United States Office of Air Quality EPA-454/R-01-001
Environmental Protection Planning and Standards December 2000
Agency Research Triangle Park, NC 27711
Air
Quality Assurance
Guidance Document
Final
Quality Assurance Project Plan:
PM2.5 Speciation Trends
Network Field Sampling
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Foreword
This document represents the Quality Assurance Project Plan (QAPP) for the field operations involved
in the PM2 5 Speciation Trends Network (STN). This QAPP was generated using the U.S.
Environmental Protection Agency (EPA) Quality Assurance (QA) regulations and guidance described
'mEPA QA/R-5, EPA Requirements for Quality Assurance Project Plans and the accompanying
document EPA QA/G-5, Guidance for Quality Assurance Project Plans. All pertinent elements of
the regulations and guidance are addressed in this QAPP.
This document has been reviewed by EPA Regional Offices responsible for implementing the STN in
their respective Regions, the QA Manager for EPA's Office of Air Quality Planning and Standards
(OAQPS), the EPA Technical Monitors for the network, and the QA Manager for the contract
laboratory for the STN. It is considered acceptable that the Reporting Organizations (ROs) of the state
and local air pollution agencies use this document in lieu of writing their own field QAPP if the EPA
Regional Offices sign the approval page (see following approval page).
Please note that from time to time, technical guidance documents, will be sent out to the Delivery Order
Project Officers, whom will distribute these to the State and Local Agencies. These should be added
to this QAPP in the office and field. Appendix A-7 is designed to accommodate these technical
guidance documents that will have updated information concerning quality assurance and quality control
issues that may affect how the STN is operated.
Mention of corporation names, trade names, or commercial products does not constitute endorsement
or recommendation for use.
The following persons may be contacted concerning the contents of this document. All inquiries can be
made to:
Dennis Mikel OAQPS-MQAG MD-14 Research Triangle Park, NC mikel.dennisK@epa.gov
James Homolya OAQPS-MQAG MD-14 Research Triangle Park, NC homolya.james@epa.gov
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Acronyms and Abbreviations
ADQ audit of data quality
AIRS aerometric information retrieval system
AMTIC Ambient Monitoring Technical Information Center
ANSI American National Standards Institute
APDLN air pollution distance learning network
APTI (EPA) Air Pollution Training Institute
ASQC American Society for Quality (Control)
CAA Clean Air Act
CAFDF custody and field data form
CAR corrective action request (form)
CASAC (EPA) Clean Air Scientific Advisory Committee
CFR Code of Federal Regulations
CMD (EPA) Contract Management Division
COC chain of custody
CV coefficient of variation
DBMS data base management system
DFR draft finding report
DGM dry gas meter
DOPO (EPA) delivery order project officer
DQA data quality assessment
DQO data quality objective
EC/OC elemental carbon/organic carbon
EDXRF energy-dispersive X-ray fluorescence
EMAD (EPA) Emissions, Monitoring, and Analysis Division
EPA Environmental Protection Agency
FR Federal Register
FR findings report
FRM Federal Reference Method (for PM2 5 sampling)
GALP good automated laboratory practices
GLP good laboratory practices
h hour
1C ion chromatography
IMPROVE Interagency Monitoring of Protected Visual Environments (network or sampler)
ISO International Organization for Standardization
IUPAC International Union of Pure and Applied Chemistry
L/min liters per minute
LCD liquid crystal display
LSPM laboratory services program manager
M25 mass of PM25
m3 cubic meter
MASS Mass Aerosol Speciation Sampler (URG, Corp.)
max./min. maximum/minimum (thermometer)
-------
min minute
mL milliliter
mmHg millimeters of mercury (pressure)
mo month
MQAG (EPA) Monitoring and Quality Assurance Group
MQO measurement quality objective
MSA metropolitan statistical area
MSR management systems review
NAAQS national ambient air quality standard
NAMS national air monitoring station
NAREL National Air and Radiation Environmental Laboratory
NERL (EPA) National Exposure Research Laboratory
NIST National Institute of Standards and Technology
NTN national trends network
OAQPS Office of Air Quality Planning and Standards
OAR (EPA) Office of Air and Radiation
ORIA (EPA) Office of Radiation and Indoor Air
PAMS photochemical air monitoring station
PE performance evaluation
PM25 particulate matter, 2.5 micrometer diameter
PO project officer
QA quality assurance
QAM quality assurance manager
QAPP Quality Assurance Project Plan
Qavg average flow rate
QC quality control
QMP quality management plan
RAAS Reference Ambient Air Sampler (Andersen Instruments, Inc.)
R&IE Radiation and Indoor Air
RO reporting organization
R&P Rupprecht and Patashnick Co.
RSC regional speciation coordinator
RTI Research Triangle Institute (the STN support laboratory)
RTP Research Triangle Park (North Carolina)
SASS Spiral Ambient Speciation Sampler (Met One Instruments, Inc.)
SHAL sample handling and archival laboratory
SLAMS State and local air monitoring station
SOP standard operating procedure
SPM (laboratory) services program manager
STN (PM25) Speciation Trends Network
SVOC semivolatile organic compound
T & A testing and acceptance
TSA technical systems audit
USEPA United States Environmental Protection Agency
VOC volatile organic compound
XRF X-ray fluorescence
0 C degree Celsius
ug/m3 micrograms (of PM) per cubic meter (of air sampled)
ill
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Tables
Number Section Page
3-1 Distribution List 3 1
6-1 Critical Measurements in the PM2 5 STN 6 3
6-2 Checklist of PM2 5 STN Field Activities 6 4
6-3 Critical Filter and Denuder Holding and Use Times 6 9
6-4 Critical Documents and Records 6 11
7-1 MQOs for Total Measurement Error 7 3
9-1 STN Reporting Package Information 9 5
10-1 Schedule of Activities for State and Local PM2.5 STN Field Site Participants 10 2
10-2 Schedule of Activities for Contracting STN Laboratory 10 3
10-3 Propo sed Sites for the PM2.5 STN 10 5
11-1 Summary of Information Provided by Speciation Sampler 11 2
11-2 STN Field Operations Corrective Actions 11 6
12-1 Explanation of STN Custody and Field Data Form 12 4
14-1 MQOs and Associated QC Activities for the PM2.5 STN 14 2
15-1 Testing and Acceptance Criteria Checklist for PM2.5 Speciation Samplers 15 2
15-2 Preventive Maintenance of STN Field Equipment 15 3
16-1 Acceptance Criteria and Calibration and Maintenance Frequencies for
PM2.5 Chemical Speciation Samplers 16 4
16-2 Calibration Standards for PM2.5 Chemical Speciation Samplers 16 6
17-1 STN Field Equipment and Supplies 17 2
19-1 Laboratory Data Record Archival Summary 19 8
19-2 Validation Check Summaries 19 9
19-3 Raw Data Calculations 19 10
19-4 Data Transfer Operations 19 12
20-1 Assessment Summary 20 1
21-1 QA Reports to Management for STN 21 2
22-1 Data Verification Activities for the PM2.5 STN 22 2
22-2 Quality Control Data for STN Data Verification and Validation 22 6
22-3 Statistical Validation Limits for Blanks 22 10
22-4 Statistical Validation Limits for Routine Data 22 10
22-5 Mapping of Outlier Flags onto AIRS Codes 22 11
22-6 Automated Range Checks 22 11
22-7 Data Verification and Validation Summary 22 12
IV
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Figures
Number Section Page
4-1 STN Organization 4 2
4-2 Laboratory Technical Management and Staff Organization for STN
Filter Analysis and Data Reporting 4 9
6-1 Summary of STN Project Operations 6 2
6-2 Sample Analysis Delivery Order Process 6 6
6-3 Diagram of Laboratory Filter Processing and Analysis Activities,
by Filter Type 6 7
11-1 Quality Bulletin 11 4
12-1 Custody and Field Data Form for the PM2 5 STN 12 3
14-1 STN QA/QC Report Form 14 4
19-1 STN Data Flow Overview 19 2
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PM2 5 STN QAPP
Section No. 1
Re vision No.: 4
Date: 6/00
Page 1 of 2
1.0 QA Project Plan Identification and Approval
Title: Quality Assurance Project Plan for the PM2 5 Speciation Trends Network
QAPP Category: Category 1
By signing below, the monitoring agency commits to implement the latest version of the Quality
Assurance Project Plan referenced above and the EPA approves this monitoring agency QAPP
submittal.
State/Local/Tribal Agency
Print Name:
PM 2 5 Monitoring Coordinator
Print Name:
Quality Assurance Officer
Print Name:
Air Program Director
Print Name:
Print Name:
Print Name:
Project Officer
Signature:_
Signature:_
Signature:
PM2 5 Monitoring Coordinator
EPA Regional Approval
Signature:_
Quality Assurance Manager
Signature:_
Signature:_
Date:
Date:
Date:
Date:
Date:
Date:
Print Name:
Grants, Audits & Procurement
Program Director
Signature:
Date:
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PM2 5 STN QAPP
Section No.2
RevisionNo.: 4.1
Date: 12/00
Page 1 of 4
2.0 Table of Contents
Section
Foreword
Acknowledgments
Acronyms and Abbreviations
Tables
Figures
1.0 QA Project Plan Identification and Approval
2.0 Table of Contents
3.0 Distribution
4.0 Project/Task Organization
4.1 Trends Network Coordination Activities
4.2 Trends Network Field Site Activities Organization
4.3 Trends Network Laboratory Activities Organization
5.0 Background and Problem Definition
5.1 Background
5.2 Problem Definition
5.3 PM2 5 Speciation Sampling Techniques and Ongoing Research
5.4 Monitoring Network Design Considerations
Page
Revision
Dale
i
ii
iii
vi
vii
1/1
1/6
1/4
1/10
2/10
6/10
7/10
1/3
1/3
1/3
2/3
3/3
4.1
4.1
4.1
4
4
4.1
4.1
4.1
4.1
4.1
12/00
12/00
12/00
6/00
6/00
12/00
12/00
12/00
12/00
12/00
6.0 Project/Task Description
6.1 Description of Work to be Performed
6.2 Field Activities
6.3 Laboratory Activities
6.4 Schedule of Activities
6.5 Proj ect Assessment Techniques
6.6 Proj ect Records
7.0 Quality Objectives and Criteria For Measurement Data
7.1 Data Quality Objectives Process
7.2 Development of DQOs for the PM2 5 Chemical STN
7.3 Measurement Quality Objectives
7.4 References
1/11
1/11
3/11
5/11
8/11
10/11
10/11
1/4
1/4
1/4
2/4
4/4
4.1
12/00
4.1
12/00
8.0 Special Training Requirements/Certification
8.1 Training
8.2 Certification
8.3 Contacts for More Information
1/3
1/3
3/3
4/3
4.1
12/00
9.0 Documentation and Records
9.1 Information in the Management and Organization
Reporting Package
1/6
1/6
4.1
6/00
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2.0 Table of Contents (continued)
PM2 5 STN QAPP
Section No.2
RevisionNo.: 4.1
Date: 12/00
Page 2 of 4
Section
9.2
9.3
9.4
9.5
9.6
Information in the Field Operations Reporting Package
Information in the Laboratory Operations Reporting Package
Information in the QA Reporting Package
Reports to Management
Archival and Retrieval of Data Reporting Packages
10.0 Sampling Process Design
10.1 Scheduled Proj ect Activities, Including Management Activities
10.2 Rationale for the Design
10.3 References
Page
Revision Date
1/6
3/6
4/6
5/6
6/6
1/8
1/8
3/8
4.1
12/00
11.0 Sampling Methods Requirements
11.1 Sample Collection and Preparation
11.2 Sampling/Measurement System Corrective Action Process
11.3 Avoiding Sample Contamination; Temperature and
Holding Time Requirements
12.0 Sample Handling and Custody Requirements
12.1 Introduction
12.2 Presampling Sample Handling and Custody Procedures
12.3 Postsampling Sample Handling and Custody Procedures
12.4 Filter and Sample Archival in the STN Laboratory
13.0 Analytical Methods Requirements
14.0 Quality Control Requirements
14.1 QC Checks
14.2 QC Samples
14.3 Collocated Samplers
14.4 Calculations of Accuracy, Bias, Precision, and Completeness
14.5 References
1/7
1/7
3/7
5/7
1/6
1/6
1/6
5/6
6/6
1/1
1/8
3/8
5/8
5/8
6/8
4.1
12/00
4.1
12/00
4.1
4.1
12/00
12/00
15.0 Instrument/Equipment Testing, Inspection, and Maintenance Requirements
15.1 Testing and Acceptance Criteria
15.2 Maintenance
15.3 Critical Spare Parts
16.0 Instrument Calibration and Frequency
16.1 Overview
16.2 Calibration and Verification of Field Instrumentation
16.3 Calibration and Verification of Laboratory Instrumentation
1/4
1/4
1/4
3/4
1/6
1/6
1/6
3/6
4.1 12/00
4.1 12/00
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PM2 5 STN QAPP
Section No.2
RevisionNo.: 4.1
Date: 12/00
Page 3 of 4
2.0 Table of Contents (continued)
Section Page Revision Date
17.0 Inspection/Acceptance for Supplies and Consumables Vi 4.1 12/00
17.1 Purpose 1A
17.2 Critical Supplies and Consumables Vi
17.3 Acceptance Criteria 1A
17.4 Tracking and Quality Verification of Supplies and Consumables 2/2
18.0 Data Acquisition Requirements (Nondirect Measurements) 1/2 4.1 12/00
18.1 Acquisition of Nondirect Measurement Data 1II
19.0 Data Management 1/12 4.1 12/00
19.1 Overview 1/12
19.2 Data Management Activities at the STN Laboratory 3/12
19.3 Data Management Activities at the RO 3/12
19.4 Recommended Data Management Practices 5/12
19.5 Data Validation 7/12
19.6 Data Transformations 10/12
19.7 Data Transmittal 11/12
19.8 Data Reduction 11/12
19.9 Data Analysis 11/12
19.10 Data Storage and Retrieval 11/12
20.0 Assessment and Response Actions 1/7 4.1 12/00
20.1 Types of Assessments 1/7
20.2 Assessment Frequency 1/7
20.3 Acceptance Criteria 2/7
20.4 Assessment Schedules 2/7
20.5 Assessment Personnel 2/7
20.6 Assessment Reports 5/7
20.7 Implementation of Response Actions 6/7
20.8 References 7/7
21.0 Reports to Management 1/5 4.1 12/00
21.1 NAMS Reporting 1/5
21.2 Additional Quality-Related Reports for the STN 4/5
22.0 Data Review, Validation, and Verification Requirements 1/12 4.1 12/00
22.1 Data Verification and Validation Responsibilities 1/12
22.2 Corrective Action Reporting Process 1/12
22.3 Use of QC Information for Verification and Validation 5/12
22.4 Use of Calibration Information for Verification and Validation 5/12
22.5 Level 0 Verification 7/12
22.6 Level 1 Data Validation 8/12
22.7 Data Screening Techniques used by RTI 9/12
22.8 Treatment of Deviations from Requirements 11/12
22.9 Verification and Validation Criteria: Field Component 12/12
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PM2 5 STN QAPP
Section No.2
RevisionNo.: 4.1
Date: 12/00
Page 4 of 4
2.0 Table of Contents (continued)
Section
23.0 Validation and Verification Methods
23.1 Interorganizational Responsibilities for Data Validation
23.2 Personnel Responsibilities within the Reporting Organization
23.3 Completion of Level 0 Data Verification and Validation
23.4 Identification of Outliers and Data Flagging Techniques
24.0 Reconciliation with Data Quality Obj ectives
24.1 DQO for Chemical Speciation Trends
24.2 Interim Evaluations of Data Quality
24.3 Assessing and Reporting Chemical Speciation Trends
24.4 Reconciling Other Chemical STN Research Objectives
24.5 References
Page
1/4
1/4
2/4
2/4
3/4
1/7
1/7
2/7
6/7
6/7
7/7
Revision Date
4.1 12/00
4.1
12/00
Appendix A
A-l
A-2
SOP5000 STN Condensed Standard Operating
Procedure for Field Installation Of PM2 5 Speciation
Samplers
SOPS 100 STN Condensed Standard Operating
Procedure For The Met One SASS
9/99
9/99
A-3 SOP5200 STN Condensed Standard Operating
Procedure For The Andersen RAAS
9/99
A-4 SOP5300 STN Condensed Standard Operating
Procedures For The URG MASS 400 And
URG MASS 450
9/99
A-5 SOP5400 STN Packing Instructions for the Speciation Sampler
Modules
12/00
A-6 CY-2001 Normal and Alternate Sampling Schedule for the Speciation Trends
Network 1
A-7 Technical Guidance Document Updates
1
12/00
12/00
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PM2 5 STN QAPP
Section No. 3
RevisionNo.: 4.1
Date: 12/00
Page 1 of 4
3.0 Distribution
A hardcopy of this QAPP has been distributed to the individuals listed in Table 3-1. The Regional Speciation
Coordinators (RSCs) will be responsible for distributing the QAPP to each field site and regional analysis laboratory
in the environmental data operations of the STN. The RSCs may also want to provide a copy of this QAPP to their
Regional QA Managers. Upon completion, the QAPP for the PM2 5 STN will be available on the EPA's Ambient
Monitoring Technical Information Center (AMTIC) Web site.
TABLE 3-1. DISTRIBUTION LIST
Name
Address
Phone No.
Electronic Mail
OFFICE OF AIR QUALITY PLANNING & STANDARDS
Vickie Presnell
James Homolya
Joann Rice
Dennis Mikel
Michael Papp
USEPA
Office of Air Quality Planning &
Standards
MQAG(MD-14)
RTP,NC 27711
USEPA
Office of Air Quality Planning &
Standards
MQAG(MD-14)
RTP,NC 27711
USEPA
Office of Air Quality Planning &
Standards
MQAG(MD-14)
RTP,NC 27711
USEPA
Office of Air Quality Planning &
Standards
MQAG(MD-14)
RTP,NC 27711
USEPA
Office of Air Quality Planning &
Standards
MQAG(MD-14)
RTP,NC 27711
(919)541-7620
(919)541-4039
(919)541-3372
(919)541-5511
(919)541-2408
presnell.vickie@epa.gov
homolya.james@epa.gov
rice.joann@epa.gov
mikel.dennisK@epa.gov
papp.michael@epa.gov
CONTRACTING ANALYSIS LABORATORY
R.K.M. Jayanty
Robert Perkins
Research Triangle Institute
3040 Cornwallis Road
P.O. Box 12194
RTF, NC 27709
Research Triangle Institute
3040 Cornwallis Road
P.O. Box 12194
RTF, NC 27709
(919)541-6483
(919)541-6800
rkmj@rti.org
rlp@rti.org
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PM2 5 STN QAPP
Section No. 3
RevisionNo.: 4.1
Date: 12/00
Page 2 of 4
TABLE 3-1. (continued)
Name
James Flanagan
Address
Research Triangle Institute
3040 Cornwallis Road
P.O. Box 12194
RTF, NC 27709
Phone No.
(919)541-7739
Electronic Mail
jamesf@rti.org
DELIVERY ORDER PROJECT OFFICERS
M. Kantz
P. Schraufnagel
K.Wang
Region 2 (East)
USEPA-Region2
Raritan Depot /MS 103
2890 Woodbridge Avenue
Edison, NJ 08837-3679
Region 5 (Midwest)
USEPA-Region 5
77 West Jackson Blvd. / AR-18J
Chicago, IL 60604-3507
Region 8 (West)
USEPA-Region 8
999 18th Street / 8TMS-Q
Suite #500
Denver, CO 80202-2466
(732) 321-6690
(312)886-5955
(303)312-6738
kantz .marcus@epa. go v
schraufnagel.patricia@epa.gov
wang .kenneth@epa. go v
REGIONAL SPECIATION COORDINATORS
Region 1
RSC
Mary Jane
Cuzzupe
Region 2
RSC
Clinton Cusick
Region 3
RSC
Theodore Erdman
Region 4
RSC
Herb Barden
Richard Guilliot
Region 5
RSC
Gordon Jones
USEPA-Region 1
New England Regional Laboratory
60 Westview Street
Lexington, MA 02421
USEPA-Region 2
Raritan Depot /MS 103
2890 Woodbridge Avenue
Edison, NJ 08837-3679
USEPA-Region 3
1650 Arch St
Philadelphia, PA 19103-2029
USEPA-Region 4
Science and Ecosystem Support
Division
980 College Station Road
Athens, GA 30605-2720
USEPA-Region 5
77 West Jackson Blvd. / AR-18J
Chicago, IL 60604-3507
(781) 860-4383
(908) 321-6881
(215)597-1193
(706) 355-8737
(404) 562-9050
(312)353-3115
cuzzupe.maryjane@epa.gov
cisocl/c linton@epa.gov
erdman.ted@epa.gov
barden.herbert@epa.gov
guiillot.richard@epa.gov
jones.gordon@epa.gov
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PM2 5 STN QAPP
Section No. 3
RevisionNo.: 4.1
Date: 12/00
Page 3 of 4
TABLE 3-1. (continued)
Name
Region 6
RSC
Kuenja Chung
Region 7
RSC
Mike Davis
Region 8
RSC
Joe Delwiche
Region 9
RSC
Matthew Plate
Region 10
RSC
Karen Marasigan
Address
USEPA-Region 6
First Interstate Bank Tower at Fountain
Place
1445 Ross Avenue
Dallas, TX 75202-2733
USEPA-Region 7
ENSV/EMWC
25 Funston Road
Kansas City, KS 66115
USEPA-Region 8
999 18th Street / 8P2-A
Suite #500
Denver, CO 80202-2466
USEPA-Region 9
75 Hawthorne St. / PMD-3
San Francisco, CA 94105
USEPA-Region 10
1200 Sixth Ave. /ES-095
Seattle, WA 98101
Phone No.
(214)665-8345
(913)551-5081
(303)312-6448
(415)744-1493
(206) 553-1792
Electronic Mail
chung .kuenj a@epa. go v
davis.michael@epa.gov
delwiche j o seph@epa. go v
plate.matthew@epa.gov
marasigan.karen@epa.gov
MINITRENDS STATE CONTACTS
Tom Moore
Arizona
Tom Tamanini
Florida
Bob Lamorte
Illinois
Jerry Sheehan
Massachusetts
Bern Johnson
Missouri
Arizona Department of Environ. Quality
Air Quality Division
3033 North Central Avenue, 5th Floor
Phoenix, AZ 85012
Hillsborough County EPC
1410 N. 21" Street
Tampa, FL 33605
Cook County Dept. of Environmental
Control
Maybrook Civic Center
1500 May wood Drive
May wood, IL 60609
State of Massachusetts DEP
Air Quality Bureau
37 Shattuck Street
Lawrence, MA 01 843
State of Missouri
DNR/DEQ/APCP
P.O. Box 176
Jefferson City, MO 65102-0176
(602) 207-2353
(813)272-5530
(708)865-6184
(978) 975-3215,
ext. 309
(573) 526-2027
moore.tom@ev. state. az.us
tamanini@epcj anus . epchc . org
ccdects@wwa.com
jerry. sheehan@state.ma.us
nrjohnb@mail.dnr.state.mo.us
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PM2 5 STN QAPP
Section No. 3
RevisionNo.: 4.1
Date: 12/00
Page 4 of 4
TABLE 3-1. (continued)
Name
Dirk Felton
New York
Daniel E. Harman
North Dakota
Steve Aalbers
Oregon
Norman Glazer
Pennsylvania
Ed Michel
Texas
Robert Neal
Olson
Utah
Jim Frost
Washington
Address
New York State Dept. of Environmental
Conservation
Division of Air Resources
Bureau of Air Quality Surveillance
80 Wolf Road, Room 403
Albany, NY 12233-3256
North Dakota Department of Health
Environmental Engineering
1200 Missouri Avenue
P.O. Box 5520
Bismarck, ND 58506-5520
Oregon Department of Environmental
Quality
81 1SW Sixth Avenue
Portland, OR 97204
Technical Services Group
Air Management Services
1501 EastLycoming Street
Philadelphia, PA 19124
TNRCC
P.O. Box 13087, Mail Code 165
Austin, TX 7871 1-3087
State of Utah DEQ
Division of Air Quality
2861 Parkway Blvd.
West Valley City, UT 841 19
Washington Department of Ecology
Air Quality Program
P.O. Box 47600
Olympia, WA 98504-7600
Phone No.
(518)457-9137
(701)328-5188
(503) 229-6798
(215)685-1085
(512)239-1384
(801) 877-0764
(425)649-7108
Electronic Mail
hdfelton@g w. dec . state .ny . us
dharman@state.nd.us
aalbers. steven@deq. state. or. us
norman.glazer@phila.gov
emichel@tnrcc. state.tx.us
rolson@deq. state. ut. us
JFR046 1 @ecy .wa.gov
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PM2 5 STN QAPP
Section No. 4
RevisionNo.: 4.1
Date: 12/00
Page 1 of 10
4.0 Project/Task Organization
This section provides all parties involved in the Speciation Trends Network with a clear understanding
of their roles and the lines of authority, communication, and reporting for the project.
The organization of the STN involves three interacting entities: Federal and Regional EPA offices, state
and local air monitoring and reporting organizations, and one or more contracting laboratories to service
the collection sites with supplies, sample analysis, and data reporting. To make the best use of available
resources and to meet demanding timelines for collection and analysis of samples, the flow of
information and samples must be optimally organized. The deployment and operation of the network is
a shared responsibility among all the involved parties. This section describes the roles of all parties and
establishes the lines of communication and reporting, with the goal of facilitating a smoothly operating
network.
Information on the STN's organization is first presented from the perspective of all involved agencies
and contractors. Section 4.1 and Figure 4-1 provide a unified view of the network's operating
structure and lines of communication and reporting. Block A of Figure 4-1 points out the network's
coordination activities, led by EPA's Office of Air Quality Planning and Standards with advice from the
Chemical Speciation Workgroup, the Clean Air Scientific Advisory Council (CASAC), the Expert
Panel on the EPA Speciation Network, and a group of advisors from EPA's National Exposure
Research Laboratory (NERL). The Quality Assurance (QA) Manager, the network's Project Officer
(PO), the EPA-(RSCs, and three Delivery Order Project Officers (DOPOs) are also included in the
network's planning and coordination activities component.
Section 4.2 focuses on the roles of the EPA Regional QA Offices and the State and local agencies that
will operate the 54 sampling sites on a day-to-day basis. Block B of Figure 4-1 shows the field
activities the State and local agency STN sampling and QA/Quality Control (QC) personnel will
perform and their lines of communication to the DOPOs, the STN PO, and the contract laboratory.
Section 4.3 and Figure 4-2 discuss the contracting laboratory's managerial and technical organization
and roles and illustrate the laboratory's interactions with the EPA DOPOs and PO and with the State
and local agencies, which will operate the samplers and ship the samples to the laboratory. Block C of
Figure 4-1 shows the contract laboratory and the EPA Regional QA Laboratories.
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PM2 5 STN QAPP
Section No. 4
RevisionNo.: 4.1
Date: 12/00
Page 2 of 10
PMzs STN Coordination Activities
OAQPS Group Leader
R. Scheffe
PM2.5 Chemical
Speciation Workgroup
Project Manager
J. Homolya
Delivery Order
Project Officers
East: M. Kantz
Midwest: P. Schraufnagel
West: K. Wang
Trends Network Laboratory Activities
Chemical Speciation
Contract Laboratory (RTI)
State and Local
Agencies
Lab QA Auditing
and Technical
Assistance OR IA
-NAREL
M. Clark
Program Manager R. Jayanty
Field QA
Assessments
E. Braganza
Figure 4.1 STN Organization
4.1 Trends Network Coordination Activities
The STN is made up of three interactive working groups, as illustrated in Figure 4-1. Block A of this
figure includes the PM2 5 Chemical Speciation Workgroup, the OAQPS network coordination office,
three advisory groups, the QA Manager, and the PO and DOPOs. These groups assist in
coordinating, advising, planning, and managing the activities of the STN field and laboratory activities.
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4.1.1 PM2 5 Chemical Speciation Workgroup
The PM2.5 Chemical Speciation Workgroup was formed to provide input and review of all aspects of
the chemical Speciation program, which includes the 54 trends national air monitoring station (NAMS)
network sites and up to 250 nonroutine State and local air monitoring station (SLAMS) sampling sites.
Members of the group include personnel from EPA OAQPS, EPA Regions, the EPA Office of
Research and Development's (ORD's) NERL, and State and local air monitoring organizations. This
workgroup meets monthly or more often to discuss various planning, operational, and QA issues.
Meetings are organized and planned by OAQPS. The workgroup acts in an advisory role and has
assisted (and will continue to assist) in the development and review of the speciation network's
implementation plan, field and laboratory standard operating procedures (SOPs). In January 2001, a
new QA workgroup will form that will oversee the development of QAPP, Quality Management Plan
(QMP) and other QA guidance documents.
4.1.2 Office of Air Quality Planning and Standards Coordination Office
OAQPS has oversight concerning the quality of the Nation's ambient air data. OAQPS has developed
specific regulations for the development of a quality system as found in 40 Code of Federal
Regulations (CFR) Part 58, Appendix A. One specific element of this quality system is the
development and coordination of the PM2 5 STN. OAQPS will ensure the orderly development and
operation of this network through the following activities:
Coordinating and overseeing the STN
Providing a contractual vehicle for the manufacture, procurement, and distribution of PM2 5
speciation samplers and their components
• Working with the EPA Regions and State/local organizations to determine the best sampling
locations
Providing a contract vehicle for a laboratory to support the field sites and provide filter analysis
and associated functions
• Developing documents for the STN, including the strategic plan for the quality system of trends
sites, SOPs for field sites and laboratory operations, and the QAPP
Developing field and laboratory personnel requirements and training activities
Securing national experts and advisors to answer specific technical questions and review the
network; responding to recommendations provided by national experts and advisory
committees
Assessing the species concentration information entered into the Aerometric Information
Retrieval System (AIRS) database
• Developing an information management system and other means to archive data, assess data
sets, and release trends information to stakeholders, data users, and the general public
Initiating and instituting a communications network and acting as a liaison to groups working on
the STN data sets
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Interacting with Regional, State, and local agency personnel and the contracted laboratory
concerning the setup and operation of the STN and its data results
Ensuring the success of the network by coordinating various oversight activities such as
management systems reviews (MSRs) and technical systems audits (TSAs).
Most budgetary and technical planning activities will be coordinated through the OAQPS. The
Monitoring and Quality Assurance Group (MQAG) within the Emissions, Monitoring, and Analysis
Division (EMAD) is ultimately responsible for the implementation of the Speciation Trends Network.
This includes most of the technical components (with support from ORD, Regional offices and
laboratories, and State and local agencies) and the resource estimates underlying program
implementation. The QA Coordinator (QAC) will provide guidance and oversight to the development
of the STN quality system, including this QAPP. Resource guidance necessary for the State and Tribal
Assistance Grants (STAG) distribution is coordinated through the Planning, Resources, and Regional
Management staff within OAQPS. In addition, the Information Transfer and Program Integration
Division (ITPID) is responsible for the AIRS data management system.
4.1.2.1 Speciation Trends Network Quality Assurance Coordinator
The STN-QAC, Mr. Dennis Mikel, will coordinate the implementation of the quality system of the
STN. The QAC will:
• Review the national network's QAPP and other quality-related documents and coordinate
their approval
Ensure that RTFs SOPs are reviewed and updated as required
Coordinate with the QA workgroup, the Regional QA laboratories and others to ensure that
periodic systems reviews and performance reviews of the field and laboratory activities are
accomplished.
periodic of the field and laboratory activities
4.1.2.2 Speciation Trends Network Project Manager
Mr. James Homolya is the delegated OAQPS program manager of the STN. He is responsible for the
OAQPS activities that are implemented as part of normal data collection activities. His responsibilities
include:
•communication with EPA Project Officers and EPA QA personnel on issues related to routine
sampling and QA activities;
•understanding EPA monitoring and QA regulations and guidance, and ensuring all key personnel
understand and follow these regulations and guidance;
•reviewing acquisition packages (contracts, grants, cooperative agreements, inter-agency
agreements) to determine the necessary QA requirements.
•developing budgets and providing program costs necessary for EPA allocation activities
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•ensuring that all personnel involved in environmental data collection have access to any training or
QA information needed to be knowledgeable in QA requirements, protocols, and technology;
•recommending required management-level corrective actions.
4.1.3 Advisory Panels
Three advisory panels will consult with OAQPS on technical matters related to the STN. These panels
are the Clean Air Scientific Advisory Committee, the Speciation Expert Panel, and a panel of
ORD/NERL technical experts.
Clean Air Scientific Advisory Committee—This committee is a subcommittee of the Science
Advisory Board (SAB) and reports directly to the SAB administrator. It will serve as the principal
review body for the PM2 5 monitoring program and will emphasize review of the speciation network.
This committee will interact with the OAQPS coordination office.
Expert Panel on Speciation—The Expert Panel on Speciation was formed to advise OAQPS on
structural and technical matters related to the PM2.5 speciation network. It is composed of recognized
technical experts in the fields of network monitoring strategy, sampling and monitoring methods for
PM2 5, physical and chemical characterization of fine particles, and data analysis and interpretation.
Members of the Speciation Expert Panel are Drs. Petros Koutrakis (chair), Tom Cahill, Phil Hopke,
Lara Gundel, and John Ondov, and Mr. Robert Stevens. This panel has focused on review of the
guidance documents for the speciation network and instrumentation. It will report to and interact with
the OAQPS STN coordinating office.
ORD/NERL Expert Panel—This panel is composed of scientists and engineers in EPA's ORD, in
particular the NERL. Members of this panel (including Drs. Russel Weiner and Paul Solomon) led
efforts to design, test, and approve PM2 5 mass samplers as Federal Reference Methods (FRMs).
They have also bench- and field-tested most of the available PM2 5 speciation samplers. This panel will
be called upon for expert advice on technical and operational aspects of the speciation samplers,
handling samples, and laboratory analyses of PM2.5. They will communicate with the OAQPS
coordinating office.
4.1.4 Speciation Trends Network Project Officer
The STN Project Officer (PO), Ms. Vickie Presnell, is with EPA/OAQPS. She will be the liaison
between the EPA Contracts Management Division and the various contractors and vendors. The PO
will interact with others in OAQPS, EPA Contracts Management Division personnel, the DOPOs, and
the contract laboratory's Services Program Manager to ensure contract details are followed, including
the submittal and review of required draft and final semi-annual data summary reports from the
contracted laboratory.
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4.1.5 Regional Speciation Coordinator
The Regional Speciation Coordinator (RSC) will receive PM2.5 speciation analytical needs requests
from State or local agencies. The RSC then consolidates all requests received from States within his or
her region and submits them to the DOPO for that region. The RSC interacts with the State and local
agencies and provides assistance on field related QA issues.. Any special equipment or nonroutine
analytical needs requested by the monitoring agencies are relayed to the STN Project Office for action.
The names of the RSCs are listed in Section 3.0, Table 3-1.
4.1.6 Delivery Order Project Officer
The Delivery Order Project Officer (DOPO) will consolidate the requests for sampling media and
sample analysis received from the RSCs. A DOPO will be assigned to the East (Regions 1-4 and
Puerto Rico), Midwest (Regions 5-7), and West (Regions 8-10) of the United States. Once the STN
is in full operation, the delivery order process is expected to become fairly routine because all sites in
this network will request analyses of specific analytes on samples collected every third day for a number
of years. The DOPO will communicate with the STN Project Officer and with the laboratory
contracted for analysis of filters and other sampling media. The DOPO will also review the monthly
analytical data packages from the contracting laboratory, ensure they are complete, and, after approval,
make arrangements for payment of the invoice for the various delivery orders.
EPA Contracts Management Division—The Contract Management Division (CMD) is located within
the Office of Acquisition Management (OAM). CMD is responsible for all communications with
vendors and extramural contract organizations. For the STN, it will:
• Provide a Contract Officer to represent the government.
Develop national contracts for speciation sampler purchases, some filter purchases, sample
shipping, and laboratory support and analyses of speciation sampler filters.
Communicate with OAQPS to provide the above services.
4.2 Trends Network Field Site Activities Organization
Personnel from State and local agencies will install speciation samplers at NAMS sites, operate the
sites, and promptly ship samples to the contract laboratory to ensure schedules are met. State or local
personnel will also implement QC procedures as given in the SOPs for sampler operation and sample
shipping. Another line of communication from the States will be to the DOPO and the RSC. Dialogues
concerning sampling equipment and laboratory supply or sample analysis problems occur here.
Interested State and local personnel may also participate in Chemical Speciation Workgroup
discussions.
State or local site operators and supervisors should communicate directly with the contracted sample
analysis laboratory only when there are concerns about timely shipment and receipt of supplies,
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sampling media, and data packages. Field sites will also communicate with OAQPS and with the EPA
Regional QA laboratories for technical assistance and QA services. The State or local site operations
and records will be subject to systems and performance reviews, which will be coordinated through the
EPA's Speciation Trends Network QA Manager.
4.2.1 Organization for Routine Field Sampling Operations
The State and local air monitoring agencies are responsible for day-to-day operation of STN sites.
The management and technical organizations already in place at these agencies will be used to
implement operations. Personnel will need to be assigned and organized to accomplish the following
tasks, among others:
Site selection and platform and utility installations
Purchase, receipt, acceptance testing, and installation of sampler, calibration equipment, and
meteorological equipment
Operator hiring and training
Communication with the RSC and DOPO regarding sample analysis task orders
Scheduled operation of the sampling site, including internal QA/QC activities
Monthly validation of draft data sets received from the contract laboratory
Interactions with STN network management personnel. Participation in external QA activities.
4.2.2 QA/QC Organization for State and Local Agency Field Site Operations
Quality assurance activities supporting the STN sites will be arranged through the QA Manager at each
State or local agency. QA personnel will be identified prior to field data collection and will be assigned
and organized to accomplish the following tasks, among others:
Implementation of the quality system for the STN
• Review and approval of the network's field QAPP or acceptance of this as the field QAPP
Site inspections and review of procedures to ensure specified QA/QC checks are being made
and measurements systems are in control. Issuance of corrective action memoranda and
monitoring of follow-up actions.
• Participation in monthly validation of draft data sets received from the contract laboratory
Arrangement for and participation in QA activities called for by EPA Regional offices.
4.3 Trends Network Laboratory Activities Organization
Block C of Figure 4-1 illustrates the organization of the trends network laboratory activities sector.
Laboratory activities will include QA related work by the EPA Office of Radiation and Indoor Air
(ORIA) and the EPA Region 1 Laboratory, and routine laboratory work by Research Triangle
Institute (RTI), the contracted field site supply and filter analysis laboratory.
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4.3.1 EPA QA Laboratories
EPA's Office of Radiation and Indoor Air (ORIA) laboratories in Montgomery, Alabama and Las
Vegas, Nevada will be working in concert with the EPA Region 1 Laboratory, and OAQPS. These
two laboratories are the National Air and Radiation Environmental Laboratory (NAREL) in
Montgomery, Alabama and the Radiation and Indoor Air (R&IE) laboratory in Las Vegas, Nevada.
These laboratories will:
• Provide speciation laboratory QA support to the State and local agencies and to the contracted
analysis laboratory
Provide QA auditing and technical assistance to the field sites and to the contracting analysis
laboratory.
The EPA QA laboratories will be establish lines of communication with the following:
Access to the STN PO to send and receive information concerning the performance of the
contracted laboratory and the status and quality of operations at the field site/contract
laboratory interface
Contact with OAQPS coordinators and technical monitors, their advisory panels, and the QA
office
Interactions with the contracted laboratory to conduct systems and performance reviews.
4.3.2 Contracted Filter Analysis Laboratory Organization
Figure 4-2 illustrates the organization of management, QA, and technical staff for the PM2 5 analysis
laboratory.
Management Organization—The PM2 5 speciation analysis laboratory is headed by a Laboratory
Services Program Manager (LSPM) and a Deputy Manager. The LSPM receives site servicing
delivery orders from the EPA DOPOs and is the official contact person for sending or receiving
sampling media and for release of analytical and other data sets. The management office will oversee
activities of the technical laboratories and the data management office. The LSPM will also receive and
respond to quality systems findings provided by the laboratory QA Manager and staff as well as to
external audit reports.
Quality Assurance Organization—The laboratory's QA Office is staffed by a QA Manager (QAM),
a Deputy QA Manager, and support staff. The QA Manager interacts with each of the technical area
laboratories or offices to conduct scheduled and follow-up systems and performance evaluations (PEs).
Findings from internal QA activities are reported to the LSPM for review and action. This office
summarizes QA activities for inclusion in the monthly reports to EPA. The QA Office also prepares
and updates the laboratory QAPP and associated SOPs.
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Technical Organization—The laboratory is composed of seven entities that will provide the following
analytical services and data report packages to STN sites:
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Sample Handling and Archival Laboratory (SHAL) Supply each Speciation Trends
Network site with all necessary sampling supplies to include coated denuders, sampling filter
media, assembled sampling modules, shipping containers, and documentation paperwork. (The
laboratory will use hardware purchased by the State or local organization; the contractor will
supply only the filters.)
Gravimetric and Microscopy Laboratories. PM2 5 mass by microbalance determination.
Scanning electron and optical microscopy studies of particles.
Elemental Analysis Laboratory. Elements by energy-dispersive X-ray fluorescence
(EDXRF) determination.
Cations/Anions Laboratory. Cations and anions by ion chromatography (1C) analysis.
Carbon Species and Semivolatile Organic Carbon Compounds Laboratory. Carbon
species by elemental carbon/organic carbon (EC/OC) analysis. Determination of semivolatile
organic compounds (SVOC's) as needed.
Denuder Refurbishment Laboratory. Denuder refurbishment.
Data Management Office. Track sampling media components and manage all data. This
includes issuance of monthly and quarterly data sets to State/local agencies and to the EPA
DOPO and entry of validated data to the AIRS database system.
Details on these activities can be found in the companion laboratory QAPP for this program.
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PM2 5 STN QAPP
Section No. 5
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5.0 Background and Problem Definition
For environmental pollutants, the term particulate matter (PM) is used to describe a broad class of
chemically and physically diverse substances that are natural in origin, emitted directly from stationary
and mobile sources, or formed in the atmosphere by reactions of gaseous emissions such as nitrogen
oxides, sulfur dioxide, and volatile organic compounds (VOCs).
5.1 Background
The CAA also requires EPA to revise or update the air quality standards based on review of the latest
scientific information on known and potential human health effects associated with PM levels typically
found in the ambient air. In fulfilling these obligations, the EPA recently reviewed the air quality criteria
and National Ambient Air Quality Standards (NAAQS) for PM and epidemiological evidence that
shows an association between ambient concentrations of PM and a range of serious health effects.
Based on the results of its review, the EPA revised and promulgated two new primary standards for the
fine fraction of PM (i.e., particles with aerodynamic diameters less than or equal to 2.5 • m, referred to
as PM2 5) and the regulatory requirements for monitoring the chemical composition of these particles.
In meeting the requirements to monitor and gather data on the chemical makeup of these particles, EPA
is establishing a chemical speciation network consisting of approximately 300 monitoring sites. These
sites will be placed at various NAMS and SLAMS across the Nation. It is currently anticipated that
54 of these chemical speciation sites will be used to determine, over a period of several years, trends in
concentration levels of selected ions, metals, carbon species, and organic compounds in PM2 5. Further
breakdown on the location or placement of the trends sites requires that approximately 20 of the
monitoring sites be placed at existing Photochemical Assessment Monitoring Stations (PAMS). The
placement of the remaining trends sites will be coordinated by EPA, the Regional offices, and the State
and local agencies. Locations will be primarily in or near larger Metropolitan Statistical Areas (MSAs).
The remaining chemical speciation sites will be used to enhance the required trends network and to
provide information for developing effective State implementation plans (SIPs). This QAPP focuses on
required measures for ensuring that data of adequate quality are provided by the 54 trends network
sites.
5.2 Problem Definition
The STN is a component of the National PM2 5 Monitoring Network. Although the STN is intended to
complement the activities of the much larger gravimetric PM2 5 measurements network component
(whose goal is to establish if NAAQS standards are being attained), STN data will not be used for
attainment or nonattainment decisions. The programmatic objectives of the STN network are:
Annual and seasonal spatial characterization of aerosols;
Air quality trends analysis and tracking the progress of control programs;
Compare the chemical speciation data set to the data collected from the IMPROVE
network; and
• Development of emission control strategies.
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Stakeholders in the STN will be those at EPA seeking to determine concentration trends of PM2 5
chemical species over a period of 3 or more years and decision-makers at State and local levels who
will use the data as input to models and for development of emission control strategies and
determination of their long-term effectiveness. Other users will be public health officials and
epidemiological researchers. However, expectations for data sets from the STN must be put in
context. A number of limitations are recognized, (for instance, the 24-h integrated sample approach,
taken every 3rd day, is not suitable for determination of diurnal patterns and may have limited use to
those who study acute health effects). EPA recognizes these data use limitations and limitations on the
sampling and analysis methodologies. Thus, EPA does not rule out the possibility that objectives,
requirements, and methods for speciation sampling may need to be adjusted in the future.
5.3 PM2 5 Speciation Sampling Techniques and Ongoing Research
The samplers will have the capability of collecting 24-h integrated samples. The three commercial
sampler designs currently available under the EPA sampler contract for use in the STN are the
Reference Ambient Air Sampler (RAAS™), the Mass Aerosol Speciation Sampler (MASS), and the
Spiral Ambient Speciation Sampler (SASS™). Another sampler that has been in use for several years,
the Interagency Monitoring of Protected Visual Environments (IMPROVE) sampler, is also available
for use. In the near future, Rupprecht and Patashnick Co. (R&P) Model 2300 will soon be available
to the ROs. However, this sampler must pass the EPA's acceptance procedures before it can be
considered for the STN. In addition to the R&P sampler, there are several sequential samplers that
will be commercially available in the near future. EPA is currently conducting tests on these instruments
and assuming that the sequential samplers pass these tests, the EPA will make these instrument available
to the ROs.
All filter-based STN samplers use Teflon™, nylon, and quartz filter media for the collection of target
analytes. The Teflon™ filter will be used to collect particles for the analysis of mass and metals
composition, samples to be analyzed for carbon components of particles will be collected on the quartz
filters, and samples for ion analysis will be collected on nylon and/or Teflon filters. Each sampler's
operating manual and the corresponding field SOP (refer to Appendix A-l through A-4) should be
consulted for further details.
At the recommendation of the Speciation Expert Panel, the operation and acceptable performance of
the commercial samplers have been tested (and continue to be tested) in a series of field and laboratory
research and intercomparison studies. The samplers are being tested against each other and against the
Federal Reference Method (FRM) sampler and historically accepted speciation samplers such as the
IMPROVE sampler and the Versatile Air Pollution Sampler (VAPS) in a four-phase study. In Phase I,
which occurred in the winter and spring of 1998/1999, tests were conducted in four cities (Philadelphia,
PA; Research Triangle Park, NC; Phoenix, AZ; and Rubidoux, CA) during the period to determine
response to differing aerosol compositions. Phase n took place in Seattle, WA; from March to July
1999. Phase in was carried out in Atlanta, GA, during the summer of 1999 as part of a Supersite
study. Phase IV is a 12-city mini-trends and operational evaluation study, to be operated by the States,
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in which each site will have at least two speciation samplers for comparison. The Mini-Trends Study
will begin in November 1999 and continue for 6 months. The Mini-Trends Study is a part of the STN.
Therefore, this QAPP will be used for the Mini-Trends Study and will be revised, based upon needed
improvements for the full STN.
Each phase of the testing program seeks to refine the samplers' designs and operation and to better
understand topics such as the following:
A sampler's ability to collect, size-selective, fine particle mass, sulfate, and elements;
A sampler's ability to collect carbonaceous aerosols and nitrate; and
The ease and reliability of a sampler's operation, including its ability to hold steady
calibrations of temperature, pressure, and flow.
5. 4 Monitoring Network Design Considerations
The design of the STN was influenced by the need to place sites primarily in populated areas of the
country and to link PM2 5 speciation data sets to data collected at collocated PAMS and PM2 5 mass
sampling sites. Appendix D of the Part 58 PM2.5 regulations (62 FR38763) provides the general
criteria to apply in choosing new monitoring stations for PM2.5. General requirements for chemical
speciation specify that approximately 20 sites must be located at existing type 2 PAMS sites. PAMS
network design and monitoring objectives are explained in Appendix D of Part 58, Code of Federal
Regulations (CFR).
Selection of the remaining STN sites was based on EPA recommendations, with review and advice
from State and local agencies. Most of the remaining sites will be located in MS As. Their specific
locations will be based on factors such as:
Location of existing PAMS and IMPROVE network sites
Geographic locations of MS As using 1996 population statistics
Ozone nonattainment areas
PM10 nonattainment areas.
STN sites will be placed at the one MSA community-oriented PM2 5 mass site that is experiencing the
maximum concentration in the area.
Sites will also be placed at population centers in the central, midwest, and southeast portions of the
country to bring the total number of STN sites to 54. Where feasible, sites will be equipped with 10-m
height meteorological towers and instrumentation to collect data on wind speed and direction,
temperature, and humidity.
Refer to Table 10-3 and Figure 10-1 for further information on the locations of sites in the PM2 5 STN.
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6.0 Project/Task Description
This section provides trends network partcipants with a background understanding of the STN project
and the types of activities to be conducted, including acquiring the samples; performing chemical
analysis; carrying out quality assurance/quality control goals and procedures; and meeting the schedules
for network implementation, operation and data reporting.
6.1 Description of th Work to be Performed
6.1.1 Overview of the STN Operations
The operation of the STN can be diagrammed as a series of interlocking field and laboratory activities.
Figure 6-1 depicts 10 steps involved in implementing and operating the network and the delineation of
responsibilities for required tasks. Each step is briefly described below:
1. The PM2 5 STN site contact person makes arrangements for purchase and delivery of
sampling equipment to the site. Information about field site contact names; mailing and
shipping addresses; telephone numbers; supplies; sampling schedule; and the requirements
for number and type of sample filters, denuders, and sample analyses is sent to the Regional
Speciation Coordinator by the site contact person or other State coordinator.
2. The RSC conveys the site's needs to the DOPO. The DOPO consolidates several
requests and informs the contract laboratory's Services Program Manager (SPM) of each
site's address, point of contact, sampling schedule, needed sampling equipment and filter
media, and suite of analytes. The DOPO authorizes the contract laboratory to begin
supplying the site, analyzing samples received, and sending analytical results. The DOPO
keeps the STN Project Officer informed about these requests.
3. The analytical support laboratory ships sampling supplies to the site contact address.
4. Site personnel conduct sampler quality control checks (e.g., time and date, leakage,
temperature, barometric pressure, flow rates, and cleanliness), conduct QC checks on the
meteorological sensors (e.g., examine anemometer and wind vane for damage; check real-
time data display for wind speed, wind direction, temperature, and relative humidity versus
independent observations), collect the PM2 5 samples, deploy and retrieve field or trip
blanks, pack all samples, complete the custody and field data forms, and download data
stored in the sampler's memory to a computer disk.
5. Site personnel ship routine samples and field data to the support laboratory. Nonroutine
and quality assurance samples are sent to the designated QA laboratory. The RSC informs
the site when there are nonroutine or QA samples and how and where to send them.
6. The support laboratory analyzes filter samples and conducts level 0 and level 1 data
validation. The data is sent to the State and locals who review and accept the level 0 and 1
validated data or provide edits. The information is sent back to RTI who corrects data.
RTI makes final AIRS database entry.
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7. The support laboratory archives filter extracts for 6 months. Upon request, the laboratory
can send filters back to the ROs who would like to store filters for a longer period of time.
RTI will archived the filters for three years.
8. The support laboratory prepares monthly analysis and QA/QC activity reports.
9. The support laboratory submits the monthly analysis report to STN site personnel for
review, further validation, and verification. This report is also submitted to the DOPO.
10. State and local personnel conduct level 2 and 3 data validations; questions about results are
directed to the laboratory through the DOPO. Data users and stakeholders interpret and
summarize the validated data sets to detect trends according to their own established
protocols.
I
PM2.5 STN Site
Contact Person
RSC
DOO
PM2.5 STN PO
1
5B
Contracted Support
and Sample
Analysis Laboratory
- Sampler QA checks
- Install sampling media
- Collect samples
- Pack and ship samples and field data
EPA QA Labs
Perform analysis and
report to States
- Sample analysis
- Conduct level 0, 1 data validations
- Data review by State/local
- Airs database entry
Filter and filter
extract archival
J
7
Assemble
monthly data and
QA/QA reports
9B
PM2.5 STN
DOPO
10
- Conduct level 2, 3 data validations
- Data summarization and interpretation
Figure 6.1 Summary of STN project operations
6.1.2 Field Site and Laboratory Measurements for the PM2 5 STN
Table 6-1 lists critical field and laboratory measurements for the PM2.5 STN and gives the methods to
be used to acquire the data.
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TABLE 6-1. CRITICAL MEASUREMENTS IN THE PM^ STN
Measurement and/or Analyte
Methodology
Field Site
Site name, sample date, and sample ID
Temperature, ambient (Celsius)
Temperature, ambient (Celsius)**
Relative humidity (percentage)**
Pressure, atmospheric (mmHg)
Date and elapsed sample time (h)
Flow rate, sampler (L/min)
Total volume sampled (m3)
Wind speed (m per s)**
Wind direction (degrees of compass)**
Free-form notes on sampling difficulties and unusual
conditions at the site
Commercial speciation sampler's sensor
Meteorological package
Meteorological package
Commercial speciation sampler's sensor
Commercial speciation sampler's clock and timer
Commercial speciation sampler's flow rate sensor
Commercial speciation sampler's display
Anemometer
Wind vane
Analytical Support Laboratory
Temperature, shipment cooler (Celsius)
Mass, PM2 5 (Teflon™ filter) (• g/filter and • g/m3 of air)
Elements (Teflon filter) (• g/m3)
Cations (various filters) (• g/m3)
Anions (various filters) (• g/m3)
Carbon species (• g/m3)
Digital thermometer
Balance, microgram
Energy-dispersive X-ray fluorescence (EDXRF) (Na
through Pb)
Ion chromatography (1C) (NH4+, Na+, K+)
1C (nitrate, sulfate)
Thermal/optical analysis (total, organic, elemental,
and carbonate carbon)
**
- Optional at site
6.2 Field Activities
6.2.1 Checklist of Field Activities
The field site operator and the sampling site he or she operates are considered the most important
components of the STN and its scientific output. Strict attention to procedures and constant awareness
of the possibility for sample contamination are keys to obtaining a valid sample. Table 6-2 lists the
activities the field site operator is expected to accomplish for the STN. The table also gives the
frequency at which the activity should be performed.
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TABLE 6-2. CHECKLIST OF PM,.S STN FIELD ACTIVITIES
Activity
Attend training sessions.
Assist with equipment selection, contact with RSC,
and ordering of laboratory analytical services.
Equipment (sampler, calibration or verification
devices, and so on) receipt, inspection, inventory,
and operability checkout. Maintain spare parts
inventory.
Install sampler(s) at site.
Sampler calibrations
QC checks of sampler operation (checks of time and
date display, leaks, ambient and interior temperature
sensors, pressure sensor, and flow rate).
Sampler operation. Includes preventive
maintenance, maintaining sampler cleanliness,
installing denuders and sampling media,
programming sampler start/end times, and keeping
field activities notes in site logbook and/or on field
data forms.
Retrieval and packaging of samples, field blanks, and
denuders into cooler. Completion of custody and
field data forms, and shipment of samples to
laboratory via Federal Express.
Data download from instrument
Participate in data validation training session.
Review initial data from laboratory; conduct levels 2
and 3 data validation. Inform DOPO of data
acceptability.
Communicate with State or local management, STN
management, and contract laboratory (through
DOPO).
Participate in scheduled STN QA activities (for
example, on-site and field office inspections,
handling of special QA samples, installation and
periodic operation of a collocated sampler).
Frequency
Once, prior to site operation.
Updated training as required.
Once, prior to site operation.
Once, initially, and whenever
new or replacement parts arrive.
Once, at beginning of STN
participation.
Prior to first sampling event;
annually thereafter or whenever
out-of-tolerance checks occur
that cannot be corrected;
following repairs affecting flow
rate.
Check dependent see table 14-1
Every 3rd day with dates and
start/end times specified by
EPA.
Every 3rd day for regular STN
operation.
As soon as practicable
Initial training. Follow-up
sessions. Monthly review of
data sets.
As required and appropriate.
As scheduled by EPA Office of
Air Quality Planning and
Standards (OAQPS) or EPA
Regional QA Officers.
Comment or
Reference
Document 2. 12,
Section 4
Refer to
Appendix A- 1
Refer to
Appendices A-2,
A-3, andA-4
Refer to Table 14-1
Appendices A-2,
A-3, andA-4
Cleaning process
must be thorough
and avoid
contamination of
sample pathways
Refer to
Appendix A- 1
Refer to PM2 5
Speciation Guidance
Document, Section
2.0, "Data Analysis"
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6.3 Laboratory Activities
The STN will require extensive laboratory activities. A single contract laboratory will be employed for
analysis of routine samples from the network. Research Triangle Institute has been chosen to fulfill
these duties. The following subsection summarizes the laboratory activities that will occur to support
the STN.
6.3.1 Presampling Activities
1. Teflon, nylon, and quartz filters will be received from various vendors and examined for
integrity and background analyte concentrations.
2. Filters (or their containers) will be numbered or otherwise identified to allow tracking and
accurate data entry.
3. Filters will be tested, equilibrated, and weighed as required and stored awaiting use.
4. Filters will be prepared or packaged for field activities.
5. The laboratory will maintain shipping/receiving supplies to include cooler containers, ice
substitute packs, and custody and field data forms.
6.3.2 Postsampling Activities
1. Shipments of filters bearing PM2 5 deposits will be received in the laboratory, checked for
integrity (damage, shipment temperature, and so on), and logged in. Information on the
custody and field data form will be reviewed.
2. Filters will be stored (refrigerated or frozen) until ready for analysis.
3. Filters will be promptly distributed to individual laboratories for weight determination and
other analyses so that strict time frames for completion of activities are met.
4. Results of analyses will be entered into the laboratory database.
5. Sampled volume data will be entered into the data entry system in order to calculate
concentrations of species in terms of a mass per unit volume of air sampled (• g/m3).
6. Filters and filter extracts will be archived (frozen or refrigerated) for 6 months.
7. Data will be transferred to the AIRS database, to the DOPO, and to the designated person
in the State operating the trends network site for review and approval.
8. All paperwork, including custody and field data forms, chromatographs, analyzer data
reports, results of QA/QC studies, and free-form notes, will be filed for ready retrieval and
inspection as required for at least a 3-yr period.
The details for these activities are included in the laboratory SOP, which are part of the contracting
laboratory's QAPP. Figure 6-2 is a simplified flow diagram of the sample analysis delivery order
process. Figure 6-3 is a flow diagram of handling and analysis steps for the filters with the exception
that the URG sampler also collects samples for ions on PTFE (Teflon).
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State identifies need for
analysis and forwards
request to RSC
RSC sends
consolidated
request to DOPO
DOPO consolidates
and forwards
request to contract
lab SPM
Sites collect
samples and
return filters to
contract lab
Contract lab
prepares and ships
filters and supplies
to sites.
-Routine
Contract lab
performs analysis
Field QA/nonroutine-
~Technical Assistance
EPA and regional
QA labs perform
analysis
RTI performs
Level 0/1 Data
Validation
• Data forwarded
I
/ Datat° / 30 Days / Data to 7
/ State / / DOPO /
Figure 6-2 Sample analysis delivery order process
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Page 8 of 1 1
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Figure 6-3. Diagram of laboratory field processing and analysis activities, by
filter type
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6.3.3 Critical Laboratory Processes and Measurements
In order to generate a mass concentration, the most critical measurements of the laboratory are the
unexposed filter preweights and the exposed filter postweights or concentrations in terms of
• g/filter.The difference between these two measurements provides the net weight of particles (or
particle components) in micrograms (• g) that, when combined with the field sampler air volume
in cubic meters (m3), provides a final concentration in micrograms per cubic meter (• g/m3). Table 6-1
lists all the analytes to be quantified for the STN samples.
6.4 Schedule of Activities
In order to ensure that the implementation of the additional trends sites is accomplished, many aspects
of the program must be completed in a timely, efficient fashion.
6.4.1 Planning Time Lines
Table 10-1 in Section 10.0 provides the key planning aspects of the program.
6.4.2 Implementation Time Lines
Other important dates must be met during implementation activities. They involve both laboratory and
field activities. One aspect of the field site implementation process that is critical is the time-efficient use
and return of denuders and filter media to the support laboratory. As shown in Table 6-3 and
stipulated in the Code of Federal Regulations (CFR), Teflon filters must be used at the field site
within 30 days (d) of presampling weighing or they must be reconditioned and reweighed.
Furthermore, the contracting laboratory must submit validated speciation concentration data to EPA
within 20 business d following receipt of any sample from the field. Therefore, it is critical that the
contract laboratory and the field sites develop, agree on, and consistently follow a schedule that will
satisfy the requirement that the mass of PM2 5 on Teflon filters be determined within 10 d after the
sampling period ends and that determination of all analytes be completed, validated, and submitted to
the DOPO for review and acceptance within 20 business d.
6.4.3 Field Time Lines
Table 6-3 indicates that filters should be collected and be prepared and ready for shipment to the
laboratory within 48 hours (h) of the end of the sample period to prepare for the next l-in-3 d sampling
period. Please see Appendix A-6 on the CY2001 calendar, which indicates the sample run days for
the STN. In some circumstances, this may not be practical or possible. If the agency cannot collect
the samples on weekend, then an alternate schedule must be adopted. Please see Appendix A-6 for
the Monday and Friday dates that must be collected. It is noted that if a Friday run is operated and
collected on Monday, as noted in the alternate schedule, then the hold time will be greater than 48
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hours. This should be noted on the COC form. Any other instance where a sample is not shipped
within 48 hours should also be noted.
TABLE 6-3. CRITICAL FILTER AND DENUDER HOLDING AND USE TIMES
Filter or Denuder Type
Teflon (*)
Quartz (*)
Nylon (*)
Nitric acid denuder (sodium
carbonate) (**)
Nitric acid denuder (magnesium
oxide) (**)
Field Deadlines
Use within 30 days of preweighing;
retrieve and must ship within 48 h
of sample completion.
Retrieve and ship within 48 h of
sample completion.
Retrieve and ship within 48 h of
sample completion.
Replace after 3 months' use.
Replace after 3 months' use.
Laboratory Deadlines
Condition and reweigh within 10
business d of receipt from field site.
Analyze filter catch within 20
business d of receipt of sample.
Analyze filter catch within 20
business d of receipt of sample.
Refurbish as required.
Refurbish or replace as required.
(*) Special deadlines for use and shipment may apply to field blank and collocated sampler filters.
(**) Limitations on denuder lifetime are tentative.
Data should be downloaded from the speciation samplers on the day of filter sample retrieval and
stored on two media (computer hard drive and diskette). Data may also be transmitted using a modem.
In addition, the most critical data values will also be recorded from each sampler's liquid-crystal display
(LCD) screens onto a custody and field data form and sent to the laboratory with the samples.
Figure 12-1 is an example of such a data form.
6.4.4 Data Assessment Time Line
Data Availabilit^-ln order to compare the speciation and routine samplers' mass data, data from the
routine sampler must also be available in AIRS. State/local requirements for data upload to AIRS is 90
d after the quarter in which the data were collected. However, the time frame for pre- and postsampling
weighing, as indicated in Table 6-3, is also a requirement for the routine samplers. Therefore, data for
the routine sampler evaluated could be available within 30 d of the sample end date. This requirement
is written into the laboratory contract with OAQPS. Submittal of routine sampler data as soon as
possible is encouraged if data assessment is to occur in a timely manner.
Assessments— After both routine (mass only) data and speciation data for a site are in the AIRS
database, OAQPS, Regions, and State and local agencies can use the AIRS data evaluation programs,
based on data quality assessment (DQA) techniques, to assess this information. This assessment will be
part of the level 2 and level 3 data validation process.
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6.4.5 OAQPS Reporting Time Lines
OA Reports—As mentioned in Section 3.0, OAQPS plans to develop a yearly QA Final Report
(QAFR) and an interpretive QA report every 3 yr. The yearly report will be based on a calendar year
and will be completed 6 months from the last valid entry of routine data by the State and local agencies.
The 3-yr QA report will be generated 9 months after the last valid entry of routine data by the State
and local agencies for the final year.
6.5 Project Assessment Techniques
An assessment is an evaluation process used to measure the performance or effectiveness of a system
and its elements. As used here, assessment is an all-inclusive term used to denote any of the following:
management systems reviews (MSRs), network reviews, technical system audits (TSAs), performance
evaluations (PEs) and, audits of data quality (ADQs). Table 20-1 specifies the agencies responsible for
these assessments.
6.6 Project Records
The field and laboratory programs will establish and maintain procedures for the timely preparation,
review, approval, issuance, use, control, revision, and maintenance of documents and records. Table
6-4 represents the categories and types of records and documents applicable to document control for
PM2 5 information. Information on key documents in each category is explained in more detail in
Section 9.0.
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TABLE 6-4. CRITICAL DOCUMENTS AND RECORDS
Categories
Record or Document Types
Management and organization
Organizational structure
Quality system strategic plan
Implementation plan
Reporting agency information
Personnel qualifications, training records, certifications
Quality management plan
Document control plan
EPA and State directives
Support contract documentation
Site information
Network description
Site characterization file
Site maps (paper or digital)
Site photographs
Environmental data
operations
QAPP
Standard operating procedures (SOPs), including operating manuals
Guidance document (laboratory)
Guidance document (sampling sites)
Field site and laboratory notebooks
Sample handling and custody records
Inspection/maintenance/safety records
Any original data (routine and QC data), including data entry forms and
diskette/hard drive data
Raw data
Data reporting
Data, summary and progress reports
Trends evaluation reports and other data summaries
Reports to management
Journal articles, papers, presentations
QA Reports
Data management
Data algorithms
Data management plans and flow charts
PM2 5 speciation data
Data management systems
Field and Laboratory Quality
Assurance
Calibration and QC check records
Good laboratory practices (GLP) documentation, including good automated
laboratory practices (GALPs)
Network reviews
Control charts
Data quality assessments (DQAs)
QA reports
System and performance review reports
Response or corrective action documentation
Site visits and audits (technical system audits)
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7.0 Quality Objectives and Criteria for Measurement Data
7.1 Data Quality Objectives Process
The data quality objectives (DQO) process is a strategic planning approach used to prepare for a data
collection activity in order to achieve data of adequate quality to support decision-making. The DQO
process helps to ensure that the type, quantity, and quality of environmental monitoring data will be
sufficient for the data's intended use, while simultaneously ensuring that resources are not wasted
collecting unnecessary, redundant, or overly precise data. The formal DQO process consists of the
following seven steps that allow an experimental design to be developed to meet specific decision
criteria specified by stakeholders in the decision, as described in EPA QA/G-4, Guidance for the
Data Quality Objectives Process (U.S. Environmental Protection Agency , 1994):
State the problem.
Identify the decision.
Identify the inputs to the decision.
Define the boundaries of the study.
Develop a decision rule.
Specify tolerable limits on decision errors.
Optimize the design.
A Speciation DQO Workgroup was established to develop and document DQOs for the PM2 5
chemical Speciation Trends Network (STN). The DQO process that the workgroup employed is fully
documented in its report (U.S. EPA, 1998), which is available online at the AMTIC Web page for
speciation:
http://www.epa.gov/ttn/amtic/pmspec.html
7.2 Development of DQOs for the PM25 Chemical STN
The primary DQO, detection of trends in the chemical speciation data, was defined as follows by the
EPA workgroup, who acted as stakeholders for the program:
... to be able to detect a 3 to 5 percent annual trend in the concentrations of selected chemical species
with 3 to 5 years of data on a site-by-site basis after adjusting for seasonality, with power of 0.80.
(U.S. EPA, 1999a)
[It should be noted that although the DQO statement says "3 to 5 percent" and "3 to 5 years," the
default assumptions in this QAPP will be detection of a 5 percent trend after 5 yr.]
Statistical power is defined as the likelihood that a particular statistical test will correctly reject the null
hypothesis when it is false. Because the null hypothesis is that a trend does not exist, the DQO
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statement means that there must be an 80 percent probability of detecting a trend of 5 percent after 5 yr
at any particular site, for any single analyte.
Several secondary objectives for data collected at the STN sites and other chemical speciation sites
were identified, but these were not evaluated quantitatively by the workgroup. Four important
secondary data uses are as follows:
Model evaluation, verification, and/or validation
Emission inventory
Source attribution
Spatial and seasonal characterization of aerosol distributions.
The desirable data quality characteristics for these secondary uses are probably significantly different
from those applicable to trend assessment. This document only considers the needs of the primary
objective for trend detection.
The DQO study also concluded that by sampling every 3rd d for 5 yr, trends greater than 5 percent (or
less than -5 percent) per year can be detected for sulfate, calcium, and total carbon, on a single-site
basis. For nitrate, however, the annual trend must exceed ±6.3 percent to be detected with a power of
80 percent. The decision-makers concluded that this was not sufficiently different from the 5 percent
goal to require adjustment to the sampling design. Sampling daily instead of every 3rd d provides little
improvement in the ability to detect trends; however, the model showed that cutting the sampling rate to
every 6th d begins to impair the ability to detect concentrations trends within 5 yr.
7.3 Measurement Quality Objectives
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 are designed to
evaluate and control various phases (sampling, preparation, analysis) of the measurement process to
ensure that total measurement uncertainty is within the range prescribed by the DQOs. The MQOs can
be defined in terms of the following data quality indicators:
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.
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.
Detectabilitv- The determination of the low range critical value of a characteristic that a method specific
procedure can reliably discern.
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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. Data completeness requirements are
included in the reference methods (40 CFR Pt. 50).
Comparability - a measure of confidence with which one data set can be compared to another.
Accuracy has been a term frequently used to represent closeness to "truth" and includes a combination
of precision and bias error components.
For the field activities Section 14 presents the MQOs and the calculations for accuracy, precision, bias,
and completeness. Representativeness is determined through the original STN DQO and sampling
design process and detectability is discussed in the Quality Assurance Project Plan: Chemical
Speciation of PM25 Filter Samples. Comparability is achieved in the STN by use of appropriate
(performanced based) sampling instruments, and adherence to standard SOPS, and QAPPS and the
use of a single laboratory for analysis and data reporting.
The STN strategic plan (U.S. EPA, 1999b) quotes measurement quality objectives (MQOs) for the
overall measurement process that must be achieved in order to meet the DQO for trend detection.
These MQOs, which should be interpreted as the total coefficient of variation (CV) attributable to
sampling and analysis, are summarized in Table 7-1.
TABLE 7-1. MQOS FOR TOTAL MEASUREMENT ERROR
Analysis
Ions (anions and cations) by 1C
Total Carbon by TOA
Elements by EDXRF
MQO for Total Measurement
Error (Expressed as % CV)
10
15
20
Source: U.S. EPA, 1999b.
To calculate the total measurement error corresponding to the values given in Table 7-1, it is necessary
to quantify the individual components of random error using QC data collected by the monitoring
program. This process is described in Section 24.0. The limits on total error given in Table 7-1 apply
only to major ions and elements. Elements present at significantly lower concentrations will have much
larger CVs, both from natural variability and from measurement uncertainty.
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7.4 References
U.S. EPA (Environmental Protection Agency). 1994. Guidance for the Data Quality Objectives
Process: EPA QA/G-4, Report No. EPA/600/R-96/055, U.S. EPA, Washington, DC.
U.S. EPA (Environmental Protection Agency). 1998. Data Quality Objectives for the Trends
Component of the PM2 5 Speciation Network., U.S. EPA, Research Triangle Park, NC, 1999.
Available online on AMTIC at http://www.epa.gov/ttn/amtic/files/ambient/pm25/spec/dqo3.pdf.
U.S. EPA (Environmental Protection Agency). 1999. Particulate Matter (PM2 5) Speciation
Guidance Document (ThirdDraft)., U.S. EPA, Research Triangle Park, NC, January 5, 1999.
U.S. EPA (Environmental Protection Agency). 1999b. Strategic Plan: Development of the
Particulate Matter (PM2 $) Quality System for the Chemical Speciation Monitoring Trend Sites.,
U.S. EPA, Research Triangle Park, NC, April 16, 1999.
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8.0 Special Training Requirements/Certification
8.1 Training
Personnel assigned to perform PM2 5 chemical speciation monitoring activities must meet the
educational, work experience, responsibilities, personal attributes, and training requirements for their
positions. Each State or local monitoring agency is ultimately responsible for adequately training the
personnel performing supervisory, QA/QC, data handling, and other duties related to the PM2 5
chemical speciation network. Monitoring agency management must ensure that these personnel have
access to the relevant guidance documents, SOPs, QAPPs, and sampler operations manuals. Each
monitoring agency is also responsible for assessing the adequacy of their personnel's training and
performance and for ensuring training information is adequately documented.
Section 8.1.1 lists the minimum requirements and some additional suggestions and ideas for training
State and local personnel who may be unfamiliar with the operation of PM2.5 speciation samplers and
sample handling requirements. Section 8.1.2 describes sources of targeted training and Internet
addresses that are specifically applicable to operating the Speciation Trends Network.
8.1.1 State and Local Agency PM2 5 Training
Minimum requirements for training personnel in field and/or laboratory operations for the STN network
are as follows:
• Review of QAPPs for field operations and/or laboratory operations, as applicable
Site operators are to review the pertinent speciation sampler manual(s) for their site(s)
Review of two EPA documents, Particulate Matter Speciation Guidance Document
(January 1999) and Strategic Plan: Development of the PM2.5 Quality System for the
Chemical Speciation Monitoring Trend Sites (April 1999).
Suggestions for State and local management personnel for training site operators in STN site operations
are as follows:
Supply an overview of the NAMS PM2 5 STN through a video presentation. A video is
available online through the OAQPS' Education and Outreach Group at
http://www.epa.gov/oar/oaqps/eog.
Schedule meetings and/or teleconferences with personnel from the State and local agencies,
OAQPS, the Regional Speciation Coordinator, the support laboratory, and the Delivery
Order Project Officer prior to beginning trends network sampling operations.
Offer operator training classes at a centralized location. For operators who cannot attend,
a video of the procedures for operating the sampler and submitting the samples and data
reports could be supplied for training.
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• Field personnel who are unfamiliar with operating and quality assuring data from
meteorological monitoring systems should review the system's operating manual and consult
EPA's Quality Assurance Handbook for Air Pollution Measurement Systems, Volume
IV: Meteorological Measurements (EPA/600/R-94/038d).
Continue training through update memoranda, personal instruction during on-site systems
and performance reviews, and information distributed by the OAQPS/AMTIC Technology
Transfer Network and Public Forum under the speciation topic area. This Web site is
available at http://www.epa.gov/ttn/amtic/amticpm.html.
8.1.2 Targeted Training for PM2 5 Sampling and Laboratory Operations
Videos—The video, "Filter Handling and Analysis for PM2 5 Chemical Speciation Monitoring," is
available from the EPA OAQPS contact person listed in Section 8.3.
Telecourses—The Air Pollution Distance Learning Network (APDLN) is a digital state-of-the-art
educational satellite-broadcasting network of more than 100 governmental and university broadcast
affiliates located across the United States. The APDLN is the result of a collaborative partnership
between the EPA, State and local air pollution control agencies, and North Carolina State University
(NCSU). During seminars and telecourses, participants are able to interact with the Nation's leading
authorities on the latest air pollution control findings, monitoring devices, and systems. Participants can
ask questions of regulators and litigators and interact with the implementers on the APDLN.
The official listing of telecourses available from the EPA's APTI is announced on a 3-month rolling
schedule that is updated on the APDLN Web site and available from APDLN site coordinators. The
Web site is available at http://www.epa.gov/oar/oaqps/cog.
Workshops—The workshop titled "PM2 5 Monitoring Training: Chemical Speciation" was presented in
February 1999. Contact APTI and OAQPS to be placed on notification lists for future workshops.
Internet Resources—The following Internet resources are specifically applicable to the PM2 5
speciation monitoring program:
Ambient Monitoring Technical Information Center
http://www.epa.gov/ttn/amtic/amticpm.html—PM2 5 monitoring information: Contains links to other
areas including chemical speciation documents.
http://www.epa.gov/ttn/amtic/pmspec.html—Current chemical speciation documents.
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EPA/OAQPS
http://www.epa.gov/oar/oaqps/pm25/—PM2 5 data analysis: Contains ongoing activities of the data
analysis virtual workgroup, including background information, the data analysis workbook, analysis
tools (software), data sets, contacts, and links to documents and to other PM2.5 sites.
National Park Service
http://www.nature.nps.gov/ard/vis/vishp.html—National Park Service's visibility monitoring
information, including the Interagency Monitoring of Protected Visual Environments (IMPROVE)
network.
http://www.nature.nps.gov/ard/vis/sop/index.html—IMPROVE standard operation procedures
(SOPs).
http://www.nature.nps.gov/ard/impr/index.htm—IMPROVE newsletters.
PM2 5 Speciation Sampler Manufacturers' Information and Contacts
http://www.graseby.com/fpm.htm—Andersen Instruments Inc., manufacturer of RAAS 2.5-400
sampler.
URGCorp@compuserve.com—URG Corp., manufacturer of MASS 400 and 450 samplers.
metone@metone.com—Met One, manufacturer of SASS sampler.
8.2 Certification
There are no special certification requirements applicable to operation of the chemical speciation trends
monitors.
8.3 Contacts for More Information
OAOPS Contact for PM2 .-Related Training
Ms. Jan Cortelyou-Lee
Office of Air Quality Planning and Standards (MD-14)
Research Triangle Park, NC 27711
(919)541-5393
Internet: cortelyoulee.jan@epa.gov
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9.0 Documentation and Records
This section defines the records critical to the Speciation Trends Network, the information to be
included in reports or to be available for inspection, the data reporting format, and the document
control procedures to be used.
The STN will structure its records management system in a manner similar to the EPA records
management system and follow the same coding scheme in order to facilitate easy retrieval of
information during internal and external systems audits and reviews. Table 6-4 in Section 6 identifies
the documents and records that will be filed according to the statute of limitations discussed in Section
9.7. The field and laboratory SOPs will provide instructions on the proper distribution and filing of data
collected during specific procedures.
The following subsections describe the documents and records to be included in the QA reporting
packages for management, field operations, laboratory operations, data management, and quality
assurance functions of the STN. The term reporting package is defined as all the information required
to support the chemical speciation concentration data (and ancillary data) reported to EPA, which
includes all data required to be collected as well as other data deemed to be important by the STN.
Implementation of new or modified field or laboratory procedures may require concurrent comparison
against the old method. The document control feature (generally the date of issuance) of the new
version will be clearly marked, and the field or laboratory user will be asked to discard the old version.
Table 6-4 in Section 6 identifies these documents and records.
9.1 Information in the Management and Organization Reporting Package
There are three distinct management organizations associated with the STN: (1) the EPA Office of Air
Quality Planning and Standards and Regional EPA offices, (2) the State and local monitoring offices,
and (3) the contract site supply and sample analysis laboratory. The management reporting package
for these organizations will vary but would normally consist of at least an organizational structure
diagram; records of personnel qualifications and training (e.g., resumes); a quality management plan;
and files containing records of grants, contracts, and official correspondence regarding the STN.
9.2 Information in the Field Operations Reporting Package
9.2.1 Site Information
A file containing site documentation will be maintained in the State or local agency's central or field
office for each STN monitoring site. At a minimum, the site information file must contain the following:
site characterization information that documents how and why the site was selected, including
identification of the scale of the site and the locations of nearby sources of particulate matter; site maps
and sketches; and slides, prints, or digitized images of the site taken soon after installation of the PM2.5
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speciation samplers). The STN coordination office or the Regional Speciation Coordinator may ask
for copies of this material for a central file.
9.2.2 Field Operations
Operators of individual field sites must maintain records as well. The documents and records to be
maintained at the field office are listed under "Field Operations" in Table 9-1. The following types of
notebooks or binders are to be used by field personnel to keep documents in order and readily
accessible during a site systems review.
Field Notebooks—Each field site operator will obtain hard-bound notebooks. The notebooks will be
uniquely numbered and associated with the individual and the STN program. Generally, all data from
all routine field operations will be entered on field data forms or downloaded electronically from the
sampler's memory. The field notebook is used to record additional information about these operations,
such as information regarding weather conditions and activities in the area that may influence the sample
content and concentration (wind or electrical damage to equipment, construction or mowing activities in
the area, welding, traffic). Such information should be included in the comments section of the field
data form so the laboratory is made aware a sample may be compromised. Maintenance needs for the
sampler and the platform (appearance, upkeep, and safety concerns) should be relayed to the site
operator's supervisor for consideration and action. In addition the field operator may use this notebook
to record important communications.
Some organizations may have the capability of substituting the field notebook for electronic
communications (i.e., electronic site notebooks). This is appropriate as long as it is used consistently.
Field Binders—A 3-ring binder is a convenient repository for the appropriate data forms for routine
operations, inspection and maintenance forms, systems audit and corrective action forms, the field
QAPP, SOPs, and updates or advisories received from EPA or from other management sectors.
Sample Shipping/Receipt—One uniquely numbered notebook to record information about sample
receipt and shipment will be used by the field site operator. These notebooks are to be dedicated to
STN work. It will include examples of standard shipping/receiving forms and areas for free- form notes
about shipment difficulties or concerns such as equipment that arrives damaged or has missing parts.
9.2.3 Electronic Data Collection at Field Sites
All electronic data stored in the PM2.5 speciation sampler will be downloaded to a laptop computer or
other electronic transfer device at each field site. A diskette containing information from each of the
every-third-day sampling events will be created. It will be retained in the field operator's files for
sampler troubleshooting and for later use in data validation. It is recommended that data be
downloaded after each run; however, data from a number of runs may be accumulated in the sampler's
memory if bad weather or scheduling difficulties prevent prompt downloads.
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9.2.4 Hand-Entered Data at Field Sites
A number of field forms will require hand entry of data. These forms are primarily associated with the
field sites. An example of the combined custody and field data form can be found in the SOPs of
Appendix A to this QAPP and in Section 12.0. The forms should be in 3-part carbonless paper
format. A quality assurance/quality control report form, shown in Section 14.0 and in the SOPs in
Appendix A to this QAPP, also requires hand-entry of data from checks of the flow, temperature, and
pressure sensors of a sampler. Information should be entered clearly with a black or blue indelible
ballpoint pen. Any entry errors should be marked out with a single line and the correct information
entered above this line. The operator must sign or initial the form to verify the accuracy and
completeness of the entries.
Information recorded on these field forms is very important because it serves as a backup in case the
diskette data become corrupted or lost. Difficulties with or suggestions for improved operation of the
samplers should be recorded here and in the field notebook. Such comments will be very valuable
during the initial months of the network operation. Information about significant events near the site that
may affect the representativeness of the sample should also be entered into this form so the laboratory
will be on alert for an unusually high concentration sample.
A form for audit findings from the internal (or external) systems audits of the field site or the contract
laboratory is another example of a hand-entered data form. The response to the audit finding, a
Corrective Action Response (CAR) form, may also be hand-entered. Copies of all field site reviews
conducted by internal or external agencies and the site's responses to them should be retained at the
field site office.
9.3 Information in the Laboratory Operations Reporting Package
9,3,1 General Laboratory Information
A file or files of general laboratory information should be available for inspection. It will include
schematics of the laboratories showing locations of analytical stations, a record of equipment purchases
or leases, warranty information, and maintenance and service agreements with instrument vendors and
suppliers. The laboratory's safety manual should be a part of this information.
9.3.2 Laboratory Operations
Information related to the laboratory operations and data management reporting packages is given in
the QAPP for the STN contract laboratory.
9.4 Information in the QA Reporting Package
Four distinct QA organizations are associated with the PM2 5 STN.
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9.4.1 Network QA Manager
The OAQPS management organization has a QA Manager. This Manager and staff members will
produce and update the quality system and will review QA documents from the STN's field and
laboratory functions. QA document updates and directives will be issued from this office. The QA
Manager for OAQPS has overall approval authority for the STN QAPP and any subsequent changes
made to it.
9.4.2 State and Local Field Site QA Offices
The various State and local agencies whose personnel will operate the STN sites will keep a file of
documents and procedures that are part of their customary QA plan for site and sampling, equipment
receipt and acceptance testing, equipment maintenance, sampler operational checks, and operator
training. Documented results of and CAR responses to internal site inspections and external reviews
will also be kept on file for reference and inspection.
9.4.3 Contract Laboratory QA Manager's Office
The contract laboratory's QA Manager and staff will develop and periodically update the laboratory
QAPP and SOPs for routine servicing of the sites and analysis of filter samples. Results of internal
systems and performance reviews of laboratory operations will be kept on file and available for
inspection by EPA.
9.4.4 EPA QA Laboratory Offices
EPA and Regional laboratories will provide QA services to the field and laboratory components of the
STN. Their documented procedures will be kept on file and updated as necessary using document
control methods. EPA Region 1, NAREL and R&IE laboratories will provide QA services for STN
field and laboratory activities.
9.5 Reports to Management
The State and local field site operators will follow their customary procedures for reporting information
to their local or State managers. It is suggested that any verbal communications be documented in the
field notebook or that a copy of the notebook entry be sent to the manager and to the RSC as
appropriate. Field site operators will also report information on PM2 5 sample and meteorological data
capture rates and problems with sampling equipment and check devices for the speciation samplers.
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Table 9-1 STN Reporting Package Information
Categories
Record/Document Types
Management and
Organization
Organizational structure
Personnel qualifications and training
Training Certification
Quality management plan
EPA Directives
Support Contracts
Site Information
Site characterization file
Site maps
Site Pictures
Field and
Laboratory
Environmental
Data Operations
QA Project Plans
Standard operating procedures (SOPs)
Field and laboratory notebooks communications
Sample handling/custody records
Inspection/Maintenance records
Raw Data
Any original data (routine and QC data) including
data entry forms
Data Reporting
Data/summary/progress reports
Journal articles/papers/presentations
Data Management
Data algorithms
Data management plans/flowcharts
PM2.5 Data
Data Management Systems
Quality Assurance
Good Laboratory Practice
Control charts
Data quality assessments
QA reports
System audits
Response/Corrective action reports
Site Audits
They may also report on their review and levels 2 and 3 validation of the draft data sets supplied by the
contract laboratory, if they perform these validation activities.
The contracted laboratory is responsible for forwarding completed level 0 and level 1 data validation
checklists (Section 22) and the results of filter analyses to the EPA DOPO and to the State or local
contact who submitted the delivery order within 20 business from receipt of the sample. Level 0 and 1
data validation is described in the laboratory QAPP. Upon approval, the final data set will be released
from the laboratory in hardcopy and electronic format to the EPA DOPO, the State or local agency
contact, and the Aerometric Information Retrieval System (AIRS) electronic database. Draft and final
composite semiannual data summary reports will be issued from the laboratory to the State or local
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contact, the DOPO, and the EPA Project Officer. Results of resolution of problems with data sets will
also be prepared, sent to the concerned parties, and filed for the record.
9.6 Archival and Retrieval of Data Reporting Packages
Each organization participating in the STN is expected to keep updated versions of the documents and
data sets listed in Table 9-1 on file and accessible for the duration of the trends network's operation or
a specified lesser time. The files of the sites, the contract laboratory, Regional and EPA QA offices,
and validated electronic AIRS data sets must be retrievable for inspection and review during regular
business hours by OAQPS management or other U.S. Government authorities.
Limits on the time of data (and sample filter) retention will be decided by OAQPS program
management. Storage and archival of all field and laboratory data associated with each analysis in
electronic format for up to 3 yr following sample analysis is presently required, with the exception of
particle photomicrographs and associated spectral data in electronic format which may be discarded 12
months after receipt of the sample for examination. Data archivists should contact OAQPS a month
before the data discard date to ask for a decision on further archival or disposal.
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10.0 Sampling Process Design
This section describes all components associated with on-site field operations of the nationwide PM2 5
STN. The network will be operated by State and local agencies in 39 States, the District of Columbia,
and Puerto Rico. This section describes the key parameters to be estimated, the locations of primary
speciation samplers and collocated quality assurance speciation samplers, the frequency of sampling
using the primary and QA samplers, and the location and frequency of on-site systems and
performance evaluations PEs. The network design components comply with the regulations specified in
40 Code of Federal Regulations Part 58, Section 58.13, Appendices A and D, which are further
described in the document Guidance for Network Design and Optimum Site Exposure for PM2.5
andPM10 (U.S. EPA 1997).
10.1 Scheduled Project Activities, Including Management Activities
The STN will be sampling for chemical components of PM2 5 at 54 locations. Fifty-four primary
speciation samplers and 7 collocated QA speciation samplers will be employed. Of the 54 sites, 20
will be located at existing Type 2 PAMS, which are part of the NAMS network. The remaining 34
sites will be located at existing sites, or sites to be established, in selected (MSAs or CMSAs. All 54
sites will have a collocated Federal Reference Method monitor present to collect samples for
determination of particle mass concentration.
Installation of the speciation samplers and operator training occurred during the third quarter of 1999
and the first quarter of 2000. Twelve sampling sites in 12 States were installed in October 1999 as a
Mini-Trends Study and an initial operational evaluation component of the network. The installation
sequence then proceeded to each of the existing PAMS sites and then to NAMS sites in the chosen
MSAs. Those sampling locations that did not have an existing site available will come online as the
locations are approved and readied for use. The goal is to have all 54 samplers installed and tested,
operators trained, and laboratory support arrangements and schedules in place by December 2000. A
time line schedule of activities that apply to sites in the STN is given in Table 10-1.
Attaining a complete understanding of the interactions and scheduling of field and support laboratory
activities is a very important consideration during the design, installation, and startup phases of the STN.
A schedule of activities for the supporting contract laboratory for the NAMS trends network is
presented in Table 10-2.
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TABLE 10-1. SCHEDULE OF ACTIVITIES FOR STATE AND LOCAL PM25 STN
FIELD SITE PARTICIPANTS
Select sites. Arrange for space, electrical
power, personnel.
Network participants meet (12-site Mini-
Trends Study initially).
Order speciation sampler(s) and accessories
under national contract (12-site Mini-Trends
Study initially).
Acquire 10-m meteorological tower and sensor
package, if appropriate
Review, conditionally approve STN quality
assurance project plan (QAPP) and pertinent
standard operating procedures (SOPs).
Receive and install sampler(s).
Confer with Regional Speciation Coordinator
(RSC) and others.
Attend training sessions and/or review video.
Complete site preparation and sampler
installation, (a) 12-site Mini-Trends Study (b)
42 additional sites.
Begin Mini-Trends sampling at 12 sites.
Incorporate lessons learned and comments
from 12-site Mini-Trends network into draft
STN field QAPP.
Resolve sampling problems experienced by
the 12-site Mini-Trends Study. Revise
procedures accordingly and obtain network-
wide approval.
Begin routine, every 3rd-d speciation sampling
at all STN sites.
Participate in routine and nonroutine trends
sampling and field QA programs.
Review and level 2 ,3 validation of monthly
data reports received from laboratory.
Report problems and suggestions for
improvement to State/local management and
so on.
Consolidate STN QAPPs for field, laboratory,
audit program.
Anticipated Date
July 1999 through March
2000
July 1999 and continuing
August 1999 and
continuing
August 1999 and
continuing
August and September
1999
September 1999 through
March 2000
September 1999 and
continuing as sites come
on line.
October 1999 and
continuing
(a) By October 1999
(b) By Decemberl 2000
November 1, 1999
July 2000-Dec. 2000
Final Approval Jan. 2001
Prior to April 2000
sampling date
February 1,2001
December 2000 and
continuing
Each month. Complete
review within 30 d
As required
Notes
Confer with U.S. Environmental
Protection Agency (EPA) prior to
ordering to confirm sampler
selection and need for collocated
sampler.
Confer with EPA prior to ordering.
Order only if needed at site(s).
Contingent on vendor schedule.
Finalize mechanism and schedule
for delivery order process for
routine, nonroutine, and QA
samples.
Consult EPA's Office of Air Quality
Planning and Standards (OAQPS)
and EPA Regional Offices for plans.
Obtain site documentation and
photographs/slides for site file.
Involve field staff, RSC, laboratory,
OAQPS as required.
Refer to every 3rd-d sampling
schedules for 2000 and beyond.
Interact with RSC.
Interact with RSC and OAQPS to
resolve problems.
Interact with RSC and OAQPS.
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TABLE 10-2. SCHEDULE OF ACTIVITIES FOR CONTRACTING STN LABORATORY
Activity
Prepare and obtain approval of QAPP and
SOPs for laboratory activities and field site
support.
Meet with OAQPS project scientists, RSCs,
and Delivery Order Project Officers (DOPOs).
Receive and analyze routine speciation
samples.
Assemble, validate, and report data. Review
field and laboratory interactions; review and
resolve problems.
Complete analyses within 20 business d of
sample receipt. Prepare and submit monthly
draft summary data reports to DOPO and State
agencies for review and validation.
Submit final data packages following
State/local and DOPO approval of draft data.
QA auditing and inspections.
Systems audit and review of data archives.
Date
Draft: August 1999
Final: September 1999
September 1999
November 1999 and
continuing
November 1999 and
continuing
Submit summary data
report by 1 5th d of month
following month of
analyses
Quarterly
Various times; quarterly
Annually
Notes
Includes laboratory SOPs, tested
and approved for use.
Receive details on initial STN site
contacts and sampler requirements.
Finalize mechanism and schedule
for delivery order process for
routine samples.
Conduct level 0 and level 1
validation of data.
Enter data into Aerometric
Information Retrieval System
(AIRS).
QA Manager for contract
laboratory conducts audits.
Coordinated by EPA.
10.2 Rationale for the Design
10.2.1 Network Design
The rationale for the design of the STN is in part found in the requirements and principles set forth in the
Federal Register (62 FR 38763), promulgated as part of the PM2 5 National Ambient Air Quality
Standards review completed in 1997. This rule specifies that a 50-site chemical speciation trends
network be established as a component of the overall PM2 5 criteria pollutant study effort. These sites
should include approximately 20 PM2.5 core sites to be collocated at PAMS sites.
The remaining speciation trends sites are located to include major population areas in the central,
Midwestern, and southeastern United States, which, in many cases, also include areas with the region's
higher PM10 and PM2.5 precursor emissions. In locating speciation sites within each of the suggested
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MS As, it is recommended that the speciation trends site be a community-oriented PM2.5 core site,
which is expected to receive the maximum PM2 5 concentrations for the MSA. Where feasible, each
MSA speciation trends site should be outfitted with a 10-m eter meteorological tower to collect data on
wind speed and direction, temperature, and humidity. Please note that for modeling purposes, wind
speed and direction vector, the standard deviation of wind direction (sigma theta), ambient temperature
and relative humidity should be collected. Most modern data acquisition systems have the capability to
collect the vector and sigma theta data. If a meteorological tower is not feasible, then the RO should
attempt to collect the nearest meteorological data from the National Weather Service or nearby
airports. However, the weather station should be within 10 miles of the station for the weather data to
useable. If this is not feasible, the meteorological data used must represent the airshed. If, after
collection and review of data from several samples, a site is judged to be biased by emissions from a
nearby source or by poor ambient air exposure, the data will be examined, recommendations will be
made by the local agency for relocating the site, and a decision will be made by the networks
coordinating office based on the findings. Examples of causes of sampling bias could be detection of
unusually high concentrations of a metal or filter loadings much higher than other sites in the airshed.
OAQPS scientists and peer review members of the Subcommittee on Fine Particle Monitoring (a
subcommittee of the Clean Air Scientific Advisory Committee, have participated in numerous meetings
to discuss the STN's design and how it should begin operations. It was decided that the network
should first begin as a 12-site, 12-State Mini-Trends Study. The Mini-Trends Study's purposes are to
provide State personnel with hands-on experience in the operation and selection of speciation samplers
and to gain knowledge about PM2 5 chemical composition and sampler operations during cold weather
and in woodsmoke emissions areas.
10.2.2 Speciation Sampler Design and Selection
Sampler design requirements stated in 40 CFR Part 53 require that speciation samplers incorporate
particle inlets and size fractionators having comparable particle size discrimination curves as the
reference method for PM2.5, employ denuder technology to remove acidic and organic gases, have face
velocities and sample volume capture similar to the FRM, and be reliable and rugged in field use.
However, speciation samplers are not required to attain reference or equivalent method designation and
should be selected on performance in order to meet the STN data quality objectives. Desirable
features of speciation samplers are discussed in the PM2.5 speciation guidance document (U.S. EPA
1999).
Speciation sampler(s) will also be collocated at 7 of the 54 sites in the network. These sites are
identified in Table 10-3. The collocated samplers provide a set of PM2 5 speciation data, originating
from a separate but otherwise identical sampler, in order to estimate the precision of the total sample
collection, handling, and analysis/data reporting process. The collocated QA sampler will also be
operated every 3rd d to coincide with the start and end run times of the site's primary monitor. Samples
and data from the QA sampler will be handled in exactly the same way as those from the primary
sampler. Section 14.0 discusses this precision check in more detail.
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TABLE 10-3. PROPOSED SITES FOR THE PM,< STN
EPA
Region
1
2
3
4
5
6
State or
Commonwealth
Connecticut
Maine
Massachusetts
Massachusetts
Rhode Island
Vermont
New York
New Jersey
Puerto Rico
Washington, DC
Maryland
Pennsylvania
Virginia
Alabama
Florida
Georgia
Mississippi
North Carolina
South Carolina
Tennessee
Illinois
Indiana
Michigan
Minnesota
Ohio
Wisconsin
Louisiana
Oklahoma
Texas
MSA or PAMS
City Site Name
East Hartford (M)
Kittery (P)
Boston, U. (P, 1)
Chicopee (P)
East Providence (P)
Burlington (M)
Queens (P)
Rochester (M)
New Brunswick (1
San Juan (M)
McMillan Reservoir
(P)
Essex (P)
E. Lycoming (P)
Pittsburgh (M)
Norfolk (M)
Birmingham (M)
Miami (M)
Tampa (M)
S. Dekalb (P)
Biloxi (M)
Charlotte (M)
Charleston (M)
Memphis (M)
Northbrook(l,P)
Indianapolis (M)
Detroit (M)
Minneapolis (M)
Cleveland (M)
Milwaukee (P)
Capitol (P)
Tulsa (M)
Deer Park. (1,P)
Hinton (P)
Chamizal (P)
AIRS Number
09-003-1003
23-031-3002
25-025-0042
25-013-0008
44-007-1010
36-081-0097
36-005-6001
34-023-0011
11-001-0043
24-005-3001
42-101-0004
13-089-0002
17-031-4201
55-079-0041
22-033-0009
48-201-1035
48-113-0069
48-141-0044
Local Sampling and QA/QC Contacts
Jerry Sheehan, 978-975-3215
(jerry. sheehan@state.ma.us)
Jerry Sheehan, 978-975-3215
(jerry. sheehan@state.ma.us)
Dirk Felton, 5 1 8-457-9 1 37
(hdfelton@gw. dec . state.ny .us)
Norman Glazer, 215-685-1085
(norman.glazer@phila.gov)
Tom Tamanini 813-272-5530
(tamanini@epcj anus . epchc . org )
Terry Sweitzer, 217-782-7438
(epa2204@epa. state. il.us)
Bob Lamorte, 708-865-6184
(ccdects@wwa.com)
Ed Michael, 512-239-1384
(emichel@tnrcc.state.tx.us)
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TABLE 10-3 (continued)
EPA
Region
7
8
9
10
Network
Totals
State or
Commonwealth
Kansas
Missouri
Nebraska
Colorado
Montana
North Dakota
Utah
Arizona
California
Nevada
Idaho
Oregon
Washington
30 States
MSA or PAMS
City Site Name
Kansas City (M)
St. Louis (M)
Omaha (M)
Denver (1, M)
Missoula (M)
Bismark (M)
Salt Lake City (M)
Phoenix (M)
Riverside
(Rubidioux)(l,M)
El Cajon (P)
Simi Valley (P)
Sacramento (P)
Bakersfield (M)
Fresno (M)
San Jose (M)
Reno (M)
Boise (M)
Portland (M)
Seattle (1,M)
34 MSAs/Sites; 19
PAMS
Sites; 53 Total
AIRS Number
06-065-8001
06-073-0003
06-111-2002
06-067-0006
06-029-0014
06-019-0008
06-085-0004
Local Sampling and QA/QC Contacts
Bern Johnson, 573-526-2027
(nrjohnb@mail.dnr.state.mo.us)
James Brunnert, 573-751-2706
(nrbrunj @dnr. state.mo.us)
Daniel E. Harman, 701-325-5200
(dharman@state.nd.us)
RobertNeal Olson, 801-877-0764
(rolson@deq. state.ut.us)
Tom Moore, 602-207-2353
(moore.tom@ev.state.az.us)
Steve Aalbers, 503-229-6798
(aalbers.steven@deq.state.or.us)
1 Selected as collocated speciation sampling sites.
2 MSA is Metropolitan Statistical Area, coded by (M) following the site name. PAMS is photochemical air
monitoring station, coded by (P)
following the site name.
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PM2 5 STN QAPP
Section No. 10
RevisionNo.: 4.1
Date: 126/00
Page 7 of 7
10.2.3 Sampling Frequency
The entire STN will sample consistently every 3rd d. Routine samples will be collected for a 24-h
period beginning and ending at midnight on the assigned day. The every 3rd-d sampling schedules for
CY2001 is available in Appendix A-6. This should be distributed to all site supervisors and operators.
Sites in the STN will not acquire samples on any other days unless specifically directed to do so by
network authorities. Should nonroutine sampling be requested, such samples must be taken on days
other than those set by the every-3rd-d schedule and must be handled separately when submitted to the
laboratory for analysis.
10.2.4 Deviations from the Sampling Plan
Because the STN's major goal is to determine trends in PM2 5 chemical speciation concentrations over
time and within geographical areas, deviations from the sampling plan are not allowed. Should an
occasional deviation occur at a site, the site operator must note this in his or her field site notebook and
on the field data form that is returned to the laboratory with the sample filters so the resulting data can
be flagged. Continued deviations from the sampling plan at one or more sites will give rise to a review
of the site's operating plan, the personnel involved, and a request for prompt corrective action.
Furthermore, the data sets acquired during periods when deviations from the sampling plan occurred
may be sequestered and not used in trends analysis studies.
10.3 Reference
U.S. Environmental Protection Agency. 1997. Guidance for Network Design and Optimum Site
Exposure for PM2.5 and PM10. Publication No. EPA-454/R-99-022. December 1997.
U.S. Environmental Protection Agency. 1999. Paniculate Matter (PM2 5) Speciation Guidance
Document. Third Draft. January 1999.
-------
PM2 5 STN QAPP
Section No. 11
RevisonNo.: 4.1
Date: 12/00
Page 1 of 7
11.0 Sampling Methods Requirements
The Speciation Trends Network provides for measurement of the mass and chemical component
concentrations of fine particulate matter with an aerodynamic diameter less than or equal to a nominal
PM2 5 in ambient air over a 24-h period. Three different brands of PM2 5 speciation monitors will be
used to collect PM2.5 samples. These three samplers have been subjected to bench testing and to
comprehensive multicity field test intercomparisons against each other and against the FRM and the
IMPROVE samplers and have met the requirements stated in the EPA requisition for speciation
samplers. Standard operating procedures for setup, operation, and quality control of the samplers are
given in Appendix A to this quality assurance project plan.
11.1 Sample Collection and Preparation
11.1.1 Preparation
Before a site visit, the operator must gather sampling modules, data forms, and sampler verification
equipment to check flow, temperature, and pressure (if a QC check is scheduled). The sampling
modules must be transported to the sites in a protected environment and not subjected to high
temperatures.
Shipment of sampling modules to the laboratory will require the use of ice substitutes and coolers. The
operator must freeze the ice packs prior to use. During transport to/from the sites, the ice substitutes
may be placed in an electric transport cooler to maintain their frozen state, if desired.
11.1.2 Field Sample Collection
The speciation sampler will be permanently installed within 1 to 4 m of the site's routine FRM sampler.
The proper operation of the speciation samplers and the collocated FRM sampler must be confirmed
before the first run. A testing and acceptance checklist appears in Section 15.0 of this QAPP.
Sampling modules will be installed and the samplers will run every 3rd day, from midnight- to- midnight
on local standard time the whole year. Refer to Appendix A for details on setup and operation of the
sampler, handling of filter sampling modules, hand-entry of data, downloading of electronic files, and
sampler QC check requirements.
11.1.3 Sampler Recorded Measurements
Table 11-1 lists the information that is expected to be provided by any of the speciation samplers. This
information will be stored in the sampler's memory and can be downloaded to disks. Essential
information will also be transcribed from the display screen of the sampler and hand-entered on to a
custody and field data form. This form is described in Section 12.0 of this QAPP.
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PM2 5 STN QAPP
Section No. 11
RevisonNo.: 4.1
Date: 12/00
Page 2 of 7
TABLE 11-1. SUMMARY OF INFORMATION PROVIDED BY SPECIATION SAMPLER
Information to be Provided
Flow rate, average, for the sample
period
Flow rate, CV, for the sample period
Flow rate, 5-min average out of
specification (FLAG)
Sample volume, total
Temperature, ambient, min., max.,
average, for the sample period
Barometric pressure, ambient, min.,
max., average, for the sample period
Filter temperature, differential, 30-
min interval, out of specification
(FLAG)
Date and time
Sample start and stop time settings
Sample period start time
Elapsed sample time
Elapsed sample time out of
specification (FLAG)
Power interruptions >1 min, start
time of first ten interruptions
LJser-entered information, such as
sampler and site identification
Units
L/min
L/min
m3
°C
mmHg
yr/mo/d/h/mi
n
yr/mo/d/h/mi
n
yr/mo/d/h/mi
n
h min
h min
Availability
Anytime
• (optional)
•
•
•
•
•
•
•
•
—
•
—
•
•
End of Period
• (required)
•
•
•
•
•
•
—
•
•
•
•
•
•
Visual Display
•
•
•
•
•
•
•
•
•
•
•
•
•
•
Provided to
AIRS Database
•
•
•
•
•
•
—
•
•
•
•
The sample volume is essential to determining the concentration of the species. The total volume of air
collected by a speciation sampler will vary by brand and sampling channel. Samples are expected to
be 24 h in duration; however, in some cases, a shorter sample period may be necessary, but it should
not be less than 23 h or more than 25 h. Because capture of the fine particulate is predicated on a
particular sampler channel's design flow, deviations of greater than 10 percent will set a flag for that
sample period. Further, if a sampling period is less than 23 h or greater than 25 h, the sample will be
flagged. Other conditions may cause a flag to be set. These include power losses and extreme
difference in ambient and sampler interior temperatures.
11.1.4 Sampling Module Transportation
The used sampling modules must be stored in a protective transport container and transported to the
contract laboratory as soon as possible. Sampling modules should be shipped out by overnight
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PM2 5 STN QAPP
Section No. 11
RevisonNo.: 4.1
Date: 12/00
Page 3 of 7
express within 48 h following the end of a sample run. If an agency must deviate from sending the
sample out within 48 hours, please see the discussion in Section 6.4.3 and Appendix A-6.
ll.l.SField Maintenance and Calibration
A maintenance schedule must be developed for field sampling equipment and verification devices. See
Section 15.0 of this QAPP for more information. Consult the operator's manuals, the SOPs in
Appendix A, and Section 16.0 of this QAPP for requirements and procedures for calibration of
temperature and pressure sensors and the flow rates of sampling channels.
11.2 Sampling/Measurement System Corrective Action Process
11.2.1 Corrections to the SOPs
The State and local agency field site operators and their supervisors are responsible for implementing
this QAPP and the field SOPs and are in part responsible for the quality of the data. If changes or
corrections are suggested for the SOP methods or QAPP, State or region personnel will notify the QA
Manager in the Office of Air Quality Planning and Standards (OAQPS) Coordination Office. The QA
Manager will review the information and convey the issue to the Chemical Speciation Workgroup. The
workgroup will review the proposed change and attempt to classify the change according to the effect
the change would have on the data. Class types follow:
Class 1—The change improves the data and the new procedure replaces the current procedure. If
found to be acceptable by the workgroup, a new SOP will be issued that can be inserted into the
QAPP. The document control information in the heading will contain a new revision number and date.
A quality bulletin will be filled out describing the change and distributed to all affected National Trends
Network (NTN) personnel.
Class 2—The change provides for an alternative that does not affect the quality of the data but may
provide for efficiencies in some circumstances or be cost-effective. If found to be acceptable by the
workgroup, the original SOP will not be altered, but an addendum to the procedure will be issued that
describes the modification and provides for the use of the alternative method.
Class 3—The change is grammatical in nature and does not reflect a change in the procedure. The
changes will be highlighted and modified during a Class 1 change (where appropriate) or corrected
during the development of a full revision to the document.
Upon agreement by the speciation workgroup to institute a change, hard copies of Class 1 and 2
changes will be distributed using the quality bulletin illustrated in Figure 11-1. The STN laboratory, each
site, and the management of each site will be notified. New versions of SOPs will be mailed to STN
participants with instructions to discard the old version.
-------
PM2 5 STN QAPP
Section No. 11
RevisonNo.: 4.1
Date: 12/00
Page 4 of 7
Quality Bulletin
Subject:
Number
Date
Page of _
Supersedes No.
Dated
Replace and Discard Original
Add Material to Document
Notes:
PM2 5 QA Coordinator
Retain this bulletin until further notice
Discard this bulletin after noting contents
This bulletin will be invalid after (Date)
This bulletin will be incorporated into quality
Procedure No. by (Date)
Figure 11-1 Quality bulletin
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PM2 5 STN QAPP
Section No. 11
RevisonNo.: 4.1
Date: 12/00
Page 5 of 7
11.2.2 Data Operations
Corrective action measures in field operations of the STN will be taken to ensure the data quality
objectives are attained. Potentially, there are many types of sampling and measurement system
corrective actions. Table 11-2 is an attempt to forecast the expected problems and corrective actions
needed for a well-run speciation trends network.
11.3 Avoiding Sample Contamination; Temperature and Holding Time
Requirements
This section details the requirements needed to prevent sample contamination, the temperature
preservation requirements, and the permissible holding times to limit degradation of the sample catch.
11.3.1 Sample Contamination Prevention
The STN must have rigid requirements for preventing sample contamination. Powder-free antistatic
gloves are worn while handling filter cassettes or sampling modules in the laboratory. Once the filter
cassette or sampling module leaves the laboratory, it must not be opened due to the potential for filter
damage or contamination. Filter cassettes (used with the Andersen RAAS sampler) will be stored in
protective containers. Other sampling modules (used with the URG MASS or the Met One SASS)
will be capped and protected in plastic wrap or polyurethane foam during shipment to and from the site.
When used cassettes or sampling modules are removed from the sampler, they must be promptly
capped or otherwise protected to prevent contamination from dusts, gases, or abrasion. The site
operator's hands must be clean when handling sampling modules and is suggested that they are cleaned
immediately before the sample handling step. It is recommended that plastic gloves be used.
11.3.2 Temperature Preservation and Holding Time Requirements
During shipment from the laboratory to the sample location, there are no specific requirements for
temperature control; however, the filters or sampling modules should remain in their protective
containers and inside the transport container. Excessive heat must be avoided (e.g., do not leave in
direct sunlight or a closed-up car during summer). During the sampling (24-h period), the filters will be
subject to ambient temperatures and should not exceed the ambient temperature by more than 5 °C for
more than 30 min continuously. Sampling modules should be removed from the sampler within 48
hours after the sampling period ends. The temperature of sampling modules must be brought to 4 °C as
soon as possible and the shipment package, cooled to 4 °C, should be ready for pickup by the courier
service as soon as possible, unless the samples will be transported back to the field office and stored in
a refrigerator (i.e., Friday sample collection).
-------
PM2 5 STN QAPP
Section No. 11
RevisonNo.: 4.1
Date: 12/00
Page 6 of 7
TABLE 11-2. STN FIELD OPERATIONS CORRECTIVE ACTIONS
Item
Sampling media inspection
(presample)
Note: This inspection will
apply only to the
Andersen RAAS sampler.
Sampling media filter
inspection (postsample)
Note: This inspection will
apply only to the
Andersen RAAS sampler.
Sample flow rate
verifications)
Leak test
Problem(s)
Filter with pinhole(s) or
tears. Missing component
of sampling module.
Mismatched module and
chain-of-custody (COC)
form.
Torn or suspect filter
catch
Out of specification
(+10 percent of transfer
standard)
Leak outside acceptable
tolerance
Action
1 . If additional sampling
module available, use
it; void filters with
pinholes or tears
2. Use new field blank
module as sample filter
3. Obtain a new sampling
module from laboratory
1 . Inspect filter holder and
connections
2. Check sampler
pneumatics
1 . Completely remove
flow rate measurement
adapter; reconnect and
perform flow rate check
again
2. Perform leak test
3. Check flow rate at three
points to determine if
flow rate problem is
with zero bias or slope
4. Recalibrate flow rate
1 . Completely remove
flow rate measurement
adapter; reconnect and
perform leak test again
2. Inspect all seals and O-
rings; replace as
necessary and perform
leak test again
3. Check sampler with
different leak test
device
Notification
1. Document on field data
form
2. Document on field data
form
3. Notify Delivery Order
Project Officer (DOPO)
and laboratory
1. Document on field data
form
2. Document in site
notebook; notify field
manager
1. Document on QA/QC
field data form
2. Document on QA/QC
field data form
3. Document on QA/QC
field data form and
notify supervisor and
sampler vendor
4. Document on field
calibration data form
and notify supervisor
1 . Document in field
notebook and on
QA/QC field data form
2. Document in field
notebook and on
QA/QC field data form;
flag data since last
successful leak test.
3. Document in field
notebook and on
QA/QC field data form
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PM2 5 STN QAPP
Section No. 11
RevisonNo.: 4.1
Date: 12/00
Page 7 of 7
TABLE 11-2. (continued)
Item
Sample flow rate
Ambient temperature
verification and filter
temperature verification
Ambient pressure
verification
Elapsed sample time
Elapsed sample time
Power
Power
Data downloading
Problem(s)
Consistently low flows
documented during
sample run
Out of specification (+2°C
of standard)
Out of specification
(+10 mmHg of standard)
Out of specification
(+5 min)
Sample did not run
Power interruptions
Liquid-crstal display
(LCD) panel on, but
sampler not working
Data will not transfer to
laptop computer
Action
1 . Check programming of
sampler flow rate
2. Check flow with a flow
rate verification filter
and determine if actual
flow is low
1 . Recalibrate sensor;
replace sensor
1 . Make certain pressure
sensors are exposed to
the ambient air and are
not in direct sunlight
2. Call local airport or
other source of ambient
pressure data and
compare that pressure
to pressure data from
monitors sensor;
pressure correction
may be required
3. Connect new pressure
sensor
1 . Check programming;
verify power outages
2. Reset
1 . Check programming
2. Try programming
sample run to start
while operator is at site;
ensure the transport
filter is in the unit
1 . Check line voltage
1. Check circuit breaker;
some samples have
battery backup for data
but will not work
without AC power
1. Document key
information on sample
data sheet. Make
certain problems are
resolved before data
are written over in
sampler microprocessor
Notification
1. Document in field
notebook
2. Document in field
notebook
1. Document in field
notebook and on
QA/QC field data form
1. Document in field
notebook and on
QA/QC field data form
2. Document in field
notebook and on
QA/QC field data form
3. Document as above
1 . Document on data
sheet
2. Document in field
notebook
1. Document in field
notebook
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PM2 5 STN QAPP
Section No. 12
RevisonNo.: 4.1
Date: 12/00
Page 1 of 6
12.0 Sample Handling and Custody Requirements
12.1 Introduction
This section describes sample handling and custody procedures that are necessary to ensure that
Speciation Trends Network site operators properly handle the sampling components from
the time of receipt at the field office until they are released to the shipping agency for return
to the STN laboratory.
• Field site use COC and subsequent laboratory COC is maintained for each sample,
beginning with placement of the filters in the sampler collection modules and extending
through all analytical steps to final sample archival.
12. 2 Presampling Sample Handling and Custody Procedures
Care must be taken when handling, storing, and transporting filters at all stages in their use due to the
small mass of particles collected on exposed filters, the potential for sample losses due to rough
handling or sample volatilization, and the potential for weight gain due to contamination or uptake of
reactive gases on the filter and particulate matter surfaces. Care must also be exercised in handling
denuders to ensure acidic gases are quantitatively removed from the sample air stream and that the
denuder's coating does not dislodge and fall onto the sample filter. Sample handling procedures must
be consistently followed in order to provide data meeting the data quality objectives . These
procedures are discussed below and presented more fully in the PM2.5 sampler SOPs which are
included in Appendix A to this quality assurance project plan.
12.2.1 Procedures in the STN Laboratory
Details on how the contract laboratory handles the denuders and filters, loads the filters into sampling
modules, and packages the components for shipment to the field office are given in the STN
laboratory's QAPP.
Sample custody procedures are required to avoid misplacement of samples or confusion of one sample
with another, and to provide documentation to assist in detection and resolution of COC problems. A
sample is considered to be in custody if it is in one's actual physical possession or stored in a secured
area restricted to authorized personnel.
Each set of sampling modules and other equipment supplied by the laboratory (such as cyclones and
denuders) will be accompanied by a three-page, carbonless PM2 5 custody and field data form
(CAFDF). This form will contain the filter identification number, filter type, container (module or
cassette) identification number, and date by which the sampling media must be used. An example
CAFDF is illustrated in Figure 12-1 and its contents are explained in Table 12-1. The laboratory will
fill in much of the information required in parts A, B, and C of the form and will retain the third copy.
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PM2 5 STN QAPP
Section No. 12
RevisonNo.: 4.1
Date: 12/00
Page 2 of 6
The information on the CAFDF will ultimately be entered into a sample tracking system, where an
electronic record will be kept.
12.2.2 Procedures at the Field Office
Upon receipt at the field office of a set of sampling components for a particular speciation sampler, the
STN site operator must carry out the following documentation and handling steps:
Enter receipt of the shipment in the operator's field notebook, noting the date and time of
receipt and any air bill or other identifying numbers associated with the shipment.
Inspect the exterior of the shipping cooler, note any evident damage, and record
observations in the operator's field notebook.
Open the shipping container and ensure that a CAFDF is present for each set of sampler
components sent in the shipment. Also check to be sure shipping items such as ice
substitute gel packs and a min./max. thermometer (if required) are present. Ensure each
identifying number printed on the CAFDF corresponds to an enclosed sampling channel
component. Do not use any sampling component whose identifying bar code number is not
listed on the CAFDF. Notify the STN laboratory about any discrepancies. Remove the
gel packs and freeze them.
Sign and date the custody record portion of the CAFDF.
Store all components for a sampler run together in a container in an air-conditioned secure
area for later transport to the site. Adopt a first-in, first-out use schedule. Sampling
components should be stored and tracked so that the correct set of sampling components
reaches the designated field collection site for use on the designated sampling day.
Do not interchange sampler channel components intended for use with a particular speciation sampler at
a particular site with components for any other sampler or site. The STN laboratory has labeled each
sampler channel component for use at a particular site. Should an interchange occur, the STN site
operator must fully document the variance and inform the laboratory so the analytical results can be
associated with the correct sampler and site.
It has been noted by RTI, that the temperature of some of the coolers that have been received by the
SHAL have been above 4°C. RTI staff believe the problem may be due to the gel packs not being
frozen long enough or at a cold enough temperature. This QAPP recommends that gel packs be frozen
for at least 3 days at a temperature of -32°C. This will insure that the filters do arrive at the RTI
laboratory at or under 4°C.
-------
PM2 5 STN QAPP
Section No. 12
RevisonNo.: 4.1
Date: 12/00
Page 3 of 6
BAR CODE GOES
Custody/Data Form
HERE
No.
PM2.5 STN CUSTODY AND White - return to lab
FIELD DATA FORM ^.ablTs
A. CUSTODY RECORD (Name, Date)
1. Laboratory, Out
Date
2 Site, In
Date
3. Site, Out Date
4. Lab. In Date
B. SITE AND SAMPLER INFORMATION
1. Site AIRS Code
2. Sampler S/N
3. Sampler Type
4. Sampler POC
5. Site Name
6. Intended date of use
7. Date of sampler set-up
8. Operator's name
C. SAMPLER CHANNEL COMPONENTS
Channel
Number
1
1
2
2
3
3
D. START, END,
Channel No.
1
2
3
Component ID
No.
kept at site
11234568
kept at site
11234570
kept at site
11234572
Component Description
SASS cyclone
SASS cassette (Teflon filter) (GREEN)
SASS cyclone
SASS cassette (MgO denuder, nylon filter) (RED)
SASS cyclone
SASS cassette (quartz filter) (ORANGE)
AND RETRIEVAL TIMES
Start date Start time
End date End time Retrieval Retrieval
date time
E. SAMPLER CHANNEL INFORMATION (Post-Sampling)
Channel Run Run
No. Time Time, Flag
1
2
3
Channel "T Avg. Filter
No. Flag T (°C)
1
2
3
Sample
Volume
(m3)
Max. Filter
T(°C)
Avg. Avg. Avg. Max. Min.
flow flowCV ambient ambient ambient
(L/min) (L/min) T (°C) T (°C) T (°C)
Min. Filter Avg. BP Max. BP Min. BP
T(°c) (mm MS) (mmHg) (mm MS)
Figure 12-1. Custody and field data form (CAFDF) for the PM2 5 STN.
-------
PM2 5 STN QAPP
Section No. 12
RevisonNo.: 4.1
Date: 12/00
Page 4 of 6
TABLE 12-1. EXPLANATION OF STN CUSTODY AND FIELD DATA FORM
CAFDF Section
Top of form
A. Custody Record
B. Site and Sampler
Information
C. Sampler Channel
Components
D. Start, End, and
Retrieval Times
E. Sampler Channel
Information
F. Comments
Explanation of Section Contents
The custody /data form number will be unique to each sample set and assigned in
advance by the laboratory. The 3-part carbonless form will be distributed as
follows:
• Top copy (white original) — returned to the analytical laboratory
• Second copy (yellow) - retained by the field site office
• Third copy (pink) — retained by the originator
Acknowledge relinquishing and receiving custody in this section. Persons should
sign their name (legibly) and record the date.
Information about the site and the date the sampler modules are to be used. Most
of this information will be pre-entered by the laboratory.
The sampling components needed for a particular sampler and its multichannel
sampling arrangement are listed here. They are identified by bar code tracking
number and by a free-form description. The brand of the sampler is identified. This
information will be entered by the laboratory, preprinted on the form. A separate
custody /data form will be used for each set of sampling modules intended for
routine sampling, field blank studies, and trip blank studies.
These entries are made by the site operator. The start and end times correspond to
those programmed into the sampler during the setup phase. The operator must
enter these data clearly and must double-check the values against the sampler
display screen. The retrieval date and time indicate when the sampling modules
were removed from the sampler.
Postsampling information can be transcribed by hand directly from the display
screen of the sampler. The operator is responsible for making these entries at the
site. The sample volumes will be used by the laboratory to compute analyte
concentrations. The State and local agencies will use these data in level 2 and 3
validations to identify problems with the sampler. Again, the operator must enter
these data clearly and must double-check the values against the sampler display
screen.
This section offers a place to record further notes on any part of the form as well as
observations of abnormally high emissions in the vicinity. The person recording
information here should refer to the sections of the form. Detailed information
should also be recorded in the field or laboratory notebook and referenced to the
iininue custodv/data form number location samnler and samnline date
12.2.3 Procedures at the Field Collection Site
Sampling components/modules must be used at the field collection site on the sampling date specified
on the CAFDF. Unused sampling modules and denuders should remain sealed or capped and kept
from exposure to ambient air, temperature extremes, or vibrations.
Upon arrival at the site to set up a sampling event, the STN site operator should follow the SOP written
for the particular sampler. Refer to Appendix A for instructions for the installation of sampling modules
and denuders and programming of the sampler. Once the sampling modules are installed at the site and
the sampler is programmed to begin operation, the operator should complete the appropriate sections
of the CAFDF.
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PM2 5 STN QAPP
Section No. 12
RevisonNo.: 4.1
Date: 12/00
Page 5 of 6
12.3 Postsampling Sample Handling and Custody Procedures
The following procedures represent brief descriptions of more detailed standard operating procedures.
For more detailed information about the process of removing sampling modules and denuders from a
sampler, filling in field data forms, downloading data electronically, and packaging samples in a cooler
for shipment, refer to the specific sampler's SOPs in Appendix A to this QAPP, to SOPs concerning
sample packaging and shipment in the STN laboratory's QAPP, and to the sampler's operating manual
12.3.1 Procedures at the Field Collection Site
The following is a brief description of the post sampling procedures at the field site.. Within 48 h after
the end of a sampling period, the STN site operator should remove the sampling modules from the
sampler.
At the site, the operator must complete the following:
• Read selected data from the sampler's display screen and enter them in Section E of the
custody and field data form. Double-check all entries against the sampler display.
Print clearly. Be certain the entries are clear on the second page of the carbonless
form. Refer to the custody and field data form example in Figure 12-1 and to Table 12-1
for details.
Remove the filter cassettes or sampling modules from the sampler. Briefly examine the
cassette or module for damage and ensure it is, in fact, the correct module for the sampling
channel from which it was removed.
• Place the sampling modules in protective containers); cap the denuders if they are to be
returned. Place all sampling materials in the shipping/transport container containing ice
substitutes but do not seal.
Download data from the sampler via a laptop computer to a labeled diskette. Alternatively,
download to a data transfer device for later entry to a diskette.
• Return to the field office.
12.3.2 Procedures at the Field Office
Within 48 h following the end of the sampling period, the STN site operator will: return the modules to
the field office; complete all paperwork; seal the CAFDF in a plastic bag and tape the bag on the inside
of the cooler and package the modules and denuders in the cooler for pickup by the shipping agency
(Federal Express). It is strongly recommended that the site operator not freeze the samples
before they are shipped to RTI. The freezing of the filters may cause some of the ionic constituents
to change chemically The sample filters should be stored between 0° and 4° Centigrade until
they are placed in the coolers to be shipped to RTI. Illustrated packing instructions for the
modules can be found in Appendix A-5. Please see that appendix for details on packing the modules
for shipment to RTI. At the field office, the operator must complete the following:
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Retain the second page of the 3-page CAFDF and package the top copy in the shipping
container. Package the sampling modules, insert the ice packs in the shipping container,
and take the cooler or package to a drop point or arrange for pickup by the contracted
overnight air shipping company (Federal Express). Chain of custody seals on the shipping
coolers or containers are not required.
Complete the shipping air bill, attach it to the shipping container, and present the package to
the shipping agent.
12.3.3 Procedures in the STN Laboratory
The STN laboratory's procedures for receiving the sampling components and field data, disassembling
the sampling modules, and handling the filters and denuders after their distribution to the various
laboratories are covered in the STN laboratory's QAPP.
12.4 Filter and Sample Archival in the STN Laboratory
The laboratory database will assign a tracking number to all sample filters. Extracts and remnants of
filters will be archived in cold storage. Custody procedures for inventorying and archiving these
materials are given in the document Quality Assurance Project Plan: Chemical Speciation ofPM25
Filter Samples. Please contact Research Triangle Institute (see address in Table 3-1) for a copy of
this QAPP.
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13.0 Analytical Methods Requirements
Analytical methods requirements are given in the QAPP for the contract laboratory, Research Triangle
Institute, which will serve the Speciation Trends Network and other State and local agency speciation
sampling programs. Refer to that QAPP, Quality Assurance Plan for Chemical Speciation ofPM25
Filters for more information.
The analytes sought in PM2 5 for the STN include ions, metals, and various carbon-containing species.
Refer to Table 6-1 for specific analytes and the analytical methods for their determination. Figure 6-2
is a schematic of the sample analysis delivery order process to be followed by STN participants. The
flow diagram of Figure 6-3 shows how the filters will be processed and analyzed.
The STN laboratory's technical management and staff organization are presented in Section 4.0 of this
QAPP. Refer to Figure 4-2 for more information.
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14.0 Quality Control Requirements
Quality control is the overall system of technical activities that measures the performance of a process
against established standards to verify that such performance meets the stated requirements established
by the data user or stakeholder. In the case of the STN, QC activities are used to ensure and
document that measurement uncertainties, as discussed in Section 7.0, are maintained within specified
limits so that the data quality objective for trend detection can ultimately be met.
There are three distinct but interrelated functions that the PM2 5 STN QC program requires of State
and local field site participants, as follows:
1. The State or local site operator and his or her supervisor must make every effort to keep
the sampler maintained, cleaned, and operating properly; to retrieve samples according to
the network schedule; and to ship samples, field blanks, and trip blanks with supporting
hand-entered and computer-downloaded data to the STN laboratory on schedule.
2. The site operator must control the sampler's collection process through activities including
handling cassettes and sampling modules, properly calibrating samplers, and conducting
both scheduled and as-needed checks for leaks, flow rate, temperature, and pressure. Any
out-of-tolerance findings must be followed by corrective actions.
3. The third function is carrying out validation of data sets sent from the STN laboratory to the
State and local contacts and then reporting the data quality statistics that describe how
effective the QC system has been in achieving accuracy, bias, precision, and completeness
goals.
Table 14-1 contains a complete listing of field QC procedures, their frequency of performance, and the
acceptance criteria, i.e.; measurement quality objectives. Laboratory QC procedures are included in
the companion Quality Assurance Plan for Chemical Speciation ofPM25 Filters.
The MQOs have been established in two ways. Some of the MQOs have been derived to help ensure
that the DQO for identifying a trend of 5 percent (in either direction) can be made after 5 yr of
sampling. Other MQOs are based on requirements set forth in the Code of Federal Regulations or
by standards of good practice described in Section 2.12 of the U.S. Environmental Protection Agency
Quality Assurance Handbook for Air Pollution Measurement Systems (U. S. EPA, 1998). The
strategic plan for the STN (U.S. EPA, 1999) summarizes the QC requirements for field and laboratory
activities.
Table 14-1 also lists the action to be taken if a QC check shows a parameter to be out of specifications
and how the effectiveness of the corrective action is demonstrated and documented. Specific
procedures for implementing field QC activities are described in the sampler-specific SOPs given in
Appendix A to this quality assurance project plan
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TABLE 14-1. MQOs AND ASSOCIATED QC ACTIVITIES FOR THE PM,S
Measurement
Filter visual checks
Collocation with
another chemical
speciation monitor
Temperature:
check
audit
Pressure:
check
audit
Flow rate:
one-point
operational
check
one-point audit
Blanks:
trip blanks
field blanks
Frequency
before and after
each exposure
each sampling
day for 12 mini-
trends sites.
Then 7 or 55 sites,
each sampling
day thereafter.
monthly
quarterly
monthly
quarterly
monthly
quarterly
one set every 30 d
one set every 10
sampling d
Acceptance Criteria
(MQO)"
free of visible defects
see Table 7-3 for
maximum total error
of various chemical
species
+/-2°C of a certified
transfer standard
+1-1 °C of
independent standard
+/-10 mmHg vs.
certified transfer
standard
+/-10mmHg vs.
independent certified
transfer standard
+/- 10 percent of
working standard
+/-10 percent vs.
independent transfer
standard
unspecified at this
time
30 ug (gravimetric);
other limits to be
developed for
chemical species
concentrations
Corrective Action if Out
of Specification
record in lab database
and/or field data form;
filter may be discarded
prior to use; flagged or
invalidated after use
result used to calculate
replicate precision of
measurement system
note on QC data form;
troubleshoot; recalibrate
sensor and conduct
recheck; note on QC data
form
note on data form;
recalibrate sensor and
conduct recheck
note on data form;
recalibrate sensor and
conduct recheck
note on data form;
recalibrate sensor and
conduct recheck
troubleshoot (e.g., perform
leak check)
same as above
N/A
retroactive
troubleshooting and/or
data validation after
notification by laboratory
STN
Samples or
Channels
all filter types
all sampling
media
all temperature
sensors
all temperature
sensors
barometric
pressure
sensor
barometric
pressure
sensor
all flow
channels
all flow
channels
one per
channel
one per
channel
•Source: U.S. EPA, 1999.
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The remainder of this section describes the types of QC checks called for in the PM2 5 STN and the
procedures used to calculate values for the principal QC indicators. QC results should be recorded on
a form or in a field notebook dedicated to this purpose. Figure 14-1 illustrates the QA/QC data report
form proposed for use in the STN program. It is recommended that results of the QC checks be
entered into a control chart or graph to help visualize changes or drifts in sensor responses and to alert
the site operator to the need for preventive maintenance or repair of a speciation sampler. Detailed
information on multipoint calibrations and repairs should be recorded in the field notebook.
14.1 Quality Control Checks
14.1.1 Checks
A check, for this QAPP, is described as a verification by use of a transfer standard that the sampling
instrument is operating within acceptance limits. Usually, if the check fails to meet specification
troubleshooting would occur that might lead to recalibrating the instrument. Calibration is discussed in
Section 16.
14.1.2 Audits and Independent Checks
The chemical speciation samplers will be audited with an independent transfer standard on a quarterly
basis. Flow rate, temperature, and barometric pressure will be checked. For samplers with multiple
flow channels, each channel and the associated sensors will be audited. The transfer standards are to be
recertified or recalibrated annually.
14.1.3 Performance Evaluations
EPA has conducted several intercomparison studies of chemical speciation samplers. Intercomparisons
will continue with the 12-site mini-trends network, which will operate annually starting in December
2000.
The STN laboratory must also assess the accuracy of its analytical measurements. This will include
assessment of field blanks and other samples supplied by the EPA QA laboratory. Refer to the STN
laboratory QAPP for more information.
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QA/QC Form No. p^ g SJN QA/QC R
A. SITE AND SAMPLER INFORMATION
1. Site AIRS Code
2. Sampler S/N
3. Sampler Type
4. Sampler POC
B. DATE AND TIME CHECKS (Transfer Standard Name
Sample display date/time Transfer standard date/time
C. LEAK CHECKS (Transfer Standard Name
Channel number Manufacturer's s
1
2
3, etc.
D. TEMPERATURE CHECKS (Transfer Standard Name
Sensor location Sampler display (°C) Transfer
(°c
Ambient
Filter
Dry gas meter
Manifold
E. PRESSURE CHECKS (Transfer Standard Name
Sensor location Sampler display, Transfer
(mmHg) (mn
Ambient
Manifold
F. FLOW RATE CHECKS (Transfer Standard Name
Channel number Sampler display, Transfer
(L/min) standard display,
(L/min)
1
2
3, etc.
- P Pi R T PPi R M c. 1 (site retains)
trUKI hUKM c. 2 (Agency QAM)
c. 3 (Send to Lab)
5. Site Name
6 Interval: Month Quarter Special
7. Date(s) of QA/QC Checks
8. Operator's Name
Transfer Standard ID Number )
Date and time agree ±5 min? Action taken3
Transfer Standard ID Number )
Dedications met? Action taken and recheck results"
Transfer Standard ID Number )
standard Agreement ± 2 °C ? Action taken and
y) recheck results"
Transfer Standard ID Number )
standard, Agreement within Action taken and
iHg) ±10 mmHg? recheck results"
Transfer Standard ID Number )
Design flow rate, Agreement within Action taken and
(L/min) ±10percent?b recheck results"
Figure 14-1. STN QA/QC report form.
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14.2 QC Samples
Several types of standard QC samples are defined. The field program will mainly be concerned with
blanks sent by the STN laboratory to assess the effects of field operations and shipping and handling.
14.2.1 Blanks
Field Blanks—These provide an estimate of total measurement system contamination. By comparing
information from laboratory blanks against the field blanks, the amount of contamination due to field
activities can be estimated. In addition, if trip blanks are utilized, one can further evaluate contamination
occurring during field operations. Field blanks, loaded in sampling modules, for each type of filter will
be sent from the laboratory. The field operator is to handle the field blank sampling module just as
he/she would a module to be exposed but without drawing a sample through it. Corrective actions will
be taken when excessive contamination is found on field blanks.
The STN laboratory will also determine blank concentrations of analytes for each lot of Teflon™,
nylon, or quartz fiber filters received. The STN laboratory's QAPP and its SOPs discuss the
procedures.
Trip Blanks - These provide an estimate of measurement system contamination during transport to and
from the field sites. Trip blanks are usually instituted when field blank contamination is a problem or to
understand the measurement uncertainty occurring during transport. Trip blanks would be sent to the
field as a normal sample but would remain unopened. They would processed as a normal field sample
and sent back to the laboratory and treated as a routine sample from the point of sample receipt and
beyond.
14.3 Collocated Samplers
Collocated sampling will occur at 7 of the 55 sites in the full STN network. Data sets from collocated
samplers are intended to assess the precision of the total sampling, analysis, and data handling process,
but they can also be very useful in troubleshooting sampler siting and operational problems. Thus, such
data are useful in detecting quality problems that may not be evident from the results of periodic QC
checks of flow rates, temperature, and pressure. Workup and interpretation of collocated sampler data
sets are discussed in Section 22.0 of this QAPP.
14.4 Calculations of Accuracy, Bias, Precision, and Completeness
Accuracy is defined as the degree of agreement between an observed value and an accepted reference
value and includes a combination of random error (precision) and systematic error (bias). The
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following four accuracy checks are implemented in the chemical speciation program:
• Flow rate, temperature, barometric pressure, and other checks against a known standard
Collocation with an Federal Reference Method (FRM) sampler (gravimetric only)
Collocation with another PM2 5 speciation sampler (all analytes)
• Balance checks and other laboratory performance audits.
14.4.1 Accuracy of a Single Measurement
The error inherent in any single measurement is a function of both the underlying bias and the
imprecision (noise) in the measurement. Only after repeated measurements over a period of time is it
possible to separate bias and precision. The accuracy of a single measurement, dh can be calculated as
the difference between the measured value and a standard value and is expressed in the same units as
the original measurement.
di=Xi-Yi (14-1)
In addition, accuracy is often calculated as a percent difference from a standard of known value.
Calculate the percentage difference (d',) for a single calibration check /' is calculated using the following
equation:
d'i= xlOO (14-2)
where
d't = percentage difference for a single calibration check
Xi = standard value
Yt = indicated (measured) value
14.4.2 Calculation of Bias
Bias is a systematic deviation from the true value. Data must be averaged or aggregated over a period
of time or over a set of measurements in order to assess bias. Bias can be used to assess systematic
errors of a single sampler, a reporting organization, or an entire network. The following equation is
used to calculate bias:
(Yt-Xt) = Y-X (14-3)
2=1
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where
Xj = standard value
Yj = indicated (measured value)
N = total number of observations in a set of observations
Tand 3T = averages of all the Yf and Xf values, respectively.
Bias can also be expressed as a percentage of the standard or expected value. This definition is
applicable to flow rate, temperature, barometric pressure, and derived quantities such as air volume
through a filter. Laboratory biases can be calculated in a similar way.
14.4.3 Calculation of Precision
Precision defines the random variability of a set of measurements and excludes systematic bias.
Precision is given either in the units of measurement (e.g., standard deviation) or in relative units (relative
standard deviation or coefficient of variation [CV]). Like the calculation of bias, precision calculations
require a set of data collected over a period of time or over multiple observations.
Precision can be used to assess the random errors inherent in a single sampler, a reporting organization,
or an entire network. Random errors, characterized by the precision calculations, can be used as input
to the DQO model for the assessment of data trends. Excessive variability or noise in data can also
indicate equipment malfunction and the need for corrective action.
There are several other ways of expressing precision of a measurement, including the CV and the
confidence interval. The precision of a measurement is often a function of several different sources of
random variation. For example, the precision of a calculated particulate concentration may be a
function of the variability of measurement in calculating the flow rate, sampling temperature, and
pressure or the variability introduced in shipping/handling and by the laboratory. Assessment of these
errors is out of the scope of this QAPP but should be considered when performing advanced statistical
analysis of the data.
14.4.4Calculation of Completeness
The goal for completeness is 75%. Meeting the DQO for identification of a systematic trend in the data
requires that the data meet minimum completeness criteria. Data must span the time range of interest,
and there must be a sufficient number of measurements to reduce the statistical uncertainties. The DQO
analysis found that l-in-3 d sampling was sufficient to meet the DQO for assessing a data trend after
5 yr provided other uncertainties described above are controlled. Significant data loss, however, could
compromise the ability to assess the DQO.
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Completeness should be assessed quarterly and annually as shown in the following equation:
Nt " N'nmlld
= x 100 (14-5)
•'* ?
where
%C = percentage completeness
Nt = the total number of possible or potential measurements in the data set
N^iid = the number of missing or invalidated measurements
Assessment of completeness is applicable to derived measurements such as elemental concentration in
the air (for assessment of the DQO). Maintaining the level of data completeness ensures that the
minimum number of valid concentration data points are available to meet the DQO for speciation trends
identification after 5 yr of monitoring. To be counted for completeness, a sample must have passed all
of the various screens in the data validation process. Thus, a particular sample can be invalidated in
several different ways. Completeness assessment is an important element in the oversight of operational
and laboratory activities. Poor or marginal completeness figures should prompt the reporting
organization to re-evaluate and improve operating procedures.
14.5 References
U.S. EPA (Environmental Protection Agency). 1998. Quality Assurance Guidance Document 2. 12.
Monitoring PM25 in Ambient Air Using Designated Reference or Class I Equivalent Methods.
April 1998.
U.S. EPA (Environmental Protection Agency). 1999. Strategic Plan: Development of the
Particulate Matter (PM2^ Quality System for the Chemical Speciation Monitoring Trend Sites.
April 16, 1999.
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Page 1 of 4
15.0 Instrument/Equipment, Testing, Inspection and Maintenance
Requirements
This section discusses procedures to test, inspect, and maintain instruments and equipment to be used at
Speciation Trends Network field sites.
15.1 Testing and Acceptance Criteria
The STN will employ a set of testing and acceptance (T & A) criteria that were used to accept FRM
samplers. Table 15-1 lists the 13-step procedure by which final acceptance of each speciation sampler
will occur. If any deficiencies are discovered, the vendor should be called to report the deficiency and
begin the process of resolving the deficiency. Receiving papers, warranty information, and the 13-step
checklist noting the deficiency should be kept on file for reference and to document problem resolution.
A copy of the completed checklist is sent to the STN Project Officers .
Sampler calibration and verification devices also will require testing and acceptance upon receipt. Each
of the following devices must arrive with a certificate of National Institute of Standards and Technology
(NIST) traceability, an instruction booklet, and a warranty statement. Simple testing and acceptance
methods are listed below:
• Flow rate transfer standard (check against another flow rate standard)
Temperature transfer standard (check against a room thermometer, ice bath, or other
known temperature standard)
• Pressure transfer standard (check against another barometer or against a corrected
barometric pressure reading from a nearby national weather station).
Testing and acceptance criteria for the STN laboratory are discussed in the QAPP prepared by the
STN laboratory.
15.2 Maintenance
Many items may require maintenance in the STN. Preventive maintenance should be practiced in
accordance with the manufacturer's instructions given in the operator's manual and as experience is
gained. This section describes maintenance items for STN field equipment. The STN laboratory
QAPP discusses laboratory equipment maintenance. Maintenance of speciation samplers will become
increasingly important as the equipment ages over this multi-year study. STN site operators and
managers should read and follow maintenance instructions given in the sampler operator's manual and
updates and any maintenance bulletins that may be issued. Table 15-2 lists field items known to require
preventive maintenance. Others may be added to this list as experience is gained.
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TABLE 15-1. TESTING AND ACCEPTANCE CRITERIA CHECKLIST FOR
SPECIATION SAMPLERS
Check or Criteria
1. Check the enclosed packing list. Were all parts included in the delivery of the
sampler? (Including filter packs, denuders, and an operator's manual)
2. Were any of the enclosed parts broken during shipment of the sampler?
3. Check the enclosed assembly instructions. Did all the parts fit together during
assembly of the sampler?
4. Does the sampler's pump turn on when supplied with electrical power?
5. Using an independent timer, check to ensure the timer (clock) operates
properly. Check to see if the timer will automatically turn the sampler on and
off during a fixed time by setting the timer to turn the sampler on and off for a
short period while the operator observes.
6. Does the sampler's computer (display screen) boot up and operate properly?
Check to see if the computer (microprocessor) has working software (firmware)
by performing manual input of information to the sampler through the keyboard
and observe the results on the display screen.
7. Does the computer download information properly? Check this process by
attempting to download stored information through the RS232 port to a
computer and then to a diskette.
8. Does the internal cooling fan operate properly? Check this function by
supplying electrical power to the unit and listening for and observing the fan
turn on and off.
9. Do the temperature sensors operate properly? Check this function by
comparing sensor readings to an independent thermometer (or by warming the
sensor tip between your lingers to see if the temperature rises).
10. Does the filter holder (sampling module, cassette, or filter pack) hold the filter
correctly and does it connect easily and snugly to other components of the
sampling stream? Check this function by installing a filter in the sampling
module and by connecting the module to the sampling manifold, denuder, and
so on.
1 1 . Does the sampler' s casing or other enclosure protect internal units from the
weather? Check by visually inspecting the unit's latches, locks, seals, and
gaskets for gaps, holes, and leaks. Do not disassemble the unit.
12. Does the support structure (base, tripod, and so on) hold the sampling unit
secure, upright, and level?
1 3 . When all sampler parts are assembled and operated as a unit, does the sampler
function properly? Check this function by assembling the unit per
instructions, installing a filter or sampling module, setting the timer, activating
the sampler, and running it for 24 h as would be done for routine sampling.
Certifying Official's Signature Date Circle one ••
Yes?
Accept?
No?
Reject?
Note: Send copy of completed checklist to STN PO.
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Section No. 15
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TABLE 15-2. PREVENTIVE MAINTENANCE OF STN FIELD EQUIPMENT
Maintenance Item
Recommended Frequency
PM2.5 Speciation Samplers
1. Inspect and empty water collection bottle (f applicable).
2. Clean or change out impactor well (if applicable).
3. Check sampling intake lines/hoses (if applicable).
Each visit to site
Every 5th sampling day
1. Clean sampler inlet surfaces.
2. Clean impactor housing and jet surfaces (if applicable). Examine O-rings.
3. Clean interior of sampler case (if applicable).
4. Clean impactor downtube (if applicable).
5. Inspect denuder for breakage (RASS and MASS only). Replace denuders with
freshly coated ones and return used denuder to laboratory for refurbishment.
6. Inspect and service cooling air intake filter and fans.
Every 30 sampling events
or more often as needed or
as specified by the
network
1. Inspect O-rings of inlet and impactor assembly (if applicable). Apply light coat
of vacuum grease if required.
2. Clean sampler downtube (unless it contains a denuder).
3. Inspect and service O-rings of inlet and water seal gasket at downtube entry to
case.
4. Clean cyclones and manifolds upstream of sampler module.
5. Inspect and service O-rings of impactor assembly.
6. Inspect and service vacuum tubing, tube fittings, and other connections to
pump and electrical components.
7. Overhaul or replace sampling pump and solenoids.
Quarterly (every 3 months)
Per vendor guidance
Calibration and Check Devices
Flow rate transfer standard
1. Recertify vs. NIST standards.
2. Replace batteries (if applicable).
3. Visually check orifices for dust or breakage.
Temperature transfer standards (digital thermometer and TEOM)
1. Recertify vs. NIST standards.
2. Replace batteries.
3. Inspect probe tip and connecting cord.
Pressure transfer standard
1. Recertify vs. NIST standards.
2. Replace batteries.
Annually
As needed
Each use
Annually
As needed
Each use
Annually
As needed
15.2 Critical Spare Parts
Maintain an inventory of critical spare parts at the field office to prevent sampler downtime or
interruption of the required QC checks. The STN Laboratory will also maintain a spare parts inventory
to service the sampler modules and denuders. The field site should send the laboratory any spare parts
associated with the components the laboratory is supplying to the site (for example, O-rings that are
part of the sampling module that is sent back and forth between the laboratory and field site).
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Section No. 15
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Speciation sampler
O-rings for downtube connections (if applicable)
Connecting pressure tubing and compression or other types of fittings
• Filter packs or cassettes (to be forwarded to STN laboratory)
• Denuders (to be forwarded to STN laboratory)
Sampling lines/tubing (as applicable)
• Fuses
Digital thermometer, pressure device and orifice-based flow transfer standard
Spare batteries
Spare temperature probe
• Spare tubing
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Section No. 16
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16.0 Instrument Calibration and Frequency
16.1 Overview
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. For PM2 5 chemical speciation
instruments, calibration activities follow a two step process:
1. Certifying the calibration standard and/or transfer standard against an authoritative standard
(usually the National Institute of Standards and Technology).
2. Comparing the routine sampling or analytical instrument against a calibration or transfer
standard.
Parameters of the chemical speciation samplers that are subject to routine calibration checks in the field
include the following:
Flow rate (all filter channels)
Ambient temperature (one per instrument)
Filter or manifold temperature (one per channel or instrument)
• Barometric pressure (one per instrument).
Calibrations that involve permanent changes due to instrument adjustments should only be initiated
when it is obvious that a measurement parameter does not meet its acceptance criteria. Therefore, the
STN uses a two-tiered approach to calibration that involves the following:
Checks (see Section 14) to ensure that calibration is within acceptance criteria.
• Multipoint calibration when there is a failure during a one-point check. Instrument
adjustments occur during multipoint calibrations and are followed by a one-point check to
ensure that the transfer check standard is also operating properly.
16.2 Calibration and Verification of Field Instrumentation
Calibrations and checks for the chemical speciation samplers should generally follow the schedule set
for the PM2.5 gravimetric monitoring program. The speciation samplers are identical to the gravimetric
samplers with respect to ambient temperature, barometric pressure, date/time, and elapsed time. They
may differ from the gravimetric samplers, however, with respect to the flow rates, the number of
sampling channels that need to be calibrated, and the number and location of internal temperature
sensors.
After receipt and acceptance of a new chemical speciation sampler, single point calibrations of
temperature, barometric pressure, and multipoint calibrations of the flow rate sensors will be
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Section No. 16
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performed. After installation, regular checks and maintenance are carried out by the STN site operator
at the specified intervals. During each quarter, an internal audit is performed using an independent set
of standards. These checks are detailed along with the acceptance criteria in Table 16-1.
The following calibrations are performed in the field:
Verification/calibration of sampler's temperature probes and against the working
temperature standard,
Verification/calibration of the sampler barometric pressure against the working pressure
standard,
Verification/calibration of volumetric flow rate meter in the samplers against the working
flow rate standard, and
Verification of the sampler's internal clock against a timepiece.
Temperature Probes—The STN chemical speciation sampler has both ambient and internal
temperature probes. The STN site operators will perform one-point field verifications of both sensors
as needed or at least every month using a digital NIST-traceable temperature probe. A quarterly
temperature audit will be performed using an independent temperature standard.
Barometric Pressure—A NIST-traceable digital handheld pressure indicator will be used in the field
for one-point check of the sampler's pressure sensor as needed or at least every month. A quarterly
pressure audit will be performed using an independent pressure standard. A NIST-traceable digital
manometer will be used in the field office or field as a primary standard.
Time Sensor—The time sensor should be within + 5 min of a watch that has been recently checked and
set. Time (operators watch) can be set against an atomic clock that can be found on the Internet
(available online at http://www.fyi.net/~tharvey/time.html) or through a phone number (303-499-7111).
Flow Rate—As needed or at least monthly, a one-point flow rate verification will be performed for
each sampling stream using a NIST-traceable flow rate transfer standard. A quarterly flow rate audit
will be performed using an independent flow rate standard. The NIST-traceable calibration standard
will be used in the field office or field as a primary standard to perform multipoint calibrations once a
year or after a one-point verification failure.
Calibration Standards—Calibration standards for the temperature, barometric pressure, and flow rate
verifications and calibrations are given in Table 16-2. All calibration standards must be recertified
annually. The recertifications must be traceable to NIST. These recertifications may be done by the
standards' manufacturer or by a third-party metrology laboratory and must be performed in
accordance with American National Standard for Calibration - Calibration Laboratories and
Measuring and Test Equipment - General Requirements (ANSI/NCS1 Publication No. Z540-1-
1994). Records of all certifications must be maintained, including the identity of the NIST reference,
the procedure used to establish traceability, and a certificate of traceability.
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Temperature, barometric pressure, and flow rate transfer standards that are used to perform routine
verifications of STN chemical speciation samplers should be recertified at the same intervals as the
transfer standards for the PM2.5 gravimetric samplers. When both gravimetric samplers and chemical
speciation samplers are situated at the same monitoring location, the same equipment and transfer
standards may be used for both sets of samplers (if they are compatible with all samplers).
Calibration Procedures—Procedures for temperature, barometric pressure, and clock/timer
calibrations are typically identical to those used for the PM2 5 gravimetric samplers from the same
manufacturer, and it may be possible to follow SOPs developed for the gravimetric samplers.
Procedures for performing flow rate calibrations and leak checks for the chemical speciation samplers
may differ from the gravimetric sampler by the same manufacturer. Chemical speciation samplers
typically have several different air sampling streams, each of which is used to sample a different group
of chemical species. Whenever possible, the individual flow rates should be calibrated
independently of each other. In some models, however, this may not be possible due to the use of
vacuum manifolds and passive flow rate controls (e.g., flow control orifices). The manufacturer's
procedures for flow rate calibration should be followed.
Calibration Frequency—See Table 16-1 for a summary of calibration frequencies.
Documentation—All verifications and calibrations, as well as sampler and calibration equipment
maintenance, will be documented in field data records and notebooks and annotated with the flags
required in Appendix L of 40 Code of Federal Regulations (CFR) Part 50, the manufacturer's
operating instruction manual, and any others indicated in the field and laboratory SOPs. The records
will normally be controlled by the STN site operators, and they will be located in the field offices or
field collection sites when in use. Eventually, all calibration records will be appropriately filed (see
Section 9.0).
16. 3 Calibration and Verification of Laboratory Instrumentation
Calibration and verification of laboratory analytical equipment will follow the procedures given in
Quality Assurance Project Plan: Chemical Speciation of PM25 Filter Samples, prepared by the
STN contract laboratory.
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TABLE 16-1. ACCEPTANCE CRITERIA AND CALIBRATION AND
MAINTENANCE FREQUENCIES FOR PM,, CHEMICAL SPECIATION SAMPLERS
Criteria
Acceptance
Criterion
Frequency
SOP
Comments
Field Calibrations and Routine Checks
One-point flow rate
check
External leak check
Internal leak check
One-point
temperature check
Pressure
verification
Clock/timer
verification
Other calibrations
as specified by
manufacturer
±10 percent of
transfer standard
<80 mL/min
<80 mL/min
±2 °C of standard
ilOmmHg
1 min/mo
per manufacturer's
SOP
Monthly
Every five sampling
events or when
impactor serviced
If external leak
check fails
Monthly
Monthly
Monthly
Per manufacturer's
SOP
A-2, A-3,
A-4
A-2, A-3,
A-4
A-2, A-3,
A-4
A-2, A-3,
A-4
A-2, A-3,
A-4
Same as for gravimetric
samplers. Applies to all flow
channels.
Same as for gravimetric
samplers. Applies to all flow
channels.
Same as for gravimetric
samplers. Performed as a
troubleshooting procedure
only. May not be applicable
to all sampler designs.
Same as for gravimetric
samplers. Applies to all
temperature sensors.
Same as for gravimetric
samplers.
Same as for gravimetric
samplers.
Quarterly Checks and Audits
External leak check
Internal leak check
Temperature audit
Pressure audit
Flow rate audit
<80 mL/min
<80 mL/min
±2°C
ilOmmHg
±10 percent of audit
standard
±10 percent of
design flow rate
Quarterly
If external leak
check fails
Quarterly
Quarterly
Quarterly
Same as for gravimetric
samplers. Applies to all flow
channels.
Same as for gravimetric
samplers. Performed as a
troubleshooting procedure
only. May not be applicable
to all sampler designs.
Same as for gravimetric
samplers.
Same as for gravimetric
samplers.
Same as for gravimetric
samplers. Applies to all flow
channels.
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TABLE 16-1. (continued)
Criteria
Acceptance
Criterion
Frequency
SOP
Comments
Initial Installation Calibration
Temperature
calibration
Pressure calibration
Multipoint flow
rate calibration
Design flow rate
adjustment
±2 °C of standard
ilOmmHg
±10 percent of
transfer standard at
each flow rate
±2 percent of
design flow rate
On installation,
annually, or if
verification is failed
On installation, then
annually or if
verification is failed
On installation,
annually ,or if
verification is failed
As needed
Applies to ambient
temperature and all internal
filter temperature sensors.
Same as for gravimetric
samplers.
Applies to all flow channels
individually.
Applies to all flow channels
individually.
Sampler Maintenance
Impactor
Inlet/do wntube
cleaning
Filter chamber
cleaning
Cyclone and
manifold cleaning
Circulating fan filter
cleaning
Manufacturer-
recommended
maintenance
cleaned/changed
cleaned
cleaned
cleaned
cleaned/changed
per manufacturer's
SOP
Every five sampling
events
Every 15 sampling
events
Monthly
Approximately
every 30 use days.
To be determined.
Monthly
Per manufacturer's
SOP
If applicable to sampler
design. External leak check
should be performed
immediately after impactor
maintenance.
Same as for gravimetric
samplers.
If applicable to sampler
design.
Consult operator's manual
Same as for gravimetric
samplers.
Recertification of Standards (audit and calibration)*
Flow rate transfer
standard
Field thermometer
Field barometer
±2 percent of NIST-
traceable standard
±0.1 °C resolution,
±0.5 °C accuracy
±1 mmHg
resolution,
+S mmHa nr.r.iirflr.v
Annually
Annually
Annually
Same as for gravimetric
samplers.
Same as for gravimetric
samplers.
Same as for gravimetric
samplers.
' Recertifications may be done in-house, by the manufacturer of the device, or by a third party.
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TABLE 16-2. CALIBRATION STANDARDS FOR PM2S CHEMICAL SPECIATION
SAMPLERS
Description of Calibration
Standard
Digital thermometer
Digital pressure gauge
Flow meters
QA Objective
Acceptance
Criterion3
±0.5 °C
±0.7 percent13
±2 percent
Listed Uncertainty
for Calibration
Standard
Manufacturer
of Calibration
Standard
Model Number
of Calibration
Standard
a Acceptance criteria taken from page 1 of Element 16 in the Quality Assurance Project Plan for the PM2 5
Performance Evaluation Program (U.S. EPA, OAQPS. February 1999).
bThe pressure criterion (±5 mmHg) is equivalent to ±0.7 percent of atmospheric pressure (760 mmHg).
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17.0 Inspection/Acceptance for Supplies and Consumables
17.1 Purpose
This section establishes and documents a system for inspecting and accepting all collection site supplies
and consumables that may directly or indirectly affect the quality of the STN data. Documented
inspection and acceptance criteria will ensure the consistency of sampling media and associated
supplies and thus minimize their effect on analyte concentrations. The inspection and acceptance
process is of utmost importance to data sets that will be compiled for years to detect concentration
trends. The quality of the supplies and consumables used in the STN laboratory is of utmost
importance to the quality of the data set. Sampling media and chemicals used to calibrate the analytical
instruments are major concerns. The STN laboratory quality assurance project plan should be
consulted for details.
17.2 Critical Supplies and Consumables
17.2.1 Field Sites
This section describes the supplies needed by the field sites. The choice of field supplies and
consumables is, in part, dictated by the choice of speciation sampler. Table 17-1 lists the major items of
equipment needed for the STN. The State or local office must keep an inventory of all supplies and the
warranty period and certifications of equipment and can use Table 17-1 for this activity. Since
participants in the STN are also operating routine samplers for the mass PM2.5 Program, the calibration
and check standards may be used for the STN since they should meet the performance standards.
The contract laboratory will care for and track the cassettes and modules used in servicing the sampling
and analysis needs of the sites but will not carry them on its own inventory list.
As consumables run low or replacement purchases are required, the site operator will be responsible
for assisting in the procurement of these items by following the policies and procedures of the State or
local agency. The operator should purchase the same model equipment and spare parts and the same
consumables as were initially acquired, unless told to do otherwise.
17.3 Acceptance Criteria
Selection of major pieces of capital equipment is based on the item's advertised specifications and
performance in analysis of particulate matter and particulate matter extracts. Newly received field
equipment will be inspected to ensure all parts are present and undamaged. If damage has occurred in
shipping, the shipping agent will be notified. All new equipment for field or laboratory use should carry
a warranty for a 6-month to 1-yr period
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TABLE 17-1. STN FIELD EQUIPMENT AND SUPPLIES
Quantity
per Site
Operator
Equipment and Supply Description
Vendor/
Catalog No.
Make/Model No.
Speciation Sampling Equipment and Supplies
1
1
1
6 sets
To be
determined
Transport cases for loose equipment, supplies
Speciation sampler
Speciation sampler operating manual
Filter cassettes or sampling modules for speciation
sampler
Denuders for acid gases
Custody and field data form for each sample run
Sample shipping containers/ice packs (from lab)
Max./min. thermometer (if required)
Mounting Equipment and Tools
1
Tool kit
Calibration/Check Standards and Related Equipment
1
1 or more
1
1
Flow rate adapter (size depends on sampler brand)
Flow transfer standard (Chinook, BIOS, dry gas meter)
Pressure transfer standard (portable barometer)
Digital thermometer (or thermocouple calibrator)
Spare Parts
O-rings, tubing, fuses, impactor oil (if applicable),
impactor filters (if applicable), compression fittings
Cleaning and Maintenance Supplies and Equipment
Distilled water in spray bottle
Lint-free cloths and lint-free laboratory wipes
Additional warranty periods may be purchased; check equipment stated to NIST-traceable that is
subject to wear and tear during use (for example, temperature, pressure, and flow rate check devices)
should be returned annually to the vendor or an appropriate metrology laboratory for cleaning,
servicing, and recertification vs. NIST standards.
State and local agency personnel should use procurement logs for purchases of new equipment and
consumables. These logs should also indicate whether the items were accepted or rejected. In
addition, the laboratory and field personnel must keep an equipment inventory form that lists each piece
of equipment and its warranty dates. Section 15.0 of this QAPP contains the STN testing and
acceptance checklist, which State agencies may find useful to accept or reject a new sampler based on
the operational evaluation steps given in the T&A checklist.
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18.0 Data Acquisition Requirements (Nondirect Measurements)
This section identifies the types of indirectly acquired data needed for implementation and continuation
of the STN. These data are obtained from nonmeasurement sources and historic or concurrently
acquired databases not under the direct control of the STN.
18.1 Acquisition of Nondirect Measurement Data
The STN will produce almost all required data through its own field and laboratory operations. Some
data, however, will come from outside the network. This section lists several such data sources,
considers the quality of the data, and gives cautionary notes.
18.1.1 Chemical and Physical Properties Data
Physical and chemical properties data and values of fundamental constants are often needed in ambient
air studies. Examples of acceptable sources for fundamental units and constants and the relationships
between metric and U.S. or British units are
National Institute of Standards and Technology (available online at www.nist.gov)
International Organization for Standardization (ISO) (available online at www.iso.ch),
International Union of Pure and Applied Chemistry (IUPAC) (available online at
www.iupac.org), American National Standards Institute (ANSI) (www.ansi.org), and other
national and international standards organizations
U.S. Environmental Protection Agency (available online at www.epa.gov) sources
Current editions of handbooks on chemistry and physics such as the Handbook of Chemistry
and Physics (CRC Press) and Lange 's Handbook.
18.1.2 Sampler Operation and Manufacturers' Literature
Important information is found in the manufacturers' literature and operating manuals. Manuals for the
speciation samplers, the devices used to verify a sampler's proper operation (temperature sensors,
pressure gauges, and flow meters) and to calibrate it, data acquisition devices (laptop computers and
the programs they contain), and all analytical instrumentation used in the laboratory will be available.
18.1.3 Site Location Information
The highest priority objective of the PM2.5 STN data is the development of common spatial and
seasonal/annual compilations and displays of the concentrations of fine particle constituents across the
major urban areas of the country that can be used to determine if trend exist. Characterization of PM2 5
constituents in rural or regional environments (especially when data sets are combined with IMPROVE
data) is also possible if some sites are in transport and/or background locations. To select the best
locations for trends sites (especially any new sites), the network designers rely on several external
sources of information to minimize the collection of samples with components that are uncharacteristic
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of urban areas. Information about local emissions sources will be needed, for example, to avoid
locating a sampler too close to a particle source such as a chimney or an industrial vent. Information in
State or local agency databases could be appropriate, but this information needs to be spot-checked
for accuracy by visiting the proposed site and surveying the immediate (within a 300-m radius) area for
hot spots of particulate emissions.
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19.0 Data Management
19.1 Overview
This section presents information on how field and analytical data for the STN will be managed. It does
not address any data sets obtained outside the network nor does it include management of data that
may be given in summary and interpretive reports. This section addresses these data management
topics: recording, transformation, transmittal, reduction, validation, analysis, management, storage, and
retrieval. For the latest detailed information, refer to the STN Laboratory QAPP for chemical
speciation of PM2.5 filter samples.
Data for the STN come from several sources at both the STN Laboratory and the reporting
organizations that perform the field operations. The general flow of data between organizations is
illustrated in Figure 19-1. This figure emphasizes the organizational responsibilities, database systems,
and major operations. The STN laboratory, shown at the top of Figure 19-1, is responsible for
integrating data from the various laboratories with the shipping/receiving and chain-of-custody
information for the sample module sets provided to the ROs. After level 0 and level 1 validation, the
data are sent monthly through the Delivery Order Project Officer to the respective ROs for completion
of data validation. The accepted data sets are then sent by the ROs to RTI for upload to the
Aerometric Information Retrieval System (AIRS) database.
The following list describes the data management activities in more detail. This list is presented in
chronological order:
1. Presampling Laboratory Activities. This stage is conducted by the STN laboratory and
includes inputting weight values for the Teflon™ filters, filter lot acceptance test results, quality
control (QC) information such as the background concentrations of analytes on blank filters,
and records of laboratory temperature and humidity conditions during weighing sessions.
Secondly, information about shipping and COC are entered so that shipments of modules to
and from the various ROs can be tracked.
2. Field Activities. These data are initially written on the CAFDF and input by the STN
laboratory to its database management system (DBMS). Items include data on operation of the
speciation sampler (sample identification numbers, volume collected, ambient air temperature,
sampling flags indicating nonstandard operation, and so on) as well as operator's notes that can
be used for validating the data. All data necessary for the laboratory to calculate concentration
values and to validate data will be entered on the form, which is illustrated in the field SOPs
contained in the appendices to this QAPP.
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STN Laboratory
Reporting Organization
Internal QA/QC Data:
-COCD Forms
-Logbooks
-Shipping Records
-Audit Results
-Ca. Data, etc.
Figure 19.1 STN data flow overview
Postsampling Laboratory
Activities. The STN
laboratory will enter the
analytical chemistry data for
particle mass, elements,
ions, and carbon species
into the DBMS in this
stage. Data from QC
operations such as results
of multipoint calibrations
and linearity or span checks
and analysis of duplicate
samples, split samples,
blanks, and spiked samples
are also entered.
Data Validation at the
STN Laboratory. Data
validation will be carried
out at both the STN
laboratory and at the ROs.
The STN laboratory will
base its validation on
CAFDF forms, shipping
records, and analytical
QA/QC information.
These activities are
explained in Section 22.0
of this QAPP.
5. Data Reporting to the DOPO. The STN laboratory will transmit its validated data monthly to
the DOPO, who will pass the hardcopy and electronic data sets to the appropriate ROs. Data
from the laboratory and field are combined at this stage of operations and expressed in terms of
concentration units such as micrograms per cubic meter (• g/m3) of air. The electronic data set
will be in the AIRS format and accompanied by a QC report that further describes the flagging
of the data.
6. Data Validation Activities at the ROs. The ROs will further validate the data sets at levels 2
and 3, based on its internal records, analytical results of collocated sampling, and additional
screening tests. These activities are described in Section 22.0 of this QAPP.
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19.2 Data Management Activities at the STN Laboratory
Data management activities in the STN laboratory are described in the QAPP for laboratory analysis of
PM2.5 filters.
19.3 Data Management Activities at the RO
This section describes in more detail the data management activities and responsibilities of the ROs.
These data management activities should be conducted in accordance with the recommended practices
for data management described in Section 19.4.
19.3.1 Shipping and Receiving Records
The first stage of data management activities at the RO begins with receipt of a sampling module set
containing a partially completed CAFDF. The RO should record whenever a set of sampling modules
is received or shipped. Recording the following information in the RO's shipping/receiving area is
recommended:
Before Sampling:
• Date an unexposed set of sampling modules is received
Site and sampling date that the module set is to be used
Condition of the shipping container (if the container was damaged in shipment, the STN
laboratory should be notified through the DOPO)
• Warehousing area, if the set of sampling modules is not to be picked up immediately
• Person to whom the set of sampling modules is released for installation at the monitoring site
(the site operator or someone who will drop the modules at the site)
After Sampling:
• Person bringing the exposed set of sampling modules back to the shipping area
Site and sampling date that the sampling module set was exposed
Condition of the modules and the external shipping container
• Whether the ice substitute was precooled as required
• Federal Express air bill number and destination (the STN laboratory's address should be
pre-printed on air bills supplied in each module set)
Date and time that the cooler package was sent
One copy of the multipart CAFDF should be retained by the RO and checked to ensure
that all information is complete and legible.
These shipping and receiving records may be necessary references in case there is a discrepancy later
in data attribution. Each RO should develop its own system for maintaining shipping and receiving
records.
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19.3.2 Custody and Field Data Form
The CAFDF is shown in the sampler-specific SOPs in Appendix A and in Section 12.0 to this QAPP.
The field operator is responsible for filling the form in fully, completely, and accurately. The handwritten
notations on the form are the only source that the STN laboratory will have for critical information,
including the following:
Site/date that sampling actually occurred (usually preprinted on the custody and field data
form, but the operator may indicate changes)
Total volume(s) sampled for each of the sampling channels
Average temperature(s), flow(s), barometric pressure, and so on during the sampling
period
Actual sampling time
Data validation flags issued by the sampler
Information about any field and/or trip blanks included with the set of sampling modules
Operator's name and free-form notes.
The CAFDF will be formatted so that there is a specific space for each item above and will be
customized for the different speciation samplers to be used in the STN program. The operator will
repack the exposed modules and return the top copy of the CAFDF in the cooler package. The
operator is responsible for keeping the middle copy of the CAFDF and returning it to the designated
person at the RO for filing and later use in data validation.
19.3.3 Data Management Activities during Data Validation by the RO
Approximately 30 to 60 d after sampling has occurred, the DOPO will give each RO a data summary
and QC report prepared by the STN laboratory. The data summary will include an electronic file of
partially validated AIRS-formatted data that will require further validation by the RO. The STN
laboratory will have performed the following level 0 and level 1 validations on the delivered data:
Data attribution and COC verification
Validation of laboratory analytical data
Screening for data input/output problems.
Refer to Section 22 of this QAPP or the STN laboratory QAPP and its accompanying data
management SOPs for a full description of the data validation procedures that it will apply and the
checklist that is used.
The QC report delivered with the data file will include the following information that the RO will need in
order to complete the data validation:
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• Data records with missing or uncertain attribution or COC information (principally the
site/date of exposure or defective COC)
Data records marked questionable or invalid due to sampler data flags
Data records marked questionable or invalid due to laboratory problems
• Data records marked as possible outliers as a result of data screens applied by the STN
laboratory.
The RO will use its in-house records to examine data that have been flagged for attribution, sampler
flags, and outliers. It is possible that other data such as operator's notes, shipping/receiving records,
and QA/QC records can be used to validate the questioned data. There is usually little that can be done
if a measurement is flagged due to a laboratory problem. Questions about flags applied by the STN
laboratory should be sent through the DOPO.
After reviewing the STN laboratory's QC information, the RO must perform further validation on the
data set.
The specific procedures used for data validation are described in Section 22.0 of this QAPP. Data
handling methods and means for ensuring correct inputs/outputs during data handling are described in
Section 19.4.
19.3.4 Reporting Data to AIRS
After the data set has been finalized, each RO is responsible for returning the data set to the STN
laboratory for reporting to AIRS. The DOPO should be notified whenever a finalized data set is
transmitted to the STN laboratory for AIRS reporting.
19.4.Recommended Data Management Practices
This section describes recommended data handling practices that are applicable to the STN laboratory
and to the ROs. It is expected that all organizations participating in the STN program will follow EPA
guidelines such as good automated laboratory practices (GALPs).
19.4.1 Manual Data Entry
Manually entered data will include entries from the CAFDFs and chemical analyst's notes and
calculated concentrations for certain analyses. Hand-recorded data must necessarily also be manually
entered. The following techniques apply to manual data entry:
100 Percent Data Verification on Input—Manually entered data will be reviewed,
preferably by a different operator before it is committed to the database. Analytical data,
however, may be entered and proofed by the analyst who is responsible for generating the
data. Large amounts of data entered in bulk, such as a group of custody and field data
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forms entered by a data clerk, will be verified by duplicate entry in which two clerks enter
the same data. The two sets of inputs are then compared and discrepancies are resolved.
This is one of the most cost-effective methods for entering large amounts of data with
extremely high accuracy.
Range Checking—Many parameters lend themselves to checking for reasonable range
during or after data input. This type of checking is frequently very useful for manual entry
into screen forms to catch misplaced decimal points, incorrect units, and omitted or extra
digits.
19.4.2 Electronic Data Entry
The data sets sent from the STN laboratory to the ROs in electronic format will be delivered in AIRS
format. The data set will be visually reviewed before the file is closed and transmitted to the DOPO.
No further checking of data integrity will be done for electronic file transfers because these are internally
validated by the transmission medium.
The site operator will download a full set of information retained in the memory of the speciation
sampler by use of a download program and a laptop computer or data transfer device connected to the
sampler's RS232 port. The diskette will be retained by the site operator. No further checking of data
integrity will be done for electronic file transfers because these are internally validated by the
transmission medium. However, any information entered by the site operator (AIRs code, filter
numbers etc.) should be checked.
19.4.3 Sample and Data Tracking
Within the STN laboratory, a laboratory information management system will track the cycle of activity
for any filter for any sampling date and provide the history and present status of each sample. Analytical
samples will be internally tracked using a batch-oriented internal CO form. Module sets sent from the
STN laboratory to the ROs will be tracked in the laboratory's database system. These processes will
be described further in the STN laboratory QAPP and the data management SOP.
Each RO must also develop methods for tracking, shipping, and receiving data and for filing custody
and field data forms, audit reports, and other STN-related paperwork. These records may be
hardcopy or electronic, at the organization's discretion. Adoption of procedures similar to those
already in use for other programs such as the NAMS is encouraged. Recommendations for file
retention of documents and records are given in Section 9.0 of this QAPP.
19.4.4 Data Recording, Security, and Archiving
ROs and the STN laboratory should address data security in their data management processes for STN
and other reportable environmental data. ROs should implement practices such as the following (or
equivalent):
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Organizations must perform regular backups of the STN database.
As insurance against fires and other problems affecting an entire building, backup sets
should be kept off-site.
Weekly full backups of the database, with nightly incremental backups of changed
information, are recommended (at a minimum).
• Use of passwords should be required and enforced. Passwords should be issued to each
individual user of the data system that contains the STN data.
Dial-in modem access to computers or networks containing unreleased STN data should
be password-restricted, if possible, to authorized users.
Access to unreleased STN data should be restricted to personnel working on the STN
program.
Archival of raw data and other program information is important because it allows the processing and
validation of questioned data items to be reconstructed in the event of challenge or for research
purposes. Table 19-1 summarizes the data and records that must be retained by the STN laboratory
or RO for the life of the contract or for a term of 5 yr, unless otherwise specified by EPA. The
Location or Responsibility column describes a typical location where such information is often stored;
however, it may be preferable to store some information in a more centralized location. Laboratory
data records should be stored in a secure location with limited personnel access and with protection
against fire and natural disasters or with suitable backup copies stored separately.
19.5 Data Validation
19.5.1 Validation Checks and Procedures
Data validation is a combination of checking that data processing operations have been carried out
properly and of monitoring the quality of field and laboratory operations. If a problem is identified, the
data can be corrected or invalidated, and corrective actions can be taken to prevent its recurrence.
The following considerations relative to data management practices during data validation will apply:
Flags denoting error conditions or QA status will be associated with each observation
down to the level of individual analyses, but flags must never overwrite the data values so
that recovery and review of the original data will be possible. However, if a value is
deemed invalid, based upon associated flags and other evaluations, a null data code will be
substituted for the original value during entry to AIRS.
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TABLE 19-1. LABORATORY DATA RECORD ARCHIVAL SUMMARY
Type of Record
Completed custody and field data forms
Shipping records
Internal custody forms
Analytical and weighing raw data and instrument
traces
Analytical and weighing control charts
Weighing room environmental records
Certificates for all equipment and materials
standards (e.g., NIST or manufacturer's certificate)
Instrument calibration and QC records
Instrument maintenance and service records
Audit trails generated during data validation
QA records, including audit checklists and audit
reports
Copies of all partially validated data sets sent from
the STN laboratory to the DOPO
Copies of all fully validated data sets sent from
the ROs to AIRS
Purchasing records related to the STN program
Correspondence with the DOPO, including
consolidated sample requests
Correspondence and business records with
subcontractors involved with the STN
Training records
Laboratory 1
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
§
•
•
•
•
•
•
•
•
•
•
Data Archival Location or Responsibility
Lab: sample handling and archival
laboratory; RO: STN Manager's files
Shipping department files
Sample handling and archival laboratory
Weighing laboratory files
Laboratory files
Weighing laboratory files
Laboratory or QA Officer's files
Laboratory or QA Officer's files
Laboratory or field organization's files
Data processing department's files
QA files
STN Laboratory Program Manager's files
RO STN Manager's files
STN Laboratory Program Manager's files
RO: STN Manager's files
Lab: Program Manager's files
Program Manager's files
Program Manger's files
Data validation must include 100 percent manual review of both flagged and unflagged
data. A qualified reviewer, such as a qualified analyst or the QA Officer, should examine
each entry for reasonableness before it is reported out of the organization.
Completeness checks of the data set must be included in the validation system. This can
sometimes be automated, particularly for within-record checks. The RO should verify the
completeness of the data set created by the STN laboratory by checking that all exposures
have been accounted for by comparison with its custody and field data forms and other
records.
An audit trail is strongly recommended to document all changes made to the data set during
validation operations. Audit trails are described later in this section.
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Table 19-2 summarizes the validation checks applicable to the STN data sets.
Refer to Sections 22.0 and 23.0 of this QAPP for specific data validation procedures to be applied.
Validation procedures applicable to the STN laboratory are described in the laboratory QAPP.
19.5.2 Data Flagging
As a result of data validation, individual items will be marked by a variety of validation flags that
generally indicate that the item is suspicious or invalid. Invalid data should not be reported to
TABLE 19-2. VALIDATION CHECK SUMMARIES
Type of Data Check
Data parity and transmission protocol checks
Data review
Date and time consistency
Completeness of required fields
Range checking
Statistical outlier checking
Manual inspection of charts and reports
Sample batch data validation
Electronic
Transmission and
Storage
•
Manual Checks
•
•
•
•
Automated
Checks
•
•
•
•
•
AIRS. The STN laboratory database may contain a superset of the AIRS flags for internal use to
facilitate QC reporting; however, these flags will be mapped onto the set of approved AIRS flags
before they are released from the laboratory.
This section will be updated to include a summary of AIRS data flags after the parameter codes
for PM2 5 chemical speciation data have been issued by EPA.
19.5.3 Audit Trails
The audit trail is an important means for documenting changes to a data set made during validation. The
audit trail is important for establishing the reason for data changes, the authority under which the change
was made, and the data values before and after the change was applied. Organizations are strongly
urged to implement audit trails for the STN program. Typical reasons for making audit trail entries
include the following:
Corrections of data input due to human error
Application of revised calibration factors to sample results from an analytical run queue
Addition of new or supplementary data
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• Flagging of data that are invalid or suspect based on manual examination or automated
validation of the data
Logging of the date and time when automated data validation programs are run (this is an
instance when the audit trail entry is not record-specific).
Audit trail records usually include the following fields:
Operator's identify (identification code)
• Date and time of the change
Table and field names for the changed datum
Complete identifying information for the item changed (date, time, and so on)
Value of the item before and after the change (or image of the entire record before and
after the change).
19.6 Data Transformations
Calculations for transforming analytical data in units of mass per filter or mass per volume of extraction
solution to concentration units are relatively straightforward. Table 19-3 summarizes transformations
applied to analytical data to produce volume, mass, and concentration data.
TABLE 19-3. RAW DATA CALCULATIONS
Parameter
Volume of air
sampled through
filter
Total mass on filter
(M2.5)
PM25
concentration
(CPM25)
Units
m3
• j?
&
• g/m3
Conversion type
Calculated from average flow rate (Qavg) in L/min and
total elapsed sampling time, t, multiplied by the unit
conversion (m3/L)
Calculated from filter postsampling weight (Mf) and
filter presampling weight (M;) in mg, multiplied by the
unit conversion (• g/mg)
Calculated from laboratory data and sampled air
volume
Equation
V = O x t x 10"3
va Vavg L 1VJ
M2.5 = (Mf-Mi)X 1()3
CPM2 5 = M2 5/Va
NOTE: Table 19-3 is applicable to the general categories ofanalytes to be produced by the
STN program. Calculations within these categories are similar. Standard calculations such as
unit conversions and equations for calculating standard statistics are not provided. Calculations
involved in instrument calibrations are described in the respective SOPs and operating manuals
for the PM2 5 speciation sampler.
19.7 Data Transmittal
Transmittal of data occurs when one person or location transfers data to another or when data are
copied from one form to another. Examples of data transmittal include copying entries from a notebook
to a data entry form, keying information from a handwritten data entry form to a computer file, and
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transferring data electronically via telephone or computer network connections.
Table 19-4 summarizes data transfer operations and the QA measures applied to ensure accurate and
complete transfers into the organization's database management system.
19.8 Data Reduction
Data reduction is the process of aggregating and summarizing results so they can be understood and
interpreted. Examples of data reduction products are
Average PM2 5 mass or species concentration
Accuracy, bias, and precision statistics based on accumulated FRM and speciation sampler
data
Data completeness reports based on the number of valid samples collected and analyzed
during a defined period of time versus the expected number of samples.
19.9 Data Analysis
Management of data analysis techniques and products is beyond the scope of the STN field or
laboratory QAPP. Management procedures will be developed by data analysis participants.
19.10 Data Storage and Retrieval
STN laboratory data storage and retrieval techniques are described in the laboratory QAPP and
SOPs.
Data storage and retrieval techniques for the ROs should be described in their system documentation or
through in-house SOPs developed for the STN program. Documentation of data storage and retrieval
should include a summary of the type of data, the media on which they are stored, security measures for
safeguarding the data against destruction and access by unauthorized persons, and the retention time for
the data.
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TABLE 19-4. DATA TRANSFER OPERATIONS
Description of Data
Transfer
Keying weighing data
and chemical analysis
results into the STN
laboratory's database
Electronic data transfers
Filter receipt, custody and
field data forms
Verifications/calibrations
and audit data
• Field site sampler
• Laboratory instruments
AIRS data summaries
Finalized AIRS data
summaries
Originator
Laboratory analyst
(handwritten data forms)
Between computers or
over networks
Site operator
Field auditor; field site
operator
laboratory auditor;
laboratory analysts
Laboratory data clerk and
data supervisor
STN laboratory
Recipient
Laboratory analyst
(enters data into the
database using screen
forms)
—
Laboratory data clerk
Laboratory data clerk
AIRS (EPA) (via the
DOPO)
AIRS
QA Measures Applied
100 percent review;
random checks by the QA
Manager or staff
Parity checking;
transmission protocols;
test messages
Filter numbers are
verified; data checked for
completeness and
accuracy; duplicate key
entry for custody and
field data forms
Field data entries are
checked by field operator.
Laboratory data checked
by laboratory supervisor
and spot-checked by QA
staff
Entries checked by
laboratory data clerk and
data supervisor; OAQPS
QA Officer
Checked by the
laboratory's Program
Manager or QA Officer
The contract laboratory will reduce data consistently to an agreed upon format in order to
upload it to AIRS. Each RO may choose to develop additional data reduction procedures for
data interpretation to assist with data validation and reporting of its own data. Development of
unified procedures to be applied across the STN is encouraged. EPA 's Office of Air Quality,
Planning and Standards will assist in coordinating the development of such procedures. Simple
reports are easily generated using a PC equipped with a modern spreadsheet program such as
Microsoft Excel® or Lotus® or with a more specialized statistical package such as SAS®.
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20.0 Assessment and Response Actions
20.1 Types of Assessments
The following types of assessments will be performed by the STN:
Management systems reviews (MSRs)
Network reviews
Technical systems audits (TSAs)
Performance evaluations (PEs)
Audits of data quality (ADQs)
Data quality assessments (DQAs)
MSRs are described in Guidance for Preparing, Conducting, and Reporting the Results of
Management Systems Reviews (U.S. Environmental Protection Agency Publication No. EPA QA/G-
3). TSAs, PEs, and ADQs are described in Guidance on Technical Audits and Related
Assessments for Environmental Data Operations (EPA Publication No. EPA QA/G-7). DQAs are
described in Guidance for Data Quality Assessment (EPA Publication No. EPA QA/G-9).
Information in these documents follow the specifications and guidance given in the American Society for
Quality Publication ANSI/ASQC E4-1994.
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20.2 Assessment Frequency
Assessments will be performed at the frequency described in Table 20-1.
Table 20-1 Types of Assessments for the STN
Agency
NAREL
R&IE
R&IE
OAQPS-EMAD
OAQPS-EMAD
Regional Offices
Type of Assessment
ISA, DQAs, MSRs and PEs
TSAs
Performance Audits
TSAs
MSRs
Network Reviews
Agency Assessed
RTI
State and local
agencies
State and local
agencies
RTI, NAREL, State
and Local agencies,
Regional offices and
R&IE
RTI, NAREL, State
and Local agencies,
Regional offices and
R&IE
State and local
agencies
Frequency
Annually
Annually*
Annually*
As needed by
EMAD
determination
As needed by
EMAD
determination
Once every 3
years
! Not all STN samplers will be audited. Perhaps up to 25 % of the network annually.
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20.3 Acceptance Criteria
Assessments will be based on the acceptance criteria to be developed based on the DQOs and findings
from the 12-site mini-trends network. Figure 20-1 outlines the TSA acceptance criteria for field and
laboratory operations for the gravimetric portion of the STN.
20.4 Assessment Schedules
TSAs for the 12-site mini-trends network will be conducted between 3 to 6 months of the start of
sampling. TSAs for the remaining sites in the full PM2 5 STN will be conducted within 1 year of the
start of sampling.
20.5 Assessment Personnel
Assessors should have a minimum of 4 years' full-time appropriate and practical experience (not
including training) in air quality monitoring, including at least 2 years in quality assurance activities.
Lead assessors should have assessment, technical, and quality system experience. Other assessment
team members also may have such experience, or they may have only technical experience and
currently be receiving assessment and QA training.
Lead assessors should have knowledge and understanding of the applicable environmental statutes and
regulations. They should be familiar with EPA management systems and with the organizational and
operating procedures for environmental data collection. Lead assessors should have a working
knowledge of the technical assessment techniques for examining, questioning, evaluating, and reporting
environmental data operations and for following up on response actions. They need to understand the
assessment planning process. They also need technical understanding of the PM2 5 STN. In general,
they need to be able to evaluate the PM2.5 STNs scope of work, its management system structure, and
its operating procedures and to judge the PM2.5 STN's adequacy compared to this QAPP.
Assessment team members should be familiar with technical assessment concepts and techniques and
with the structure and operating procedures for environmental data collection. They should have
technical knowledge of the PM2 5 STN. Depending on the scope of the technical assessment,
assessors may need to meet additional qualifications, including health and safety requirements.
Technical specialists, who have specialized knowledge of PM2.5 STN and basic knowledge of
assessment techniques and procedures, may participate in assessments. They may need basic training
in assessment techniques and procedures. Under the direct supervision of the lead assessor, they may
help prepare the technical portions of assessment checklists and may conduct the technical portions of
an assessment. They can verify findings and observations that are made by other assessment team
members concerning any specialized technical aspects of the PM2.5 STN.
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Three general standards for assessors are as follows:
The assessors assigned to conduct a specific assessment should collectively possess
adequate professional proficiency for the tasks required. This standard places
responsibility on the assessors' organization to ensure that the assessment is conducted
by assessors who collectively have the technical knowledge and assessment skills
necessary for the assessment. This standard applies to the assessors as a group, not
necessarily to every individual assessor.
The assessors should be free from personal and external barriers to independence,
organizationally independent, and able to maintain an independent attitude and
appearance. This standard places responsibility on the assessors' organization and on
individual assessors to maintain independence so that assessment findings will be both
objective and viewed as objective by knowledgeable third parties.
The assessors should use due professional care in conducting the assessment and in
preparing related reports. This standard places responsibility on the assessors'
organization and on individual assessors to follow all applicable standards in conducting
assessments. Assessors should use sound professional judgment in determining the
standards that are to be applied to the assessment.
The authority and independence of assessors, and the limits on their authority, must be clearly defined in
the organization's quality documents. Assessment personnel should have sufficient authority, access to
programs and managers, and organizational freedom to
Identify and document problems that affect quality;
Identify and cite noteworthy practices that may be shared with others to improve the
quality of their operations and products;
Propose recommendations (if requested) for resolving problems that affect quality;
Independently confirm implementation and effectiveness of solutions; and
When problems are identified, provide documented assurance (if requested) to line
management that further work performed will be monitored carefully until the
deficiencies are suitably resolved.
Prior to an assessment, it is important to establish whether the assessors have the authority to stop or
suspend work if they observe conditions that present a clear danger to personnel health or safety or that
adversely affect data quality. If not, assessors need to know what communication they may be required
to have with the authorized official who can stop work. Safely is paramount; no assessments will be
made in any unsafe conditions.
20.6 Assessment Reports
The product of an assessment is a written report. The objective of the report is to communicate
assessment findings to the proper levels of management in EPA and the assessed organization. The
report must include
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Assessment/review title and number and any other identifying information;
The lead assessor, assessment team members, and the management and key personnel
of the assessed organization;
Background information about the PM2 5 STN activity being assessed, the purpose and
date(s) of the assessment, the particular parameter evaluated, and a brief description of
the assessment process;
Summary and conclusions of the assessment and proposed response actions; and
Attachments and appendices that include all evaluation and finding information.
Typically, two reports are produced: the draft findings report (DFR) and the quality assurance final
report (QAFR). The lead assessor is responsible for producing the DFR and should organize the work
to get the report written during the audit debriefing that should occur at the end of the audit. In this case
the DFR might simply be a listing of the positive findings as well as the findings that call for some
corrective action. A full DFR should be written with 15 working days of the audit.
The DFR will be submitted for review by the EPA Speciation QA Coordinator and the EPA project
official. The EPA Lead Assessor will send the DFR, through the EPA project official, to the assessed
organization for its comments. The assessed organization should be given the maximum opportunity to
respond to the DFR. This response should address the findings and discuss how any response actions
will be resolved. If the assessed organization disagrees with the findings, the response can contain a
rebuttal. Upon receipt of this response, the lead assessor should determine if the response adequately
addresses the findings, if a follow-up assessment is required, and when it is appropriate to close out the
assessment.
After the assessed organization's comments have been addressed, the FR should be prepared. The FR
should be similar in format to the DFR and should be based on the DFR. Typically, the assessed
organization's response will be integrated into the summary of findings and response actions sections.
The lead assessor is responsible for correcting any findings that are demonstrated to be incorrect by
objective evidence to the contrary supplied by the assessed organization. Opinions of the assessed
organization that differ from those of the assessors are not valid reasons to alter the report. The FR
should be submitted to the EPA Speciation QAC and copies should be sent to the EPA project official
and to the assessed organization.
Documentation for TSAs and network reviews will be archived at the EPA Regional Offices and
tracked using the AIRS. The results of MSRs will be on file in EPA's Monitoring and Quality
Assurance Group, which is ultimately responsible for implementing the PM2 5 monitoring network.
20.7 Implementation of Response Actions
After an assessment, any necessary response actions should be timely and effective. In certain cases, it
may be necessary to perform response actions as quickly as possible. Such cases may include adverse
impacts on data quality and threats to personnel health and safety. Verbal approval from responsible
parties suffices under these conditions.
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OAQPS uses a response action form to document any nonconformances that require actions and the
resolution of them. This form includes the signatures of the individual identifying the need for response
action, the EPA project official, the EPA Speciation QAM, and the individual responsible for
implementing the response action. The problem requiring response action, the proposed response
action, and the approach for evaluating the response action should be described.
Response actions encompass immediate actions to eliminate problems such as errors in calibrations,
weighing, and other internal procedural problems and long-range response actions instituted to improve
overall data quality. Management of the assessed organization responsible for the assessed activities is
responsible for ensuring that effective and timely response actions occur. The response actions should
address the following:
Measures to correct each nonconformance,
Identification of all root causes for significant deficiencies,
Determination of the existence of similar deficiencies,
Response actions to preclude recurrence of like or similar deficiencies,
Assignment of response action responsibility, and
Completion dates for each response action.
Management of the assessed organization should implement the response actions and provide objective
evidence to EPA of the effectiveness of the correction. Once such objective evidence is received, the
assessment will be closed unless a reassessment is planned. In some cases, the assessment team may
be needed to confirm the successful implementation of response actions.
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20.8 References
American Society for Quality. 1994. Specifications and Guidelines for Quality Systems for
Environmental Data Collection and Environmental Technology Programs. ANSI/ASQC E4-
1994. Milwaukee, WI.
U.S. Environmental Protection Agency. 1994. Guidance for Preparing, Conducting, and Reporting
the Results of Management Systems Reviews. Draft EPA Publication No. EPA QA/G-3.
Washington, DC.
U.S. Environmental Protection Agency. 1998a. Quality Assurance Handbook for Air Pollution
Measurement Systems, Volume II: Part 1 Ambient Air Quality Monitoring Program Quality
System Development. EPA Publication No. EPA-454/R-98-004. Washington, DC.
U.S. Environmental Protection Agency. 1998b. SLAMS/NAMS/PAMS Network Review Guidance.
EPA Publication No. EPA-454/R-98-003. Washington, DC.
U.S. Environmental Protection Agency. 1998c. Guidance for Data Quality Assessment: Practical
Methods for Data Analysis. EPA Publication No. EPA QA/G-9. Washington, DC.
U.S. Environmental Protection Agency. 1999. Guidance on Technical Audits and Related
Assessments for Environmental Data Operations. EPA Publication No. EPA QA/G-7. Washington,
DC.
U.S. Government Accounting Office. 1994. Government Auditing Standards. Washington, DC.
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21. 0 Reports to Management
This section describes the type, content, distribution, and frequency of submission of QA reports for the
PM2 5 Speciation Trends Network. Regular QA reporting to management serves the following needs:
Documentation of adherence to schedules for delivery of equipment, data, and reports
Documentation of deviations from approved QA and SOPs, and the impact of these
deviations on data quality
Analysis of the potential uncertainties in decisions based on the data.
Section 21.1 discusses how QA information for the new STN sampling sites, as part of the NAMS
network, will be reported along with other NAMS QA data by the reporting organization. Section
21.2 describes additional QA reporting and information sources that are applicable to the STN
sampling sites during the implementation phase of the program.
21.0 NAMS Reporting
As part of the NAMS network, the STN must adhere to basic reporting schedules, as described in the
Quality Assurance Handbook for Air Pollution Measurement Systems, Volume n, Part 1, Section
16 (EPA 454/R-98-004, August 1998). The handbook should be consulted for recommendations and
suggestions regarding report preparation and formats. Table 21-1 lists standard QA reports to
management that are applicable to the STN. A reporting organization may have other reports to add to
the list or may create reports that are combinations of those listed in the table.
Corrective Action Reports—Corrective Action Reports (CARs) for the STN should be modeled on a
reporting organization's existing CAR system, if possible. The CARs themselves are typically retained
by the organization, but summaries and narratives based on CARs should be included in the annual QA
report to management. The CAR file is also subject to system audit to ensure that the file is being
maintained and that CARs are being turned in and acted upon as needed.
Control Charts—The control chart is primarily a tool used internally to maintain control of an
organization's quality systems. Each reporting organization should define a control charting program
that meets its needs. Some considerations are as follows:
• What parameters should be charted? For the STN field program, regular flow checks
against a standard reference device and temperature sensor or transducer output in
response to a standard input should be considered for charting.
How frequently to chart? Each measurement of the same standard or reference should be
charted. Avoid mixing results obtained from different standards on a single control chart.
• How to calculate control limits? Parameters may be assessed against fixed limits rather
than by statistically derived limits. Variations are frequently encountered (for example,
certain parameters may have only one control limit).
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Table 21-1 Types of Assessment Reports
Type of Report
Corrective
Action
Request
Control Chart
Self-
Assessment
Results
Independent
Assessment
Results
Data Set
Review
Annual
Quality
Assurance
Report to
Management
Annual
Quality
Assurance
Final Report
Contents
Description of problem;
recommended action;
feedback on resolution
Repetitive activity; plot
of control limits vs.
time. Update whenever
a new check or
calibration is
performed.
Summary of internal
technical systems
audit, audits of data
quality, and
performance evaluation
results;
recommendations for
action, as needed
Summary of external
technical systems
audits, audits of data
quality, and
performance
evaluations; corrective
actions if
unsatisfactory results
(out of limits)
Notes on Level 2 and
Level 3 data validation;
actions taken to correct
or sequester data
Executive summary.
Precision, bias, and
system and
performance audit
results.
Executive summary.
Precision, bias, and
system and
performance audit
results.
Report Author
EPA Regional
Office
STN site
operator or
State/local
Agency
State and
Local
Agencies
EPA Regional
Office, NAREL
andR&IE
State and
Local
Agencies
EPA Regional
Office
OAQPS-
EMAD
Suggested Reporting Frequency
As
Required
•
•
•
Monthly
•
Quarterly
Yearly
•
•
•
•
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How often should control limits be recalculated? Statistical control limits should be
calculated as soon as there are enough observations to make a reliable sample. Seven or
eight observations are often sufficient. Control limits should not be recalculated too often.
For a parameter that is charted monthly or quarterly, annual recalculation of control limits
should be sufficient.
• What if there is a significant process change? Any significant change, such as replacement
of a standard or major overhaul of the instrument, may be reason to restart the control
charting process. This means that existing control limits may not apply to subsequent
observations, and it is necessary to collect a new set of data for calculating revised control
limits.
Self-Assessment Results—STN samplers should be subject to internal technical systems audits, audits
of data quality, and performance evaluations by State and local agencies like all other monitoring
equipment atNAMS sites. If problems are found, corrective actions should be initiated immediately
and documented using the CAR process. Results of self-assessments should be summarized in the next
annual QA report to management. Unsatisfactory results and corrective actions should be discussed.
Independent Assessment Results—Under the STN, external technical system audits, audits of data
quality, and performance evaluations may be conducted by a variety of authorities including EPA
Regional Offices, particularly during the initial phases of network operation. If deficiencies are found,
corrective actions should be initiated and documented. Recommendations and corrective actions should
be discussed in the annual QA report to management.
Data Set Review— Following Level 0 and Level 1 data validation by the STN Laboratory, chemical
species concentration data will be sent to the State and local agencies for review. Upon acceptance of
the level 0 & 1 data it will be entered into AIRS data base. State and local agencies will perform
Level 2 and Level 3 data validation and will report the results of the validation in the annual QA report
to management. These two data validation levels are defined as follows:
• Level 2 data validation involves comparisons with other independent data sets for external
consistency. These comparisons include, for example, intercomparing collocated
measurements.
• Level 3 validation involves a more detailed analysis as part of the data interpretation
process when inconsistencies in analysis and modeling results are found to be caused by
measurement errors.
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Quality Assurance Report to Management—The annual QA report to management is a key synopsis
of an organization's operations. It should include an executive summary of all activities; a detailed
summary of accuracy and precision achieved; and discussion of outstanding problems, CARs, and audit
findings. STN samplers should be discussed specifically with regard to achieving the measurement
quality objectives for total error defined in Section 7.0 of this QAPP. Because the STN is a new effort,
systematic problems should be highlighted so that corrective actions can be taken at a networkwide
level.
Information about the STN monitoring sites operated by an organization should be an integral part of
the annual QA report to management. The QA handbook recommends the following general content
for the annual QA report to management:
• Executive summary—a short section summarizing the report. It should contain a checklist
graphic showing how the reporting organization has met its quality goals during the reporting
period.
Network background and present status
• Data quality objectives for measurement systems
QA procedures
Results of QA activities
Recommendations for further QA work, with suggestions for improving performance and
fixing problems with equipment, personnel training, infrastructure needs, and so on.
21.2 Additional Quality-Related Reports for the STN
The primary additional quality-related report for the STN is the STN Sample Request. Success of the
STN is critically dependent on planning and communications among the reporting organization, the DO
PO, and the STN Laboratory. Because the laboratory is responsible for distributing filters and sampling
modules on an extremely tight schedule, it must know monitoring schedules and filter requirements well
in advance. This is done through the STN sample request process. Accurate sample requests must be
transmitted to the STN Laboratory no less than 3 months in advance. Ordering the correct number of
filters and other media can be a lengthy process because some manufacturers require several months
for the special filter conditioning required for STN. Firing of quartz filters and conditioning of nylon
filters can take extra time if done at the STN Laboratory.
The format of the STN Sample Request Form will be developed by the DOPOs, EPA/OAQPS, and
the STN Laboratory. Each sample request should provide the following information for each site, at a
minimum:
AIRS site code
Name and address of the STN sampling site
• Name and address of reporting organization
• Name, telephone number, and e-mail address of reporting organization's administrative
contact for the STN program
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Section No. 21
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Page 5 of 5
• Name, telephone number, and e-mail address of STN site operator
Address for receiving unexposed module sets
Number of STN samplers operated at the site
Type of STN sampler(s) (i.e., manufacturer and model number)
Summary of filters and denuders to be used and analytes to be determined (the normal
configuration for each monitor type will be sent unless exceptions are specified in the
request; these exceptions include extra sampling channels, filter types, and so on)
Any special requests, such as "extra" modules for the reporting organization's quality control
program
Scheduled dates of sampling (specific dates are necessary, not" l-in-3" for example)
21.2.1 STN Sample Request Changes
Because the sample requests are made several months in advance, a reporting organization may need to
make changes to previously submitted requests before the sampling date. This could occur because of
a substitution of a different sampler model, change of shipping address, addition of filter channels, and
so on In this case, the DOPO will be informed immediately so that the STN Laboratory can be
notified of the change. Small changes can usually be accommodated, but changes involving substantially
more filters (e.g., going from every-third-day sampling to daily sampling at a site) might require
significant lead time for the STN Laboratory to accommodate.
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PM2 5 STN QAPP
Section No. 22
Re vision No.: 4
Date: 6/00
Page 1 of 13
22.0 Data Review, Validation, and Verification Requirements
This section describes the verification and validation process, which is used to decide the degree to
which each data item has met applicable quality specifications. The specific requirements for
verification and validation will be developed by estimating the potential effect that each error component
may have on the usability of the associated data item, its contribution to the quality of the reduced and
analyzed data, and its effect on attainment of the DQOs.
Verification and validation are not the same as data quality assessment or evaluation of the DQOs,
processes which are described later in this QAPP. Only after the data set has been verified and
validated can it be fully assessed and/or used to address the specific scientific and regulatory questions
embodied in the DQOs.
After the data set has been subjected to the verification and validation process, it is reported to the
AIRS by the STN Laboratory. Data validation reports should be included in regular quality control
reports to management. These reports should include the following information, at a minimum:
Time interval covered by the report
Site identification(s)
Sampler identification(s)
Total number of valid observations sent to AIRS
Number of flagged observations sent to AIRS, categorized by analyte and flag
Number of invalid observations (not sent to AIRS), by analyte
Statement of significant corrective actions taken.
22.1 Data Verification and Validation Responsibilities
Verification of data for the PM2 5 chemical Speciation Trends Network is the joint responsibility of the
reporting organization, which runs the field component of the program, and the STN laboratory, which
analyzes the samples and calculates and reports the data. Table 22-1 describes the respective
responsibilities of the field and laboratory components for data verification and validation.
22.2 Corrective Action Reporting Process
Each reporting organization and the STN laboratory should have a Corrective Action Reporting (CAR)
process in place. Ideally, this process should closely resemble corrective action procedures used on
other monitoring activities conducted by the organization. This process should consist of the following
elements:
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TABLE 22-1. DATA VERIFICATION ACTIVITIES FOR THE PM,. SPECIATION TRENDS NETWORK
Verification Activity
Reporting Organization
STN Laboratory
Data source attribution. Verify that the site, date, time,
and channel assignments are correct. Logbooks,
reporting forms, data custody sheets, and electronic
data transmittals should be checked for consistency.
The reporting organization should compare the
information on the custody and field data form
(CAFDF) with labels on modules received. Report any
discrepancies to the STN laboratory.
The CAFDF forms should be corrected to reflect the
actual module used for a particular sampling channel, if
other than originally assigned by the laboratory.
Discrepancies in module assignment due to procedural
errors in the field operation should be noted and
corrected using the CAR process.
The STN Laboratory is responsible for
generating the CAFDF sheets and placing
corresponding labels on sample modules sent
to the field.
The laboratory should respond immediately to
notifications from the field of shipped modules
that do not agree with the CAFDF sheet.
The laboratory database management system
(DBMS) will accommodate changes of module
assignment reported by the field.
Discrepancies in module assignment due to
procedural errors in the laboratory sample
handling operation should be noted and
corrected using the CAR process.
Results for samples that cannot be positively
identified must be flagged as invalid in AIRS.
Site selection and monitor placement.
The reporting organization is responsible for ensuring
that all siting criteria have been met when originally
siting an STN monitor. Continued compliance with
siting criteria should be verified at least annually by the
reporting organization.
If the Laboratory is notified that a particular
STN monitor is in violation of siting criteria,
the corresponding AIRS data may have to be
flagged or invalidated. This decision should be
made jointly with the reporting organization
and EPA.
Integrity of sample handling. This involves verification
that the SOPs for sample handling have been followed
so that the physical integrity of the sample and its
positive identity are ensured. This requires that both
the field and laboratory operations follow the approved
SOPs and that any discrepancies are followed up and
resolved. System Audits should include a step-by-step
review of sample handling procedures. Data audits
should include examination of original custody sheets
and other records to look for discrepancies in sample
identification.
The reporting organization should develop and follow
SOPs for sample handling.
The field operation should conduct internal audits and
submit to external audits and reviews of its sample
handling and data processing systems.
The field operation should cooperate with
investigations of data integrity initiated by the STN
laboratory, U.S. Environmental Protection Agency
(EPA), or others.
The CAR process should be followed when
investigating isolated or systematic discrepancies.
Systematic problems should be addressed by revision
of the appropriate SOP.
The STN laboratory should develop and
follow SOPs for sample handling.
The laboratory should conduct internal audits
and submit to external audits and reviews of its
sample handling and data processing systems.
The STN laboratory should cooperate with
investigations of data integrity initiated by a
reporting organization, EPA, or others.
The CAR process should be followed when
investigating isolated or systematic
discrepancies. Systematic problems should be
addressed by revision of the appropriate SOP.
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TABLE 22-1. (continued)
Verification Activity
Reporting Organization
STN Laboratory
•hecks on sample containers and preservation methods.
Specific checks on sample containers include
examination for physical integrity and comparison with
the CAFDF sheet for correct identification. The chief
preservation method for exposed sample modules is the
use of a chilled ice substitute in insulated shipping
containers to reduce the temperature to 4°C.
The field operation is responsible for checking the
integrity of shipping containers and individual modules
upon receipt or deployment at the site. The laboratory
should be notified immediately of any damage that may
have occurred in shipment.
The field operator is responsible for chilling the ice
substitute and inserting a properly initialized min/max
thermometer prior to shipping the exposed sample
modules back to the STN laboratory. Use of the
thermometer is optional, depending on the study.
The CAR process should be followed if a systematic
problem is suspected.
The STN laboratory is responsible for
properly packaging the modules in shipping
containers that include the required number of
ice substitutes.
The STN laboratory is responsible for
notifying the carrier and initiating claims for
shipping damage.
The STN laboratory is responsible for
checking the condition of the shipping
container, its interior temperature, and
individual modules upon receipt from the field.
The STN laboratory must note any
discrepancies that might affect sample validity
in the DBMS. The reporting organization
should be notified if the problem might be due
to packaging procedures.
The CAR process should be followed if a
systematic problem is suspected.
Procedures to ensure that data were generated as
specified in the sampling or analysis SOP.
This is typically ensured using systems audits, EPA
Regional reviews, and results of performance audits.
Failure on any of these checks could imply that some
samples acquired prior to the check are suspect or
invalid.
The STN laboratory and the EPA STN Regional
Coordinator should be notified if serious procedural
issues are raised.
The CAR process should be followed to rectify
systematic procedural problems.
Integrity of laboratory analysis procedures is
typically ensured using internal and external
systems audits and results of performance
audits. Failure on any of these could imply
that some samples analyzed prior to the check
are suspect or invalid.
Reporting organizations) with affected
samples and the EPA Project Officer (PO) for
the STN laboratory contract should be notified
if serious procedural issues are raised.
The CAR process should be followed to
rectify systematic procedural problems.
o o
» p
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TABLE 22-1. (continued)
Verification Activity
Activities to determine how seriously a sample
deviated beyond the acceptable limit so that the
potential effect on the validity of data can be evaluated.
Reporting Organization
Systematic problems that lead to unacceptably large
biases should be investigated and documented using the
CAR process.
A person within the organization should be designated
to investigate serious discrepancies affecting sample
data. This designation should be formalized in the
organization's quality management plan (QMP) or in an
appropriate SOP.
The STN laboratory should be notified when a data
discrepancy is first suspected and again when the
discrepancy is quantified and the investigation is
closed.
Although it would be impossible to prepare SOPs for
assessing every contingency, the organizational
responsibility and general approach for investigating
discrepancies should be clearly documented.
STN Laboratory
Systematic problems that lead to unacceptably
large biases should be investigated and
documented using the CAR process. The
laboratory supervisor is usually in a position
to investigate such occurrences, but this
responsibility can also be delegated to a
qualified analyst or to the project QA staff
with the concurrence of the laboratory
supervisor and the Services Program Manager.
Data should be corrected, flagged, or
invalidated based on the best assessment of the
individual situation.
Corrections to previously sent data should be
transmitted to AIRS as soon as feasible. The
reporting organization should also be notified
when its data are flagged.
Data corrections and flagging should be noted
in regular OC rpnorts to manngpmpnt
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Section No. 22
RevisonNo.: 4
Date: 6/00
Page 5 of 13
A description of the organizational responsibilities and procedures for instituting corrective
actions for the STN program. This would be appropriately placed in the organization's STN
SOPs or in the QMP. If an adequate process already exists in the organization, it is not
necessary to document it separately for the STN.
A reporting form (i.e., the CAR form) describing the event or problem along with a suspected
cause; a recommended solution is optional. Other information should include the date and the
submitter's name.
A means for assigning responsibility for the corrective action investigation, as well as for
scheduling and appropriating resources to it.
All active and just-completed CAR investigations should be reported in the next annual QC
report to management or equivalent document. Dates and sites of reportable data affected by
the problem should a provided in detail. Delayed or canceled CAR investigations should be
identified and the reason for delaying or canceling the investigation justified.
The CAR files should be subject to regular audits and reviews.
22.3 Use of QC Information for Verification and Validation
The various QC samples used with the STN are also potential sources for verification/validation
information. Table 22-2 summarizes QC information and its uses in data verification and validation.
22.4 Use of Calibration Information for Verification and Validation
Calibrations can generate information that is useful in the verification and validation process. Because
this information is often not directly associated with a particular sample, procedures must be in place to
identify data that were dependent on a particular instrument when the calibration data indicate that the
instrument's performance was suspect. These considerations apply to most analytical chemistry
instruments; the balances used to weigh filters; and the field calibrations of flow, temperature, and
barometric pressure. Each SOP that involves the use of multipoint calibrations must include the
following considerations related to eventual use of that data for data verification and validation:
A mechanism for reporting calibrations that are out of specifications
A means for identifying all data that might be affected by the problem (all sample data back to
the last acceptable calibration should initially be considered suspect; investigation may be
required to estimate the maximum probable error and to decide on the validation status of
sample data)
A set of acceptance limits on the calibration that address zero/offset, bias/gain/slope, and
linearity/noise
A procedure for verifying out-of-limits calibrations
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Section No. 22
RevisonNo.: 4
Date: 6/00
Page 6 of 13
TABLE 22-2. QUALITY CONTROL DATA FOR STN DATA VERIFICATION AND
VALIDATION
Type of QC Data
Responsibility
Usage for Verification and Validation
Field Blanks
Joint lab and
field
High field blank values may indicate high levels of contamination at field sites. Data
should not be numerically corrected for field blank levels. Data should not generally be
invalidated or flagged unless the field blank levels approach environmental levels. The
STN laboratory must notify the reporting organization when a high field blank is found.
Trip blank
Joint lab and
field
High trip blanks (with or without a corresponding high field blank) may indicate a
laboratory problem. Corrective actions should begin in the laboratory. Reportable data
should not be corrected for trip blank values. Data should not be flagged or invalidated
unless the blank value approaches environmental levels.
Sampler leak check
failed
Field
Leak checks should be investigated as soon as they are detected. Any leak that could
potentially cause a data error (i.e., one that directly affects the flow through one or more
sampling modules) must be documented. If possible, the operator making the leak check
should estimate the extent of the leak. It is not generally possible to provide an exact
correction factor for data taken while a leak exists. The operator should also try to
determine when the leak began. Data back to the last successful leak check may be
suspect. Leaks that could potentially cause an error of 10% or more in actual flow rate
should be brought to the attention of the STN laboratory immediately so that data can be
flagged or invalidated appropriately.
Sampler temperature
or barometric
pressure sensor failed
Field
Sensor failures should be investigated as soon as they are detected. Sensor failures may
directly affect the flow through one or more sampling modules and therefore must be
documented. The operator discovering the problem should describe the error
quantitatively, if possible. The operator should also try to determine when the sensor
began to malfunction. Data back to the last successful check may be suspect. The
problem should be analyzed by someone with an understanding of how the sampler's flow
depends on the sensor reading; it may be necessary to contact the manufacturer to
determine this. If it appears that the failure could cause an error of 10% or more in
actual flow rate, the problem should be brought to the attention of the STN laboratory so
that data can be flagged or invalidated appropriately.
Filter integrity
inspections
Lab and field
Filters that fail the visual integrity inspection should not be used. If the filter has not
been used for sampling, its number can be voided in the laboratory's DBMS and no further
action is necessary.
Failure of visual inspection after sampling usually results in data invalidation or flagging.
The person making the inspection should document it on the CAFDF form. Data entry
personnel should make the appropriate entry when the form is input into the DBMS.
The original data or CAFDF form may have to be consulted during data validation to
determine the seriousness of the problem and the validity status of the reported data.
Repeated or systematic filter failures may be caused by many different factors including
rough handling, manufacturing defects, environmental factors during sampling, defective
packing materials, or contamination in the sampler before or after sampling. Systematic
problems should be investigated using the CAR process and documented in QC reports to
management.
Laboratory QC
samples
Laboratory
A large number of QC samples are run in the gravimetric and chemical laboratories. In
many cases, instrumentation problems can be corrected before any sample data are
affected. The specific acceptance criteria for laboratory QC samples are generally
determined by statistical methods (e.g., control charts) or by set limits defined in the
method.
Reserve aliquots or specimens of the original media should be retained until successful
post analysis QC results have been obtained. (Aliquots and specimens are also archived
for a period of time under the STN program, so reanalysis may be possible at a later time;
however, this is less accurate and more costly than immediate reanalysis.)
If QC results indicate an unacceptable uncertainty and the analysis cannot be reproduced,
the data must be invalidated or flagged.
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• Procedures for correcting data taken with out-of-limits calibrations. (This must be done
carefully.) Errors other than simple drift (e.g., noise and nonlinearity) should generally not be
corrected by recalculation; instead, the instrument should be repaired and the samples rerun if
possible.
Other considerations regarding calibrations that facilitate their use in the data verification/ validation
process include the following:
Calibrations should be performed within an acceptable time before and after analysis of field
samples; the acceptable time window is typically a function of the instrument's drift
characteristics.
Calibrations, other QC samples, and field samples should be done in proper sequence; the
positions of vials in an autosampler should be double-checked and all vials should be labeled if
possible.
Calibration points must bracket the concentration range of interest and should be spaced
according to the needs of the method (typically, either arithmetically or logarithmically
equidistant).
• Enough points should be included to assess noise and linearity (it may not be necessary to
assess noise and linearity on a daily basis, depending on the type of instrument).
22.5 Level 0 Verification and Validation
Basic review of data with respect to their provenance is referred to as "Level 0" verification and is
performed by the STN laboratory. The elements below summarize the criteria to be applied during
Level 0 verification of the data set:
Data source attribution—Verify that the site, date, time, and channel assignments are correct.
Logbooks, reporting forms, data custody sheets, and electronic data transmittals should be
consulted if a problem of attribution is suspected.
CAFDF verification—All CAFDF forms for filters and denuders will be checked for
completeness at the STN laboratory before they are entered into the database and archived.
Missing CAFDF information should be identified by the data entry operator and brought to the
attention of the SHAL supervisor. The laboratory QC supervisor should determine the validity
of any samples for which mandatory CAFDF information is missing. It may be necessary to
contact the reporting organization to attempt to fill in this information.
• Holding times and conditions—The shipping and receiving documentation for all PM2.5
chemical speciation samples (filters and denuders) should be checked to verify that holding
times have been met and that required storage conditions such as temperature met the
requirements. Data should be flagged in AIRS if holding times and shipping/storage conditions
were violated. The STN laboratory QA Manager, in consultation with EPA and the laboratory
supervisors), will decide the validity of any samples for which these conditions have been
violated.
Data transmission and recording integrity—Each error in data integrity that is identified must be
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PM2 5 STN QAPP
Section No. 22
RevisonNo.: 4
Date: 6/00
Page 8 of 13
investigated and corrected and/or appropriate actions taken. The QC supervisor should
determine whether an uncorrectable data transmission error affects data validity. The CAR
process should be used with problems of a systematic nature.
Calibration status of sampler and sensors—The reporting organization must have a means for
verifying that samplers were calibrated or checked within the required windows of time.
Samples taken when the instrument was past due on any calibration or recertification interval
must be appropriately flagged in AIRS. It is the responsibility of the reporting organization to
identify such data to the STN laboratory because sampling records received by the laboratory
may not include all the necessary information.
Audit status—The reporting organization must verify that all monthly, quarterly, and other
scheduled audits have been performed on time. Samples taken when a systems audit or
transfer standard recertification was past due must be appropriately flagged in AIRS. It is the
responsibility of the reporting organization to identify such data to the STN laboratory because
sampling records received by the laboratory may not include all the necessary information.
Operational flags—All operational flags generated by the sampler electronically or recorded on
a data sheet by the operator will be entered into the database. A translation between sampler
codes and AIRS validation flags will be developed as the STN program progresses. Some
serious sampler flags may also result in automatic invalidation of the corresponding sample.
22.6 Level 1 Data Validation
Validation (Level 1) is the process of evaluating the correctness and acceptability of individual items or
groups of items within the data set using statistical methods and other screening techniques. This
process involves evaluating the impact of verification problems, QA or QC problems, and statistically
detected anomalies on the usability of the data for their intended purpose.
Level 1 validation of field data will first involve the processing of verification results and data screens
into AIRS data flags and then providing an overall assessment of the validity of the data item or items.
Based on the number and types of data flags and other information generated during the verification and
validation process, some data may be designated as invalid. Invalid data are not reported to AIRS.
The following items are involved with validation of the PM2 5 chemical speciation field data:
Operational data screening—temperature, barometric pressure, flow, and other operational
data are screened for compliance with acceptance limits established for the STN program.
Filter inspections and other manual verification procedures performed by the site operator and
STN laboratory personnel.
Validation flags attached and reported—A limited number of flags are provided in AIRS to
document exceptional conditions that apply to specific data items. Only valid data are reported
to AIRS.
Invalid data are identified—Based on the number and types of data flags and other information
generated during the verification and validation process, some data may be designated as
invalid. Invalid data are not reported to AIRS.
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Section No. 22
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• Random data assessment and review—The STN laboratory QA Manager or designee will
manually review up to 5 percent of the data. This review may be done either before or after
transmission to AIRS (any corrections will be made retroactively). The check will include an end-
to-end check of data entry, calculations, and identification. Original CAFDF files will be examined
and compared to final data printouts. Flagged data will be checked to ensure that flags have been
correctly applied. Reporting organizations are encouraged to implement a similar program of data
checking.
Additional validation pertaining to laboratory analyses.
22.7 Data Screening Techniques used by RTI
The following procedures will be performed by RTI before the data is sent to the DOPOs.
Preliminary Crosstab Reports by site, POC, and scheduled dates
These are examined and anomalous results are investigated and corrected. The following crosstab
tables will be generated:
Chain of Custody form number for each event - include field and trip blanks, routine samples,
unscheduled blanks. Missing cells in the table are investigated.
• total counts of AIRS-deliverable records - each sampler type should generate a specific
number of counts; exceptions are investigated.
counts of invalid or suspicious analyte records
sampled date (i.e., the date actually sampled, as recorded on the COC form) - date scheduled
is compared against date sampled. Any event where these do not agree is investigated.
Examination of Chain of Custody Forms
COC forms are inspected for completeness by QA personnel. Flags assigned by the site operator or
by SHAL or data entry personnel are reviewed and corrections are made if necessary.
Statistical Outlier Checks and Range Checks.
Limits used for outlier checking are provided in Tables 1-4 below. The QAO reviews these results
and investigates problems. Outlier checks include the following:
Lower Limit on PM2.5 Mass - Routine samples only
• Mass Balance - Routine samples only
Anion/Cation ratios - Routine samples only
Sulfur/Sulfate ratios - Routine samples only
Upper Limit on PM2.5 Mass - Blank samples only
These steps are repeated until the data base is consistent and all exceptional conditions are explained.
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Section No. 22
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Page 10 of 13
Entry and Verification of Data Changes from the States and AIRS Data Verification
The following step is done approximately two months after validation of the preliminary data set.
Changes requested by the state agencies are entered into RTI's data base.
The AIRS text file is generated and is copied back into a QA table in the data base which is
used for reporting and automated comparisons.
Crosstab tables are made from the AIRS data table which are compared with previously
generated crosstab tables for that reporting batch. These are inspected as described in step 1
above.
After any anomalies are corrected the AIRS text file is regenerated. This is repeated until all
problems are corrected. See Tables 22-3 through 22-6.
Table 22-3. Statistical Validation Limits for Blanks
Percentile
5.0
5.0
Tail
UPPER
UPPER
Analyte(s)
PM25 Mass
PM25 Mass
Sample Type
FIELD BLANK
TRIP BLANK
Limit
•g
50.00
34.00
Flagged
Analytes
PM25 Mass
PM25 Mass
Internal
Flag
QL1
OL1
Table 22-4 Statistical Validation Limits for Routine Data
Percentile
2.0
2.0
2.0
2.0
2.0
2.0
•7 n
Tail
LOWER
LOWER
UPPER
LOWER
UPPER
LOWER
TTPPT7TJ
Analyte(s)
PM25 Mass Cone.
Anion/Cation Ratio
Anion/Cation Ratio
Mass Ratio
Mass Ratio
Sulfur/Sulfate Ratio
Siilfiir/Siilfato TJati^
Sample Type
ROUTINE
ROUTINE
ROUTINE
ROUTINE
ROUTINE
ROUTINE
TjnTTTTMT?
Limit
•g/m3
2.98
0.86
2.82
0.60
1.32
0.25
n A^
Flagged
Analytes
PM25 Mass Cone.
all ions
all ions
all analytes
all analytes
ions, XRF
i™ic YTJTT
Internal
Flag
QL1
QAC
QAC
QMP
QMP
OCR
npp
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Section No. 22
RevisonNo.: 4
Date: 6/00
Page 11 of 13
Table 22-5. Mapping of Outlier Flags onto AIRS Codes
Objective Cause Found for Level 1 Outlier
• Lab Error
• Filter Damage
• Module Assignment Error
• Sampler Malfunction
• Unusual Conditions noted by operator
• Unknown Cause
AIRS codes
If NOT Invalid
(Suspicious)
• [1]
• [1]
• [1]
(N/A)
• P]
T
If Invalid
AR
AJ
AQ or AR
AN
• [3]
AS
Notes:
[1] - No appropriate AIRS validity status code exists in current AIRS.
[2] - Use the applicable AIRS validity status code, or T.
[3] - Use the applicable AIRS null value code, or AM.
(N/A)-Not Applicable
Table 22-6. Automated Range Checks
Parameter
Exposure Duration, texp
Holding Time before removal from sampler,
pick-up
Average Flow Rate, F
Temperature Reasonableness (all
temperature channels)
Barometric Pressure (all)
Limits
23
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PM2 5 STN QAPP
Section No. 22
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Date: 6/00
Page 12 of 13
Invalidate Data in AIRS—Data of uncertain provenance and data with unacceptable levels of
uncertainty should not be included in AIRS. These data will be reported as missing.
CAR Process—The CAR process should be followed in cases of systematic problems or problems
affecting a significant number of data points. The CAR process is described in Section 22.2.
Revision of SOP s and Other Project Documentation—One of the most significant of the possible
outcomes of the CAR process is the identification of the need for revising SOPs and other project
documentation. Procedural changes to overcome identified problems are a key element in the
continuous improvement of the STN program.
Consultation to Determine Impact of Deviation—The cognizant QA supervisor in an organization is
typically charged with the responsibility of determining the impact of a deviation from requirements.
This process should involve consideration of the primary DQO of trend detection described in Section
7.0.
Notification of EPA or Other Stakeholders—The investigation of a serious or systematic problem
should consult operators, analysts, and other personnel involved with the situation being investigated, as
well as stakeholders who might be impacted by the decision to validate or invalidate data. Field
organizations should contact the STN laboratory (through channels approved by the DOPO) to
provide documentation of corrective actions that might affect the data validation status of reportable
data. The State reporting organizations should include significant QA problems in their annual QA
reports to management.
22.9 Verification and Validation Criteria: Field Component
Table 22-3 summarizes the verification and validation criteria applicable to the field program. The
verification and validation (Level 0 and Level 1) criteria are combined into a single table because the
criteria overlap.
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TABLE 22-7. DATA VERIFICATION AND VALIDATION SUMMARY
Item
Sampler and site identification
Date and time identification
Filter or denuder channel assignment
CAFDF records for filters and
denuders
Holding times and shipping and
storage conditions:
• unexposed samples, holding time,
and storage temperature
• exposed samples, residence time in
sampler before retrieval
• exposed samples, on-site holding
time plus shipping time, and
shipping temperature
• holding time and storage
temperature after receipt in the
laboratory prior to analysis
Electronic data transmission
Sensors checked or calibrated within
required time frame
Transfer standards recertified within
required time frame
Sampler-generated flags (electronic
data):
• filter/ambient temperature
difference
• flow rate out of specification
• total sampling time out of
specification
• sampling start or stop time out of
specification
Operator flags and other information
from field data forms:
• filter inspections
• other conditions noted by operator
that could impact the sample
Statistical screening of operational
data:
• temperature
• barometric pressure
. flow
• other operational data
Criteria
Must be
correct
Must be
correct
Must be
correct
Must be
present
See criteria
tables in
Section 20.0.
No errors
reported
All
temperature,
barometric
pressure, and
flow rate
sensors
All transfer
standards
routinely used
by site
operator
See criteria
table
See field data
form
See criteria
tables
Applicable
to
Data forms
Data forms
Data forms
CAFDF
forms,
sample labels
All filter
Electronicall
y transmitted
data
Routine
calibration
records
Audit and
recertificatio
n records
Electronic
data
Field data
forms
Data
summaries
Comment
Investigate and correct, if
possible; invalidate data if
identification cannot be
established
Review and determine impact on
data validity
Review and determine impact on
data validity
Review and determine impact of
the error on data validity
Dates of required sensor checks
should be verified before data are
reported
Dates of recertifications should
be verified before data are
reported
Data should be reviewed and
evaluated to determine validity
for reporting to AIRS
Operator's notes should be
evaluated regarding probable
impacts on data validity
Development of statistical data
screens will be coordinated with
the laboratory
Flag in
AIRS if
Violated
(see notes)
Invalidate
if
Violated
(see notes)
!
!
Notes:
" Flagging or invalidation is optional. Reporting organization should review the circumstances and the potential impact on the data.
When bom columns are marked with mis symbol, there are three choices: (1) report to AIRS without a flag if the data need not be
qualified to the data user, (2) flag the data and report to AIRS if the user might need to know that the data are qualified but may be
usable for certain purposes, and (3) invalidate the data (invalid data are not reported to AIRS).
! Flagging or invalidation is mandatory. When this symbol is shown in the "Flagging" column and the "Invalidation" column is blank,
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23.0 • Validation and Verification Methods
The processes for verifying and validating the measurement phases of the chemical Speciation Trends
Network data collection operation have been discussed in the previous section. If these processes are
followed, the quality of data should be achieved to meet the DQOs for trend detection. This section
describes the organizational implementation of the validation procedures, the applicability of corrective
actions, and the reporting requirements and schedules.
The process of data validation and verification is a cooperative effort between the reporting
organization responsible for field sampling and the STN laboratory, which conduct the chemical
analyses and reports the validated concentration values to AIRS. This section focuses on the
verification and validation methods applied by the reporting organizations after the first stages of
validation have been completed by the STN laboratory.
23.1 Interorganizational Responsibilities for Data Validation
The sequence of data verification and validation steps and the corresponding organizational
responsibilities are as follows:
1. The STN laboratory issues unexposed sample module kits to the reporting agencies along
with a partially completed custody and field data form CAFDF.
2. The reporting agency exposes the filters, fills in the necessary data about the exposure on
the CAFDF form, and returns them to the STN laboratory.
3. The STN laboratory enters the data recorded on the CAFDF, performs the data analyses,
and enters the results into the data system.
4. The STN laboratory performs level 0 and level 1 data validation based on the data to which
it has access. This includes validation of laboratory results and entry of any validation flags
associated with problems noted on the CAFDF received from the field.
5. After all validation is completed for a data set, the STN laboratory transmits the data and
associated validation flags in hardcopy and electronic form to the DOPO, who in turn
distributes the data to the respective ROs.
6. The RO completes the verification and validation process at levels 2 and 3 based on
information compiled from previous PM2 5 research programs, guidance from CAS AC and
Expert Panel on PM2 5 Speciation, its own internal records, audit results, and other
information available from site operators and other local sources.
7. The ROs forwards the validated data back to the STN laboratory for submission to AIRS.
8. Further statistical validation may be performed by EPA and others as needed.
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23.2 Personnel Responsibilities within the Reporting Organization
The RO should assign data validation responsibilities according to its organizational structure and the
needs of this program.
Within the RO, the following roles and responsibilities for STN data validation may be defined.
Program Manager—The RO's manager for the PM2 5 chemical STN is ultimately responsible for
meeting schedules, for ensuring that qualified staff perform data management and validation functions,
and for delivering valid data to AIRS. The RO's STN Manager should ensure that data validation and
data management responsibilities have been assigned to individuals with the appropriate educational
background, training, and knowledge of the STN program.
Data Validation Specialist—The Data Validation Specialist is the person who conducts the actual
examination of data received from the STN laboratory via the DOPO. This person should be
knowledgeable about quality assurance principles, particulate measurement methods, and basic
statistics and chemistry and should be familiar with network operations including sampler operation and
shipping and receiving of sample modules. Often, the QA supervisor responsible for the STN program
will be assigned to validate the data. The Data Validation Specialist should be supported by data
management personnel, chemists, environmental scientists, and statisticians to deal with questions that
arise during the validation process. It is critically important that field personnel, particularly the operator
responsible for STN sampling and his/her supervisor, be available to answer questions. The Data
Validation Specialist should also have ready access to project files and relevant data sets.
The following sections describe the verification and validation procedures that should be applied by
ROs to the partially validated data received from the STN laboratory.
23.3 Completion of Level 0 Data Verification and Validation
The first step in the RO's data verification and validation process should be to confirm that the data are
correctly accounted for according to the RO's own records. The STN laboratory will have checked
the data according to its shipping and receiving records and the CAFDFs and will have flagged any
discrepancies in data attribution. The Data Validation Specialist should examine each discrepancy that
the STN laboratory has flagged as suspicious due to uncertain attribution or problems with chain of
custody. The RO should examine its copy of the CAFDF, shipping and receiving records, operator
logbooks, and any other relevant records to address the problem. (The STN laboratory may have
already contacted the RO, via the DOPO, regarding problems of data attribution, so a repeated check
of a previously investigated problem may not be necessary.) The RO can deal with this type of flagged
data in a number of different ways, as follows:
If the level 0 flag can be explained and the data are correct, the flag may be removed or
changed to a more appropriate flag.
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If the STN laboratory has flagged data as misassigned (i.e., assigned to the wrong sampling
date, site, analyzer, or channel), the RO may edit the data so that monitoring data are
correctly assigned. This may only be done if verifiable information can be found in the RO's
operating records that allows the correct data assignments to be made.
If concentration values that have been flagged can be corrected numerically (e.g., by
correcting an incorrect sample volume recorded on the CAFDF sheet), the RO can make
this correction directly, but it is recommended that this information be passed back to the
STN laboratory, via the DOPO, so that the calculation can be verified.
If the RO cannot find an explanation for a flagged discrepancy, the data flag should be
allowed to stand.
23.4 Identification of Outliers and Data Flagging Techniques
23.4.1 Manual Methods
To fully complete the validation process, the RO must examine the data set, both flagged and unflagged
data, for validation criteria based on information sources available within the organization. The
validation tables in Section 22.0 of this document should be consulted for specific validation criteria.
Some validation criteria that are not easily automated are listed below:
Manual Data Inspection—The purpose of manual data inspection is to spot unusually high
(or low) values that might indicate a gross error in the data collection system. It is often
helpful to plot data in a time series.
Systems Audit Report Results—Audits occasionally turn up serious deficiencies that could
affect the validity of the data. For example, if it is found that a field operator is mounting
sample modules incorrectly, it would be necessary to flag or invalidate all the data
corresponding to that sample module when that operator was working.
Performance Audit Results—Large audit bias found in critical measurements such as
sample volume accuracy could result in data invalidation or flagging back to the last
previous acceptable audit or control check result.
Collocated Sample Results—Performance on collocated duplicates should be evaluated if
information is available. Poor performance audit results should be investigated further, and
if a specific, identifiable problem is uncovered that affects reportable data, that data should
be flagged or invalidated. In general, reportable data should not be invalidated unless a
specific, identifiable cause for the discrepancy can be found.
Operator's Notes and Site-Specific Information—Operator's notes can contain
information that would call for data invalidation due to lack of sampling representativeness.
Examples include meteorological events such as sand storms, temporary violations of siting
criteria such as nearby construction, or operational difficulties with the sampling equipment.
The RO should use its best judgment about the impact of site conditions on the acceptability
of the data and may consult with EPA via the DOPO or the Regional Office if there are
questions.
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Shipping Records—Shipping records can be compared with CAFDF records to identify
exposed sample sets that were held too long before shipping. Unexposed sampling media
should not be used if more than 30 d have elapsed since the initial weighing of the Teflon™
filters. Sample module sets should be used at a designated site in the order they were
received from the STN laboratory.
Corrective Action Requests that Affect Data Quality—The Data Validation Specialist
should review any CARs in effect when the samples were acquired. Any CARs that could
affect the data should be evaluated and appropriate actions taken with regard to flagging or
invalidating the data.
23.4.2 Automated Methods
Because the data will be delivered from the STN laboratory to the ROs in electronic format, automated
checking could be implemented. Some automated screening methods that might be considered include
the following:
Inter parameter Checks—These include ion ratio and mass balance checks that use data
from a number of different channels. Samples with atypical results could be examined more
closely as part of the validation process.
Time Series Analysis—This analysis is typically the examination of a set of data for a single
observable (e.g., a particular chemical species at a certain site) acquired over a period of
time. Time series data are often best examined graphically, and it is often helpful to chart
related variables together on the same graph.
Outlier Checks—Statistical outlier checks for screening PM2 5 chemical speciation
concentration measurements (the actual environmental measurements, rather than QA
quality control data) are another means of identifying potential problems. An
environmental observation should never be invalidated simply because it is
identified as a possible outlier by statistical techniques. Observed environmental
concentration distributions tend to be somewhat skewed, so that a small number of
concentrations significantly higher than the long-term average should be expected.
Selecting the top 1 or 2 percent of values in a data set for investigation, however is often a
good rule of thumb for data assessment because high data values are sometimes the result
of analytical, procedural, or calculation errors.
Specific information about the automated screening methods will be coordinated by EPA and
distributed to STN field and laboratory personnel.
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24.0 Reconciliation with Data Quality Objectives
Results obtained must be reconciled with the requirements defined by the data user or decision-maker,
as specified by the DQOs for the project (U.S. EPA, 1994). The methods used to analyze the data are
based on the statistical model described fully in Data Quality Objectives for the Trends Component
of the PM2.5 Speciation Network (U.S. EPA, 1999a) and outlined in Section 7.0 of this QAPP. It is
expected that actual data acquired under the Speciation Trends Network will depart in various ways
from the original conditions and assumptions of the DQO study. This section discusses these issues
along with how they will be resolved and how limitations on the use of the data will be reported to
decision-makers.
24.1 DQO for Chemical Speciation Trends
The primary DQO for the chemical Speciation network is defined as the ability to detect a ±5 percent
annual trend within 5 yr with statistical power of 0.80. A research study (U.S. EPA, 1999a)
summarized in Section 7.0 of this QAPP indicated that this would be a feasible DQO for the chemical
STN, based on a review of similar species concentration data obtained from samples collected in the
past at an urban site in the IMPROVE network.
To assess whether this DQO has been met, it is necessary to determine if a significant time trend can be
detected (or rejected, when there is no trend) with the requisite statistical power after 5 yr of data have
been collected.
Note that by satisfying the DQO it is not necessary to show that a trend definitely exists or does not
exist; a legitimate finding is that a trend cannot be either diagnosed or rejected with the required
certainty. In fact, this is a likely outcome when a trend of intermediate size (e.g., +2 to 3 percent per
yr) exists or when a trend is present but highly variable over time. On the other hand, if all sources of
error and uncertainty are particularly well-controlled, it may be possible to diagnose a trend smaller
than ±5 percent or to identify a trend in less than 5 yr.
To satisfy the primary DQO, it is only necessary to demonstrate that the 5-yr data set is capable of
detecting a 5 percent trend (or failing to find a trend when none exists) with the requisite level of
confidence. This is done on a species-by-species basis. It is hoped that the DQO for diagnosing
trends will be met for PM2 5 mass as well as for the chemical species used in the DQO feasibility study
(U.S. EPA, 1999a). All the species used in the study, however, were present at a relatively high level;
it is not likely that the trend detection DQO will be met for all chemical species. Reasons for failing to
meet the trend detection DQO for a particular species include the following:
• Low concentration (typical of certain uncommon elements reported by energy-dispersive
X-ray fluorescence [EDXRF])
Large background variability near the analytical method's detection limit
Large proportion of nondetects, thus weakening the statistical power of the analysis
High variability in concentration of the species in the environment
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Seasonal variability
The presence of local sources (ocean, nearby construction, industrial or residential
sources).
24.2 Interim Evaluations of Data Quality
The STN and its constituent monitoring agencies should perform interim evaluations of data quality
annually to assess whether the goal of meeting the DQO for trend detection can be met within 5 yr.
There are two primary ways of performing interim evaluations of data quality: comparison of the
project's quality control (QC) statistics against measurement quality objectives (MQOs) and direct
modeling using the method used by EPA in the DQO study. The following sections describe these two
approaches and suggest corrective actions that can be taken if interim analysis indicates that the DQO
may not be met after 5 yr.
24.2.1 Evaluations Based on MQOs
Estimating the measurement error being achieved based on available QC data is perhaps the quickest
interim measure of assessing progress toward meeting the DQO for trend detection. Objectives for
total measurement error based on the DQO study are provided in Section 7.0 of this document. This
quick but inexact method of data quality assessment (DQA) is appropriate after 1 yr of sampling;
however, more exhaustive analysis should be done after 2 or 3 yr of data have been collected, as
described in the next section.
The STN program has various measures of bias and precision available as a result of the QC data
being taken. Measurement error must be assessed as the total end-to-end error. Some QC samples
assess only part of the total system and thus underestimate the total error. Some of the QC samples
that are useful in assessing total measurement error are as follows:
Flow Rate Checks—These checks are carried out at various intervals using different independent flow
standards. Total volume is directly proportional to flow rate, and calculated concentration is inversely
related to flow rate. Thus, a 5 percent bias error in flow rate will result in a -5 percent error in
calculated concentration (approximately, not accounting for the effect of such an error on the particle
size range distribution). Likewise, a 5 percent coefficient of variation (CV) in flow rate (random error)
will result in a 5 percent CV in the concentration (approximately). Flow rate is a significant contributor
to overall error, but it is an incomplete estimate of total measurement error because it does not include
several sampling representativeness and analytical errors.
Analytical QC Samples Including Analysis of Standards. Duplicates, and Matrix Spikes—These
samples provide information about the analytical component of bias and reproducibility. Theoretical
estimates of uncertainty are also available for the EDXRF data (elemental analysis). These estimates do
not completely characterize the total measurement system because they omit field errors, including flow
rate and sampling representativeness.
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Field Blank Results—Field blanks provide information on contamination due to handling operations.
Normally, field blank levels should be kept quite small by early corrective actions and should never be
allowed to become a significant component of total measurement error.
Collocated Sampling Results—These results are potentially the most complete of the measurements of
end-to-end error. When starting up a new chemical speciation sampler at a site, it is a good idea to
collect a number of duplicates with the collocated sampler. Approximately 10 valid duplicate samples
should be considered the minimum for estimating the total error. Continued collocations should be
done on a regular schedule so that data can be developed over all seasons of the year. Although the
collocated sampling results provide a relatively complete picture of end-to-end measurement error, two
components of measurement are not included.
The first is related to the fact that collocated samples are generally analyzed in the same laboratory on
the same day. The collocated sampling error will underestimate the true total measurement error by an
amount related to the laboratory's day-to-day variability. This error can be controlled, or at least
estimated, by tracking the results of daily analyses of laboratory standards. The variability in repeat
analyses of laboratory standards should be kept small with respect to the targeted MQO. The STN
laboratory will provide EPA with regular QA summary reports that will include the necessary
information for assessing this and other components of analytical error.
The second error that collocated sampling omits is due to field sampling representativeness caused
when the paired samplers are not equivalently sited. This factor can be controlled by careful
observance of the siting requirements as well as by using common sense in making the two sampler
locations as equivalent as possible. Problems with siting might also be detected by assessing the
duplicate precision for total mass. Consistent relative differences in total mass of more than about
10 percent may indicate that a siting problem exists. Low-level chemical species are likely to show
larger relative variability than mass measurements—this is to be expected and may not indicate a
problem.
The recommended interim method for estimating total measurement error is to calculate the total error
based on 10 or more collocated measurements for each chemical species and mass. The following
method of calculation is adapted from the method given in 40 Code of Federal Regulations (CFR)
Part 58, Appendix A, Section 5.5.2.1:
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"
1. Calculate the duplicate difference for each observation, as follows:
where
dj = percent difference for observation /'
Yj = primary (station) sampler concentration value
Xj = duplicate (reference) sampler concentration value.
Note : Omit data for which the average concentration in the denominator is less than 3 times the
method detection limit (MDL). This may result in inadequate data for evaluating some trace species.
2. Calculate the CV for a single check. The following equation for calculating the CV is
provided in 40 CFR Part 58, Appendix A, Section 5.5.2.2:
^ - = (24-2)
V2
where
CVt = CV for observation /'
4 = duplicate percentage difference for observation /'.
3 . Calculate the single sampler precision. The following equation is adapted from 40 CFR
Part 58, Appendix A, Section 5.5.2.3, which calculates precision for collocated samplers
of identical type. CVj represents an average error value over all observations within a given
time period for a particular chemical species (or total mass) designated by the subscripty :
(24-3)
where
CVj = pooled CV for speciesy over the specified time period
CVtj = CV for speciesy, observation /'
rij = number of paired observations made for speciesy over the time period.
4. Compare the CVj results against the MQO. If the CV does not meet established criteria
for a species of interest, corrective actions such as those discussed in Section 24.2.3 should
be considered.
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24.2.2 Evaluations Based on Direct Assessment of the Monitoring Data
Using the statistical model described in the DQO (U.S. EPA, 1999a), an assessment of progress
toward meeting the DQO can be made with less than 5 years' worth of data but with reduced statistical
power. The statistical power of the tests should be extrapolated to 5 yr, based on the error levels
computed for the preliminary data. If this extrapolation indicates that the DQO for detecting a trend
will not be satisfied for a critical species of interest, corrective actions should be taken as described in
the next section. It is important to do a careful assessment of the actual monitoring data as early in the
program as possible, typically after the second or third full year of sampling, because the assumptions
used in the DQO study may not hold at any particular STN site.
24.2 3 Interim Corrective Actions
If an interim assessment indicates that the DQO for trend detection is not being met, modification to the
experimental design should be considered after any obvious measurement quality problems have been
resolved to. Experimental design factors include site selection, frequency of sampling, frequency and
precision of QC measurements, and frequency of equipment maintenance. The experimental design
changes most likely to improve data quality are listed below in decreasing order of effectiveness:
Increase the Frequency of Sampling—The DQO study (U.S. EPA, 1999a) showed that
l-in-3 d sampling was adequate to meet the DQO based on the IMPROVE data set, while
daily sampling was unnecessary and l-in-6 d sampling was not adequate to meet the
DQO. Increasing the sampling frequency may be helpful when measurement error and
unexplained variability are larger than expected. Increasing the frequency of sampling is
unlikely to affect variability attributable to seasonality.
Add Additional Samplers—Locating one or more additional samplers in the same impact
area may help decrease the statistical uncertainty in the same way that increased sampling
frequency does. In addition, locating samplers at some distance from one another may be
effective in reducing unexplained variability due to local sources and siting variables.
Remedy Siting Problems—Factors such as proximity of local sources or shielding by
nearby buildings and other objects should be eliminated as potential sources of excessive
variability.
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Improve QC and Maintenance—Measurement errors can, in principle, be reduced by
increasing the frequency of QC checks, audits, and maintenance. Increasing the intensity of
the QC program, however, may not be the most effective approach for reducing total
uncertainty for two reasons: the relative contribution of measurement error to the total
uncertainty is small, and a point of diminishing returns may be reached after which little
improvement in measurement quality can be achieved. Purchasing more precise or accurate
standards is unlikely to make a meaningful difference in overall data uncertainty. On the
other hand, increasing the frequency of QC and maintenance can sometimes be effective at
sites where a excessive numbers of operational problems and malfunctions are being seen
and will certainly be effective in the latter years of network operation as the equipment ages
and major maintenance is required.
24.3 Assessing and Reporting Chemical Speciation Trends
At the end of the first 5 yr of monitoring, each reporting agency will assess whether or not the DQO for
trend detection has been met and will apply suitable statistical tests to test for a trend in the
concentration data for all chemical species of interest. Detailed description of the trend assessment
method is outside the scope of this QAPP. Network and reporting agency personnel should use
methods similar to those in the DQO document (U.S. EPA 1999a) as a point of departure for their
analysis of concentration trends, but they are encouraged to use the most appropriate statistical model
for their individual situations. Specific assistance can be obtained from OAQPS in Research Triangle
Park, NC.
The interim DQO analyses should address the following questions for each analyte:
Was an annual trend of ±5 percent or greater indicated by the analysis?
Was an annual trend of as much as ±5 percent excluded by the analysis?
• Was the statistical test inconclusive about the existence of a trend?
If the test was inconclusive, was the data of sufficient quality to make the assessment with
the requisite power if a trend had been present?
24.4 Reconciling Other Chemical STN Research Objectives
There are several important research objectives for the STN data other than trend identification (U.S.
EPA, 1999b). These include model development and validation, source attribution, State
implementation plan (SIP) attainment and strategy development, and emissions inventory. The ultimate
users of the data include environmental researchers, regulators, and State and Federal policymakers.
The DQO for trend detection focuses on changes in concentrations of individual species over time.
Other data uses, however, may rely on different characteristics, such as concentration ratios between
species, seasonal variations in concentrations or concentration ratios, or the absolute concentration of
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certain chemical species at a particular point in time. Meeting the DQO for trend detection does not
guarantee suitability of the data for another purpose. To be useful for objectives other than trend
detection, the primary data set must be accompanied by a complete set of supporting data so that the
user can derive information that might be applicable to other research objectives.
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24.5 References
U.S. EPA (Environmental Protection Agency). 1994. Guidance for the Data Quality Objectives
Process: EPA QA/G-4, Report No. EPA/600/R-96/055, U.S. EPA, Washington, DC.
U.S. EPA (Environmental Protection Agency). 1998. Guidance for Data Quality Assessment -
Practical Methods for Data Analysis, EPA/600/R-96/084, U.S. Environmental Protection Agency,
Office of Research and Development, Washington, DC. January 1999.
U.S. EPA (Environmental Protection Agency). 1999a. Data Quality Objectives for the Trends
Component of the PM2 5 Speciation Network, U.S. EPA, Research Triangle Park, NC, 1999.
(Available online on the Ambient Monitoring Technical Information Center [AMTIC] at
http ://www.epa.gov/ttn/amtic/files/ambient/pm25/spec/dqo3 .pdf)
U.S. EPA (Environmental Protection Agency). 1999b. Paniculate Matter (PM2 $) Speciation
Guidance Document (ThirdDraft), U.S. EPA, Research Triangle Park, NC. January 5, 1999.
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APPENDIX A-l
SOP 5000STN
CONDENSED OPERATING PROCEDURE
FOR FIELD INSTALLATION
OF PM2 5 SPECIATION SAMPLERS
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SOP # 5000STN PM2 5 Sampler Installation
Rev. # 1
Date: September 30, 1999
Page 1 of 5
CONDENSED STANDARD OPERATING
PROCEDURE (SOP) FOR FIELD INSTALLATION
OF PM2 5 SPECIATION SAMPLERS
Prepared by: Date:
Prepared by: Date:
Prepared by: Date:
Reviewed by: Date:
Approved by: Date:
PM2 5 Speciation Trends Network
Office of Air Quality Planning and Standards
U.S. Environmental Protection Agency
Research Triangle Park, NC 27709
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SOP # 5000STN PM2 5 Sampler Installation
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Page 2 of 5
1.0 Purpose and Applicability
This document outlines the procedure for field installation and setup of several
commercially available PM2 5 speciation samplers. For more detailed information
regarding field installation of these samplers, refer to the specific sampler's operator's
manual.
2.0 Safety Precautions
2.1 To avoid electrical hazards, all sampler installation procedures should be conducted with
the sampler disconnected from the AC power source.
2.2 Observe proper lifting procedures when unpacking and moving sampler components.
2.3 Read, understand, and follow all safety precautions for each sampler outlined in the
sampler's operator's manual.
2.4 Once sampler installation is complete, secure the sampler to the field sampling platform to
ensure that it does not tip over during high wind speed events.
2.5 Care must be taken when operating or calibrating the units in inclement weather. Safety is
paramount.
3 .0 Siting
3.1 Ensure the sampler is level.
3.2 Ensure the sampler inlet is separated by at least 1 m, but no more than 4 m, from other
PM2 5 samplers and that the sampler has an unobstructed air flow of a minimum of 2 m in
all directions. For collocated sampler studies, position the sampler's inlets exactly 1 meter
apart.
4.0 Sampler Setup Procedures
4.1 Andersen (RAAS) - Sampler Installation
4.1.1 Basic Assembly Steps
1. Locate the pump/base stand and attach the four stabilizing "L" shaped bracket feet.
2. Locate the base stand so one of the widest sides will represent the front or back.
Carefully lift the main housing squarely onto the base stand.
3. Open the housing door. Locate the four holes inside on the bottom panel to align, insert
and tighten the four Vi-20 screws and washers provided.
4. Remove one front or backside panel to the pump base by loosening the four captive
screws.
5. Pump base vacuum and power lines can be extended up through the round hole in the
housing base.
6. Attach tubing to the available compression thread fitting nearest the large ball valve
connected to the flow manifold assembly on the floor of the housing base.
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SOP # 5000STN PM2 5 Sampler Installation
Rev. # 1
Date: September 30, 1999
Page 3 of 5
7. Insert the pump power cord into the outlet labeled "pump."
8. Locate the sample flow splitter assembly. Install the downtube and sample inlet
components. Refer to the operator's manual for this multi-step process.
9. Next, install the two large sample manifolds. Note: The left and right devices are mirror
images and are interchangeable. Install the left side manifold first. The manifolds slide into
grooves provided on the inside roof of the sampler case.
10. Locate and install the two cyclone assemblies.
11. Select one of the two possible locations for the ambient temperature radiation shield.
Secure the unit upright so the support arm extends upward at 45 degrees and the shield's
protective fins angle downward.
12. Run the ambient thermocouple through the middle hole and plug it into the ambient
temperature receptacle on the inside back panel.
13. Set up the flow manifold and its flow sensors and critical orifices. Ensure the vacuum
pump pressure sensor tubing (small) is connected on the right side of the flow manifold and
to the labeled panel position "pressure pump." Refer to the operator's manual.
14. Install the sampling train assemblies. Refer to the operator's manual for details.
15. General system setup is complete.
4.2 Met One (SASS^ - Sampler Installation
4.2.1 Tripod and Mast Installation
1. Spread the three legs of the tripod by applying tension to the support brackets. Make the
tripod steady.
2. Note the "UP" mark on the mast. Slide the mast into the top of the tripod collar allowing
the lower-most stop to pass the collared key-way. The paired stops in the mast limit the
mast from striking the ground.
3. Position the lower support brackets and tighten all hardware using a crescent wrench.
4. Securely anchor the tripod feet to the sampling platform using wood screws.
4.2.2 Sampling Head and Solar Shield Installation
Note: This installation may require two workers.
1. Remove the pin from the lower shield and slide down the mast. Allow the solar radiation
shield to rest on the paired stops.
2. Install two 8-32 x 3/16" cap-screw stops into tapped holes at the top of the mast and
tighten them.
3. While supporting the upper sample head/shield assembly, feed the tube and cable harness
into the top of the mast. Lift the sample head/shield and place the hub onto the top of the
mast.
4. Rotate the sample head and the shield until the hub engages the notch and the cap screw
stops.
5. Tighten the two alien key screws in the hub and the two thumbnuts.
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SOP # 5000STN PM2 5 Sampler Installation
Rev. # 1
Date: September 30, 1999
Page 4 of 5
6 Raise the lower radiation shield and engage the slot for positioning. Insert the pin into the
shield and mast.
7 Lift the entire mast assembly, allowing the lowermost stops to pass through the top collar
key-way. Rotate the mast, allowing stops to align and drop into the top collar groove.
8 Secure the mast to the tripod by tightening the bolts in the upper and lower collars.
4.2.3 Control Box Installation
1. Install the control box onto the mast using the two U-bolts. Position the bottom of the
control box on the top of the upper collar on the mast.
2. Connect the sampling head fan and filter temperature cable to the third connector from the
right on the bottom of the control box.
3. Connect the ground cable on the control box stud to an electrical earth-ground connector.
4.2.4 Ambient Temperature Sensor Installation
1. Install the ambient temperature sensor onto the mast using two U-bolts.
2. Position the sensor onto the mast immediately above the top of the control box. Sensor
position should be at a 180 degree angle from the control box door.
3. Connect the ambient temperature sensor cable to the second connector from the right on
the bottom of the control box.
4.2.5 Pump Box Installation
1. Place the pump box on the sampling platform between the legs of the tripod.
2. Connect the five numbered sample flow lines, exiting the bottom of the mast, to the
numbered quick disconnects located on the side of the pump box.
3. Connect the 14-pin communication cable, exiting the bottom of mast, to the first connector
from the right on the bottom of the control box. Note: The quick disconnects have
internal shut-off valves if a sample channel is not used.
4. Connect the AC power cable to the 115 VAC/60 Hz source to provide power to the
SASS.
4.3 URG (MASS 400 and MASS 450V-Sampler Installation
1. Position the MASS sampler's case so that it is resting on the top cover.
2. Align the stand on the bottom of the unit and attach it using the provided V4-20 nuts and
washers.
3. Turn the sampler's case to the upright position.
4. Remove the top and the back panel of the sampler.
5. Run the ambient temperature thermocouple through the middle hole on the top cover.
6. Reinstall the top cover and the back panel.
7. Install the ambient temperature radiation shield and insert the ambient air thermocouple
sensor assembly.
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SOP # 5000STN PM2 5 Sampler Installation
Rev. # 1
Date: September 30, 1999
Page 5 of 5
8. Install the sampler inlet tube (downtube/denuder) and WINS impactor. As this is done,
verify that all O-rings are in place, fit snugly, and none are frayed, split or broken.
9. The MASS 400 and MASS 450 sampler units must be placed on the platform according
to the inlet height (within 1 m) and inlet horizontal separation (greater than 1, but less than
4 m) specifications that apply to collocated samplers.
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APPENDIX A-2
SOP 5100STN
CONDENSED STANDARD OPERATING
PROCEDURE FOR THE MET ONE SASS
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SOP # 5100STN Met One SASS
Rev. # 1
Date: September 30, 1999
Page 1 of 10
CONDENSED STANDARD OPERATING
PROCEDURE (SOP) FOR THE MET ONE SASS
Prepared by: Date:
Prepared by: Date:
Reviewed by: Date:
Approved by: Date:
PM2 5 Speciation Trends Network
Office of Air Quality Planning and Standards
U.S. Environmental Protection Agency
Research Triangle Park, NC 27709
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SOP # 5100STN Met One SASS
Rev. # 1
Date: September 30, 1999
Page 2 of 10
1.0 Purpose and Applicability
This condensed standard operating procedure (SOP) outlines procedures for field
operations and quality control checks of the Met One SASS PM2 5 speciation sampler. For
more detailed information regarding operation of this sampler, refer to the Met One SASS
operator's manual.
2.0 Precautions
2.1 Read and thoroughly understand the operator's manual before beginning field operations.
The flow rate and temperature calibrations of the sampler must be checked and, if
necessary, adjusted to specifications prior to taking the first sample. Consult the operator's
manual for calibration instructions.
2.2 Use only the sampling cassettes, sent to you from the laboratory, for the designated
sampler and location.
2.3 Exercise great care in placement and handling of sampling cassettes to avoid
contamination.
2.4 The sharp cut cyclone must be attached to the inlet of the sampling cassette before
sampling.
3.0 Equipment and Supplies
3.1 Have the STN Custody and Field Data Form for the particular sampler, for the particular
sampling day, with you when visiting the site. Have an STN QA/QC Report Form if a
quality control check is due.
3.2 Sampler operator's manual and field notebook.
3.3 Met One SASS speciation sampler, accessories, and any tools needed.
3.4 SASS cassettes, pre-loaded with filters and denuders for up to five channels. Field blank
cassette(s) for use on every 10th sampling day. All these items will be supplied from the
support laboratory.
3.5 Sharp cut cyclone for each sampling cassette. Label the cyclone to correspond to a single
sample channel position and dedicate the cyclone to use with this channel.
3.6 Shipping coolers, frozen ice substitutes, and Federal Express labels for shipment of
sampling modules and reports to analytical support laboratory. These will be supplied by
the support laboratory.
3.7 Independent methods for quality control checks of sampler operation.
3.7.1 Date and time. Calendar check. Accurately set watch.
3.7.2 Leaks. Device to close sample flow pathway (plug for inlet to sharp-cut
cyclone).
3.7.3 Temperature. Thermocouple or thermistor-based digital thermometer transfer
standard, with current NIST traceability.
3.7.4 Pressure. Aneroid barometer or equivalent transfer standard with current
NIST traceability.
3.7.5 Flow rate. Low pressure flow transfer standard with leak-tight connection
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SOP # 5100STN Met One SASS
Rev. # 1
Date: September 30, 1999
Page 3 of 10
tubing. Examples: frictionless piston or soap film flowmeter; orifice-type
flowmeter, either with current NIST traceability.
4.0 Sampler Operating Procedures
Record information about the sample, the field blank, or the trip blank on an individual PM2 5
STN Custody and Field Data Form (CAFDF) (see Figure 4-1).
4.1 Sample Preparation and Programming the Met One Sampler
1. Remove the protective end caps from the cassette. Attached a dedicated sharp cut cyclone to
each cassette. Install loaded filter cassettes in predetermined (color-coded) sampling channel
locations according to the information given on the CAFDF sent from the support laboratory.
Load field blank cassette(s) every 10 sampling days. Do not activate flow to field blank
channel(s). Place cassette caps in a clean plastic bag and store for later use to seal used
cassettes for return to the laboratory.
2. Press F2 key to set up Start/Stop times in the sampler.
3. If possible, key in information (including the unique custody/data form number assigned by the
laboratory) to the sampler memory to allow later matching of the stored data with the analytical
results.
4. Edit START Date/Time, and END Date/Time using the arrow keys. The STN network will
collect 24-hour samples, beginning at midnight.
5. Select "SAVE" to save the programmed event.
6. Press Fl to review the programmed event, and then select "EXIT".
7. Make entries to the CAFDF.
4.2 Data Retrieval
1. At the end of the sample run, select "SUMMARY" option from the main screen.
2. Record end date/time, sample retrieval date/time, specified post-sampling information, and
free-form comments on the CAFDF. Please double-check entries and write clearly!
3. Download sampler data from RS232 port to laptop computer or to Met One SASS data
transfer module.
4.
4. Retain data file disk file for later use in data validation. Do not ship it to the support
laboratory. .
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SOP # 5100STN Met One SASS
Rev. # 1
Date: September 30, 1999
Page 4 of 10
5. Select "EXIT" to complete the data retrieval.
4.3 Filter Cassette Handling
The field operator will encounter filter cassettes for several uses. These are for routine (every
third day) sampling, field blanks (sent from the laboratory for use on every tenth sampling day),
and trip blanks (sent every thirty sampling days).
It is highly recommended that sampling modules (i.e. cassettes, filter packs) be removed
from the sampler within 48 hours after the sampling period ends. For a one-in-three day
schedule this will be necessary since the next sampling day's cassettes must be installed.
Once the sampled cassettes are removed, separate the sharp cut cyclone for reinstallation with
the next set of cassettes, cap or cover the cassette openings, store the cassettes in the shipping
container or cooler, complete the CAFDF, and return all to the field office. The sampled cassettes
and paperwork must be properly packaged in a cooler, ready for pickup by Federal Express,
within 96 hours after the sampling period ends. The support laboratory will provide specific
directions for packaging and shipment and days for shipment. Protect samples from direct sunlight
and extreme heat during transport from the site to the field office; store them in a secure, air-
conditioned area until just before packaging them in the cooler.
Days of the week for shipment will be arranged in coordination with the DOPO and
laboratory. Do not ship on Fridays unless prior arrangements are made with the DOPO and
laboratory.
Routine Samples
1. At the end of the sample run, lower the sampler's lower radiation shield.
2. Rotate each canister counterclockwise to remove from its sampling position. Remove the
cyclone. Cap the cassette inlet and outlet with yellow end caps. Place or store the
cyclones in a clean spot. Reinstall cyclones on the cassettes for the next sampling run.
Every 30 days of use, clean the cyclone per instructions given in the operator's manual.
3. Place each filter cassette into a zip-lock style bag and then place it in the proper location
in the storage bin or cooler.
4. Complete all paperwork.
5. Clean the area around the sample head; wipe connections with a clean cloth or paper
towel. Install a new filter cassette by aligning screws in slots and rotate it
counterclockwise to secure. Take care to properly match the SASS cassette to the
correct sampler inlet.
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SOP # 5100STN Met One SASS
Rev. # 1
Date: September 30, 1999
Page 5 of 10
Field Blank Filters
1. Field blank filters, loaded into cassettes, will be shipped from the laboratory. They will
have a separate STN Custody and Field Data Form (CAFDF) with them. They are to be
used during the same time interval as the routine sample cassettes.
2. Visit site at the time regularly scheduled for setting up a new sampler run. Install the field
blank cassettes (and sharp-cut cyclones) in the channel locations as indicated by the
CAFDF.
3. After a minute or two, remove the field blank cassettes from the sampler, detach the
cyclones, cap the cassettes, and return them to their spot in the shipping bin or cooler.
4. Proceed to install the routine sample cassettes according to schedule.
5. Complete and sign the CAFDF for the field blank cassettes and ship them back to the
laboratory, in their own cooler, at the same time as the routine samples.
Trip Blank Filters
1. Trip blank filters, loaded into cassettes, will be shipped from the laboratory. They will
have a separate CAFDF with them. They are to be used during the same time interval as
the routine sample cassettes.
2. These cassettes should be carried to the site but left in the cooler or carrying container.
They should not be installed in the sampler.
3. Complete and sign the CAFDF for the trip blank cassettes and ship them back, in their
own cooler, to the laboratory at the same time as the routine samples are shipped.
4.4 Denuder Handling
The support laboratory will change the denuder when it is due for replacement. The denuder is
an integral part of the sampling cassette.
5.0 Sampler QA/QC Procedures
Certain quality control checks must be conducted at the time of sampler startup and at monthly or
quarterly intervals thereafter. Carry out these checks before making any adjustments to the
sampler. Record information about the site, the sampler, and the results of scheduled or special
(unscheduled) quality control checks on the PM2.5 STN QA/QC Report Form, Figure 5-1. This
report form originates at the field site. The site operator should keep the original on file and send
a copy to the State or local agency QA Manager. Do not send the QA/QC Report Form to the
support laboratory. Any actions taken to service or calibrate the speciation sampler after the
check must be recorded in brief on the form and in detail in the field operator's notebook.
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SOP # 5100STN Met One SASS
Rev. # 1
Date: September 30, 1999
Page 6 of 10
5.1 Date and Time Checks
Conduct these checks monthly or whenever daylight savings time changes occur. Compare the
date and time displayed on the sampler to the known date and to an accurately set watch.
Record information on the QA/QC data form. Refer to Figure 5-1.
5.2 Monthly Leak Check
Performed upon startup, then monthly.
1. Place cassette containing filter/denuder and attached sharp cut point cyclone at the channel
location to be leak-checked. Use this cassette assembly for leak checks and flow rate
checks only. The cassette must contain the type of filter (and denuder, if included in the
cassette) normally used at this sampling channel location.
2. Press F3 key, and select "PUMP ON".
3. Plug the Sample Inlet (e.g., Channel 1) with cap. Note the displayed flow. The indicated
flow rate should drop to 0.0 L/min. If it does not, check for leaks and repeat the
procedure until the leak check is completed successfully. Repeat for all channels in use.
4. Select "PUMP OFF" to stop the pump, and "EXIT".
5. Release the vacuum slowly to avoid damaging the leak check filter.
5.3 Monthly Temperature Control Check
Performed upon startup and then monthly. Check the ambient and filter temperature sensors of
the sample by positioning the probe of a certified transfer standard digital thermometer in close
proximity to the sampler sensors. Allow time to achieve stable readings and record the results in the
field notebook and on the STN QA/QC report form. If the sampler and control check temperature
readings differ by more than + 2°C, trouble-shoot the system and recheck. If still out of tolerance,
conduct a multipoint calibration or replace the faulty sensor. Consult the manufacturer and the
operator's manual for procedures.
5.4 Quarterly Temperature Control Check
Performed each calendar quarter. Follow the same steps as in Section 5.3, but use a
temperature transfer standard that is independent of the one used for the monthly checks. Should
a temperature sensor not maintain its calibration after the monthly or quarterly checks,
maintenance and/or replacement of the faulty parts must occur.
5.5 Monthly Pressure Control Check
1. Compare the ambient barometric pressure readout from the sampler display screen with
the reading from a certified transfer standard barometer.
2. If the pressure readings differ by more than + 10 mm Hg, perform a multipoint calibration
of the sensor or replace the faulty sensor.
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SOP # 5100STN Met One SASS
Rev. # 1
Date: September 30, 1999
Page 7 of 10
5.6 Quarterly Pressure Control Check
Follow the same steps as in Section 5.5, but use a pressure standard that is independent of the
one used for the monthly checks. Should the pressure sensor system not maintain its calibration after
the monthly or quarterly checks, maintenance and/or replacement of the pressure sensor system must
occur.
5.7 Monthly Flow Rate Control Check
Perform flow rate check upon startup, then monthly.
1. Use same cassette assembly called for in monthly Leak Check Procedure (Section 5.2).
2. Connect an external flow audit device to the cyclone sample inlet (e.g., Channel 1). Use a
low pressure drop certified flow transfer standard.
3. Press the F3 key, and select "PUMP ON".
4. Compare the flow rate measured by the external flow device with displayed value. (The
sampler is preset at 6.7 L/min). If the flow deviation exceeds + 4% (+ 0.27 L/min)
contact Met One for technical support since the critical orifice flow rates are set at the
factory.
5. Repeat the procedure for all flow channels in use.
5.8 Quarterly Flow Rate Control Check
Performed each calendar quarter. Follow the same steps as in Section 5.7, but use a flow rate
transfer standard that is independent of the one used for the monthly checks. Should the flowrate
mechanism not maintain its calibration after the monthly or quarterly checks, maintenance and/or
replacement of the flow controller system(s) must occur. Consult the manufacturer or the
operator's manual for procedures for maintenance, adjustment, and calibration of sample flow
rates.
6.0 Sampler Maintenance and Troubleshooting
1. Clean the solar radiation shield with wet cloth as required.
2. If flow rate falls off, or is variable, the unit may need factory servicing of the pump or of the
particle filter/critical orifice flow controllers.
3. Check O-rings for wear or damage. Make a comment on the CAFDF to the laboratory
of problems with cassette assemblies.
4. Record all maintenance and troubleshooting activities in the site notebook. On the
CAFDF, record activities that may affect the sample weight or analysis.
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SOP # 5100STN Met One SASS
Rev. # 1
Date: September 30, 1999
Page 8 of 10
BAR CODE GOES HERE
Custody/Data Form
No.
A. CUSTODY RECORD
1 . Laboratory, Out
2. Site. In
PM2.5 STN CUSTODY AND White - return to lab
FIELD DATA FORM ^^^"*
(Name, Date)
3. Site, Out
B. SITE AND SAMPLER
1. Site AIRS Code
2. Sampler S/N
3. Sampler Type
4. Sampler POC
INFORMATION
4. Lab, In
5. Site Name
6. Intended date of use
7. Date of :
8. Operate
>a
's
mpler set-up
name
C. SAMPLER CHANNEL COMPONENTS
Channel
Number
1
1
2
2
3
3
D. START, END,
Channel No.
1
2
3
Component ID
No.
kept at site
11234568
kept at site
11234570
kept at site
11234572
Component Description
SASS cyclone
SASS cassette (Teflon filter)
(GREEN)
SASS cyclone
SASS cassette (MgO denuder
nylon filter) (RED)
SASS cyclone
SASS cassette (quartz filter)
(ORANGE)
AND RETRIEVAL TIMES
Start date Start time
End date
End time Retrieval Retrieval
date time
E. SAMPLER CHANNEL INFORMATION (Post-Sampling)
Channel Run
No. Time
1
2
3
Channel -T
No. Flag
1
2
3
F. Comments
Run
Time, Flag
Avg. Filter
T(°C)
Sample
Volume
(m3)
Max. Filter
T(°C)
Avg.
flow
(L/min)
Min. Filter
T(°C)
Avg. Avg. Max. Min.
flow CV ambient ambient ambient
(L/min) T(°C) T(°C) T(°C)
Avg.BP Max. BP Min.BP
(mm Hg) (mm Hg) (mm Hg)
(Revised 9/27/99:5103)
Figure 4-1. STN Custody and Field Data Form With Entries for the Met One SASS Sampler.
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SOP # 5100STN Met One SASS
Rev. # 1
Date: September 30, 1999
Page 9 of 10
QA/QC Form No.
PM2 5 STN QA/QC REPORT FORM '^^IM,
A. SITE AND SAMPLER INFORMATION
1. Site AIRS Code
7 Sampler S/N
3 Sampler Tvpe
4. Sampler POC
B. DATE AND TIME CHECKS (Transit
5. Site Name
6 Interval: Month Quarter Special
7. Date(s) of QA/QC (
8. Operator's Name
Checks
T Standard Name Transfer Standard ID Number )
Sample display date/time Transfer standard date/time
C. LEAK CHECKS
Date and time agree ± 5 min? Action taken (a)
(Transfer Standard Name Transfer Standard ID Number )
Channel number
1
2
3
4
5
Manufacturer's specifications met?
Action taken and recheck results (a)
D. TEMPERATURE CHECKS (Transfer Standard Name Transfer Standard ID Number )
Sensor location
Ambient
Filter
Sampler display (°C) Transfer standard (°C) Agreement ± 2 °C ? Action taken and
recheck results (a)
E. PRESSURE CHECKS (Transfer Standard Name Transfer Standard ID Number )
Sensor location
Ambient
Sampler display, Transfer standard, Agreement within Action taken and
(mm Hg) (mm Hg) ±10 mm Hg? recheck results (a)
F. FLOW RATE CHECKS (Transfer Standard Name Transfer Standard ID Number )
Channel number
1
2
3
4
5
G. COMMENTS
Sampler display,
(L/min)
Transfer standard
display, (L/min)
Design flow rate,
(L/min)
Agreement within Action taken and
± 10 percent? (b) recheck results (a)
(Revised 09/23/99)
(a)Fully describe actions taken in field notebook.
(b) Sampler flow rate must agree with both transfer standard and design flow rate to pass.
Figure 5-1. STN QA/QC Report Form.
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SOP # 5100STN Met One SASS
Rev. # 1
Date: September 30, 1999
Page 10 of 10
7.0 References
1. Operation Manual (Draft). Spiral Aerosol Speciation Sampler SASS. Met One
Instruments. June 8, 1998.
2. Met One SASS (Chemical Speciation) Sampler "Quick Operation." Met One
Instruments. Not dated.
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APPENDIX A-3
SOP 5200STN
CONDENSED STANDARD OPERATING
PROCEDURE FOR THE ANDERSEN RAAS
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SOP # 5200STN Andersen RAAS
Rev. # 2
Date: February 14,2001
Page 1 of 12
CONDENSED STANDARD OPERATING
PROCEDURE (SOP)
FOR THE ANDERSEN RAAS
Prepared by: Date:
Prepared by: Date:
Reviewed by: Date:
Approved by: Date:
PM2 5 Speciation Trends Network
Office of Air Quality Planning and Standards
U.S. Environmental Protection Agency
Research Triangle Park, NC 27709
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SOP # 5200STN Andersen RAAS
Rev. # 2
Date: February 14,2001
Page 2 of 12
1.0 Purpose and Applicability
This condensed standard operating procedure (SOP) outlines procedures for field
operations of the Andersen RAAS PM2.5 speciation sampler. For more detailed information
regarding operation of this sampler, refer to the latest edition of the Andersen RAAS
operator's manual.
2.0 Precautions
2.1 Read and thoroughly understand the operator's manual before beginning field operations.
The flow rate, temperature, and barometric pressure calibrations of the sampler must be
checked and, if necessary, adjusted to specifications prior to taking the first sample.
Consult the operator's manual for calibration instructions.
2.2 Use only the sampling modules, sent to you from the laboratory, for the designated
sampler and location.
2.3 Exercise great care in placement and handling of sampling modules to avoid contamination.
3.0 Equipment and Supplies
3.1 Have the STN Custody and Field Data Form for the particular sampler, for the particular
sampling day, with you when visiting the site. Have an STN QA/QC Report Form if a
quality control check is due.
3.2 Sampler operator's manual and field notebook.
3.3 Andersen RAAS speciation sampler and accessories.
3.4 A set of three laboratory-supplied, pre-loaded sampling modules (filter holders) containing
Teflon, nylon, and quartz filters, respectively. A separate sampling module containing a
cassette with glass fiber or other filter for use in the fourth flow channel to maintain proper
flow distribution (the latter module is kept at the site). Field blank modules for use on
every 10th sampling day. Denuder tube to remove acidic vapors. Shipping containers
(coolers), frozen ice substitutes, and Federal Express labels for shipment of sampling
modules, denuders, and reports to the analytical laboratory. All these items will be
supplied from the support laboratory.
3.5 Independent methods for verifying proper sampler operation.
3.5.1 Date and Time. Calendar check. Accurately set watch.
3.5.2 Leaks. Device to close sample flow pathway (flow rate adapter).
3.5.3 Temperature. Thermocouple or thermistor-based digital thermometer, with
current NIST traceability. Tegam® temperature calibrator assembly.
3.5.4 Pressure. Aneroid barometer or equivalent transfer standard with current
NIST traceability.
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SOP # 5200STN Andersen RAAS
Rev. # 2
Date: February 14,2001
Page 3 of 12
3.5.5 Flow rate. Low-pressure flow device with leak-tight connection tubing.
Examples: frictionless piston or soap film flowmeter; orifice-type flowmeter; or
RAAS flow calibration kit with reference dry gas meter. Each should have
current NIST traceability.
3.5.6 As an option, a multi-purpose device for checking temperature, pressure, and
flow rate simultaneously.
4.0 Sample Operating Procedures
Record information about the sample, the field blank, or the trip blank on an individual PM2 5
STN Custody and Field Data Form (CAFDF) (see Figure 4-1).
4.1 Sample Preparation and Programming the Andersen RAAS Sampler
1. Remove the plastic tranport bin containing the three capped sampling modules from the
cooler. Each sampling module is bar-coded with a number and is color-coded. Care
must be taken to place the correct sampling module in the corresponding RAAS sampling
channel. Place the plastic caps in plastic bags in the bin to maintain their cleanliness and
for safekeeping. These will be used to seal the modules following sampling. Install fresh
denuder(s) if a change is due.
2. Install the loaded sampling modules in predetermined sampling channel locations
according to instructions in the RAAS Operator's Manual and sample channel
information given on the CAFDF sent from the support laboratory. Refer to Section 4.3,
below, for sample module handling techniques.
3. Consult the RAAS operator's manual, section 5, for guidance on entering site
information. If desired, key in the custody/data form number (this is printed on the
CAFDF) to the "User Info 1" field. Double-check the entry. Press the "Enter" key and
return to the main menu.
4. From main menu, choose the "Setup Run" option, and press the "Enter" key to select
Filter 1.
5. Press the "Enter" again.
6. Enter the start date (MMDDYY format) and press the "Enter" key.
7. Enter the sample duration in hours, press "Enter" to complete setup.
8. Make entries to the CAFDF.
4.2 Data Retrieval
3. At the end of the sample run, return to the main screen.
4. Select "View Run", and choose the "Last Sample" option.
5. Record end date/time, sample retrieval date/time, specified post-sampling information,
and free-form comments on the CAFDF. Please double-check entries and write
clearly using a ball-point pen!
6. Return to the main screen by pressing the "Cancel" button.
7. Download data electronically to a laptop computer or to the Andersen DataLink
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SOP # 5200STN Andersen RAAS
Rev. # 2
Date: February 14,2001
Page 4 of 12
accessory. Refer to Section 7 of the operator's manual for further instruction on data
logging. Retain the data file disk for later use in data validation. Do not send it to the
support laboratory.
4.3 Sample Module Handling
The field operator will receive pre-loaded sampling modules for several uses. These are for
routine (every third day) sampling, field blanks (sent for use on every tenth sampling day), and
trip blanks (sent every thirty sampling days).
It is required that sampling modules be removed from the sampler within 48 hours after
the sampling period ends. For a one-in-three day schedule this will be necessary since the
next sampling day's sampling modules must be installed.
Once the sampling modules are removed from the sampler, cap them, store in plastic bags in
the correct spot in the transport bin, and return all to the field office. The used sampling modules and
paperwork must be properly packaged in a cooler, ready for pickup by Federal Express,
according to the schedule provided by the support laboratory. Protect samples from direct sunlight
and extreme heat during transport from the site to the field office; store them in a secure, air-
conditioned area until just before packaging them in the cooler.
Days of the week for shipment will be arranged in coordination with the DOPO and the
support laboratory. Do not ship on Fridays or the day before a holiday unless prior
arrangements are made with the DOPO and laboratory.
Routine Samples
1. Within 48 hours after the end of a sample run, remove the sampling module(s) from the
upstream SVL coupler and from the downstream tubing assembly. Cap both ends of the
module.
2. Install a new sampling module for the next run.
3. Place used sampling modules (capped and inside a plastic bag) in slots in the transport
bin. Complete all paperwork, insert it in the plastic bag provided, and place on top of the
modules in the bin. Place the plastic top on the bin and place the bin in the cooler for
shipment to the laboratory. Follow packing directions provided by the laboratory.
Field Blank Filters
1. Field blank filters, pre-loaded into sampling modules, will be shipped from the laboratory
for use every 10th sampling day. They will have a separate CAFDF with them. They
are to be used during the same time interval as the routine sampling modules.
2. Visit the site at the time regularly scheduled for setting up for a new sampler run. Install
the field blank modules in the channel locations as indicated by the CAFDF.
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SOP # 5200STN Andersen RAAS
Rev. # 2
Date: February 14,2001
Page 5 of 12
3. After a minute or two, remove the field blank modules, cap them, place each inside a
plastic bag, and return them to the transport bin.
4. Proceed to install the routine sample modules according to schedule.
5. Complete and sign the CAFDF for the field blank modules and ship it and the field blank
modules back to the laboratory at the same time as the routine samples are shipped.
Trip Blank Filters
1. Trip blank filters, loaded into capped sampling modules, will be shipped from the
laboratory for use every 30th sampling day. They will have a separate CAFDF with
them. They are to be used during the same time interval as the routine sample modules.
2. Trip blank modules should be carried to the site but left in the transport bin inside the
cooler. They should not be installed in the sampler.
3. Complete and sign the CAFDF for the trip blank filter cassettes and ship it and the trip
blank modules back to the laboratory at the same time as the routine samples are
shipped.
4.4 Denuder Handling
If it is time to refurbish the denuder(s), remove it, cap the ends, wrap it in protective material
(polyurethane foam pipe insulation and bubble packaging), and place it in a sturdy cardboard box for
shipment back to the laboratory for refurbishment. Install a fresh denuder, supplied from the support
laboratory.
5.0 Sampler QA/QC Procedures
Certain quality control checks must be conducted at the time of sampler startup and at monthly
or quarterly intervals thereafter. Carry out these checks before making any adjustments to the
sampler. Record information about the site, the sampler, and the results of scheduled or special
(unscheduled) quality control checks on the PM2 5 STN QA/QC Report Form, Figure 5-1.
This report form originates at the field site. The site operator should keep the original on file
and send a copy to the State or local agency QA Manager. Any actions taken to service or
calibrate the speciation sampler after the check must be recorded in brief on the form and in
detail in the field operator's notebook.
5.1 Date and Time Checks
Conduct these checks monthly or whenever daylight savings time changes occur. Compare the
date and time displayed on the sampler to the known date and to an accurately set watch.
Record information on the QA/QC report form. Refer to Figure 5-1.
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SOP # 5200STN Andersen RAAS
Rev. # 2
Date: February 14,2001
Page 6 of 12
5.2 Monthly Leak Check
Perform leak check upon startup, then monthly.
1 Install a sampling module containing a filter at the channel location to be leak-checked.
Use this sampling module for leak checks and flow rate audits only. The module must
contain the type of filter normally used at this sampling channel location. A denuder must
also be in place if called for in the sampling protocol.
2 Remove the sampler inlet assembly. Attach an Andersen flow audit adapter to the down
tube and close the adapter.
3 From the main menu select the "Leak Check" option and press "Enter." The system
evacuates air and the pump continues to run. The screen must indicate a flow of less than
0.08 L/min for a period of at least 3 minutes. If the system fails this criterion, check for
leaks in the system and repeat the leak check until it is passed successfully. Press the
"Cancel" key when finished.
4 Release vacuum slowly to avoid filter damage.
5.3 Monthly Temperature Control Check
Performed upon startup, then monthly.
1. From the main menu, choose "Maintenance" option and then select "Monitor" option.
The screen will display real-time values for temperature and pressure.
2. Check the ambient, manifold, and cabinet temperature sensors of the sampler by
positioning the probe of a certified transfer standard digital thermometer in close proximity
to each sampler sensor. Allow time to achieve stable readings and record the results in
the field notebook.
3. Alternatively, use the Tegam thermocouple calibrator to input -30, 0, and 45°C settings
and record the corresponding temperatures indicated by the RAAS. (Allowable error is
+ 2 °C.) If the sampler and control check temperature readings differ by more than +
2°C, trouble-shoot the system and recheck. If still out of tolerance, conduct a multipoint
calibration or replace the faulty sensor.
5.4 Quarterly Temperature Control Check
Performed each calendar quarter. Follow the same steps as in Section 5.3, but use a
temperature transfer standard that is independent of the one used for the monthly checks.
Should a temperature sensor not maintain its calibration after the monthly or quarterly checks,
maintenance and/or replacement of the faulty parts must occur.
5.5 Temperature Calibration
1. Unplug the thermocouple labeled "Ambient" on the panel and connect a Tegam®
temperature calibrator.
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SOP # 5200STN Andersen RAAS
Rev. # 2
Date: February 14,2001
Page 7 of 12
2. From the main screen select "Maintenance" option, then choose "Calibrate", and select
"Ambient" to calibrate the ambient temperature in the system.
3. When the system prompts for a low ambient temperature value (-20°C), enter low value
on the Tegam calibrator.
4. Enter value of the Tegam calibrator into the system using numeric keypad.
5. Now the system prompts for a high ambient temperature value (40°C). Enter high value
on the Tegam calibrator.
6. Enter value of the Tegam calibrator into the system using numeric keypad.
7. Change value of the Tegam calibrator and verify this change in the display screen. (The
allowable error is + 2°C.)
8. At the end of ambient temperature calibration, save the calibration by selecting "Yes"
option when the sampler display prompts to do so.
9. Repeat the procedure to calibrate the meter temperature and the filter temperature.
5.6 Monthly Pressure Control Check
Performed upon startup, then monthly.
1. Compare the ambient barometric pressure readout from the sampler display screen with
the reading from a certified transfer standard barometer.
2. If the pressure readings differ by more than +10 mm Hg, perform a multipoint calibration
of the sensor or replace the faulty sensor.
5.7 Quarterly Pressure Control Check
Performed each calendar quarter. Follow the same steps as in Section 5.6, but use a pressure
standard that is independent of the one used for the monthly checks. Should the pressure sensor
system not maintain its calibration after the monthly or quarterly checks, then calibration, maintenance,
and/or replacement of the pressure transducer must occur.
5.8 Meter and Barometric Pressure Calibrations
1. Connect a pressure calibration apparatus to the port on the panel located inside of the
unit. Connect one end of a tee to a NIST-traceable external pressure gauge by tubing.
Connect the other end of the tee to the pressure calibration port in the system by tubing.
Attach a plastic syringe to the tee's middle junction by tubing.
2. From the main screen select "Maintenance" option, then choose "Calibrate," and select
"Meter Drop" to calibrate the meter pressure drop in the system.
3. When the system prompts for a low pressure value, pull the plunger from the syringe until
the external pressure gauge reads approximately 600 mm Hg.
4. Clamp the tubing between the syringe and the tee to hold the pressure, and key the exact
value shown by the external pressure gauge into the system.
5. When the system prompts for a high pressure value, push the plunger until the external
pressure gauge reads approximately 800 mm Hg.
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SOP # 5200STN Andersen RAAS
Rev. # 2
Date: February 14,2001
Page 8 of 12
6. Hold pressure, and enter the exact value shown by the external pressure gauge into the
system using the keypad.
7. Change the value in the external pressure gauge using the syringe and check whether the
value matches with the value shown on the screen. (The allowable error is + 5 mm Hg.)
8. At the end of meter drop pressure calibration, save the calibration by selecting the "Yes"
option when the sampler screen prompts to do so.
9. Repeat the above procedure to calibrate the barometric pressure sensor.
5.9 Monthly Flow Rate Control Check
Perform the flow rate control check upon startup, then monthly.
1. Use same sampling module called for in Monthly Leak Check procedure (Section 5.2).
2. For denuder channels, disconnect the top of the denuder from the sample manifold
channel outlet. For other channels, disconnect the sampler module from the sample
manifold outlet. Use compression fittings supplied with the sampler to attach a certified
flow transfer standard to the denuder inlet or the sampling module inlet, depending on the
channel to be checked.
3. From the main menu select the "Verify Flow" option to start the flow verification process.
4. After one minute, compare the flow displayed on the screen with the flow indicated by the
external flow meter.
5. Repeat the flow audit procedure for all channels. Channels 1, 2, 5, and 4 flow rates are
preset at 16.7, 7.3, 7.3, and 16.7 L/min, respectively. If the channel's flow rate error is
greater than 10%, the channel requires flow calibration using a reference dry gas meter
(consult operator's manual), or maintenance of the pump, or maintenance of the critical
orifice flow controller.
5.10 Quarterly Flow Rate Control Check
Performed each calendar quarter. Follow the same steps as in Section 5.9, but use a flow rate
transfer standard that is independent of the one used for the monthly checks. Should the flow
rate mechanism not maintain its calibration after the monthly or quarterly checks, maintenance
and/or replacement of the flow controller system(s) must occur.
6.0 Sampler Maintenance and Troubleshooting
1. Clean dust from the interior of the sampling cabinet. Use a damp cloth. Clean at least
monthly or more often if local conditions warrant.
2. Pay close attention to O-rings for signs of wear or loosening. Replace O-rings promptly
and leak check the system after replacement.
3. The sample inlet, down tube, and fine paniculate cyclones will require periodic cleaning
and maintenance for proper operation. The manufacturer recommends the cyclones be
disassembled and cleaned every 30 sampling days. Refer to Section 11 of the RAAS
operator's manual for detailed information.
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SOP # 5200STN Andersen RAAS
Rev. # 2
Date: February 14,2001
Page 9 of 12
4. Refer to the Andersen RAAS operator's manual, Section 12, for a thorough discussion of
troubleshooting techniques.
5. Record all maintenance and troubleshooting activities in the site notebook. On the
CAFDF, record activities that may affect the sample weight or analysis results.
7.0 References
1. RAAS™ Operator's Manual. Model RAAS2.5-400 Chemical Speciation Monitor.
Thermo-Andersen Instruments, Inc. Smyrna, GA. Revision 2. September 27, 2000.
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SOP # 5200STN Andersen RAAS
Rev. # 2
Date: February 14,2001
Page 10 of 12
BAR CODE GOES HERE
Custody/Data Form No.
PM2 5 STN CUSTODY AND c White (return to lab)
FIELD DATA FORM c' Yellow (site retains)
MtLU UAIA I-UKIVI c Pink (lab)
A. CUSTODY RECORD (Name, Date)
1. Laboratory, Out
2. Site, In
BIN ID:
3. Site. Out
4. Lab, In
B. SITE AND SAMPLER INFORMATION
1. Site AIRS Code
2. Sampler S/N
3. Sampler Type
4. Sampler POC
5. Site Name
6. Intended date of use
1 ' . Date of sar
3. Operator's
ncler set-uc
name
C. SAMPLER CHANNEL COMPONENTS
Channel
Number
1
2
2
5
4
Component ID
No.
11234567
Kept at Site
11234569
11234570
Kept at Site
Component Description
RAAS module (filer holder) (Teflon filter) (GREEN)
RASS denuder assembly (MgO) (RED)
RAAS module (nylon filter) (RED)
RAAS module (quartz filter) (YELLOW)
RAAS module (cellulose filter) (BLUE). Operator replaces filter after each run.
D. START, END, AND RETRIEVAL TIMES
Channel No.
1
2
5
4
Start date St;
E. SAMPLER CHANNEL INFORMATIC
Channel
No.
Elapsed
sample time
1
2
5
4
Channel
No.
Avg. BP
(mm Hg)
1
2
5
4
F. Comments
E. S. time
Flag
Max. BP
mm Hg)
art time End date
End time
Retrieval
date
Retrieval
time
)N Post-Sampling)
Sample
Volume (m3)
Min.BP
(mm Hg)
Avg. flow
(L/min)
•Flow
Flag
Avg. ambient
T(°C)
•T
Flag
Max. ambient
T(°C)
PumpP
(mm Hg)
Min. ambient
T(°C)
Manifold
T(°C)
(Revised 02/1 4/01: 5200)
Figure 4-1. STN Custody and Field Data Form With Entries for the RAAS Sampler.
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SOP # 5200STN Andersen RAAS
Rev. # 2
Date: February 14,2001
Page 11 of 12
QA/QC Form No.
PM2 5 STN QA/QC REPORT FORM c ' (slte retalns)
Z'^ ^ ^ c. 2 (Agency QAM)
A SITE AND SAMPLER INFORMATION
1. Site AIRS Code
2 Sampler S/N
3. Sampler Tvpe
4. Sampler POC
B. DATE AND TIMI
5. Site Name
6 Interval: Month Quarter Special
7. Date(s) of QA/QC Checks
8. Operator's Name
] CHECKS (Transfer Standard Name Transfer Standard ID Number )
Sample display date/time Transfer standard date/time
C. LEAK CHECKS
Date and time agree ± 5 min? Action taken (a)
(Transfer Standard Name Transfer Standard ID Number )
Channel number Manufacturer's specifications met? Action taken and recheck results (a)
1
2
5
4
D. TEMPERATURE CHECKS (Transfer Standard Name Transfer Standard ID Number )
Sensor location
Ambient
Cabinet
Manifold
Sampler display (°C) Transfer standard (°C) Agreement ± 2 °C ? Action taken and
recheck results (a)
E. PRESSURE CHECKS (Transfer Standard Name Transfer Standard ID Number )
Sensor location
Ambient
Pump
Sampler display, Transfer standard, Agreement within Action taken and
(mm Hg) (mm Hg) ±10 mm Hg? recheck results (a)
F. FLOW RATE CHECKS (Transfer Standard Name Transfer Standard ID Number )
Channel number
1
2
5
4
G. COMMENTS
Sampler display, Transfer standard
(L/min) display, (L/min)
Design flow rate, Agreement within Action taken and
(L/min) ± 10 percent? (b) recheck results (a)
(Revised 02/1 4/99: 5200)
(a)Fully describe actions taken in field notebook.
(b) Sampler flow rate must agree with both transfer standard and design flow rate to pass.
Figure 5-1. STN QA/QC Report Form.
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APPENDIX A-4
SOP 5300STN
CONDENSED STANDARD OPERATING
PROCEDURES
FOR THE URG MASS 400 AND URG MASS 450
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SOP # 5300STN URG MASS 400 & 450
Rev. # 1
Date: September 30, 1999
Page 1 of 5
CONDENSED STANDARD OPERATING
PROCEDURES (SOP)
FOR THE URG MASS 400 AND URG MASS 450
Prepared by: Date:
Prepared by: Date:
Reviewed by: Date:
Approved by: Date:
PM2 5 Speciation Trends Network
Office of Air Quality Planning and Standards
U.S. Environmental Protection Agency
Research Triangle Park, NC 27709
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SOP # 5300STN URG MASS 400 & 450
Rev. # 1
Date: September 30, 1999
Page 2 of 5
1.0 Purpose and Applicability
772/5 condensed standard operating procedure (SOP) outlines procedures for field
operations of the University Research Glassware (URG) Models 400 and 450 MASS PM2 5
speciation samplers. The MASS 400 is a stand-alone system designed to collect trace
metals, onions, and cations. The MASS 450 is a stand-alone system designed to collect
samples for analysis of organic and elemental carbon and semivolatile organic particles.
For more detailed information regarding operation of either sampler, refer to the URG
MASS operator's manual.
2.0 Precautions
2.1 Read and thoroughly understand the operator's manual before beginning field operations.
The flow rate, temperature, and pressure calibrations of the sampler must be checked and,
if necessary, adjusted to specifications prior to taking the first sample. Consult the
operator's manual for calibration instructions.
2.2 Use only filter packs and denuders, sent to you from the laboratory, for the designated
sampler and location.
2.3 Exercise great care in placement and handling of sampling modules (i.e., filter packs and
denuders) to avoid contamination.
3.0 Equipment and Supplies
3.1 Have the STN Custody and Field Data Form for the particular sampler, for the particular
sampling day, with you when visiting the site. Have an STN QA/QC Report Form if a
quality control check is due.
3.2 Sampler operator's manual and field notebook.
3.3 URG MASS 400 and 450 speciation samplers and accessories.
3.4 Teflon filter packs, pre-loaded with filters, for two channels. Field blank modules for use
on every 10th sampling day. Annular denuder for the MASS 400 sampler. Shipping
containers, frozen ice substitutes, and Federal Express labels for shipment of sampling
modules, denuders, and reports to analytical support laboratory. All of this equipment will
be supplied from the support laboratory.
3.5 Independent methods for verifying proper sampler operation.
3.5.1 Date and time. Calendar check. Accurately set watch.
3.5.2 Leaks. Device to close sample flow pathway (flow rate adapter).
3.5.3 Temperature. Thermocouple or thermistor-based digital thermometer transfer
standard with current NIST traceability. Tegam temperature calibrator assembly.
3.5.4 Pressure. Aneroid barometer or equivalent transfer standard with current NIST
traceability.
3.5.5 Flow rate. Low-pressure flow device with leak-tight connection tubing.
Examples: frictionless piston or soap film flowmeter; orifice-type flowmeter; or
reference dry gas meter with thermometer and tubing connections. Each should
have current NIST traceability.
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SOP # 5300STN URG MASS 400 & 450
Rev. # 1
Date: September 30, 1999
Page 3 of 5
4.0 Sampler Operating Procedures
Record information about the sample, the field blank, or the trip blank on an individual PM2.5
STN Custody and Field Data Form (CAFDF) (see Figure 4-1). The procedures given below
apply to both the MASS 400 and MASS 450 stand-alone systems.
4.1 Sample Preparation and Programming the URG MASS 400 or 450 Sampler
3.
4.
5.
6.
Remove caps from the filter packs. Store the caps in a clean plastic bag. The caps will be
used to seal the filter pack following sampling. Install loaded filter packs in the sampling
channel locations according to the sample channel information given on the CAFDF sent
from the support laboratory. Channel 1 is the MASS 400 sampler; channel 2 is the
MASS 450 sampler. Refer to Section 4.3.
From main menu, choose the "Setup Run" option, and press the "Enter" key to select
Filter 1. User information and filter ID number can be entered at this time. Key in the
custody/data form number (this is printed on the CAFDF). Double-check the entry.
Press the "Enter" key again.
Enter the start date (MMDDYY format) and press the "Enter" key.
Enter the sample duration in hours, then press "Enter" to complete setup.
Make entries to the CAFDF.
4.2 Data Retrieval
1. At the end of the sample run, return to the main screen.
2. Select "View Run", and choose "Last Sample" option to view information about the
previous sampling event.
3. Record the end date/time, sample retrieval date/time, specified post-sampling information,
and free-form comments on the CAFDF. Please double-check entries and write
clearly!
4. Return to the main screen by pressing the "Cancel" button.
5. Download data electronically to a laptop computer or to the MASS Data Link accessory.
Refer to Section 7 of the operator's manual for further instruction on data logging. Retain
the data file disk for later use in data validation. Do not send it to the support laboratory.
4.3 Filter Pack Handling
The field operator will be shipped filter packs for several uses. These are for routine (every third
day) sampling, field blanks (sent for use on every tenth sampling day), and trip blanks (sent every
thirty sampling days).
It is highly recommended that sampling modules (i.e. filter packs) be removed from the
sampler within 48 hours after the sampling period ends. For a one-in-three day schedule this
will be necessary since the next sampling day's filter packs must be installed.
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SOP # 5400STN Packing Instructions
Rev. # 1
Date: December 20,2000
Page 4 of4
Once the sampled filter packs are removed from the sampler, cap both ends, place the filter
packs in plastic zip-lock bags, store them in the shipping container, and return them to the field
office. The sampled filter packs and paperwork must be properly packaged in a cooler,
ready for pickup by Federal Express, within 96 hours after the sampling period ends. The
support laboratory will provide specific directions for packaging and shipment and days
for shipment. Protect samples from direct sunlight and extreme heat during transport from the
site to the field office; store them in a secure, air-conditioned area until just before packaging
them in the cooler.
Days of the week for shipment will be arranged in coordination with the DOPO and
laboratory. Do not ship on Fridays or the day before a holiday unless prior arrangements
are made with the DOPO and laboratory.
Routine Samples
6. At the end of sample run, remove the tubing located at the bottom of the filter pack.
7. Gently twist (Vi turn) to unlock the WINS impactor/filter assembly from the down tube
connector. Note: The filter holder is threaded to the WINS impactor.
8. Holding the WINS upright in one hand, unscrew the filter pack from the WINS.
9. Cap both ends of the just-removed filter pack. Attach a new filter pack to the WINS
impactor.
10. Align WINS to the down tube connector and twist (1/4 turn) to lock.
11. Connect tubing to the bottom of the filter pack.
12. Place each used filter pack into individual, prelabeled zip-lock style bags and place in the
cooler.
Field Blank Filters
1. Field blank filters, loaded into filter packs, will be shipped from the laboratory. They will
each have a separate CAFDF with them. They are to be used during the same time
interval as the routine sample filter packs.
2. Visit the site at the time regularly scheduled for setting up for a new sampler run. Install
the field blank filter packs in the MASS 400 and MASS 450 sampling channel locations
as indicated by the CAFDF.
3. After a minute or two, remove the field blank filter packs, cap them, place each inside a
plastic zip-lock bag, and return them to the shipping container.
4. Proceed to install the routine sample filter packs according to schedule.
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SOP # 5300STN URG MASS 400 & 450
Rev. # 1
Date: September 30, 1999
Page 5 of 11
Trip Blank Filters
1. Trip blank filters, loaded into filter packs, will be shipped from the laboratory. They will
have a separate STN Custody and Field Data Form (CAFDF) with them. They are to
be used during the same time interval as the routine sample filter packs.
2. The trip blank filter packs should be carried to the site but left in the cooler
containers. They should not be installed in the sampler.
3. Complete and sign the CAFDF for the trip blank filter packs and ship them back to the
laboratory at the same time as the routine samples.
4.4 Denuder Handling
If it is time to refurbish the denuder(s), follow these steps for the MASS 400 or 450.
1. Remove the sampler inlet head. Disconnect the downtube (it contains the denuder),cap
it, and place it in the cooler. Replace with a fresh downtube/denuder. Reinstall the
sample inlet.
2. Place the denuder in the appropriate slot in the shipping cooler to be returned to the
laboratory for refurbishment.
5.0 Sampler QA/QC Procedures
Certain quality control checks must be conducted at the time of sampler startup and at
monthly or quarterly intervals thereafter. Carry out these checks before making any
adjustments to the samplers. Record information about the site, the samplers, and the
results of scheduled or special (unscheduled) quality control checks on the PM2.5 STN
QA/QC Report Form, Figure 5-1. The site operator should keep the original on file and
send copies to the State or local agency QA Manager and to the analytical laboratory. This
report form originates at the field site. Any actions taken to service or calibrate the
speciation sampler after the check must be recorded in brief on the form and in detail in the
field operator's notebook.
5.1 Date and Time Checks
Conduct these checks monthly or whenever daylight savings time changes occur. Compare the
date and time displayed by the samplers to the known date and to an accurately set watch.
Record this information on the QA/QC field data form. See Figure 5-1.
5.2 Monthly Leak Check
Perform leak check upon startup, then monthly.
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SOP # 5300STN URG MASS 400 & 450
Rev. # 1
Date: September 30, 1999
Page 6 of 11
1. Place filter pack containing filter at channel location to be leak-checked. Use this
filter pack assembly for leak checks and flow rate checks only. The filter pack must
contain the type of filter normally used at this sampling channel location. A denuder
should also be in place if called for in the sampling protocol.
2 Attach a flow rate adapter to the down tube and close the adapter.
3. From the main menu select the "Leak Check" option and press "Enter". The system
evacuates air and the pump continues to run. The screen must indicate a flow of less
than 0.08 L/min for a period of 10 minutes. The timer will reset if flow exceeds 0.08
L/min. If the system fails this criterion, check for leaks in the system and repeat the leak
check until it is passed successfully. Press "Cancel" or any other key when finished.
4. Release vacuum slowly to avoid filter damage and splashing impactor oil.
5.3 Monthly Temperature Control Check
Performed upon startup, then monthly.
1. From the main menu, choose "Maintenance" option and then select "Monitor" option.
The screen will display real-time values for temperature and pressure.
2. Check the ambient, meter, and filter temperature sensors of the sample by positioning
the probe of a certified transfer standard digital thermometer in close proximity to the
sampler sensors. Allow time to achieve stable readings and record the results in the field
notebook and on the STN QA/QC report form.
3. Alternatively, use the Tegam thermocouple calibrator to input -30, 0, and 45EC
settings and record the corresponding temperatures indicated by the MASS sampler.
(Allowable error is + 2 EC.) If the sampler and control check temperature readings
differ by more than + 2 EC, trouble-shoot the system and recheck. If still out of
tolerance, conduct a multipoint calibration or replace the faulty sensor.
5.4 Quarterly Temperature Control Check
Performed each calendar quarter. Follow the same steps as in Section 5.3, but use a
temperature transfer standard that is independent of the one used for the monthly checks.
Should a temperature sensor not maintain its calibration after the monthly or quarterly
checks, maintenance and/or replacement of the faulty parts must occur.
5.5 Temperature Calibration
1. Unplug the thermocouple labeled "Ambient" on the panel and connect a Tegam
temperature calibrator.
2. From the main screen select "Maintenance" option, then choose "Calibrate", and
select "Ambient" to calibrate the ambient temperature in the system.
3. When the system prompts for a low ambient temperature value (-20 EC), enter low
value on the Tegam Calibrator.
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SOP # 5300STN URG MASS 400 & 450
Rev. # 1
Date: September 30, 1999
Page 7 of 11
4. Enter value of the Tegam Calibrator into the system using numeric keypad.
5. Now the system prompts for a high ambient temperature value (40 EC). Enter high
value on the Tegam Calibrator.
6. Enter value of the Tegam Calibrator into the system using numeric keypad.
7. Change value of the Tegam Calibrator and verify this change in the display screen
(The allowable error is + 2EC.)
8. At the end of ambient temperature calibration, save the calibration by selecting "Yes"
option when the instrument prompts.
9. Repeat the procedure to calibrate the meter temperature and the filter temperature.
5.6 Monthly Pressure Control Check
Performed upon startup, then monthly.
1. Compare the ambient barometric pressure readout from the sampler display screen
with the reading from a certified transfer standard barometer.
2. If the pressure readings differ by more than +10 mm Hg, perform a multipoint
calibration of the sensor or replace the faulty sensor.
5.7 Quarterly Pressure Control Check
Performed each calendar quarter. Follow the same steps as in Section 5.6, but use a
pressure standard that is independent of the one used for the monthly checks. Should the
pressure sensor system not maintain its calibration after the monthly or quarterly checks,
maintenance, and/or replacement of the pressure transducer must occur.
5.8 Meter and Barometric Pressure Calibrations
1. Connect a pressure calibration apparatus to the port on the panel located inside of the
unit. Connect one end of a tee to an external pressure gauge by tubing. Connect the
other end of the tee to the pressure calibration port in the system by tubing. Attach a
plastic syringe to the middle tee junction by tubing.
2. From the main screen select "Maintenance" option, then choose "Calibrate", and
select "Meter Drop" to calibrate the meter pressure drop in the system.
3. When the system prompts for a low pressure value, pull the plunger from syringe until
the external pressure gauge reads approximately 600 mm Hg.
4. Clamp the tubing between the syringe and the tee to hold the pressure, and key the
exact value shown by external pressure gauge into the system.
5. When the system prompts for a high pressure value, push the plunger until the
external pressure gauge reads approximately 800 mmHg.
6. Hold the pressure, and enter the exact value shown in external pressure gauge into the
system using keypads.
-------
SOP # 5300STN URG MASS 400 & 450
Rev. # 1
Date: September 30, 1999
Page 8 of 11
7. Change the value in the external pressure gauge using the syringe and check whether
the value matches with the value shown on the screen. (The allowable error is + 5 mm
Hg.)
8. At the end of meter drop pressure calibration, save the calibration by selecting the
"Yes" option when the instrument prompts.
9. Repeat the procedure to calibrate the barometric pressure sensor.
5.9 Monthly Flow Rate Control Check
Perform flow rate control check upon startup, then monthly.
1. Use same filter pack assembly called for in monthly Leak Check Procedure
(Section 5.2).
2. Connect a flow audit adapter to the down tube. Open the adapter and connect a
certified flow transfer standard to the adapter inlet.
3. From the main menu select the "Verify Flow" option to start the flow verification
process.
4. After one minute, compare the average flow displayed on the sampler's screen with
flow indicated by the external flow meter.
5. Repeat the flow audit procedure for the other URG unit. The channels are preset at a
flow of 16.7 L/min. If the channel's flow error is greater than 2%, that channel's
flow rate control mechanism requires calibration or servicing.
6. If a dry gas meter is used for flow rate checks, the meter's calibration coefficient,
initial and final volume readings, and temperature must be entered in response to the
screen prompts in order for the sampler to compute a flow rate for comparison. Refer
to the operator's manual for details.
5.10 Quarterly Flow Rate Control Check
Performed each calendar quarter. Follow the same steps as in Section 5.9, but use a flow
rate transfer standard that is independent of the one used for the monthly checks. Should
the flowrate mechanism not maintain its calibration after the monthly or quarterly checks,
maintenance and/or replacement of the flow controller system(s) must occur.
6.0 Sampler Maintenance and Troubleshooting
1. Clean dust from the interior of the sampling cabinets. Use a damp cloth. Clean at
least monthly or more often if local conditions warrant.
2. The MASS 400 and MASS 450 employ the FRM WINS impactor system to remove
coarse particles. A periodic cleaning and maintenance schedule similar to that for FRM
samplers should be instituted.
• Every 5 sampling days. Service water collector bottle and clean or change out
the impactor well filter and oil.
• Monthly. Clean sampler inlet surfaces. Examine O-rings of WINS and replace if
needed.
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SOP # 5300STN URG MASS 400 & 450
Rev. # 1
Date: September 30, 1999
Page 9 of 11
• Quarterly. Inspect O-rings of inlet. Clean sampler downtube (denuder
downtube is cleaned and refurbished in the laboratory). Inspect and service
other O-rings, vacuum tubing, and other pneumatic and electrical connections.
Inspect and service cooling air intake filter and fan.
3. Refer to the URG MASS 400 and 450 operator's manual for further information on
electrical and pneumatic system maintenance.
7.0 References
1. Model MASS 400, Model MASS 450 Operator's Manual. URG Inc. Chapel Hill,
NC. April 17, 1998.
-------
SOP # 5300STN URG MASS 400 & 450
Rev. # 1
Date: September 30, 1999
Page 10 of 11
QA/QC Form
No PM2 5 STN QA/QC REPORT FORM
c. 1 (site retains)
c. 2 (Agency QAM)
A. CUSTODY RECORD (Name, Date) BIND):
1. Laboratory, Out 3. Site, Out
2. Site, In 4. Lab, In
B. SITE AND SAMPLER INFORMATION
1. Site AIRS Code 5. Site Name
2. Sampler S/N 6. Intended date of use
3. Sampler Type 7. Date of sampler set-up
4. Sampler POC 8. Operator's name
C. SAMPLER CHANNEL COMPONENTS
Channel Component ID Component Description
Number No.
1
1
2
11234567 MASS 400 denuder (sodium carbonate
11234567 MASS 400 Filter Pack (Teflon, Nylon filers)
11234569 MASS 450 Filter Pack (quartz)
D. START,
END, AND RETRIEVAL TIMES
Channel No. Start date Start time End date
1
2
End time
Retrieval
date
Retrieval
time
E. SAMPLER CHANNEL INFORMATION Post-Sampling)
Channel
No.
1
2
Channel
No.
1
2
Elapsed E. S. time Sample Avg.flow
sample time Flaa Volume (m3) (L/min)
Avg. BP Max. BP Min.BP -Flow
(mm Ha) (mm Ha) (mm Ha) Flaa
Avg. ambient
T(°C)
•T
Flaa
Max. ambient
T(°C)
PumpP
(mm Ha)
F. Comments
Min. ambient
T(°C)
Manifold
T(°C)
(Revised 02/1 4/01: 5200)
Figure 4-1. STN Custody and Field Data Form With Entries for the RAAS Sampler.
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SOP # 5300STN URG MASS 400 & 450
Rev. # 1
Date: September 30, 1999
Page 11 of 11
QA/QC Form No.
PM2 5 STN QA/QC REPORT FORM
c. 1 (site retains)
c. 2 (Agency QAM)
A. SITE AND SAMPLER INFORMATION
1. Site AIRS Code
2. Sampler S/N
3. Sampler Type
4. Sampler POC
5. Site Name
6. Interval: Month Quarter Special
7. Date(s) of QA/QC Checks
8. Operator's Name
B. DATE AND TIME CHECKS (Transfer Standard Name
Transfer Standard ID Number
Sample display date/time
Transfer standard date/time
Date and time agree ± 5 min?
Action taken (a)
C. LEAK CHECKS (Transfer Standard Name
Transfer Standard ID Number
J
Channel number
Manufacturer's specifications met?
Action taken and recheck results (a)
D. TEMPERATURE CHECKS (Transfer Standard Name
Transfer Standard ID Number
Sensor location
Sampler display (°C)
Transfer standard (°C)
Agreement ± 2 °C ?
Action taken and
recheck results (a)
Ambient
Filter
Dry Gas Meter
Manifold
E. PRESSURE CHECKS (Transfer Standard Name
Transfer Standard ID Number
Sensor location
Sampler display,
(mm Hg)
Transfer standard,
(mm Hg)
Agreement within
± 10 mm Hg?
Action taken and
recheck results (a)
Ambient
Manifold
F. FLOW RATE CHECKS (Transfer Standard Name
Transfer Standard ID Number
Channel number
Sampler display,
(L/min)
Transfer standard
display, (L/min)
Design flow rate,
(L/min)
Agreement within
± 10 percent? (b)
Action taken and
recheck results (a)
G. COMMENTS
(Revised 02/14/99: 5200)
(a)Fully describe actions taken in field notebook.
(b) Sampler flow rate must agree with both transfer standard and design flow rate to pass.
Figure 5-1. STN QA/QC Report Form.
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APPENDIX A-5
SOP 5400STN
PACKING INSTRUCTIONS FOR THE
SPECIATION SAMPLER MODULES
-------
SOP # 5400STN Packing Instructions
Rev. # 1
Date: January 18,2001
Page 1 of 6
STANDARD OPERATING PROCEDURES
FOR PACKING INSTRUCTION OF THE
SPECIATION SAMPLERS
Prepared by: Date:
Reviewed by: Date:
Approved by: Date:
PM2 5 Speciation Trends Network
Office of Air Quality Planning and Standards
U.S. Environmental Protection Agency
Research Triangle Park, NC 27709
-------
SOP # 5400STN Packing Instructions
Rev. # 1
Date: January 18,2001
Page 2 of 6
1.0 Purpose and ApplicabUity
This condensed standard operating procedure (SOP) outlines the procedures for packing
the modules for the speciation samplers. The URG Models 400 and 450, Andersen RASS
and Met One SASS PM2 5 speciation sampler instructions are included in this SOP.
-------
SOP # 5400STN Packing Instructions
Rev. # 1
Date: January 18,2001
Page 3 of 6
PACKAGING INSTRUCTIONS FOR ANDERSEN PM25 FILTER MODULES
1
Make sure the horizontal and vertical
dividers are arranged in the transport bin as
shown in the photo.
2
Place eight frozen FREEZ PAK®s
(sealed in bags) and three of the
polyethylene foam squares in the bin
p arti
t ion
as
ho
n.
3
Place the three Andersen sampling
modules (sealed in bags) on top of the
foam squares in the bin.
4
Place the remaining three polyethylene
foam squares on top of the three Andersen
sampling modules.
5
Place the PM 2.5 STN CUSTODY AND
FIELD DATA FORM in the resealable
plastic bag and place the bag on top of the
bin contents.
6
Place the clear plastic lid on the bin. (See
separate instructions for preparing the
cooler for shipment.)
-------
SOP # 5400STN Packing Instructions
Rev. # 1
Date: January 18,2001
Page 4 of 6
PACKAGING INSTRUCTIONS FOR URG PM2 5 SAMPLING MODULES
1
Make sure the horizontal and vertical dividers are
arranged in the transport bin as shown below.
2
Place eight frozen FREEZ PAK®s (in sealed bags)
and two of the polyethylene foam squares in the bin
partitions as shown.
3
Place the two URG sampling modules (in sealed
bags) on top of the polyethylene foam squares in
the bin.
4
Place the remaining two polyethylene foam squares
on top of the two URG sampling modules.
5
Place the PM 2.5 STN CUSTODY AND FIELD DATA
FORM in the resealable plastic bag and place the
bag on top of the bin contents.
6
Place the clear plastic lid on the bin. (See separate
instructions for preparing the cooler for shipment.)
-------
SOP # 5400STN Packing Instructions
Rev. # 1
Date: January 18,2001
Page 5 of 6
PACKAGING INSTRUCTIONS FOR MET ONE PM2 5 SAMPLING MODULES
1
Make sure the horizontal and vertical dividers are
arranged in the transport bin as shown in the photo.
2
Place eight upright frozen FREEZ PAK®s (in sealed
bags) and three of the polyethylene foam squares in
the bin partitions as shown.
3
Place the three Met One sampling modules (in sealed
bags) on top of the polyethylene foam squares in
the bin.
4
Place the remaining three polyethylene foam
squares on top of the three Met One sampling
modules.
5
Place the PM 2.5 STN CUSTODY AND FIELD DATA
FORM in the resealable plastic bag and place the
bag on top of the bin contents.
6
Place the clear plastic lid on the bin. (See separate
instructions for preparing the cooler for shipment.)
-------
SOP # 5400STN Packing Instructions
Rev. # 1
Date: January 18,2001
Page 6 of 6
PACKAGING INSTRUCTIONS FOR IGLOO ULTRACOLD™ 50 COOLERS
1
Place one of the custom-cut large rectangular blocks of
polyethylene foam in the bottom of the Igloo
UltraCold™ 50 Cooler.
2
Place the two smaller rectangular blocks of
polyethylene foam at the ends of the cooler as shown.
3
Place the transport bin containing the sampling
modules in the cooler between the polyethylene foam
blocks.
4
Place twelve frozen FREEZ PAK®s on top of the bin in
two rows of six each. Make sure that the packs are
standing upright. Several operators have stated that
the packs may leak if they placed on their sides. It is
strongly recommended that the packs be placed
upright.
5
Place the remaining large block of polyethylene foam
on top of the bin in the cooler.
6
Close the cooler and place the preprinted return
FedEx airbill on top as shown.
-------
APPENDIX A-6
CY-2001 l-IN-3 DAY SAMPLING AND
ALTERNATE SCHEDULE FOR THE
SPECIATION TRENDS NETWORK
-------
CY-2001 STN Schedule
Rev. # 1
Date: December 20, 2000
Page 1 of4
CY-2001 l-IN-3 DAY SAMPLING AND
ALTERNATE SCHEDULE FOR THE
SPECIATION TRENDS NETWORK
Prepared by: Date:
Reviewed by: Date:
Approved by: Date:
PM2 5 Speciation Trends Network
Office of Air Quality Planning and Standards
U.S. Environmental Protection Agency
Research Triangle Park, NC 27709
-------
CY-2001 STN Schedule
Rev. # 1
Date: December 20, 2000
Page 2 of4
1.0 Purpose and ApplicabUity
This appendix is designed to allow the operators, RTI lab personnel and EPA to verify and
plan the deployment the speciation modules within the Speciation Trends Network for
Calendar Year 2001. Please note there are two schedules. The first is the normal schedule
that will be operated by those agencies that will be able to deploy the sample modules
during the weekends. The second schedule is designed to allow the agencies that will not
be able to deploy the samples during the weekend. The difference is that alternating
Mondays and Fridays will be missed.
Note: It is important to note that keeping to the schedule is extremely important to the
laboratory operations. If the modules are not placed in the sampler due to using the
Alternate Schedule, the unexposed modules must be sent back to contractor laboratory
when they are scheduled to be returned. This insures that the State or Local agency has
enough modules in the system.
-------
CY-2001 STN Schedule
Rev. # 1
Date: December 20, 2000
Page 3 of4
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-------
CY-2001 STN Schedule
Rev. # 1
Date: December 20, 2000
Page 4 of4
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-------
APPENDIX A-7
TECHNICAL GUIDANCE DOCUMENT
UPDATES
-------
Appendix A-7
Rev. # 1
Date: December 20,2000
Page 1 of 1
1.0 Purpose and ApplicabUity
This appendix is designed to be a place holder for Technical Guidance Document Updates
that will be forward from time to time. As more information is gathered concerning the
QA and QC ofspeciation sampler, this information will be disseminated from OAQPS to
the State and Local Agencies through the DOPOs. This appendix is where these updates
are stored.
-------
TECHNICAL REPORT DATA
(Please read Instructions on reverse before completing)
1. REPORT NO.
EPA-354/RO1-001
3. RECIPIENT'S ACCESSION NO.
4. TITLE AND SUBTITLE
Quality Assurance Guidance Document, Quality Assurance
Project Plan: PM2.5 Speciation Trends Network Field Sampling
5. REPORT DATE
01/01
6. PERFORMING ORGANIZATION CODE
7. AUTHOR(S)
Dennis Mikel, James Flanagan, David Musick, James Homalya
8. PERFORMING ORGANIZATION REPORT NO.
9. PERFORMING ORGANIZATION NAME AND ADDRESS
U.S. Environmental Protection Agency
Office of Air Quality Planning and Standards
Research Triangle Park, NC 27711
10. PROGRAM ELEMENT NO.
11. CONTRACT/GRANT NO.
12. SPONSORING AGENCY NAME AND ADDRESS
Director
Office of Air Quality Planning and Standards
Office of Air and Radiation
U.S. Environmental Protection Agency
Research Triangle Park, NC 27711
13. TYPE OF REPORT AND PERIOD COVERED
14. SPONSORING AGENCY CODE
EPA/200/04
15. SUPPLEMENTARY NOTES
16. ABSTRACT
The Quality Guidance Document is the Quality Assurance Project Plan that outlines the field operations for the
PM2.5 Speciation Trends Network. The guidance document gives details on how to
set-up, operate, and perform all quality control and assurance duties that are required to provide precise, accurate
and representative data for this program. This guidance document also has six appendices. The first four are
Standard Operating Procedures for Speciation samplers. The fifth appendix provides details on how to load filter
modules into coolers before they are shipped to the central laboratory. Appendix A-6 illustrates the 1 in 3 day
schedule for CY 2001. In addition, Appendix A-6 provides an alternate schedule for agencies that cannot operate
the samplers on weekends.
17.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
b. IDENTIFIERS/OPEN ENDED TERMS
c. COSATI Field/Group
Air Quality Monitoring
Quality Assurance
Air Pollution control
18. DISTRIBUTION STATEMENT
Release Unlimited
19. SECURITY CLASS (Report)
Unclassified
21. NO. OF PAGES
20. SECURITY CLASS (Page)
Unclassified
22. PRICE
EPA Form 2220-1 (Rev. 4-77) PREVIOUS EDITION IS OBSOLETE
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