Test/QA Plan for Pesticide Spray DRT in a Low Speed Wind Tunnel
May 2009
Version 1.0
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TEST/QA PLAN FOR THE VALIDATION OF THE VERIFICATION PROTOCOL FOR
LOW SPEED PESTICIDE SPRAY DRIFT REDUCTION TECHNOLOGIES FOR ROW
AND FIELD CROPS
ALION
TECHNOLOGY
HRTI
INTERNATIONAL
Alion Science &
Technology
1000 Park Forty Plaza, Suite 200
Durham, NC 27713
Phone: 919-549-0611
FAX: 919-549-4665
E-mail: drake.zora@epa.gov
RTI International
3040 Cornwallis Road
P.O. Box 12194
Research Triangle Park, NC 27709-
2194
Phone: 919-541-3742
FAX: 919-541-6936
E-mail: jwt@rti.org
USEPA-ETV
109 T.W.Alexander Drive
E434-02
Research Triangle Park, NC 27711
Phone: 919-541-2734
FAX: 919-541-0359
E-mail: kosusko.mike@epa.gov
This plan has been reviewed and approved by:
Signed by Zora E. Drake
Z. E. Drake, Technical Leader, Alion Science and Technology
Signed by Paulette S. Yongue
P. S. Yongue, Quality Manager, Alion Science and Technology
Signed by Jonathan W. Thornburg
J. W. Thornburg, Project Leader, RTI International
Signed by W. Gary Eaton
W.C. Eaton, Quality Manager, RTI International
Signed by Michael Kosusko
M. Kosusko, EPA Project Manager
Signed by Paul W. Groff
P. W. Groff, EPA Quality Manager
May 4, 2009
Date
May 4, 2009
Date
May 5, 2009
Date
May 5, 2009
Date
May 22, 2009
Date
May 22, 2009
Date
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A2: Table of Contents
List of Figures iv
List of Tables iv
List of Acronyms/Abbreviations v
Group A: Project Management 1
A4: Project/Task Organization 1
A4.1 Management Responsibilities 1
A4.2 Quality Assurance Responsibilities 3
A5: Problem Definition/Background 4
A6: Project/Task Description 4
A6.1 Description 4
A6.2 Schedule 5
A7: Quality Objectives and Criteria 6
A8: Special Training/Certifications 9
A9: Documentation and Records 9
Group B: Data Generation and Acquisition for Low Speed Wind Tunnel Tests 10
Bl: Sampling Process Design (Experimental Design) 10
B2: Sampling Methods for Measurement of Droplet Size, Deposition Flux, and
Test Conditions 11
B2.1 Sampling Locations 11
B2.2 Wind Tunnel Measurement of Spray Drift: Flux Volume 13
B2.3 Wind Tunnel Measurement of Spray Drift: Deposition 14
B2.4 Wind Tunnel Measurement of Spray Drift: Spray Size Distribution 14
B2.5 Measurement of Droplet Size Spectrum near the Nozzle (Determination
of appropriate reference test system) 16
B3: Sample Handling and Custody Requirements 17
B4: Analytical Methods 17
B5: Quality Control 17
B6: Instrument/Equipment Testing, Inspection, and Maintenance 18
B7: Instrument/Equipment Calibration and Frequency 18
B8: Inspection/Acceptance of Supplies and Consumables 19
B9: Non-Direct Measurements 19
BIO: Data Management 19
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B10.1 Data Acquisition and Management 19
B10.2 Reporting 20
Group C: Assessments and Oversight Elements 22
Cl: Assessments and Response Actions 22
Cl.l Internal Audits 22
C1.2 Audits of Data Quality 22
C1.3 External Audits 22
C1.4 Corrective Action 22
C2: Reports to Management 22
Group D: Data Validation and Usability Elements 23
Dl: DataReview, Verification, and Validation 23
D2: Verification and Validation Methods 23
D3: Reconciliation with Data Quality Objectives 23
Appendix A: Applicable Documents and Procedures 24
1. EPA Documents 24
2. RTI Documents 24
3. Alion Science & Technology SOPs 24
4. USDA/ARS SOPs 25
5. Other Documents 25
Appendix B: Organizational Charts for Testing the Low Speed Pesticide Spray DRT Protocol. 26
Appendix C: Alion SOP-WDE-08-02 - Standard Operating Procedure for the Turner Quantech
Digital Filter Fluorometer 27
Appendix D: Alion SOP-WDE-08-03 - Standard Operating Procedure for Analysis of Uranine-
Tagged Aerosols 36
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List of Figures
Figure 1. Schedule 5
Figure 2. Plan view of aerosol wind tunnel 12
Figure 3. ETV data management system for Alion 20
Figure 4. Organizational chart for the high speed pesticide spray DRT protocol validation 26
List of Tables
Table 1. Data Quality Indicator Goals (DQIGs) 6
Table 2. Quality Control Samples for Low Speed Wind Tunnel Tests 18
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List of Acronyms/Abbreviations
ADQ audit of data quality
ANSI American National Standards Institute
APCT Center Air Pollution Control Technology Center
AS ABE American Society of Agricultural and Biological Engineers
ASAE American Society of Agricultural Engineers (precursor to ASABE)
ASHRAE American Society of Heating, Refrigerating, and Air Conditioning Engineers
ASME American Society of Mechanical Engineers
ASTM ASTM International, formerly American Society for Testing and Materials
ATF aerosol test facility
°C degrees Celsius
cfm cubic feet per minute
cm centimeter
cP centipoise
CV coefficient of variance
DQIG data quality indicator goal
DQO data quality objective
DRT drift reduction technology
Dyo.x droplet diameter (|im) at which 0.x fraction of the spray volume is contained in
smaller droplets
dyne/cm dynes per centimeter
EC emulsifiable concentrates
EPA United States Environmental Protection Agency
ESTE Environmental and Sustainable Technology Evaluations
ETV Environmental Technology Verification
fpm feet per minute
ft foot
gal/acre gallons per acre
gpm gallons per minute
GVP Generic Verification Protocol
HELOS helium neon laser optical system
HETS human exposure test section
HSWT high speed wind tunnel
Hz hertz
in. inches
ISO International Standards Organization
kPa kilopascal
L liter
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Lpm, L/min liters per minute
m meters
mg milligram
min minute
mL milliliter
mm millimeter
mph miles per hour
ms millisecond
m/s meters per second
NTS nonionic surfactant
NIST National Institute of Standards and Technology
uL microliter
um microns
OPP Office of Pesticide Programs
ORD Office of Research and Development
PE performance evaluation
PES performance evaluation system
PMT photo multiplier tube
psi pounds per square inch
QA quality assurance
QC quality control
QM quality manager
QMP quality management plan
QSM quality system manual
RFU relative fluorescence units
RH relative humidity
Rpm revolutions per minute
RTI Research Triangle Institute
s second
SNR signal to noise ratio
SOP standard operating procedure
TSA technical systems audit
USDA-ARS United States Department of Agriculture - Agricultural Research Service
VMD volume median diameter
v/v volume/volume
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A3: Distribution List
U.S. EPA
Michael Kosusko
Paul Groff
RTI International
Jonathan Thornburg, Ph.D.
W. Gary Eaton, Ph.D.
Jenia Tufts
Andrew Dart
Alion Science & Technology
William Ellenson, Ph.D.
Zora Drake-Richman
Paulette Yongue
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Group A: Project Management
A4: Project/Task Organization
The U.S. Environmental Protection Agency (EPA) Office of Research and Development (ORD)
has overall responsibility for the Environmental Technology Verification (ETV) Program and for
the Verification of Pesticide Drift Reduction Technologies project under the Environmental and
Sustainable Technology Evaluations (ESTE) Program. The EPA's Office of Pesticide Programs
(OPP) is a major contributor to the project.
Management and testing of pesticide drift reduction technologies (DRTs) will be performed in
accordance with procedures and protocols defined by a series of Air Pollution Control
Technology (APCT) Center quality management documents. The primary source for the APCT
Center quality system is EPA's Policy and Program Requirements for the Mandatory Agency-
Wide Quality System, EPA Order 5360.1 A2 (May 2000). The quality system that will govern
testing under this plan is in compliance with the following:
• EPA Requirements for Quality Management Plans (EPA Q A/R-2)
• EPA Environmental Technology Verification Program, Quality Management Plan
(EPA ETV QMP), for the overall ETV program
• APCT Center's Verification Testing of Air Pollution Control Technology—Quality
Management Plan (APCT Center QMP)1
• RTF s Draft Generic Verification Protocol for the Verification of Pesticide Spray
Drift Reduction Technologies for Row and Field Crops (GVP)
• Alion Science & Technology Standard Operating Procedures (SOPs)
• This test/quality assurance plan (test/QA plan).
• Appendix A lists full citations for these documents. This test/QA plan is in
conformance with EPA Requirements for Quality Assurance Project Plans (EPA
QA/R-5), EPA Guidance for Quality Assurance Project Plans (EPA QA/G-5), and the
documents listed above.
Alion Science & Technology (Alion) will perform the testing, analyze samples/data collected,
and report and document the data. RTI will use the data to prepare the project reports and
recommend revisions to the GVP. The various QA and management responsibilities are divided
among Alion, RTI, and EPA key project personnel as defined below. The lines of authority
among key personnel for this project are shown on the project organization chart in Figure 4
(Appendix B).
A4.1 Management Responsibilities
Project management responsibilities are divided among the Alion, RTI, and EPA staff as
described below.
1 Each ESTE project is required to have a QMP in place and is allowed to use the QMP of an existing ETV Center.
This project has elected to use the QMP from the APCT Center. The verification organization for DRT verifications
that occur after completion of this ESTE project is anticipated to be the APCT Center and this document reflects that
assumption. This does not preclude other testing organizations from using the protocol.
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A4.1.1 EPA Project Manager
The EPA project manager, Michael Kosusko, has overall technical responsibility for the
program. He is responsible for obtaining final approval of GVPs, test/QA plans, and reports, and
he recommends the resources necessary to meet project objectives and requirements.
A4.1.2 RTI Project Leader
The RTI project leader is Jonathan Thornburg. He has overall responsibility for liaison with the
EPA project manager and technical and administrative oversight of project activities. He
prepared this Test/QA plan and technical questions should be directed to him. He will assign task
leaders and review project documents, as appropriate.
A4.1.3 RTI Task Leader
The RTI task leader is Jenia Tufts. She has overall responsibility for data review and reporting.
She will review the draft report prepared and submitted to RTI by Alion and will prepare the
final report for submission to EPA.
A4.1.4 RTI Test Lead
The RTI test lead is Andrew Dart, who will:
• Review test/QA plans,
• Provide oversight of test site activities.
A4.1.5 Testing Organization Technical Leaders
As manager of all projects in the ATF, William Ellenson will provide general project oversight.
The Alion technical leader is Zora Drake-Richman, who will:
• Assist the RTI project leader with the test scope,
• Review/prepare operating procedures applicable to the testing,
• Review test apparatus and procedures prior to commencement of testing,
• Oversee testing of the pesticide spray DRT systems,
• Review test data/results for attainment of data quality indicator goals (DQIGs) and
reasonableness,
• Initiate corrective actions when needed,
• Review test results,
• Prepare test report, and
• Submit test report to the RTI proj ect leader.
Drake-Richman has overall responsibility for technical and administrative activities, and
exercises technical leadership to promote quality in project performance. She will also function
as liaison to RTI and U.S. EPA in specific technical areas and supervise the activities of project
leaders at Alion.
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A4.2 Quality Assurance Responsibilities
QA responsibilities are divided among the EPA, RTI, and Alion personnel as listed below.
A4.2.1 EPA Quality Manager
The EPA quality manager (EPA QM), Paul Groff, will conduct audits of RTFs QA system and
of specific technical activities on the project. He will be available to resolve any QA issues
relating to performance and EPA's QA requirements. Specific functions and duties of the EPA
QM include approving the contents of this test/QA plan and subsequent revisions and reviewing
QA reports prepared by RTI, including QA evaluations and audits. In addition, the EPA QM
will:
• Communicate quality systems requirements, quality procedures, and quality issues to
the EPA project manager and the RTI project leader,
• Review and approve this test/QA plan specific to Alion,
• Oversee technical systems audits (TSAs) as appropriate,
• Review and approve project test reports, and
• Provide assistance to project personnel in resolving QA issues.
A4.2.2 RTI Quality Manager
The RTI quality manager (RTI QM), W. Gary Eaton, is organizationally independent of the RTI
project leader and is responsible for ensuring that the QA/quality control (QC) procedures
described in this test/QA plan are followed. In addition, Eaton will:
• Maintain regular communication with the EPA QM and RTI project staff regarding
QA issues,
• Report on the adequacy, status, and effectiveness of the QA program on a regular
basis to the RTI project leader,
• Conduct audits of lab activities as necessary and prepare audit reports,
• Ensure that corrective action, if necessary, is properly implemented and documented,
• Review and approve test/QA plans and SOPs,
• Review any TSA reports of Alion testing,
• Review the audit of data quality (ADQ) reports of Alion testing,
• Review and approve test (including QC) reports, and
• Prepare the QA section of the project report.
A4.2.3 Testing Organization Quality Managers
The Alion QM, Paulette Yongue, plays a central role in the introduction, implementation, and
consistent application of continuous quality improvement at Alion. She will fulfill the role as
quality management representative for the department and conduct audits of all pertinent quality
standards to ensure compliance. Yongue will conduct an audit of data quality (ADQ) of a
random selection of 10% of the data for all measured parameters at the end of each verification
test in accordance with the requirements of sections A9.1 and B4.2 of Environmental Technology
Verification Program Quality Management Plan (EPA, 2002a). Yongue will determine if these
measurements allow attainment of the DQOs specified in the GVP and the DQI acceptance
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criteria specified in the test/QA plan. She is organizationally independent of the unit generating
the data. Yongue will:
• Maintain regular communication with the RTI QM and testing staff regarding QA
issues,
• Report on the adequacy, status, and effectiveness of the QA program on a regular
basis to the Alion technical leader,
• Conduct audits of lab activities as necessary and prepare audit reports,
• Ensure that corrective action, if necessary, is properly implemented and documented,
• Review and approve input of the test organization to the test/QA plans and SOPs,
• Review and approve test data, documentation and reports submitted to RTI (including
QC), and
• Provide input to the QA section of the project report.
A5: Problem Definition/Background
In 2007, U.S. EPA completed a draft protocol for the verification of pesticide spray drift
reduction technologies for row and field crops. The Draft Generic Verification Protocol for the
Verification of Pesticide Spray Drift Reduction Technologies for Row and Field Crops
(http://www.epa.gov/etv/pubs/600etv07021.pdf) was developed by U.S. EPA with input and
commentary from stakeholders that included academia, industry, and other government agencies.
Before the pesticide spray DRT protocol can be implemented as an approved protocol for use by
the ETV APCT Center, the draft protocol requires testing and evaluation. This test/QA plan for
low speed wind tunnel testing at the U.S. EPA Aerosol Test Facility describes how the draft
protocol for pesticide spray DRTs verification at low speeds, to simulate ground applications,
will be validated. Once U.S. EPA approves the final report, U.S. EPA, RTI, vendors, test
facilities, and other stakeholders will use the validation report to evaluate the low speed pesticide
spray DRT protocol and suggest changes that will provide improvements.
Pesticide spray drift is defined as the movement of spray droplets through the air at the time of
application or soon thereafter from the target site to any non- or off-target site, excluding
pesticide movements by erosion, migration, volatility, or windblown soil particles after
application. Low speed DRTs include nozzle designs and chemical adjuvants. Low speed is
defined as a speed of the air in the wind tunnel crossing the nozzle representative of ground
application. For this test/QA plan, the pesticide spray DRT protocol will be validated only for
nozzle designs. Validation of the protocol through spray liquid formulation modifications to the
viscosity, surface tension or other characteristics will not be conducted.
A6: Project/Task Description
A6.1 Description
This test/QA plan describes the test and QA procedures that will validate the Generic
Verification Protocol for the Verification of Pesticide Spray Drift Reduction Technologies for
Row and Field Crops for spray nozzles in a low speed wind tunnel. This test/QA plan is written
to conform to all specifications of EPA Requirements for Quality Assurance Project Plans, EPA
QA/R-5, the EPA ETV QMP, and the ETV APCT Center QMP. It describes the quality system
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required of Alion and the procedures applicable to meeting EPA quality requirements that are
common to all ETV tests. This document will be reviewed and approved by EPA prior to testing.
This testing will gather information and data for evaluating the applicability of the pesticide
spray DRT protocol for successfully testing commercially ready pesticide spray DRT nozzles
that will be used for ground spraying applications. All low speed tests will be conducted in the
U.S. EPA Aerosol Test Facility located at the U.S. EPA research facility in Research Triangle
Park, NC. Alion is an on-site support contractor to U.S. EPA charged with operating and
maintaining the Aerosol Test Facility. Alion, under a subcontract with RTI, will operate the low
speed wind tunnel. The specific operating conditions used during the testing will be documented
as part of the testing process. Table 1 in element A7 presents a summary of measurements that
will be made to evaluate the performance of the DRT and document the test conditions.
Two candidate nozzles and a reference nozzle will be tested using the pesticide spray DRT
protocol. The AI-11003 VS nozzle (Teejet Technologies, Wheaton, IL) is one candidate nozzle
to be tested. This air eduction nozzle will produce a "very coarse" spray, as defined by ASAE
S572 (1999), at the operating conditions defined in element Bl. This nozzle is used extensively
by industry and its performance characteristics have been extensively studied. The ULD 120-04
nozzle (Hypropumps, New York, NY) is the second candidate nozzle to be tested. This dual air
eduction nozzle also is extensively used by industry. The ULD 120-04 nozzle will produce a
"coarse" spray at the operating conditions defined in element Bl. The characteristics of the
reference nozzle to be used during the testing are specified in element Bl. USDA-ARS will
provide the reference nozzle for the LSWT tests.
A report containing results of the pesticide spray DRT protocol validation tests will be prepared
by Alion; see element BIO.2. RTI will review and approve the report before submittal of the
entire data package to U.S. EPA.
A6.2 Schedule
Figure 1 shows the schedule for completion of the high speed wind tunnel pesticide spray DRT
protocol validation. Testing was completed May 18-July 2, 2009.
Item
1
2
O
4
5
6
Milestone
Test/QA Plan - Submission to EPA for Approval
Test/QA Plan - Review Comments
Final, Revised, Approved Test/QA Plan
Testing
Report - Draft to RTI
Final Report to EPA
By Whom?
RTI
EPA
RTI
Alion
Alion
RTI
Schedule
May 5, 2009
May 12, 2009
May 18, 2009
May 18-July 2, 2009
July 15, 2009
August 3 1,2009
Figure 1. Schedule
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A7: Quality Objectives and Criteria
The DQOs of this testing focuses on the direct and indirect measurements of spray drift
deposition using wind tunnel testing. For low speed wind tunnel testing, the primary products of
this test design will be the measurement of droplet size distribution and flux volume.
Droplet size distribution measurements will consist of 32 or more droplet size bins measured at
seven heights at a distance of 2 m from the nozzle. The degree of consistency of volume median
diameter (VMD), droplet diameter (jim) at which 10% of the spray volume is contained in
smaller droplets (Dvo.i) and droplet diameter (|im) at which 90% of the spray volume is
contained in smaller droplets (Dvo.9) are used as a measure of data quality. Variation of less than
± 7% is considered acceptable.
Flux volume measurements will be collected using monofilament lines mounted at seven heights
equally spaced between the floor and the nozzle, at a distance of 2 m from the nozzle. The flux at
the highest measurement height must be less than 1% of the cumulative flux measurements from
lower heights. If the amount of spray measured at the highest height exceeds 1% of the total
volume measured at the lower heights, additional measurements at additional heights must be
made.
Secondary measurements to be collected during testing include spray material conditions (flow,
pressure, temperature, etc.), wind tunnel air speed, and ambient environmental conditions. These
measurements may provide explanations if the droplet size distribution or flux measurement data
quality indicators are not achieved. This information may also be used for other potential
revisions to the pesticide spray DRT protocol.
The DQIG for individual measurements will conform to those specified in relevant sections of
the test protocols and referenced procedures, as shown in Table 1. The DQO for this testing is to
meet the Table 1 DQIGs or obtain sufficient information to revise the DQIGs in the final
protocol. If one or more DQIGs are not achieved during a protocol validation test, Thornburg
and Drake-Richman will jointly decide whether additional tests should be conducted or whether
sufficient information was gathered to revise the DQIGs.
Table 1. Data Quality Indicator Goals (DQIGs)
Parameter
Standard Operating
Procedure
(if applicable)
Acceptance Criteria
Droplet Size Distribution Measurement DQIGs
Spray volume in largest and
smallest droplet size class bands
in laser diffraction
measurements
Number of size class bands for
reported data
USDA SOP-4.4
USDA SOP-4.4
< 1% of total volume in each case (i.e., < 2% total of
the spray volume) to be achieved through selection of
appropriate lens and instrument configuration for the
dynamic size range of the spray being sampled
> 32
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Parameter
Standard deviation around mean
Dv0.5 for three replicate droplet
size measurements
Measured volume median
diameter (VMD), DvCU and Dv0.9
(i.e., the droplet diameter
bounding the upper and lower
10% fractions of the spray)
Obscuration for spray
measurements across a spray
diameter (for laser diffraction
systems)
Minimum obscuration for
sampling to achieve cross-
section average spray (e.g., start
and end trigger using traverse
with laser diffraction systems)
Sample size per replicate
measurement
Diode suppression (laser
diffraction systems)
Spray nozzle height
measurement
Nozzle spray angle
Spray liquid pressure (nozzle
operating pressure)
Spray liquid temperature
Spray liquid flow rate
Dynamic surface tension of
spray liquid
Viscosity of spray liquid
Wind tunnel ambient air
temperature
Standard Operating
Procedure
(if applicable)
USDA SOP-4.4
USDA SOP-4.4
USDA SOP-4.4
USDA SOP-4.4
USDA SOP-4.4
n/a
n/a
n/a
ASAE S572
ASHRAE Standard 4 1.1
ASAE S572
RTI CAT:46
RTI CAT:47
ASHRAE Standard 4 1.1
Acceptance Criteria
Vary by less than ± 3% for replicate measurements
with the same nozzle
Vary by less than ± 7% for replicate measurements
with the same nozzle
< 60% unless corrected for multiple scattering,
whereupon the report shall include the measured
obscuration, the algorithm used to correct for
multiple scattering, and the manufacturer-stated
limits of applicability for that algorithm.
2%
> 10,000 droplets for particle counting instruments or
> 5 s for laser diffraction instruments
Diodes may not be suppressed (no channels may be
killed) in sampling. Correct selection of focal length
lens, system alignment, avoidance of vibrations, and
cleanliness of optical surfaces should prevent the
need for diode suppression (data loss). (If the laser is
displaced during sampling, all diodes will measure
incorrect scattering angles. Diode suppression is not
an appropriate solution to such sampling problems.)
Within 5 mm (without airflow)
Variation within ± 5% during test.
±0.5 psi of values specified in the ASAE standard
for reference and evaluation nozzles.
Measured within 0. 1 °C
± 0.04 L/min of values specified in the ASAE
standard for reference and evaluation nozzles.
52 ± 4 dynes/cm at surface lifetime age of 10 to 20
ms for test fluids with adjuvants. 70 ± 4 dynes/cm for
water, if used as test fluid.
1.1 ±0.1 cPat20°C
Measured within 0.1 °C.
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Parameter
Wind tunnel wet bulb/dew point
temperature or percent relative
humidity
Percent relative humidity (low
speed wind tunnel)
Relative spray material and air
temperatures
Air speed inside wind tunnel
Sampling rate for air speed
Standard Operating
Procedure
(if applicable)
ASHRAE Standard 4 1.1
ISO 22856
USDA SOP-4.4
USDA SOP-4.4
ASAES561.1
Acceptance Criteria
Measured within ± 0. 1 °C or ± 1%, respectively.
80% ± 5%
Spray material temperature must be within 2 °C of
the air temperature to avoid atomization anomalies.
1 m/s measured accuracy within 0. 1 m/s, close to
nozzle location (with nozzle absent).
Sampling over a measuring period of 10 s
Drift Potential Measurement DQIGs
Spray duration for replicate
measurements
Spray duration for similar
nozzle types
Solvent volume for extraction of
tracer, if using collectors
Air speed inside wind tunnel
Sampling rate for air speed
Wind speed consistency in wind
tunnel working section
Wind tunnel working section
width
Wind tunnel turbulence
Wind tunnel ambient air
temperature
Wind tunnel wet bulb/dew point
temperature or percent relative
humidity
Percent relative humidity (low
speed wind tunnel)
n/a
n/a
n/a
USDA SOP-4.4
ASAES561.1
ISO 22856
ISO 22856
ISO 22856
ASHRAE Standard 4 1.1
ASHRAE Standard 4 1.1
ISO 22856
Minimum spray time of 5 s for each replicate
measurement should be used, to allow stability of
spray formation and to avoid under- or over-dosing
of samplers or collectors. (Appropriate spray
duration should be verified prior to measurement).
Replicate measurements for a nozzle type should be
within ± 5% of mean time duration for a given setup.
Similar nozzle types from different
vendors/manufacturers should be tested for similar
time duration, within ± 5%.
Within 5% of volume required for analytical
recovery and assessments (i.e., all collectors should
be washed with the same volume of solvent within
5% of the target volume, as described in sections
B2.2andB2.3)
1 m/s measured accuracy within 0. 1 m/s, close to
nozzle location (with nozzle absent).
Sampling should occur over measuring period of 10 s
<5%
Minimum to avoid boundary layer and blockage
effects.
<8%
Measured within 0.1 °C.
Measured within ± 0. 1 °C or ± 1%, respectively.
80% ± 5%
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Parameter
Relative spray material and air
temperatures
Standard Operating
Procedure
(if applicable)
USDA SOP-4.4
Acceptance Criteria
Spray material temperature must be within 2 °C of
the air temperature to avoid atomization anomalies.
n/a = not applicable
Standards Cited
ANSI/ASHRAE 41.1 (1986) Standard Method for Temperature Measurement., American Society
of Heating, Refrigerating and Air Conditioning Engineers, Inc. 1791 Tullie Circle, NE, Atlanta,
GA 30329.
ASAE S572 (1999) (sometimes referred to as AS ABE S572) Spray Nozzle Classification by
Droplet Spectra. Standard No. S572, American Society of Agricultural and Biological
Engineers, St. Joseph, MI.
ASAE S561.1 Procedure for Measuring Drift Deposits from Ground, Orchard and Aerial
Sprayers. American Society of Agricultural and Biological Engineers, St. Joseph, MI.
ISO Draft Standard 22856: Equipment for Crop Protection - Laboratory Drift Methods
Measurements. International Standards Organization.
A8: Special Training/Certifications
All Alion personnel associated with this program must have completed the training required by
the U.S. EPA ORD SHEM office. This training encompasses general laboratory safety and laser
safety. Training specific for spray drift reduction technology evaluation includes wind tunnel
operation, laser-diffraction instrument operation, and data handling procedures. The Alion test
leader will ensure that all persons assigned to the wind tunnel team have appropriate training and
are fully capable of performing the tasks assigned to them. Each team member will be
thoroughly familiar with this test/QA plan, the measurement equipment, procedures, and
methods for their assigned jobs.
A9: Documentation and Records
All information associated with data collection during a test will be recorded either in a
laboratory notebook or electronically. Test data will be recorded legibly in a laboratory notebook
in permanent ink and initialed and dated by the person making the entry. At a minimum, the test
data recorded will include information specified in Table 1 that is not recorded electronically. In
accordance with Part A, sections 5.1 and 5.3 of EPA's QMP, Alion will return all test-specific
documentation and records to RTI upon completion of the tests. RTI will retain all data and
reports for seven years after completion of the project, copies of all data and reports will be
provided to Mike Kosusko, EPA, for submission to OPP for storage. Archived raw data,
documents, and electronic files will be easily accessible.
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Group B: Data Generation and Acquisition
for Low Speed Wind Tunnel Tests
Bl: Sampling Process Design (Experimental Design)
All measurements described in this section of the test/QA plan will be conducted by Alion in the
human exposure test section (HETS) of the wind tunnel at the U.S. EPA Aerosol Test Facility
(ATF) in Research Triangle Park, NC. The FIETS is used for low speed work.
The measure of performance for the DRT for low speed wind tunnels will be derived from
airborne droplet size distribution and flux. These values will be used by EPA to model deposition
from 0 to 200 ft downwind of the nozzle. The basic experimental design will consist of two
separate sets of experiments to characterize the two critical measurements of the verification:
size distribution and flux volume. First, the droplet size spectrum will be measured at multiple
heights 2 m downwind with the DRT operating at specified spray pressure, air speed, nozzle
orientation, nozzle height, and environmental conditions. A separate series of experiments will
measure the flux volume at multiple heights 2 m downwind of the nozzle under identical spray
liquid and environmental conditions. For both series of tests, wind tunnel conditions and spray
parameters are important measurements for establishing the bounds of the verification test
design.
Two candidate nozzles and a reference nozzle will be tested using the pesticide spray DRT
protocol. The AI-11003 VS nozzle (Teejet Technologies, Wheaton, IL) and the ULD 120-04
nozzle (Hypropumps, New York, NY) are the candidate nozzles to be tested. Both test nozzles
will be operated at 300 kPa (43.5 psi). The AI-110 flow is 1.13 L/min (0.3 gpm). The ULD 120-
04 flow is 1.51 L/min (0.4 gpm).The reference nozzle will be one of the five ASAE S572 nozzles
associated with the size classification boundary selected as described in section B2.4. All
reference nozzles are a 110° flat-fan operated at 300 kPa (43.5 psi) and 1.18 L/min (0.31 gpm).
A single nozzle of each type will be tested at a time. Each nozzle will be oriented so the spray is
directed towards the floor and perpendicular to the direction of the airflow. The nozzle height
above the floor (virtual floor) will be 60 cm.
Spray size distribution and flux measurements for each nozzle will be collected at a single wind
speed and a single spray formulation. The wind speed inside the HETS section of the tunnel will
be 1 m/s. The spray solution for all nozzles will be a deionized water solution containing a
0.25% volume/volume (v/v) of a 90% nonionic surfactant (R-900, Wilbur-Ellis Company, San
Antonio, TX).
To meet the DQOs, three replications will be used for each set of experimental conditions
defined in sections B2.4 to B2.6. As required by the DQOs in element A7, the product of this
test design will be the measurement of a droplet size distribution and flux volume. The DQIGs
for appropriate parameters identified in sections 1 and 2 of Table 1 must be met. Additional
tests will be conducted as needed to meet the DQIGs.
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B2: Sampling Methods for Measurement of Droplet Size, Deposition Flux, and Test
Conditions
The sampling system is comprised of the aerosol wind tunnel (AWT) at the U.S. EPA ATF in
Research Triangle Park, NC (Figure 2). The AWT system can produce a wide range of air
velocities, particle sizes, and aerosol loadings with controlled temperature and humidity. In plan
view, the AWT is rectangular in shape with outside dimensions of approximately 66 ft by 46 ft
(see Figure 2). Flow through the recirculating AWT during all operations is counterclockwise.
The graphic of the tunnel shows two test sections: the human exposure test section (HETS) and
the sampler test section (STS). The HETS will be used for this series of experiments. The HETS
has a cross-section 12 ft wide, 10 ft high, and 30 ft long, and the STS has a cross-section 5.75 ft
wide, 4.75 ft high, and 20 ft long. The wind speed in the HETS can be varied from 0.1 to 1 m/s
(0.36 to 3.6 km/h) while the STS can range from 0.56 to 13.3 m/s (2 to 48 km/h).
Since the AWT is of fixed geometry, varying wind speeds are achieved by controlling the
volumetric flow rate. Major flow through the AWT is provided by a Twin City direct-drive,
adjustable blade and vane axial fan capable of providing approximately 2002 m3/min (71,500
firVmin) against 0.97 kPa (3.89 in. of water) pressure drop at 1133 rpm at a power requirement of
56 kW (75 hp). This blower is capable of driving the AWT at speeds up to 48 km/h (30 mph) in
the STS.
Because operation of the AWT releases heat to the re-circulating airstream, a cooling coil/chilled
water system is used to control the tunnel temperature. Controlled recirculation of chilled water
through the cooling coil counteracts the continued heat input and allows the AWT to be operated
at specified temperatures.
The AWT includes a bank of high-capacity, mini-pleated filters downstream of the test section to
remove aerosols not collected by the samplers. This primary filter bank effectively prevents the
continuous accumulation of material in the tunnel interior, dramatically reducing the background
level of the fluorescent material in the airstream.
B2.1 Sampling Locations
Spray size distribution measurements will be collected at the nozzle and 2 m downwind of the
nozzle. Measurements will occur across a representative cross-sectional sample of the spray.
Spray size distribution measurements for reference nozzle selection will be taken 60 cm
downwind to allow for complete atomization of ligaments and secondary break up of droplets in
the air stream without having the spray contact the wind tunnel surfaces. Spray size distribution
measurements 2 m downwind of the nozzle will be collected at seven heights, equally spaced at
10 cm increments starting at 10 cm above the wind tunnel floor.
Spray flux for drift potential will occur 2 m downwind of the nozzle at the same seven heights
used for the spray size distribution measurements.
Deposition measurements will be collected along the spray plume centerline at 5 distances from
the spray nozzle. Deposition cards will be located at 2, 3, 4, and 5 m, and 6 m from the nozzle.
Auxiliary measurements include wind tunnel operating conditions and spray liquid
characteristics. Measurement of air temperature and humidity will occur upwind of the nozzle.
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Air speed will be measured 7 m downwind of the nozzle at the nozzle height (60 cm). Air speed
measurement closer to the nozzle is not possible because the size of the anemometer available
for the measurements will induce turbulence that may impact the spray plume characteristics.
Spray liquid temperature will be measured in the reservoir tank. Spray pressure will be measured
immediately upstream of the nozzle. Spray liquid flow rate will be measured by collecting the
spray at the nozzle after the correct pressure is set.
B2.2 Wind Tunnel Measurement of Spray Drift: Flux Volume
The specific steps to be performed during an experiment for determining spray flux volume 2 m
from the nozzle are described below.
1. The spraying system will be suspended from a boom within the wind tunnel. The boom
is situated to minimize effects on airflow. The test nozzle will be positioned at the
specified height, oriented downward toward the floor. The angle of discharge will be
confirmed with a protractor and recorded.
2. The test spray nozzle(s) will be mounted at a defined height not less than 600 mm
above the wind tunnel floor and not greater than a height 100 mm below the wind
tunnel ceiling. Nozzles must be positioned in a place free from edge effects.
3. The spraying system will be primed with spray prior to measurements to ensure that
rinsing liquid is removed from the line and the liquid discharging from the nozzle is
the actual intended tank mix. The spray nozzles will be "run-in" for 5 min to ensure
removal of machining burrs or plastic mold residue.
4. For these experiments, uranine will be the fluorescent tracer added to the spray liquid
described in section Bl for easy detection of droplet deposition on the monofilament
lines. The minimum uranine concentration will be 13.6 g per gallon (3.6 g per L) of the
spray liquid.
5. Spray material conditions will be measured once per test. Flow rate will be measured
at the specified operating pressure by collecting the spray from the nozzle into a glass,
class A, graduated cylinder over a time of 10 s. Spray pressure will be measured using
a calibrated pressure gauge with 0.5 psi sensitivity.
6. The wind tunnel floor will be covered with an artificial turf surface to minimize droplet
bounce and mimic stubble vegetation for field conditions.
7. Air speed in the wind tunnel will be 1 m/s ±0.1 m/s, as measured with a CSAT3 sonic
anemometer (Campbell Scientific). The minimum data collection rate will be one
measurement per 30s.
8. To minimize evaporation effects, the relative humidity in the working section of the
wind tunnel at the time of measurements will be at least 80 ± 5%. Temperature inside
the wind tunnel will be measured at the same location. Temperature and relative
humidity are determined using a HMT 330 probe (Vaisala).
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9. Monofilament line approximately 2 mm in diameter will be used as sample collectors.
These will be extended horizontally across the wind tunnel at seven heights starting at
10 cm above the floor and spaced in 10 cm increments. Each end of the monofilament
line will be supported in enclosed boxes within the AWT to prevent contamination of
the unused portion of sampling line.
10. Spray duration for an experiment will be 10 ± 0.5 s.
11. Immediately after an experiment, the exposed monofilament line will be collected into
a labeled plastic bag. 30 mL of O.OlNNaOH will be added to the bag to dissolve the
uranine into solution. The bag contents will be shaken for 10s before an aliquot of the
liquid is removed for fluorometric analysis (section B4).
12. A 100 mL sample of spray liquid will be collected directly from the spray tank
reservoir for viscosity and surface tension analysis, as described in section B4.
B2.3 Wind Tunnel Measurement of Spray Drift: Deposition
Spray drop deposition at multiple horizontal distances from the nozzle will be collected
simultaneously with the spray flux volume samples. Deposition sampling onto mylar cards will
be used to measure horizontal deposition within the wind tunnel (see element B2.5).
1. Test conditions described in section B2.2 will be followed in addition to the conditions
specific to deposition measurements, specified below.
2. Deposition samples will be collected on 10 cm by 10 cm (100 cm ) mylar cards (GE
Healthcare Biosciences, VWR part # 95017-735).
3. Mylar cards will be placed directly downwind from the nozzle aligned with the plume
centerline on metal support stands located 2, 3, 4, 5 and 6 m downwind of the nozzle.
The cards will be at a height of 0.1 m above the wind tunnel floor to avoid boundary
layer effects.
4. Immediately after an experiment, the exposed mylar cards will be collected and placed
in a labeled plastic bag. 30 mL of 0.01N NaOH will be added to the bag to dissolve the
uranine into solution. The bag contents will be shaken for 10 s before an aliquot of the
liquid is removed for fluorometric analysis (section B4).
B2.4 Wind Tunnel Measurement of Spray Drift: Spray Size Distribution
Separate experiments from those described in sections B2.2 and B2.3 will be conducted to
measure the spray size distribution 2 m from the nozzle. Separate experiments are required
because the wind tunnel is not configured to allow simultaneous measurement of spray flux
volume, deposition, and size distribution. The experimental procedure to collect the size
distribution data is described below.
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1. Droplet size distribution will be measured with a Sympatec HELOS laser diffraction
system (Sympatec Inc., Lawrenceville NJ). Instrument model number, serial number,
scale range, software version number, and calibration verification will be recorded.
2. For each height, the sampling system will be configured to measure the entire dynamic
size range of the instrument with less than 2% total of the spray volume contained in
the uppermost or lowermost size classes.
3. The spraying system will be suspended from a boom within the wind tunnel. The boom
will be situated to minimize effects on airflow.
4. The test spray nozzle(s) will be mounted at a defined height not less than of 60 cm
above the wind tunnel floor and not greater than a height 10 cm below the wind tunnel
ceiling and oriented toward the floor. The angle of discharge will be confirmed with a
protractor and recorded. Nozzles must be positioned in a place free from edge effects.
5. The spraying system will be primed with spray prior to measurements to ensure that
rinsing liquid is removed from the line and the liquid discharging from the nozzle is
the actual intended tank mix. The spray nozzles will be "run-in" for 5 min to ensure
removal of machining burrs or plastic mold residue.
6. For these experiments, spray liquid will be the same as described in section B2.2 to
provide consistency between the spray flux and size distribution measurements.
7. Spray material conditions will be measured once per test. Flow rate will be measured
at the specified operating pressure by collecting the spray from the nozzle into a glass,
class A, graduated cylinder over a time of 30 s. Spray pressure will be measured using
a calibrated pressure gauge with 0.5 psi sensitivity.
8. The wind tunnel floor will be covered with an artificial turf surface to minimize droplet
bounce and mimic stubble vegetation for field conditions.
9. Air speed in the wind tunnel will be 1 m/s ±0.1 m/s, as measured with a CSAT3 sonic
anemometer (Campbell Scientific). The minimum data collection rate will be one
measurement per 30s.
10. To minimize evaporation effects, the relative humidity in the working section of the
wind tunnel at the time of measurements will be 80 ± 5%. Temperature (± 0.1 °C) and
relative humidity (± 1%) inside the wind tunnel will be measured at the same location
downwind of the experimental setup using an HMT 330 probe (Vaisala).
11. Spray duration for an experiment will be 10 ± 0.5 s.
12 A 100 mL sample of spray liquid will be collected directly from the spray tank
reservoir for viscosity and surface tension analysis, as described in section B4.
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B2.5 Measurement of Droplet Size Spectrum near the Nozzle (Determination of
appropriate reference test system)
These tests will determine the appropriate reference nozzle for comparison with the test nozzles
during the tests described in sections B2.2, B2.3 and B2.4.
Spray size distributions of candidate test nozzles are compared to a reference spray system based
on the ASAE S572 standard for droplet size. Before drift potential measurements are conducted,
the candidate test nozzle is categorized into droplet size category for very fine, fine, medium,
coarse, very coarse, and extremely coarse using ASAE S572. The reference nozzle selected for
the spray drift experiments will be the ASAE S572 reference nozzle associated with the lower
(coarser) boundary of the droplet size category in which the candidate test nozzle falls.
Using the methodology described in USD A SOP-4.4, the spray size distribution produced by the
five reference nozzles that define the boundary curves in ASAE S572 and the test nozzles will be
measured. The standard spray reference solution consisting of distilled water and a 0.25%
volume/volume (v/v) of a 90% nonionic surfactant (R-900, Wilbur-Ellis Company, San Antonio,
TX) will be used. Three replicate measurements of size distribution will be collected for each
nozzle to satisfy the DQIGs. Additional requirements for the size distribution measurements are
listed below.
1. Droplet size spectra for spray drift tests are made under the same conditions (e.g.,
spray material, spray pressure, nozzle settings) and following the same procedures
outlined in element B2.4 except the measurements will be made with wind speed set at
Om/s.
2. Droplet size will be measured using the same laser diffraction measurement system
used for section B2.4. The instruments and apparatus used in the test will be listed.
Names, model numbers, serial numbers, scale ranges, software version number, and
calibration verification shall be recorded.
3. A representative cross-section average sample will be obtained, using a mass-weighted
traverse or multiple chordal measurements of the full spray (or half spray for axi-
symmetric spray plumes).
4. Spray size distribution will be measured 60 cm below the nozzle. This distance allows
sufficient time for complete spray atomization into droplets. The minimum traverse
distance will be 84 cm.
5. The sampling system will be configured to measure over the entire dynamic size range
of the Sympatec HELOS with less than 2% total of the spray volume contained in the
uppermost and lowermost size classes.
6. The droplet size measurements will include assessment of the droplet size category of
the candidate test system and reference system according to ASAE S572.
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B3: Sample Handling and Custody Requirements
Monofilament line samples and horizontal deposition samples require manual handling. Prior to
use, each horizontal sampler and monofilament line will be stamped with a unique identification
number or other numbering system to identify test type, test run, and position. A plastic bag, for
storage after the experiment, will also be labeled with the unique identification number. All
samples will be placed inside an opaque storage container or kept in a dark environment to
prevent ultraviolet degradation of the tracer prior to fluorometric analysis.
Wind tunnel operating conditions measurements will be collected and recorded by the computer-
controlled data systems associated with the wind tunnel.
B4: Analytical Methods
Measurement of deposited material will occur by extracting the fluorescent tracer from the
horizontal samplers and monofilament lines followed by quantification of tracer in the extract.
All samples will be extracted with 30 mL of 0.01 N NaOH. The relative fluorescence in a 5 mL
aliquot of the extract will be measured using a Turner digital fluorometer (Thermo Scientific)
using Alion SOP-WDE-08-02 and SOP-WDE-08-03. The fluorometer uses a 12 x 75 mm round
cuvette. A narrow band (NB360) excitation filter and emission filter (NB460) will be used. A
calibration curve linking fluorescence units to mass of fluorescent material will be generated for
each batch of 50 samples. The curve will span the detection range of the fluorometer and
demonstrate linearity in the instrumentation response as a function of mass deposited. From this
curve, fluorescent tracer measurements will be converted to the fraction of spray liquid applied.
Spray liquid viscosity and surface tension will be measured. A GV-2100 falling ball viscometer
(Gilmont Corp., Barrington, IL) will measure the spray liquid viscosity following ASTM Method
D445-06. A DuNuoy ring tensiometer (CSC Scientific, Fairfax, VA) will measure the surface
tension of the spray liquid following ASTM Method D1331.
B5: Quality Control
Quality control samples will be collected to ensure the desired accuracy and precision of the
fluorometric measurements are maintained. The types and quantities of quality control samples
are described in Table 2.
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Table 2. Quality Control Samples for Low Speed Wind Tunnel Tests.
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Sample
Description
Acceptance Criteria
Spiked monofilament line
A monofilament line will be spiked with a
known quantity of fluorescent tracer to
quantify the extraction efficiency of the 30
mLO.OlNNaOHwash.
> 93% recovery of fluorescent tracer
Spiked mylar card
A mylar card will be spiked with a known
quantity of fluorescent tracer to quantify the
extraction efficiency of the 30 mL 0.0 IN
NaOH wash.
> 93% recovery of fluorescent tracer
Duplicate mylar cards
A duplicate mylar card will be positioned at a
selected distance from the nozzle. 5% of the
samples collected will be duplicate cards.
< ± 10% variation in the
measurements
Blank monofilament line
New monofilament line will be handled as
experiment blanks to monitor for background
fluorescence. 5% of the samples collected
will be monofilament line blanks.
Acceptable fluorescence will be less
than three times the minimum
detection limit of the fluorometer,
which will be determined during
analysis. Otherwise, a correction
factor will be applied to the
fluorescence data.
Blank mylar cards
Clean mylar cards will be used as experiment
blanks to monitor for background
fluorescence. 5% of the samples collected
will be mylar card blanks.
Acceptable fluorescence will be less
than three times the minimum
detection limit of the fluorometer.
Otherwise, a correction factor will be
applied to the fluorescence data.
Blank spray liquid
Three samples of the spray liquid without
uranine will be analyzed fluorometrically to
determine any background fluorescence.
Acceptable fluorescence will be less
than three times the minimum
detection limit of the fluorometer.
B6: Instrument/Equipment Testing, Inspection, and Maintenance
Wind tunnel temperature and relative humidity will be measured using HMT 330 (Vaisala)
probes. The airspeed will be measured using CSAT3 sonic anemometer (Campbell Scientific).
Manufacturer's specified procedures for calibration and maintenance of these instruments will be
followed; calibration results will be documented in the project notebook.
B7: Instrument/Equipment Calibration and Frequency
The Sympatec HELOS System will be calibrated and certified by Sympatec-provided technicians
on a yearly basis. A copy of this calibration procedure and all appropriate documents will be
kept in the Sympatec Operator's Manual. The calibration procedure follows ASTM Standard
Test Method E 1458 "Test Method for Calibration Verification of Laser Diffraction Particle
Sizing Instruments using Photomask Reticles."
Calibration of all other instrumentation will be current and documented.
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B8: Inspection/Acceptance of Supplies and Consumables
Inspection and acceptance criteria for vendor-supplied or Alion purchased materials and
equipment are coordinated by the Alion technical leader.
The primary supplies and consumables for this exercise consist of the horizontal samplers,
monofilament lines, and spray liquid materials. Prior to labeling, each sampler will be visually
inspected and discarded if any damage is found. The uranine tracer is stable and nonvolatile and
the tracer concentration in the spray liquid will allow for adequate sensitivity to measure
deposition at all test distances.
B9: Non-Direct Measurements
All data used in this project will be generated by this project. No non-measurement sources,
such as computer databases, programs, literature files, and historical databases, will be used.
BIO: Data Management
B10.1 Data Acquisition and Management
Data acquisition and data management will be performed according to USD A SOP-4.4 and 4.5.
The planned data streams, with responsibilities of the Alion technical leader and Alion QM, are
depicted in Figure 3. The Alion technical leader is operationally responsible for all aspects of a
test. The Alion QM is operationally responsible for all data quality aspects of a test, with
primary focus, but not exclusive focus, on the areas indicated in the figure. Alion will conduct a
QA analysis and review and develop the data report for submission to RTI. RTI will also
conduct a QA analysis and review and develop the final test report for submission to EPA.
These data steps are described schematically in Figure 3, and this flow chart includes all data
activities from the initial pretest QA steps to the passing of the data to EPA.
The spray droplet size distribution, spray flux, spray deposition, and wind tunnel operating
conditions are captured by the data management system. Alion will collect and assemble the
data and conduct calculations and data analysis.
Spray flux and deposition are calculated from the output of the fluorometric analysis, the number
of relative fluorescence units (RFU) per mL of fluid. Equation (1) shows the formula for
conversion of the RFU per mL to the fraction of spray liquid deposited on the monofilament line
or mylar card.
„ ,. (FMV] n.
Fraction = —, r^ (1)
(Qtc]
Where F is the fluorescence per mL reported by the fluorometer, Mis the number of grams of
uranine per RFU determined by the calibration curve, Fis the volume of extraction fluid, Q is
the spray material flow rate, t is the spray time, and C is the uranine concentration in the spray
liquid.
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Oversight
: Test Oversight and Data Production
Data Flow
DRT Information from
Manufacturer/Vendor
Sampling Data and
Instrument Data
QC Data
Assemble Data
Zora Drake-Richman
Calculations & Data Analysis
Zora Drake-Richman
QA Review
Paulette Yongue
Report
Zora Drake-Richman
Data Flow •
Figure 3. ETV data management system for Alion.
B10.2 Reporting
The data report shall be sufficiently detailed with background information to allow complete
description of the testing in the report. The final test report, which will be prepared by Jenia
Tufts, RTI, includes a results summary and a detailed discussion of the testing. An outline of the
test report is provided in the GVP, element E. 1, and the report will include each of the elements
listed. The description of the testing will be based on the data report. The following is an
outline of the test report:
• Executive summary
- DRT manufacturer/vendor information
- Summary of the test program including testing location and type (LSWT)
- Results of the test
- Droplet size classification, using ASAE S572.
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- Any limitations of the results
- Brief QA statement
• Introduction
• Description and identification of the DRT
• Procedures and methods used in testing
- The instruments and measurement apparatus used for droplet size measurement
(including name and type, model number, serial number, scale ranges, software
version number, and date of most recent calibration verification)
- Spray flux and deposition sampling (including description of monofilament lines,
size and type of horizontal samplers, placement of monofilament lines and mylar
samplers, and photographs of sampler locations for collection)
• Statement of operating range and testing conditions over which the tests were
conducted including:
- Nozzle orifice height
- Spray pressure at nozzle
- Volume/unit time produced by nozzle
- Test spray material composition
- Source of spray materials (including water)
- Sampling locations
- Temperature
- Humidity
- Wind speed - wind tunnel testing only
- Flight speed or ground equipment speed - field testing only
- Wind speed/direction - field testing only
- Atmospheric stability (Pascal) - field testing only
- Results of the ASAE S572 droplet size measurement
• Summary and discussion of results
- Discussion of test results
- Deviations and explanations from test plan
- Discussion of QA and QA statement
• References
• Appendices
- QA/QC activities and results
- Raw test data
- Equipment calibration results
- Sample handling
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Group C: Assessments and Oversight Elements
Cl: Assessments and Response Actions
Cl.l Internal Audits
Internal audits conducted by Alion will conform to element Cl (Assessments and Response
Actions) and C2 (Reports to Management) of EPA QA/R-5.
C1.2 Audits of Data Quality
In accordance with Table 9.1 of the EPA ETV QMP, the Alion QM will conduct an audit of data
quality (ADQ) of at least 10% of all test data collected during testing. The ADQ will be
conducted in accordance with EPA's Guidance on Technical Audits and Related Assessments for
Environmental Data Operations, EPA QA/G-7, including:
• a study of data transfer and intermediate calculations,
• a review of QA and QC data, including reconciliation to user requirements (e.g.,
DQOs and DQIGs), and
• a study of project incidents that resulted in lost data, and a review of study statistics.
The Alion ADQ report will end with conclusions about the quality of the data from the project
and their fitness for their intended use.
C1.3 External Audits
Alion will cooperate with any external assessments by the EPA or RTI. RTI or EPA will
conduct a single technical systems assessment of Alion during the test. The external assessments
will be conducted as described in EPA QA/G-7.
C1.4 Corrective Action
Corrective action to any audit or assessment at Alion will conform to required elements B5
(Quality Control) and Cl (Assessments and Response Actions) of EPA QA/R-5. Actions taken
will be documented.
C2: Reports to Management
Internal assessment reports will be reviewed by the Alion QM, who will respond as noted in
element Cl of EPA QA/R-5. The written report of the ADQ will be submitted for review as
noted in element C1.2 of this test/QA plan.
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Group D: Data Validation and Usability Elements
Dl: Data Review, Verification, and Validation
The Alion QM reviews and validates the data and the draft data report using the site-specific
test/QA Plan, test methods, general SOPs, and project-specific SOPs. Data review and
validation will primarily occur at the following stages:
• On the Alion test site following each test run by Alion technical leader
• On the Alion test site following completion of the test program by technical leader
• Before writing the draft data report
• During QA review of the draft report and audit of the data quality
• The criteria used to review and validate the data will be the QA/QC criteria specified
in each test procedure, protocol, guideline, or method (see Table 1) and the DQIG
analysis of the parameter test data. Those individuals responsible for onsite data
review and validation are noted in Figure 3, element BIO, and above. The Alion
technical leader is responsible for verification of data with all written procedures.
• Jenia Tufts of RTI will review the draft data report.
D2: Verification and Validation Methods
The process for validating and verifying data are described in element B of this protocol and
conform to required element D2 (Verification and Validation Methods) of EPA QA/R-5.
D3: Reconciliation with Data Quality Objectives
The DQO is defined as meeting the DQIGs in Table 1. This reconciliation step is an integral part
of the test program and will be done at the test site. Attainment of the DQO is confirmed by
analyzing the test data as described in element A7 and will be completed by Alion at the
conclusion of the scheduled test runs.
The reconciliation of the results with the DQO will be evaluated using the data quality
assessment process. This process begins with the review of the DQOs and the sampling design to
assure that the sampling design and data collection documentation are consistent with those
needed to meet the specified DQOs. When the preliminary data are collected, the data will be
reviewed to ensure they are consistent with expectations and to identify patterns, relationships,
and potential anomalies. The data will be summarized and analyzed using appropriate statistical
procedures. The impact of any deviations from procedures will be assessed relative to their
impact on data quality and meeting the DQOs. Finally, the quality of the data will be assessed in
terms of precision, bias, and statistical significance as they relate to the measurement objectives
and the DQO.
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Appendix A: Applicable Documents and Procedures
1. EPA Documents
EPA. Policy and Program Requirements for the Mandatory Agency-wide Quality System. EPA
Order 5360.1 A2. U.S. Environmental Protection Agency. May 2000.
EPA. EPA Requirements for Quality Management Plans. EPA QA/R-2, EPA Publication No.
EPA/240/B-01/002. U.S. Environmental Protection Agency, Office of Environmental
Information. Washington, DC. March 2001.
EPA. Environmental Technology Verification Program, Quality Management Plan. EPA
Publication No. EPA/600/R-03/021. Office of Research and Development, U.S. Environmental
Protection Agency. Cincinnati, OH. December 2002.
EPA. EPA Requirements for Quality Assurance Project Plans. EPA QA/R-5, EPA Publication
No. EPA/240/B-01/003. Office of Environmental Information, U.S. Environmental Protection
Agency. March 2001.
EPA. Guidance for Quality Assurance Project Plans. EPA QA/G-5, EPA Publication No.
EPA/600/R-98/018. Office of Environmental Information, U.S. Environmental Protection
Agency. February 1998.
EPA. Draft Generic Verification Protocol for the Verification of Pesticide Spray Drift Reduction
Technologies for Row and Field Crops. Office of Research and Development, U.S.
Environmental Protection Agency. April 2007.
EPA. Guidance on Technical Audits and Related Assessments for Environmental Data
Operations. EPA QA/G-7, EPA Publication No. EPA/600/R-99/080. Office of Environmental
Information, U.S. Environmental Protection Agency. January 2000.
2. RTI Documents
RTI International. Verification Testing of Air Pollution Control Technology - Quality
Management Plan, Revision 2.2. RTI International. Research Triangle Park, NC. February
2005. http://www.epa.gov/nrmrl/std/etv/pubs/600etvl001 l.pdf.
3. Alion Science & Technology SOPs
Alion SOP-WDE-08-02: "Generation of Calibration Curves for the Turner Digital Fluorometer,"
March 2009.2
Alion SOP-WDE-08-03: "Extraction of Samples and Measurement of Fluorescence using the
Turner Digital Fluorometer," March 2009.3
: This Alion SOP is provided as Appendix C.
1 This Alion SOP is provided as Appendix D.
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4. USDA/ARS SOPs4
USDA SOP-4.1: Personnel Records, Training Logs, and Laser Safety. September 2007.
USDA SOP-4.2: Measurement of Physical Properties of Liquids. September 2007.
USDA SOP-4.3: Reception, Storage, and Distribution of Active Chemicals. September 2007.
USDA SOP-4.4: Determining Cross-Section Average Drop-Size Distributions of Sprays.
September 2007.
USDASOP-4.5: Corrective and Preventive Actions. September 2007.
5. Other Documents
ANSI/ASHRAE 41.1 (1986) Standard Method for Temperature Measurement, American Society
of Heating, Refrigerating and Air Conditioning Engineers, Inc. 1791 Tullie Circle, NE, Atlanta,
GA 30329.
ASAE S572 (1999) (sometimes referred to as AS ABE S572) Spray Nozzle Classification by
Droplet Spectra. Standard No. S572, American Society of Agricultural and Biological
Engineers, St. Joseph, MI.
ASAE S561.1 Procedure for Measuring Drift Deposits from Ground, Orchard and Aerial
Sprayers. American Society of Agricultural and Biological Engineers, St. Joseph, MI.
ASTM D445-06 Standard Test Method for Kinematic Viscosity of Transparent and Opaque
Liquids (and Calculation of Dynamic Viscosity).
ASTM D1331 Standard Test Methods for Surface and Interfacial Tension of Solutions of
Surface-Active Agents.
ASTM E 1458 Standard Test Method for Calibration Verification of Laser Diffraction Particle
Sizing Instruments Using Photomask Reticles.
ISO Draft Standard 22856: Equipment for Crop Protection - Laboratory Drift Methods
Measurements. International Standards Organization.
4 The USDA SOPs can be obtained from Bradley Fritz of USDA-ARS in College Station, TX, at
brad.fritz@ars.usda.gov.
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Appendix B: Organizational Charts for Testing the
Low Speed Pesticide Spray DRT Protocol
DRT Vendor
EPA Project Manager
Michael Kosusko
•
EPA Quality Manager
Paul Groff
;
RTI Project Leader
Jonathan Thornburg
•
RTI Test
.
Lead
Andrew Dart
enotes normal lines of
enotes informal commi
enotes organizational i
:ommunication
nication
idependence
RTI Quality Manager
Gary Eaton
1
1
_ J
Quality Manager
Paulette Yongue j
Technical Leader
Zora Drake-Richman
Task Leaders
Technical Staff
Figure 4. Organizational chart for the low speed pesticide spray DRT protocol validation.
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Appendix C: Alion SOP-WDE-08-02 -
Standard Operating Procedure for the
Turner Quantech Digital Filter Fluorometer
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Standard Operating Procedure for the
Turner Quantech Digital Filter
Fluorometer
SOP-WDE-08-02
January 2008
Prepared for
National Homeland Security Research Center
U.S. Environmental Protection Agency
Research Triangle Park, NC 2771 I
Contract EP-D-05-065
ALIGN
TCCHNGLGGY
Aligned with your needs.
P.O.Box 12313
Research Triangle Park, NC 27709
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Turner Fluorometer
SOP-WDE-08-02
Revision 0
January 2008
Page I of 7
Standard Operating Procedure for the
Turner Quantech Digital Filter Fluorometer
c
Prepared by: X/GA^q^ 7_ j\~4--^rajfej_ Date: 1/24/08
T
Reviewed by: %j7/i*m P (lUr&fr^ Date: 1/24/08
Approved by: /ZMS&&*- <2->f^l0-*(2**-*— Date: 1/24/08.
Prepared for
National Homeland Security Research Center
U.S. Environmental Protection Agency
Research Triangle Park, NC 2771 I
Al ION
SCIENCE AND TECHNOLOGY
Aligned with your needs.
P.O.Box 12313
Research Triangle Park, NC 27709
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Turner Fluorometer
SOP-WDE-08-02
Revision 0
January 2008
Page 2 of 7
Contents
Section Page
1.0 Scope and Application 3
2.0 Summary of Method 3
3.0 Definitions 3
4.0 Health and Safety Warnings 3
5.0 Cautions 3
6.0 Interferences 3
7.0 Personnel Qualifications 4
8.0 Apparatus and Materials 4
9.0 Method Calibration 4
10.0 Sample Analysis Procedure 7
11.0 Troubleshooting 7
12.0 Data Analysis and Calculations 7
13.0 Computer Hardware and Software 7
14.0 Data and Records Management 7
15.0 Quality Control and Quality Assurance 7
16.0 References 7
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Turner Fluorometer
SOP-WDE-08-02
Revision 0
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1.0 Scope and Application
This document outlines the procedure used to prepare, calibrate, and verify proper operation of
the Turner Quantech digital filter fluorometer.
2.0 Summary of Method
The fluorometric method is used for detecting aerosols by optical fluorescence. The most
commonly used fluorescing materials in the aerosol test facility (ATF) are uranine and
fluorescein. Calibration standards will be prepared from standard stock solutions of these
materials (see SOP-WDE-08-03, Standard Operating Procedure for Analysis of Uranine-Tagged
Aerosols, and SOP-4423-03-24, Standard Operating Procedure for the Calibration of the Sequoia-
Turner Model 450 Fluorometer—Fluorescein Quantitation).
3.0 Definitions
|jL microliter
ATF aerosol test facility
DIH2O deionized water
mL milliliter
MSDS Material Safety Data Sheet
ng nanogram
4.0 Health and Safety Warnings
4.1 Read and understand all applicable Material Safety Data Sheets (MSDSs).
4.2 Always keep open chemical containers in fume hoods and wear adequate protective
clothing according to the MSDS for each chemical.
4.3 Always label secondary containers.
5.0 Cautions
5.1 Always wear clean, dust-free disposable gloves when handling any sample cuvette or
labware.
5.2 To minimize risk of contamination, use proper precautions during preparation and use of
the 1- and 0.1-ng/mL calibration standards. Containers used for preparation and storage of
these standard solutions should be used for no other purpose and should be labeled
accordingly.
6.0 Interferences
There are no known interferences with this equipment.
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Turner Fluorometer
SOP-WDE-08-02
Revision 0
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Page 4 of 7
7.0 Personnel Qualifications
Personnel should have sufficient background in operating the equipment to use it without
supervision.
8.0 Apparatus and Materials
8.1 General Equipment
12- by 75-mm disposable cuvettes
7-mL transfer pipettes
Disposable gloves 1000-mL volumetric glass flask, Pyrex Class A
100-mL volumetric glass flask, Pyrex Class A
Various sizes of volumetric glass pipettes, Pyrex Class A
Disposable pipette tips
8.2 Apparatus
Turner Quantech digital filter fluorometer
Excitation filter (NB360) Emission filter (NB460)
8.3 Chemicals
Appropriate calibration standards and laboratory blank solutions
9.0 Calibration
For detailed instructions regarding the fluorometer, please see the operating manual supplied with
the instrument.
9.1 Setup and Filter Placement
1. Set up the fluorometer on a level surface.
2. Turn on the main power switch located on the back of the unit.
3. Lift the cover on the sample chamber and place the excitation filter (NB360) in the holder
directly above the sample cuvette holder and place the emission filter (NB460) in the
holder to the left of the cuvette holder (see Figure 1).
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Turner Fluorometer
SOP-WDE-08-02
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January 2008
Emission filter
NB460
Excitation filter
N B360
Figure 1. Turner Quantech analysis chamber.
9.2 Calibration
1. Allow a minimum 15-minute warm-up period prior to calibration. It is recommended that the
fluorometer lamp be left on after use unless the fluorometer will not be used for time periods
longer than a week.
2. After the unit has initialized (15 minutes), the display will show "Main Menu," or if the unit
has been on for some time, the display will show "Press Enter."
3. Press
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Turner Fluorometer
SOP-WDE-08-02
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name, the new calibration data will be written over the older data.) Press .
9. The display responds with "Enter no. of points (2-9)." Since three standards will be used for
calibration other than zero, select 3 by using the up or down arrow, then press . A 0
ng/mL standard is not considered a point in the above count; however, it will be required
later.
10. At this point the display reads "0000.000," where "" indicates
fluorescence units. Enter the value of the highest concentration standard (e.g., 40 ng/mL). At
this point "" should be selected as shown by the blinking ">"; if not, toggle using the
left or right arrow key and select "" until the ">" blinks. Using the up and down
arrows, select "ng/mL" as the units. Then using the left arrow, go to the tens digit and
select "4" by repeatedly using the up arrow. At this point, the display should read
"0040.000." Press .
11. The display reads "Insert Known Sample 1." Insert the cuvette with the standard solution
and press . The display goes through a series of gain selections and eventually reads the
sample. Do not leave samples in the sample chamber longer than necessary, as sample
temperature will drift and result in errors.
12. The display responds with "000.000." Input the value for the second standard
(e.g., 10 ng/mL) as in step 10 so that the display reads "010.000" and press
. When the display shows "Known Sample 2," remove the first standard and insert a
cuvette with the mid-range standard solution and then press .
13. When the display shows "000.000," input the value for the third standard (e.g., 2
ng/mL) as in step 10. When the display reads "002.000," press . When the
display shows "Known Sample 3," remove the second standard and insert a cuvette with
the lowest concentration standard solution and press .
14. When the display reads "Insert Blank Sample," remove the standard and insert a cuvette
with 0 ng/mL solution.
15. Press as the display instructs. After reading this sample, the display should show the
coefficient of determination (regression coefficient). The number appears only briefly on
screen and then disappears, so pay close attention. This should ideally be "1" and not less than
"0.99". If it is less than 0.99, then either the calibration or standards preparation may have to
be repeated. Press . The display reads "Insert Unknown Sample." The "Named"
method is now ready.
After calibration is complete, check the calibration by remeasuring all standards. The instrument
must read within 3% of their values. A standard resulting in a higher difference may indicate that
an error was made in preparing that standard or the stock solution is going bad. If any standard is
replaced, the calibration should be repeated. During the measurement of unknown samples,
periodically check calibration by remeasuring the midrange standard to ensure there is no drift. If
the reading drifts by more than 3% of the standard's value, recalibrate the instrument.
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10.0 Sample Analysis Procedure
Insert the prepared test sample solution (unknown) in a cuvette and press . The
instrument gives out a reading (ng/mL). If the concentration is too low (less than the low
standard), a negative value may result. Also, if the concentration is higher than the high standard,
the instrument may read "Out of Range." Mark all samples that are out of range to run later either
as diluted samples or against a different calibration curve.
11.0 Troubleshooting
Refer to the user's manual for troubleshooting guidelines.
12.0 Data Analysis and Calculations
Use the following calculation to obtain an unknown's fluorometric content:
Cone (ng/mL) = reading * dilution ratio,
Where Cone is the fluorometric concentration of the solution being tested (ng/mL),
reading is the reading from the display of the fluorometer (ng/mL), and
dilution ratio is any dilution that may have been done prior to measurement.
13.0 Computer Hardware and Software
Spreadsheet software may be used with this method to assist in data analysis.
14.0 Data and Records Management
Records of use and maintenance are to be kept in the operator's laboratory notebooks.
15.0 Quality Control and Quality Assurance
As noted in the calibration procedure, verification within prescribed standard-dependent limits
must be made prior to use of the fluorometer for analytical purposes.
16.0 References
Alion Science and Technology. 2008. Standard Operating Procedure for Analysis of Uranine-
Tagged Aerosols, SOP-WDE-08-03. Research Triangle Park, NC.
ManTech Environmental Technology, Inc. Standard Operating Procedure for the Calibration of
the Sequoia-Turner Model 450 Fluorometer—Fluorescein Quantitation, SOP-4423-03-24.
Research Triangle Park, NC.
Thermo Scientific. February 2007. Turner Digital Filter Fluorometer Operation Manual, Dubuque,
Iowa.
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Appendix D: Alion SOP-WDE-08-03 - Standard Operating Procedure for Analysis of Uranine-
Tagged Aerosols
Standard Operating Procedure for
Analysis of Uranine-Tagged Aerosols
SOP-WDE-08-03
January 2008
Prepared for
National Homeland Security Research Center
U.S. Environmental Protection Agency
Research Triangle Park, NC 2771 I
ALION
SCIENCE »HO 1ECHNOLOGY
Aligned with your needs.
P.O.Box 12313
Research Triangle Park, NC 27709
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Uranine-Tagged Aerosols
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Standard Operating Procedure for
Analysis of Uranine-Tagged Aerosols
Prepared by: \CKQ_. /
Reviewed by:
Approved by:
0,
Date: 1/24/08
Date: 1/24/08
Date: 1/24/08
Prepared for
National Homeland Security Research Center
U.S. Environmental Protection Agency
Research Triangle Park, NC 2771 I
ALIGN
SCIENCE AND TECHNOLOGY
Aligned with your needs.
P.O.Box 12313
Research Triangle Park, NC 27709
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Uranine-Tagged Aerosols
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Contents
Section Page
1.0 Scope and Application 3
2.0 Summary of Method 3
3.0 D efiniti ons 3
4.0 Health and Safety Warnings 3
5.0 Cautions 3
6.0 Interferences 4
7.0 Personnel Qualifications 4
8.0 Apparatus and Materials 4
9.0 Method Calibration 4
10.0 Sample Generation and Testing 6
11.0 Preservation 7
12.0 Sample Analysis Procedure 7
13.0 Troubleshooting 7
14.0 Data Analysis and Calculations 7
15.0 Computer Hardware and Software 7
16.0 Data and Records Management 7
17.0 Quality Control and Quality Assurance 7
18.0 References 8
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1.0 Scope and Application
This document outlines the procedures used to prepare calibration standards for and to verify the
proper operation of the Turner Quantech digital filter fluorometer for the quantitation of uranine
in aqueous alkaline solutions. This procedure is used prior to the quantitation of unknown
samples (refer to SOP-WDE-08-02, Standard Operating Procedure for the Turner Quantech
Digital Filter Fluorometer, for this procedure).
2.0 Summary of Method
Calibration standards of 100, 5, 1, and 0.1 ng/mL will be prepared from a standard stock solution of
106 ng/mL uranine in 0.01 N NaOH. The 100 ng/mL standard is used to span the instrument daily
and the 5, 1, and 0.1 ng/mL standards are used to verify the instrument's linear response over the
entire measurement range.
3.0 Definitions
(iL microliter
DIH2O deionized water
g gram
mL milliliter
mm millimeter
MSDS Material Safety Data Sheet
N normal solution
NaOH sodium hydroxide
ng nanogram
4.0 Health and Safety Warnings
4.1 Read and understand all applicable Material Safety Data Sheets (MSDSs).
4.2 Always keep open chemical containers in fume hoods and wear adequate protective
clothing according to the MSDS for each chemical.
4.3 Always label secondary containers.
5.0 Cautions
5.1 Always wear clean, dust-free disposable gloves when handling any sample cuvette or
labware.
5.2 Read and follow the manufacturer's guidelines for proper use of micropipettes used in
this procedure.
5.3 To minimize risk of contamination, use proper precautions during preparation and use of
the calibration standards. Containers used for preparation and storage of these standard
solutions should be used for no other purpose and should be labeled accordingly.
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6.0 Interferences
There are no known interferences with this equipment.
7.0 Personnel Qualifications
Personnel should have sufficient background in operating the equipment to use it without
supervision.
8.0 Apparatus and Materials
8.1 General Equipment
12- by 75-mm disposable cuvettes
7-mL transfer pipettes Disposable gloves
32-oz amber bottles
20-L LDPE carboy with spigot
Volumetric glass pipettes, Pyrex Class A sizes as needed
Pipette bulb
Weigh boats and/or papers
1000-mL volumetric glass flask, Pyrex Class A
100-mL volumetric glass flask, Pyrex Class A
2-in magnetic stir bars Magnetic stir plate
8.2 Apparatus
Fluorometer, Turner Quantech
Analytical balance
8.3 Chemicals
DI H2O—allow system to run for 15 minutes prior to using
NaOH, 0.1N
Uranine, purified grade, Fisher Brand A833-500
9.0 Method Calibration
9.1 Preparation of 0.01 N Sodium Hydroxide
1. Add approximately 5 L of DI H2O to a clean 20-L capacity carboy.
2. Using a 1000-mL graduated cylinder, add 2 L of 0.1 N NaOH to the carboy.
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3. Dilute the carboy contents to the 20-L line using DI IrhO.
4. Cap the carboy and thoroughly mix the contents prior to initial use.
5. Label the carboy with the date, composition, and operator's name.
9.2 Preparation of 1000 pg/mL Uranine in 0.01 N NaOH Stock Solution
1. Zero and calibrate the analytical balance using techniques described in SOP-WDE07-04,
Standard Operating Procedure for Operation and Maintenance of the Sartorius CP324S
Balance.
2. Place a clean, dry weighing dish on the weighing pan.
3. Tare the balance and ensure that the reading is stable before proceeding.
4. Carefully add uranine to the dish until a reading of 1.000 ± 0.01 g is achieved. Record
the final value and remove the container from the balance. Zero the balance.
5. Using 0.01 N NaOH, transfer the uranine to a clean, dry 1000-mL volumetric flask,
ensuring that the uranine is transferred from all surfaces of the weighing dish to the flask.
6. Gently swirl the container until the uranine has been dissolved.
7. Dilute the container's contents to 1000 mL using 0.01 N NaOH.
8. Label the flask and record the following information on the label: date, exact
composition (calculated from the mass recorded in step 4), and operator's name.
9. Carefully insert a clean, 2-in-long magnetic stirrer into the container and place the
container on the stir plate. Stir the solution for approximately 15 minutes using a
moderate stir rate.
10. Transfer the solution contents into a clean, prelabeled amber bottle. Tightly cap the
container and store it in a cool, dark environment.
Note: This solution has a shelf life of approximately 6 months. At the end of that time
period, discard the remaining solution properly.
9.3 Preparation of 1000 ng/mL Uranine in 0.01 N NaOH Intermediate
Stock Solution
1. In a clean, dry 1000 mL volumetric flask, add approximately 100 mL of 0.01 N NaOH.
Transfer 1 mL of the stock solution to the volumetric flask using a clean, dry volumetric
pipette.
2. Gently swirl the volumetric flask.
3. Dilute the container's contents to 1000 mL using 0.01 N NaOH.
4. Label the flask and record the following information on the label: date, calculated
concentration, and operator's name.
5. Carefully insert a clean, 2-in-long magnetic stirrer into the container and place the
container on the stir plate. Stir the solution for approximately 15 minutes using a
moderate stir rate.
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6. Transfer the solution contents into a clean, prelabeled amber bottle. Tightly cap the
container and store it in a cool, dark environment.
Note: This solution has a shelf life of approximately 3 months. At the end of that time
period, discard the remaining solution properly.
9.4 Preparation of the Working Uranine Standard Solutions
Working standards of various concentrations can be prepared from the intermediate stock
solution. (Be careful not to exceed the range of the fluorometer.) Prepare at least three
working standards to be used to calibrate the fluorometer.
1. Determine the amount of intermediate stock solution to be added to a 100-mL
volumetric flask using the calculations in section 14.0.
2. Add a small amount (~ 25 mL) of 0.01 N NaOH to the volumetric flask.
3. Transfer the calculated amount of intermediate stock solution into the 100-mL
volumetric flask using a glass volumetric pipette.
4. Bring the flask to volume using 0.01 N NaOH.
5. Label the container with the date, composition, and operator's name.
6. Store the container in a cool, dark environment.
7. Prepare at least two additional working standards at different concentrations using
procedures outlined in steps 1-6.
8. Set up the fluorometer according to procedures outlined in SOP-WDE-08-02,
Standard Operating Procedure for the Turner Quantech Digital Filter Fluorometer.
Note: These solutions have a short shelf life and should be discarded within a few hours of
preparation. Prepare new working standards daily.
9.5 Calibration of the Turner Quantech Fluorometer
See SOP-WDE-08-02, Standard Operating Procedure for the Turner Quantech Digital Filter
Fluorometer.
9.6 Verification of Proper Instrument Operation
Following initial setup, proper instrument operation is verified by measuring the
instrument's response to previously prepared calibration standards. Insert each standard into
the fluorometer as "unknown" and allow the fluorometer to determine the
concentrations. Read each working standard three times. Proper instrument response is
verified if the average of the actual responses is within acceptable limits (± 3%) of the
expected response.
lO.OSample Generation and Testing
This section is not applicable for this method.
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11.0 Preservation
Sample preservation is not relevant for this method.
12.0 Sample Analysis Procedure
Unknown samples can be analyzed according to the procedures in SOP-WDE-08-02, Standard
Operating Procedure for the Turner Quantech Digital Filter Fluorometer.
13.0 Troubleshooting
Refer to the user's manual for troubleshooting guidelines.
14.0 Data Analysis and Calculations
The following concentration calculations are used:
G/F=g/mL, (1)
Where G is number of grams of material determined gravimetrically, and
Vis volume (mL).
Vl*Cl = V2*C2, (2)
Where V is volume (mL), and
C is concentration.
15.0 Computer Hardware and Software
Spreadsheet software can be used with this method to assist in data analysis.
16.0 Data and Records Management
Records of calculations, use, and maintenance are to be kept in the operator's laboratory
notebooks.
17.0 Quality Control and Quality Assurance
Calculate the relative standard deviation for the three readings by dividing the sample standard
deviation by the mean. If the relative standard deviation is less than or equal to 3%, preparation of
the working standards is considered to be correct. If the relative standard deviation exceeds 3%,
the samples should be discarded and new standards prepared. Should the problem persist, refer to
the manual for troubleshooting guidelines.
As noted in the calibration procedure, verification within prescribed standard-dependent limits
must be made prior to use of the fluorometer for analytical purposes.
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Test/QA Plan for Pesticide Spray DRT in a Low Speed Wind Tunnel Version 0.0
May 2009 Page 44
Uranine-Tagged Aerosols
SOP-WDE-08-03
Revision 0
January 2008
Page 8 of 8
18.0 References
Alion Science and Technology. 2008. Standard Operating Procedure for the Turner Quantech
Digital Filter Fluorometer, SOP-WDE-08-02. Research Triangle Park, NC.
Alion Science and Technology. 2007. Standard Operating Procedure for Operation and
Maintenance of the Sartorius CP324S Balance, SOP-WDE-07-04. Research Triangle Park,
NC.
Thermo Scientific. February 2007. Turner Digital Filter Fluorometer Operation Manual, Dubuque,
Iowa.
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