United States Office Of Air Quality EPA-454/R-00-026
Environmental Protection Planning And Standards May 2000
Agency Research Triangle Park, NC 27711
_
&EPA
HOT MIX ASPHALT PLANTS
TECHNICAL SYSTEMS AUDIT of
TESTING at PLANT C
ASPHALT PLANT C
LOS ANGELES, CALIFORNIA
U.S. Environmental Protection Agency
Region 5, Library (PL-12J)
77 West Jackson Boulevard, 12th Floor
Chicago, IL 60604-3590
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EPA-454/R-00-026
HOT MIX ASPHALT PLANTS
TECHNICAL SYSTEMS AUDIT of TESTING at PLANT C
ASPHALT PLANT C
LOS ANGELES, CALIFORNIA
U.S. Environmental Protection Agency
Region 5, Library (PL-12J)
U.S. ENVIRONMENTAL PROTECTION AGENCY
Office of Air and Radiation
Office of Air Quality Planning and Standards
Research Triangle Park, North Carolina 27711
May 2000
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DISCLAIMER
The information in this document has been funded wholly or in part by the Office of Air
Quality Planning and Standards, U.S. Environmental Protection Agency (EPA) under contract
68-D4-0091 to Research Triangle Institute. It has been reviewed and revised by the Emissions
Measurement Center Quality Assurance Officer. It has been approved for publication as an EPA
document. Mention of trade names or commercial products is not intended to constitute
endorsement or recommendation for use.
in
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IV
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Preface
This report was produced by the Source Measurement Technology Group of EPA's Emissions
Measurement Center located in Research Triangle Park, NC. It is one of a series of twelve
reports prepared to document an EPA emission test program to characterize emissions to the air
from hot mix asphalt plants. These twelve reports and their associated EPA document numbers
and publication dates are:
Document Tide
Hot Mix Asphalt Plants
Emission Assessment Report
Hot Mix Asphalt Plants
Kiln Dryer Stack Instrumental Methods Testing
Asphalt Plant A, Gary, North Carolina
Hot Mix Asphalt Plants
Kiln Dryer Stack Manual Methods Testing
Asphalt Plant A, Gary, North Carolina
Volume 1 of 2
Volume 2 of 2
Hot Mix Asphalt Plants
Kiln Dryer Stack Instrumental Methods Testing
Asphalt Plant B, Clayton, North Carolina
Hot Mix Asphalt Plants
Kiln Dryer Stack Manual Methods Testing
Asphalt Plant B, Clayton, North Carolina
Volume 1 of 2
Volume 2 of 2
Hot Mix Asphalt Plants
Truck Loading and Silo Filling Instrumental Methods Testing
Asphalt Plant C, Los Angeles, California
Hot Mix Asphalt Plants
Truck Loading and Silo Filling Manual Methods Testing
Asphalt Plant C, Los Angeles, California
Volume 1 of 8
Volume 2 of 8
Volume3 of 8
Volume 4 of 8
Volume 5 of 8
Volume 6 of 8
Volume 7 of 8
Volume 8 of 8
EPA Document
Number
EPA454/R-00-019
EPA 454/R-00-020
EPA454/R-00-021a
EPA454/R-00-021b
EPA 454/R-00-022
EPA 454/R-00-023a
EPA 454/R-00-023b
EPA 454/R-00-024
EPA 454/R-00-025a
EPA 454/R-00-025b
EPA 454/R-00-025C
EPA 454/R-00-025d
EPA 454/R-00-025e
EPA 454/R-00-025f
EPA 454/R-00-025g
EPA 454/R-00-025h
Publication
Date
April 2000
April 2000
April 2000
April 2000
April 2000
April 2000
May 2000
May 2000
May 2000
May 2000
May 2000
May 2000
May 2000
May 2000
May 2000
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Document Title
Hot Mix Asphalt Plants
Technical Systems Audit of Testing at Asphalt Plant C
Asphalt Plant C, Los Angeles, California
Hot Mix Asphalt Plants
Truck Loading Instrumental Methods Testing
Asphalt Plant D, Barre, Massachusetts
Hot Mix Asphalt Plants
Truck Loading Manual Methods Testing
Asphalt Plant D, Barre, Massachusetts
Hot Mix Asphalt Plants
Response to Comments on Testing Program for Asphalt
Plants C and D
Hot Mix Asphalt Plants
Stakeholders Opinions Report
EPA Document
Number
EPA 454/R-00-026
EPA 454/R-00-027
EPA 454/R-00-028
EPA 454/R-00-029
EPA 454/R-00-030
Publication
Date
May 2000
May 2000
May 2000
May 2000
These documents, including this Response to Comments document, are available for downloading, on
CD-ROM and in paper.
Downloads can be made from:
http//www.epa.gov/ttn/emc/asphalt.html
Copies of the CD ROM can be requested by mail at:
Emission Measurement Center, MD-19
US Environmental Protection Agency
Research Triangle Park, NC 27711
Paper copies of the reports can be obtained from:
National Technical Information Service
5285 Port Royal Road
Springfield, VA 22161
Phone orders 1-800-553-6847 or (703) 605-6000; FAX orders (703) 605-6900
http://www.ntis.gov/products/environment.htm
Acknowledgments
Many individuals contributed to the development of this report. Laura Autry of EPA's Air Quality
Trends Analysis Group, R.K.M. Jayanty of Research Triangle Institute (RTI) and Robert S. Wright of
RTI are the primary authors of the report. David Mobley, Acting Director of EPA's Emissions
Monitoring and Analysis Division, Conniesue Oldham of EPA's Air Quality Trends Analysis Group,
Bill Lamason and Gary McAlister of EPA's Emission Measurement Center provided advice in
resolving some findings identified by the RTI audit team.
VI
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Glossary
ASTM - American Society for Testing Materials
CO - Carbon Monoxide
CTS - Calibration Transfer Standard
EPA - United States Environmental Protection Agency
FID - Flame lonization Detector
FTIR - Fourier Transform Infrared Spectroscopy
HAP - Hazardous Air Pollutant
MCEM - Methylene Chloride Extractable Particulate Matter or Organic Extractable Particulate
Matter
MQL - Minimum Quantitation Limit
MRI - Midwest Research Institute
NIST - National Institute of Standards and Technology
NOx - Nitrogen Oxides
OAQPS - Office of Air Quality Planning and Standards
PAH - Polynuclear Aromatic Hydrocarbons
PES - Pacific Environmental Services, Inc.
PM - Particulate Matter
ppb - parts per billion
ppm - parts per million
QAPP - Quality Assurance Project Plan
RAP - Recycled Asphalt Pavement
RSD - Relative Standard Deviations
RTI - Research Triangle Institute
SED - Silo Exhaust Duct
SF6 - Sulfur Hexafluoride
SO2 - Sulfur Dioxide
SSTP - Site Specific Test Plan
SVOHAP - Semi-volatile Organic Hazardous Air Pollutant
THC - Total Hydrocarbons
TSA - Technical Systems Audit
VOHAP - Volatile Organic Hazardous Air Pollutant
VOST - Volatile Organic Sampling Train
Vli
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Vlll
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Table of Contents
Disclaimer iii
Preface v
Acknowledgements vi
Glossary vii
Table of Contents .- ix
Chapter 1
1.0 Quality Assurance Audit Results 1.1
1.1 Overview 1.1
1.2 Process Description 1.1
1.2.1 Aggregate Processing Operations 1.2
1.2.2 Silo Filling Operations 1.2
1.2.3 Load-Out Operations 1.2
1.3 Emission Testing 1.2
1.4 Technical Systems Audit 1.3
1.4.1 General Reviews 1.4
1.4.2 Technical Assessment of MRI's Testing 1.4
1.4.3 Technical Assessment of PES's Testing 1.5
Chapter 2
2.0 Technical Systems Audit - Midwest Research Institute 2.1
Technical Systems Audit Checklist 2.4
A. Quality System Documentation 2.4
B. Organization and Responsibilities 2.7
C. Training and Safety 2.10
D. Data Quality Indicator Goals and Performance Testing 2.10
E. Extractive Sampling System 2.12
F. Extractive Fourier Transform Infrared (FTIR) Instrument 2.16
G. Sample Concentrator for Ftir Instrument 2.24
H. Total Hydrocarbons (THC) Analyzer 2.32
1. Capture Efficiency Test 2.37
Chapter 3
3.0 Technical Systems Audit - Pacific Environmental Services Inc 3.1
Technical Systems Audit Checklist 3.2
A. General Quality Assurance Information 3.2
B. Organization and Responsibilities 3.5
C. Method Specific - EPA Method 1 3.7
ix
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D. Method Specific - EPA Method 2 3.8
E. Method Specific - EPA Method 4 3.9
F. Method Specific - EPA Method 315 3.10
Laboratory Information Necessary for EPA Method 315 3.12
Calibration and General 3.13
G. Method Specific - EPA Method 18 3.16
Apparatus 3.17
H. Method Specific - SW-846 Method 0030 (VOST) 3.19
I. Method Specific - SW-846-0010 (Modified Method 5) 3.21
Train Components 3.22
Preparation of the Train > 3.23
Running the Train 3.25
Sample Recovery 3.25
J. Sampling General 3.27
K. Quality Assurance/quality Control/general 3.28
L. Sample Custody and Integrity 3.29
M. Miscellaneous Measurements 3.30
N. Estimation of Particulate Deposition 3.30
P. Estimation of Particulate Deposition on the Inside Walls of the Temporary
Silo Exhaust and Wind Tunnel Exhaust 3.31
Q. Direct Interface Portable GC/MS 3.32
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Chapter 1
Quality Assurance Audit Results
Hot Mix Asphalt Plant C,
Los Angeles, CA
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1.0 QUALITY ASSURANCE AUDIT RESULTS
1.1 Overview
The United States Environmental Protection Agency (EPA) Office of Air Quality Planning and
Standards (OAQPS) is investigating hot mix asphalt plants to characterize emissions during silo filling
and truck loading operations. In support of this investigation, OAQPS issued work assignments to
Pacific Environmental Services, Inc. (PES) and Midwest Research Institute (MRI) to conduct emission
testing of these sources. Additionally, due to the complexity and importance of this testing, OAQPS
issued a work assignment to Research Triangle Institute (RTI) to perform an independent technical audit
of MRI and PES's emissions testing through a technical review. RTI conducted the audit according to
the principles of the EPA Office of Research and Development's Quality Assurance Division. These
principles are described in their working draft of EPA Guidance for Technical Assessments for
Environmental Data Operations (EPA QA/G-7).
The primary objective of the emissions testing was to characterize the uncontrolled emissions of
paniculate matter (PM), organic extractable particulate matter (methylene chloride extractable particulate
or MCEM) and organic hazardous air pollutants (HAP's) from silo filling and truck loading operations at
a hot mix asphalt production plant. The organic HAP emissions quantified included polynuclear
aromatic hydrocarbons (PAHs), semi-volatile organic hazardous air pollutants (SVOHAPs), and volatile
organic hazardous air pollutants (VOHAPs). Other emissions that were characterized included methane,
carbon monoxide (CO), sulfur dioxide (SO2), and nitrogen oxides (NOx).
It was concluded from the technical systems audit that the overall quality assurance objectives of
the test were met. Except for some minor deviations, the test team members performed the testing
according to the procedures outlined in ,he Site Specific Test Plan (SSTP) and Quality Assurance Project
Plan (QAPP). These deviations from the QAPP or SSTP were discussed with and approved by the EPA
Work Assignment Manager. The equipment used was appropriate for the emissions testing and was
operated satisfactorily during the testing.
1.2 Process Description
An asphalt plant located south of Los Angeles, CA, (also called Asphalt Plant C or Plant C), was
selected as the host facility. Testing was performed over five consecutive days beginning on July 24,
1998. Testing of transport truck loading operations was performed under two conditions - normal
operations and a background condition. Additionally, a secondary objective of the emission testing was
to characterize controlled emissions of VOHAPs, CO, SO2 and NOx from the aggregate dryer.
This plant was selected for the emissions testing due to its high production rate, ventilation of the
storage silos and enclosure/ventilation of the load-out bay. The Plant C facility has a rated production
capacity of 650 tons per hour (tph). Daily production varies from approximately 2,000 tons per day (tpd)
to 6,000 tpd depending on demand. The plant produces five different categories of hot mix asphalt: 3/8
in, 1/2 in, 3/4 in, fines, and recycled asphalt (RAP). These categories indicate the average size and type
of aggregate in the mix. In RAP, small amounts of recycled asphalt are added to the mix. The plant also
adds small amounts of rubber to some products as a crack inhibitor. The plant uses two different kinds of
liquid asphalt: AR-4000 and AR-8000. AR-4000 is a softer asphalt and is used approximately 90% of
Quality Assurance A udit Results 1.1
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the time. The percent by weight of liquid asphalt in the mix varies from 4.8% to 6.0% depending on the
size of the aggregate (the smaller the aggregate, the higher the liquid asphalt content).
The following paragraphs describe the three operations tested at Plant C.
1.2.1 Aggregate Processing Operations
In this continuous process, cold aggregate is introduced to the rotary drum dryer. As the drum
rotates, the aggregates move toward the other end of the drum. The cold aggregate is first dried and then
is heated as it moves through the drum. After exiting the dryer drum into a mixing drum, the heated and
dried aggregate is mixed with the liquid asphalt cement and recycled asphalt pavement (RAP). A
ventilation system exhausts the gases and condensed particulate from the rotary drum dryer through a
baghouse and exhaust stack.
1.2.2 Silo Filling Operations
Hot mix asphalt produced in the aggregate processing operation is transported by bucket elevator
into temporary storage silos. Plant C has five 200-ton heated silos that sit on top of the load-out tunnel.
The silos serve as a holding station between production and the loading of the hot mix asphalt into
transport trucks. Depending on customer requirements, a different product can be stored in each silo.
The hot mix asphalt in storage can have a temperature up to 160° C (320° F). A 10" inside diameter
ventilation duct exhausts the gases and condensed particulate from each of the five silos to an exhaust
duct that ventilates the load-out tunnel.
1.2.3 Load-Out Operations
The hot mix asphalt is dropped from the storage silos into transport trucks within a load-out
tunnel that is approximately 183 ft long with open doorways at both ends. During a full load-out
schedule, trucks enter the tunnel approximately every one to three minutes. Single bed trucks hold
approximately 21 tons of asphalt cement. Dual bed trucks (i.e., a truck and trailer) hold approximately
25 tons. Typically, the temperature of the asphalt cement, after it drops from the silo into the truck, is
approximately 300° F.
The truck is positioned under the silo containing the desired product where it is loaded into the
truck bed. During loading, emissions are captured by activating a double-slotted capture hood at each
silo. With the truck positioned under the silo, one freestanding slot will be at the forward edge and one
at the aft edge of the truck bed. No more than one silo can operate at a given time and only the capture
hood associated with that silo is activated to capture the emissions. It typically takes 15 to 30 seconds to
load a truck. One capture hood is always active, even when no loading is occurring. Each of the capture
hoods connects to the 32 inch inside diameter tunnel exhaust duct. Constant flow is maintained by the
fan setting, thus, a constant airflow is always exhausted from the load-out tunnel to the emission
abatement system. The tunnel, ventilation system, and capture hoods work together to form a near-total
enclosure for the loading operations. The selected test site, however, did not meet all of the criteria for a
permanent total enclosure as defined by EPA Method 204, "Criteria for Verification of a Permanent or
Temporary Total Enclosure," Federal Register, Vol. 62, No. 115, June 16, 1997.
Quality Assurance Audit Results 1.2
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1.3 Emission Testing
The emissions testing consisted of triplicate runs of the silo and load-out ventilation systems.
Additionally, a fourth test run was performed using two trucks that traversed the load-out area like
normal operations, while no loading was occurring to determine background emissions contributed by
diesel truck exhaust. For all four test runs, capture efficiency testing of the load-out system was
performed. The silo ventilation system was tested intermittently whenever silo loading operations
occurred. Two test runs were performed on the dryer stack using only instrumental test methods. The
three ventilation systems are referred to as the load-out system, the silo storage system, and the hot mix
dryer system. The specific tests performed at each ventilation system are summarized below:
• The Load-out system was tested for HAPs, CO, SO2, and NOx, using extractive Fourier
Transform Infrared Spectroscopy (FTIR) (EPA Method 320) and FTIR with sample
concentration. Total hydrocarbons (THC) were measured using a flame ionization detector (FID)
(Method 25A). A single SW-846 Method 0010 Modified Method 5 (MM5) sampling train was
used to collect both PAHs and SVOHAPs. Three different procedures were used to measure
VOHAPs: 1) sampling procedure SW 846 Method 0030 in combination with analytical
procedure SW 846 Method 8260, 2) EPA Method 18, and 3) on-site GC/MS. During background
testing no measurements were made using the on-site GC/MS.
• The Silo storage system was tested for HAPs, CO, SO2, and NOx, using extractive FTIR (EPA
Method 320) and FTIR with sample concentration. Total hydrocarbons (THC) were measured
using a flame ionization detector (FID) (Method 25A). A single SW-846 Method 0010 Modified
Method 5 (MM5) sampling train was used to collect both PAHs and SVOHAPs. Three different
procedures were used to measure VOHAPs: 1) sampling procedure SW 846 Method 0030 in
combination with analytical pro;edure SW 846 Method 8260, 2) EPA Method 18, and 3) on-site
GC/MS.
• The Hot mix dryer system was tested for HAPs, CO, SO2, and NOx, using extractive FTIR (EPA
Method 320) and FTIR with sample concentration. Total hydrocarbons (THC) were measured
using a flame ionization detector (FID) (Method 25A).
• Capture efficiency tests of the load-out system were also performed simultaneously with the
load-out system tests. Tracer gas was released from a manifold in the load-out bay, was collected
by the ventilation system, and air concentrations were measured, allowing capture efficiency to
be calculated.
The responsibilities for this testing were divided between PES and MRI. The instrumental test
methods were performed by MRJ under the direction of Scott Klamm. The manual test methods were
performed by PES under the direction of Frank Phoenix. Mike Toney of EPA was on site and overall
responsibile for the testing.
1.4 Technical Systems Audit
The technical systems audit (TSA) was performed by R.K.M. Jayanty and Robert S. Wright of
Research Triangle Institute (RTI) under EPA Contract 68-D4-0091, work assignment 99-03, from July
Quality Assurance Audit Results 1.3
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20, through July 26, 1998. The purpose of the audit was to conduct an independent technical assessment
of MRI and PES's emissions testing through a technical review. The review included an in-depth
evaluation of documents, on-site activities, equipment, procedures, record keeping, data validation, data
management, and reporting to ensure that established requirements are satisfied. The TSA was
conducted following principles described in a working draft version of EPA Guidance for Technical
Assessments for Environmental Data Operations (EPA QA/G-7), which was being developed by EPA's
Quality Assurance Division at the time. Detailed findings and Technical Systems Audit Checklists as
revised by EPA for the tests performed by MRI and PES are presented in Chapters 2 and 3 respectively.
Summaries of the findings and descriptions of the EPA revisions are presented below.
1.4.1 General Reviews
In general, RTI found that the PES and MRI team members performed the testing according to
the procedures outlined in the Site Specific Test Plan (SSTP) and Quality Assurance Project Plan
(QAPP). Deviations from the QAPP or SSTP were discussed with the EPA Work Assignment Manager.
RTFs assessment proceeded after approval of the deviations. The equipment used was found by RTI to
be appropriate for the planned emissions testing and generally operated satisfactorily during the testing.
RTI found that the PES and MRI team members, who were present at the site, to be well qualified and
experienced to perform the emissions testing and conducted themselves in a professional manner.
Although RTFs assessment of the performance of the testing by MRI and PES is valid, a few
revisions of their findings were made. While most of the revisions were made to clarify the finding or
eliminate unnecessary comments, one revision was made that altered the determination of the potential
effect on Data Quality. Some of the items in the TSA checklist for PES were not completed by RTI due
to lack of information available at the on-site operations. After the field test, RTI requested this
information from PES, but it was not received by RTI by the date of their report to EPA. The checklist
was completed based on the RTI auditors' observations during sampling and their discussions with the
PES task manager, sampling train operators, custodians, and PES quality assurance (QA) coordinator at
the site. Additional information on the calibration of the equipment in the laboratory prior to the on-site
testing was requested, but had not been received by RTI. Examples of blank data sheets, custody forms,
and labels have been supplied to the auditors and were included with the draft version of the checklist.
The following paragraphs describe the revisions that EPA made to the findings and technical
system audit checklists RTI submitted to EPA on September 29, 1998.
1.4.2 Technical Assessment of MRI's Testing
RTI identified as a finding, which may have a potential effect on data, that besides all reports
generated by this project being reviewed formally by senior project personnel, quality control data should
be audited by the project's quality assurance officer. While the letter RTI received from MRI did not
address the auditing of quality control data, MRI's standard procedures require a senior project person to
review raw test data and to randomly select data to be followed through the analysis and data processing.
In addition, EPA performed a quality control audit of the data and reproduced the calculations from raw
data to final results. As a result, the clarifying statements by RTI were removed and this finding was
changed to one that is unlikely to have a effect on data quality.
Quality Assurance A udit Results 1.4
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In the findings which are unlikely to have an effect on data quality table, wording of the third
finding was changed to better characterize the level of detail used to describe the FTIR procedures
without indicating the adequacy of the procedures. The complexity of the FTIR procedures precludes a
description as detailed and thorough as most other methods. In the Technical Systems Audit Checklist,
sentences were removed from items 3 and 10 of the Quality System Documentation. In Item 3, the
sentence indicating the QAPP and SSTP were not revised has been deleted. In Item 10, the sentence was
completed by stating that the THC calibration data was recorded on a legal pad.
1.4.3 Technical Assessment of PES's Testing
In the findings that may have a potential effect on data quality, items 1 and 2 were revised. A
sentence was added to Item 1 explaining that this was a research study and that testing was not meant to
have validation. This was the first attempt to measure many of the pollutants at these sources. It would
be highly unusual and expensive to also attempt to validate the test methods at these sources without
some prior knowledge of the performance of some initial testing. The paragraph for Item 2 discussing
the spiking of surrogate compounds for the VOST cartridges has been completely revised to properly
reflect that the analytical laboratory spiked compounds before transport to the field-testing location. The
sentence identifying a better spiking methodology was removed.
In the findings that are unlikely to have an effect on data quality, Items 1 and 2 have been
revised. In Item 1, the sentence identifying a better spiking methodology was removed. In Item 2 one
sentence was revised and one was removed. This corrects an incorrect and contradictory statement in
one sentence that a dedicated notebook was not maintained to record any problems or process changes.
In the Technical Systems Audit Checklist, a clarifying statement was added to the comment for
Item 2 under General Quality Assurance Information indicating that key personnel provided sample train
operators with information from the QAPP and SSTP as needed for their tasks.
Quality Assurance A udit Results 1.5
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Chapter 2
Technical Systems Audit
Instrumental Test Methods Performed by
Midwest Research Institute at
Hot Mix Asphalt Plant C,
Los Angeles, CA
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2.0 TECHNICAL SYSTEMS AUDIT - MIDWEST RESEARCH INSTITUTE
This chapter is the final technical systems audit (TSA) of the emissions testing performed by
Midwest Research Institute (MRI) at Hot Mix Asphalt Plant C in the Los Angeles, California area. As
explained in detail in Chapter 1, the final TSA includes revisions by the EPA Quality Assurance Officer.
The draft TSA report from Research Triangle Institute (RTI) was delivered to the EPA Quality
Assurance Officer on September 29, 1998. The TSA was performed by R.K.M. Jayanty and Robert S.
Wright of RTI under EPA Contract 68-D4-0091, work assignment 99-03, from July 20, through July 26,
1998. The purpose of the TSA was to conduct an independent technical assessment of MRI's emissions
testing through a technical review, which included an in-depth evaluation of documents, on-site
activities, equipment, procedures, and record keeping to assure that quality assurance requirements were
satisfied. The TSA was conducted in accordance with principles described in the EPA Quality
Assurance Division's working draft version of EPA Guidance for Technical Assessments for
Environmental Data Operations (EPA QA/G-7).
In general, MRI did a very good job during the emissions testing at the hot mix asphalt plant.
The emissions testing was executed according to the quality assurance project plan (QAPP) and the site-
specific test plan (SSTP) to a large degree. The equipment that was used is appropriate for the planned
emissions testing and it generally operated satisfactorily. The on-site project personnel were well-
qualified to perform the emissions testing and conducted themselves in a professional manner.
Checklist
Section
G3, G31
Findings which may have a Potential Effect on Data Quality
The sample concentrator method for the FTIR instrument does not appear to have
been throughly validated or throughly documented. In 1993, Entropy
Environmentalists conducted a method validation at a coal-fired boiler, which was
published as EPA Report No. EPA/454/R-95/004, July 1993 (NTIS Order No. PB95-
193199INZ). This method validation found that EPA Method 301 validation criteria
were met for toluene and xylenes in concentrated samples. Pacific Environmental
Services found these compounds during its preliminary measurements at the hot-mix
asphalt plant. If MRI discovers significant concentrations of other chemical
compounds in the asphalt plant emissions, then the report of MRI's emissions testing
should note that the FTIR sample concentrator method has not been validated for
these additional compounds, which it does.
Checklist
Section
A3
Findings which are Unlikely to have an Effect on Data Quality
Some equipment and procedures that were used during the emissions testing in July
differ from those documented in the QAPP, which was submitted to EPA in March.
In many cases, these changes are documented in the SSTP. Some changes were
made as recently as 3 weeks before the testing and are not documented in either
document. Revisions and/or amendments to both documents should have occurred,
according to procedures outlined within the QAPP.
Technical Systems Audit of Test Methods Performed by MRI
2.1
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Checklist
Section
Findings which are Unlikely to have an Effect on Data Quality
A8
The total hydrocarbon (THC) analyzer's calibration data were recorded on a legal
pad, rather that on a formal data sheet as was used for other measurements. Section
5.1 of the QAPP states that information will be entered in standard data forms.
A14
A letter from MRI to RTI indicates that all reports that are generated by this project
will be reviewed formally by senior project personnel. It is assumed these reports did
receive review by senior personnel.
A-Comments
The QAPP does not describe the FTIR procedures in a lot of detail. It cites EPA Test
Method 320 and the FTIR Protocol, which are pretty general to describe the specifics
of the data collection effort at the hot-mix asphalt plant.
F31
Test Method 320 specifies an accuracy of ±2% for the CTS. The CTS used for this
study had an accuracy of ±5%. The concentration of the CTS was not independently
verified by MRI.
F-Comments
QAPP Section 3.1.1 states that the time for 5 cell volumes to pass through the cell is
considered the minimum interval separating independent samples. If the cell volume
is 8.5 L, then 5 cell volumes corresponds to 42.5 L. If the FTIR sample gas flow rate
is 5 L/min and the FTIR sample interval is 2.5 minutes, only 12.5 L (or 1.5 cell
volumes) of sample gas passes through the cell between measurements. Therefore,
an individual FTIR measurement cannot be considered to be completely independent
of the measurements that immediately precede it. Scott Klamm confirms that it takes
3 to 4 samples to flush the cell for CTS measurements.
F-Comments
During the emissions testing, MRI analyzed a nine-component hydrocarbon
calibration standard (Spectra Gases cylinder number CC91245) that had been
brought to the hot mix asphalt plant by Emissions Monitoring, Inc. The analysis of
this calibration standard does not constitute a performance evaluation of the
extractive FTIR method because MRI was not informed of the analysis prior to the
emissions testing nor during our initial on-site meeting on 20 July 1998. The results
of the analysis were not available during the RTI assessor's conversation with MRI's
Thomas Geyer on August 27, 1998. RTI suggests that the results of the MRI's
analysis of this calibration standard be included in MRI's emissions testing report,
which will allow EPA to compare the MRI analytical results with the attached
certificate of analysis for the calibration standard.
G21
The SSTP indicates that a preheated vapor-phase surrogate spike will be loaded onto
the Tenax cartridge via the sampling probe. The surrogate spike was actually loaded
in the monitoring trailer at room temperature.
G25
A duplicate train sample was collected on 25 July 1998, but the FTIR sample
spectrum was not saved. A second attempt to collect a duplicate train sample was
scheduled for 27 July 1998 after the assessors departure. The results of the post
sampling analysis of this sample were not available for review as of 27 August 1998.
Technical Systems Audit of Test Methods Performed by MRI
2.2
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Checklist
Section
Findings which are Unlikely to have an Effect on Data Quality
H-Comments
There appear to be some errors in the draft THC calibration data the MR1 submitted
for review. The span drift data for stack dryer Runs 1 and 2 are identical, which is an
unlikely occurrence. There appear to be errors in the calculated span drifts for Dryer
Stack Run 1 and Load-out Run 1. These errors do not appear to be major problems.
Technical Systems Audit of Test Methods Performed by MRI
2.3
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Technical Systems Audit Checklist
Project:
Organization:
Assessment Location:
Assessors:
Assessment Dates:
Emissions Testing at a Hot Mix Asphalt Plant
Midwest Research Institute (Kansas City, Missouri)
Asphalt Plant C, Los Angeles, California
Robert S. Wright and R.K.M. Jayanty, Research Triangle Institute (Research
Triangle Park, North Carolina)
July 20 through July 26, 1998
Brief Project Description: EPA is investigating hot mix asphalt plants to identify and quantify particulate
matter and hazardous air pollutants (HAPs) emitted from asphalt cement load-out operations. EPA has
issued a work assignment to MRI to conduct an air emissions test program to collect data in support of
the investigation. Asphalt Plant C in Los Angeles, California was chosen primarily because load-out
emissions are controlled by a silo exhaust system and a load-out tunnel. The plant has a production
capacity of more 650 tons per day. Approximately 2,000 tons per 4 hour period were produced, during
the test. The primary objective of the project was to characterize air emissions of organic HAPs from the
storage silos, the load-out tunnel, and the hot mix dryer.
AUDIT QUESTIONS
RESPONSE
N
N
COMMENT
A. QUALITY SYSTEM DOCUMENTATION
Is there an approved quality
assurance project plan (QAPP) for
the project and has it been
reviewed by all appropriate
personnel?
A QAPP was submitted to EPA on
March 27, 1998. Additionally, MRI
submitted a site-specific test plan
(SSTP) on June 22, 1998. Both
documents have been approved by EPA.
Is a copy of the QAPP maintained
at the field site? If not, briefly
describe how and where QA and
quality control (QC) requirements
and procedures are documented.
Copies of the QAPP and SSTP are
available in plain sight in the monitoring
trailer. No one has been observed
consulting these documents.
Technical Systems Audit of Test Methods Performed by MRI
2.4
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AUDIT QUESTIONS
3 . Is the design and conduct of the
project as is specified in the
QAPP?
4. Are there deviations from the
QAPP?
RESPONSE
Y
/
/
N
N
A
COMMENT
In general, the project is being
implemented as was specified in the
QAPP. However, some equipment and
procedures have changed since the
QAPP was submitted to EPA. In many
cases, these changes are documented in
the SSTP. Some changes were made as
recently as 3 weeks before the testing
and are not documented. Revisions
and/or amendments to both documents
should have occurred, according to
procedures outlined within the QAPP.
There are some noticeable deviations,
which do not appear to affect the quality
of the data being collected. For
example, QAPP Section 3.1.2 states that
Tenax will be spiked with an analyte or
surrogate compound during sample
collection if practical. The sample
concentration description in the QAPP
also mentions a post-test, laboratory
gaseous spiking procedure and other
procedures. SSTP Section 5.1.3 states
that a vapor phase spike will be
preheated and injected into the back of
the sampling probe. However, the
surrogate spike gas was loaded onto the
Tenax trap in the trailer prior to
sampling using the cool thermal
desorption system for the traps.
Technical Systems Audit of Test Methods Performed by MRI
2.5
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AUDIT QUESTIONS
RESPONSE
N
N
COMMENT
5. How are any deviations from the
QAPP noted?
QAPP Section 6.3 indicates that the
QAPP will be amended to correct minor
discrepancies that have no effect on the
overall conduct of the study. The QAPP
presents a form for documenting such
amendments. An entire chapter of the
QAPP will be revised if major changes
in the conduct of the study occur.
However, no amendments or revisions
have been submitted to EPA. Any
deviations that arise before or during the
testing should be documented.
For each measured parameter, does
the QAPP list the frequency of
calibration, acceptance criteria for
the calibration, and the process for
calibration data reduction and
review?
QAPP Table 2-1 and SSTP Table 5-2
give the calibration frequencies and
accuracy and precision objectives for
some field test methods. SSTP Table 5-
1 lists the calibration frequencies,
acceptance limits, reference standards,
and calibration techniques for other
methods.
7. Are written and approved standard
operating procedures (SOPs) used
in the project? If so, list them and
note whether they are available at
the field site. If not, briefly
describe how and where the project
procedures are documented.
No SOPs were observed at the testing
site. The Fourier transform infrared
(FTIR) sample concentration procedure
is attached to the QAPP. EPA test
methods are cited and, in some cases,
attached to the QAPP and SSTP (i.e.,
Methods 25A and 320 and the FTIR
Protocol).
Briefly describe how calibration
and other QC data are documented.
Operational parameters and calibration
data were recorded on paper data sheets
and Excel spreadsheets except for total
hydrocarbon (THC) analyzer's
operational parameters and calibration
data, which were recorded on a legal
pad.
9. Does the calibration
documentation show that
calibrations are being performed at
the required frequency and in the
required manner??
MRJ calibration data indicates that the
extractive FTIR instrument and the THC
analyzer were calibrated at the required
frequency and in the required manner.
Technical Systems Audit of Test Methods Performed by MRI
2.6
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AUDIT QUESTIONS
10. Are there standard paper or
electronic forms to record
calibration data and operational
parameters?
1 1 . Are the standard data forms dated?
12. Is the person who recorded the data
identified on the form?
1 3 . Are any paper records written in
indelible ink?
1 4. Are the QC data reviewed by
another qualified person such as
the QA officer or the project
leader? Who is this individual?
15. Is the project team adhering to the
planned schedule? If not, explain
the new schedule. Verify that all
schedule changes have been
authorized.
RESPONSE
Y
/
/
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/
N
/
/
N
A
COMMENT
Standard paper data sheets and Excel
spreadsheets were used for all
measurements except the THC
measurements, which was recorded on a
legal pad.
The forms have a line for the entry of
the date.
The forms have a line for the entry of
the operator's name.
All reviewed data forms were filled out
in ink.
A letter from MRI to RTI indicates that
Scott Klamm, Thomas Geyer, John
Hosenfeld, Bruce Diel, and Jack
Balsinger will review formally all
reports generated by this project.
However, there is no indication whether
the raw QC data are reviewed directly
by any MRI personnel.
The schedule is being followed to the
extent allowed by unexpected
equipment breakdowns in the asphalt
plant and FTIR instrumentation
problems. All schedule modifications
were authorized by the EPA Work
Assignment Manager.
Additional Questions or Comments: The QAPP does not describe the FTIR procedures in enough
detail. It cites EPA Test Method 320 and the FTIR Protocol, which are too general to describe the
specifics of the data collection effort at the test site. For example, QAPP Section 2.2. 1 . 1 states that
ethylene in nitrogen will be used as the FTIR calibration transfer standard (CTS) and FTIR Protocol
Section 4.5 gives selection criteria for the CTS. However, nowhere is it stated why ethylene in
nitrogen was selected as the CTS for this project. A similar problem exists for selection of the Tenax
trap surrogate spike gas.
Technical Systems Audit of Test Methods Performed by MRI
2.7
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AUDIT QUESTIONS
RESPONSE
Y
N
N
A
COMMENT
B. ORGANIZATION AND RESPONSIBILITIES
Identify the following personnel and determine whether they have the listed responsibilities:
1 . MRI Work Assignment Leader:
John Hosenfeld (Kansas City, MO)
• responsible for overall
performance of the project, and
• communications with EPA
2. MRI Quality Assurance Officer:
Jack Balsinger (Kansas City, MO)
• prepare QAPP
• review and monitor QA activities
3. MRI Project Task Leader:
Scott Klamm (Kansas City, MO)
• responsible for the on-site
emissions testing effort
• supervision of all MRI on-site
and off-site staff
• communication with other on-
site personnel.
4. MRI FTIR Oversight:
Thomas Geyer (RTF)
• guidance for FTIR field data
collection
• direct spectral analysis effort
5. MRI FTIR Operators:
Scott Klamm and Andy Page
• operation of FTIR instrument
and sample concentrator,
• calibration of FTIR instrument
and sample concentrator, and
• recording operational parameters
6. THC Analyzer Operators:
Bob Gulick and Bobby Edwards
• operation of THC analyzer,
• calibration of THC analyzer, and
• recording operational parameters
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/
/
/
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/
Mr. Hosenfeld was not present at the
emissions testing.
Mr. Balsinger was not present at the
emissions testing.
Mr. Klamm is also responsible for the
FTIR instrument.
Mr. Geyer was not present at the
emissions testing, but was available for
consultation by telephone. After testing
was completed, he analyzed the FTIR
spectra to identify compounds and
quantify concentrations.
Mr. Klamm has primary responsibility
for operating the FTIR instrument
during the emissions testing.
Mr. Edwards is also a gas sampling train
operator.
Technical Systems Audit of Test Methods Performed by MRI
2.8
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AUDIT QUESTIONS
7. MRI SF6 Tracer Gas Operator:
Dan Neal
• operation of SF6 tracer gas
release manifold
8. Other MRI Testing Staff:
Jim Surman and Pam Murowchick
9. EPA Work Assignment Manager:
Michael L. Toney
• oversight of emissions testing
and problem solving
• communication with all on-site
personnel
10. EPA QA Officer:
Lara P. Autry
• review and approve QAPP
• review and approve QA activities
RESPONSE
Y
N
N
A
/
/
/
/
COMMENT
Mr. Neal is also a gas sampling train
operator.
Mr. Surman is a gas, sampling train
operator. Ms. Murowchick collects
process monitor data in the asphalt plant
control room and alerts the SF6 tracer
gas operator of load-out tunnel
activities.
Mr. Toney was present throughout the
entire testing program and coordinated
the efforts of the emissions testing
teams. He authorized all changes in
testing schedule and procedures.
Ms. Autry was not present at the
emissions testing.
Additional Questions or Comments:
Technical Systems Audit of Test Methods Performed by MRI
2.9
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AUDIT QUESTIONS
RESPONSE
Y
N
N
A
COMMENT
C. TRAINING AND SAFETY
1 . Does the FTIR instrument operator
have special training or experience
for the operation of the instrument?
2. Does the THC analyzer operator
have special training or experience
for the operation of the instrument?
3. Does the project maintain current
summaries of the training and
qualifications of project personnel?
4. Does the project maintain
descriptions of assignment
responsibilities?
5. Is there special safety equipment
required to ensure the health and
safety of project personnel?
6. Is each project team member
appropriately outfitted with safety
gear?
7. Are project personnel adequately
trained for their safety during the
performance of the project?
8. Who is authorized to halt
emissions testing in the event of a
health or safety hazard?
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/
Mr. Klamm has 8 years experience with
extractive FTIR and open-path FTIR in
laboratory and field applications.
Mr. Gulick has 10 years experience with
emissions testing and 5 additional years
of experience with analytical
instrumentation.
A letter from MRI to RTI includes brief
resumes for project personnel.
The QAPP contains descriptions of
senior project personnel. A letter from
MRI to RTI states that the
responsibilities for other personnel were
assigned in meetings before and during
the project.
The asphalt plant required personnel to
wear hard hats while walking under
conveyor belts.
Each team member wore safety shoes
and a hard hat when outside of the
trailer. Eye and ear protection were
worn on an as-needed basis.
Question not asked, but observation of
the team members demonstrates that
they were adequately trained about
safety.
The EPA Work Assignment Manager
retained authority to halt emissions
testing as necessary to protect health
and safety.
Additional Questions or Comments:
Technical Systems Audit of Test Methods Performed byMRI
2.10
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AUDIT QUESTIONS
RESPONSE
Y
N
N
A
COMMENT
D. DATA QUALITY INDICATOR GOALS AND PERFORMANCE TESTING
1 . Is the anticipated use of the data
known and documented in the
QAPP?
2. What are the critical
measurements?
3. Have data quality indicator goals
for each critical measurement been
documented in the QAPP?
4. Do the above data quality indicator
goals appear to be based on
documented performance criteria
for the measured parameter or on
actual QC data compiled for the
particular measured parameter?
5. Has the performance of each of the
critical measurements been
assessed and documented?
6. Are there established procedures
for corrective or response actions
when measurement performance
criteria or the data quality indicator
goals (e.g. out-of-control
calibration data) are not .net? If
yes, briefly describe them.
7. Are the corrective action
procedures consistent with the
QAPP?
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/
The study objectives are briefly
described in the QAPP.
The QAPP describes extractive Fourier
transform infrared (FTIR) spectroscopy,
FTIR by sample concentration, and total
hydrocarbons (THC).
QAPP Table 2-1 presents accuracy and
precision goals for direct and indirect
FTIR, THC, moisture, temperature,
velocity, oxygen, and carbon dioxide.
The accuracy and precision goals for
extractive FTIR and THC are based on
EPA Test Methods 320 and 25A. The
accuracy and precision goals for FTIR
by sample concentration are based on
EP \ Method 301 validation criteria
from Entropy Environmentalists' 1993
method validation at a coal-fired boiler.
Calibration data for direct and indirect
FTIR and THC were obtained and
recorded on a daily basis.
The corrective action procedures are
informal and are implemented on an as-
needed basis. For example, problems
with the FTIR instrument prompted a
call to a FTIR consultant, who was able
to provide suggestions for corrective
actions.
QAPP Section 4.6 describes general
corrective action procedures that are
followed when problems occur.
Technical Systems Audit of Test Methods Performed by MRI
2.11
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AUDIT QUESTIONS
8. Have any such corrective actions
been taken?
RESPONSE
Y
/
N
N
A
COMMENT
A few minor corrective actions have
been taken, but none were significant
enough to halt work on the project or to
involve the MRI work assignment leader
or the MRJ quality assurance officer.
Additional Questions or Comments:
E. EXTRACTIVE SAMPLING SYSTEM
1 . Describe locations of the sampling
ports.
2. Describe the sampling probes.
3 . Are the sampling probes heated to
prevent condensation?
4. Does each of the sample probes
have a calibration valve assembly
for sampling system bias tests?
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/
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/
During the testing of the hot mix drying
exhaust, the sampling ports were located
at the baghouse exhaust stack
approximately 10 feet below the outlet.
The sample ports for the testing of the
load-out tunnel were located in the
exhaust ducting between Silos 1 and 2.
The sampling ports for the testing of the
silos were located in the exhaust ducting
of Silo 2 between the silo vent and the
damper.
The sampling probes were short,
straight lengths (i.e., 1 to 2 feet) of
stainless steel tubing that were
connected to the particulate filters.
The sampling probes were located
inside the sampling ports and remained
at that those temperatures. The dryer
baghouse exhaust temperature was
approximately 260° C, the silo duct
temperature was approximately 240° C,
and the load-out tunnel exhaust was
near ambient air temperatures.
The sample probes have calibration
valve assemblies for delivering
calibration gas to the FTIR and THC
instruments via the sampling lines.
Technical Systems Audit of Test Methods Performed by MRI
2.12
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AUDIT QUESTIONS
5. Describe the sampling lines.
6. Are the sampling lines heated to
prevent condensation?
7. Describe any sample
conditioning/moisture
removal/dilution air system.
8. Describe how the instrument
operators switch from sampling
from one location to sampling to
another location.
9. Is any sample conditioning system
maintained according to schedule?
10. Describe the particulate filter.
RESPONSE
Y
'
N
N
A
'
'
'
'
COMMENT
Two 1 00-foot lengths of Technical
Heaters Model 22129-02-01-01
sampling line containing three Teflon®
tubes were used between the dryer
baghouse exhaust sampling port and the
sampling pumps outside of the trailer.
One tube conveyed sample gas, another
tube conveyed calibration gas, and the
third tube was not used. For the load-
out tunnel and silo testing, one length of
sampling line was used between the silo
and load-out sampling ports and another
was used between the load-out tunnel
sampling ports and the sampling pumps.
Two Teflon® tubes conveyed sample
gas and the third tube conveyed
calibration gas. A Furon Unitherm
Model 220-666 sampling line containing
three Teflon® tubes was used between
the sampling pumps and the sample
distribution manifold inside the trailer.
The sampling line is heated to 300° C
using a control and display box in the
trailer.
There was no sample conditioning or
dilution system.
FTIR and THC instrument operators
switch between sampling lines using
valves in the sample distribution
manifold.
Not applicable.
A Balston particulate filter is contained
in a stainless steel housing.
Technical Systems Audit of Test Methods Performed by MRI
2.13
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AUDIT QUESTIONS
11. Is the filter changed according to
schedule?
12. Describe the sample pump.
1 3 . Describe the sample flow control
apparatus.
14. Describe how the total sample
volume is measured.
1 5 . Describe how the sample volume
meter is calibrated.
1 6. When was the last time that the
sample volume meter was
calibrated?
17. Is the volumetric calibration
traceable to NIST standards?
1 8. How is the gas meter temperature
measured?
19. How is the gas meter thermometer
calibrated?
RESPONSE
Y
N
N
A
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COMMENT
Question not asked. There did not
appear to be enough particulate matter
in the sample streams to require
changing the filter.
Two KNF Model UN035ST.1 11
diaphragm pumps with stainless steel
heads.
The sample flow rate was controlled by
a shutoff valve in the sample
distribution manifold and it was 1 2
L/min. The FTIR instrument required a
sample flow rate of 5 L/min and the
THC analyzer required a flow rate of
2.5 L/min. All three flow rates were
indicated by a flow meter in the
manifold. These flow rates were not
critical measurements and were not
recorded on data sheets. A back-
pressure regulator maintained the
manifold pressure at 4 to 5 psig. Excess
sample not used by the two instruments
was discarded through the sample
distribution manifold vent.
Not applicable.
Not applicable.
Not applicable.
Not applicable.
Not applicable.
Not applicable.
Technical Systems Audit of Test Methods Performed by MRI
2.14
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AUDIT QUESTIONS
20. When was the last time that the gas
meter thermometer was calibrated?
21. Is the thermometer calibration
traceable to NIST standards?
22. How is the stack gas stream
temperature measured?
23. How is the temperature sensor
calibrated?
24. When was the last time that the
temperature sensor was calibrated?
25. Is the thermometer calibration
traceable to NIST standards?
26. How is barometric pressure
measured?
27. How is the barometer calibrated?
28. When was the last time that the
barometer was calibrated?
29. Is the barometric pressure
calibration traceable to NIST
standards?
RESPONSE
Y
/
N
/
N
A
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COMMENT
Not applicable.
Not applicable.
A Type-K thermocouple was mounted
on the Pitot tube and was measured with
an Omega Model HH81 digital
thermometer.
The thermocouple was calibrated in a
boiling water bath, an ice water bath, or
a newly-acquired dry well and the
calibration temperature was measured
with an ASTM mercury-in-glass
thermometer.
24 March 1998
ASTM thermometers are traceable to
NIST standards.
Taylor aneroid barometer (Asheville,
NC) with a 600-foot altitude correction.
The asphalt plant is 540 feet above
mean sea level.
The aneroid barometer is compared to a
Sargent-Welch Model S-4519 mercury
column barometer.
14 July 1998
The mercury column barometer is
generally considered to be a primary
standard.
Technical Systems Audit of Test Methods Performed by MRI
2.15
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AUDIT QUESTIONS
RESPONSE
N
N
COMMENT
30. Describe the sample manifold.
Sample gas enters the sample
distribution manifold where it is
distributed by switching valves, shutoff
valves, and flow meters to the FTIR and
THC instruments. A back-pressure
regulator maintains the pressure in the
manifold. Excess flow is vented outside
the trailer.
31. Describe the calibration gas
manifold and associated calibration
gas lines to the sample probe and
sample manifold.
Calibration gas enters the sample
distribution manifold where it is
distributed by switching valves, needle
valves and flow meters either directly to
the FTIR and THC instruments or
indirectly to them via the sampling lines
and the calibration valves on the
sampling probes.
Additional Questions or Comments:
F. EXTRACTIVE FOURIER TRANSFORM INFRARED (FTIR) INSTRUMENT
1. Describe the extractive FTIR
instrument. List the brand, model
number, and serial number.
KVB Analect (Irvine, CA) Model RFX-
40 FTIR instrument with a glow-bar
light source and a liquid-nitrogen-
cooled mercury-cadmium-telluride
(MCT) detector. The FTIR instrument
has a 1 cm resolution, 400 to 4400 cm"
spectral range.
2. Does the instrument operate
according to an EPA method?
EPA Test Method 320
Technical Systems Audit of Test Methods Performed by MRI
2.16
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AUDIT QUESTIONS
3 . Describe the gas containment cell.
4. Is the pressure in the gas
containment cell monitored?
5. Describe the sample lines between
the sample distribution manifold
and the gas cell.
6. How are FTIR data recorded (e.g.,
data acquisition system)? Briefly
describe the system, giving its
brand, model, and serial number.
7. Does the data recording system
have a provision for documenting
operating parameters (e.g.,
resolution, pathlength, scan
number, sampling time, etc.) for
individual spectra? If not, are
these parameters documented in
some other manner?
8. Is there a back-up for the data
recording system?
RESPONSE
Y
/
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/
N
N
A
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/
COMMENT
Infrared Analysis Model D-22H variable
pathlength White cell inside an Infrared
Analysis G-5-22-V-BA-AU heated gas
cell oven that was maintained at a
temperature of 250 ° C. The light path
was aligned with a laser. The
pathlength was approximately 9 to 1 0
meters and was determined on a daily
basis by measurement of the calibration
transfer standard (CTS).
The cell pressure was monitored with an
Edwards Model W60041 1 1 1 Barocel
pressure sensor with a 0 to 1 000 mm Hg
range. This sensor is calibrated
annually at the factory and its readings
were verified using the barometer.
A 20-foot length of Technical Heaters
sampling line connected the FTIR
instrument to the sample distribution
manifold. The sampling line was
maintained at a temperature of 300° F.
Interferograms and sample spectra were
recorded on the hard drive of the
personal computer running the FTIR
software and on an external Iomega Jaz
drive.
The data recording system recorded
parameters (e.g., resolution) that were
directly related to the operation of the
FTIR instrument. Parameters (e.g.,
pathlength) that were not related to the
operation of the FTIR instrument were
recorded on a paper data sheet.
The external Iomega Jaz drive was the
back-up data recording system.
Technical Systems Audit of Test Methods Performed by MRI
2.17
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AUDIT QUESTIONS
9. Can raw FTIR spectra be recovered
from the backup?
10. Describe the routine sampling and
analysis procedure for the
instrument.
1 1 . What is the leak volume for the gas
containment cell?
12. What is the noise level in each
analytical region?
1 3 . What is the sample absorption
pathlength for each analytical
region?
14. What is the fractional analysis
uncertainty for each analytical
region?
15. What is the calibration frequency?
RESPONSE
Y
/
N
N
A
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COMMENT
Interferograms and sample spectra could
be recovered from the back-up data
recording system.
Sample gas flowed through the gas
containment cell on a continuous basis.
The sample flow rate was 5 liters per
minute. Over a 2- to 2.5-minute
sampling interval, 1 00 interferometer
scans were coadded. The FTIR
instrument converted the coadded
Interferograms into sample spectra.
Daily leak checks indicate that the cell
leak rate meets the acceptance criterion
of less than 4 %/minute.
Typical noise levels range between 10"3
and 10'4. On the morning of 22 July 98,
the noise level was 10'4 in the 1000 to
1300 cm"1 spectral region in which
volatile organic compounds (VOC)
absorb light. In general, noise levels are
dependent on sample moisture levels,
which will vary from source to source.
The nominal pathlength is 10.5 meters.
The actual pathlength was determined
from measurements of the CTS. See
Item G35 below.
The calculated uncertainty in the
measured concentration of the CTS
because of errors in the mathematical
comparison of reference and sample
spectra will be determined during the
post sampling analysis phase of the
project .
The CTS was measured at the beginning
and end of each test. The sulfur
hexafluoride (SF6) calibration gas and
the SF6/toluene sampling bias check gas
were measured daily.
Technical Systems Audit of Test Methods Performed by MRI
2.18
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AUDIT QUESTIONS
1 6. Describe the routine calibration
procedure for the instrument.
1 7. Does the calibration
documentation show that the
calibration procedures are being
followed?
1 8. What is the sampling system bias
according to the calibration
documentation?
19. How frequently are background
spectra collected?
RESPONSE
Y
N
N
A
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/
COMMENT
The gas containment cell was evacuated
to a pressure of 10 mm Hg and then was
filled to atmospheric pressure with the
CTS. The mean CTS concentration
across the entire project was compared
with the certified value to determine the
pathlength of the cell. The SF6 standard
was used for the capture efficiency tests.
The SF6/toluene sampling bias check
was used to determine sampling line
losses by comparing the ratio of direct
FTIR measurements of the two
compounds in the gas mixture with the
corresponding ratio for measurements of
the same gas mixture after it passed
through the sample probe calibration
valve and the sampling line.
A letter from MRI to RTI presents CTS
calibration data which were collected
several times each day. No SF6 or
SF6/toluene calibration data were
presented in the letter because they will
be determined during the post sampling
analysis phase of the project.
The SF6/toluene calibration mixture is
delivered to the calibration valve on the
sample probe and directly to the FTIR
instrument. The bias will be determined
during the post sampling analysis phase
of the project by comparison of the two
sets of SF^/toluene data.
Background spectra using pure nitrogen
were collected at the beginning and end
of the day. The first spectrum was used
routinely for the entire day unless the
second spectrum seemed to be more
representative.
Technical Systems Audit of Test Methods Performed by MRI
2.19
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AUDIT QUESTIONS
20. Are emissions measurements
corrected for background
interference?
2 1 . How are compounds in the sample
identified?
22. What is the source of reference
spectra and absorption coefficients
for identified compounds?
23. What will be done for compounds
without reference spectra?
24. How will unidentified peaks be
reported?
25. How are concentrations
calculated?
RESPONSE
Y
/
N
N
A
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COMMENT
Sample spectra were corrected for
background interferences associated
, with the light source, the gas cell, and
the detector.
Thomas Geyer will, analyze sample
spectra and will identify detected
compounds after the completion of the
testing using reference spectra or other
spectroscopic analysis techniques.
The EPA reference spectra database will
be the primary source of reference
spectra. Other spectral databases will
be used if necessary.
If MRI discovers significant,
unidentified spectral features in the
sample spectra, the EPA Work
Assignment Manager will be consulted
regarding whether these features are to
be identified by laboratory
measurements.
The primary goal of the testing was not
to identify all compounds in the sample
spectra, but to determine the
concentrations in the emissions of a
specific list of hazardous air pollutants
(HAPs) and other compounds.
QAPP Section 4.4 states that a K-matrix
analytical procedure used uses sample
spectra collected during the emissions
testing and reference spectra for
identified compounds from the EPA
library to calculate a least-squares fit of
the spectral features and to determine a
concentration for each identified
compound.
Technical Systems Audit of Test Methods Performed by MRI
2.20
-------
AUDIT QUESTIONS
26. What are the minimum detectable
concentration for the compounds
of interest?
27. Does the FTIR instrument have
any spectral interferants for the
compounds of interest?
28. How are the FTIR data corrected
for analytical interferants?
RESPONSE
Y
/
N
N
A
/
/
COMMENT
Scott Klamm estimated that the
minimum detectable concentration
ranges between 0.5 and 5 ppm
depending on the compound. Thomas
Geyer noted that the sensitivity limit is
at low ppb-levels and the minimum
quantitation limit (MQL) is in low ppm-
levels for samples containing
considerable amounts of water and
carbon dioxide. For toluene and the
xylenes, the MQL is estimated to be
greater than the 1 00 ppb that was
measured during preliminarv testing.
Water vapor and carbon dioxide are
common analytical interferants in
sample spectra.
An integrated bag sample of the
emissions was collected for each test
run. The bag's moisture and carbon
dioxide levels were determined with an
Orsat analyzer. The measured levels
were used to select appropriate water
vapor and carbon dioxide reference
spectra for use in sample spectra
analysis by Thomas Geyer after
completion of the field portion of the
project.
Technical Systems Audit of Test Methods Performed by MRI
2.21
-------
AUDIT QUESTIONS
29. List the calibration transfer
standards (CTSs) for the FTIR
instrument
30. Do the CTSs have appropriate gas
mixtures and concentrations for the
sample gas mixtures and
concentrations?
3 1 . What is the analytical uncertainty
of the CTSs?
RESPONSE
Y
N
N
A
COMMENT
The CTS was Scott Specialty Gases
cylinder number ALM005893
containing 99.9 parts per million (ppm)
ethylene in nitrogen. This gas mixture
was analyzed on 31 March 1998.
The SF6 tracer calibration gas was Scott
Specialty Gases cylinder number
ALM033887 containing 0.205 ppm SF6
in nitrogen. It was analyzed 7 April
1998.
The sampling bias check gas was Scott
Specialty Gases cylinder number
AAL 17264 containing 3.83 ppm SF6
and 105 ppm toluene in nitrogen. It was
analyzed on 7 April 1998.
FTIR Protocol Section 4. 5.1 specifies
that each analytical region lie within
25% of the CTS position. The CTS for
this testing is a compressed gas
calibration standard containing 1 00 ppm
(±2 %) ethylene in nitrogen. This gas
mixture was selected as the CTS
because it has an light absorption line at
949 cm , which meets the specification
for SF6 (942 cm'1), toluene (727 cm'1),
and xylenes (740 to 797 cm"1).
A letter from MRI to RTI presents
certificates of analysis for CTS, SF6,
and SF6/toluene calibration standards.
All three standards have an analytical
uncertainty of ±5%. Section 7.2 of Test
Method 320 directs the analyst to
"obtain a NIST-traceable, gravimetric
standard of the CTS (±2 percent)".
Technical Systems Audit of Test Methods Performed by MRI
2.22
-------
AUDIT QUESTIONS
32. Are the CTSs traceable to NIST
SRMs or otherwise traceable to
NIST? EPA Test Method 320
specifies that the CTS be a NIST-
traceable gravimetric standard (±
2%).
33. Have the CTSs been independently
verified by MRI?
34. Are the CTS regulators and
delivery system properly
maintained?
35. What is the variation of successive
CTS absorbency measurements
relative to their mean value?
36. Is there a schedule of preventive
maintenance for the FTIR
instrument?
37. Are calibration and maintenance
logs kept for the FTIR instrument?
RESPONSE
Y
/
N
/
/
/
/
N
A
/
COMMENT
A letter from MRI to RTI states that the
calibration standards are traceable to the
specialty gas producer's primary
reference standards, which are prepared
using gravimetric procedures. These
calibration standards are not traceable to
NIST as NIST defines traceabiliry for
compressed gas standards. NIST does
not have SRMs for this gas mixture.
The calibration standards were not
independently verified by MRI.
The pressure regulators and the
associated gas handling equipment
appear to be well-maintained.
A letter from MRI to RTI presents the
CTS calibration data, which yielded a
mean pathlength of 10.475 meters and a
maximum deviation from the mean of
0.337 netersor3.2%ofthemean.
These data meet the QAPP's precision
specification of agreement to within
±%5 of the mean.
The instrument is three years old and
Scott Klamm indicated that it had not
been serviced by a factory
representative during that period. All
maintenance is done on an as-needed
basis.
Calibration data are recorded on data
sheets, rather than in logbooks. There
are no maintenance logs.
Technical Systems Audit of Test Methods Performed by MRI
2.23
-------
AUDIT QUESTIONS
38. Review any maintenance and
operational records for the FTIR
instrument. Based on these
records, does the instrument appear
to be in good operating condition?
39. Are the manufacturer's operating
manuals readily available to the
FTIR instrument operators?
RESPONSE
Y
/
N
/
N
A
COMMENT
The FTIR instrument was manufactured
by KVB Analect, which is located in
Irvine, California. A factory service
representative optimized the
interferometer on 20 July 1998 in the
presence of the assessors. The FTIR
instrument appeared to be in good
operating condition after it was
optimized.
Neither MRI's FTIR operator nor the
KVB Analect factory service
representative had a copy of the
operating manual.
Additional Questions or Comments: QAPP Section 3.1.1 states that the time for 5 cell volumes to
pass through the cell is considered the minimum interval separating independent samples. If the cell
volume is 8.5 L, then 5 cell volumes corresponds to 42.5 L. If the FTIR sample gas flow rate is 5
L/min and the FTIR sample interval is 2.5 minutes, only 12.5 L (or 1.5 cell volumes) of sample gas
passes through the cell between measurements. Therefore, a individual FTIR measurement cannot be
considered to be completely independent of the measurements that immediately precede it. Scott
Klamm confirms that it takes 3 to 4 samples to flush the cell for CTS measurements.
During the emissions testing, MRI analyzed a nine-component hydrocarbon calibration standard
(Spectra Gases cylinder number CC91245) that had been brought to the hot mix asphalt plant by
Emissions Monitoring, Inc. The analysis of this calibration standard does not constitute a
performance evaluation of the extractive FTIR method because MRI was not informed of the analysis
prior to the emissions testing nor during our initial on-site meeting on 20 July 1998. The results of
the analysis were not available during the RTI assessor's conversation with MRI's Thomas Geyer on
August 27, 1998. RTI suggests that the results of the MRI's analysis of this calibration standard be
included in MRI's emissions testing report, which will allow EPA to compare the MRI analytical
results with the attached certificate of analysis for the calibration standard.
Technical Systems Audit of Test Methods Performed by MRI
2.24
-------
AUDIT QUESTIONS
RESPONSE
Y
N
N
A
COMMENT
G. SAMPLE CONCENTRATOR FOR FTIR INSTRUMENT
1 . Describe the sample concentrator.
2. Does the concentrator operate
according to an EPA method?
3. If it is not an EPA method, what
documentation exists concerning
laboratory and field validations of
the concentrator?
/
/
Samples were concentrated for FTIR
analysis by pulling source gas through
two traps containing 20 grams of Tenax
adsorbent. VOCs that were collected on
the Tenax were desorbed by heating the
trap to 220° C. Nitrogen flowing
through the heated trap transferred the
VOCs to an evacuated gas containment
cell, which has a volume of 8.5 L. If the
source gas flowed through the Tenax
trap for 4 hours at a flow rate of 1 .5
L/min, source gas samples were
concentrated by a factor of about 42.
The method is still experimental and has
not been standardized as an EPA test
method.
Set comment below Item G32.
Technical Systems Audit of Test Methods Performed by MRI
2.25
-------
AUDIT QUESTIONS
4. Have the validations involved the
compounds of interest to this
study?
5. Describe the sample lines between
the sample distribution manifold
and the concentrator.
6. Describe how sample is drawn
through the Tenax adsorbent trap.
RESPONSE
Y
/
N
N
A
/
/
COMMENT
SSTP Section 4.1.2 states that
preliminary measurements by Pacific
Environmental Services (PES) at the
asphalt plant indicated the presence of
toluene and xylenes at concentrations
below 1 00 ppb. '
The 1993 FTIR method validation
report by Entropy Environmentalists
included the following correction
factors and relative standard deviations
(RSDs) in concentrated samples:
Correction
Compound Factor RSD(%)
toluene 0.83 10.31
m-xylene 0.78 4.85
p-xylene 1.16 14.25
For the method to be acceptable, the
correction factor must be between 0.70
and 1 .30 and the RSD must be < 50%.
MRI does not plan to correct the
indirect FTIR data for the surrogate
spike gas collection efficiency.
The sample concentrator was not
connected to the sample distribution
manifold. It was mounted on a separate
VOST sampling train at the sampling
port.
Source gas is pulled through the
sampling probe, a 5-foot run of heated
sampling line, an intake manifold, a
condenser, one Tenax trap, a water
drop-out trap, a second condenser, a
second Tenax trap, and a Nutech Model
280/0 1BVOST pump box.
Technical Systems Audit of Test Methods Performed by MRI
2.26
-------
AUDIT QUESTIONS
7. What are the sample flow rate,
sample duration, and sample
volume?
8. Describe how the flow rate is
measured and controlled.
9. Describe how the total sample
volume is measured.
1 0. Describe how the sample volume
meter is calibrated.
1 1 . When was the last time that the
sample volume meter was
calibrated?
12. Is the volumetric calibration
traceable to NIST standards?
13. How is the first condenser's
temperature measured?
14. How is the first condenser's
thermometer calibrated?
15. When was the last time that the
first condenser's thermometer was
calibrated?
1 6. Is the thermometer calibration
traceable to NIST standards?
RESPONSE
Y
/
N
N
A
/
/
/
/
/
/
/
/
COMMENT
The sample flow rate was 1 .5 L/min, the
sample duration was 4 hours, and the
sample volume was 360 L.
A Matheson rotameter measured the
sample flow rate and a needle valve
controlled the flow rate.
A Single Model 802 dry gas meter in the
VOST pump box measured the sample
volume.
The dry gas meter and the rotameter
were calibrated by a wet test meter in
three separate runs of 14 to 21 L each
13 July 1998
The wet test meter was calibrated on an
annual basis with a calibrated water
volume, which MRI considers to be a
primary standard. A wet test meter
calibration data sheet dated 2 May 1997
shows that it was calibrated according to
ASTM Method D 107 1-83.
The temperature was measured with a
Type-K thermocouple and a Omega
Model HH81 digital thermometer.
The thermocouple was calibrated with a
boiling water bath, an ice water bath, or
a recently-acquired dry well as
appropriate. An ASTM mercury-in-
glass thermometer was the reference
standard.
24 March 1998
ASTM thermometers are traceable to
NIST.
Technical Systems Audit of Test Methods Performed by MRI
2.27
-------
AUDIT QUESTIONS
1 7. How is Tenax cleaned prior to
sampling?
1 8. Has the Tenax used in this project
passed the 5-ppb THC pass/fail
criterion for cleanliness?
19. What is the surrogate spike gas?
RESPONSE
Y
N
/
N
A
/
/
COMMENT
Precleaned Tenax was purchased for the
emissions testing. Before a Tenax trap
was used, it was further cleaned by
being heated in the thermal desorber to
180° C for 1 hour while nitrogen
removed any residual VOCs. The
Tenax trap was then desorbed into the
FTIR instrument and a blank spectrum
for the cleaned trap was recorded.
Cleanliness for cleaned Tenax traps was
verified by field FTIR checks, rather
than by laboratory FID checks, which
are associated with the 5 ppb cleanliness
criterion.
Scott Specialty Gases cylinder number
ALM031809, 10.6 ppm toluene-d8 in
nitrogen, analyzed 2 April 1998. The
attached certificate of analysis lists the
analytical accuracy of ±5%. Section 9.1
of Test Method 320 specifies the use of
"a certified standard (accurate to ±2
percent) of the target analyte, if one can
be obtained".
Technical Systems Audit of Test Methods Performed by MRI
2.28
-------
AUDIT QUESTIONS
20. Does the surrogate spike gas have
an appropriate gas mixture and
concentration for the sample gas
mixture and concentration?
2 1 . How is the surrogate spike gas
added to the sample?
RESPONSE
Y
/
N
A
/
COMMENT
SSTP Section 5.2 states that toluene was
chosen as the surrogate spiking gas
based on results reported by PES from
preliminary sampling conducted during
their pretest site survey. These
measurements indicated the presence of
toluene and xylenes at concentrations
below 100 ppb. Item Gl above
determines the Tenax concentration
factor to be 42. If the sample
concentration method had been used
during PES' preliminary measurements,
the toluene concentration in the gas cell
would have been less than 4.2 ppm.
This calculated concentration differs
from the surrogate spiking gas
concentration by a factor of 2.5.
Appendix D in the QAPP states that
surrogate spiking gas concentrations
should approximate the levels expected
in the trap after sample collection.
Approximately 1 gas cell volume of the
surrogate spike gas was loaded onto the
Tenax trap before sampling using the
thermal desorber at ambient
temperature. Note that this spiking
procedure deviated from QAPP Section
5.1.3, which states that the vapor-phase
spike will be heated and injected into
the back of the sampling probe, similar
to the Method 320 analyte spike
procedure. This deviation was
necessary because a VOST train was
used to pull source gas directly from the
source through about 5 feet of heated
sample line into the Tenax trap.
Technical Systems Audit of Test Methods Performed by MRI
2.29
-------
AUDIT QUESTIONS
22. Describe any ambient air samples
that are collected.
23 . Describe any train blanks that are
collected.
24. Describe any preliminary sampling
that occurs.
25. Describe any duplicate train
samples that are collected.
26. Describe any breakthrough traps
that are used in the sample train.
27. Describe how Tenax samples are
stored prior to analysis.
28. How much time elapses between
sampling and analysis of Tenax
samples?
RESPONSE
Y
N
N
A
/
/
/
/
/
/
/
COMMENT
An ambient air sample was collected on
the morning of Wednesday, 22 July
1998 using VOST Control Box #3. The
sample was collected at the load-out
tunnel entrance where diesel trucks wait
to be loaded.
A train blank was collected in the trailer
at the beginning of the emissions testing
by passing 90 L (1 .5 L/min for 1 hour)
of nitrogen through the Tenax train
No preliminary sampling was conducted
due to time delays at the beginning of
the emissions testing due to asphalt
plant equipment breakdowns.
A duplicate train sample was collected
on 25 July 1 998, but the FTIR sample
spectrum was not saved. A second
attempt to collect a duplicate train
sample was scheduled for 27 July 1998
after the assessors departure. The
results of the post sampling analysis of
this sample were not available for
review as of 27 August 1998.
A second Tenax trap was mounted
downstream of the first trap to collect
any VOCs that might break through.
Tenax traps were capped after sampling
and then were stored on ice until they
were analyzed.
In general, the Tenax traps are analyzed
within an hour or two of the end of a
test run. However, the traps of 24 July
1998 were not analyzed until 25 July
1998 due to the need to produce cleaned
traps for the next day.
Technical Systems Audit of Test Methods Performed by MRI
2.30
-------
AUDIT QUESTIONS
29. How are Tenax samples identified?
30. How is the sample desorbed from
the Tenax and transferred to the
gas containment cell?
3 1 . What current or previous data are
available concerning the
desorption efficiencies for the
compounds of interest and the
surrogate gas?
32. What is the detection limit for the
compounds of interest using the
sample concentrator?
RESPONSE
Y
N
N
A
/
/
/
/
COMMENT
All Tenax traps had an engraved
number on their bodies. Additionally,
green sticky tape with the intended
usage was attached to the traps after
cleaning.
The FTIR gas containment cell was
evacuated to a pressure of 10 mm Hg.
The Tenax trap was heated to 220° C in
the thermal desorber. A heated transfer
line at 250° C was opened between the
thermal desorber. Nitrogen carried the
VOCs into the 8.5-L gas cell at a flow
rate of 1 L/min until the cell returned to
atmospheric pressure.
The 1993 FTIR method validation
report by Entropy Environmentalists
included the following correction
factors:
toluene 0.83
m-xylene 0.78
p-xylene 1.16
For the method to be acceptable, the
correction factor must be between 0.70
and 1 .30 as per EPA Method 301 . No
information is available for the
desorption efficiencies for other
compounds that might be found in the
asphalt plant.
The attached letter from MRI implies
that sampling parameters were chosen to
obtain minimum detectable
concentrations of 1 00 ppb for toluene
and xylene, which were identified by
PES' preliminary measurements.
Technical Systems Audit of Test Methods Performed by MRI
2.31
-------
AUDIT QUESTIONS
RESPONSE
Y
N
N
A
COMMENT
Additional Questions or Comments: The sample for the morning of 22 July 1998 had an ambient
air leak for an unknown period of time (10 minutes?) due to the first condenser separating from the
inlet manifold.
There is little documentation for the FTIR sample concentration method. The QAPP contains a fairly
general discussion of the method that only briefly mentions the validations of the method. The
validations were reported to EPA in project reports by Entropy Environmentalists and MRI. In 1993,
Entropy performed a FTIR method validation at a coal-fired boiler. Multi component gas mixtures
were spiked into boiler emissions, which were sampled by four parallel sample concentrators similar
to the one used in this emissions testing.
This method validation found that EPA Method 301 validation criteria were met for toluene and
xylenes in concentrated samples. Pacific Environmental Services found these compounds during its
preliminary measurements at the hot-mix asphalt plant. If MRI discovers significant concentrations
of other chemical compounds in the asphalt plant emissions, then the report of MRI's emissions
testing should note that the FTIR sample concentrator method has not been validated for these
additional compounds.
The 1993 tests used a KVB Analect Model RFX-40 FTIR instrument with a MCT detector and an
Infrared Analysis Model 5-22H gas containment cell with a pathlength of 22 m. The sample volume
was 280 L. The target gas mixture concentrations in the FTIR gas cell were 20 ppm. The CTS was
100 ppm ethylene in nitrogen.
H. TOTAL HYDROCARBONS (THC) ANALYZER
1 . Describe the THC analyzer. List
the brand, model number, and
serial number.
2. Does the THC analyzer operate
according to an EPA method?
3. How are THC data recorded (e.g.,
data acquisition system)? Briefly
describe the system, giving its
brand, model, and serial number.
/
/
/
Two J.U.M. Engineering Model VE7
total hydrocarbon analyzers were used
for the emissions testing. A third
analyzer was rented when one of the
original analyzers failed.
EPA Test Method 25A
THC data were recorded with a
Winbook XP laptop computer with a
data acquisition system docking station
and Labtech Notebook software. Data
were collected at 1 -second intervals and
1 -minute mean concentrations were
stored on the computers hard drive.
Technical Systems Audit of Test Methods Performed by MRI
2.32
-------
AUDIT QUESTIONS
4. Does the THC data recording
system have a provision for
documenting changes in operating
parameters? If not, are changes in
operating parameters documented
in some other manner?
5 . Is there a hard copy back-up for the
THC data recording system?
6. Can THC data be recovered from
the hard copy backup?
7. Describe the sample lines between
the sample distribution manifold
and the THC analyzer.
8. Describe how sample is drawn
through the THC analyzer.
9. What is the sample flow rate and
the bypass flow rate?
1 0. Describe how the flow rates are
measured and controlled.
1 1 . Describe how the flow rate meters
is calibrated.
RESPONSE
Y
/
/
N
/
N
A
/
/
/
/
/
COMMENT
The data recording system collected the
date and time, but not other operational
parameters. Other parameters,
including calibration data, were
recorded on a legal pad.
A paper copy of data from the computer
is printed by a Panasonic KX-P1 180i
printer.
Data would have to be reduced by hand
from the paper copy.
Approximately 6 feet of heated
sampling line connect the sample
distribution manifold to the THC
analyzer. The sampling line was
maintained at 300° C.
A pump pulled sample into an oven
heated to 300° C and through a sample
filter at a flow rate of approximately 2.5
L/min. The pump pushed sample
through a sample capillary into the
flame ionization detector (FID). The
excess sample was vented through a
bypass capillary. A back-pressure
regulator and a pressure gauge controls
the sample pressure to approximately
200 millibar (or 3 psig) inside the
instrument.
The total sample flow rate was
approximately 2.5 L/min and the flow
rate into the FID was approximately 20
mL/min.
The flow rates are controlled by the
capillaries and the back-pressure
regulator. The flow rates are not
measured.
Not applicable.
Technical Systems Audit of Test Methods Performed by MRI
2.33
-------
AUDIT QUESTIONS
12. When was the last time that the
flow rate meters were calibrated?
1 3 . List the flame ionization detector
hydrogen (vendor, grade, etc.).
14. List the flame ionization detector
burner air (vendor, grade, etc.).
15. What is the THC analyzer
calibration frequency?
1 6. Describe the routine THC analyzer
calibration procedure.
1 7. Does the THC analyzer calibration
documentation show that the
calibration procedures are being
followed?
1 8. List the THC calibration gases
(including zero gas).
RESPONSE
Y
/
N
N
A
/
/
/
/
/
/
COMMENT
Not applicable.
Air Products cylinder number
SGKK064 (40%hydrogen, 60% helium,
analyzed on 11 June 1998).
Ambient air is drawn through a charcoal
scrubber by an internal pump and
hydrocarbons in the air are removed.
Bob Gulick indicated that methane
passes through the scrubber.
As per Method 25A, the THC analyzer
is calibrated at the beginning of the test
run and a drift check is done at the end
of the run. Bob Gulick will do more
frequent drift checks if he is concerned
about possible drift during a test run.
Calibration gas mixtures of varying
concentrations (e.g., 0, 25, 50, and 90
ppm) are prepared in the Environics
Model 2020 gas dilution system from a
propane calibration standard and
nitrogen. The calibration gas mixtures
flow through the sample line to the
calibration valve in the sample probe.
The attached letter from MRJ presents
draft calibration data for the THC
analyzer, which indicate that the
calibration procedures were followed.
Air Products and Chemicals cylinder
number SG91 68085, 3690 ± 23 ppm
propane in nitrogen (EPA Protocol
Gas), analyzed by gas chromatography-
FIDonS August 1996.
Technical Systems Audit of Test Methods Performed by MRI
2.34
-------
AUDIT QUESTIONS
19. Do the THC calibration gases have
appropriate gas mixtures and
concentrations for the sample gas
mixtures and concentrations?
20. What is the analytical uncertainty
of the THC calibration gases?
2 1 . Are the THC calibration gases
traceable to NIST SRMs or
otherwise traceable to NIST?
22. Have the THC calibration gases
been independently verified by
MRI?
23. Are the THC calibration gas
regulators and delivery system
properly maintained?
24. What is the THC analyzer
calibration error according to the
calibration documentation?
25. What is the THC analyzer linear
error according to the calibration
documentation?
RESPONSE
Y
/
/
/
N
/
N
A
/
/
/
COMMENT
The THC calibration gas mixture is
appropriate. The concentration is
appropriate because the gas mixture is
diluted by an Environics Model 2020
gas dilution system, whose flow meters
were calibrated at the factory using a
Sierra Cal Bench on 23 April 1998.
The analytical uncertainty of the THC
calibration gas is 23 ppm or 0.6 percent
of the certified concentration. The
specified uncertainty of the gas dilution
system's flow rates is 0.5 percent.
The THC calibration gas is traceable via
a 4723 ppm propane gas manufacturer's
internal standard (GMIS), which is
directly traceable to a NIST SRM.
An independent verification is not
necessary because the THC calibration
gas is an EPA Protocol Gas.
No problems were observed.
The attached letter from MRI presents
draft calibration data for the THC
analyzer, which indicate that the
calibration error ranged between 0.0%
and 4.8%, which is less than the ±5%
criterion specified in Test Method 25A.
Section 2.2.1.2 of the QAPP specifies a
±2% accuracy criterion for linear.
However, this criterion does not appear
in Test Method 25A and appears to be
an error in the QAPP.
Technical Systems Audit of Test Methods Performed by MRI
2.35
-------
AUDIT QUESTIONS
26. What are the THC analyzer zero
and calibration drifts according to
the calibration documentation?
27. What is the sampling system bias
according to the THC analyzer
calibration documentation?
28. Is there a schedule of preventive
maintenance for the THC
analyzer?
29. Are calibration and maintenance
logs kept for the THC analyzer?
30. Review maintenance and
operational records for the THC
analyzer. Based on your findings,
does it appear to be in good
operating condition?
3 1 . Are the manufacturer's operating
manuals readily available to the
THC analyzer operator?
RESPONSE
Y
/
/
N
/
/
N
A
/
/
COMMENT
The attached letter from MRI presents
draft calibration data for the THC
analyzer, which indicate that zero drift
ranged between 0.0% and 1 .0%, which
is less than the ±3% criterion specified
in Test Method 25A. Span drift ranged
between 0.0% and 1 .4%, which is less
than the ±3% criterion.
Section 2.2.1 .2 of the QAPP specifies a
±5% accuracy criterion for systems bias.
However this criterion does not appear
in Test Method 25A and appears to be
an error in the QAPP.
Maintenance is performed on an as-
needed basis in MRI's laboratories and
in the field.
No logs are available.
Visual Inspection of the two THC
analyzers indicates that they were in
good operating condition at the
beginning of the project. See additional
comment below.
The operator has a manual for the THC
analyzer.
Technical Systems Audit of Test Methods Performed by MRI
2.36
-------
AUDIT QUESTIONS
RESPONSE
Y
N
N
A
COMMENT
Additional Questions or Comments: Something associated with emissions from the silo seemed to
be damaging THC analyzers. Beginning on 23 July 1998, one THC analyzer sampled the load-out
tunnel and another THC analyzer sampler the silo. On 24 July 1998, the silo THC analyzer's FID
flamed out and could not be relighted. The remaining THC analyzer sampled both locations until
early afternoon on 25 July 1998 when it also flamed out. A rental THC analyzer arrived at noon on
25 July 1998 and was used for the remainder of the day. The second THC analyzer's FID was baked
at high temperature and appeared to be operational on 26 July 1998, although it was not used for that
day's sampling. One hypothesis is that heavy hydrocarbons from the silo or their oxidation products
may be clogging the FID burner tip. However, a 20 August 1996 e-mail message from a JUM
Engineering representative to RTI indicates that a number of their THC instruments are operating at
asphalt plants for raw emissions as well as for emissions after treatment.
There appear to be some errors in the draft THC calibration data the MRI submitted for review. The
span drift data for stack dryer Runs 1 and 2 are identical, which is an unlikely occurrence. There
appear to be errors in the calculated span drifts for Dryer Stack Run 1 and Load-out Runl. These
errors do not appear to be major problems.
I. CAPTURE EFFICIENCY TEST
1 . Describe the apparatus for
releasing the tracer gas.
2. How is the tracer gas measured?
3. How does the tracer gas operator
switch from one release point 10
another release point?
/
/
/
Tracer gas passes from a compressed
gas cylinder through a pressure gauge
and a mass flow meter to four sets of
toggle valves and needle valves, which
are set to deliver 4 L/min. Teflon®
tubing goes from each needle valve to
six critical orifices that are set at the
base of one asphalt silo. Each critical
orifice has a maximum flow rate of 0.8
L/min.
Tracer gas is measured by the extractive
FTIR instrument .
The tracer gas operator uses the toggle
valves to control silo at which tracer gas
is being released. Information about
which silo is being used is radioed to the
operator from an observer in the asphalt
plant's control room.
Technical Systems Audit of Test Methods Performed by MRI
2.37
-------
AUDIT QUESTIONS
4. Describe the tracer gas.
5 . Does the tracer gas have an
appropriate gas mixture and
concentration for the capture
efficiency test?
6. What is the analytical uncertainty
of the tracer gas?
7. Is the tracer gas traceable to NIST
SRMs or otherwise traceable to
NIST?
8. Has the tracer gas been
independently verified by MRI?
9. Is the tracer gas regulator and
delivery system properly
maintained?
1 0. What is the tracer gas flow rate?
1 1 . Describe how the tracer gas flow
rate is measured and controlled.
1 2. Describe how the tracer gas flow
rate meter is calibrated.
1 3 . When was the last time that the
tracer gas flow rate meter was
calibrated?
RESPONSE
Y
/
/
N
/
/
N
A
/
/
/
/
/
/
COMMENT
Scott Specialty Gases cylinder number
ALMO 13870, 1 .99 percent sulfur
hexafluoride (SF6) in nitrogen (certified
working standard), analyzed on 2 April
1998.
If the load-out tunnel emissions control
system has a flow rate of 1 5,000 dscm,
the FTIR instrument will sample a SF6
concentration of 0.19 ppm, which is
easily detected by the extractive FTIR
instrument with a 10-meter pathlength.
The SF6 calibration gas has a
concentration of 0.205 ppm , which
closely matches the sample's SF6
concentration
±5 percent
The tracer gas is traceable to the
specialty gas producer's primary
standards.
The equipment appears to have been
properly maintained.
4 L/min
The flow rate is measured by a mass
flow meter and is controlled by a needle
valve.
The flow meter was calibrated with a
Sierra Instruments Cal-Bench™ (serial
number AN0125), which has a 1%
accuracy.
30 April 1998
Technical Systems Audit of Test Methods Performed by MRI
2.38
-------
AUDIT QUESTIONS
14. Is the tracer gas flow rate
calibration traceable to NIST
standards?
RESPONSE
Y
/
N
N
A
COMMENT
The Sierra Instruments Cal-Bench™
automated primary gas flow calibration
system is traceable to NIST length and
time standards.
Additional Questions or Comments:
Technical Systems Audit of Test Methods Performed by MRI
2.39
-------
Midwest Research Institute Standard Data Forms for
Emissions Testing at a Hot Mix Asphalt Plant
Technical Systems Audit of Test Methods Performed by MRI 2.40
-------
' " "\ *\ "* t *
^ /
MIDWEST RESEARCH INSTII
Kansas City, Missouri
Tefephone JB16) 753
Telefax (816) 753
SUBJECT TO CAA CGKRDENTIAL
BUSiNESS INFORMATION CLAIM
Does Not Conteinflafiona! security Information
August 14, 1998
Mr. Robert Wright
Research Triangle Institute
3040 Comwallis Road
Post Office Box 12 194
Research Triangle Park, NC 27709
Dear Mr. Wright,
Enclosed are responses to your request for technical information related to the
technical system audit of the recent emissions testing at a hot-mix asphalt plant
performed by Midwest Research Institute (MRI), In attempting to respond to your need
for timeliness of a draft report (August 21), all issues easily completed have been
included in this response. Several issues, however, cannot be completed at this time, and
are expected to be available through our report to EPA, which is due by September 30,
1998. These issues have been appropriately marked in the following list. I have also
included your original references to "checklist section" for clarity.
1. (A9) Raw quality control/calibration data sheets and/or calculated calibration data for
the FTJR instrument (e.g. CTS, SF6, or SF6/toluene measurements) and the total
hydrocarbon instrument (e.g. calibration error, linearity error, zero and calibration
drift, sampling system bias.
Both the FTIR and THC met all calibration requirements during the test program,
FTIR pathlength determination and CTS calculations are attached. Criteria for
pass/fail for the CTS spectra are +/- 5%, which all of the CTS spectra met.
SF6/toluene determinations are not yet complete, but will be included in the final
report.
THC calibration error, zero drill and calibration drift calculations are also attached.
The THC analyzer met all criteria, which include +/- 5% for calibration error, and +/-
3% for zero drift and calibration drift. Procedures followed EPA Method 25A, which
requires calibrations through the sample line. Thus, there are no other linearity or
system bias checks associated with this method.
Note that the attached data have not been finalized and approved by MRI's QA
procedures and have been stamped as "Draft."
-------
24. (HIS) A copy of the certificate of analysis for the THC analyzer's calibration gas and
information about its analytical uncertainty, traceability, and any independent
concentration verifications.
The THC calibration gas certificate of analysis is attached. The gas is an EPA
Protocol gas, and meets all requirements of that certification.
25. (HIS) Information about the annual factory calibration of the Environics Model 2020
gas dilution system and any field evaluations according to EPA Test Method 205.
Calibration records for the Environics gas dilution system are attached
26. (H30) Information about any maintenance logs for the THC analyzer
THC maintenance is performed on an as needed basis in MRI's laboratories and in
the field. No other maintenance logs are available.
I hope you find the attached information helpful and allow you to complete those
sections of your audit. If you have additional questions, please feel free to call me at
816-753-7600, ext. 1228.
Sincerely,
MIDWEST RESEARCH INSTITUTE
Scott W. Klamm
Environmental Engineer
cc: J. Hosenfeld
J. Balsinger
T. Geyer
M. Toney
-------
2. (AID) Blank copies of data sheets used for recording load-out operations data and
tracer gas release data.
Blank copies of data sheets used for recording load-out operations data and tracer gas
release data are attached.
3. (A14) Identification of any MRI personnel performing reviews of QC data from the
emissions testing.
MRI has a formal review process for all reports generated under this contract. The
review process includes a review and signature requirement by the Work Assignment
Leader, Program Manager, and Senior Quality Assurance Officer. Specific to this
project, these individuals would be Mr. Scott Klamm (Field Team Leader), Dr. Tom
Geyer (FT1R Oversight), Mr. John Hosenfeld (Work Assignment Leader), Dr. Bruce
Diel (OPPT Program Manager), and Mr. Jack Balsinger (Senior Quality Assurance
Officer). These individuals are in accordance with the organizational chart (Figure
1-1) of the QAPP.
4. (C3) Information about any current summaries (e.g. training files) of the training and
qualifications of each project team member.
MRI maintains a file of personnel resumes and curriculum vitae for each project team
member detailing their experience and qualifications. Single page summaries for
each team member are attached.
5. (C4) Information about any descriptions of individual project team member
responsibilities.
Individual project team member responsibilities are briefly summarized in the QAPP,
Section 1.4. Specific responsibilities not described in the QAPP were assigned at
MRI project coordination meetings prior to the field phase, and were updated on a
daily basis during the field effort
6. (D4) Information about the source (e.g. documented performance criteria or actual
QC data) for the data quality indicator goals for the sample concentration FTIR
method.
This comment will be addressed in the report
-------
7. (F12) Information about noise levels for each FTIR analytical region
As demonstrated to RTI in the field, RMSD noise levels in the sample spectra were
on the order ofO.OOOl absorbance units in the 1000-1300 wavenumber region, In the
report, RMSD in the residual (subtracted) spectra will also be calculated (i.e. after
analysis).
8. (F13) Information about sample absorption pathlengths for each FTIR analytical
The average pathlength for the test program was determined from the daily CIS
spectra, and is included in the CIS stability calculations described earlier in Item 1,
and contained in the attachment for Item 1. These preliminary pathlengths were
calculated from raw field parameters and are subject to revision in the report,
9. (F14) Information about fractional analysis uncertainties for each FTIR analytical
region.
This comment will be addressed in the report.
10. (F25) A description about how analyte concentrations are quantitated from FTIR
absorption spectra.
These procedures are outlined in EPA Method 320 and the FTIR Protocol included in
the QAPP. Specific aspects of the analyses and deviations from the methods will be
included in the report.
11. (F26) Information about minimum detectable concentrations for the compounds
found during the emissions testing by the extractive FTIR method.
A summary of minimum detectable concentrations for non-detects will be included in
the report
12. (F29) A copy of the certificates of analysis for the CTS, the SF6, and the SF6/toluene
standards.
Copies of certificates of analysis for the CTS, SF6, and SF6/toluenc gases have been
attached.
-------
13. (F30) Information relating to the basis for selection ofthe CIS gas mixture and
concentration relative to the selection criteria given in Section 4.5 ofthe FTIR
Protocol.
Ethylene has been used as a CIS gas on numerous EPA test programs, and meets the
criteria given by the FTIR Protocol.
14. (F3 1) Information about the uncertainty of the analysis of the CIS, the SF6, and the
SF6/toluene standards.
Analytical accuracy for each of these gas standards is contained on their respective
certificates of analyses. All are listed as +/- 5%.
15. (F32) Information about the traceability ofthe analysis ofthe CIS, the SF6, and the
SF6/toluene standards to MIST.
Scott Specialty Gases uses gravimetric procedures to generate their gas standards.
They do not claim NIST traceability, but, rather, are certified by their own internal
calibrations and standard procedures.
16. (F33) Information about any independent concentration verifications of the CIS, the
SF6, and the SF6/toluene standards by MRI.
See Items 14 and 15, above
17. (F34) Information about the variability of successive CIS measurements.
Variability of successive CIS measurements will be included in the report, and can
be seen from the calculations presented earlier in Item 1. The CTS measurements
met the Protocol requirements of +/- 5% precision.
18. (F37) Information about any maintenance logs for the FTIR instrument
CTS stability is the primary indicator of instrument operations. When necessary,
FTIR maintenance is performed on an as needed basis in MRJ's laboratories and in
the field. For this particular test program, the instrument was serviced by an Analect
representative on July 20, was found to be in good working order, and did not require
any corrective actions.
-------
19. (G3) Information about any Entropy Environmentalists or MRI laboratory or field
validations of the sample concentration FTIR method for the compounds found
during the emissions testing.
This information was provided to RTI while in the field (Fourier Transform Infrared
Method Validation at a Coal-tired Boiler, Entropy Environmentalists, July 1993,
published by EPA in 1994).
20. (G12) Information about the calibration traceabiliry of the wet test meter used to
calibrate dry gas meters in the VOST sampling trains associated with the sample
concentration FTIR method.
MRI calibrates the dry gas meters versus a wet test meter located at our Kansas City
laboratories, The wet test meter is calibrated according to the displacement method
and is, therefore, considered a primary standard. Calibration records for the wet test
meter and the VOST consoles are kept on tile and are available upon request.
21. (G19) A copy of the certificate of analysis for the toluene-d8 surrogate spiking gas
and information about its analytical uncertainty, traceability, and any independent
concentration verifications.
A copy of the toluene-d8 certificate of analysis is attached. The gas is certified to +/-
5%.
22. (G3 1) Information about any Entropy Environmentalists or MRI laboratory and/or
field determinations of the collection and desorption efficiencies of the sample
concentration FTIR method for the compounds found during the emissions testing.
See Item 19. above.
23. (G32) Information about minimum detectable concentrations for the compounds
found during the emissions testing by the sample concentration FTIR method.
Minimum detectable concentrations for this method are, by nature, dependent upon
the compound and sampling parameters, and will be estimated in the report. For this
test, sampling parameters were chosen to obtain 100 ppb of toluene and xylene,
which were identified by PES in a preliminary screening.
-------
Attachment 1
Item 1 (A9)
-------
CIS Pathlength and % Difference Calculations
Filename ctspath Temp. (C) Pathlength (m) % Diff.
c0721b
c0721c
c0721d
c0721e
c0722a
c0722b
c0723a
c0723b
c0723c
c0724a
c0724b
c0725a
c0725b
c0725c
c0726a
c0726b
c0727a
c0727b
c0727c
c0727d
2.7207
2.6321
2.6718
2.6181
2.6234
2.6280
2.6131
2.6162
2.6420
2.6242
2.6536
2.6122
2.6247
2.6582
2.6390
2.6378
2.6220
2.6268
2.6283
2.6234
124
124
124
124
124
124
124
124
124
124
124
124
124
124
124
124
124
124
124
124
10.812
10.460
10.618
10.404
10.425
10.444
10.364
10.397
10.499
10.429
10.545
10.381
10.430
10.564
10.487
10.483
10.420
10.439
10.445
10.425
3.22
-0.14
1.37
-0.67
-0.47
-0.30
-0.86
-0.74
0.24
-0.44
0.68
-0.89
-0.42
0.85
0.12
0.08
-0.52
-0.34
-0.28
-0.47
Average =
10.475
Pathlength is based on use of a 99.9 ppm ethylene standard.
% Difference is based on the average calculated pathlength.
DRAFT
-------
THC
Run 1 • Dryer Stack • 7/21/98
Calibration Error Determination
DRAFT
Cal Gas
Value
0.0
90.3
50.2
25.0
Measured
Value
0.0
90.2
50.9
25.0
Difference
As % Error
0.0
0.1
1.4
0.0
Pass/ F
Pass
Pass
Pass
Pass
Instrument Span for THC is 100 ppm
Pass/Fail Criteria is +/- 5% of Cal Gas for THC
Zero Drift
Initial
Value
0.0
Drift Check
Value
1 st Drift Check
Value
0.3
Final
Value
Difference
As % Error
0.3
Difference
As % Error
Pass/Fail
Pass
Pass/Fail
0.3
0.3
0.0
Pass
Span Drift
Initial
Value
90.2
1 st Drift Check
Value
1 st Drift Check
Value
89.9
Final
Value
Difference
As % Error
0.7
Difference
As % Error
Pass/Fail
Pass
Pass/Fail
89.9
89.5
0.4
Pass
-------
Run 2 -Dryer Stack - 7122198
Calibration Error Determination
DRAFT
THC
Cal Gas
Value
0.0
90.3
50.2
25.0
Measured
Value
0.2
90.1
50.6
25.6
Difference
As % Error
0.2
0.2
0.8
2.4
Pass/ F
Pass
Pass
Pass
Pass
Instrument Span for THC is 100 ppm
Pass/Fail Criteria is +/- 5% of Cal Gas for THC
initial
Value
Zero Drift
1 st Drift Check
Value
Difference
As % Error
Pass/Fail
0.2
1 st Drift Check
Value
-0.1
Final
Value
0.3
Difference
As % Error
Pass
Pass/Fail
-0.1
0.3
0.4
Pass
Span Drift
initial
Value
90.2
1 st Drift Check
Value
Drift Check
Value
89.9
Final
Value
Difference
As % Error
0.7
Difference
As % Error
Pass/Fail
Pass
Pass/Fail
89.9
89.5
0.4
Pass
-------
Run 1 - Load Out. 7/23/98 (aborted)
Calibration Error Determination
DRAFT
THC Silo
Instrument Span
Cal Gas
Value
0.0
899.0
498.0
249.0
for THC Silo
Pass/Fail Criteria is +/- 5% of
THC Tunnel
Cal Gas
Value
0.0
90.4
50.2
25.0
Measured
Value
3.6
900.0
504.0
256.0
is 1000 ppm
Cal Gas for THC
Measured
Value
0.2
90.2
49.8
27.7
Difference
As % Error
0.4
0.0
1.2
2.8
Difference
As % Error
0.2
0.2
0.8
1.2
Pass/ Fail
Pass
Pass
Pass
Pass
Pass/ Fail
Pass
Pass
Pass
Pass
Instrument Span for THC Tunnel is 100 ppm
Pass/Fail Criteria is +/- 5% of Cal Gas for THC
Zero Drift
Initial
Value
THC Silo 0.0
Initial
Value
THC Tunnel 0.0
Initial
Value
THC Silo 900.0
Initial
Value
Final
Value
9.8
Final
Value
0.5
Final
Value
914.0
Final
Value
Difference
As % Error
1.0
Difference
As % Error
0.5
Span Drift
Difference
As % Error
1.4
Difference
As % Error
Pas&Fail
Pass
Pass/Fail
Pass
Pass/Fail
Pass
Pass/Fail
THC Tunnel 90.2
89.7
0.5
Pass
Pass/Fail Criteria for Drift is +/-3% of THC Span
-------
Run1 .Load Out -7124198
Calibration Error Determination
THC
instrument
Pass/Fail
THC
Cal Gas
Value
0.0
899.0
498.0
249.0
Span for THC Silo is 1000 ppm
Criteria is +/- 5% of Cal Gas for
Initial
Value
1.2
Initial
Value
Measured
Value
1.2
905.0
508.0
246.0
THC
Final
Value
-0.2
Final
Value
Difference
As % Error
0.1
0.7
2.0
1.2
Zero Drift
Difference
As % Error
0.1
Span Drift
Difference
As '/o Error
Pass/ Fai
Pass
Pass
Pass
Pass
Pass/Fail
Pass
Pass/Fail
THC Silo 905.0
907.0
0.0
Pass
Pass/Fail Criteria for Drift is W-3% of THC Soan
-------
Run 2 . Load Out - 7/25/98
Calibration Error Determination
AFT
Cal Gas
Value
THC 0.0
899.0
498.0
249.0
Instrument Span for THC is 1000
Pass/Fail Criteria is +l- 5% of Cal
Initial
Value
I-HC 1.7
Initial
Value
Measured
Value
1.7
902.0
506.0
254.0
ppm
Gas for THC
Final
Value
2.0
Final
Value
Difference
As % Error
0.2
0.3
1.6
2.0
Zero Drift
Difference
As % Error
0.0
Span Drift
Difference
As % Error
Pass/ Fai
Pass
Pass
Pass
Pass
Pass/Fail
Pass
Pass/Fail
THC Silo
902.0
900.0
0.0
Pass
Pass/Fail Criteria for Drift is +/-3% of THC Span
-------
Intermittent Load Dump - 7/25/98
Calibration Error Determination
DRAFT
Cal Gas Measured
THC
Instrument
Value
0.0
90.4
50.2
25.0
Span for THC is 100 ppm
Value
0.2
90.7
50.9
25.7
Difference
As % Error
0.2
0.3
1.4
2.8
Pass/ Fai
Pass
Pass
Pass
Pass
Pass/Fail Criteria is +/- 5% of Cal Gas for THC
THC
Initial
Value
0.2
Initial
Value
Final
Value
0.4
Final
Value
Zero Drift
Difference
As % Error
0.2
Span Drift
Difference
As % Error
Pass/Fail
Pass
Pass/Fail
THC Silo
90.7
90.4
0.3
Pass
Pass/Fail Criteria for Drift is -i-/-3% of THC Span
-------
THC
Run 4-Baseline. 7126198 Dl?/\FT
Calibration Error Determination
Instrument Span for THC is 100 ppm
Pass/Fail Criteria is +/- 5% of Cal Gas for THC
Zero Drift
Cal Gas
Value
0.0
90.3
50.2
25.0
Measured
Value
0.2
90.5
51.1
25.5
Difference
As % Error
0.2
0.2
1.8
2.0
Pass/ F
Pass
Pass
Pass
Pass
Initial
Value
0.2
1st Drift Check
Value
0.1
Drift Check
Value
0.1
Final
Value
Difference
As % Error
0.1
Difference
As % Error
Pass/Fail
Pass
Pass/Fail
0.1
0.0
Pass
Span Drift
Initial
Value
90.5
1st Drift Check
Value
1st Drift Check
Value
90.4
Final
Value
Difference
As % Error
0.3
Difference
As % Error
Pass/Fail
Pass
Pass/Fail
90.4
90.8
0.4
Pass
-------
Run 3 . Load Out . 7/23/98
Calibration Error Determination
Instrument Span for THC Tunnel is 100 ppm
Pass/Fail Criteria is *•/- 5% of Cal Gas for THC
THC Silo
Instrument Span
Pass/Fail Criteria
THC Tunnel
Cal Gas
Value
0.0
899.0
498.0
249.0
for THC Silo
is +/- 5% of
Cal Gas
Value
0.0
90.4
50.2
25.0
Measured
Value
1.1
907.0
504.0
260.0
is 1000 ppm
Cal Gas for THC
Measured
Value
0.2
90.4
50.9
25.5
Difference
As % Error
0.1
0.9
1.2
4.0
Difference
As % Error
0.2
0.0
1.3
2.0
Pass/ Fail
Pass
Pass
Pass
Pass
Pass/ Fail
Pass
Pass
Pass
Pass
Zero Drift
THC Silo
THC Tunnel
THC Silo
Initial
Value
1.1
Initial
Value
0.2
Initial
Value
907.0
Initial
Value
Final
Value
-0.1
Final
Value
0.1
Final
Value
903.0
Final
Value
Difference
As % Error
0.1
Difference
As % Error
0.1
Span Drift
Difference
As % Error
0.0
Difference
As % Error
Pass/Fail
Pass
Pass/Fail
Pass
Pass/Fail
Pass
Pass/Fail
THC Tunnel 90.4
Pass/Fail Criteria for Drift is +/-3% of
90.6
0.2
Pass
-------
Response Times
Analyzer Response Time
THC Silo 1 min. 25 sec.
THC Tunnel 35 sec.
THC Dryer Stack 1 min. 30 sec.
-------
Attachment 2
Item 2 (A10)
-------
Load-Out Log Spreadsheet
Sheet
of
«n Protect No
Clwn/Sourc*
Product
10
4701-08-03-04
Product Description
Job
Name
Time
Of
Loading
Actual
Tons
Loaded
Drt
Truck
No
•
Run No.
DUr
RMOKM By-
Silo
No.
Mix
Temp.
in Truck
Comments
mn niestttirtormVProdoctionData
Midwest Research Institute
07/13/98
-------
SF6 Gas Delivery data Spreadsheet
Sheet
of
Mn P«j|«« No
Client/Source.
Sampling Locxbon
Dry GasMetar No-
Time
470? -08-03-0'
PTE Loadout
SfloNo.
1
DGM Reading
Ptes. PSI
Run No
Date:
Operator.
GuCyfintoNa
Comments
-
-------
Attachment 3
Item 4 (C3)
-------
Thomas J. Geyer
Principal Chemist
Dr. Geyer specializes in molecular spectroscopy, FTDR. test method development and
validation, EPA protocol development, FTIR data analysis, analytical software
development, and project management. Dr. Geyer has developed EPA FTIR applications
for emissions testing in the field and managed the first field evaluation of an FTIR
continuous emission monitoring system for measuring HAPs. He has led many field test
programs and developed analyte spiking procedures for hazardous air pollutants (HAPs).
Dr. Geyer helped develop the EPA FTIR analytical protocol to measure reference spectra
and to apply spectra for field measurements.
Recently, Dr. Geyer developed FTIR test Methods 3 18 for wool fiberglass, 320 for
hazardous air pollutants and Performance Specification 15 for FTIR continuous emissions
monitoring applications. He also does analytical programming for instrumental methods.
Based at MRI's North Carolina Office, Dr. Geyer develops hardware, software, and
measurement techniques using FTIR Spectrometry for the analysis of pollutant emissions.
His project assignments have included a number of FTIR method development and test
programs.
Before joining MRI in 1995, Dr. Geyer was a Senior Chemist and Group Leader in the
Research Division of Entropy, Inc. He directed an EPA FTIR emission test project at five
electric utilities, conducted field studies with FTIR emissions tests, and managed in-house
laboratory projects. He helped develop procedures to analyze FTIR validation data and
helped develop FTIR validation sampling procedures. He directed laboratory and field
evaluations to expand the capabilities of FTIR emissions testing.
From 1989 to 1991, Dr. Geyer was Assistant Professor of Chemistry at the U.S. Naval
Academy. Previously, he spent a year as an Office of Naval Technology Postdoctoral
Felllow at China Lake, California, He performed studies to characterize material ejected by
laser ablation from the surface of YBa2Cu3O7 high-temperature superconductor. As a
Research Assistant at the University of South Carolina from 1984 to 1988, he conducted
original research in molecular spectroscopy to determine structures and conformational
equilibria of substituted cyclobutane and cyclopentane molecules.
Dr. Geyer has a Ph.D. in Physical Chemistry from the University of South Carolina
(1988). He is a member of the American Chemical Society, American Physical Society, Air
and Waste Management Association, and Sigma Xi (Scientific Research Society of North
America). Entropy honored him with an Outstanding Contribution Award in 1992. He is
the coauthor of more than 20 technical publications and presentations.
-------
Scott W. Klamm
Senior Environmental Engineer
Mr. Klamm specializes in air toxics, combustion processes, emission control
technologies, and related environmental engineering programs. He has worked extensively
on the development and operation of laboratory and field equipment for point source and
ambient testing. His recent activities at MR! include leading an EPA field method
comparison project on acetaldehyde, performing data analysis for a comparison of three
methods for HF, and leading the data analysis and reporting activities for an EPA
incineration project to identify and measure products of incomplete combustion using a
wide range of field and analytical methods. Mr. Klamm has also recently led field studies
for two industrial clients to demonstrate collection efficiency on a control device in one, and
to determine measurement errors of an on-line mass spectrometer for emission monitoring
in the other.
Mr. Klamm developed an experimental extended-period ambient organic sampler and
carried out laboratory testing of the system. For the electronics industry, he examined the
use of CFC solvents and alternative technologies for emission control. Mr. Klamm
prepared the test plan and matrix design as well as special sampling equipment for a field
study of organic compound adsorption in boiler soot for EPA. On several occasions, he has
served as an EPA field auditor for the disposal of chemical agents and munitions at an Army
facility. He ran tests on stack sampling equipment and emissions monitors and made
recommendations on the equipment and monitors. Mr. Klamm has also been field auditor
and reviewer of trial bum data as part of permit review assistance to the states of Utah and
Kansas, EPA Headquarters, and EPA Region VII.
As part of an evaluation of the Alaska CO inventory, Mr. Klamm tested various
locations in an urban area for mobile-source CO emissions, applied meteorological
information, assisted in modeling, determined accuracy of existing monitors compared to
MRI-gathered data, and helped prepare recommendations to the State of Alaska. For the
U.S. Air Force, Mr. Klamm designed a test matrix to study airborne pollutants and toxic
gases formed during extinguishment of jet fuel fires with Halon agents at firefighter training
exercises. He assisted in operation of SUMMA, ambient VOST, open-path FTIR, PUF,
particulate, and CO monitors. He also performed data reduction, coauthored reports and
papers, and assisted in risk assessment and dispersion modeling,
Regulatory work has involved coauthoring EPA guidance documents on setting permit
conditions, reporting trial bum results, and related incineration topics, such as combustion
gas velocity, treatment of gasoline-contaminated soils, and solid waste feed systems.
Mr. Klamm graduated magna cum laude from the University of Missouri-Rolla with a
B.S. in Chemical Engineering in 1985. He has taken additional courses in solid and
hazardous waste management, human environmental biology, and dispersion modeling. He
is a member of the Air and Waste Management Association. He received the 1990 Bidstrup
Award from MRI for outstanding technical contribution and the [997 Achievement Award
from MRTs Council of Principal Scientists.
116121 I/'W
-------
Robert G. Gulick
Supervisor of Field Programs
Mr. Gulick specializes in the operation and maintenance of continuous emission
monitors in compliance with appropriate EPA methods. As Supervisor of Field
Programs, Mr. Gulick is responsible for assuring that all equipment for source sampling
is available, calibrated, and in working condition. In addition, he has responsibility for
operating and maintaining continuous emission monitors during field sampling at
industrial facilities. Recent programs include:
. Performed continuous emission monitoring of carbon monoxide, carbon dioxide,
sulfur dioxide, nitrogen oxides, total hydrocarbons, and hydrogen chloride on
source sampling projects. These have included a hysteresis boiler study in
Pennsylvania and a kiln study in Nebraska.
. Evaluated 24-hour sampling for total hydrocarbons to determine capture
efficiency in the development of total temporary enclosure model.
. Project Leader on a study that assessed and recommended a full complement of
continuous emission monitors for a hazardous waste facility's continuous
emission monitor replacements.
In 1988 and 1989, Mr. Gulick was a Technical Sales Engineer with Torotel
Products of Grandview, Missouri. He negotiated price and delivery of electronic
components, expedited production to meet delivery schedules, and monitored
engineering changes to meet customer specifications. During 1986 and 1987,
Mr. Gulick was the owner and manager of a home electronics retail sales and service
business. He was responsible for retail sales, inventory purchase and control, service
and repair of audiovisual and computer products, advertising, and personnel
management
Mr. Gulick's background includes rive years as a Field Service Engineer with
Perkin-Elraer. He installed and repaired analog and digital test instrumentation,
computers, and peripherals. He handled inventory control, trained junior engineers, and
sold service contracts.
In 1981, Mr. Gulick received an AA.S. in Electronic Engineering Technology from
Western Iowa Technical College. In 1990, he completed special training in hazardous
waste operations. He has certification of OSHA safety and health training.
A-16
-------
Andrew E. Page
Assistant Environmental Scientist
Mr. Page performs work in the Air Quality Engineering Section of the Applied
Engineering Department. His experience includes field and laboratory testing for fugitive
dust sources as well as ducted emission sources using various types of sampling equipment
He performs laboratory analysis on emission sources; Method 18 analysis on ducted
emission sources by gas chromatography, including data reduction for these analyses; and
assists in operation and maintenance of mobile laboratory and field sampling equipment and
analytical instrumentation (IR and GC with FID, PID, and BCD).
From 1994 to March of 1997, Mr. Page worked for Ken Wilcox Associates where he
tested leak detection systems and prepared certification reports according to EPA
protocols. While at KWA he gamed extensive experience in working with and testing leak
detection equipment for aboveground and underground storage tanks and pipeline systems.
His other responsibilities included assistance in development of a fuels management research
center; product development testing for clients; data reduction and analysis for various
types of testing; preparation of estimates for analysis on environmental cleanup projects;
soil and water analysis using gas chromatography (GC) and infrared spectroinetry (IR); and
maintenance of GC and IR, calibration, troubleshooting, and repair.
As a research and teaching assistant at the University of Missouri, from 1992 to 1994,
he worked on various research projects, namely development of reverse-bum gasification as
a thermal treatment process for petroleum sludge, sewage sludge, and other wastes.
Presented research at various conferences. As a teaching assistant, he taught help sessions
and laboratory sessions for general chemistry courses.
Mr. Page received a B.A. in Chemistry from Central Methodist College in 1993
I2SQJOT1
-------
Pamela S. Murowchick
Associate Environmental Engineer
Ms. Murowchick provides engineering support on environmental contracts ranging
from incinerator trial bums to protocol development to test monitoring systems. The
diversity of her assignments has required versatility in applying her engineering knowledge
and the ability to work effectively with project management, project team members, and
client personnel. Her experience at MN has included:
• Prepared trial bum plans and associated QA plans.
• Operated the sampling console for Modified Method 5 testing during RCRA and
TSCA trial bums of hazardous waste incinerators.
1 Performed laboratory preparation and recovery tasks for incinerator sampling and
analysis projects.
• Performed test data reduction and reporting.
• Assisted on EPA regulatory support assignments involving waste management.
• Coauthored a conference presentation on incineration options for waste
management.
• Coauthored a conference presentation on emissions of organic compounds and
combustion gases from an industrial boiler during hazardous waste cofiring.
• Assisted with EPA protocol development work for underground storage tanks at
MRTs Experimental Tank Facility.
• Assisted with evaluations of commercial equipment for tank tightness testing.
• Assisted on a study of solar energy for waste disposal.
From 1988 to 1989, Ms. Murowchick was a Plant Chemist with Lubripac in Kansas
City, Kansas. She performed routine physical and chemical testing of oil in the Quality
Control Laboratory. Ms. Murowchick monitored the progress of special projects involving
cleanup in the tank farm, and she tested and adjusted new oil formulations in the laboratory
before full-scale production was begun.
Ms. Murowchick received a B.S. (with honors and distinction) in Chemical Engineering
from Pennsylvania State University in 1985. hi 1987 and 1988 she did course work in
Secondary Education and Chemistry at Mercyhurst College. She is certified in CPR and
completed OSHA's RCRA safety training. Her computer skills include Fortran
programming and WordPerfect, Quattro, and Lotus applications.
-------
James S. Surman, Jr.
Senior Environmental Scientist
Mr. Surman has over 28 years of direct experience in stationary source air emissions
testing, continuous emission monitoring, and related QA/QC procedures. His work at MRI
focuses on the evaluation of hazardous waste incinerators, municipal waste combustors,
boilers and industrial furnaces, and other sources of air pollution. He has been Field
Sampling Task Leader on 63 projects and Project Leader on 8 emission studies of
incinerators, boilers, and kilns, Mr. Surman has also participated as an operator and
sampler on numerous field programs and has audited RCRA trial bums of hazardous waste
incinerators and emissions tests at power plants for regulatory agencies. In addition to field
assignments, he participates in EPA-sponsored work assignments relevant to quality
assurance and emissions standards development.
Field assignments have involved sampling for volatile and semivolatile organic
compounds; particulate matter, including PM,, by the EGR method; particle size distri-
bution; multiple metals, including hexavalent chromium, acid gases, and other emissions.
Mr. Surman has prepared and assisted engineers in preparing proposals, test plans, work
plans, QA plans, and project final reports. He also has been responsible for the hands-on
preparation and execution of field sampling projects involving as many as 15 field personnel
for periods up to one month at a test site.
From 1978 to 1987, Mr. Surman was Quality Assurance Manager and Project
Supervisor with Mostardi-Platt Associates of Bensenville, Illinois. He evaluated all testing
procedures, equipment maintenance and calibrations, and techniques in the performance of
new or innovative test methods. He helped implement EPA reference methods as they
became available and supervised air pollution source testing and air pollution control
evaluation for various industries. He also conducted ambient air monitoring studies and
audits and developed a QA plan for testing activities.
Earlier experience with air pollution source testing was with Kin Associates at Chicago
Heights, Illinois (1977) and Commercial Testing and Engineering Company in South
Holland, Illinois (1973-1977). Mr. Surman initially worked in Commercial Testing and
Engineering Company's services for the sampling and analysis of coal, iron ore, water, soils,
and other materials for chemical and physical characteristics (1970-1973). With Rand
Development Corporation in Cleveland, Ohio (1966- 1970), he aided in field investigations
related to water pollution control, groundwater contamination, and strip mine reclamation.
Mr. Surman received the B.S. in Biology with a minor in Chemistry from Cleveland
State University (1966). He is a member of the Source Evaluation Society and coauthor of
a municipal waste combustion multipollutant study (EPA-600/8-89-064)
"7 I
-------
Bob J. Edwards
Senior Technician
Mr. Edwards joined MRI's Field Measurements Section in 1992. He has participated in
a number of industrial projects around the country for hazardous waste incinerator testing
and analysis services. He also has worked on assignments under MRI's subcontract for
technical assistance to EPA for the implementation of RCRA regulations for hazardous
waste management facilities.
In support of various field sampling and analysis programs, Mr. Edwards calibrates
equipment, performs routine and corrective maintenance on equipment, operates an EPA
Method S console during stack sampling, performs Orsat analysis on gas streams, and
titrates EPA Method 6 samples. He stages and destages equipment for field sampling and
sets up the equipment on-site. In addition, he performs data entry for reports, investigates
equipment and vendors to assist with equipment purchasing decisions, and orders materials.
His background includes six years in the U.S. Navy, followed by three years in
manufacturing and industrial facilities. He has worked extensively in environmental
maintenance, pneumatics, hydraulics, and electrical and mechanical equipment and systems.
Mr. Edwards also has experience with quality assurance, radiological controls, gauge
calibration, hazardous materials, and security and safety issues.
In the Navy, Mr. Edwards was a missile technician. He operated and maintained the
Poseidon Ballistic Missile System as launcher operations supervisor. He performed
colateral duties, such as nuclear weapons handling supervisor, departmental coordinator for
maintenance and material management, nuclear weapons radiological controls assistant,
missile and readiness equipment expert, departmental publications coordinator, quality
assurance inspector, field metrology technician, and nuclear weapons security guard. He
completed several training programs in the Navy that covered electricity, electronics,
hydraulics, pneumatics, digital computers, radiological controls, QA, gauge calibration,
theory and practice of equipment maintenance, and related specific disciplines. He has also
taken courses in electronic engineering at Maple Woods Community College in Kansas
City.
With a division of Kraft-General Foods, Mr. Edwards worked as plant maintenance
supervisor/trainee. He oversaw maintenance aspects of production and packaging,
interacted with contractors and the company upgrade team in monitoring progress during
equipment improvement and expansion, and served on the plant's hazardous materials
response team after required OSHA training.
-------
Daniel 0. Neal
Senior Technician
Mr. Neal provides technical support on programs for environmental monitoring,
sampling, and analysis in the Field Measurements Section of MRTs Environmental
Technology and Engineering Department. His responsibilities include staging and destaging
equipment for field tests, setup and operation of equipment, and calibration and
maintenance of test equipment.
Since joining MRI in 1993, Mr. Neal has accompanied field measurement teams on
several projects for clients in government and industry. In addition to equipment setup, he
performs various tasks, including running the Method 5 console and operating the stack
probe. Project work has included an emissions test of a kiln at a brick manufacturing plant
for EPA, compliance, and performance tests of cooling towers, and various trial bum,
miniburn, and performance tests for industrial clients.
Prior to joining MRI, Mr. Neal worked as a sales representative for a publishing
company and an appliance company. From 1976 to 1984, he worked for the Power
Division of Burns and McDonnell Engineers in Kansas City, Missouri. As a Design Detailer
and Electrical Substation Drafting Supervisor, Mr. Neal assisted with design and layout of
power substations, Mr. Neal has completed undergraduate courses at Kansas State
University, Johnson County Community College, and Longview College.
-------
Attachment 4
Items 12,21, and 24 (F29, G19, and HIS)
-------
Scott Specialty Gases
[prom:
6141 EASTON ROAD
PLUMSTEADVILLE
Phone: 215-766-8861
CERTIFICATE
PO BOX 310
?A 18949-0310
O F
-Fax: 215-766-2070
ANALYSIS
MIDWEST RESEARCH
SCOTT KLAMM
425 VOLKER BLVD
KANSAS CITY
PROJECT #: 01-01788-004
P0#: 033452
ITEM #: 01023822 5AL
DATE: 4/07/98
MO 64110
CYLINDER #: ALM033887
FILL PRESSURE: 2000 PSIG
ANALYTICAL ACCURACY: +/-5%
BLEND TYPE
COMPONENT
CERTIFIED WORKING STD
REQUESTED GAS
CONG MOLES
ANALYSIS
(MOLES)
SULFUR HEXAFLUORIDE
NITROGEN
.2
PPM
BALANCE
0.205
PPM
BALANCE
ANALYST:
O.
--C2> 10 ^^
ROJAS
-------
Scott Specialty Gases
Shipped
From:
6141 EASTON ROAD
PLUMSTEADVILLE
Phone: 215-766-8861
CERTIFICATE
PO BOX 310
PA 18949-0310
O F
Fax: 215-766-2070
ANALYSIS
MIDWEST RESEARCH
SCOTT KLAMM
425 VOLKER BLVD
KANSAS CITY
PROJECT &: D1-Q1788-001
P0#: 033452
ITEM #: 0102S3000815AL
DATE: 4/07/98
MO 64110
CYLINDER #: AAL17264
FILL PRESSURE: 1280 PSIG
ANALYTICAL ACCURACY: +/-5%
BLEND TYPE
COMPONENT
CERTIFIED WORKING STD
REQUESTED GAS
CONG MOLES
SULFUR HEXAFLUORIDE
TOLUENE
NITROGEN
4.
100.
PPM
PPM
BALANCE
ANALYSIS
(MOLES)
3.83
105.
PPM
PPM
BALANCE
ANALYST:
l.LiUDWIG U
-------
Scott Specialty Gases
CERTIFICATE OF ANALYSIS
- OS Rw Qwponetit Ho Couponed
Project No 8HI7SB
lihmierfb
! fliultjucal HCCUMOJ »/•:.
Grade CERTIFIED UKKINE SIO
!215)^S-886I RJJfiTOO/ttJl P9 18SC
--^v^ ••^S^¥~r.:?r J-»'--"-••-!:/?•-j -^g-^.^H-^y-ty?!-^ ?^a
ScottrSpedatty dases
CSTnFJCATE OF ANALYSIS
05 Rs$ Cospatent Ha
2551-S-*
7T27-27-3
l Mo 8H1788
C'jhnder Ho. fU813878
!,:B No 2S8239ES2 5R.
xeonier/Servicc icnuet
-------
Scott Spedaity Gases
CERTIFICATE OF ANALYSIS
FONo K3452
CflS Reg Component No
TOLUDCOB
NITHKH
2837-26-5
7727-37-S
Project to 8HI788
Cvhnder HP. RJ8318B9
tot No 8IB2T2B!<725fl
fcojrtti) +>-St
Grate CESnnOl UK I* STQ
121537SS-88S1 PLlTSTEHWlLil « I0Q
Reorder/Service wmact
-------
08/10/98
15:29 ©215 766 2070
Scott Specialty Gases
Shipped
From:
6141 EASTON ROAD
PLUMSTEADVILLE
Phone: 215-766-8861
PO BOX 310
PA 18949-0310
CBRTIFIC AT EOF
Fw: 215-766-2070
ANALYSIS
MIDWEST RESEARCH
SCOTT KLAMM
425 VOLKER BLVD
KANSAS CITY
PROJECT #: 01-017ii8-005
P0#: 033452
ITEM #: 01021951 SAL
DATE: 3/31/98
MO 64110
CYLINDER #: AU4005893
FILL PRESSURE: 2000 PSIG
ANALYTICAL ACCURACY: +/-S%
BLEND TYPE
COMPONENT
ETHYLENE
NITROGEN
CERTIFIED WORKING STD
REQUESTED GAS
CONC MOLES
100.
PPM
BALANCE
ANALYSIS
(MOLES)
99.9
PPM
BAI/.NCE
ANALYST:
GENYA KOG'
f
-------
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1C, TO EPA 'TRACEABILITY PROTOCOL FOR ASSAY AND CERTIFICATION OF GASEOUS CALIBRATION STANDARDS (PROCEDURE #G 1 }
Order No:312-020638-01
Batch No: HG1-33SB2
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-------
Attachment 5
Item 25 (HIS)
-------
Eri vironic s
Daniel A. Kaplinski
Sales Engineer
vironics Inc. ^_aLi
-------
ENVIRONICS FLOW CONTROLLER CALIBRATION SHEET
Mf #: 2. Description: AIR
Size:
3CCM, K—factor:
SERIAL #
This flaw controller was calibrated using
Primary Flow Standard Calibration System.
dry air at a temperature o-f ,22.F ( _ C) and
a Sierra Gal Bench (TM), a traceable
This calibration i s "re-f erenced Vto
a pressure of 29.92 in.Hg <760Tohr}
5
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20
30
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Calibration dats was last saved on
Thursday 23 April
'•-'erified by:
-------
ENVIRONICS FLOW COh4TROLLER CALIBRATION SHEET
Mf #: 3, Description: AIR , 3izs; 10£"? -0 SCCH, K—factor: 1.
SERIAL #_
This -flON controller was calibrated using a Sisrrs Cal Bench (TM) , a traceable
Primary Flow Standard Cal i brat i on System. This calibration is referenced to
dry air at a temperature o-f 3^F C C) and a pressure of 29.92 in.Hg (760Tor.r>
True FlDW
44.233 CCM
94.S68 CCM
196.33 CCM
293.36 CCM
3^9.54 CCM
4VR.17 CCM
593.72 CCM
6-~-3,oB CCH
799.52 CCM
^01.61 CCM
1003.6 CCM
5 /
10 /
20 /
30 >
40 •
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60 "/
70 •
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100.0
200.0
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7 '30. '-i
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ccn
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ccr,
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Calibration data v-j
-------
ENVIRQNICS FLOW CONTROLLER CALIBRATION SHEET
Mf #: 4, Description: AIR , Size: 1&&.& 3CCM, K— Factor: l.S
SERIAL * /»!/ IG&Ctt?
This flow controller was calibrated using a Sierra Cal Bench (TM) , a traceable
Primary Flow Standard Calibration System. This calibration is re-f erenced t o
dry air at a temperature of Qf ( _ C) and a pressure of 29. ?2 in,H<3 (760Tonr>
Set Flow . True Flow
' 5,013' CCJ1
l V. 50.0 CCM 5(-'.2S4 CCM
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70 /I 7»i.0 CCM 79.371 CCM
30 y. 3«3.<3 CCM 3ML44 CCM
"0 "1 '-'ii1 . <<' CCM "'I: . 504 CCM
I'El'iiV. 1-ZI0...D CCM 1 ••?!•:-. 57 CCM
Calibration data was 1 ast =«vecl on Thursday 23 April "S at 1-.- 2S:i''
Ver \ -f i ed b •/: ^>A-^-»^^ (^O] Date: ' - 2*3 -
-------
Chapter 3
Technical Systems Audit
Manual Emissions Test Methods Performed by
Pacific Environmental Services Inc.
at Hot Mix Asphalt Plant C,
Los Angeles, CA
-------
3.0 TECHNICAL SYSTEMS AUDIT - PACIFIC ENVIRONMENTAL SERVICES INC.
This Chapter is the final technical systems audit (TSA) of the manual emissions testing at Hot
Mix Asphalt Plant C in the Los Angeles, California area performed by Pacific Environmental Services,
Inc. (PES). As explained in detail in Chapter 1, the final TSA includes revisions by the EPA Quality
Assurance Officer. The draft TSA report from Research Triangle Institute (RTI) was delivered to the
EPA Quality Assurance Officer on September 29, 1998. The TSA was performed by R.K.M. Jayanty
and Robert S. Wright of Research Triangle Institute (RTI) under EPA Contract 68-D4-0091, work
assignment 99-03, from July 20, through July 26, 1998. The TSA was conducted in accordance with
principles described in the EPA Quality Assurance Division's working draft version of EPA Guidance
for Technical Assessments for Environmental Data Operations (EPA QA/G-7).
In general, PES and its team members have performed the testing according to the procedures
outlined in the Site Specific Test Plan (SSTP) and Quality Assurance Project Plan (QAPP). Any
deviations from the QAPP or SSTP have been discussed with the EPA Work Assignment Manager. PES
and its team members who are present at the site are well qualified and experienced in the work to which
they are assigned.
Item
1
2
3
Findings that may have a potential effect on data quality
The EPA Methods, VOST and Modified Method 5 (MM5), have not been validated
for all the chemical compounds of interest in the asphalt plant emissions. Some of
the compounds may have been recovered during the laboratory testing in other
programs, but none have been validated in the asphalt plant emissions matrices.
This was a research study, however, and not meant to have validation.
The VOST cartridges were spiked with surrogate compound(s) before field
sampling at Triangle Labs.
The precision and accuracy goals indicated in the QAPP are based on estimates
from the VOST and semi- VOST methods, but they are not established values for
many of the compounds of interest in this program.
Item
1
2
3
Findings that are unlikely to have an effect on data quality
The spikes into the XAD-2 resin (MM5) and Anasorb 747 (M-18) were loaded
directly onto the cartridges in the field.
The train operators have noted the readings on the data sheets. The data sheets do
not have any column to note any comments during sampling. Similarly, a notebook
was maintained at the site to record any problems or process changes, etc., during
sampling.
The flow rates used for VOST at the tunnel exhaust were too low to maintain
constant on the rotameter or VOST console, which may cause some error in the total
volume collected.
Technical Systms Audit of Test Methods Performed by PES
3.1
-------
Technical Systems Audit Checklist
Project: Emissions Testing at a Hot Mix Asphalt Plant
Organization: Pacific Environmental Services
Location: Asphalt Plant C - Los Angeles, CA
Assessors: R.K.M. Jayanty and R.S. Wright (Research Triangle Institute; Research Triangle Park,
North Carolina)
Audit Dates: July 20 through July 26, 1998
Brief Project Description: EPA is investigating hot mix asphalt plants to identify and quantify
particulate matter and hazardous air pollutants (HAPs) emitted from asphalt cement load-out operations.
EPA has issued a work assignment to PES to conduct an air emissions test program to collect data in
support of the investigation. Asphalt Plant C in Los Angeles, California was chosen primarily because
load-out emissions are controlled by a silo exhaust system and a load-out tunnel. The plant has a
production capacity of more 650 tons per day. Approximately 2,000 tons per 4 hour period were
produced, during the test. The primary objective of the project will be to characterize air emissions of
organic HAPs from asphalt cement load-out operations and operation of the hot mix dryer; however, PES
is not responsible for the testing of the hot mix dryer stack. Testing will be performed to characterize
emissions from the storage silos, the load-out tunnel, and the hot mix dryer.
AUDIT QUESTIONS
RESPONSE
Y
N
N
A
COMMENT
A. GENERAL QUALITY ASSURANCE INFORMATION
1 . Is there an approved quality
assurance (QA) plan for the overall
project and has it been reviewed by
all appropriate personnel?
2. Is a copy of the approved QA plan
maintained at the field site? If not,
briefly describe how and where
QA and quality control (QC)
requirements and procedures are
documented at the field site.
/
/
A QAPP was submitted to EPA in
January 1998. Subsequently, two
revisions have been made and a final
QAPP was submitted on July 14, 1998.
Additionally, PES submitted a SSTP in
June 1998. Both documents have been
approved by EPA.
Copies of the QAPP and SSTP are
available in the trailer. Few operators of
the trains have used these documents;
however, key personnel provided them
with information from these documents
as needed for their tasks.
Technical Systms Audit of Test Methods Performed by PES
3.2
-------
AUDIT QUESTIONS
3. Is the design and conduct of the
project as specified in the QA
plan? Are there deviations from
the QA plan? How are any
deviations from the QA plan
noted?
4. Are written and approved standard
operating procedures (SOPs) used
in the project? If so, list them and
note whether they are available at
the field site. If not, briefly
describe how and where the project
procedures are documented.
5. For each measured parameter, do
any SOPs clearly define the data
quality indicator goals for
precision and accuracy?
6. Do the above data quality indicator
goals appear to be based on
documented performance criteria
for the measured parameter or on
actual QC data compiled for the
particular measured parameter?
7. Are there established procedures
for corrective or response actions
when measurement performance
criteria or the data quality indicator
goals (e.g. out-of-control
calibration data) are not met? If
yes, briefly describe them. Are
they consistent with the QA plan?
RESPONSE
Y
/
/
N
/
N
A
/
/
COMMENT
In general, the project is being
implemented as was specified in the
QAPP. However, some procedures have
changed since the revised QAPP was
submitted to EPA. This was
communicated to EPA WAM in a letter
form on July 8, 1998. The proposed
deviations do not appear to affect the
quality of the data being generated.
No SOPs were observed at the testing
site. EPA test methods are used as they
are and those methods are attached to
the QAPP.
Data quality indicator goals defined in
the EPA methods were used.
Data quality indicator goals appear to be
based on EPA methods.
Whenever there are deviations from the
QAPP or established procedures in EPA
methods, the EPA Work Assignment
Manager was informed by the PES Task
Manager.
Technical Systms Audit of Test Methods Performed by PES
3.3
-------
AUDIT QUESTIONS
8. For each measured parameter, do
the SOPs specify the frequency of
calibration, acceptance criteria for
the calibration, and the process for
calibration data reduction and
review?
9. Briefly describe how calibration
and other QC data are documented.
] 0. Does the calibration
documentation show that
calibrations are being performed at
the required frequency and in the
required manner?
1 1 . Are there standard paper or
electronic forms to record QC data
and operational data? Are the
records dated? Is the person who
completed the record identified?
Are paper records written in
indelible ink?
12. Are the QC data reviewed by
another qualified person such as
the QA officer or the plant
manager? Who is this individual?
13. Is the project team adhering to the
planned schedule? If not, explain
the new schedule. Verify that all
schedule changes have been
authorized.
14. Are there written plans to report
changes in the QAPP during data-
gathering activities?
RESPONSE
Y
/
/
/
N
/
N
A
/
/
COMMENT
PES used the specifications established
in the EPA methods. All calibration data
sheets will be given to RTI at a later
date. Mr. Dennis Holzschuh, ST., will be
responsible for QA coordination and
review of the calibration data.
Operational parameters and calibration
data were recorded on paper data sheets.
Standard paper data sheets were used
for all measurements and blank data
sheets were supplied to RTI. The data
sheets are dated and the operator name
was noted. All data forms were filled
out in ink.
Mr. Dennis P. Holzschuh, Sr., PES QA
Coordinator, will review all QA data
sheets. He performed internal QA at the
field site.
The schedule is being followed to the
extent allowed by unexpected
equipment breakdown and process
changes in the asphalt plant. All
schedule modifications were authorized
by the EPA Work Assignment Manager.
There are no written plans to report
changes in the QAPP during sampling.
However, the PES Task Manager
informed EPA WAM and other staff
verbally concerning schedule modifi-
cations and any deviations from the
QAPP.
Technical Systms Audit of Test Methods Performed by PES
3.4
-------
AUDIT QUESTIONS
RESPONSE
Y
N
N
A
COMMENT
Additional Questions or Comments:
B. ORGANIZATION AND RESPONSIBILITIES
1 . Identify the following personnel
and determine whether they have
the listed responsibilities:
PES Principal Investigator:
C. Wavne Westbrook
• responsible for overall
performance of the project, and
• communications with EPA
2. PES QA Officer:
Dennis Falgout
• assist with and will be
responsible for review and
monitoring of all QA/QC
activities
3. PES Project On-Site Manager:
Frank Phoenix
• coordination with PES principal
investigator,
• Planning and scheduling the
demonstration project
4. PES On-Site Quality Assurance
Coordinator:
Dennis P. Holzschuh. Sr.
• QC activities
/
/
/
/
Wayne Westbrook was identified as
Program Manager for PES in the QAPP,
whereas the SSTP identified John
Chehaske as the Program Manager for
PES. In either case, it will not affect the
data quality or scope of the project.
Dennis Falgout was not present at the
emissions testing.
Frank Phoenix is the Task Manager and
is responsible for all the project
activities at the emissions testing site.
Mr. Holzschuh is responsible for the on-
site QA/QC activities and was present.
Technical Systms Audit of Test Methods Performed by PES
3.5
-------
AUDIT QUESTIONS
RESPONSE
N
N
COMMENT
5 . Have there been any changes in the
project organization and the
personnel as outlined in the
QAPP?
In general, there are no significant
changes except staff from Atlantic
Technical Services, Inc., were not
present. MM5 train samples for the
Analysis of PAHs will be analyzed by
Quanterra laboratories instead of
Triangle Labs. This was approved by
EPA WAM prior to the field testing.
Quanterra labs have high resolution
GC/MS analysis capability for PAHs.
6. Manual Test Methods
Operators:
Mike Maret VOST at TED
Trov Abernathv. VOST Ml8 at
SED
Dennis Holzschuh. Jr.. MM5 at
SED
Joe Rubio. MM5& M315 at SED
Brian Purser. Ml8 at TED
NickNeilson. M315 at TED
Jessica Swift. MetStation
Jairo Barreda. Shipping & Sample
Custodian
Laura Kinner, GC/MS Operator
Jim Peeler, GC/MS Operator
Josh Letomeau, Process Monitor
Each identified operator was
responsible for sample collection and
sample recovery for that method.
7. EPA Work Assignment -
Manager
Michael L. Toney
Mr. Toney was present throughout the
entire testing program and coordinated
the efforts of the emissions testing
teams. He authorized all changes in
testing schedule and procedures.
Technical Systms Audit of Test Methods Performed by PES
3.6
-------
AUDIT QUESTIONS
8. EPA QA Officer:
Lara P. Autry
• review and approve QAPP
• review and approve QA activities
9. Does the project maintain a current
summary of the training and
experience of each individual
engaged in the project?
10. Does the project maintain
descriptions of assignment
responsibilities and required
proficiency levels?
RESPONSE
Y
/
N
/
N
A
/
COMMENT
Ms. Autry was not present at the
emissions testing.
Training and experience of each
assigned person were maintained at the
office.
Responsibilities are assigned for each
person and it appears that they are all
well qualified. Only two persons,
Jessica Swift and Jairo Barreda, are
summer interns and they have been
given sufficient training for the work
assigned to them.
Additional Questions or Comments:
C. METHOD SPECIFIC - EPA Method 1
1 . Is stack diameter properly
determined?
2. Is distance to nearest upstream
disturbance properly determined?
3. Is distance to nearest downstream
disturbance properly determined?
4. Is number of sampling points
properly selected?
5. Is points properly marked on pitot
tube?
6. Verification of cyclonic flow is
acceptable?
/
/
/
/
/
/
The tunnel exhaust is a horizontal 32
inch diameter duct which leads from the
load-out tunnel to the Smog Hog.
For isokinetic testing, a 24-point
traverse matrix consisting of 12 traverse
points on each of two perpendicular
traverse lines was used.
Points are noted on the tape which is
attached to the pitot tube and probe.
Technical Systms Audit of Test Methods Performed by PES
3.7
-------
AUDIT QUESTIONS
7. Prior to sampling, all duct
dimensions are checked against
preliminary information to verify
measurement at locations, location
of test ports, and stack inside
dimensions?
8. Are the stack inside dimensions,
wall thickness, and sample post
depths measured to the nearest
1/16 inch?
RESPONSE
Y
/
/
N
N
A
COMMENT
The stack dimensions and locations of
the traverse points were verified prior to
sampling.
Performed prior to the testing.
Additional Questions or Comments:
The new silo exhaust duct was installed at Silo 2 instead of Silo 3. Since the new SED is 10 inches in
diameter, Method 1 A was used instead of Method 1 . This change was approved by EPA WAM.
Some of the work was performed prior to the auditor's arrival to the site.
The silo exhaust and tunnel exhaust duct dimensions and locations of the traverse points were
verified prior to testing. Prior to testing, the silo exhaust and tunnel exhaust ducts were checked for
the presence of nonparallel flow by recording yaw angle misalignment at each isokinetic sampling
point. The details are in the PES site-specific Test Plan.
D. METHOD SPECIFIC - EPA Method 2
1 . Is pitot tube, lines and manometer
assembled correctly?
2. Is manometer leveled and zeroed
before and after each test?
3. Is pitot tube checked for chips?
Performed leak checks before and
after each test run?
4. Is cyclonic flow checked properly?
5 . Is orientation of pitot tube correct
during traverse?
6. Is sampling port adequately sealed
around pitot tube?
/
/
/
/
/
/
A type S pitot tube is connected to an
inclined-vertical manometer.
The box containing the manometers is
kept on a bench. Noticed zero before
and after each run.
Leak checks were performed before and
after each test run. Leak rates are noted
in data sheets.
Noticed the orientation of pitot tube and
found to be acceptable during traverse.
It is sealed either with gloves or a cloth.
Technical Systms Audit of Test Methods Performed by PES
3.8
-------
AUDIT QUESTIONS
7. Is process operating at correct
conditions?
8. Is stable reading taken at each
traverse point?
9. Is static pressure measured?
10. Is temperature measured?
11. Is moisture content determined? If
so, what method used?
12. Is data recorded properly?
1 3 . Are calculations correct?
RESPONSE
Y
/
/
/
/
/
N
N
A
/
/
COMMENT
Sampling was done whenever the
process was operating properly and at
correct conditions (determined prior to
the sampling).
Readings are noted in the data sheets.
The effluent gas temperature is recorded
at each traverse point using type-K
thermocouple.
Moisture content was measured by EPA
Method 3 15.
Data are recorded in data sheets.
Calculations will be performed in the
office and not at the site.
Additional Questions and Comments:
E. METHOD SPECIFIC - EPA Method 4
1 . Is method conducted in
conjunction with pollutant test
methods 3 15 and MM-5?
2. Are impingers properly placed?
Impinger contents - 1, 2, 3, 4, 5.
3 . Sampling time per point?
4. Number of points?
5. Is probe heater on? What
temperature? Is it stable?
/
/
/
/
Method 3 1 5 and MM-5 trains were run
simultaneously both at the silo tunnel
and silo exhaust.
For Method 3 1 5, the first and second
impingers contained 100 mL of DI
water each, the third impinger is empty,
and the fourth and fifth impingers
contained 200 g of silica gel.
10 min at the silo tunnel
5 m in at the silo exhaust
24 points
Probe is heated at 250 °F. Temperature
readings are noted in the data sheets.
Technical Systms Audit of Test Methods Performed by PES
3.9
-------
AUDIT QUESTIONS
6. Is filter heater on? What
temperature? Is it stable?
7. Is crushed ice in ice bath around
impingers?
8. Is the exit temperature being kept
below 68 °F?
9. Is pretest leak check conducted?
Leakage rate?
10. Is sampling rate constant? Is it
isokinetic sampling?
11. Is port leak check performed?
Leakage rate?
1 2. Is electronic balance calibrated
with reading within 0.1 grams of
known reference standard?
13. All data are recorded properly?
RESPONSE
Y
/
/
/
/
/
/
/
N
N
A
/
COMMENT
Filter is heated at 250 °F. Temperature
readings are noted every 10 min in the
data sheets.
Crushed ice added periodically to
maintain the impingers at 0 °C.
Temperatures are periodically recorded
in the data sheets (every 5 min).
Data sheets will be provided. Leakage
rate was within the acceptable limits.
Sampling rate is 1.5 ft3 /min and found
to be within the specifications.
Isokinetic sampling was followed.
Data sheets will be provided. Leakage
rate was within the acceptable limits.
Calibration was performed in the
laboratory but not at the site. Calibration
data will be provided.
Noted in data sheets.
Additional Questions and Comments:
Moisture was determined from EPA Method 315 instead of EPA Method 5. Audit questions were
completed based on EPA Method 315 sampling procedures. Method 4 was performed in conjunction
with each EPA Method 315 test run.
F. METHOD SPECIFIC - EPA Method 315
Apparatus
1 . Is the probe nozzle made of glass
or glass lined? What is its design?
Is it clean?
2. Is the probe liner made of
borosilicate or quartz and is it
clean?
/
/
Probe nozzle was made of glass.
Cleaned with methylene chloride and
methanol (50:50 mixture). It appears to
be clean.
Probe liner is made of borosilicate.
Cleaned with methylene chloride and
methanol mixture (50:50). It appears to
be clean.
Technical Systms Audit of Test Methods Performed by PES
3.10
-------
AUDIT QUESTIONS
3. Is it type S pitot tube and is it
properly attached?
4. Is the differential pressure gauge as
two inclined manometers?
5. Is the filter holder borosilicate
glass; glass frit-support; or silicone
rubber gasket?
6. Describe number of impingers in
the condenser and its contents?
7. What type of barometer? Mercury
or Aneroid?
8. What type of gas density
determination equipment used?
- sensor type
- pressure gauge
Temperature sensor attached to
probe?
9. Has filters checked visually for
inequalities?
10. Has filters properly labeled?
1 1 . Has pretest and post-test leak
check performed properly?
12. Has impingers properly
assembled?
13. Has pitot tube lines checked for
plugging or leaks?
1 4. Has meter box leveled
periodically?
1 5 . Have manometers zeroed?
RESPONSE
Y
/
/
/
/
/
/
/
/
/
/
/
N
N
A
/
/
COMMENT
S-type pitot tube was used and it is
properly attached.
The meter box contained two inclined
manometers.
The filter holder is a borosilicate glass.
The first and second impingers
contained 200 mL of DI water, the third
impinger is empty, and the fourth
impinger contained 200 g of silica gel.
Aneroid barometer was used. It was
calibrated against mercury manometer.
Glass fiber filter appears to be good.
Filters after collection were kept in an
amber glass bottle and labeled.
Leak checks performed properly before
and after each run and noted in the data
sheets.
Impingers were assembled according to
the Method 315 specifications.
Leak-checked before and after each run.
Meter box was kept on a horizontal
surface.
Technical Systms Audit of Test Methods Performed by PES
3.11
-------
AUDIT QUESTIONS
16. Has acetone-insoluble head-stable
silicone grease added to all ground
glass joints?
17. Is probe heat uniform along length
of probe?
1 8. Has effective seal made around
probe when in-stack?
19. Nozzle & pitot tube parallel to
stack wall at all times.
20. Has filter changed during run?
Any particulate lost?
2 1 . Have data sheets complete and data
properly recorded?
RESPONSE
Y
/
/
/
/
N
/
N
A
/
COMMENT
No silicone grease was used to the
ground glass joints. They are used only
when it leaks.
Probe is kept at 250 °F and the
temperatures are noted in the data sheets
every 5 min.
Sealed with hand gloves or a cloth and
found to be acceptable.
No filter changed during the run. No
particulate was lost.
Data sheets are filled out properly with
a legible ink pen.
Additional Questions and Comments:
1 . Due to problems in the silo tunnel and silo exhaust, the samples collected on the first da>
(7/23/98) were voided after approval from EPA WAM. After 2 hr sampling, it was noted that
the silo exhaust damper was closed. Therefore, the damper was operated and continued the
sampling for another 2 hr. The first day run will be repeated on 7/27/98.
2. Observed the Method 3 1 5 sampling run at the silo 2 exhaust at the roof on 7/25/98. Flow rate
0.75 ft3/min. Sampling was done only for 2 hr due to expected high concentrations. Method 315
and MM5 trains were operated at two different times. Due to smaller stack diameter, traverse
readings were taken from one place and probe was kept in another hole and readings were noted
for every 5 min. Stack is at negative pressure. Stack hole is covered with gloves.
3. 4-hr sampling was performed from the silo 2 tunnel while two trucks were going through the
tunnel to get the background emissions.
LABORATORY INFORMATION NECESSARY FOR EPA METHOD 315
1 . Was the calibration information
documented in log books?
2. Have the previous calibrations met
the acceptable tolerances?
/
Technical Systms Audit of Test Methods Performed by PES
3.12
-------
AUDIT QUESTIONS
3. Has the Type-S pitot tube been
verified using standards outside of
the laboratory?
4. Describe the pitot tube calibration
apparatus.
RESPONSE
Y
N
N
A
COMMENT
Additional Questions and Comments:
Calibrations were performed in the laboratory prior to the testing on the site. Calibration sheets will
be supplied to the auditors after the field test.
Calibration and General
1 . Have the dry gas meters been
calibrated against a standard? (If
so, which standard?)
2. Have the stack and train
temperature sensors been
calibrated against a reference
thermometer?
3. Has the nozzle been calibrated to
nearest 0.025 mm (0.001 in), and
has the nozzle size been properly
selected?
4. Is the train correctly setup up and
leak-checked to less than 4% or
0.00057 m3/min (0.02 ft3/ min),
whichever is less?
5. Are the train components clean and
free of breaks, cracks and leaks,
and is the probe liner clean and
leak free at 380 mm (1 5 in) Hg?
6. Are the pitot tube lines free of
plugs or leaks?
7. Is the probe heating system
operating correctly?
/
/
/
/
/
/
/
Leak checks were performed before and
after the sample collection and found to
be acceptable.
Technical Systms Audit of Test Methods Performed by PES
3.13
-------
AUDIT QUESTIONS
8. Are the pitot tube and temperature
sensors properly attached to probe?
9. Are the nozzle and pitot tube
located parallel to stack wall?
Observe handling and positioning
of the probe.
1 0. Is the filter holder temperature
maintained at 120 ± 14°C (248 ±
25 °F) throughout the tests?
11. Is the sample gas temperature at
the last impinger maintained at <
20 °C (68 °F) throughout the tests?
12. Is isokinetic sampling maintained
within ± 10% and checked every
five minutes?
13. Is the sample site selection an
appropriate distance downstream
from any flow disturbance?
14. Are filters free of irregularities,
properly installed, and properly
labeled?
1 5 . Do the equipment operators have
access to test protocols and
methods, are data sheets available,
and is equipment in good repair.
1 6. Are all data recorded and
calculations checked? Is at least
one decimal point beyond that of
acquired data retained?
1 7. Are all impingers cooled in an ice
bath at all times?
18. Is full stack traversing being
conducted?
19. Do recovery methods prevent
contamination?
RESPONSE
Y
/
/
/
/
/
/
/
/
/
/
/
/
N
N
A
COMMENT
Equipment operators have copies of the
protocols and methods. Data sheets are
available to each train operator.
Calculations will be checked in the
office.
Crushed ice was added periodically to
maintain the temperature.
Sample recovery was performed in the
trailer, which is relatively clean.
Technical Systms Audit of Test Methods Performed by PES
3.14
-------
AUDIT QUESTIONS
20. Are graduated cylinders within 2
ml (or less) subdivisions used?
2 1 . Are all openings capped during
train disassembly?
22. Is the clean-up area clean and
protected from the wind?
23. Are any particulates spilled?
24. Do any visible particles remain
inside the probe?
25. How is the pitot tube cleaned?
26. Are sample containers labeled and
sealed tight, and is the liquid level
marked?
27. What is the history of the S-type
pitot being calibrated against a std
pitot?
28. How was the inside diameter of the
stack measured?
29. How is the probe marked to ensure
proper sampling locations?
30. How long does the probe remain at
each sample point? Is the reading
stable?
3 1 . How is alignment ensured while
sampling? Guidance manuals
specify visual observations and not
the highest delta p.
RESPONSE
Y
/
/
/
/
/
N
/
/
/
N
A
/
/
COMMENT
Graduated cylinders within 2 mL
subdivisions were not used. However,
standard impingers were used and a
known volume of solutions was added.
Capped with Teflon tape.
It was performed in the trailer. The area
is relatively clean.
The operators are very careful in
transferring the filter paper to the glass
jar.
None was noticed inside the probe.
Cleaned with methylene chloride and
methanol (50:50) mixture.
Electronically printed labels were
affixed to the containers. Liquid level is
marked with a pen and sealed with
Teflon tape.
The calibration was performed in the
laboratory and the calibration data will
be supplied to the auditors after the field
test.
It was measured prior to the testing and
noted to be 32 inches.
Probe is wrapped with tape at each
traverse point and marked with a pen.
The probe remained at 10 min at each
sample point. Readings are noted in the
data sheets.
Visual observations indicate that
alignment appears to be QC.
Technical Systms Audit of Test Methods Performed by PES
3.15
-------
AUDIT QUESTIONS
32. Were the unused ports plugged
while sampling occurred?
3 3 . Was the equipment damaged
during the test? Explain.
34. How is static pressure measured,
and what is it? ...sampling?
35. How is steady state process
indicated during sampling?
....would be the impact?
36. Were they any changes in the
facility emissions during sampling?
37. If changes in emissions did occur
during sampling, what was the
impact?
RESPONSE
Y
/
/
N
/
N
A
/
COMMENT
Unused ports were sealed with electric
tape.
A few of the glass nozzles were broken
during recovery operation. They were
replaced with new ones for the next run.
Static pressure was measured with an
inclined manometer.
It will not be a steady-state process.
Impact will be minimal due to an
integrated sample.
Emissions may vary at the facility due
to the nature of the operation.
Impact will be minimal due to an
integrated sample collection method.
Additional Questions and Comments:
G. METHOD SPECIFIC - EPA Method 18
1 . Have you performed presurvey
sampling using Method 1 8
procedures?
2. What are the approximate
concentrations of the targeted
compounds?
3. What is the sampling rate? Is it
constant or proportional?
4. What is the sample time?
/
/
/
Presurvey sampling was not performed
using Method 1 8 procedures. However,
grab samples were collected and
analyzed using canisters. Method SW
846 M0030 VOST data were collected
at the hot mix dryer stack.
Sampling rate was 1 L/min and sampled
for 4 hr at silo tunnel, whereas 2 hr
sampling was done at silo exhaust.
4 hr at the silo tunnel, 2 hr at the silo
exhaust.
Technical Systms Audit of Test Methods Performed by PES
3.16
-------
AUDIT QUESTIONS
5 . Probe heat or not. If so, what
temperature?
RESPONSE
Y
N
N
A
/
COMMENT
Not heated. Teflon lines were used.
Ambient temperature.
Additional Questions and Comments:
Apparatus
6. What type of probe is used —
stainless steel, glass or Teflon?
7. Is it heated and any filter used?
8. Silica gel tube or extra adsorption
tube used prior to adsorption tube
when moisture content is > 3
percent.
9. Is the leakless sample pump
calibrated within limiting (sonic)
orifice or flow meter?
10. Is rotameter used to detect changes
in flow?
1 1 . Are the two sampling trains run in
parallel?
12. Are the pre-spiked adsorbent tubes
used in one train and non- spiked
adsorbent tubes used in the second
train?
1 3 . What are the compounds spiked
and at what concentrations?
14. Is accurately measured sample time
with a stop watch?
/
/
/
/
/
/
/
/
Teflon lines were used.
No filter was used and Teflon lines are
not heated.
None was used at the silo 2 tunnel
emissions sampling. However, two
impingers at ice path temperature were
used at the silo exhaust.
KNS Teflon pump was used to pull the
sample gas. The pump was calibrated in
the laboratory with a bubble flow meter.
The gas is pulled through a T-
connection into spiked and unspiked
sampling tubes.
Two different probes but pulled through
a common pump.
200 ug each of benzene, toluene,
xylene, hexane, and cumene was spiked.
Liquid mixture was spiked onto the
cartridge prior to sampling.
Technical Systms Audit of Test Methods Performed by PES
3.17
-------
AUDIT QUESTIONS
15. Is the sampling pump and flow
meter recently calibrated with
bubble meter?
1 6. Whether extreme care is taken to
ensure that no sample is lost in the
probe or sample line prior to the
adsorption tube.
1 7. Is pretest leak check acceptable?
(No flow indicated or meter.)
1 8. Total sample time, sample flow
rate, barometric pressure, and
ambient temperature are recorded?
19. Total sample volume
commensurate with expected
concentration and recommended
sample loading factors?
20. Is post-test leak check and volume
rate meter check acceptable? (No
flow indicated on meter, post-test
calculated flow rate is within 5
percent of pretest flow rate?)
21. Is desorption efficiency determined
for adsorbent to be used for field
sampling? If so, what are the
desorption efficiencies?
22. Is collection efficiency determined
for adsorption tubes used for actual
field sampling?
23 . Are the adsorbent tubes stored
properly after sampling?
RESPONSE
Y
/
/
/
/
/
/
N
N
A
/
/
COMMENT
Recorded in data sheets.
4 hr sampling was performed at the silo
tunnel. 2 hr sampling at the silo exhaust.
The gas sample is pulled into spiked and
unspiked sampling tubes.
The analyst reported that the desorption
efficiencies were determined in the lab
prior to the testing and they are 95
percent for each compound.
The analyst reported that the collection
efficiencies were determined in the lab.
The acceptable range is 70-130 percent.
However, 85 percent was found.
They were stored in an ice cooler after
sampling.
Technical Systms Audit of Test Methods Performed by PES
3.18
-------
AUDIT QUESTIONS
RESPONSE
Y
N
N
A
COMMENT
Additional Questions and Comments:
AnaSorb 747 (1,000 mg front + 1,000 mg backtrap) was used. Carbon disulfide + dimethyl
formanide will be used for desorption. No glass wool was used in the Teflon lines. Sample gas is
pulled through a vacuum pump and maintained a flow through a critical orifice. There may be a
small pulsation and the impact is minimal. Method 18 was performed for two losses at 1 L/min at the
silo exhaust. Impingers were used prior to the sampling tubes at the silo exhaust to condense the
water vapor.
H. METHOD SPECIFIC - SW-846 Method 0030 (VOST)
1 . Will the total run time be a
minimum of 2 hours?
2. Is the maximum load time 20 min.
For each pair of cartridges? At
1 L/min sampling rate?
3 . Is a quartz liner wed inside the
stainless steel probe?
4. Is the probe maintained at a
temperature greater than 150°C?
5. Do the sorbent cartridges appear to
be sealed tightly in their carry
cases?
6. Have the sorbent cartridges been
placed correctly in the sample train
(1st cartridge Tenax; 2 cartridge
Tenax/charcoal)?
7. Do all vacuum gauges, pump
connections, calibrated rotameters,
and dry gas meters appear in good
working order with leak-tight
seals?
/
/
/
/
/
/
/
The total run time is 20 min. Four runs
were performed on each day.
Generally, 1 L/min sampling rate was
used at silo 2 tunnel emissions.
However, 0.25 L/min for 10 min was
used at the silo exhaust emissions.
Glass wool was inserted in the front of
the quartz liner to remove any
particulates.
Probe temperature was maintained at
255 °F.
The sealed cartridges were kept in
carrying cases.
Technical Systms Audit of Test Methods Performed by PES
3.19
-------
AUDIT QUESTIONS
8. Is there an available thermal couple
reading between the first condenser
and first Tenax cartridge? CHECK
TEMPERATURE. MUST BE
LESS THAN 20 °C.
9. Is the sample line between the
probe and the first condenser less
than 5 ft.?
— Is it Teflon?
— Is it heat traced to 1 50 °C?
— Are compression fittings used?
10. Does each individual cartridge
have its own unique ID number
and flow direction arrow marked
on it?
1 1 . Were the sorbent cartridges
received in the field on cold packs
(~4°Q?
12. Is the cooling water to the
condenser being maintained at or
near 0°C?
13. Is the train leak-checked at the
beginning of a run to the following
specifications? (1) pull a vacuum
to 250 mm Hg (10 in Hg), (2) leak
rate less than 2.5 mm Hg after 1
minute?
14. Is a charcoal canister used to filter
the ambient air used to return
system to ambient pressure after
the leak check?
15. Was the sample train leak-checked
after 20L of gas was sampled and
was the highest pressure drop
encountered recorded so that his
value can be used during the
second leak test?
RESPONSE
Y
/
/
/
/
/
/
/
N
/
N
A
COMMENT
Temperature was measured and it is less
than 20 °C.
Teflon line was used. It is not heat
traced.
Higher than 0 °C, but lower than 20 °C.
Ice water circulated.
Leak test was performed before and
after each run. The sampling rate and
volume are different at the silo exhaust
emissions testing. It was approved by
the EPA WAM.
Technical Systms Audit of Test Methods Performed by PES
3.20
-------
AUDIT QUESTIONS
16. Are the field blanks exposed for
the same amount of time as it takes
to change sorbent cartridges in the
VOST?
1 7. Was there a field blank exposed for
each run?
RESPONSE
Y
/
N
/
N
A
COMMENT
Field blank was performed on 7/25/98.
Field blank was performed on 7/25/98.
Additional Questions and Comments:
7/25/98. Due to higher concentrations at the silo exhaust, it was authorized to run VOST at 0.25
L/min for 10 min. Four runs were done each day. Stack is at negative pressure. No moisture
condensation was observed in the impinger. The flow rate of 0.25 L/min is at low setting in the
VOST console box. Rotameter setting is 0.2, which is the bottom of the scale.
I. METHOD SPECIFIC - SW-846-0010 (Modified Method 5)
1 . Is the probe nozzle made of 3 1 6
stainless steel or glass with a sharp,
tapered (30° angle) leading edge?
2. Is the nozzle of buttonhook or
elbow design and seamless?
3 . Is the nozzle calibrated?
4. Is the probe glass lined and heated
to 120 ± 1 4 °C at the exit end
during sampling?
5. Is the type s pitot tube on a plane
even with or above the nozzle entry
plane during sampling?
6. Does the pitot tube have a known
coefficient? What is it?
7. Does the train have two
manometers: one for velocity-head
(AP) readings and one for orifice
differential pressure readings
(AH)?
8. Is the filter holder made of glass,
and the gasket of Teflon?
/
/
/
/
/
/
/
/
The probe nozzle is made of glass.
The nozzle is buttonhook.
It is calibrated in the laboratory.
The coefficient is 0.84.
Two inclined manometers were used.
Glass
Technical Systms Audit of Test Methods Performed by PES
3.21
-------
AUDIT QUESTIONS
RESPONSE
N
N
A
COMMENT
9. Is the XAD-2 module cooled to 17
±3°C?
Ice water bath was maintained.
10. Is there a thermocouple in the glass
well of the sorbent module to
monitor temperature of the trap?
The temperature is 42 °F.
Additional Questions and Comments:
Train Components
1. Is the sorbent module followed by
a condensate knockout trap?
2. Is stack gas moisture being
monitored with four 500 mL
impingers following the knockout
trap? List the impinger solutions.
First impinger is empty. Second and
third impingers contained 200 mL of
HPLC-DI water. Fourth impinger is
empty. Fifth impinger 200 g of silica
gel.
3. Is the metering system consisting
of vacuum gauge, leak-free pump,
thermometer, and dry gas meter,
keeping the sampling rate of the
MM5 train within 10% of
isokinekticity?
4. Is the metering system determining
the sample volume within 2% of
the true volume?
5. Is the barometric pressure being
recorded and corrected for
elevation differences between the
location of the barometric and the
sampling point at a rate of-2.5 mm
Hg per 30-m elevation increase (or
+2.5 mm Hg per 30-m elevation
decrease)?
Barometric pressure is noted from the
Met Station and at the truck.
Technical Systms Audit of Test Methods Performed by PES
3.22
-------
AUDIT QUESTIONS
6. Is the stack gas temperature sensor
attached to the pitot tube, such that
the tip of the sensor extends
beyond the leading edge of the
probe sheath and does not interfere
with the pitot tube opening?
7. Are calibration and preparation
data being recorded in a
permanently bound laboratory
notebook (i.e., filter and silica get
tare weights, clean XAD-2,
QA/QC check results, dry-gas
meter, and thermocouple
calibrations)?
8. Is the train grease-free upstream of
the module?
RESPONSE
Y
/
/
/
N
N
A
COMMENT
Noted in the data sheets but not in the
bound notebook.
Additional Questions and Comments:
Preparation of the Train
1 . Are the probe liner brushes
provided at least as long as the
probe?
2. Are the probe brushes made of
nylon bristles and stainless steel
wire handles with extensions?
3. Are the wash bottles made of
Teflon or glass?
4. Are the sample storage bottles
made of amber glass and screw-
type Teflon lined caps?
5. Are the filters made of glass or
quartz fiber?
6. Has the XAD-2 resin been cleaned
prior to use and QC to a blank less
than 4 mg/kg?
/
/
/
/
/
/
Probe brushes were made of nylon
bristles.
Teflon bottles were used.
Amber glass bottles with Teflon-lined
caps were used.
Glass fiber filters were used.
Quanterra labs provided the XAD-2
cartridges.
Technical Systms Audit of Test Methods Performed by PES
3.23
-------
AUDIT QUESTIONS
7. Is distilled organic-free water
(Type II) provided for the impinger
solutions?
8. Are the clean up solvents pesticide
grade?
9. Are the filters desiccated at 20 ±
5.6°C and ambient pressure for at
least 24 hours, weighed at intervals
of at least 6 hours to a constant
weight (± 0.5 mg), and recorded at
0.1 mg?
1 0. Have the number of minimum
sampling points been determined
for each sampling location (inlet,
outlet, and stack): What are the
numbers?
1 1 . Have the pitot lines been leak
checked?
12. Has the stack gas moisture content
been determined? What is it?
1 3 . Were there any nozzle changes
during sampling?
14. Is the sample volume as outlined in
the sampling plan being pulled?
What is it?
15. Are all openings to the train kept
covered with Teflon film prior to
assembly?
16. Are the XAD-2 modules assembled
off-site?
1 7. Is the filter placed in the filter
holder with tweezers or while
wearing surgical gloves?
RESPONSE
Y
/
/
/
/
/
/
/
/
/
N
/
/
N
A
COMMENT
HPLC grade DI water was used.
Methylene chloride + methanol (50:50)
pesticide grade solvents were used.
Weight of particulates is not measured
with MM5 train.
24 points.
Leak checked before and after the run
and found to be leak free within the
specifications.
Stack gas moisture content at the silo
tunnel is -1-2 percent. The moisture is
higher at silo exhaust.
No nozzle changes during sampling.
Nozzle diameter is 0.252 inches.
0.75 ft3/min for 4 hr at the silo tunnel.
0.75 ft/min for 2 hr at the silo exhaust.
XAD-2 modules were supplied by
Quanterra labs. Assembled in the rack.
Technical Systms Audit of Test Methods Performed by PES
3.24
-------
AUDIT QUESTIONS
18. Is a pre-test leak check of the train
administered?
19. If a train component is changed
during sampling, is the train leak-
checked prior to the change? Is the
leakage rate less than 4% of the
average sampling rate?
20. Is a post- test leak check
performed? Is the leakage rate less
than 4% of the sampling rate?
RESPONSE
Y
/
/
N
/
N
A
COMMENT
Noted in the data sheets.
No components were changed during
sampling.
Leak rate is 0.02 inch.
Additional Questions and Comments:
Running the Train
1 . Is the sampling rate maintained
within 10% of true isokinetic?
2. Is the filter maintained at 120 ±
14°C?
3 . Is the sorbent module maintained
at 17±3°C?
4. Are the dry gas meter readings
recorded on field data sheets?
/
/
/
/
Ice water temperature was maintained.
The module is covered with aluminum
foil.
Noted in the data sheets.
Additional Questions and Comments:
Sample Recovery
1 . Is the filter removed from the filter
holder and placed in an identified
Petri dish container with tweezers?
2. Is the filter folded with the filter
cake inside?
/
/
The filter was kept in an amber glass
jar.
The filter is folded and kept in an amber
glass jar.
Technical Systms Audit of Test Methods Performed by PES
3.25
-------
AUDIT QUESTIONS
3 . Is any particular matter adhering to
the filter-holder gasket transferred
to the Petri dish?
4. Is the Petri dish sealed and labeled
container No. 1?
5 . Is the participate matter from the
probe nozzle, probe fitting, probe
liner, and front half of the filter
holder recovered quantitatively by
washing with (1:1 v/v)
methanol/methylene chloride into a
glass container? Labeled container
No. 2?
6. Is a solvent blank retained and
analyzed?
7. Is the sorbent module labeled
container No. 3, capped, and
packaged cold for shipment?
8 Is the condensate from the back
half of the filter module and the
knockout trap measured and
transferred to container No. 4?
9. Are the sample train components
between the filter and the first wet
impinger rinsed into container No.
5?
1 0. Is the silica gel transferred to
container No. 6?
11. Is the volume of the impinger
water in the first three impingers
measured to ± 1 ml and any color
or film noted? Is the impinger
catch discarded?
12. Are all containers sealed and all
shipped refrigerated except the
filter?
RESPONSE
Y
/
/
/
/
/
/
/
/
/
N
N
A
/
COMMENT
The particulate matter adhering to the
filter-holder gasket was transferred into
the glass jar.
The amber glass jar is sealed and
labeled.
Collected into amber glass container
and labeled. The liquid level is marked
on the container with a pen.
The sorbent module weighed, labeled,
and kept in blue ice.
Collected into amber glass jar and
labeled. The liquid level is marked on
the jar with a pen.
Weighed for the moisture content; silica
gel changed for each train.
No color or film was noticed. The
impinger catch is saved in the glass jars.
Technical Systms Audit of Test Methods Performed by PES
3.26
-------
AUDIT QUESTIONS
RESPONSE
Y
N
N
A
COMMENT
Additional Questions and Comments:
J. SAMPLING GENERAL
1 . Is the duration of sampling
sufficient to detect all important
pollutant(s) generated by the
process under investigation?
2. Are there specified limits for
which sampling will be stopped?
Describe.
3 . Were duplicate or replicate
samples taken for each sampling
location?
4. Was the sampling performed in
accordance with the approved
QAPP?
5 . Do sample tracking numbers
indicate when, how, and where the
samples were collected?
6. Are records available of who
collected the sample?
7. Are field log books and laboratory
log notebooks recorded in ink?
8. Are audit histories recorded in the
field log notebooks?
— thermocouple
— solid state temperature
— wood scale performance
— other
/
/
/
/
/
/
/
/
Sampling for 4 hr at the silo 2 tunnel
and 2 hr at the silo exhaust is quite
sufficient.
Sampling will be stopped only when
loading or process problems
experienced at the site.
One run was performed on each day.
Generally followed the approved QAPP.
However, few changes such as sampling
rate at the silo exhaust testing were
made at the site after EPA WAM
authorization.
Labels were attached to the glass jars.
Noted in the data sheets.
Data sheets were used. Recorded legibly
with ink.
Noted in the data sheets in the office.
Additional Questions and Comments:
Technical Systms Audit of Test Methods Performed by PES
3.27
-------
AUDIT QUESTIONS
RESPONSE
Y
N
N
A
COMMENT
K. QUALITY ASSURANCE/QUALITY CONTROL/GENERAL
1 . Have there been any changes in the
project organization and the
personnel as outlined in the
QAPP?
2. Are there written plans to report
changes in the QAPP during data-
gathering activities?
3. Were field biased blanks and/or
trip blanks used?
4. Calibration information and data
sheets available for:
— Probe/nozzle
— Type-S pitot
— Meter Box including: dry gas
meter and thermocouple
— Barometer
/
/
/
/
One field blank was collected.
Data sheets will be given.
Additional Questions and Comments:
Technical Systms Audit of Test Methods Performed by PES
3.28
-------
AUDIT QUESTIONS
RESPONSE
Y
N
N
A
COMMENT
L. SAMPLE CUSTODY AND INTEGRITY
1 . Is there an SOP or other source of
documentation which describes the
organization's sample custody
procedures?
2. Are records available of when,
how, and where the sample was
collected?
3 . Are records available of who
collected the sample?
4. Who is the field custodian for the
samples? (Name)
5. Are samples individually identified
by number or code so that they can
be traced?
6. Were deviations (if any) from all
SOPs or protocols properly
documented?
7. Sample liquid levels marked on
each container such that the mark
can be seen on the container or on
the label itself.
8. Sample container lids sealed on
outside with Teflon tape and
sample label covered with solvent
resistant tape?
9. Are integrity seals affixed over the
caps of each container?
10. Are seals signed and numbered by
recovery person?
/
/
/
/
/
/
/
/
/
/
There is no SOP at the site. However,
sample custody data sheets and
procedures are available.
Data sheets are available. Information is
noted in the data sheets and labeled on
the bottles.
Recorded on the data sheets.
Jairo Barreda, a summer intern, is
responsible for the shipping and sample
custody.
Labels are electronically made, printed
for each run with identification, and
affixed to the glass jars.
Recorded by the Task Manager in a
small notebook. It would have been
better if the train operators noted on the
data sheets also.
Marked with a pen on the container.
Solvent-resistant tape is not used to
cover the sample label.
Labels are affixed on the side of the
glass jar.
Seals are not signed. Numbered on the
labels.
Additional Questions and Comments:
Technical Systms Audit of Test Methods Performed by PES
3.29
-------
AUDIT QUESTIONS
RESPONSE
Y
N
N
A
COMMENT
M. MISCELLANEOUS MEASUREMENTS - Wind Speed, Wind Direction, Ambient
Temperature and Humidity
1 . Is the meteorological station
operated according to the
manufacturer's specification?
2. Is the manufacturer's
specifications manual available at
the site?
3 . Are the readings recorded
continuously through out the test
period?
4. Was the wind speed measured and
calibrated?
5 . How the wind direction measured
and calibrated?
6. How the temperature is measured
and what is the range?
7. Is the ambient humidity measured
once per test run by wet bulb using
a sling psychrometer and properly
recorded?
/
/
/
/
/
/
/
Recorded on a data-logger.
Calibrated at the office but not at the
site.
Calibrated at the office but not at the
site.
Thermometer -50 to 50 °C
Measured once in the beginning and
once at the end of the day.
Additional Questions and Comments:
The MET Station was kept at the top of the load-out tunnel near the entrance.
N. Estimation of Particulate Deposition on the Ceiling of the Load-Out Tunnel
Downstream and Silo No. 5
1 . Is one test plate for each section is
installed properly in the beginning
of the test program?
2. Are the test plates and ceiling
sections cleaned with acetone
properly in the beginning and at
the end of the test program?
/
/
Technical Systms Audit of Test Methods Performed by PES
3.30
-------
AUDIT QUESTIONS
3. Have they collected three acetone
rinse samples and analyzed
gravimetrically?
RESPONSE
Y
N
N
A
COMMENT
Analysis will be performed in the office.
Additional Questions and Comments:
Measured the distance from Silo No. 5 to the end of the tunnel which is approximately 57 feet.
Divided the distance into three equal areas. Three test plates and ceiling sections were cleaned with
acetone. Each test plate is screwed to the top of the roof at 19 feet distance from one another on
7/2/98 morning. They were removed on 7/26/98 and rinsed with acetone and will be analyzed
gravimetrically.
O. Estimation of Particulate Deposition on the Inside Walls of Loud-Out-Tunnel
Exhaust Plenum
1 . Are six pieces of box pipe installed
properly inside the exhaust plenum
under Silo No. 3 in the beginning
of the test program?
2. Are the box pipes and installation
sections cleaned with acetone
properly in the beginning and at
the end of the test program?
3. Have they collected six acetone
rinse samples and analyzed
gravimetricallv?
/
/
/
Charged under Silo No. 2 on 7/23/98
and removed on 7/26/98 morning.
Installation sections were no1 cleaned at
the end of the test program.
Acetone rinse samples will be analyzed
later in the laboratory.
Additional Questions and Comments:
Installed at the downstream of the exhaust plenum.
P. Estimation of Particulate Deposition on the Inside Walls of the Temporary
Silo Exhaust and Wind Tunnel Exhaust
1 . Have they collected one acetone
rinse sample from inside walls of
the temporary silo exhaust and four
samples from the wind tunnel
exhaust?
/
One was kept at the silo exhaust and
three samples were taken from the wind
tunnel exhaust.
Technical Systms Audit of Test Methods Performed by PES
3.31
-------
AUDIT QUESTIONS
2. Have they cleaned the areas and
installed the test plates properly?
RESPONSE
Y
/
N
N
A
COMMENT
Additional Questions and Comments:
Old silo exhaust pipe was cleaned and taken for metals analysis.
0. Direct Interface Portable GC/MS
1 . Is heated sample line used to draw
the sample into the GC/MS?
2. How the instrument was
calibrated?
•
3. What is the flow rate and sample
volume collected?
4. How is the sample concentrated?
5. Is the thermal desorption technique
used and at what temperature it
was desorbed?
6. Are there blank runs performed?
7. How is the moisture interference
that was eliminated or minimized
during the analysis?
/
/
/
/
/
/
Teflon lines were used at ambient
temperature.
Calibrated with 36 compounds in the
laboratory. Checked with 9 component
mixture at the field site daily.
Sample is drawn at 2 L/min.
Subsequently 1 50 cm /mm is diverted
into the mass spectrometer. A 20-30 uL
sample was used to inject into the GC.
No concentration step.
No concentration step. Therefore,
thermal desorption is not required.
Nitrogen blank daily was performed.
Up to 8 percent moisture levels, no
conditioning is required. Above that day
the sample used an impinger before
introducing it into GC/MS.
Additional Questions and Comments:
1 . GC/MS runs were done at silo tunnel, silo exhaust, ambient air, end of the tunnel, and dryer
exhaust.
2. Lot of moisture was condensed at the silo exhaust and dryer exhaust. Impinger was used to
collect the water. Linearity checked in the laboratory, 6 injections ±20 percent RSD.
Technical Systms Audit of Test Methods Performed by PES
3.32
-------
AUDIT QUESTIONS
RESPONSE
N
N
COMMENT
Additional Questions and Comments:
Column used: SPB-1 3-inch wound capillary column sample drawn through 0.3 urn glass fiber filter.
Detection limits vary from compound to compound.
Technical Systms Audit of Test Methods Performed by PES
3.33
-------
TECHNICAL REPORT DATA
(Please read Instructions on reverse before completing)
1 REPORT NO
EPA-454/R-00-026
3 RECIPIENTS ACCESSION NO.
4 TITLE AND SUBTITLE
HOT MIX ASPHALT PLANTS
TECHNICAL SYSTEMS AUDIT of TESTING at PLANT C
ASPHALT PLANT C
LOS ANGELES, CALIFORNIA
5 REPORT DATE
May 2000
6 PERFORMING ORGANIZATION CODE
7 AUTHOR(S)
Lara Autry (EPA)
R.K.M. Jayanty (RTI)
Robert S. Wright (RTI)
8 PERFORMING ORGANIZATION REPORT NO
9 PERFORMING ORGANIZATION NAME AND ADDRESS
Research Triangle Institute
Center for Environmental Measurements and Quality Assurance
3040 Cornwallis Road, Post Office Box 12194
Research Triangle Park, NC 27709-2194
10 PROGRAM ELEMENT NO
CONTRACT/GRANT NO
68-D4-0091
12 SPONSORING AGENCY NAME AND ADDRESS
Office of Air Quality Planning and Standards
Office of Air and Radiation
U.S Environmental Protection Agency
Research Triangle Park, NC 27711
13 TYPE OF REPORT AND PERIOD COVERED
Final
14 SPONSORING AGENCY CODE
EPA/200/04
15 SUPPLEMENTARY NOTES
16 ABSTRACT
The United States Environmental Protection Agency (EPA) Emission Factors and Inventory Group (EFIG) is
investigating the Hot Mix Asphalt industry to identify and quantify criteria and hazardous air pollutants (HAP's) emitted from
transport truck loading and silo filling. EFIG requested that EPA's Emission Measurement Center (EMC) conduct the required
testing. Under separate EPA contracts, Midwest Research Institute (MRI) and Pacific Environmental Services (PES)
performed this emissions testing. An independent technical systems audit was performed as part of the quality assurance
evaluation of this testing effort. The EMC issued a work assignment to Research Triangle Institute (RTI) to perform this
technical system audit. The primary objective of the testing program was to characterize uncontrolled emissions of the critena
pollutants paniculate matter (PM) and total hydrocarbons (THC) and emissions of volatile and semi-volatile organic HAP's
including polycyclic organic matter, phenol, benzene, toluene, xylene, emylbenzene, 2-butanone, cumene, formaldahyde,
hexane, isooctane and others.
This report includes a summary of the independent audit results and detailed Technical Systems Audit checklists of
the evaluations RTI performed of the testing by MRI and PES.
17 KEY WORDS AND DOCUMENT ANALYSIS
a DESCRIPTORS
b IDENTIFIERS/OPEN ENDED TERMS
c COSATI Field/Group
Hot Mix Asphalt
Silo Filling
Truck Loading
Particulate Matter
Volatile Organic Compounds
Total Hydrocarbons
Hazardous Air Pollutants
Polycyclic Organic Matter
Air Pollution control
18 DISTRIBUTION STATEMENT
Release Unlimited
19 SECURITY CLASS (Report)
Unclassified
21 NO. OF PAGES
142
20 SECURITY CLASS (Page)
Unclassified •
22 PRICE
EPA Form 2220-1 (Rev. 4-77) PREVIOUS EDITION IS OBSOLETE
------- |