May 1980
INHALABLE PARTICULATE NETWORK
OPERATIONS AND QUALITY ASSURANCE MANUAL
U.S. Environmental Protection Agency
Office of Research and Development
Environmental Monitoring Systems Laboratory
Research Triangle Park, North Carolina 27711
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May 1980
INHALABLE PART1CULATE NETWORK
OPERATIONS AND QUALITY ASSURANCE MANUAL
U.S. Environmental Protection Agency
Office of Research and Development
Environmental Monitoring Systems Laboratory
Research Triangle Park, North Carolina 27711
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CONTENTS
Section
INTRODUCTION 1
1.1 BACKGROUND 1
1.2 PURPOSE 1
1.3 SCOPE 2
1.4 DOCUMENTATION 3
OPERATIONS AND MAINTENANCE 1
2.1 INTRODUCTION 1
2.1.1 Inhalable Particulate
Network 1
2.1.2 Purpose 1
2.1.3 Suspended Partic-
ulates 2
2.1.4 Glossary of Terms .... 4
2.2 OPERATOR'S SUMMARY 1
2.2.1 Operation of the IP
Network Samplers--, .... 1
2.2.2 Field Data Measure-
ments 10
2.2.3 Recording the Field
Data 11
2.2.4 Sample Validation 18
2.2.5 Operator's Field
Calibration Check
Procedures 19
2.2.6 Operator's (Five-
Point) Field Cali-
bration of High
Volume Samplers 26
2.2.7 General Trouble-
shooting 28
2.3 OPERATING PROCEDURE FOR
CONVENTIONAL HIGH VOLUME
SAMPLER
2.
2.
2.3.3
Introduction . . .
Description of the
Volume Sampler . .
Operation of the
Conventional High
Volume Sampler . .
High
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CONTENTS (continued)
Section
2.4
2.5
2.3.4
2.3.7
Recording the Field
Data .
Sample Validation .
Operator's Field
Calibration Check
Procedures
Five-Point Calibra-
tion of the Conven-
tional High Volume
Sampler
OPERATING PROCEDURE FOR
HIGH VOLUME SAMPLER WITH
SIZE SELECTION INLET . .
2.4.3
2.4.4
2.4.7
Introduction
Description of the High
Volume Sampler with
Inlet Fractionator . . .
Operation of High
Volume Sampler with
Inlet Fractionator .
Recording the Field
Data
Sample Validation . . .
Operator's Field
Calibration Check
Procedures
Five-Point Calibra-
tion of the SSI High
Volume Sampler
OPERATING PROCEDURE FOR THE
BECKMAN SAMPLAIR DICHOTOMOUS
SAMPLER
2.5.1 Introduction
2.5.2 Description of the
Beckman SAMPLAIR
Dichotomous Sampler .
2.5.3 Operation of Beckman
SAMPLAIR
2.5.4 Recording the Field
Data
2.5.5 Sample Validation . .
2.5.6 Operator's Field
Calibration Check
Procedures
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IV
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CONTENTS (continued)
Section
3.1
3.2
2.6 OPERATING PROCEDURE FOR
THE SIERRA 244 AND 244E
DICHOTOMOUS SAMPLERS . . .
2.6.1 Introduction . .
2.6.2 Description of the
Sierra Series 244
Sampler and 244E
Dichotomous Samplers
2.6.3 Operation of Sierra
Model 244 and 244E
Dichotomous Samplers
2.6.4 Recording the Field
Data
2.6.5 Sample Validation .
2.6.6 Operator1s Field
Calibration Check
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3.2.2 Procedures for Selecting
Site Location ....
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Procedures
2.6.7 Routine Maintenance . . .
SITING
INTRODUCTION
3.1.1 Inhalable Particulate
Network . . ."
3.1.2 Purpose of the IP Network
Siting Document ....
3.1.3 Siting Criteria for the
IP Network
SELECTING SITE LOCATIONS ....
3.2.1 General
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3.3 SPECIAL CONSIDERATIONS IN SITE
SELECTION
3.3.1 Probe Siting
3.3.2 Physical and Electrical
Site Requirements for
3.4 REFERENCES
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CONTENTS (continued)
Section
ANALYTICAL PROCEDURES
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4.1 IP NETWORK HIGH VOLUME FILTER
HANDLING PROCEDURES
4.1.1
High Volume Filter Tare
Weighing Procedure . .
4.1.2 High Volume Filter Final
Weighing Procedure . .
4.1.3 Internal Quality
Control
4.1.4 References
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4.2 IP NETWORK DICHOTOMOUS FILTER
HANDLING PROCEDURES
4.2.1
4.2.2
4.2.3
4.2.4
Dichotomous Filter Tare
Weighing Procedure ... 1
Dichotomous Filter Final
Weighing Procedure . . 2
Internal Quality
Control 6
References 6
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4.3 (TENTATIVE) DICHOTOMOUS FILTER
EXTRACTION PROCEDURE FOR
SULFATES AND NITRATES
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4.4 PROCEDURE FOR THE ANALYSIS OF
SULFATES IN ATMOSPHERIC
PARTICULATES COLLECTED BY HIGH
VOLUME SAMPLERS (AUTO-TECHNICON
II PROCEDURE)
4.4.1 Principle and
Applicability
4.4.2 Range and Discrimination
Limit
4.4.3 Interferences
4.4.4 Precision and Accuracy .
4.4.5 Apparatus
4.4.6 Reagents
4.4.7 Analytical Procedure . .
4.4.8 Calculations .
4.4.9 Quality Control
4.4.10 References
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CONTENTS (continued)
Section
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4.5 PROCEDURE FOR THE ANALYSIS OF
NITRATES IN ATMOSPHERIC
PARTICULATES COLLECTED BY
HIGH VOLUME SAMPLERS AUTO-
TECHNICON II PROCEDURE) ....
4.5.1 Principle and Applic-
ability
4.5.2 Range and Discrimination
Limit
4.5.3 Interferences
4.5.4 Precision and Accuracy .
4.5.5 Apparatus
4.5.6 Reagents
4.5.7 Analytical Procedure . .
4.5.8 Calculations
4.5.9 Quality Control ....
4.5.10 References
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4.6 PROCEDURE FOR THE ANALYSIS OF
SULFATES IN ATMOSPHERIC PARTIC-
ULATES (DIONEX METHOD) . . . .
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4.7 PROCEDURE FOR THE ANALYSIS OF
LEAD IN ATMOSPHERIC PARTICU-
LATES ( METHOD) .
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4.8 PROCEDURE FOR THE ELEMENTAL
ANALYSIS OF ATMOSPHERIC PARTIC-
ULATES (X-RAY FLUORESCENCE
METHOD)
QUALITY ASSURANCE.
5.1
5.2
5.3
5.4
INTRODUCTION.
ORGANIZATION.
QUALITY ASSURANCE POLICY AND
OBJECTIVES
5.3.1 Quality Assurance
Policy
5.3.2 Quality Assurance Pro-
gram Objectives. . . .
DOCUMENTATION AND DOCUMENT
CONTROL
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CONTENTS (continued)
Section
5.4.1 Document Control 6
5.4.2 Reports 7
5.4.3 Internal Documentation . . 7
5.5 TRAINING • • 7
5.6 PREVENTIVE MAINTENANCE 8
5.7 SAMPLE COLLECTION AND
ANALYSIS 8
5.8 CALIBRATION 9
5.8.1 Balance Calibration. ... 9
5.8.2 Sampler Flow Rate
Calibration 9
5.8.3 Analytical Instrument
Calibration 42
5.9 CORRECTIVE ACTION 45
5.10 IP NETWORK AUDIT PROGRAM 45
5.11 DATA VALIDATION AND STATISTICAL
ANALYSIS OF DATA 46
5.12 DATA QUALITY ASSESSMENT: PRE-
CISION AND ACCURACY 46
5.12.1 Precision and Accuracy
of Sampler Performance . . 47
5.13 ASSESSMENT OF PRECISION AND
ACCURACY OF PROCEDURES USED
FOR ANALYSIS OF IP NETWORK
FILTERS 54
5.13.1 Mass Determination—Pre-
cision and Accuracy. ... 54
5.13.2 Chemical and Elemental
Analysis—Precision and
Accuracy 55
5.14 EVALUATION AND VALIDATION OF IP
METHODOLOGY 60
5.14.1 Validation of Dichotomous
Samplers 60
5.14.2 Flow Measurement and
Field Audit Device .... 61
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CONTENTS (continued)
Section Page Revision Date
5.14.3 Evaluation of Dichotomous
Samplers 61 0 5/7/80
5.14.4 Wind Tunnel Test of the
Inlet 61 0 5/7/80
6 DATA VALIDATION 1 0 5/7/80
6.1 INTRODUCTION 1 0 5/7/80
6.1.1 Definition 1 0 5/7/80
6.1.2 Purpose 1 0 5/7/80
6.1.3 Scope 2 0 5/7/80
6.2 IP NETWORK FIELD AND
LABORATORY VALIDA-
TION PROCEDURES 2 0 5/7/80
6.2.1 Filter Processing 2 0 5/7/80
6.2.2 Analysis 6 0 5/7/80
6.3 IP NETWORK DATA
PROCESSING AND
VALIDATION PROCEDURES 7 0 5/7/80
6.3.1 Data Validation
Criteria . . 7 0 5/7/80
6.3.2 Data Processing
and Reporting 8 0 5/7/80
6.4 REFERENCES 11 0 5/7/80
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FIGURES
SECTION 2.1
Number
2.1.1 Inlet for a typical dichotomous sampler ........... 5
2.1.2 Operation of dichotomous sampler using virtual
impaction ......................... 6
SECTION 2.2
2.2.1 Beckman dichotomous sampler modified for manual
operation ........... . ............. 5
2.2.2 The bonded Beckman dichotomous filter magazine ........ 6
2.2.3 IP Network data sheet ..................... "12
2.2.4 IP Network data sheet .................... 13
2.2.5 IP Network data sheet .................... 14
2.2.6 IP Network data sheet ............. • ....... 15
2.2.7 IP data card — completed for conventional high volume
sampler ......................... 17
2.2.8 Tork master timer ...................... 21
SECTION 2.3
2.3.1 TSP high volume sampler used in IP Network .......... 2
2.3.2 Dickson chart recordings—typical examples .......... 4
2.3.3 IP Network field -data sheet for TSP high volume sampler ... 7
2.3.4 Sample IP data cards — completed for TSP high volume
samplers .......................... 9
2.3.5 Tork master timer ...................... 13
2.3.6 IP Network field calibration check assembly for TSP
high volume samplers .................... 15
2.3.7 Sample high volume flow orifice calibration curve ...... 16
2.3.8 Sample interpolation table for high volume flow orifice
calibration ........................ 17
2.3.9 Sample TSP high volume sampler flow rate calibration curve. . 18
2.3.10 Sample TSP high volume sampler flow rate calibration--
interpolation table .......... . ......... 19
2.3.11 IP Network Flow Check Data Sheet ............... 20
2.3.12 IP Network calibration assembly for TSP high volume
sampler .......................... 22
2.3.13 IP Network high volume field calibration data form ...... 24
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FIGURES (continued)
Number Page
SECTION 2.4
2.4.1 SSI high volume sampler used in the IP Network 2
2.4.2 Filter holder and inlet fractionator for SSI high
volume sampler 3
2.4.3 Dickson chart recordings—typical examples 5
2.4.4 Schematic of filter holder for SSI high volume samplers ... 7
2.4.5 IP Network field data sheet for SSI high volume samplers. . . 9
2.4.6 Sample data cards—completed for SSI high volume sampler. . . 10
2.4.7 Tork master timer 15
2.4.8 IP Network field calibration check assembly for SSI
high volume samplers 16
2.4.9 Sample high volume flow orifice calibration curve 17
2.4.10 Sample interpolation table for higji volume flow orifice
calibration 18
2.4.11 Sample SSI high volume sampler flow rate calibration
curve - . . "20
2.4.12 Sample SSI high volume sampler flow rate calibration
interpolation table 21
2.4.13 IP Network Flow Check Data Sheet 22
2.4.14 IP Network calibration assembly for SSI high volume
samplers 24
2.4.15 IP Network high volume field calibration data form 25
SECTION 2.5
2.5.1 Beckman-SAMP LAIR dichotomous sampler used in IP Network ... 2
2.5.2 Sampler changer subsystem for the Beckman SAMPLAIR 5
2.5.3 Range of temperature control in Beckman SAMPLAIR. . . . . 8
2.5.4 Wiring connections for temperature controller and
thermal switches 9
2.5.5 Simplified block diagram of Beckman SAMPLAIR electronics
system 11
2.5.6 Detailed diagram of electronics system in Beckman SAMPLAIR. 12
2.5.7 Internal controls in the Beckman SAMPLAIR 14
2.5.8 Beckman dichotomous sampler modified for manual operation . . 16
2.5.9 The bonded Beckman dichotomous filter magazine 18
2.5.10 Typical printout from the Beckman SAMPLAIR 23
2.5.11 Printout showing interrupted timing in the Beckman
SAMPLAIR 25
2.5.12 IP Network data sheet 27
2.5.13 Sample IP data cards — completed for Beckman dichotomous
sampler 28
2.5.14 Tork master timer 34
2.5.15 Calibration orifice assembly for IP Network dichotomous
samplers 35
2.5.16 Sample calibration curve for Beckman "fine" rotameter .... 36
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FIGURES (continued)
Number
2.5.17 Sample interpolation table for Beckman "fine" rotameter
calibration 37
2.5.18 Sample calibration curve for Beckman "coarse" rotameter ... 38
2.5.19 Sample interpolation table for Beckman "coarse" rotameter
calibration 39
2.5.20 Sample dichotomous flow orifice calibration curve 40
2.5.21 Sample interpolation table for dichotomous flow orifice
calibration 41
2.5.22 IP Network Flow Check Data Sheet 42
SECTION 2.6
2.6.1 Manual dichotomous sampler used in IP Network—Sierra
Model 244 and 244E 2
2.6.2 The Sierra Models 244/244E virtual impactor, principle
of operation 5
2.6.3 Control module for Sierra Model 244 d>chotomous sampler .... ~ 6
2.6.4 Control module for Sierra Model 244E dichotomous sampler. . . 7
2.6.5 Sample "total" rotameter calibration curve for the
Sierra dichotomous sampler 11
2.6.6 Sample interpolation table for Sierra "total" rotameter
calibration 12
2.6.7 Sample "coarse" rotameter calibration curve for the Sierra
dichotomous sampler 13
2.6.8 Sample interpolation table for Sierra "coarse" rotameter
calibration ,. "." 14
2.6.9 IP Network field data sheet for Sierra dichotomous samplers . 18'
2.6.10 Sample IP data cards completed for Sierra dichotomous
sampler 19
2.6.11 Tork master timer 24
2.6.12 IP Network dichotomous sampler calibration check orifice
assembly 26
2.6.13 Sample dichotomous flow orifice calibration curve 27
2.6.14 Sample interpolation table for dichotomous flow orifice
calibration 28
2.6.15 IP Network Flow Check Data Sheet 29
2.6.16 Disassembled sampling module of Sierra dichotomous
sampler (Model 244 or 244E) 32
SECTION 3
3.1 The influence of building air flow on pollution
dispersion 10
3.2 Schematic representation of the air flow around an
obstacle 11
3.3 Acceptable zone for siting IP monitors 13
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FIGURES (continued)
Number Page
**..
SECTION 4.1
4.1.1 Sample coding form—high volume filter tare weights . . 2
4.1.2 Sample coding form—high volume filter final weights 4
SECTION 4.2
4.2.1 Sample coding form--dichotomous filter tare weights ... 3
4.2.2 Sample coding ,form--dichotomous filter final weights. ... 5
SECTION 4.4
4.4.1 Schematic diagram of the automated Technicon II
analyzer. ... . . . . 3
4.4.2 IP Network data reporting form—inorganic analysis 14
SECTION 4.5
4.5.1 Schematic diagram of the automated Technicon II
analyzer. . . . . . . 4
4.5.2 IP Network data reporting form—inorganic analyses. . . 12
SECTION 5
5.1 Organizational structure of EMSL/RTP . 3
5.2 Organizational structure of the" IP Network 4
5.3 Block diagram of transfer standard calibration setup. ... 13
5.4 Sample transfer standard calibration form 14
5.5 Sample interpolation table for a mass flowmeter . .... 16
5.6 Sample mass flowmeter calibration curve . . . . 17
5.7 Schematic of Beckman laboratory calibration setup using
a mass flowmeter as a transfer standard . . 18
5.8 Sample laboratory calibration sheet . 20
5.9 Sample dichotomous flow orifice calibration curve ... 23
5.10 Sample interpolation table for dichotomous flow orifice
calibration . 25
5.11 Sample calibration curve for Beckman "fine" rotameter ... 26
5.12 Sample interpolation table for Beckman "fine" rotameter
calibration 27
5.13 Sample calibration curve for Beckman "coarse" rotameter ... 31
5.14 Sample interpolation table for Beckman "coarse" rotameter
calibration 32
5.15 Schematic of Sierra laboratory calibration setup using a
mass flowmeter as the transfer standard 33
5.16 Sample calibration curve for the Sierra "total" rotameter . 38
5.17 Sample interpolation table for the Sierra "total" rota-
meter calibration . 39
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FIGURES (continued)
Number Page
5.18 Sample calibration curve for Sierra "coarse" rotameter. ... 43
5.19 Sample interpolation table for Sierra "coarse" rotameter
calibration 44
5.20 Audit data sheet for dichotomous samplers 50
5.21 Audit data sheet for conventional high volume samplers. ... 52
5.22 Audit data sheet for SSI high volume samplers 53
SECTION 6
6.1 Operations process chart for the IP Network 3
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TABLES
Number
SECTION 2.5
2.5.1 Beckman SAMPLAIR Specifications 3
2.5.2 Beckman SAMPLAIR Front Panel Controls, Indicators, and
Circuit Breakers 13
SECTION 2.6
2.6.1 Specifications for the Sierra Model 244 Dichotomous
Sampler 3
SECTION 3
3.1 Space and Electrical Requirements for IP Network Samplers . 14
SECTION 5
5.1 IP Network—Key Personnel 5
5.2 Analytical Range of Blind Audit Samples 56
5.3 Analytical Range of Blind Audit Samples 57
5.4 Distribution of Blind Audit Samples Across Analytical
Range 58
SECTION 6
6.1 IP Data Card Validation CriterTa 9
6.2 IP'Network Validation Criteria for Mass Data 10
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CONTENTS
Section Paqe Revision Date
INTRODUCTION 1 0 5/7/80
i.l BACKGROUND 1 0 5/7/80
1.2 PURPOSE 1 0 5/7/80
1.3 SCOPE 2 0 5/7/80
1.4 DOCUMENTATION 3 0 5/7/80
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SECTION 1
INTRODUCTION
1.1 BACKGROUND
Research on the health effects of suspended participates in ambient air
has focused increasingly on those particles that can be inhaled into the res-
piratory system, i.e., particles of aerodynamic diameter less than 10 to
15 |jm. It is now generally recognized that, except for toxic materials, it
is this fraction of inhalable particulates- (IP) that is of major significance
in health effects. Furthermore, these effects are primarily chronic and re-
quire long-term monitoring of exposures for adequate assessment.
With this awareness has come a growing concern that the current total
suspended particulate (TSP) ambient air standard is inappropriate in relation
to health effects. As a result of this concern, the 1977 Clean Air Act
Amendments were enacted, requiring the Environmental Protection Agency (EPA)
to reassess its position on the TSP standard by December 31, 1980. The need
for reassessment was further reinforced by a 1978 report from EPA's Office
of Air Quality Planning and Standards indicating that more than 400 areas in
the United States were not meeting the TSP standard. This report concluded
that nonattainment was due largely to reentrainment of fugitive dust in the
conventional high volume samplers used for TSP monitoring. Because this
fugitive dust contributes disproportionately to the larger particle size
(>15 urn) fraction of the TSP and therefore does not constitute a recognized
health hazard, the need to reassess the existing TSP standard and to consider
an alternative IP ambient air standard was further emphasized.
1.2 PURPOSE
To meet the Clean Air Act Amendment requirement of a reappraisal of the
TSP standard by 1981 and to obtain the necessary data on which to base a pro-
posed standard revision, EPA's Environmental Monitoring Systems Laboratory
at Research Triangle Park,. NC (EPA/EMSL-RTP), has designed and is implement-
ing a nationwide monitoring network for inhalable particulates, with primary
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emphasis on objectives relating to health effects and control strategy plan-
ning. Specific goals of the I? Network are to:
1. Provide a nationwide data base on IP and on IP/TSP ratios.
2 Further refine the IP data base into "fine" (<2.5 urn) and "coarse"
(2.5 to 15 um) fractions through the use of dichotomous samplers
in the Network.
3 Identify localized source influences through determination of mass
ratios and their spatial and temporal distribution patterns, and
through subsequent chemical and elemental sample analyses.
4. Relate, where possible, Network IP measurements to those made by
other aerosal samplers, such as the British _Smoke Shade Sampler,
used in previous important health effects studies.
1.3 SCOPE
A detailed overview of the IP Network scope and design is given in
Appendix A of this document. In brief, the IP Network design is based upon
a 4-year sampling plan, which is scheduled to run from 1978 to 1982.
Because IP samplers and their associated technology are at this time
essentially state-of-the-art, an initial two-phase pilot study was conducted
to: (1) evaluate the precision and reliability of available IP samplers,
both dichotomous and modified high volume with a 15 urn size-selective inlet
(SSI); and (2) obtain a,more extensive intercomparison of all sampler types
(TSP and IP) under a wide variety of aerosol and meteorological conditions.
The full scale IP Network design evolved from the initial pilot study
sites. Network implementation and management are under the direction of the
EPA/EMSL-RTP. All Network maintenance, calibrations, and quality assurance
are directed by EMSL. A combination of EPA and contractor personnel is used
to support Network operations. A list of persons responsible for key areas
of the Network who can be contacted for further information is given in Sec-
tion 5.1 of this manual.
Approximately 100 IP sites were scheduled to be set up in 1979 (65 are
currently on-line), with an additional 100 each in 1980 and 1981, for a total
of 300 by 1982. Most of the current IP sites are located at existing or pro-
posed NAMS/SLAMS high volume TSP sampling sites. However, specific siting
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criteria for IP sampling are being developed and will be used when available.
All sites are scheduled to contain at least one high volume TSP sampler
and one dichotomous IP sampler. Additional sites will also be equipped with
modified (SSI) high volume samplers. The samples from the IP Network studies
are collected on either glass fiber (high volume) or Teflon membrane (dichot-
omous) filters.
All samplers and equipment are supplied by EPA; samplers are routinely
operated by EPA-trained state and local agency personnel. The frequency of
operation for most of the samplers in the IP Network is every sixth day.
Samples are returned to EPA/RTP for weighing and analysis by an EPA con-
tractor. Mass concentrations are determined on all samples. Chemical analy-
sis for sulfates (SO^), nitrates (N03), and lead (Pb), and elemental analysis
by X-ray fluorescence are performed on a designated portion (normally 25 per-
cent) of all samples.
Data processing and reporting are the responsibility of EPA/EMSl-RTP-
A Network goal is to make validated mass data available to the operating
agency within 30 to 45 days, and analytical data available within 75 to 90
days.
In order to assure uniform data quality, a comprehensive quality assur-
ance (QA) plan has been prepared and integrated into the overall IP Network
design as detailed in Section 5.
1.4 DOCUMENTATION
This manual is primarily a result of QA efforts to document all Network
operational and quality control procedures. It includes both overviews and
detailed self-contained subsections that may be removed and used as field or
laboratory operating procedures. Thus, it is deliberately redundant in those
sections that may be used as operating manuals (e.g., data recording proce-
dures are included in each section for sampler operation). It also is de-
signed to provide the "who/what/when/where" details that are critical in the
operation of a measurement system of this magnitude.
Summary information is presented for sampler operation (Section 2.2),
filter and data flow (Section 6), and quality assurance checks (Section 5).
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This information is intended to be of use to managers in conducting total
system reviews of Network functions, and to operating personnel in clarify-
ing their specific roles and responsibilities in the IP Network.
Detailed information is also presented for siting procedures (Sec-
tion 3); sampler operation, maintenance, and field calibration checks (Sec-
tion 2); audit procedures and sampler laboratory (multipoint) calibration
(Section 5); filter weighing and analysis (Section 4); and data processing
and validation (Section 6). These sections are designed to be used as work-
ing documents by personnel performing these specific functions. They also
serve to document details of sampling and analysis procedures for users of
IP-generated data.
This manual is designed under a system of document control so that all
revisions may be readily documented and incorporated to ensure that the
manual reflects current Network plans and procedures. A distribution record
is maintained, and all additions, corrections, and/or'deletions are automa-
tically sent to all users of this manual.
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CONTENTS
Section
OPERATIONS AND MAINTENANCE
2.1
2.2
-
2.3
INTRODUCTION
2.1.1 Inhalable Particulate
Network
2.1.2 Purpose
2.1.3 Suspended Partic-
ulates
2.1.4 Glossary of Terms ....
OPERATOR'S SUMMARY
2.2. 1 Operation of the IP
Network Samplers
2.2.2 Field Data Measure-
ments
2.2.3 Recording the Field
Data
2.2.4 Sample Validation ....
2.2.5- Operator's Field
Calibration Check-
Procedures
2.2.6 Operator's (Five-
Point) Field Cali-
bration of High
Volume Samplers
2.2.7 General Trouble-
shooting
OPERATING PROCEDURE FOR
CONVENTIONAL HIGH VOLUME
SAMPLER
2.3.1 Introduction
2.3.2 Description of the High
Volume Sampler
2.3.3 Operation of the
Conventional High
Volume Sampler
2.3.4 Recording the Field
Data
2.3.5 Sample Validation ....
2.3.6 Operator's Field
Calibration Check
Procedures
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CONTENTS (continued)
Section
2.3.7
Five-Point Calibra-
tion of the Conven-
tional High Volume
Sampler
Page
"21
Revision
2.4 OPERATING PROCEDURE FOR
HIGH VOLUME SAMPLER WITH
SIZE SELECTION INLET 1
2.4.1 Introduction .......... 1
2.4.2 Description of the High
Volume Sampler with
Inlet Fractionator .... 1
2.4.3 Operation of High
Volume Sampler with
Inlet Fractionator .... 4
2.4.4 Recording the Field
Data 8
2.4.5 Sample Validation .... 12
2.4.6 Operator's Field
Calibration Check
Procedures . 13
2.4.7 Five-Point Calibra-
tion of the SSI High
Volume Sampler 23
2.5 OPERATING PROCEDURE FOR THE
BECKMAN SAMPLAIR DICHOTOMOUS
SAMPLER 1
2.5.1 Introduction 1
2.5.2 Description of the
Beckman SAMPLAIR
Dichotomous Sampler ... 1
2.5.3 Operation of Beckman
SAMPLAIR 10
2.5.4 Recording the Field
Data ...'.. 26
2.5.5 Sample Validation .... 30
2.5:"6 Operator's Field
Calibration Check
Procedures 32
2.6 OPERATING PROCEDURE FOR
THE SIERRA 244 AND 244E
DICHOTOMOUS SAMPLERS 1
2.6.1 Introduction 1
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CONTENTS (continued)
Section
Revision
2.6.2 Description of the
Sierra Series 244
Sampler and 244E
Dichotomous Samplers
2.6.3 Operation of Sierra
Model 244 and 244E
Dichotomous Samplers
2.6.4 Recording the Field
Data
2.6.5 Sample Validation .
2.6.6 Operator's Field
Calibration Check
Procedures
2.6.7 Routine Maintenance
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SECTION 2
OPERATIONS AND MAINTENANCE
2.1 INTRODUCTION
2.1.1 Inhalable Particulate Network
The Clean Air Act Amendments require the Environmental Protection Agencyr
(EPA) to reassess its position on the existing participate standard by Decem-
ber 31, 1980. The existing participate standard is based on a mass'concentra-
tion of total suspended particulate matter without regard to size. However,
it is generally recognized that the particles that have significant health ef-
fects are those that can be inhaled into jthe .respiratory system. These "ip-
halable" particles are less than 15 urn, aerodynamic diameter. Hence, EPA.has
established an Inhalable Particulate (IP) Network to develop a nationwide data
base on IP concentrations and on the ratio, of inhalable to total suspended-
particulates (TSP). The IP Network uses conventional high volume samplers for
measuring total suspended particulates and both SSI high volume and dichoto-
mous samplers capable of sampling primarily inhalable particulates.
2.1.2 Purpose
This document describes the operation and maintenance of-the four types
of samplers most generally used in the IP Network. Two of these samplers are
dichotomous samplers manufactured by Beckman, and Sierra, which, in addition
to sampling inhalable particulates, further divide the "sample into a coarse
fraction (2.5 to 15 urn, aerodynamic diameter) and a fine fraction (<2.5 urn,
aerodynamic diameter). The remaining two are high volume samplers: one is
conventional and the other modified. The modified high volume sampler col-
lects primarily inhalable particles but does not further subdivide the sample
into coarse and fine fractions. Section 2.2 briefly summarizes the sampler
operating procedures used in the IP Network. This section is designed for the
operator who already has some knowledge of the samplers and practices in use
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in the IP Network. Sections 2.3 through 2.6 discuss in detail each of the
samplers. These sections will be used as field operation manuals, and include
detailed sampler descriptions as well as complete, current information on pro-
cedures for sampler operation, recording field data, sample validation, field
calibration checks, and maintenance.
i
The remainder of this introductory section provides the operator with a
basic understanding of particle sampling and sizing.
2.1.3 Suspended Particulates
2.1.3.1 General--
In addition to gaseous constituents, the atmosphere contains a wide as-
sortment of solid and liquid particles that remain suspended for varying peri-
ods of time. From a practical standpoint, suspended particles may range in
size from a few tenths of a micrometer [1 micrometer = 10 m] to a hundred
micrometers. However, even a fine particle, approximately 1pm in diameter,
is still hundreds of times larger than a gas molecule. Because suspended par-
ticulates are larger and heavier than gas molecules, they behave differently.
This allows them to be separated from the gaseous medium. Separation of par-
ticles from the air occurs aerodynamically not only in particulate sampling
instruments but also in the human lung.
2.1.3.2 Sampling Suspended Particulates--
The main reason for sampling particulate, matter suspended in the atmos-
phere is to determine the mass of particulate per volume of air (mass concen-
tration). The following procedure is typical of the sampling protocol used to
determine mass concentrations with either dichotomous or high volume samplers.
The sampler is run for a fixed period of time, typically 24 hours. If the
flow rate is constant over this period, the volume of air sampled is calcu-
lated by multiplying the flow rate by the duration of the sampling period.
The exposed filter is weighed, and the final weight is compared with the in-
itial filter weight to determine the mass of the collected material. Dividing
the weight of the collected material by the volume of air sampled gives an av-
erage mass concentration of the collected material in the sampled air.
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Errors in the mass concentration figure can be associated with either the
sample weight or air volume measurements. From an operator's standpoint, er-
rors associated with mass measurements can be minimized by careful handling of
the filter (to avoid tearing or loss of collected material) and tightening the
gasket properly for an airtight seal. Errors associated with air volume meas-
urements are controlled by proper calibration and monitoring of the sampler
flow system.
2.1.3.3 Calibration--
Calibration is defined as the establishment of a relationship between the
scale readings on an instrument and the true value of the quantity being meas-
ured. Particulate sampling instruments are calibrated with respect to both
particle sampling efficiency and volume of air sampled. At present, no method
exists for field calibration of instruments with respect to aerosol sampling
efficiency. (This type of calibration is carried out in a laboratory.) How-
ever, field calibration checks of the flow rate can be made readily by compar-
ison with a calibrated flowmeter or by measurement of the pressure drop across
the differential pressure meter. This calibration check is necessary to en-
sure that the volume of air sampled is--accurately estimated by multiplying the
sampling period by the flow rate. Details for field calibration checks of the
instruments discussed in this manual are given in the appropriate subsections
(2.3.6, 2.4.6, 2.5.6, and 2.6.6). Section 5.8.2 (Quality Assurance) gives the
laboratory calibration procedures.
2.1.3.4 Sizing Suspended Particulates-
For purposes of this manual, the-only particle sizing of interest is that
based on aerodynamic diameter. Aerodynamic diameter, as opposed to actual
physical diameter (i.e., length measured under a microscope), determines the
behavior of particles in inertia! devices such as dichotomous samplers. Meas-
urements by a dichotomous sampler indicating all particles on a filter are
less than 2.5 urn aerodynamic diameter signify that those particles behaved
like unit density spheres of less than 2.5 urn diameter.
As mentioned above, suspended participates are much larger and heavier
than the gas molecules comprising the atmosphere. Particle-laden air passing
through an inertia! device such as a dichotomous sampler is forced around
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obstacles, causing the air to take a sharp turn. Because of their greater
weight (inertia!), particles of certain sizes cannot make this turn and will
continue moving in their original direction. Figure 2.1.1 illustrates this
effect for the inlet of the dichotomous sampler. Most of the noninhalable
particles (>15 urn, aerodynamic diameter) do not make the turn into the inlet;
therefore, the sampler samples primarily inhalable particles. (The same prin-
ciple holds true for the modified high volume sampler.)
Figure 2.1.2 illustrates the same principle used in dichotomous samplers
to further divide the aerosol into a coarse fraction (2.5 to 15 urn, aerodynam-
ic diameter) and a fine fraction (<2.5 urn, aerodynamic diameter). After pas-
sing through the inlet, the air containing inhalable particles is forced to
pass through an acceleration jet and then turn around a lower jet haying a
lower velocity air flow. Most of the fine particles can make this turn and
pass on to the fine filter. The larger or coarse particles, however, fall
through the lower jet and eventually are captured on the coarse particle fil-
ter. This particular design is sometimes called "virtual impaction" because
the particles impact on a slowly pumped void rather than on a solid plate.
2.1.4 Glossary of Terms
Aerodynamic diameter—The diameter of a unit density sphere having the same
terminal settling velocity as the particle in question. Operationally,
the size of a particle as measured by an inertia! device.
Calibration—Establishment of a correspondence between scale readings on an
instrument and the true value of the measured quantity.
Dichotomous sampler—An inertia! sizing device that separates a particle-laden
stream into coarse and fine fractions.
Differential pressure meter—Any of various flow measuring devices that oper-
ate by restricting the flow and' measuring the pressure drop across the
restriction.
Mass flowmeter--A flow measuring device that measures the mass flow rate of
air passing a point, usually using the rate of cooling or heat transfer
from a heated probe.
Particulate, partide--A single unit of solid or liquid material that contains
many molecules and is suspended in air.
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FLOW
MAIN
DEFLECTOR
FLOW
STILLING
CHAMBER
BUG SCREEN
10 x 18 MESH
SHIELD
FLOW TO DICHOTOMOUS SAMPLER
Figure 2.1.1. Inlet for a typical dichotomous sampler.
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INLET
Section No. 2.1
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TO
COARSE
PARTICLE
FILTER
TO FINE
PARTICLE
FILTER
Figure 2.12. Operation of dichotomous sampler using virtual impaction.
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Coarse parti culate--Partic1e having an aerodynamic diameter approxi-
mately between 2.5 and 15 urn.
Fine particulate--Particle having an aerodynamic diameter less than
2.5 pm.
Inhalable participate—Particle having an aerodynamic diameter less than
15 |jm.
Respirable suspended participate (RSP)--Interchangeable with "fine par-
ticulate."
Traceability to NBS--A procedure documented by the National Bureau of Stand-
ards by which one standard is related to another that is generally ac-
cepted as more reliable.
Virtual impact!on—Impaction of particles on stagnant air rather than a solid
plate.
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2.2 OPERATOR'S SUMMARY
The following summary provides a brief synopsis of the sampler operat-
ing procedures, used in the IP Network. It is intended to be a quick refer-
ence guide for the experienced operator who is already familiar with the
sampling instruments and site operation in the IP Network.
2.2.1 Operation of the IP Network Samplers
During routine IP Network operation, the operator will be required to
remove the exposed filters and replace them with fresh filters. Procedures
for this operation for the four samplers discussed in this section are given
in Sections 2.2.1.1 to 2.2.1.4.
2.2.1.1 Operation of the Conventional High Volume Sampler--
1. Open the roof of the shelter. Unscrew the four wing nuts
holding the face plate until the bolts can be pushed back
sufficiently to permit the removal of the plate. Remove the
face plate by lifting it up carefully.
2. With great care, use the corner of the filter folder to lift
the filter from the holder. Slide the folder under the fil-
ter, center it, and fold carefully lengthwise at the center
of the exposed area making--sure that exposed areas overlap
and do not contact the clean filter margins. Examination of
the filter at the end of a sampling period will show whether
the filter was properly placed and sealed. The edges of the
sample area should be sharply defined with a ^-inch clean
margin on each side (see Section 2.2.3).
3. Place the folder containing the filter in the plexiglass
sheets provided. Seal the plexiglass with the binder pro-
vided.
4. Remove the Dickson chart and place it in the envelope pro-
vided. Be sure that sample type (TSP), filter number, date,
site number, and average Dickson reading are recorded on back
of Dickson chart.
5. Record the field data on the data sheet and card as
described in Section 2.2.2; record in daily logbook.
6. Examine the screen. If it is dirty, it should be wiped clean
with a clean Kimwipe paper towel. Place a clean filter in
position on the screen of the filter holder. If the filter
has a smooth and a rough side, the smooth side should be
placed down. Be sure the filter is centered on the screen so
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Section No. 2.2
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that when the face plate is in position, the gasket will make
an'airtight seal on the outer edges of the filter.
7. Place the plate in position on the filter holder being care-
ful not to move the filter out of position. Move the bolts
into place and gently tighten the wing nuts, working from
opposite corners. The plate is tightened properly about one
turn after the nut contacts the face plate. It j_s important
that the wing nuts be tightened evenVy and properly to pre-
vent air leakage around the filter. I_f they are too tight,
the gasket becomes flattened and will not recover its elas-
ticity sufficiently to seal properly. On the other hand,
i_f the face plate has not been sufficiently tightened, the
edges £f the sample area wi 11 tie i rregul ar and signs £f ai r
leakage wi 11 be shown by_ streaks across the clean margins.
Close the roof of the shelter carefully to avoid damaging the
filter.
8. Install a new chart (#106 Dickson) on the Dickson pr-essu-re"
recorder. Record sampler type, site, filter number, and sam-
pling date on the back of the chart before placing on the re-
corder. Place the chart on the recorder. Care should be
taken to ensure that the edges are properly located under the
two small retainers, and that the center section, which is
the driving spindle, is inserted properly. Set the chart at
the proper starting position.
9. Advance to correct starting time. Insert a coin in the
slotted drive spindle and turn clockwise to the required
time.
10. Zero the pen by gently tapping the side of the recorder and
adjusting the potentiometer, if necessary.
11. Record the Dickson information in the daily logbook on the
appropriate data sheet.
2.2.1.2 Operation of the Modified High Volume Sampler with Size Selective
Inlet—
1. Release the four spring latches holding the inlet fraction-
ator. Tilt the inlet fractionator back and secure the sup-
port rod to the cabinet catch plate.
2. With great care, use the corner of the folder- to lift the
filter from the holder. Slide the folder under the filter,
center it, and fold carefully lengthwise at the center of the
exposed area, making sure that exposed areas overlap and do
not contact the clean filter margins.
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Examination of the filter at the end of a sampling period
will show whether the filter was properly placed and sealed.
The edges of the sample area should be sharply defined with a
- clean margin on each side (see Section 2.2.3).
3. Place the folder containing the filter in the plexiglass
sheets provided. Seal the plexiglass with the binder provid-
ed.
4. Remove the Dickson chart and place it in the envelope provid-
ed. Record the sample type (SSI), filter number, sampling
date, site, and average Dickson reading on the back of the
chart.
5. Record the field data as described in Section 2.2.2. Record
in daily logbook.
6. Place a clean filter in position on the screen of the filter
holder. If the filter has a smooth and a rough side, the
smooth side should be placed down. Be sure the filter is
centered on the screen so that when the fractionator is in
position the gasket will make an airtight seal on the outer
edges of the filter.
7 Release the inlet fractionator from the cabinet support rod.
Lower the fractionator over the filter. Secure the fraction-
ator with the spring latches. _
8. Install a new chart (#106 Dickson) on the Dickson pressure
recorder. Record the type, site, filter number, and sampling
date on the back of the chart before placing on the recorder
Place the chart on the recorder. Care should be taken to en-
sure that the edges are properly located under the two small
retainers, and that the center section, which is the driving
spindle, is inserted properly. Set chart at proper starting
position.
9. Advance to correct starting time. Insert a coin in the slot-
ted drive spindle and turn clockwise to the required time.
10. Zero the pen by gently tapping the side of the recorder and
adjusting the zero potentiometer, if necessary.
11. Record the Dickson information in the daily logbook on the
appropriate data sheet.
2.2.1.3 Operation of the Beckman Dichotomous Sampler--
2.2.1.3.1 Manual operation—Because of filter shuttle and seal prob-
lems, the Beckman Automatic Dichotomous sampler is currently operated in a
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manual' mode for use in the IP Network. A special bypass switch has been in-
stalled so that the vacuum system can be controlled by the master timer, in-
dependent of the sampler's microprocessor unit. Thus, the microprocessor
clock can function independently and the field operator can shuttle filters
manually. The following procedure is used for operation of the sampler with
this modification.
1. Connect both power cords. One cord connects to a 110- to
125-V source that remains on at all times. The other con-
nects to the master timer for manual operation.
2. Turn the main power on at the microprocessor (yellow push
button).
3. Set the EPA-installed bypass switch to MANUAL. This switch
is located on the right" side of the sampler above the rotame-_
ter, next to the filter trays (Figure 2.2.1). It is only
used to allow the. pumps to operate independently of the
microprocessor. If the master timer has been set for opera-
tion on this day, the pumps will operate. In this instance,
switch the master timer to a nonsampling day in accordance
with Section 2.2.4.1.
4. At the base of the microprocessor unit, there is a small door
that pulls down; the sampler.-manual switches are here. Switch
the microprocessor to MANUAL by placing the first switch (far
left) in MANUAL position.
5. Load the filters into the trays (one filter in each tray)
according to the procedure in the Beckman SAMPLAIR Manual
AM-2704-302 (October 1978), with the following modifications:
a. Wearing plastic gloves, take two filters from their
petri dishes. (Never touch filters with bare
hands. )
b. Hold the tray in the left hand in an upright posi-
tion with the open side to the right and the num-
bers (1-36) facing away; the number 1 should be the
first number at the top (right corner back). With
the right hand, slide the filter (smooth side of
filter frame up) into the tray so that the notch in
the right corner of the filter is located next to
number 1 on the side of the tray (Figure 2.2.2).
c. Replace both trays in the sampler.
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2
0
IMPACTOR
ASSEMBLY
Figure 2.2.1. Beckman dichotomous sampler modified for manual operation.
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2
0
L-SHAPED
CORNER CUTOUT,
SMOOTH EDGE
INDENTED EDGE
SMOOTH
EDGE
\
MAGAZINE BLOWUP
INDENTED EDGE
INSTRUCTIONS FOR LOADING
1. Place the empty magazine, numbers facing you as shown,
with opening 1 on top and opening number 36 on bottom.
2. Notice that one edge of the filter cassette has an indented
lip with L-shaped corner cutout.
3. Wearing gloves, hold the indented lip edge of the cassette
between the thumb and index finger of your right hand so
that your thumb is on the smooth (top) side of the edge
and your index finger follows the groove of the indented
edge (bottom). The L-shaped corner cutout should face
the "V" of your hand. Look at the magazine blowup. Place
the cassette, indented edge facing out, into the first empty
numbered opening (starting with number 1) so that the L-
shaped corner cutout lines up with the opening number,
the smooth side of the indented edge facing up (toward the
number 1 opening) and the indented side of the edge facing
down (toward the number 36 opening).
4. Fill the remaining openings as described above.
L-SHAPED
CORNER CUTOUT
MAGAZINE
Figure 2.2.2. The bonded Beckman dichotomous filter magazine.
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6. Using the manual switches located at the base of the micro-
processor (-Step 4), set the first switch to the left to
MANUAL ON. Push the second switch (filter shuttle) to
shuttle the filters into place. Push the third switch
(filter seal) to seal the filters.
7. Place the Beckman orifice into the sampler inlet. Attach the
manometer to the orifice. Zero the manometer. Using the
master timer, with the EPA-added switch in MANUAL position,
turn the sampler on. Set the rotameters to the points indi-
cated by the calibration curve provided for the sampler.
Check the manometer reading. If the filters are properly
sealed, the orifice manometer should read within ±10 percent
of 16.7 L/min "total" flow. A reading of greater than
±10 percent difference in flow rate usually indicates that
the fine flow filter is not sealing. Using gloves, push back
and forth on filters slightly. If one is not sealed pro-
perly, it should snap into place. This should allow manome-
ter to read correctly. If not, try another set of filters.
8. Switch the sampler off at the master timer. In accordance
with the procedure in Section 2.2.4.1, set the master timer
for the next operational sampling period.
9. Leave the EPA-added switch in MANUAL position, the micropro-
cessor manual switch in MANUAL ON position, and all filters
in sealed position. Place the inlet back on the sampler.
Record all filter numbers and field data in the logbook as
described in Section 2.2.2. Replace the front door. If the
master timer has been set correctly for the next sampling
period, the sampler should operate correctly.
10. After sampling, adjust the master timer to turn the sampler
back on. Record the final rotameter reading. Reverse the
filter installation procedure to remove filters. (Wear
gloves. ) Place the filters back into their original petn
dishes. Fill out an IP data card as described in Sec-
tion 2.2.2 for each filter.
2.2.1.3.2 Automatic operation—Because of filter shuttle and seal
problems, this procedure is currently not in use in the IP Network.
1. Turn On Power Switch.
2. Set Calendar Clock. Key in a three-digit "day" (Julian date)
number, 001 to 365; a two-digit "hour" number, 00 to 23; and
a two-digit "minute" number, 00 to 59.
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3. Insert Filter Trays. Lower tray carriage and firmly seat
against lower tray stops.
4. Sampler Start Date/Time. Key in a three-digit number for
"day"(Juliandate),a two-digit number for "hoar," and a
two-digit number for "minute."
5. Sampling Time. Key in a three-digit number, 000 to 364, for
the number of days of sampling time per filter; a two-digit
number, 00 to 23, for the number of hours; and a two-digit
number, 00 to 59, for the sampling time in minutes.
5. Group Delay Time. This is the time interval between the
first filter of each group of filters. Key in three digits
for days, two digits for hours, and two digits for minutes.
7. Filter Group Count. Key in a two-digit number, 00 to 36, for
the number of filter pairs per group.
NOTE: For normal IP Network sampling, key in 04 for the
number of filter pairs per group.
8. Printer Format. The printer will automatically print out all
setup oata entered in Steps 4, 5, 6, and 7.
9. Calendar Clock. Depress the PRINT CLOCK key. Verify that
the date/time entered in step 4 is later than the calendar
date/time. If not, depress "TRESET key and repeat steps 4, 5,
6, and 7.
10. Standby. The STANDBY LED indicates that the sampler is in a
wait' mode and will start when the calendar clock equals the
start date/time.
11. INTPT Key. Depressing the INTERRUPT key terminates the pump
cycle. New filter trays may be inserted, or the tray may be
advanced to a selected filter and pumping continued with the
original setup sampling sequence.
12. CONT Key. The CONTINUE key is depressed to restart (con-
tinue) the sampling mode following an "interrupt" cycle or
following completion of the thirty-sixth filter sample.
13. Record the field data as described in Section 2.2.2.
2.2.1.4 Operation of Sierra Model 244 and 244E Dichotomous Samplers—
1. Open the front cover of the enclosure of the Control Module.
The latch is released by turning the knob counterclockwise
and by turning the indicator one-quarter turn counterclock-
wise. It is locked by reversing this process.
-------
Section No. 2.2
Revision No. 0
Date 5/7/80
Page 9 of 2S
2. For the Model 244, turn the SAMPLER switch on the Model 302
Digital Timer/Programmer tcr OFF For the Model 244E, turn
the mechanical timer off.
3. Be sure the flow selector valve on the bottom of the total
rotameter is open.
4. Remove both filter holders. Put filter holders in marked
plastic petri dish.
5. Unscrew the knurled filter holder nuts by hand. Install the
filter containing the preweighed 37-mm diameter Teflon filters
in the Sampling Module. Put both filter cassettes on the fil-
ter screens. The lower half of the cassette goes over the
filter screen. The lower half is the side having the shortest
distance (approximately 1/16 in.) to the filter surface.
Screw on both knurled filter holder nuts tightly by hand.
The coarse-particulate filter is the one with the 1/4-in. O.D.
tubing. The filters can also be distinguished by the fact
that the coarse-particulate filter is on the center line of
the' virtual impactor head and aerosol inlet, and the fine-
particulate filter is off-set (see Figure 2.1.1). (The coarse
filter holder has coarse-knurled nuts and the fine filter
holder has tne fine-knurlea nut.) These are clearly marked
on ihe Model 244E.
6. For the Model 244, depress the POWER switch on the Model 302
Digital Timer/Programmer. Tne pump will turn on. For the
Model 244E, switch the mechanical turner to ON.
7. Turn the SAMPLER switch on the Model 302 to ON.
8. Set the total flow rate. Turn the flow selector valve on the
bottom of the total rotameter to obtain a flow rate of
16.7 L/min from the rotameter calibration curve provided.
The vacuum gauge will read approximately 1 to 2 in. Hg for a
2- to 3-i-im pore size filter. The flow selector valve should
require only slight adjustments between tests.
9. Set the coarse particle flow rate. Turn the flow selector
valve on the bottom of the coarse rotameter to obtain a flow
rate of 1.67 L/min. The vacuum gauge will read approximately
zero. The flow selector should require only minor adjustments
between tests.
NOTE: If the Model 244 or 244E is operated at flow rates
other than those given above, particle size fractiona-
tion will be inaccurate.
-------
Section No. 2.2
Revision No. 0
Date 5/7/80
Page 10 of 28
10. Under normal IP Network practices, the unit should be left on
for manual operation. 'liming is controlled by the master
timer.
11. Record the field data as described in Section 2.2.2.
2.2.2 Field Data Measurements
2.2.2.1 Sampling Frequency—
Except in special cases all samples will be collected every sixth day
for 24 hr from midnight to midnight on the same schedule as the NAMS/SLAMS
samplers. Samplers must operate only on the day scheduled. Alternative
(makeup) days will not be used.
2.2.2.2 Measurement of Air Flow--
All instruments will be set initially to their desired flow rates ..from
their respective flow calibration tables. Flow measurement devices (orifices
or mass flowmeters) are supplied by EPA/EMSL-RTP to check the operating flow
rates. Dickson recorders are used for monitoring the flows of the TSP and
SSI high volume samplers. Their charts can be visually integrated to give
an average flow rate for the sampling period. Initial and final flows for
the aichotomous samplers must be measured and averaged.. Therefore, dicho-
tomous samplers must be turned on before the exposed filters are removed to
obtain a final flow rate. Average flow rates in cubic meters per minute for
each filter are recorded on the data form by the operator.
2.2.2.3 Measurement of Time—
Each site .will be equipped with an electromechanical timer to turn all
samplers (except the automated dichotomous sampler) ON and OFF at the same
time. Resettable elapsed timers are used on all samplers to record the
period of sampling. Nonresettable elapsed hour timers indicate instrument
operating time for the scheduling of required maintenance on items such as
pumps and blowers.
-------
Section No. 2.2
Revision No. 0
Date 5/7/80
Page 11 of 2£
2.2.2.4 Flow Calibration Checks--
In general, the field operators will only be required to check the flow
calibration of a sampler. Initially this will be required at every other
sample change. On high-volume samplers, the calibration check consists of
placing the calibration check orifice and a clean filter on the sampler and
comparing the indicated orifice flow rate at one point with that indicated
by the Dickson flow rate recorder. On dichotomous samplers, an orifice is.
placed on the inlet to check the total inlet flow rate against the indicated
flow rates of the rotameters. If the calibration checks indicate a discrep-
ancy of more than 10 percent, arrangements should be made immediately with
the Field Manager at RTP to have the sampler recalibrated. Flow calibration
graphs and interpolated tables will be provided by EPA-RTP. The flow check
results will be calculated as a percent error (a calculation sh.eet.wi VI be
provided) and the result entered in blocks 40 through 43 on the data card
for the sample to be collected. Periodically (initially quarterly) an audi-
tor (EPA contractor) will be sent to each site to perform an unadjusted flow
audit and recalibrate the samplers if necessary.
2.2.2.5 Collocated Samplers--
Since accuracy is not currently attainable in routine aerosol monitor-
ing, reproducibility will be obtained by operating collocated (side-by-side)
samplers (of the same type) at selected sites. The results from these mea-
surements will be used to qualify the precision of the measurement data.
Samples collected by the collocated samplers are identified by marking box 2
on the IP data card.
2.2.3 Recording the Field Data
The site operator(s) is responsible for keeping records pertaining to
sample identification and sampler operation. Sampling information will be
recorded on data sheets for each type of sampler. Examples of these are shown
in Figures 2.2.3 to 2.2.6. A new data sheet should be used whenever the sam-
pler rotameter setpoint is changed. Return data sheets at least quarterly
to: Environmental Protection Agency, EMSL (MD-76), Research Triangle Park,
NC 27711, ATTN: Inhalable Particulate Network.
-------
TSPIII Vol
Site Number:
Location:
flow ra(o: Set Dickson reading at (or 1.42 m^/min.
Oatii
Iniliali
Filter
number
•
Average
Oickiun
reading
"
Elapsed
lime.
minute}
!
Remarki
~0 C3 ^3 U1
cu 01 m fD
CQ (-< < O
fD fD -"• r+
h-1 Ul -•• 0
ro ^-v. o zj
Use a now/ data shed whunever Dickson selpuint is changed. Reluni data slioels to MD-76 at RTP at least quarterly. 5, OO o"
o -z_ •
r^> o
CD - INi
Fiyure 2.2.3. IP Network data sheet.
o
3/28/79
-------
SSI HI Vol
Site Number:
Location:
Sampler S/N:
Flow rate: Set Dickson reading at
lor 1.13 m3/min.
DltB
Initials
Filter
number
Avenge
Dickson
reading
Elapsed
time,
minutes
Remarks
Use a new data slioet whenever Dickson setpoint is changed. Return data sheets to MD 76 at R 1 P at least quarterly.
Figure 2.2.4. IP Network data sheet.
'V O 70 On
o> O) ro ro
to rH < n
ro rt> -••<-+
Cn —i.
I—' (_n ->- o
OO ^^ O Z)
--J 3
O ~^ -21
-+> 00 O
O ~Z. •
ho o
00 • ho
CD ho
3/28/V9
-------
Site Number:
Beckman Automated Dichotomous Sampler
Location:
Flow ralei: Sal COAflSE rotameter at
Set FINE rolamaler at
Date
Initials
COARSE
tillur
number
FINE
filter
number
Final
COARSE
rotainuter
reading
Final
FINE
rotainetcr
reading
(or
lor 16.00
Average
COARSE
rotameter
leading
1.67 l/min.
-/min.
Average
FINE
rotameter
reading
!
1
Elapicd
lima
minutes
Remarks
TP o 70 • c-t
I— • tn -•• o
-(^ \v o r>
0 \ Z
-ti O3 0
If samplar automatically changes filter sets during a sampling period, enter each sol separately. Use a now data slioul whonuvor eotamolor satpoint(s) it changed, flolurn data shoots CD •
to MO 76 at HTP at (cost quarterly. o
Figure 2.2.5. IP Network data sheet.
3/28/79
-------
Sierra Manual Dichotomous Sampler (Models 244 and 244E)
Site Number:
location: SamplerS/N: .__
Flow rates: Set COARSE rcrtimeter at... lor 1.67 L/niin.
Set TOTAL rotametei
-------
Section No. 2.2
Revision No. 0
Date 5/7/80
Page 16 of 28
Each exposed sample filter will be placed in a separate envelope along
with an IP Network data card (Figure 2.2.7) completed from information on
the data sheets. A note should be made of any unusual adverse weather con-
ditions (e.g., high winds, rain, or dust from nearby construction) and sent
to the laboratory with the IP data card. The IP data card is designed to be
keypunched using 43 of the normal 80 columns. The coding will follow the
EPA SAROAD format as used in previous networks, including site numbers.
2.2.3.1 Logbooks--
Each sampling site will be supplied with a bound logbook in which infor-
mation should be recorded in a diary format. This log should indicate when
sampler maintenance is performed, periods- when samplers are out of service,
dates of field calibration checks and audits, unusual occurrences such as
power outages, dates of sampler replacements, operating personnel changes,
etc. This log will be used to help identify unusual trends or patterns that
may be site-, operator-, or sampler-induced.
2.2.3.2. Completing the Data Card(s) —
Each exposed filter should be sent with the IP data card to: Inhalable
Particulate Filter Bank, Environmental Protection Agency, Mail Drop 8, Re-
search Triangle Park, NC 27711.
The data cards should be filled out in the following manner (see Figure
2.2.7):
a. Station name
b. Site location
c. Filter type (1)
d. Collocated sample (2): An IP Network sampler located at the site
for comparison with a second Network sampler of the same type at
that site.
e. Station code (3-11): SAROAD code. The first two digits refer to
state, the middle four to station, and the last three to site.
f. Agency (12): A (SAROAD code for EPA).
g. Project (13,14): 07 (SAROAD code for IP Network).
-------
Section No. 2.2
Revision No. 0
Date 5/7/8G
Paae 17 of 28
Do not writa in this ipacs
1
2
3
4
5
6
Filtw Typ«
• Hi-Voi
•SSI-Hi-Vol
- Coarse Dichot
- Fine Oichot
• other
• ottiw
En»f
No.
(1 )
Enw X
if y»i
Codocatsd Sampi*
(2)
LACS
Station Nam«
L n r.
Sits Location
INHALA8LE PARTICIPATE NETWORK
Station Cod«
Agency Protect
i» |o M o Is
(3-11)
Yr Mo Day
(15-20)
Filter No.
6 If 0
(24-30)
Sampfing Rata. m3/min
(31-3S)
mm. ismpled
JE]
(36-39)
PC Chock.1*
(4
-------
Section No. 2.2
Revision No. 0
Date 5/7/80
Page 18 of 28
h. Date sample was run (15-20).
i. Starting hour (21,22): 00 (SAROAD code for midnight).
j. Time (23): 7 (SAROAD code for 24-hr sampling period).
k. Filter number (24-30): Identification number found on the filter's
petri dish or the filter itself.
1. Sampling rate (31-35): After averaging the initial and final air
flow rate obtained from the rotameter or the Dickson Chart, refer
to the most recent calibration table to find the actual flow rate
in m3/min.
m. Minutes sampled (36-39): Total minutes sampled taken from elapsed
time meter.
n. QC Check, % (40-43): Performed every other sampling period.
o. Operator's initials, lower right corner.
2.2.4 Sample Validation
2.2.4.1 Validation Criteria—
In order to assist the operator in determining whether a sample is
valid, the following validation criteria have been established for all IP
Network samp!es:
1. Timing
All samplers must turn ON and OFF within 1/2 hour of midnight.
All samplers must operate for at least 2_3 but no more than 25
hours.
2. Flow Rates
Decreases in flow rate during sampling of more than 10 percent
from the initial setpoint are questionable.
Changes in flow rate calibration of more than 10 percent, as
determined by a field calibration check, will invalidate all
samples collected back to the last acceptable flow check.
3. Filter Quality
All particulate deposits that do not have well-defined borders
(possible leak) should be voided.
Any filter that is obviously damaged (i.e., torn or frayed)
should be voided.
-------
Section No. 2.2
Revision No. 0
Date 5/7/80
Page 19 of 28
2.2.4.2 Handling of Valid Samples--
1. Calculate flow rates and fill out IP Network data cards completely
(see Section 2.2.2).
2. Send the filters accompanied by the completed data cards to EPA-
RTP, MD-8, for weighing and analysis according to the preestab-
lished schedule. This procedure guarantees a smooth flow of sam-
ples to the laboratory
2.2.4.3 Handling Invalid Samples--
When a filter is determined to be invalid for any of the previous
reasons:
1. Complete as much of the IP data card as possible.
2. Mark "VOID" in the lower right corner and explain.
3. Mark "VOID" in the logbook and on the data sheet.
4. Do not discard the filter.
5. Mail filter with data card to EPA-RTP, MD-8, where a final decision
on sample validity will be made.
2.2.4.4 Handling of Questionable Samples--
If uncertain as to whether or not a sample should be voided, the oper-
ator should:
1. Complete as much as possible of the IP data card.
2. Put a circled question mark in the lower right corner along with a
short explanation.
3. Mark "Questionable" in the logbook and on the data sheet.
4. Mail filter with data card to EPA-RTP, MD-8, where a final deci-
sion on sample validity will be made.
2.2.5 Operators' Field Calibration Check Procedures
During routine IP Network operation, the operator will be required to
check the calibration of the instruments every other sampling period. Cali-
bration checks of the sampler flow rate require the instruments to be run-
ning, and hence that timed operation of the master timer be bypassed. Pro-
cedures for operation of the master timer and field calibration checks of
the samplers are given below.
-------
Section No. 2.2
Revision No. 0
Date 5/7/80
Page 20 of 28
2.2.5.1 Operation of the Tork Time Control (Master_Timer)--
All samplers are controlled by a master timer to ensure all samplers
operate for a 24-hour period every sixth day. The operator does not need to
be concerned with the master timer except when the timer must be bypassed
for field calibration checks, or in the event of a power failure. However,
the operator should check the master timer at each sample change to make sure
that the next sampling period will be correct.
2.2.5.1.1 Bypassing the master timer during field calibration checks--
The samplers must be operative during the calibration check. Since the cali-
bration check cannot be accomplished when the equipment is collecting a sam-
ple, the master timer must be bypassed. To-bypass the timer:
1. Refer to the timer in Figure 2.2.8.
2. Rotate the skip wheel until the day indicator is pointing to the
sampling day (lug removed).
3. Power is now supplied to all samplers.
4 To turn power off, rotate the skip wheel 10 a no-sampling day (lug
in place).
5. When the calibration check is complete, reset the timer as de-
scribed in the next section.
2. 2. 5.1. 2 Resetting1 the master timer after power failure p_r cal ibration
check--
1. Set the hour dial so that the 'Station time is opposite the
hour indicator.
2. Set the skip wheel so that the number of lugs (clockwise) be-
tween the missing lug and the day indicator is equal to the
number of days before the next sampling date.
2.2.5.2 Field Calibration Check of High Volume Samplers-
Procedures are given below for field calibration checks of both conven-
tional and SSI high volume samplers. These checks are to be performed by
the operator after every other sampling period. If the calibration check
indicates that the sampler flow rate is not within ±10 percent of the cali-
bration setpoint, the sampler must be recalibrated. Recalibration is per-
-------
Section No. 2.2
Revision No. 0
Date 5/7/80
Page 21 of 28
MICRO SWITCH
ACTUATOR
ARM
HOUR
INDICATOR
6-LUG
SKIP WHEEL
MISSING LUG
DAY
INDICATOR
Figure 2.2.8. Tork master timer.
-------
Section No. 2.2
Revision No. 0
Date 5/7/80
Page 22 of 28
formed in the field by the operator. Calibration procedures for high volume
samplers are given in Section 2.2.6.
2.2.5.2.1 Equipment—The following equipment is required for a field
calibration check:
Calibrated orifice (with adapter bars for SSI high volume sampler).
Orifice calibration curve and interpolation table.
Sampler calibration curve and interpolation table.
Water manometer (0 to 12 in. H20).
No. 106 Dickson charts and ink.
IP Network Flow Check Data Sheet.
Screwdriver.
Extension cord.
2.2.5.2.2 Procedure--
I. Before making flow measurements, check all fittings for possible
leaks, particularly where the filter adapter fits the motor hous-
ing. Make sure the gasket is'properly seated.
2. Remove the face plate (TS?) or fractionator inlet (SSI) and attach
the field calibration check orifice. Use special adapter bars for
the SSI sampler
3. Install a No. 106 Dickson Recorder chart and advance time by means
of a screwdriver or coin to establish the zero trace. Make sure
the pen is inking properly. (If Dickson Recorder is not zeroed,
it should be set to zero by adjusting zero screw on face of unit.)
4. Hang the manometer on the side of the high volume shelter. Unscrew
the manometer taps one turn to open the built-in valves and shake
down any water trapped at the top of the tubes. Add water if
necessary. Connect the manometer to the calibration orifice and
zero the scale.
5. Do not disconnect the high volume motor power cord from the flow
control device.
6. Remove the upper section of the calibration orifice and insert a
clean filter.
-------
Section No. 2.2
Revision No. 0
Date 5/7/80
Page 23 of 28
7 Start high volume operation by bypassing timed operation of the
master timer" as described in Section 2.2.4.1. Allow the sampler
to operate for 1 minute to achieve steady operating conditions.
8. While tapping lightly on the Dickson face, advance chart to estab-
lish flow rate trace. Mark the Dickson's reading on the chart and
record the observed value on the data sheet. Measure the obtained
vacuum in the manometer (AP in in. of H20) and record the value on
the data sheet.
9. Turn off the high volume sampler at the master timer.
10. Remove the calibration check orifice assembly and replace the face
plate (TSP) or fractionator (SSI).
11. Set sampler up for next sample run. Make appropriate calculations
on the IP Flow Check Data Sheet and record all information on the
log sheets. Record the OC Check percent on the IP data card. If
the percent error is less than ±10 percent, mail Dickson chart and
Flow Check Data Sheet to IP Network, USEPA, Mail Drop 76, Research
Triangle Park, NC 27711. If the percent error is greater than
±10 percent, recalibration is required (see Section 2.2.6). Con-
tact the IP Network Field Manager (Mack Wilkins. 919-541-3049),
USEPA, Research Triangle Park, NC 27711.
2.2.5.3 Field Calibration Check of Dichotomous Samplers--
A field calibration check of the total flow rate is performed after
every other sampling period for IP Network dichotomous samplers. The check
is made by installing an orifice device calibrated in the operating range of
the sampler The calibration of the orifice device is performed by the EPA's
Environmental Monitoring System Laboratory (EMSL) located in Research Tri-
angle Park, NC. The laboratory calibration procedures are fully described
in Section 5.8.2.1 of this manual.
There are two separate flow paths for the operation of the virtual
impactor. These two flow systems have a total flow rate of 16.7 L/min
(1 ms/hr.). Ninety percent of the flow (15.0 L/min) passes through the fine
side and 10 percent (1.67 L/min) through the coarse side. At present, only
the total flow rate is checked against the field calibration check orifice
device. It is expected that in the near future, calibration checks for the
individual rotameters will be approved and incorporated into these proce-
dures.
-------
Section No. 2.2
Revision No. 0
Date 5/7/80
Page 24 of 28
2.2.5.3.1 Field calibration check procedure for the Beckman dichotg-
mous sampler--
1. Shuttle clean filters into both the "fine" and "coarse" side of
the sampler, as described in sampler operation procedure (Sec-
tion 2.5.3.2).
2. Remove the sampler head from the sampler and replace with the
"total" flow calibration check orifice device.
3. Turn on the sampler and allow it to warm up to operating tempera-
ture (approximately 5 minutes).
4. Adjust both the "fine" and "coarse" rotameters to their respective
setpoints as recorded on the laboratory calibration curve or in-
terpolation table.
5. Observe the pressure drop, AP, across the orifice and the corre-
sponding flow rate from the calibration data provided with the
orifice. Record both values on the IP Network Flow Check Data
Sheet. Also record the rotameter setpoints and their correspond-
ing flow rates on the data sheet.
6. Using the above information, and the formulas provided in the IP
Network Flow Check Data Sheet, calculate the QC Check percent.
Record this value on the Flow Check Data Sheet and the IP data
card.
7. If the calculated QC Check percent is within ±10 percent of
16.7 L/min total flow, the sampler is operating properly. Return
the Flow Check Data Sheet to:
Environmental Protection Agencv
EMSL (MD-76)
Research Triangle Park, NC 27711
ATTN: Inhalable Particulate Network
8. Turn off the sampler, remove the orifice device, and replace the
standpipe.
9. Remove the filters from both "fine" and "coarse11 channels of the
sampler.
10. Set the sampler up for the next sampling period according to the
procedure in Section 2.5.3.1.
11. A calculated QC Check % greater than ±10.0 percent of the
16.7 L/min total flow rate usually indicates that the fine flow
filter is not sealed properly. Using gloves, gently push back and
-------
Section No. 2.2
Revision No. 0
Date 5/7/80
Page 25 of 28
forth on the filters; if one is not properly sealed, it should snap
into place. The pressure drop (AP) across the orifice device
should now yield a QC Check value within 10 percent of the set-
point, 16.7 L/min. If the QC Check value is still outside the
±10 percent range, try another set of filters. If this does not
yield a QC check value within the interval 16.7 L/min ±10 percent,
record the value on the Flow Check Data Sheet. Contact the IP
Field Manager (Mack Wilkins, 919-541-3049) to arrange for recali-
bration. Send the Flow Check Data Sheet to the address above.
2.2.5.3.2 Field calibration check procedure for the Sierra dichotomous
sampler--
1. Insert clean filters into both the "fine" and "coarse" filter
cassettes in the sampler, as described in the operating procedure
(Section 2.6.3.1).
2. Remove the standpipe from the sampler and replace with the "total"
flow calibration check orifice device.
3. Turn on the sampler and allow it to warm up to operating tempera-
ture (approximately 5 minutes).
4. Open both "total" and "coarse" flow control valves full counter-
clockwise. Adjust both the "total" and "coarse" rotameters to
their respective setpoints as recorded on the laboratory calibra-
tion curves or interpolation .tables provided with the sampler.
5. Observe the pressure drop, AP, across the orifice, and its corre-
sponding flow rate from the calibration data provided with the
orifice. Record both values on the IP Network Flow Check Data
Sheet. Also record the rotameter setpoints and their correspond-
ing flow rates on the Flow Check Data Sheet.
6. Using the above information and the formulas provided in the Flow
Check Data Sheet, calculate the QC Check %. Record this value on
the Flow Check Data Sheet and the IP data card.
7 If the calculated QC Check % is within ±10 percent of the 16.7
L/min total flow rate, the sampler is operating properly. Return
the Flow Check Data Sheet to:
Environmental Protection Agency
EMSL (MD-76)
Research Triangle Park, NC 27711
ATTN: Inhalable Particulate Network
8. Turn off the sampler, remove the orifice device, and replace the
standpipe.
-------
Section No. 2.2
Revision No. 0
Date 5/7/80
Page 26 of 28
9. Remove the filters from both "fine" and "coarse" cassettes.
10. Set the sampler up for the next sampling period according to the
operating procedure in Section 2.6.3.1.
11. A calculated QC Check % greater than ±10 percent of the 16.7 L/min
total flow rate usually indicates that the fine flow filter is not
sealed properly. Using gloves, gently push back, and forth on the
filters. If one is not properly sealed, it should snap into place.
The pressure drop (AP) across the orifice device should now yield
a QC Check value within 10 percent of the setpoint, 16.7 L/min.
If the QC check value is still outside the ±10 percent range, try
another set of filters. If this does not yield a QC check value
within the interval 16.7 L/min ±10 percent, the sampler requires
recalibration. Record the value on the Flow Check Data Sheet.
Contact the IP Field Manager (Mack Wilkins, 919-541-3049) to
arrange for recalibration. Return the Flow Check Data Sheet to
the address above.
2.2.6 Operator's (Five-Point) Field Calibration of High Volume Samplers
2.2.6.1 Equipment--
The following equipment is required for calibration of high volume sam-
plers:
Calibrated orifice (with adapter bars for SSI high volume sampler)
- Orifice calibration curve and interpolation table
Water manometer (0 to 12 in. H20)
No. 106 Dickson charts and ink
IP Network Field Calibration Data Forms
Screwdriver
Extension cord
2.2.6.2 Procedure—
1. Before making flow measurements, check all fittings for possible
leaks, particularly where the filter adapter fits the motor hous-
ing. Make sure the gasket is properly seated.
2. Remove the face plate (TSP) or inlet fractionator (SSI) and attach
the field calibration orifice. (Use special adapter bars for the
SSI sampler.)
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Section No. 2.2
Revision No. 0
Date 5/7/80
Page 27 of 28
3. Place a clean chart (No. 106) on the Dickson Recorder—Check the
zero by turning the front panel screw. A gentle tap on the face
may be necessary after each adjustment. Make sure the pen is ink-
ing properly. Zero the water manometer.
4. Attach the water manometer (0 to 12 in. H20) to the calibration
ori fice.
5. Disconnect the high volume sampler power cord from the flow con-
trol device.
6. Remove the upper section of the calibration orifice and insert the
18-hole plate. Tighten the upper section of the calibration ori-
fice securely (Make sure it is not cross-threaded.)
7 Connect the power cord of the high volume sampler to 110 V a.c.
power supply. (Use of an extension cord may be necessary ) After
allowing approximately 1 minute for the Dickson Recorder to stabi-
lize, record the Dickson reading on the calibration data sheet.
Also record the plate number and the manometer reading (AP) in
inches of water, which is the sum of both sides.)
8. Advance the Dickson Recorder chart advance shaft with a screw-
driver or coin to make a trace on the chart. Record aopropriate
restriction plate numoer adjacent to the trace on the Dickson
chart.
9. Disconnect the power cord "to the sampler and insert the next
restriction plate. Repeat Steps 5 through 9 for all restriction
plates.
10. Remove the calibration orifice and replace the original face plate
(TSP) or inlet fractionator (SSI). Remove the Dickson Recorder
chart and attach it to the calibration data sheet.
11. After all readings are complete, the calibration curve should be
plotted. This is done by calling EPA, Research Triangle Park, NC
(919-541-3049), and furnishing all information to the IP Network
Field Manager. In addition, the calibration data sheet and the
Dickson Recorder chart should be mailed to:
U.S. Environmental Protection Agency
MD-76
Research Triangle Park, NC 27704
Attn: IP Network
A calibration curve will be plotted and new calibration informa-
tion will be furnished for the sampler.
-------
Section No. 2.2
Revision No. 0
Date 5/7/80
Page 28 of 28
2.2.7 General Troubleshooting
During the operation of any air sampling network, two general problems
are likely to arise: power outages and severe storms. Inspection of the
Dickson Recorder chart will reveal any drop in the flow rate that occurred
over the 24-hour sampling period; therefore, it provides a record of power
outages. If these chart recorders were not functioning (e.g., clogging of
pens), an unusually light particulate loading should best be treated as
"questionable" since there may have been a power outage during the sampling
period. During severe storms, some or all of the samplers may become
flooded. This will be obvious if the pump is damaged or if the sampler is
still full of water. However, if the fil-ter were flooded without damage to
the sampler, and the filter subsequently dried, flooding may not be obvious.
In such cases, careful inspection of the filter may show evidence of water
marks or an unusual appearance of the exposed filter. In obvious cases of
flooding, the filter samples should be voided; otherwise, they should be
marked "questionable" with an explanation that flooding may have occurred.
-------
Section No. 2.3
Revision No. 0
Date 5/7/80
Page 1 of 25
2.3 OPERATING PROCEDURE FOR CONVENTIONAL HIGH VOLUME SAMPLER
2.3.1 Introduction
This section of the manual presents operating procedures for the conven-
tional high volume sampler. In large part, these operating procedures were
taken from Col lection of Samples of Airborne Particulates by_ Means of High
Volume Samplers, published by Rockwell International. However, they have
been modified and expanded to conform to IP Network practices.
2.3.2 Description of the High Volume Sampler
2.3.2.1 General--
The TSP high volume sampler (General- Metals model 2310-105 or equiva-
lent) used in the IP Network is the Federal Register (3_6 (84), 4/30/71) sam-
pler equipped with a mass flow controller, electromechanical elapsed timers,
and a flow recording device (see Figure 2.3.1.). The nominal operating flow
rate is 1.42 mVmin (50 ftVmin).
The sampler consists of a blower unit to which a filter holder is
attached. The filter holder consists of two parts: (1) a stainless steel
filter adapter, which forms an 8-in. x 10-in. rectangular opening at the top,
covered with a coarse stainless steel screen and which ends in a circular
screw-on connector at the bottom, and (2) an open rectangular face plate of
cast iron or aluminum with a sponge rubber gasket. In sampling, a filter is
placed between the filter support screen and the gasketed face plate. The
adapter screws onto the blower unit using a circular rubber gasket to make
an airtight seal. The sampler is identified by an LA or EPA number Use
these numbers in reporting samples collected. The sampler is designed to
operate with the filter in a horizontal position. A standard shelter is pro-
vided for protection. The sampler operates at 110 V a.c. and requires
approximately 7 A (550 W). A three-conductor emission cord of at least 16-
gauge wire should be used to connect the sampler to the power source.
2.3.2.2 Flow System Description--
Flow measurement is obtained by using a Dickson Mini-corder, which is
permanently installed on the front of the sampler shelter. This recorder
provides continuous flow rate readings and is attached via a section of Tygon
-------
Section No. 2.3
Revision No. 0
Date 5/7/80
Page 2 of 25
-52"
FLOW
FILTER
FLOW
CONTROLLER
FLOW
RECORDER
(DICKSON
CHART)
INLET COVER
WT. -65 LB
Figure 2.3.1. TSP high volume sampler used in IP Network.
-------
Secti on No. 2.3
Revision No. 0
Date 5/7/30
Page 3 of 25
tubing to the blower housing. The recorder runs continuously, independently
of the sampler On startup, the pen rises from zero to indicate the obtained
flow rate making a trace indicating the start time. The end of the sampling
period is marked on the Dickson by the flow drop back to zero. Thus, the
Dickson chart will record the start time, stop time, and any power interrup-
tions as well as the flow rate during the operating period. Figure 2.3.2
gives three examples of Dickson chart recordings.
Under normal conditions with a clean filter in place, the Dickson re-
corder should read in the range of 50 stdftVmin for TSP monitoring. In some
instances, due to low operating voltage, worn motor, etc., the reading may
be somewhat lower. Flow rate readings outside the range of 50 ±10 percent
are more often due to malfunction of the Dickson recorder than to malfunction
of the sampler Particulate levels are very seldom high enough to cause the
flow rate to drop more than 10 percent.
If the filter becomes wet during a severe storm, the moior may overheat
sufficiently to damage it beyond repair Therefore, whenever ccssib;e, the
unit should be shut off during storms.
2.3.2.3 Control System Description—
2.3.2.3.1 Time measurement—The total sampling time is measured with
an ordinary electromechanical time meter located on the face of the flow con-
troller. It is turned on and off simultaneously with the sampler by the mas-
ier timer. It measures the time in minutes and can be reset by pushing a
button to return all counters to zero.
2.3.2.3.2 Master timer—Timed operation of the conventional high volume
sampler is controlled by the Tork master timer. The operator need not con-
cern himself with the master timer except during a calibration or calibration
check, or if a power outage occurs during the sampling period (see Sec-
tion 2.3.6.3). However, the operator should check the master timer at each
sample change to make sure that the next sampling period will be correct.
2.3.3 Operation of the Conventional High Volume Sampler
2.3.3.1 Filter Handling--
Each filter has to be weighed in the laboratory before and after sam-
pling. Therefore, to prevent contamination, handle filters by the edges when
-------
Section No. 2.3
Revision No. 0
Date 5/7/80
Page 4 of 25
TYPICAL 3-7 DICKSON CHART
TYPICAL 24-HOUR
DICKSON CHART
YP1CAL DICKSON CHART SHOWING
SHORT SAMPLING PERIOD DUE TO
MOTOR FAILURE
FAILURE
Figure 2.3.2. Dickson Chart recordings—typical examples.
-------
Section No. 2.3
Revision No. 0
Date 5/7/80
Page 5 of 25
removing them from the sampler and folding them and avoid handling the fil-
ters with dirty fingers. Damaged filters should not be used for sampling.
2.3.3.2 Operation of the Conventional High Volume Sampler--
1. Open the roof of the shelter Unscrew the four wing nuts
holding the face plate until the bolts can be pushed back suf-
ficiently to permit the removal of the plate. Remove the face
plate by lifting it up carefully.
2. With great care, use the corner of the filter folder to lift
the filter from the holder. Slide the folder under the fil-
ter, center it, and fold carefully lengthwise at the center
of the exposed area. When folded, only exposed areas should
contact exposed areas.
Examination of the filter at the end of a sampling period will
show if the filter was properly placed and sealed. The edges..
of the sample area should be sharply defined with a Vinch
clean margin on every side.
3. Place the folder containing the filter in the plexiglass
sheets provided. Seal the plexiglass with the binder pro-
vi ded.
4. Remove the Di-ckson chart and place it, the filter, and the
plexiglass holder in the envelope provided. Be sure that the
sample type (TSP), filter number, date, site number, and aver-
age Dickson reading are recorded on the back of the Dickson
chart.
5. Note elapsed time in minutes.
6. Reset the mechanical time meter.
7 Check electronic timer for proper time synchronization.
8. Record the field data on the data sheet and card as described
in Section 2.3.4; record in the daily logbook.
9. Place a clean filter in position on the screen of the filter
holder. If the screen appears dirty, it should be wiped off
with a clean Kimwipe paper towel. If the filter has a smooth
and a rough side, the smooth side should be placed down. Be
sure the filter is centered on the screen so that when the
face plate is in position, the gasket will make an airtight
seal on the outer edges of the filter.
10. Place the plate in position on the filter holder, being care-
ful not to move the filter out of position. Move the bolts
into place and gently tighten the wing nuts, working from
-------
Section No. 2.3
Revision No. 0
Date 5/7/80
Page 6 of 25
opposite corners. The plate is tightened properly about one
turn after the nut contacts the face plate. rt is important
that the wi ng nuts b_e tightened evenly and properly to _ p_r_e -
venr aj_r VejsKaGe around the fjjter. vf they are too tigntL
the~gasket becomes flattened and will not recover its elasti-
city sufficiently to seal pnscerN. I_f the face plate has
not been sufficiently tightened. t_hj3 gdges p_f the s_amp 1 e area
wTTl b_e irregular and signs or a_i r ]eakage' wljj be shown by
streaks across the cjean margins. Close the roof of the
shelter careful ly to avoid damaging the filter.
11. Install a new chart (#106 Dickson) on the Dickson pressure
recorder. Record sample type, site, filter number, and sam-
pling date on the back of the chart before installing. Place
the chart on the recorder. Care should be exercised to en-
sure that the edges are properly located under the two small
retainers and the center section, which is the driving
spindle, is inserted properly. Check to see that the. chart
is set at the proper starting position. To advance the chart
to the correct starting time, insert a coin in the slotted
drive spindle and turn it clockwise to the required time.
Zero the pen by gently tapping the siae of the recorder ana
adjusting the zero potentiometer, if necessary.
~Ji. Record the Dickson information in the daily logbook on the
appropriate data sheet.
2.3.3.4 Miscellaneous--
Under adverse weather conditions, precautions must be taken to avoid
damage to the filter. During periods of high wind or heavy precipitation,
it may be necessary to turn off the sampler and postpone removal of the fil-
ter until weather conditions improve.
Sometimes the filter adheres to the gasket when tne face plate is re-
moved. When this occurs, the filter may be dislodged by gently jarring the
face plate. Dusting the gasket with talc before installing new filters and
exercising caution against excessive tightening of the wing nuts help to
minimize the tendency of the filter to stick to the gasket. Excess talc
should be removed from the gasket by wiping with a clean Kimwipe paper
towel
2.3.4 Recording the Field Data
The site operator(s) is responsible for keeping records pertaining to
sample identification and sampler operation. Sampling information will be
-ecorded on data sheets like the one in Figure 2.3.3. A new data sheet
-------
TSP HI-Vol
Site Nunib«r:
Date
Initials
Location:
Flow rale: Set Dickson reading at
Sampler S/N:
(or 1.42 m /mm.
Filter
number
Average
Dick son
reading
Elopsed
time,
miiiu Ics
Remarks
Use a now dnla sheet whenever Dickson sctpoiitt is changed. Rclurn data sheets to MD 76 at I! (\' HI loasl quarterly.
~0 CO ^J 1/1
DJ DJ (D
CO (-1- < O
fD rt) -J- r<-
cn — '•
^j en _.. O
\. O 3
c» o
Figure 2.3.3. IP Network Field Data Sheet for TSP high volume sampler.
-------
Section No. 2.3
Revision No. 0
Date 5/7/80
Page 8 of 25
should be used whenever the sampler rotameter setpoint is changed. Return
data sheets at least quarterly to: Environmental Protection Agency, EMSL
(MD-76), Research Triangle Park, NC 27711, ATTN: Inhalable Particulate Net-
work.
Each exposed sample filter will be placed in a separate envelope along
with an IP Network data card (Figure 2.3.4) completed f,rom information on
the data sheets. A note should be made of any unusual adverse weather condi-
tions (e.g., high winds, rain, or dust from nearby construction) and sent to
the laboratory with the IP data card. The IP data card is designed to be key-
punched using 43 of the normal 80 columns. The coding will follow the EPA
SAROAD format as used in previous networks,_including site numbers.
2.3.4.1 Logbooks--
Each sampling site will be supplied with a bound logbook in which infor-
mation should be recorded in a diary format. This log should indicate when
sampler maintenance is performed, periods when samplers are out of service,
cates of field calibration checks and audits, unusual occurrences such as
power outages, dates of sampler replacements, operating personnel changes,
etc. This log will be used to help identify unusual trends or patterns that
may be site-, operator-, or sampler-induced.
2.3.4.2 Completing the Data Card(s)--
Each exposed filter should be sent with the IP data card to: Inhalable
Particulate Filter Bank, Environmental Protection Agency, Mail Drop 8, Re-
search Triangle Park, NC 27711.
The data cards should be filled out in the following manner (see Figure
2.3.4):
a. Station name
b. Site location
c. Filter type (1)
d. Collocated sample (2): An IP Network sampler located at the site
for comparison with a second Network sampler of the same type at
that site.
-------
Do not wnt» tn tftii ipaca
INHALABLE PARTICIPATE Nl
Station Code AOKICY Project
Lr. ——____ _J
FiltBf Typ«
2 -SSI-Hi-VoJ No.
3 - Co*rw oichot r~i"\
4 • Fin« Dtchot ~™
5 - otTwr
5 - trtti*r
Enter X
.f_Y«
(2)
Z^CS
o r ]<-' i / / ! c i o ! a = 1 A i [ ° izJ
(3-11) (12) (13-141
Yr Mo DSY St Hr Tima
— "" — i 1 — i — i ( ' i m
7 ! -7 o 2-\ i \
-------
Section No. 2.3
Revision No. 0
Date 5/7/80
Page 10 of 25
e. Station code (3-11): SAROAD code. The first two digits refer to
state, the middle four to station, and the last three to site.
f. Agency (12): A (SAROAD code for EPA).
g. Project (13,14): 07 (SAROAO code for IP Network).
h. Date sample was run (15-20).
i. Starting hour (21,22): 00 (SAROAD code for midnight).
]. Time (23): 7 (SAROAD code for 24-hr sampling period).
K. Filter number (24-30): Identification number found on the filter
folder.
1. Sampling rate (31-35): After averaging the flow rate obtained from
the Dickson chart, refer to the most recent calibration table to
find the actual flow rate in m3/min.
m. Minutes sampled (36-39): Total minutes sampled taken from elapsed
time meter.
n. OC Check, % (40-43): Performed every other sampling period.
o. Operator's initials, lower right corner.
2.3.5 Sample Validation
2.3.5.1 Validation Criteria--
In order to assist the operator in determining whether a sample is val-
id, the following validation criteria have been, established for all IP Net-
work samples:
1. Timing
All samplers must turn ON and OFF within 1/2 hour of midnight.
All samplers must operate for at least 2_3 but no more than _25
hours.
2. Flow Rates
Decreases in flow rate during sampling of more than 10 percent
from the initial setpoint are questionable.
Changes in flow rate calibration of more than 10 percent, as
determined by a field calibration check, will invalidate all
samples collected back to the last acceptable flow check.
-------
Section o. 2.3
Revisio No. 0
Date 5/ 30
Page 11 f 25
3. Filter Quality
All participate deposits that do not nave well-defined orders
(possible leak) should be voided.
Any filter that is obviously damaged (i.e.. torn or rayed)
should be voided.
2.3.5.2 Handling of Valid Samples--
1. Calculate average flow rate and fill out IP data card co; letely
(see Section 2.2.2, Figure 2.3.4a).
2. Send the filter in its folder accompanied by the complex 1 data
card to EPA-RTP, MD-8, for weighing and analysis accordin< to the
preestablished schedule. This procedure guarantees a smo< h flow
of samples to the laboratory.
2.3.5.3 Handling Invalid Samples--
When a filter is determined to be invalid for any of the previ s rea-
sons:
1. Complete as much as possible of the IP da^s card (Figure 2.3 D).
2. Mark "VOID" in the lower right corner and explain.
3. Mark "VOID" in the logbook and on the data sheet.
4. Do not discard the filter.
5. Mail filter with data card to EPA-RTP, MD-5. where a final c cision
on sample validity will be made.
2.3.5.4 Handling of Questionable Samples--
If uncertain as to whether or not a sample should be voided, th( opera-
tor should:
1. Complete as much as possible of the IP data card (Figure 2.3. c).
2. Put a circled question mark in the lower right corner alone with a
short explanation.
3. Mark "Questionable" in the logbook and on :~e data sheet.
4. Mail filter with data card to EPA-RTP, '• where a final c cision
on sample validity will be made.
-------
Section No. 2.3
Revision No. 0
Date 5/7/80
Page 12 of 25
2.3.6 Operators' Field Calibration Check Pjrocedures
During routine IP Network operation, the operator will be required to
check the calibration of the instruments every other sampling period. Cali-
bration checks of the sampler flow rate require the instruments to be run-
ning, and hence that timed operation of the master timer be bypassed. Pro-
cedures for operation of the master timer and field calibration checks of
the samplers are given below.
2.3.5.1 Operation of the Tork Time Control (Master Timer)--
All samplers are controlled by a master timer to ensure all samplers
operate for a 24-hour period every sixth day. The operator does not need to
be concerned with the master timer except when the timer must be bypassed
for field calibration checks, or in the event of a power failure. However,
the operator should check the master timer at each sample change to make sure
that the next sampling period will be correct.
2.3.6.1.1 Byoassi ng the master timer duri ng fie Id calibrati on checks--
The samplers must be operative during the calibration check. Since the cali-
bration check cannot be accomplished when the equipment is collecting a sam-
ple, the master timer must be bypassed."To bypass the timer:
1. Refer to the timer in Figure 2.3.5.
2. Rotate the skip wheel until the day indicator is pointing to the
sampling day (lug removed).
3. Power is now supplied to all samplers.
4 To turn power off, rotate the skip wheel to a no-sampling day (lug
in place).
5. When the calibration check is complete, reset the timer as describ-
ed in the next section.
2.3.6.1.2 Resetting the master timer after power failure or
calibration check--
1. Set the hour dial so that the station time is opposite the
hour indicator
2. Set the skip wheel so that the number of lugs (clockwise) be-
tween the missing lug and the day indicator is equal to the
number of days before the next sampling date.
-------
Section No. 2.3
Revision No. 0
Date 5/7/30
Page 13 of 25
MICRO SWITCH
ACTUATOR
ARM
HOUR
INDICATOR
6-LUG
SKIP WHEEL
MISSING LUG
DAY
INDICATOR
Figure 2.3.5. Tork master timer.
-------
Section No. 2.3
Revision No. 0
Date 5/7/80
Page 14 of 25
2.3.6.2 One-Point Field Calibration Check Procedure—
This procedure provides a flow rate calibration check of high volume
samplers in the field. No adjustments are to be made to the sampler before
or during the test other than turning it ON or OFF. The procedure is
written specifically for conventional (TSP) high volume samplers with Dick-
son flow rate recorders and mass flow controllers.
2.3.6.2.1 Equipment—The following equipment is required for a field
calibration check:
Calibrated orifice (Figure 2.3.6)
Orifice calibration curve (Figure 2.3.7) and interpolation table
(Figure 2.3.8)
High volume sampler calibration curve (Figure 2.3.9) and interpo-
lation table (Figure 2.3.10)
Water manometer (0 to 12 in. K-O) (Figure 2.3.6)
#106 Dickscn Recorder charts and ink
IP NetworK Flow Check Data Sheet (Figure 2.3.11)
Screwdriver
Extension cord
2.3.5.2.2 Procedure—Refer to Figure 2.3.5 for the following proce-
dures.
1. Before making flow measurements, check all fittings for possible
leaks, particularly where the filter adapter fits the motor hous-
ing. Make sure the gasket is properly seated.
2. Remove the high volume face plate and attach the field calibration
check orifice.
3. Place a clean chart (#106) on the Dickson Recorder. Zero the Dick-
son Recorder by turning the front panel screw. A gentle tap on
the face may be necessary after each adjustment. Make sure it is
inking properly. Zero the water manometer.
4. Attach the water manometer (0 to 12 in. H^O) to the calibration
orifice.
5. Do not disconnect the high volume motor power cord from the flow
control device.
-------
Section No. 2.3
Revision No. 0
Date 5/7/80
Paae 15 of 25
CALIBRATION/CHECK
ORIFICE ASSEMBLY
CALIBRATED
^ORIFICE
^•TYGON TUBING
////////
RESTRICTION
PLATES WITH
GASKET
ORIFICE
ADAPTER
PLATE
GASKET
FILTER
SHUTOFF VALVES
WATER
MANOMETER
ACE PLATE
FILTER
ADAPTER
GASKET
MOTOR
HOUSING
DICKSON
RECORDER
Figure 2.3.6. IP Network field calibration check assembly for TSP high volume samplers.
-------
I s\
u
in
ru
x
2:
2:
s
10 ? n
: IN ^r-R
;M:n
•0. 0
-H
IT?;
HI.4
-r
INi-
PARTICULATg\NETWOpK.pp
VOU;::AUDIT ORIFICE1;
CALIBRATION:.;
;!!••" ! ; :'!i:
rr
~e 1-
-+— H
_, , , 1_
-i --4-
DATE 4/ 2/ 79
24. Z C :
t 756f 0 hyiHg
0 1 23456789 10 1 1 12 13 14 15 16 17
DELTA P, IN H2O
Figure 2.3.7. Sample high volume flow orifice calibration curve.
~XJ O ^D CO
CU H> (D (Ti
CQ r* < O
(T> rp -•• c+
(/I —*•
I—' CJi -•• O
en ^ o r>
o ^^ ^z:
-h 00 O
CD Z '
tXJ O
tn • IV)
CD C.J
-------
**HI YOL AUDIT ORIFICE CALIBRATION DATA**
Section No. 2.3
Revision No. 0
Date 5/7/80
Page 17 of 25
****** AUDIT ORIFICE * IP 8 DATE
4/ 2
SITE
HAN
RDG
2 .0
2.1
n '7
2.3
2.4
2.5
2.6
"2 . 7
2.8
2.9
3,0
3,1
3.2
3.3
3.4
3.5
3.6
3.7
3.8
3.9
4.0
4 , i
4.2
4.3
4.4
4.5
4,6
4.7
4.8
4.9
SCFM
25,009
25.617
26.211
26.791
27.359
27.915
28.460
28.994
29.519
30.034
30.540
31.038
31,527
32.009
32.483
32.951
33.411
33,866
34,314
34.756
35,192
35.623
36.049
36.469
36.885
37.296
37.702
38,104
38.501
38.395
M3/MIN
0.708
0,725
0.742
0.759
0.775
0,791
0.806
0.821
0.836
0.851
0.865
0.879
0.893
0.906
0 .920
0.933
0.946
0.959
0.972
0.9S4
0 . ??7
1 .009
1.021
1,033
1,045
1.056
1.068
1.079
1.090
1.101
MAN
RDG
5,0
5,1
5.2
5.3
5.4
5.5
5,6
5,7
5.8
5.9
6.0
6, 1
6,2
6.3
6,4
6,5
6.6
6.7
6.8
6.9
7.0
•' t ^
7 , 2
7,3
7.4
7.5
7.6
7.7
7.8
7.9
SCFM
39.284
39.669
40.051
40.428
40,803
41.173
41.540
41.904
42,265
42.623
42.977
43.329
43.678
44.023
44.366
44.707
45.044
45.380
45.712
46.042
46.370
46.695
47.018
47.339
47.658
47-974
48,288
48.600
48.910
49.218
M3/HIN
1.113
1 . 123
1 . 134
1 . 145
1 . 156
. 166
,176
, 187
,197
.207
1 .
1 ,
1 ,
1 ,
1.
1,217
1.227
1.237
1.247
1.256
1 .266
1.276
1 .285
1.295
1.304
1 .313
1 .322
1.332
1.341
1,350
1,359
1.368
1.376
1.385
1.394
MAN
RDG
3.0
8. 1
S.2
8.3
8.4
8.5
8.6
8.7
8.8
8,9
9.0
9, 1
9.2
9.3
9.4
9,5
9,6
9.7
9.8
9 . 9
10,0
10. 1
10.2
10.3
10.4
10.5
10.6
10.7
10.8
10.9
SCFM
49.524
49.829
50,131
50.431
50.730
51.027
51.322
51.615
51.906
52, 196
52.485
52.771
53.056
53.340
53.622
53.902
54.181
54.458
54 .734
55,009
55.2S2
55,554
55 . 824
56.093
56.361
56.628
56.893
57.157
57.419
57.681
M3/MIN
1 .403
1.411
1 ,420
1.42S
1.437
1 .445
1,453
1 .462
1.470
1.478
1 .486
1.494
1.503
-1.511
1 .519
1.527
1 .534
1.542
1 .550
1,558
1 . 56o
1 .573
1 .581
1.589
1.596
1.604
1.611
1.619
1.626
1.634
0.492SSO
M3/MIN= 0,503267(MANOMETER READING)
-f ,v V
SCFM
0.492880
17.770713CMANQMETER READING)
MANOMETER READING = MANOMETER READING. IN, H20
M3/MIN « CUBIC METERS/MIN (25Cr760 MMH<3)
SCFM = CUBIC FEET/MIN <25Cr760 MMHS)
Figure 2,3.8, Sample interpolation table for high volume flow orifice calibration.
-------
INHALABLE PARTICIPATE NETWORK
TSP
HI-VOL CALIBRATION
L)
in
c\s
2 0 -
£~» IM
m
x
(0
SLOPE 0. 03075Q
INTCPT 0.215414
C. COEF 0.997210
se-r-or*
borsef®
5 H
1. 0 H
X
(T)
0. 5 J
•tpoint. « 39. 0
0. 0 -
0
I — 9 — I
10
i — » — I - 1 - 8 — » — S — ! - ! - S — « — t-j-4
! - »— J — j - S
S/N 124318
AUO ORFsf! IP 1
DATE 2/
24. 2 C
752. 2
i—i—»—i—i—a—a -T »
30 40 50 60 70
DICKSON READING
Figure 2.3.9. Sample TSP high volume sampler flow rate calibration curve.
-o ra x; tn
(1J 01 fD (T)
id r'- < n
ID ro -•• ri-
(/i —>-
i—• en -•• o
CO ^-^ o 3
---i 3
o \ ;z
-h CO O
CD iZ '
ro o
en • i-o
o o>
-------
EPA« 173701
** B/N 12-1018
DIXON
RDO
25.0
25.3
26.0
24,5
27.0
27.5
20. 0
28. 5
29.0
29.3
3O.O
30.5
31 .0
31.3
32.0
32,3
33.0
33.5
34.0
34.5
35.0
35.5
36.0
36.5
37.0
37.3
38.0
30.3
39.0
39.3
BCFM
34. 737,
35.300
35.B43
36.306
36.929
37.472
38.015
3B.538
39.101
3?. 644
40.187
40.730
41.273
41 .816
42.359
42.902
43.445
43.968
44.531
45.074
43.617
46.160
46.703
47.246
47.7U9
40.332
4B.B73
49.418
49.961
30.504
M3/M3M
O.VB4
l.OOO
1.015
1,030
1.046
1.061
1 .077
1.092
1.107
1.123
1.138
1 .153
1.169
1.1B4
1.200
1.213
1.230
1.244
1.261
1.277
1.292'
1.307
1.323
1.339
1.333
1.369
1.304
1.400
1.413
1.430
SP HI Vlll MKIII CAI.I UKAI II IN lift) A
DATE
1JIXIIN
KDI3
40.0
40.3
41 .0
41.5
42.0
42.5
43. O
4;i.3
44.0
44.5
43.0
43.3
46.0
46.3
47.0
47.3
40.0
48.5
49.0
49.3
50,0
50.5
51 .0
51.5
32.0
32.3
33.0
33.5
54.0
34,5
2/ 20/
9CFH
31 ,047
51 .390
52,133
32.676
53.21V
33,762
54 .303
54.848
33,391
53.934
56.477
57.020
57.563
38, 1Q6
5B.64V
39. 593
39.736
60.279
60,822
61 .365
61,908
62.451
62.994
63.5:57
64.0BO
64.623
63. 166
65.709
66.232
66.795
UO HJlt:
i
M3/MIM
1 , 446
1 . 4 f. \
I .476
1 .492
1 ,307
1 .32.5
1 .iri.il]
1.333
1 .3A9
1 ,5»4
1 .5VV
1 .61:3
1 .6.10
1 .646
1 .661
1 .676
1 .692
1 .707
1 .722
1.7JH
1 , 7 3 J
1 .769
1 . 7fJ1
1 .799
1.013
1 ,8 JO
1 .843
1.861
1 .076
1 ,872
II 1 XljN
HUH
;>:-) . o
i; 3 . -'1
;j3/Bin(S«)cri») >• 39.0
Flowchsck f_ iOX DicKoon r«sdin-< ran** - Jh.l in 42. V
I
Audit orlfica » • IP 1 Cai Mr»i.t- * 11 / 21/ /V
factor - 0.50252O >?>-)
01XON KIMJ - UII.KSnil 1,'lHHIrtii
H.l/rtlN » CUBIC hi. ll.KS/MIN (,",i ,,•„•> null'
FJ/fliN •= cuiiii: fii I/TUN (.>r,i:,/.•.,, mni
QJ fD fD rt)
to r+ < n
CD ro —<• H
in —'.
h-' tn ->• O
in --•-, o a
--J Z3
o '~~^ :zr
-Ii CO O
Figure 2.3.10. Sample TSP high volume sampler flow rate calibration—interpolation table.
-------
IP NETWORK
Flow Check Data Si eat
Section No. 2.3
Revision No. 0
Date 5/7/30
Page 20 of 25
3AROAD site number:
location: __^_~_^ *-> '•'•-.'•v'?_-
'
Wontn
Oats
Year
Atrocsphsris pressjre:
Temperature:
Operston —.
Sampler EPA Number:
_ mm Hg, in. Hg
IS? KiVOL ( •/} SSi H1VQL ( ) MAN. DICHOT ( ) AUTO DICKOT
Dickson/rotsmBter reading(s)
S
: a ; C
Caares rotametEn
Fine ratamaten
Total nramfftEn
Dicksen recorder:
-------
Section No. 2.3
Revision No. 0
Date 5/7/80
Page 21 of 25
6. Remove the upper section of the calibration orifice and insert a
clean filter.
7. Switch on the sampler at the master timer. After allowing approx-
imately 1 min for the Dickson Recorder to stabilize, record the
Dickson reading on the Flow Check Data Sheet (Figure 2.3.11). Also
record the sampler flow (mVmin) from the sampler calibration data
(Figures 2:3.9 and .2'. 3.10), the orifice AP (inches of water), the
orifice flow rate (m3/min) from the orifice calibration data (Fig-
ures 2.3.7 and 2.3.8), and other information requested.
8. Advance the Dickson Recorder chart advance shaft with a screwdriver
or coin to make a trace on the Dickson Recorder chart.
9. Switch off the sampler at the master timer.
10. Remove the calibration orifice and replace the original face plate.
Remove the Dickson Recorder chart and attach it to the Flow Check
Data Sheet. . -
11. Set up the sampler for the next sample run. Make appropriate cal-
culations on the Flow Check Data Sheet. Record the information on
the log sheets. Record the QC Check % on the IP data card. If
the percent error is less than ±10 percent, send the Dickson chart
and Flow Check Data Sheet to IP Network, USEPA, Mail Drop 76, Re-
search Triangle Park, NC 27711. If the percent error is greater
than ±10 percent, recalibration is required (See Section 2.3.7).
Contact the IP Network FielcTManager (Mack Wilkins, 919-541-3049),
USEPA, Research Triangle Park, NC 27711.
2.3.7 Five-Point Calibration of the Conventional High Volume Sampler
The following calibration procedure is applicable to both laboratory
and field calibration of the conventional TSP high volume samplers used in
the IP Network.
2.3.7.1 Equipment--
The following equipment is required for calibration:
Calibrated orifice (Figure 2.3.12)
Orifice calibration curve (Figure 2.3.7) and interpolation table
(Figure 2.3.8)
1 set of 5 restriction plates (18, 13, 10, 7, and 5 holes) (Fig-
ure 2.3.12)
-------
Section No. 2.3
Revision No. 0
Date 5/7/80
Page 22 of 25
CAUBKATION/AUDH
ORIFICE ASSEMBLY
RESTRIC70R PLATES
CALIBRATED
'ORIFiCS
TYGON TUBING
RESTRICTION
^, PLATES WITH
GASKET
RESTRICTOR
• PLATE
ORIFICE
XADAPTER
PLATE
GASKET
—'SHUTOF? VALVES
WATER-
MANOMETER
FACE PLATE
FILTER
ADAPTER '
GASKET
MOTOR
HOUSING
.
RECORDER
Figure 2.3.12. IP Network calibration assembly for TSP high volume samplers.
-------
Section No. 2.3
Revision No. G
Date 5/7/80
Page 23 of 25
Water manometer (0 to 12 in. hLO)
#106 Dickson Recorder charts and ink
IP Network field calibration data form" (Figure 2.3.13)
Screwdriver
Extension cord
2.3.7 2 Procedure--
Refer to Figure 2.3.12 in the following procedure.
1. Before making flow measurements, check all fittings for possible
leaks, particularly where the filter adapter fits the motor hous-
ing. Make sure the gasket is properly seated.
2. Remove the high volume sampler face plate and attach the field-cal-
ibration orifice.
3. Place a clean chart (#106) on the Dickscn Recorder Zero the Dick-
son Recorder by turning the front panel screw. A gentle tap on
4. Attach the water manometer (0 to 12 in. hLO) to the calibration
orifice.
5. Disconnect the high volume sampler motor power cord from the flow
control device.
6. Remove the upper section of tne calibration orifice and insert the
18-hole plate. Tighten the upper section of the calibration ori-
fice securely. (Make sure unit is not cross threaded.)
7 Connect the power cord of the high volume sampler to 110 V a.c.
power supply (use of extension cord may be necessary). After
allowing approximately 1 min for the Dickson Recorder to stabilize,
record the Dickson reading on the calibration data sheet (Fig-
ure 2.3.13). Also record the plate number and the manometer read-
ing (AP in inches of water, which is the sum of both sides).
8. Advance the Dickson Recorder chart advance shaft with a screwdriver
or coin to make a trace on the Dickson Recorder chart. Record
appropriate restriction plate number adjacent to the trace made on
the Dickson Recorder chart.
9. Disconnect the power cord to the high .volume sampler and insert
the next restriction plate. Repeat Steps 6 through 9 for the 13-,
10-, 7-, and 5-hole restriction plates.
-------
Data
Operator
Hiyh Volume Field Calibration with Audit Orifice
Projiict _..._. Iligti volume s/ii
Site _. Audit orifice sVn
T«rnp
A tin. PreL
C
mm llj
Ins! numbar
Example
1
2
3
4
S
6
7
8
Plato
number
15
Manomotur
AP
led niyhi
5.00
i
2. BO
Audit
orilico, AP*
in. H20
(L + R)
7.80
Hicksoi]
reading
51.5
*AP = Piossiire drop.
Orifice calibration ilate
Exponent
I'KCllIt
Figure 2.3.13. IP Network high volume field calibration data form.
(i> (U (D (D
1Q r+ < n
fp rt> ->• r<-
ui —<-
txi tn -•• o
-P» ~\ o n
•~~j n
o \ 2:
-Hi CO O
o z •
ro o
on • ivi
CD CO
-------
Section No. 2.3
Revision No. 0
Date 5/7/3G
Page 25 of 25
10. Remove the calibration orifice and replace the original face plate.
Remove the Dickson Recorder chart and attach it to the calibration
data sheet.
11. After all readings are complete the calibration curve should be
plotted. This is done by calling Research Triangle ParK, NC
(919-541-3049) and furnishing all information to the IP Network
Field Manager. Also, the calibration data sheet and the Dickson
Recorder chart should be mailed to IP Network, USEPA, Mail Drop 76,
Research Triangle Park, NC 27711. A curve will be plotted and
new calibration information (Figures 2.3.9 and 2.3.10) will be fur-
nished for the sampler.
-------
Section No. 2.4
Revision No. 0
Date 5/7/80
Page 1 of 27
2.4 OPERATING PROCEDURE FOR HIGH VOLUME SAMPLER WITH SIZE SELECTION INLET
2.4.1 Introduction
This section of the manual presents operating procedures for the high
volume sampler with a 15-um inlet fractionator (Texas A & M design). This
modified high volume sampler measures the total mass of particulate in the
size range of 0 to 15 urn. In large part, these operating procedures were
taken from the Col lection o_f Samples £f Airborne Particulates bv; Means £f
Hj_g_h Volume Samplers, published by Rockwell International. These procedures
have been modified and expanded to conform to IP network practices.
2.4.2 Description of the High Volume Sampler with Inlet Fractionator
2.4.2.1 General--
The Size-Selective Inlet (SSI) high volume sampler is a conventional
TSP sampler, equipped with a special inlet to collect 0 to 15 urn (aerodynamic
diameter) particulate (see Figure 2.4.1). The nominal operating flow rate
is 1,13 mVmin (40 ftVmin). The only significant changes from the TSP high
volume are the elimination of the face plate and hold-down screws, which are
replaced by a spring clamp mechanism. Figure 2.4.2 shows a blowup of the
filter holder and inlet fractionator. The inlet fractionator consists of a
specially designed 15-pm size selective inlet using fractionating baffles.
The filter holder consists of a stainless steel filter adaptor with an
8-in. x 10-in. rectangular opening at the top covered with a coarse stainless
steel screen, and a circular screw-on connector at the bottom. In sampling,
a glass fiber filter- is placed between the filter support screen and the
gasketed inlet fractionator. The adaptor latches on to the blower unit using
a circular rubber gasket to make an airtight seal. The sampler operates at
110 V a.c. and requires approximately 7 A.
2.4.2.2 Flow System Description—
Flow measurement is recorded by using a Dickson Mini-corder, which is
permanently installed on the front of the sampler shelter. This recorder
provides continuous flow readings and is attached via a section of tubing to
the blower housing. The recorder runs continuously, independently of the
sampler. On startup the pen rises from zero to indicate the obtained flow
-------
Section No. 2.4
Revision No. 0
Date 5/7/80
Page 2 of 27
INLET COVER
INLET RiNG-
FILTER
ulWi
!! FLOW
CONTROLLER
FLOW
RECORDER
(DICKSON
CHART)
FLOW
!\_ STANDARD
HIGH VOLUME
SAMPLER
FLOW
n
Figure 2.4.1. SSI high volume sampler used in the IP Network.
-------
Section No. 2.4
Revision No. 0
Date 5/7/80
Page 3 of 27
ACCELERATION
NOZZLES
IMPACTION
CHAMBER
LATCH (4)
BLOWER/MOTOR
HIGH VOLUME ^^^
FILTER HOLDER
1
-
-
^^
Figure 2.4.2. Filter holder and inlet fractionator for SSI high volume sampler.
-------
Section No. 2.4
Revision No. 0
Date 5/7/80
Page 4 of 27
rate-and the start time. The end of the sampling period is marked on the
Dickson paper by the flow drop back to zero. Thus, the Dickson chart will
record the start time, stop time, and any power interruptions as well as the
flow rate "during the operating period. Figure 2.4.3 gives three examples of
Dickson chart recording.
Under normal conditions and with a clean filter in place, the Dickson
recorder should read in the range of 35 to 45 stdftVmin. NOTE: These read-
ings should correspond to 40 stdftVmin ±10 percent on the calibration curve
provided. In some instances, due to low operating voltage, worn motor, etc.,
the reading may be somewhat lower. Particulate levels are seldom high enough
to cause the flow to drop below this reading.
If the filter becomes wet during a severe storm, the motor may overheat
sufficiently to damage it beyond repair. Therefore, whenever passib.le,~ the
unit should be shut off during storms.
2.4.2.3' Control System Description—
2.4.2.3.1 Tijne Measurement—The total sampling time is measured with
an ordinary electromechanical time meter located on the face of the flow con-
troller- It is turned on and off simultaneously with the sampler by the mas-
ter timer. It measures the time in minutes and can be reset by pushing a
button to return all counters to zero.
2.4.2.3.2 Master Timer—Timed operation of the conventional modified
high volume sampler is controlled by the Tork master timer. The operator
need not concern himself with the master timer except during a calibration
check or if a power outage occurs during the sampling period. (See Sec-
tion 2.4.6.2.) However, the operator should check the timer at every sample
change to ensure that it operates properly for the next sampling period.
2.4.3 p^e_ratj_on_o_f__High VoJ_ume Sampler With Inlet Fractionator
2.4.3.1 Filter .Handling-
Each filter has to be weighed in the laboratory before and after sam-
pling. Therefore, to prevent contamination, handle filters by the edges when
removing them from the sampler and folding them, and avoid handling the fil-
ters with dirty fingers. Damaged filters should not be used for sampling.
-------
Section No. 2.4
Revision No. 0
Date 5/7/80
Paoe 5 of 27
TYPICAL 3-7 DICKSON CHART
FLOW RATE
START TIME
TYPICAL 24-HOUR
DICKSON CHART
TYPICAL DICKSON CHART SHOWING
SHORT SAMPLING PERIOD DUE TO
MOTOR FAILURE
MOTOR FAILURE .
Figure 2.4.3. Dickson chart recordings-typical examples.
-------
Section No. 2.4
Revision No. 0
Date 5/7/80
Page 6 of 27
2.4.3.2 Operation of the SSI High Volume Sampler--
1. Release the spring latches holding the inlet fractionator. Tilt
the inlet fractionator back and secure it with the cabinet support
rod (Figure 2.4.4).
2. With great care, use the corner of the flter folder to lift the
filter from the holder. Slide the folder under the filter, center
it, and fold carefully, lengthwise, at the center of the exposed
area. When folded, only exposed areas should contact exposed
areas.
Examination of the filter at the end of a sampling period will show
if the filter was properly placed and sealed. The edges of the
sample area should be sharply defined with a 1/2-inch clean margin
on each side.
3. Place the folder containing the filter in the plexiglass sheets
provided. Seal the plexiglass with the binder provided.
4. Remove the Dickson chart and place it in the envelope provided.
Be sure that the sample type (SSI), filter number, date, site num-
ber, and average Dickson reading are recorded on the back of the
Dickson chart.
5. Note tne elapsed sampling time in minutes.
6. Reset the mechanical time meter.
7. Check electronic timer for proper time synchronization.
8. Record the field data on the data sheet and card as described in
Section 2.4.4; record in the logbook.
9. Place a clean filter in position on the screen of the filter hold-
er. If the screen appears dirty, it should be wiped clean with a
Kimwipe paper towel. If the filter has a smooth and a rough side,
the smooth side should be placed down. Be sure the filter is cen-
tered on the screen so that when the inlet'fractionator is in posi-
tion the gasket will make an airtight seal on -the outer edges of
the fi Her.
10. Release the inlet fractionator from the cabinet support rod. Low-
er the fractionator over the filter. Secure the fractionator with
the spring latches.
11. Install a new chart (#106 Dickson) on the Dickson pressure re-
corder. Record sampler type (SSI), site, filter number, and sam-
pling date on back of the chart before installing. Place the chart
on the recorder. Care should'be exercised in installing the new
-------
HOUSING
UPPER BASE PLATE
SUPPORT ROD
SPRING LATCH
QJ ni o> CD
CQ (-1- < n
ID rn —'• ( ^
(n —'.
^J Cn -•• O
^v. o r^
O ~^J ZI
-I. ^-- Z
CO O
ro CD z: •
•-J o
ro
o -P>
Figure 2.4.4. Schematic of filter holder for SSI high volume samplers.
-------
Section No. 2.4
Revision No. 0
Date 5/7/80
Page 8 of 27
cnart to ensure that the edges are properly located under the two
small retainers and the center section, which is the driving sec-
tion, is inserted properly. Check to see that the chart is set at
the proper startinc position. To advance the chart to the correct
starting time, insert a coin in the slotted drive spindle and turn
it clocKwise to the required time. Zero the pen by gently tapping
the side of the recorder and adjusting the zero potentiometer, if
necessary.
2.4.2.4 Mi seel 1aneous--
Uncer adverse weather conditions, precautions must be taken to avoid
damage to the filter. During periods of nigh wind or heavy precipitation,
it may be necessary to turn off the sampler and postpone removal of the fil-
ter until weather conditions improve.
Sometimes the filter adheres to the gasket when the inlet fractionator
is removed. When this occurs the filter may be dislodged by gently jarring
the fractionator. Dusting the gasket with talc before installing new filters
helps to minimize the tendency of the filter to stick to the gasket. Excess
talc should be removed from the gasket by wiping with a clean Kimwipe paper
towe i
2.4.4 Recordina the Field Data
— --- - -J-t- _ - - T _,_
The site operator(s) is responsible for keeping records pertaining to
sample identification and sampler operation. Sampling information will be
recorded on the data sheet shown in Figure 2.4.5. A new data sheet should
De used whenever the sampler rotameter setpoint is changed. Return data
sheets at least quarterly to: Environmental Protection Agency, EMSl (MD-76),
Research Triangle Park, NC 27711, ATTN: Inhalable Particulate Network.
Each exposed sample filter will be placed in a separate envelope along
with an IP Network data card (Figure 2.4.6) completed from information on
the data sheets. A note should be made of any unusual, adverse weather condi-
tions (e.g., high winds, rain, or dust from nearby construction) and sent to
the laboratory with the IP data card. The IP data card is designed to be key-
punched using 43 of the normal 80 columns. The coding will follow the EPA
SAROAD format as used in previous networks, including site numbers.
-------
SSI HI-Vo!
Site Number:
Location:
Sampler S/H:
Flow (ate: Sot Dickjnn reading at
for 1.13 m3/min.
Data
Initials
Filler
number
Average
Dickson
reaciing
Remark*
Ike a nnw cl.ila sliool whonowor Dickson solpoint is cliiinyud. riotiirn iliilii shoels to MIJ-7fi ;i( II I P ;it loasl i|ii,ii (oily.
"O O ^O 1/1
ai cu ru o>
IQ r+ < n
(t> 05 -». r+-
cn —i.
kO LJl — '• O
--. O Z3
OJ O
tr> 2: •
o
Figure 2.4.5. IP Network field data sheet for SSi high volume samplers.
CD
3/2B/7U
-------
Filar TYBS
1 - Hi-Voi Ensw
: - SSI-Ht-V« Wo.
^ - rrrr* DK
6 - c-13-vc^
cmsr X
if yw
- D
Sta Locaoon ^
Rltw Type
2 - SSI-Hi-Vrt
i 3 - CJETSS Olchct
4- Fin« OlcOcn
5-i
Mo.
r—™|
ED
ID
Cafwratsd
Entsr X
ff yes
(~~1
LJ
(21
, .-: •>-**•>!><. „!//-
Section No. 2.4
Revision No. 0
Date 5/7/80
Page 10 of 27
INKALASLE "ARTICULATE .NETWORK
St Hr Tims
uHf"' LZJ
(21-22) ''23!
ComrmFfits
a. Valid data card
n ,/t
__—. '•<- ^
Station Coda
(3-111
Yr Mo Ds-f
EiSSL !
TH NETWORK
Agency
S EZ]
(12! 113-1*1
(1S-JOI
St Hr Tims
cm] 0
-21.22) (23!
crr\
b. Invalid data card
L£l£LLLd
INHALASUE P ARTICULATE NETWORK
i Code
(15-20)
RltsrNo,
v3
/ j
i oj
(24-301
(21-22) (22)
(31-3S)
136-331
OC CJieCT.%
1*0-431
c. Questionable data card
E4SL l«1S/7i f
figure 2.4.6, Sample data cards-completed for SSI high volume sampler.
-------
Section No. 2.4
Revision No. 0
Date 5/7/80
Page 11 of 27
2.4.4.2 Logbooks--
Each sampling site will be supplied with a bound logbook in which infor-
mation should be recorded in a diary format. This log should indicate when
sampler maintenance is performed, periods when samplers are out of service,
dates of field calibration checks and audits, unusual occurrences such as
power outages, dates of sampler replacements, operating personnel changes,
etc. This log will be used to help identify unusual trends or patterns that
may be site-, operator-, or sampler-induced.
2.4.4.2 Completing the Data Card(s)--
Each exposed filter should be sent with the IP data card to: Inhalable
Particulate Filter Bank, Environmental Protection Agency, Mail Drop 8, Re-
search Triangle Park, NC 27711.
The data cards should be filled out in the following manner "(see Figure
2.4.6):
a. Station name.
b. Site location.
c. Filter type (1).
d. Collocated sample (2): An IP Network sampler locatea at the site
for comparison with a second Network sampler of the same type at
that site.
e. Station code (3-11): SAROAD code. The -first two digits refer to
state, the middle four to station, and the last three to site.
f. Agency (12): A (SAROAD code for EPA).
g. Project (13,14): 07 (SAROAD code for IP Network).
h. Date sample was run (15-20).
i. Starting hour (21,22): 00 (SAROAD code for midnight),
j. Time (23): 7 (SAROAD code for 24-hr sampling period).
k. Filter number (24-30): Identification number found on the filter
folder.
1. Sampling rate (31-35): After averaging the flow rate obtained from
the Dickson chart, refer to the most recent calibration table to
find the actual flow rate in m3/min.
-------
Section No. 2.4
Revision No. 0
Date 5/7/80
Page 12 of 27
m. Minutes sampled (36-39): Total minutes sampled taken from elapsed
time meter
n. QC Check, % (40-43): Performed every other sampling period.
o. Operator's initials, lower right corner.
2.4.5 S amp 1 e_ _V a_]_i_da t i_g_n
2.4.5.1 Validation Criteria—
In order to assist the operator in determining whether a sample is
valid, the following validation criteria have been established for all IP
Network samples:
1. Timing
All samplers must turn ON and OFF within 1/2 hour of midnight.
All samplers must operate for at least 23 but no more than 2_5
hours.
2. Flow Rates
Decreases in -low rate during sanio'ing cf more than 10 per-
cent from the initial setpoint are questionable.
Changes in flow rate calibration of more than 10 percent, as
determined by a field calibration check, will invalidate all
samples collected back to the last acceptable flow check.
.
Fi 1 ter Dual ity
All particulate deposits that do not have well-defined borders
(possible leak) should be voided.
Any filter that is obviously damaged (i.e., torn or frayed)
should be voided.
2.4.5.2 Handling of Valid Samples--
1. Calculate the average flow rate and fill out the IP Network data
card completely (see Section 2.2.2, Figure 2.4.6a).
2. Send the filter in its folder accompanied by the completed data
card to EPA-RTP, MD-8, for weighing and analysis according to the
preestabl 1 shed schedule. This procedure guarantees a smooth flow
of samples to the laboratory
-------
Section No. 2.4
Revision No. 0
Date 5/7/80
Page 13 of 27
2.4.5.3 Handling Invalid Samples--
When a filter is determined to be invalid for any of the previous rea-
sons:
1. Complete as much of the IP data card as possible (Figure 2.4.6b).
2. Mark "VOID" in the lower right corne^ and explain.
3. Mark "VOID" in the logbook and on the data sheet.
4. D_o not di scard the filter.
5. Mail filter with data card to EPA-RTP, MD-8, where a final decision
on sample validity will be made.
2.4.5.4 Handling of Questionable Samples--
If uncertain as to whether or not a sample should be voided, the opera-
tor should:
1. Complete as much as possible of the IP data card (Figure 2.4.6c)
2. Put a circled question mark in the lower right corner along wiih a
short explanation.
3. Mark "Questionable" in the logbook and on the data sheet.
4. Mail filter with data card to EPA-RTP, MD-8, where a final decision
on sample validity will be made.
2.4.6 Operator's Field Calibration Check Procedures
During routine IP Network operation, the operator will be required to
check the calibration of the instruments every other sampling period. Cali-
bration checks of the sampler flow rate require the instruments to be run-
ning, and hence that timed operation of the master timer be bypassed. Pro-
cedures for operation of the master timer and field calibration checks of
the samplers are given below.
2.4.6.1 Operation of the Tork Time Control (Master Timer)--
All samplers are controlled by a master timer to ensure all samplers
operate for a 24-hour period every sixth day. The operator does not need to
be concerned with the master timer except when the timer must be bypassed
for field calibration checks, or in the event of a power failure. However,
-------
Section No. 2.4
Revision No. 0
Date 5/7/80
Page 14 of 27
the operator should check the master timer at each sample change to make sure
that the next sampling period will be correct.
2.4.6.1.1 Bypassing the master timer during field calibration checks—•
The samplers must be operative during the calibration check. Since the cal-
ibration check cannot be accomplished when the equipment is collecting a sam-
ple, the master timer must be bypassed. To bypass the timer:
1. Refer to the timer in Figure 2.4.7.
2. Rotate the skip wheel until the day indicator is pointing to the
sampling day (lug removed).
3. Power is now supplied to all samplers.
4. To turn off power, rotate the skip wheel to a no-sampling day (lug
in place).
5. When the calibration check is complete, reset the timer as de-
scribed in the next section.
2.4.6.1.2 Resetting the master timer after power fai1ure or cal ibration
check--
1. Set the hour dial so that the station time is opposite the
hour indicator
2. Set the skip wheel so that the number of lugs (clockwise) be-
tween the missing lug and the day indicator is equal to the
number of days before the next sampling date.
2.4.6.2 One-Point Field Calibration Check Procedure--
This procedure provides a method to check the calibration of the flow
rate of SSI high volume samplers in the field. No adjustments are to be made
to the sampler before or during the test other than turning it ON or OFF,
The procedure is written specifically for SSI high volume samplers with Dick-
son flow rate recorders and mass flow controllers.
2.4.6.2.1 Equipment—The following equipment is required for a field
calibration check:
Calibrated orifice with adapter bars (Figure 2.4.8)
Orifice calibration curve (Figure 2.4.9) and interpolation table
(Figure 2.4.10)
-------
Section No. 2.4
Revision No. 0
Date 5/7/80
Page 15 o
MICRO SWITCH
ACTUATOR
ARM
HOUR
INDICATOR
6-LUG
SKIP WHEEL
MISSING LUG
DAY
INDICATOR
Figure 2.4.7. Tork master timer.
-------
Section No. 2.4
Revision No. 0
Date 5/7/80
Page 16 of 27
ORIFICE
r
CALIBRATION/CHECK
ORIFICE ASSEMBLY
i////////
TUBING
SHUTOFF VALVES
RESTRICTION
PLATES WITH i
GASKET
-WING NUTS
ORIFICE
ADAPTER
GASKET
FILTER
FACE PLATE ADAPTER BAR
WATER
MANOMETER
FILTER
ADAPTER
MOTOR
HOUSING
DICKSON
'RECORDER
Figure 2.4.8. IP Network field calibration check assembly for SS! high volume samplers.
-------
u
in
CM -•
0. 0
iir;
I I
INHALED PARTICULAR
NETWORK H!:l;f!j
; AUDIT ORIFIC| JCA^JBRATION.-.
DATE 4/ 2/ 79
24. 2 C .
0 1 2 3 4 5 6 7 8 9 1011121314151617
DELTA P, IN H20
Figure 2.4.9. Sample high volume flow orifice calibration curve.
"O O ?0 OO
OJ 0J (T> fD
CQ r+ < n
rt) rt> -•• tr+
tn -*•
h- ' en — •• o
--J ^^ o z>
_
CXD O
o -z- •
O
o
-------
**lll VOL ADLH r UK II 1C.L CAL I UK A f I ON UAIA+*
****** AUDIT ORIFICE * IP B DATE
4/ 2/ 79
SITE
HAH
RDG
2.0
2.1
2.2
2.3
2.4
2.5
2.6
2 . 7
2.8
2 .9
3.0
3.1
3.2
3.3
3.4
3.5
3.4
3.7
3.8
3.?
4.2
4.3
4.4
4.3
4. 4
4.7
4.8
4.9
SCFM
25.00Q
25.617
24.211
24.791
27.359
27.915
28.440
28.774
29.519
30.034
30.540
31.030
31.527
32.009
32.4B3
32.951
33.411
33.064
34.314
34.754
35.172
35.423
34.049
34.449
34.BBS
37.274
37.702
38.104
38.501
38.895
0.
0.
0,
0,
H3/HIH
0.70Q
0.725
0.742
.759
.775
.791
.BOA
0.821
0.834
O.B51
0.845
0.879
0.893
0.904
0.920
0.933
0.944
0.959
0.972
0.984
0.997
.009
.021
.033
.045
.054
.048
,079
1.090
1.101
HAN
KDO
5.0
5. 1
5.2
5.3
5.4
5.3
5.4
5.7
5.8
5.9
4.0
4. 1
4.2
4.3
4.4
4.5
4.4
4.7
4.8
4.9
7.0
7. 1
7.2
7.3
7.4
7.5
7.4
7.7
7.8
7.9
SCFH
39.204
39.469
40.051
40.42B
40.B03
41.173
41.540
41.904
42.245
42.423
42.977
43.329
43.478
44.023
44.344
44.707
45.044
45.380
43.712
44.042
44.370
44.495
47.ioiO
47.339
47.458
47.974
48.288
48.400
48.910
49.218
H3/MIN
1.113
1 .123
1 . 134
1 . 145
1 . 154
1. 164
, 174
. 187
, 197
,207
1 .217
1 .227
1 .237
1 .247
1.254
1 .244
1.274
1 .285
1.295
1 .304
1.313
,322
.332
,341
,350
.359
,348
.374
.385
.394
MAN
RUG
B.O
B. 1
8.2
8.3
8.4
0.5
8.4
8.7
8.8
0.9
9.0
9. 1
9.2
9.3
9.4
9.5
9.4
9.7
9.8
9.9
10.0
10. 1
10.2
10.3
10.4
10.5
10.4
10.7
10.8
10.9
SCFH
49.524
49.829
50. 131
50.431
50.730
51 .027
51 .322
51.415
51 .904
52. 194
32.405
52.771
53.054
53.34O
53.422
53.902
54. 101
54.438
54.734
55.009
55.202
55.554
55.824
54.093
54.341
54.428
54.893
57.157
57.419
37.681
M3/HIN
1.403
1.411
1 .420
1 .428
1 .437
1 .445
1 . 453
1.442
1.470
1 .470
1 .406
1 .494
1 .503
1.511
.519
.527
.534
.542
.550
.558
.544
.573
.581
.589
1 .594
1.404
1.411
1.419
1..424
1 .434
0.492000
H3/HIN= Q.^03247(MANOMETER READING)
0.492000
SCFH = 17.770713(HANOHETER READING)
HANOMETER READING = MANOMETER REAPINGr IN. M20
M3/MIN = CUBIC METERS/HIM (25Cr760 MMMU)
SCFM = CUEtIC FEEIYMIN (25C,760 HMIla)
~O O TO U~i
o> cu a> a>
(Q <-*• < o
rt> (D -J- r+
(/! —'.
t—' en ->. o
00 \ O Z>
-•J 3
o \ ^
-h CD O
o -z •
Figure 2.4.10. Sample interpolation table for high volume flow orifice calibration.
-------
Section No. 2.4
Revision No. 0
Date 5/7/80
Page 19 of 27
SSI high volume sampler calibration curve (Figure 2.4.11) and
interpolation table (Figure 2.4.12)
Water manometer (0 to 12 in. H20)
No. 106 Dickson Recorder charts and ink
IP Network Flow Check Data Sheet (Figure 2.4.13)
Screwdriver
Extension cord
2.4.6.2.2 Procedure—Refer to Figure 2.4.8 for the following procedure.
1. Before making flow measurements, check all fittings for possible
leaks, particularly where the f-liter adapter fits the motor hous-
ing. Make sure the gasket is properly seated.
2. Release the four spring latches securing the SSI head to the shel-
ter. Tilt the head back so that support brackets hold it in place
(Figure 2.4.4). Lift filter adapter out enough to attach calibra-
tion unit. Since SSI filter adapter has no face plate, special
face plate adapter bars are used to secure calibration check unit
in place.
3. Place a clean chart (#106) on the Dickson Recorder. Check the zero
of the Dickson Recorder by turning the front panel screw. A gentle
tap on the face may be necessary after each adjustment. Make sure
it is inking properly Zero the water manometer
4. Attach the water manometer (0 to 12 in. H20) to the calibration
orifice.
5. Do not disconnect the high volume motor power cord from the flow
control device.
6. Place a clean filter on the adapter under the orifice device just
as though a sample were being collected. (Note: No restrictor
plates are used for this one-point check; use orifice and filter
only.)
7. Switch sampler on at the master timer. After allowing approximate-
ly 1 min for the Dickson Recorder to stabilize, record Dickson
reading on flow check data sheet (Figure 2.4.13). Also record the
sampler flow rate (m3/min) from the sampler calibration data (Fig-
ures 2.4.11 and 2.4.12), the orifice AP (inches of water), the ori-
fice flow rate (nrVmin), and other information requested from the
orifice calibration data (Figures 2.4.9 and 2.4.10).
-------
INHALABLE PARTICULATE NETWORK
SSI
HI-VOL CALIBRATION
(J
in
2. 0 -.
70
SLOPE 0.034120
10% »rror band*
0)
I
(D
v^»
INTCPT -0.072922
OB C. COEF 0. 998321
5 -
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1. 0 -
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20
10
0. 0
i i i ii
i i
0
Dioh»or> • otpolrit •* 35. 3
EPAi¥175680
B/N 09215
AUD ORFif IP-1
DATE 3/ 14/ 80
20. 8 C
758. 0 mrtiHg
I t t I !•>-•< i >-i ill i » i—i > i t t • r t
10 20 30 40 50 60
DICKSON READING
70
Figure 2.4.11. Sample SSI high volume sampler flow rate calibration curve.
"O CJ 3D CD
CU O) (D (D
U3 r+ < O
(D CD -•• r+
1/1 —••
f\o en -J. O
O \ O D
~vj ZJ
O "\ Z
-*i c» o
o -z. •
ro o
~j • ro
-------
I I HIM Hi* I O *-K
1 /S
•n.
rnxiin
KMU
i!;i . o
2S . T,
26.0
2A.!i
27.0
27 . 1,
211.0
2ll.b
2V. 0
2V . Ji
30.0
30. S
3 1 . 0
31.:;
3.T.O
32.3
33.0
33.3
34.0
34.5
35.0
35.5
3A.O
36.5
37.0
37.5
3B.O
311.5
39.0
39.5
SCI H
27.'., 45
!tl. 1 4U
.'11 . 750
JV..K',2
J9 .955
10.557
51 . 1AO
Jl .762
12.364
32.967
33.569
34.172
34.774
33.376
33.979
3A.5B1
37.184
37.786
3B.3H9
30.991
39.593
40.196
40.798
41 .401
42.003
42.605
43.208
43.H10
44.413
45.015
M.J/HIN
0,71:10
0.797
0.1)14
0.031
O.H4I3
0.11 A3
0 . (313'J
0 . 900
0.917
0.934
0.931
0.9AI1
0 . 9U5
1 .002
1 .019
1 . 036
1 . 053
1.070
1.0H7
1.104
1,121
1 .13(3
1,135
1.172
1.190
1 .207
1 .224
1 .241
1 . 250
1.275
11 1 XI IM
Mil
40
10
11
-11
42
4 2
I'.J
43
41
44
4 3
45
4 A
4A
47
47
11:1
113
49
4V
50
50
31
5J
32
52
53
33
51
51
i
.0
. :/
.0
. 3
.()
. 5
.0
. 3
,0
. 5
.0
.5
.0
. '.i
.0
.5
.0
. 3
.0
• • J
.0
.5
.0
.5
.0
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.0
.3
.0
.5
43
4.'.
46
1 /
413
•HI
4V
4V
30
31
51
3:-
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53
54
34
3 3
35
56
57
37
513
5 1.3
59
AO
AO
61
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62
63
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//.3i::i
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IM/ II I i-l
1 , IK) 1
1 .1:1'.' 1
1 . H.tll
i .H:)r,
1 .«/:••
1 .131 IV
1 . VOA
1 , v::.t
1 .9-10
1 »v:./
1 . V/1
1 . Wl
V'.OOII
:?.().^.
•J.04.1
? . OAO
•;_'.()//
2.OV4
2.111
•J . 1 .'13
2.14:..
2.1A'..'
2.1 /V
2 . 1 VA
2 . ;.' 1 3
a. 2. »o
2 . '. ' 4 /
•-J.2A4
•.?.2II1
'J . '.!VH
M3/MIN- 0.034120 (DIXON REAI)1NO)+ . -0.072922
(
F3/MIN= 1.204CI07 (DIXON READING) + -2.374937
Dickeon setpoint for 1.13 iii3/min( 40<:fm ) = 33.3
Flouchoek i._ 10X
I. on flow I •- 1P-1
0.311/40
rcaiJin--! r-jnHia = 31.13 t.u 313 . V
.'/ .'o/
O.4V:v..'')
130
|i I /IMJ l-'IHi • M 11.1.: >> >iJ Kl Mil 11)1.
h'l/Hiii •- i:ui:|i: ni u i.1:.' n i ••> i '.'M: • <'<••< nun
l.i/'itlii - 1:111:11: ill I.IIKJ i. M../O.O iiiiii-i;
Figure 2.4.12. Sample SSI high volume sampler flow rate calibration interpolation table.
(u o> n> o>
to c-i- < n
(T> CD —•- (-h
tn —>.
ro en -•• o
i—' ^^ o n
\i 3
o \ z
-h CX> O
O Z •
ro o
-------
SAROAD site number:
L2_-
» y /
Location! L
Data:
y
Month
$\c o
o £ fl^x
/
33
Data
o 5
''*
7
xi ^ /,- £^
7~
Year
IP NETWORK
Flow Check Data Sheet
Atmospheric pressure:
Temperature: ^_«_
Operator i
Sectfon No. £.4
Revision No. 0
Date 5/7/80
Page 22 of 27
Hg, in.
/8C,"°F
,\ . ,
Sampler EPA Number:
TSP HIVOL ( ) SSI HIVOL
MAN. DICHOT ( ) AUTO DICHOT { )
01
H-
<
|
.J
u.
Dickson/rotameter rsadingis)
A Coana rnTamatar*
B Finn rrttafnntur; _ _
D Dickon recDrriar , _. 3_.5 • "^
Total sampler flow raw: (1)
Sampler flow rates m /min*
B Ft™* rntamBt"r , ,
D Dickon nwnrriw ._.,,L.-..' — '
m /min (A •+• 8, C, «' 0)
OrifJcs serial number
Calibration data
y /.: ''7?
j|
Orrfics manomeTEr reading:
0rifles flow rate: (2}
O
inches !
Calculations
Percent error
(2)
100 - (3)
QC check % (3) + 100 = (4) _/_ £ i., 2- %
Enter (4) in spaces 4043 on IPN Data Card
*F!ow rates determined from sampler calibration carve.
Figure 2.4.13. IP Network Flow Check Data Sheet.
-------
Section No. 2.4
Revision No. 0
Date 5/7/80
Page 23 of 27
8. Advance the Dickson Recorder chart advance shaft with a screwdriver
or coin to make a trace on the Dickson Recorder chart.
9. Switch the sampler off at the master timer.
10. Remove the calibration orifice and replace the fractionator. Re-
move the Dickson Recorder chart and attach it to the Flow Check
Data Sheet.
11. Set sampler up for next sample fun. Make appropriate calculatioRS
on Flow Check Data Sheet. Record information on log sheets. Re-
cord the QC check percentage on the IP data card. If the percent
error is less than ±10 percent, mail Dickson chart and the Flow
Check Data Sheet to IP Network, USEPA, Mail Drop 76, Research Tri-
angle Park, NC 27711. If the percent error is more than ±10 per-
cent, recalibration is required (see Section 2.4.7). Contact the
IP Network Field Manager (Mack Wilkins, 919-541-3049), USEPA, Re-
search Triangle Park, NC 27711.
2.4.7 Five-Point Calibration of the SSI High Volume Sampler
The following calibration procedure is applicable to both laboratory
and field calibration of the SSI high volume sampler used in the IP network.
2.4.7.1 Equipment--
The following equipment is required for calibration:
Calibrated orifice with adapter bars (Figure 2.4.14)
Orifice calibration curve (Figure 2.4.9) and interpolation table
(Figure 2.4.10)
1 Set of 5 restriction plates (18, 13, 10, 7, and 5 Holes) (Figure
2.4.14)
Water manometer (0 to 12 in. H20)
No. 106 Dickson Recorder charts and ink
IP Network high volume field calibration data form (Figure 2.4.15)
Screwdriver
Extension cord
2A.1.2 Procedure--
Refer to Figure 2.4.14 in the following procedure.
-------
Section No. 2.4
Revision No. 0
Date 5/7/80
Page 24 of 27
18
RESTRICTOR PLATES
CALIBRATION/AUDIT
ORIFICE ASSEMBLY
ORIFICE
^-TYGON TUBING
RESTRICTION
^PLATES WITH
s' GASKET
|/// / / / / / ~7~ ~ X*
^^ PLATE
.-WING NUTS
^5E? _ M ^sb ORIFICF I
1 1
-3 X 3
^"
T
|
7 SHUTOFF VA
WATER
MANOMETER
i /
jr/
FACE PLATE ADAPTER BAR i I
FILTER
ADAPTER
MOTOR
HOUSING
DICKSON
'RECORDER
Figure 2.4.14. IP Network calibration assembly for SSI high volume samplers.
-------
High Volume Field Calibration with Audit Orifice
Date Project High vnlume t/n Temp C
Operator Site Audit nrifirp i/n Atm Prev mm HQ
Tast number
Example
1
2
3
4
6
6
7
8
Plate
number
15
•*"
*AP = Pressure drop.
Orifice calibration date
Exponent
Manometer
AP
Left Right
5.00
2.80
Audit
orifice, AP*
in. H20
(L + R)
7.80
Factor
Dickson
reading
51.5
Figure 2.4.15. IP Network high volume field calibration data form.
o> o> re ID
to r+ < n
ct> m -•. t-+
LO — '.
[\5 (_n _i. o
un \. o n
oo
CD
o
-------
Section No. 2.4
Revision No. 0
Date 5/7/80
Page 25 of 27
1. Before making flow measurements, check all fittings for possible
leaks, particularly where the filter adapter fits the motor hous-
ing. Make sure the gasket is properly seated.
2. Release the four spring latches securing the SSI fractionator head
to the shelter. Tilt the head back so that support brackets hold
it in place. Lift filter adapter out enough to attach calibration
unit. Since SSI filter adapter has no face plate, special face
plate adapter bars are used to secure calibration unit in place
(Figure 2.4.14).
3. Place a clean chart (#106) on the Dickson Recorder. Check the zero
of the Dickson recorder by turning the front panel screw. A gentle
tap on the face may be necessary after each adjustment. Make sure
it is inking properly. Zero the water manometer.
4. Attach the water manometer (0-12 in. H20) to the calibration ori-
fice.
5. Disconnect the high volume sampler motor power cord from the flow
control device.
6. Remove the upper section of the calibration orifice and insert the
18-hole plate. Tighten the upper section of the calibration ori-
fice securely. (Make sure unit is not cross-threaded.)
7. Connect the power cord of the high volume sampler to a 110 V a.c.
power supply. (Use of an extension cord may be necessary.) After
allowing approximately 1 min for the Dickson Recorder to stabilize,
record the Dickson reading on the calibration data sheet (Figure
2.4.15). Also record the plate number and the manometer reading
(AP in inches of water, which is the sum of both sides).
8. Advance the Dickson Recorder chart advance shaft with a screwdriver
or coin to make a trace on the Dickson Recorder chart. Record ap-
propriate restriction plate number adjacent to the trace made on
the Dickson Recorder chart.
9. Disconnect the power cord to the high volume sampler and insert
the next restriction plate. Repeat Steps 6 through 9 for the 13-,
10-, 7-, and 5-hole restriction plates.
10. Remove the calibration orifice and replace the fractionator. Re-
move the Dickson Recorder chart and attach it to the calibration
data sheet.
11. After all readings are complete the calibration curve should be
plotted. This is done by calling Research Triangle Park, NC
(919-541-3049), and furnishing all information to the IP Network
Field Manager.
-------
Section No. 2.4
Revision No. 0
Date 5/7/80
Page 27 of 27
12. Mail the calibration data sheet and the Dickson Recorder chart to
IP Network, USEPA, Mail Drop 76, Research Triangle Park, NC 27711.
A curve will be plotted and new calibration information (Fig-
ures 2.4.11 and 2.4.12) will be furnished for the sampler.
-------
Section No. 2.5
Revision No. 0
Date 5/7/80
Page 1 of 44
2.5 OPERATING PROCEDURE FOR THE BECKMAN SAMPLAIR DICHOTOMOUS SAMPLER
2.5.1 Introduction
This section of the manual presents operating procedures for the Beckman
Automated Dichotomous Sampler. The Beckman operates on the principle of vir-
tual impaction as described earlier in the manual (Section 2.1.3.4); it is
automated in the sense that the filters, both coarse and fine, can be changed
automatically. However, because of filter shuttle and seal problems, the
Beckman Sampler has been modified to operate manually for current use _i_n the
I_P Network. Procedures for both manual and automatic operation are detailed
in this section. In large part, these operating procedures were taken from
the operation manual for the Beckman SAMPLAIR Manual AM-2704-302, dated
October 1978. The procedures have been modified where necessary to conform
to IP Network practices.
2.5.2 Description of the Beckman SAMPLAIR Dichotomous Sampler
2.5.2.1 General--
The Beckman SAMPLAIR is shown in Figure 2.5.1 with the front cover re-
moved. The virtual impaction stage is directly below the inlet, the auto-
matic filter changer is at right center, and sample pumps are located on the
lower level. Specifications for the Beckman are given in Table 2.5.1. Flow
control is by a feedback controller operating on the pressure drop across a
needle valve in the fine particle suction line. Timing for filter changes
and other operations is controlled electronically.
2.5.2.2 Flow System Description--
The sampling flow system is also illustrated in Figure 2.5.1. The frac-
tionating inlet, which protrudes from the top of the SAMPLAIR, provides the
path for the particulate or aerosol collection. The geometry of the inlet
is symmetrical, so that sampling characteristics do not change appreciably
with wind direction. A coarse screen prevents very large particulates (and
insects and other debris) from being entrained. The inverted air path acts
as a separator to prevent particles greater than about 30 urn from being sam-
pled.
-------
I
a
ui
I
o>
to r+ < n
o> n> -•• r+
(n -i.
ho en -•• o
\ o 3
o --J n
oo
o
Figure 2.5.1. Beckman SAMPLAIR dichotomous sampler used in IP Network.
o
-------
Section No. 2.5
Revision No. 0
Date 5/7/80
Page 3 of 44
TABLE 2.5.1. BECKMAN SAMPLAIR SPECIFICATIONS
Participate size range:
Inlet upper cutoff point (50%):
Virtual imoactor cutpoint (50%):
Sharper than ACGIH criteria
Virtual impactor losses:
Wind velocity;
Sample flow rate:
Sample flow stability:
Timing accuracy:
Start time selection:
Delay period between samoles
or sample groups:
Number of filters per sample
group:
Fi Her material:
Filter size:
Filter capacity:
Housing:
Ambient operating temperature
range:
Operating humidity range:
Power required:
Power failure:
Power cord:
Dimensions:
Instrument weight:
Shipping weight:
1 to 15 urn
15 urn
2.5 urn (3.5 urn option)
-------
Section No. 2.5
Revision No. 0
Date 5/7/80
Page 4 of 44
The air sample then enters the virtual impactor. The sample flow is
split into two separate flow systems. About 10 percent of the total flow
(1.67 L/min) goes through the coarse particulate filter. Filter rupture or
a missing filter is detected by a pressure switch, PS1, which is nominally
set at 1.0 inch of water. The air sample is carried into ballast volume Cl ,
which acts as a flow smoothing device for the WISA vibrator pump. Control
and indication of the flow is provided by a needle valve and a rotameter.
The fine particulate side of the flow stream samples at a rate of 15
L/min. This is 90 percent of the total flow. Air leaving the filter goes
through a Moore 63BD flow controller which, in conjunction with a precision
needle valve, provides a regulated flow. The flow setting is initially ad-
justed to 15 L/min by the needle valve and rotameter. The needle valve then
functions as a fixed flow control orifice.
A Thomas dual diaphragm pump provides the vacuum necessary to induce
flow through the system. A differential pressure switch, PS3, is connected
across the needle valve to sense loading of the fine filter. If the fine
filter resistance rises enough to cause a 5 percent decrease in regulated
flow because of a pollution episode, then the next pair of filters is auto-
matically inserted. The flow controlTer maintains an essentially constant
flow rate up to a fine filter loading of about 8 in. of water pressure drop.
Experience with the Teflon filters indicates that they are effectively fully
loaded at that point. With the two independent flow systems, individual ad-
justments are simple, one-step operations. This greatly simplifies flow sys-
tem maintenance.
2.5.2.3 Sample Changer Subsystem—
The sample changer subsystem (Figure 2.5.2) consists of three mecha-
nisms: filter shuttle drive, tray index, and filter seal. The mechanisms
are mechanically independent, but all are under microprocessor control.
The shuttle drive is a cam-slider mechanism. The cam is a face cam of
simple eccentric design, located under the changer plate. It is driven by
an a.c. gearmotor. The roller follower of the cam is attached to the recip-
rocating filter shuttle assembly on top of the changer plate. A milled slot
in the changer plate provides guidance to the follower roller for smooth lin-
-------
FILTER TRAYS
RECIPROCATING
SHUTTLE
SHUTTLE DRIVE
ECCENTRIC
SHUTTLE DRIVE
MOTOR
CARRIAGE RELEASE KNOB
OPTICAL DETENT
FILTER SEAL
ECCENTRIC
VERTICAL
FILTER
TRAY
FILTER SEAL
MOTOR
MOVABLE CLAMPING
PLATEN
OPTICAL DETENT
PICKUP HEAD
JACKSCREW
TRAY DRIVE MOTOR
Figure 2.5.2. Sampler changer subsystem for the Beckman SAMPLAIR.
oi cu ro ci>
to <-i- < n
fl> CD —'• <™t-
in —'•
en cn —•• o
"^^ o n
O —J Z)
co o
-£> O
rv)
o en
-------
Section No. 2.5
Revision No. 0
Date 5/7/80
Page 6 of 44
ear motion. Position feedback is provided by two mechanical limit switches
actuated by a pin on the rotating eccentric.
The tray index vertically steps the filter trays so that fresh pairs of
filters can be loaded sequentially by the filter shuttle mechanism. The
mechanism is driven by an a.c. gearmotor. A linear motion output is provided
by a jackscrew that engages the tray index carriage. Engagement is by means
of a movable split nut controlled by a knob on top of the carriage. Turning
the knob disengages the carriage from the jackscrew to allow initial posi-
tioning of the carriage. Unlike the other two mechanisms in the sample
changer, the tray index has multiple rest positions. Therefore, position
feedback is provided by a multiposition optical limit switch rather than
simple limit switches. In the illustration (Figure 2.5.2), the notched
detent mask and pickup heads are shown on the front of the trays- for clar-
ity. The optical detent is behind the tray, since access is not normally
required.
The filter seal mechanism serves to clamp and seal filter slides into
the pneumatic system when the shuttle drive pushes them into place for sam-
pling. It also is driven by an a.c. gearmotor operated in sequence with the
other mechanisms, under program control: The rotary motion of the gearmotor
is converted into linear motion of the filter clamping tubes by a simple
eccentric cam. Position readout of the mechanism is accomplished through
limit switches actuated by two eccentrics on-the end of the shaft.
2.5.2.4 Thermostat System—
The SAMPLAIR housing is internally heated to +33° C (+91° F) using a
fixed-setpoint, 250-W, proportional temperature controller. This controller
will maintain the housing at the control temperature through variations in
ambient air temperature from +30° C to -40° C. If ambient temperatures rise
above the controller setpoint (+33° C), the temperature inside the housing
wi 11 rise accordingly.
In addition to the proportional temperature controller, several other
thermal switches are included in the system to help control the internal tem-
perature and to protect circuitry and components.
-------
Section No. 2.5
Revision No. 0
Date 5/7/80
Page 7 of 44
Where ambient temperatures are very high, a high-temperature
thermal switch will actuate at +48° C (+118° F) to energize
the intake blower fan. The fan directs air flow over the
microprocessor circuit board and associated electronics to
prevent extended operation at highly elevated temperatures.
This thermal switch is located inside the electronics housing
assembly on the filter changing assembly.
A low temperature thermal switch disconnects both the battery
power and the +5-V d.c. regulated power to the microprocessor
when internal housing temperatures go below 0° C. The instru-
ment must warm up to +4° C (+39° F) before power is restored.
This thermal switch is located within the electronic housing
on the Interconnect Circuit Board.
A third thermal switch, mounted.on the underside of the in-
strument base plate, closes at -7° C. This connects a second
25-W heating element to the controller, to increase internal
heating for operation at extremely low ambient temperatures.
Figure 2.5.3 shows the thermal switch actuating temperatures and the
control ranges for the SAMPLAIR.
Figure 2.5.4 shows the wiring connections for the temperature control-
ler and thermal switches used in the SAMPLAIR. The temperature controller
consists of a thermistor sensor, integrated-circuit zero-voltage switch, out-
put pulse transformer, Triac switch, and heater element. The controller
operates from the 115-V a.c. line voltage and does not require a d.c. power
supply. The zero-voltage integrated circuit is wired as a proportional con-
troller with an isolated sensor. Power (22 V a.c.) is derived from the sec-
ondary winding of the main transformer and applied to the proportional con-
troller through a 750-ohm current-1imiting resistor.
The zero-voltage switch integrated circuit consists of a diode limiter,
zero-crossing detector, comparator amplifier, and Darlington output driver.
An external resistor-capacitor network is added to force the sense amplifier
to operate as a free-running multivibrator. As the thermistor resistance
varies with temperature, the multivibrator duty cycle varies; a decrease in
temperature causes an increase in resistance, and a corresponding increase
in the output pulse "on" time portion of the multivibrator cycle.
Output trigger pulses from the proportional controller are transformer-
coupled to the Triac gate terminal. Line power is applied to the heater ele-
ments and the Triac switch through a circuit breaker. A neon indicator lamp,
-------
Section No. 2.5
Revision No. 0
Date 5/7/80
Page 8 of 44
TEMPERATURE
CONTROLLER
INTAKE FAN
MAX HEATER
POWER
BATTERY AND
H? POWER
33° C
FULL ON
PROP
OFF
ON
OFF
(T;)+37° C +48° C
250 W
500 W
-T C +4U C(Ta) 33° C
ON
OFF
-40° C
-7°C +4°C(T
T, -INTERNAL TEMPERATURE
T -AMBIENT TEMPERATURE
a
+50 C
Figure 2.5.3. Range of temperature control in Beckman SAMPLAIR.
-------
A9CB2
10A
ZERO
VOLTAGE
SWITCH
115 Va.c.
HEATER
POWER
~U O XJ U~>
QJ CU fl> ff
(Q r+ < O
ft) rt> —»• c~^
O
Figure 2.5.4. Wiring connections for temperature controller and thermal switches.
o
rv>
CD en
-------
Section No. 2.5
Revision No. 0
Date 5/7/80
Page 10 of 44
which is visible on the front side of the power supply, is connected across
the heater elements to indicate when the heaters are fully on (lamp on con-
tinuously), in proportional control (lamp flashing), or off (lamp off).
2.5.2.5 Electronics System--
The electronics system generates a sequence of timed commands that con-
trol visual displays, keyboard, printer, and motors. Different control
modes, or timing sequences, may be selected by the operator.
System operation is controlled by an 8-byte microprocessor-based system
using an 8085 Central Processing Unit (CPU). Control programs are stored in
4K of ROM (read only memory). Input/output signals are interfaced with TTL
logic circuits that control the peripheral-equipment. Figure 2.5.5 is a sim-
plified functional block diagram of the system. A detailed diagram is shown
in Figure 2.5.6. For additional details concerning the electronics system,
refer to the most recent Beckman SAMPLAIR manual.
2.5.3 Operation of Beckman SAMPLAIR
2.5.3.1 Controls and Connections--
Before attempting to set up and operate the SAMPLAIR, familiarize your-
self with the function of all the controls and connections.
2.5.3.1.1 Front dooi—The operating controls are located behind the
housing door. The door can be removed by turning the keylock clockwise and
pulling the door out and down. The door is not hinged and will pull clear.
2.5.3.1.2 Front panel controls--The operating controls are located on
the control panel. These controls are described in Table 2.5.2. Several
other controls below the changer plate are shown in Figure 2.5.7.
2.5.3.1.3 Filter and filter magazine—A special filter and filter tray
are required for operation. The filter material is normally 1-um unbacked
Teflon, specially bonded to a frame. The frame is available in two styles:
a standard solid polyester frame that weighs approximately 4.5 g and a sep-
arable filter frame that weighs about 0.10 g.
The filter magazine holds 36 filters. The same type of magazine is used
for both coarse and fine particle filters. Both magazines are installed in
a common holder. The filters are notched on one corner to provide a vis-
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Section No. 2.5
Revision No. 0
Date 5/7/80
Page 11 of 44
KEYPAD
DISPLAY
LIGHTS
nann
DDDD
nann
anna
— o o—
._o o—
— o o —
—o o —
—o o —
— o o
— o o
POWER
SUPPLY
BATTERY
BACKUP
PRINTER
MICRO-
PROCESSOR
REAL TIME
CLOCK
PRESSURE
SWITCH
SAMPLE CHANGER
FILTER
SHUTTLE
FILTER
SEAL
VERTICAL
TRAY
I
PUMPS
MANUAL SWITCHES
Figure 2.5.5. Simplified block diagram of Beckman SAMPLAIR electronics system.
-------
LIMIT
SWITCHES
SWITCHES
-A
-J
r*-
QUAD
1 LINE TO 1
MUK
-• l>31 «- IHAP
SBC 80/04
COMPUTER
BOARD
pco
IRST6BI
KEYPAD
n
-V
— V
PBO 3
4 1O 16 LINE
DECODER
PBO. 2
3 TO S LINE
DECODER
^
c
n
I
POR
tAICM
J
y
T
f
SIA1US
DATA
LAICH
INSTRUCTION
LED
LATCH
— N
— J
i »-
j
ft1
-fr
PAO r
ENBL Pn,MIEB
CLK OAtA
DPI
EMBL
IATCIIE!
PA4-7
CLK
ENUL
OPT ENUL
J
=5
-^
n
40 M<
ntinio
MV
*-J
LEU
DISPLAY
OPIICAL
COUPLERS
=5
COUPLER
- 16 V -20V
PRINTER
~o o xj tn
CU 01 ID (t>
IQ r+ < n
fD fD ->• r+
in _J.
I— « Cn -J- O
K> \ O 3
Figure 2.5.6. Detailed diagram of electronics system in Beck man SAMPLAIR.
> O3
CD
-------
Section No. 2.5
Revision No. 0
Date 5/7/80
Page 13 of 44
TABLE 2.5.2.
BECKMAN FRONT PANEL CONTROLS, INDICATORS,
AND CIRCUIT BREAKERS
Control
Function
Power
Keypad
Status and
instruction
lights
Paper advance
Manual control
switches
Heaters and
motors;
circuit breakers
Main power
circuit breaker
Fine and coarse
flowmeters
Applies power to the instrument when switch is depressed;
pushbutton illuminates to indicate when power is applied.
The keypad switches control all electrical instrument
functions for instructions and operation.
The 16 status and instruction LEDs help the operator to
set up the instrument, verify the operational mode, and
identify malfunctions.
Paper in the printer is advanced when switch is depressed.
Manual OFF-ON. When ON, this permits using the four
remaining switches (below) to test operation manually.
SEAL MOTOR. This pushbutton switch, when depressed,
will drive the filter seal motor
FLOW PUMP OFF-ON. This toggle switch controls power to
both the fine and coarse flow pumps.
FILTER TRAY. This pushbutton switch, when depressed,
will arive the filter tray indexing motor.
SHUTTLE. This pushbutton switch, when depressed, will
drive the shuttle mechanism motor.
Individual circuit'breakers are provided for the heaters
and motors. These circuit breakers trip and remove the
a.c. line power from the equipment when an overload con-
dition exists. To reset a circuit breaker, first turn
the SAMPLAIR off with the POWER pushbutton switch, then
reset the tripped circuit breaker by pushing in on the
circuit breaker momentarily. Turn the SAMPLAIR on again
and note its operation. If the circuit breaker trips
again, do not reset it. Consult a qualified service man
as the instrument may require repairs.
This is the main circuit breaker Tor the instrument. To
reset, first turn the sampler off with the POWER push-
button switch; then reset the tripped circuit breaker by
pushing in on the circuit breaker momentarily. Turn the
sampler on again and note its operation. If the circuit
breaker trips again, do not reset it. Consult a quali-
fied service man as the instrument may require repairs.
The flow control valves are located near the bottom and
adjacent to the rotameters. The largest (left) rotameter
and its valve are for adjustment of fine flow. The fine
flow is nominally set at about 15 L/min and should be
carefully set with an accurate inlet flow calibrator.
The coarse flow is set at 1.7 L/min. No special calibra-
tor is required.
-------
Section No. 2.5
Revision No. 0
Date 5/7/80
Page 14 of 44
LIMIT
SWITCH
A8S2
PRESS
SWITCH
A8S3
COARSE FILTER FLOWMETER
COARSE FILTER NEEDLE
PUMP
A9VP1
FINE FILTER FLOWMETER
kFINE FILTER NEEDLE VALVE
MOTOR A9B1
BASE PLATE
A9TB3
THERMISTOR SENSOR A8R1
Figure 2.5.7. Internal controls in the Beckman SAMPLAIR.
-------
Section No. 2.5
Revision No. 0
Date 5/7/80
Page 15 of 44
ual indication of correct positioning. The correct orientation (right side
up) is required for proper sealing in the sampling position.
2.5.3.2 Manual Operation of the EPA Modified Beckman SAMPLAIR--
Because of filter shuttle and seal problems, the Beckman Automatic
Dichotomous sampler is currently operated in a manual mode for use in the
IP Network. A special bypass switch has been installed so that the vacuum
system can be controlled by the master timer, independent of the sampler's
microprocessor unit. Thus, the microprocessor clock can function indepen-
dently and the field operator can shuttle filters manually. The following
procedure is used for operation of the sampler with this modification.
1. Connect both power cords. One cord connects to a 110- to
125-V source that remains on at all times. The other connects
to the master timer for manual operation.
2. Turn the main power on at the microprocessor (yellow push
button).
3. Set the EPA-instal led bypass switch to MANUAL. This switch
is on the right side of the sampler above the rotameter, next
to the filter trays (Figure 2.5.8). It is only used to allow
the pumps to operate independently of the microprocessor. If
the master timer has been set for operation on this day, the
pumps will operate. In this instance, switch the master timer
to a nonsampling day in accordance with Section 2.5.6.1.1.
4. At the base of the microprocessor unit, there is a small door
that pulls down; the sampler manual switches are here. Switch
the microprocessor to MANUAL by placing the first switch (far
left) in MANUAL position.
5. Load the filters into the trays (one filter in each tray) ac-
cording to the procedure in the Beckman SAMPLAIR Manual
AM-2704-302 (October 1978), with the following modifications:
a. Wearing plastic gloves, take two filters from their
petri dishes. ( Never touch fiIters with bare
hands.)
b. Hold the tray in the left hand in an upright posi-
tion with the open side to the right and the numbers
(1-36) facing away; the number 1 should be the first
number at the top (right corner back). With the
right hand slide the filter (smooth side of filter
frame up) into the tray so that the notch in the
-------
Section No. 2.5
Revision No. 0
Date 5/7/80
Page 16 of 44
IMPACTOR
ASSEMBLY
Figure 2.5.8. Beckman dichotomous sampler modified for manual operation.
-------
Section No. 2.5
Revision No. 0
Date 5/7/80
Page 17 of 44
right corner of the filter will be located next to
number 1 on the side of the tray (Figure 2.5.9).
c. Replace both trays in the sampler as described in
the Beckman manual.
6. Using the manual switches at the base of the microprocessor
(Step 4), set the first switch to the left to MANUAL ON. Push
the second switch (filter shuttle) to shuttle the filters into
place. Push the third switch (filter seal) to seal the fil-
ters.
7 Place the Beckman orifice into the sampler inlet. Attach the
manometer to the orifice. Zero the manometer. Using the mas-
ter timer, with the EPA-added switch in MANUAL position, turn
the sampler on. Set the roameters to the points indicated by
the calibration curve provided for the sampler. Check the
manometer reading. If the filters are properly sealed, the
orifice manometer should read within ±10 percent of 16.7-L/nn.n
total flow. A reading of greater than ±10 percent difference
in flow rate usually indicates that the fine flow filter is
not sealing. Using gloves, push back and forth on filters
slightly. If one is not sealed properly, it should snap into
place. This should allow the manometer to read correctly.
If not, try another set of filters.
8. Switch the sampler off at the master timer. In accordance
with the procedure in Section" 2. 5. 6.1.1, set the master timer
for the next operational sampling period.
9. Leave the EPA-added switch in MANUAL position, the micropro-
cessor manual switch in MANUAL ON position, and all filters
in sealed position. Place the inlet back on the sampler.
Record all filter numbers and field data in the logbook as
described in Section 2.5.4. Replace the front door. If the
master timer has been set correctly for the next sampling per-
iod, the sampler should operate correctly.
10. After sampling, adjust the master timer to turn the sampler
back on. Record the final rotameter reading. Reverse the
filter installation procedure to remove filters. (Wear
gloves. ) Place the filters back into their original petri
dishes. Fill out an IP data card as described in Sec-
tion 2.5.4 for each filter.
11. The sampler is now ready to load for the next sampling period.
-------
Section No. 2.5
Revision No. 0
Date 5/7/80
Paae 18 of 44
L-SHAPED
CORNER CUTOUT,
SMOOTH EDGE
INDENTED EDGE
SMOOTH
EDGE
\
f"»< /•>» «f I «Q
Di_OvVur
INDENTED EDGE
INSTRUCTIONS FOR LOADING
1. Place the empty magazine, numbers facing you as shown,
with opening 1 on top and opening number 36 on bottom.
2. Notice that one edge of the filter cassette has an indented
lip with L-shaped corner cutout.
3. Wearing gloves, hold the indented lip edge of the cassette
between the thumb and index finger of your right hand so
that your thumb is on the smooth (top) side of the edge
and your index finger follows the groove of the indented
edge (bottom). The L-shaped corner cutout should face
the "V" of your hand. Look at the magazine blowup. Place
the cassette, indented edge facing out, into the first empty
numbered opening (starting with number 1) so that the L-
shaped corner cutout lines up with the opening number,
the smooth side of the indented edge facing up (toward the
number 1 opening) and the indented side of the edge facing
down (toward the number 36 opening).
4. Fill the remaining openings as described above.
L-SHAPED
CONNER CUTOUT
MAGAZINE
Figure 2.5.9. The bonded Beckman dichotomous filter magazine.
-------
Section No. 2.5
Revision No. 0
Date 5/7/80
Page 19 of 44
2.5.3.3 Automatic Operation of the Beckman SAMPLAIR--
It is anticipated that filter shuttle and seal problems will soon be
resolved, enabling the following automatic operation procedures to be used
for the Beckman SAMPLAIR dichotomous sampler.
TURN ON
SET
CALENDAR
DATE/TIME
MECHANICAL
HOMING
TRAY
LOADING
START
SAMPLING
DATE/TIME
SAMPLING
TIME
Depress POWER switch. POWER switch should light. The printer
paper will advance approximately 2 inches, and the pump will
turn on momentarily.
The INSTRUCTION LEDs (light emitting diodes), CALENDAR TIME,
and DAY will light.
Key in a three-digit number--001 through 363--corresponding
to the day of the year on the keyboard. The DAY will turn
off and the HOUR will light.
Key in a two-digit number—00 through 23--corresponding to
the hour. The HOUR will turn off and MINUTE will light. Key
in a two-digit number--00 through 59--corresponding to the
minute. The MINUTE will turn off and the printer will print
out the calendar date and time in the following format:
1
Day
XXX
Hour
XX
Minute
XX
The shuttle and seal mechanisms will automatically go to home
position following the 'calendar printout. The seal mechanism
will drive open, followed by the shuttle retracting to the
home position. Upon completion of the homing mode, the tray
INDEX ERROR will light.
Insert both filter trays. Lower the tray assembly and
firmly seat the assembly against the stops.
Depress RESET key on keypad for approximately 1 second. If
the tray assembly is seated in the load position, the INDEX
ERROR will go out and START TIME and DAY will light.
Key in a three-digit number—001 through 365—for the sam-
pler starting day. The DAY will turn off and HOUR will light.
Key in two-digit number for hour 00 through 23. The HOUR
light will turn off and MINUTE light will come on.
Key in a two-digit number--00 through 59—for the sampler
starting minute. START TIME and MINUTE will turn off and SAM-
PLE DURATION and DAY will light.
Key in a three-digit number--000 to 364--for the required
days (24-hour increments) of sample pumping time. The DAY
will turn off and HOUR will light.
-------
Section No. 2.5
Revision No. 0
Date 5/7/80
Page 20 of 44
FILTER GROUP
DELAY TIME
FILTERS
PER GROUP
Key in a two-digit number—00 to 23—for the required number
of hours of pumping time. HOUR will turn off and MINUTE will
light.
Key in a two-digit numbei—00 to 59—for the required number
of minutes of pumping time. MINUTE will turn off and DELAY
TIME and DAY will light.
the required
between the
Key in a three-digit number—000 to 364—for
number of days (24-hour increments) of delay
start of each group of filters. The DAY will turn off and
HOUR will
light.
Key in a two-digit numbei—00 to 23—for the required number
of hours of delay between the start of each- group of filters.
The HOUR will turn off and MINUTE will light.
Key in a two-digit number—00 to 59--for the r-equired number
of minutes of group delay. The MINUTE will turn off -and"the
GROUP FILTER COUNT will light.
Key in a two-digit numbei—00 to 36—for the required number
of filters (samples) per group.
NOTE: If a DELAY TIME of zero days, hours, and minutes is
keyed in, the instrument automatically switches into a
continuous mode, sampling consecutively through all 36
filter pairs.
PRINT DATA Following the group/count data entry, the printer will list
entry data^. The print format will be as follows:
#2
#3
#4
#5
Day
XXX
XXX
XXX
Hour
XX
XX
XX
Minute
XX
XX
XX
Start Date/Time
Sampling Time
Group Delay Time
Filter Count
CALENDAR Push CLOCK PRINT key to verify that the selected Start
TIME VS Date/Time is Uter than the Calendar Time. If the Start
START TIME Time is earlier than the Calendar Time, depress RESET and
CHECK properly re-enter printer entries #2 through #5, above.
IN With all INSTRUCTION LEDs off and STANDBY on, the program
OPERATION is waiting for the Calendar Time to coincide with the Start
Date/Time, at which time the instrument will start the auto-
matic sampling process.
When the calendar clock time coincides with the programmed Start/Date
Time, the sampler starts automatic control. The initial setup data are
-------
Section No. 2.5
Revision No. 0
Date 5/7/80
Page 21 of 44
printed, followed by the shuttle mechanism inserting a filter pair, the seal
mechanism closing, and the flow pump turning on. Filter number and pumping
start time are printed automatically.
Pumping will continue for the programmed sampling time unless one of
the following conditions is detected: (1) low-pressure drop across one or
both filters, or (2) low-flow system rate. If either of these conditions is
detected within 5 seconds following pump startup, the filter pair will be
recycled to the tray and the next filter pair inserted. The date/time and
symbol designator "M" will print out. A 5-second delay allows sufficient
time for the flow rate to stabilize at the preset rate.
Pumping will continue for the programmed pumping time, unless a filter
overload occurs, detected by a decrease in fine particle flow rate. If the
flow rate decreases below a preset rate, a signal from the low-pressure de-
tector terminates the pumping cycle and the filter pair is recycled to the
tray. Calendar date/time is automatically recorded on the printer tape.
The symbol "<>" is printed to identify the overload condition.
Following an overload condition, the next filter pair is inserted and
pumping continues. The pumping time for the followup filter will be the
balance of the programmed sampling time". For example, assume a 12-hour sam-
pling time program and that overload occurs in 8 hours. Pumping time for
the followup filters will be 4 hours. (Sampling time does not include fil-
ter mechanism transfer time—which is about 25 seconds. )
In the event that a second overload occurs during the 4-hour pumping
interval, filters will again recycle. The pumping time on the third set of
filters will be the time remaining of the programmed 12-hour time.
Two modes of sampling control may be selected during the initial setup:
Continuous Mode or Group Mode. In the Continuous Mode, the sampler program
sequences through all 36 filter pairs. In the Group Mode, the program se-
quences through a preselected number of filter pairs per group with a pro-
grammed interval (Delay Time) between the first filter pair of each group.
The Continuous Mode is selected automatically if the Delay Time was pro-
grammed for zero time delay. Normal operating procedures for the IP Network
call for Group Filter Mode operation.
-------
Section No. 2.5
Revision No. 0
Date 5/7/80
Page 22 of 44
Continuous Mode Operation—This mode is automatically selected if the
initial setup delay time was programmed for zero time. In this mode, the
sampler sequences through all 36 filter pairs, pumping for the programmed
Sample Time for each pair. If a filter overload or a damaged filter is de-
tected, the filters are recycled as previously described.
Group Filter Mode Operation—Group Mode control is selected when the
operator initially keys in a Group Delay Time other than zero. In Group Mode
operation, the sampler sequences through the number of filters—GROUP FILTER
COUNT—programmed during the initial setup. Following completion of the last
filter in each group, the sampler goes to STANDBY until completion of the
interval. At this time, the sampler will start the sequence through the next
filter group. The delay-time interval is the interval between the first
filter £f each group.
If a defective or missing filter is detected, the filters are recycled.
Defective filters are not counted as one sample of the group count. If an
overload condition occurs, filters are recycled and the following filter is
counted as one sample of the filter group.
Printer Format Description—The printer tape provides the sampler test
history for each sample cycle. Data for each printout consist of a code num-
ber or filter number, date/time data, and sampler function designator.
Figure 2.5.10 shows a typical printout.
Reset Procedure—Depressing the RESET key clears all of the instructions
except clock time to allow entry of a new set of instructions. Sampler
operation is terminated and the filters are cycled to the tray if the instru-
ment is sampling. Date/time information is not printed at reset.
Depressing RESET while the tray is at any filter slot other than number
one results in an INDEX ERROR indication. The filter tray must be reseated
at filter number one, followed by depressing the RESET key to enter new in-
structions.
Depressing RESET while the tray is at filter slot number one immediately
resets the program to the input mode. START TIME and DAY will light; input
data may now be entered.
-------
Section No. 2.5
Revision No. 0
Date 5/7/80
Page 23 of 44
CODE
# 2
# 3
* 4
# 5
# 1
# 2
# 3
# 4
# 5
DAY
1 2 8
000
0 0 1
1 2 8
1 2 8
000
0 0 1
HR MIN
1 n n ^ *• .
n R n n * , , .
On n n <
n ° ^ ,
1 o n n «
1003
0600
0000
0 2
FILTER
NO.
0 1
0 1
0 2
0 2
0 3
0 3
0 4
0 4
0 1
0 1
DAY
1 2 8
1 2 8
1 2 8
1 2 8
1 2 8
1 2 8
1 2 8
1 2 8
1 2 8
1 2 8
1 2 8
1 2 8
HR MIN CODE
1 n fi 1 ° .*-
1 n n ° T — -
1003 S
1 n n ? M-*.
1004 S
1 n n 4. A -— -
1004 S
1 n n A •*-
1 n n ^ i •*-
1006 T
1008 S
i n n P Y-*_
PROGRAMMED INPUT
air
Automatic printout at sampler start
OPERATIONAL PRINTOUT
me
mode
Figure 2.5.10. Typical printout from the Beckman SAMPLAIR.
-------
Section No. 2.5
Revision No. 0
Date 5/7/80
Page 24 of 44
Interrupt Procedure—The INTERRUPT sequence allows the operator to in-
terrupt a pumping cycle, change filter trays, and/or preselect a specific
filter, and then to continue sampling with the existing instructions intact.
Depressing the INTPT key terminates the pumping cycle, recycles the fil-
ters to the tray, and switches the program into a "wait" mode. During this
mode, all LEDs are turned off.
When all LEDs are off, filter trays may be changed as the carriage
assembly is reseated at filter number 1. The sampling sequence is continued
on filter number 1 by depressing the CONT key. If sampling is to continue
at some other filter, depress the TRAY ADV key followed by a two-digit num-
ber, 01 through 36, for the selected filter. The trays will advance to the
selected filter. When the trays stop, depress the CONT key and sampling will
continue in the initial timing sequence.
The pumping time on the first filter after the interrupt cycle is the
balance of the initial pumping interval. An example of the INTERRUPT timing
is shown in Figure 2.5.11.
2.5.3.4 Description of Keypad—
INTPT INTPT key interrupts -the sampler during automatic cycling
and forces the program into a "wait" mode. The key is active
during automatic sampler operation. Instrument operation
following actuation of the INTPT key depends on the operat-
ing mode at the time the key is depressed.
Actuating the INTPT key during the filter insertion cycle or
during the seal closure cycle results in a 5-second pumping
time followed by the seal opening and recycling filters to
the tray. The designator "X" and calendar date/time infor-
mation are printed at completion of the pumping cycle.
Actuating the INTPT switch during the pumping cycle causes
the pump to turn off, and filters are recycled to the tray.
The designator "X" and date/time are printed at completion
of the pumping time.
Actuating the INTPT key during the seal opening cycle or dur-
ing the shuttle return cycle forces the instrument into the
"wait" mode after the filters are recycled to the tray. The
"X" designator is not printed.
PRINT CLOCK Depressing the PRINT CLOCK key prints the current calendar
date/time information. This key is disabled only during
-------
Section No. 2.5
Revision No. 0
Date 5/7/80
Page 25 of 44
•
44- O
TT £
• ! r*
TT 0
# 4
# 5
226
000
000
1332
0005
0000
3 6
0 1
0 1
2 0
2 0
2 1
2 1
3 4
3 4
3 5
3 5
0 1
0 1
0 2
0 2
226
226
226
226
226
226
226
226
226
226
226
226
226
226
1332
1333
1335
1337
1337
1337
1341
1342
1343
1344
1344
1348
1348
1353
S
X
S
T
S
X
S
T
S
X
S
T
S
T
-« Start date/time
-* Sample time— 5 minutes
•^ Zero delay— continuous modej
** Start-filter #1
<* INTPT
-* Tray advanced to filter #20
•* Start pumping #20
-* Terminate pumping— 5 minutes from
start of filter #1
~* Start #21
-« INTPT
-* Advance tray to filter #34
*« Start #34
-*^: Terminate pumping— 5 minutes from
start of #21
•* Start #35
-« INTPT
•* Insert new filter tray
-* Start filter #1
«« Terminate #1—5 minutes from
start of #35
•« Start #2
•+ Terminate #2 after 5 minutes
of pumping
Figure 2.5.11. Printout showing interrupted timing in the Beckman SAMPLAIR.
-------
Section No. 2.5
Revision No. 0
Date 5/7/80
Page 26 of 44
RESET
printer operation, and is active at all other times. A typ-
ical clock printout is shown in the Printer Format descrip-
tion.
Depressing the RESET key terminates the sampling mode, recy-
cles the filters to the tray, and resets all input program
data. The RESET key is active at all times after' initially
entering the calendar date/time information.
Resetting the sampler will cause a TRAY INDEX error signal
if the RESET key is actuated while sampling filter pairs
other than pair number one. Following filter recycle, the
RESET key must be depressed before entering operating data.
This key is used in conjunction with the INTPT key to allow
selection of a specific filter pair for the next sampling
position. The key is active only after the INTPT key is de-
pressed.
The TEST key selects the instrument self-test mode. Depres-
sing the TEST key followed by a numerical key elects a speci-
fic self-test routine. This key is active only at power on,
before entering calendar clock data, and following the com-
pletion of sample pair number 36. The key is inactive dur-
ing sampler operation.
CONT (Continue) This key restarts sampler operation under the initial timing
parameters. The key "is active only after depressing the
INTPT key and following sample completion of filter pair num-
ber 36. ,
TRAY ADV
(Tray advance)
TEST
2.5.4 Recording the Field Data
The site operator(s) is responsible for keeping records pertaining to
sample identification and sampler operation. Sampling information will be
recorded on data sheets like the one shown in Figure 2.5.12. A new data
sheet should be used whenever the sampler rotameter setpoint is changed.
Return data sheets at least quarterly to: Environmental Protection Agency,
EMSL (MD-76), Research Triangle Park, NC 27711, ATTN: Inhalable Particulate
Network.
Each exposed sample filter will be placed in a separate envelope along
with an IP Network data card (Figure 2.5.13) completed from information on
the data sheets. A note should be made of any unusual adverse weather condi-
tions (e.g., high winds, rain, or dust from nearby construction) and sent to
the laboratory with the IP data card. The IP data card is designed to be
-------
Site Number:
Beckman Automated Dichotomous Sampler
Location: Simpler S/N:
Flow rites: Set COARSE rotameter at
for 1.67 L/min.
Set FINE rot
Data
Initials
COARSE
filter
number
FINE
filter
number
Final
COARSE
rotameter
reading
imettnt for 1500
Final
FINE
rotameter
reading
Average
COARSE
rotameter
reading
,/min.
Average
FINE
rotameter
reading
Elapsed
time
minutes
Remarks
-0 0 ?0 CO
id r+ < O
ft) (t) ->• <-+
ro en -j- o
^J \ o n
0 "\ Z
— H CO O
If sampler automatically changes filter sets during a sampling period, enter each set separately. Use a new data sheet whenever rotameter setpoint(s) is changed. Return data sheets f-^ . fsj
to MD 76 at RTP at least quarterly. o ^-,
Figure 2.5.12. IP Network data sheet.
3/28/79
-------
Donotwnun ow»i
INHALABLE PARTICULAR NETWORK
SoreonCeb*
\c\s\
RltwTyp.
1 • Ht-Vot
2-SSJ-HWoi
Sour
Na
9-o»i
Yr
(3-11)
Ma Orr
(15-20)
RlwNc.
HI Lil I°I7I
(12) (13-141
St Hf Tim*
(21-22) (23)
(24-30)
EnwX
a
(2)
(31-35)
LACS
I/I Vl VI71
I3»3»
KOMdi.%
am
(4O43) QM. IMVT1
INHALABLE PARTICULATE NETWORK
1
Do not «*ra in tfm itwc» 1
1
1
FrtwTyp.
1 - Ht-Vol Erar
2 • SSI-Ht-Vol ' No.
3 • Com Oicnat ju j
4 - Fin* Dienot ~
a.om«»
Enar X
Colloand SvnpM Q
(2!
Z/?(^S
iten^n NVIM
SaLoaaon
Stnm Cod* Aowcy Proj*et
^[s|v
/ |f|'4<
c. Questionable data card
J^X '
Figure 2.5.13. Sample IP data cards-completed for Beckman dichotomous sampler.
-------
Section No. 2.5
Revision No. 0
Date 5/7/80
Page 29 of 44
keypunched using 43 of the normal 80 columns. The coding will follow the
EPA SAROAD format as used in previous networks, including site numbers.
2.5.4.1 Logbooks-
Each sampling site will be supplied with a bound logbook in which infor-
mation should be recorded in a diary format. This log should indicate when
sampler maintenance is performed, periods when samplers are out of service,
dates of field calibration checks and audits, unusual occurrences such as
power outages, dates of sampler replacements, operating personnel changes,
etc. This log will be used to help identify unusual trends or patterns that
may be site-, operator-, or sampler-induced.
2.5.4.2 Flow Rate Measurement and Reporting--
Prior to the start of each sampling period, the coarse and fine rotame-
ters are adjusted to predetermined setpoints to yield flows of 1.67 L/min
and 15.0 L/min, respectively. Therefore, initial rotameter readings [I^(i),
I (i)] will always be the setpoints.
At the end of a sampling period, final rotameter indications
[If(f), I (f)] are read and recorded. If the final "fine" rotameter indica-
tion is between 13.5 and 16.5, i.e.,-15.0 L/min ±10 percent, and the final
"coarse" rotameter indication is -between 1.50 and 1.84, i.e, 1.67 L/min ±10
percent, the average flow rates are calculated. The average flow rates are
calculated by:
Average fine flow rate K = (If(i) + If(f))/2, and
Average coarse flow rate I = (I (i) + I (f))/2.
However, if either the final "fine" or "coarse" rotameter indication is
outside its respective range as given above, the sample is invalidated. Re-
cord initial, final, and average readings for the fine and coarse rotameters
on the IP network data sheet of Figure 2.5.12.
2.5.4.3 Completing the Data Card(s)—
Each exposed filter should be sent with the IP data card to: Inhalable
Particulate Filter Bank, Environmental Protection Agency, Mail Drop 8, Re-
search Triangle Park, NC 27711.
-------
Section No. 2.5
Revision No. 0
Date 5/7/80
Page 30 of 44
The data cards should be filled out in the following manner (see Figure
2.5.13):
a. Station name
b. Site location
c. Filter type (1)
d. Collocated sample (2): An IP Network sampler located at the
site for comparison with a second Network sampler of the same
type at that site.
e. Station code (3-11): SAROAD code. The first two digits refer
to state, the middle four to station, and the last three to
site.
f. Agency (12): A (SAROAD code for EPA).
g. Project (13,14): 07 (SAROAD code for IP Network).
h. Date sample was run (15-20).
i. Starting hour (21,22): 00 (SAROAD code for midnight).
j. Time (23): 7 (SAROAD'code for 24-hr sampling period).
k. Filter number" (24-30): Identification number on the filter's
petri dish or the filter itself.
1. Sampling rate (31-35): After averaging the initial and final
air flow rate obtained from the rotameter, refer to the most
recent calibration table to find the actual flow rate in m3/
min.
m. Minutes sampled (36-39): Total minutes sampled taken from
elapsed time meter.
n. QC Check, % (40-43): Performed every other sampling period.
o. Operator's initials, lower right corner.
2.5.5 Sample Validation
2.5.5.1 Validation Criteria—
In order to assist the operator in determining whether a sample is
valid, the following validation criteria have been established for all IP
Network samples:
-------
Section No. 2.5
Revision No. 0
Date 5/7/80
Page 31 of 44
1. Timing
All samplers must turn ON and OFF within 1/2 hour of mid-
night.
All samplers must operate for at least 23 but no more
than 25 hours.
2. Flow Rates
Decreases in flow rate during sampling of more than 10
percent from the initial setpoint are questionable.
Changes in flow rate calibration of more than 10 percent,
as determined by a field calibration check, will invali-
date all samples col lected. back to the last acceptable
flow check.
3. Fi1ter Quality
All particulate deposits that do not have well-defined
borders (possible leak) should be voided.
Any filter that is obviously damaged (i.e., torn or
frayed) should be voided.
2.5.5.2 Handling of Valid Samples—
1. Calculate flow rates and fill out IP Network data cards com-
pletely (see Section 2.2.2, Figure 2.5.13a).
2. Send the filters in the cassettes accompanied by the complet-
ed data cards to EPA-RTP, MD-8, for weighing and analysis
according to the preestablished schedule. This procedure
guarantees a smooth flow of samples to the laboratory.
2.5.5.3 Handling Invalid Samples--
When a filter is determined to be invalid for any of the previous rea-
sons:
1. Complete as much of the IP data card as possible (Figure
2.5.135).
2. Mark "VOID" in the lower right corner and explain.
3. Mark "VOID" in the logbook and on the data sheet.
-------
Revision No. 0
Date 5/7/80
Page 32 of 44
4. Do not discard the filter.
5. Mail filter with data card to EPA-RTP, MD-8, where a final
decision on sample validity will be made.
2.5.5.4 Handling of Questionable Samples—
If uncertain as to whether or not a sample should be voided, the opera-
tor should:
1. Complete as much as possible of the IP data card (Figure
2.5.13C).
2. Put a circled question mark in the lower right corner along
with a short explanation.
3. Mark "Questionable" in the logbook and on the data sheet.
4. Mail filter with data card to EPA-RTP, MD-8, where a- final ~
decision on sample validity will be made.
2.5.6 Operator's Field Calibration Check Procedures
During routine IP Network operation, the operator will be required to
check the calibration of the instruments every other sampling period. Cali-
bration checks of the sampler flow rate require the instruments to be run-
ning, and hence that timed operation of the master timer be bypassed. Pro-
cedures for operation of the master timer and field calibration checks of
the samplers are given below.
2.5.6.1 Operation of the Tork Time Control (Master Timer)—
All samplers are controlled by a master timer to ensure all samplers
operate for a 24-hour period every sixth day. The operator does not need to
be concerned with the master timer except when the timer must be bypassed
for field calibration checks, or in the event of a power failure. However,
the operator should check the master timer at each sample change to make sure
that the next sampling period will be correct.
2.5.6.1.1 Bypassing the master timer during field calibration checks--
The samplers must be operative during the calibration check. Since the cali-
bration check cannot be accomplished when the equipment is collecting a sam-
ple, the master timer must be bypassed. To bypass the timer:
-------
Section No. 2.5
Revision No. 0
Date 5/7/80
Page 33 of 44
1. Refer to the timer in Figure 2.5.14.
2. Rotate the skip wheel until the day indicator is pointing to
the sampling day (lug removed).
3. Power is now supplied to all samplers.
4. To turn power off, rotate the skip wheel to a no-sampling day
(lug in place).
5. When the calibration is complete, reset the timer as described
in the next section.
2.5.6.1.2 Resetting the master timer after power failure £r field
calibration check—
1. Set the hour dial so that the station time is opposite the
hour indicator.
2. Set the skip wheel so that the number of lugs (clockwise) be-
tween the missing lug and the day indicator is equal to the
number of days before the next sampling date.
2.'5. 6. 2 Equipment--
The following equipment is required for a field calibration check:
Calibrated orifice (Figure 2.5.15)
Beckman dichotomous sample "fine" and "coarse" rotameter calibra-
tion curves (Figures 2.5.16 and 2.5.18) and interpolation tables
(Figures 2.5.17 and 2.5.19)
Orifice calibration curve (Figure 2.5.20) and interpolation table
(Figure 2.5.21)
Manometer or magnahelic gauge
IP Network Flow Check Data Sheet (Figure 2.5.22).
2.5.6.3 Field Calibration Check Procedure--
A field calibration check of the total flow rate rotameter is required
after every other sampling period for the Beckman dichotomous sampler. The
check is made by installing an orifice device (Figure 2.5.15) calibrated in
the operating range of the flowmeter. The calibration of the orifice device
is performed by EPA's Environmental Monitoring Systems Laboratory (EMSL)
located in Research Triangle Park, N.C. The laboratory calibration proce-
dure is fully described in Section 5.8.2.1 of this manual.
-------
Section No. 2.5
Revision No. 0
Date 5/7/80
Page 34 of 44
MICRO SWITCH
ACTUATOR
ARM
HOUR
INDICATOR
6-LUG
SKIP WHEEL
MISSING LUG
DAY
INDICATOR
Figure 2.5.14. Tork master timer.
-------
8
18 NPT
•% O.D. TUBING
PLUNGE MILL % x 0.040 DP.
DRILL THRU NO. 55
PIPE NIPPLE (4")
ORIFICE PLATE
Figure 2.5.15. Calibration orifice assembly for IP Network dichotomous sampler.
~O O 70 GO
B) CU CD fD
IQ C+ < O
O) — '• r+
cn -<•
oo cn -•• o
in \ o o
o "^
-h CD
o
o
• r-o
CD en
-------
INHALED PARTICIPATE NETWORK
BECKMAN DICHOTOMOUS SAMPLER EPAtf 176108 S/N 056-909
FINE ROTAMETER CALIBRATION BY M. WILKINS
cu
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01
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a:
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20.
16.
14.
-00
10
Data Point* - 3
Slaf>»(A)~ 0.9896
Jnttroopt Of) - 2. 0914
(R) ~ 0. 9922
'.-00
6.00
1H.00
SETPOINT- 14.21
—i
12.00 14.00 16.00
18.00 20.00
ROTAMETER READING
Figure 2.5.16. Sample calibration curve for Beckman "fine" rotameter.
T3 O 33 l/l
O> (D (D (!)
CQ r+ < n
(I) (D -<• r+
cn —J.
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-------
INHALED PARTICIPATE NETWORK
BECKMAN DICHOTOMOUS SAMPLER EPAtf 176100 S/M 056-909
COARSE ROTAMETER CALIBRATION BY M. WILKINS
UJ
o:
2.00
1.75
1.58
1.25
1.00
0.75
0.50
0.25 ..-
0 4-
_m „ ,_,
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Slap«W~ 'J.B617
Jntoru»f>t (D)« O.
Coefficient - 0. 9965
0.25
0.75
1.00
1.25
KETPOINT- 1. OU
1.50
i.751
2.00
ROTAMETER READING
Figure 2.5.18. Sample calibration curve for Beckman "coarse" rotameter.
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(U PJ (T> CD
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n> a> ->• H-
Ut -••
co en -•• o
Co ^\ o 3
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Figure 2.5.19. Sample interpolation table for Beckman "coarse" rotameter calibration.
~o r~i ^o (y">
(u 0) ft) (t>
U3 r+ < O
(D (D —'• r^
tn —'•
CO cn —•• O
UD ~-\ O 3
C»
o
-------
INHALED PARTICULrATE NETWORK
DICHOTOMOUS FLOfcKJRIEICE CALIBRATION
EXPDNT 0.463812
FACTOR 0. 007
C. COEF 0. 9S957
CALIB. BY
1
DCT ORFiCIPD-45
DATE 10/ 30/ 79
23. 0 C
759f 5
6 7 G 9 10 11 12
MANOMETER READING^ IN H2O
Figure 2.5.20. Sample dichotomous flow orifice calibration curve.
.UuA+4j
"P O ^O U~l
cu 0) rp ID
IQ r* < n
(t) (D ->• c+
in —>•
4* en -•• o
o ^. o rj
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o \ z
-•» CD O
o z •
^=> o
-t» • ro
o tn
-------
****** AUDIT ORIFICE
MAN
RDO
0.0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
O.B
0.?
1.0
1.1
1.2
1.3
1.4
1.3
1.6
1.7
1.8
1.9
2.'0
2.1
2.2
2.3
2.4
2.3
2. A
2.7
2.8
2.9
3.0
3.1
3.2
3.3
3.4
3.3
3. A
3.7
3.8
3.9
4.0
4.1
4.2
4.3
4.4
4.5
4. A
4.7
4.B
4.9
5.0
SLPM
0.0000
2.5563
3.5256
4.2551
4.B625
5.3927
5.B6B6
A. 3035
A.70A3
7.0B2B
7.4373
7.7737
8.0938
8.4000
B.A937
B.97A4
9.2492
9.312?
9.7A83
10.016A
10.2377
10.4925
10.7213
10.9447
11.1A29
11.3762
11.3631
11.7896
11.9902
12.1869
12.3B01
12.5698
12.7363
12.9396
13.1200
13.297A
13.4725
13.A44B
13.9146
13.9821
14.1472
14.3102
14.4710
14.6298
14.7867
14.9416
15.0947
15.2460
15.3956
15.5436
15.6B99
M3/MIN
0.0000
0.0026
0.0035
0.0043
0.0049
0.0054
0.0059
0.0063
O.OOA7
0.0071
0.0074
0.0078
O.OOB1
0.0084
0.0087
0.0090
0.0092
' 0.0093
0.0098
0.0100
0.0103
0.0105
0.0107
0.0109
0.0112
0.0114
0.0116
0.0118
0.0120
0.0122
0.0124
0.012A
0.0128
0,0129
0.0131
0.0133
0.0135
0.0136
0. 01'38i
0.0140
0.0141
0.0143
0.0145
0.014A
0.014B
0.0149
0.0151
0.0132
0.0154
0.0155
0.0157
MAN
RDO
5.1
5.2
3.3
5.4
5.5
5.6
5.7
3.8
3,9
A.O
6.1
A. 2
A. 3
A. 4
ft. 3
A. A
A. 7
A. 8
A. 9
7.0
7.1
7.2
7.3
7.4
7.5
7. A
7.7
7.8
7.9
8.0
8.1
8.2
8.3
8.4
8. '3
8. A
8.7
8.8
8.9
9.0
9.1
9.2
9.3
9.4
9.5
9.6
9.7
9.B
9.9
10.0
10.1
SLPH
15.8347
15.9779
16.1197
16.2601
16.3990
16.5367
16.6730
16.80BO
1A.941B
17.0744
17.205B
17.3360
17.4652
17,3932
17,7202
17.8461
17.9710
18.0949
18.2179
18.3398
18.4609
18.5810
18.7003
18.8187
18.9362
19.0529
19, 1688
19.2838
19.3981
19.3116
19,6244
19.7364
19.8476
19.93B2
20.06BO
20.1772
20.2857
20.3935
20.5006
20.6072
20.7130
20.8183
20.9230
21.0270
21 .1305
21.2333
21.3356
21.4374
21.5386
21 .6392
21.7393
M3/MIN
0.0158
0.0160
0.0161
0.0163
0.0164
0,0165
0.0167
0.0168
0.0169
0.0171
0.0172
0.0173
0.0175
0.0176
0.0177
0.017B
0.0180
0.0181
0.01B2
0.01B3
0.01B5
0.01B6
0.0187
0.01B8
0.0189
0.0191
0.0192
0.0193
0.0194
0.0193
0.0196
0.0197
0.0198
0.0200
0.0201
0.0202
0.0203
0.0204
0.0205
0.0206
0.0207
0.0208
0.0209
0.0210
0.0211
0.0212
0.0213
0.0214
0.0215
0.0216
0.0217
MAN
Rno
10.1
10.2
10.3
10.4
10.5
10.6
10,7
10.8
10.9
11.0
11.1
11.2
11.3
11.4
11.5
11. A
11.7
11.8
11.9
12.0
12.1
12.2
12>3
12.4
12.5
12. A
12.7
12,8
12,9
13.0
13,1
13.2
13.3
13.4
13,5
13. A
13.7
13.8
13.9
14.0
14.1
14.2
14.3
14.4
14.5
14.6
14.7
14.8
14.9
15.0
15.1
SLPM
21.7393
21.03(39
21.9379
22.0364
22.1345
22.2320
22.3290
22.4256
22.5216
22.6172
22,7124
22.8070
22.9013
22.9950
23.0884
23. 1813
23.2738
23.3658
23.4574
23,5487
23.6395
23.7299
23.B199
23.9095
23.9988
24.0876
24.1761
24.2642
24.3520
24.4393
24.5264
24.6130
24.6993
24.7B53
24.8709
24.9562
25.0411
25. 1257
25.2100
25.2940
25.3776
25.4609
25.5439
25.6266
25.70-90
25.7911
25.0729
25.7544
26.0356
26. 1165
26. 1971
M3/MIN
0.0217
0.0218
0.0219
0.0220
0.0221
0.0222
0.0223
0.0224
0.0225
0.0226
0.0227
0.0228
0,0229
0.0230
0.0231
0.0232
0.0233
0.0234
0.0235
0,0235
0.0236
0.0237
0.023B
0.0239
0.0240
0.0241
0.0242
0.0243
0.0244
0.0244
0.0245
0.0246
0.0247
0.0248
0.0249
O.O250
0.0250
0.0251
0.0252
0.0253
0.0254
0.0255
0.0255
0.0256
0.0257
0.0250
0.0259
0.0260
0.0260
0.0261
0.026?
MAN
RUG
15.1
15.2
15.3
15.4
15.5
15.6
15,7
15,8
15,9
16.0
16.1
1A.2
16.3
16.4
16.3
16.6
16.7
16.8
16.9
17.0
17.1
17.2
17,3
17.4
17.3
17.6
17.7
17.8
17.9
1B.O
18.1
18.2
IB. 3
18.4
18.3
IB. 6
IB. 7
1(3.8
18.9
19.0
19.1
19.2
19.3
19.4
19.5
19.6
19.7
19. Q
17.9
20.0
20. 1
SLPM
26.1971
26.2774
26.3574
26.4372
26.5167
26.5959
26.6748
26.7535
26.8319
26.9100
26,9879
27.0653
27,1429
27,2200
27.2969
27.3735
27.4498
27.3260
27.6018
27.6775
27.7528
27.B2BO
27.9029
27.9776
28.0521
28.1263
28,2003
28.2741
28,3477
28.4210
28.4941
2B.5671
2B.A397
28.7122
28.7845
28.8566
28.9284
29.0001
29.0715
29.1427
29.2138
29.2846
29.3553
29.4257
29,4960
29.5660
29.6359
29.7056
29.7751
29.8444
29.9135
M3/MIN
0.0262
0.0263
0.0264
0.0264
0.0265
0.0266
0,0267
0.0268
0.0268
0.0269
0.0270
0.0271
0.0271
0.0272
0.0273
0.0274
0.0274
0.0273-
0.027A
0.0277
0.0278
0.0278
0.0279
•0.02BO-
0.0281
0.02B1
0.02B2
0.0283
0.0283
0.0284
0.0283
0.0286
0.028A
0.0287
0.0288
0.0289
0.0289
0.0290
0.0291
0.0291
0.0292
0.0293
0.0294
0.0294
0.0295
0.0296
0.0296
0.0297
0.0298
0.0290
0.0299
~D O 33 CD
(D OJ fD CD
(Q C»- < D
(T> — '• <-f
in — ".
_£> (_n _i. o
f-1 \ O 3
CD
O
• ro
o in
Figure 2.5.21. Sample interpolation table for clichotomous flow orifice calibration.
-------
SAROAD sits number:
£,
—1
U
I
%
0
Q
(\
£
Location:
Data: _
/-
IP NETWORK
Flow Check Data Sheet
Atmospheric pressure:
Temperature: -
Section No. 2.5
Revision No. 0
Date 5/7/80
Page 42 of 44
mm Hg, in. Hg
os
Operator
Sampler EPA Number:
Month
Date
TSP HIVOL
Year
SSI HIVOL
MAN. DICHOT { ) AUTO DICHOT
LU
h-
e
3
a
_j
u.
Dieksan/ratamfltBr reading^)
A P.narot pfrranwtBr- ' / • £ S
R Finn m«mirt,t- / ^ , O ^
C Total rotamatur-
D Diekmn reenrdafr , .
Total sampiar flow raffi! (1) ' J / 5 7
Sampler flow rates m /min*
A Cnarn rntamatBr- _ - - -^ / . ~
B Finn rntamemr- • Oim / 3 ^
C Tiffa) riwamRTpr-
D Diclcuin racnrriar;
m3/min (A-+ B, C. or D)
LU
^
<
s
C
.J
LU
Qrifica serial number! . ,J~P C) - V^r" r.ailhration data / " . ' ,- "
f ->
.Qrifica manomatBrmBdinq: ,.-"..; . _ , 'PCh<« HnO
Qrifics flow rate: (21 , O / ^ f .. . m3/IT,jn
Calculations
Percent error
(2)
X 100 = (3)
QC cheek % (3) + 100 « (4) J_ £1 _2_ . Ji %
Entar (4) in spaces 4043 on IPN Data Card
*Flow rates determined from sampler calibration curve.
Figure 2.5.22. IP Network Flow Check Data Sheet.
-------
Section No. 2.5
Revision No. 0
Date 5/7/80
Page 43 of 44
There are two separate flow paths (Figure 2.5.1) for the operation of
the virtual impactor- These two flow systems have a total flow rate of
16.7 L/min (1 m3/hr). Ninety percent of the flow (15.0 L/min) passes
through the fine side and 10 percent (1.67 L/min) through the coarse side.
The flows through each individual leg are adjusted separately 'by needle
valves and monitored with rotameters. At the present time only the total
flow rate is checked against the calibration check orifice device. It is
expected that in the near future, individual checks for the "coarse" and
"fine" rotameters will be approved and incorporated into this procedure. To
check the field calibration:
i
1. Shuttle clean filters into both" the "fine" and "coarse" side
of the sampler as described in sampler operation procedure
(Section 2.5.3.2).
2. Remove the sampler head from the sampler and replace with the
"total" flow calibration check orifice device (Figure 2.5.15).
3. Turn on the sampler and allow it to warm up to operating tem-
perature (approximately 5 minutes).
4. Adjust both the "fine" and "coarse" rotameters to their re-
spective setpoints as recorded on the laboratory calibration
curves (Figures 2.5.16 and 2.5.18) or interpolation table
(Figures 2.5.17 and 2.5.19).
5. Observe the pressure drop, AP, across the orifice, and its
corresponding flow rate from the calibration data (Fig-
ures 2.5.20 and 2.5.21) provided with the orifice. Record
both values on the IP Network Flow Check Data Sheet (Fig-
ure 2.5.22). Also record the rotameter setpoints and their
corresponding flow rates on the data sheet.
6. Add the "fine" and the "coarse" flow rates to obtain the
"total" sampler flow rate.
7. Using the above information, and the formulas provided in the
IP Network Flow Check Data Sheet, calculate the QC Check %.
Record this value on the Flow Check Data Sheet and the IP data
card (Figure 2.5.13).
8. If the calculated QC Check % is within ±10 percent of
16.7 L/min total flow, the sampler is operating properly.
Return the Flow Check Data Sheet to:
-------
Section No. 2.5
Revision No. 0
Date 5/7/80
Page 44 of 44
Environmental Protection Agency
EMSL (MD-76) "
Research Triangle Park, NC 27711
ATTN: Inhalable Participate Network
9. Turn off the sampler, remove the orifice device, and replace
the standpipe.
10. Remove the filters from both "fine" and "coarse" channels of
the sampler.
11. Set the sampler up for the next samping period according to
bet the sampler up tor tne nex
the procedure in Section 2.5.3.1
12. If the calculated QC Check % is greater than ±10.0 percent of
16.7 L/min total flow rate, this usually indicates that the
fine flow filter is not sealed properly. Using gloves, gently
push back and forth on. the filters. If one is not properly
sealed it should snap into place. The pressure drop (AP)
across the orifice device should now yield a QC check value
within 10 percent of the setpoint, 16.7 L/min. If the QC
check value is still outside the ±10 percent range, try
another set of filters. If this does not yield a QC check
value within the ±10 percent of the setpoint, the sampler re-
quires recalibration. Record the value on the Flow Check Data
Sheet (Figure 2.5.22) and contact the IP Field Manager (Mack
Wilkins, 919/541-3049) to arrange for recalibration. Send
the Flow Check Data Sheet to the address above.
-------
Section No. 2.6
Revision No. 0
Date 5/7/80
Page 1 of 33
2.6 OPERATING PROCEDURE FOR THE SIERRA 244 and 244E DICHOTOMOUS SAMPLERS
2.6.1 Introduction
This section presents operating procedures for the Sierra Series 244
Dichotomous Sampler and the modified 244E Dichotomous Sampler. In large
part, these operating procedures were taken from the Instruction Manual,
Series 244, published by Sierra Instruments, Inc. The procedures have been
modified and/ or expanded where necessary to conform to IP Network practices.
2.6.2 Description of the Sierra Series 244 Sampler and 244E Dichotomous
Samplers
2.6.2.1 General--
The dichotomous sampler is a low flow rate (16.7 L/min) sampler that
divides the air stream passing the 15-um inlet into two portions that" are
filtered separately. It is often referred to as a "virtual" impactor since
the particle size separation is accomplished by pseudo-impaction into an air
stream of differing velocity, rather than onto an impaction surface. The
current IP dichotomous samplers cut the 0- to 15-um total sample into 0- to
2.5-um "fine" and 2.5- to 15-um "coarse" fractions that are collected on
separate 37-mm (diameter) Teflon filters. The "fine" and "coarse" concentra-
tions are determined gravimetrically and must be added to give the total IP
fraction.
Two models of manual dichotomous samplers are currently used-in the IP
Network. The Sierra Model 244 Manual Dichotomous Sampler (Figure 2.6.1) con-
sists of two modules: the sampling module and the flow control module.
Specifications for the Sierra Model 244 are given in Table 2.6.1. This sam-
pler is equipped with a digital timer/programmer and elapsed time indicator.
The digital clock has an LED display and d.c. battery standby. The 37-mm
diameter Teflon filters are shipped from the lab in nylon cassettes for ease
of loading and removal by the operator from the sampler module. The filters
remain in these cassettes during sampling and shipment.
The modified Sierra Model 244E Dichotomous Sampler (Figure 2.6.1) is
identical to the Model 244 except that the Model 244E has been modified so
that it can be calibrated at the control module as well as at the sampling
module. The 244E also uses a mechanical timer for operation instead of a
-------
VACUUM
GAUGE
Manual Dichotomous Sampler Flow Schematic (Sierra Model 244)
THOMAS
DIAPHRAGM
VACUUM PUMP
1.67 liiers/min
COARSE
FLOWMETER
EXHAUST
16.7 Q L/mIn
(1 m3/lir»
TOTAL
FLOW METER
MODEL 244
MODEL 244E
~o O ya 01
D» (U (D n>
UD r+ < O
n> n> -••«-*•
in —••
l\> (_n _•. O
^^ O ZJ
o -~J zj
00
CO CD Z
to o
• Particulates < 2.5 pm
o Particulates 2.5 to 15 ;mi
ho
CD CTl
Figure 2.6.1. Manual clichotomous sampler used in IP Network—Sierra Model 244 and 244E.
-------
Section No. 2.6
Revision No. 0
Date 5/7/80
Page 3 of 33
TABLE 2.6.1. SPECIFICATIONS FOR THE SIERRA MODEL 244
DICHOTOMOUS SAMPLER
Collection efficiency Mass median diameter at 50 percent collection effi-
ciency for equivalent spherical particles at g/cm3
is 2.5 pm; sigma "g" = 1.2.
Internal losses
Flow rates
Flowmeters
Concentration ratio
Vacuum pump
Timer/programmer
Elapsed time indicator
Filter media
Filter holder
Interconnecting tubing
Aerosol inlet
Power required
Overall dimensions
Net weight
Total shipping weight
Maximum value over range of 0 to 20 urn is less than
1 to 2 percent and occurs at 2.5 pm. Average loss
for all particles is less than. 1 percent.
Total flow: 1 m3/hr, or 16.7 L/min., fine-particle
flow: 0.9 ms/hr or 15.0 L/min; coarse-particle
flow: 0.1 m3/hr, or 1.67 L/min.
Precision rotameters, ±1.5 accuracy at above flows.
10:1
Diaphragm type, split phase motor, 1/4 hp.
Sierra Model 302 Digital Timer/Programmer; built-
in; all functions digital and quartz crystal con-
trolled, has digital clock with 1/2-in. LED display
and d.c. battery standby; includes first sample
period delay up to 9 days, sampler period of 1, 2,
3, 4, 6, 8, 10, 16, 20, or 24 hours, and skipped
time between "s'ample periods of 1 to 9 days.
XXXX.XX hours; nonresettable.
37-mm membrane or glass fiber; Teflon membrane
media recommended.
Circular, anodized aluminum, 1.750 inches O.D.
10 m long; 3/8 inch O.D. for fine-particle flow;
1/4 inch O.D. for coarse-particle flow.
15-um nominal cutpoint over approximately 0 to
20 km/hr wind speed range; includes bug screen.
115 V a.c. ±15 percent, 50-60 Hz, 200 W; 230 V a.c.
±10 percent, 50-60 Hz, optional-add suffix "X" to
model number.
Control module: 16"H x 22"W x H"D; sampling
module: 40"H x 25.63" Dia. tripod base bolt circle.
Control module: 50 Ib; sampling module: 15 Ib.
85 Ib.
-------
Section No. 2.6
Revision No. 0
Date 5/7/80
Page 4 of 33
digital timer/programmer. The Model 244E will eventually replace the Model
244 Samplers in the IP Network.
2.6.2.2 Flow System Description--
Figure 2.6.2 shows the principle of operation of the Sierra dichotomous
sampler; Figure 2.6.1 also shows a flow schematic. The coarse-particle flow
Q (0.1 rnVhr) is controlled by its flow selector valve, which feeds into
pressure P2 at the inlet of the pump. Flow Qc is relatively constant except
for small decreases in P4, which can occur during sampling. Because Qc is
small, an error in Q can cause an error of only about 10 percent in particle
mass concentration.
2.6.2.3 Control Panel —
The control panel is positioned behind a weathertight door and contains
vacuum gauge, rotameter, and digital timer/programmer displays. The control
panels for the Model 244 and 244E are shown in Figures 2.6.3 and 2.6.4,
respectively.
The functions of the various displays and controls are described below.
2.6.2.3.1 Flow control and measurement—Flow selector valves and rota-
meters are provided for setting the total and coarse-particle flow rates (Qt
and Q in Figure 2.6.1). Vacuum gauges measure the pressure drop across the
fine and coarse particle filters (P3 and P4 in Figure 2.6.1).
2.6.2.3.2 Digital timer programmer--(The Model 302 Digital Timer/Pro-
grammer is used on only a limited number of older Model 244 Sierra Dichoto-
mous Samplers; newer 244E samplers are equipped with a Paragon 7-day mechan-
ical timer).
1. Clock
a. Display-LED; 0.5 in. high; hours and minutes; 24-hr format.
b. Time Base—Quartz Crystal
c. DISPLAY Switch:
OFF display is turned off to prolong battery life; all
timing functions continue.
TIME OF DAY—Present time is displayed.
SAMPLE START TIME—Time, of day when sampling period
starts is displayed.
FAST/SLOW switch (both momentary; used for setting TIME
OF DAY and SAMPLE START TIME):
FAST—Minutes advance at 60 Hz rate.
SLOW—Minutes advance at 2 Hz rate.
-------
FROM AEROSOL INLET
FINE PARTICLES,
<3.5 tun
COARSE PARTICLES,
> 3.5 nm
FILTER
CASSETTE
FINE
PARTICLE
FILTER
Section No. 2.6
Revision No. 0
Date 5/7/80
Page 5 of 33
3
A
c
0.9 m3/hr
I
0.1 m3/hr
30-ft TUBING TO CONTROL MODULE
INLET TUBE
VIRTUAL
IMPACTOR NOZZLE
VIRTUAL IMPACTOR
RECEIVER TUBE
FILTER
CASSETTE
COARSE PARTICLE
FILTER, 37-mmdia.
Figure 2.6.2. The Sierra Models 244/244E virtual impactor, principle of operation.
-------
Figure 2.6.3. Control module for Sierra Model 244 dichotomous sampler.
-o O 70 tr>
CD O> CD (D
IQ <-l- < O
fl> fl> —'• r+
in —'•
cn en -•• o
"^ O 3
o -J r>
-h -\ Z
CO O
OJ CD Z •
U) O
CD en
-------
VACUUM VACUUM
COARSE
FLOW
Hnrni
^-X
ELAPSED TIME
OFF OFF OFF
66 6
ON ON ON
FLOW CALIBRATE
(oj
OUT
TOTAL
FLOW
(O) (O)
IN < OUT
COARSE
FLOW
ADJUST
O
TOTAL
FLOW
ON OFF
o
FUSE
SIERRA VIRTUAL IMPACTOR
MECHANICAL 7-DAY SKIP TIMER
(REPLACES MODEL 302 DIGITAL
TIMER/PROGRAMMER)
U
01 OJ
ta r+
ro ro
Co
ro
o
en —i. o
\ o r>
Figure 2.6.4. Control module for Sierra Model 244E dichotomous sampler.
oo
OO CD Z
CO O
(V)
CD CTl
-------
Section No. 2.6
Revision No. 0
Date 5/7/80
Page 8 of 33
2. SAMPLE AFTER Switch:
Sample After X Days. Delays start of first sampling period 0 to 8
days in 1-day increments.
3. SAMPLE EVERY Switch:
Sample Every Y Days. Permits sampling every 1 to 9 days in 1-day
increments.
4. SAMPLE FOR Switch:
Sample for Z hours. Sets number of hours sampler stays on--l, 2,
3, 4, 6, 8, 10, 16, 20, or 24 hours.
5. SAMPLER Switch:
a. ON--Sampler is turned on manually; timing is unaffected and
elapsed time runs.
b. TIMED—Sampler is controlled by timer.
c. OFF—Sampler is turned off; timer is unaffected.
6. SET Switch: Normally in DISPLAY position.
TIMER—Turns sampler off; resets all time functions (SAMPLE AFTER,
SAMPLE EVERY, and SAMPLE FOR), except the present time and SAMPLE
START TIME.
7. Power Fail: Flashing time display digits with DISPLAY switch on
indicates battery power failure. All timed functions must be re-
set. AC POWER FAILURE light indicates a.c. line power has failed
during a sampling period.
8. TOTAL SAMPLING TIME Display:-- Indicates the total elapsed time the
sampler is on; nonresettable; 9999.99 hours (416 days) before roll
over.
9. POWER/CIRCUIT BREAKER switch (115/230 V a.c. , 15 A):
a. UL approved; CSA approved.
b. ON—Push in; all power on; timing commences.
c. OFF--Push up; all a.c. power off; no sampling; optional bat-
tery continues to run timer.
10. Fast Check on Operation of the Model 302 Digital Timer/Programmer:
The operation of the 302 can be demonstrated or checked by setting
all functions of the 302 and then setting the clock in the FAST
mode. The 302 will start and stop the 302 on the programmed times.
However, because of the digital logic in the 302, SAMPLING PERIOD
can only be set to 24 hours for this fast check. Other sampling
times cannot be used, even though in real time they will function
properly.
-------
Section No. 2.6
Revision No. 0
Date 5/7/80
Page 9 of 33
2.6.3 Operation of Sierra Model 244 and 244E Dichotomous Samplers
2.6.3.1 General Operating Procedure--
The following is the operating procedure for both the Model 244 and
244E. (The operating procedure for the Model 302 Digital Timer/Programmer
is given in Section 2.6.3.2. )
1. Be sure the Sampling Module is clean and free of particulate depo-
sition on its inner surfaces. Be sure the bug screen is clean.
See Section 2.6.3.3 for cleaning details.
2. Bolt down the Sampling Module (optional). If desired, the Sam-
pling Module can be bolted down to the roof of the monitoring sta-
tion or other mounting surface. Use 10-32 or 1/4-20 bolts on a
25.63-in. bolt circle.
3. Unscrew the knurled filter holder nuts by hand. Install the fi-lter
cassettes containing the preweighed 37-mm diameter Teflon'filters
in the Sampling Module. Put both filter cassettes on the filter
screens. The lower half of the cassette goes over the filter
screen. The lower half is also the side having the shortest dis-
•tance (approximately 1/16 in.) to the filter surface. Screw on
both knurled filter holder nuts tightly by hand. The coarse-
particulate filter holder is the one with the 1/4-in. O.D. tubing
and the fine-particulate filter holder is the one with the 3/8-in.
O.D. tubing. As shown in f-igure 2.6.2, the filters can also be
distinguished by the fact that the coarse-particulate filter is on
the center-line of the virtual impactor head and aerosol inlet,
and the fine-particulate filter is offset. These are clearly
marked on the Model 244E.
4. Connect the two tubes. The 1/4-in. O.D. and 3/8-in. O.D. tubes
should be interconnected between the Sampling Module and the Con-
trol Module. First, hand-tighten the nuts on the tube connectors
as much as possible and then wrench-tighten 1-1/4 revolutions.
(This may already have been done by persons setting up samplers.)
5. Locate the Control Module either next to the Sampling Module or
remotely, as in a monitoring station. The Control Module can also
be bolted down to its mounting surface. The four bolt holes are
0.281 in. diameter and are in a rectangular pattern with dimen-
sions of 19-1/16 in. x 7-1/4 in. between centers.
6. Open the front cover of the enclosure of the Control Module. The
latch is opened by turning the knob counterclockwise and released
by turning the indicator one-quarter turn counterclockwise. It is
locked by reversing this process.
-------
Section No. 2.6
Revision No. 0
Date 5/7/80
Page 10 of 33
7. For Model 244, turn SAMPLER Switch on the Model 302 Digital Timer/
Programmer to OFF. For Model 244E, switch mechanical timer to
OFF.
8. Plug male cord into line voltage—Model 244: 115/60 Hz, 5 A maxi-
mum; Model 244E: 230/50 Hz, 2.5 A maximum.
9. Be sure the flow selector valve on the bottom of the total rota-
meter is open.
10. For the Model 244, turn SAMPLER switch on the Model 302 Digital/
Timer Programmer to ON. Turn mechanical timer switch on the
Model 244E to ON.
11. For the Model 244, depress the POWER switch on the 302. The pump
will turn on.
12. Set the total flow rate. Turn the flow selector valve on the Bot-
tom of the total rotameter to the setpoint indicated on the total
rotameter calibration curve (Figure 2.6.5) or interpolation table
(Figure 2.6.6) provided with the sampler to give a total flow rate
of 16.7 L/min. The vacuum gauge will read approximately 1 to 2
in. Hg for a 2- to 3-um pore size Teflon filter. The flow selector
valve will require, at most, only slight adjustment between sam-
plers.
13. Set the coarse flow rate. . lurn the flow selector valve on the
coarse rotameter to adjust the rotameter to the setpoint indicated
on the coarse rotameter calibration curve (Figure '2.6.7) or inter-
polation table (Figure 2.6.8) provided with the sampler to give a
coarse flow rate of 1.67 L/min. The vacuum gauge will read approx-
imately zero. The flow selector will require, at most, only minor
adjustment between samples.
NOTE: If either the Model 244 or 244E is operated at flow rates
other than those given above, particle size fractionation
will be inaccurate.
14. The Model 244 (and 244E) is now ready to sample. If desired, the
unit can be left on for manual (untimed) operation. The elapsed
time indicator will yield the sampling time. In most cases, sam-
pling is timed by the mechanical master timer (Section 2.6.6.1)
15. Close the front cover of the Control Module.
16. After sampling, remove both filter cassettes. Put the filter cas-
settes in the marked plastic petri dishes that contained the fil-
ters before sampling.
-------
INHALED PARTICULATE NETWORK
SIEKRA DICHOTOMOUS SAMPLER EPA0175479 S/N 216
TOTAL ROTAMETER CALIBRATION
a.
UJ
h-
•<.
a:
o
Data Point* - 6
Slop»(A)- 1.5639
(B) - -/. 1859
(R) - 0. 9995
Y-AX+B
2.03 4.00 8.00 8.00 10.00 12.00 14.00 10.00 IB. 00 20.00
ROTAMETER READING
Figure 2.6.5. Sample "total" rotameter calibration curve for the Sierra dichotomous sampler.
~O O TO Ln
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Figure 2.6.6. Sample interpolation table for Sierra "total" rotameter calibration.
-------
INHALED PARTICIPATE NETWORK
SIERRA DICHOTOMOUS SAMPLER EPA0175479 S/N 216
COARSE ROTAMETER CALIBRATION
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Figure 2.6.8. Sample interpolation table for Sierra "coarse" rotameter calibration.
-------
Section No. 2.6
Revision No. 0
Date 5/7/80
Page 15 of 33
17. Record sampling time from elapsed time indicator.
18. On the Model 244, note if A.C. POWER FAIL light is on.
2.6.3.2 Operating Procedure for the Model 302 Digital Timer/Programmer
(Sierra Model 244)--
NOTE: Under normal IP Network operating conditions, the Sierra
dichotomous sampler will be controlled by a master timer
used for control of all IP Network samplers at a partic-
ular site. Use of the Digital Timer on the Model 244 is
therefore likely only under special circumstances.
1. Open cover of enclosure.
2. Turn SAMPLER switch OFF.
3. Plug male cord into line voltage (110 V a.c. for 302, 220 V_a.c.
for 302X).
4. Push POWER switch ON (push in). Pump will not turn on. Set flow
controller, etc., of sampler. (See other instructions.)
5. Set SAMPLE START TIME of Day: (NOTE: Digits will flash until
set. )
NOTE: SAMPLE START TIME must be at least 10 minutes after
TIME OF DAY. The DISPLAY Selector Switch must not be
in the SAMPLE START TIME position 10 minutes prior to
sampling.
a. DISPLAY Switch: Set to SAMPLE START TIME.
b. FAST/SLOW Switch: Hold up or down as appropriate to set sam-
ple start time (24-hour format).
6. Set Present Time of Day (NOTE: Digits will flash until set):
a. DISPLAY Switch: Set to TIME OF DAY.
b. FAST/SLOW Switch: Hold up or down to set present time of day
(24-hour format).
7. Delay Start (Sample after X Days, 0-8 Days):
Set SAMPLE AFTER switch to number of days to be skipped before
first sampling period. Position "0" will initiate first sampling
period the first time the TIME OF DAY = SAMPLE START TIME. Thus,
for example, if the present time of day is 10:00 and the start time
is 8:00, the first sample will start in 22 hours. Position "1"
will delay the start 1 day (24 hours) after TIME OF DAY = SAMPLE
START TIME. Position "2" will delay start 2 days (48 hours), etc.
-------
Section No. 2.6
Revision No. 0
Date 5/7/80
Page 16 of 33
8. Skip Timer (Sample Every Y Days. 1-9 Days):
Set the SAMPLE EVERY switch to initiate 1 sample each Y days.
Position "1" samples every day. Position "2" samples every 2 days.
Position "6" samples every 6 days, etc.
9. Sampling Period (Sample for Z Hours, 1-24 Hours):
Set the SAMPLE FOR switch for the number of hours the 'sampler is
to remain on each sampling period.
NOTE: The switches referred to in steps 9, 10, and 11 are posi-
tive detent switches that provide exact timing. If the
switch is not in the detent, it is not usable.
10. Set Timer:
Push SET switch down to TIMER position for approximately 2 seconds.
NOTE: Steps 7, 8, 9, 10, and 11 can be done in any sequence,
but Step 12 must be done after Steps 7, 8, 9, 10,_ and
11.
11. Timed Sampling:
Place SAMPLER switch in TIMER position. This initializes all tim-
ing functions.
NOTES:
(1) Flashing time display indicates a.c. and battery power failure.
(2) AC POWER FAIL light (dot) indicates failure of a.c. power during sam-
pling period.
(3) Display may be left on; however, standby battery life may be shortened
if a.c. power fails.
(4) The Digital Elapsed Time Indicator (9999.99 hours maximum, nonresetta-
ble) records the total elapsed time the sampler is on (both TIMED and
ON positions of SAMPLER switch). A.C. power fail stops elapsed time
indicator until power returns.
(5) Power switch incorporates circuit breaker. When circuit is broken, the
power ON button pops up. If more than 15 A are drawn, the circuit
breaker will trip even if the button is held on (in). Reset is accom-
plished by pushing ON button in.
(6) Manual Operation:
The timer can be bypassed by placing the SAMPLER switch in the ON posi-
tion to independently turn the sampler on during noncycle periods. The
OFF position turns both timed and manual sampler power off.
-------
Section No. 2.6
Revision No. 0
Date 5/7/80
Page 17 of 33
2.6.3.3 Seven-Day Mechanical Skip Timer and Elapsed Time Indicator
(Model 244E)--
The Model 244E is provided with a mechanical 7-day skip timer. This
timer is supplied in lieu of the standard Model 302 Digital Timer/Programmer.
Timing accuracy is ±15 min/24-hr sampling period. Operating instructions
follow:
NOTE: Under normal operating procedures of the IP Network, the
Sierra dichotomous samplers will be controlled by a mas-
ter timer used for control of several instruments. Use
of the 7-day timer on the Model 244E is therefore likely
only under special circumstances.
1. Open front door of enclosure.
2. Turn TIMER switch OFF.
3. Plug male power cord of Sampling Module into line voltage (110 V a.c.,
60 Hz) going to master timer.
4. Set correct time on dial by grasping dial and rotating clockwise only
until correct day and time-of-day appear at the red pointer.
5. Set the elapsed time indicator to 0000.00 minutes by pressing the rec-
tangular button to the left of the-digits.
6. Check the 8-A "slo-blo" fuse by manually turning the sampler on.
7. Leave power on. The master timer will operate the sampler on the
scheduled sampling day.
2.6.4 Recording the Field Data
The site operator(s) is responsible for keeping records pertaining to
sample identification and sampler operation. Sampling information will be
recorded on data sheets like the one in Figure 2.6.9. A new data sheet
should be used whenever the sampler rotameter setpoint is changed. Return
data sheets at least quarterly to: Environmental Protection Agency, EMSL
(MD-76), Research Triangle Park, NC 27711, ATTN: Inhalable Particulate Net-
work.
Each exposed sample filter will be placed in a separate envelope along
with an IP Network data card (Figure 2.6.10) completed from information on
the data sheets. A note should be made of any unusual adverse weather con-
ditions (e.g., high winds, rain, or dust from nearby construction) and sent
-------
Sit* Number:
Sierra Manual Dichotomous Sampler (Models 244 and 244E)
Location:
Flow rates: Set COARSE rotimele
Set TOTAL lolimeUr at
Data
Initials
COARSE
filter
number
FINE
filter
number
Fine)
COARSE
rotameler
reading
r al for t R7 1 /min
lor
Final
TOTAL
rotametar
reading
COARSE
Average
reading
ivenje m /min
6.67 L/min.
TOTAL
Average
nadiiw
avaiaga m /min
FINE"
anreg.
m3/min
___
~- — -——______
' — - —
"~~~~ — — _______
" ~~ —-_____
~~~ _____
^~~~ — — — _____
- — _____
•
• — ______
" — — - —
" — _____
Elapwd
lima.
minutes
Remarks
Use a now data sheet whenever rotameter setpoint(s) is changed. Return data sheets to MD 76 at RTF at least quarterly. (Q <-*- < o
•FINE flow rate calculated by subtracting COARSE average m /min from TOTAL average in^/min. • t+
Figure 2.6.9. IP Network field data sheet for Sierra dichotomous samplers.
S '
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Co \ o n
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-------
1 INHALABL6 PAHT1CULATE NETWORK
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Section No. 2.6
Revision No. 0
Date 5/7/80
Page 19 of 33
a. Valid data card
b. Invalid data card
c. Questionable data card
Figure 2.6.10. Sample IP data cards completed for Sierra dichotomous sampler.
-------
Section No. 2.6
Revision No. 0
Date 5/7/80
Page 20 of 33
to the laboratory with the IP data card. The IP data card is designed to be
keypunched using 43 of the normal 80 columns. The coding will follow the
EPA SAROAD format as used in previous networks, including site numbers.
2.6.4.1 Logbooks-
Each sampling site will be supplied with a bound logbook in which in-
formation should be recorded in a diary format. This log should indicate
when sampler maintenance is performed, periods when samplers are out of
service, dates of field calibration checks and audits, unusual occurrences
such as power outages, dates of sampler replacements, operating personnel
changes, etc. This log will be used to. help identify unusual trends or
patterns that may be site-, operator-, or sampler-induced.
2.6.4.2 Flow Rate Measurement and Reporting—
Prior to the start of each sampling period, the "coarse" and "total"
rotameters are adjusted to predetermined setpoints to yield flows of 1.67
L/min and 16.7 L/min, respectively. Therefore, initial rotameter readings
[I 0), It(i)] will always be the setpoints.
At the end of a sampling period, final rotameter indications [I (f),
It(f)] are read and recorded. If the final "total" rotameter indication is
between 15.0 and 18.4, i,e., 16.7 L/min ±10 percent, and the final "coarse"
rotameter indication is between 1.50 and 1.84, i.e., 1.67 L/min ±10 percent,
the average flow rates are calculated. The average flow rates are calculat-
ed by:
Average total flow rate It = dt[i] + It[f])/2, and
Average coarse flow rate I = (I [i] + I [f])/2.
However, if either the final "total" or "coarse" rotameter indication
is outside its respective range as given above, the sample is invalidated.
Record initial, final, and average readings for the fine and coarse
rotameters on the IP Network data sheet of Figure 2.6.9.
2.6.4.3 Completing the Data Card(s)—
Each exposed filter should be sent with the IP data card to: Inhalable
Particulate Filter Bank, Environmental Protection Agency, Mail Drop 8, Re-
search Triangle Park, NC 27711.
-------
Section No. 2.6
Revision No. 0
Date 5/7/80
Page 21 of 33
The data cards should be filled out in the following manner (see Figure
2.6.10):
a. Station name
b. Site location
c. Filter type (1)
d. Collocated sample (2): An IP Network sampler located at the site
for comparison with a second Network sampler of the same type at
that site.
e. Station code (3-11): SAROAD code. The first two digits refer to
state, the middle four to station, and the last three to site.
f. Agency (12): A (SAROAD code for EPA).
g. Project (13,14): 07 (SAROAD code for IP Network).
h. Date sample was run (15-20).
i. Starting hour (21,22): 00 (SAROAD code for midnight).
j. Time (23): 7 (SAROAD code for 24-hr sampling period).
k. Filter number (24-30): Identification number found on the filter's
petri dish or the filter itself.
1. Sampling rate '(31-35): After averaging the initial and final air
flow rate obtained from the rotameter, refer to the most recent
calibration table to find the actual flow rate in mVmin.
m. Minutes sampled (36-39): Total minutes sampled taken from elapsed
time meter.
n. QC Check, % (40-43): Performed every other sampling period.
o. Operator's initials, lower right corner.
2.6.5 Sample Validation
2.6.5.1 Validation Criteria—
In order to assist the operator in determining whether a sample is
valid, the following validation criteria have been established for all IP
Network samples:
-------
Section No. 2.6
Revision No. 0
Date 5/7/80
Page 22 of 33
1. Timing
All samplers must turn ON and OFF within 1/2 hour of midnight.
All samplers must operate for at least-2_3 but no more than 25
hours.
2. Flow Rates
Decreases in flow rate during sampling of more than 10 percent
from the initial setpoint are questionable.
Changes in flow rate calibration of more than 10 percent, as
determined by a field calibration check, will invalidate all
samples collected back to the last acceptable flow check.
3. Filter Quality
All particulate deposits that do not have we 11-defined borders
(possible leak) should be voided.
Any filter that is obviously damaged (i.e., torn or frayed)
should be voided.
2.6.5.2 Handling of Valid Samples—
1. Calculate flow rates and fill out IP Network data cards completely
(see Section 2.2.2, Figure 2/6.lOa).
2. Send the filters in the cassettes accompanied by the completed data
cards to EPA-RTP, MD-8, for weighing and analysis according to the
preestablished schedule. This procedure guarantees a smooth flow
of samples to the laboratory.
2.6.5.3 Handling Invalid Samples—
When a filter is determined to be invalid for any of the previous rea-
sons:
1. Complete as much as possible of the IP data card (Figure 2.6.10b).
2. Mark "VOID" in the lower right corner and explain.
3. Mark "VOID" in the logbook and on the data sheet.
4. Do not discard the filter.
5. Mail filter with data card to EPA-RTP, MD-8, where a final decision
on sample validity will be made.
-------
Section No. 2.6
Revision No. 0
Date 5/7/80
Page 23 of 33
2.6.5.4 Handling of Questionable Samples--
If uncertain as to whether or not a sample should be voided, the oper-
ator should:
1. Complete as much as possible of the IP data card (Figure 2.6.10c).
2. Put a circled question mark in the lower right corner along with a
short explanation.
3. Mark "Questionable" in the logbook and on the data sheet.
4. Mail filter with data card to EPA-RTP, MD-8, where a final decision
on sample validity will be made.
2.6.6 Operators' Field Calibration Check Procedures
During routine IP Network operation, the operator will be required to
check the calibration of the instruments every other sampling period. Cali-
bration checks of the sampler flow rate require the instruments to be run-
ning, and hence that timed operation of the master timer be bypassed. Pro-
cedures for operation of the master timer and field calibration checks of
the samplers are given below.
2.6.6.1 Operation of the Tork Time Control (Master Timer)--
All samplers are controlled by a master timer to ensure all samplers
operate for a 24-hour period every sixth day. The operator does not need to
be concerned with the master timer except when the timer must be bypassed
for field calibration checks, or in the event of a power failure. However,
the operator should check the master timer at each sample change to make sure
that the next sampling period will be correct.
2.6.6.1.1 Bypassing the master time_r during field cal ibration checks--
The samplers must be operative during the calibration check. Since the cali-
bration check cannot be accomplished when the equipment is collecting a sam-
ple, the master timer must be bypassed. To bypass the timer:
1. Refer to the timer in Figure 2.6.11.
2. Rotate the skip wheel until the day indicator is pointing to the
sampling day (lug removed).
3. Power is now supplied to all samplers.
-------
Section No. 2.6
Revision No. 0
Date 5/7/80
Page 24 of 33
MICRO SWITCH
ACTUATOR
ARM
HOUR
INDICATOR
6-LUG
SKIP WHEEL
MISSING LUG
DAY
INDICATOR
Figure 2.6.11. Tork master timer.
-------
Section No. 2.6
Revision No. 0
Date 5/7/80
Page 25 of 33
4. To turn power off, rotate the skip wheel to a no-sampling day (lug
in place).
5. When the calibration check is complete, reset the timer as de-
scribed in the next section.
2.6.6.1.2 Resetting the master timer after power failure p_r cal ibra-
tion check—
1. Set the hour dial so that the station time is opposite the
hour indicator.
2. Set the skip wheel so that the number of lugs (clockwise) be-
tween the missing lug and the day indicator is equal to the
number of days before the next sampling date.
2.6.6.2 Equipment--
The following equipment is required for a field calibration check:
Calibrated orifice (Figure 2.6.12).
Orifice calibration curve (Figure 2.6.13) and interpolation table
(Figure 2.6.14).
Sierra dichotomous sampler "total" and "coarse" rotameter calibra-
tion curves (Figures 2.6.5 and 2.6.7) and interpolation tables
(Figures 2.6.6 and 2.6.8).
Magnahelic gauge or manometer.
IP Network Flow Check Data Sheet (Figure 2.6.15).
2.6.6.3 Field Calibration Check Procedure--
A field calibration check of the "total" flowmeter is required after
every other sampling period for Sierra dichotomous samplers. The check is
made by installing an orifice device calibrated in the operating range of
the "total" rotameter. The calibration of the orifice device (Figure 2.6.12)
is performed by the U.S. Environmental Protection Agency's (EPA) Environmen-
tal Monitoring Systems Laboratory (EMSL) located in Research Triangle Park,
NC. The laboratory calibration procedure is fully described in Sec-
tion 5.8.2.1 of this manual.
At the present time only the total flow rate is checked against the
field calibration check orifice device. It is expected that in the near fu-
ture individual checks for the "total" and "coarse" rotameters will be
-------
8
18 NPT
O.D. TUBING
PLUNGE MILL
1
^ -i ^.
SILVER a
sni npn I
x 0.040 DP.
SOLDER
/
U3ZZ2LLI/ /////////////// 777 /,
* 8
rtnii i TLJDI i ivirt rrr:
I
'////////////Af/// ////////////.
V////////Y/A
^ r\
^- PIPE NIPPLE (4")
8
T'
3 —
8
ORIFICE PLATE
Figure 2.6.12. IP Network dichotomous sampler calibration check orifice assembly.
TJ O TO t/1
OJ 01 ID (D
in <+ < n
rt> (D -•• r+
1/1 —".
K> LH -•• O
en -v^ o 3
~~J a
o ~-^. z
-h CD O
O Z •
U) O
(jj • ro
C3 CTl
-------
INHALED PART I CURATE NETWORK
DICHOTOMOUS FLOJskaRIFICE CALIBRATION
EXPONT 0. 463812
FACTOR 0.0074^75
i
C. COEF 0. 9B-957
DATE 10/
23. 0 C
759 5
0.
6 7 8 9 10 11 12
MANOMETER READING, IN H20
~o o ;t> GO
CU OJ (T> (T>
CQ r+ < O
CD O> — '• <-+
en -J.
rv> en -•• o
-~J \ O Z)
.
-Hi OO O
o 'z •
Co O
Figure 2.6.13. Sample dichotomous flow orifice calibration curve.
CD en
-------
INHALED PARTICIPATE NETUORK
**DICHOTOHOU8 FLOW ORIFICE CALIBRATION DATA**
****** AUDIT ORIFICE • IPD-43 DATE 10/ 30/ 79
HAN
RDO
0.0
0.1
0.2
0.3
0.4
0.3
0.4
0.7
o.a
0.?
.0
.1
.2
.3
.4
.9
.4
.7
.8
.?
2/0
2.1
2.2
2.3
2.4
2.3
2.4
2.7
2.8
2.9
3.0
3.1
3.2
3.3
3.4
3.3
3.4
3.7
3.9
3.9
4.0
4.1
4.2
4.3
.4
.3
.4
.7
.8
4.9
5.0
BLPN
0.0000
2.5363
3.3234
4.2331
4.B423
3.3927
3.8686
4.3033
4.7043
7.0028
7.4373
7.7737
•.0930
B. 4000
S. 4937
0.9744
V.2492
9.3129 "
9.7483
10.0144
10.2377
10.4923
10.7213
10.9447
11.1429
11.3742
11.3831
11.7894
11.9902
12.1849
12.3801
12.3498
12.7343
12.9394
13.1200
13.2974
13.4723
13.4448
13.8144
13.9821
14.1472
14.3102
14.4710
14.6298
14.7847
14.9416
13.0947
13.2460
13.3936
13.5434
13.6899
H3/HIN
0.0000
0.0024
0.0033
0.0043
0.0049
0.0034
0.0039
0.0043
0.0047
0.0071
0.0074
0.0078
0.0081
0.0084
0.0087
0.0090
0.0092
0.0093
0.0098
0.0100
0.0103
0.0103
0.0107
0.0109
0.0112
0.0114
0.0114
0.0118
0.0120
0.0122
0.0124
0.0124
0.0128
0.0129
0.0131
0.0133
0.0133
0.0134
0.0130
0.0140
0.0141
0.0143
0.0143
0.0144
0.0148
0.0149
0.0131
0.0132
0.0134
0.0133
0.0137
HAN
RDO
3.1
3.2
3.3
3.4
3.3
3.4
3.7
3.6
3.9
4.0
4.1
4.2
4.3
4.4
4.3
4.4
4.7
4.8
4.9
7.0
7.1
7.2
7.3
7.4
7.3
7.4
7.7
7.8
7.9
8.0
8.1
8.2
8.3
8.4
8.3
8.4
8.7
8.8
8.9
.0
.1
.2
.3
.4
.3
.6
.7
.8.
.9
10.0
10.1
8LPM
13.8347
13.9779
14.1197
16.2601
16.3990
16.3367
16.6730
16.8080
16.9418
17.0744
17.2038
17.3340
17.4632
17.3932
17.7202
17.8461
17.9710
18.0949
18.2179
18.3398
18.4609
18.3810
18.7003
18.8187
18.9362
19.0329
19.1488
19.2838
19.3981
19.3116
19.6244
19.7364
19.8476
19.9382
20.0680
20.1772
20.2837
20.3933
20.3006
20.6072
20.7130
20.8183
20.9230
21.0270
21.1303
21 .2333
21.3336
21.4374
21.3386
21.4392
21.7393
H3/HIN
0.0138
0.0160
0.0141
0.0143
0.0164
0.0143
0.0167
0.0168
0.0149
0.0171
0.0172
0.0173
0.0173
0.0174
0.0177
0.0178
0.0180
0.0181
0.0182
0.0183
0.0183
0.0184
0.0187
0.0188
0.0189
0.0191
0.0192
0.0193
0.0194
0.0193
0.0194
0.0197
0.0198
0.0200
0.0201
0.0202
0.0203
0.0204
0.0203
0.0204
0.0207
0.0208
O.02O9
0.0210
0.0211
0.0212
0.0213
0.0214
0.0213
0.0216
O.O217
HAN
RDO
1O.1
10.2
10.3
10.4
10.3
10.6
10.7
10.8
10.9
11.0
11.1
11.2
11.3
11.4
11.3
11.4
11.7
11.8
11.9
12.0
12.1
12.2
12.3
f 12.4
12.3
12.4
12.7
12.8
12.9
13.0
13.1
13.2
13.3
13.4
13.3
13.4
13.7
13.8
13.9
14.0
14.1
14.2
14.3
14.4
14.3
14.6
14.7
14.8
14.9
13.0
13.1
8LPH
21.7393
21.8389
21.9379
22.0364
22.1343
22.2320
22.3290
22.4236
22.3214
22.6172
22.7124
22.8070
22.9013
22.9930
23.0884
23.1813
23.2738
23.3638
23.4374
23.3487
23.6393
23.7299
23.8199
23.9093
23.9988
24.0876
24.1761
24.2642
24.3320
24.4393
24.3264
24.6130
24.6993
24.7833
24.8709
24.9342
23.0411
23.1237
23.2100
23.2940
23.3774
23.4609
23.3439
23.6266
23.7090
23.7911
23.8729
23.9344
26.0336
24.1163
2A.1971
'H3/MIN
0.0217
0.0218
0.0219
0.0220
0.0221
0.0222
0.0223
0.0224
0.0223
0.0226
0.0227
0.0228
0.0229
0.0230
0.0231
0.0232
0.0233
0.0234
0.0233
0.0233
0.0236
0.0237
0.0238
0.0239
0.0240
0.0241
0.0242
0.0243
0.0244
0.0244
0.0243
0.0246
0.0247
0.0248
0.0249
0.0230
0.0230
0.0231
0.0232
0.0233
0.0234
0.0233
0.0233
0.0236
0.0237
0.0238
0.0239
0.0260
0.0260
0.0261
0.0262
HAN
RDO
13.1
13.2
13.3
13.4
13.3
13.6
13.7
13.8
13.9
14.0
14.1
14.2
14.3
14.4
16.3
16.4
14.7
14.8
14.9
17.0
17.1
17.2
17.3
17.4
17.3
17.6
17.7
17.8
17.9
18.0
18.1
18.2
18.3
18.4
18.3
18.4
18.7
18.8
18.9
19.0
19.1
19.2
19.3
19.4
19.3
19.4
19.7
19.8
19.9
20.0
20.1
BLPM
24.1971
26.2774
26.3374
26.4372
26.3167
26.3939
26.6748
26.7333
26.8319
26.9100
24.9879
27.0433
27.1429
27.2200
27.2949
27.3733
27.4498
27.3240
27.4018
27.4773
27.7328
27.8280
27.9029
27.9774
28.0321
28.1243
28.2003
28.2741
28.3477
28.4210
28.4941
28.3471
28.4397
28.7122
28.7843
28.8344
28.9284
29.0001
29.0713
29.1427
29.2138
29.2844
29.3333
29.4237
29.4960
29.3660
29.6339
29.7036
29.7731
29.8444
29.9133
H3/HIN
0.0262
0.0263
0.0264
0.0264
0.0263
0.0244
0.0247
0.0248
0.0248
0.024V
0.0270
0.0271
0.0271
0.0272
0.0273
0.0274
0.0274
0.0273-
0.0274
0.0277
0.0278
0.0271
0.027V
'0.0280-
0.0281
0.0281
0.0282
0.0283
0.0283
0.0284
0.0283
0.0284
0.0284
0.0287
0.0288
0.0289
0.0289
0.0290
0.0291
0.0291
0.0292
0.0293
0.0294
0.029.4
0.0293
0.0294
0.0294
0.0297
0.0298
O.0298
0.0299
OJ (U CD It)
(Q r+ < n
fD fD —'• r+
o> —'•
ho cn -•• o
CO \ O 3
O
o \
-b CD
O
CO O
CO • t\J
o cn
Figure 2.6.14. Sample interpolation table for dichotomous flow orifice calibration.
-------
IP NETWORK
Flow Check Data Sheet
Section No. 2.6
Revision No. 0
Date 5/7/80
Page 29 of 33
SAROAD site number:
3
/*
y
/
/
7
/•>
-^
r>
/*s
t— ,
Location:
Date:
on: "° S ,ft;i c //' r ^- //
Month
Date
Year
Atmospheric pressure:
Temperature:
Operator
Sampler EPA Number:
mm Hg, in. Hg
TSP HIVOL
SSI HIVOL ( ) MAN. DICHOT (
-------
Section No. 2.6
Revision No. 0
Date 5/7/80
Page 30 of 33
approved and incorporated into this procedure. To perform the field calibra-
tion check:
1. Insert clean filters into both the "fine" and "coarse" filter cas-
settes in the sampler, as described in the operating procedure
(Section 2.6.3.1).
2. Remove the standpipe from the sampler and replace with the "total"
flow calibration check orifice device.
3. Turn on the sampler and allow it to warm up to operating tempera-
ture (approximately 5 minutes).
4. Open both "total" and "coarse" flow control valves full counter-
clockwise. Adjust both the "total" and "coarse" rotameters to
their respective setpoints as recorded on the laboratory calibra-
tion curves (Figure 2.6.5 and 2.6.7) or interpolation tables (Fig-
ures 2.6.6 and 2.6.8) provided with the sampler.
5. Observe the pressure drop, AP, across the orifice, and its corres-
ponding flow rate from the calibration data (Figures 2.6.13 and
2.6.14) provided with the orifice. Record both values on the IP
Network Flow Check Data Sheet (Figure 2.6.15). Also record the
rotameter setpoints and their corresponding flow rates on the Flow
Check Data Sheet.
6. Using the above information--and the formulas provided in the Flow
Check Data Sheet, calculate the QC Check %. Record this value on
the Flow Check Data Sheet and the IP data card (Figure 2.6.10).
7. If the calculated QC Check % is within ±10 percent of the 16.7 L/
min total flow rate, the sampler is operating properly. Return
the Flow Check Data Sheet to:
Environmental Protection Agency
EMSL (MD-76)
Research Triangle Park, NC 27711
ATTN: Inhalable Particulate Network
8. Turn off the sampler, remove the orifice device, and replace the
standpipe.
9. Remove the filters from both "fine" and "coarse" cassettes.
10. Set up the sampler for the next sampling period according to the
operating procedure in Section 2.6.3.1.
11. A calcu-lated QC check % not within ±10 percent of the 16.7 L/min
total flow rate usually indicates that the fine flow filter is not
sealed properly. Using gloves, gently push back and forth on the
-------
Section No. 2.6
Revision No. 0
Date 5/7/80
Page 31 of 33
filters. If one is not properly sealed, it should snap into place.
The pressure 'drop (AP) across the orifice device should now yield
a QC Check value within 10 percent of the setpoint, 16.7 L/min.
If the QC Check value is still outside the ±10 percent range, try
another set of filters. If this does not yield a QC Check value
within the interval 16.7 L/min ±10 percent, the sampler requires
recalibration. Record the value on the Flow Check Data Sheet and
contact the IP Field Manager (Mack Wilkins, 919-541-3049) to
arrange for recalibration. Return the Flow Check Data Sheet to
the address above.
2.6.7 Routine Maintenance
2.6.7.1 Cleaning the Sampling Module—
The Sampling Module is disassembled as shown in Figure 2.6.16. All
parts are sealed with "0" rings. Particulate internal loss deposits accumu-
late primarily on the outer and inner surfaces of the tip of the receiver
tube in the virtual impactor head. The receiver tube should be inspected
periodically for such particulate deposits and cleaned as required. A re-
ceiver tube cleaning schedule of every 3 to 4 months is typical. The remain-
ing inner surfaces should be cleaned every 6 to 12 months. Cleaning should
be done with alcohol or water using a camel's hair brush or by washing.
The diametral "0" rings in the-aerosol inlet and. the flow splitting
chamber should be conditioned periodically with vacuum grease.
The bug screen in the aerosol inlet should be cleaned periodically dur-
ing the summer months. The bug screen is exposed for cleaning by pulling
the aerosol inlet off the aerosol inlet tube. A diametral "0" ring in the
aerosol inlet acts as the seal.
2.6.7.2 Control Module—
CAUTION: UNPLUG THE LINE POWER CORD FROM ITS RECEPTACLE BEFORE REMOV-
ING THE FRONT PANEL OF THE MODEL 244 CONTROL MODULE ENCLOSURE.
2.6.7.2.1 Filter elements—After approximately 12 to 24 months of sam-
pling, the inlet filters for the coarse and fine particle flows may need re-
placement. In normal operation, air entering these filters is filtered by
the two 17-mm membrane filters in the Sampling Module. Hence, inlet filter
replacement is infrequent. To replace these filters, unplug the line power
cord and remove the front panel of the Control Module by removing the six
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Figure 2.6.16. Disassembled sampling module of Sierra dichotomous sampler
(Model 244or244E)
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screws. The filter jar for the coarse-particle flow is the small jar (ap-
proximately 1.5 in. dia. x 3 in. L) in the upper left side of the enclosure.
Unscrew the jar, remove the old filter element, and replace with a new ele-
ment. Tighten the jar very tightly when reinstating to avoid leaks. The
fine-particulate filter jar is behind the coarse-particulate filter jar. It
is approximately 3 in. dia. x 5 in. L and is the one closest to the bulkhead
fitting on the side of the enclosure. Filter element replacements are avail-
able from Sierra.
2.6.7.2.2 Vacuum pump—The diaphragm of the Model 727CA418 Diaphragm
Vacuum Pump is replaced routinely at 1- to 2-year intervals or if sudden re-
ductions in sampler vacuum occur and a leak check indicates there are no
leaks in the system.
To replace the diaphragm, unplug the line voltage and remove the front
panel. Remove the finned head of the pump by removing the six head screws.
Remove the four diaphragm plate holddown screws and change the diaphragm.
To reassemble, reverse the procedure making sure that the screw clearance
cavity in the plate is lined up under the intake valve screw heads and that
all head screws are tightened evenly.
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CONTENTS
Section Page
3 SITING 1
3.1 INTRODUCTION • 1
3.1.1 Inhalable Particulate
Network 1
3.1.2 Purpose of the IP Network
Siting Document 1
3.1.3 Siting Criteria for the
IP Network 1
3.2 SELECTING SITE LOCATIONS .... 2
3.2.1 Genera] 2
3.2.2 Procedures for Selecting
Site Location 4
3.3 SPECIAL CONSIDERATIONS IN SITE
SELECTION 9
3.3.1 Probe Siting 9
3.3.2 Physical and Electrical
Site Requirements for the
IP Network 12
3.4 REFERENCES 15
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SECTION 3
SITING
3.1 INTRODUCTION
3.1.1 Inhalable Particulate Network
Recent findings indicate that onl.y those particles less than 15 urn
(aerodynamic diameter) are inhalable and, hence, constitute a potential health
hazard.1 2 Traditional total suspended particulate (TSP) sampling with con-
ventional high volume samplers includes collection of particles greater than
15 urn. Thus, in accordance with the 1977 Clean Air'Act Amendments requirement
of a review of existing ambient pollutant standards by December 31, I960,3 the
Environmental Protection Agency will establish an Inhalable Particulate (IP)
Network that will provide a data base of IP concentrations and IP/TSP ratios.
3.1.2 Purpose of the IP Network Siting Document
The monitoring objective of the IP Network, as stated in the study pro-
tocol (Appendix A), is to collect IP and TSP samples representative of general
site types in sampling areas not unduly influenced by single sources. The
site types identified are industrial, commercial, residential, and nonurban.
Establishment of 300 IP Network stations nationwide by 1981 is projected.
Many of these stations will be located in existing national, state, and local
air monitoring stations, although some may be located in new sites. It is
essential that these IP stations be sited properly to ensure that measurements
made at a particular location are representative of the spatial and temporal
scales appropriate for the monitoring objectives of the station. This docu-
ment describes the criteria and procedures for selection of IP Network sites.
3.1.3 Siting Criteria for the IP Network
Because little is known about IP distributions at this time, the siting
criteria contained in this document are largely those used for TSP monitor-
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ing.4 5 Sampling of the inhalable fraction should, in fact, entail less
restrictive criteria, due to the exclusion of very large particles, which in
TSP sampling tend to settle quickly and be unevenly distributed. For example,
Pace and Myer,6 in a review of existing IP data, found that the gradients of
particulate distributions around sources such as roadways may not be as steep
for IP as has been shown for TSP. Therefore, although the procedures outlined
in this document may be conservative, they should still be applicable to the
IP Network.
3.2 SELECTING SITE LOCATIONS
3.2.1 General
Inhalable particulate concentration data always represent some volume of
air sampled over a definite period of time. In a statistical sense, these
concentration data may be considered sample points taken from a general popu-
lation consisting of a much larger volume of air. As with any type of sampl-
ing where the sample data are used to draw inferences about a general popula-
tion, m the validity of the inferences depends on the representativeness of the
sampled population. Therefore, the goal in site selection is to select a
location, or locations, where the concentration in the sample volume is
representative of the spatial and temporal scale appropriate for the monitor-
ing objectives of the s-tat ion.
The first step in siting an IP monitor must be to define the monitoring
objectives in terms of a spatial and temporal scale. Four spatial scales are
usually of interest in IP monitoring. These are:
Middle Scale—defines concentrations typical of areas ranging in
dimension from about 100 m to 0.5 km. Areas appropriate for this
scale include street canyons, traffic corridors, and roadways.
Neighborhood Scale—defines concentrations within some extended
region of an urban area that has relatively uniform land use with
dimensions in the 0.5- to 4.0-km range.
Urban Scale—defines overall citywide conditions with dimensions on
the order of 4 to 50 km. Urban scale consists of a variety of
middle and neighborhood scales. Because of the nonhomogeneity of an
urban area, a network of smaller stations must be used to charac-
terize the urban scale.
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Regional Scale—defines an area, usually rural, of reasonably
homogeneous geography extending from tens to hundreds of kilometers.
Regional, neighborhood, and middle scales provide the most convenient
classification of sites, and procedures for locating these types of stations
are given in Section 3.2.2. The urban scale is not included in this siting
scheme, since typically, one station alone is not sufficient to characterize
an entire urban area. Urban areas can be characterized by networks of middle
and neighborhood sampling sites covering a range of conditions within the
area. Similarly, source-oriented stations, used to determine the impact of
large single sources, will not be used for routine monitoring in the IP Net-
work and are, therefore, not included in this siting scheme. However, the IP
Network will be requested to provide locale-specific information for future
control strategy planning. Therefore, consideration must be given to proper
site selection to determine the impact of either localized fugitive' dust or
general source categories on metropolitan air quality.
In addition to defining the sampling objectives in terms of spatial
scale, the temporal scale must also be considered. Under most circumstances
interest will focus primarily on either a 24-hr average concentration or an
annual average concentration, and the choice of temporal scales will affect
the location of the sampler. For example, the siting of most monitors
requires a consideration of the most frequent wind direction. There is no
guarantee, however, that the wind direction on a given day will accurately
represent the long-term prevailing wind direction. Therefore, a sampler
located to monitor trends in annual air quality is not necessarily well placed
to monitor violations of a 24-hr standard.
An additional factor to consider is the initial cost of implementing new
monitoring sites. The IP Network, as other networks, is resource-limited in
the number of sites available to represent a given area. This restriction
will, in most cases, be the limiting factor in site selection. In order to
conserve resources, first consideration will be given to existing national,
and state and local air monitoring sites (NAMS and SLAMS).
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3.2.2 Procedures For Selecting Site Location
Specific procedures for siting regional, neighborhood, and middle scale
stations are given below. Each of these procedures can be broken down into
five basic steps:
1. Obtain background information.
2. Identify specific sampling objectives.
3. Select tentative areas.
4. Judge suitability of tentatively selected areas.
5. Site the probe.
The fourth step usually presents the greatest number of technical
problems. Judging the suitability of tentative areas can often only be accom-
plished by conducting a small-scale sampling program.
Often the selection of tentative areas (Step 3) follows so directly from
the identification of specific sampling objectives (step 2) that the two can
be considered a single step and will be treated as such in the text. This
observation points to the key to successful site selection: definition of the
goals of sampling, first in terms of the spatial and temporal scales of repre-
sentativeness, and second in terms of specific objectives, such as charac-
terizing background levels entering a city.
3.2.2.1 Siting Regional Scale Stations--
Obtain Background Information—Background information for siting regional
scale stations is of three basic kinds: geographical, climatological, and
emissions-related. Geographical data are used to identify topographical
features, such as hills and valleys, that may affect regional air flow pat-
terns. Maps and aerial photographs are useful here. Cl imatological sum-
maries, prepared by the National Climatic Center, are most useful for deter-
mining the frequency distribution of wind speed and direction. Emission
inventory data are useful for identifying large point sources of particulates
in the region. The Environmental Protection Agency has a computerized data
bank, AEROS (Aerometric and Emissions Reporting System), which contains infor-
mation on the location and source strength of point sources in specific
regions.
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Identify Specific Sampl ing Objectives and Select Tentative Areajs —Sampl-
ing on a regional scale may be done for one of two reasons: (1) to establish
a background concentration of participates entering a city, or (2) to charac-
terize the participate concentration over a relatively homogeneous region
(e.g., rural). In either case, if only one monitoring station is planned,
tentative siting areas should be located downwind of the nearest urban area
for the least frequently occurring wind directions. If two stations are plan-
ned to measure the background particulate concentration upwind of a city, one
station should be placed upwind of the most frequent wind direction, and the
other should be placed upwind of the most frequent of all wind directions that
are at least 90° from the most frequent direction.
Judge Suitability of Tentatively Selected Areas—Areas suitable for re-
gional stations will be:
more than 10 km from the nearest urban area;
more than 1 km from the nearest major (i.e., 3,000 vehicles per day)
roadway;
relatively uninfluenced by major point sources; and
well away from very local dust sources.
Areas unsuitable for regional stations may be:
located in heavily vegetated areas;
within 150 m of a paved road;
within 150 m of an unpaved road with traffic greater than a few
vehicles per day; and
near major topographical obstructions.
Probe Si ting--Locate the monitor inlet vertically at a height of between
2 and 15 m, as specified in Section 3.3.1.
3.2.2.2 Siting Neighborhood Scale Stations—
Obtain Background Information—For neighborhood scale stations, land use,
climatological, and emissions-related data should be collected. Aerial photo-
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graphs, traffic maps, and city planning maps are most useful for determining
land use in the city. Climatological information is readily available from
the National Climatic Center; the "STAR" program provides a joint frequency
distribution of winds and atmospheric stability.5 As with regional stations,
EPA's AEROS data bank can provide information about large point sources. It
may be necessary, however, to further resolve these data into areas smaller
than the usual countywide summary of point sources. This further subdivision
can be done on the basis of population or housing units.
Identify Specific Sampling Objectives and Select Tentative Sites—True
neighborhood sampling consists of attempting to characterize a homogeneous
area, such as a commercial or industrial area. Areas dominated by a large
single source, or areas containing street canyons or traffic corridors, are
best considered source-oriented and middle scale sites rather than neighbor-
hood sites (see Section 3.2.2.4). It is advisable to make an onsite survey, of
the prospective areas and identify tentative sites on a map.
Judge Suitabil ity o_f Tentatively Sel ected Sites—If a preliminary sampl-
ing program is conducted to provide better data on the relative particulate
concentrations in the various candidate neighborhoods, it may be desirable to
use a direct-reading instrument such as an optical particle counter instead of
gravimetric techniques which require additional analysis after sampling. The
preliminary sampling program is likely to be of short duration, and, conse-
quently, it will be difficult to typify "average1' concentrations. A prelimi-
nary sampling program may not take into account stagnant pollution conditions
or seasonal variability and may thus misrepresent an area if the program is
carried out during unusual weather conditions. One way of eliminating daily
variations is to sample biweekly and on random days.7
Probe Siting (see also Section 3.3. l)—Locate the sampler at least 20 m
from any street and at least 400 m from roadways with greater than 50,000
vehicles per day. The sampler inlet should be at a height of 2 to 15 m and at
a distance from any obstacle that is at least twice the height the obstacle
extends above the sampler. The ground surface should have ground cover or
pavement to minimize reentrainment of settled dust.
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3.2.2.3 Siting Middle Scale Stations--
Middle scale locations include street canyons, traffic corridors, and
parking lots. In general, the concentrations measured at middle scale sites
are not representative of typical population exposures over the 24-hr and
annual averaging periods on which air quality standards are based. Neverthe-
less, both for evaluation of possible short-term or localized health effects
of particulate pollution and for characterization of particulate exposures in
urban areas (Section 3.2.1), it is often desirable to monitor particulate con-
centrations at these sites.
These locations can present very difficult particulate sampling problems
because of the complex wind velocity fields and the high concentrations of par-
ticulates emitted from vehicles. In addition, it should be noted that reen-
trainment of settled dust may contribute significantly to middle scale high
volume TSP samples, especially those collected in street canyons. A more com-
plete discussion of some of these problems is given in Section 3.3.1.
Obtaining Background Information—Detailed information is necessary for
locating a middle scale station: climatological information should include a
wind rose of the local wind; land use data should include traffic totals on
all streets in the area, building heights, and street widths; and emissions
data should inventory all, sources in the area.
Identify Specific Sampling Objectives—Middle scale sampling may be done
to characterize "worst" conditions or to characterize "typical" conditions.
In either case, areas where IP concentrations are dominated by individual point
sources should be avoided. Specific procedures for satisfying these objectives
when monitoring street canyons and roadways are given below.
Selecting Tentative Areas—For "worst" condition sampling, areas of great-
est particulate emissions should first be identified. In the case of street
canyons, samplers should be located on a street as near perpendicular to the
most frequent wind direction for strong winds, and on the side of the street
from which these winds blow. This siting criterion is a function of the eddy
circulation that is likely to occur in a street canyon during a strong wind
(see Section 3.3.1).
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For sampling "typical" conditions in street canyons, those blocks where
the daily traffic is closest to the average daily traffic in the area should
be identified. The next step is to determine the frequency distribution of
wind velocities in the area (wind rose). If the wind rose is symmetrical,
streets parallel to the axis of symmetry should be used. If the wind rose is
asymmetrical, or no street parallel to the axis of symmetry can be found,
those streets parallel to the most frequent wind direction should be used.
If the sampler is located on a street parallel to the axis of symmetry,
there is no preferred side of the street for sampler siting, since the wind
blows most frequently parallel to the street (rather than transverse., which
gives rise to large eddies). However, if the wind rose is not symmetrical, it
may be necessary to augment the sampling site with a monitor placed on the
opposite side of the street and one at roof level to determine if samples
taken at the regular monitor are representative of the street canyon.
Monitoring near roadways is very similar to monitoring in street canyons.
To characterize "worst" conditions, areas of greatest daily traffic should be
identified; the monitor is placed downwind of the most frequent wind direc-
tion. To characterize "typical" conditions, roadways parallel to the axis of
symmetry of the wind rose sho.uld be used. If the wind rose is asymmetrical or
a suitable roadway is not available, the monitor should be placed parallel to
the most frequent wind direction. Again, a small sampling program could be
conducted to determine if a sample collected on one side of the roadway is
representative of the entire roadway area.
Probe Siting (see also Section 3.3.1)—
Street canyons—Locate the sampler inlet about 3 ± 0.5 m high, midblock,
over the sidewalk, at least 2 m from any building. Avoid areas of unusual
traffic such as bus stops and loading zones.
Roadway—Locate the sampler inlet at a height of 2 to 15 m outside the
highway right-of-way. If characterization of "typical" population exposure is
desired, the site should be at a distance from the roadway, which is about
equal to the average building setback. If a "worst" example is sought, the
sampler should be as near the edge of right-of-way as possible. In both
cases, the sampling site should be well removed from major obstructions; in
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general, the distance between the sampler and the nearest large obstruction
should be about twice the height the obstruction extends above the sampler.
Avoid unusual roadway sites such as toll gates and on-ramps, which may repre-
sent anomalous source areas.
3.3 SPECIAL CONSIDERATIONS IN SITE SELECTION
Several aspects of site selection require more extensive treatment than
given in Section 3.2. Special considerations in probe siting and site re-
quirements are discussed below.
3.3.1 Probe Siting
3.3.1.1 Vertical Placement--
The most desirable height for an IP monitor is at the breathing zone.
Practical considerations, however, such as prevention of vandalism, security,
and availability of electricity, often require that the sampler be elevated.
The recommended range of sampler inlet heights in this document,.2 to 15 m,
represents a compromise between these practical considerations, the need to
avoid reentrainment from dusty surfaces, and the need to provide a measure of
population exposure.
3.3.1.2 Flow Effects Around Buildings--
Figure 3.1 illustrates building effects on pollution dispersion. Figure
3.la shows that in very narrow street canyons, the vortex created by the trans-
verse prevailing wind is insufficient to flush the canyon. The wider canyon
in Figure 3.1b, however, is flushed by the vortex circulation. Figures 3.1c
and 3.Id show the effect of "downwash." In Figure 3.1c, downwash occurs be-
cause the stack has been placed in the suction zone above the roof of the tall
building. In Figure 3.Id, downwash occurs because the plume from the neighbor-
ing building is caught in the eddy of the cavity zone induced by the taller
building. Figure 3.2 illustrates air flow around a building and shows why
downwash (Figures 3.1c and 3.Id) occurs.
Placement of Probe Near Obstacles—It is apparent from the above discus-
sion that the effects of buildings on air flow and, consequently, on pollutant
dispersion, are significant. Hence, for regional or neighborhood scale moni-
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(a)
(b)
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Figure 3.1. The influence of building air flow on pollution dispersion.^
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DISPLACEMENT
ZONE
CAVITY ZONE
Figure 3.2. Schematic representation of the air flow around an obstacle.
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toring, the .sampler should be located so that the distance between the
obstacle and the sampler is at least twice the height the obstacle extends
above the sampler. Existing sampling stations that are closer to obstacles
than this distance should be classified as middle scale stations.
It is also apparent that middle scale sampling, particularly in street
canyons, is especially complex. There is no simple relationship between
canyon width and wind speed that can predict whether the canyon will be
flushed or not (Figures 3. la and 3.1b). Therefore, unless a particular street
canyon is the object of some special study, placement of middle scale stations
in narrow street canyons that are frequently transverse to the prevailing wind
should be avoided.
Spacing from Roads—Figure 3.3 shows the recommended spacing (Zone A) of
samplers from roads with average daily traffic of 3,000 vehicles or greater.
Zone B represents locations that should be avoided to minimize undesirable
roadway influences (e.g., reentrainment of settled roadway dust). Where the
traffic is less than 3,000 vehicles per day, the monitor inlet should be
located more than 5 m from the edge of the nearest traffic lane and 2 to 15 m
above ground level (either Zone A or Zone B).
Spacing from Other Obstacles—Sampler inlets should not be- located near
any short stacks because of the potential for downwash (Figure 3.1c). The
sampler should be placed at least 20 m from trees.
3.3.2 Physical and Electrical Site Requirements for the IP Network
At present, a number of different types of samplers are planned for use
in the IP Network, including manual and automated dichotomous samplers, TSP
high volume samplers, and size-selective inlet (SSI) high volume samplers.
The desired minimum spacing between sampler inlets is 2 m. The maximum spac-
ing between inlets should be 4m. All inlets at the same site should be
vertically within 1 m of one another. Space and electrical requirements for
the various sampler configurations are summarized in Table 3.1.
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r
0)
I
O
20
15
10
0
ZONE C (UNACCEPTABLE)
ZONE A (ACCEPTABLE)
-ZONE B (NOT RECOMMENDED)
05 10 15 20 25 30
DISTANCE FROM EDGE OF NEAREST TRAFFIC LANE, meters3
aAPPLIES WHERE ADT > 3.000
Figure 3.3. Acceptable zone for siting IP monitors.
35
-o o ?o 01
O) OJ fD (D
Id <-•- < O
0> fD -". r+
l/l —'•
I—" <_n -•• o
oo ~\ o ^
•~-j n
o "^-.
-h CD z z
CD O O
CD Cx)
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TABLE 3.1. SPACE AND ELECTRICAL REQUIREMENTS FOR IP NETWORK SAMPLERS
Sampler type configurations (amps)
A.
B.
C.
TSP high volume (7)
Manual dichotomous (5)
TSP high volume (7)
Automated dichotomous (3)
TSP high volume (7)
Manual dichotomous (5)
SSI high volume (7)
Total Approximate
current3 No. of , space
(amps) circuits0 (m2 (ft2))
12 14 (65)
10 14 (65)
19 27 (120)
D.
E.
TSP high volume (7)
Automated dichotomous
SSI high volume (7)
(3)
TSP high volume (7)
Automated dichotomous (3)
SSI high volume (7)
AISI tape (3)
British smokeshade (1)
17
21
7 (120)
16 (230)
All samplers are 120 V a.c., 60 Hz. Currents are operating current.
Starting currents are higher and require slow-blow type breakers.
315- or 20-amp circuits.
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3.4 REFERENCES
1. "Health Effects Considerations for Establishing a Standard for Inhaled
Particulate Matter," EPA/HERL internal report, January 1979, submitted to
JAPCA for publication.
2. Air Quality Criteria Document for Particulate Matter, DHEW/USPAS,
National Air Pollution Control AdmThistrati on, A-49, 1969, pp. 17-23,
111-125.
3. Amendments to the Clean Air Act of 1970, Public Law 9595. August 1977.
4. Federal Register, Volume 44, No. 92, 5/10/79.
5. Ludwig, F. L., J. S. Kealoha, and C. Shelar, "Selecting Sites for Moni-
toring Total Suspended Particulates," EPA 450/13-77-018, 1977, 141 pp.
6. Pace, T. G. , and E. L. Meyer, "Preliminary Characterization of Inhalable
Particulates in Urban Areas," paper presented at the 72nd Annual Meeting
of the Air Pollution Control Association, Cincinnati, Ohio, June 24-29,
1979.
7. U.S. Public Health Service, Air Pollution Measurements of the National
Air Sampling Networks, Publ. No. 637, 1958, 259 pp.
8. Oke, T. R. , Boundary Layer Climates, Methuen & Co., Ltd., London, 1978,
p. 239.
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CONTENTS
Section
ANALYTICAL PROCEDURES
Page
1
4.1 IP NETWORK HIGH VOLUME FILTER
HANDLING PROCEDURES 1
4.1.1 High Volume Filter Tare
Weighing Procedure .... 1
4.1.2 High Volume Filter Final
Weighing Procedure .... 3
4.1.3 Internal Quality
Control 5
4.1.4 References 6
4.2 IP NETWORK DICHOTOMOUS FILTER
HANDLING -PROCEDURES 1
4.2.1 Dichotomous Filter Tare
Weighing Procedure .... 1
4.2.2 Dichotomous Filter Final
Weighing Procedure .... 2
4.2.3 Internal Quality
Control 6
4.2.4 References 6
4.3 (TENTATIVE) DICHOTOMOUS "FILTER
EXTRACTION PROCEDURE FOR
SULFATES AND NITRATES 1
4.4 PROCEDURE FOR THE ANALYSIS OF
SULFATES IN ATMOSPHERIC
PARTICULATES COLLECTED BY HIGH
VOLUME SAMPLERS (AUTO-TECHNICON
II PROCEDURE) 1
4.4.1 Principle and
Applicability 1
4.4.2 Range and Discrimination
Limit 1
4.4.3 Interferences 2
4.4.4 Precision and Accuracy . . 2
4.4.5 Apparatus 2
4.4.6 Reagents 5
4.4.7 Analytical Procedure ... 8
4.4.8 Calculations 11
4.4.9 Quality Control 13
4.4.10 References 16
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4.5 PROCEDURE FOR THE ANALYSIS OF
NITRATES IN ATMOSPHERIC
PARTICULATES COLLECTED BY
HIGH VOLUME SAMPLERS AUTO-
TECHNICON II PROCEDURE) 1
4.5.1 Principle and Applic-
ability 1
4.5.2 Range and Discrimination
Limit 1
4.5.3 Interferences 2
4.5.4 Precision and Accuracy . . 2
4.5.5 Apparatus 2
4.5.6 Reagents 5
4.5.7 Analytical Procedure. ... 8
4.5.8 Calculations 10
4.5.9 Quality Control 11
4.5.10 References 15
4.6 PROCEDURE FOR THE ANALYSIS OF
SULFATES IN ATMOSPHERIC PARTIC-
ULATES (DIONEX METHOD) 1
4.7 PROCEDURE FOR THE ANALYSIS OF
LEAD IN ATMOSPHERIC PARTICU-
LATES ( METHOD) ... 1
4.8 PROCEDURE FOR THE ELEMENTAL
ANALYSIS OF ATMOSPHERIC PARTIC-
ULATES (X-RAY FLUORESCENCE
METHOD) .' 1
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Section No. 4.1
Revision No. 0
Date 5/7/80
Page 1 of 6
SECTION 4
ANALYTICAL PROCEDURES
4.1 IP NETWORK HIGH VOLUME FILTER HANDLING PROCEDURES
4.1.1 High Volume Filter Tare Weighing Procedure
1. Upon receipt of new high volume filters from the EPA representative
(8-in. x 10-in. glass fiber), take them to the climate controlled room,
remove from the paper and plastic envelope (wearing clean plastic
gloves), place each on edge in a clean metal file rack., and cover with
clean white paper towels.
2. Allow the filters to equilibrate in the metal file rack in the weighing
room atmosphere for at least 24 hours. Humidity and temperature must
be within Federal Reference 'Method Specifications,1 i.e., <50 percent
and 15° to 35° C, respectively.
3. Zero the high volume balance in that room before weighing.
4. Weigh each filter, and record filter numbers and tare weights on an IBM
coding form (Figure 4.1.1). Number IBM forms sequentially in the upper
right corner.
5. Return the weighed filters to the plastic and paper envelopes while
wearing gloves. Deliver the filters, along with the original and two
copies of the completed IBM form, to the EPA project officer. He will
initial and return the original as a receipt. These originals should
be bound and kept as the laboratory notebook. [The EPA project officer
will deliver the packaged filters and their referent photocopied IBM
forms to the Environmental Monitoring Division (EMD) for distribution
to the field, and one each of the copied forms to the Automatic Data
Processing (ADP) contact.]
-------
INIIALAOLE PAHTICULATE NETWORK HIGH VOLUME FILTER TARE WEIGHTS
FILTER TARE FILTEH TARE FILTER TARE
NO. WT. NO. WT. NO. WT.
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-------
Section No. 4.1
Revision No. 0
Date 5/7/80
Page 3 of 6
4.1.2 High Volume Filter Final Weighing Procedure
1. Exposed filters will have been logged into the computer (Section 6.2)
and will be received in individual manila folders^ with computer
printed identification labels affixed. No exposed filter should be
touched until this label is affixed. Some folders will have the words
"To Be Analyzed" on the label. All folders will contain two extra
filter labels.
2. Separate the filters into two groups according to whether or not the
label reads "To Be Analyzed" (those so labeled will undergo further
analysis).
3. Condition all filters in the manner -specified by the Federal Reference
Method.:
4. Weigh all filters according to the Tare Weighing Procedure in Sec-
tion 4.1.1. Record final weights on serially numbered IBM forms
(Figure 4.1.2). Filters are identified on the IBM forms by five-
character codes consisting of a blank space followed by four letters.
For those filters not to be analyzed, put an asterisk in the space pre-
ceding the four-letter code. Leave this space blank for samples to be
analyzed. Sign and date the IBM forms.
5. Deliver all filters and IBM forms to the filter bank room, keeping
groups from Step 2 separate.
6. Archive asterisked high volume filters. File alphabetically by state,
city, and date. Keep separate from National Air Sampling Network
(NASN) files.'
7. Cut one 3/4-in. x 8-in. and one 1-in. x 8-in. strip from each filter
"to be analyzed" by placing the filter face up on a flat surface and
cutting with a pizza cutter. Use extra labels to identify these sample
strips. Place strips in glassine envelopes, then in separate boxes so
that two sets are prepared for analysis.
8. Deliver the IBM forms, plus two photocopies each, with the two sample
sets to the EPA project officer who will sign and return the originals
as receipt.
-------
INIIAIAULE PADTICULATE NETWORK HIGH VOLUME FILTER FINAL WEIGHTS
FINAL FINAL
CODE WEIGHT CODE WEIGHT CODE
I 67 11 17 II 23 2S 33 31
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-------
Section No. 4.1
Revision No. 0
Date 5/7/80
Page 5 of 6
9. File filter remnants in a separate file alphabetically by state, city,
date. "Bind" the serially numbered IBM forms as the record book for
this activity.
4.1.3 Internal Quality Control (QC)
4.1.3.1 Operator QC—
Weigh filters in lots of approximately 100, if possible. After every
fifth weighing, recheck the zero of the balance. Note the satisfactory com-
pletion of this by placing a check (V) to the left and between the two fil-
ter ID's that bracket the physical check. "Satisfactory" means 1 mg or less
difference from zero. All differences should be corrected. Any difference
exceeding 1 mg requires reweighing the previous five filters.
Any filter weight outside the normal range of 3.5 to 5.0 g requires
immediate investigation.
4.1.3.2 Supervisor QC—
Assign someone not weighing that day to go to the balance room late in
the morning, pick four filters at random from those weighed in the morning,
and reweigh them. If the second weight is within 2.8 mg of the original
weight for blanks, and within 5 mg of"the original weight for exposed fil-
ters, accept all weights. If not, troubleshoot and reweigh.
Record this procedure in a bound organized QC notebook. Reference the
pages and IBM forms so that QC data may be traced back to IBM forms.
Repeat this procedure at the end of the day so that eight reweighings
are done in any day.
Before delivery of data sheets, all signatures and blanks must be
filled in. The operator must sign and date data collection. Someone else
must certify by his/her signature that all activities have been done and
meet specifications.
Physical separation of NASN and IP Network samples in the filter bank
room is required. Adequate physical separation is specified as: no inter-
mingling of samples on any given work surface, file top, drawer, cabinet, or
any other place.
External audits should be expected at unannounced intervals.
-------
4.1.4 References
Section No. 4.1
Revision No. 0
Date 5/7/80
Page 6 of 6
"Appendix B - Reference Method for the Determination of Suspended Par-
ticulates in the Atmosphere (High Volume Method)," Federal Register,
36(84): 8191-6194, 30 April 1971.
-------
Section No. 4.2
Revision No. 0
Date 5/7/80
Page 1 of 6
4.2 IP NETWORK DICHOTOMOUS FILTER HANDLING PROCEDURE
4.2.1 Di'chotomous Filter Tare Weighing Procedure
1. Fabric filters, 37-mm in diameter, with a circumferential plastic rein-
forcing ring, will be received in small boxes. Open boxes in the
climate-controlled room under conditions suitable for high volume weigh-
ing,1 cover with a clean lab paper towel, and allow to equilibrate for
24 hr.
2. Filters are weighed on a Mettler microbalance; each balance is identi-
fied by a balance number.
3. Each balance is assigned a block of 7-digit sample numbers to be used
sequentially. A sample number is assigned to each filter when it is
tared. Inaccuracies J_n this aspect £f the procedure will cause irre-
mediable sample loss.
4. Turn on the balance and allow it to warm up for at least 15 min. If it
is in use daily, leave it on at all times.
5. Set the range knob to 10 mg with the automatic tare turned off.
6. Turn the release lever to "1" and zero the balance using the tare ad-
justing knob.
7. To calibrate, turn the 10 mg tare knob to "C" and adjust the fine and
coarse calibrating screws for a reading of 10.000 ± 0.002. Return the
release level to "0" and the 10 mg tare knob to "0."
8. Using clean nonserrated tweezers that will not damage the filter, re-
move the filter from the Lexan jig and place it on the weighing pan.
Turn the release lever to "1" and dial in tare weights until a reading
between 0.000 and 7.000 is obtained. Allow the reading to stabilize.
This may require 2 to 4 min. Record the reading and the dialed-in tare
weight as specified in Step 12. Return the release lever to "0" and
remove the filter from the weighing pan.
9. Place a white label on a clean 50-mm diameter plastic petri dish (tight
fitting lid type).
10. Assign a sample number to each filter (from those assigned to that bal-
ance), taking extreme care to avoid duplication or missed numbers.
-------
Section No. 4.2
Revision No. 0
Date 5/7/80
Page 2 of 6
11. Record legibly the assigned sample number on the petri dish label, leav-
ing sufficient room for one more letter to be written following the num-
ber. Do not record the balance number on this label, although it wil1
go onto the IBM form (Figure 4.2.1).
12. Record the balance number, the assigned sample number, the' dialed-in
tare weight, and the digital-displayed tare weight on the IBM coding
form. Number each sheet of the IBM form sequentially in the upper
right-hand corner. Write "Tare Weight, Dichot Filters" on the top of
each sheet. These forms may serve, when bound, as the laboratory note-
book.
13. Place the weighed filter in its numbered petri dish.
14. Deliver the weighed filters along with the originals and two copies each
of the completed IBM forms to the EPA project officer. He w_ill initial
and return the originals as receipt, and deliver one copy each to the
Automatic Data Processing (ADP) operation, where the information will
be entered into the computer.
4.2.2 Dichotomous Filter Final Weighing Procedure
1. Filters will be returned from the field with a computer printed label
affixed to the petri dish. The label will contain a five-character
identification code' that is different from the original sample number
(Step 3, Section 4.2.1), a balance ID, the balance tare, and other in-
formation. All filters will be accompanied by extra labels. Some will
have the words "To Be Analyzed" on the labels. The filter in each petri
dish will rest in a Lexan jig.
2. Each filter must be reweighed on the balance on which its tare weight
was obtained. In the climate-controlled room, group the filters accord-
ing to recorded balance numbers. Open the petri dishes, making certain
that lids are placed under the bottoms and that no mixup occurs. Cover
with a clean white lab paper towel and allow to equilibrate.
-------
INHALABLE PARTICULATE NETWORK DICIIOTOMOUS FILTER TARE WEIGHTS
BAL. FILTER BALANCE TARE BAL. FILTER BALANCE TARE BAL. FILTER BALANCE TARE
NO. NO. TARE WT. NO. NO. TARE WT. NO. NO. TARE WT.
OPERATOR
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-------
Section No. 4.2
Revision No. 0
Date 5/7/80
Page 4 of 6
3. Repeat Steps 4 through 7 of the dichotomous filter tare weighing proce-
dure (Section 4.2.1).
4. Perform "Standard Filter" quality control check (Section 4.2.3) to
assure validity of reweighing.
5. Using clean nonserrated tweezers that will not damage the filter, re-
move the filter from the Lexan jig and place it on the weighing pan.
Dial in the tare weight recorded on the information label and turn the
release lever to "1." If the filter is covered with a pad (most will
not be), remove the pad. Note on the IBM data form (Figure 4.2.2) if
the pad is clean (0) or soiled with particulates (1); discard the pad.
Record the digital output reading and the five-character code on the
IBM-form. These forms will serve as the laboratory notebook when prop-
erly signed and bound.
6. If the dichotomous filter is not to be analyzed, place it, using tweez-
ers, in a small glassine envelope to which one of the extra labels has
been affixed. Place an asterisk before the five-character code on the
IBM form. Deliver these filters to the filter bank for archiving, along
with the high volume filters collected at that site on that date.
7. If the filter is to be analyzed,""carefully put it'back into the petri
dish using tweezers. Place the petri dish carefully in a box.
8. Place one label on a sheet of 8*5-in. x 11-in. paper labeled NOs/SO^,
and the other on a similar sheet labeled XRF. Indicate the IBM page
number and balance number on each list. Please keep samples in the box
in an order corresponding with the lists.
9. Without jostling the box containing filters to be analyzed, deliver it,
the two lists, and the original IBM forms with two copies each to the
EPA project officer. He will initial the original IBM forms and return
them as receipt. (All samples will be submitted for elemental analysis
by X-ray fluorescence (XRF), extraction, and NOs/SO^ analyses.)
10. Discard used petri dishes.
11. Return jigs to EPA project officer promptly.
-------
INHALABLE PARTICIPATE NETWORK DICHOTOMOUS FILTER FINAL WEIGHTS
FINAL
CODE WEIGHT
1 57 11
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-------
Section No. 4.2
Revision No. 0
Date 5/7/80
Page 6 of 6
4.2.3 Internal Quality Control (QC)
4.2.3.1 Supervisor QC--
1. Keep a. bound QC notebook.
2. Reference all QC data in that notebook to IBM form codes.
3. Appoint an independent corps of QC officers to do dichotomous filter
weighing QC daily.
4. At the beginning of each day of weighing, after zeroing and calibration
are done by the operators, tare weigh one of a set of "standard" fil-
ters arbitrarily selected for that purpose. The digital readout for
each balance may differ. Once established, however, it must be repeat-
able to within 20 pg of the original value. If not, the balance per-
formance is unacceptable. Troubleshoot and reweigh as necessary. Un-
less this procedure is adhered to, many samples will be lost.
5. Reweigh 5 to 7 filters/balance/day of operation. Weights should be
within 20 ug of original values for clean or exposed filters; if not,
troubleshoot and reweigh.
6. Certify acceptability of data and completed archiving on IBM form daily.
7. External audits should be expected at unannounced times.
4.2.3.2 Operator QC—
After every fifth weighing, recheck the zero and calibration of the bal-
ance. Acceptable checks should be indicated by placing a check (V) to the
left between the two filter codes bracketing the physical check. "Accept-
able" means zero within 4 ug of true zero and calibration within 2 ug of
10 mg. Discrepancies should be corrected immediately. Unacceptable checks
require reweighing the previous five filters. Any filter weight outside of
the normal range of 90 to 110 mg requires immediate investigation.
4.2.4 References
1. "Appendix B - Reference Method for the Determination of Suspended Par-
ticulates in the Atmosphere (High Volume Method)," Federal Register,
35(84): 8191-6194, 30 April 1971.
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Section No. 4.3
Revision No. 0
Date 5/7/80
Page 1 of 1
4.3 (TENTATIVE) •DICHOTOMOUS FILTER EXTRACTION PROCEDURE FOR SULFATES AND
NITRATES
1. Using nonserrated tweezers, place the filter, exposed side up, flat on
the bottom of a clean 60-mL straight-sided wide-mouth polypropylene
jar.
2. Place a clean 37-mm-long Teflon-coated stirring bar on top of the
filter.
3. Prepare approximately 100 jars in this manner; then pipet exactly 2 ml
ACS reagent grade methanol into each jar.
4. To minimize loss of methanol by evaporation allow only enough time for
complete wetting of filters; then add"18 ml distilled water to each jar
and screw cap into place. Filters should be completely covered.
(Limited experiments show that the volumes are additive within accept-
able analytical limits; i.e., total sample extract volume is 20 ml.)
5. Place samples in an ultrasonic bath; keep screw caps above the water
surface; ultrasonicate for 30 min.
6. Take an aliquot directly for analysis, or if necessary, decant and
centrifuge at 2,000 rpm for approximately 20 to 30 min, and then analyze
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Section No. 4.4
Revision No. 0
Date 5/7/80
Page 1 of 17
4.4 PROCEDURE FOR THE ANALYSIS OF SULFATES IN ATMOSPHERIC PARTICULATE
COLLECTED BY HIGH VOLUME SAMPLERS (AUTO-TECHNICON II PROCEDURE)
4.4.1 Principle and Applicability
4.4.1.1 Participate sulfate is collected by drawing air through a glass-
fiber filter with a high volume sampler. A portion of the filter is ex-
tracted with water. The extract is analyzed for sulfate by the methyl thymol
blue (MTB) method using a single channel Technicon Autoanalyzer II system
equipped with a linearizer. The amount of the basic form of MTB monitored
colorimetrically at 460 nm is the measure of sulfate concentration in the
sample.:
4.4.1.2 This method is applicable to the collection of 24-hr samples in the
field and subsequent analysis in the laboratory.
4.4.2 Range and Discrimination Limit
4.4.2.1 The range of the analysis is 3.0 to 95.0 M9 SO^/mL. With 40 mL of
extract from 1/12 of the exposed high volume filter, collected at a sampling
rate of 1.7 nrVmin (60 ftVmin) for 24 hr, the range of the method is 0.6 to
19 ug/m3. The lower limit may be extended by increasing the portion of fil-
ter extracted. Determination of concentrations greater than 95 pg/mL re-
quires dilution with distilled water.
4.4.2.2 A limit of discrimination must be defined so that possible S04 con-
tributions from filters are not falsely reported as particulate sulfate.
Since individual blanks are not available from each filter used for sampl-
ing, the mean unexposed filter value is subtracted from each result to ob-
tain the best estimate of particulate sulfate concentration.
Randomly select 30 unexposed filters from the batch of filters used.
Cut one 3/4-in. by 8-in. strip (see Section 4.1.2) from each filter anywhere
in the filter. Analyze all strips separately for S04 content (Mfa).
Calculate the filter batch mean, "f^, from the Mb values for each fil-
ter; and the standard deviation, crblan(c- If T£ is less than the instru-
mental detection limit, no correction for the sulfate in the filters is
necessary. If MT is greater than the instrumental detection limit, Mfa is
-------
Section No. 4.4
Revision No. 0
Date 5/7/80
Page 2 of 17
subtracted from the total sulfate content of each particulate-bearing filter
when calculating the net sulfate concentration in the particulate.
Determine the smallest atmospheric concentration of sulfate that can be
reliably distinguished from the filter's contribution by multiplying the
standard deviation for the filter batch by 3.3, and dividing by the average
volume of air sampled, usually 2,500 m3.
LD = 3'3 (ablank)/2'500 = ^/m3
l_n = the discrimination limit. This is the smallest concentration of
sulfate per cubic meter of air sampled that can be reliably distinguished
from a possible false contribution of an individual filter.
If LD is unacceptably large, another batch of filters must be sought.
4.4.3 Interferences
Cations, such as calcium, aluminum, and iron interfere by complex!ng
the methylthymol blue. These ions are removed by passage through a cation-
exchange column.
4.4.4 Precision and. Accuracy
4.4.4.1 A single laboratory's relative standard deviation based on the
analyses of duplicate strips is about 4 percent.
4.4.4.2 Recoveries on spiked high volume strips and SRM (Standard Reference
Material) 1648 exceed 90 percent.
4.4.5 Apparatus
4.4.5.1 Sampling—
Apparatus as specified in "Appendix B - Reference Method for the Deter-
mination of Suspended Particulates in the Atmosphere (High Volume Method)"2
is appropriate.
4.4.5.2 Analysis—
4.4.5.2.1 Technicon I_I analyze!—An automated analytical system
(Figure 4.4.1) must be used for the determination of water soluble sulfate
-------
SULFATE IN ATMOSPHERIC PARTICIPATES
RANGE: 3-95 /jg/mL SO^
RATE: 40SAMPLES/HR
SAMPLE TO WASH TIME RATIO: 2:1
ION EXCHANGE COL.
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15 mm F/C x
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ORN/ORN (0.42) SODIUM HYDROXIDE
GRN/GRN (2.00) FROM FC (SILICON)
WASTE
NOTE: 1 FIGURES IN PARENTHESES SIGNIFY FLOW RATE (mL/min)
2 PUMP TUBES ARE TYGON UNLESS OTHERWISE MARKED
Figure 4.4.1. Schematic diagram of the automated Technicon II analyzer.
"O O 73 O~i
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-------
Section No. 4.4
Revision No. 0
Date 5/7/80
Page 4 of 17
by this method. Alkaline solutions of methylthymol blue decompose on expos-
ure to air. The method, therefore, cannot be adapted to a manual procedure.
The Technicon II Automated Analyzer System (manufactured by Technicon
Instrument Corp., Tarrytown, NY 10591) consists of the following com-
ponents:
Technicon autoanalyzer sampler IV—With a 40 sample/hr cam having a 2:1
sample to wash time ratio.
Proportioning pump III—Capable of supplying independently variable
flow rates in eight supply lines as shown in Figure 4.4.1.
Mixing coils—Two double 10-loop mixing coils 1.75 in. (43 mm) long and
1.25 in. (30 mm) wide. One 5-loop mixing "coil 1.25 in. (30 mm) long.
Ion-exchange column—A glass U-tube about 3.5 in. (87 mm) long (Tech-
nicon No. 116-G-006-01).
Single channel colorimeter—A stable colorimeter' suitable for use at
460 nm.
Flow ce11--15-mm tubular flow cell.
Linearizer—The sulfate response does not conform to Beer's Law. The
linearizer is required to obtain readings directly proportional to concen-
tration.
Dual channel recorder—Strip chart recorder matched to the linearizer
output.
Modular digital printer—Converts analog signal from the recorder to
digital printout in ug/mL.
Pump tubing—Certified flow-rated tubing of the capacities shown in
Figure 4.4.1.
4.4.5.2.2 Volumetric flasks—Class A, 100-, 200-, 500-, 1000-mL capac-
ity.
4.4.5.2.3 Pipets—Class A, assortment from 1-mL to 100-mL volumetric.
4.4.5.2.4 Pyrex glass wool
4.4.5.2.5 Rubber pi pet bulb
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Section No. 4.4
Revision No. 0
Date 5/7/80
Page 5 of 17
4.4.5.2.6 Polyethylene bottles—120-mL (4 oz) capacity fitted with
polyseal caps.
4.4.5.2.7 Glass bottles (clear)—60-mL (2 fl oz) capacity with poly-
seal caps.
4.4.5.2.8 Glass bottles (amber)—500-mL capacity with polyseal caps.
4.4.5.2.9 Technicon sample cups (disposable)
4.4.5.2.10 Repipet
4.4.5.2.11 Centrifuge tubes--5Q-mL capacity.
4.4.5.2.12 Centrifuge—Drucker 803 or equivalent.
4.4.5.2.13 Ultrasonic bath—Sonix IV or equivalent.
4.4.6 Reagents
4.4.6.1 Sampling—
4.4.6.1.1 Filter media—Filter media as specified in "Appendix B -
Reference Method for the Determination of Suspended Particulates in the
Atmosphere (High Volume Method)."2
4.4.6.2 Analysis—
4.4.6.2.1 Ammonium chloride—ACS reagent grade.
4.4.6.2.2 Ammonium hydroxide, concentrated—ACS reagent grade, 28
to 30 percent NH3.
4.4.6.2.3 Ion-exchange resin—300 to 850 urn (20 to 50 mesh) Bio-
Rex 70, sodium form, or equivalent.
4.4.6.2.4 Deionized water—Specific conductance of 2 umho or less.3
4.4.6.2.5 Etnanol — 95 percent U.S.P.
4.4.6.2.6 Methyltnymol blue (MTB)—3' t3"-bis[N, N-bis (carboxymethyl)-
amino]methyl thymolsulfone-phthalein pentasodium salt. 96 percent minimum
by spectro analysis. Eastman No. 8068 or equivalent.
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Section No. 4.4
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4.4.6.2.7 Potassium chloride—ACS reagent grade.
4.4.6.2.8 Sodium hydroxide—ACS reagent grade.
4.4.6.2.9 Hydrochloric acid, concentrated—ACS reagent grade, 36.5
to 38.0 percent HC1.
4.4.6.2.10 Sodium sulfate—ACS reagent grade, anhydrous.
4.4.6.2.11 Tetrasodium salt of EDTA--Tetr'asodiuni ethylenediamine
tetraacetate, technical grade.
4.4.6.3 Reagent Preparation—
4.4.6.3.1 Sodium hydroxide solution .(0-08 N)--Disso1ve 1.5 g of sodium
hydroxide in distilled water in a 500-mL volumetric flask and dilute to
volume.
°4.4.6.3.2 Hydrochloric acid solution (1.0 N)—Add 8.3 mi of concen-
trated hydrochloric acid to distilled water in a 100-mL volumetric flask and
dilute to volume.
4.4.6.3'. 3 Barium chloride solution (0.006 M)—Dissolve 1.4659 g of
barium chloride dihydrate (BaCl2-2H20-)- in distilled water in a 1-L volumet-
ric flask and dilute to volume.
4.4.6.3.4 Methyl thymol blue solution (0'. 0062 M)—To 0.1350 g of MTB in
a 500-mL volumetric flask add, successively, 25 ml of barium chloride solu-
tion and 4 ml of 1.0 N hydrochloric acid. Dilute to volume with 95 percent
ethanol. Prepare fresh daily, and store in an amber glass bottle.
4.4.6.3.5 Buffer (pH 10.1)—Dissolve 6.75 g of ammonium chloride
(NH4C1) in 500 ml of distilled water. Add 57 ml of concentrated ammonium
hydroxide (NH4OH) and dilute to 1,000 ml with distilled water. Adjust the
pH to 10.1 with additional HN4OH.
4.4.6.3.6 Buffered EDTA (wash solution)—Dissolve 40 g of tetrasodium
EDTA in pH 10.1 buffer solution and dilute to 1,000 ml with additional buf-
fer solution.
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Section No. 4.4
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4.4.6.3.7 Stock sulfate solution (1,000 mg SCU/L)--Disso1ve 1.4789 g
of sodium sulfate (Na2S04), which has been dried at 105° C for 4 hr and
equilibrated to room temperature in a dessicator over anhydrous magnesium
perchlorate, in distilled water in a 1-L volumetric flask, and dilute to
volume. Store under refrigeration.
4.4.6.3.8 Blank reagent color solution—To a 500-mL volumetric flask,
add 4 ml of 1.0 N hydrochloric acid and dilute to volume with 95 percent
ethanol.
4.4.6.3.9 Potassium chloride solution (0.05 M)--Dissolve 3.7 g of KC1
in 1,000 ml of C02-free distilled water.
4.4.6.3.10 Ion-exchange column preparation—Stir the resin into dis-
tilled water; decant the fines before they settle. Soak the resin .before
use, at least overnight; store under distilled water until used.
To pack the column, insert a small piece of glass wool into one end of
a clean U-tube. Attach a rubber pipet bulb to the end of the tube contain-
ing the glass wool plug. Place the other end of the tube in the vessel con-
taining the prepared resin and operate the rubber bulb until the tube is
filled with resin. Replace the resin column after each fuTl day's use.
4.4.6.3.11 Calibration standard preparation—Pipet 50.0 ml of stock
sulfate solution containing 1,000 mg SO^/L into a 500-mL volumetric flask
and dilute to volume with distilled water. This intermediate sulfate solu-
tion contains 100.0 pg SO^/mL. Pipet 25, 40, 55, 70, 80, and 95 ml of this
intermediate solution into separate 100-mL volumetric flasks and dilute to
volume with distilled water to obtain standard solutions containing 25, 40,
55, 70, 80, and 95 ug SO^/mL, respectively.
4.4.6.4 Cleaning—
4.4.6.4.1 Tubing and samp 1 e cups—Use sample cups once, as received,
and discard. Flush tubing for 15 min with deionized water after installa-
tion on the instrument.
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Section No. 4.4
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4.4.6.4.2 Extraction vessel cleaning—Using laboratory detergent and
brush, scrub the vessels and caps thoroughly. Rinse well with copious quan-
tities of tap water. Finish with a thorough deionized water rinse. Allow
to air dry, covered, in a clean room or in a convection oven at a low tem-
perature.
4.4.7 Analytical Procedure
4.4.7.1 Sample Extraction-
Using gloves or forceps, fold or roll the sample and fit it into the
bottom of the centrifuge tube. Using a repipet, or other device of similar
accuracy and precision, add 40 ml of deionized water to the tube. The water
should completely cover the filter. Cap the tube tightly. Allow to stand
at room temperature for several hours, usually overnight.
Operate the ultrasonic cleaner for 30 min after adjusting the bath
level to the correct height. (This will raise bath 'temperature to about
50° C.)
Place tubes upright in a rack in the ultrasonic cleaner so that filters
are well under the level of the bath liquid, but the bath liquid remains
well below the cap of the tube. If ...centrifuge tubes with screw caps are
used, loosen all-, caps slightly, making them "finger tight." (Tubes will not
withstand repeated cycling to elevated pressures.) If snap caps are used,
no other preparations are required.
Ultrasonicate for a period of 30 min. Remove from the bath. Dry the
exterior and centrifuge at 2,000 rpm for 20 min.
Decant the centrifuge sample carefully, without disturbing the solids,
into a clean, labeled, storage bottle or take directly to analysis.
4.4.7.2 General —
A Technicon II Analyzer is employed for analysis. A flow diagram and
reagent flow rates are shown in Figure 4.4.1. The absorbance is measured at
460 nm using a flow cell with a path length of 15 mm. The sample turntable
rate is 40 samples per hour with a 2:1 sample to wash time ratio. The
elapsed time between sample pickup and the corresponding peak is approxi-
mately 6 min.
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Section No. 4.4
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4.4.7.3 Autoanalyzer Startup—
Turn on the analyzer. Place the MTB line and NaOH line in distilled
water for 2 to 3 min. Remove the ion-exchange column and replace it with
transmission tubing. Transfer the MTB, NaOH lines, and the sample dilution
line to the EDTA solution container for 10 min. Finally, wash all liquid
lines with distilled water for 10 min.
Set the ion-exchange column in place and flush with water for 5 to
10 min. Start reagents flowing through the system. The sample in the flow
cell must be free of bubbles during operation. Refer to manufacturer's
instructions for general operating procedures.
Operate the instrument until a stable baseline is obtained. This nor-
mally requires a minimum of 30 min.
When operating the automatic analyzer, air bubbles should not be
allowed to enter the ion-exchange column. If air bubbles become trapped,
the ion-exchange column should be replaced with a new column.
4.4.7.4 Setting the Baseline--
The full range of the recorder is used, from 0 to 100 percent, and must
be adjusted appropriately. Set the ba'sreline to zero at the beginning of the
analysis and do not adjust thereafter.
With the linearizer set on "Direct," and the colorimeter on "Damp 2,"
turn on recorder "Chart Drive."
With aperture "A" on the colorimeter kept open (turned all the way
counterclockwise), turn aperture "B" counterclockwise until recorder pen
approaches "0" baseline.
To synchronize the recorder with the printer:
1. Turn rotary display switch to "Full Scale."
2. Set recorder indicator to 100 using "Full Scale" screw.
3. Set meter on printer to 100 with "Calibration" control.
4. Turn rotary display switch to "zero."
5. Set recorder indicator to 0 using "zero" screw.
Return the rotary display switch to "Damp 2." Turn the "Baseline" control
on the colorimeter all the way counterclockwise and then back five times.
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Section No. 4.4
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Use aperture "B" to adjust the recorder pen to about 2. Use the "Baseline"
control for fine adjustment of the pen to 0. Observe the baseline and allow
to s-tabilize. Deflection should not be more than 0.3.
4.4.7.5 Calibration of Linearizer--
When a steady baseline has been established, calibrate the linearizer
by analyzing five 100-ppm standards and then four deionized water blanks,
and by adjusting the equipment:
1. Load five 100-ppm standards and four water blanks onto the sampler
turntable, filling the sample cups to capacity.
2. Start the sampler by pressing the "Power" control.
3. Observe the recorder chart and press the printer "Start Pr_int"
control at the apex of first peak. If the concentration of this
standard reads 98.0 to 99.5 ppm, observe the second peak before
making any adjustments. If necessary, adjust the "STD CAL" con-
trol (potentiometer or pot) on the colorimeter. A one-unit change
in pot setting will result in a 0.4-ppm change on the recorder
chart. (Note: potentiometer setting is usually 430 to 440).
4. Immediately after the fourth blank has been recorded, adjust the
"Baseline" control on the colorimeter so the concentration meter
on the printer reads 0 or 0.1.
5. Repeat the five 100-ppm standards by returning the sampler turn-
table to the starting position after the fourth blank has been
sampled. (This occurs while first blank is being recorded.) It
may be necessary to advance or retard the printer timing to syn-
chronize printing with the peak apex. Use the "Advance Print"
and/or "Retard Print" controls on the printer while the recorder
pen is moving upscale.
For ease in predicting peak location, position the recorder chart paper
so that printing occurs on a vertical grid marker.
Repeat calibration steps until the last three 100-ppm standards read
99.8 to 100.2 and exhibit good reproducibility.
Reset the linearizer control to "linear."
4.4.7.6 Sample Analysis—
Load the sample tray with the set of calibration standards so that two
samples from each standard are run at the beginning of each day's activity.
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Section No. 4.4
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The standards should be in a completely random order on any given day, and
the order should change on different days.
Following the standards, load the tray with the samples to be analyzed.
In every tenth position, place one of the quality control standards (see
Section 4.4.10.1). The final sample analyzed before shutdown should be a
quality control standard (or both of them if two are used).
If any extracts to be analyzed are colored, rerun that group of ex-
tracts after replacing the MTB solution in the analyzer with the "Blank
Reagent Solution" (Section 4.4.6.3.8).
4.4.7.7 System Shutdown—
After completing the final analysis, the system should be cleaned with
deionized water. The sample line may be conveniently washed during "this
operation by shutting off the turntable when the sample probe is in the wash
position. All liquid lines should be left filled with water after the
system has been washed if daily use is anticipated. However, if the system
is idle for one week or more, all lines must be drained and dried. A coat-
ing that cannot be removed by the EDTA wash will slowly build up on the flow
cell windows. This buildup is indicated by a loss in colorimeter sensitiv-
ity and may be corrected by washing the cell with 1 N HC1 followed by an
acetone and then a distilled water wash.
4.4.8 Calculations
Calculations must be done in the following order:
1. Correct for carryover.
2. Correct for instrument drift.
3. Correct for intrinsic extract color.
4. Correct for filter contribution.
5. Compute atmospheric concentration.
4.4.8.1 Carryover Contamination—
Carryover contamination occurs because of the small wash volume used
between samples. For the sample of interest, a simple mass balance on a
volume element, assuming adjacent sample contamination only, is expressed
as:
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Section No. 4.4
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- vC
correct ^observed J previous
The correction factor, y; is determined empirically. (In the IP Net-
work analysis laboratory, -y = 0.03 ug/mL.)
Correct all data, including standards, in order by applying 'this rela-
tion. (It will be adequate to use observed rather than corrected values of
the previous sample.)
4.4.8.2 Instrument Drift--
Determine the instrument drift using quality control samples and the
procedure described in Section 4.4.9.1. If necessary, apply this drift cor-
rection to the sample results.
4.4.8.3 Linearizer Digitize)—
It is assumed that the linearizer digitizer is set to read solution con-
centrations directly and that they are acceptably accurate (±5 percent). If
not, the calibration data must be fitted to a linear relation using least
squares:
Correct Cone = m(observed concentration) + b
If necessary, this relation is applied to the corrected data to obtain accu-
rate concentrations. Apply any necessary special dilution factor.
4.4.8.4 Instrinsic Color Contribution-
Subtract any intrinsic color contribution (see Section 4.4.7.6) after
completing Steps 4.4.8.1 to 4.4.8.3.
4.4.8.5 Mean Blank Filter Contribution--
Subtract the mean blank filter contribution, M, (computed in Section
4.4.2.2), if any.
4.4.8.6 Results-
Multiply the result (|jg SO^/mL) from Step 4.4.8.5 by: (40 ml/sample)
x (12 samples/filter); divide by the sample air volume (usually 2,500 m3) to
obtain the final concentration, C.
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Section No. 4.4
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4.4.8.7 Report--
Compare final result, C, with the discrimination limit, LD (Section
4.4.2.2). If C < LD, report BD (below detection); if C > I_D> report C.
Report on IBM forms (Figure 4.4.2) in appropriate keypunch format.
4.4.8.8 Computer Processing—
If computer processing is used, label samples as follows:
Type NAMS IP Network
Regular (4 letters) (4 letters)
Color Correction (4 letters)X (4 letters)X
Blind Duplicate (Up to 4 Numerals)Q (Up to 4 Numerals)P
QAB Strips (Last 4 Digits on (Last 4 Digits on
Strip)K Strip)K
Blanks (Serial Numerals)B (Serial Numerals)B
4.4.9 Quality Control
4.4.9.1 Quality Control Standards--
At least one quality control standard, prepared independently from
calibration standards, should be run routinely in every tenth position of a
tray. Its concentration should be near the middle of the working range
(50 ug SOj/mL).
Correct these QC data for carryover (Section 4.4.8.1). Then fit them
(least squares) to a linear relation in position number, assuming all posi-
tions in multiple tray runs are numbered sequentially, to obtain:
Cx = mx + CQ ,
where
C = observed concentration of quality control standard (QCS), cor
x rected for carryover, at position x;
CQ = concentration of QCS, estimated at position number 0;
x = position number of QCS;
m = slope of least squares line; and
mx = the drift correction.
-------
OATK.
PAGE.
-OF PAGE
Figure 4.4.2. IP Network data reporting form—inorganic analyses.
-o D TO en
fu cu fl> 0>
n> ->• H-
in —i.
M en -•• O
-£« ^^ O zj
CO O
O "Z. •
O
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Section No. 4 4
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Date 5/7/80
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Compute a , the standard deviation of m, and test (t-test) whether or
not m is signicantly different from zero. (Preprogrammed packages on desk
calculators are useful for this.)
If m ^ 0, correct all data for drift as below:
Correct = Cx ' mx
Correct values (ccorrect) should be within ±15 percent of expected (CQ).
Not more than seven consecutive values should be on the same side of the
mean, and the correction for the highest QCS position' number x should not be
more than about 10 percent C .
If m = 0, the above tests on corrected values should be applied direct-
ly to carryover corrected data.
If all tests are acceptable, continue data processing. Otherwise,
trouble shoot and rerun.
A second QC standard at 10 ug SO^/mL should be run and treated as if it
were a sample. This is below the calibration range but greater than 3l~.
It should be stable (a ±15 percent) and. accurate (±5 percent).
Blind replicate samples from which repeatability of performance can be
established are routinely included in sample sets. Pairs of results should
be collected and all pairs where any datum js below detection discarded.
The parameters of the distribution of differences of the remaining pairs
should -"be calculated in the usual manner. The standard deviation of this
distribution divided by V2 yields the estimate of the standard deviation for
an individual measurement.
4.4.9.2 System Maintenance—
4.4.9.2.1 Pump tubing—Certified flow rated tubing of the capacities
shown in Figure 4.4.1. Deviations from these flow rates are acceptable only
to the extent that a proper calibration curve and acceptable quality control
checks are obtained. The use of silicon rubber tubing in place of the
standard pump tubing is highly recommended for the MTB lines. Standard pump
tubing should be replaced every 21 days used. Other available tubing has
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Section No. 4.4
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Page 16 of 17
correspondingly longer life, with silicon rubber tubing having performed
satisfactorily for as long as 5 weeks. If a plasticized tubing is used, it
should be washed with acetone followed by distilled water prior to its use.
A broadening of the colorimeter output with a corresponding loss in
peak height usually indicates a performance decay in the pump tubing. At
the first indication of peak broadening, the pump tubing should be replaced.
The flow rates in the autoanalyzer system should be checked when the
system is originally set up and once a week thereafter. They should also be
checked when any system substitutions are made. Disconnect the specific as
it leaves the pump, and insert the line into a 10-mL graduated cylinder.
Operate the pump for 2 min. If the flow rate is in error by more than 5
percent, change the pump tubing and recheck the flow.
Preventive Maintenance—
Clean plates and pump rollers with ethanol.
Before installing ion exchange resin column, check passage of
one or more air bubbles through sample line. If breakup
occurs, pump ethanol through sample line briefly. If this
does not correct the .problem, replace segment of line in
which break appears.
a.
b.
a.
b.
c.
Monthly:
a.
b.
Replace sampler pump line and all tubing from sampling probe
to injection port.
Rinse sampling line connectors and probe well.
Clean sampling probe with nichrome wire.
Rinse system thoroughly with I N HC1 by pumping HC1 through
the MTB, sample dilution, and NaOH lines.
Replace all pump lines after HC1 rinse.
4.4.10 References
1. Lazrus, A. L. , K. C. Hill, and J. P. Lodge, "A New Colorimetric Micro-
determination of Sulfate Ion," presented at the Technicon Symposium,
Automation in Analytical Chemistry, New York, September 8, 1965.
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Section No. 4.4
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Page 17 of 17
2. "Appendix B - Reference Method for the Determination of Suspended Par-
ti culates in the Atmosphere (High Volume Method)," Federal Register, ^36
(84):8191-6194, 30 April 1971.
3. ASTM Standards (Water, Atmospheric Analysis), Part 23, October 1969
(p. 225).
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Section No. 4.5
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Page 1 of 15
4.5 PROCEDURE FOR THE ANALYSIS OF NITRATES IN ATMOSPHERIC PARTICULATES
COLLECTED BY HIGH VOLUME SAMPLERS (AUTO-TECHNICON II PROCEDURE)
4.5.1 Principle and Applicability
4.5.1.1 Particulate matter is collected by drawing air through a glass-
fiber filter with a high volume sampler. The exposed high volume filters
are extracted with water and analyzed for nitrates by reduction of the
nitrate to nitrite by a copperized-cadmium reductor column. The nitrite is
reacted with sulfanilamide in acidic solution to form a diazo compound.
This compound then couples with N-1-naphthylenediamine dihydrochloride to
form a reddish-purple azo dye that is determined colorimetrically at 520 nm.
4.5.1.2 The method is applicable to the collection of 24-hr samples in the
field and subsequent analysis in the laboratory.
4.5.2 Range and Discrimination Limit
4.5.2.1 The range of the analysis is 0.1 to 20.0 ug NOs/mL. With a 40-mL
extract from 1/12 of the exposed high volume filter (3/4-in. by 8-in. strip)
collected at a sampling rate of 1.7 nrVmin (60 ftVmin) for 24 hr, the range
of the method is 0.05 to 7.4 ug/m3.
The lower limit of the range may be extended by increasing the portion
of filter extracted. Concentrations greater than 20 ug/mL are determined
after appropriate dilution with distilled water.
4.5.2.2 A limit of discrimination must be defined so that possible N03 con-
tributions from filters are not falsely reported as particulate nitrate.
Because individual blanks are not available from each filter used for sam-
pling, the mean unexposed filter is subtracted from each result to obtain
the best estimate of particulate nitrate concentrations.
Randomly select 30 unexposed filters from the batch of filters used.
Cut one 3/4-in. by 8-in. strip from each filter anywhere in the filter.
Analyze all strips separately for N03 content (M^).
Calculate the filter batch mean, M^", from the Mfa ^values for each fil-
ter. Calculate the standard deviation, CTblank. If Mb is less than the
instrumental detection limit, no correction for the nitrate in the filter is
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Section No. 4.5
Revision No. 0
Date 5/7/80
Page 2 of 15
necessary. If M, is greater than the instrumental detection limit, subtract
TT from the total nitrate content of each particulate-bearing filter when
D
calculating the net nitrate concentration in the particulate.
Determine the smallest atmospheric concentration of nitrate that can be
reliably distinguished from the filter's contribution by multiplying the
standard deviation for the filter batch by 3.3, and dividing by the average
volume of air sampled, usually 2,500 m3-
LD = 3-3 (ablank)/2'500 = MS/"3
Ln = The discrimination limit. This is the smallest concentration of
nitrate per cubic meter of air sampled that can be reliably distinguished
from a possible false contribution of an individual filter.
If LO is unacceptably large, another batch of filters must be sought.
4.5.3 Interferences
Some metal ions may form colored complexes having absorption bands in
the region of 520 nm.
4.5.4 Precision and Accuracy
4.5.4.1 Precision—
A single laboratory's repeatability based on the analyses of duplicate
strips from a given filter is about 6 percent.
4.5.4.2 Accuracy—
Recoveries on spiked high volume strips and SRM 1648 typically exceed
90 percent.
4.5.5 Apparatus
4.5.5.1 Sampling—
Apparatus as specified in "Appendix B - Reference Method for the Deter-
mination of Suspended Particulates in the Atmosphere (High Volume Method)"1
is appropriate.
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Section No. 4.5
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4.5.5.2 Analysis—
4.5.5.2.1 Technicon _U analyzer—An automated analytical system
(Figure 4.5.1) is used for the determination of nitrates by this method.
The Technicon II Automated Analyzer System (manufactured by Technicon
Instruments Corp., Tarrytown, NY 10591) consists of the following com-
ponents:
Technicon autoanalyzer sampler J.V—With a 40 sample/hr cam having a 1:3
sample to wash time ratio.
Proportioning pump III—Capable of supplying independently variable
flow rates in eight supply lines shown in Figure 4.5.1.
Mixing coils—One double 11-loop mixing coil 1.75 in. (43 mm) long and
1.25 in. (30 mm) wide. One 5-loop mixing coil 1.25 jn. .(.30-mm)
long.
Cadmium-reduction column—A U-shaped 14-in. length of 2.0-mm i.d. glass
tubing (Technicon No. 180-0000-01).
Single channel colorimeter
Flow cell — 15-mm tubular flow cell.
Dual channel recorder
Modular digital printer—Converts analog signal from the recorder to
digital printout in micrograms/milliliter.
Pump tubing—Certified flow-rated tubing of the capacities shown in
Figure 4.5.1.
4.5.5.2.2 Volumetric flasks—Class A, 100-, 200-, 500-, 1000-mL capac-
ity.
4.5.5.2.3 Pipets—Class A, assortment from 1-mL to 100-mL volumetric.
4.5.5.2.4 Pyrex glass wool
4.5.5.2.5 Centrifuge tubes—50-mL capacity.
4.5.5.2.6 Centrifuge—Drucker 803 or equivalent.
4.5.5.2.7 Repipet
-------
NITRATE IN ATMOSPHERIC PARTICULATES
RANGE: 0.1-20^g/mL NO^
RATE: 40SAMPLES/HR
SAMPLE TO WASH TIME RATIO: 1:3
6 TURNS f^ BLK/BLK (0.321 AIR
(170-0103-01) 1 vJ AMMONIUM
A2 QQQQ | /"^ GRN/GRN (2.00) CHLORIDE
rADM,,,MBEm,r.T,nM 1 »«-o«B9-oi ~ W...TE/ORN .0.23, SAMPLE
COLUMN ^-^
1 ^^ BLK/BLK (0.321 AIR
22 TURNS 1 1 ^
XXB.Jt- ... .. I...I COLOR REAGENT
1670370 | H6-0489-01 ^^ BLK/BLK (0.321 (NEDA)
O
__ WHITE/WHITE (0.60| WASTE
WASTF «^ J)
TO SAMPLER IV ^ ^^ GRN/GHN (2.001 WATER
_^ GRY/GHY (1.001 FROM F/C
WASTE WA-TC ^ VJ
^
NOTE: 1 FIGURES
•*5^^ FLOW R^
J^A^^L 2 PUMP TU
1 , _. *^ JQ p/c PUMP TUDC
INPARENTH
ME (mL/min)
BES ARE TYG
ISE MARKED
SAMPLER IV
COLORIMETER
620 uni
IS mm F/C 20 mm ID
199 B023-01
~O O 3D O1
CD (U n> (t)
»Q r+ < O
fD fD ->• c+
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Section No. 4.5
Revision No. 0
Date 5/7/80
Page 5 of 15
4.5.5.2.8 Technicon sample cups (disposable)
4.5.5.2.9 Ultrasonic bath—Som'x IV or equivalent.
4.5.5.2.10 Polyethylene bottles—120-mL (4-oz) capacity fitted with
polyseal caps.
4.5.5.2.11 Glass bottles (amber)--l-L capacity with polyseal caps.
4.5.6 Reagents
4.5.6.1 Sampling--
4.5.6.1.1 Filter media—Filter media as specified in "Appendix B -
Reference Method for the Determination of Suspended Particulates in the
Atmosphere (High Volume Method)."1
4.5.6.2 Analysis--
4.5.6.2.1 Ammonium chloride—ACS reagent grade.
4.5.6.2.2 Ammonium hydroxide, concentrated--ACS reagent grade, 28
to 30 percent NH3.
4.5.6.2.3 Wetting agent--Brij-35 (Technicon No. T-21-0110) 30 percent
solution.
4.5.6.2.4 Cadmium fil ings--Technicon No. Tll-5063.
4.5.6.2.5 Copper sulfate pentahydrate—ACS reagent grade.
4.5.6.2.6 Distil led water—Having a specific conductance of 2 umhos or
less.2
4.5.6.2.7 Hydrochloric acid, concentrated--ACS reagent grade, 36.5 to
38.0 percent HC1.
4.5.6.2.8 Nitric acid, concentrated--ACS reagent grade, 69.0 to 70.0
percent HN03.
4.5.6.2.9 NEDA, [n-(l-naphthyl)ethy1enediamine dihydrochloride]—ACS
reagent grade.
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Section No. 4.5
Revision No. 0
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Page 6 of 15
4.5.6.2.10 Phosphoric acid, concentrated"ACS reagent grade, 85 per-
cent H3P04.
4.5.6.2.11 Potassium nitrate—ACS reagent grade, anhydrous KN03.
4.5.6.2.12 Sulfani 1 amide—Eastman 4378.
4.5.6.3 Reagent Preparation—
•
4.5.6.3.1 Ammonium hydroxide working solution—To approximately
1,200 ml of distilled water add enough concentrated ammonium hydroxide to
obtain a pH of 8.5.
4.5.6.3.2 Ammonium chloride solution—Weigh 10.0 g NH4C1 (ammonium
chloride) and transfer to a 1-L volumetric flask. Add about 500 ml of the
ammonium hydroxide working solution and swirl to dissolve. Dilute to'volume
with ammonium hydroxide working solution. Add 0.5 ml wetting agent with a
pipet. Mix well and store at room temperature. (This reagent may have to
be filtered before use if it has stood for more than a day. If filtering is
necessary, use a 150-ml capacity Buchner funnel with a coarse pore fritted
glass filter.)
4.5.6.3.3 Color reagent—Weigh 0.60 g NEDA [n-(l-naphthyl )-ethy1ene-
diamine dihydrochloride] and 10.0 g sulfanilamide. Transfer to a 1-L volu-
metric flask. Add about 500 ml of distilled water and swirl to mix. Care-
fully add 100 ml concentrated phosphoric acid (H3P04). Stir mechanically
until solution is homogeneous. Dilute to volume with distilled water and
mix by inverting several times. Add 0.5 ml Brij-35. Mix well. Refrigerate
in an amber bottle.
Due to variable purity of the NEDA [n-(l-naphthyl)-ethylenediamine
dihydrochloride], the amount of this reagent necessary may vary from lot to
lot. If there is insufficient NEDA reagent, a nonlinear calibration curve
will result.
4.5.6.3.4 Nitrate stock standard (1,000 uq/mL)—Weigh 0.8153 g of pre-
viously dried potassium nitrate (KN03) and transfer to a 500-mL volumetric
flask. Dilute to volume with distilled water. Store under refrigeration.
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Section No. 4.5
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4.5.6.3.5 Hydrochloric acid solution (1.0 N) — Add 8.3 ml of concen-
trated hydrochloric acid to distilled water in a 100-mL volumetric flask and
dilute to volume with distilled water.
4.5.6.3.6 Stock copper sulfate solution (2 percent W/W)--Weigh 2.0 g
CuS04-5HO; transfer to a 100-mL volumetric flask and dilute to volume with
distil led water.
4.5.6.3.7 Working copper so1ution--Pipet 5 ml 2 percent CuS04 solution
into a 50-mL volumetric flask and dilute to volume with distilled water.
4.5.6.3.8 Cadmium reduction column preparation—A copper-cadmium
column is included in the autoanalyzer system to reduce nitrate to nitrite.
Columns may be reused. Prepare a new column each week (or after 200
analyses). Instructions are given below for preparation of new-columns" and
for handling if reused.
Note: Use caution in handling cadmium and wash hands thoroughly afterwards.
1. Fill U-tube with 1 N HC1.
2. Cd filings are stored under 1 N HC1 in a glass beaker. Add Cd
filings to within 3/4 in. of-each end of tube.
3. Insert wet glass wool plugs into each end of the tube.
4. Place column into autoanalyzer system immediately after the debub-
bler.
5. Allow deionized water to flow through column for 10 to 15 min to
remove HC1.
6. Place NH4C1 line into CuS04 solution for 2 to 3 min. Cd will turn
black in the first 2 to 3 in. of column. Allow to coat until
brown Cu color begins to appear.
7. Reverse column and treat other end with CuS04 solution about lh
min, so that both ends of column are well coated. Note: The first
end treated will be more heavily coated.
8. Again, reverse the column so that the first end coated is adjacent
to the debubbler.
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Section No. 4.5
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9. Change NH4C1 line to flask of deionized water for 10 min to rinse
column.
If a column is to be reused, insert it into the system and "activate"
it as follows:
1. Place NH4C1 line into CuS04 solution for about 20 seconds.
2. Reverse column and repeat CuS04 treatment if necessary.
3. Return first end coated to position adjacent to debubbler.
4. Place NH4C1 line in deionized water for 10 min to rinse column.
4.5.6.3.9 Calibration Standards—
4.5.6.3.9.1 100 ug/ml working standard—Pipet 50 ml of the nitrate
stock standard (Section 4.5.6.3.4) into a 500-mL volumetric flask. Dilute
to volume with distilled water.
4.5.6.3.9.2 Standard calibration solutions—Into seven clean 100-mL
volumetric flasks, pipet 20, 10, 8, 5, 2, 1, and 0.5 ml of the 100 vg/mL
working standard. Dilute to volume with distilled water and mix.
4.5.6.3.10 Cleaning £f sample cups and tubing—Use sample cups once,
as received, and discard. Flush tubing for 15 to 20 min with deionized
water after installation on the instrument.
4.5.7 Analytical Procedure
4.5.7.1 Sample Extraction—
Using gloves or forceps, fold or roll the sample and fit it into the
bottom of the centrifuge tube. Using a repipet, or other device of similar
accuracy and precision, add 40 ml of deionized water to the tube. The water
should completely cover the filter. Cap the tube tightly. Allow to stand
at room temperature for several hours, usually overnight.
Operate the ultrasonic cleaner for 30 min after adjusting the water
level to the correct height. (This will raise the bath temperature to about
50° C. )
Place tubes upright in a rack in the ultrasonic cleaner, so that the
filters are well under the level of the bath water, but the bath liquid
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Section No. 4.5
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remains well below the cap of the tube. If centrifuge tubes with screw caps
are used, loosen all caps slightly, making them "finger tight." (Tubes will
not withstand repeated cycling to elevated pressures.) If snap caps are
used, no other preparations are required.
Ultrasonicate for a period of 30 min. Remove tubes from the bath. Dry
the exterior and centrifuge at 2,000 rpm for 20 min.
Decant the centrifuged sample carefully, without disturbing the solids,
into a clean, labeled storage bottle; store or take directly to analysis.
These samples are stable at room temperature for 2 weeks.
4.5.7.2 General —
A Technicon II Analyzer is employed for analysis. A flow diagram with
reagent flow rates is given in Figure 4.5.1. Absorbance is measured at
520 nm using a flow cell with a path length of 15 mm. The sample turntable
rate is 40 samples per hour with a 1:3 sample to wash ratio. The elapsed
time between sample pickup and corresponding peak is approximately 7 min.
4.5.7.3 Autoanalyzer Startup—
Turn on the analyzer and start reagents flowing through the system.
The sample in the flow cell must be free of air bubbles during operation.
Refer to manufacturer's instructions for general operating procedures.
Operate the instrument until all the reagents are flowing through the
instrument properly and a stable baseline is obtained. This normally
requires a minimum of 15 min.
When operating the automatic analyzer, air bubbles should not be
allowed to enter the cadmium reduction column. If air bubbles become
trapped, the reduction column must be replaced with a new column.
An inability to adjust the lower calibration standards to read properly
while maintaining proper peak heights on the high calibration standards
usually indicates a performance decay in the pump tubing. At the first
indication of this, the pump tubing should be replaced.
The full range of the recorder (0 to 100 percent) is used. Adjust
appropriately. Adjust the baseline to zero at the beginning of the analysis
and do not reset thereafter.
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Section No. 4.5
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4.5.7.4 Sample Analysis and Calibration--
Load the sample tray with the set of calibration standards so that two
samples from each standard are run at the beginning of each day's activity.
The standards should be in a completely random order on any given day, and
the order should change on different days.
Following the standards, load the tray with samples to be analyzed. In
every tenth position, place one of the quality control standards (Section
4.5.10.1). The final sample analyzed before shutdown should be a quality
control standard (or both, if two are used).
4.5.7.5 System Shutdown--
After completing the final analysis, place the NH4C1 and NEDA solution
lines in distilled water for 5 min. Remove the cadmium reduction coT-umn,
being careful not to allow air bubbles in the column, and replace it with
transmission tubing. Continue washing the system for 30 min before shutting
down the analyzer. The sample line may be conveniently washed during this
operation by shutting off the turntable when the sample probe is in the wash
position. All lines should be left filled with water after the system has
been washed if daily use is anticipated. If, however, the system will be
idle for one week or more, all lines must be drained and dried.
4.5.8 Calculations
Calculations must be done in the following order:
1. Correct for instrument drift.
2. Correct for filter contribution.
3. Compute atmospheric concentration.
4.5.8.1 Instrument Drift--
Determine instrument drift using quality control samples and the proce-
dure described in Section 4.5.9.1. If necessary, apply this drift correc-
tion to the sample data.
4.5.8.2 Linearizer Digitizer—
It is assumed that the linearizer digitizer is set to read solution
concentrations directly and that they are acceptably accurate (±5 percent).
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If not, the calibration data must be fitted to a linear relation using least
squares:
Correct Cone = m(observed concentration) + b
If necessary, this relation is applied to the corrected data to obtain accu-
rate concentrations. Apply any special dilution factor if necessary.
4.5.8.3 Mean Blank Filter Contribution—
Subtract the mean blank filter contribution, M, (computed in Section
4.5.2.2), if any.
4.5.8.4 Results--
Multiply the result (ug NOs/mL) from Section 4.5.8.3 by: (40 ml/
sample) x (12 samples/filter). Divide by the sample air volume (usually
2,500 m3). It should be noted that no color correction is included due to
lack of detectable color interference in the N03 analysis.
4.5.8.5 Report--
Compare the final result, C, with the discrimination limit, Lr., calcu-
lated in Section 4.5.2.2. If C < LQ-, report BD (below detection); if C
> LD, report C. Record on IBM data forms (Figure 4.5.2) in appropriate key-
punch format.
4.5.8.6 Computer Processing—
If computer processing is used, label samples as follows:
Type NAMS IP Network
Regular (4 letters) (4 letters)
Color Correction (4 letters)X (4 letters)X
Blind Duplicate (Up to 4 Numerals)Q (Up to 4 Numerals)?
QAB Strips (Last 4 Digits on Strip)K (Last 4 Digits on Strip)K
Blanks (Serial Numerals)B (Serial Numerals)B
4.5.9 Quality Control
4.5.9.1 Quality Control Standards—
At least one quality control standard, prepared independently from
calibration standards, should be run routinely in every tenth position of a
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DATE.
PAOE. OF PAGE
Figure 4.5.2. IP Network data reporting form—inorganic analyses.
-u o x> to
(U (U (D fD
IQ c-l- < O
(T» O> -•• r»-
1-0 \ O 3
^J n
o ~^ :z
-h CO O
CD Z •
M O
Ul • -t^
CD en
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Section No. 4.5
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Page 13 of 15
tray. Its concentration should be near the middle of the working range
(10 ug NOs/mL).
Fit these data (using least squares) to a linear relation in position
number, x, assuming all positions in multiple tray runs are numbered sequen-
tially, to obtain:
= mx + CQ
where
C = observed concentration of quality control standard (QCS) at posi-
A.
tion x;
Cn = concentration of QCS, estimated at position number 0;
x = position number of QCS;
m = slope of the least squares line; and
mx = the drift correction.
Compute a , the standard deviation of m, and test (t-test, 95 percent
confidence level) whether or not m is significantly different from zero.
(Preprogrammed packages on desk calculators are useful for this.)
If m 2 0, correct all data for dr'fft as below:
C = C - mx
correct x
Correct values (C ,) should be ±15 percent of expected (CQ). Not
more than seven consecutive values should lie on the same side of the mean,
and the correction for the highest QCS position number should not be more
than about 10 percent C .
If m = 0, the tests for corrected values are applied directly. If all
tests are acceptable, continue data processing. Otherwise troubleshoot and
rerun.
Blind replicate samples from which repeatability of performance can be
established are routinely run in sample sets. These should be treated as
normal samples. When final results are computed, lists of pairs of results
should be prepared, discarding any pair where either result is below detec-
tion.
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Section No. 4.5
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The parameters of the distribution of the set of differences should be
computed in the standard manner. The standard deviation of this difference
distribution divided by V2 is the estimate of the standard deviation for a
single determination.
4.5.9.2 Preventive Maintenance—
Daily:
a. Clean plates and pump rollers with ethanol.
b. Treat cadmium column with copper sulfate solution.
c. Reverse column to alternate direction of flow.
Replace sampler pump line and all tubing from sampling probe to
injection port.
b. Rinse sampling line connectors and probe well.
Monthly:
a. Rinse system thoroughly with 1 N HC1 by pumping HC1 through NH4C1,
NEDA, and sampling lines (remove still probe first).
b. Replace all pump lines after HC1 rinse.
As needed, replace soiled glass wool plugs in Cd column.
4.5.9.3 Routine Maintenance—
4.5.9.3.1 Flow Rates—The flow rates in the autoanalyzer system should
be checked when the system is originally set up and once a week thereafter.
They should also be checked when any system substitutions are made. Discon-
nect each line as it leaves the pump and insert into a 10-mL graduated
cylinder. Operate the pump for 2 min. If the flow rate is in error by more
than 5 percent, change the pump tubing and recheck the flow.
4.5.9.3.2 Colorimeter Wavelength—The reddish-purple azo dye has a
maximum absorbance at 520 nm. The colorimeter wavelength accuracy should be
checked prior to use and quarterly thereafter. Maximum transmission of the
filter should occur at 520 ±15 nm.
4.5.9.3.3 Cadmiurn Reduction Column—If the response of the standards
becomes nonlinear, baseline separation becomes poor, or the Cd reduction
column appears shiny or silvery in spots, the column needs regeneration.
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Section No. 4.5
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Dump the column contents carefully into a beaker of dilute hydrochloric
acid. Decant into drum using copious quantities of water. Rinse the fili-
ngs with deionized water several times and proceed as directed in Section
4.5.6.3.7. Do not discard any Cd.
4.5.10 References
1. "Appendix B - Reference Method for the Determination of Suspended Par-
ticulates in the Atmosphere (High Volume Method)," Federal Register,
36(84): 8191-6194, 30 April 1971.
2. ASTM Standards (Water, Atmospheric Analysis), Part 23, October 1969
(p. 225).
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Section No. 4.6
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Page 1 of 1
4.6 PROCEDURE FOR THE ANALYSIS OF SULFATES IN ATMOSPHERIC PARTICULATES
(DIONEX METHOD)
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4.7 PROCEDURE FOR THE ANALYSIS OF LEAD IN ATMOSPHERIC PARTICIPATES
( METHOD)
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4.8 PROCEDURE FOR THE ELEMENTAL ANALYSIS OF ATMOSPHERIC PARTICULATES (X-RAY
FLUORESCENCE METHOD)
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CONTENTS
Section Page
5 QUALITY ASSURANCE 1
5.1 INTRODUCTION 1
5.2 ORGANIZATION 2
5.3 QUALITY ASSURANCE POLICY AND
OBJECTIVES 2
5.3.1 Quality Assurance
Policy 2
5.3.2 Quality Assurance Pro-
gram Objectives 6
5.4 DOCUMENTATION AND DOCUMENT
CONTROL 6
5.4.1 Document Control 6
5.4.2 Reports 7
5.4.3 Internal Documentation . . 7
5.5 TRAINING 7
5.6 PREVENTIVE MAINTENANCE 8
5.7 SAMPLE COLLECTION AND
ANALYSIS 8
5.8 CALIBRATION 9
5.8.1 Balance Calibration. ... 9
5.8.2 Sampler Flow Rate
Calibration 9
5.8.3 Analytical Instrument
Calibration 42
5.9 CORRECTIVE ACTION 45
5.10 IP NETWORK AUDIT PROGRAM 45
5.11 DATA VALIDATION AND STATISTICAL
ANALYSIS OF DATA 46
5.12 DATA QUALITY ASSESSMENT: PRE-
CISION AND ACCURACY 46
5.12.1 Precision and Accuracy
of Sampler Performance . . 47
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CONTENTS (continued)
Section
5.13 ASSESSMENT OF PRECISION AND
ACCURACY OF PROCEDURES USED
FOR ANALYSIS OF IP NETWORK
FILTERS 54
5.13.1 Mass Determination--Pre-
• cision and Accuracy. ... 54
5.13.2 Chemical and Elemental
Analysis—Precision and
Accuracy 55
5.14 EVALUATION AND VALIDATION OF IP
METHODOLOGY . . 60
5.14.1 Validation of Dichotomous
Samplers 60
5.14.2 Flow Measurement and
Field Audit Device .... 61
5.14.3 Evaluation of Dichotomous
Samplers 61
5.14.4 Wind Tunnel Test of the
Inlet 61
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Section No. 5
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SECTION 5
QUALITY ASSURANCE
5.1 INTRODUCTION
Th§ EPA Environmental Monitoring Systems Laboratory (EMSL/RTP) has the
responsibility of establishing a nationwide monitoring network for inhalable
particulates (IP). The rationale for and purpose of establishing the IP Net-
work are described in the "Protocol for Establishment of a Nationwide Inhal-
able Participate Network," included as Appendix A in this document.
Implementation of the Network requires siting, equipping, and maintain-
ing 300 sites; providing mass determination and chemical analysis of the
collected samples; and processing the resulting data.
Inherent in the design and implementation of any field monitoring net-
work is a detailed program of quality assurance (QA). QA functions are de-
fined in federal regulations for the monitoring of criteria pollutants. The
importance of a well-defined QA program has recently been reemphasized by
issuance of an EPA Quality Assurance Policy Statement, which mandates the
establishment of QA programs in all EPA monitoring activities. The objec-
tive of a QA program is to ensure that data produced meet the user's require-
ments in terms of completeness, precision, accuracy, representativeness, and
comparability.
Quality assurance has been an integral part of the IP Network from the
planning stages on. In particular, an effort has been made to incorporate
QA elements into each of the major program areas of the IP Network: siting,
field monitoring, sample analysis, and data reduction and validation. The
QA plan developed for and implemented in the IP Network describes the QA
activities for each of these areas.
This section outlines the overall QA plan for the IP Network. More
detailed information is given in those sections of this document covering
specific areas of the IP Network.
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Section NO. =>
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5.2 ORGANIZATION
The operation and maintenance of the IP Network are the responsibility
of EMSL/RTP (Figure 5.1). The organizational structure within EMSl/RTP for
the IP Network is shown in Figure 5.2. Key personnel of the IP Network are
listed in Table 5.1.
Dr. Thomas Mauser, Director of the Laboratory, is responsible for
program direction.
Mr. Charles Rodes, project officer for the IP Network, has overall
responsibility for operation of the IP Network and supervises all
network field operations, including site selection and setup,
equipment purchase and setup, resupply, and maintenance.
Dr. Joseph Walling is responsible for analytical operations for
the Network. This includes filter weighing and chemical and-ele-
mental analyses.
»
Mr. Ralph Baumgardner is the QA coordinator for the Network. It
is his responsibility to carry out the QA plan developed for the
Network, to assess all data generated in the QA program, and, when
necessary, to recommend to the Project Officer changes to assure
better Network data quality.
Mr. Gardner Evans is responsible for data collection and valida-
tion. These responsibilities include designing and implementing
procedures for data storage, reduction, and validation, and provid-
ing for statistical analysis of the Network data.
Mr. Mack Wilkins is the IP Network Field Manager. He is responsi-
ble for all field site operations, including purchase and instal-
lation of equipment, site setup and instrument calibration, and
filter shipment and supply.
5.3 QUALITY ASSURANCE POLICY AND OBJECTIVES
5.3.1 Quality Assurance Policy
The QA policy for the IP Network is to provide support that will ensure
that all IP data are of sufficient quality to meet the Network objective of
establishing a valid data base for regulation and control of inhalable par-
ti culates.
The protocol for the IP Network (Appendix A) discusses the involvement
of QA in the Network operation and emphasizes its importance. In response,
a QA Program Plan has been designed and is being implemented.
-------
ENVIRONMENTAL MONITORING
SYSTEMS LABORATORY
Director
Dr. Thomas R. Mauser
829 2106
Deputy Director
Mr. Franz J. Burniann
629 21 00
1
Assurance
vision
inias Claifc
•2I9S
Methods
dilation Branch
litry Purdue
B29 2666
erformance
uation Branch
Vacant
B29-2723
Source
Branch
odney Midgelt
629 2195
ADMINISTRATION
AND SUPPORT OFFICE
Ms. Nell Cams
629 2351
1
Data Management and
Analysis Division
Mr. Gerald Akland
629-2346
Analysis and
Reports Branch
Mr. Harold Sauls
629 3123
Design and
, Analysis Section
Mi. Harold Sauls'
629-3123
Fuel Registration
and Reports Section
Mr. Donald Fair
629 2732
Data Management
Branch
Mr. Jon Clark
629-2346
Data Acquisition
Systems Section
Mr. Van Wheeler
629 2442
Data Base
Management Section
Mr. Thomas Lawless
029 2291
<
Environmental
Monitoring Division
Or. John Clements *
629 2454
Environmental Monitoring and
Techniques Branch
Mr. Thomas llartlage
629 3007
Field Monltorini
Section
Mr. Barry Martin
629 3076
Monitoring Techniques
Section
Mr. Charles Rodes
629 3076
Pollutant Analysis
Branch
Dr. Joseph Walling
629 2454
Source, Fuels, and Molecular
Chemistry Section
Mr. Joseph Bumgarncr
629 2430
Trace Element Analysis
Section
Mr. Warren Lesaks
629 2173
Commercial Telephone No. (919) 541 * Extension
February 1980
"Acting
Advanced Analysis
Techniques Branch
Dr. Richard Thompson
629 2454
~0 O 70 GO
QJ QJ fD fD
(Q r^ < O
fD fD —J- r+
(/) —".
co <_n ->. o
co -z.
CH CD O
IV)
Figure 5.1. Organizational structure of EMSL/RTP.
-------
Laboratory Director
Dr. T. Mauser
IP Network Project Officer
C. Rocles
Monitoring Techniques Section
Field Site
Operations
Mack Wilkins
Laboratory
Sample Analysis
Dr. J. Walling
QA
Data
Assessment
R. Baumgardner
Data
Validation
G. Evans
Monitoring
Data Assessment
C. Rocles, G. Evans
Field Flow
Audit
RTI
1
Lab Blind
Audit
J. Puzak
Lab Split
Sample
J. Puzak
External
Filter
Reweigh-NSI
TJ O TO U~\
a> (u n> CD
IQ r»- < n
n> (D —'• et-
ui -j.
-£=• en -"• o
"~-x O 3
o --j r>
-h -\
CD -z. ^
en CD o o
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Section No. 5
Revision No. 0
Date 5/7/80
Page 5 of 62
TABLE 5.1. IP NETWORK—KEY PERSONNEL
Name
Dr. Thomas R. Hauser
(Director, EMSL/RTP)
Mr. Charles E. Rodes
Responsibility
Program Direction
Overall Network
Telephone
919/541-2106
919/541-3076
EPA/RTP*
Mail drop
75
76
(IP Network project
officer)
Dr. Joseph F. Walling
Mr. Ralph E. Baumgardner
Mr. Gardner Evans
Mr. Mack Wilkins
(IP Network Field
Manager)
Implementation
and Management
Sample Analysis
Quality Assurance
Data Management
Maintenance and
Resupply
919/541-2455 78
919/541-2723 77
919/541-2292 75
919/541-3049 76"
^General Address: Environmental Protection Agency, EMSL
Research Triangle Park, North Carolina 27711
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Section No. 5
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Page 6 of 62
5.3.2 Quality Assurance Program Objective
The objective of the QA Program for the IP Network is to provide,
through well-defined QA functions, complete, precise, accurate, representa-
tive, and comparable data. This objective is accomplished using a number of
interrelated techniques.
Involvement of the QA coordinator in the planning and management of the
Network allows definition of areas where QA measures can be applied. Once
these areas are defined, procedures are developed to ensure that the data
gathered meet the objectives. These procedures combine internal quality con-
trol (QC) of the measurement process and QA elements such as corrective ac-
tion, data validation, and external assessment of precision and accuracy.
The interplay of each of these functions ensures that the data gathered in
the IP Network are accurate and precise within well-defined limits.
5.4 DOCUMENTATION AND DOCUMENT CONTROL
5.4.1 Document Control
A system of document control has been established for documentation of
all IP Network operations and procedures (i.e., siting, sampling, analysis,
quality assurance, data handling, and validation), and has been adhered to
in preparation of this "Inhalable Particulate Network Operations and Quality
Assurance Manual." This system is patterned after the indexing format of
the Quality Assurance Handbook for Air Pollution Measurement Systems, Vo 1. I,
March 1976, EPA-600/9-76-005, and allows for the updating of operational pro-
cedures and the addition of results of special studies and documents issued
in connection with the IP Network. The indexing format at the top of each
page includes:
Section No.
Revision No.
Date (of revision)
Page
This manual is provided in a loose!eaf binder to facilitate incorpora-
tion of revisions. A distribution list is maintained so that further ver-
sions of the manual and new sections can be routinely distributed to all man-
ual users.
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Section No. 5
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5.4.2 Reports
In addition to this manual, other reports will be issued by the IP
Network. These include the results of two IP pilot studies, the Philadelphia
Intensive Study, final reports of grants and contracts, an evaluation and
validation of IP methodology, and results of special studies such as the
Sample Loss in Shipment Study. Annual reports summarizing Network activities
and the status of the IP Network will be prepared. The QA coordinator for
the IP Network will issue a quarterly report summarizing the QA information
obtained during the period.
5.4.3 Internal Documentation
A central file of calibration data for all IP samplers will be main-
tained. A file will also be maintained for all calibrations of secondary
standards used, in calibration and performance auditing. A file of quality
control charts will also be maintained for analytical operations.
5.5 TRAINING
It is essential that all persons involved in any function affecting data
quality have sufficient training to p-erform their appointed tasks satisfac-
torily. It is the responsibility of the IP Network project officer and the
QA coordinator for the IP Network to evaluate the level of training neces-
sary to perform tasks related to the IP Network and to recommend appropriate
training.
Many separate and somewhat autonomous groups have various levels of re-
sponsibility in carrying out tasks related to the IP Network (contractors,
state and local air pollution agencies, and other EPA laboratories). Often
training can be most easily carried out by EMSL/RTP personnel directly
assigned to the IP project. For example, a program is underway in which
EMSL/RTP personnel are training contractor personnel in setting up IP sites.
The contractor will, in turn, train local and state agency personnel in this
function. Similar training programs in other areas will be instituted as
state and local agencies assume more responsibility for the Network opera-
tions. Training will be provided to other personnel in the IP Network as
required.
-------
Section No. 5
Revision No. 0
Date 5/7/80
Page 8 of 62
5.6 PREVENTIVE MAINTENANCE
A good program of preventive maintenance will increase measurement sys-
tem reliability and provide for more complete data acquisition. Preventive
maintenance is defined as a program of positive actions for preventing fail-
ure of monitoring and analytical systems.
A program of preventive maintenance is being developed for the IP Net-
work encompassing all sampling and analytical operations of the IP Network.
Specific preventive maintenance procedures and schedules are being developed
for field operations, filter weighing operations, and chemical analysis
operations. These maintenance procedures will follow guidelines- suggested
in the Quality Assurance Handbook for Air Pollution Measurement Systems,
Volume I, EPA-600/ 9-76-005 (March 1976).
5.7 SAMPLE COLLECTION AND ANALYSIS
In the IP Network, samples are collected onsite and transported to a
different location for analysis. In this multistep process, QC checks are
provided at each stage.
Filters used for collection of IP samples are weighed initially at
EMSL/RTP, using procedures outlined in Section 4 of this manual. Internal
QC checks are also detailed in that section. The filters are then shipped
to the IP site where sampling is performed. Quality control checks on sam-
pler flow rate, and sample validation criteria are detailed in Section 2 of
this manual.
The exposed filters are returned to EMSL/RTP, where they are logged in
and undergo further validation. The. filters are reweighed, additional QC
checks are performed, and those filters selected for chemical and elemental
analyses are sent to the appropriate laboratory. Weighing procedures, ana-
lytical methods, and relevant QC checks are detailed in Section 4 of this
manual.
Control charts are used to record results from selected QC checks to
determine if the analysis system is out of control. If the system is out of
control, corrective action will be taken.
-------
Section No. 5
Revision No. 0
Date 5/7/80
Page 9 of 62
5.8 CALIBRATION
A calibration plan has been developed for and implemented in the IP Net-
work. Calibration procedures for individual analytical or measurement proc-
esses are listed in the appropriate sections of this manual (Operations and
Maintenance, and Analysis). Calibration standard quality and calibration
interval or frequency are discussed below.
Calibrations are required in the IP Network areas of:
1. weighing operations (balances),
2. field operations (sampler flow rate), and
3. analytical operations (analysis "instrumentation).
5.8.1 Balance Calibration"
Balance calibration is performed each analysis day using internal bal-
ance standards. External weights traceable to NBS are used to check balance
calibration once per week. Specific procedures are given in Sections 4.1.3
and 4.2.3.
5.8.2 Sampler Flow Rate Calibration
5.8.2.1 Laboratory Calibration Procedures--
High volume, size selective, and dichotomous samplers used in the IP
Network are calibrated at EMSL/RTP using flow measurement devices (mass flow-
meters and dry test meters) that have been referenced to a positive displace-
ment volume standard traceable to the NBS, before being sent to the field.
Each sampler and each flow check device is calibrated for a specific sampling
site using temperature and pressure corrections based on the estimated sea-
sonal average site barometric pressure and temperature for the sampling peri-
od. Calibration data for IP Network samplers are updated semiannually.
5.8.2.1.1 Five-point laboratory calibration procedures for _IP Network
conventional and SSI high volume samplers—The procedures used for labora-
tory calibration of high volume samplers in the IP Network are identical to
those outlined for field calibration in Sections 2.3.7 and 2.4.7 of this
manual.
-------
Section No. 5
Revision No. 0
Date 5/7/80
Page 10 of 62
5.8.2.1.2 Laboratory calibration procedures for If Network dichotomous
samplers—This section presents technically sound flow rate calibration pro-
cedures for dichotomous samplers and for the field calibration check device
used in the IP Network. The procedures are designed to maximize the amount
of the total calibration, measurement, and data reduction function's that can
be performed in a laboratory situation, thereby reducing the burden of the
field operator in performing these activities in the field.
Standard operating procedures for the IP Network are as follows:
Each dichotomous sampler's rotameters are calibrated in the EMSL/
EPA-RTP facility before being shipped to the field.
A field calibration check device is calibrated in the EMSL/EPA-RTP
facility and shipped with the sampler(s) for performing calibra-
tion checks in the field.
Sampler rotameter calibrations are performed only when the field
calibration check shows the sampler's calibration to be out of
specification.
Important features of the calibration procedures presented here include:
Each sampler and each field calibration check device is calibrated
for a specific site. The average site barometric pressure is cal-
culated from the site elevation or based on measured values. Cali-
bration data for both sampler rotameters and calibration check de-
vices are calculated from the seasonal average site barometric
pressure and temperature for the period during which the sampler
is operating. Temperature and pressure corrections to calibration
data are updatecTsemiannually.
Flow rate calibrations are in terms of volumetric flow rates at
ambient conditions since the sampler's cutpoints are dependent on
a fixed actual flow and not a fixed flow at standard conditions.
The criterion for judging acceptability of the sampler's rotameter
calibration in the field is an agreement of ±10 percent or better
between the total flow rate indicated by the laboratory calibration
check device and that indicated by the rotameters adjusted to their
"set-points."
5.8.2.1.2.1 Traceability—Calibrations of the sampler rotameters and
the field calibration check device are traceable to the National Bureau of
Standards (NBS) via the following procedure. Primary standards such as bub-
ble flowmeters, spirometers, and frictionless pistons certified by NBS
-------
Section No. 5
Revision No. 0
Date 5/7/80
Page 11 of 62
are used to calibrate the mass flowmeter and dry gas meter as transfer stan-
dards which, in turn, are utilized to calibrate the sampler's rotameters and
the field calibration check device.
5.8.2.1.2.2 Precision and accuracy—The precision and accuracy of the
methods will be determined after sufficient data have been collected and
analyzed.
5.8.2.1.2.3 Apparatus--
Transfer standards—mass flowmeter, dry gas meter, or other flow mea-
suring devices traceable to NBS and capable of accurately (±2 percent at the
95 percent confidence level) measuring flows over the ranges of 0 to 20 L/min
and 0 to 5 L/min.
Barometric pressure gauge—a barometer capable of measuring barometric
pressure to the nearest 5 mm Hg (0.5 in. H20).
Timer—timer capable of measuring to 0.1 second for time intervals of
30 seconds up to several minutes.
Field calibration check device—a device designed to accurately measure
flow rates in the range of 5 to 20 L/min at conditions ranging from -5 to
+50° C and 550 to 800 mm Hg. Orifices with a liquid manometer or a magne-
helic gauge to read the pressure drop are satisfactory.
Dichotomous sampler—a dichotomous sampler properly serviced and checked
out for field use.
Filters—a set of filters similar to those used to collect samples in
the field.
Mi seellaneous—adapter to connect the orifice unit to the sampler.
Flexible tubing to connect the orifice unit to the manometer and to the mass
flowmeter.
Dry air—a dry air source capable of providing a flow of up to 40 L/min
at laboratory conditions.
NOTE: Dry air is recommended when using a mass flowmeter as the transfer
standard; room air is acceptable when using a dry gas meter as the
transfer standard.
-------
Section No. 5
Revision No. 1
Date 7/15/80
Page 12 of 52
5.8.2.1.2.4 Mass flowmeter calibration— A calibrated transfer standard
(mass flowmeter or dry gas meter) is provided by the Quality Assurance Divi-
sion (QAD) of EMSL/RTP. The mass flowmeter is accompanied with a properly
documented, computer-generated calibration curve and interpolation table.
The calibration is in terms of flow rate at standard conditions (750 mm Hg
and 298 K) as a function of the voltage.
The calibration setup should be configured so that only clean, dry air
passes through the mass flowmeter. A simple block diagram of the calibra-
tion setup is given in Figure 5.3. The primary standard may be a spirometer,
frictionless piston meter, or a bubble flowmeter, as appropriate for the flow
being measured. To calibrate the mass flowmeter:
1. Adjust the flow rate to approximately 19 L/min and let it flow un-
til a constant reading is obtained on the mass flowmeter (voltage
constant within 0.02 volts).
2. Time the flow of a predetermined volume (V ) through the primary
standard. Record V to the nearest 0.01 L and the time (t) in
minutes to the nearest 0.001 minute (or 0.1 second), whichever is
most convenient for the timer used. (Use the primary standard such
that t ^ 0.5 minutes.) Figure 5.4 is a sample transfer calibration
data form.
3. Read and record the mass flowmeter voltage at the beginning, mid-
dle, and end of the timed interval. Average the readings and re-
cord the average (F ) on a form such as in Figure 5.4.
4. Read and record the barometric pressure (P-,) and ambient tempera-
ture (T.j) in the laboratory.
5. Calculate the flow rate for the primary standard at standard con-
ditions by
= .392(Vm/t)(P1/T1).
NOTE: Vm, as measured by the primary standard, -must be corrected for
the volume of water vapor if the sample comes into contact with
water while in the primary standard.
Record the calculated value of Qstd(c) to the nearest 0.01 L/min
on the calibration form in Figure 5.4.
.
-------
CLEAN DRY
AIR SOURCE
^—
MASS
FLOWMETER
W
^*
PRIMARY
STANDARD
t^
^
VACUUM
PUMP
EXHAUST
Figure 5.3. Block diagram of transfer standard calibration setup.
-O 0 70 GO
CU CU (D
IQ r+ < O
fD (D —'• r+
in —'•
h-1 <_n —'• o
OJ ^ O 3
O ^^
-f> co 2: 2:
C3 O O
cn
ho
CD cn
-------
Section No. 5
Revision No. 0
Date 5/7/80
Page 14 of 62
Mass flowmeter S/N:
Date of calibration:
Calibrated by:
TRANSFER STANDARD CALIBRATION FORM
Barometric pressure (P,):
Ambient temperature (T-):
7 /
mm Hg
K
Cal ib ra-
tion
point
1
2
3
4
5
6
7
8
Primary standard
V,
t
Wc>
Transfer standard
Fv^
--
W")
Percent
difference
Power curve
regression
Y = A(X)B
A =
B =
r2 =
Figure 5.4. Sample transfer standard calibration form.
-------
Section No. 5
Revision No. 0
Date 5/7/80
Page 15 of 62
7. Repeat Steps 1-6 for flow rates of 15, 11, 7, 3, 2, 1, and 0 L/min.
8. Using the above eight data pairs, calculate a power curve regres-
sion of the form
Y = A(X)B
where
Y = Qstd(c), and
Both A and B should be very near 1.00 and the coefficient of
correlation (r2) should be r2 > 0.9990 for an acceptable set of
cal ibration data.
9. Use the average F recorded for the calibration flow rate -in the
regression equation and calculate the corresponding flow rate
(Q t(,(P), predicted flow rates). Record each predicted flow rate
on the calibration form in Figure 5.4.
10. Calculate the percent difference in the flows determined by the
primary standard and those predicted by the regression equation by
Percent difference = 100 (Qstd(P) - Qstd(C))/Qstd(C)
11. Any point showing a percent difference outside the range of ±2.0
should be rechecked.
12. Generate an interpolation table from the power curve regression
using voltage intervals of 0.1 V as illustrated in Figure 5.5 and
a calibration curve as illustrated in Figure 5.6.
5.8.2.1.2.5 Beckman dichotomous sampler and orifice cal ibration pro-
cedures—To calibrate the sampler and orifice:
1. Check the QAD-supplied calibration curve (Figure 5.6) and interpo-
lation table (Figure 5.5) to verify that they are correct for that
mass flowmeter (i.e., check the serial number) and that the cali-
bration is still valid (i.e., current within 3 months).
2. Set up the calibration system as illustrated in Figure 5.7. The
inlet of the mass flowmeter is connected to a vented manifold sup-
plied with a surplus of clean, dry air. The outlet of the mass
flowmeter is connected to the inlet of the field calibration check
orifice device having a similar operating range (0-20 L/min). A
-------
POWER CURVE REGRESSION - Y=A(X)
COEFFICIENT A = 1.035
COEFFICIENT B = 0.988
COEFFICIENT OF DETERMINATION (r2) = 0.9997
B
Section No. 5
Revision No. 0
Date 5/7/80
Page 16 of 62
FAMILY REGRESSION - SOLVING FOR Y
X
0.000000
0.500000
1.000000
1.500000
2.000000
2.500000
3.000000
3.500000
4.000000
4.500000
5.000000
5.500000
6.000000
6.500000
7.000000
7.500000
8.000000
8.500000
9.000000
9.500000
10.000000
10.500000
11.000000
11.500000
12. 000000
12.506000
13.000000
13.500000
14.000000
14.500000
15.000000
15.500000
16.000000
16.500000
17.000000
17.500000
18.000000
18.500000
19.000000
19.500000
20.000000
Y
0.000000
0.522051
1.035246
1.545151
2.052931
2.559137
3.064091
3.568008
4.071038
4.573293
5.074862
5.575814
6.076206
6.576085
7.075491
7.574459
8.073018
8.571194
9.069009
9.566485
10.063639
10.560487
11.057045-
11.553325
12.049341
12.545102
13.040619
13.535902
14.030960
14.525801
15.020432
15.514860
16.009892
16.503135
16.996993
17.490673
17.984180
18.477518
18.970693
19.463708
19.956567
Figure 5.5. Sample interpolation table for a mass flowmeter.
-------
20.0
18.0
16.0
Y=AXB
A= 1.00
B= 1.00
r2= 1.000
14.0
12.0
0 8.0
Mass Flowmeter S/N
Date of Calibration /_
Calibrated by:
6.0
4.0
2.0
0
0 2.0 4.0 6.0 8.0 10.0 12.0 14.0 16.0 18.0 20.0
Fv (volts)
CO
~O O 7C
Q) ft)
IQ r+ < n
O) rt> -"• r+
01 —'
t—' en ->• o
-•J
O
O ^^
-*i oo z z
O O O
en
rv>
CD en
Figure 5.6. Sample mass flowmeter calibration curve.
-------
DRY AIR
SUPPLY
T
MASS FLOWMETER
ORIFICE (FIELD CALIBRATION
CHECK DEVICE)
IP SAMPLER
COARSE
ROTAMETER
FINE
ROTAMETER
Figure 5.7. Schematic of Beckman laboratory calibration setup using a mass flowmeter
as a transfer standard.
T3 O 50 Cn
ID Ot (t> CD
ia <-+ < O
CD (t) —'• c+
M cn —'• o
oo ^^ o n
o \
-*> Co 2: z
o o o
ai
ho
CD cn
-------
Section No. 5
Revision No. 0
Date 5/7/80
Page 19 of 62
special adapter is attached to the orifice-manometer unit that
permits the unit to be connected to the sampler's inlet tube in
place of the standpipe.
3. With sampler in manual mode, shuttle a pair of filters into the
sampler according to the operational procedures in' Section
2.5.3.2.
4. Adjust the dry air supply to provide a flow rate well 'in excess of
the sampler requirements to the open manifold. (A flow rate of
30 to 40 L/min at laboratory conditions should be sufficient.)
5. Turn the sampler and mass flowmeter on and allow to warm up to
operating temperature (at least 5 minutes). The sampler's flow
control valves for both "coarse." and "fine" flowmeters should be
opened wide (full counterclockwise).
6. Leak-check the system by removing the manometer fro.m the orftice
and plugging both pressure taps and disconnecting and plugging the
mass flowmeter inlet line from the dry air manifold. The sam-
pler's rotameters should read zero. Check the sampler's vacuum
gauge and record its reading on the data sheet, as shown in Fig-
ure 5.8. If the mass flowmeter indicates that a leak exists, it
must be found and eliminated prior to continuing the calibration.
In particular, check to ensure that both filters are properly
sealed. Gently slide filters back and forth; if they have not
been sealed properly they wiTl snap into place.
7. Reconnect the 'manometer to the orifice and the mass flowmeter's
inlet line to the dry air manifold.
A. "Fine" rotameter and orifice calibrations--
1. Close the "coarse" flow control .valve finger tight (full clock-
wise); the rotameter ball should drop to the bottom of the tube.
2. Adjust the "fine" control valve to give a 20 percent of range
reading on the "fine" rotameter.
3. Read the following parameters and record on the data form:
Room (ambient) temperature (T,), K
Barometric pressure (P,), mm Hg
Mass flowmeter reading (F ) V
Pressure drop across the orifice (AP), in. H20
Sampler "fine" rotameter indication (I), arbitrary units
-------
Sampler type:
Serial no..
"I hie" or)I ice-manometer ID Mo
Calibrated by:
itl ibi'atinn standard type:
Serial nu..
Dale ul caIibratiun:
_ Site lucation:
Site elevation:
"Cojise" orifice-manometer III Nu.
(address)
Average silt barometric pressure (P*):
Average seasonal silt tempera I lire (I.):
laboratory (ambient) temperature (I,,) K lalioralory taiiimelrtc i)iub<.iiru (I',,). nu» lly leak Clieck Vacmin Cage Keailing: . in lly
IT K
leak check vacuum yage ceailiny: . in. lly
point
number
lion
•
H
Indication
volts
ass fluwuielei
flow rate
«w
stilLAiJn
(• low rdte
(Q rl- < O
fD n> —>• c+
1/1 —••
ro in —•• o
CD \ O 3
en
. oo z z
o o o
-------
Section No. 5
Revision No. 1
Date 7/15/80
Page 21 of 62
4. Repeat Steps 2 and 3 for rotameter settings representing flow rates
of 40, 60, 75, and 90 percent of the operating range (0-20 L/min).
5. Using the calibration curve (Figure 5.6) or the interpolation table
(Figure 5.5) provided with the mass flowmeter, calculate (or look
up on the table) the flow rate Q .. for the voltage reading (F )
for each calibration point. Record on the data form the value of
Qstd to four significant digits for the "fine" flows, for example,
15.01 stdL/min.
6. Convert the flow rates measured with the mass flowmeter to labora-
tory conditions using the following relationship:
Q! = WPstd/TstdWPl>
where
Q-, = volumetric flow through the mass flowmeter at laboratory
conditions, L/min;
Q td = flow rate at standard conditions indicated by the mass
flowmeter, stdL/min;
T-,, P, = laboratory temperature and pressure, respectively, K and
mm Hg; and
T t ,, P , . = standard temperature and pressure, respectively, K and
5LQ sza mm Hg.
Record the calculated Q, values on the data form shown in Fig-
ure 5.8.
7. Determine by measurement or calculation from the site elevation
the average site or field barometric pressure (P,) and record it
on the data form of Figure 5.8.
Note: The calculation based on site elevation is:
Pf(mm Hg) = 760(mm Hg) - 0.075(mm Hg/m) x elevation (m),
or = 760(mm Hg) - 0.023(mm Hg/ft) x elevation (ft),
where elevations above sea level are defined to be positive and
those below sea level are negative.
8. Determine the average seasonal site or field temperature (Tf) and
record it on the data form in Figure 5.8.
-------
Section No. 5
Revision No. 1
Date 7/15/80
Page 22 of 62
9. Calculate the flow rate at average seasonal site or field condi-
tions of P£ and T,; for each calibration point using tne relation-
, . i i
ship,
Qf = Q1C(P1/T1)(Tf/Pf)]1/2
where
Qf = the flow rate at average seasonal site or field con-
ditions of Tf, PT-, L/min;
Q, = the flow rate at laboratory conditions of T^, P-|,
L/min;
T,, P, = laboratory temperature and pressure, respectively,
1 ' K, mm Hg; and
T., P. = average seasonal site or field temperature and pres-
sure, respectively, K, mm Hg.
Note: This conversion for the orifice is accurate to within about
2 percent for the temperature and pressure ranges of this
project. Its applicability to the sampler's flow measure-
ment system is not known.
Record the calculated Q. values in the data form of Figure 5.8.
10. Field calibration check orifice unit calibration curve—Using the
five data points of Q^ and AP for the orifice in Figure 5.8, gener-
ate a calibration equation of the form
Qf (orifice) = A(AP)B
where
Qf = flow rate through the orifice unit at average seasonal
field or site conditions of temperature and pressure,
L/min; and
AP = pressure drop across the orifice, in. H20.
Note: If the exponent B is outside the range of 0.45 to 0.55 the
calibration results should be rechecked.
Generate a calibration plot of Q. (L/min) as the ordinate or
y axis and AP (in. H20) as the abcissa or x axis. A sample orifice
calibration curve is shown in Figure 5.9.
-------
INHALED PARTICUMTE NETWORK
DICHOTOMOUS FLOfcKJRIFICE CALIBRATION
EXPONT
FACTOR
C. COEF
0.463812
0. 007375
0.
CALIB.
DCT ORFiCIPD-45
0. 000-
DATE 10/
23. 0 C
. 759, 5
30/ 79
0
4 5 6 7 8 9 10 11 12
MANOMETER READING, IN H2O
Figure 5.9. Sample dichotomous flow orifice calibration curve.
~1
~T2 d> ~2& (y>
Cu DJ rt> ro
to r+ < n
rt) ID —«• H-
l\j tn —'• o
C.J \ O n
en
ro
CD Z 2:
C3 o O
-------
Section No. 5
Revision No. 1
Date 7/15/80
Page 24 of 62
Generate an interpolation table for the orifice-manometer unit
using the above calibration equation to calculate flow rates (Q_-)
at average field conditions for increments of AP of 0.10 in. H26.
A sample interpolation table is given in Figure 5.10.
This interpolation table will be used by the operator in the
field for the QC check on the sampler's total flow rate (see Sec-
tion 2.5.6.2)
10. "Fine" rotametei—using the five data pairs of Qj. and I in the
data form of Figure 5.8 under "fine" flow rate calibration, gener-
ate a linear regression equation of the form
Q- (sampler) = A I + B,
where
Q. ~ sampler's "fine" flow rate at field or site conditions;
L/min;
I = rotameter indication, arbitrary units;
A = slope of the linear regression equation, (L/min)/(rotam-
eter units); and
B = intercept of the regression equation, L/min.
Generate a calibration curve and interpolation table as illus-
trated in Figures 5.11 and 5.12, respectively.
The sampler flow rate at standard conditions in stdnrVmin is
calculated from the actual flow rate in mVmin at field conditions
by
Qstd = Qf
Qstd=.392Qf(Pf/Tf)
Calculate and record on the calibrated curve (Figure 5.11)
the setpoint for the rotameter; that is, calculate the rotameter
indication, I, that will yield a Q. (sampler) of 15.0 L/min.
NOTE: The interpolation table will be used by the field operator
to determine and report the sampling rate in nrVmin at
standard conditions based on an average rotameter indica-
tion for the sampling period. The provision of pre-
calculated Qstd values relieves the operator of making any
calculations other than to average the initial and final
rotameter readings.
-------
InMALED PARTICIPATE NETWORK
••OICHOTOMOU8 FLOW ORIFICE CALIBRATION DATA**
****** AUDIT ORIFICE t
~ *
HAN
RDO
0.0
0.1
0.2
0.3
0.4
0.3
0.4
0.7
O.B
0.9
1.0
1.1
1.2
1.3
1.4
1.3
1.4
1.7
1.8
l.V
2.'0
2.1
2.2
2.3
2.4
2.3
2.4
2.7
2.8
2.9
3.0
3.1
3.2
3.3
3.4
3.3
3.6
3.7
3.B
3.9
4.0
4.1
4.2
4.3
4,4
4.3
4.4
4.7
4.0
4.9
5.0
SLPM
0.0000
2.3563
3.5254
4.2551
4.Q42S
3.3927
3,8686
4.3033
4.7043
7.0B28
7.4373
7.7737
8.093B
B.4000
B.4V37
fl.9764
9.24V2
7.3129 "
9.74B3
10.0144
10.2377
10.4923
10.7213
10.9447
11.1429
11.3742
11.3831
11.7894
11.9902
12.1849
12.3801
12.349B
12.7343
12.9396
13.1200
13.2974
13.4723
13.4448
13.8144
13.9821
14.1472
14.3102
14.4710
14.6298
14.7847
14.9414
13.0947
13.2440
13.3936
15.5434
13.6899
M3/MJN
0.0000
0.0026
0.0033
0.0043
0.0049
0.0034
0.0039
0.0043
0.0047
0.0071
0.0074
0.0078
O.OOB1
0.0084
0.0087
0.0090
0.0092
0.0093
0.0098
0.0100
0.0103
0.0103
0.0107
0.0109
0.0112
0.0114
0.0116
0.0118
0.0120
0.0122
0.0124
0.0126
0.0128
0.0129
0.0131
0.0133
0.0133
0.0136
0.0138
0.0140
0.0141
0.0143
0.0143
0.0146
0.0148
0.0149
0.0131
0.0132
0.0134
0.0135
0.0157
HAN
RDO
3.1
3.2
3.3
3.4
3.3
3.4
3.7
3.B
3.7
4.0
6.1
4.2
4.3
4.4
4.3
4.4
4.7
4.8
4.9
7.0
7.1
7.2
7.3
7.4
7.3
7.4
7.7
7.8
7.9
B.O
8.1
B.2
8.3
8.4
8.3
8.4
8.7
8.8
8.9
9.0
7.1
7.2
9.3
7.4
7.3
7.6
7.7
9.B
9.9
10.0
10.1
SLPM
13.8347
13.9777
16.1177
16.2601
16.3770
16.3367
16.6730
16.8080
16.7418
17.0744
17.2058
17.3360
17.4632
17.3732
17.7202
17.8461
17.7710
18.0747
18.217?
18.3378
18.4607
18.3810
18.7003
IB. 8187
18.9362
19.0527
19.1688
19.2838
19.3781
19.3116
17.6244
17.7364
19.8476
19.7382
20.0680
20.1772
20.2837
20.3733
20.3006
20.6072
20.7130
20.8183
20.7230
21 .0270
21 . 1303
21.2333
21.3354
21 .4374
21 .3386
21.6392
21 . 73V3
M3/MIN
0.0158
0.0160
0.0161
0.0163
0.0164
0.0163
0.0167
0.0168
0.0169
0.0171
0.0172
0.0173
0.0173
0.0176
0.0177
0.0178
0.0180
0.0181
0.0182
0.0183
0.0183
0.0186
0.0187
0.0188
0.0189
0.0191
0.0172
0.0173
0.0174
0.0173
0.0176
0.0177
0.0178
0.0200
0.0201
0.0202
0.0203
0.0204
0.0203
0.0206
0.0207
0.0208
0.0207
0.0210
0.0211
0.0212
0.0213
0.0214
0.0215
0.0216
0.0217
HAN
RDQ
10.1
10.2
10.3
10.4
10.5
10.6
10.7
10.8
10.7
11.0
11.1
11.2
11.3
11.4
11.3
11.6
11.7
11.8
11.7
12.0
12.1
12.2
12.3
' 12.4
12.3
12.6
12.7
12.8
12.7
13.0
13.1
13.2
13.3
13.4
13.3
13.6
13.7
13.8
13.9
14.0
14.1
14.2
14.3
14.4
14.3
14.6
14.7
14.8
14.7
13.0
15.1
8LPH
21.7373
21.8387
21.7377
22.0364
22.1343
22.2320
22.3290
22.4236
22.5216
22.6172
22.7124
22.8070
22.7013
22.7750
23.0884
23.1813
23.2738
23.3658
23.4374
23.3487
23.6373
23.729?
23.817?
23.9093
23.7788
24.0876
24.1761
24.2642
24.3320
24.4373
24.3264
24.6130
24.6773
24.7853
24.8707
24.9362
23.0411
23.1257
23.2100
23.2740
23.3776
23.460?
23.343?
23.6266
23.7090
25.7711
25.8727
25.7344
26.0356
26.1165
26.1971
H3/MIN
0.0217
0.0218
0.0219
0.0220
0.0221
0.0222
0.0223
0.0224
0.0223
0.0226
0.0227
0.0228
0.022?
0.0230
0.0231
0.0232
0.0233
0.0234
0.0233
0.0233
0.0236
0.0237
0.0238
0.0237
0.0240
0.0241
0.0242
0.0243
0.0244
0.0244
0.0243
0.0246
0.0247
0.0248
0.024?
0.0230
0.0230
0.0231
0.0232
0.0233
0.0254
0.0253
0,.0253
0.0236
0.0237
0.0258
0.0237
0.0240
0.0260
0.0261
0.0262
HAN
RDO
13.1
15.2
13.3
13.4
13.3
13.6
13.7
13.8
13.9
16.0
14.1
16.2
16.3
16.4
16.3
16.6
16.7
16.8
16.7
17.0
17.1
17.2
17.3
17.4
17.3
17.6
17.7
17.8
17.7
18.0
18.1
18.2
18.3
18.4
18.3
18.6
18.7
18. 8
18.7
17.0
17.1
17.2
17.3
17.4
17.3
17.6
17.7
17.8
17.7
20.0
20.1
SLPM
26.1771
24.2774
26.3574
26.4372
24,5167
26.373?
26,6748
26.7333
26.831?
26.7100
26.987?
27,0633
27.142?
27.2200
27.276?
27.3733
27.4478
27.3260
27.6018
27.6773
27.7328
27.8280
27.702?
27, 9 77 6
28.0321
28.1263
28.2003
28.2741
28.3477
28.4210
28.4741
28.3671
28.6377
28.7122
28.7843
28.8366
28.7284
27.0001
27.0713
27.1427
27.2138
27.2844
27.3333
27.4237
27.4740
29.3660
29.633?
27.7056
27.7751
29.8444
29.9133
H3/HIN
0.0262
0.0263
0.0264
0.0264
0.0263
0.0266
0.0267
0.0268
0.0268
0.024V
0.0270
~ 0.0271
0.0271
0.0272
0.0273
0.0274
0.0274
0.0273
0.0276
0.0277
0.0278
0.0278
0.0279
'0.02BO
0.0281
0.0281
0.0282
0.0283
0.0283
0.0284
0.0283
0.0284
0.0286
0.0287
0.0288
O.O289
0.0289
0.0270
0.0271
0.0271
0.0272
0.0293
0.0294
0.0294
0.0273
0.0276
0.0274
0.0277
0.0278
O.0278
0.027?
Figure 5.10. Sample interpolation table for clichotomous flow orifice calibration.
~o o 20 u~>
CU OJ CD (D
(O
-------
INHALED PARTICIPATE NETWORK
BECKMAN DICHOTOMOUS SAMPLER EPA# 176108 S/N 056-909
FINE ROTAMETER CALIBRATION BY M. WILKINS
-
UJ
-c
QL
I*
o
_J
?
18.4)0 Data Point* " 3
Slops (A)' 0.9886
\6 4J0 Intiroapt (If) - 2. 0914
Co+ffioiwt (R) - 0. 9922
14.4*0 *-
0 i-
0
t - \-— -- -i—--- —H- - — i— -—i
2.00 4.00 6.00 8.00 10.00 12.00 14.00 16.
18.00 20.00
ROTAMETER READING
Figure 5.11. Sample calibration curve for Beck man "fine" rotameter.
~o o ;a en
(u (u CD a>
CQ c+ < n
fD (D -J- r+
in —>.
ro cn -j- o
en "\ o zj
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CD (_n
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ID fa m ID
to r-l < O
ID fD —'• r+
ivi t_n —•• o
^J ^^ O Z3
--I ZJ
o ^^
~t, ^ ^:
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O
-------
Section No. 5
Revision No. 1
Date 7/15/80
Page 28 of 62
B. "Coarse" rotameter calibration—
1. Remove the "fine" orifice-manometer unit and connect the mass /low
meter directly to the sampler.
2. Close the "fine" flow control valve finger tight (full clockwise);
the ball should drop to the bottom of the column.
3. Adjust the "coarse" flow control valve to yield a flow rate of
approximately 20 percent of the operating range (0-2 L/min).
4. Read and record on the data form (Figure 5.8) the following param-
eters:
room (ambient) temperature (T-|), K (if different from Step 3
of the previous subsection).
barometric pressure (P-,), mm Hg (if different from Step 3 of
the previous subsection;.
mass flowmeter reading (F ), volts.
sampler "coarse" rotameter indication (I), arbitrary.
5. Repeat Steps 3 and 4 for rotameter settings representing flow rates
of 40, 60, 75, and 90 percent of the operating range (0-2 L/min).
6. Using the calibration curve (Figure 5.6) or the interpolation table
(Figure 5.5) provided with t/he mass flowmeter, calculate (or look
up on the table) the flow rate Q t . for the voltage reading (F )
for each calibration point. Record on the data form (Figure 5.8)
the value of Q ., to three significant figures for the "coarse"
flow, for example, 1.67 stdL/min.
7 Convert the flow rates measured with the mass flowmeter to labora-
tory conditions using the following relationship:
i
where
Q = /C = 2-550
QI = volumetric flow through the mass /flowmeter at
laboratory conditions, L/min;
Q td = flow rate at standard conditions indicated by
the mass flowmeter, stdL/min;
T.| , P, = laboratory temperature and pressure, respec-
tively, K and mm Hg; and
-------
Section No. 5
Revision No. I
Date 7/15/80
Page 29 of 62
TctH P 4. , = standard temperature and pressure, respective-
sta, sud
Record the calculated Q, values on a data form such as that
shown i n Figure 5. 8.
8. Determine by measurement or calculation from the site elevation
the average seasonal site or field barometric pressure (Pf) and
record it on the data form of Figure 5.8.
Note: The calculation based on site elevation is:
Pf(mm Hg) = 760(mm Hg) - 0.075(mm Hg/m) x elevation (m),
or = 760(mm Hg) - 0.023(mm Hg/ft) x elevation (ft),
where elevations above sea level are defined to be positive and
those below sea level are negative.
9. Determine the average seasonal site or field temperature (Tf) and
record it on the data form in Figure 5.8.
10. Calculate the flow rates at average seasonal site or field condi-
tions of Pf and Tf for each calibration point using the relation-
ship, T T
Qf =Q]C(P1/T1)(Tf/Pf)]1/2
where
Qf = the flow rate at site or field conditions of Tf,
T Pf, L/min;
Q, = the flow rate at laboratory conditions of T^ , P^ ,
L/min;
T,, P, = laboratory temperature and pressure, respectively,
K, mm Hg; and
T Pf = average seasonal site or field temperature and pres-
sure, respectively, K, mm Hg.
Note: This conversion for the orifice is accurate to within about
2 percent for the temperature and pressure ranges of this
project. Its applicability to the sampler's flow measure-
ment system is not known.
Record the calculated Qf values on the data form in Fig-
ure 5.8.
-------
Section No. 5
Revision No. 0
Date 5/7/80
Page 30 of 52
II. "Coarse" rotameter calibration curve—Using the five data pairs of
Q, and I in the data form of Figure 5.8 under "coarse" flow rate
calibration, generate a linear regression equation of the form
Qf (sampler) = A I + B,
where
Qf = sampler's "coarse" flow rate at average seasonal fiela
or site conditions, L/min;
I = rotameter indication, arbitrary units;
A = slope of the linear regression equation, (L/min)/(rotam-
eter units); and
B = intercept of the regression equation, L/min.
Generate a calibration curve and interpolation table as illus-
trated in Figures 5.13 and 5.14, respectively.
Calculate and record on the calibration curve the setpoint
for the rotameter; that is, calculate the rotameter indication, I,
that will yield a Q^ (sampler) of 1.57 L/min.
Note: The interpolation table will be used by the field operator
to determine and report the sampling rate in m3/min at stan-
dard conditions based on an average rotameter indication
for the sampling period. The provision of precalculated
Qe+H va^ues relieves the operator of making any calculations
other than to average the initial and final rotameter read-
ings.
5.8.2.1.2.6 Sierra dichotomous sampler and orifice calibration proce-
dures—To calibrate the sampler and orifice:
1. Check the QAD-supplied calibration curve (Figure 5.5) and inter-
polation table (Figure 5.5) to verify that they are correct for
that mass flowmeter (i.e., check the serial number) and that the
calibration is still valid (i.e. , current within 3 months).
2. Set up the calibration system as illustrated in Figure 5.15. The
inlet of the mass flowmeter is connected to a vented manifold sup-
plied with a surplus of clean, dry air. The outlet of the mass
flowmeter is connected to the inlet of the field calibration check
orifice device having a similar operating range (0-20 L/min). A
special adapter is attached to the orifice-manometer unit that per-
mits the unit to be connected to the sampler's inlet tube in place
of the standpipe.
-------
INHALED PARTICIPATE NETWORK
BECKMAN DICHOTOKOUS SAMPLER EPA# 176108 S/M 056-909
COARSE ROTAMETER CALIBRATION BY M. WILKINS
CO
a
2.00 —
1.75
1.50-
1.25
UJ 1.00-
0.58
0.25 .
0 4-
0
Data Point* " 4
SI op* (A)- 3.9617
Intorompt (B)« 0. 1106
Coefficient (K) - 0L 9965
Y-AX+B
0.25
0.50
0.75
1.00
1.25
ROTAMETER READING
_i
SETPOINT- 1. 80
1.50
1.75"
2.00
~X? d5 PO C/~>
Cu fU fD (D
CQ r+ < n
(/I —I.
oj en -^. o
l—' ^ o Z3
CTl
C» z z
CD O O
Figure 5.13. Sample calibration curve for Beckman "coarse" rotameter.
-------
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-------
DRY AIR
SUPPLY
O O
o
COARSE
ROTAMETER
TOTAL
ROTAMETER
T
MASS FLOWMETER
ORIFICE (FIELD CALIBRATION
CHECK DEVICE)
IP SAMPLER
Figure 5.15. Schematic of Sierra laboratory calibration setup using a mass flowmeter as the transfer standard.
-o en ;o GO
Q} 0> CD (T>
CQ r+ < O
(D fD — '• r+
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cn
co ^: ^:
O O O
-------
Section No. 5
Revision No. 0
Date 5/7/80
Page 34 of 62
3. Place a pair of Nylon filter cassettes with 2-|jm Teflon filters
into the filter holders.
4. Adjust the dry air supply to provide a flow rate well in excess of
the sampler requirements to the open manifold. (A flow rate of
30 to 40 L/min at laboratory conditions should be sufficient.)
5. Turn on the sampler and mass flowmeter and allow them to warm up
to operating temperature (at least 5 minutes). The sampler's flow
control valves for both "coarse" and "fine" rotameters should be
opened wide (full counterclockwise).
6. Leak-check the system by removing the manometer from the orifice
and plugging both pressure taps and disconnecting and plugging the
mass flowmeter inlet line from the dry air manifold. The sampler's
rotameters should read zero. Check the sampler's vacuum gauge and
record its reading on the data sheet, as shown in Figure 5.8. If
the mass flowmeter indicates that a leak exists, it must be found
and eliminated prior to continuing the -calibration.
7. Reconnect the manometer to the orifice and. the mass flowmeter's
inlet line to the dry air manifold.
A. "Total" rotameter and orifice calibrations—
1. Close the "coarse" flow control valve finger tight (full clock-
wise); the rotameter ball should drop to the bottom of the tube.
2. Adjust the "total" flow control valve to give a 20 percent of range
reading on the "total" rotameter.
3. Read the following parameters and record on the data form:
Room (ambient) temperature (T,), K
Barometric pressure (P-j), mm Hg
Mass flowmeter reading (F ) V
Pressure drop across the orifice (AP), in. H20
Sampler "total" rotameter indication (1^), arbitrary units
4. Repeat Steps 2 and 3 for rotameter settings representing flow rates
of 40, 60, 75, and 90 percent of the operating range (0-20 L/min).
5. Using the calibration curve (Figure 5.6) equation or the interpola-
tion table (Figure 5.5) provided with the mass flowmeter, calculate
(or look up on the table) the flow rate Q , for the voltage read-
ing (F ) for each calibration point. Recife? on the data form (Fig-
ure 5.8) the value of Q . , to four significant digits for the
"total" flows, for example,T6.67 stdL/min.
-------
Section No. 5
Revision No. 1
Date 7/15/80
Paae 35 of 62
6. Convert the flow rates measured with the mass flowmeter to labora-
tory conditions using the following relationship:
= Wpstd/Tstd
where
= volumetric flow through the mass flowmeter at laboratory
conditions, L/min;
= flow rate at standard conditions indicated by the mass
flowmeter, stdL/min;
T.J , P-| = laboratory temperature and pressure, respectively, K and
mm Hg; and
T tH, P , . = standard temperature and pressure, respectively, K and
StQ sta mm Hg.
Record the calculated Q, values on the data form shown in Fig-
ure 5.8. - '
7. Determine by measurement or calculation from the site elevation
the average site or field barometric pressure (Pf) and record it
on the data form of Figure 5.8.
Note: The calculation based on site elevation is:
Pf(mm Hg) = 760(mm Hg) - 0.075(mm Hg/m) x elevation (m),
or = 760(mm Hg) - 0.023(mm Hg/ft) x elevation (ft),
where elevations above sea level are defined to be positive and
those below sea level are negative.
8. Determine the average seasonal site or field temperature (Tf) and
record it on the data form in Figure 5.8.
9. Calculate the flow rates at average seasonal site or field condi-
on F
a/2
tions of P. and Tf for each calibration point using the relation-
ship, f
Qf = Q1[(P1/T1)(Tf/Pf)]-
where
Qf = the flow rate at site or field conditions of Tf,
Pf, L/min;
-------
Section No. 5
Revision No. 0
Date 5/7/80
Page 36 of 62
Q, = the flow rate at laboratory conditions of T, , P-| ,
L/min;
- p = laboratory temperature and pressure, respectively,
1 ' K, mm Hg; and
T p^ = average seasonal site or field temperature and pres-
1 sure, respectively, K, mm Hg.
Note: This conversion for the orifice is accurate to within about
2 percent for the temperature and pressure ranges of this
project. Its applicability to the sampler's flow measure-
ment system is not known.
Record the calculated Q?- values' on the data form in Figure 5.8.
10. Field calibration check orifice unit calibration curve — Using the
five data points of Q. and AP for the orifice in Figure 5.8, gene-
rate a calibration equation of the form
Qf (orifice) = A(AP)B
where
Q, = flow rate through the orifice unit at average seasonal
field or site conditions of temperature and pressure,
L/min; and
AP = pressure drop across the orifice, in. H20.
Note: If the exponent B is outside the range of 0.45 to 0.55 the
calibration results should be rechecked.
Generate a calibration plot of Q. (L/min) as the ordinate or
y axis and AP (in. H20) as the abcissa or x axis. A sample orifice
calibration curve is shown in Figure 5.9.
Generate an interpolation table for the orifice-manometer unit
using the above calibration equation to calculate flow rates (Q*)
at average seasonal field conditions for increments of AP of 0.16
in. H20. A sample interpolation table is given in Figure 5.10.
This interpolation table will be used by the operator in the
field for the QC check on the sampler's "total" rotameter (see Sec-
tion 2.6.6.2).
-------
Section No. 5
Revision No. i
Date 7/15/80
Page 37 of 62
11. "Total" rotameter—using the five data pairs of Q^ and I in the
data form of Figure 5.8 under "total" flow rate calibration, gene-
rate a linear regression equation of the form
Qf (sampler) = A I + B,
where
Qf = sampler's "total" flow rate at average seasonal field or
site conditions of temperature and pressure; L/min;
I = rotameter indication, arbitrary units;
A = slope of the linear regression equation, (L/min)/(rotam-
eter units) ; and
B = intercept of the regression equation, L/min.
Generate a calibration curve and interpolation table as il-
lustrated in Figures 5.16 and 5.17, respectively.
The sampler flow rate at standard conditions in stdmVmin is
calculated from the actual flow rate in mVmin at average seasonal
field conditions by
= 0.392Qf (Pf/Tf)
Calculate and record on the calibration curve (Figure 5.16)
the setpoint for the rotameter; that is, calculate the rotameter
indication I that will yield a Q, (sampler) of 15.0 L/min.
NOTE: The interpolation table will be used by the field operator
to determine and report the sampling rate in m3/min at
standard conditions based on an average rotameter indica-
tion for the sampling period. The provision of precalcu-
lated Q . . values relieves the operator of making any cal-
T ^ * X ^^
cuiations other tnan to average the initial and final rota-
meter readings.
B. "Coarse" rotameter calibration—
1. Remove the "total" orifice-manometer unit and connect the mass
flowmeter directly to the sampler.
-------
INHALED PARTICIPATE NETWORK
SIERRA DIDIOTOMOUS SAMPLER EPA0175479 S/N 216
TOTAL ROTAMETER CALIBRATION
Q.
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ROTAMETER READING
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-------
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-------
Section No. 5
Revision No. 1
Date 7/15/80
Page 40 of 62
2. Disconnect the "fine" channel flow tubing (3/8 in.) from the bottom
of the filter holder. Attach the blue filter cassette to the tub-
ing inlet (flow in direction of arrow). Plug the opening at the
bottom of the filter holder.
3. Adjust the "coarse" flow control valve to yield a flow rate of ap-
proximately 20 percent of the operating range (0-2 L/min).
4. Read and record on the data form the following parameters:
room (ambient) temperature (T,), K (if different from Step 3
of the previous subsection).
barometric pressure (P,), mm Hg (if different from Step 3 of
the previous subsection;.
mass flowmeter reading (F ), volts.
sampler "coarse" rotameter indication (I), arbitrary.
5. Repeat Steps 3 and 4 for rotameter settings representing flow rates
of 40, 60, 75, and 90 percent of the operating range (0-2 L/min).
6. Using the calibration curve (Figure 5.6) or the interpolation table
(Figure 5.5) provided with the mass flowmeter, calculate (or look
up on the table) the flow rate Q ,. for the voltage reading (F )
for each calibration point. Recorcr on the data form (Figure 5.8)
the value of Q . . to three significant figures for the "coarse"
flow, for example, 1.67 stdL/min.
7. Convert the flow rates measured with the mass flowmeter to labora-
tory conditions using the following relationship:
V = 2-550
where
Q^ = volumetric flow through the mass flowmeter at
laboratory conditions, L/min;
= flow rate at standard conditions indicated by
the mass flowmeter, stdL/min;
.| , P.J = laboratory temperature and pressure, respec-
tively, K and mm Hg; and
~std %td = s^ndard temperature and pressure, respective-
' ly, K and mm Hg.
Record the calculated Q, values on a data form such as that
shown in Figure 5. 8.
-------
Section No. 5
Revision No. 1
Date 7/15/80
Page 41 of 62
8. Determine by measurement or calculation from the site elevation
the average site or field barometric pressure (P^) and record it
on the data form of Figure 5.8. '
Note: The calculation based on site elevation is:
Pf(mm Hg) = 760(mm Hg) - 0.075(mm Hg/m) x elevation (m),
or = 760(mm Hg) - 0.023(mm Hg/ft) x elevation (ft),
where elevations above sea level are defined to be positive and
those below sea level are negative.
9. Determine the average seasonal site or field temperature (Tf) and
record it on the data form in Figure 5.8.
10. Calculate the flow rates at average seasonal site or field condi-
tions of Pf and Jf for each calibration point using the relation-
ship, T T
Qf = Q1[(P1/T1)(Tf/Pf)]1/2
where
Q, = the flow rate at average seasonal site or field con-
ditions of Tf) Pf, L/min;
Q, = the flow rate at laboratory conditions of T, , P, ,
1 L/min; ' '
T,, P-, = laboratory temperature and pressure, respectively,
K and mm Hg; and
Tf, Pf = average seasonal site or field temperature and pres-
' sure, respectively, K and mm Hg.
Note: This conversion for the orifice is accurate to within about
2 percent for the temperature and pressure ranges of this
project. Its applicability to the sampler's flow measure-
ment system is not known.
Record the calculated Qf values on the data form in Fig-
ure 5.8.
11. "Coarse" rotameter calibration curve—Using the five data pairs of
Qf and I in the data form of Figure 5.8 under "coarse" flow rate
calibration, generate a linear regression equation of the form
Qf (sampler) = A I + B,
-------
Section No. 5
Revision No. 0
Date 5/7/80
Paoe 42 of 62
where
Q = sampler's "coarse" flow rate at average seasonal field
or site conditions, L/min;
I = rotameter indication, arbitrary units;
A= slope of the linear regression equation, (L/min)/(rotam-
eter units); and
B = intercept of the regression equation, L/min.
Generate a calibration curve and interpolation table as illus-
trated in Figures 5.18 and 5.19, respectively.
Calculate and record on the calibration curve the setpoint
for the rotameter; that is, calculate the rotameter indication I
that will yield a Q- (sampler) of 1.67 L/min.
Note: The interpolation table will be used by the field operator
to determine and report the sampling rate in nrVmin at stan-
aard conditions based on an average rotameter indication for
the sampling period. The provision of precalculated Q,«.,j
values relieves the operator of making any calculations ot'e'r
than to average the initial and final rotameter readings.
5.8.2.2 Field Calibration Check Procedures—
The laboratory calibration is checked after setup in the field and a
calibration check of sampler flow rate is performed by the operator after
every other sampling period. Sampler-specific field calibration check pro-
cedures are detailed in Section 2 of this manual. If the calibration check
indicates the sampler flow rate is not within ±10 percent of the original
calibration, a recalibration of the sampler flow rate is required.
5.8.3 Analytical Instrumentation Calibration
Calibration of analytical instrumentation for sulfate and nitrate deter-
mination is performed each analysis day as described in Sections 4.4 and 4.5,'
respectively. Standards for calibration of analytical methodology used in
the determination of sulfates and nitrates on high volume and dichotomous
filters are compared to standards from NBS. These standards are chemical
deposits on glass fiber and Teflon filters.
-------
INHALED PARTICIPATE NETWORK
SIERRA DICHOTOMOUS SAMPLER EPA0175479 S/N 216
COARSE ROTAMETER CALIBRATION
Data Point* - 5
SJcpmW" 0.1355
Intercept (W- 0. 5645
Co*ffioi*ttt (R) - 0. 9925
Y-AX+B
a, 2.50
m 2.0fi
16.00 18.00 20.00
ROTAMETER READING
Figure 5.18. Sample calibration curve for Sierra "coarse" rotameter.
~T3 CD PO CO
o> OJ ro
IQ c-i- < n
n> ro -i- c+
o ^
-h CD Z Z
CD O O
-------
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i * 11 +« t * K +1 14 .. i ; 4 i 4 i * < * t i i i i 11 t t »•> i t I : f
••;. I
I t I 4 1 .) i M 4 •
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f ;• ; i I.. i ; ; 4 I 1141.1 ; M + t .H t •; \ \- \ \. M M M * * * r 11 >
I'lui.iiii MI !•• it'iii : i.' ,.,-".•»> h../hliJ O..)I,DI i'Kiii,,ni in i.> , ni INC. .'
Figure 5.19. Sample interpolation table for Sierra "coarse" rotameter calibration.
tn
CD
i oo :z z:
ooo
o tn
-------
Section No. 5
Revision No. 0
Date 5/7/80
Page 45 of 62
5.9 CORRECTIVE ACTION
The identification of problems and the resulting corrective action is
evidence of the QA plan at work in the measurement system. Corrective action
encompasses immediate action to eliminate problems such as errors in calibra-
tion, reweighs, and other internal procedural problems. It also encompasses
long-range corrective action to improve overall data quality.
Assessment of internal QC checks (e.g., sampler field calibration checks
and filter reweighs) to determine the need for corrective action is the re-
sponsibility of the operator.
Assessment of external QA checks (e.g., audits) is the responsibility
of the QA coordinator for the IP Network; The QA coordinator contacts the
organization responsible for providing data and alerts the IP project offi-
cer to potential and existing problems-. Once a problem area is "identified,
the project officer determines the acceptability of data recorded during the
period under question.
Specific limits and assessments criteria for corrective action are in-
cluded in the description of each Network operation in this manual.
5.10 IP NETWORK AUDIT PROGRAM
Providing audits and independent checks to evaluate the quality of data
provided by the total measurement system is an important part of an overall
QA plan. An audit program has been established for the IP Network. This
program includes performance audits of sampling and analytical procedures,
and site audits at IP monitoring sites.
Performance audits are conducted in the field of the flow measurement
systems of all IP samplers. Procedures for conducting flow audits are out-
lined in Section 5.12. Flow rate audits are being conducted initially at a
frequency of once per quarter as the IP Network is being established.
External audits of the analytical operations, i.e., filter weighing and
the chemical analysis for sulfates and nitrates, are also being conducted.
An external filter reweigh and a check of balance accuracy have been
established for IP filter weighing operations. The accuracy of IP balances
is checked weekly using NBS-traceable calibrated weights. A discussion of
these procedures is found in Section 5.13.1.
-------
Section No. 5
Revision No. 0
Date 5/7/80
Page 46 of 62
A blind sample audit program has been established for the IP Network
analytical operation for determining sulfates, nitrates, and lead on IP fil-
ters. Each analysis day, blind audit samples for sulfate, nitrates, and lead
are analyzed along with IP samples. A detailed discussion of this program
can be found in Section 5.13.2.
A similar blind sample audit program has been instituted for the ele-
mental analysis of the IP dichotomous filters using X-ray fluorescence (XRF).
Using elemental standards and previously characterized field samples, blind
audit samples will be included with each sample tray labeled for XRF analy-
sis.
The results of this audit program are evaluated by the QA coordinator
for the IP Network.
5.11 DATA VALIDATION AND STATISTICAL ANALYSIS OF DATA
Data validation is the process of filtering data, 'then accepting or re-
jecting them based on a set of criteria. The body of data must be critically
reviewed to identify and isolate errors. Data validation occurs at each step
of the measurement process, beginning with sample validation in the field
followed by a preliminary physical screening process when the sample is re-
ceived from the field. Once data enter the storage and retrieval system, a
more detailed screening process is undertaken. This screening process, along
with additional information on data flow and validation and statistical anal-
ysis of data, is detailed in Section 6 of this manual.
5.12 DATA QUALITY ASSESSMENT: PRECISION AND ACCURACY
Determination of the precision and" accuracy of monitoring data provides
a quantitative assessment of data quality. Procedures for determining pre-
cision and accuracy are dependent on the monitoring technique. Measurement
methodologies used in the IP Network are those for the manual integrated type
of sampling. Measurements using manual methods follow a two-step process:
(1) collection of the sample on a suitable medium, for a specified time; and
(2) subsequent analysis. Quality assurance assessment is provided at each
step.
Precision of sampling methods is determined using collocated samplers;
accuracy is determined by an external audit of the flow rate of the sampler.
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Section No. 5
Revision No. 0
Date 5/7/80
Page 47 of 62
Precision of the analytical methods is determined from duplicate sample anal-
ysis; accuracy is determined by a blind sample audit program.
The purpose of the data quality assessment program is to quantitatively
document data quality. The day-to-day internal QA measures instituted in
each program area will provide for short-term corrective action o'f sampling
and analytical problems. The data quality assessment program will provide
an estimate of the reliability of this internal QA program.
5.12.1 Precision and Accuracy of Sampler Performance
5.12.1.1 Sampler Flow Rate Precision Check--
The field operator at each site will verify the flow rate calibration
of samplers at specified flow rates. Field calibration checks are scheduled
to occur every other sampling period. This procedure serves to: (1) a-llow
for immediate corrective action of flow problems; and (2) allow estimation
of flow rate precision.
Calibration of both conventional and SSI high volume flow-controlled
samplers is checked by placing a calibrated orifice (without a plate) on the
sampler, with a clean filter, and comparing the observed orifice flow rate
with that indicated on the Dicksorv- recorder (see Sections 2.3.6.2 and
2.4.6.2). For dichotomous samplers, a specially fabricated calibrated ori-
fice device is placed over the sampler inlet, and the indicated orifice flow
rate is compared with that indicated by the combined rotameter readings (see
Sections 2.5.6.2 and 2.6.6.2).
Precision estimates of sampler flow rate are calculated-as follows:
where
di = [(y. - x.)/x.] 100
d. = percent difference between indicated and calibration flow
rates for the i-th precision check,
y. = sampler's indicated flow rate from i-th precision check, and
c. = known (orifice) flow rate for i-th precision check.
2
/n
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Section No. 5
Revision No. 0
Date 5/7/80
Page 48 of 62
where
S. = standard deviation of flow rate for j-th sampler,
d- = difference between indicated (orifice) flow rate and recorded
1 flow rate for i-th precision check, and
n = number of precision checks.
5.12.1?2 Estimate of Sampler Precision, Collocated Samplers--
Precision estimates for manual samplers will be obtained by duplicate
sampling using collocated samplers. One out of every ten sites in the IP
Network will have duplicate samplers of each type used in the study; dichot-
omous, size-selective, and regular high volume. The collocated samplers will
operate whenever routine sampling is scheduled. The collocated sampler will
be set up in a manner consistent with the siting criteria used in the IP
study. Whenever possible, collocated samplers will be set up in sites where
the mass loading is expected to be moderate to heavy.
The IP sample data card has a space for indicating whether or not the
sample is collocated. Data from the collocated sampler will be compared to
the station sampler. The difference in concentration measured (in mg/m3)
between two samplers will be used to-calculate precision. For each of the
paired measurements, a percentage difference will be calculated using:
= ECy,- - x.)/x.] 100
where
d. = percent difference,
y.j = concentration measured by the duplicate sampler, and
x.j = concentration measured by the station sampler.
On a quarterly basis, a precision estimate (standard deviation) will be
calculated for each site containing collocated samplers.
where
n
I
d,2
i=l
Vn
S.
J
= quarterly standard deviation of j-th instrument,
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Section No. 5
Revision No. 0
Date 5/7/80
Page 49 of 62
d.j = percent difference for i-th precision check, and
n = number of precision checks on the instrument made during the
calendar quarter.
A value will be obtained for each type of sampler.
Precision data from each site will be used to calculate an overall pre-
cision estimate, S by sampler type for the IP Network.
a
K
S = (1/K) I S,2 "2
3 j=l J
where
Sfl = pooled standard deviation for all collocated samplers of a
given type (a).
S. = standard deviation of j-th sampler
J
K = number of collocated samplers of a given type (a) within the
IP Network
5.12.1.3 Estimate of Sampler Flow Rate Accuracy--
Estimates of the accuracy of the particulate sampling systems will be
determined from external flow rate audits. The flow rate through the sam-
pler is one of the most critical parameters, and one that is subject to
change. As discussed in the section on sampler operation, the site operator
will perform a flow check every other sampling period. As an external veri-
fication of the sampler calibration and this flow check, an audit of sampler
flow rate will be performed each quarter on all operative IP samplers.
The procedures used to perform the flow rate audits are described below.
5.12.1.3.1 Audit procedure for dichotomous samplers—Audit procedures
for dichotomous samplers are identical with those described for field cali-
bration checks (see Sections 2.5.6.2 and 2.6.6.2). Audit data will be
reported on standard forms (Figure 5.20).
5.12.1.3.2 Audit procedure for size-selective and high volume sam-
plers—Principle: A Reference Flow Device (ReF) is used to audit the flow
rate calibration of a total suspended particulate high volume sampler. The
ReF is a restrictive orifice device that readily yields checks of sampler
-------
DICHOTOMOUS AUDIT DATA SHEET
Section No. 5
Revision No. 0
Date 5/7/80
Page 50 of 62
Time start:
Station:
Address:
Sampler Model:
Calibration information:
Total flow
Standard (std) m -
b -
Dry gas ineter model:
Correction factor:
BuBble flow kit model:
Orifices:
Large S/N:
S/N:
Date:
Audi tor:_
Observer:
Coarse flow
Standard (std) m =
S/N:
S/N:
Small S/N:
ID =_
b =_
Mass flowmeter noael:
m =_
b =_
Barometric pressure:
S/N:
Temperature:
Flow
type
Instr.
flow rd.
EPA mass
flow rd.
Orifice
used
(audit)
Audit
man. rd.
(in. iH,0)
Audit
flow
(stdL/min)
Instr.
flow
( stdL/min)
EPA
flow
( stdL/min)
i
Difference Percent j
(L/min) j diff.
i
' : J
|
i
1
Figure 5.20. Audit data sheet for dichotomous samplers.
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Section No. 5
Revision No. 0
Date 5/7/80
Page 51 of 62
flow rate by measuring the pressure drop on a water manometer caused by the
orifice. This pressure drop is translated into a flow rate at either stand-
ard or actual conditions using the appropriate calibration equation. Trace-
ability is established by calibrating the ReF using an NBS-traceable Roots
meter system or some other primary volume measurement device.
Applicability: The device may be used to audit high volume samplers,
equipped with or without flow controllers, operating in the range of 0.5 to
2.4 stdmVmin.
Sensitivity: The ReF typically exhibits a sensitivity of 0.09 ms/min
per 1.0 in. change in pressure on the water manometer.
Precision and Accuracy: Extensive internal data are not available for
the precision of the method. The limited data available indicate that a pre-
cision of less than ±2 percent is readily attainable.
The accuracy of the ReF device when calibrated against a standard Roots
meter system is on the order of 2 percent absolute.
Equipment/Information:
ReF device
Resistance plates (5-, 7-, 10-, 13-, 18-hole)
Water manometer and connecting lines
Barometer
Thermometer
Glass fiber filter
Audit Procedure for High Volume and Size Selective Samplers—The exter-
nal audit group will routinely (quarterly initially) conduct a performance
audit of the high volume and size-selective samplers. A ReF device shall be
used and all flows will be corrected to standard conditions. The data will
be reported on standard forms (Figures 5.21 and 5.22).
5.12.1.4 ReF Recertification--
At least once a year, the ReF calibration is checked using the Roots
meter system. This procedure involves a comparison of the flow rates deter-
mined using the ReF device calibration equation and the flow rate as deter-
mined by the Roots meter. If the percent difference for each pair of values
for all five resistance plates is on the average of less than 3 percent, the
ReF calibration is considered satisfactory.
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Section No. 5
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Date 5/7/80
Page 52 of 62
HIGH VOLUME AUDIT DATA SHEET
Time start: Date:
Station: Auditor:
Address:__ Observer:
Sampler No.: Motor No.:_
Calibration information:
Slope (m) =
Intercept (b) =
ReF device S/N:
Standard (std) m = Actual (act) m =
b = b =
Barometric pressure (Pb):
Temperature (T ):
Weather conditions:
Audit
manometer
Plate reading
number (in. H-0) \
Audit Sampler Sampler Differ-
flow response flow ence Percent
m3/min) ( m3/min) (mVmin)
No
Plate
18
13
10
clf no mass flow controller installed, use resistance plates.
Figure 5.21. Audit data sheet for conventional high volume samplers.
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Section No. 5
Revision No. 0
Date 5/7/80
Page 53 of 62
SIZE SELECTIVE HIGH VOLUME AUDIT DATA SHEET
Time start: Date:_
Station: Auditor:
Address: Observer:_
Sampler No.: Motor No.:
Calibration information:
Slope (m) =
Intercept (b) =
ReF device S/N:
Standard (std) m = Actual (act) m =
b = b =
Barometric pressure (PK):
Temperature (T ):
Weather conditions:
b-
Audit
manometer
reading
(in. H20)
\
Ph
AH2Q*p
3
Audit flow
( m /min)
Sampler
response
( )
Sampler
flow
( m /min)
Difference
(m /min)
Percent
differ-
ence
Figure 5.22. Audit data sheet for SSI high volume samplers.
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Section No. 5
Revision No. 0
Date 5/7/80
Page 54 of 62
5.13 ASSESSMENT OF PRECISION AND ACCURACY OF PROCEDURES USED FOR ANALYSIS
OF IP NETWORK FILTERS
Following the collection of filter samples in the field, the filters
are returned to EPA/RTP (MD-8) for mass determination and chemical analysis.
The filters are weighed before and after sampling for mass determination.
Selected filters are sent for analysis of sulfate, nitrate, and lead using
automated wet-chemical techniques. X-ray fluorescence (XRF) is used on se-
lected dichotomous filters to analyze for a number of elements. Quality con-
trol functions are integrated into each step of filter analysis as detailed
in Section 4.
5.13.1 Mass Determination—Precision and Accuracy
In calculating the mass concentration of the sampled particulate,_ the
weighings of the filter before and after the sampling period can be sources
of significant error. An internal quality control program is conducted to
monitor the weighing operation.
As a check on the quality of operator-balance repeatability, five to
eight filters (8 hi-vol; 5-7 dichot) are reweighed each day at the RTP labo-
ratory (NSI) and compared with the original weights. All reweighings are
performed by the regular operating personnel using the appropriate analyti-
cal balances. Filters are selected at random for reweighing. Details of
the reweighing procedure are given in Section 4 of this manual.
Balance accuracy is checked weekly. A set of NBS-traceable calibrated
weights are weighed on the IP Network balances, and the calibration and indi-
cated weights are compared.
Accuracy and operator technique are also checked by an external auditor
once per week. A series of filters are reweighed by the audit team; balance
accuracy is checked against calibrated weights.
The shipping procedure is also evaluated with respect to possible data
quality problems resulting from damage of filters in shipment. Two filters
from each lot are selected as controls; they are weighed, packaged, and sent
to a sampling site according to normal procedures. They are then returned
unopened to EPA/RTP MD-8, inspected for damage, and processed through the
usual filter reweighing procedure. The shipping procedure will be further
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Section No. 5
Revision No. 0
Date 5/7/80
Page 55 of 62
investigated by placing balances at selected field sites and comparing the
field-recorded filter weights with those obtained at the laboratory.
5.13.2 Chemical and Elemental Analysis — Precision and Accuracy
5.13.2.1 Chemical Analysis of Sulfate, Nitrate, and Lead--
In order to assess the precision and accuracy of the chemical analysis
performed on the high volume and dichotomous filters, two separate quality
assurance programs are conducted. The internal QC program, provided by the
analytical laboratories, is described in Section 4 of this manual. An exter-
nal QA program conducted by the Performance Evaluation Branch (PEB), Quality
Assurance Division (QAD), EPA/EMSL, is described below.
The external QA program for the analysis laboratories consists of two
parts: blind sample audits and split sample analyses. The blind sample au-
dit program is designed to provide information on the precision and accuracy
of the analytical methodology of the analysis laboratory; the split sample
program provides information on the comparability of the IP Network filter
analysis laboratory and the referee laboratory.
5.13.2.1.1 B1 ind sample audit program—In the blind sample audit pro-
gram, the PEB supplies the analysis "laboratory with bl'ind quality control
samples that simulate actual field samples containing sulfate, nitrate, and
lead. The samples used for blind audits were developed by PEB as part of
its overall QA effort. Each lot of samples is.analyzed by PEB/QAD and a cor-
roborative laboratory before it is accepted for use in the blind sample audit
program. The QAD analysis, the corroborative analysis, and the target spike
value must agree to within 5 percent; the relative standard deviation for
any given concentration must be less than 2.5 percent or the samples are re-
jected. Blind audit sample concentrations and distributions for each type
of IP Network sample are given in Tables 5.2, 5.3, and 5.4.
Blind audit samples are analyzed by the IP analysis laboratory on each
IP sample analysis day. The laboratory distributes the audit samples as
evenly as possible among the analysis days during the audit period and inter-
sperses the audit samples throughout its routine analysis of IP samples.
5.13.2.1.2 Split sample analysis program—In the split sample analysis
program, a PEB in-house contractor performs duplicate (split) sample analy-
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TABLE 5.2. ANALYTICAL RANGE OF BLIND AUDIT SAMPLES3
(High volume and size selective high volume samples)
High level
Mid level
Low level
Blanks
so;
(ug/m3)
>20
5 to 20
0 to 5
0
NOs
(ug/m3)
>9
3 to 9
0 to 3
0
pb
(ug/m3)
>3
--
0 to 3
0
Levels are subject to revision depending on concentrations actually found
in IP Network samples.
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TABLE 5.3. ANALYTICAL RANGE OF BLIND AUDIT SAMPLES3
(Dichotomous samples)
High level
Mid level
Low level
Blanks
S04
(pg/f liter)
150 to 300
50 to 150
0 to 50
0
NOs
(pg/f liter)
150 to 300
50 to 150
0 to 50
0
Pb
(pg/f liter)
75 to 150
25 to 75
0 to 25
0
aLevels are subject to revision depending .on concentrations actually found
in IP Network samples.
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TABLE 5.4. DISTRIBUTION OF BLIND AUDIT SAMPLES ACROSS ANALYTICAL RANGE
(High volume, size selective high volume, and dichotomous samples)
S04 and NOs ?b
(samples/set) (samples/set)
High level 2 2
Mid level 2 2
Low level 2 2
Blanks 1 1
Total 7 7
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ses on approximately 5 percent of the high volume and dichotomous filter sam-
ples previously analyzed by the IP analysis laboratory.
Samples to be used for split analysis are randomly selected from the
collected samples. Duplicate 3/4-in. x 8-in. strips from the high-volume
filters and extracts from the dichotomous filters are sent to the referee
laboratory, once a week, for analysis. Results from both the referee and
the IP analytical laboratories are compared by the IP QA coordinator. Limits
of acceptable differences will be established at the beginning of the chemi-
cal analysis program for each type of sample. Periodically thereafter sam-
ples will be split between the analytical and referee laboratory to deter-
mine comparability of laboratory performances in routine analysis.
5.13.2.2 Elemental Analysis by X-Ray Fluorescence--
A portion of the dichotomous filters collected in the IP Network will
be analyzed by X-ray fluorescence (XRF) to characterize the elemental compo-
sition of the samples. A program has been designed and implemented to assess
the precision and accuracy of the XRF method.
5.13.2.2.1 Blind sample audit program—Blind audit samples are included
in each tray of sample filters to be-analyzed. These audit samples consist
of blank filters on which known concentrations of elements have been depos-
ited and actual field samples previously characterized for elemental composi-
tion.
5.13.2.2.2 Split sample analysis program—In addition, 5 percent of
the IP Network field samples analyzed by the analysis laboratory are reanal-
yzed by a referee laboratory to provide split sample analysis.
5.13.2.3 Reporting and Evaluating Audit Data—
The results from all blind audit samples analyzed are reported to PEB
on a monthly basis. The mean and range are determined for each pollutant
level and plotted on their respective control charts. Since a primary pur-
pose of the blind audit program is to chronologically document the precision
and accuracy achieved by the IP Network analytical laboratory, the control
chart provides a convenient display of precision and accuracy versus time.
Control charts also provide direct quantitative criteria to assess un-
acceptable bias or variability of the methods used by the analytical labo-
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ratory. Whenever the blind audit results do indicate greater than normal
bias or variability during an analytical period, both the QA officer and the
analytical laboratory are immediately notified. However, because of the time
involved in transmitting the results to PEB, the common use of control charts
to detect and immediately correct any analytical irregularities' cannot be
made. Short-term corrective action of analytical problems is, therefore,
based on internal QC data.
Summary reports for both blind and split sample analyses are periodi-
cally made to the IP Project Officer. Split sample and blind audit results
are reported to the IP QA officer at the end of each month.
5.14 EVALUATION AND VALIDATION OF IP METHODOLOGY
Methodology for both IP sampling and analyses systems is, for the-most
part, state-of-the-art. Sampling techniques for collecting reliably sized
particulates, specifically in the inhalable range, from ambient air in a
large network are relatively new. The samples thus obtained are on differ-
ent filter materials and in a form different than that worked with in the
usual high volume sampling methodology. Thus, modification of existing ana-
lytical techniques and development of- new, appropriate' techniques for the
dichotomous sample filters are required.
5.14.1 Validation of Dichotomous Samplers
The theory and operation of impactors for collecting size-segregated
particulates have been studied for the past 30 years, and are, at present,
feasible for network operations. Accurate calibration techniques for char-
acterizing their sampling efficiency as a function of particle size are not
yet available for field use, and require extensive laboratory support for
adequate calibration (see Section 5.8.2.1.1).
In order to calibrate the dichotomous sampler system independently, with
respect to particle sampling efficiency, EPA has awarded a grant for wind
tunnel characterization of selected size-selective, high volume, and dichot-
omous samplers. Because it has not yet been determined that sampler calibra-
tion remains fixed over a period of a year or more, these samplers will be
calibrated initially, sent to the field for use in the IP Network, and then
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recalibrated after one year's use. In this way any deviations in the sam-
pling diameter cutpoints will be characterized and documented.
5.14.2 Flow Measurement and Field Audit Device
Flow measurement and related flow measurement audit techniques for the
high volume sampler are well standardized. This is not true for the dichot-
omous (virtual impactor) sampler; thus, standardized multipoint field audit-
ing and/or calibration equipment is not presently available. Instruments
are being evaluated by EPA for performance precision and accuracy. It is
anticipated that at least one such device will be determined suitable for
calibrations and audits during the early phases of IP Network operation.
5.14.3 Evaluation of Dichotomous Samplers
Several dichotomous samplers will be evaluated, including those manu-
factured by Beckman Instruments and Sierra Instruments. The samplers will
be tested with laboratory-generated aerosols as follows:
a. Measurement of critical dimensions, such as orifice diameters that
affect sampling efficiency and particle sizing, w-ill be made.
These dimensions must agree with the manufacturer's specifications
so that the tests are representative.
b. Tests for the presence of air leaks and calibration of air flow
rates will be performed.
c. Measurements to- determine sampling efficiency vs. particle diame-
ter will be made. Particle sizes will be determined for the coarse
particle filter, the fine particle filter, and the sampler walls.
Liquid and solid particles will be used to test the sampler's re-
sponse to both sticky and bouncy particles such as those encoun-
tered in ambient air. Liquid particles of glycerol and solid par-
ticles of potassium biphthalate will be used with a uranine tra-
cer.
d. The uniformity of the filter deposits will be measured for both
fine and coarse fractions and for several particle sizes spanning
the outpoint. Methylene blue particles will be used to produce a
visible deposit that will be scanned with a microdensitometer.
5.14.4 Wind Tunnel Test of the Inlet
The sampling efficiency of the dichotomous sampler inlet is being tested
in a wind tunnel equipped with an aerosol generator. Liquid particles of
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oleic acid and solid particles of potassium biphthalate with a uranine tracer
are being used. The aerosol concentration in the wind tunnel is measured
before and after each test of the inlet by isokinetic sampling into a mani-
fold equipped with six filters. The inlet is coupled to a filter and the
flow rate set to the standard flow rate of the dichotomous sampler'(1 mVhr).
The sampling efficiency is then determined from the filter deposits.
The sampling efficiency is measured for particle sizes from 5 to 20 urn
and windspeeds from 1.5 to 12 m/s (5 to 43 km/hr). Measurements will also
be made at two different turbulence levels, e.g. , 1 and 8 percent.
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CONTENTS
Section
DATA VALIDATION
6.1 INTRODUCTION ......
6.1.1 Definition. . . .
6.1.2 Purpose
6.1.3 Scope
6.2 IP NETWORK FIELD AND
LABORATORY VALIDA-
TION PROCEDURES. . . .
6.2.1 Filter Processing
6.2.2 Analysis
6.3 IP NETWORK DATA
PROCESSING AND
VALIDATION PROCEDURES.
6.3.1 Data Validation
Criteria. . . .
6.3.2 Data Processing
and Reporting .
6.4 REFERENCES
Page
1
1
1
1
2
2
2
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7
7
8
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SECTION 6
DATA VALIDATION
6.1 INTRODUCTION
6.1.1 Definition
As defined in EPA's Quality Assurance Handbook for Air Pollution Meas-
urement Systems,1 "Data validation is the process whereby data are filtered
and accepted or rejected based on a set of criteria." Implicit in this
statement is the critical review of a body of data with the intent of iden-
tifying erroneous data points. This frequently involves analyzing similar,
previously collected data for statistically and physically significant
trends and relationships. For example, in the Inhalable Particulate (IP)
Network, one would expect that the mass concentrations measured using an SSI
high volume sampler and a collocated dichotomous sampler should be closely
related. If incoming data violate a well-established historical relation-
ship, then those data are scrutinized to identify the reason for the aber-
ration.
6.1.2 Purpose
Data validation is essential to ensure the reliability of the large
quantities of data that will be processed as a result of the IP Network.
The use of data generated by the IP Network is not completely foreseeable at
this time. However, once entered into the data base, the data will gener-
ally be accepted as accurate, frequently without further evaluation. For
this reason, the IP data validation process is devised to test all data as
thoroughly as possible, and to identify possible errors for further critical
evaluation. This aspect of the overall quality assurance program may be
summed up as an effort to identify and flag the questionable or "bad" data,
but not delete them from the data base.
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6.1.3 Scope
The IP data flow, shown schematically in Figure 6.1, is of three basic
types: (1) the physicochemical data collection and generation process
(e.g., filter weights, chemical analysis), (2) computerized data processing
and validation, and (3) professional review and evaluation of data and
results. As indicated, the data are obtained at a variety of locations, and
inputs to the IP Bank are from a variety of sources. It is essential that
the data be accurately processed, summarized, and made available to the IP
project officer in a timely fashion.
IP data validation involves five distinct phases: field or laboratory
validation, (computer-assisted) preliminary screening of raw data, critical
evaluation of questionable raw data, disposition of these data, and checks
to verify that the computer data file is an accurate representation of the
raw data. Once a data point is flagged as possibly in error, the individual
notebooks, data sheets and cards, logbooks, etc., must be examined to deter-
mine whether the datum has been accurately entered into the data base. If a
clearly identifiable mistake is discovered (e.g., keypunch error), the datum
is corrected and resubmitted to the data stream for reprocessing. However,
if no mistakes can be identified, a professional decision is made on the
validity of the datum and its inclusion in the analysis.
6.2 IP NETWORK FIELD AND LABORATORY VALIDATION PROCEDURES
6.2.1 Filter Processing
6.2.1.1 Sample Validation—
As noted in Section 2.2.3, all IP Network samples are validated by the
field operator at the time of removal from the sampler. The field valida-
tion criteria are:
Sampling must start and stop at midnight ±1/2 hour.
Sampling time must be between 23 and 25 hours.
Sampler flow rate decreases must be less than 10 percent from
initial set point.
Flow rate calibration must change less than 10 percent from the
previous calibration.
-------
OUTSIDE CONTRACT
LABORATORY
LABORATOHV
ANALYSIS
CUTTING ROOM*
FILTER BANK
WEIGHING
ROOM
NIIALnttLE PARTICUl ATE VALIDATION R. REPORTING MONIT ORING TECHNIQUES FIELU OPERATION
III') BANK DATA BASE SYSTEM SECTION (MIS)
(V& HI
OPERATIONS PROCESS CHART
FOR THE IP NETWORK
o
Operation
= Inspection
= Operation and inipection
/ I = Transportation
\ / - Storage
~O CD XJ Cn
O) PL) ftl rt)
(Q c+ < n
(D (D —.. f-(-
1/1 —i.
(jO C_n —i. O
\ O Z3
O -^1 Z>
^L 'Z.
I—' CD O O
CD
Figure 6.1. Operations process chart for the IP network.
-------
Key to Figure 6.1
Out tide Contract Laboratory
6 I Receive dicbolnmous (dims
02 Analy/u dicboloinous lillcis by X lay
llunrcscunce (XRF)
03 Send lusufis and lifleis back in EPA lali
Laboratory Analyst)
L I Receive SSI and hfyli volume littui mips
12 Analyse lot inorganics (SO.]j, NO~ |
13 Send results to IP Bank
L4 Analyse lor metals jPb)
15 Send results to IP Dank
I.G Receive dicbolomom lit to is
L7 Send out dichotomous fillets loi elemental
analysis by X ray ffuoresceitce (Xftf)
IB Receive XRF results and ilicbutomous lilteft
L9 Send results 10 IP Dank
LIO Analyze for inorganics (SO^j, NO^ t
Lit Analyse for metals (Pl>)
III
Cutting Room and Filter Bank
C| Receive fillers Irum IP Dank
C2 Cut SSI ami lii(>h volume fillers to l>e analysed
C3 Store remainder of cut SSI and hiyli volume
fillers anil all SSI. fiiijri volume, and dicboto-
mous tillers not designated foi analysis
C4 Send cut litters to EPA lab lor analysis
C6 Send dicbolomous fillois to EPA lali
Weiyliing Room
W) Receive blank filters from
W2 Weigh and cude fillets for laie wcifjtits
W3 Transport tillers lu MTS.
W4 ScnJ coded tare weiybis to IP Hank
W5 Receive exposed fillers from IP flank
W6 Wciyli ami code for final wvigbls
W/ Semi fillers tu culling loum
WH Send ctxlod linal weifjlil and comincnls to
fP Banfc
P»rlfcul«t« (IP| Dank
II PIOCCSJ taie wuiyltis
12 Receive fillers from field (and Questionable
filter liomMTSt
13 fnsfwct fvi&uallyl ^ifstinnable fil|eis;|Hil hi
box foi MfS(M)
14 Ilold tpiestionable fillers
Ifi Loy iit;<.tK!ck for duplicates; <|ut)s(fonabtu
filters IdMTSbox {I'll
16 Syileiri entry lu computeri/ed checks; (|Ues-
\ton*\,lc (Himi to M rS bow (14)
11 Transport <|Ufstjotial)le litters to MTS
18 Code comments, cieate (alwls, label fillers
19 Send labeled liltcis to wetyJiingf oont
IIU Send comments to V and R
Iff Receive cmnments and final weiybts fi om
weiybing loom; inspect and process linal weigbls
112 Transpuii comments and SAROAD foimalcd
final wclyltls to V and R
113 Receive anil process innry.inic (SOT/NO^)
data
IM Set id JnnKjaiiic data tu v* ami ft
115 Receive and process eleinenial (Pb) data
116 Send elemental dala lo V and R
117 llt'ceive dicbolouiDui XRI: lesulls and process
IIB Send diclmlomous res«itts to V and R
VI Receive comments or data
V2 Updale comments or process Operating
Agency Listing, labels, and Investigation Rc|M>rl
V3 Send Operating Agency Listings, labels.
Investigation deport lo MTS
V4 Receive institictions and cofnmcnts Irom
Investigation Rupuil; eliminate voided data;
update comments; pcrlonn computer ins|)ec-
lioii for collect coding
V6 UjHlate raw data files
VG Produce Validation Reports
V7 Send Validation Kopoils lo M TS
V8 Receive Validation Kuporl collection and
process accoiding to instructions received
Figure 6.1. (continued)
Validation and llepoiling Data Bait Syilem IV and Rl
(conllnued)
V9 Uiul.ilo I'lilihc Atcc-sl Files wild mwly
valiitaled
•f* in -•• o
O ^J ^3
-h "X.
CD Z z
I-1 O O O
M • •
o cn
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Participate deposits on the filter must indicate an adequate seal
around the filter.
The filter must be physically intact (not frayed, torn, etc.).
In addition, the operator is instructed to note, on the filter data card
and in the logbook, events such as sampler flooding and nearby construction
that may adversely affect data quality. Alert, informed operators have a
key role in ensuring the validity of all recorded sample data.
6.2.1.2 Filter Weighing-
Methods for assessment of the precision and accuracy of filter weighing
procedures are detailed in Sections 4.1, 4.2, and 5.5.1. These sections are
briefly summarized here as they relate to- data processing, data collection,
and validation procedures (see Figure 6.1).
On receipt of a batch of filters from the supplier, each filter is
weighed and assigned a unique IP identification number. The weight is logged
into the IP Bank, and the number recorded on the filter envelope (or petri
dish). The filters are then delivered to the EPA project officer for storage
and shipment to field sampling sites as required.
Following sampling, the filters (with completed data cards) are sent to
EPA/RTP MD-8. The samples are inspected for completeness of field data
(i.e., coding and IP number) and obvious filter faults. Field data are
logged into the IP Bank and each sample is assigned a unique four-digit
laboratory identification number. Each filter is appropriately labeled; cer-
tain filters are selected and marked "To Be Analyzed."
All filters are sent to the laboratory for final weighing. As part of
the overall Quality Assurance Program (Section 5), 5 percent of the exposed
filters are randomly selected for reweighing. In addition, at least two fil-
ters per lot are processed as indicated above, except that they are not
exposed in the field. This is done to monitor the effects of handling and
environment that sample filters encounter during shipment and in the field.
Final weights are coded. Designated high volume filters are sectioned
for further analysis. All filters not to be analyzed, along with unused
portions of those high volume filters to be analyzed, are filed alphabeti-
cally by state, city, and date in a self-contained area.
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All coded final weights and filter samples to be analyzed are returned
to the EPA project officer. Coded data are forwarded to the Data Management
and Analysis Division (DMAD), where they are entered into the IP Bank.
Filter samples are sent to the appropriate laboratories for designated
analyses.
6.2.2 Analysis
Procedures for assessment of the precision and accuracy of the analyt-
ical methods for the determination of sulfate (SCO and nitrate (N03) are
detailed in Sections 4.4, 4.5, and 5.5.2.
In brief, two forms of quality assurance are conducted. The internal
QA program provided by the analytical laboratories is described in Section 4
of this manual. An external QA program (Section 5.5.2) is provided by the
Performance Evaluation Branch (PEB), Quality Assurance Division (QAD), EMSL,
EPA, and consists of two parts: split sample analysis and blind sample
audits.
The PEB supplies the analysis laboratory with blind quality control
samples, which simulate actual field samples containing sulfate, nitrate,
and lead. A PEB in-house contractor performs duplicate (split) sample anal-
yses on approximately 5 percent of the high volume and dichotomous filter
samples previously analyzed by the analysis laboratory. The blind sample
program provides information on the precision and accuracy of the analytical
methodology of the analysis laboratory. The split sample program provides
information on the comparability of the Network filter analysis laboratories
and the referee laboratory.
Analytical results, which have been validated by the above procedures,
are forwarded to the EPA project officer who is responsible for entering the
data into the IP Bank.
6.3 IP NETWORK DATA PROCESSING AND VALIDATION PROCEDURES
Raw data entered into the IP Bank are processed (to give final mass con-
centrations and analytical results in ug/m3) and passed on to the data vali-
dation and reporting system (see Figure 6.1).
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6.3.1 IP Data Validation Criteri;
Errors can occur in the computerized data set in at least two ways.
The raw data may be incorrect, or there may be an error in the transcription/
transfer of the raw data to their computer representation. QC field meas-
urements of instrument precision, and split sample and blind sample audits,
are aimed at preventing errors in the raw data and have been discussed above.
Transcription/keypunch -error rates can be estimated by sampling from
the computer output data set and comparing the sample with the corresponding
raw data. At present the IP computerized data set is 100 percent hand-vali-
dated and hand-corrected. Eventually it is anticipated that checks on rela-
tively small random samples from the output data set will suffice to ensure
that the data transcription process is sufficiently error-free.
Application of outlier detection techniques to the computerized data
set can reveal both types of errors. Simple checks for physically meaning-
less negative values or for values less than minimum detection limits (based
on evaluation of the total measurement process) can identify suspect data.
Similarly, local daily and seasonal variations in particulate mass concen-
trations may be used to establish "windows" within which data may reasonably
be assumed to be valid.
The same techniques can be applied to subsets of the data defined by
measurements of interrelated variables from the same region in time and
space. For example, each IP Network site will have a minimum of two samplers
operating during a given sampling period: a conventional high volume sampler
for total suspended particulates, and one of several available samplers for
inhalable particulates. Total suspended particulate (TSP) data and inhalable
particulate (IP) data (further subdivided into fine (F) and coarse (C) frac-
tions by the dichotomous sampler) will be available from each valid sampling
period at each site. The data are not strictly comparable due to the exclu-
sion of particles with aerodynamic diameters greater than 15 urn by the IP
samplers; however, the ratios IP/TSP, (F+O/TSP, etc., should show correla-
tion in most instances, and are used to establish IP data validation cri-
teria. Similarly, one could anticipate that the total mass concentration
sampled by a size selective high volume sampler (SSI) should be functionally
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related to the fine fraction (F) and coarse fraction (C) as sampled by a
collocated dichotomous sampler, and thus the ratio of (F+C) to (SSI) is also
used as a data validation check.
In addition to the particulate mass relationships used in the data vali-
dation process, compositional interrelationships may also be useful. For
instance, evidence suggests that predictable relationships exist between
ambient concentrations of sulfate and nitrate, and mass. Specifically, it
has been observed that sulfate mass will normally be less than 60 percent of
the total sample mass. Thus, a "ceiling" value for sulfate concentrations
may be set as one data validation criterion.
Initial IP validation criteria require that the total analyte mass not
exceed total sample weight. Tables 6.1 and 6.2 list other specific criteria
against which IP Network data are presently validated.
6.3.2 IP Data Processing and Reporting
For each data set, data are screened for false negative or extreme
values beyond reasonably expected limits as described above. The resultant
Operating Agency History, which lists all data in a particular batch or data
set and flags suspicious data points, is sent to all appropriate operating
agencies for their review.
Data are further screened by testing each value against all others in
the data set, using statistical tests such as Grubbs test, t-test, skewness,
and sequential differences. Data determined to be of questionable validity
via this process are tabulated in a Screen Report.
Flagged data from the Operating Agency Listing and the Screen Report
are combined into an Investigation List, which is sent to the IP project of-
ficer for review and evaluation by the Environmental Monitoring Division
(HMD) staff.
Necessary corrections to the data are made by the operating agencies
and the EMD staff. When no obvious sources of error can be found, a profes-
sional decision must be made, and documented, on how to treat the data. The
data are resubmitted to the data system and updated in the data file via
routine processing. Resulting Validation Listings are sent to the investi-
gators (EMD staff) for additional review and validation. The investigators
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TABLE 6.1. IP DATA CARD VALIDATION CRITERIA
I.
II.
Sampling rate criteria
1. TSP high volume
2. SSI high volume
3. "Coarse" dichotomous (C)
4. "Fine" dichotomous (F)
Sampling time criteria
Target (mVmin)
1.42
1.13
0.0017
0.0150
Target (min)
Allowable range*
(mVmin)
low high
1.13 1.70
1.02 1.24
0.0015 0.0019
0.0135 0.0165
Allowable range*
(min)
low high'
1. All samples 1,440
III. Quality control check criteria Target (%)
1. All samples 100.0
1,380 1,500
Allowable range*
low high
90.0 110.0
All data outside this range are flagged.
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TABLE 6.2. IP NETWORK VALIDATION CRITERIA FOR MASS DATA
1.
If
~TSP
SSI
Coarse (C)
Fine (F)
Total (F+C)
value is <
~20"
15
5
10
15
ug/m3, or >
~120"
100
60
40
100
ug/m3, flag
value.
2. If SSI/TSP ratio is >1.09 or <0.40, flag both values.
3. If (F+O/TSP ratio is >1.09 or <.40, flag both values.
4. If (F+C)/SSI ratio is >1.20 or <0.8€, flag both values.
5. If C/F ratio is >1.30 or <0.30, flag both values.
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Section No. 6
Revision No. 0
Date 5/7/80
Page 11 of 11
may enter further corrections. This is an iterative process that is com-
pleted only when no further corrections are entered into the data file.
At this time the data are considered to be validated and the validated
data set is forwarded to the Public Access Files.
6.4 REFERENCES
1. Quality Assurance Handbook for Air Pollution Measurement Systems.
Volume 1, Principles, EPA-600/9-76-005, March 1976. Section No.
1.4.17, Page 2 of 13.
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APPENDIX A
Protocol for Establishment of a Nationwide
IP Network
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PROTOCOL FOR ESTABLISHMENT OF A NATIONWIDE
INHALABLE PARTICULATE NETWORK
Charles E. Rodes
Environmental Monitoring and Support Laboratory
U.S. Environmental Protection Agency
Research Triangle Park, North Carolina 27711
May 15, 1979
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TABLE OF CONTENTS
Background 1
Purpose ..... 4
Scope 5
Network Design
General 10
Pilot Study Design 12
Urban Area Intensive Studies 17
Full Scale Network 19
P^eferences 22
Tables 1-11
Figure 1
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PROTOCOL FOR ESTABLISHMENT OF A NATIONWIDE
INHALABLE PARTICIPATE (IP) NETWORK
I. Background
Researchers involved in health effects studies relating to suspended
particulates have become more concerned with the smaller particles
capable of entering the respiratory system. The particles in this size
range have historically been called "Respirable Suspended Particulates"
(RSP)*. The EPA's Health Effects Research Laboratory (HERL) has recently
defined the size range of particles that can be inhaled as 0-15 ym
(microns). -1 The criteria document written in 1969 on which the present
"Total Suspended Particulate" (TSP) ambient standard is based, recognized
that the particle sizes of concern to health effects were primarily
those below 10-15 ym (aerodynamic diameter) which can be inhaled into
F21
the respiratory system.1 J Particles larger than this can be taken into
the body by ingestion, but except in cases of toxic materials have
little effect on health. •* The current feeling of the health community
is that the effect of inhaling small particles on health is primarily
F41
chronic, requiring long term assessment of exposure levels.1 J
The health related studies conducted by EPA in the past decade have
relied primarily on three ambient particulate sampler types: the hi-
vol, the ht-vol cascade impactor, and the low-volume (lo-vol) cascade
impactor. The general specifications of the hi-vols used in these
studies are given in the Federal Register. *• ^ The criteria document
noted that the hi-vol was capable of collecting particles as large as
100 um, but that the majority of particles in the ambient air were less
than 10 ym.'-6-' Recent work by McFarland indicates that the hi-vol is
very inefficient, less than 20% for particles greater than 30 ym.L -1 At
the time the criteria document was prepared (1969) the only substantial
aerosol data bases had been generated with the hi-vol or British Smoke
Shade samoler. The hi-vol cascade impactor has been used by the EPA-
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CHAMP program since 1972 to obtain size distribution information.L
* The current preferred designation is Inhaled Particulate (IP)
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These distribution data are important in determining the deposition -
location in the respiratory system. This sampler is multistage (2-4
stages), operates at flowrates of 1.0 to 1.4 m /min, and has an inlet
which excludes particles greater than approximately 26 um. The lo-vol
cascade is also a multistage (typically 5) sampler, but operates at
approximately one- tenth the flowrate of the hi-vol cascade and has an
inlet designed to be roughly equivalent to the standard hi-vol. This
F9l
lower flowrate version has also been used extensively by EPA.L J The
British Smoke Shade sampler, which is reported to collect particles less
than 5-10 um, has not been used in EPA soonsored health studies in this
country, but was compared in Europe with the hi-vol and lo-vol cascade
The Clean Air Act Amendments require EPA to reassess by December 31,
1980 its position on the existing particulate standard especially as
related to health. ' ^ This assessment requirement is .reinforced by
a pending legal action against EPA asking that the criteria for establishment
of the TSP standard must be reevaluated by January 1979 and a new standard
proposed. A draft document entitled Health Effects of Particulate
Pollution— Reappraising the Evidence was prepared by a committee of
British epidemiologists and health specialists as supporting evidence
for the plaintiff.'- ^ This report is very critical of the TSP standard
because of the inclusion of large particles in the measurements made by
the hi-vol .
An associated reason for concern by EPA over the TSP standard
involves the recent publication by EPA's Office of Air Duality Planning
and Standards (OAQPS) of more than 400 areas in the United States currently
not meeting the TSP standard.'-15-' The states which contain these non-
attainment areas are required to prepare implementation plans by January 1979
describing how the non-attainment can be corrected. One of the current
recommendations of OAQPS is for examination of "fugitive" dust sources
because of their contribution of larger (greater than 15 um) particles
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to the TSP measurement.L -" The state and local control agencies are
requesting practical guidance since controlling many fugitive dust
sources such as agricultural fields and unpaved roads is very difficult.
An alternative measure would be to revise or replace the existing TSP
primary standard to consider only that particulate size fraction (less
than 15 urn) that is respired. This would concurrently eliminate from
the measurement a majority of the larger particles associated with
"fugitive" dust.'- -" If the current TSP standard were replaced with an
IP primary standard, TSP would probably revert to a secondary standard.
In examining the primary sources of small (inhaled) particulate,
the criteria document listed photochemical activity as a principle
source of particles less than 2-4 ym. The compendium entitled Airborne
Particles prepared for the National Academy of Sciences describes an
atmospheric "accumulation mode" where particles less than 0.1 ym coalesce
(accumulate) while suspended to form laraer particles with a size range
fl8l
of approximately 0.1 to 3 um. J The Environmental Sciences Research
Laboratory (ESRL) of EPA has sponsored extensive research and development
in examining measurement techniques for ambient particulate and transport
patterns. Development efforts in the past 4 years have centered on the
"dichotomous" sampler which collects two sized fractions of aerosols
ri9i
using an inertia! non-impaction separation technique. J The smaller
of the two sized fractions collects particles up to 2.5 um to identify
the "accumulation mode" contribution. The larger particle fraction
collects the balance of particles up to approximately 15 ym. This
separation is useful for identifying source contributions since individual
constituents tend to be generated in specific size ranges (e.g., mobile
source generated Pb is typically less than 1 ym). In addition, these
size ranges are also useful for identifying deposition patterns in the
respiratory system.'-20-' A recent EPA sponsored aerosol sampler comparison
study showed that there is currently no ideal particulate sampler for
F211
all sampling and analysis requirements. J However, the dichotomous
sampler is the current EPA "method of choice" as a research monitoring
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device for collection of a less than 15 urn sample that is divided into
two fractions at a 2.5 urn cut-point. For measurements requiring only a
total 0-15 urn sample, two alternative sampling methods are also being
investigated by EPA—(1) a size selective hi-vol with a 15 urn cut-off
inlet and (2) a sampler similar to the dichotomous sampler but having no
mechanism for obtaining the 2.5 urn cut.
In order to meet the Clean Air Act Amendment requirement of a
reappraisal of the TSP standard by 1980, it is apparent that first the
f22l
magnitude of the IP fraction of TSP must be identified.1- J This should
be established at numerous selected sites across the United States,
identifying the mass ratios and the localized source influences through
subsequent sample analysis. It would then be desirable to relate the IP
measurement not only to the hi-vol (TSP), but also to other samplers
such as the British Smoke Shade sampler used in important health effects
studies. To provide information for implementation planning subsequent
to a revised standard, data on spatial distribution localized source
impact, and sampler reproducibilities must also be collected.
II. Purpose
This document describes the rationale and imolementation procedures
to be followed by the Environmental Monitoring and Support Laboratory
(EPA/EMSL/RTP) for the monitoring network which will establish a nationwide
data base on Inhalable Particulates (IP). Primary emphasis will be en
objectives relating to health effects and control strategy imolementation.
Because new concurrent epidemic!ogical studies are beyond the time and
resource constraints of this effort, the primary siting considerations
will be given to those locations with an on-going or historical health
studies data base. Analyses of size fractioned aerosol samples—primarily
those defined as IP (less than 15 um)—will be compared with analyses of
TSP samples collected by the hi-vol. The distribution of these measurements
across selected metropolitan areas will be determined along with some
indication of the impact of localized source contributions. Detailed
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studies of macro- and microscale concentration gradients of IP are
needed for explicit siting guidance, but because of resource constraints
will be accomplished in one or two metropolitant areas. At selected
sites the IP measurements will be compared with those made by aerosol
samplers used in previous health studies to determine the agreement
among the samplers under existing source conditions.
•
III. Scope
In order to meet the requirements of the Clean Air Act Amendments
and-provide a nationwide long term data base for chronic exposure assessment
the IP network will be established with two Key target dates.'-23^ The
first is the date required for promulgation of a new or revised particulate
standard, December 31, 1980. The second is the completion date on which
a four year sampling plan will be based, December 31, 1982. The latter
date would provide time for supplementary monitoring to determine the
impact of revised implementation plans.
Specific funding for this effort began in FY-78 and continues into
FY-79 with no current direction on subsequent year funding. To adequately
meet the long term objectives and make the first year's monitoring
meaningful, subsequent funding is assumed until the end of 1982. The
estimated resources requirements by fiscal year are shown in Table 1.
Only the budget totals for FY-78 (5400K) and FY-79 ($1,600K) have been
designated and even though subsequent funding is considered a necessity,
accomplishment provisions must be provided if only one, two or three
years are funded. Note in Table 1 that in-house manyears are desianated
as being required for successful implementation even with every effort
made toward contract services. Specifically the areas of site selection
and setup, program management, external quality control, and data processing
and reporting require total or partial EPA personnel involvement.
Analytical support services will be handled almost entirely by contract
and interagency agreement.
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Distribution of FY-78 and FY-79 resource allocations is shown in
Table 2. Note that capital equipment and analytical support will require
the largest expenditures. These estimates are based on setup of up to
100 sites during the first year.
In order to answer key questions such as sampler precision and
reliability, and interelation of sampler types for collection of 24-hour
samples, the full scale network design will be preceeded by a oilot
study. It is currently planned to test the currently available manual
dichotomous samplers (Sierra and Environmental Research), an automated
dichotomous sampler (Beckman), a hi-vol with a 15 urn size selective
inlet (Texas A&M design) and the EPA Reference Method Hi-Vol. This
study will require approximately 3-4 months of data collection initially
in Durham and Los Angeles, and then at 3 other selected locations.
Testing will be conducted during the first phase of the pilot study in
Durham at the EPA/EMSL air monitoring station. This test will require
3-4 weeks and will provide information such as sampler precisions and
reliabilities through side-by-side sampler testing of 3 samplers of each
brand/type. Only mass, sulfates, and nitrate measurements will be
considered during this phase. This period of time will also be used for
preparation of procedures, including those needed for sampler operation,
quality control, and data collection. The Durham location represents an
area for aerosol testing with light loadings and only a small expected
proportion of large particles (fugitive dust). The 3-4 week comparability
test will then be repeated in Los Angeles, California at EPA/EMSL's Los
Angeles Catalyst Study field site, adjacent to the San Diego Freeway.
This location will provide a "worst case" ambient aerosol samoling
situation becasue of the reintrained larger particles, air turbulence,
and moderately heavy loadings.
From the tests at these two locations the appropriate statistical
analyses will be applied to estimate the comparability of data sets
between samplers of the same brand/type and between samples of different
brand/types. Since there is no aerosol collection reference system the
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accuracy of collection cannot be determined. The ability of the samplers
to maintain a flowrate calibration will be quantified through flow
records and audits carried out during the tests. An attempt will also
be made to estimate the reliability of each sampler during the tests and
the expected reliability in network operation. Because some of the
devices to be tested will be relatively new in concept and aoplication,
it is expected that a variety of mechanical problems will arise. These
problems will be examined by EMSL oersonnel to determine if a correction
can be made in a "reasonable" period of time, or if major sampler revision
is necessary. Since this program does not have the resources or the
time to undertake instrument development, samplers with unresolvable
problems cannot be utilized in the network. The data from the reproducibility
and reliability tests will be utilized to prepare a procurement to be
solicited in early 1979 for purchase of the balance of samolers needed
for the first 100 sites.
A second phase of the pilot study will follow the initial reproducibility
and reliability tests of Phase I. Because IP samplers and their associated
technology are relatively new a more extensive intercomparison of sampler
types is necessary at several additional sites. This would permit
sampler comparison under a larger variety of aerosol and meteorological
conditions, and at the same time begin collection of network data. Only
one sampler of each brand/type would be at each location instead of the
triplicate testing done under Phase I.
The 5 sites for Phase II are shown in Table 3, and represent a
cross-section of expected sources and loadings. These sites were selected
also for future utilization in the full scale network. The selection of
only 5 sites for this portion of the pilot study was based on a compromise
between the number of samplers of all types that will be available and
the resources required. If possible, additional sites will be added to
this study as equipment and resources permit.
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The comparability data from the Pilot Studies are crucial to further
deployment of the network. If the automated and manual dichotomous
samplers are not determined to provide comparable data, the utilization
of the both types of samplers would obviously be impossible until differences
are resolved. This is also true if the dichotomous sampler results did
not agree with those of the size selective inlet hi-vol. The degree of
comparability will have to be determined by using statistically valid
comparison tests. These comparability data will represent the current
state-of-the-art and will be used as guidelines in future data interpreta-
tion.
The field sampling second phase of the pilot study will require 3-4
months depending on favorable meteorology and the percentage of valid
data obtained. The total time required for both phases should be approximately
6 months.
The sampling equipment to be used in the pilot study is indicated
in Table 4. Manual dichotomous samplers designed to have the same
aerosol collection characteristics as the automated versions will be
tested and compared along with a recently designed 15 um inlet hi-vol
sampler designed by Dr. Andrew McFarland at Texas A&M University. The
meteorological equipment will be used as required in Birmingham and
Philadelphia to assess, if possible, spatial distribution, local source
impact, and transport. British Smoke Shade samplers, identical to those
used in the early health studies in Europe, will be collocated in the
urban area locations. For comparison purposes and investigation of
alternatives, other types of aerosol samplers may be added to selected
sites for short term study.
Operation of the sites in the pilot study will be conducted by a
combination of EPA employees, contractors and state and local agency
personnel. Samplers will operate every third day during Phase II of the
pilot study. All samples will be analyzed at RTP by on-site contractors.
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The full scale network will evolve from the initial pilot study
sites. Since resources will provide for up to 100 sites during the
first year, the remaining sites will be deployed after completion of the
pilot study. The primary siting consideration will be based on population
density, but geographical coverage will also be stressed. Until other
information is obtained the TSP siting criteria published on pages
34924-34926 of the 8/7/78 Federal Register will be utilized. Site
operation of the full scale network samplers will in general be by state
and local agency personnel. Contract services for these ooerations
would be prohibitively expensive, and will be avoided.
In order to assure uniform data quality, a comprehensive quality
assurance plan must be prepared at the outset, including provision for a
siting criteria document, complete operating procedures, and flow and
aerosol calibration test procedures. These procedures will be prepared
primarily by EPA and contractor personnel, who will then implement a
transfer of technology program to train the field ooerators in sampling
and the field laboratories in mass determination. Contractors will also
be used to assist in an external flow audit test program as well as a
program to routinely reassess aerosol collection characteristics.
The analysis contractor at RTF will transfer the laboratory data to
a prescribed computer compatible format and transmit the data to EHSL/RTP
for processing. A contractor will be used to assist in computer programming
for IP data processing and output. An attempt will also be made to
integrate QA data, such as collocated sampler results, into the monitoring
data base to qualify the data. The overall management of the network as
well as external auditing, data assessment, and report writing will also
be performed by EMSL/RTP-
It is anticipated that no more than 100 additional sites could be
established in the second year of the network while maintaining adequate
control over site selection criteria and operator performance. It is
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estimated that at least 300 sites will be needed nationwide for adequate
coverage. Thus at TOO sites/year all sites could be on-line by the end
of 1981 to produce at least 1 year of data by the end of 1982.
IV. Network Design
General
The primary objectives for the establishment of a nationwide IP
network are related to health effects and control strategy implementation.
The IP network data are needed to revise the existing primary ambient
particulate standard which is based on health effects related to hi-vol
measurements , and to assist in implementation plan preparation for
control strategies to; meet the standard. The objectives are emphasized
by the Clean Air Act Amendments which impose a time constraint (December 31,
1980) on the promulgation of'a new or amended particulate standard, and
f24l
hence on the data bases necessary to support the standard. J
In addition to these primary objectives, it is desirable to incorporate
where feasible related objectives into the study design. The degree of
consideration given to the secondary objectives is dependent on the
resources remaining after implementation of the primary objectives. The
three most important secondary objectives are to determine: (1) atmospheric
transport of IP, (2) energy related source contributions to IP, and (3)
the acidity of IP as compared to wet precipitation (e.g. rain). Since
these three items will have EPA funding in FY-79 in ORD orogram areas
other than the IP Network, it is important to coordinate all IP monitoring
efforts within EPA to not only be cost effective, but also provide the
data in compatible collection methodology and data output formats for
ease of intercomparison. Additional objectives for the network may be
considered if resources permit and/or the site locations can serve more
than one objective. For example, several of the sites being selected
for measurement of IP contribution of Western Energy sources, (coordinated
by EMSL/LV) will also have nephelometers. This would provide the possibility
10
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of intercomparison of the IP mass measurements with the measurements of
the nephelometer for possible air pollution indices application.
Another consideration might be the determination of indoor versus outdoor
levels of IP for exposure determination. This type of measurement may
be done as part of the non-EPA sponsored Harvard Study and could be
included in the IP network data base if the data are compatible.
The most significant difference in considering the various objectives
for inclusion in a unified monitoring network is site selection criteria.
Because of the emphasis on comparison of IP data with health studies
data, the first priority for siting of the IP stations will be to
locate near historical, existing, or planned monitoring locations for
epidemiology studies. The requirements for selecting sites for EPA
health studies include: (1) location in a community school district
with a relatively uniform socio-economic structure, (2) lack of influence
on the area by emissions from a localized source, (3) location in areas
representing low, medium and high expected concentration exposure levels,
(4) location in areas that are easily related to other urban locations,
roc pc ~]
and (5) location in areas with a reasonably high population density. ' J
These criteria would then also apply to the IP monitors located at the
health study locations.
Since there are only a limited number of these health study sites,
the second priority for site selection would be to concentrate on urban
metropolitan areas in order to provide control strategy information such
as spatial distribution, local source influence, and effect of various
source categories (e.g., mobile, industiral, etc.). The two urban areas
of Philadelphia and Birmingham have been selected for intensive study
for up to 1 year.
The third priority for site selection is to establish representative
sites at enough locations around the U.S. to "characterize" the nationwide
distribution of IP and its relationship to the TSP at the individual
11
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locations. The order of establishment of these sites would be by population
density, degree of attainment of the existing IP standard, and geographic
coverage. Because of the limited number of samplers that will be available
during 1979 and the emphasis that will probably be placed on the first
years data, these sites must be selected carefully.
Pilot Study Design
Before the long term IP monitoring efforts begin, a two part pilot
study will be conducted which will provide information necessary to
establish a technically sound, comprehensive, and cost effective full
scale network. The key areas in the pilot study are determination of
(1) the precisions of the test samplers under a variety of field conditions,
(2) the inter-relationships (comparability) of the measurements under
field conditions, and (3) the expected reliabilities of the samplers.
At the beginning of the pilot study preliminary sampler operation,
calibration and audit procedures will have to be devised along with
formats for data collection and preliminary software for data storage
and retrieval. Preparation of three draft documents will be initiated
to individually cover the areas of: (1) Sampler Operation, Calibration
and Aerosol Characterization, (2) Data Collection Formats and Procedures,
and (3) Siting Criteria for IP Monitoring. These three documents will
be part of a larger document covering the Qua! ity Assurance for I_P_
Network Operation. This latter document will be prepared accordina to
' F281
the format specified in the EPA Quality Assurance Handbook.1 J
These reports will be prepared primarily under contract. A qrant
to the Air and Industrial Hygiene Laboratory (AIHL) in Berkeley, California,
is contemplated for the evaluation, testing, and method preparation
needed for the first document. This grant will be monitored by the
Quality Assurance Branch (OAB) of EMSL. An on-site contractor will be
used to assist in preparation of the data collection formats, computer
software and procedures. This contract has already been awarded to
12
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Systems Research and Development, Inc. and will be monitored by the
Statistical and Technical Analysis Branch (STAB) of EMSL. The preparation
of a siting criteria document will require determination of spatial
distributions, effects of localized sources, etc. This document will be
prepared by a contractor based in part on data collected during intensive
studies of Philadelphia and Birmingham.
The determination of sampler comparability during the pilot study
will be performed following a similar format used in determining the
precision of integrating samplers used in the Los Angeles Catalyst
Study. This format not only provides precision information, but can
be used to identify variance components related to the individual
operation steps, such as sampler operation, -filter cutting, and analysis.
This testing requires at least two samplers of each tyoe operated for at
least 12 to 15 days.
Since the aerosol calibration of the IP samplers at present cannot
be done in the field, field auditing will be concerned primarily with
flowrate testing. For all of the samplers, transfer standards such as
orifices, Venturis, or mass flow meters will be used by the sampler
operator as field calibration devices. Similar devices will also be
mailed (or taken by an auditor) to the operator as part of an external
audit program operated by a QAB contractor. All transfer standards will
be referenced against NBS traceable volumetric standards keot by OAB at
RTP. Flow calibration checks will be performed at least monthly and
audited quarterly at all locations.
The aerosol collection efficiencies for each of the sampler types
used in the network must also be known at the outset of the study. If
sufficient data are not available at the start of the pilot study on
inlet efficiencies and wall losses, representative samplers will be sent
to a contractors test laboratory (aerosol wind tunnel facility) for
characterization. These tests will probably be oerformed at Texas ASM
University under an existing contract, and/or through the proposed grant
13
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to AIHL. Because of the resources required to perform controlled aerosol
testing, it is desirable to establish a test scheme where only a representative
number of samplers can be tested to represent the batch of samplers
received under each order. A separate contractual effort will also be
undertaken to examine the feasibility of a portable aerosol collection
efficiency audit device which could be used in the field for subsequent
tests. Since this effort may require a substantial period of time for
completion, the samplers in the field will be rotated back to a central
test lab periodically to reassess the collection characteristics. This
testing will also be augmented by collocated samplers operated periodically
at each site.
The results of these initial reproducibility, reliability, and
aerosol collection tests will be used as the bases for future procurements
of samplers for the IP network. In addition, EMSL will begin in FY-79
to collect the information necessary to designate either a' method of
choice and/or a set of sampler performance specifications. This program
will be conducted primarily by the OAB, with assistance from this network
and outside contractors as required.
The pilot study will be conducted in two parts—one at RTP and Los
Angeles to determine the parameters such as precision and reliability
under "best-case" operation — close operator attention, frequent calibrations,
highly skilled personnel, etc. This portion of the study will require
approximately two months to complete and will contain 3 samplers of each
type of automated dichotomous sampler, manual dichotomous sampler, high
volume sampler, smoke shade sampler, and a hi-vol with a size selective
15 um inlet.
Phase I of the pilot study will be followed by a second phase to be
conducted at 3 additional urban area locations. A summary of the proposed
area locations and their site selection rationales is shown in Table 5.
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The number of sites selected at each of these locations is governed
primarily by the number of samplers that are expected to be available at
the start of the study.
The utilization of both manual and automatic dichotomous samplers
for the pilot study as shown in Table 4 is based on the premise that
automated samplers are needed for intensive investigations, determination
of diurnal patterns, episode monitoring, or locations where sampler
operators visit infrequently. Because of the current substantial cost
differential between the 2 sampler types (manual--$3.5K, automatic—
$7.8K), there will undoubtedly be many applications where a manual
sampler would be more cost effective. This would be especially true at
locations requiring only every 6th day sampling. Since the sampler
inlets and separation heads for the manual and automatic versions are
theoretically identical, the characteristics of the hardware and electronics
relating to the sample changing mechanism should be easy to identify.
The relative merits of the two sampling capabilities will be quantified
in the second portion of the pilot study. It is expected that a mix of
automated and manual samplers will be utilized for the full scale network,
depending on individual site requirements.
A key area in the IP network will be operation of the samplers in
the field by trained personnel. The first phase of the pilot study will
be conducted by EPA employees. The sites in Phase II will be operated
by either EPA/EMSL employees (Durham), contractor personnel procured for
the pilot study (Philadelphia and Birmingham), or contractor personnel-
associated with the existing health studies (Los Angeles and Akron/Canton).
The site selection and set up arrangements will be directed by EMSL
personnel. Meetings will be held with Regional Office and local agency
personnel to obtain assistance in site selection and coordination.
The analytical services other than mass measurements required for
the pilot study will be performed at RTP by both EPA and contractor
15
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employees. A complete document on analysis of the filter samples must
be prepared prior to the start of analysis, describing the Analytical
Procedures for IP_ Network Samples. This document will describe analysis
procedures for hi-vol, dichotomous, and smoke shade samples. Some of
the procedures for the hi-vol samples have already been prepared as part
of the LACS and CHAMP programs. Procedures for the dichotomous sample
analyses will be prepared with the assistance of ESRL. The smoke shade
sample measurement procedures will be those described by the World
Health Organization
The samples from the IP network studies will be collected on either
glass fiber (hi-vol), Teflon membrane (dichotomous), or Whatman (smoke
shade) filters. The expected sample volumes for the oilot study are
shown in Table 6. All filter samples (except the AISI tape and smoke
shade samples) will require gravimetric analysis to determine mass.
Because of the nossible cost advantages of beta gauging the membrane
dichotomous filters, this approach will be investigated to determine the
comparability with gravimetric analysis. A laboratory system will be
built by Lawrence Berkeley Laboratory to ESRL specifications for utilization
by the Analytical Chemistry Branch (ACB) of EMSL. Sample loss from the
filters and the impactor plates during transport will be identified
early in the pilot 'Study because of the potential effect on other analyses.
All dichotomous mass measurements in the pilot study will be made using
electronic micro-balances procured for the network.
Selected dichotomous filters upon arriving at the lab in RTP will
be subjected to X-Ray Fluorescence Analyses (XRF) to determine elemental
concentrations. Initially as many as 30 elements will be examined, but
subsequently reduced to a smaller number to minimize data storage requirements
After the non-destructive XRF analyses, selected wet chemical
analyses of the hi-vol and dichotomous sampler filters will also be made
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on the pilot study samples. The analyses will Include water soluble
sulfates (S04) and nitrates (N0~). A summary of the pilot study analyses
is shown in Table 7. The analytical methods of cnoice for wet chemistry
will be selected at the time of preparation of the analytical methods
document and will be methods that can be automated. If possible a
portion of each filter will be archived for several months for later
analyses. Using cost estimates assuming an on-site (RTF) contractor was
oerforming the analyses, the total analysis costs for Phase II of the
pilot study are shown in Table 8. It is assumed that selected existing
analysis equipment in EMSL can be utilized for the pilot study and only
the capital equipment listed in the notes would have to be purchased.
After the pilot study samples are analyzed the results will be put
into the proper data format and stored using programs (software) provided
by EMSL. The data will be validated by on-site contractor personnel on
a bi-weekly basis and output in a summary form at the completion of the
pilot study. These data will then be summarized in a final report which
will address the comparability of the various sampler types, the precision,
and the reliabilities. This final report will be the basis for the full
scale operation network.
Urban Area Intensive Studies
In order to provide as much information as possible by the end of
1979 for control strategy planning, an intensive IP monitoring effort in
two metropolitan areas is planned. The IP distributions in the cities
of Philadelphia and Birmingham, which are already part of the pilot
study, will be studied to obtain limited data on: (1) the spatial
distribution of IP as compared to that of TSP, (2) the urban IP concentrations
as compared to the background, (3) transport of IP from the urban area,
(4) the approximate contributions of mobile sources, stationary sources,
and photochemistry to the overall IP level, and (5) diurnal IP concentrations
as related to local urban activities.
17
-------
These intensive studies will collect samples for up to 12 months
beginning in Apri.1 1979 after the pilot studies are completed. The
sites in Philadelphia and Birmingham will be supplemented to increase
the number of sites to 10 in Philadelphia and 5 in Birmingham. The
number of sites in each area is based on a compromise between the total
number of IP samplers expected to be available in early 1979 and the
study objectives. After approximately 2 months of monitoring, the data
will "be evaluated to determine if additional sites are needed to obtain
the desired information.
Both locations will require specific site meteorology data, and met
stations for wind speed, wind direction, temoerature, and relative
humidity will be erected as needed. It is anticipated that no more than
2 or 3 stations will be needed. The number of met stations required
will also be reassessed after 2 months of data collection.
The types of samplers operated in the intensive study will be fri-
vols, dichotomous samplers, smoke shade samplers, and size selective
inlet hi-vols. The sampling frequencies will be a combination of every
other day and every sixth day for the sites collecting 24 hour trend
data.
Operation of the samplers during this intensive effort w^U be
handled by local agency oersonnel. The analyses performed would be
those defined in the pilot study.
The results from the Urban Area Intensive Study will be summarized
in a report following completion of sampling in 6otn locations. Host of
the computer software for tlrrs study irfll be prepared during or before
the pilot study, but several site specific programs are anticipated to
require preparation in early 1979.
18
-------
fjjll Scale Network
In order to provide a nationwide data base for IP and IP/TSP ratios,
a large scale monitoring network beyond the Pilot Studies and Urban Area
Intensive Study must be established. This network should characterize
the ambient concentration distribution in the U.S. in a manner similar
to that attempted by the NASN network for TSP- The draft IP Siting
Criteria Document prepared during the pilot study will be finalized for
use in siting the permanent full scale network sites. Careful preparation
of this document as part of the overall quality assurance plan is critical
if the proposed objectives for the network are to be accomplished.
Based on information gained in the pilot study a final set of
sampler performance specifications will be prepared so that samplers to
establish additional sites can be procured in 1979. A long-term schedule
relating the network establishment to key target dates is shown in
Figure 1. Prior to beginning site selection EMSL personnel will brief
the Regional Offices on the objectives of the IP network and how local
agency personnel can participate. Since contractor operation of all
sites in a nationwide sampling network would be prohibitively expensive,
it is planned that local agency personnel would provide assistance by
operating the samplers, completing the data forms, performing routine
flow checks, and mailing the samples to RTP. EPA/EMSL/RTP would provide
the samplers, supplies, filters, analytical services, and return copies
of the validated IP data to the local agency. In addition EPA/ EMSL
would perform the flow and aerosol characterization external audit
testing needed for quality assurance.
Setup of the sampling sites in 1979 will require at least 6 months,
such that some samplers would be on-line in early 1979 and others not
until July 1979. All sites will contain a TSP Hi-Vol and a dichotomous
sampler with a 15 micron and a 2.5 micron cuptoint. In addition to
examine the relative merits of a 15 micron size-selective inlet developed
19
-------
for hi-vols, 50 sites will also be equipped with these experimental
samplers. In most cases the IP sites will be at existing hi-vol sampling
locations or at proposed NAMS/SLAMS sampling sites which meet the network
sitinq criteria. Until more definitive information can be obtained, the
(31)
August 8, 1978, Federal Register TSP siting criteria will be utilized/ '
In order to assure uniform data quality the hi-vols used in the IP
network must be similar in shelter design (FEDERAL REGISTER specifications)
and have a flow recorder instead of Visi-Float'-type readout. Mass flow
controllers will not be a requirement. The IP hi-vol samples can be
used as the collocated sampler with the local agency sampler per NA.MS/
SLAMS requirements, however, IP analyses will have priority over other
analytical requirements. Because of these qualifications on the hi-
vols, it is anticipated that most of the hi-vols needed in 1979 will
have to be procured or modified as part of this network.
The frequency of operation for most of the samplers used in the
full scale network will be everyi6th day. The sample volume, analyses
to be performed, and expected analysis costs for the full scale network
in 1979 are shown in Table 9. Because the analysis of every sample from
the full scale operation would be very expensive (^SSOOK) and would
provide more data than is needed to establish a data base, only a portion
of the 1979 samples will be analyzed beyond mass. Mass concentrations
will be determined on all samples. Analyses beyond mass will be continued
on 50% of the samples 'for the first 6 months at each site and 25;; thereafter.
Filter materials will add nearly S50K to the cost of miscellaneous
operating supplies in 1979.
The tentative list of the first 96 sites are shown in Table 10.
These sites will be established from March thru July, 1979, in the
approximate order listed. The intensive studies in Philadelphia and
Birmingham are reflected in the larger number of sites in these cities.
The distribution of samplers by site classification was primarily the
result of OADPS recommendations. The definitions of the site classifications
20
-------
are general with the assumption that no site will be unduly influenced
by a single source. Selection of the actual site locations will be made
utilizing the recommendations of the Regional Offices and State/local
agency personnel. Table II defines the distribution of samplers by
metropolitan area. The automated dichotomous samplers will be located
either in the expected highest concentration areas and/or the areas in
which diurnal pattern data are desired. Because there is a potential in
some locations for dichotomous sampler filter overloading before collection
of a 24 hour sample, some redistribution of automated and manual dichotomous
samplers may be required.
The maintenance, resupply (periodic shipment of samplers and flow
devices for external audits) for the full scale network be set-up and
operated initially by in-house personnel and then turned over to a
contractor. Data processing and reporting will be handled by EMSL
personnel .
As the network is enlarged (subsequent year funding) a transfer of
technology program must be setup to control the quality of operations
performed in the field. This includes sampler operation, gravimetric
analyses, completion of data forms, routine flow checks and maintenance.
This training program will be designed during the first year of operation
and implemented by contract.
21
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References
(1) "Health Effects Considerations for Establishing a Standard for
Inhaled Participate Matter," EPA/HERL internal report,
January, 1979; Submitted to JAPCA for publication.
(2) Air Quality Criteria Document for Particulate Matter, DHEW/USPHS,
National Air Pollution Control Administration, A-49, 1969,
pp. 17-23, 111-125.
(3) "Health Hazards of Atmospheric Particulate Matter," by J.R.
Goldsmith, M.D., presented at Third Interagency Symposium on
Quality Assurance in Particulate Matter, Berkeley, California,
May 18, 1977.
(4) Internal Memorandum, J.H. Knelson to G.G. Akland, January
1978.
(5) Federal Register, Vol. 36, No. 84," April 30, 1971, pp. 8191-8194.
(6) Ibid, p. 8187.
(7) "Large Particle Collection Characteristics of Ambient Aerosol
Samplers," by J.B. Weddina, A.R. McFarland and J.E. Cermak, ES&T,
Vol. 11, No. 4, pp. 387-390, April 1977.
(8) "Size Distribution Characteristics of Airborne Suspended Particulate
Matter in Selected Sites," by W.M. Kozel, R.M. Burton, W.L. Crider
and F.B. Benson, EPA/HERL CHAMP Internal Report, February 1973.
(9) "National Air Surveillance Cascade Impactor Network, I. Size
Distribution Measurements of Suspended Particulate Matter in Air,"
by R.E. Lee and S. Goranson, ES&T, Vol. 6, No. 12, November 1972,
pp. 1019-1024.
(10) "Atmospheric Pollution in Leicester (1945)," Atmospheric Pollution
Research Technical Paper No. 1, London: His Majesty's Stationery
Office, pp. 8-15.
(11) "The Evaluation of Methods for Measuring Suspended Particles in
Air," by R.E. Lee, J.S. Caldwell and G.B. Morgan, Atmos. Envir.,
Vol. 6, 1972, pp. 593-622.
(12) "Amendments to the Clean Air Act of 1970," Public Law 9595, August
1977.
-------
(13) Ibid, p. 8187.
(14) Health Effects of Particulate Pollution—Reappraising the Evidence,
prepared by A.E. Bennett, I.R. Cameron, C. du V. Florey, W.W. Holland,
S.R. Leader, R.S.F. Skhilling, A.V. Swan, and R.E. Waller for the
American Iron and Steel Institute, December 1977.
(15) State by State Listing of Counties Failing to Meet Federal Ambient
Air Quality Standards for Total Suspended Particulates ," OAQPS Report,
February 1978.
(16) "EPA Looks at Fugitive Emissions," E.J. Lillis and D. Young, JAPCA,
Vol. 25, No. 10, October 1975, pp. 1015-1018.
(17) "The Mass Distribution of Large Atmospheric Particles and How It
Relates to What a Hi-Volume Sampler Collects," by D.A. Lundgren
and H.J. Paulus, Presented at the 66th Annual APCA Meeting, Chicago,
Illinois, June 24, 1973.
(18) Airborne Particles. Report Prepared for National Academy of Sciences,
Washington, D.C., 1977.
(19) "Ambient Air Analyses with a Dichotomous Sampler and X-Ray Fluorescence
Spectrometer," T.G. Dzubay and R.K. Stevens, ES&T, Vol. 9, 1975,
pp. 663-668.
[20) Ibid, p.
(21) "Intercomparison of Aerosol Samplers for Mass, Sulfur, and Other
Elements," by D.C. Camp, A.L. VanLehn, and B.W. Loo, To be Published
as Final Report for EPA Interagency Agreement IAG-D7-F1108 with
Lawrence Livermore Laboratory, March 1978.
(22) Ibid.
(23) Ibid.
(24) Ibid.
(25) "Air Monitoring Siting Requirements for Human Exposure Assessment,"
EPA/HERL CHAMP Internal Report, 1975.
(26) Private Communication, D. Mage (EPA/HERL) to C. Rodes (EPA/EHSL),
April 1978.
(27) Ibid.
23
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(28) Quality Assurance Handbook for Air Pollution Measurement Svstems,
Volume I. Principles. EPA/ORD Publication EPA-600/4-77-027,
May 1976.
C29) "Precision of LACS Sampling and Analytical Methods," by G.F. Evans,
as part of The Los Angeles Catalyst Study Symposium, EPA 600/4-77-034,
pages 207-264.
(30) Selected Methods of Measuring Air Pollutants, WHO Publication No. 24,
World Health Organization, Geneva, 1976, pages 17-23.
(31) Air Quality Surveillance and Data Reporting, Federal Register Vol. 43,
No. 152, August 7, 1978, pages 34924-34926.
24
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Table 1
FY-78 FY-79b FY-8QC FY-81C FY-82°
Resource Totala (x 1000) $400 $1,600 $2,000 $1,500 $1,700
In-House Manyears 2.3 6.0 3.0 2.0 1.5
In-House and Extramural
nonding budgeted in Accoiplishment Plans; Manyears are needed
but not budgeted
indication has been received for subsequent year funding.
These estimates reflect a need for a 300 station network.
-------
Table 2. Resource Requirements for IP Network
Funding ($ x 1000) Manyears
FY-78 FY-79 FY-78 FY-79
Study Design — — 0.2 0.2
Sampling Equipment Procurement 310 480 0.2 0.3
Site Selection/Set-up/Travel 10 50 0.6 2.0
Transfer of Technology — 20 — 0.4
Quality Assurance 30 350 0.2 1.0
Analytical Support-EPA Equipment/ — 500 — 0.2
Contractor Operation
Contractor Services-Sampling/Calibration — 120 — 0.1
Data Collection 50 30 0.3 0.5
Program Management — — 0.8 1.0
Data Processing/Reporting — 50 — 0.2
Totals S400 $1,500 2.3 6.0
-------
Table 3
Pilot Study Site Locations
(Phase II)
Type
Urban
Urban
Urban
Urban
Area Location
Birmingham, AL
Akron/Cleveland ,
OH
Philadelphia, PA
Los Angeles, CA
Source Type(s)
Heavy Industry
Medium Industry
Medium Industry
Photochemical ,
Expected
IP Loadings
Med to High
Low to High
Medium
Med to High
Mobile
Urban Durham, NC Light Industry Low.to Med
-------
Table 4. Sampling Equipment Distribution - Pilot Study (Phase II)
Area Location ti Sites
Akron/Cleveland 1
I'iniiingham 1
Philadelphia 1
Los Angeles 1
Durham 1
Total 5
Hi-Vol
1
1
1
1
1
5
SSI
Hi-Vol
1
1
1
1
1
5
M. Dichot3
1
1
1
1
1
5
A. Dichot3
1
1
1
1
1
5
AISI
Tape Sampler
1
1
1
1
1
5
Smoke Shade Met
1 0
1 1
1 1
1 0
1 0
5 2
Motes: aM. Dichot - manual dichotomous sampler; A. Dichot - automated dichotomous sampler.
Met - Meteorology: wind speed, wind direction, temperature and relative humidity.
-------
Table 5. Pilot Study Site Selection Rationale
Area Location
Birmingham, AL
Akron/Cleveland, OH
Philadelphia
Los Angeles, CA
Durham, NC
Health
Related
X
X
X
Control Strategy
Related
X
X
X
X
Exceeds TSP
Standard
X
X
X
X
-------
Table 6. Pilot Studv Sancle Volume
Substrate
Total
Phase I
420
Phase
.
r_
6,100
Approximate
Substrate Costs, ?
Glass Fiber
Teflon Membrane
Whatman
80
260
80
1,100
4,800
200
$ 700
5,000
200
$5,900
Notes: a3ased on 20 days of operation.
on 90 days of operation.
-------
Table 7. Pilot Study Sairple Analyses
Substrate Sampler Mass (G)a Mass (R) SO, NO.
Glass Fiber Hi-Vol X XX
Teflon Membrane DichotorrtDUS X XX
Whatman Smoke Shade. X
Notes: aMass (G) - Gravimetric
Mass (R) - Reflectance
-------
Table 8. Pilot Study (Phase II) Analysis Volumes and Costs
Hi-Vol
Dichotorousa
Mass (R)b
Totals
Analysis
Volume
1,200
5,000
300
6,500
Est. Cost/0
Sample, S
$10
12
1
Est. Total
Cost, $
$ 12,000
60,000
300
$ 72,300
Notes: 5 electronic micro-balances must also be purchased - $15,000
5 reflectoneters must also be purchased - 5,000
Capital Equipment Total $20,000
based c
of EPA owned equipment
CCost per sample based on contractor operation
-------
Table 9. Network Sample Volumes and Analysis Costs* for 1979
Sample
Volume
Hi-Vol and 15 micron Hi-Vol 16,000
Dichotomous
Totals
17,000
33,000
Est. Cost/
Sample, S
Mass $ 2
Others $10
Mass $ 2
Others $25
Est. Total
Cost, $
$ 92,000
196,500
$ 288,500
*A11 samples will be_analyzed for mass. Selected Hi-Vol samples will be
analyzed for SOT, NOl, and Pb. Selected dichotomous samples will be analyzed
for S07, NOZ, arid XRF analyses for 10 elements. Beyond mass 50% of 1st
6 montn's samples will be analyzed and 25% thereafter.
-------
Table 10. Sites Selected for IP Network in 1979
Site Classification
Location Industrial
Philadelphia
Akron
Cleveland
Steubenville
Los Angeles
Durham
RTP
Bi rmingham
Phoenix
Buffalo
Denver
New York City
Chicago
Houston
Pittsburgh
St. Louis
Baltimore h
NFOS-Kisatchie, La/D .
NFOS-Green Mountain, Vt.
NFOS-Custer, Mt
Washington, DC
Detroit
Kansas City
Salt Lake City
San Jose
Dallas
Portland
Seattle
Oakland
Five Points (California)
Winnemucca (Nevada)
Boston
Minneapol is
Atlanta
Cincinnati
Trenton
Hartford
El Paso
Honolulu
2
0
2
1
1
0
0
2
0
2
1
0
1
1
1
1
0
0
0^
0
0
1
0
0
0
0
0
1
1
0
0
0
0
1
0
0
0
0
0-
Ccmmercial
4
0
1
0
1
1
0
1
2
1
1
2
1
1
1
0
1
0
0
0
1
1
2
2
1
1.
1
1
1.
0
0
1
1
1
1
0
1
1
J.
Residential
2
1
0
0
1
0
0
1
3
t)
3
1
1
0
0
1
1
0
0
0
0
0
0
0
1
1
0
0
0
0
0
1
1
0
0
0
JO
0
4)
Rural /Non-Urban
2
1
0
0
1
0
1
1
1
1
1
1
1
1
1
0
0
1
1
1
1
0
0
0
0
0
1
0
0
1
1
0
0
0
0
1
1
1
0
Total
10.
l
4
1
1
4
4
3
3
2
2
1
1
]
2
2
•2-
2
2
2
2
2
2
1.
1
2
2
2
1
1
2
2
1
Totals
19
36
19
23
97
a One of the sites in Cleveland and Steubenville.^two^Mn Akron, and .-three in
Phoenix and Denver are associated with on-going health studies.
b NFOS - National Forest Ozone Study (EPA/EMSL)
Rural/Non-urban locations that exceed the TSP standard but are not industrial.
-------
Table 11. Location of IP Samplers During FY-79 by Sampler Type
Location Sites'
Philadelphia 10
Akron 2
Cleveland 3
Steubenville 1
Los Angeles 4
Durham 1
RTP 1
Birmingham 5
Phoenix 6
Buffalo 4
Denver 6
New York City 4
Chicago 4
Houston 3
Pittsburgh 3
St Louis 2
Baltimore 2
NFOS- Kisatchie, La. 1
NFOS- Green Mountain, Vt. 1
NFOS- Custer, Mont. 1
Washington, D. C. 2
Detroit 2
Kansas City 2
Salt Lake City 2
San Jose 2
Dallas , 2
Portland 2
Seattle 2
Oakland 2
Five Points (California) 1
Winnemucca (Nevada) 1
Boston 2
Minneapolis 2
Atlanta 2
Cincinnati '
Trenton |
Hartford 2
El Paso 2
Honolulu —!_
Totals: 97
Automated
Dichots
5
0
1
1
2
1
0
1
1
1
4
1
1
1
1
1
1
0
1
1
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
Manual
Dichots
5
2
2
0
2
0
1
4
5
3
2
3
3
2
2
1
1
1
0
0
2
2
2
2
2
2
'2
2
2
1
1
2
2
2
1
1
2
2
1
SSI
5
2
1
1
4
1
1
3
3
1
3
1
1
0
0
0
1
1
1
1
1
1
1
1
1
1
0
1
1
1
1
1
1
1
1
25
72
49
a All sites established in'1979 will contain a TSP Hi-Vol except the
3 NFOS locations.
b Hi-Vol modified with 15 rRicrd-n -size-selective -inlet.
-------
FIGURE 1
|METWORK SCHEDULE
PILOT STUDIES (DURHAM, LOS ANGELES)
URBAN AREA INTENSIVE STUDY (PHILADELPHIA)
ESTABLISH FIRST 100 NETWORK SITES
ESTABLISH 100 ADDITIONAL SITES
ESTABLISH 100 ADDITIONAL SITES
PREPARE SEMI ANNUAL REPORTS
INITIATE REVISION OF PARTICULATE
REFERENCE METHOD
PREPARE REVISED CRITERIA DOCUMENT
PROPOSE REVISED PARTICULATE STANDARD
PROMULGATE REVISED PARTICULATE STANDARD
SIP DATA COLLECTION PERIOD
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