Quality Assurance Project Plan
For the EPA School Air Toxics
Monitoring Program
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April 2009
Quality Assurance Project Plan for the EPA
School Air Toxics Monitoring Program
Category II QAPP
U.S. Environmental Protection Agency
Office of Air Quality Planning and Standards
Air Quality Assessment Division
Research Triangle Park, North Carolina, 27711
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1.0 Signature Page
Richard Wayland Date
U.S. Environmental Protection Agency
OAQPS - AQAD Director
Lewis Weinstock Date
U.S. Environmental Protection Agency
Ambient Air Monitoring Group Leader
Michael Jones Date
U.S. Environmental Protection Agency
Program Manager
Dennis Mikel Date
U.S. Environmental Protection Agency
Quality Assurance Program Coordinator
Joseph Elkins Date
U. S. Environmental Protection Agency
OAQPS Quality Assurance Manager
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Acknowledgement
This Quality Assurance Project Plan (QAPP) was developed internally by EPA's Office of Air Quality Planning and
Standards (OAQPS), Region 3 and Region 4. Additional material and text were provided by EPA's Urban Air
Toxics Monitoring Program Contractor; Eastern Research Group (ERG). Text provided by ERG is noted throughout
the document. For more information on ERG's or its subcontractor's QAPP or procedures, contact ERG directly at
919-468-7800 or by email at http://www.erg.com/contact/res.htm.
This QAPP was generated using the EPA QA regulations and guidance as described in EPA QA/R-5, EPA
Requirements for Quality Assurance Project Plans and the accompanying document, EPA QA/G-5, Guidance for
Quality Assurance Project Plans. This is a Category II QAPP, is structured as such and has all pertinent elements of a
Category II QAPP, as suggested by the R-5 document. The R-5 guidance on developing QAPPs can be found at
http://www.epa.gov/qualitv/qa docs.html
For questions or comments please contact:
Dennis Mikel EPA-OAQPS-AQAD at mikel.dennisktgjepa.gov or 919-541-5511
Mike Jones, EPA-OAQPS-AQAD at jones.michael(@,epa.gov or 919-541-0528
Lewis Weinstock, EPA-OAQPS-AQAD at weinstock.lewis(@,epa.gov or 919-541-3661
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Acronyms and Abbreviations
APCD
ANSI
AQS
ASTM
CAA
CFR
CoC
CV
DAS
DNPH
DQA
DQOs
ECHO
EDO
EPA
ERG
GC/MS
GIS
GPS
HAPs
HPLC
ICP/MS
ISO
IUPAC
IO
LAN
LIMS
MDL
MQOs
NATA
NATTS
NIOSH
NIST
NWS
OAQPS
OSHA
PAH
PC
PD
PM10
PT
QA/QC
QA
Air Pollution Control or Management District
American National Standards Institute
Air Quality System
American Society for Testing and Materials
Clean Air Act
Code of Federal Regulations
chain of custody
coefficient of variance
data acquisition system
di-nitro phenyhydrazine
data quality assessment
data quality objectives
electron capture - hall detector
environmental data operation
Environmental Protection Agency
Eastern Research Group
gas chromatography/mass spectrometry
geographical information systems
geographic positioning system
hazardous air pollutants
high pressure liquid chromatography
ion coupled plasma/mass spectrometry
International Standards Organization
International Union of Pure and Applied Chemists
in-organic
local area network
laboratory information management system
minimum detection limit
measurement quality objectives
National Air Toxics Assessment
National Air Toxics Trends Stations
National Institute of Occupational Safety and Health
National Institute of Standards and Technology
National Weather Service
Office of Air Quality Planning and Standards
Occupational Safety and Health Administration
polycyclic aromatic hydrocarbons
personal computer
percent difference
particulate matter - 10 microns
proficiency testing
quality assurance/quality control
quality assurance
111
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Acronyms and Abbreviations
QAFR
QAM
QAPP
QC
RSEI
SATMP
S/L
SOP
TAD
TO
TSA
TSP
UATMP
uv
voc
quality assurance final report
quality assurance manager
quality assurance project plan
quality control
Risk-Screening Environmental Indicators
School Air Toxics Monitoring Program
State/Local
standard operating procedure
technical assistance document
toxic organic
technical system audit
total suspended particulates
Urban Air Toxics Monitoring Program
ultra-violet
volatile organic compound
IV
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Tables
Number Description Page No.
4-1 List of Methods and Target Analytes 7
5-1 Assessment Schedule 10
5-2 Schedule of Critical SATMP Activities 11
6-1 MQOs for Metals 19
6-2 MQOs for VOCs 19
6-3 MQOs for other compounds 20
7-1 SATMP Data and Records Storage 21
8-1 Scheduled Monitoring Activities 23
9-1 List of Target Analytes 26
9-2 Sample Setup, Run and Recovery Dates 27
9-3 Field Supplies 28
9-4 Temperature Requirements 30
9-5 Holding Times 30
12-1 Sample Invalidation Criteria for Collocated Data 44
13-1 Inspections in the Laboratory 46
17-1 Assessment Summary 58
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Figures
Figure No. Description Page No.
3-1 Overall Structure of the SATMP 1
10-1 UATMP Sample Data Sheet 32
10-2 Canister Tag 33
10-3 Carbonyl Chain of Custody Form 34
VI
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2.0 Table of Contents
Section Page
1.0 Signature Page I
Acknowledgement -
Acronyms and Abbreviations
List of Tables v
List of Figures
2. 0 Table of Contents vii
3.0 Project/Task Organization j
3. IRoles and Responsibilities ^
3.2 Sampling Frequency, Duration, and Quantity 4
4.0 Problem Definition/Background 5
4.1 Problem Statement and Background 5
4.2 Project Monitoring Design ^
4.3 Locations of Interest for the SATMP 7
5.0 Project Task/Description g
5.1 Overview of Field Activities g
5.2 Overview of Laboratory Activities 9
5.3 Project Assessment Techniques JQ
5.4 Schedule of Activities ^ Q
6. 0 Data Quality Objectives ^3
6.1 The DQO Process 13
6.2 State the Problem 14
6.3 Identify the Decision ^
6.4 Identify the Inputs to the Decision ^
6.5 Define the Study Boundaries ^
6.6 Develop a Decision Rule ^
6.7 Specify Tolerable Limits on the Decision Errors ^
6.8 Optimize the Design for Obtaining Data ^
6.9 DQOs for the SATMP
17
vii
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Section Page
7.0 Documentation and Records 21
7.1 Routine Record Data Activities 21
7.2 EPA Data and Document Control 22
7.3 Data Report, Archiving and Retrieval 22
8.0 Sampling Design 23
8.1 Scheduled Project Activities, Including Measurement Activities 23
8.2 Rationale for the Design 23
8.3 Design Assumptions 24
8.4 Procedure for Locating and Selecting Environmental Samples 25
8.5 Classification of Measurements as Critical/Noncritical 25
9.0 Sampling Methods Requirements 26
9.1 Purpose/Background 26
9.2 Sample Collection and Preparation 26
9.3 Support Facilities for Sampling Methods 27
9.4 Sampling/Measurement System Corrective Action 2g
9.5 Sampling Equipment, Preservation, and Holding Time 29
10. Sample Handling and Custody ^\
10.1 Sample Custody 31
10.2 Carbonyl Sample Custody 33
10.3 Sample Custody for other HAPs 35
10.4 Analytical Laboratory Data 35
10.5 Sampling Monitoring Data 35
11.0 Analytical Methods Requirements 26
11.1 VOC Canister Analysis and Cleanup System 26
11.2 Analysis of PAH using EPA Compendium TO-13 A 38
11.3 Metals Using ICP/MS 38
11.4 Hexavalent Chromium 3o
11.5 Diisocyanates 3g
11.6 4,4 Methylene dianiline 40
11.7 Carbonyls 40
vin
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Section Page
12. 0 Quality Control Requirements 4^
12.1QC Procedures 41
13.0 Instrument/Equipment Testing, Inspection, and Maintenance 45
13.1 Purpose/Background 45
13.2 Testing 45
13.3 Inspection 45
13.4 Maintenance 4^
14.0 Instrument Calibration and Frequency 4^
14.1 Analysis of Instruments - Laboratory 4g
14.2 Field Calibrations 49
14.3 Calibration Method 49
14.4 Calibration Standard Materials and Apparatus ^Q
15.0 Data Acquisition Requirements 52
15.1 Acquisition of Non-Direct Measurement Data 52
16.0 Data Management 54
16.1 Background and Overview 54
16.2 UATMP Contract Data Management 54
16.3 Data Tracking ^
16.4 EPA Data Reporting Requirements ^
16.5 EPA OAQPS Data Management 57
17.0 Assessment and Response to Action ^
17.1 Project Planning and Assessment Activities 59
18.0 Reports to Management gj
18.1QA Final Report 61
19.0 Data Review 62
19.1 Data Review Design ^2
19.2 Data Review 63
19.3 Data Verification
63
19.4 Data Reduction, Validation and Reporting ^4
x
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Section Page
20.0 Data Validation, Verification and Analysis ^
20.1 Process for Validating and Verifying Data ^
20.2 Data Analysis 65
21.0 Reconciliation with Data Quality Objectives ^7
21.1 Reconciling Results with DQOs 67
21.2 Five Steps of DQA Process 67
Appendix A: Schools Air Toxics Ambient Monitoring Plan, dated April 2,2009
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3.0 Project/Task Organization
3.1 Roles and Responsibilities
EPA's Office of Air Quality Planning and Standards (OAQPS) and the EPA Regional Offices
are responsible for developing and implementing the Schools Air Toxics Monitoring Program
(SATMP) with its partners in the State air agencies or Local (S/L) Air Pollution Control or
Management Districts (APCDs). The S/L APCDs and EPA Regional Offices are also
responsible for implementing the deployment and operation of monitors and, in some cases, the
laboratory analysis of samples for the program. It is the responsibility of both EPA and the
States and Local APCDs to assess the quality of the data and take corrective action when
appropriate. The responsibilities of each organization are addressed here. Figure 3-1 represents
the organizational structure of the SATMP.
Laboratory
Subcontractor
Figure 3-1 Overall Structure of the SATMP
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3.1.1 Office of Air Quality Planning and Standards
EPA OAQPS is charged under the authority of the Clean Air Act (CAA) to protect and enhance
the quality of the nation's air. OAQPS sets national emissions standards for air toxics by
industry group, and works with states and local agencies to monitor these pollutants which are
considered harmful to public health or welfare. OAQPS evaluates the need to regulate potential
air pollutants, especially air toxics, and develops national standards and works with S/L APCDs
to develop plans implement for meeting these standards.
Here are some of the roles and responsibilities for OAQPS in the SATMP;
Take the lead role in implementing the program;
Establish "a cross-Agency strike team" to implement the program;
Examine available information from external and internal sources to create the list of
schools that require monitoring;
Ensure that the methods and procedures used in making air pollution measurements are
adequate to meet the programs objectives and that the resulting data are of satisfactory
quality;
Communicate technical information to the Regions and the S/L APCDs;
Provide up-front support (i.e., equipment acquisition and procure laboratory support);
Evaluate the performance, through Technical Systems Audits (TSAs) of laboratories
making air pollution measurements;
Render technical assistance to the EPA Regional Offices and air pollution monitoring
community; and,
Provide analysis and interpretation of the results and communicate those results to the
EPA Administrator and the public at large.
3.1.2 EPA Regional Offices
The EPA Regional Offices will address environmental issues related to the States within their
jurisdiction and administer the program. The major quality assurance (QA) responsibilities of
EPA's Regional Offices, in regards to the SATMP, are the coordination of field and in some
cases the laboratory quality control (QC) and QA matters at the Regional levels with the S/L
agencies. The EPA Regional Offices are responsible for some of the technical aspects of the
program including:
Reviewing and guiding the program goals;
Reviewing and developing the QAPP;
Evaluating quality system performance, through TSAs (if needed) and network siting and
reviews; and,
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Acting as a liaison by making available the technical and quality assurance information
developed by EPA Headquarters and the Region to the S/L APCDs, and making EPA
Headquarters aware of any the unmet quality assurance objectives.
3.1.3 States and Local APCDs
The major responsibility of S/L APCDs is the implementation of a satisfactory monitoring
program, which would naturally include the implementation of an appropriate QA/QC program.
It is the responsibility of S/L agencies to implement QA/QC programs in the field portion of this
program, in their own laboratories, if utilized, and in any consulting and contractor laboratories
which they may use to obtain data or information. Here is a list of some of the responsibilities
of the S/L APCDs;
Work closely with EPA OAQPS/Regional staff and school staff to site the monitoring
stations;
If utilized, procure laboratory services to analyze the data;
Receive and inspect unexposed samples to make sure they are ready for sampling;
Operate the monitoring samplers according to the schedule stated in this QAPP;
Ship the exposed samples to the laboratory performing the analysis;
Participate in the screening and analysis of the data, and;
In co-ordination with EPA, communicate with the schools and public about the results;
and,
Follow the field approved field SOPs when operating monitors.
3.1.4 Laboratory Contractor
The SATMP requires that air toxic samples be analyzed in accordance to strict QA/QC
requirements as defined in Section 6.9. At this time, the EPA recommends that all samples be
analyzed by OAQPS' Urban Air Toxics Monitoring Program (UATMP) contract laboratory. It
is possible that several S/L APCDs may decide to analyze the samples with the laboratories
under their jurisdiction. If this is the case, then the S/L laboratories must meet the requirements
as stated in Section 68 Demonstration of their ability to be able to meet the Measurement
Quality Objectives (MQOs) is required before S/L agencies can analyze samples for this
program. OAQPS will review each laboratory's capabilities on a case by case basis. S/L
laboratories will participate in an independent laboratory Technical System Audit (TSA)
and analyze Proficiency Testing (PT) samples before analysis can be performed for this
program.
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Here is a partial list of the laboratory duties:
Sending sample containers/filters to the field operators, following strict requirements on
shipping and handling according to their Standard Operating Procedure (SOPs);
Receiving samples from the field;
Analyzing the samples relative to their QA/QC procedures and SOPs;
Performing data validation procedures on the data;
Troubleshooting and repairing any laboratory instruments that malfunction; and,
Reporting all data to EPA as required.
The UATMP contractor does not have the ability to do certain analyses, such as the
Diisocyanates and 4, 4 Methylene dianiline, which are discussed later. Therefore, the UATMP
contractor will subcontract these analyses. Samples that must be analyzed by the subcontractor
will be shipped directly to the subcontract laboratory to expedite the analyses. It is the UATMP
contractor's responsibility to get data and information from the subcontractor in a timely
manner and to maintain adherence to required chain of custody and other procedural
requirements.
3.2 Sampling Frequency, Duration, and Quantity
Ambient air sampling shall be conducted on a 1 in 6 day schedule, details of which must be
coordinated with the EPA and national contract laboratory. Start dates will vary by site as a
function of monitoring setup completion. Once monitoring operations have commenced, the
base (i.e., minimum duration) sampling period is 60 days; given a 1 in 6 sampling schedule, the
base sampling period is intended to result in 10 valid samples. There may be cases in which the
60 day sampling period is deemed to be insufficient (e.g., invalidated sample(s), insufficiently
representative data, etc.) and thus extended, typically not to exceed a total duration of 90 days.
A companion document to this QAPP, the "Schools Air Toxics Ambient Monitoring Plan,
dated April 14, 2009" (hereby known as The Monitoring Plan) has detailed information in
section 3.2. The S/L APCDs are authorized to collect up to three additional random samples
that will be set and run at the discretion of the S/L APCDs. Details on this are also in Section
3.2 of the Monitoring Plan.
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4.0 Problem Definition/Background
4.1 Problem Statement and Background
4.1.1 Introduction
EPA will monitor air quality at a number of schools as part of an initiative to understand
whether outdoor toxic air pollution poses health concerns to schoolchildren. This quality
assurance plan addresses one aspect of the initiative; ambient air monitoring.
EPA developed a list of priority schools for an initial round of monitoring that is expected to
last a minimum of 60 days. The agency selected the schools using EPA's National Scale Air
Toxics Assessment (NATA), results from a USA Todayฎ analysis, which is based on EPA's
Risk-Screening and Environmental Indicators (RSEI) model and after consulting with state and
local air agencies.
4.1.2 Project Objectives
This ambient air monitoring exercise will yield data of sufficient quality that allow a
preliminary assessment of any potential air toxics impacts specific to the school at which the
monitoring occurred. This preliminary assessment will be used to determine subsequent steps
that may include:
1) Terminating monitoring where assessments indicate low impacts,
2) Pursuing long-term emission and risk reduction activities (such as enforcement or
other actions) where monitoring data show potentially unacceptable impacts, or
3) Considering longer-term monitoring where initial data are inclusive and additional
information is needed to better characterize the potential for impacts
4.2 Project Monitoring Design
4.2.1 Meteorological Measurements
Site specific meteorological parameters that will be measured consist of wind speed and
direction data. The type of sensor provided will be of sufficient quality for its intended use.
OAQPS is purchasing sonic anemometers and data acquisition systems that will be able to
collect both scalar and vector data. Meteorological information is gathered from the National
Weather Service (NWS) stations across the nation. Parameters include: temperature, relative
humidity, barometric pressure, rainfall, wind speed, wind direction, cloud type/layers, cloud
cover and visibility range. OAQPS staff will retrieve data on temperature and rainfall from
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NWS sites near the schools being monitored, to supplement the at-school wind speed and wind
direction data for purposes of interpreting the air quality monitoring results.
4.2.2 Hazardous Air Pollutants
There are currently 187 hazardous air pollutants (HAPs) and pollutant classes that are regulated
under the Clean Air Act (CAA). These pollutants, often called air toxics, have been associated
with a wide variety of adverse health effects, including cancer, neurological effects,
reproductive and developmental effects. Air toxics are emitted from multiple sources, including
major stationary, area, and mobile sources, resulting in population exposure to these air toxics
as they occur in the environment. While in some cases the public may be exposed to an
individual HAP, people more typically experience exposures to multiple HAPs from many
sources.
Table 4-1 lists the "classes" of compounds that will be measured in the SATMP. For more
information on the instruments that will be used to collect these samples, please see
Table 4-1 lists the analytes by chemical class or group. Current information indicates that
specific pollutants in these groups may be present at the schools. While we are focusing our
effort on monitoring for specific pollutants, the measurement methods used for certain classes
of pollutants will detect other chemicals as well. For instance, under the class of compounds
known as "VOCs," benzene is a pollutant that may be present at certain schools. When the
laboratory performs the analysis for benzene, there are a number of other compounds that can
be analyzed, such as 1, 3 butadiene. This situation exists for the other classes of compounds as
well. We will report concentrations for all chemicals detected.
The Monitoring Plan has the full list of compounds that will be evaluated by the methods
chosen by this program. Please note that the pollutants of interest for this program are listed in
Section 6.9, Tables 6-lthrough 6-3.
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Target Analytes
VOCs
Carbonyls
PM10/TSP HAP Metals
Hexavalent Chromium
PAHs
4,4 Methylene dianiline
Diisocyanates
Meteorology
Method
EPA TO- 15
EPATO-11A
EPAIO-3.5
EPA-modified CARB 039
TO-13A
NIOSHNo. 5029
OSHA No. 42
Sonic Anemometry
Sampling Media
Air (via canister)
DNPH-coated silica gel cartridge
47mm Teflon and 8" x 10"quartz filters
47mm acid-washed sodium bicarbonate
impregnated cellulose filter
PUF / XAD-2
Sulfuric acid treated glass fiber filter
glass fiber filter coated with
1 -(2-pyridyl)piperazine
Wind speed and direction scalar and vector
data
Table 4-1 List of Methods and Target Analytes
4.3 Locations of Interest for the SATMP
As stated in the introduction of this section, the main goal of the SATMP is to monitor for
specific compounds in the outdoor air around the listed schools.
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5.0 Project Task/Description
The measurement goal of the SATMP is to estimate the concentration, in standard units of
micrograms per cubic meter (ug/m3) and parts per billion/volume (ppbv) of air toxic compounds
of particulates and gases at the listed schools. This is accomplished by several separate
collection media and analytical techniques. Activities for this program are divided into two
separate, yet linked activities: field monitoring and laboratory analysis. An overview of the
program follows.
5.1 Overview of Field Activities
Ambient air sampling devices will be placed at secure monitoring locations on or near schools.
Table 4-1 lists the methods and sampling media used for this program. The Monitoring Plan has
the instrument specifications necessary for this program. Appendix A of the Monitoring Plan
lists the schools and the pollutants to be monitored. In most cases, the sampling will occur for
24 hours +/- 1 hour, with the exception of Diisocyanates and 4, 4 Methylene dianiline. The
schedule and timing are discussed in detail in Section 9.2.2 of this QAPP.
All of the instruments operated in the field are vendor supplied. The samplers utilized for this
program are similar to the instruments described in the Reference Section at the end of this
chapter. All of the equipment will be supplied by vendors that specialize in manufacturing these
collection devices.
Training - EPA is partnering with experienced S/L APCDs to conduct the ambient monitoring
aspect of the school air toxics program. EPA expects that monitoring agencies will assign
experienced personnel to operate sampling equipment, and that each agency's prior experience
in operating similar criteria pollutant and/or air toxics monitors will provide adequate training to
ensure proper operation of equipment during this program. EPA will survey participating
monitoring agencies (through Regional Office contacts) to confirm availability of trained
personnel, and will support individualized training needs as appropriate, coordinated through
visits by Regional Office or Laboratory personnel. In addition and prior to the commencement
of sampling, EPA will support one or more monitoring-focused national conference calls to
provide opportunities for agency's to ask clarifying questions and to ensure a common
understanding of procedural requirements and expectations.
Standard Operating Procedures (SOPs) - EPA will provide field SOPs for each of the
methods being deployed in the schools monitoring program, complimenting the existing
laboratory SOPs that have been developed by EPA's analysis contractor. Field SOPs will be
completed once the exact type(s) of samplers being procured is established through the
contractual process. At that time, field SOPs will be distributed to participating agencies and
one or more conference calls will be supported to ensure a complete understanding of the
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requirements by the individual site operators. EPA personnel will be available throughout the
duration of the study to answer site-specific questions and/or handle other operational issues
that may arise that may not be specifically described in the field SOPs.
5.2 Overview of Laboratory Activities
Laboratory activities for the SATMP include preparing the samples, shipping/receiving, and
analysis. Here some activities associated with these phases.
Pre-Sampling
Receiving filters, canisters or cartridges from the vendors;
Checking sample integrity;
Conditioning filters, storing canisters and cartridges;
Storing samples prior to field use;
Packaging filters, canisters and cartridges for field use;
Associated QA/QC activities;
Maintaining analytical equipment at specified environmental conditions; and;
Equipment maintenance and calibrations.
Shipping/Receiving
Receiving filters, canisters and cartridges from the field and logging into database;
Storing filters, canisters and cartridges; and,
Associated QA/QC activities.
Post-Sampling
Checking filter, cartridge and canister integrity and assigning unique codes;
Extract! on of VO C s from cani sters;
Extraction of Teflon, quartz and glass fiber filters;
Extraction of Di-nitro phenyl-hydrazine (DNPH) bound compounds;
Extraction of Polyurethane Foam (PUF) and XAD-2 resin;
Analysis of samples extracted;
Data entry/upload to the Air Quality System (AQS) database;
Storing filters/archiving;
Cleaning canisters; and,
Associated QA/QC activities and data reporting.
The details for these activities are included in various sections of this document, the laboratory
SOPs, and References 1- 8.
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5.3 Project Assessment Techniques
An assessment is an evaluation process used to measure the performance or effectiveness of a
system and its elements. For this program, assessment is used to denote any of the following
activities: Network Siting and Review, Proficiency Testing (PT) and Technical System Audits
(TSAs). Section 17 will discuss the details of the SATMP assessments.
Table 5.1 provides information on the parties implementing the assessment and their frequency.
Assessing Agency
EPA
EPA
Regional Offices
Type of Assessment
PTs
TSAs
Network Siting and Review
Agency Assessed
UATMP
Laboratory and
their subcontract lab
UATMP
Laboratory and
their subcontractor
S/L agencies
Frequency
At the
beginning of
the program
At the
beginning of
the program
At the
beginning of
the program
Table 5-1 Assessment Schedule
5.4 Schedule of Activities
Table 5-2 contains a general list of the activities that will occur during this program. Please
note that the dates of these activities may change due to unforeseen circumstances. However,
this is the general timeline for this program.
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Activity
Evaluate the USA Todayฎ
Network List
Development of the EPA
Network List
EPA Network List Finalized
DQO Process Performed
QAPP Development
Monitoring Plan Development
Lab Services Procured
Sampler siting/testing
QAPP Finalized
Field Training
Sampling Begins
Laboratory Analysis Begins
Sampling Ends
Data Analysis Phase Begins
Due Date
February 2009
February 2009
March 2009
March 2009
March 2009
March 2009
March 2009
April 2009
April 2009
April - May 2009
April- May 2009
April-May 2009
July -August 2009
July 2009
Comments
List evaluation.
List of candidate schools developed considering USA Todayฎ)
analysis, NATA results, TRI data, and information from S/L
agencies.
List vetted through internal and S/L channels.
Monitoring, Analysis staff convene to develop DQOs.
Input taken and incorporated into official document.
Monitoring Plan vetted through official channels.
UATMP services in place for receiving samples.
Establishment of sites and preliminary testing of samplers.
QAPP finalized and submitted to S/L agencies.
Field and laboratory training activities and certification.
Sampler testing completed and media shipped to monitoring
locations.
Samples received and analysis begins.
If 100% data capture is obtained, samplers are shut down.
Data loaded into AQS database and data are accessible to analytical
team.
Table 5-2 Schedule of Critical SATMP Activities
References:
1. Compendium Method for the Determination of Inorganic Compounds in Air, United States
Environmental Protection Agency, June 1999, Section IO-3.5
http://www.epa.gov/ttn/amtic/inorg.html
2. Compendium Method for the Determination of Toxic Organic Compounds in Air, United States
Environmental Protection Agency, Section TO-15, January 1999
http://www.epa.gov/ttn/amtic/airtox.html
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3. Compendium Method for the Determination of Toxic Organic Compounds in Air, United States
Environmental Protection Agency, Section TO-11A, January 1999
http://www.epa.gov/ttn/amtic/airtox.html
4. OSHA Method 42, http://www.osha.gov/dts/sltc/methods/organic/org042/org042.html
5. NISOH Method 5029: http://www.cdc.gov/Niosh/nmam/pdfs/5029.pdf
6. Compendium Method for the Determination of Toxic Organic Compounds in Air, United States
Environmental Protection Agency, Section TO-13A, January 1999
http://www.epa.gov/ttn/amtic/airtox.html
7. Standard Operating Procedure for the Determination of Hexavalent Chromium in Ambient Air
Analyzed by Ion Chromatography (1C) developed for US EPA by Eastern Research Group,
http://www.epa.gov/ttn/amtic/airtox.html
8.Quality Assurance Handbook for Air Pollution Measurement Systems - Volume IV:
Meteorological Measurements Version 2.0, 2008, http://www.epa.gov/ttn/amtic/met.html
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6.0 Data Quality Objectives
The primary objective of the project is as follows:
The primary objective for this project is to collect information on ambient air concentrations
of target compounds at a targeted list of schools in the United States during a defined
monitoring period. This monitoring information will be used to assist us in identifying:
(1) Locations impacted by nearby industrial or urban sources where actions to reduce
ambient concentrations are needed.
(2) Locations where measured ambient concentrations do not indicate impacts of
potential concern and no further monitoring is needed,
(3) locations where additional information, including additional monitoring, is needed in
order to inform such a decision or for other longer-term objectives related to more
fully characterizing ambient concentrations and potential source influences in the
area,
To do this work, EPA along with its S/L APCDs partners, will collect ambient air data at the
identified schools. For some schools, the focus will be on assessing impacts associated with
nearby industrial sources. Other schools are identified for potential impacts associated with a
mix of typical urban sources (e.g., large and small stationary sources, mobile sources).
This effort will also provide information to residents that live nearby the schools with regard to
potential air toxics concerns from nearby industrial or urban sources.
The DQO process described in EPA's QA/G-41 document provides a general framework for
ensuring that the data collected by EPA or any Environmental Data Operation (EDO) meets the
needs of the intended decision makers and data users. The process establishes the link between
the specific end use(s) of the data with the data collection process and the data quality (and
quantity) needed to meet a program's goals. The following sections provide the required
information for the DQO process.
6.1 The DQO Process
This section presents an overview of the seven steps in EPA's QA/G-4 DQO process as applied
to the objectives of this project. The purpose of this section is to provide a general discussion of
the specific issues that were used in developing the DQOs for this project.
The DQO process is a seven-step process based on the scientific method to ensure that the data
collected by EPA meet the needs of its data users and decision makers in terms of the
information to be collected and, in particular, the desired quality and quantity of data. It also
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provides a framework for checking and evaluating the program goals to make sure they are
feasible and that the data are collected efficiently. The seven steps are usually labeled as:
State the Problem
Identify the Decision
Identify the Inputs to the Decision
Define the Study Boundaries
Develop a Decision Rule
Specify Tolerable Limits on the Decision Errors
Optimize the Design for Obtaining Data
Each of these elements is discussed in detail below. The pollutant specific outcomes of the
DQO process are contained in Section 6.9.
6.2 State the Problem
The EPA project team developed the following problem statement:
Information about air toxics has raised questions about outdoor air quality around some schools
in the U.S. Some of the schools are near large industries while some schools are in urban areas,
where emissions of air toxics come from a mix of large and small industries, cars, trucks, buses
and other sources. Measuring the levels of toxics in the air around the schools will help EPA
understand whether that air quality poses any health concerns. EPA will use what it learns from
this monitoring initiative to determine its next steps.
6.3 Identify the Decision
The decision statement should provide a link between the principal study question and possible
actions. The decision that the monitoring at these sites is intended to inform is as follows:
Data will be collected from selected schools based on information developed by or made
available to the EPA. Monitoring will be performed in such a way that the resulting data will be
sufficient in terms of quantity and quality to better inform our understanding of chronic air
toxics concentrations in the ambient air at these schools and the influence of nearby sources.
These data along with other information pertaining to air toxics at these locations will be relied
upon by EPA to identify:
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(1) locations impacted by nearby industrial or urban sources where actions to reduce
ambient concentrations are needed to address levels of potential public health concern;
(2) locations where further action is not needed at this time.
(3) locations where additional information, including additional monitoring, is needed in
order to inform such a decision or to help us better characterize the impact of ambient
concentrations and potential sources in the area; and
6.4 Identify the Inputs to the Decision
This section discusses the variety of inputs that are needed to make the final DQO decision for
this program. The pollutants of particular interest are listed in Tables 6-1 through 6-3. The
Monitoring Plan lists other compounds that the laboratory will report that are also measured by
the analytical methods employed. The statements included here apply implicitly to this full list
of analytes. Identical analytical methods will be used by all labs participating in the program,
therefore, overall precision, bias and detectability will be similar across all labs.
In addition to the monitoring results, other inputs potentially important to decision-making for
this project include, but not limited to, the following items (not listed in any priority order):
1. List of target schools, and target compounds;
2. Existing ambient air sampling methods and analytical techniques;
3. NATA estimates;
4. Source-specific emission inventory information;
5. Existing ambient monitoring data
6. Nearby meteorological monitoring data from the National Weather Service or
local airport weather data;
7. Topographical information pertaining to factors influencing pollutant transport;
8. Health effects information, including dose-response values and information
available on the OAQPS and ATSDR web sites;
9. Community concerns;
10. Historical monitoring, modeling, health assessments, and other information
(e.g., compliance status, voluntary emissions reduction programs, etc.) for the
area; and,
11. Funding Information.
6.5 Define the Study Boundaries
The specific location of the monitors should be established to represent ambient air in the
proximity of the school, as described in the Monitoring Plan. Ideally, monitors should be
located on the school grounds or roof of one a school buildings Siting criteria that are detailed
in Code of Federal Regulations (CFR) Chapter 40 Section 58, Appendix E2 will be followed to
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the extent that is practical, as described in the Monitoring Plan. All monitoring stations will be
located within the U.S.
6.6 Develop a Decision Rule
The decision rule is an "if... then" statement for how the various alternatives will be chosen.
If the ambient air monitoring data in combination with other information for a
school indicate the need for action to reduce air concentrations of air toxics,
then EPA will work with the S/L agencies on options for such actions in outdoor
air. If the available monitoring data and other information are insufficient to
support a conclusion in this regard, then additional data collection will be
pursued. If the available monitoring data and other information are sufficient to
reach a conclusion regarding the need for further action and do not support the
conclusion that further action is needed, then additional data collection will not
be pursued.
6.7 Specify Tolerable Limits on the Decision Errors
Budgetary constraints are a consideration in describing the DQOs. The program has a finite
budget that affects the amount of monitoring performed in this program. The initial monitoring
will include 10 samples collected on a l-in-6 day schedule. It was decided that on-site
measurements will include meteorological data such as wind direction and wind speed to help
inform our consideration of this issue. At sites where the suspected impacts are associated with
a particular source(s), the monitoring data set will need to include samples taken when the
predominant wind direction is generally from the sources in question in order to fully support
the decision making process contemplated in this exercise.
In order to understand other aspects of the quality of the data (i.e., precision and bias) the
precision estimates of each method was based on the estimates from EPA's contract laboratory
for the UATMP and other method estimates and is expressed in terms of coefficient of variance
(CV). The bias was chosen from the National Air Toxics Trends Stations (NATTS) estimates2.
The NATTS is a long term (six-year) trends program that has been in operation since 2004.
Data from proficiency testing of the laboratories within the NATTS illustrated that bias can be
controlled within 25%. Data completeness (10 samples collected over a 60 - 90 day period) will
be set at 100%. If, due to unforeseen events, 10 samples are not collected in 60 days,
monitoring will continue until 10 samples are collected. Thus, 100% completeness will be
achieved. The established minimum detection limits (MDLs) will be met in order to evaluate
the resulting data in a health-based context. The MDLs are generally set at or below the
concentrations of individual air toxics for which a lifetime, continuous exposure would pose an
excess lifetime cancer risk of one-in-one million or a hazard quotient of 0.1. Note: for a small
number of chemicals, the laboratory analytical methodology may be insufficient to achieve such
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an MDL. Where the level of the MDL substantially limits our interpretation with regard to
potential significance of health risk-related impacts, this will be recognized in reporting and
interpreting the results.
6.8 Optimize the Design for Obtaining Data
The team decided that due to resource constraints, and to compare study data with other data
collected within the U.S. (e.g., through the NATTS program; sampling would will follow a "one
every six days" schedule. A program goal of 100% data completeness is established for the
initial monitoring (60 - 90days) since this is a short-term program and the number of samples
initially collected will be small. However, if the wind does not come from the direction of the
sources of interest impacting the school, then the need for additional monitoring may be
indicated in order to evaluate the significance of source contributions. Monitoring agencies are
authorized to collect up to three additional random samples that will be set and run at the
discretion of the S/L APCD. Details on this are in Section 3.2 of the Monitoring Plan.
6.9 DQOs for the SATMP
This section combines all of the information gathered and states the action that will be followed
given the scenarios that can occur.
In order to better evaluate potential impacts of air toxics at some schools in the U.S.,
monitoring will commence at selected locations. If the following criteria are met, the data will
be considered of sufficient quantity and quality for the decision-making to commence as
described in section 6.3:
(1) Data are collected with a coefficient of variance (precision) and bias as stated in
Tables 6-1 through 6-3;
(2) Data completeness is 100% or 10 samples within a window of 60 90 days;
(3) MDLs are at or below those specified in Tables 6-1 through 6-3 and;
(4) Where applicable, sufficient samples are collected when the predominant wind
direction is from the source(s) in question.
Once a DQO is established, the quality of the data must be evaluated and controlled to ensure
that it is maintained within the established acceptance criteria. Measurement Quality Objectives
(MQOs) are designed to evaluate and control various phases (i.e., sampling, preparation, and
analysis) of the measurement process to ensure that total measurement uncertainty is within the
range prescribed by the DQOs. The MQOs can be defined below:
Precision - a measure of mutual agreement among individual measurements of the same
property usually under prescribed similar conditions. This is the random component of error.
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Precision is estimated by various statistical techniques using some derivation of the standard
deviation.
Bias - the systematic or persistent distortion of a measurement process which causes error in
one direction. Bias will be determined by estimating the positive and negative deviation from
the true value as a percentage of the true value.
Representativeness - a measure of the degree which data accurately and precisely represent a
characteristic of a population, parameter variations at a sampling point, a process condition, or
an environmental condition.
Comparability - a measure of confidence with which one data set can be compared to another.
Completeness - a measure of the amount of valid data obtained from a measurement system
compared to the amount that was expected to be obtained under correct, normal conditions.
Detectability- the determination of the low range critical value of a characteristic that a method
specific procedure can reliably discern.
In theory, if these MQOs are met, measurement uncertainty should be controlled to the levels
required by the DQO. Tables 6-1 through 6-3 list the MQOs for pollutants of concern that will
be measured for this program. More detailed descriptions of these MQOs and how they will be
used to control and assess measurement uncertainty will be described in this QAPP. Data
within these tables reflect the MQOs needed to meet the DQOs for this program. As stated in
Section 3.1.5, every laboratory that participates in this program must demonstrate their
ability to be able to meet the MQO before the lab can analyze samples for this program.
OAQPS will review each laboratory's capabilities on a case by case basis.
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Pollutant
Group
Metals
Metals
Metals
Metals
Metals
Compound
Arsenic
Cobalt
Lead
Manganese
Nickel
Reporting
Units
ug/m3
ug/m3
ug/m3
ug/m3
ug/m3
Precision
(CV)3
20%
20%
20%
20%
20%
Bias2
25%
25%
25%
25%
25%
Representativeness
Micro, Middle,
and/or
Neighborhood Scale
Micro, Middle,
and/or
Neighborhood Scale
Micro, Middle,
and/or
Neighborhood Scale
Micro, Middle,
and/or
Neighborhood Scale
Micro, Middle,
and/or
Neighborhood Scale
Comparability/
Method Selection
ICP-MS/IO-3.5
ICP-MS/IO-3.5
ICP-MS/IO-3.5
ICP-MS/IO-3.5
ICP-MS/IO-3.5
Completeness
10 samples
10 samples
10 samples
10 samples
10 samples
Minimum
Detection
Limits4
9.2 E-06
5.5 E-06
5.6 E-05
5.7E-05
1.3 E-04
Table 6-1 MQOs for Metals
Pollutant
Group
VOCs
VOCs
VOCs
Compound
Acrolein
1,3-
Butadiene
Benzene
Reporting
Units
ug/m3
ug/m3
ug/m3
Precision
(CV)3
30%
30%
30%
Bias2
25%
25%
25%
Representativeness
Micro, Middle,
and/or
Neighborhood Scale
Micro, Middle,
and/or
Neighborhood Scale
Micro, Middle,
and/or
Neighborhood Scale
Comparability/
Method Selection
GC-MS/TO-15
GC-MS/TO-15
GC-MS/TO-15
Completeness
10 samples
10 samples
10 samples
Minimum
Detection
Limits4
3.5 E-02
6.0 E-03
2.0 E-02
Table 6-2 MQOs for VOCs
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Pollutant
Group
Individual
Pollutant
PAH
PAH
Diisocyanates
Diisocyanates
Diisocyanates
Metal
Carbonyl
Compound
4,4'-
Methylene-
dianiline
Benzo (a)
pyrene
Naphthalene
2, 4 TDI
MDI
1,6 HDI
Chromium
(VI))
Acetaldehyde
Reporting
Units
ug/m3
ug/m3
ug/m3
ug/m3
ug/m3
ug/m3
ug/m3
ug/m3
Precision
(CV)
25%5
25%3
20%3
25%5
25%5
25%5
20%3
25%3
Bias
25%5
25%5
25%5
25%5
25%5
25%5
25%5
25%2
Representativeness
Micro, Middle,
and/or
Neighborhood Scale
Micro, Middle,
and/or
Neighborhood Scale
Micro, Middle,
and/or
Neighborhood Scale
Micro, Middle,
and/or
Neighborhood Scale
Micro, Middle,
and/or
Neighborhood Scale
Micro, Middle,
and/or
Neighborhood Scale
Micro, Middle,
and/or
Neighborhood Scale
Micro, Middle,
and/or
Neighborhood Scale
Comparability/
Method Selection
NIOSH 5029
TO - 13 A
TO -13 A
OSHA 42
OSHA 42
OSHA 42
EPA-modified
CARB 039
TO- 11A
Completeness
10 samples
10 samples
10 samples
10 samples
10 samples
10 samples
10 samples
10 samples
Minimum
Detection
Limits4
0.025
6.1 E-05
2.4 E-04
0.025
2.23 E-02
2.5 E-01
4.3 E-06
9.0 E-03
Table 6-3 MQOs for Other Compounds
References:
1. Guidance on Systematic Planning using the Data Quality Objectives Process (QA/G-4)
EPA/240/B-06/001 February 2006, http://www.epa.gov/qualitv/qa docs.html
2. 2007 National Air Toxics Trends Station Quality Assurance Annual Report, Draft 2009
3. Quality Assurance Project Plan, Eastern Research Group, Support for the UATMP
Program, 2009
4. Schools Air Toxics Ambient Monitoring Plan, April 2, 2009, Appendix B
5. These are estimates. The methods do not state the precision or bias
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7.0 Documentation and Records
The following information describes the documents and records that will kept on file for the
SATMP. Table 7-1 identifies these documents and records.
7.1 Routine Record Data Activities
EPA OAQPS developed an efficient archive and retrieval of records system. It is organized in a
similar manner to the EPA's records management system (EPA-220-B-97-003). Table 7-1
includes the documents and records that will be filed according to the statute of limitations
discussed in Section 7.3.
Categories
Record/Document Types
Responsible
Party
Site Information
Network description
Site characterization file
Site maps
Site Pictures
S/L agency or
EPA Region
Field Operations
Information
QA Project Plan
Standard operating procedures (SOPs)
Field and laboratory notebooks
Sample handling/custody records
Inspection/Maintenance records
EPA
OAQPS,UATMP
Contractor, S/L
agencies
Laboratory Data
Any original data (routine and QC data)
including data entry forms
Electronic deliverables of summary
analytical and associated QC and
calibration runs per instrument
Control charts
Chromatograms and spreadsheets with raw
unadjusted data
UATMP
Contractor, S/L
laboratories or
subcontractors
Quality Assurance
Information
Network siting and reviews
Data quality assessments
QA reports
Technical System Audits
Response/Corrective action reports
QA Final Report
EPA OAQPS,
Regions,
UATMP, S/L
labs or
subcontractors
Table 7-1 SATMP Data and Records Storage
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7.2 EPA Data and Document Control
Table 7-1 represents the documents and records, at a minimum, that must be filed. These
documents, including draft and intermediate versions of significant importance to the project
records will be stored and maintained consist with EPA records management policies.
7.2.1 Non-EPA Records
There are a number of S/L APCDs that will be involved in this program. It would be difficult to
describe each agency's document and record management system. However, there are some
general rules that apply. This section describes some of these practices.
Notebooks - The S/L APCDs will issue notebooks to each field and laboratory technician. This
notebook will be uniquely numbered and associated with the individual site. Although the
samples will have a Chain of Custody (CoC) with each sample, the notebooks will be used to
record additional information about these operations. All notebooks will be bound as well as
paginated so that individual pages cannot be removed unnoticeably.
Field notebooks - The SATMP will utilize sampling site notebooks. This will be 3-ring binders
that will contain the appropriate data forms for routine operations as well as inspection and
maintenance forms and SOPs. Additional notes, such as weather conditions, will be noted
whenever the site technician arrives.
Lab Notebooks - These notebooks will be uniquely numbered. One notebook will be available
for general comments/notes; others will be associated with, the temperature and humidity
recording instruments, the refrigerator, calibration equipment/standards, and the analytical
balances and instruments used for this program.
Electronic data collection - In order to reduce the potential for data entry errors, automated
systems will be utilized where appropriate and will record the same information that is found on
data entry forms. In order to provide a back-up, a hardcopy of automated data collection
information will be stored for the appropriate time frame in project files.
7.3 Data Reports, Archiving and Retrieval
In general, all the information listed in Table 7-1 will be retained for 5 years. However, if any
litigation, claim, negotiation, audit or other action involving the records has been started before
the expiration of the 5-year period, the records will be retained until completion of the action.
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Section 8.0 Sampling Design
8.1 Scheduled Project Activities, Including Measurement Activities
This section will discuss the operation and installation of samplers for the SATMP. Table 8-1
represents the activities associated with the ordering and deployment of the primary and
collocated samplers. Please note this schedule may change due to unforeseen circumstances
beyond the control of OAQPS, the Regional offices or the S/L APCDs.
Activity
QAPP Development
Monitoring Plan
Development
Lab Services Procured
Sampler siting/testing
QAPP Finalized
Field and Laboratory
Assessment and Support
Sampling Begins
Laboratory Analysis Begins
Sampling Ends
Due Date
March 2009
February - March
2009
April 2009
April- June 2009
April 2009
April - June 2009
April 2009
April 2009
Approximately
September 2009
Comments
Input taken and incorporated into official document.
Monitoring Plan vetted through official channels.
UATMP services in place for receiving samples.
Establishment of sites and preliminary testing of samplers.
QAPP finalized and submitted to S/L agencies.
Field and laboratory orientation and assessment.
Sampler testing completed and media shipped to monitoring
locations.
Samples received and analysis begins.
Dates include consideration of additional monitoring time to achieve
100% data capture and a range of starting dates for study sites to
accommodate vendor supply commitments.
Table 8-1 Scheduled Monitoring Activities
8.2 Rationale for the Design
8.2.1 Primary Samplers
To determine whether the data are of sufficient quality, the SATMP must address sampler type,
sampling frequency, and sampler siting. By employing samplers that are described in the
appropriate EPA compendia or in the OSHA, and NIOSH methods, the data collected will be
comparable to standard methods.
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By selecting sampler locations using the rules in Network Design and Site Exposure Criteria for
SelectedNoncriteria Air Pollutants,1 and 40 CFR Part 58 Appendix E2, the EPA SATMP can be
confident that the samplers are sited in a similar fashion. The sampling instruments are detailed
in the Monitoring Plan. Sampling frequency is discussed in Section 8.2.2 and 9.2, while siting
and exposure are further described in sections 8.3 - 8.4.
8.2.2 QA/collocated Samplers
The purpose of collocated samplers is to estimate the precision of the various samplers. The
goal is to have concentrations measured by a sampler having a CV of less than 30% for most
systems. Tables 6-1 through 6-3 list the individual precision CV objectives. To estimate the
level of precision being achieved in the field, the SATMP will operate collocated samplers for
all samplers, but not at every site. It is estimated that 15% of the network will have collocated
samplers. The VOCs and aldehyde samplers have dual channel configuration, which allows
collocated canisters and DNPH cartridges to be loaded on the same instrument as the primary
sample. The other samplers will require a second/collocated sampler to run along side of the
primary sampler. The QA samples will be set, run and collected on a 1 in 6 day schedule, the
same as the primary samplers. Please see Table 9-2 for details on setup and recovery of primary
and collocated samples. Section 12.1.3 outlines the equations that will be used to determine
precision. There will be two samples from each instrument that will be used to determine the
precision. Please note that if a S/L APCD does a random sample, as described in Section 3.2 of
the Monitoring Plan and there is a collocated sampler, collocated samples must be collected on
during the random sample event.
8.3 Design Assumptions
The sampling design is based on the assumption that following the rules and guidance provided
in 40 CFR Part 58 Appendix E1 and using the guidance in the Network Design and Site
Exposure Criteria for Selected Noncriteria Air Pollutants2 will result in data that can be used to
document air concentrations during the monitoring period. This information will be used in for
use in considering the potential impacts of air toxics emissions on the ambient air outside
schools. The siting design assumes that location of the monitors is within the micro, middle or
neighborhood scale, as defined in 40 CFR Part 58 Appendix D3.
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8.4 Procedure for Locating and Selecting Environmental Samples
8.4.1 Sampling Design
The design of the air toxics network must achieve the monitoring objective. For the SATMP,
the objective is to:
Collect information on ambient air concentrations of selected target compounds at a targeted
list of schools identified by EPA in the United States during a defined monitoring period.
The procedure for siting the samplers at the schools is based on best-case judgment by a
combination of EPA Regional staff, the S/L monitoring operators, and the school staff. The
best-case decisions will use utilize data from existing monitoring networks, knowledge of
source emissions and population distribution, and inference from analyses of meteorology to
select optimal sampler locations. In addition, a Geographic Information System (GIS) software
package will also be utilized to help locate the samplers.
8.5 Classification of Measurements as Critical/Noncritical
The ambient concentration and site location data will be provided to AQS. The information
collected at collocated samplers is the same as that presented in Tables 6-1, 6-2 and 6-3 for
primary samplers. All of the measurements in these tables are considered critical because they
form the basis for estimating precision, which is critical to appropriate interpretation of the
monitoring data.
References:
1. Network Design and Site Exposure Criteria for Selected Noncriteria Air Pollutants,
1984, EPA document: EPA-450/4-84-022
2. Code of Federal Regulations, Title 40 Part 58 , Appendix E
3. Code of Federal Regulations, Title 40 Part 58, Appendix D
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9.0 Sampling Methods Requirements
9.1 Purpose/Background
The methods described herein provide for measurement of the concentrations of HAPs in
ambient air for a 24-hour sampling period. Each sampler collects a discrete sample that
requires extraction and analysis performed in the laboratory. Table 9-1 lists the classes of target
analytes for this program.
Target Analytes
VOCs
Carbonyls
PM10/TSP HAP Metals
Hexavalent Chromium
PAHs
4,4 Methylene dianiline
Diisocyanates
Method
EPA TO- 15
EPATO-11A
EPAIO-3.5
EPA-modified CARB 039
TO-13A
NIOSHNo. 5029
OSHA No. 42
Sampling Media
Air (via canister)
DNPH-coated silica gel cartridge
47mm Teflon and 8" x 1 1 "quartz filters
47mm acid-washed sodium bicarbonate
impregnated cellulose filter
PUF / XAD-2
Sulfuric acid treated glass fiber filter
glass fiber filter coated with
1 -(2-pyridyl)piperazine
Table 9-1 List of Target Analytes
9.2 Sample Collection and Preparation
Sample preparation is an essential portion of the NSAMTMP. The following tasks are required
for sample preparation:
PMio/TSP - filter receipt and inspection, filter numbering, conditioning and storage;
VOC - cleaning, testing, verification and storage of canisters and sampler certification;
Carbonyls - receipt and storage of DNPH cartridges in the laboratory refrigerator;
Hexavalent Chromium - acid wash cellulose filters and soak in sodium bicarbonate;
PAHs - prepare the PUF/XAD-2 resin "sandwich;"
Diisocyanates- coat glass fiber filters with l-(2-pyridyl)piperazine;
4, 4 Methylene dianiline - treated glass fiber filters with Sulfuric acid.
Sample set-up of the air toxics samplers for the SATMP should take place at the same time as
the exposed sample has been recovered. For instance, on a Sunday - Thursday sample day set-
up when 1 in 6 day sampling is required, the pickup occurs the day after the run. However, on
Friday and Saturday run dates, the pick up is on the following Monday. Since the SATMP has
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collocated samplers, the second monitor will be set up to run at a sample frequency of 1 in 6
days and sample set-up will take place on the same day as the primary sampler. Please note:
the completeness goal of the program is to collect 10 samples, which represents 100% data
recovery. If this is not met within the 60-day period for some sites, then monitoring will
continue until the 10 samples are collected.
9.2.2 Sample Recovery
Sample recovery of any individual sample from the air toxics instruments sampler in the
SATMP network must occur within 72 hours of the end of the sample period for that sampler.
For 1 in 6 day sampling, this will normally be the day after a sample is taken. The next sample
would also be set-up at this time, see Table 9-2.
Sample
Frequency
1 in6
Weekl
1 in6
Week 2
Iin6
Week3
Iin6
Week 4
1 in6
WeekS
Iin6
Week 6
Sunday
Sample
Day 1
Monday
Recovery
& Set-up
Recovery
& Set-up
Recovery
& Set-up
Sample
Day 7
Tuesday
Sample
Day 6
Samples Run
Recovery &
Set-up
Wednesday
Sample
Day 5
Recovery &
Set-up
Thursday
Sample
Day 4
Samples Run
Recovery &
Set-up
Friday
Sample
Day 3
Recovery
& Set-up
Saturday
Sample
Day 2
Samples Run
Table 9-2 Sample Set-up, Run and Recovery dates
9.3 Support Facilities for Sampling Methods
It is envisioned that the main support facility for sampling will be the S/L APCD main
lab oratory/field operations facility or possibly at a field office or lab. Table 9-3 lists the supplies
that will be stored at each support facility.
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Item
Powder Free Gloves
Various Fuses
Temperature standard
Flow rate standards
Sampler Operations Manual
Flow rate verification filter
Tools
Filter Cassettes
Various fittings
Pumps
Data Download Cable
End caps
Aluminum foil
Ice chests
Quantity
Box
2
1
1 for each
sampler
1 per model
2
1
1
IBox
IBox
1
IBox
IBox
2
Notes
Material must be inert and powder free
Of the type specified in the sampler manual
In the range expected for this site and NIST traceable
NIST Traceable
For PMio or TSP sampler
One Tool kit with various wrenches, screwdrivers, etc.
For use with flow rate check filter or non-permeable
membrane
Of the type specified in the sampler manual
Of the type specified in the sampler manual
For use with laptop computer
For capping the DNPH cartridges
For sampler storage
Spare ice chests for transporting samples
Table 9-3 Field Supplies
Since there are other items that the field operator may need during a site visit that are not
expected to be at each site, the operator is expected to bring these items with him/her.
9.4 Sampling Corrective Action
Corrective action measures in the SATMP will be taken to ensure the MQOs are attained.
Please see the method descriptions in reference section of Chapter 5 and the individual SOPs for
information on corrective actions that may be encountered in the network.
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9.5 Sampling Equipment, Preservation, and Holding Time
This sections details the requirements needed to prevent sample contamination, the volume of
air to be sampled, how to protect the sample, temperature preservation requirements, and the
permissible holding times to protect ensure against degradation of sample integrity.
9.5.1 Sample Contamination Prevention
The quality system has rigid requirements for preventing sample contamination. Powder free
gloves are worn while handling filters, filter cassettes, canisters, and PUF/XAD-2 and DNPH
cartridges. Filter and cartridges are to be held in storage containers (static resistant zip lock
bags) as provided by the sampler manufacturer during transport to and from the laboratory.
9.5.2 Sample Volume
The volume of air to be sampled is detailed specified in the Manufacturers and Method
specifications. The different methods specify that certain minimum volumes must be collected.
For all but two collection systems, Diisocyanates and 4, 4 Methylene dianiline, samples are
expected to be collected for 24 hours; therefore, the site operators must set the flow rates to
collect sufficient sample to obtain the minimum sample volume. In some cases a shorter sample
period may occur due to power outages. If the sample period is less than 23 hours or greater
than 25 hours, the sample will be flagged and the analytical laboratory notified via a phone call
and by filling out the Chain of Custody (CoC) form.
For Diisocyanates, four 4 samples of 5.75 hours duration are expected to be collected over a 24-
hour period (beginning at 00:00, 06:00, 12:00, and 18:00) at sample rate of 0.8 liters per minute.
The four filters will be extracted together for a single analysis and effective resultant sample
volume of 960 liters. For 4, 4 Methylene dianiline, two2 samples of 10.5 hours duration over a
24- hour period at a sample rate of 0.8 liters per minute will be performed. The two filters will
be extracted together for a single analysis with an effective resultant sample volume of 1000
liters.
9.5.3 Temperature Preservation and Holding Time Requirements
The temperature requirements of the samples vary between methods. During transport from
the laboratory to the sample location there are no specific requirements for temperature control
with the exception of DNPH cartridges, Hexavalent chromium and glass fiber filters. Filters will
be located in their protective container and in the transport container. Excessive heat must be
avoided (e.g., do not leave in direct sunlight or a closed-up car during summer). The OSHA
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methods, NIOSH method, DNPH cartridges and Hexavalent chromium filters need to be stored
at 4ฐ C until they are loaded into the sampler. The temperature requirements are detailed here.
Item
PM10 or TSP filters temperature
control during sampling and until
recovery.
DNPH cartridge temperature
control pre- and post-sampling.
VOC canister pre and post
sampling
Hexavalent chromium temperature
control pre- and post-sampling.
Glass Fiber filter temperature
control pre-sampling.
PUF/XAD-2.
Temperature Requirement
No Requirements
4ฐ Cor less
No Requirements
4ฐ C or less
4ฐ Cor less
No Requirements
Reference
IO-3.5
TO-11A Compendium Section 9.4.3
TO- 15
EPA Modified -CARB 039
OHSA Method 42 and NIOSH 5029
TO-13A
Table 9-4 Temperature Requirements
Item
PM10/TSPfilter
temperature
VOC canister
DNPH Cartridge Filter
Hexavalent chromium
Filter
PUF/XAD-2
Glass Fiber filter for
OSHA 42
Glass Fiber filter for
NIOSH 5029
Holding Time
No limits
<30 days
<14 days
<30 days
<30 days
No limits
14 days in a
refrigerator
From
Completion of
sample period
Sample end
date/time
Sample end
date/time
Sample end
date/time
Sample end
date/time
Sample end
date/time
To
Time of analysis
Time of analysis
Time of analysis
Time of analysis
Time of analysis
Time of analysis
Reference
IO-3.5
TO- 15 Compendium Section
9.4.2.1
TO- 11 Compendium Section
11.1.2
EPA Modified -CARB 039
TO-13A/8270
OSHA Method 42
NIOSH 5029
Table 9-5 Holding Times
For detailed reference information, please see the reference section of Chapter 5 of this QAPP.
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Section 10.0 Sample Handling and Custody
10.1 Sample Custody
Sample custody is an extremely important aspect of this program. Samples custody procedures
must be followed in order to assure safe and secure samples are delivered both from and to the
field. All shipping to and from the S/L agencies will be handled by Federal Express with
Overnight Delivery. The next sections outline the UATMP contract sample handling regime.
Figures 10-1, 10-2 and 10-3 illustrate examples of chain of custody (CoC) forms that will be
used in this program.
10.1.1 Canister Sampling Field Data Forms
A color-coded, three-copy canister sample CoC form is shipped with each 6-liter canister to the
SATMP site. If duplicate samples are to be taken, two canisters and two data sheets are sent in
the shipping container to the site. When a sample is taken, the site operator fills out the field
data form according to the instructions in the on-site notebook. The site operator detaches the
pink copy, inserts it in the on-site notebook, and sends the remaining copies with the canister in
the shipping container to the analytical laboratory.
Upon receipt, the sample canister vacuum/pressure is compared against the field documented
vacuum/pressure to ensure the canister remained airtight during transport. If any leaks are
detected, the sample is voided. More detailed sample receipt procedures and sample acceptance
policies are presented in the SOP ERG-MOR-045. The sample specific information from the
CoC sheets is then entered into the LIMS. The sample is logged into the LIMS as described in
the SOP ERG-MOR-079. The sample is given a unique identification (ID) number and tagged,
(See Figure 10-2), noting the site location and the sample collection date. The remaining copies
of the canister sample data sheet are separated; the white copy is stored with the canister until
analysis is complete and the yellow copy is stored chronologically in a designated file cabinet.
The sample ID number is presented on the canister tag and on all ERG copies of the data sheet.
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TOXICS/SNMOC SAMPI
Ui
11
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Figure 10-1 UATMP Sample Data Sheet
10.1.1 Invalid Canister Sample
The canister sample CoC form may indicate that the sample sent from a site is invalid. When a
sample is designated as invalid, the assigned ERG ID number is voided and is invalidated on the
individual respective chain of custody form. The sites will be notified in the analytical reports of
any invalid samples.
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Analysis:
Sample ID:
Laboratory ID:
Date Sampled:
Canister #:
Site:
Press/Vac:
Dup/Rep:
Comment:
Figure 10-2 Canister Tag
10.1.2 Canister Cleanup
All canisters are cleaned prior to reuse using SOP ERG-MOR-062. All canisters are cleaned and
are entered into the canister cleanup log. The canisters received from the monitoring sites are
placed in the laboratory by ERG staff. The canister analysis hold time is 30 days from the
sampling date.
10.2 Carbonyl Sample Custody
Figure 10-3 shows the CoC form used for all carbonyl sampling documentation. A chain of
custody is shipped to the site with blank carbonyl tubes if the tubes are provided by ERG, or
blank data sheets are provided to sites supplying their own tubes for sampling. After sampling,
the field data sheet is completed by the site operator and a copy retained for site records. The
carbonyl sample tubes and field data sheet are shipped to ERG's analytical laboratory.
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CARBONYL COMPGUN
sl
I
5 is Csda
^-y ^-a-ป-
a -,c ,- n..p
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DS DATA SHEET
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-
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1
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Time
Sarspie
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Figure 10-3 Carbonyl Chain of Custody Form
When samples are received, they are given an ERG sample ID number and logged into the
LIMS (SOP ERG-MOR-071). The database records each carbonyl sample; the carbonyl tubes
and the white copy of the field data sheet are put into a bag labeled with the ERG ID number,
site code, sampling date, individual tube designations, and date of receipt and initials of
receiving personnel. This sample bag is stored in a refrigerator designated for carbonyl samples.
More detailed sample receipt procedures and sample acceptance policies are presented in the
SOP ERG-MOR-045. A yellow copy of the field data sheet is stored chronologically in a
designated file cabinet.
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10.3 Sample Custody for other HAPs
Prepared sample media (i.e., XAD, PUF, filters, etc.) and documentation during the sample
collection phase of the program will use pre-formatted forms supplied by ERG or the
subcontractor (RTI Laboratories - Levonia, Michigan). Field testing personnel will record data
on the appropriate CoC forms. The CoC forms provided by the subcontractor are presented in
their QAPP. The CoC forms provide for documentation of time, date, location, meteorological
parameters and possibly some laboratory parameters. XAD, PUF, and filters are received at
ERG's laboratory as presented in the SOP for Sample Receipt at ERG Chemistry Laboratory,
ERG-MOR-045. The HAPs samples received at the ERG laboratory will be logged into the
LIMS as described in the SOP ERG-MOR-079.
10.4 Analytical Laboratory Data
All analytical laboratories will provide sample tracking forms, narratives describing any
anomalies and any modifications to analytical procedures, data and sample handling records,
and laboratory notes for inclusion in the final report. All laboratory electronic records will be
recorded for archive on magnetic media, and all hardcopies of raw data will be included in the
project archive file. All records generated by measurement activities are signed or initialed by
the person performing the work and reviewed by an appropriate supervisor. Measurement
results become part of a project report which is reviewed by a technical reviewer. All
notebooks are kept in black ink, dated and signed by the person making the entries, and
routinely inspected by the appropriate supervisor, as evidenced by his/her initials and date of
inspection. Laboratory notebook maintenance procedures are regulated by Standard Operating
Procedure, ERG-MOR-039.
10.5 Sampling Monitoring Data
All data sheets from the monitoring sites will be collected at the end of each monitoring
episode and maintained in the laboratory/field office throughout the monitoring program. If
corrective action is required during the field monitoring activities, the reason for the correction
and action taken will be documented on a corrective action report form, as described in the
UATMP contract QAPP. All forms will be written on with indelible ink. If correction is
required on the form, a single line will be drawn through the erroneous entry, and the
correction will be dated and initialed. Any blank spaces will have a line drawn through to
ensure that the space is not filled in later. The original field data will remain in ERG custody
and is eventually stored on file with the final report for 5 years.
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11.0 Analytical Methods Requirements
The analytical instrument for this program are: gas chromatograph - mass spectroscopy
(GC/MS) for VOCs, high pressure liquid chromatograph (HPLC) for carbonyls, inductively
coupled plasma/mass spectrometer (ICP/MS) for metals, ion chromatography (1C) for
Hexavalent Chromium, HPLC for the Diisocyanates and HPLC and Electron Capture - Hall
Detector (ECHO) for 4, 4 Methylene dianiline. All analytical method SOPs are on file with
ERG or its subcontractors. Contact information for ERG is in the Acknowledgement Section of
this QAPP.
11.1 VOC Canister Analysis and Cleanup System
The atmosphere is sampled by introduction of air into a specially-prepared stainless steel
canister. A sample of air is drawn through a sampling train comprised of components that
regulate the rate and duration of sampling into the pre-evacuated and passivated canister. After
the air sample is collected, the canister valve is closed, an identification tag is attached to the
canister, and the canister is transported to the laboratory for analysis. Upon receipt at the
laboratory, the canister is recorded and is stored until analysis. Storage times of up to thirty 30
days have been demonstrated for many of the VOCs. To analyze the sample, a known volume
of sample is directed from the canister through a solid multi-sorbent concentrator. A portion of
the water vapor in the sample breaks through the concentrator during sampling, to a degree
depending on the multi-sorbent composition, duration of sampling, and other factors. Water
content of the sample can be further reduced by dry purging the concentrator with helium while
retaining target compounds. After the concentration and drying steps are completed, the VOCs
are thermally desorbed, entrained in a carrier gas stream, and then focused in a small volume by
trapping on a reduced temperature trap or small volume multi-sorbent trap. The sample is then
released by thermal desorption and carried onto a gas chromatographic column for separation.
As a simple alternative to the multi-sorbent/dry purge water management technique, the amount
of water vapor in the sample can be reduced below any threshold for effecting the proper
operation of the analytical system by reducing the sample size. For example, a small sample can
be concentrated on a cold trap and released directly to the gas chromatographic column.
A canister cleanup system has been developed and is used to prepare sample canisters for
use and reuse after analysis (SOP ERG-MOR-062). An oil-free compressor with an 80-
gallon reservoir provides source air for the system. The compressor was chosen to
minimize hydrocarbon contamination. A coalescing filter removes water mist and
particulate matter down to a particle size of 10 microns and permeation dryers remove
water vapor from the compressor source air. The permeation dryers are used with a
moisture indicator to show detectable moisture in the air leaving the dryer. Next, air is
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passed through a catalytic oxidizer to destroy residual hydrocarbons. The oxidizer is
followed by an in-line filter for secondary particulate matter removal.
A single-stage regulator controls the final air pressure in the canisters, and a metering valve is
used to control the flow rate at which the canisters are filled during a cleanup cycle. The flow
direction is controlled by a separate rotometer, installed in the clean, dried air line. A shutoff
valve exists between the clean dried air line and the humidifier system (which is a modified
SUMMAฎ-treated 6-liter canister partially filled with HPLC-grade water). One flowmeter and
flow-control valve direct the cleaned, dried air into the 6-liter canisters, where it is bubbled
through the HPLC-grade water; a second flow-control valve and flowmeter allow air to bypass
the canister/bubbler. By setting the flow-control valves separately, the downstream relative
humidity can be regulated. A setting of 100% relative humidity is used for canister cleaning
with the wet rotometer on and the dry rotometer off. Another shutoff valve is located between
the humidifier and each 8-port manifold where the canisters are connected for cleanup.
The vacuum system consists of a Precision Model DD-310 turbo-molecular vacuum pump, a
cryogenic trap, an absolute pressure gauge, and a manifold vacuum valve connected. The
cryogenic trap prevents the sample canisters from being contaminated by back- diffusion of
hydrocarbons from the vacuum pump into the cleanup system. The manifold vacuum valves
enable isolation of the vacuum pump from the system without shutting off the vacuum pump.
After sample analyses and data review are completed, a bank of eight canisters is connected
to each manifold with each canister valve open and the air pressure, vacuum, and bellows
valves closed. The vacuum pump is started and one of the bellows valves is opened, drawing
a vacuum on the canisters connected to the corresponding manifold. After reaching 10 mm
Hg absolute pressure, as indicated by the absolute pressure gauge, the vacuum is maintained
for 30 minutes. The bellows valves are then closed and the cleaned, dried air that has been
humidified is introduced into the evacuated canisters at a rate of 4.0 liters per minute until the
pressures reach approximately 20 psig. This flow rate has been recommended by the
manufacturer as the highest flow rate at which the catalytic oxidizers can handle elimination
of hydrocarbons with a minimum of 99.7% efficiency. The evacuation and pressurization of
the canisters constitutes one cleanup cycle.
The cleanup cycle is repeated twice more during the canister cleanup procedure. Following the
third pressurization, the canister valves are closed, and the canister that had the highest pre-
cleanup concentration is selected for cleanliness verification. The cleanliness of the canister is
qualified by GC/MS analysis (one canister per bank of cleaned canisters - one canister per eight
cleaned). The cleanliness criterion for each bank of eight canisters is 0.2 ppbv per analyte or
the MDL, whichever is greater. Upon meeting this criterion, the canister is reconnected to the
cleanup manifold. All canister valves are opened and the canisters are evacuated to
approximately 29.5 inches Hg absolute pressure for a fourth time, in preparation for shipment to
the site.
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11.2 Analysis of PAH using EPA Compendium Method TO-13A
Sampling modules containing polyurethane foam (PUF), petri dishes containing filters, CoC
forms and all associated documentation will be shipped to the ERG laboratory from the field.
Upon receipt at the laboratory, samples will be logged into the laboratory sample tracking
system and sent to the sample preparation laboratory. Sample preparation and analysis
procedures are based on SW-846 Method 3540C for sample preparation and EPA Compendium
Method TO-13A for analysis using Selected Ion Monitoring techniques. The hold time is two
weeks (14 days) after sampling for extraction and 45 days after extraction for analysis.
Sample extracts will be analyzed for PAHs using the analytical procedures outlined in EPA
Compendium Method TO-13 A, using Selected Ion Monitoring. Instrument operating
conditions are shown in Table 2 of EPA Compendium Method TO-13A and the laboratory
SOPs ERG-MOR-044. The mass spectrometer will be tuned and mass-calibrated as required
using perfluorotributylamine (FC-43), per the manufacturer's instructions. The tune of the
instrument is verified by injecting 50ng of DFTPP and checking the ion abundance criteria
against the ion abundance criteria listed in Table 3 of EPA Compendium Method TO-13 A. If
the DFTPP mass spectrum does not meet method specifications, the DFTPP is re-analyzed or
the mass spectrometer is re-tuned so that the instrument will meet the tuning criteria. The
DFTPP tuning criteria must be met before analysis of samples can begin. The acceptability of
the instrument tune will be verified by analysis of the DFTPP solution daily, or every 12 twelve
hours if the instrument is operated for 24 hours a day. Analytical procedures for performance of
the Selected Ion Monitoring analysis are presented in ERG-MOR-049 for analysis by EPA
Compendium Method TO-13 A.
11.3 Metals Using ICP/MS
After receipt of the sample shipment, the samples are checked against the CoC forms and then
assigned an analytical laboratory sample number. Each sample component is examined to
determine if damage occurred during travel. Color, appearance, and other particulars of the
samples are noted. Sample preparation and analysis procedures are based on EPA Compendium
Method IO-3.5A for the Determination of Metals in Ambient Parti culate Matter using ICP/MS
techniques. A complete description of the preparation and analytical procedures for metals
filters is in ERG-MOR-085.
Instrument operating conditions for the analysis of inorganics using an ICP/MS are shown in
Table 3 of EPA Compendium Method IO-3.5A and the laboratory SOPs ERG-MOR-085 for
Teflonฎ filters. The mass spectrometer will be mass calibrated and resolution checked.
Resolution at low mass is indicated by magnesium isotopes 24, 25, and 26. Resolution at high
mass is indicated by lead isotopes 206, 207, and 208. Instrument stability must be
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demonstrated by running a tuning solution containing 100 |ig/L of beryllium, magnesium,
cobalt, indium and lead. The analyses will be run five times with the resulting relative standard
deviation (RSD) of absolute signals for all analytes of less than 5 percent.
11.4 Hexavalent Chromium
Hexavalent chromium filter samples are stored in the freezer after they are received from the
field prior to analysis. Internal studies have shown that the Hexavalent chromium does not
degrade for up to 21 days if the samples they are stored in the freezer before extraction. Due to
oxidation/reduction and conversion problems between the trivalent chromium (Cr3+) and
Hexavalent chromium (Cr6+), the extraction is performed immediately prior to analysis.
Therefore, it is important that the ion chromatograph (1C) be equilibrated, calibrated and ready
for analysis before filters are extracted. Sample preparation is performed by removing the filter
from its filter cassette and placing it into a 14-mL polystyrene tube and adding 10-mL of
sodium bicarbonate in deionized water. The extraction is done on a bench-top. The extract is
sonicated for three hours before a 5-mL aliquot is removed for analysis on the 1C. Extracts are
stored in a freezer until they are analyzed. All analysis is completed the day the filters are
extracted.
The analytical separation for the Hexavalent chromium is performed using a Dionex-600 1C
with a Dionex LC 20 Chromatography Enclosure with a PC 10 Pneumatic Controller and a
GP50 Gradient Pump configured with an lonPac AS7 and an lonPac NG1 guard column.
ERG's system uses a Dionexฎ data system. Samples are injected in duplicate using a Dionex
AS40 auto-ampler. A mobile phase is used to perform the analytical separation at a flow rate of
1.5mL/min, and a post-column reagent flow rate of 0.5mL/min. The multi-wavelength UV
detector is used at 530 nm. The samples are prepped and analyzed following ERG SOP, for
Analysis of Hexavalent Chromium by Ion Chromatography ERG-MOR-063.
11.5 Diisocyanates
Samples are collected by use of a supported filter holder with a sampling pump at the
recommended flow rate with the sampling device devise in line. A known volume of air is
pulled through a three-piece styrene cassette containing a glass fiber filters coated with 0.1 mg
of l-(2-pyridyl)piperazine (1-2PP) and a backup pad. After sampling, the filters are wrapped
and shipped to the laboratory for analysis.
Samples are extracted with 90/10 (v/v) acetonitrile/dimethyl sulfoxide and analyzed by HPLC
using an ultraviolet (UV) or fluorescence detector.
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11.6 4,4 Methylene dianiline
Samples are collected by use of a supported filter holder and a sampling pump calibrated with a
representative sample in line. Samples are taken by drawing a known volume of air through a
sulfuric acid-treated glass fiber filter. The samples are transferred within four 4 hours of
completion of sampling, into a vial containing 4 mL of 0.1 N methanolic - potassium hydroxide.
Samples can be stored in the glass vials for up to one month prior to analysis.
The samples are agitated in an ultrasonic water bath before analysis. The samples are analyzed
on HPLC using a UV and electrochemical detector.
11.7 Carbonyls
A known volume of ambient air is drawn through a pre-packed cartridge coated with acidified
DNPH at a known sampling rate for an appropriate period of time. Sampling rate and time are
dependent upon carbonyl concentration in the test atmosphere. After sampling, the sample
cartridges and field blanks are individually capped and placed in shipping tubes with end caps.
Sample identifying tags and labels are then attached to the capped tubes. The capped tubes are
then placed in a polypropylene shipping container cooled to sub-ambient temperature (4ฐ C) and
returned to the laboratory for analysis. Alternatively, the sample vials can be placed in a
thermally- insulated box with appropriate padding for shipment to the laboratory. The cartridges
may either be placed in cold storage until analysis or immediately washed by gravity feed
elution with 5 mL of Acetonitrile from a glass syringe reservoir to a graduated test tube or a 5
mL volumetric flask. The eluate is then diluted to a known volume and refrigerated until
analysis. For determining carbonyls, the DNPH-carbonyl derivative can be determined using
reverse phase HPLC with an ultraviolet (UV) absorption detector operated at 360 nm. To
determine carbonyls, the HPLC system is operated in the linear gradient program mode.
Carbonyl compounds in the sample are identified and quantified by comparison of their
retention times and peak heights or peak areas with NIST traceable standard solutions.
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12.0 Quality Control Requirements
Quality Control (QC) is the overall system of technical activities that measures the attributes
and performance of a process. In the case of the SATMP, QC activities are used to ensure that
measurement uncertainty, as discussed in Chapter Section 6, is maintained within acceptance
criteria for the attainment of the DQO.
12.1 QC Procedures
Day-to-day QC is implemented through the use of various checks on the samplers. These
checks are used to verify that the sampler is operating properly. The procedures for the methods
section are described in Sections 9 (field) and 11 (laboratory), respectively. The following
information provides some additional descriptions of these QC activities, how they will be used
in the evaluation process, and what corrective actions will be taken when they do not meet
acceptance criteria.
12.1.1 Calibrations
Calibration is the comparison of a measurement standard or instrument with another standard or
instrument to report, or eliminate by adjustment, any variation (deviation) in the accuracy of the
item being compared. The purpose of calibration is to minimize bias.
Calibration activities for air toxics samplers follow a two-step process:
1. Certifying the calibration standard and/or transfer standard against an authoritative
standard; and,
2. Comparing the calibration standard and/ or transfer standard against the routine
sampling/analytical instruments.
Calibration requirements for the critical field and laboratory equipment are discussed in Section
14 of this QAPP. More detailed procedures are found in the respective instrument and sampler
SOPs.
12.1.2 Blanks
Blank samples are used to determine contamination arising from principally four sources: the
environment from which the sample was collected/analyzed, the reagents used in the analysis,
the apparatus used, and the operator/analyst performing the analysis. Three types of blanks will
be implemented in the air toxics program:
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Lot blanks - shipments of filters and cartridges will be periodically sent from the vendor to
UATMP contract lab. Each shipment must be tested to determine the length of time it takes the
filters to stabilize. Upon arrival of each shipment, threeS lot blanks will be randomly selected
for the shipment and be subjected to the conditioning/pre-sampling procedures.
Field blanks - provides an estimate of total measurement system contamination. By comparing
information from laboratory blanks against the field blanks, one can assess contamination from
field activities. Field blanks will be utilized for all samples with the exception of canister
sampling. Field blanks cannot be utilized with the VOC canisters since they arrive in the field
under vacuum.
Lab blanks -provides an estimate of contamination occurring at the analysis facility. Details of
the use of the lab blanks can be found in the SOPs. Lab blanks will be utilized for the
aldehydes, metals and VOCs. Lab blanks for VOCs are generated by the canister cleaning
system.
Blank Evaluation - The laboratory will include three 3 field and three 3 lab blanks into each
batch. The following statistics will be generated for data evaluation purposes:
Corrective action- The acceptance criteria for field blanks are discussed in the individual
SOPs. However the mean difference based upon the number of blanks in each batch will be
used for comparison against the acceptance criteria. If the mean difference of either the field or
laboratory blanks is greater than the accepted values, then these will be noted in the QA final
report. If the blank means of either the field or lab blanks are still out of the acceptance criteria,
all samples within the analysis session will be flagged with the appropriate flag, and efforts will
be made to determine the source of contamination. In theory, field blanks should contain more
contamination than laboratory blanks. Therefore, if the field blanks are outside of the criteria
while the lab blanks are acceptable, analysis can continue on the next batch of samples while
field contamination sources are investigated. If the mean difference of the laboratory blanks is
greater than the acceptance criteria, the laboratory will stop until the issue is satisfactorily
resolved. The laboratory technician will alert the Laboratory Manager and/or QA Officer of the
problem. The problem and solution will be reported and appropriately filed under response and
corrective action reports. The laboratories will take the appropriate action according to the
individual lab SOPs.
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12.1.3 Precision Checks
Precision is the measure of mutual agreement among individual measurements of the same
property, usually under prescribed similar conditions. In order to meet the data quality
objectives for precision, the EPA and S/L APCDs must ensure the entire measurement process
is within statistical control. Precision measurements will be obtained using collocated
monitoring.
Evaluation of Collocated Data- All collocated data will be reported to AQS. The following
algorithms will be used to evaluate collocated data. Collocated measurement pairs are selected
for use in the precision calculations only when both measurements are within the acceptance
criteria.
The percentage difference, dt, for each check is calculated by using the following equation,
where Xt represents the concentration produced from the primary sampler and Yt represents the
concentration reported for the duplicate sampler.
di = Yi-Xi x 100
Estimate of Precision - In 2008, the EPA changed the calculations that derive precision, i.e.,
precision is expressed as coefficient of variance (CV). The following equation is used to
calculate the CV. The precision estimate is used to assess the one-point QC checks for gaseous
pollutants described in section 3.2.1 of CFR Part 58, Appendix A1. The precision estimator is
the coefficient of variation upper bound and is calculated as follows:
\
I JJ-1
1
/O.l.H-1
2
Where % is the 10th percentile of a chi-squared distribution with n-1 degrees of freedom.
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Table 12-1 illustrates several issues that will preclude collocated data from being used for
precision calculations.
Parameter
Both samples did not run 24 hours +/- 10 min.
One or both filters are damaged or exhibit a pinhole or tear
One or both samplers has erratic flow pattern
The difference in the pressure of the VOC canisters is > 2 psig
One or both samples are not kept within the holding and storage
temperature requirements for any length of time
Decision
Do not use for precision
calculations
Do not use for precision
calculations
Do not use for precision
calculations
Do not use for precision
calculations
Do not use for precision
calculations
Table 12-1 Sample Invalidation Criteria for Collocated Data
Estimate of Bias - For the SATMP, EPA's independent PT laboratories will create single blind
PT samples. The SATMP analysis labs will analyze the samples and send the results to the
independent lab that generated the PT sample. The audit sample for each system will be mailed
directly to the analytical laboratory or subcontractor lab. The results will then be sent to the
EPA. The equation used to define percentage difference (4) for each individual compound audit
/' is calculated. Where Xt represents the audit standard concentration from a certified laboratory
(known) and Yt represents the indicated value obtained from the laboratory.
di =
References:
1. Code of Federal Regulations, Title 40 Part 58 , Appendix A
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13.0 Instrument/Equipment Testing, Inspection, and Maintenance
13.1 Purpose/Background
The purpose of this section in the SATMP QAPP is to discuss the procedures used to verify that
all instruments and equipment are maintained in sound operating condition and are capable of
operating at acceptable performance levels.
13.2 Testing
All samplers used in the SATMP will be similar to the instruments described in the TO and IO
Compendia, OSHA and NIOSH methods. Prior to field installation, field operators will
assemble and run the samplers at the laboratory facilities (if available). The field operators will
perform external and internal leak checks and temperature, pressure and flow rate verification
checks. If any of these checks are is out of specification, the field technicians will attempt to
correct them. If the problem is beyond their expertise, the field manager will contact the vendor
for guidance. If the vendor does not provide sufficient support, then the instrument will be
returned to the vendor. Once installed at the site, the field operators will run the tests at least
one more time. If the sampling instrument meets the acceptance criteria, it will be assumed to be
operating properly.
13.3 Inspection
Inspection of various equipment and components are provided here. The inspections section is
subdivided into two sections: one pertaining to laboratory issues; and one associated with field
activities.
13.3.1 Inspection in Laboratory
Table 13-1 lists several items that require inspections and how to appropriately document the
inspection. All of the different areas of the laboratory (GC/MS, 1C, HPLC and the ICP/MS
rooms) will be maintained. Other inspections will be documented in the individual SOPs and
QAPPs.
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Item
GC/MC Room
Temperature
GC/MS
Cleanliness
ICP
Temperature
ICP
Cleanliness
HPLC Room
Temperature
HPLC
Cleanliness
Extract ion
Room
Inspection
Frequency
Daily
Monthly
Daily
Monthly
Daily
Monthly
Weekly
Inspection
Parameter
20 - 30ฐ C
Use glove and
visually inspect
20 - 30ฐ C
Use glove and
visually inspect
20 - 30ฐ C
Use glove and
visually inspect
Use glove and
visually inspect
Action if Item Fails Inspection
1. ) Check H VAC System
2.) Call service provider that
holds maintenance agreement
Clean room and remove clutter
put canisters back into rack
1. ) Check H VAC System
2.) Call service provider that
holds maintenance agreement
Clean room and remove clutter
store and clean vials. Discard
old filters
1. ) Check H VAC System
2.) Call service provider that
holds maintenance agreement
Clean room and store cartridges
Thoroughly clean room and
remove all materials. Clean all
removal instrument and
autoclave
Documentation
Requirement
Document in Logbook
Document in Log Book
Document in Logbook
Document in Log Book
Document in Logbook
Document in Log Book
Document in Log Book
Table 13-1 Inspections in the Laboratory
13.3.2 Inspection of Field Items
There are several items to inspect in the field before and after a sample has been taken. Please
refer to the instrument manufacturer's operation manuals.
13.4 Maintenance
There are many items that need maintenance attention in the network. This section describes
the laboratory and field items.
13.4.1 Laboratory Maintenance Items
The GC/MS and ICP/MS systems are maintained under separate service agreements. Twice a
year, preventive maintenance is performed by a technical representative. ERG and
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subcontractor personnel perform minor maintenance, such as column and detector
maintenance, on an as-needed basis. Other maintenance information can be obtained in the
UATMP and subcontractor SOPs.
13.4.2 Field Maintenance Items
There are many items associated with appropriate preventive maintenance of a successful field
program. Please refer to the manufacturer's operating manual and the field SOPs for detail on
maintenance items for individual samplers.
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14.0 Instrument Calibration and Frequency
All instrument and samplers in this program will be calibrated using NIST traceable standards.
The field and laboratory technician that operate and maintain the instruments should also
perform verifications/calibrations as necessary. For the SATMP, the calibrations are divided
into the field and analytical laboratory portions.
14.1 Laboratory Instruments
All laboratories will maintain sets of standards for each of the laboratory systems. Below are
brief statements on how these calibrations are performed. Please refer to the UATMP or its
subcontractor's SOPs for detailed information on calibrating the laboratory instruments.
For the Gas Chromatographs, a NIST Traceable cylinder is attached to a mass flow control
calibration unit. The concentrations of benzene, propane and methylene chloride are
blended down to a value which will be in the higher 80% of the range of compounds found
in ambient concentrations. This usually is ~ 20 ppbv. The Gas Chromatographs is allowed
to reach operating conditions. The gas from the mass flow controller is injected into the
system and the carrier helium is allowed to flow. Once the calibration gas is allowed to
enter, two peaks should appear. The mass flow controller is then adjusted to allow the gas
concentration to be ~ 40%. This process is then repeated with a concentration of 20% of
range of compounds. Zero air is then generated and a baseline is determined. The system
is now ready to accept ambient concentrations. After the day's batches are run, a single
point (80%) is injected into the GC.
After the Inductively Coupled Plasma unit is allowed to come to operating conditions, a
standard solution of metals is injected into the ICP. The responses are noted. Distilled ion-
free water is then injected into the ICP. This allows the system to reach a baseline.
For the HPLC, the procedure is the same, with the exception of the compounds injected. The
compounds that are used for calibration are from standard solutions. After the HPLC has
come to operating conditions, ultra-pure diluent solution is injected. This allows the system
to reach a baseline. Different concentrations at 80% of the normal ambient concentrations
of standard solutions are injected into the HPLC. Response peaks are observed and
recorded. This procedure is repeated at the end of the analysis batch run.
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14.2 Field Calibrations
The following calibrations are performed in the field:
1 calibration of volumetric flow rate meter of each sampler against the working standard;
1 calibration of sampler temperature and pressure sensors against the working temperature
standard;
1 calibration of the min/max thermometers, normally located in the coolers in which DNPH
cartridges are transported to and from the sampler in the field, against the laboratory-
checked working standard thermometer;
1 verification of pressure sensors; and,
1 check initial wind speed and direction of the sensors.
The following section will give more details on how these procedures are performed. Please
reference the individual SOPs and/or manufacturer's operating manual.
14.3 Calibration Method
This section describes generalized calibration procedures that will be used by the laboratories
and S/L APCD field technicians.
14.3.1 Laboratory/ Field - Flow Calibration
After equilibrating the calibration device to the ambient conditions, connect the flow calibration
device on the sampler down tube or filter holding device. If the sampler has not been calibrated
before, or if the previous calibration was not acceptable, perform a leak check according to the
manufacturer's operational instruction manual, which is incorporated into SATMP SOPs.
Otherwise, place the sampler in calibration or "run" mode and perform a one-point calibration
or one-point flow rate verification. The field staff will only perform a leak check after
calibration or verification is outside of the acceptance criteria.
Following the calibration or verification, turn off the sampler pump, remove the filter, cartridge,
and remove the flow calibration device, (and flow adaptor device if applicable), and replace the
sampler inlet or hood. If the flow rate is determined to be outside of the required target flow
rate, attempt to determine possible causes by minor diagnostic and trouble shooting techniques
(e.g., leak checks), including those listed in the manufacturer's operating instruction manual.
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14.3.2 Laboratory/Field Pressure Calibration
According to ASTM Standard D 3631 (ASTM 1977)1, a barometer can be calibrated by
comparing it with a secondary standard traceable to a NIST primary standard. Protect all
barometers from violent mechanical shock and sudden changes in pressure. A barometer
subjected to either of these events must be recalibrated. Maintain the vertical and horizontal
temperature gradients across the instruments at less than 0.1 ฐC/m. Locate the instrument so as
to avoid direct sunlight, drafts, and vibration. A Fortin mercury type of barometer is used in the
laboratory to calibrate and verify the aneroid barometer used in the field to verify the barometric
sensors of samplers. Details are provided in the appropriate SOP.
14.3.3 Laboratory/Field Temperature Calibration
The operations manuals and individual laboratory and field sampler SOPs will have detailed
procedures for calibrating the temperature sensor for the particular samplers and instruments.
The EPA Quality Assurance Handbook, Volume IV (EPA 2008)2 Section 4.3.4, provides
information on calibration equipment and methods for assessing response characteristics of
temperature sensors.
14.3.4 Wind sensor Calibration
The SATMP will utilize sonic anemometers in the field. Sonic anemometry is a relatively new
technology that is gaining national acceptance, due to lower levels of detection and no moving
parts. However, because the sensors do not have any moving parts, calibration of theses sensors
can be challenging. In general, sonic anemometers must be mounted so they are level and are
oriented to true North. Please reference the instrument manufacturer's operating manual for
instruction on calibrations, orientation and alignment. Additional background information on
wind direction alignment can be obtained in the EPA's QA Handbook, Volume IV:
Meteorological Measurements2.
14.4 Calibration Standard Materials and Apparatus
Flow Rate - The flow rate standard apparatus used for flow-rate calibration (field- NIST-
traceable, piston-type volumetric flow rate meter; laboratory -NIST-traceable manual soap
bubble flow meter and time monitor) has its own certification and is traceable to other standards
for volume or flow rate which are themselves NIST-traceable. A calibration relationship for the
flow-rate standard, such as an equation, curve, or family of curves, is established by the
manufacturer (and verified if needed) that is accurate to within 2% over the expected range of
ambient temperatures and pressures at which the flow-rate standard is used. The flow rate
standard will be recalibrated and recertified at least annually.
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The actual frequency with which this recertification process must be completed depends on the
type of flow rate standard; some are much more likely to be stable than others. In addition to
providing excellent documentation of the certification of the standard, a control chart also gives
a good indication of the stability of the standard. If the two standard-deviation control limits are
close together, the chart indicates that the standard is very stable and could be certified less
frequently. The minimum recertification frequency is 1 year. On the other hand, if the limits
are wide, the chart would indicate a less stable standard that will be recertified more often.
Temperature - The temperature standard used for temperature calibration will have its own
certification and be traceable to a NIST primary standard. A calibration relationship to the
temperature standard (an equation or a curve) will be established that is accurate to within 2%
over the expected range of ambient temperatures at which the temperature standard is to be
used. The temperature standard must be re-verified and recertified at least annually. The S/L
APCDs will use NIST-traceable mercury in glass thermometer or thermistor type temperature
probes for laboratory calibration. The field temperature standards will be digital readout
thermistor type probes. Each probe will be certified against NIST-traceability standards.
Calibration Frequency - Since the SATMP is a 60 day project, calibrations must be performed
at the beginning and at the end of the sampling, or if the instrument malfunctions or is repaired.
More frequent calibrations are encouraged, but not required and are left to the field operator's
discretion. These events, as well as sampler equipment maintenance and inspections will be
documented in field data records (i.e., CoC forms) and notebooks. The records will normally be
controlled by the individual agency field managers, and located in the labs or field sites when in
use or at the manager's offices when being reviewed or used for data validation.
References:
1. ASTM. 1977. Standard test methods for measuring surface atmospheric pressure.
American Society for Testing and Materials. Philadelphia, PA. Standard D 3631-84.
2. EPA. 2008. Quality Assurance Handbook for Air Pollution Measurement Systems
Volume IV: Meteorological Measurements. U.S. Environmental Protection Agency.
Document No. EPA/454/B-08-002. http://www.epa.gov/ttn/amtic/met.html
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15.0 Data Acquisition Requirements
This section addresses data not obtained by direct measurement from the SATMP. This includes
both outside data and historical monitoring data. Non-monitoring data and historical
monitoring data are used by the SATMP in a variety of ways. The procedures described in this
section apply both to data acquired through the SATMP and to information previously acquired
and/or acquired from outside sources.
15.1 Acquisition of Non-Direct Measurement Data
The SATMP will rely on data that are generated through field and laboratory operations;
however, other significant data are obtained from sources outside the EPA or from historical
records.
15.1.1 Chemical and Physical Properties Data
Physical and chemical properties data and conversion constants are often required in the
processing of raw data into reporting units. This type of information that has not already been
specified in the monitoring regulations will be obtained from nationally and internationally
recognized sources.
> National Institute of Standards and Technology (NIST);
> International Standards Organization (ISO), International Union of Pure and Applied
Chemists (IUPAC), American National Standards Institute (ANSI), and other widely-
recognized national and international standards organizations;
U.S. EPA; and,
Operating instrument manuals and SOPs.
15.1.2 Sampler Operation and Manufacturers' Literature
Another important source of information needed for sampler operation is manufacturers'
literature. Operations manuals and users' manuals frequently provide numerical information
and equations pertaining to specific equipment. Field personnel are cautioned that such
information is sometimes in error, and appropriate cross-checks will be made to verify the
reasonableness of information contained in manuals.
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15.1.2 Other Ancillary Data
Other data, such as GIS and satellite mapping data are useful for siting and analysis of the data
collected for this project. Here is a partial list of some data that will be useful to this program.
Standard Google Earth layers;
Markers for schools to be monitored, with pop-up box indicating name, address, and
pollutants to be monitored;
Other schools in the area;
Airports;
Major roadways in the vicinity of the school, which is a standard Google Earth layer;
and;
Demographics of the area.
15.1.5 National Weather Service Data
Meteorological information is gathered from the U.S. Weather Service stations across the
nation. Parameters include: temperature, relative humidity, barometric pressure, rainfall, wind
speed, wind direction, cloud type/layers, cloud cover and visibility range.
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16.0 Data Management
16.1 Background and Overview
As laboratory analysis is completed, ERG will submit the data to the Air Quality System
(AQS). The processing of the data through AQS will be handled in a method consistent with
the existing data processing activities. Namely, the data will be screened to ensure that the data
are properly formatted and use valid coding values (for example, ensure the site id is valid).
Once the data have passed this first set of validations, the data will undergo a statistical
evaluation within AQS; the data and evaluation results will be reviewed verified and
reprocessed if necessary. Once the data are deemed of acceptable quality, they are available
from AQS. for analysis. EPA will promote the public availability of quality assured data
through the project web site. This section will detail how the data will be managed both by the
UATMP contractor and EPA.
16.2 UATMP Contract Data Management
This section describes the data management operations pertaining to field monitoring supported
by ERG, with an overview of the operations and analyses performed on raw (as-collected) data.
These operations include data recording, validation, transformation, transmittal, reduction,
analysis, management, storage, and retrieval.
The sample tracking and CoC information are entered into the ERG LIMS. All users
must be authorized by the Program Manager. The following privilege levels are
defined:
Data Entry Privilege - The individual may see and modify only data within the
LIMS that he or she has personally entered;
Administration Privilege - Data Administrators for the database are allowed to change
data as a result of QA screening and related reasons.
The Data Administrator is responsible for performing the following tasks on a regular basis:
1) merging/correcting the duplicate data entry files and 2) running verification/validation
routines, correcting data as necessary and generating summary data.
16.2.1 Data Recording
Data entry, validation, and verification functions are all integrated in the ERG LIMS.
Procedures for providing all laboratory notebook information and subsequent data entry are
provided in SOP ERG-MOR-039 for Maintaining Laboratory Notebooks.
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16.2.2 Data Validation
Data validation is a combination of checking that data processing operations have been carried
out correctly and of monitoring the quality of the field operations. Data validation can identify
problems in either of these areas. Once problems are identified, the data can be corrected or
invalidated, and corrective actions can be taken for field or laboratory operations. The following
validation functions are incorporated to ensure quality of data entry and data processing
operations:
Completeness Checks - When the data are processed, certain completeness criteria
must be met. For example, each sample must have a start time, an end time, an
average flow rate, dates analyzed, and operator and technician names.
Data Retention - Raw data sheets are retained on file at ERG for a minimum of five
years after the close of the contract, and are readily available for audits and data
verification activities. After five years, hardcopy records and computer backup media
are disposed.
Statistical Data Checks - Errors found during statistical screening will be traced back
to original data entry files and to the raw data sheets, if necessary. These checks shall
be run on an annual schedule and prior to any data submission to AQS. Data validation
is the process by which raw data are screened and assessed before they can be included
in the main data base.
16.2.3 Data Transformation
Calculations for transforming raw data from measured units to final concentrations use
standardized procedures listed in the individual SOPs or subcontractor's QAPP. All data are
double checked to ensure there are no incorrect transformations. All new spreadsheets also
go through the laboratory contractor's internal peer review, to ensure that all data submitted
are accurate. The reviewer uses hand calculations and visual verification to review all data
reported to the EPA and S/L agencies are valid following guidelines outlined in SOP ERG-
MOR-057. Separate SOPs for Developing, Documenting, and Evaluating the Accuracy of
Spreadsheet Data are presented in SOP ERG-MOR-017.
16.2.4 Data Transmittal
Data transmittal occurs when data are transferred from one person or location to another or
when data are copied from one form to another. Some examples of data transmittal are
copying raw data from a notebook onto a data entry form for keying into a computer file and
electronic transfer of data over a computer network. Each individual SOP discusses the
procedures for determining the calculations of concentrations as well as data entry. ERG will
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report all ambient air quality data and information specified by the AQS User's Guide1. The
data and information will be fully screened and validated and will be submitted directly to the
AQS via electronic transmission, in the format of the AQS, and in accordance with the annual
schedule.
16.3 Data Tracking
The ERG LIMS database contains the necessary input functions and reports appropriate to
track and account for the whereabouts of specific samples during processing operations. The
following input locations are used to track sample location and status:
Laboratory (initial receipt)
Sample receipt;
Canister number (VOC only);
Filter package for the laboratory (filter numbers in each package are recorded);
Laboratory (receipt from field)
Package receipt (package is opened and contents are logged in);
Samples are stored in correct locations (i.e., carbonyl tubes, XAD resin, and PUF are
stored in separate refrigerators, metals filters are stored in the ICP-MS laboratory,
and canisters are stored in the laboratory); and,
Refrigerator, by refrigerator number.
Security of the data in the UATMP database is ensured by the following controls:
Password protection on the data base that defines three levels of access to the
data;
Regular password changes (quarterly for continuing personnel);
Logging of all incoming communication sessions, including the originating
telephone number, the user's ID, and connect times; and
Storage of media including backup tapes in locked, restricted access areas.
16.4 EPA Data Reporting Requirements
Below are the data reporting requirements that must be adhered. If a S/L APCD is not familiar
with submitting HAPs or meteorological data, please refer to the document in the Reference
Section at the end of this chapter.
HAPs Sample Analyses - Quality assured ambient monitoring data shall be reported to the U.S.
EPA's AQS database (http://www.epa.gov/ttn/airs/airsaqs) not later than 14 calendar days
following sample collection. All data, including any values below MDL, shall be reported to
AQS. Under no circumstances are data value substitutions (e.g., /^ MDL) acceptable.
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Meteorological - Hourly scalar and vector wind speed and direction data will be downloaded
from the data loggers concurrent with sample pickup from each site (i.e., every 6th day) and
submitted for data processing and reporting to AQS. EPA will provide additional instructions
once the specific equipment types are determined.
16. 5 EPA OAQPS Data Management
The AQS is EPA's primary ambient air quality repository. In order to have the ability to submit
data to AQS, organizations must be provided access to a screening group, which defines which
monitors may be updated by the organization. Once the data has been validated by AQS, the
data must undergo a statistical evaluation to check for any pattern anomalies in the dataset.
Once that has been reviewed, the data can then be "posted" to be made available to the public.
All data that is collected for the SATMP will be submitted to the AQS using a screening group
established by EPA exclusively for this project. This includes any samples gathered and/or
analyzed by organizations other than ERG. Once the data is submitted to AQS, ERG will
perform the above mentioned statistical analysis of the data, but will not post the data at this
time.
On a frequent basis, EPA personnel will review the statistically evaluated data submitted by
ERG. Once a site has completed the study period and the data has been reviewed by EPA, ERG
will post the data for that site to be made available in AQS EPA health and air quality science
will analyze data and publically post analysis results on the project web site.
Reference:
1. Air Quality System User's Guide, http://www.epa.gov/ttn/airs/airsaqs/manuals/manuals.htm
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17.0 Assessment and Response Actions
An assessment is defined as an evaluation process used to measure the performance or
effectiveness of the quality system or the establishment of the monitoring network and sites and
various measurement phases of the data operation.
The results of quality assurance assessments indicate whether the control efforts are adequate or
need to be improved. Documentation of all quality assurance and quality control efforts
implemented during the data collection, analysis, and reporting phases is important to data
users, who can then consider the impact of these control efforts on the data quality. Both
qualitative and quantitative assessments of the effectiveness of these control efforts will identify
those areas most likely to impact the data quality and to what extent. In order to ensure the
adequate performance of the quality system, the EPA OAQPS and EPA Regional office will
perform the following assessments. Table 17-1 illustrates the assessments and when those
assessments will be performed.
Assessing Agency
EPA
EPA
Regional Offices
Type of Assessment
PTs
TSAs
Network Siting and Reviews
Agency Assessed
Analytical
Laboratory and
their subcontract lab
Analytical
Laboratory and
their subcontractor
S/L agencies
Frequency
At the
beginning of
the program
At the
beginning of
the program
At the
beginning of
the program
Tablel7-l Assessment Summary
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17.1 Project Planning and Assessment Activities
17.1.1 Network Siting and Reviews
In identifying specific monitoring locations on school grounds, EPA Regional, S/L APCD staff
and school officials will consider the following types of information:
Emission information, such as emission density maps for the region in which the
monitor is located and emission maps showing the major sources of emissions;
Best professional judgment;
GIS updates;
Access and safety issues; and,
Meteorology.
17.1.2 Technical Systems Audits
A TSA is a thorough and systematic on-site qualitative audit, where facilities, equipment,
personnel, training, procedures, and record keeping are examined for conformance to the QAPP.
EPA OAQPS staffer its designee will perform TSAs on the project contract laboratory and its
subcontractor. Other laboratories that participate in the program will have a TSA performed by
the Regional offices. Key personnel to be interviewed during the audit are those individuals
with responsibilities for: planning, field operations, laboratory operations, QA/QC, data
management, and reporting. To increase uniformity of the TSA, an audit checklist will be
developed and used. This checklist is based on the EPA G-71 guidance. The audit team will
prepare a brief written summary of findings, organized into the following areas: planning, field
operations, laboratory operations, quality assurance/quality control, data management, and
reporting. Problems with specific areas will be discussed and an attempt made to rank them in
order of their potential impact on data quality. The audit finding form has been designed such
that one is filled out for each major deficiency that requires formal corrective action. The
finding should include items like: systems impacted, estimated time period of deficiency, site(s)
affected, and reason of action. The finding form will inform the Division about serious
problems that may compromise the quality of the data and therefore require specific corrective
actions. They are initiated by the auditors, and discussed at the debriefing. During the
debriefing, if the audited group is in agreement with the finding, the form is signed by the
group's branch manager or his designee during the exit interview. If a disagreement occurs, the
auditors will record the opinions of the group audited and set a time at some later date to
address the finding at issue. OAQPS and the audited organization will work together to solve
required corrective actions.
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17.1.3 Proficiency Testing
Laboratory bias will be determined by the analysis of known reference analytes prepared by
independent laboratories, i.e., the PT samples. The UATMP contract laboratory supporting the
school monitoring project currently participates in the EPA's national PT program that supports
the NATTS and non-NATTS laboratories. The PTs for some of the compounds will be created
by Alion Inc., an EPA independent contractor. For compounds that are not currently in the
EPA's National PT program, they will be purchased by an independent PT provider. The
provider will be identified at a later date.
The PT is an assessment tool for the laboratory operations only. An EPA's Contract laboratory
independent from the UATMP contract laboratory creates "blind" samples. Upon receipt, the
laboratory logs in the samples and performs the normal handling routines as any other sample.
The PT is analyzed in accordance with the SOPs. Then the results are reported to the EPA. The
contract laboratory that creates the PT samples will write PT report and sends a copy of the
results to the laboratory and the EPA OAQPS QA coordinator. Any results outside of the
EPA's acceptance criteria are then noted in the PT report.
Reference:
1. EPA Guidance on Technical Audits and Related Assessments for Environmental Data Operations
(QA/G-7), May 2006. http://www.epa.gov/quality/qa docs.html
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18.0 Reports to Management
This section describes the quality-related reports and communications to management
necessary to support SATMP monitoring and the associated data acquisition, validation,
assessment, and reporting. Since this is a short term program, it is envisioned that one report
will be issued; a QA final report (QAFR).
18.1 QA Final Report
After the monitoring has been completed, the OAQPS staff will gather PT data, and precision,
bias and completeness information from the collocated monitoring and perform a Data Quality
Assessment (DQA). The DQA process is discussed in Section 20.0 of this QAPP. Please
reference that section for details.
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19.0 Data Review
This section describes how the UATMP contractor's procedures that will be utilized to perform
data review and validation.
19.1 Data Review Design
The contractor LEVIS is used to facilitate data storage, retrieval, analysis, and reporting. Data
summaries, QC charts, and other graphs, are generated in a cost-effective manner and aid in
maintaining consistent data quality. All data reported by ERG will use a flagging system, as
specified by the UATMP QAPP. Each sample received at the ERG Laboratory is logged into
the ERG LEVIS. The accompanying field data forms are reviewed to verify that all data entry
is complete and correct. The personnel performing the data review:
are familiar with typical diurnal concentration variations (for example, benzene,
toluene, and xylene concentrations usually increase and decrease together, since the
occurrence of these compounds is attributed to mobile sources);
are familiar with the type of instrument malfunctions which cause characteristic trace
irregularities;
recognize that cyclical or repetitive variations (at the same time each day or at periodic
intervals during the day) may be caused by excessive line voltage or temperature
variations (note that nearby source activity can also cause erroneous or non-
representative measurements}; and
recognize that flow rates showing little or no activity often indicate flow problems, or
sample line leaks.
Information used to validate air toxics data includes:
Multi-point calibrations - the multipoint calibrations are used to establish proper initial
calibration and can be used to show changes in calibration.
Instrument logs - all activities and samples analyzed are entered into the log books to
track the samples throughout the measurement procedures.
Blanks replicate and spike results - these QC indicators can be used to ascertain
whether sample handling or analysis is causing bias in the data set.
These data will include summaries for the monitoring locations in the respective cities, analysis
and interpretation of data trends for that group of prevalent compounds, illustration of changes
in ambient air concentrations of the most prevalent components of urban air pollution from year
to year, completeness report and collocated and duplicate results from the field and replicate
results from the laboratory.
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The reliability and acceptability of environmental analytical information depends on the
rigorous completion of all the requirements outlined in the QA/QC protocol. During data
analysis and validation, data are filtered and accepted or rejected based on the set of QC criteria
listed in the individual SOPs. The data are critically reviewed to locate and isolate spurious
values. A spurious value, when located, is not immediately rejected. All questionable data,
whether rejected or not, are maintained along with rejection criteria and any possible
explanation. Such a detailed approach can be time-consuming but can also be helpful in
identifying sources of error and, in the long run, save time by reducing the number of outliers.
19.2 Data Review
Prior to performing any statistical calculations, the reported data from the chain of custody
forms are checked to ensure accurate transcription. The value is double-checked and a
comparison to previously recorded data is made. Using conveniently formatted and bound
prepared data recording forms is essential; hardcopies of data can also be obtained directly from
measuring devices equipped with the necessary digital recording peripherals. Usually, this
method of recording data is sufficient if the hardcopies are properly labeled and filed, although
a periodic check will be performed to ensure the proper operation of such a device.
The collected data are reviewed by the laboratory contractor's project Analyst and the Task
Leader. The data are scrutinized daily to eliminate the collection of invalid data. The analyst
records any unusual circumstances (no matter how minor) during analysis (e.g., power loss or
fluctuations, temporary leaks or adjustments, operator error) on the chain of custody form and
notifies the analytical Task Leader.
19.3 Data Verification
Data verification consists of confirmation by examination and provision of objective
evidence that specified requirements have been fulfilled. The specific requirements are QC
checks, acceptable data entry limits, etc. Data validation is confirmation by examination and
provision of objective evidence that the particular requirements for a specific intended use are
fulfilled. Intended use deals with data of acceptable quality to permit making decisions at the
correct level of confidence. The following sections outline data validation and usability
requirements.
At least 10% of the database is checked to verify its validity. Items checked include original
data sheets, checks of all calculations (from calibration to sample analysis), and data transfers.
As the data are checked, corrections are made to the database as errors or omissions are
encountered. If errors are located, all of the data is checked to verify data quality. The
analytical reviewer examines all data for overall data quality and completeness. The project
Program Manager reviews all data before data are reported to the EPA.
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19.4 Data Reduction, Validation, and Reporting
A sample analysis logbook is maintained to detail pertinent sample information at the time of
analysis. Entries include site code, sample date, analysis date, and electronic file names.
Chromatograph and area count reports from each detector are printed for each analysis and the
analytical database for each analysis acquires, integrates, and stores the analytical data. Project
data are processed using a personal computer system containing the software. The data are
reported with the chromatogram and detailed information. Electronic copies of the data are
stored on the contractors LIMS server. The analytical procedures performed during the
monitoring program will be checked against those described in the QAPP and the SOPs.
Deviations from the QAPP will be classified as acceptable or unacceptable, and critical or
noncritical. Acceptance criteria are stated in each method and in Section 6.9 of this document.
QC samples and procedures performed during the monitoring program will be checked against
those described in Section 7 of this QAPP. Other QC results (matrix/method spike recoveries,
blank analysis, duplicate analysis, etc.) will be reviewed as well. All results outside specified
parameters will be discussed with the EPA for corrective action. In some cases, reference
methods have guidance on corrective action. Where available, the guidance in the reference
methods will be followed. Otherwise, the data will be flagged and reported to the EPA.
Documentation of equipment and instrument calibration (e.g., monitoring equipment and
analytical instruments) will be checked against the values used in data collection. The
documentation will be checked to ensure that the calibration:
Was performed within an acceptable time prior to the sampling dates;
Includes the proper number of calibration points;
Was performed using appropriate standards for the reported measurements; and
Had acceptable checks to ensure that the measurement system or analytical system was
stable when the calibration was performed.
The data processing systems will be checked by using raw data for which calculated values are
already known. The example data will be put into the system and the calculated results
compared to the known values.
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20.0 Data Validation, Verification and Analysis
This section was taken from the UATMP contract QAPP. Many of the processes for verifying
and validating the measurement phases of the data collection operation have been discussed in
Section 19. This section will outline how ERG will produce data that will meet the stated
objectives by performing software tests, plotting, and other methods of analysis.
20.1 Process for Validating and Verifying Data
20.1.1 Verification of Data
After a reporting batch is completed, a thorough review of the data will be conducted for
completeness and manual and electronic data entry accuracy. For the chromatographic data,
the entries are reviewed to reduce the possibility of entry and transcription errors. Once the
data are transferred to the ERG LIMS database, the data will be reviewed for routine data
outliers and data outside acceptance criteria. These data will be flagged appropriately.
Appropriate data qualifiers or flags can be found in the SOPs.
20.1.2 Validation
Records of all samples will be retained on file for 5 years, valid or invalid. Information will
include a brief summary of why the sample was invalidated along with the associated flags.
This record will be available on stored electronic media. Certain criteria based upon the
laboratory analyst's judgment have been developed that will be used to invalidate a sample or
measurement (i.e., water in cartridges, vacuum on canister too low, etc.). In all cases the sample
will be returned to the laboratory for further examination. When the laboratory analyst reviews
the CoC forms, he/she will look for possible problems. Filters that have flags related to obvious
contamination, filter damage, or field accidents will be examined immediately. Upon
concurrence of the associated laboratory analyst and the Analytical Coordinator, these samples
will be invalidated.
20.2 Data Analysis
Data analysis refers to the process of interpreting the data that are collected. Although there are
a large number of parameters to analyze, many of these parameters present similar
characteristics. The following describe software programs, described below, that helps with
analysis of the data.
Spreadsheets - Spreadsheets allow the user to input data and statistically analyze, plot and
graph linear data. This type of analysis will allow the user to see if there are any variations in
the data sets. In addition, various statistical tests such as tests for linearity, slope, intercept or
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correlation coefficient can be generated between two strings of data. Time series plots can
help identify the trends. Large jumps or dips in concentrations, periodicity of peaks, and
expected or unexpected relationships among species.
VOCDat - Recently, the EPA has made software available that can analyze data. One such
program is VOCDat, developed by Sonoma Technology, Inc., under contract to EPA. ERG has
a subcontract with Sonoma Technology, Inc., who provides VOCDat to S/L agencies. VOCDat
is a Windows-based program that provides a graphical platform from which to display collected
VOC data; to evaluate data according to specified quality control procedures; and for
exploratory data analysis. This program will enable ERG to rapidly validate and release their
air toxics VOC data to AQS. VOCDat displays the observed VOC concentrations using scatter,
fingerprint, and time series plots. Customizable screening criteria may be applied to the data
and the quality control codes may be changed for individual data points as well as for the entire
sample on all plots. VOCDat allows a user to find out the percentage a particular compound is
of the total. This test allows the user the ability to see if the data exceed the 3 sigma rule for
outliers.
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21.0 Reconciliation with Data Quality Objectives
21.1 Reconciling Results with DQOs
The DQOs for the air toxics monitoring network were developed in Section 6. The following is
excerpted from section 6.9.
In order to better evaluate potential impacts of air toxics at some schools in the U.S.,
monitoring will commence at selected locations. If the following criteria are met, the data will
be considered of sufficient quantity and quality for the decision-making to commence as
described in section 6.3:
1. Data are collected with a coefficient of variance (precision) and bias as stated In
Tables 6-1 through 6-3;
2. Data completeness Is 100%, that Is at least 10 samples will be collected;
3. MDLs are at or below those specified In Tables 6-1 through 6-3 and;
4. Where applicable, sufficient samples are collected when the predominant wind
direction Is from the source(s) In question.
This section of the QAPP will outline the assessment procedures that OAQPS QA staff will
follow to determine whether the data complies with the stated goals by performing a Data
Quality Assessment (DQAs) that is described in EPA QA/G-9: Guidance for Data Quality
Assessment1. The DQA will be detailed in the QAFR that is discussed in Section 18, Reports to
Management.
For the stated DQO, the assessment process must follow statistical routines. The following five
steps will discuss how this will be achieved.
21.2 Five Steps of DQA Process
As described in EPA QA/G-9, the DQA process is comprised of five steps. The steps are
detailed below.
Step 1: Review DQOs and Sampling Design - Section 6 of this QAPP contains the details for
the DQOs, including defining the objectives of the SATMP and stating the MQOs. Section 8.0
of this QAPP contains the details for the sampling design, including the rationale for the design,
the design assumptions, and the sampling locations and frequency.
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Step 2: Conduct Preliminary Data Review - A preliminary data review will be performed to
uncover potential limitations to using the data, to reveal outliers, and generally to explore the
basic structure of the data. The first step is to calculate basic summary statistics, generate
graphical presentations of the data, and review these summary statistics and graphs.
Step 3: Select the Statistical Test - OAQPS staff will generate summary statistics for each of
its primary and QA samplers. The summary statistics will be calculated from only valid
samples. The following statistical tests will be performed:
> Examination of precision of the data as described in Section 12.1.3;
> Examination of bias from the PT data.
OAQPS will generate graphs and tables to present the results from the summary QA statistics.
Step 4: Draw Conclusions from the Data - If the MQOs are met, and the study design
acceptable, then it can be assumed that the program QA objectives have been met. This
conclusion can be included in the QAFR. If any MQOs are not met, then these will be noted in
the QAFR as well.
Step 5: Action Plan Based on Conclusions from DQA - The QAFR will be presented to EPA
management and analysis staff when completed. It is outside of the scope of the QAPP or
QAFR what actions might follow this school monitoring program. However, the information
from this program will be used in considering and undertaking any additional study or
mitigation actions, if needed.
References:
1. Guidance for the Data Quality Assessment Process EPA QA/G-9 U. S. Environmental
Protection Agency, QAD EPA/600/R-96/084, July 1996.
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