EPA-450/4-84-014d
National Dioxin Study Tier 4
Combustion Sources
Ash Sampling Program
By-
Radian Corporation
Research Triangle Park, NC 27709
Contract No. 68-02-3850
EPA Project Officer: William H. Lamason
U.S. ENVIRONMENTAL PROTECTION AGENCY
Office Of Air And Radiation
Office Of Air Quality Planning And Standards
Research Triangle Park, NC 27711
January 1985
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This report has been reviewed by the Office Of Air Quality Planning And Standards, U.S.
.Environmental Protection Agency, and approved for Publication as received from the contractor.
Approval does not signify that the contents necessarily reflect the views and policies of the
Agency, neither does mention of trade names or commercial products constitute endorsement
or recommendation for use.
EPA-450/4-84-014d
111
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TABLE OF CONTENTS
Section Page
LIST OF TABLES vii
LIST OF FIGURES ix
1.0 INTRODUCTION 1
2.0 OVERVIEW OF THE ASH SAMPLING PROGRAM AND SITE SELECTION
CRITERIA 3
2.1 PROGRAM OVERVIEW! I!!!!!!!!!!!!!!!!!!!! 2
2.2 SELECTION CRITERIA 4
3.0 OVERVIEW OF ASH SAMPLING PROCEDURES 17
4.0 SAMPLING LOCATIONS AND METHODS 19
4.1 SELECTION OF A SAMPLING LOCATION 19
4.2 SAMPLE SIZE 23
4.3 SAMPLING METHODS 23
4.3.1 Sampling of Ash on Conveyor Belts or in
Screw Conveyors 24
4.3.1.1 ASTM "Stopped-Belt Cut" Method
(D2234-76) 24
4.3.1.2 ASTM "Part-Stream Cut" Method
(D2234-76) 29
4.3.2 Sampling of Ash from Live Storage Hoppers
on Control Devices or Bottom Ash Hoppers
on Combustion Devices 30
4.3.3 Sampling of Ash Slurries from Sluices or
from Pipes ; . . . 30
4.3.3.1 Dipper/Scoop 30
4.3.3.2 End of Pipe Sampling 31
4.3.4 Sampling of Ash-Containing Liquids
(e.g., Scrubbers) 32
5.0 SITE SPECIFIC DATA NEEDS 35
6.0 SAMPLE CONTROL, PACKAGING, AND SHIPPING 39
6.1 CONTROL OF ASH SAMPLING KITS 39
6.1.1 Scheduling of Ash Sampling Kits 41
6.2 LABELING AND HANDLING OF SAMPLES 42
6.2.1 Labeling of Samples 42
6.2.1.1 Specific Label Entries 42
6.3 SAMPLE CHAIN-OF-CUSTODY RECORD 44
6.4 SAMPLE SHIPMENT 47
6.5 SAMPLE CONTAINER PREWASHING 50
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LIST OF TABLES
Number Page
2-1 Tier 4 - Ash Sampling Program (ASP) Activities 6
2-2 Combustion Source Categories Considered for Tier 4
Sampling Programs (November 1984) 9
2-3 Source Characteristics of Interest for Dioxin Test
Program 12
4-1 Recommended Sampling Methods for Ash Sampling 25
vn
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LIST OF FIGURES
Number
2-1 Site selection process for the Ash Sampling Program .... 5
2-2 Source descriptions for potential sampling sites
for Tier 4 - National Dioxin Study 10
4-1 Generic plant with example ash sampling sites 22
4-2 Vacuum ash handling system 26
4-3 Air pressure ash handling system 27
4-4 Limestone wet "Scrubber 28
4-5 Schematic of tap sampling 33
5-1 Field data to be collected during sampling 36
5-2 Example ash sampling data needs. Schematic of sampling
locations . 37
6-1 Example: shipping record tracking 40
6-2a Chain-of-custody seal 43
6-2b Sample label 43
6-3 Source category codes to be used on sample labels 45
6-4 Chain-of-custody form 46
6-5 Sample box identification and markings 49
IX
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1.0 INTRODUCTION
The Environmental Protection Agency's (EPA) Office of Air Quality
Planning and Standards (OAQPS) is developing and implementing Tier 4 of the
National Dioxin Study. The purpose of Tier 4 is to assess the emissions of
dioxins/furans from combustion sources. The term "dioxins/furans" is used
generically in this document to mean the tetra- through octa-polychlorinated
dibenzo-p-dioxins and the tetra- through octa-polychlorinated dibenzofurans,
with specific detection of the isomer 2,3,7,8-tetrachlorodibenzo-p-dioxin
(2,3,7,8-TCDD).
The project plan for Tier 4 includes a program to collect ash samples
from the flue gas of combustion source categories that have a reasonable
likelihood of emitting dioxins/furans. The results of this program will
provide a qualitative indication of the presence of dioxins/furans in the
source emissions. A second use for the results would be to broaden the
emission data base if a correlation between ash sample data and stack test
data can be developed during full-scale tests.
The purposes of this document are to describe the Ash Sampling Program
and to identify the activities that are proposed to be performed by OAQPS,
the EPA regional offices, State and local agencies, and the EPA contractor,
Radian Corporation. Specific guidance is also provided for the
organizations that will perform the field sampling in the program.
The Ash Sampling Program and the site selection criteria are described
in Section 2. The procedures to be implemented when a site has been
selected for sampling are given in Section 3.
Section 4 describes the criteria for selection of the ash sampling
location at the site and the methodology to be used to collect the sample.
"National Dioxin Study Tier 4 - Combustion Sources, Project Plan" Air
Management Technology Branch, OAQPS/EPA, Research Triangle Park, NC 27711,
June 1984.
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Section 5 identifies the data that must be collected at the time of
sampling, and Section 6 provides specific information regarding sample
control, packaging, and shipping.
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2.0 OVERVIEW OF THE ASH SAMPLING PROGRAM AND SITE SELECTION CRITERIA
The purpose of the Ash Sampling Program is to broaden the coverage of
the Tier 4 sampling effort and to solicit regional inputs concerning
additional combustion source categories with the potential to emit
dioxins/furans. Ash samples from the flue gas will be obtained from a
select group of combustion source categories and will be analyzed for
2,3,7,8-TCDD, tetra- to octa-polychlorinated dibenzo-p-dioxins, and tetra-
to octa-polychlorinated dibenzofurans.
Under a separate effort in the source sampling program, the analytical
results for ash and flue gas samples will be statistically examined to see
if the presence or absence of 2,3,7,8-TCDD, or polychlorinated dioxin/furan
homologues in the ash is a meaningful and quantifiable indicator of
potential air (i.e., flue gas) emissions of dioxins/furans.
If the results of the comparisons are favorable, then the results of
the Ash Sampling Program can be used to broaden the coverage of source
categories under Tier 4, and a potentially cheaper method of screening
combustion sources for dioxin/furan emissions will have been identified.
The following sections briefly describe the activities to be conducted
under the Ash Sampling Program, a schedule for these activities, and a
description of the site selection process.
2.1 PROGRAM OVERVIEW
Several parties will be involved in the Ash Sampling Program. These
include the OAQPS, with specific direction by the Air Management Technology
*
Branch (AMTB), the EPA regional offices, State and local agencies, Troika ,
Troika is the collective term for three EPA laboratories (Duluth,
Minnesota; Bay St. Louis, Mississippi; and Research Triangle Park, North
Carolina or their contractor laboratories) that are providing analytical
support.
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and Radian Corporation. A schematic of the program is given in Figure 2-1,
and a list of activities by responsible organization is given in Table 2-1.
The Ash Sampling Program was initiated by OAQPS in mid-1984 through a
letter sent to the regions explaining the purpose of the program and
soliciting inputs. An initial list of the candidate sites was provided by
the regional offices to OAQPS. These lists have been compiled and reviewed
by OAQPS and Radian Corporation. Radian and OAQPS will select two or three
sites from each source category for ash sampling. The regions will be
notified of the site selection and will be given a sample control number and
episode number by OAQPS. Prior to sending out sampling kits, the regions
will be contacted to ensure that the type of sample and the sampling
location identified are correct* The regions should contact the site to
arrange a sampling visit and to verify all site screening information.
Radian will send out sample kits to the regions once sample control numbers
have been assigned and the type of sample and sampling locations have been
specified. These kits will contain sample containers and instructions on
sampling and shipping. The regions will conduct the ash sampling following
the procedures described in Section 3.0 of this document. Following
sampling, the sampler will send the ash samples to Radian where the samples
will be prepared for submittal to Troika for analysis. Troika will analyze
the samples and submit.the results to OAQPS. The results will be compiled
and reported in the Tier 4 final report.
2.2 SELECTION CRITERIA
The Agency has already performed an analysis to identify those
combustion source categories which have the greatest potential to emit
2,3,7,8-TCDD. This analysis was summarized in the Tier 4 Project Plan and
detailed in the report entitled "National Dioxin Study Tier 4 - Combustion
p
Sources. Initial Literature Review and Testing Options." This initial
"Final Report - Review and Evaluation of Available Dioxin Emissions Data
and Testing Options for Combustion Sources" Radian Corporation, Under
Contract No. 68-02-3513 to EPA, September 28, 1984.
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REGIONAL OFFICES
OAQPS
RADIAN
TROIKA
Request candidate
site list
Identify sites
Identify candidate
sites based on
literature and file
Compile master
data list
Prepare site
selection
criterion
Select 3-4 sites for
each category for
ash sampling and
potential stack test
candidates
Notify Regions of
site selection
Provide sample
control numbers
Region (State/
local agency)
collects
samples
Provide sample
collection kits
Ship samples
to Radian
Sample
Pretreatment
Figure 2-1. Site selection process for the Ash Sampling Program.
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TABLE 2-1. TIER 4 - ASH SAMPLING PROGRAM (ASP) ACTIVITIES
Organization
Action
Regions
Radian
OAQPS
OAQPS, Radian
Regions
Radian
OAQPS
OAQPS, SCC
Radian
Regions
Regions
Radian
Radian
*Troika/BSL
Troika/RTP and Duluth
Identify sites and prepare region-specific source
lists
Preparation of Ash Sampling Program Plan
Review and send ASP Plan and Procedures Document
to Regions and the Sample Control Center (SCC)
Select sites for sampling
Site acquisition
Prepare/acquire QA blank and spiked samples
Contact SCC to provide number of samples and
sampling schedule
Assign episode numbers
Preparation of sampling kits (to be assembled
based on site information)
Collect samples, fill out sampling forms including
site specific data needs
Packing and shipping of samples and completed
sampling forms in prelabeled, prepaid containers
Receive containers and send copy of sampling
forms to OAQPS
Prepare samples for Troika analysis (i.e. seiving,
mixing, etc.), pack prepared samples and QC
samples in shipping containers and ship to
Troika/BSL
Receive samples, prepare extract, and ship to
analysis lab (RTP or Duluth)
Receive extract, perform analysis, transmit
results to BSL/SCC
Continued
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TABLE 2-1. TIER 4 - ASH SAMPLING PROGRAM (ASP) ACTIVITIES (CONTINUED)
Organization Action
SCC Distribute results to OAQPS and regions in
quarterly reports
OAQPS Distribute results to regions
OAQPS, Radian and Analysis and review of ASP results
Regions
OAQPS and Radian Write ASP report
OAQPS, Radian and Review of ASP report
Regions
OAQPS and Radian Incorporation of ASP report results into final
Tier 4 report
__
Troika is the collective term for three EPA laboratories (Bay St. Louis,
MS; Duluth, MN; and Research Triangle Park, NC, or their control
laboratories) that are providing analytical support.
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analysis identified and assigned ranks to broad source categories as
classes, but it did not rank specific facilities within a source category.
Table 2-2 summarizes the results of the initial work and subsequent data
gathering. The site selection process for the Ash Sampling Program will be
built upon much of the previous work, but will place its focus on specific
facilities. It is anticipated that facility specific information will be
provided by each region for each site identified. A brief questionnaire
detailing the type of information needed for each site to aid in the
screening process was developed and sent to the regions by OAQPS in August
1984. A copy of this questionnaire is included as Figure 2-2.
The purpose of screening the initial lists submitted by the regions is
to select up to three ash sampling sites from each source category
represented in addition to any full scale source testing sites. In some
instances, only one or two facilities in a source category may be
identified by the regional offices. In that case, OAQPS and Radian will
identify the other one or two sites. The sites selected should be
representative of the source category as a whole, and therefore should be
typical of the source category in terms of easily definable population
characteristics, such as, size, type of combustion device, age, etc. for the
source category under consideration. There may also be a subcategory that
has a high potential for dioxin emissions relative to the remainder of the
category. Table 2-3 provides a list of some of the candidate categories for
the Ash Sampling Program, and also indicates the source characteristics that
would be desirable from the standpoint of testing for dioxins/furans. Each
of these characteristics would tend to increase the chance for dioxin/furan
emissions from the source category in question.
In identifying sites for ash sampling, the following factors (where
information is available) will be considered:
Does the combustion device burn a fuel that generates ash (i.e.,
not gaseous or liquid alone)?
Does the source have a particulate control device?
Does the combustion device have any polychlorinated
dibenzo-p-dioxin (PCDD) or polychlorinated dibenzofurans (PCDF) in
the feed or fuel?
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TABLE 2-2. COMBUSTION SOURCE CATEGORIES CONSIDERED FOR TIER 4
SAMPLING PROGRAMS (NOVEMBER 1984)*
Rank A Source Categories
Sewage Sludge Incinerators
Black Liquor Boilers
Rank B Source Categories
Industrial Incinerators (including hospital incinertors)
PCP Sludge Incinerators
Carbon Regeneration (industrial)
Wire Reclamation
Wood Boilers (firing PCP treated or salt-laden wood)
Rank C Source Categories
Charcoal Manufacturing
Wood Stoves
Mobile Sources
Small Spreader-stoker Coal Boiler
Chlorinated Organic Waste Incinerators
Lime-Cement Kilns Cofired with Chlorinated Organic Wastes
Commercial Boilers Firing Fuels Contaminated with Chlorinated Organic
Wastes
Forest Fires '
Apartment House Flue-fed Incinerators
Agricultural Burning
Landfill Flares
Residential Oil Burners Burning Waste Oil
Rank D Source Categories
Municipal Solid Waste (MSW) Incinerators
Industrial Boilers Cofiring Wastes
This list of source categories undergoes constant review and revision and
pis subject to change.
PCP = polychlorinated phenols
Rank A - Large source categories (greater than 1 million tons of fuel
and/or waste burned annually) with elevated dioxin precursor
contamination or feed/fuel. These categories have a high
potential to emit TCDD, and population exposure is expected to be
relatively high compared to other source categories.
Rank B - Small source categories (less than 1 million tons of fuel and/or
waste burned annually) or source categories with limited dioxin
precursor contamination of feed/fuel. These categories have a
high potential to emit TCDD, but population exposures are expected
to be low.
Rank C - Source categories less likely to emit 2,3,7,8-TCDD.
Rank D - Source categories which have been tested three or more times.
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FIGURE 2-2- SOURCE DESCRIPTIONS FOR POTENTIAL SCREENING SITES FOR
TIER 4 - NATIONAL OIOXIN STUDY
SOURCE IDENTIFICATION
Source Category: NEDS/SCC Number(s):
Site Name: Contact Name:
Address: Title: __Zm
Phone: 1)
COMBUSTION PARAMETERS
The design of the source affects the operating conditions and quantity of dioxin
enrfsslons. Please desclbe briefly, the type, design and size of the source, specify-
ing units of measure where necessary (e.g. HMBtu heat Input per hour, tons of fuel or
feed per year). ._
FUEL AND FEED CHARACTERISTICS
The presence of dloxlns, dioxin precursors (e.g. chlorinated phenols and ben-
zenes), and chlorine In the fuel or feed are believed to be major factors In the emis-
sion of dloxlns from combustion sources. Please Identify the types of fuels and feeds
burned (e.g. oil, coal, wood waste, etc.) and the constituents of Interest (e.g. wood
treated with chlorinated phenols, polyvlnyl chloride Insulated wire, etc.).
COMBUSTION DEVICE OPERATION
If dioxin or precursors are present 1n the fuel or feed to a combustion device,
operating conditions determine If dloxlns are formed and/or thermally destroyed.
Please desclbe briefly, the general operating conditions of the source Including
supporting engineering data , 1f available (e.g. combustion temperatures less than
800 °C, combustion zone residence time less than 1-2 seconds, high moisture content
fuel, unprocessed or bulky fuel, etc.).
CONTROL DEVICE DESI6N AND OPERATION
If dloxlns are present and are not destroyed by the combustor, a control device
which operates below dioxin condensation temperatures and with a high collection
efficiency for fine participate may reduce emissions. Please describe briefly, the
general design and operation of control devices, If known (e.g. fabric filter, ESP,
cyclones, scrubbers, etc.). If the source Is uncontrolled, write In "uncontrolled".
10
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Figure 2-2 - SOURCE DESCRIPTIONS FOR POTENTIAL SCREENING SITES FOR
TIER 4 - NATIONAL DIOXIN STUDY (CONTINUED)
ASH HANDLING SYSTEM DESIGN AND OPERATION
If dloxln 1s produced by a combustion device, the ash handling system design and
notation Is Imoortant In Identifying potential contamination areas and 1n selecting
vices briefl
s mo
ash swllM equipment. For both combustion and control devices, briefly
eny tto a"haMg ^nd disposal systems (e.g. wet sluiced bottom as , pnuematic
ally conveyed ESP ash, hoppers, settling tanks and ponds, storage piles, etc).
COMPLIANCE TEST REPORT
A CODV of the most recent source test compliance report would be beneflda'I If
available? The report would be very useful since It will provide engineering Information
on combustion operations and emissions.
ADDITIONAL PERTINENT INFORMATION (OPTIONAL)
Additional Information will be required to make final determinations of "worst case"
and -rSresen?atl!!eSl?tes and suitability for stack testing. This '"*««" "J^
requested later only for selected sampling sites. OAQPS may access some Jj ^1$ data
froVcDS and NEDS, If available. If however, It Is more wnvlent to provide ttls Infer-
matlon during this request (I.e.. data 1s Incomplete or unavailable In CDS and NEDS),
you might Include it.
The following data are additional Indicators of source performance:
Flue gas constituents - Oz_ % co *'
Emissions data (from source test) - Partlculate NOX S02 VOC .
For locating sampling sites and clarifying source descriptions, maps, plans and
schematics may be attached.
Send To: Bill Lamason, Environmental Engineer
Field Investigation Section, AMTB (MD-14)
U. S. Environmental Protection Agency
Research Triangle Park, North Carolina 27711
11
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Are there any PCDD/PCDF precursors in the feed or fuel (e.g.,
chlorophenol, chlorobenzenes)?
What is the chlorine content of the feed and fuel?
What kind of combustion conditions are present in the combustion
device?
Can an ash sample be obtained?
As discussed in the Tier 4 Project Plan , the majority of the source
categories under consideration are combusting waste products that have the
potential to be contaminated with dioxin/furan precursors such as
chlorinated phenols, chlorobenzenes, or other chlorinated organics.
Chlorinated phenols are widely used as herbicides,fungicides, or
microbiocides. Any combustion sources burning waste products which may have
been contaminated with these materials or any other precursors are potential
sites. In addition, since the formation mechanism of PCDD/PCDF is uncertain
and the precursor hypothesis has not been fully supported, any source
category combusting high chlorine content material (such as PVC or
chlorinated solvents) under poor operating conditions (i.e., low oxygen
content and temperature) may also be a potential site. During the
evaluation of potential test sites in each of the source categories, EPA
will also consider numerous other parameters that could affect the PCDD/PCDF
emissions and the ability to obtain an ash sample. These would include
factors such as combustion device design and operation, presence of a
control device, and the ash generation, collection handling, and disposal
practices. In the selection of "worst case" sites or "typical" sites,
combustion conditions will be a primary selection criteria for site
selection.
The primary inputs to the site selection process will be the source
description data supplied by the regional offices in conjunction with their
candidate list of sites. In addition to this data, general information on
each source category as a whole is being compiled by Radian. This type of
information will allow a determination of representativeness of a
recommended site compared to the overall source categories.
Another criteria that will be used in selecting potential ash sampling
sites will be the availability of data for a candidate site. As discussed
14
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earlier, several regions have submitted lists of candidate sites. However,
completed information sheets are not available for all candidates. In many
instances, only the site name and type of combustion device are provided.
Information pertaining to control devices and ash handling systems have not
been provided. As the site selection effort progresses, further contacts
with the regions may be necessary to obtain additional data on candidate
sites.
15
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3.0 OVERVIEW OF ASH SAMPLING PROCEDURES
The purpose of this section is to outline the steps to be followed by
the personnel conducting the ash sampling at any given combustion source.
As described earlier, OAQPS and Radian will select candidate sampling sites
from lists provided by regional offices. Each regional office will be
notified concerning the sites selected from their region. Sampling kits for
each site will be provided to the designated contacts in the region by
Radian Corporation. After receipt of the sampling kits, the following steps
should be taken.
1. Unpack the sampling kit to verify the contents and to check to see
if the sample jars are clean. If any bottles appear dusty or dirty, the
outside may be wiped with tissue paper wipes provided in the sampling kit.
If the inside of the bottles appear dusty or dirty, do not use the
containers. Notify Radian to receive a replacement kit.
2. Review Section 4.0 of the Ash Sampling Plan (this document)
entitled "Sampling Locations and Methods."
3. Review any site specific data available for the source. Pay
particular attention to details of the control devices, if any, and the ash
handling equipment. Make a preliminary selection of the sampling location
if possible (see Figures 4-1 through 4-4 in the document).
4. Schedule a visit to the facility, discuss the need for site
specific data with the facility prior to the visit (see Section 5.0 of the
Ash Sampling Program Plan) and the potential ash sampling locations
selection in step 3 above.
5. Visit the facility, select the final sampling location in
conjunction with plant personnel, obtain the samples.
6. Wipe off outside of the jars if used for sampling.
7. Attach identifying labels to each sample container. All sample
containers must be sealed in the field with a tamper proof seal. Initiate a
17
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chain-of-custody record for the sample set. Specific instructions for
labeling the samples and for completing the chain-of-custody forms are given
in Section 6.2 of the Ash Sampling Program Plan (this document). Pack the
samples for shipment following the instructions given in Section 6.4 of the
document.
8. Fill out all necessary data forms for the site and pack a copy of
all forms with the samples. The information needed is given in Figure 2-2
and Section 5.0 of the Ash Sampling Program Plan. Prepare and label a
schematic of the combustion device and sampling locations as described in
Section 5.0.
9. Ship the samples to Radian Corporation using the sample shipping
boxes and labels provided (see Section 6.4). Call Radian to inform them of
the date and method of shipment.
18
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4.0 SAMPLING LOCATIONS AND METHODS
This section describes the procedures to be used to identify an optimal
sampling location for the acquisition of an ash sample, and methods that
should be used to acquire the ash sample. General guidelines for the
selection of a sampling location are given. However, the ultimate selection
*
of the sampling location is at the discretion of the sampler. The methods
discussed will vary depending upon the nature of the ash at the sampling
point and the type of conveyance or storage being used. Not all methods
will be applicable to any one given combustion source. The sampling methods
described focus on sampling from moving solid or slurry streams i.e.,
conveyors, pipes, sluices, etc. For the Ash Sampling Program, it is
recommended that samples not be taken from storage piles, ponds, or
containers due to the difficulty of getting a representative sample. It may
be necessary, however, to take a sample from a live storage hopper, such as,
at the bottom of a baghouse or electrostatic precipitator. The best source
of information regarding the feasibility of any sampling location, and the
physical characteristics of the collected ash at the location is the
facility staff. The sampler should endeavor to involve facility personnel
in the sampling location selection process as early as possible.
4.1 SELECTION OF A SAMPLING LOCATION
To determine the appropriate sampling location the following general
criteria should be used:
*
Throughout this section, the term "sampler" is used to denote the
individual responsible for conducting the actual sampling. This may be
someone from a regional office, State or local agency, a facility operator,
or contractor personnel.
19
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(1) The sampling should be from the ash stream that is farthest
downstream from the combustion process or where the smallest size ash is
collected.
(2) The sampling point or points should provide representative samples
that can be collected by the standard sampling acquisition and analysis
hardware. For the Ash Sampling Program, locations where the sample jar can
be used directly to obtain samples are preferred.
(3) The sample should be collected from a moving stream of solid or
slurry (i.e., conveyor, pipe, sluice, etc.) when possible.
(4) When possible, each sampling point should provide a representative
sample of the stream. In some instances, ash or flue gas streams from
several combustion sources at a facility will be combined. Only one of the
combustion sources may be the focus of the Ash Sampling Program. In this
case, sample points downstream of where the ash streams combine will not be
representative of the one source.
In order to select the optimal sampling location that meets the above
broad characteristics, the sampler should perform the following steps:
(a) Trace the flow of combustion gases from the combustion device
through the heat recovery devices and control devices. This
involves the physical inspection of the duct work from the
combustion device to the stack.
(b) Locate and itemize control devices, stacks, and sampling locations
for ash. These include: ash hoppers at the bottom of boilers,
discharges from mechanical cleaning devices such as cyclones, and
ash hoppers on control devices such as ESP's or fabric filters.
These hoppers should be "live" storage hoppers.
(c) Determine if the physical parameters of the gas streams at each
sampling location are available. This is important since a
temperature history of the ash is needed in order to fully
interpret the data.
Since a slurry stream requires more in-depth analysis of sampling
locations, the sampler should consider the following factors:
20
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(a) The stream homogeneity. This is the most important problem that
must be addressed by the sampler. Unlike gas streams, which mix
fairly evenly, liquid streams tend to be more stratified because
of lower agitation and higher fluid viscosities.
(b) Stream flow rates. Large slow moving streams will offer more of a
chance for stratification. This factor is especially important in
large pipes or open ditches.
For all sampling the sampler should attempt to identify points where
the ash in a moving stream can be sampled. This is much preferred over
sampling from a storage bin or hopper. Sample consistency is also
important. It is preferable to sample finely divided material rather than
large coarse material since is easier to get a more representative sample
of a fine material. Finally, if several sampling locations are available,
the sampler should select the location farthest downstream from the
combustion device, or where the finest particulate is being collected.
Several studies have shown that dioxins/furans are preferentially enriched
on the smallest particulate (ash). If dioxins/furans are present, they will
most likely be found in the finest and coolest ash leaving the combustion
device or control device. For these reasons fly ash will be preferred over
bottom ash, and ash from the second control device in series is preferred
over ash from the first.
A general schematic of a generic combustion device with two control
devices in given in Figure 4-1. When faced with this situation, the sampler
should try to sample at the second control device. The preferred location
would be Point 3, the collected particulate from the control device, where
the stream is being conveyed to the storage or disposal location, not
Points 5 or 6, the storage or disposal site. Point 3 would represent the
smallest collected particulate and the coolest .ash sampling location in the
system. Following identification of the candidate sampling locations, the
sampler should review the location criteria listed above, prioritize the
locations with respect to meeting these criteria, and select the optimal
location.
21
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Process
Sludge
Solid
T
Process
'
Combustion
Device
*" *
Bottom Ash/
SI
^
Control Device
Example Cyclone
or Mechanical
Collection
^
Coll
f
icted
Control
Device
Example
Scrubber or ESP
^
Scru
t
iber
X.
Stack
ag Ash Sludge
' .^ >
or
ESP
Ash
f _
Truck/
Holding Area
.
Landfill (7
Pile
Holding Pond
*This sampling location could be extremely hot. Care shoul.d be taken if
bottom ash is to be taken directly upon leaving the combustion device.
O Denotes potential sampling locations.
Figure 4-1. Generic plant with example ash sampling sites.
22
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Prior to actual sampling, the sampler should ascertain the operating
status of the combustion device, and determine at what rate.the waste and/or
fuel of interest is being fired. After sampling, the sampler should ensure
that he has acquired all of the site specific data needs discussed in
Section 5 of this report, including the applicable flue gas temperatures and
combustion and control device operating conditions.
4.2 SAMPLE SIZE
Two 950 ml capacity sample jars will be provided. One or more grab
samples of ash (sludge, liquid, etc.) should be placed in each container.
The sample or samples should be of sufficient size to fill a container half
to three-quarters full (approximately 500 grams per jar).
Two samples should be taken for each site, and the total sample size
shipped to Radian should be 1/2 to 1 kg. This sample size will be
sufficient to fulfill all analytical requirements.
It is anticipated that the time required to obtain two samples will be
less than 1 hour. For the purposes of the Ash Sampling Program, integrated
sampling over 4 hours (the sample period for stack testing) is not
necessary.
4.3 SAMPLING METHODS
The following subsections describe the preferred methods for acquiring
samples for the Ash Sampling Program. Only grab samples of ash are needed
to fulfill the objectives of the program. The methods described below are
modified grab sampling methods based for the most part on methods proposed
by ASTM, EPA, or other organizations. In all instances, the methods have
been simplified. Methods for sampling ash from moving streams and live
hoppers are described. Only simple sampling equipment is needed to obtain
ash samples for the program. Where possible, the sample containers should
23
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be used as the sampling equipment. For example, if cool ash from a conveyor
is. to be sampled, the sample jars can be used to scoop ash from the stopped
conveyor or can be held in the falling ash stream at the discharge end of
the conveyor. The intent of the sampling methods described is to obtain an
ash sample that has not been contaminated with other materials and that is
as representative as possible.
Combustion device ash encountered during this program may be solids,
sludges, slurries, or liquids, depending upon the design of the ash handling
system and/or the type of particulate collection device. The recommended
methods for acquiring the various types of ash samples are summarized in
Table 4-1 and are discussed below.
The most typical sludge/solid streams will be bottom ash and
particulate control device solids. Sludges are defined as material which
contains at least 20 percent moisture but do not flow. They do not move
freely as a slurry would'and do not mix well when stored or contained.
Solids are defined as materials which contain less than 20 percent moisture.
Solids may or may not mix or flow well. The sampling methods utilized
during this program will depend upon the state of the material and the
sampling location.
Figures 4-2 through 4-4 show recommended sampling locations for some
particulate control devices that may be encountered. If possible, ash
samples should be taken from moving streams and not from storage or disposal
hoppers. In all instances, sampling locations and procedures should be
discussed with plant personnel. The facility operators may prefer to
conduct the ash sampling at any location because of safety problems
associated with access to moving equipment or sampling of hot streams.
4.3.1 Sampling of Ash on Conveyor Belts or in Screw Conveyors
4.3.1.1 ASTM "Stopped-Belt Cut" Method (D2234-76). This method
covers sampling of solid materials transported on conveyor belts that can be
stopped for an appreciable amount of time without disrupting plant
operations (i.e., several minutes). This sampling method can be applied to
dry bottom ash, char or slag, and sludge.
24
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TABLE 4-1. RECOMMENDED SAMPLING METHODS FOR ASH SAMPLING
Sample Location
Sample Method
Section
Ash pit
Live hopper
Conveyor belt
Sluice
End of pipe
Pipes
Scoop or shovel through
access door
Scoop or shovel through
access door
Stopped belt
Dipper/scoop
Dipper/scoop
Tap
4.3.2
4.3.1
4.3.3.1
4.3.3.2
4.3.3.3
25
-------
CL>
CD
C
o
c
T3
CM
I
OJ
3
cn
26
-------
OJ
cn
1 5?
(/I
to
-------
a <
I
t
\
t
\
\
\
\
«> ***
< ±
a e
tM
a a
u
\ 3
\
O)
O
l/l
o>
c
O
28
-------
This is the most favorable method for obtaining a representative sample
of materialon a conveyor belt. With the belt stopped, a full-stream cut is
obtained from the belt with a shovel and brush (for fine material). The
width of the cut must be at least three times the diameter of the largest
particle or 1.25 inches, whichever is greater. Also, the sides of the cut
must be as nearly parallel as possible. The sample material can be placed
into a storage container for transport to the lab or may be put directly
into sample bottles if no other processing is required.
For measuring the width of the cut required, the diameter of the top
size particles must be known (to set the minimum width allowable, as
described above). A measuring tape can be used to mark off the correct
width. Sample material can be removed with a shovel or with a dustpan and
brush for fine-grained material. Samples can be transferred to large
buckets or boxes with a large funnel or scoop. The sampling equipment must
be clean and dry before use.
The stop-belt method, as the name implies, can only be used at
facilities where the conveyor system can be interrupted long enough to
remove samples without disrupting plant operations. The sampling point(s)
selected should allow complete access to either sides of the belt and should
be close to a floor or platform a facilitate moving and storing sample
containers and equipment. There should be sufficient work space so that
sampling personnel can shovel or scoop solids or sludge directly from the
belt into containers. There should also be adequate space for personnel to
stand clear of the belt if it is accidentally started.
4.3.1.2 ASTM "Part Stream Cut" Method (D2234-76). This method covers
sampling of solids that are transported on moving conveyor belts and
vertically falling material where access to the entire belt width is limited
for some reason or cases when no full-stream sampling is available. Thus,
samples obtained by this method are somewhat less representative than those
from a full cross-section. This method may be used where a cross-stream
sampler has not been installed or where space limitations prevent taking a
complete cross-section. Typically, a shovel or trough is moved quickly
through the stream of material falling from the end of the belt, without
29
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allowing material to bounce back out of the trough or fill the trough and
overflow. The shovel may be plunged into the sample stream several times in
different locations to obtain a representative increment.
Equipment needs include a shovel to remove sample material, compositing
containers, and sample containers. For cool ash streams, the sample
containers themselves can be held under the stream of falling material at
the end of the belt. After filling the jars, wipe the outsides, label, and
pack for shipment.
Typical sample collection procedures involve inserting a large shovel
or trough into the stream of material falling off the end of the belt.
Collected material is then transferred to the sample containers, and the
process is repeated until a sufficient amount or number of samples have been
taken.
4.3.2 Sampling of Ash From Live Storage Hoppers on Control Devices or
Bottom Ash Hoppers on Combustion Devices.
In many instances, samples of dry ash or collected particulate can be
obtained directly from live storage hoppers prior to being sent to disposal.
Access doors or ports are generally available in these hoppers. The
availability of sampling locations for live hoppers and the intent of the
sampling should be discussed with plant personnel prior to the visit.
Sampling from these locations is best performed by plant personnel since the
material may be hot and access to operating equipment is necessary.
Samples can be collected by gravity flow or by shovel into clean
buckets and allowed to cool prior to placing into shipping jars.
4.3.3 Sample of Ash Slurries From Sluices or from Pipes
4.3.3.1 Dipper/Scoop. Grab samples of ash sludge or slurry material
may be collected if access to a sluiceway is available. The grab sample
should be collected with a modified dipper or with a sample container. This
method may also be applicable if access to an underground pipe through
manholes or other access points is available.
The dipper used for grab sampling is constructed of a wide mouthed
metal container (1 liter volume) attached to an end of a telescoping
30
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aluminum or fiberglass pole. The dipper collects sludge samples directly
from the sludge waste stream, and the sample is then transferred to an
appropriately sized temporary storage container.
To take a grab sample with a dipper, the dipper is cleaned, mounted on
a telescoping pole, and inserted into the stream at the desired depth with
the mouth of the container down. The dipper should be turned over to an
upright position, allowing the container to fill completely. The dipper can
then be removed from the sludge, and the sample transferred to a temporary
storage container. This process should be repeated until sludge has been
collected. If a dipper is not available, a sample can be taken by inserting
a clean sample jar into the stream, allowing it to fill, and then removing
from the stream. The outside of the jar should be wiped clean prior to
packaging.
Precaution should be taken to avoid loss of the sampling device if the
waste stream is moving at a high velocity.
4.3.3.2 End of Pipe Samp!ing. These methods provide a procedure for
obtaining slurry waste samples from a pipe discharge, for example, at a
settling pond or lagoon using a dipper sampler. The method applies to all
slurry-type wastes.
This method is less favorable than isokinetic sampling, since mixing
conditions and sample homogeneity ahead of the pipe end cannot be predicted.
The method involves using a dipper or large open-mouthed bottle or bucket to
obtain a cross-sectional portion of the liquid or slurry flowing from the
end of the pipe. Since flow streams containing solids tend to be stratified,
several samples from different locations in the stream should be taken.
End-of-pipe sampling is most conveniently done with a dipper. This can
be fabricated from a wide-mouth bottle affixed to a wooden handle or other
extension. If the pipe end is very accessible, large buckets may also be
used. Samples can be composited in buckets or other clean containers. For
Application of a dipper sampler as described in (EPA, Office of Research
and Development, "Emissions Assessment of Conventional Stationary Combustion
Systems: Methods and Procedures Manual for Sampling and Analysis," 1979).
31
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the purposes of the ash screening program, the sample jars can be used to
collect the end of pipe sample directly if no dipper or bucket is available.
The dipper, sample jar, or bucket sample at the end of a pipe is
obtained by inserting the sampler into several different portions of the
outfall, so as to collect a representative cross-section of the material.
The individual increments can be composited in a large bucket or lined drum
prior to filling the shipping jars. When these samples are taken, safety
precautions are very important, especially where the discharge has a high
velocity or where access to the pipe is somewhat precarious. [Sampling
personnel may secure the bucket with a length of line, and/or use a safety
harness secured by another person (especially around ponds or lagoons).]
4.3.4 Sampling of Ash Containing Liquids (e.g., Scrubbers)
Tap sampling, Figure 4-5, is the appropriate method for sampling moving
liquids in pipes or ducts. Slurries in motion are sometimes sampled by tap,
but this is unreliable if the solids content is much greater than
10 percent.
To acquire a tap sample, the outlet of the valve or stopcock used for
sample removal is fitted with a length of precleaned TeflonR tubing
sufficiently long to reach the bottom of the sampler container. After the
p
Teflon conduit line has been placed in the sample container, the tap is
opened to admit a moderate flow of liquid. The conduit line, but not the
sample container, should be flushed before the sample is actually taken.
Flushed material should be returned to the process.
If the sample temperature is above about 50°C, the sample should be
cooled before being placed in a sample container. Cooling the sample can be
n
affected by using a longer length of Teflon conduit line, coiling it, and
placing it in an ice-water bath. Again, the tap is opened, and the liquid
is discharged until possible sediments and gas have been flushed. Then the
sample container is filled.
A moving liquid stream, known to contain particulate matter or
immiscible phases, will be considered stratified. The optimum location for
a sampling tap will be after a bend or constriction which will induce
turbulence or at least promote mixing. Only the main pipe or stream flow
should be sampled. Taps in vents or slipstreams are not recommended because
solids can accumulate.
32
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LINE
OR
TANK
WALL
S -J-v
« A
V'
6.4 rrm
(V4 In.)
Figure 4-5. Schematic of tap sampling,
33
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-------
5.0 SITE SPECIFIC DATA NEEDS
This section describes the site specific data needed for each ash
sampling site in order to utilize the data in the final Tier 4 dioxin study.
As part of the final analysis, a comparison will be made between the
ash sampling results for various source categories and the combined ash and
stack sampling results from similar categories. Sufficient information is
needed for each ash sampling site to allow a comparison to be made or to
identify factors which may affect emissions. This information consists of
two types, source category or subcategory information, and sampling location
information. Much of the source category information will already have been
gathered and submitted to EPA by the time a source is selected for ash
sampling. As previously discussed, the regions have been asked to submit
some source specific data for each candidate site identified. This
information is summarized in Figure 2-2.
In addition to this information, the specific sampling location and
site operation information listed in Figure 5-1 is also needed. A schematic
of the sampling location indicating key parameters should also be submitted
along with the samples. An example schematic is given in Figure 5-2. If
possible, photographs of the sample locations would be a useful supplement
to the schematic drawing.
35
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FIELD DATA SHEET:
SAMPLE IDENTIFICATION AND PROCESS OPERATION
ASH SAMPLING PROGRAM
TIER 4 - NATIONAL DIOXIN STUDY
1. Sample site identification
2. Sampling organization
3. Date of sampling
4. Combustion device identification
5. Number of samples taken, frequency of samples
e.g., 3 samples, 1 every 2 hours
6. Combustion device feed rate and/or load
7. Combustion device fuel type(s) during sampling
8. Sampling locations
Brief description of location and pertinent stream characteristics;
e.g., from figure, sample port in scrubber blowdown line,
ash slurry, X percent solids combined with limestone.
9. Physical characteristics of gas stream at inlet and outlet of
collection device.
Temperature, Q£, CO, particulate concentration.
10. Schematic of location and ash handling system (See Figure 5-2).
11. Notes or comments on unusual conditions occurring during the sampling
period, if any.
Figure 5-1. Field data to be collected during sampling.
36
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i- S.
OO "O
C7>
C
2
O
o
2
o
-------
-------
6.0 SAMPLE CONTROL, PACKAGING, AND SHIPPING
The purpose of this chapter is to outline the procedures for sample
scheduling, identification, documentation, and shipping. The States and
EPA regional offices performing the ash sampling will interface with OAQPS
which will coordinate acquisition of sample control numbers and requisition
of sampling kits. Radian Corporation will provide all of the sampling kits
to the State and EPA regional offices. Following site selection by Radian
and OAQPS (see Section 2), the regional offices will be informed of the
number and type of sites in their region to be sampled. At this time, the
region should ensure that all of the necessary site specific information has
been provided and that the type of sample and the sampling location has been
specified. At the time of site selection, Radian will indicate the
anticipated sample type and sample location based upon available
information.
The regions should contact the site(s) and schedule a sampling visit.
At least 2 weeks prior to the visit, Radian Corporation should be contacted
to schedule shipping of sample kits (see Section 6.1). Following sampling,
the samples should be labeled as prescribed in Section 6.2. Chain-of-
custody procedures and shipping requirements are given in Section 6.3.
6.1 CONTROL OF ASH SAMPLING KITS
To ensure that the ash sampling study fulfills project objectives, a
shipment tracking system will be utilized at Radian to facilitate proper
identification and timely analysis of all collected samples. Once a source
has been identified and is included in the sampling program, a sampling kit
tracking record will be initiated at Radian/RTP through use of a
microcomputer based software program. Example printouts of the information
which will be recorded for every site are given in Figure 6-1.
39
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SITE SAMP. CODE SCCtt EPISODE* CONTACT
DATE AIR BILL* TRANS,
LOCATION:
SAMPLE CODE:
SCC NO.:
EPISODE NO.:
CONTACT NAME:
SHIP TO DATE:
AIR BILL NO.:
HONEY-RYE FIELD
AGB-1
DQO00101
2487
T.HARRISON(DOA)
9-25-84
XXXXXXX
TRANS. MODE: FEDERAL EXPRESS
RETURN DATE:
AIR BILL NO.:
TRANS. MODE:
REC'D. BY:
COMPOSITED BY:
SAMPLE COND.:
10-3-84
289-783-266
FEDERAL EXPRESS
R.JONGLEUX
R.JONGLEUX
SCREENED ASH
ANALYZING LAB I.D.: EPA-BSL
SHIP TO DATE: 10-19-84
AIR BILL NO.: 298-783-491
TRANS. MODE: FEDERAL EXPRESS
Figure 6-1. Example: Shipping record tracking
40
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In order to ensure continuity with the National Dioxin Study, sample
control numbers will be coordinated through Mr. Ed Hanks of OAQPS/AMTB at
(919) 541-5575 or FTS 629-5575. Mr. Hanks will issue the SCC numbers and
episode numbers which he will obtain from the SCC. This information will be
entered into Radian Tier 4 sample kit tracking system.
6.1.1. Scheduling of Ash Sampling Kits
Radian Corporation's Research Triangle Park office under EPA contract
will provide sampling kits for the collection of ash samples for
dioxin/furan analysis. Once sampling is scheduled, and at least 2 weeks in
advance of the sampling date, the region should contact Radian Corporation
(919)541-9100 to obtain sampling kits. Refer to the Tier 4 - Ash Sampling
Program. At this time, the region should provide the following information:
Name and address to which sampling kits should be sent,
Number and type of samples to be collected;
The type of sample to be collected (e.g., dry bottom ash, ESP
catch, scrubber blowdown) and the proposed sampling location
(e.g., access port on a line bottom hopper, convey or belt, tap,
or blowdown line. Some of this information may have been provided
as part of the initial data submitted by the regional offices.
The sampler may have to call or visit the facility prior to
sampling to ensure that this information is available;
Name of requester;
- Group that will be performing sampling (e.g., regional sampling
team, contractor organization), with name, telephone number, and
address of sampling contact(s);
Name and telephone number of primary regional or contractor
contact(s) for problem resolution;
Site name and location (city and State), an EPA site
identification number (if applicable), and latitude and longitude
of site;
Scheduled date(s) of sample collection;
41
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Any other pertinent information that may.impact sample scheduling
and shipment (e.g., any changes from original site sampling plan,
anticipated delays due to weather, equipment, or other
conditions); and
Date kits must be received by regions or samplers.
The sampling kits will contain precleaned glass bottles and sample
collection devices if required, as well as other items needed to package and
ship the samples.
6.2 LABELING AND HANDLING OF SAMPLES
In order to ensure data quality and sample record maintenance,
established quality assurance procedures must be followed in the labeling
and transport of samples. This section described the detailed procedures
for transfer of samples to the Radian laboratory for compositing.
6.2.1 Labeling of Samples
Each sample collected for analysis will be placed in a 1 liter (!)
sample container per the procedures described in Section 3. Each sample
bottle shall have a sample label as shown in Figure 6-2, with the following
information:
Sample code,
Container number,
Date,
Facility location,
Field number (Episode),
SCC number, and
Remarks.
6.2.1.1 Specific Label Entries. The sample labels shall identify
specifically the sample site and type of sample. Each site will be
identified by a 4-digit episode number (listed in the upper right hand
corner of the sample label under field number and chain-of-custody record
enclosed in the sampling kit). The consistent use of these label entries
will aid in the comparison of like samples and accounting of the types of
42
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ATTENTION:
BEFORE OPENING
MOTf IF BOTTLE WAS
TAMKftEO WITH.
RADIAN
SAMPLE CODE:
SCC NO
Progrms C«fll«f / 3200 E Chap*) Mill Bo i
Nvison Highway / P O 801 13000
R«MWCh TriangM Park. NC 27709'(9l9lS4i 9100
.CONTAINER NO.
ATTENTION:
BEFORE OPENING
NOTE IF BOTTLE WAS
TAMPERED WITH.
Figure 6-2a. Chain-of-custody seal.
CORPORATION
Progress C«ntsf/3200 E. Chap«l HIM Rd./
N^son Highway/P.O. Boi 13000
R«s««reli Trianflto Park, NC 27709/(919)541-9100
FIELD NO:
SAMPLE CODE
SCC NO
CONTAINER NO.
LOCATION:
DATE:
REMARK:
.CONTRACT:
__FINAL WT:
TARE:
SAMPLE WT:
Figure 6-2b. Sample label.
43
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samples received by the laboratory. Site coding will be by type of source
category and a numeric sequence. There are 18 source categories. There may
be up to four sites in each category (see Figure 6-3 for list of source
category codes). A record of site assigned numbers will be maintained
through the source of a sample tracking system at Radian/RTP.
An example entry for the first industrial boiler site supplying a
sample for the Ash Sampling Program would be as follows:
RADIAN
CORPORATION
R«M*rch TrlangU Park, NC 27709/<919) 541-9100
SAMPLE CODE X B - I
SCC NO.
CONTAINER NO. _i
LOCATION: _
DATE \\l*/Q4r _ CONTRACT:
REMARK: _ FINAL WT:
SAMPLE WT:
When the label is completed, it should be firmly attached to the sample
container and covered with clear tape. At least two tape strips should
completely circle the sample container to prevent losing the label
(Figure 6-2). Place a chain-of-custody seal across the taped lid so that
the jar cannot be opened without tearing the seal.
6.3 SAMPLE CHAIN-OF-CUSTODY RECORD
Each group of sample bottles shipped to Radian/RTP will be accompanied
by a sample chain-of-custody record (Figure 6-4). A separate chain-of-
custody will be completed for each site sampled. This record includes the
information on the sample label as well as a record of the chain-of-custody
of the particular sample.
44
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SEQUENTIAL CODE, SOURCE CATEGORY
AHI Apartment House Incinerator
AK Aggregate Kiln
AP Asphalt Plant
BLB Sulfate Black Liquor Recovery Boiler
CB Commercial Boiler
CEM Carbon Electrode Manufacturing
CK Cement Kiln
CM Charcoal Manufacturing
CRF Carbon Regeneration Furnace
DBR Drum and Barrel Reconditioning
HWI Hazardous Waste Incinerator
IBa Industrial Boiler
MET Metals Processing
MSWI Municipal Solid Waste Incinerator
OB Open Burning
SLB Sulfite Liquor Recovery
SSI Sewage Sludge Incinerator
UB Utility Boiler
ISW Industrial Solid Waste Incinerator
Including Hospital Incinerators
WRI Wire Reclamation
WFB Wood-Fired Boilers
alncludes wood fired and coal (spreader stoker) boilers.
Includes blast furnaces, ferrous and nonferrous foundries, secondary
copper and aluminum smelters, and wire reclamation incinerators.
Figure 6-3. Source category codes to be used on sample labels
45
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When the sample is taken, the sampler signs the custody record under
chain of possession and also enters the date and time sampled. The
chain-of-custody form must be placed inside the plastic pouch provided and
taped to the inside lid of the shipping box. A chain-of-custody seal is
placed on the outside of the shipping container once all labeling and
package sealing have been completed (see Figure 6-2a for an example of the
seal) so that the package cannot be opened without tearing the seal. If and
when the sample is passed to a second party for transport, no signature will
be required on the custody record. The bill of lading or air bill will
serve as documentation.
The receiving party signs line 2-of-the chain of possession record
upon receipt. The receiver also enters his name and address in the "sample
receiver" section. (When the sample is transferred to the Troika
laboratory, the inclusive date will be closed by the Radian laboratory.
All Dioxin Shipment Record (DSR) forms will be completed by Radian at
RTP once the ash samples have been composited. The DSR form will be
completed for each sample site and checked to verify its accuracy against
the shipping information received for individual sites. The use of the SCC
DSR form at this point in the process will allow for a coordinated control
point so that the ash samples can be effectively scheduled for analysis with
SCC. Distribution of the five part DSR form will be- the responsibility of
Radian once the sample is composited.
6.4 SAMPLE SHIPMENT
For purposes of collecting and shipping ash samples for the EPA Tier 4
National Dioxin Study (Ash Sampling), a shipping container has been
*
developed. This container measures 12 x 12 x 12 and will accommodate two
1-liter bottles.
47
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The procedure for use of these containers is as follows:
1. Radian will ship the bottles in the container without markings on the
box. Enclosed will be two bottles, the sampling procedure, and the
required labels, forms, and Teflon tape for sealing the samples.
2. The sampler will remove all of the materials, collect the samples as
specified in the Ash Sampling Program Plan and repack as follows:
a. Seal the bottle lids with the enclosed teflon tape, stretch the
tape around the licU-and label per the sampling procedure.
b. Place the filled bottle in a bag and horse tail tie the bag.
c. Place the bagged sample in the fitted box liner.
d. Tape the plastic pouch with the chain-of-custody form and sampling
data sheet to the inside lid of the box.
e. Place the enclosed shipping label on the outside of the box per
the diagram and tape securely around all four edges. Be sure not
to cover any sample labeling.
f. Notify Radian at (919) 541-9100 when shipping the samples. Please
refer to Tier 4 - Ash Sampling.
There should be little confusion regarding box packaging as boxes will be
*
form fitted with foam for the bottles. Due to gross weight limitations,
ship only two samples per box.
All samples should be shipped immediately to Research Triangle Park, NC
by Federal Express, or other expeditious means as provided with the enclosed
shipping order. Sample boxes should be identified and labeled as shown in
Figure 6-5.
48
-------
TOP
OF
BOX
TOP OF BOX
HAZARDOUS SUBSTANCE,
SOLID, NOS.
ORM-E
NA 9188
ADDRESS LABEL
SIDE
HAZARDOUS SUBSTANCE SOLID NOS.
ORM-E
NA 9188
ADDRESS LABEL
ATTACH SHIPPER'S CERTIFICATION ON SIDE OF BOX
FEDERAL EXPRESS FORMS (folded with
address information visible)
Figure 6-5. Sample box identification and markings.
49
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Any questions may be directed to:
Radian Corporation
Post Office Box 13000
3200 E. Chapel Hill Blvd/Nelson Highway
Research Triangle Park, North Carolina 27709
(919) 541-9100
Attention: Andrew Miles or Bob Jongleux
Please reference: Tier 4 - Ash Sampling
6.5 SAMPLE CONTAINER PREWASHING
.In order to prevent contamination of samples and to provide a
consistent analysis basis, all sample containers must be precleaned using
the same procedure. All sample bottles and materials in the sample kit have
been precleaned for your convenience.
The sample bottle cleaning procedure is as follows:
USE DISPOSABLE GLOVES AND ADEQUATE VENTILATION
___
1. Soak all glassware in hot soapy water (Alconox ) 50°C or higher.
2. Tap H20 rinse (x3).
3. Distilled/deionized H^O rinse (x3).
4. Chromerge rinse if glass, -otherwise skip to 6.
5. HPLC H20 rinse (x3).
6. Acetone rinse (x3), (pesticide grade).
7. Hexane rinse (x3), (pesticide grade).
8. 'Oven dry (110°C - 1 hr).
9. Cap containers with Teflon lids. Foil wrap the sampling equipment.
50
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eest reaa instntenons on me reverse oefon completing}
1. REPORT NO.
EPA-450/4-84-014d
4. TITLE ANO SUBTITLE
National Dioxin Study Tier 4
Ash Sampling Program
2.
Combustion Sources
7. AUTHORS)
A. J. Miles, R. F. Jongleaux
9. PERFORMING ORGANIZATION NAME Af
Radian Corporation
P.O. Box 13000
Research Triangle Park, Nort
4Q ADDRESS
ti Carolina 27709
12. SPONSORING AGENCY NAME ANO ADDRESS
EPA, Office of Air Quality Planning and Standards
Monitoring and Data Analysis
Research Triangle Park, N.C.
Division
27711
:i. RECIPIENT'S ACCESSION NO.
9. REPORT DATE
January 1985
6. PERFORMING ORGANIZATION CODE
10. PROGRAM ELEMENT NO.
B53B2K
11. CONTRACT/GRANT NO.
68-02-3850
13. TYPE OF REPORT ANO PERIOD COVERED
Final
14. SPONSORING AGENCY CODE
IS. SUPPLEMENTARY NOTES
EPA, Project Officer: William H. Lamason II
18. ABSTRACT
This document describes the Ash Sampling Program that will be conducted at selected
combustion sources under Tier 4 of the National Dioxin Study. Flue gas ash samples
will be collected and analyzed for 2,3,7,8-tetrachlorodibenzo-p-dioxin (2,3,7,8 TCDD),
tetra- through octa-polychlorinated dibenzo-p-dioxins (PCDD), and tetra- through octa-
polychlorinated dibenzofurans (PCDF). The activities that will be performed by EPA's
Office of Air Quality Planning and Standards, the EPA Regional Offices, State and local
agencies, and the EPA contractor, Radian Corporation, in the program are identified.
Specific guidance is provided for the organizations that will perform the field sampling
in the program.
17.
a.
KEY WORDS ANO DOCUMENT ANALYSIS ~"~
DESCRIPTORS
Ash Screening
Ash Sampling
Combustion Source Sampling
Dioxins TCDD
Furans TCDF
2,3,7,8 Tetrachlorodibenzo-p-dioxin PCDD
- Polychlorinated dibenzofurans PCDF
18. O'STRiauT-ON STAT
5M6NT
b.lOENTI PIERS/OPEN ENDED TERMS
Air Pollution Sampling
Waste Sampling
19. SECURITY CLASS tTliU Repon)
Unclassified
20. SECURITY CLASS (THu ptftl
Unclassified
c. COSAT1 Field/Group
21. NO. Of PAGES
60
22. PRICE
2220-1 (R«». 4-77)
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