv
sv
'~M
Analysis
Method"
GC, GC/MS
GC/MS
HPLC, GC/MS
GC/MS
GC/MS
HPLC, GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
HPLC, GC/MS
GC, GC/MS
GC/MS
GC/FPD
GC/MS
HPLC
GC/MS
GC/MS
GC/MS
AAS
GC/MS
AAS
AAS
AAS
AAS
GC/MS
HPLC
ICAPAAS
ICAP.AAS
T, C
GC/MS
GC, GC/MS
GC, GC/MS
AAS
GC, GC/MS
GC/MS
GC/MS
GC, GC/MS
GC, GC/MS
GC, GG/MS
GC/MS
GC, GC/MS
GC, GC/MS
ICAPAAS
33
-------
Analysis Methods for Appendix VIII Hazardous Constltutents (continued)
EPA-600/8-84-002 SW-846 Compound Analysis
Compound Method No.' Method No." Type' Method"
Bis{2-ch!oroethoxy)methane
Bis(2-chtoroethyl)ether
N,N-Bis{2-chloroethyl)-2-naphthyl-amine
Bis(2-chloroisopropyl) ether
Bis{chtoromethyl) ether
Bis(2-othylhexyl) phthalate
Bromoacetone
Bromomethane
4-Bromophenyl phonyl ether
Bfucine
2-Butanono peroxide
Butyl benzyl phthallde
2-sec-Bulyl-4,6-dlnitrophenol (DNBP)
Cadmium and compounds, N.O.S.
Calcium chromate
Calcium cyanide
Carbon disulfide
Carbon oxylluorlde
Chloral (as hydrate)
Chtorambucil
Chlordane (a and Y isomers)
Chlorinated benzenes, N.O.S.
Chlorinated ethane, N.O.S.
Chlorinated (luorocarbons, N.O.S.
Chlorinated naphthalene, N.O.S.
Chlorinated phenol, N.O.S.
Chloroacetaldehyde
Chloroalkyl ethers, N.O.S.
p-Chloroaniline
Chlorobenzene
Chtorobenzilate
p-Chtoro-m-cresol
1-Chtoro-2,3-epoxypropane
2-Chloroethyl vinyl ether
Chloroform
Chloromethane
Chloromethyl methyl ether
2-Chloronaphlhalene
2-Chlorophenol
Chloropreno
1-{c-Crilorophenyl)thiourea
3-Chtoropropene
3-Chloroproptonitnle
Chromium and compounds, N.O.S.
Chrysene
Citrus Red No. 2
Coal tars
Copper cyanide
Creosote
Cresols
Crotonatdehyde
Cyanides (soluble salts and complexes), N.O.S.
Cyanogen
Cyanogen bromide
Cyanogen chloride
Cycasin
2-Cyclohexyl-4,6-dinitrophenol
Cyclophosphamide
Oaunomycin
ODD
DDE
DDT
Diallate
A121
A121
A121
A121
A121
A121
A101
A101
A121
A148
A121
A121
A121
A225
A226
A252
A101
A141
A101
A131
A122
A121
A101
A121
A101
A101
A121
A121
A131
A101
A121
A101
A121
A121
A122
A101
A101
A101
A101
A101
A121
A121
A122
A123
A121
-A226
A121
A149
A121
A252
A121
A121
A123
A131
A252
A138
A138
A138
A150
A121
A122
A121
A121
A121
A121
8010, 8240, 8250
8010, 8240, 8250
A
8010, 8240, 8250
8010, 8250
8060, 8250
8010, 8240
8250
8250
8250
8060, 8250
8040, 8250
7130, 7131
7190, 7191
9010
8015, 8240
It
8010,8240
*
8080, 8250
8010, 8240
8020,8250
8010,8240
*
8120, 8250
8040, 8250
8010, 8240
*
* '
8020, 8240
*
8040, 8250
*
8010, 8240
8010, 8240
8010, 8240
8010
8120, 8250
8040, 8250
*
*
*
8250
7190, 7191, 7195,
7196, 7197
8100, 8250, 8310
*
#
9010
8100, 8250
8040, 8250
*
9010
9010
9010
9010
8040, 8250
*
8080, 8250
8080, 8250
8080, 8250
*
to co co co co co
V
V
iSV
SV
SV
SV
SV
M
M
CN
V
G
V
V
SV
SV
V
SV
V
V
SV
SV
V
V
SV
V
SV
sv
sv
V
V
V
V
V
sv
sv
sv
sv
sv
M
sv
sv
sv
CN
sv
sv
sv
sv
CN
G
G
G
SV
SV
SV
sv
sv
sv
GC, GC/MS
GC, GC/MS
GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
S>/^/k JO
GC/MS
GC, GC/MS
GC/MS
GC/FID, HPLC
GC/MS
GC, GC/MS
GC, GC/MS
ICAPAAS
ICAP.AAS
ICART, C
GC/MS
GC/TCD
GC/MS
GC, GC/MS,
HPLC
HPLC
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS,
HPLC
GC/MS
GC/MS
GC, GC/MS
GC/MS
GC, GC/MS
HPLC
GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
HPLC
HPLC
GC/MS
ICAPAAS
GC, GC/MS
HPLC
GC/MS
T,C
GC, GC/MS
GC, GC/MS
HPLC
GC/MS
. T,C
GC/TCD, T-C
GC/TCD, T, C
GC/TCD, T, C
GC, GC/MS
HPLC
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC/MS
34
-------
Analysis Methods for Appendix VIII Hazardous Constitutents (continued)
EPA-600/8-84-002 SW-846
Compound Method No.' Method No."
Dibenz(a,h)acridine
Dibenz(a,j)acridine
Dibenz(a,h)anthracene
7H-Dibenzo(c,g)carbazole
Dibenzo(a,e)pyrene
Dibenzo(a,h)pyrene
Dibenzo(a,i)pyrene
1,2-Dibromo-3-chloropropane
1,2-Dibromoethane
Dibromomethane
Di-n-butyl phthalate
Dichlorobenzene (meta, ortho and para isomers)
Dichlorobenzene, N.O.S.
3,3 ' -Dichlorobenzidine
1 ,4-Dichloro-2-butene
Dichlorodifluoromethane
1,1-Dichloroethane
1,2-Dichloroethane
trans-1,2-Dichloroethene
Dichloroethylene, N.O.S.
1 ,1-Dichloroethylene
Dichloromethane
2,4-Dichlorophenol :.
2,6-Dichlorophenol
2,4-Dichlorophenoxyacetic acid
Dichlorophenylarsine
Dichloropropane, N.O.S.
1 ,2-Dichloropropane
Dichloropropanol, N.O.S.
Dichlpropropene, N.O.S.
1 ,3-Dichloropropene
Dieldrin
1 ,2:3,4-Diepoxybutane
Diethylarsine
N,N-Diethylhydrazine
0,0-Diethyl S-methyl ester of phosphorodithioic acid
0,0-Diethylphosphoric acid, 0-p-nitrophenyl ester
Diethyl phthalate
0,0-Diethyl 0-2-pyrazinyl phosphorothioate
Diethylstilbestrol
Dihydrosafrole
3,4-Dihydroxy-a-(rnethylamino)methyl
benzyl alcohol [Epinephrine]
Diisopropylfluorophosphate (DFP)
Dimethoate
3-,3 ' -Dimethoxybenzidine
p-Dimethylaminoazobenzene
7,12-Dimethylbenz(a)anthracene.
3,3 ' -Dimethylbenzidine
Dimethylcarbamoyl chloride
1,1-Dimethylhydrazine
1,2-Dimethylhydrazine
3,3-Dimethyl-1-(methylthio)-2-butanone,0-((methylamirio)
carbonyljoxime [Thiofanox]
a.a-Dimethylphenetriylamine
2,4-Dimethylphenol - -
Dimethyl phthalate
Dimethyl sulfate
Dinitrobenzene, N.O.S.
4,6-Dinitro-o-cres'ol (and salts)
2,4-Dinitrophenol
2,4-Dinitrotoluene
2,6-Dinitrotoluene
A121
A121
A121
A121
A121
A121
A121
A101
A101
A101
A121
A101
A121
A101
A121
A121
A101
A101
A101
A101
A101
A101
A101
A101
A121
A122
A121
A122
A122
A133
A222
A101
A101
A121
A101
A101
A121
A121
A222
A121
A121
A121
A121
A121
A123
A121
A123
A121
A121
A121
A121
A121
A121
A144
A121
A121
A183
A121
A121
A121
A121
A121
A121
A122
A121
A122
A121
A121
8100
8100
8100, 8310, 8250
8100
8100
8100
8100
8010, 8240
8010, 8240
8010, 8240
8060, 8250
8010,8120
8250
8010, 8120
8250
8250
8010, 8240
8010
8010, 8240
8010, 8240
8010, 8240
8010
8010
8010, 8240
8040, 8250
8040, 8250
8150, 8250
7060, 7061
8010, 8240
8010, 8240
8120, 8250
8240
8240
8080
* ' ,
7060/7061
*
8250
8250
8060, 8250
8250
*
*
*
8140
*
*
*
*
*
*
*
*
»
8040, 8250
8060, 8250
8250
8090, 8250
8040, 8250
8040, 8250
8090, 8250
8090, 8250
Compound Analysis
Type0 Method"
SV
sv
SV
sv
sv
sv
sv
V
V
V
sv
V
sv
V
sv
sv
V
V
V
V
V
V
V
V
sv
sv
sv
sv
sv
sv
M
V
V
sv
V
V
sv
sv
M
sv
sv
sv
sv
sv
sv
sv
sv
sv
sv
sv
sv
sv
sv
sv
sv
sv
sv
sv
sv
sv
sv
sv
sv
sv
sv
sv
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC.GC/MS
GC/MS -
GC, GC/MS
GC/MS
GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
HPLC
GC, GC/MS
HPLC
GC, GC/MS,
HPLC
GC/MS
AAS
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC/MS
GC/MS
GC, GC/MS
GC/MS
AAS
GC/MS
GC/MS
GC/MS
GC, GC/MS
GC/MS
HPLC
GC/MS
HPLC
GC/MS
GC, GC/MS
GC/MS
GC/MS
GC/MS
' GC/MS
GC/MS
. GC/MS
GC/FPD
GC/MS
GC, GC/MS
GC, GC/MS
GC/MS
GC, GC/MS
GC, GC/MS
HPLC
GC, GC/MS
HPLC '
GC, GC/MS
GC, GC/MS
35
-------
Analysis Methods for Appendix VIII Hazardous Constitutents (continued)
Compound
Dl-n-octyl phthalate
1,4-Dioxane
Diphenylamine
1,2-Diphenylhydrazine
Di-n-propylnitrosamine
Disulfoton
2,4-Dithiobiuret
Endosulfan
Endrin (and metabolites)
Ethyl carbamate
Ethyl cyanide
Ethyleneblsdithiocarbamic acid (salts and esters)
Ethylenelmine
Ethyfene oxide
Ethyfene thiourea
Ethyl methacrylate
Ethyl methanesulfonate
Fluoranthene
Fluorine
2-Fluoroacetamide
Fltioroacatic acid, sodium salt
Formaldehyde
Formic acid
Qlycldylatdehyde
Hatomethane, N.O.S.
Heptachlor
Heptachlor epoxlde (a, p, and y isomers)
Hexachtorobenzcno
Hexachlorobutadiene
Hexachtorocyclohexane (all isomers)
Hexachtorocyclopenladiene
Hexachlorodibenzo-p-dioxins
Hexachlorodibenzofurans
Hcxachtoroethane
1,2,3,4l10,10-Hexachloro-1,4,4a,5,8,8a-hexahydro-
1,4:5l8-endo,endo-d!methanonaphthalene
Hexachtorophene
Hexachloropropene
Hexaethyl tetraphosphate
Hydrazlne
Hydrocyanic acid
Hydronuorlcacid
Hydrogen sulfide
Hydroxydimethylarslne oxide
lndono(1,2,3-c,d)pyrene
lodomethane
Iron dextran (complex)
Isocyanic acid, methyl ester
Isobutyl alcohol
isosafrole
Kepone
Lasiocarplne
Lead and compounds, N.O.S.
Lead acetate
Lead phosphate
Lead subacetate
Maleic anhydride
Maleic hydrazlde
Malononitrile
Melphalan
Mercury fulminate
Mercury and compounds, N.O.S.
Methacrylonitrile
Methanethiol
Methapyriline
EPA-600/8-84-002 SW-846 Compound Analysis
Method No.' Method No." Type' Method"
A121
A101
A121
A121
A121
A121
A121
A121
A121
A121
A252
A121
A156
A123
A121
A121
A121
A137
A157
A121
A131
A101
A121
A133
A131
A101
A121
A121
A121
A121
A121
A121
A101
A121
A121
A121
A101
A121
A101
"A141
A141
A251
A251
A141
A222
A121
A101
A101
A134
A121
A121
A160
A227
A227
A227
A227
A121
A121
A121
A122
A228
A228
A121
A101
A121
8060, 8250
*
*
*
*
8140
*
8080, 8250
8080, 8250
*
9010
*
*
*
8100,8250,8310
*
*
8015, 8240
*
8250
*
*
*
8080, 8250
8080, 8250
8120, 8250
8120, 8250
8120
8120, 8250
8280
8280
8010, 8240
8120, 8250
*
*
*
*
*
* '
*
*
7060, 7061
8100, 8250, 8310
*
.
8080
*
7420, 7421
7420, 7421
7420, 7421
7420, 7421
8250
*
*
*
7470, 7471
7470, 7471
*
*
SV
V
SV
SV
SV
SV
SV
SV
SV
SV
CN
SV
V
SV
I sv
' SV
SV
G
*
SV
V
V
SV
SV
SV
V
SV
SV
SV
SV
SV
SV
SV
SV
V
SV
SV
SV
V
SV
V
G
G
AN
AN
G
M
SV
V
V
V
SV
SV
M
M
M
M
SV
SV
SV
SV
M
M
SV
V
SV
GC, GC/MS
GC/MS
GC/MS
GC/MS
GC/MS
GC, GC/MS
GC/MS
GC, GC/MS
GC, GC/MS
GC/MS
T,C
GC/MS
GC/FID
HPLC
GC/MS
GC/MS
GC, GC/MS
*
GC/FID
GC/MS
GC, GC/MS,
HPLC
GC/MS
GC/MS
GC/MS
GC/MS, HPLC
GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC/MS
GC/MS
GC, GC/MS
GC, GC/MS
GC/MS
GC/MS
GC/MS
GC/MS
GC/MS
GC/TCD
GC/TCD
1C
1C
GC/TCD
AAS
GC, GC/MS
GC/MS
'
GC/MS
GC/MS
GC/MS
GC, GC/MS
ICAPAAS
ICAPAAS
ICAPAAS
ICAPAAS
GC/MS
GC/MS
GC/MS
HPLC
CV/AAS
CV/AAS
GC/MS
GC/MS
GC/MS
36
-------
Analysis Methods for Appendix VIII Hazardous Constitutents (continued)
EPA-600/8-84-002 SW-846
Compound Method No.* Method No.6
Metholmyl
Methoxychlor
2-Methylaziridine
3-Methylcholanthrene
Methylchlorocarbonate
4,4 ' -Methylenebis(2-chloroaniline)
Methyl ethyl ketone (MEK)
Methyl hydrazine
2-Methyllactonitrile
Methyl methacrylate
Methyl methanesulfonate
2-Methyl-2-(methylthio)propionaldehyde-0-
(methylcarbonyl)oxime
N-Methyl-N ' -nitro-N-nitroso-guanidine
Methyl parathion
Methylthiouracil
Mustard gas
Naphthalene
1 ,4-Naphthoqui none
1-Naphthylamine
2-Naphthylamine
1-Naphthyl-2-thiourea
Nickel and compounds, N.O.S.
Nickel carbonyl
Nickel cyanide
Nicotine (and salts)
Nitric oxide
p-Nitroaniline
Nitrobenzene
Nitrogen dioxide
Nitrogen mustard (and hydrochloride salt)
Nitrogen mustard N-Oxide (and hydrochloride salt)
Nitroglycerine
4-Nitrophenol
4-Nitroquinoline-1-oxide
Nitrosamine, N.O.S.
N-Nitrosodi-n-butylamine
N-Nitrosodiethanolamine
N-Nitrosodiethylamine
N-Nitrosodimethylamine
N-Nitroso-N-ethylurea
N-Nitrosomethylethylamine
N-Nitroso-N-methylurea
N-Nitroso-N-methylurethane
N-Nitrosomethylvinylamine
N-Nitrosomorpholine
N-Nitrosonornicotine
N-Nitrosopiperid i ne
N-Nitrosopyrrolidine
N-Nitrososarcosine
5-Nitro-o-toluidine
Octamethylpyrophosphoramide
Osmium tetroxide
7-Oxabicyclo[2.2.1 ]heptane-2,3-dicarboxylic acid
Paraldehyde
Parathion
Pentachlorobenzene
Pentachlorodibenzo-p-dioxins
Pentachlorodibenzofurans
Pentachloroethane
Pentachloronitrobenzene (PCNB)
Pentachlorophenol
Phenacetin
A122
A121
A121
A121
' A121
A101
A121
A101
A121
A121
A121
A121
. A183
A121
A121
A121
A139
A121
A121
A121
A121
A123
A229
A229
A229
A252
A121
A141
A121
A121
A141
A139
A139
A121
A121
A122
A121
A121
A121
A121
A121
A121
A121
A121
A121
A121
A121
A121
A121
A121
A121
A122
A121
A230
A133
: A131
A121
A121
A121
A121
A121
A174
8250
8080
* -
8100
*
*
8015, 8240
*
. *
*
*
*
*
*
*
8140
_ *
*
8100, 8250, 8310
8090, 8250
*
*
*
7520, 7521
7520, 7521
7520, 7521
9010
*
*
*
8090, 8250
*
*"
*
8040, 8240
8250
*
8250
8250
8250
8250
8250
8250
8250
8250
8250
8250
8250
8250
8250
8250
8250
*
* -
*
*
8015, 8240
8140
*
8280
8280
*
*
8040, 8250
*
Compound Analysis
Type' Method"
SV
sv
SV
sv
sv
V
sv
V
sv
sv
sv
sv
*
sv
sv
sv
V
sv
sv
sv
sv
sv
M
M
M
CN
SV
G
SV
SV
G
V
V
SV
SV
sv
sv
sv
sv
sv
sv
sv
sv
sv
sv
sv
sv
sv
sv
sv
sv
sv
sv
M
sv
V
sv
sv
sv
sv
sv
sv
sv
sv
GC, GC/MS,
HPLC
GC, GC/MS
GC/MS
GC, GC/MS
GC/MS
GC, GC/MS
GC/MS
GC/MS
GC/MS
GC/MS
GC/MS
GC/MS
GC/FPD
GC/MS
GC, GC/MS
GC/MS
GC/FPD
GC, GC/MS
GC, GC/MS
GC/MS
GC/MS
HPLC
ICAP.AAS
ICARAAS
ICAP.AAS
T,C
GC/MS
GC/TCD
GC/MS
GC, GC/MS
GC/TCD
GC/FPD
GC/FPD
GC/MS
GC, GC/MS
GC/MS, HPLC
GC/MS
GC/MS
GC/MS
GC/MS
GC/MS
GC/MS
GC/MS
GC/MS
GC/MS
GC/MS
GC/MS
GC/MS
GC/MS
GC/MS
GC/MS
HPLC
GC/MS
ICARAAS
GC/MS
GC, GC/MS,
HPLC
GC, GC/MS
GC/MS
GC/MS
GC/MS
GC/MS
GC/MS
GC, GC/MS
HPLC
37
-------
Analysis Methods for Appendix VIII Hazardous Constltutents (continued)
EPA-600/8-84-002
Compound Method No.'
Phenol
Phenylenediamine
Phenylmercury acetate
N-Phenylthiourea
Phosgene
Phosphine
Phosphorodithloic acid, 0,0-dlethyl
Sn((ethylthio)methyl) ester [Phorate]
Phosphorothioic acid, 0,0-dimethyl 0-(p-((dimethylamino)sulfonyl)
phony!) ester [Famphur]
Phthalicacid esters, N.O.S.
Phthalic anhydride
2-PicoHne
Polychlorinated biphenyl, N.O.S.
Potassium cyanide
Potassium silver cyanide
Pronamtde
1,3-Propane suifone
n-Propylamine
Propylthiouracil
2-Propyn-1-ol
Pyridine
Reserplne
Resorcinol
Saccharin (and salts)
Safrole
Selenious acid
Selenium and compounds, N.O.S.
Selenium sulfide
Selenourea
Silver and compounds, N.O.S.
Silver cyanide
Sodium cyanide
Streptozotocin
Strontium sulfide
Strychnine (and salts)
1,2,4,5-Tetrachlorobenzene
2,3,7,8-Tetrach!orodibenzc~p-dioxin(TCDD)
Tetrachtorodibenzo-p-dioxins
Tetrachlorodibenzofurans
Tetrachtoroethane, N.O.S.
1,1,1,2-Tetrachloroethane
1,1,2,2-Telrachloroethano
Tetrachloroethylene
Tetrachloromethane
2,3,4,6-Tetrachlorophenol
TetraBthyldithiopyrophosphate
Tetraethyl lead
Tetraethylpyrophosphate
Totranltromethane
Thallium and compounds, N.O.S.
Thalllc oxide
Thallium(l) acetate
Thallium(l) carbonate
Thallium(l) chloride
Thallium(l) nitrate
Thallium selenite
Thallium(l) sulfate
Thioacetamide
Thiosemlcarbazide
Thiourea
Thiuram
Tbluene
Toluenediamine, N.O.S.
2,4-Toluencdiamine
2,6-Toluenediamine
A121
A122
A121
A228
A123
A138
A136
A121
A121
A121
A121
A121
A121
A252
A232
A252
A121
A121
A121
A121
A134
A121
A122
A134
A121
A123
A121
A231
A231
A231
A231
A232
A232
A252
A252
A122
A233
A180
A121
A121
A101
A101
A101
A101
A101
A121
A122
A121
A227
A121
A101
A234
A234
A234
A234
A234
A234
A234
A234
A123
A123
A123
A122
A101
A121
A121
A121
SW-846
Method No."
8040, 8250
*
7470, 7471
*
*
8140
'8140
8060
8090, 8250
8090, 8250
8080,8250
9010
7760, 7761
9010
*
*
8090, 8250
*
*
*
*
7740, 7741
7740, 7741
7740, 7741
7740, 7741
7760, 7761
7760, 7761
9010
9010
*
*
8120, 8250
8280
8280
8280
8010, 8240
8010, 8240
8010, 8240
8010, 8240
8010, 8240
8040 8250
*
7420, 7421
*
*
*
*
8020, 8240
8250
8250
8250
Compound
Type0
SV
SV
SV
M
SV
G
V
SV
sv
SV
SV
SV
SV
CN
i M
CN
SV
SV
SV
SV
V
SV
SV
SV
SV
SV
SV
M
M
M
M
M
M - :
; CN
CN
SV
M
SV
SV
SV
SV
SV
V
V
V
V
V
SV
SV
SV
M
SV
V
M
M
M
M
M
M
M
M
SV
SV
, sv
SV
V
SV
SV
SV
Analysis
Method"
GC, GC/MS
HPLC
GC/MS
CV/AAS
LJDI /"*
HrLO
GC/TCD
GC/FPD
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
TC
ICAPAAS
l^ C
GC/MS
GC/MS
GC/MS:
GC/MS
GC/FID, GC/MS
GC, GC/MS
HPLC
GC/FID, GC/MS
GC/MS
HPLC
GC/MS
AAS
AAS
AAS
AAS
ICAPAAS
ICAPAAS
TC
T C
LJDI O'
HrL(_>
ICAPAAS
HPLC
GC, GC/MS
GC/MS
GC/MS
GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
HPLC
GC/MS
ICAPAAS
GC/MS
GC/MS
ICAPAAS
ICAPAAS
ICAPAAS
ICAPAAS
ICAPAAS
ICAPAAS
ICAPAAS
ICAPAAS
HPLC
HPLC
HPLC
HPLC
GC, GC/MS
GC/MS
GC/MS
GC/MS
38
-------
Analysis Methods for Appendix VIII Hazardous Constitutents (continued)
EPA-600/8-84-002
Compound Method No.'
SW-846
Method No."
Compound
Type'
Analysis
Method"
3,4-Toluenediamine
o-Toluidine hydroohloride
Tolylene diisocyanate
Toxaphene
Tribromomethane
1,2,4-Trichlorobenzene
1,1,1-Trichloroethane
1,1,2-Trichloroethane
Trichloroethene
Trichloromethanethiol
Trichloromonofluoromethane
2,4,5-Trichlorophenol
2,4,6-Trichlorophenol
2,4,5-Trichlorophenoxyacetic acid (2,4,5-T)
2,4,5-Trichlorophenoxypropionic acid (2,4,5-TP) (Silvex)
Trichloropropane, N.QS.
1,2,3-Trichloropropane
0,0,0-Triethyl phosphorolhioate
sym-Trinitrobenzene
Tris-(1-azridinyl)phosphinesulfide
Tris(2,3-dibromopropyl) phosphate
Trypan blue
Uracil mustard
Vanadic acid, ammonium salt
Vanadium pentoxide
Vinyl chloride
Zinc cyanide
Zinc phosphide
A121
A121
A121
A101
A121
A101
A101
A101
A121
A101
A121
A122
A121
A122
A122
A133
A122
A133
A101
A101
A121
A121
A190
A121
A123
A235
A235
A101
A252
A253
8250
*
8250
8080, 8250
8010, 8240
8120,8250
8010, 8240
8010,8240
8010, 8240
*
8010, 8240
8040,8250
8040,8250
8150,8250
8150,8250
8010, 8240
8010,8240
8010, 8240
9010
SV
SV
SV
V
SV
V
V
V
SV
V
SV
SV
SV
SV
SV
SV
SV
SV
V
V
SV
SV
V
SV
SV
M
M
V
CN
S
GC/MS
GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC, GC/MS
GC/MS
GC, GC/MS
GC, GC/MS
HPLC
GC, GC/MS
HPLC
GC, GC/MS
GC/MS
GC, GC/MS
GC/MS
GC, GC/MS
GC, GC/MS
GC/MS
GC/MS
GC/FPD
GC/MS
HPLC
ICAP.AAS
ICAP.AAS
GC, GC/MS
1C
GC/FPD
Source: Arthur D. Little, Inc., "Sampling and Analysis Methods for Hazardous Waste Combustion," EPA-600/8-84-002 PB84-155845
February 1984.
= No method given.
" Sources: (1) "Test Methods for Evaluating Solid Waste Physical/Chemical Methods," EPA/OSW, Third Edition, SW-846 November 1986
(2) 40 CFR Part 261, Appendix III. - . '
(3) All VOST tube, analysis must be by Method 5040. Other methods are applicable to other matrices
= Method not specified for the substance in SW-846, but SW-846 methods may apply
= No method given. - , '
c V = Volatile substance
SV = Semivolatile substance
M = Metal
CN = Cyanide
S = Solid
AN = Anion
G = Gas
* = Not found
" GC = Gas chromatography
GC/MS = Gas chromatography/mass spectromeJry
GC/FID = Gas chromatography with flame lonization detector ;
GC/TCD = Gas chromatography with thermal conductivity detector
GC/FPD = Gas chromatography with flame photometric detector
HPLC = High performance liquid chromatography
AAS SB Atomic absorption spectroscopy
CV/AAS = Cold vapor/atomic absorption spectroscopy
ICAP = Inductively coupled argon plasma emission spectroscopy
1C = Ion chromatography
C = Colorimetry
T = Titration
= No method found
* = No method available
39
-------
-------
Appendix B
Measurement Checklists
B.1 Introduction
Checklists have been prepared to assist the permit writer
in determining the completeness of a trial burn plan and
permit application relative to process monitoring, sam-
pling, and analysis of samples. These checklists show
the parameters required by regulation or typically recom-
mended for measurement during a trial burn and the
essential information which should be given in the trial
burn plan for the measurement, sampling, or analysis of
each parameter. Table B-1 is the checklist for the monitor-
ing parameters, Table B-2 is for the sampling parameters,
and Table B-3 is for the analysis of samples.
One important aspect of any trial burn plan or permit
application is the description of the QA/QC procedures.
A checklist of the QA/QC items which should be
addressed in the project Quality Assurance (QA) plan for
each of the monitoring, sampling, and analysis parame-
ters is given in Table B-4.
The checklists should be filled in by the permit writer as
the trial burn plan and permit application are reviewed. In
each column indicate Y for yes, N for no, I for incomplete,
or NA for not applicable. The blanks which have an N or I
result in an incomplete,trial burn plan and permit applica-
tion and should be subsequently addressed to complete
the documents. The checklists address only information
related to measurements; they do not include other infor-
mation required for complete applications and trial burn
plans.
The following discussion provides a description of each
checklist, followed by the checklists.
B.2 Process Monitoring
The process monitoring checklist (Table B-1) contains
both parameters that must be monitored continuously
during the trial burn and subsequent operation of the
incinerator, as provided in the Code of Federal Regula-
tions, 40 CFR Parts 264.345 and 264.347, and others
typically recommended for measurement during trial
burns. Parameters on the checklist are (1) waste feed
rate, (2) combustion temperature, (3) a measure of com-
bustion gas velocity, (4) combustion chamber pressure,
(5) carbon monoxide concentration (CO) in the stack
gases, (6) oxygen concentration in the stack-gases, (7)
the waste feed pressure, (8) auxiliary fuel flow rate and
pressure, (9) waste atomization airflow rate and pressure,
(10) input quench water flow rate, (11) input and output
scrubber water flow rates and output pH, (12) other air
pollution control device(s) parameters, (13) waste feed
cutoff system parameters, and (14) other parameters as
appropriate.
The essential information which should be included in the
trial burn plan and permit application for each selected
process monitoring parameter is shown in the columns in
Table B-1. This information includes (1) whether ornot the
parameter will be monitored, (2) the monitoring method,
(3) monitoring equipment, (4) monitoring location, (5)
monitoring frequency, and (6) method of data recording.
These subjects should be addressed in the trial burn plan
and permit application. Other information such as meth-
ods of data reduction and storage, calibration of equip-
ment, and inspection and maintenance of the equipment
should be given in the project QA plan.
B.3 Sampling
The sampling checklist (Table B-2) contains a list of sam-
ples which may be taken during the trial burn and ana-
lyzed in accordance with 40 CFR Parts 264.341
264.342, 264.343, 264.345, 270.19, and 270.62.7 The
samples required by regulation are (1) waste feed, (2)
stack gases, (3) scrubber water, (4) ash, and (5) other
samples, as appropriate. Collection of auxiliary fuel and
scrubber inlet samples are optional. None of these sam-
ples are required during the subsequent operation of the
incinerator unless specified in the permit.
The essential information which should be included in the
trial burn plan for each sampling parameter is shown in
the columns of Table B-2. This information includes (1)
whether or not the sample(s) will be taken, (2) the sam-
pling method, (3) sampling equipment, (4) sampling loca-
tion, (5) sampling frequency, and (6) method of data
recording. These subjects should be addressed in the
trial burn plan. Other information such as calibration and
maintenance of the equipment, data reduction, and data
storage should be given in the project QA plan.
B.4 Analysis
The checklist for analysis of the samples (Table B-3)
contains parameters which may be evaluated for the trial
burn, in accordance with 40 CFR Parts 270.19 and
41
-------
270.627 Some of the analyses including the principal
organic hazardous constituents (POHCs) in the auxiliary
fuel and metals may be appropriate only in some cases.
Essential information which should be included in the
trial burn plan for each analytical parameter is shown in
the columns in Table B-3. This information includes (1)
whether or not the sample(s) will be analyzed, (2) analyti-
cal procedure, (3) analytical equipment, (4) sample trace-
ability, and (5) data recording. These subjects should be
addressed in the trial burn plan. Other information such
as calibration and maintenance of equipment, data
reduction and validation, data reporting, and data storage
should be given in the project QA plan.
B.5 Quality Assurance/Quality Control
Each permit application and trial burn plan must have a
quality assurance (QA) plan. The QA plan must address
all data-gathering activities (e.g., process monitors as
well as sampling and analytical activities). This plan
should conform to the specifications established in
SW-846, Test Methods for Evaluating Solid Waste
Physical/Chemical Methods,6 and Interim Guidelines and
Specifications for Preparing Quality Assurance Project
Plans," and must address all measurement parameters.
The purpose of the QA plan is to establish a specific
program to (1) help ensure that the monitoring data,
sampling, and analytical activities meet specific quality
objectives; and (b) routinely assess the quality of the
data. The QA/QC checklist (Table B-4) includes all of the
monitoring, sampling, and analytical parameters given in
the previous three checklists and shows the QA/QC
items required for each parameter in the Interim Guide-
lines and Specifications for Preparing Quality Assurance
Project Plans." Each of the QA/QC items is discussed in
Section 4.0. i
It should be noted that there is redundancy among the
information required in Tables EM to B-4. This informa-
tion may be provided in either the trial burn plan and
permit application or the QA plan, or both. QA/QC infor-
mation provided in the trial bum plan should be refer-
enced in the Q A plan.
42
-------
Table B-1. Checklist for Process Monitoring Parameters for RCRA Incinerators
Monitoring To be Monitoring Monitoring Monitoring Data
parameter monitored* method Equipment location frequency recording
Waste feed rate"
Stream No. 1 ' '
Stream No. 2
Stream No. 3
Combustion temperature(s)"
Combustion gas velocity indicator . f
Combustion chamber pressure
Primary _____
Secondary '
CO in stack gases" ..
Oxygen in stack gases
Waste feed pressure(s) "
Auxiliary fuel
Feed rate " .
Pressure '
Waste atomization , ,
Airflow - _i
Pressure J
Quench water
Input flow rate
Scrubber water
Input flow rate
Output flow rate ,
Output pH _____
Air pollution control device(s) parameters
Waste feed cutoff system
Other
* Indicate Y = Yes; N = No; I = Incomplete; NA = Not applicable.
a Continuous monitoring specifically required by RCRA regulations.
43
-------
Table B-2. Checklist for Sampling Parameters for RCRA Incinerators
Sampling Tobe Sampling
parameter
sampled*
_...r....a Sampling Sampling Data
method Equipment location frequency recording
Waste feed
Stream No. 1
Stream No. 2
Stream No. 3
Stack gases
Particulates
HCI
H,O
POHCs
O,
CO,
Stack gas flow rate
Stack gas temperature
Auxiliary fuel
Quench water
Inlet
Scrubber water
Inlet
Outlet
Ash
Other
Indicate Y = Yes;N = No; I = Incomplete; NA = Not applicable.
44
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Table B-3. Checklist for Analysis of Samples for RCRA Incinerators
Analytical To be
parameter analyzed* Procedure
Equipment
Sample
traceability
Data
recording
Waste feed analysis
High heating value
Chlorine
POHCs
Ash
Viscosity
H2O
Metals
Volatile matter
Stack samples
Particulates
HCI
POHCs
02
CO2
Metals
Auxiliary fuel
POHCs
HHV
Chlorine
Ash
Quench water input
POHCs
PH
Scrubber water input
POHCs
PH
Scrubber water output
POHCs
PH
Ash residue
POHCs
Heavy metals
TCLP
Other
Indicate Y = Yes;N = No; I = Incomplete; NA = Not applicable.
45
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Table B-4. Quality Assurance/Quality Control Checklist for Monitoring, Sampling, and Analysis Parameters for Incinerators
Mnnltnrlno. «amn1ina Quality assurance/quality control Items* :
-sa? SSL ±ax aag.ass. Ja, j±. JJSL.'JS?
Monitoring
Waste faod rate N/A
Combustion temperature N/A
Combustion gas velocity N/A
CO In stack gas N/A
Auxiliary fuel N/A
Atomlzation pressure N/A
Combustion chamber
pressure N/A
Quench water N/A
Scrubber water N/A
Air pollution control
devices N/A
Waste feed cutoff system N/A
Other N/A
Sampling
Waste feed sampling
Stack gas sampling
Auxiliary fuel
Scrubber water
Ash sampling
Other
Waste feed analysis
High heating value
Chlorides
POHCs
Ash
Viscosity
Stack samples
Particulars
HCI
0,
CO,
POHCs
Auxiliary fuel POHCs
Scrubber water
POHCs
pH
Ash residue
POHCs
Heavy metals
Other
GeneralQA/QC
Project description
Project organization and responsibility
Organization chart
Resumes of key Individuals
Description of individual responsibilities
Performance and system audits
Internal performance audits
Internal systems audits
External performance audits
External systems audits
Corrective action
OA reports to management
Types of reports
Individual^) responsible
Frequency
* Indicate Y » Yes;N = No; I = Incomplete; NA = Not applicable.
&U.S. GOVERNMENT PRINTING OFFICE:
1992 - «48-003/4183I
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