Baltelle
The Business of Innovation
Environmental Technology
Verification Program
Advanced Monitoring
Systems Center
Quality Assurance Project Plan
For Verification of
ANDalyze LeadlOO Test Kit and
ANDlOOOFluorimeter
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FINAL
Verification of
ANDalyze Lead 100 Test Kit
and AND 1000 Fluorimeter
July 3, 2012
Prepared by:
Brian Yates
Amy Dindal
Battelle
505 King Avenue
Columbus, OH 43201-2693
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SECTION A
PROJECT MANAGEMENT
Al VENDOR APPROVAL PAGE
ETV Advanced Monitoring Systems Center
Quality Assurance Project Plan
for Verification of
ANDalyze Lead 100 Test Kit and AND 1000 Fluorimeter
DRAFT
Name
Company
Date
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A2 TABLE OF CONTENTS
Section Page
SECTION A PROJECT MANAGEMENT 3
Al VENDOR APPROVAL PAGE 3
A2 TABLE OF CONTENTS 4
A3 DISTRIBUTION LIST 7
A4 LIST OF ACRONYMS AND ABBREVIATIONS 8
A5 VERIFICATION TEST ORGANIZATION 10
A5.1 Battelle 10
A5.2 Lead 100/AND1000 Vendor 14
A5.3 EPA AMS Center 15
A5.4 Verification Test Peer Reviewers 16
A6 BACKGROUND 16
A6.1 Technology Need 17
A6.2 Technology Description 18
A7 VERIFICATION TEST DESCRIPTION AND SCHEDULE 19
A7.1 Verification Test Description 19
A7.2 Verification Test Schedule 22
A7.3 Test Site Descriptions 22
A7.4 Health and Safety 26
A8 QUALITY OBJECTIVES AND CRITERIA FOR MEASUREMENT DATA 27
A9 SPECIAL TRAINING/CERTIFICATION 28
A10 DOCUMENTATION AND RECORDS 29
SECTIONS MEASUREMENT AND DATA ACQUISITION 31
Bl EXPERIMENTAL DESIGN OVERVIEW 31
Bl.l Detailed Test Procedures 38
Bl.1.1 Glassware 38
Bl.l.2 Reagents 38
Bl.l.3 Laboratory Equipment 41
Bl.l.4 Analytical Procedures 41
Bl.l.5 Preparation of Pb Stock Solution 42
Bl.l.6 Preparation of Pb-spiked Samples 42
B.I.1.7 Preparation of Synthetic Waters for DEI Testing 44
B.I.1.7.1 Preparation of High TDS Water 44
B.I.1.7.2 Preparation of Low TDS Water 45
B.I.1.7.3 Preparation of High Iron Water 46
Bl.l.8 Sequence of Procedures 47
Bl.l.8.1 IDC Testing 47
Bl.l.8.2 TPC Testing 47
Bl.l.8.3 ICC Testing 49
Bl.l.8.4 DLOD Testing 49
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B.I.1.8.5 DLR Testing 50
B.I.1.8.6 DEI Testing 50
B 1.1.8.7 Finished Drinking Water Testing 51
Bl.1.8.8 Environmental Water Testing 53
Bl.1.8.9 Wastewater Effluent Water Samples 56
B1.2 Statistical Analysis 58
Bl.2.1 Accuracy 58
Bl.2.2 Precision 59
Bl.2.3 Linearity of Response 60
Bl.2.4 Limit of Detect! on 61
B2 SAMPLING METHODS REQUIREMENTS 62
B2.1 Sample Collection, Storage and Shipment 62
B3 SAMPLE HANDLING AND CUSTODY REQUIREMENTS 62
B4 ANALYTICAL METHODS REQUIREMENTS 63
B5 QUALITY CONTROL 63
B5.2 Acceptance Criteria and Root Cause Analyses 64
B5.3 Control Charts 67
B6 INSTRUMENT/EQUIPMENT TESTING, INSPECTION, AND MAINTENANCE . 67
B7 CALIBRATION/VERIFICATION OF TEST PROCEDURES 67
B8 INSPECTION/ACCEPTANCE OF SUPPLIES AND CONSUMABLES 68
B9 NON-DIRECT MEASUREMENTS 68
BIO DATA MANAGEMENT 68
SECRTION C: ASSESSMENT AND OVERSIGHT 70
Cl Assessments and Response Actions 70
Cl.l Performance Evaluation Audit 70
C1.2 Technical Systems Audits 71
C1.3 Data Quality Audits 71
C1.4 QA/QC Reporting 72
C2 Reports to Management 72
SECTIOND DATA VALIDATION AND USABILITY 74
D1 DATA REVIEW, VALIDATION, AND VERIFICATION REQUIREMENTS 74
D2 VALIDATION AND VERIFICATION METHODS 74
D3 RECONCILIATION WITH USER REQUIREMENTS 75
SECTION E REFERECNES 76
El REFERENCES 76
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List of Figures
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Page
Figure 1. Organization Chart for the Verification Test 11
Figure 2. Site Map Showing the Locations of Two of the Environmental Samples 25
Figure 3. Site Location Map Showing the Location of the Seawater Sample 25
List of Tables
Table 1. General Verification Test Schedule 23
Table 2. Sampling Locations and Descriptions 27
Table 3. Summary of Records to be Collected and Maintained 30
Table 4. Experimental Matrix and Sample Summary for PT 33
Table 5. Sample Summary for Water Sample Testing 38
Table 6. Reagents Used During Verification Testing 40
Table 7. Laboratory Equipment Used During Verification Testing 41
Table 8. Volume of Pb Standard Solution Additons to 100 mL of Sample to Obtain Required
Pb Spike 43
Table 9. Composition of High TDS Water 45
Table 10. Composition of Low TDS Water 46
Table 11. Composition of High Iron Water 47
Table 12. Verification Schedule and Test Matrix 48
Table 13. Summary of Quality Assessment and Control Reports 72
Appendices
Appendix A. AND1000 Fluorimeter for Water Testing (AND-Prod-1000-2-2012)
Appendix B. Lead Testing and On-Site Calibration for Water Testing (AND-Lead-100-02-2012)
Appendix C. Environmental Water Testing: Surface Water, Groundwater, Hard Water, Wastewater
and Seawater Solution Notes (AND-Sol-Env-02-2012)
Appendix D. Iron Interference with LeadlOO Sensor Solution Notes (AND-Sol-Lead-02-2012)
Appendix E. 3-Point Laboratory Calibration (AND-Sol-Cal-02-2012)
Appendix F. Root Cause Analysis Flowchart: On-site Calibration and IDC
Appendix G. Root Cause Analysis Flowchart: On-Site Calibration, ICC and 3-Point Calibration
Appendix H. Root Cause Analysis Flowchart: On-Site Calibration, DEI, Finished Drinking Water,
Environmental Water, Wastewater Effluent
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A3 DISTRIBUTION LIST
EPA
John McKernan, Sc.D., Cffl
U.S. Environmental Protection Agency
26 West Martin Luther King Drive
Mail code: 208
Cincinnati, OH 45268
Peer Reviewer
CITY OF PHOENIX, AZ
Randy Gottler
Water Services Department
Environmental Services Division
2474S. 22Ave. Bldg. #31
Phoenix, AZ 85009
Peer Reviewer
Julius Enriquez U.S. Environmental
Protection Agency
26 West Martin Luther King Drive
Cincinnati, OH 45268
Battelle
Rosanna Buhl
Elizabeth Cutie
Amy Dindal
Brian Yates
Battelle Memorial Institute
505 King Ave.
Columbus, OH 43201
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A4 LIST OF ACRONYMS AND ABBREVIATIONS
ADQ Audit of Data Quality
AMS Advanced Monitoring Systems
CaSC>4 calcium Sulfate
COC chain of custody
CV coefficient of variation
DEI determination of the effects of interferences
DI deionized
DLOD determination of the limit of detection
DLR determination of linear range
DQO data quality obj ective
EPA Environmental Protection Agency
ETL Environmental Treatability Laboratory
ETV Environmental Technology Verification
FCU failure cause unknown
Fe iron
HOPE high density polyethylene
HNO3 nitric Acid
ICC Initial Calibration Check
ICP-MS inductively-coupled plasma mass spectroscopy
IDC initial demonstration of capability
IFE instrument failure electrical
IFM instrument failure mechanical
IOFM instrument operator failure to follow method
JHA job hazard analysis
KC1 potassium Chloride
LFM laboratory-fortified matrix
LOD limit of detection
LRB laboratory record book
MCL maximum contaminant level
MGD million gallons per day
MgSC>4 magnesium sulfate
MLC minimum water level change
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NaCl sodium Chloride
NaHCOs sodium Bicarbonate
Pb lead
PEA performance evaluation audit
PO Project Officer
ppb parts per billion
ppm parts per million
PT performance testing
QA quality assurance
QAPP quality assurance project plan
QC quality control
QCS quality control standard
QM Quality Manager
QMP Quality Management Plan
KB reagent blank
RMO Records Management Office
SD standard deviation
SFC sensor failure chemical
SFM sensor failure mechanical
SOP standard operating procedure
TDS total dissolved solid
TL tolerance limit
TPC three point calibration
TSA technical systems audit
VTC Verification Test Coordinator
WHO World Health Organization
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A5 VERIFICATION TEST ORGANIZATION
The verification test will be conducted under the U.S. Environmental Protection
Agency's (EPA's) Environmental Technology Verification (ETV) Program. It will be performed
by Battelle, which manages the ETV Advanced Monitoring Systems (AMS) Center through a
cooperative agreement with EPA. The scope of the AMS Center covers verification of
monitoring technologies for contaminants and natural species in air, water, and soil.
The day-to-day operations of this verification test will be coordinated and supervised by
Battelle, with the participation of ANDalyze, Inc. (Vendor), the Vendor who will be supplying
the Lead 100 test kit and the AND 1000 fluorimeter (Lead 1007AND 1000) for performance
verification. The verification test will be performed using laboratory facilities (i.e., Battelle's
Environmental Treatability Laboratory [ETL]) under highly-controlled conditions and selected
field sites (e.g., river reaches and reservoirs) under partially-controlled conditions. Verification
tests will require the participation of the Vendor and Battelle staff. Vendor representatives,
expert peer reviewers and EPA AMS Center management will review this Quality Assurance
Project Plan (QAPP), verification reports, and verification statements. The verification
statements are then approved by the EPA AMS Center management.
The organization chart in Figure 1 identifies the responsibilities of the organizations and
individuals associated with the verification test. Roles and responsibilities are defined further
below. Quality assurance (QA) oversight will be provided by the Battelle Quality Manager
(QM) and also by the EPA AMS Center QM, at his/her discretion. This verification test is
Quality Category III, which requires a QA review of 10% of the test data (see Section Cl).
A5.1 Battelle
Mr. Brian Yates is the AMS Center's Verification Test Coordinator (VTC) for this test.
In this role, Mr. Yates will have overall responsibility for ensuring that the technical, schedule,
and cost goals established for the verification test are met. Specifically, Mr. Yates will:
• Prepare the draft QAPP, verification report, and verification statement;
• Establish a budget for the verification test and manage staff to ensure the budget is
not exceeded;
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Battelle
Management
AMS Center
Stakeholders
Rosanna Buhl
Battelle
Quality Manager
Amy Dindal
Battelle AMS
Center Manager
Verification Test Peer
Reviewers
Brian Yates
Battelle
Verification
Test Coordinator
John McKernan
EPA AMS Center
Project Officer
EPA AMS Center
Quality Manager
ANDalyze
Technology
Vendor
Representatives
Battelle
Technical Staff
i
;
Figure 1. Organization Chart for the Verification Test
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• Revise the draft QAPP, verification report, and verification statement in response to
reviewer comments;
• Conduct verification testing using the vendor's technology;
• Collect the data and samples during verification testing;
• Direct the team in performing the verification test in accordance with this QAPP;
• Organize and lead a kick-off meeting approximately one (1) week prior to the start of
the verification test to review the critical logistical, technical, and administrative
aspects of the verification test. Responsibility for each aspect of the verification test
will be reviewed to ensure each participant understands his/her role;
• Ensure that all quality procedures specified in this QAPP and in the AMS Center
Quality Management Plan[1] (QMP) are followed;
• Serve as the primary point of contact for Vendor representatives;
• Ensure that confidentiality of sensitive Vendor information is maintained;
• Assist Vendor as needed during verification testing;
• Familiarize himself with the operation and maintenance of the technologies through
instruction by the Vendor;
• Respond to any issues raised in assessment reports, audits, or from test staff
observations, and institute corrective action as necessary;
• Coordinate distribution of the final QAPP, verification report, and verification
statement; and
• Respond to QAPP deviations and any issues raised in assessment reports, audits, or
from test staff observations, and institute corrective action as necessary.
Ms. Amy Dindal is Battelle's Manager for the AMS Center. As such, Ms. Dindal will
oversee the various stages of verification testing. Specifically, Ms. Dindal will:
• Review the draft and final QAPP;
• Attend the verification test kick-off meeting;
• Review the draft and final verification reports and verification statements;
• Ensure that necessary Battelle resources, including staff and facilities, are committed
to the verification test;
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• Ensure that confidentiality of sensitive Vendor information is maintained;
• Support Mr. Yates in responding to any issues raised in assessment reports and audits;
• Maintain communication with EPA's technical and quality managers; and
• Issue a stop work order if Battelle or EPA QA staff discover any situation that will
compromise test results.
Battelle Technical Staff will support Mr. Yates in planning and conducting the
verification test. Specifically, the technical staff will:
• Assist in planning for the test and making arrangements for the receipt of and training
on the technologies;
• Attend the verification test kick-off meeting;
• Assist Vendor staff as needed during technology receipt and training;
• Arrange for and/or acquire adequate supplies, equipment, and facilities/locations for
performing verification tests and disposing of generated wastes;
• Perform statistical calculations specified in this QAPP on the technology data as
needed;
• Provide results of statistical calculations and associated discussion for the verification
reports as needed;
• Support Mr. Yates in responding to any issues raised in assessment reports and audits
related to statistics and data reduction as needed; and
• Conduct and observe verification testing on-site, as appropriate. Immediately report
deviations to this QAPP to the VTC.
Ms. Rosanna Buhl is the Battelle QM for the AMS Center. Ms. Buhl will:
• Review the draft and final QAPP;
• Attend the verification test kick-off meeting and lead the discussion of the QA
elements of the kick-off meeting checklist;
• Review and approve the QAPP, QAPP amendments, deviations and audit reports;
• Work with the VTC and Battelle's AMS Center Manager to resolve data quality
concerns and disputes; and
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• Recommend a stop work order if audits indicate that data quality or safety is being
compromised.
• Assign a Quality Assurance Officer (QAO). Ms. Betsy Cutie is assigned as QAO for
this test. She will perform the following functions:
o Prior to the start of verification testing, verify the presence of applicable training
records, including any vendor training on test equipment;
o Conduct a technical systems audit (ISA) at least once during the verification test;
o Conduct audits to verify data quality;
o Prepare and distribute an audit report for each audit;
o Verify that audit responses for each audit finding and observation are appropriate
and that corrective action has been implemented effectively;
o Provide a summary of the QA/quality control (QC) activities and results for the
verification report;
o Review the draft and final verification report and verification statement;
o Communicate to the VTC and/or technical staff the need for immediate corrective
action if an audit identifies QAPP deviations or practices that threaten data
quality;
A5.2 LeadlOO/ANDlOOO Vendor
The responsibilities of the Vendor are as follows:
• Review and provide comments on the draft QAPP;
• Accept (by signature of a company representative) the final QAPP prior to test
initiation to confirm that the conditions of the test are understood. Provide
technology for evaluation during the verification test;
• Supply training on the use of the technology and provide written consent and
instructions for test staff to carry out verification testing, including written
instructions for routine operation of their technology;
• Provide maintenance and repair support for the technology, onsite if necessary,
throughout the duration of the verification test; and
• Review and provide comments on the draft verification report and statement.
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A5.3 EPA AMS Center
EPA's responsibilities in the AMS Center are based on the requirements stated in the
"Environmental Technology Verification Program Quality Management Plan" (ETV QMP)^.
The roles of specific EPA staff are as follows:
For the verification test, the EPA's AMS Center QM will:
• Review and provide comments on the draft QAPP;
• Perform at his/her option one external technical systems audit (TSA) during the
verification test;
• Notify the EPA AMS Center Project Officer (PO) of the need for a stop work order if
the external audit indicates that data quality is being compromised;
• Prepare and distribute an assessment report summarizing results of the external audit;
• Perform audits of data quality;
• Notify the EPA AMS Center PO of the need for a stop or modify work order if the
audit of data quality indicates that data quality is being compromised; and
• Review draft verification reports and verification statements.
Dr. John McKernan is EPA's PO for the AMS Center. Dr. McKernan, or designee will:
• Review and provide comments on the draft QAPP;
• Approve the final QAPP;
• Review the draft verification reports and verification statements;
• Oversee the EPA review process for the QAPP, verification reports, and verification
statements;
• Coordinate the submission of verification reports and verification statements for final
EPA approval;
• Post the QAPP, verification reports, and verification statements on the ETV Web site;
and
• Review and authorize any QAPP deviations by phone and provide the name of a
delegate to the Battelle AMS Center Manager should he not be available during the
testing period.
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A5.4 Verification Test Stakeholders
This QAPP and the verification report and verification statement based on testing
described in this document will be reviewed by experts in the fields related to lead detection
technology performance and statistics. The following stakeholders have agreed to provide
review:
• Randy Gottler, City of Phoenix, Arizona
• Dr. Edward F. Askew, Askew Scientific, Iowa
A6 BACKGROUND
The ETV Program's AMS Center conducts third-party performance testing of
commercially available technologies that monitor, sample, detect, and characterize contaminants
or naturally occurring species across all matrices. The purpose of ETV is to provide objective
and quality assured performance data on environmental technologies so that users, developers,
regulators, and consultants can make informed decisions about purchasing and applying these
technologies. Stakeholder committees of buyers and users of such technologies recommend
technology categories, and technologies within those categories, as priorities for testing.
Lead (Pb) is a naturally occurring metal in the aquatic environment; however, most Pb
contamination of concern arises from anthropogenic sources (such as deposition of Pb dust from
combustion processes in natural waterways or due to its use in plumbing materials). Although
Pb is not commonly found in natural waters, high concentrations of Pb in the natural
environment can compromise the health of ecosystems and lead to their degradation. Humans
are exposed to Pb through ingestion of Pb-laden foods or waters, or inhalation of Pb-containing
dust which can lead to numerous health effects. Specifically, Pb in drinking water can cause a
variety of adverse health effects including delays in physical and mental development, along
with deficits in attention span and learning disabilities in children. In adults, consumption of Pb-
contaminated drinking water over the EPA maximum contaminant level (MCL) can lead to acute
high blood pressure or, if ingested over long periods of time, can lead to chronic kidney
problems including necrosis or hepatic cancers^.
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Due to the importance of Pb in both the natural environment and in finished drinking
waters, there is an immediate need for the determination of soluble, bioavailable aqueous Pb at
relevant toxicological levels (|ig/L [ppb] range). A number of instrumental methods exist for the
determination of Pb in environmental aqueous samples such as graphite furnace atomic
absorption spectroscopy, inductively-coupled plasma mass spectroscopy (TCP-MS) and
electrochemical methods such as cyclic voltametry and chronoamperometric methods. While
well established, these methods are time consuming and, in general, expensive to carry out on a
routine basis. Other shortcomings associated with traditional methods for the determination of
Pb in the aquatic environment is that these methods are not portable and analysis time (time-to-
result) are too long for the determination of Pb at relevant time-scales. In addition, an accurate
and rapid method of Pb detection is also necessary to ensure that municipal wastewater and
industrial wastewater effluents discharged to natural waterways will not exceed the total
maximum daily load permissible for Pb to said waterways.
The purpose of this QAPP is to specify procedures for a verification test applicable to Pb
sensing in environmental water samples, finished drinking water samples, and municipal
wastewater and industrial wastewater effluent water samples. The purpose of the verification
test is to evaluate the performance of Lead 100/AND 1000 for Pb measurement by challenging it
under a variety of combinations of Pb concentrations and water compositions.
A6.1 Technology Need
The World Health Organization (WHO) has recommended the upper limit for Pb in
natural waterways at less than 10 |ig/L^ while the EPA has set an MCL for Pb in drinking water
of 15 |ig/LJ3^. In addition, EPA has also set discharge limits for industrial wastewater and
municipal wastewater effluents to natural waterways depending on the sensitivity of the
receiving water body and the probability of Pb contamination from the specified source. It is
therefore essential that accurate and precise methods for detection of aqueous Pb at relevant Pb
concentrations be developed and verified in a systematic and scientific fashion so that citizens,
regulators and operators of facilities from which Pb discharges are probable can have the access
to and confidence in Pb measurements in natural waterways, drinking water and municipal
wastewater and industrial wastewater effluents. Specifically, these technologies should:
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• be able to precisely and accurately detect aqueous Pb at levels relevant to
regulations and adverse health effects (1 to 100 |ig/L [ppb]);
• be able to detect aqueous Pb in a variety of aquatic matrices such as finished
drinking water, groundwater, freshwater, wastewater effluents and seawater;
• have high sample throughput;
• be easy to operate with little chemistry or engineering background;
• be rugged and portable.
A6.2 Technology Description
The Lead 100/AND 1000 is designed to test for Pb in drinking water and environmental
waters. Testing is intended to take place onsite at the source of collection or in a temperature
controlled facility a minimal distance from the collection site without sample preservation. The
test makes use of two primary components: a handheld fluorimeter (AND 1000) and a
consumable test kit (Lead 100) specific to each metal or target; in the present case, Pb.
The AND 1000 fluorimeter is specifically coded to provide an interactive experience and
allow testing, data storage, and signal output without the use of a separate computational device.
The fluorimeter has the capability to analyze multiple targets with the appropriate test kit, though
the sole target discussed in this method is aqueous Pb in drinking water, wastewater effluent and
environmental waters. The AND 1000 fluorimeter enables field testing to be done in two steps.
The fluorimeter uses a sensitive measurement technique to determine the levels of Pb
contaminants. ANDalyze's catalytic DNA sensors use a metal-specific DNAzyme reaction that
leads to an increase in fluorescence in the presence of a target contaminant substance such as Pb.
The fluorescence of the reaction is measured by a fluorimeter to determine the concentration of
the target heavy metal and is reported in ppb. Using the product to test for metals is a simple,
quantitative test that allows for detection in a linear range of 2 to 100 ppb — at and below EPA
standards in drinking water. The test is performed by taking a buffered 1 mL water sample,
injecting it through the sensor, and into the AND 1000 fluorimeter. This sample is then
automatically analyzed and reports results in less than two minutes.
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The second component is the LeadlOO test kit specific to Pb, which provides all
necessary materials for in-field instrument calibration and sample testing with minimal sample
pretreatment. This kit contains the DNA sensors specific to a given analyte. The kit is color
coded for ease of use and a product manual is provided with detailed step-by-step instructions
including photographs. It should be noted that laboratory evaluation may require additional
supplies and standard laboratory glassware.
A7 VERIFICATION TEST DESCRIPTION AND SCHEDULE
This verification test will assess the performance of the LeadlOO/AND 1000 relative to
key verification parameters including accuracy, precision, sample throughput and ease of use.
These performance parameters will be evaluated using multiple variables that will challenge the
Lead 1007AND 1000's ability to detect Pb in a variety of aqueous matrices. In performing the
verification test, Battelle will follow the technical and QA procedures specified in this QAPP and
will comply with the data quality requirements in the AMS Center QMP^ and the ETV QMP^ .
This verification test is an EPA designated QA Level III verification.
A7.1 Verification Test Description
Specific procedures described herein are based on Battelle's experience and expertise in
testing of heavy metals in aqueous solution and peer reviewer input. The LeadlOO/AND 1000
technology evaluation is organized as four main tests. Each test evaluates the performance of
LeadlOO/AND 1000 to operate under different laboratory and field conditions. The four tests are:
1. Initial demonstration of capability and performance testing (PT) including
determination of the limit of detection (DLOD), determination of linear range (DLR)
and determination of the effects of interferences (DEI)
2. Testing accuracy and precision of the instrument for the analysis of finished drinking
water samples
3. Testing accuracy and precision of the instrument for the analysis of environmental
water samples
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4. Testing accuracy and precision of the instrument for the analysis of wastewater
effluent samples.
The initial demonstration of capability, PT (including DLOD and DLR) as well as the
DEI will be performed in a highly-controlled environment within Battelle's ETL and involve the
detection of a Pb spike (25 ppb) in reagent grade water. The DLOD will be performed by
measuring seven replicates of Pb spiked at five times the purported limit of detection (10 ppb).
The DLR will be carried out by measuring the Lead 100/AND 1000's ability to precisely and
accurately measure five samples with Pb concentrations of 0 ppb, 5 ppb, 15 ppb, 25 ppb, 50 ppb,
75 ppb and 100 ppb. The samples will be analyzed in triplicate and the coefficient of
determination will be used to assess the linearity of the response of the instrument within this
range. Finally, DEI will be determined using three synthetic water samples. The first sample
will have low total dissolved solids concentration (Low TDS Water), the second high total
dissolved solids concentration (High TDS Water) and the third will contain high iron (Fe)
concentration and other dissolved solids (High Fe Water). Each of these synthetic water samples
will be split into required 100 mL subsamples and receive a Pb spike of 25 ppb and 50 ppb
before Pb is measured in triplicate from each subsample by Lead 100/AND 1000. Normal sample
preparation procedures will be followed for the Low TDS Water and High TDS Water, and a
special sample preparation procedure for the removal of Fe interference will be used to prepare
the High Fe Water sample for Pb analysis. The accuracy and precision of the instrument will be
evaluated for DEI.
The next set of tests will determine the accuracy and precision of the Lead 100/AND 1000
in recovery of Pb spikes in finished drinking water. Three sets of samples will be prepared with
Pb spikes of 25 ppb: finished drinking water samples collected from a water fountain (Water
Fountain), bottled mineral water purchased from a local supermarket (Bottled Water) and
finished drinking water collected from the effluent of a local water treatment facility treating
groundwater (Finished Well Water). All waters will be analyzed in triplicate both with and
without a Pb spike of 25 ppb.
The third series of tests aims at determining the accuracy and precision of the
Lead 100/AND 1000 in recovering Pb spikes in environmental water samples. The environmental
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water samples proposed for this study include samples collected from both freshwater and
saltwater sources. Three freshwater sources will be sampled including water collected from the
reach of a freshwater river (River Water), samples collected from a freshwater reservoir
(Reservoir Water) and raw groundwater collected at the source of a drinking water treatment
facility (Raw Well Water). For consistency and logistical simplicity, the Raw Well Water will
be collected from the source that feeds the facility from which the Finished Well Water will be
collected. In addition, one seawater sample will be collected for testing (Seawater) to determine
the accuracy and precision of the Lead 100/AND 1000 in testing natural waters with high salinity.
All four environmental samples will be analyzed in triplicate after the addition of a Pb spike to
25 ppb and one sample with no spike in the field. Performance of tests on Seawater differ from
the performance of tests on freshwater in that seawater will be diluted tenfold before being
subjected to LEAD 1007AND 1000 testing and results will be analyzed qualitatively, not
quantitatively as with freshwater samples.
The final series of tests aims at determining the accuracy and precision of the
Lead 100/AND1000 in recovering Pb spikes in wastewater effluent samples. Three samples will
be analyzed during this series of tests: two effluent samples collected from two separate
traditional activated sludge treatment facilities treating domestic wastewater (Municipal
Wastewater Effluent #1 and Municipal Wastewater Effluent #2) and a sample collected from the
effluent of a metal finishing works (Metal Finishing Wastewater Effluent). The Metal Finishing
Wastewater Effluent will be collected from a facility conforming to 40 CFR 433 and/or 40 CFR
413 after all on-site pretreatment.
All tests will be performed with the Lead 100/AND 1000 operating according to the
vendor's recommended procedures as described in the user's instructions/manual (see
Appendices A and B) and/or during training provided to the operator. Similarly, calibration and
maintenance of the technologies will be performed as specified by the vendor. Results from the
technologies being verified will be recorded in laboratory record books (LRBs) and transferred
to an appropriate electronic format (i.e., Microsoft® Excel).
A verification report describing the results obtained during the evaluation will be drafted.
In addition, a verification statement summarizing the results will be drafted. The report and
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verification statement will be reviewed by the Vendor, EPA, and the peer reviewers. In
performing the verification tests, Battelle will follow the technical and QA procedures specified
in this QAPP and comply with the data quality requirements in the AMS Center QMP^. Quality
procedures include a ISA and audits of data quality (ADQs). The Battelle QAO will perform
the ISA.
A7.2 Verification Test Schedule
Table 1 shows a general schedule of testing and data analysis/reporting activities to be
conducted in this verification test.
A7.3 Test Site Descriptions
PT (including DLOD, DLR and DEI) will be completed at Battelle's ETL according to
this QAPP.
Finished drinking water samples will be collected from three separate sources. Water
Fountain will be collected from a water fountain located within Battelle headquarters in
Columbus, OH. Battelle receives its finished drinking water from the Dublin Road Water
Purification Plant in Columbus, OH, which treats raw water from Scioto River within the city
limits. Bottled Water will be purchased from a local supermarket (e.g., Kroger, Giant Eagle) in
1-gal quantities and transferred to ETL for analysis. Finished Well Water will be collected from
a small water treatment facility at the Plainview Christian School located in Plain City, OH. An
on-site measurement will be made immediately after sample collection and a 1 L sample of the
Finished Well Water will be transferred to ETL for analysis under highly-controlled laboratory
conditions.
Environmental samples include River Water, Reservoir Water, Raw Well Water and
Seawater. River Water will be collected from the east bank of the Scioto River in Columbus,
OH, no more than 5 miles north of Griggs Reservoir (see Figure 2). The Scioto River is one of
the longest rivers in Ohio as it runs over 230 miles from Auglaize County, in the western part of
the state, through Columbus to Portsmouth where it empties into the Ohio River. Two dams
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Table 1. General Verification Test Schedule
Approximate
Month of
Completion
July
August
September
Testing Activities
• Training of Battelle VTC by vendor
• Prepare sampling and analysis equipment for
upcoming testing
• Organize shipment of Seawater and Metal
Finishing Wastewater Effluent
• Completion of performance evaluation audit
(PEA)
• Completion of initial demonstration of
capability including on-site calibration and
three point calibration
• Completion of PT including DLOD, DLR and
DEI
• Collection and testing on Water Fountain,
Bottled Water and Finished Well Water
• Completion of TSA
• Collection and testing on River Water,
Reservoir Water and Raw Well Water
• Receipt and testing on Seawater
• Collection and testing on Municipal
Wastewater Effluent #1 and Municipal
Wastewater Effluent #2
• Receipt and testing on Metal Finishing
Wastewater Effluent
• None
• None
• None
• None
• None
• None
Data Analysis and Reporting
• Prepare LRB for data recording
• Record testing data in LRB and/or data
recording forms
• Transfer testing data to electronic format
as convenient
• Record testing data in LRB
• Transfer testing data to electronic format
as convenient
• Record testing data in LRB
• Transfer testing data to electronic format
as convenient
• Record testing data in LRB
• Transfer testing data to electronic format
as convenient
• Compilation and transfer of all data to
electronic format
• Statistical analysis of data
• Draft Verification Report completed
• Draft Verification Statement completed
• Audits of data quality by Battelle QAO
• Draft Verification Report and Verification
Statement sent to Vendor
• Address reviewers comments
• Revise Verification Report and
Verification Statement
• Draft Verification Report and Verification
Statement sent to Peer Reviewers
• Address reviewers comments
• Revise Verification Report and
Verification Statement
• Draft Verification Report and Verification
Statement sent to EPA Project Office for
QA review
• Submission of final of Verification Report
and Verification Statement to EPA for
approval
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have been built on the Scioto River, both in Columbus, for drinking water and recreation
purposes^. River Water will be collected from the surface of the river no more than 1 ft below
the water surface and no more than 20 ft from the eastern shoreline. Reservoir water will be
collected from Griggs Reservoir on the Scioto River in Columbus, OH. Griggs Dam was the
first dam to be built on the Scioto River in Columbus, Ohio in 1908, which forms the Griggs
Reservoir. Griggs Reservoir is a long, narrow body of water at almost 6 miles long and 500 feet
wide with a 1.2 million gallon capacity. The Reservoir is a major drinking water source for
Columbus. Reservoir Water will be sampled from within the boundaries of Griggs Reservoir,
and, similarly to the River Water, will be sampled from the surface, no more than 1 ft below the
water surface and no more than 20 ft from the eastern shore of the reservoir (see Figure 2). Raw
Well Water will be collected from a well located in Plain City, OH. Note that this is the raw
groundwater that serves as the water source for the Plainview Christian School, the same
treatment facility that is providing Finished Well Water. The treatment system operating at the
Plainview Christian School is an on-demand coagulation/filtration system treating approximately
10 gallons per minute. Seawater will be collected from the Atlantic Ocean off West Palm Beach,
FL (see Figure 3). Seawater will be collected from the surface of the ocean no more than 1 ft
below the water surface and no more than 20 ft from the shoreline.
Wastewater effluent samples will be collected from three separate sources. Municipal
Wastewater Effluent #1 will be collected from the final effluent sampling location within the
Southerly Wastewater Treatment Plant in Columbus, OH (Southerly). Southerly, built in 1967,
is one of two treatment plants servicing Columbus, OH, located south of the city in Lockbourne,
Ohio (see Figure 2). Southerly receives and treats influent from the northeast and eastern half of
Franklin County through a series of physical and biological processes. Southerly has the capacity
to treat 114 million gallons per day (MGD) and discharges into the Scioto River. Municipal
Wastewater Effluent #2 will be collected from the final effluent sampling location within the
Jackson Pike Wastewater Treatment Plant in Columbus, OH (Jackson Pike). Jackson Pike, built
in 1935, is the original treatment plant servicing Columbus, OH and is located on the southern
limit of the city (see Figure 2). Jackson Pike receives and treats influent from the northwestern
and western half of Franklin County through a series of physical and biological processes.
Jackson Pike has the capacity to treat 68 MGD with a peak treatment capacity of 102 MGD and,
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Figure 2. Site Map Showing the Locations of Two of the Environmental Samples (River Water and
Reservoir Water) and Municipal Wastewater Effluent #1 (Jackson Pike Wastewater Treatment
Plant) and Municipal Wastewater Effluent #2 (Southerly Wastewater Treatment Plant)
Figure 3. Site Location Map Showing the Location of the Seawater Sample
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like Southerly, discharges into the Scioto River. The third effluent sample, Metal Finishing
Wastewater Effluent, will be collected by the vendor from a facility conforming to 40 CFR 433
and /or 40 CFR 413 (electroplating, electroless plating, anodizing, coating [chromating,
phospating and coloring], chemical etching and milling, and printed circuit board
manufacturing). Table 2 indicates the sampling locations and brief test site descriptions for all
samples considered in this QAPP.
A7.4 Health and Safety
Battelle will conduct all sample collection and verification testing following the safety and health
protocols in place for the locations used for testing. In addition, a job hazard analysis (JHA) will
be prepared to describe the specific hazards associated with sampling efforts and sample
handling, as well as the use of engineering controls and other procedures required to reduce the
possibility of adverse health and safety issues. These include not only the use of personal
protective equipment (e.g., lab coat, gloves, protective eyewear) but also the implementation of
engineering controls (e.g., chemical hood). Promoting awareness of safe chemical and waste
handling methods will also be emphasized. Standard Battelle JHA forms will be completed once
any potential hazardous activities are defined. The JHA forms will be physically present at the
location where verification testing is being conducted (both in the field and at ETL). All test
participants will be required to review and understand the JHA forms prior to initiating
laboratory or field work and adhere to its procedures during all verification tests. In addition, all
recommended safety procedures for the use of Vendor equipment will be discussed with an
authorized Vendor representative during the training session and diligently followed for all
activities involving the use of the Vendor equipment.
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Table 2. Sampling Locations and Descriptions
Sample Name
Water
Fountain
Bottled Water
Finished Well
Water(a)
River Water(a)
Reservoir
Water(a)
Raw Well
Water(a)
Seawater
Municipal
Wastewater
Effluent #l(a)
Municipal
Wastewater
Effluent #2(a)
Industrial
Effluent
Description
Water Fountain sample to be collected from a water fountain
within Battelle
Bottled spring water sample to be purchased in 1-gal
quantities from a local supermarket (e.g., Kroger, Giant
Eagle)
Finished well water sample to be collected from the Plainview
Christian School in Plain City, Ohio
River water sample to be collected from the surface of the
Scioto River in Columbus, OH. Sample will be collected no
more than 1 ft below the river surface and no more than 20 ft
from the eastern shoreline no more than 5 miles north of
Griggs Reservoir (see Figure 2)
Reservoir water sample to be collected from the surface of
Griggs Reservoir in Columbus, OH. Sample will be collected
no more than 1 ft below the reservoir surface and no more
than 20 ft from the eastern shoreline (see Figure 2)
Raw Well Water sample to be collected from the raw water
intake at the Plainview Christian School in Plain City, Ohio
Seawater to be collected from the surface of the Atlantic
Ocean in West Palm Beach, FL. Sample will be collected no
more than 1 ft below the ocean surface and no more than 20 ft
from the shoreline (see Figure 3)
Municipal Wastewater Effluent #1 to be collected from the
effluent sampling location at the Jackson Pike Wastewater
Treatment Facility in Columbus, OH (see Figure 2)
Municipal Wastewater Effluent #2 to be collected from the
effluent sampling location at the Southerly Wastewater
Treatment Facility in Columbus, OH (see Figure 2)
Industrial Effluent to be collected by the vendor from a
facility that has been classified as a 40 CFR 413 or 40 CFR
433. The sample will shipped to ETL in Columbus, OH
(a) Samples will be analyzed both on-site and at ETL.
A8 QUALITY OBJECTIVES AND CRITERIA FOR MEASUREMENT DATA
In performing the verification test, Battelle will follow the technical and QA/QC
procedures specified in this QAPP and comply with the data quality requirements in the AMS
Center QMP [1] and ETV QMP[2]. Data quality objectives (DQOs) have been established to
ensure that this verification test provides suitable data for a robust evaluation of performance.
The DQOs are used to develop the testing variable tolerances required to meet the objectives of
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the verification test. The DQOs for this verification test were established to assess the
performance of the Lead 1007AND 1000 and its ability to detect Pb in laboratory, environmental,
waste and drinking water effluent samples. For this verification test, the DQOs are evaluated by
the acceptance criteria determined in Section B5 to detect Pb in laboratory, environmental, waste
and drinking water effluent samples. The DQOs of this verification test are to:
• Evaluate the ability of the Lead 1007AND 1000 to accurately and precisely detect Pb
in laboratory, environmental, waste and drinking water effluent samples
• Determine the limit of detection and linear range of the Lead 100/AND 1000 for the
detection of Pb in laboratory samples
• Evaluate the effect of matrix and interfering species on the ability of the
Lead 100/AND 1000 to accurately and precisely measure Pb in laboratory,
environmental, waste and drinking water effluent samples
• Evaluate the effect of environmental control (i.e., partially-controlled field
environments vs. highly-controlled laboratory environments) on the ability of the
Lead 100/AND 1000 to accurately and precisely measure Pb in environmental and
wastewater effluent samples
Assessing the DQOs is also a key component of the ETV PEA process. The PEA will be
used to independently confirm the accuracy of the reference analytical measurements (e.g., EPA
Method 200.8).
The Battelle QAO will perform a TSA at least once during this verification test to verify
that testing and analysis were performed according to the QAPP. The EPA QM also may
conduct an independent TSA, at his/her discretion.
A9 SPECIAL TRAINING/CERTIFICATION
Documentation of training related to sample collection and handling, technology testing,
analytical method analysis, operation of ancillary equipment used to collect supporting data,
routine laboratory procedures, and reporting is maintained for all Battelle technical staff in
training files at their respective Battelle location. The Battelle QAO will verify the presence of
appropriate training records prior to the start of testing. The Vendor will train the Battelle
technical staff prior to the start of testing. Battelle will document this training with a consent
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form, signed by the Vendor or designated representative, which identifies Battelle technical staff
who have been trained to use their technologies and can train other staff. In the event that other
staff members are required to use the technologies, they will be trained by staff trained by the
Vendor. All technical staff will have a minimum of a bachelor's degree in science/engineering.
Battelle will conduct all verification testing using the engineering controls and safety
procedures described in the JHA forms and will document that all testing staff have read,
understood, and agreed to adhere to the procedures described in the JHA prior to and during
work on the test.
A10 DOCUMENTATION AND RECORDS
The documents for this verification test will include the QAPP, Vendor instructions, verification
report, verification statement, and audit report. Project records will include: LRBs and/or data
collection forms, supporting laboratory records, training records, electronic files (both raw data
and spreadsheets), JHA forms, and QA audit files. Table 3 summarizes the types of data to be
recorded. The raw and final results from the test measurements will be collected by Battelle, and
technology data will be copied from the AND 1000 fluorimeter result screen. Section BIO details
the data recording practices and responsibilities. Documentation of Battelle staff training by the
Vendor and copies of other project specific training will also be included in the project files. All
of these records will be maintained at the test site, ETL or in the VTC's office during the test and
then transferred to permanent storage at Battelle's Records Management Office (RMO) at the
conclusion of the verification test.
All data generated during the conduct of this project will be recorded directly, promptly,
and legibly in permanent ink in the LJAB and/or data collection forms. All data entries will be
dated on the date of entry and signed or initialed by the person entering the data. Any changes
will be made so as not to obscure the original entry, dated and signed or initialed at the time of
the change, and indicate the reason for the change.
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Table 3. Summary of Records to be Collected and Maintained
(a)
Record/Data
Dates, sampling
locations, times of sample
collection and test events
Test variables
Technology data
Field data
PEA records
Analytical method,
sample preparation,
sample analysis, chain of
custody, and results
Where Recorded
LRB sand/or data
collection sheets
LRB sand/or data
collection sheets
LRB sand/or data
collection sheets
LRB sand/or data
collection sheets
LRBs and/or data
collection sheets
LRB sand/or data
collection forms, chain
of custody forms, or data
acquisition system, as
appropriate
How often recorded
Start/end of each
collection event and test
run
When set or changed, or
as needed to document
notable details during
testing
During each test run
During each collection
event and field test run
Before testing begins
When test samples are
aliquoted for the analysis
and throughout sample
handling and analysis
process
Disposition of
Data
Use to organize/check test
results; manually incorporate in
data spreadsheets
Use to organize/check test
results; manually incorporate in
data spreadsheets, or visually
record test
Use to document and interpret
performance of the technology
Use to interpret performance of
the technology under specified
field conditions
Use to verify the accuracy of the
reference analytical equipment
Use to organize/check test
results; manually incorporate in
data spreadsheets; transfer to
spreadsheets/agreed upon report;
project files; retain for
documentation of analytical
method performance
(a) Battelle is responsible for collecting and maintaining all specified records.
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SECTION B
MEASUREMENT AND DATA ACQUISITION
Bl EXPERIMENTAL DESIGN OVERVIEW
This verification test is designed to evaluate the accuracy, precision, functionality and
ease-of-use of the Lead 1007AND 1000 in detecting Pb in laboratory, environmental, waste and
drinking water effluent samples including deionized (DI) water with and without interfering
species. The characteristics of independent variables have been selected and will be established
during the runs to determine the response of the dependent variables. Performance parameters
will be evaluated based on the responses of the dependent variables (i.e., comparison of the
Lead 1007AND 1000 performance to reference method performance) and used to characterize the
Lead 1007AND 1000 performance.
Dependent Variable Responses—The Lead 100/AND 1000 will be evaluated with respect
to its ability to accurately and precisely determine aqueous Pb concentrations in a variety of
water samples. Detection of aqueous Pb concentration thus represents the only quantitative
dependent variable included in the test. In addition, functionality and ease of use will be
evaluated on a subjective basis.
Independent Variable Levels—The levels of the independent variables with respect to
water samples to be tested will be the following: (1) prevailing water quality characteristics
dictated by environmental conditions (e.g., pH, major anions, major cations); and/or (2) water
quality characteristics artificially imparted on synthetic environmental or laboratory samples
including synthetic matrices and Pb spikes. Additionally, other qualitative independent variables
include operator ability and prevailing field conditions.
The verification test will consist of four portions (in addition to QA testing): (1)
performance testing (including DLOD, DLR and DEI ); (2) finished drinking water sample
testing; (3) environmental water sample testing; and (4) wastewater effluent water sample
testing. The four tests are described in further detail in the following:
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1. Performance Testing
PT is focused on initial demonstration of capability (IDC) and determination of the
inherent features and limitations of Lead 100/AND 1000. In addition to the IDC and three point
calibration (TPC), PT tests also include DLR, DLOD, and DEI. In all cases, the tests are
designed to determine the instrument response to a known concentration of aqueous Pb
contamination in controlled laboratory samples (both DI and DI with added interferences).
Instrument accuracy, precision and ease of use during aqueous Pb detection in the laboratory
samples will be determined during these tests. Before a new sample matrix is analyzed, the
Lead 100/AND1000 will be subjected to on-site calibration as outlined in the Vendor instrument
manuals. An experimental matrix for performance testing is presented as Table 4.
IDC aims at demonstrating the technology with clean samples spiked with a known
concentration of Pb. DI will be spiked with 25 ppb Pb before being analyzed with the
Lead 100/AND 1000. Further, these analyses will be carried out in triplicate to assess the
precision of the Lead 100/AND 1000.
TPC is carried out to provide a baseline calibration in DI water. Subsequent calibrations
(on-site calibrations) augment this TPC and correct measurements for matrix effects. The TPC is
stored in the Lead 100/AND 1000 and is augmented each time Pb is measured in a new matrix
(on-site calibration). The TPC consists of analyzing one sample each of DI spiked with Pb at 25
ppb, 50 ppb and 75 ppb. Initial Calibration Check (ICC) serves to confirm calibration accuracy.
DLR of the instrument will be accomplished through a series of triplicate tests on DI
spiked with Pb at six different concentrations within the purported linear range of the
Lead 100/AND 1000 (2 to 100 ppb). The six Pb concentrations specified for the DLR
experiments are 0 ppb, 5 ppb, 15 ppb, 25 ppb, 50 ppb, 75 ppb and 100 ppb. The accuracy and
precision of the instrument as well as the linearity of the concentration curve will be the
performance metrics for the DLR tests.
Limit of detection (LOD) of the Lead 100/AND 1000 has been reported by the Vendor as
2 ppb Pb and will be confirmed through a series of seven replicate tests of DI samples spiked
with one concentration of Pb at five times the purported detection limit (10 ppb).
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Table 4. Experimental Matrix and Sample Summary for PT
Test Name
Initial Demonstration of
Capability
IDC
Three-Point Calibration
TPC
Initial Calibration Check
ICC
Determination of Linear
Range
DLR
Determination of Limit of
Detection
DLOD
Determination of the
Effect of Interferences
DEI
Matrix
DI
DI
DI
DI
DI
Low TDS(a)
HighTDS(b)
Highlron(c)
Pb Spike (ppb)
25
25
50
75
25
0
5
15
25
50
75
100
10
25
50
25
50
25
50
Number of analyses
3
1
1
1
3
o
J
o
J
o
J
o
J
o
J
o
J
o
J
1
o
3
o
J
o
3
o
J
6(d)
6(d)
(b)
Low TDS water has the following makeup: 95 ppm NaHCO3, 50 ppm CaSO4, 60 ppm MgS04,4 ppm KC1 and 10 ppm
glucose.
High TDS water has the following makeup: 380 ppm NaHCO3,200 ppm CaSO4, 240 ppm MgS04, 16 ppm KC1 and 100
ppm glucose.
High Iron water has the following make-up: 1 ppm Fe, 3 ppm NaCl and 142 ppb CaSO4.
Three samples analyzed by Lead 100/AND 1000 with special pretreatment procedure for the removal of the
effects of Fe interference and three additional samples analyzed by Lead 100/AND 1000 without the special
pretreatment procedure.
The final aspect of PT is the DEI on the instrument's ability to accurately and precisely
measure Pb in aqueous samples with added interferences. Triplicate interference tests will be
carried out each on three samples of DI not only with added interferences (referred to as Low
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IDS Water, High IDS Water or High Fe Water) but also spiked with Pb in the amount of 50
ppb. The ability of the Lead 1007AND 1000 to accurately and precisely measure Pb at the
specified concentration will be the performance metric for the interference tests. The first two
samples will be analyzed after pretreatment with only the vendor-recommended buffer (required
for all samples; see Appendices A and B), while the third will be pretreated with both the
vendor-recommended buffer and a special vendor-provided pretreatment method for the removal
of effects of Fe interference. Note that an on-site calibration must be performed separately for
each of the two samples (i.e., one on-site calibration for the un-treated sample and one on-site
calibration for the treated sample). A series of three measurements will also be made on the
High Fe Water with only the vendor-provided buffer to assess the utility of the additional
pretreatment method for removal of the effects of Fe interference. The specific water makeup
of the three samples is as follows (see Section Bl.1.7 for detailed sample preparation methods):
• Low TDS Water:
o 95 ppm NaHCO3
o 50 ppm CaSO4
o 60 ppm MgS04
o 4 ppm KC1
o 10 ppm glucose
• High TDS Water:
o 380ppmNaHCO3
o 200 ppm CaSO4
o 240 ppm MgS04
o 16ppmKCl
o 100 ppm glucose
• High Iron Water:
o 1 ppm Fe
o 3 ppm NaCl
o 142 ppb CaSO4
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The tests outlined in this section do not explicitly include the QA samples required (see
Section B5). Data collected during the PT include concentration of Pb reported by the
Lead 1007AND 1000 and the reference method and qualitative data collected regarding ease of
operation.
2. Analysis of Finished Drinking Water Samples
Analyses of finished drinking water samples aims at determining the accuracy and
precision of the Lead 100/AND1000 in measuring soluble Pb in water matrices other than highly
controlled, "clean" laboratory samples, but not as complex as environmental samples. Three
samples will be analyzed in triplicate each spiked with 25 ppb Pb: Water Fountain, Bottled
Water and Finished Well Water. In addition, Finished Well Water will not only be analyzed in
triplicate ETL with a Pb spike of 25 ppb but also once in the field with no spike. Samples
collected from the treatment facility in Plain City, OH will be transferred to the ETL and
analyzed with Lead 100/AND 1000 under highly-controlled laboratory conditions to determine
the differences (if any) between the Lead 100/AND 1000 performance in the field and in the
laboratory. The tests outlined in this section are in addition to QA samples required (see Section
B5). Data collected during this phase of the test include concentration of Pb reported by
Lead 100/AND 1000 and the reference method and qualitative data collected regarding ease of
operation especially differences in ease of use between field and laboratory analyses and
difficulties encountered in field analyses (if any).
3. Analysis of Environmental Water Samples
The analysis of environmental water samples aims at determining the accuracy and
precision of the Lead 100/AND 1000 in measuring soluble Pb in water matrices naturally
occurring in the environment. Three samples will be analyzed in triplicate each spiked with 25
ppb Pb: River Water, Reservoir Water and Raw Well Water. River Water will be collected from
a reach of the Scioto River and Reservoir Water will be collected from south of the River Water
sampling location in Grigg's Reservoir (see Figure 2 for a map of sampling locations). Both
samples will be collected from the shore of the water bodies (less than 20 ft from shore). The
samples will also be collected from the surface of the water bodies (less than 1 ft depth). The
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Raw Well Water will be collected from the raw water intake tap at a small water treatment
facility at the Plainview Christian School located in Plain City, OH; note that this is the same
facility from which the Finished Well Water will be collected. The freshwater environmental
samples will be analyzed in the field without a Pb spike to determine the ability of the
Lead 100/AND 1000 to detect background Pb levels in the samples. In addition to field analyses,
both freshwater environmental samples will be transferred to the ETL with a 25 ppb Pb spike and
analyzed with Lead 100/AND 1000 identically as in the field under highly-controlled laboratory
conditions to determine differences (if any) between Lead 100/AND 1000 performance in the
field and in the laboratory. The tests outlined in this section are in addition to QA samples
required (see Section B5). Data collected during this phase of the test include concentration of
Pb reported by Lead 1007AND 1000 and the reference method and qualitative data collected
regarding ease of operation; especially differences in ease of use between field and laboratory
analyses and difficulties encountered in field analyses (if any).
In addition to the two freshwater samples, one additional sample (Seawater) will be
collected from a location off West Palm Beach, FL (see Figure 3 for the Seawater sampling
location). The Seawater sample will be collected in the same manner as the two freshwater
samples (i.e., less than 20 ft from the shoreline and less than 1 ft depth). The Seawater sample
will be shipped by overnight services to ETL where two samples will be separately spiked with
25 ppb Pb and 50 ppb Pb and analyzed by the Lead 1007AND 1000 in triplicate each to determine
the accuracy of the Lead 100/AND 1000 in recovering the Pb spike as well as the precision of the
instrument. In addition to spiked samples, Seawater will also be analyzed without a Pb spike to
determine the ability of the Lead 100/AND 1000 to detect background Pb levels in the samples.
Due to the high dissolved solids anticipated in Seawater, the results of the analysis of Seawater
(both spiked and un-spiked) will be qualitative in nature indicating whether or not the Seawater
samples have low, medium or high concentrations of Pb.
4. Analysis of Wastewater Effluent Samples
The final series of tests for the verification will be the analysis of three effluent water
samples collected from wastewater treatment operations. Two samples (Municipal Wastewater
Effluent #1 and Municipal Wastewater Effluent #2) will be collected from two separate domestic
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wastewater treatment facilities in Columbus, OH (see Figure 2 for the locations of the treatment
facilities). Municipal Wastewater Effluent #1 will be collected from the final effluent sampling
location at Jackson Pike and Municipal Wastewater Effluent #2 will be collected from the final
effluent sampling location at Southerly (see Figure 2 for a map of the facilities' locations). Due
to the nature of the Lead 100/AND 1000 and the high levels of interferences in the municipal
wastewater effluent samples, all samples will be diluted ten-fold with DI before any sample
preparation (i.e., Pb spike) or analysis. Note that dilution of Municipal Wastewater Effluent #1
raises the limit of detection from 2 ppb Pb to 20 ppb Pb for these samples. After dilution,
samples will be analyzed in the field without a Pb spike. Samples will then be transferred to the
ETL where they will be analyzed in triplicate after spiking to 25 ppb Pb.
In addition to the two municipal wastewater effluent samples (i.e., Municipal Wastewater
Effluent #1 and Municipal Wastewater Effluent #2), one industrial wastewater effluent sample
(Metal Finishing Wastewater Effluent) will be supplied by the vendor. The industrial wastewater
effluent sample will be collected from a metal finishing operation conforming to 40 CFR 433
and/or 40 CFR 413. Due to the nature of the Lead 1007 AND 1000 and the high levels of
interferences in the industrial wastewater effluent samples, Metal Finishing Wastewater Effluent
will be diluted ten-fold with DI before any sample preparation (i.e., Pb spike) or analysis
Samples will be collected by the vendor after all on-site pretreatment and shipped to ETL where
they will be spiked with 25 ppb Pb and analyzed by the Lead 100/AND 1000 in triplicate to
determine the accuracy of the Lead 100/AND 1000 in recovering the Pb spike as well as the
precision of the instrument. One additional aliquot of unspiked effluent from each facility will
be analyzed to determine the ability of the Lead 100/AND 1000 to detect background Pb levels in
each of the samples. Note that dilution of the Metal Finishing Wastewater Effluent raises the
limit of detection from 2 ppb Pb to 20 ppb Pb for these samples.
Table 5 summarizes the water samples to be tested.
Other Monitoring Data—Other variables may influence the operability of the
Lead 100/AND 1000 and information on these other variables will be collected during the tests
but not controlled. Monitoring data that will be recorded include field and laboratory
temperature, field and laboratory barometric pressure and general field conditions (e.g., weather).
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Bl.l Detailed Test Procedures
B1.1.1 Glassware
All glassware, whether used at ETL or in the field, will be purchased and cleaned before first use
and between uses with the following procedure:
1. Scrub with 1% Alconox solution in tap water
2. Triple rinse with DI
3. Soak overnight in 10% HNO3
4. Triple rinse with DI
5. Air dry for at least 8 hours
All glassware used to measure volume will be Class A and all stoppered glassware will be
equipped with ground-glass stoppers.
Bl.l.2 Reagents
All reagents not provided by the vendor will be purchased from reputable sources (e.g., Fisher
Scientific, Sigma-Aldrich) and will be accompanied with a certificate of analysis. Table 6
provides the details of reagents to be used in this verification. DI water will be obtained from
ETL and will have a resistance of >18.2 MQ.
Table 5. Sample Summary for Water Sample Testing
Test
Analysis of
Finished
Drinking
Water
Samples
Test Sample
Water Fountain
Bottled Water
Performance Parameter
• Percent recovery of 25
ppb Pb spike
• Standard deviation and
coefficient of variation
of triplicate analyses
• Percent recovery of 25
ppb Pb spike
• Standard deviation and
coefficient of variation
of triplicate analyses
Independent Variables
• Water composition
(metals and anions)
• Prevailing field
conditions (e.g.,
temperature)
• Water composition
(metals and anions)
• Prevailing field
conditions (e.g.,
temperature)
# of Analyses
4 (three 25 ppb
spikes; 1
unspiked)
4 (three 25 ppb
spikes; 1
unspiked)
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Test
Analysis of
Environmental
Water
Samples
Analysis of
Wastewater
Effluent
Samples00
Test Sample
Finished Well Water
River Water
Reservoir Water
Seawater(a)
Municipal
Wastewater Effluent
#1
Municipal
Wastewater Effluent
#2
Metal Finishing
Wastewater Effluent
Performance Parameter
• Percent recovery of 25
ppb Pb spike
• Standard deviation and
coefficient of variation
of triplicate analyses
• Percent recovery of 25
ppb Pb spike
• Standard deviation and
coefficient of variation
of triplicate analyses
• Percent recovery of 25
ppb Pb spike
• Standard deviation and
coefficient of variation
of triplicate analyses
• Percent recovery of 25
ppb Pb spike
• Standard deviation and
coefficient of variation
of triplicate analyses
• Percent recovery of 25
ppb Pb spike
• Standard deviation and
coefficient of variation
of triplicate analyses
• Percent recovery of 25
ppb Pb spike
• Standard deviation and
coefficient of variation
of triplicate analyses
• Percent recovery of 25
ppb Pb spike
• Standard deviation and
coefficient of variation
of triplicate analyses
Independent Variables
• Water composition
(metals and anions)
• Prevailing field
conditions (e.g.,
temperature)
• Water composition
(metals and anions)
• Prevailing field
conditions (e.g.,
temperature)
• Water composition
(metals and anions)
• Prevailing field
conditions (e.g.,
temperature)
• Water composition
(metals and anions)
• Prevailing field
conditions (e.g.,
temperature)
• Water composition
(metals and anions)
• Prevailing field
conditions (e.g.,
temperature)
• Water composition
(metals and anions)
• Prevailing field
conditions (e.g.,
temperature)
• Water composition
(metals and anions)
• Prevailing field
conditions (e.g.,
temperature)
# of Analyses
4 (three 25 ppb
spikes; 1 without
a Pb spike)
4 (three 25 ppb
spikes; 1 without
a Pb spike)
4 (three 25 ppb
spikes; 1 without
a Pb spike)
7 (three 25 ppb
spikes; three 50
ppb spikes; 1
unspiked at ETL)
4 (three 25 ppb
spikes; 1 without
a Pb spike)
4 (three 25 ppb
spikes; 1 without
a Pb spike)
4 (three 25 ppb
spikes; 1
unspiked at ETL)
(a)
Samples will be diluted tenfold before any sample preparation or analysis
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Table 6. Reagents Used During Verification Testing
Reagent
NIST-Traceable
Lead Solution
Sodium
Bicarbonate
Anhydrous
Calcium Sulfate
Hemihydrate
Magnesium
Sulfate Anhydrous
Potassium
Chloride
Anhydrous
Sodium Chloride
Anhydrous
Glucose aqueous
solution
Iron Solution
CAS Number
10099-74-8
144-55-8
10034-76-1
7487-88-9
7447-40-7
7647-14-5
50-99-7
7437.89-6
Description of use
Preparing lead spikes;
preparing calibration
standards; preparing PEA
standards
Preparing Low TDS and High
TDS synthetic Waters
Preparing Low TDS and High
TDS and High Fe synthetic
Waters
Preparing Low TDS and High
TDS synthetic Waters
Preparing Low TDS and High
TDS synthetic Waters
Preparing Low TDS, High
TDS and High Fe synthetic
Waters
Preparing Low TDS and High
TDS synthetic waters
Preparing High Fe Water
Purity/
Concentration
1,000 ppm
>99.7%
97%
>97%
>99%
>99%
20%w/v
1,000 ppm
Mass/Volume
100 mL
500 g
100 g
500 g
500 g
500 g
100 mL
100 mL
Vendor
Fisher
Scientific
Fisher
Scientific
Fisher
Scientific
Fisher
Scientific
Fisher
Scientific
Fisher
Scientific
Ricca
Chemical
Acros
Organics
Catalogue
Number
SL21-100
S233500
AC38535-1000
AC41348-5000
P2 17-500
S271500
R3254000100
AC19605-1000
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Bl.1.3 Laboratory Equipment
Table 7 summarizes the specifications of general laboratory equipment that will be used
throughout the verification test.
Table 7. Laboratory Equipment Used During Verification Testing
Equipment
Analytical
Balance
Drying Oven
Pipette
Stir Bars
DI Water
System
Make/Model
Sartorius Cubis
VWR1330FSM
Eppendorf Research
VWR
Barnstead Nanopure®
Diamond
Notes
iO.OOOOlg
275°C Max
1-5 mL (±0.1
mL)
1/8" diameter;
1/2" length
>18.2MQ
Bl. 1.4 Analytical Procedures
All samples analyzed by Lead 100/AND 1000 will also be analyzed by a reference method
to determine the accuracy of the Lead 100/AND 1000 in recovering Pb spikes. Pb will be
measured by ICP-MS by EPA Method 200.8 (Pb Reference Method). In addition, each of the
finished drinking water, environmental water and wastewater effluent samples will be analyzed
once for metals and cations by EPA Method 200.8 (Cation Reference Method), major anions by
EPA Method 300.1 (Anion Reference Method) and alkalinity (including total, carbonate,
bicarbonate and hydroxide alkalinity) by Standard Method 2320B (Alkalinity Reference
Method). Cation Reference Method reports the concentrations of the following species:
aluminum, antimony, arsenic, barium, beryllium, cadmium, chromium, cobalt, copper, lead,
manganese, mercury, molybdenum, nickel, selenium, silver, thallium, thorium, uranium,
vanadium and zinc. Anion Reference Method reports the concentrations of the following
species: bromide, chloride, fluoride, nitrate, nitrite, ortho-phosphate and sulfate. Samples will be
preserved as per the methods indicated and sent at 4±2°C to DHL Analytical (Round Rock, TX)
for analysis within the hold times specified by the reference methods.
The Lead 100/AND 1000 will be operated exactly as specified in the vendor-provided
"AND 1000 Fluorimeter for Water Testing User Manual" (AND-prod-1000-2-2012) and the
"Lead Testing and On-Site Calibration for Water Testing" (AND-Lead-100-02-2012) (see
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Appendices A and B). Any deviation in procedure from these documents as suggested by the
vendor will be explicitly noted in the LRB for this verification test. In addition, environmental
water testing, use of the iron interference pretreatment and three-point calibration will be carried
out as described in the appropriate solution notes (see Appendices C, D and E, respectively).
Bl.1.5 Preparation ofPb Stock Solution
A single standard solution will be used for Lead 100/AND 1000 three-point calibration,
spiking of samples and PEA and will be prepared from a NIST-traceable 1,000 ppm Pb standard
solution in 3% HNOs. The 1 ppm standard solution will be prepared by filling a 1,000 mL
volumetric flask halfway with DI water. Next, 1 mL of the 1,000 ppm Pb standard solution will
be pipetted to the volumetric flask. The volumetric flask will then be filled to the line with DI
water washing down the insides of the volumetric flask to ensure that a 1:1000 dilution is made.
The resulting solution is a 1 ppm Pb standard solution in DI water (Pb Stock Solution). All other
Pb standards will be prepared from the Pb Stock Solution. Pb Stock Solutions will be prepared
at least daily and each will be analyzed by the Pb Reference Method to ensure the ongoing
accuracy of the Pb Stock Solution.
Bl.1.6 Preparation of Pb-spiked Samples
Throughout the verification study, several spikes to 100 mL samples will be necessary in
order to prepare samples with specific Pb concentrations (depending on the test). As the required
volume for each Lead 100/AND 1000 analysis is only 5 mL, all spiked samples will be prepared
in 100 mL volumetric flasks which will be sufficient for each test. In order to determine the
volume of Pb Stock Solution to be spiked to samples, a mass balance equation was used (see
below):
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By simply multiplying the target Pb concentration (in ppb) of the 100 mL sample by
0.100 L-mL/|ig, the volume of Pb Stock Solution (in mL) to be added to the 100 mL sample is
obtained. Table 8 presents the amount of Pb Stock Solution to be spiked to each 100 mL sample
required for analysis.
Table 8. Volume of Pb Standard Solution Additions to 100 mL of Sample to Obtain
Required Pb Spike
Sample
Volume (mL)
100
100
100
100
100
100
Target Pb Concentration
(ppb)
5a
10b
15C
25d
50e
75'
Volume of Pb Stock
Solution spike (mL)
0.5
1.0
1.5
2.5
5.0
7.5
(a) ForDLR
(b) ForDLOD
(c) ForDLR
(d) For DLR, DEI, Water Fountain, Bottled Water, Finished Well Water, River Water, Reservoir Water,
Raw Well Water, Seawater, Municipal Wastewater Effluent # 1, Municipal Wastewater Effluent #2
and Metal Finishing Wastewater Effluent
(e) For DLR, DEI and Seawater
(f) For DLR
To prepare Pb-spiked samples, a 100 mL volumetric flask will be filled halfway with the
appropriate matrix (i.e., DI, finished drinking water sample, environmental sample or wastewater
effluent sample) and spiked with Pb by pipetting the appropriate amount of Pb Stock Solution to
the 100 mL flask (see Table 8). The 100 mL volumetric flask will then be filled to the line with
DI water by washing down the insides of the flask using a squirt bottle. The 100 mL volumetric
flask will be stoppered and inverted three times to ensure proper mixing. All spiked samples will
be prepared in this manner.
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B.I. 1.7 Preparation of Synthetic Waters for DEI Testing
B. 1.1.7.1 Preparation of High IDS Water
High TDS Water will be prepared in a 1 L volumetric flask. AIL volumetric flask will
be filled halfway with DI water. Approximately 10 g each of NaHCO3, CaSO4'0.5H2O, MgSO4
and KC1 will be placed in separate glass weigh dishes and dried at 105°C in the drying oven for
30 minutes. After drying, the samples will be individually removed from the drying oven. A
stock solution of 8,400 ppm NaHCOs will be prepared by weighing 8,400 mg ± 10 mg of
NaHCOs in a plastic weigh dish in the analytical balance and washed into a 1 L volumetric flask
with DO water by means of a squirt bottle. The plastic weigh dish will then be triple rinsed with
DI water by means of a squirt bottle and the rinsate also added to the 1 L volumetric flask. A
stock solution of 7,455 ppm KC1 will be prepared by weighing 7,455 mg ± 10 mg of KC1 in a
plastic weigh dish in the analytical balance and washed into a 1 L volumetric flask with DO
water by means of a squirt bottle. The plastic weigh dish will then be triple rinsed with DI water
by means of a squirt bottle and the rinsate also added to the 1 L volumetric flask. The following
will be weighed separately on individual plastic weigh dishes 202 mg ± 10 mg CaSO4»0.5H2O,
240 mg ±10 mg MgSO/t. All measured weights will be recorded in the LRB. After weighing,
the CaSO4»0.5H2O and MgSO4 samples will be washed into the 1 L volumetric flask with DI
water by means of a squirt bottle. The plastic weigh dish will then be triple rinsed with DI water
by means of a squirt bottle and the rinsate also added to the 1 L volumetric flask. After the salts
have been added to the 1 L volumetric flask, 5 mL of 20% (w/v) glucose solution will be
pipetted to the 1 L volumetric flask. Finally, 45.700 mL of the NaHCOs stock solution and
2.146 mL of the KC1 stock solution will be added to the volumetric flask. The 1 L volumetric
flask will be filled to the line with DI water before the addition of a stir bar. The High TDS
Water will then be allowed to mix by means of the magnetic stir bar for 30 minutes at 120 rpm to
ensure that the salts have dissolved. Table 9 presents the composition of the High TDS Water.
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Table 9. Composition of High TDS Water
Component
NaHC03(a)
CaSO4
MgSO4
KCltb)
Glucose(c)
Component Volume
(mL)
45.700
NA
NA
2.146
5
Component Mass
(mg)
380
200
240
16
100
Final Volume (L)
1
1
1
1
1
Component
Concentration
(ppm)
380
200
240
16
100
wNaHCO3 added as a 8,400 ppm stock solution
^ KC1 added as a 7,455 ppm stock solution
(c) Glucose added as a 20% (w/v) solution
B. 1.1.7.2 Preparation of Low TDS Water
Low TDS Water will be prepared in a 1 L volumetric flask. AIL volumetric flask will
be filled halfway with DI water. Approximately 10 g each of NaHCO3, CaSO4'0.5H2O, MgSO4
and KC1 will be placed in separate glass weigh dishes and dried at 105°C in the drying oven for
30 minutes. After drying, the samples will be individually removed from the drying oven and
weighed on a plastic weigh dish in the analytical balance to the following weights: 50 mg ± 1 mg
CaSCVO.SH^O and 60 mg ±0.1 mg MgSO/i. The measured weights will be recorded in the
LRB. After weighing, each sample will be washed into the 1 L volumetric flask with DI water
by means of a squirt bottle. The plastic weigh dish will then be triple rinsed with DI water by
means of a squirt bottle and the rinsate also added to the 1 L volumetric flask. After the salts
have been added to the 1 L volumetric flask, 0.5 mL of 20% (w/v) glucose solution will be
pipetted to the 1 L volumetric flask. Finally, 11.400 mL of the NaHCCb stock solution and
0.537 mL of the KC1 stock solution will be added to the volumetric flask. The 1 L volumetric
flask will be filled to the line with DI water before the addition of a stir bar. The Low TDS
Water will then be allowed to mix by means of the magnetic stir bar for 30 minutes at 120 rpm to
ensure that the salts have dissolved. Table 10 presents the composition of the Low TDS Water.
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Table 10. Composition of Low TDS Water
Component
NaHC03(a)
CaS04
MgSO4
KCl(b)
Glucose(c)
Component Volume
(mL)
NA
NA
NA
NA
5
Component Mass
(mg)
95
50
60
4
10
Final Volume (L)
1
1
1
1
1
Component
Concentration
(ppm)
95
50
60
4
10
(a)NaHCO3 added as a 8,400 ppm stock solution
(b:i KC1 added as a 7,455 ppm stock solution
(c) Glucose added as a 20% (w/v) solution
B.I. 1.7.3 Preparation of High Fe Water
The salts of the High Fe Water will be prepared in a 1 L volumetric flask at one hundred
times concentration and diluted by pipetting 10 mL of the concentrated solution to a 1 L
volumetric flask. Fe will then be added by means of a 1000 ppm solution before filling to the
line (1 mL of 1000 ppm Fe solution diluted to 1 L). For preparation of the one hundred-times
concentrated salt solution, a 1 L volumetric flask will be filled halfway with DI water.
Approximately 1 g each of NaCl and CaSC>4 will be placed in separate glass weigh dishes and
dried at 105°C in the drying oven for 30 minutes. After drying, the samples will be individually
removed from the drying oven and weighed on a plastic weigh dish in the analytical balance to
the following weights: 300 mg ± 10 mg NaCl and 14.2 mg ± 1 mg CaSO4»0.5H2O . The
measured weights will be recorded in the LRB. After weighing, each sample will be washed into
the 1 L volumetric flask with DI water by means of a squirt bottle. The plastic weigh dish will
then be triple rinsed with DI water by means of a squirt bottle and the rinsate also added to the 1
L volumetric flask. The volumetric flask will be filled to the line with DI water before the
addition of a stir bar and then be allowed to mix by means of the magnetic stir bar for 30 minutes
at 120 rpm to ensure that the salts have dissolved. 10 mL of the solution will then be pipetted to
a separate 1 L volumetric flask pre-filled halfway with DI water. 1 mL of 1,000 ppm Fe solution
will be pipetted to the volumetric flask (1 mg Fe) and the flask will be filled to the line and
inverted 16 times to ensure proper mixing. Table 11 presents the composition of the High Fe
Water.
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The pH of the High Fe Water will be confirmed by the pH Meter and the pH will be
recorded in the LRB. Depending on the pH of the High Fe Solution, pH adjustment may be
necessary as described in the vendor-provided literature.
Table 11. Composition of High Fe Water
Component
NaClw
CaSO4w
Few
Component Volume
(mL)
NA
NA
1
Component Mass
(mg)
3
0.142
1
Final Volume (L)
1
1
1
Component
Concentration
(ppm)
95
0.142(c)
1
Diluted from a one hundred-times concentrated stock solution; 10 mL concentrated stock to 1000 mL final volume
(b:i Diluted from a one hundred-times concentrated stock solution; 10 mL concentrated stock to 1000 mL final volume
(c) Equivalent to 100 ppb SO4
(d) Fe added from a 1,000 ppm solution in 3% HNO3
Bl.1.8 Sequence of Procedures
The entire verification test will be conducted over a period of four working days; Table 12
indicates the experimental matrix for the verification test.
B 1.1.8.1 IDC Testing
IDC testing will be carried out at ETL. IDC-25 will be prepared by spiking DI water to
25 ppb Pb before it is analyzed in triplicate by the Lead 100/AND 1000 as per vendor-provided
manuals and guidance given during training. Results obtained from the Lead 100/AND 1000
analysis will be promptly recorded in the LRB. The remainder of the IDC-25 sample will be
filtered through a 0.20 jim Nylon filter into a properly labeled and preserved sample bottle
provided by DHL Analytical and stored at 4±2°C until it is sent for Pb Reference Analysis.
B 1.1.8.2 TPC Testing
TPC testing will be carried out at ETL. TPC-25 will be prepared by spiking DI water to
25 ppb Pb. Similarly, TPC-50 and TPC-75 will be prepared by spiking DI water to 50 ppb Pb
and 75 ppb Pb, respectively. Each of the TPC samples will be analyzed once by the
Lead 100/AND 1000 and results recorded in LRB. If TPC samples have a recovery within 85 -
115%, then a TPC will not be stored in the AND 1000 and factory calibration will be used for
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Table 12. Verification Schedule and Test Matrix"
Test
Day
1
2
3
4
Test Name
IDC
TPC
ICC
DLOD
DLR
DEI
Finished
Drinking
Water
Samples
Environmental
Water
Samples
Wastewater
Effluent Water
Samples'1
Sample
Name
IDC-25
TPC-25
TPC-50
TPC-75
ICC-25
DLOD- 10
DLR-5
DLR- 15
DLR-25
DLR-50
DLR-75
DLR- 100
HLDS-0
HLDS-25
HLDS-50
LLDS-0
LLDS-25
LLDS-50
HFe-0
HFe-25
HFe-50
WF-0
WF-25
BW-0
BW-25
FWW-0
FWW-25
RWW-0
RWW-25
ReW-0
ReW-25
RiW-0
RiW-25
SW-0
SW-25
SW-50
MWWE#1-
0
MWWE#1-
25
MWWE#2-
0
MWWE#2-
25
MFWWE-
0
MFWWE-
25
Matrix
DI
DI
DI
DI
DI
High LDS
Water
Low LDS
Water
High Fe
Water
Water
Fountain
Bottled
Water
Finished
Well Water
Raw Well
Water
Reservoir
Water
River
Water
Seawater
Municipal
Wastewater
Effluent
#le
Municipal
Wastewater
Effluent
#2f
Metal
Finishing
Wastewater
Effluent8
Pb
Spike
(ppb)
25
25
50
75
25
10
5
15
25
50
75
100
0
25
50
0
25
50
0
25
50
0
25
0
25
0
25
0
25
0
25
0
25
0
25
50
0
25
0
25
0
25
AND1000
Analyses
3
1
1
1
3
7
3
3
3
3
3
3
1
3
3
1
3
3
2b
6b
6b
1
3
1
3
2C
3
T
3
2C
3C
2C
3C
1
3
3
T
3
T
3
1
3
Pb
Reference
Analyses
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
Cations
Reference
Analyses
0
0
0
0
0
0
0
0
0
0
0
0
1
0
0
1
0
0
1
0
0
1
0
1
0
1
0
1
0
1
0
1
0
1
0
0
1
0
1
0
1
0
Anions
Reference
Analyses
0
0
0
0
0
0
0
0
0
0
0
0
1
0
0
1
0
0
1
0
0
1
0
1
0
1
0
1
0
1
0
1
0
1
0
0
1
0
1
0
1
0
Alkalinity
Reference
Analyses
0
0
0
0
0
0
0
0
0
0
0
0
1
0
0
1
0
0
1
0
0
1
0
1
0
1
0
1
0
1
0
1
0
1
0
0
1
0
1
0
1
0
a. Does not include all required QA samples. Required QA samples are discussed in Section B1.
b. Lhree samples analyzed by LeadlOO/ANDlOOO with special pretreatment procedure for the removal of the effects of Fe
interference and three additional samples analyzed by LeadlOO/ANDlOOO without the special pretreatment procedure.
c. Lwo sets of samples analyzed by LeadlOO/ANDlOOO each in the field and at ELL.
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d. All Wastewater Effluent Samples diluted 1:10 in DI water and filtered through a 0.20 \im Nylon filter before addition of Pb
spike.
e. Obtained from Jackson Pike Wastewater Treatment Plant (Columbus, OH).
f Obtained from Southerly Wastewater Treatment Plant (Columbus, OH).
g. Provided by vendor from 40 CFR 433/413 facility after all on-site treatment, properly labeled and preserved sample bottle
provided by DHL Analytical and properly stored until they are sent for Pb Reference Analysis.
ICC, DLOD, DLR tests. If recovery is outside this range, then TPC will be stored in AND 1000
as per vendor provided literature. In any case, results obtained from the Lead 100/AND 1000
analysis will be promptly recorded in the LRB. The remainder of the TPC samples will be
filtered through a 0.20 jim Nylon syringe filter into a properly labeled and preserved sample
bottles provided by DHL Analytical and properly stored until they are sent for Pb Reference
Analysis.
B 1.1.8.3 ICC Testing
ICC testing will be carried out at ETL. ICC-25 will be prepared by spiking DI water to
25 ppb Pb before it is analyzed in triplicate by the Lead 1007AND 1000 as per vendor-provided
manuals and guidance given during training. Results obtained from the Lead 100/AND 1000
analysis will be promptly recorded in the LRB. The remainder of the ICC-25 sample will be
filtered through a 0.20 jim Nylon syringe filter into a properly labeled and preserved sample
bottle provided by DHL Analytical and properly stored until they are sent for Pb Reference
Analysis.
B 1.1.8.4 DLOD Testing
DLOD testing will be carried out at ETL. DLOD-10 will be prepared by spiking DI
water to 10 ppb Pb before it is analyzed in septuple! by the Lead 1007AND 1000 per vendor-
provided manuals and guidance given during training. Results obtained from the
Lead 100/AND 1000 analysis will be promptly recorded in the LRB. The remainder of the
DLOD-10 sample will be filtered through a 0.20 jim Nylon filter into a properly labeled and
preserved sample bottle provided by DHL Analytical and properly stored until it is sent for Pb
Reference Analysis. Note that the reported LOD is applicable only for the matrix under
investigation and does not apply to the other matrices evaluated in this QAPP.
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B. 1.1.8.5 DLR Testing
DLR testing will be carried out at ETL. DLR-5 will be prepared by spiking DI water to 5
ppb Pb. Similarly, DLR-15, DLR-25, DLR-50, DLR-75 and DLR-100 will be prepared by
spiking DI water to 15 ppb Pb, 25 ppb Pb, 50 ppb Pb, 75 ppb and 100 ppb Pb, respectively. Each
of the DLR samples will be analyzed in triplicate by the Lead 100/AND 1000 as per vendor-
provided manuals and guidance given during training. Results obtained from the
Lead 100/AND 1000 analysis will be promptly recorded in the LRB. The remainder of the DLR
samples will be filtered through a 0.20 jim Nylon filter into a properly labeled and preserved
sample bottle provided by DHL Analytical and properly stored until they are sent for Pb
Reference Analysis.
B.I. 1.8.6 DEI Testing
DEI testing includes testing the accuracy and precision of Lead 100/AND 1000 on three
different synthetic waters (High TDS Water, Low TDS Water and High Fe Water). The methods
for preparing these waters can be found in Section B1.1.7.
DEI testing on High TDS Water will be carried out at ETL. HTDS-25 and HTDS-50 will
be prepared by spiking High TDS Water to 25 ppb Pb and 50 ppb Pb, respectively, before they
are analyzed in triplicate by the Lead 1007AND 1000 as per vendor-provided manuals and
guidance given during training. Results obtained from the Lead 100/AND 1000 analysis will be
promptly recorded in the LRB. The remainder of the HTDS-25 and HTDS-50 samples will be
filtered through a 0.20 jim Nylon filter into two separate properly labeled and preserved sample
bottles provided by DHL Analytical and stored at 4±2°C until they are sent for Pb Reference
Analysis, Cation Reference Analysis, Anion Reference Analysis and Alkalinity Reference
Analysis.
DEI testing on Low TDS Water will be carried out at ETL. LTDS-25 and LTDS-50 will
be prepared by spiking Low TDS Water to 25 ppb Pb and 50 ppb Pb, respectively before they are
analyzed in triplicate by the Lead 1007AND 1000 as per vendor-provided manuals and guidance
given during training. Results obtained from the Lead 100/AND 1000 analysis will be promptly
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recorded in the LRB. The remainder of the LTDS-25 and LTDS-50 samples will be filtered
through a 0.20 jim Nylon filter into two separate properly labeled and preserved sample bottles
provided by DHL Analytical and stored at 4±2°C until they are sent for Pb Reference Analysis,
Cation Reference Analysis, Anion Reference Analysis and Alkalinity Reference Analysis.
DEI testing on High Fe Water will be carried out at ETL. HFe-25 and HFe-50 will be
prepared by spiking High Fe Water to 25 ppb Pb and 50 ppb, respectively, before they are
analyzed in triplicate each by the Lead 100/AND 1000 as per vendor-provided manuals and
guidance given during training. Two sets of triplicate experiments will be carried out: one using
a special vendor-recommended pretreatment method for removal of Fe interference and one
using the standard pretreatment method. Results obtained from the Lead 1007AND 1000 analysis
will be promptly recorded in the LRB. The remainder of the HFe-25 and HFe-50 samples will
be filtered through a 0.20 jim Nylon filter into two separate properly labeled and preserved
sample bottles provided by DHL Analytical and stored at 4±2°C until they are sent for Pb
Reference Analysis, Cation Reference Analysis, Anion Reference Analysis and Alkalinity
Reference Analysis.
B 1.1.8.7 Finished Drinking Water Testing
Finished drinking water testing includes testing the accuracy and precision of the
Lead 100/AND 1000 on three different finished drinking waters (Water Fountain, Bottled Water
and Finished Well Water).
Water Fountain will be collected from a water fountain within Battelle. The water
fountain will be activated and water will be allowed to flow through the tap for 60 seconds (1-2
L throughput) before samples are collected in a 1 L high-density polyethylene (HOPE) container.
Water Fountain will be collected in a manner to avoid sample agitation and entrainment of air.
The 1 L sample collection container will be sealed and transported to ETL where it will be
subsampled to two 100 mL volumetric flasks. WF-25 will be prepared by spiking Water
Fountain to 25 ppb Pb before it is analyzed in triplicate by the Lead 1007AND 1000 as per vendor-
provided manuals and guidance given during training. Results obtained from the
Lead 100/AND 1000 analysis will be promptly recorded in the LRB. The remainder of the WF-
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25 sample will be filtered through a 0.20 jim Nylon filter into a properly labeled and preserved
sample bottle provided by DHL Analytical and stored at 4±2°C until it is sent for Pb Reference
Analysis. In addition the 100 mL sample without the Pb spike (WF-0) will be analyzed once by
the Lead 100/AND 1000 and the remainder of the sample will be filtered through a 0.20 jim
Nylon filter into two separate properly labeled and preserved sample bottles provided by DHL
Analytical and stored at 4±2°C until they are sent for Pb Reference Analysis, Cation Reference
Analysis, Anion Reference Analysis and Alkalinity Reference Analysis.
Bottled Water is a 1 gal sample of spring water obtained from a local supermarket in
Columbus, OH (e.g., Kroger, Giant Eagle). The 1 gal Bottled Water will be transported to ETL
where it will be subsampled to two 100 mL volumetric flasks. BW-25 will be prepared by
spiking one of the 100 mL samples to 25 ppb Pb before it is analyzed in triplicate by the
Lead 1007AND 1000 as per vendor-provided manuals and guidance given during training. Results
obtained from the Lead 100/AND 1000 analysis will be promptly recorded in the LRB. The
remainder of the BW-25 sample will be filtered through a 0.20 jim Nylon filter into a properly
labeled and preserved sample bottle provided by DHL Analytical and stored at 4±2°C until it is
sent for Pb Reference Analysis. In addition, the 100 mL sample without the Pb spike (BW-0)
will be analyzed once by the Lead 100/AND 1000 and the remainder of the sample will be filtered
through a 0.20 jim Nylon filter into two separate properly labeled and preserved sample bottles
provided by DHL Analytical and stored at 4±2°C until they are sent for Pb Reference Analysis,
Cation Reference Analysis, Anion Reference Analysis and Alkalinity Reference Analysis.
Finished Well Water will be collected from the effluent sample tap at a small water
treatment facility at the Plainview Christian School located in Plain City, OH. The effluent
sample tap will be opened and water will be allowed to flow through the tap for 60 seconds
(approximately 40 L throughput) before samples are collected in a 1 L HOPE container.
Finished Well Water will be collected in a manner to avoid sample agitation and entrainment of
air. FWW-0 (Finished Well Water with no Pb spike) will be analyzed onsite once by the
Lead 1007AND 1000 as per vendor-provided manuals and guidance given during training. Results
obtained from the Lead 100/AND 1000 analysis will be promptly recorded in the LRB. The
remainder of the FWW-0 sample will be filtered through a 0.20 jim Nylon filter into a properly
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labeled and preserved sample bottle provided by DHL Analytical and stored at 4±2°C until it is
sent for Pb Reference Analysis, Cation Reference Analysis, Anion Reference Analysis and
Alkalinity Reference Analysis. The remainder of the 1 L sample will be transported to ETL
where FWW-0 will be analyzed once by Lead 100/AND 1000 and FWW-25 will be prepared and
analyzed in triplicate. The remainder of the FWW-25 sample will be filtered through a 0.20 jim
Nylon filter into a properly labeled and preserved sample bottle provided by DHL Analytical and
stored at 4±2°C until it is sent for Pb Reference Analysis. Any differences in results between
field and ETL measurements as well as any subjective data concerning ease of use in the field
compared to ETL will be noted in the LRB.
B1.1.8.8 Environmental Water Testing
Environmental water testing includes testing the accuracy and precision of
Lead 100/AND 1000 on four different environmental waters (Raw Well Water, Reservoir Water,
River Water and Seawater).
Raw Well Water will be collected from the raw water intake tap at a small water
treatment facility at the Plainview Christian School located in Plain City, OH; note that this is the
same facility from which the Finished Well Water will be collected. The raw water intake will
be activated and water will be allowed to flow through the tap for 60 seconds (approximately 40
L throughput) before samples are collected in a 1 L HOPE container. Raw Well Water will be
collected in a manner to avoid sample agitation and entrainment of air. RWW-0 (Raw Well
Water with no Pb spike) will be analyzed onsite once by the Lead 100/AND 1000 as per vendor-
provided manuals and guidance given during training. Results obtained from the
Lead 100/AND 1000 analysis will be promptly recorded in the LRB. The remainder of the
RWW-0 sample will be filtered through a 0.20 jim Nylon filter into a properly labeled and
preserved sample bottle provided by DHL Analytical and stored at 4±2°C until it is sent for Pb
Reference Analysis, Cation Reference Analysis, Anion Reference Analysis and Alkalinity
Reference Analysis. The remainder of the 1 L sample will be transported to ETL where RWW-0
will be analyzed once by Lead 100/AND 1000 and RWW-25 will be prepared and analyzed in
triplicate. The remainder of the RWW-25 sample will be filtered through a 0.20 jim Nylon filter
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into a properly labeled and preserved sample bottle provided by DHL Analytical and stored at
4±2°C until it is sent for Pb Reference Analysis. Any differences in results between field and
ETL measurements as well as any subjective data concerning ease of use in the field compared to
ETL will be noted in the LRB.
Reservoir Water will be collected from the surface of Grigg's Reservoir on the Scioto
River in Columbus, OH (see Figure 2 for sampling location). The sample will be collected by
means of a retractable pole with an attached 1 L HOPE sample collection container. The sample
pole will be extended to its full length (-20 ft) and a sample will be collected from the surface
(no more than 1 ft below water surface) of the reservoir. The sample pole will be retracted and
brought to the reservoir shore. ReW-0 (Reservoir Water with no Pb spike) will be analyzed
onsite once by the Lead 1007AND 1000 as per vendor-provided manuals and guidance given
during training. Results obtained from the Lead 100/AND 1000 analysis will be promptly
recorded in the LRB. The remainder of the ReW-0 sample will be filtered through a 0.20 jim
Nylon filter into a properly labeled and preserved sample bottle provided by DHL Analytical and
stored at 4±2°C until it is sent for Pb Reference Analysis, Cation Reference Analysis, Anion
Reference Analysis and Alkalinity Reference Analysis. The remainder of the 1 L sample will be
transported to ETL where ReW-0 will be analyzed once by Lead 1007AND 1000 and ReW-25 will
be prepared and analyzed in triplicate. The remainder of the ReW-25 sample will be filtered
through a 0.20 jim Nylon filter into a properly labeled and preserved sample bottle provided by
DHL Analytical and stored at 4±2°C until it is sent for Pb Reference Analysis. Any differences
in results between field and ETL measurements as well as any subjective data concerning ease of
use in the field compared to ETL will be noted in the LRB.
River Water will be collected from the surface of the Scioto River in Columbus, OH (see
Figure 2). The sample will be collected in a manner identical to that for the Reservoir Water
sample by means of a retractable pole with an attached 1 L HOPE sample collection container.
RiW-0 (River Water with no Pb spike) will be analyzed onsite once by the Lead 100/AND 1000
as per vendor-provided manuals and guidance given during training. Results obtained from the
Lead 100/AND1000 analysis will be promptly recorded in the LRB. The remainder of the RiW-0
sample will be filtered through a 0.20 jim Nylon filter into a properly labeled and preserved
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sample bottle provided by DHL Analytical and stored at 4±2°C until it is sent for Pb Reference
Analysis, Cation Reference Analysis, Anion Reference Analysis and Alkalinity Reference
Analysis. The remainder of the 1 L sample will be transported to ETL where RiW-0 will be
analyzed once by Lead 100/AND 1000 and RiW-25 will be prepared and analyzed in triplicate.
The remainder of the RiW-25 sample will be filtered through a 0.20 jim Nylon filter into a
properly labeled and preserved sample bottle provided by DHL Analytical and stored at 4±2°C
until it is sent for Pb Reference Analysis. Any differences in results between field and ETL
measurements as well as any subjective data concerning ease of use in the field compared to ETL
will be noted in the LRB.
Seawater will be collected in two separate 1 L HOPE sample bottles from the shore of
West Palm Beach, FL (see Figure 3 for sampling location) no more than 20 ft from the shoreline
and no more than 1 ft depth. Two Seawater samples will be collected for redundancy, however,
only one of the samples will be used for testing. The samples will be sealed and placed in a
cooler with ice and transported to ETL. Upon receipt, the Seawater sample will be opened and
the temperature measured to ensure that the sample remained at 4±2°C during transit. The
sample will then be allowed to warm to ambient temperature before further testing. Seawater
samples will be diluted 1:10 in DI water and filtered through a 0.20 jim Nylon filter before
analysis.
SW-25 and SW-50 will be prepared by spiking Seawater to 25 ppb Pb and 50 ppb Pb,
respectively, before they are analyzed in triplicate each by the Lead 1007AND 1000 as per vendor-
provided manuals and guidance given during training. Results obtained from the
Lead 100/AND 1000 analysis will be promptly recorded in the LRB. The remainder of both the
SW-25 and SW-50 samples will be separately filtered through a 0.20 jim Nylon filter into
separate properly labeled and preserved sample bottles provided by DHL Analytical and stored
at 4±2°C until they are sent for Pb Reference Analyses. In addition, a 100 mL sample without
the Pb spike (SW-0) will be analyzed once by the Lead 100/AND 1000 and the remainder of the
sample will be filtered through a 0.20 jim Nylon filter into two separate properly labeled and
preserved sample bottles provided by DHL Analytical and stored at 4±2°C until they are sent for
Pb Reference Analysis, Cation Reference Analysis, Anion Reference Analysis and Alkalinity
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Reference Analysis. The Lead 100/AND 1000 analyses of Seawater samples will be considered a
qualitative test and will not be subjected to the rigorous statistical analysis of the other samples
(see SectionB 1.2).
B1.1.8.9 Wastewater Effluent Water Samples
Wastewater effluent testing includes testing the accuracy and precision of
Lead 100/AND 1000 on three different wastewater effluent waters (Municipal Wastewater
Effluent #1, Municipal Wastewater Effluent #2 and Metal Finishing Wastewater Effluent). All
three of the wastewater effluent water samples will be diluted 1:10 in DI water and filtered
through a 0.20 jim Nylon filter before analysis.
Municipal Wastewater Effluent #1 will be collected from the effluent sampling location
tap at Jackson Pike (see Figure 2 for facility location). Municipal Wastewater Effluent #1 will
be collected in a 1 L HOPE container. AIL volumetric flask will be filled halfway with DI
water and 100 mL of the Municipal Wastewater Effluent #1 sample will then be pipetted to the
volumetric flask; the flask will be filled to the line resulting in a 1:10 dilution of Municipal
Wastewater Effluent #1. Note that dilution of Municipal Wastewater Effluent #1 raises the limit
of detection from 2 ppb Pb to 20 ppb Pb for these samples. MWWE#1-0 (Municipal Wastewater
Effluent with no Pb spike) will be analyzed onsite once by the Lead 100/AND 1000 as per
vendor-provided manuals and guidance given during training. Results obtained from the
Lead 100/AND 1000 analysis will be promptly recorded in the LRB. The remainder of the
MWWE#1-0 sample will be filtered through a 0.20 jim Nylon filter into a properly labeled and
preserved sample bottle provided by DHL Analytical and stored at 4±2°C until it is sent for Pb
Reference Analysis, Cation Reference Analysis, Anion Reference Analysis and Alkalinity
Reference Analysis. The remainder of the 1 L sample will be transported to ETL where
MWWE#1-0 will be analyzed once by Lead 100/AND1000 and MWWE#l-25 will be prepared
and analyzed in triplicate. The remainder of the MWWE#l-25 sample will be filtered through a
0.20 jim Nylon filter into a properly labeled and preserved sample bottle provided by DHL
Analytical and stored at 4±2°C until it is sent for Pb Reference Analysis. Any differences in
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results between field and ETL measurements as well as any subjective data concerning ease of
use in the field compared to ETL will be noted in the LRB.
Municipal Wastewater Effluent #2 will be collected from the effluent sampling location
tap at the Southerly Wastewater Treatment Plant in Columbus, OH (see Figure 2). Municipal
Wastewater Effluent #2 will be collected in a 1 L HDPE container. AIL volumetric flask will
be filled halfway with DI water and 100 mL of the Municipal Wastewater Effluent #2 sample
will then be pipetted to the volumetric flask; the flask will be filled to the line resulting in a 1:10
dilution of the Municipal Wastewater Effluent #2. Note that dilution of Municipal Wastewater
Effluent #2 raises the limit of detection from 2 ppb Pb to 20 ppb Pb for these samples.
MWWE#2-0 (Municipal Wastewater Effluent with no Pb spike) will be analyzed onsite once by
the Lead 1007AND 1000 as per vendor-provided manuals and guidance given during training.
Results obtained from the Lead 100/AND 1000 analysis will be promptly recorded in the LRB.
The remainder of the MWWE#2-0 sample will be filtered through a 0.20 jim Nylon filter into a
properly labeled and preserved sample bottle provided by DHL Analytical and stored at 4±2°C
until it is sent for Pb Reference Analysis, Cation Reference Analysis, Anion Reference Analysis
and Alkalinity Reference Analysis. The remainder of the 1 L sample will be transported to ETL
where MWWE#2-0 will be analyzed once by Lead 1007AND 1000 and MWWE#2-25 will be
prepared and analyzed in triplicate. The remainder of the MWWE#2-25 sample will be filtered
through a 0.20 jim Nylon filter into a properly labeled and preserved sample bottle provided by
DHL Analytical and stored at 4±2°C until it is sent for Pb Reference Analysis. Any differences
in results between field and ETL measurements as well as any subjective data concerning ease of
use in the field compared to ETL will be noted in the LRB.
Metal Finishing Wastewater Effluent will be collected by the vendor from a metal
finishing facility conforming to 40 CFR 433 and/or 40 CFR413 in a 1 L HDPE sample collection
bottle and sent on ice to ETL. The method of sampling will be documented by the vendor and
provided to Battelle. Upon arrival, the sample bottle will be opened and the temperature of the
sample will be confirmed. MFWWE-25 will be prepared by spiking Metal Finishing Wastewater
Effluent to 25 ppb Pb before it is analyzed in triplicate by the Lead 100/AND 1000 as per vendor-
provided manuals and guidance given during training. Results obtained from the
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Lead 100/AND 1000 analysis will be promptly recorded in the LRB. The remainder of the
MFWWE-25 sample will be filtered through a 0.20 jim Nylon filter into a properly labeled and
preserved sample bottle provided by DHL Analytical and stored at 4±2°C until it is sent for Pb
Reference Analysis. In addition a sample of Metal Finishing Wastewater Effluent without the Pb
spike (MFWWE-0) will be analyzed twice (once with a pretreatment method for the removal of
Fe interference and once without) by the Lead 100/AND 1000 and the remainder of the sample
will be filtered through a 0.20 jim Nylon filter into two separate properly labeled and preserved
sample bottles provided by DHL Analytical and stored at 4±2°C until they are sent for Pb
Reference Analysis, Cation Reference Analysis, Anion Reference Analysis and Alkalinity
Reference Analysis.
B1.2 Statistical Analysis
Where appropriate, the following statistical analyses will be carried out on results from
both the Lead 1007AND 1000 and the reference method. In all cases, appropriate statistical
analyses will be reported for each analysis and the results of those statistical analyses will be
used to quantitatively determine the performance of Lead 100/AND 1000 under different analysis
scenarios. The only exception to this are the Seawater-derived samples (i.e., SW-25 and SW-
50), the results of analyses of which are considered qualitative.
B1.2.1 Accuracy
Accuracy of the Lead 100/AND1000 will be assessed by comparing Pb values obtained
from the Lead 100/AND 1000 (PbANo) and those reported by the Pb Reference Analysis (PbREr)
on the same samples. The relative percent difference (RPD) between the two measurements will
serve as a quantitative measure of the accuracy of the Lead 100/AND 1000 as detailed in Equation
1.
Equation 1:
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RPD will be reported for all Lead 1007AND 1000 and Pb reference measurement pairs of data and
will be summarized by an average value, however, results from Seawater will be reported
qualitatively as high, medium or low Pb concentrations.
RPD will also be calculated between the LFM and LFMD when determining whether to
accept an on-site calibration according to the control charts. RPD as defined by the equation
below provides a measure of the agreement between the LFM and LFMD.
Percent recovery will also be calculated for the LFM and LFMD when determining whether to
accept an on-site calibration according to the control charts. Percent recovery is calculated as
shown below for the LFM.
Where s is a dilution correction, P^LFM is the ANDalyze meter reading for the LFM and Pbo is
the ANDalyze meter reading for the un-spiked sample (if the reading is "Below Limit" a value of
0 ppb will be used). The LFM spike is 25 ppb Pb,
Bl.2.2 Precision
Precision of the Lead 100/AND1000 will be assessed by comparing the spread of Pb
concentration data obtained by Lead 100/AND 1000 on triplicate samples. Precision will be
expressed quantitatively through the standard deviation (SD) and the coefficient of variation
(CV).
The SD of triplicate samples Si, 82 and 83 will be computed as expressed in Equation 2.
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Equation 2:
where |i is the mean value of the three samples expressed in Equation 3.
Equation 3:
The CV of triplicate samples Si, 82 and 83 will be computed as expressed in Equation 4.
Equation 4:
The mean, SD and CV will be reported for all triplicate samples analyzed by
LeadlOO/ANDlOOO.
Bl.2.3 Linearity of Response
During the DLR testing, a series of samples with known concentrations of Pb will be
analyzed in triplicate by Lead 1007AND 1000 (0 ppb, 5 ppb, 15 ppb, 25 ppb, 50 ppb, 75 ppb and
100 ppb). In addition to the accuracy and precision of the instrument for these tests, linearity
shall be assessed by linear regression, with the analyte concentration measured by the reference
method as the independent variable and the reading from Lead 1007AND 1000 as the dependent
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variable. Linearity is expressed in terms of slope, intercept and the coefficient of determination
(r2) as calculated by Microsoft® Excel standard computation tools.
Bl.2.4 Limit of Detection
The LOD for the Lead 100/AND 1000 shall be assessed from seven replicate analyses of a
fortified sample with an analyte concentration of five times the vendor's estimated detection
limit. In the case of the Lead 100/AND 1000, the vendor's estimated detection limit is 2 ppb.
Thus, the LOD tests will be carried out on 2 ppb Pb * 5 = 10 ppb Pb samples as described in
Section Bl.1.8.4. The LOD is calculated from Equation 5.
Equation 5:
where t is the Student's t-test value for a 99% confidence interval and SD is the standard
deviation of the replicate samples.
B1.3 Reporting
The data obtained in the verification test will be reported and the statistical analyses
described above will be conducted separately for each analysis. Information on the performance
parameters will be compiled, and a verification test report will be prepared. The report will show
verification results from the Lead 1007AND 1000, the test procedures and test data, as well as the
results of the statistical evaluation of those data.
All actions taken on the technology (such as maintenance, cleaning, and calibration) will
be documented at the time of the test and reported. In addition, descriptions of the data-
recording procedures, use of vendor-supplied software, and water samples or other consumables
used will be presented in the report. The verification test report will briefly describe the ETV
program, the AMS Center, and the procedures used in verification testing. The results of the
verification test will then be stated quantitatively (or in the case of Seawater analysis,
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qualitatively) without comparison to any other technology or comment on the acceptability of the
technology performance.
B2 SAMPLING METHODS REQUIREMENTS
B2.1 Sample Collection, Storage and Shipment
All samples will be collected in 1 L HDPE sample containers. If samples are to be
transported over a period of more than 12 hours, they will be placed in a cooler on ice, or by
some other means maintained at 0 to 4±2°C until they are received at their final destination.
Before samples are subsampled, analyzed or in any way manipulated (with the exception of
confirming the sample temperature upon receipt), they will be allowed to equilibrate with
ambient conditions until they are within 17 to 30°C. In all cases, laboratory testing will be
carried out at 20-25 °C If ambient conditions do not allow for the samples to reach within this
temperature range, the samples will be placed in an artificial environment (e.g., laboratory,
vehicle) until equilibration within this temperature range has been achieved. In no case will any
samples be analyzed by Lead 100/AND 1000 if the sample temperature is unknown or known to
be outside of the 17 to 30°C range.
B3 SAMPLE HANDLING AND CUSTODY REQUIREMENTS
Each sample will be labeled with a unique sample identifier along with the date/time
collected and the name of the sample collector. Sample custody will be documented throughout
collection and analysis of the test samples following the Battelle Standard Operating Procedure
(SOP) for chain of custody[6]. A chain-of-custody (COC) form will include details about the
sample such as the time, date, location, and person collecting the sample. The COC form will
track sample release from the sampling location to the analysis laboratory. Each COC form will
be signed by the person relinquishing samples once that person has verified that the COC form is
accurate. Upon arrival at the analytical laboratory, COC forms will be signed by the person
receiving the samples (if different from the sample collector) once that person has verified that
all samples identified on the COC forms are present. Copies of all COC forms will be delivered
to the VTC and maintained with the test records.
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B4 ANALYTICAL METHODS REQUIREMENTS
All samples analyzed by the Lead 100/AND 1000 will also be analyzed by a reference
method to determine the accuracy of the Lead 100/AND 1000 in recovering Pb spikes. Pb will be
measured by ICP-MS according to EPA Method 200.8 (i.e., Pb Reference Method). In addition,
each of the laboratory, environmental, waste and drinking water effluent samples will be
analyzed once for cations according to EPA Method 200.8 (i.e., Cation Reference Method),
major anions according to EPA Method 300.1 (i.e., Anion Reference Method) and alkalinity
(including total, carbonate, bicarbonate and hydroxide alkalinity) according to Standard Method
2320B (i.e., Alkalinity Reference Method). Samples to be analyzed by Pb Reference Method
and Cation Reference Method will be preserved with (1+1) HNCb top pH<2, samples to be
analyzed by the Anion Reference Method do not require chemical preservation. Samples will be
sent at 4±2°C to DHL Analytical (Round Rock, TX) for analysis within the hold times specified
by the reference methods. Data for the reference method will be accompanied by a QC narrative,
the results of initial and on-going calibration, quality control results, and a statement that data
have been independently reviewed for compliance with the reference methods.
The Lead 100/AND 1000 will be operated exactly as specified in the vendor-provided
"AND 1000 Fluorimeter for Water Testing User Manual" (AND-prod-1000-2-2012) and the
"Lead Testing and On-Site Calibration for Water Testing" (AND-Lead-100-02-2012). Any
deviation in procedure from these documents as recommended by the vendor will be explicitly
noted in the LRB for this verification test.
B5 QUALITY CONTROL
B5.1 OVERVIEW AND REQUIREMENTS
Steps will be taken to maintain the quality of data collected during this verification test.
QC samples are incorporated into the sampling and analysis design to assess the quality of the
method of assessment.
Prepared QC samples include both laboratory reagent blanks (RB) and laboratory-
fortified matrix (LFM) samples. The RB samples are prepared from DI water and exposed to
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identical handling and analysis procedures as other prepared samples, including the addition of
all reagents. These samples are used to help ensure that no sources of contamination are
introduced in the sample handling and analysis procedures. Acceptance criteria for KB are
discussed in the next section.
The LFM and LFMD samples are prepared as aliquots of environmental samples and
spiked in the field to increase the Pb concentration of the samples to 25 ppb. The Pb Standard
Solution used to prepare the LFM is prepared in the laboratory and brought to the field site.
These samples are used to help identify whether matrix effects have any influence on the
analytical results. At least 10% of all the prepared samples to be analyzed will be RBs, and at
least two samples taken from each sampling site will be LFM and LFMD. The following
samples satisfy the LFM requirements for field-collected samples: WF-25, BW-25, FWW-25,
RWW-25, ReW-25, RiW-25, SW-25, MWWE#l-25, MWWE#2-25, and MFWWE-25.
Acceptance criteria for LFM and LFMD are discussed in the next section.
Quality control standards (QCS) are used as a calibration check to verify that
Lead 100/AND 1000 and the reference instruments are properly calibrated and reading within
defined control limits. QCS is defined as 30 ppb Pb. These standards will be purchased from
Fisher Scientific and will be subject only to dilution. The calibration of all instruments will be
verified using a QCS before and after each testing day, as well as after every tenth sample. In
addition, instruments and equipment used for this verification will operate at the expected ranges
and calibration records will be verified and kept for all monitoring instruments and equipment
used during this verification test.
B5.2 Acceptance Criteria and Root Cause Analyses
Acceptance criteria for QC samples vary depending on the sample(s) being analyzed. For
each set of samples a root cause analysis may be required before testing begins (see Appendices
F, G and H for root cause analysis flow-charts).
For IDC, an initial on-site calibration must be passed before LFM and LFMD samples are
analyzed. If on-site calibration is not passed the first time it will be repeated and if a second
failure occurs a root cause analysis will be performed and the Vendor will be contacted with the
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results of the analysis. If on-site calibration is passed either during the first or (if necessary) the
second attempt, LFM and LFMD samples will be analyzed. The acceptance criteria for the LFM
and LFMD are recovery of the Pb spike of 75-125% and an RPD of less than 30%. If these
criteria are not met on-site calibration will be repeated. Only when LFM and LFMD criteria are
met will analysis of the samples be initiated (see Appendix F for root cause analysis flowchart).
For ICC and TPC, an initial on-site calibration must be passed before LFM and LFMD
samples are analyzed. If on-site calibration is not passed the first time it will be repeated and if a
second failure occurs a root cause analysis will be performed and the Vendor will be contacted
with the results of the analysis. If on-site calibration is passed either during the first or (if
necessary) the second attempt, LFM and LFMD samples will be analyzed. The acceptance
criteria for the LFM and LFMD are recovery of the Pb spike of 85-115% and a standard
deviation of ± 15% of the expected Pb value. If these criteria are not met on-site calibration will
be repeated. Only when LFM and LFMD criteria are met will analysis of the samples be
initiated (see Appendix G for root cause analysis flowchart).
For DEI, finished drinking water, environmental waters and wastewater effluents an
initial on-site calibration must be passed before LFM and LFMD samples are analyzed. If on-
site calibration is not passed the first time it will be repeated and if a second failure occurs a root
cause analysis will be performed and the Vendor will be contacted with the results of the analysis
as well as information regarding the samples (e.g., pH, color, turbidity and conductivity). If on-
site calibration is passed either during the first or (if necessary) the second attempt, LFM and
LFMD samples will be analyzed. The acceptance criteria for the LFM and LFMD are recovery
of the Pb spike of 75-125% and RPD of less than 30%. If these criteria are not met on-site
calibration will be repeated. Only when LFM and LFMD criteria are met will analysis of the
samples be initiated (see Appendix H for root cause analysis flowcharts).
Acceptance criteria for KB are set at less than the vendor-reported method detection limit
of 2 ppb Pb making the method detection limit and reporting limit identical. If
Lead 1007AND 1000 reports values of Pb equal to or greater than 2 ppb Pb, a second KB will be
analyzed and if Lead 100/AND 1000 indicates a value equal to or greater than 2 ppb Pb, on-site
calibration will be repeated before analysis is continued. A value of less than 2 ppb Pb is
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indicated by the AND1000 displaying the message "*BELOW LIMIT*" while values measured
equal to or greater than 2 ppb Pb is indicated by AND 1000 as a quantitative result.
Acceptance criteria for QCS are set at ±25% of the expected Pb concentration (i.e., 30
ppb Pb) in QCS samples for both Lead 1007AND 1000 and Reference Methods.
In the case that a root cause analysis must be completed, the laboratory analyst(s) will
perform a root cause analysis. The analysis will have at a minimum the following areas described
in detail:
1. Identify the problem: Identify the QC failure. Include instrument, reagent, sampling,
personnel and any other problems.
2. Investigate to identify the root cause: Determine how each problem identified
interacted with each other to create the QC problem.
3. Come up with the solution: Develop an encompassing solution to address all
problems that created the QC failure. This may require contacting ANDalyze
4. Implement the solution: Develop an implementation plan that includes all
components of the developed solution and have laboratory management implement it.
5. Document the solution: Document all corrective action steps taken under laboratory
management implementation of the corrective action.
6. Communicate the solution: Develop training and management programs to
communicate and evaluate all personnel included in the corrective action solution.
7. Evaluate the effectiveness of the solution: Document QC results in trend charts and
laboratory staff performance to validate corrective action solution.
The following root cause analysis QC identifiers will be used:
• IFM Instrument Failure Mechanical
• IFE Instrument Failure Electrical
• IOFM Instrument Operator Failure to Follow Method
• SFC Sensor Failure Chemical
• SFM Sensor Failure Mechanical
• FCU Failure Cause Unknown
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B5.3 Control Charts
Control charts will be maintained throughout the entire verification testing process as per
Standard Methods Section 1020 B[7]. Control limits will be calculated after the first five samples
and after every ten samples thereafter. If analysis of the control charts indicate non-conformance
as described in Standard Methods Section 1020 B, the vendor will be contacted to determine the
cause of the problem, which may include a root cause analysis.
B6 INSTRUMENT/EQUIPMENT TESTING, INSPECTION, AND MAINTENANCE
The instruments used during the verification test will be inspected and maintained
according to the instrument manuals or the laboratory standard operating procedures of DHL
Analytical. Operation of the Lead 100/AND 1000 during the verification test will be performed
by Battelle technical staff as directed by the vendor user manuals and during on-site training.
B7 CALIBRATION/VERIFICATION OF TEST PROCEDURES
The instruments used during the verification test (i.e., Lead 100/AND 1000 and reference
instruments) will be calibrated per the instrument manual, the methods being used to make each
measurement, or the SOPs of the analysis laboratory. For each measurement, the equipment
calibration will be verified. Calibration procedures, checks, and results will be documented in
the project files. Testing will not occur until instrument calibration results meet the acceptance
criteria as defined in the root cause analyses (see Appendices F-H).
All calibrations performed will be documented by the verification staff in the project
LRB. The Lead 100/AND 1000 technology vendor will provide the Battelle verification staff
with the necessary training/information to properly calibrate and maintain Lead 100/AND 1000.
Calibration of Lead 1007AND 1000 will be done as often as indicated in the Lead 1007AND 1000
user manual or as suggested by the vendors. Vendors will be required to describe the necessary
calibration procedures specific to Lead 100/AND 1000.
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B8 INSPECTION/ACCEPTANCE OF SUPPLIES AND CONSUMABLES
All materials, supplies, and consumables used to establish the test conditions will be
ordered by the VTC or designee. Where possible, Battelle will rely on sources of materials and
consumables that have been used previously as part of ETV verification testing without
problems.
Supplies must meet the following criteria:
• Solvent and reagent grades are based on the intended use. All reagents will be of
>96% purity (see Table 6)
• Equipment used to generate data must provide appropriate sensitivity.
• A certificate of analysis must be provided and retained for reagents and standards.
• The quality and purity of expendable materials must be documented and adequate to
meet the DQOs of the client.
B9 NON-DIRECT MEASUREMENTS
No non-direct measurements will be used during this verification test.
BIO DATA MANAGEMENT
Various types of data will be acquired and recorded electronically or manually by
verification staff during this verification test. All data and observations for the operation of the
Lead 100/AND 1000 will be documented by the vendors or verification staff in LRBs, data forms
or captured electronically. Results from the laboratory analytical instruments will be compiled
by laboratory staff in electronic format and submitted to the VTC or other verification staff upon
obtaining results. Hand-transcribed data must be 100% verified by a second person.
Records received or generated by any of the verification staff during the verification test
will be reviewed by the VTC or designee within two weeks of receipt or generation, respectively,
before the records are used to calculate, evaluate, or report verification results. The review will
be documented as the dated initials of the reviewer. If a Battelle staff member generated the
record, this review will be performed by a Battelle technical staff member involved in the
verification test, but not the staff member that originally received or generated the record. The
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review will be documented by the person performing the review by adding his/her initials and
date to the hard copy of the record being reviewed. In addition, data calculations performed by
verification staff will be spot-checked by Battelle technical staff to ensure that calculations are
performed correctly. Calculations to be checked include any statistical calculations described in
this QAPP. The data obtained from this verification test will be compiled and reported.
All electronic testing records and documents will be stored on a test-specific networked
ETV SharePoint site and common drive within Battelle's network. Testing data will be uploaded
to the SharePoint Site within two days of receiving said data. This site is within the protected
Battelle network and is backed up regularly. The goal of this data delivery schedule is prompt
identification and resolution of any data collection or recording issues.
In addition, once testing is complete, all testing records and documents are sent to
Battelle's RMO for archival within two months of project close-out.
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SECTION C
ASSESSMENT AND OVERSIGHT
Cl ASSESSMENTS AND RESPONSE ACTIONS
Every effort will be made in this verification test to anticipate and resolve potential problems
before the quality of performance is compromised. One of the major objectives of this QAPP is
to establish mechanisms necessary to ensure this. Internal quality control measures described in
this QAPP will give information on data quality on a daily basis. The responsibility for
interpreting the results of these checks and resolving any potential problems resides with the
VTC, who will contact the Battelle AMS Center Manager, Battelle AMS Center QM, EPA AMS
Center Project Officer, and EPA AMS Center QM if any deviations from the QAPP are
observed. The VTC will describe the deviation in a teleconference or by email, and once a path
forward is determined and agreed upon with EPA, the deviation and corrective action will be
documented in writing. Technical staff have the responsibility to identify problems that could
affect data quality or the ability to use the data. Any problems that are identified will be reported
to the VTC. Technical staff and the VTC will work with the Battelle QM to resolve any issues.
Action will be taken by the VTC and Battelle testing staff to identify and appropriately address
the issue, and minimize losses and correct data, where possible. Independent of any EPA QA
activities, Battelle will be responsible for ensuring that the following audits are conducted as part
of these verification tests.
Cl.l Performance Evaluation Audit
Performance evaluation (PE) audits for the Lead 100/AND 1000 will be conducted by
having two analysts independently take triplicate measurements for a 25 ppb Pb standard (in DI
water). To be considered acceptable, the average of the two analysts' results should agree within
20% and CV of each analysts triplicate measurements should be no more than 20% .
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C1.2 Technical Systems Audits
The Battelle QM or designee will perform a TSA during performance evaluation
activities. The purpose of these audits is to ensure that the verification tests are being performed
in accordance with the AMS Center QMP1 and this QAPP. The Battelle QM will compare actual
test procedures to those specified or referenced in this plan, and review data acquisition and
handling procedures. The Battelle QM or designee will prepare a project-specific checklist
based on the QAPP requirements to guide the TSA, which will include a review of the test
location and general testing conditions; observe the testing activities; and review test
documentation. She will also check data acquisition procedures, and confer with Battelle staff.
The Battelle QM will prepare an initial TSA report and will submit the report to the EPA QA
Manager (with no corrective actions documented) and VTC within 10 business days after
completion of the audit. A copy of each final TSA report (with corrective actions documented)
will be provided to the EPA AMS Center Project Officer and QM within 20 business days of
completion of the audit. At EPA's discretion, EPA QA staff may also conduct an independent
on-site TSA during the verification tests. The TSA findings will be communicated to technical
staff at the time of the audit and documented in the TSA reports.
C1.3 Data Quality Audits
The Battelle QM, or designee, will audit at least 10% of the sample results data acquired
in the verification tests and 100% of the calibration and QC data versus the QAPP requirements.
Two ADQs will be conducted for this project: Data collected on the first day of testing will be
audited within 10 business days of receipt and assessed using a project-specific checklist. The
remaining data will be audited at the conclusion of testing and will be completed within 10
business days of receipt of all test data. During these audits, the Battelle QM, or designee, will
trace the data from initial acquisition (as received from the vendor's technology), through
reduction and statistical comparisons, to final reporting. All calculations performed on the data
undergoing the audit of data quality (ADQ) will be checked. Data must undergo a 100%
validation and verification by technical staff (i.e., VTC, or designee) before it will be assessed as
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part of the data quality audit. All QC data and all calculations performed on the data undergoing
the audit will be checked by the Battelle QM or designee. Results of each ADQ will be
documented using the checklist and reported to the VTC and EPA within 10 business days after
completion of the audit. A final ADQ that assesses overall data quality, including accuracy and
completeness of the technical report, will be prepared as a narrative and distributed to the VTC
and EPA within 10 business days of completion of the audit.
C1.4 QA/QC Reporting
Each assessment and audit will be documented in accordance with Section 3.3.4 of the
AMS Center QMP^. The results of all audits will be submitted to EPA within 10 business days
as noted above. Assessment reports will include the following:
• Identification of Findings and Observations;
• Recommendations for resolving problems;
• Response to adverse findings or potential problems;
• Confirmation that solutions have been implemented and are effective; and
• Citation of any noteworthy practices that may be of use to others.
C2 REPORTS TO MANAGEMENT
During the laboratory evaluation, any QAPP deviations will be reported immediately to
EPA. The Battelle QM and/or VTC, during the course of any assessment or audit, will identify
to the technical staff performing experimental activities any immediate corrective action that
should be taken. A summary of the required assessments and audits, including a listing of
responsibilities and reporting timeframes, is included in Table 13. If serious quality problems
exist, the Battelle QM will notify the AMS Center Manager, who is authorized to stop work.
Once the assessment reports have been prepared, the VTC will ensure that a response is provided
for each adverse finding or potential problem and will implement any necessary follow-up
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corrective action. The Battelle QM will ensure that follow-up corrective action has been taken.
The QAPP and final report are reviewed by the EPA AMS Center QM and the EPA AMS Center
Project Officer. Upon final review and approval, both documents will then be posted on the
ETV website (www.epa.gov/etv).
Table 13. Summary of Quality Assessment and Control Reports1
Assessment
LeadlOO/ANDlOOO
ISA
(within the first
week of testing)
ADQ (Day 1 data)
ADQ (Remaining
data and verification
report)
Prepared By
Battelle
Battelle
Battelle
Report Submission Timeframe
10 business days after TSA is
complete
TSA response is due to QM within 10
business days
TSA responses will be verified by the
QM and provided to EPA within 20
business days
ADQ will be completed within 10
business days after receipt of first data
set
ADQ will be completed within 10
business days after completion of the
verification report review
Submitted To
EPA ETV AMS Center
EPA ETV AMS Center
EPA ETV AMS Center
Any QA checklists prepared to guide audits will be provided with the audit report.
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SECTION D
DATA VALIDATION AND USABILITY
Dl DATA REVIEW, VALIDATION, AND VERIFICATION REQUIREMENTS
The key data review requirements for the verification test are the collection of QC
samples as outlined in the QAPP, a comparison of raw data sheets and comments against final
data to flag any suspect data, and a review of final data to resolve any questions about apparent
outliers. The QA audits, as described within this document, are designed to ensure the quality of
these data. The key data verification requirements for this test are stated in Section Cl of this
QAPP. The data generated during this test will be reviewed by a Battelle technical staff member
within two weeks of receipt or generation of the data. The reviewer will be familiar with the
technical aspects of the verification test but will not be the person who generated the data. This
process will serve both as the data review and the data verification and will ensure that the data
have been recorded, transmitted, and processed properly. Furthermore, this process will ensure
that the monitoring systems data were collected under appropriate testing conditions.
D2 VALIDATION AND VERIFICATION METHODS
Data verification is conducted as part of the data review as described in Section Cl of this
QAPP. A visual inspection of handwritten data will be conducted to ensure that all entries were
properly recorded or transcribed and any erroneous entries were properly noted. All calculations
used to transform the data will be reviewed to ensure the accuracy and the appropriateness of the
calculations. Calculations performed manually will be reviewed and repeated using a handheld
calculator or commercial software (e.g., Microsoft® Excel). Calculations performed using
standard commercial office software (e.g., Microsoft® Excel) will be reviewed by inspection of
the equations used for the calculations and verification of selected calculations by a handheld
calculator. Calculations performed using specialized commercial software (i.e., for analytical
instrumentation) will be reviewed by inspection and, when feasible, verified by a handheld
calculator or standard commercial office software.
To ensure that the data generated from this test meet the goals of the test, a number of
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data validation procedures will be performed. Sections B and C of this QAPP provide a
description of the validation safeguards employed for this verification test. Data validation
efforts include the completion of QC activities and the performance of a ISA as described in
Section C. The data from this test will be evaluated relative to the measurements to ensure that
the DQOs are met. Data failing to meet these criteria will be flagged in the data set and not used
for evaluation of the technologies, unless these deviations are accompanied by descriptions of
their potential impacts on the data quality.
An ADQ will be conducted by the Battelle QAO to ensure that data review, verification,
and validation procedures were completed and to ensure the overall quality of the data.
D3 RECONCILIATION WITH USER REQUIREMENTS
This QAPP and the resulting ETV verification report will be subjected to review by the
vendor, EPA, and expert peer reviewers. These reviews will ensure that this QAPP and the
resulting verification report meet the needs of potential users of the Lead 100/AND 1000.
Performance data for the Lead 100/AND 1000, collected under conditions where the QC
requirements for the replicate and PEA samples were met, will be presented in the final
verification report without any further comment. Performance data and variable measurements
that do not meet these criteria will be noted, and a discussion of the possible impact of the failed
requirements on the performance evaluation will be presented in the final verification report.
The final verification report will be submitted to EPA in Word (DOC) and Adobe portable
document format (PDF) and subsequently posted on the ETV Web site (www.epa.gov/etv).
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SECTION E
REFERENCES
El REFERENCES
1. Quality Management Plan for the ETV Advanced Monitoring Systems Center, Version 8.
U.S. Environmental Technology Verification Program, Battelle, April 2011.
2. Environmental Technology Verification Program Quality Management Plan. January,
2008(EPA/600/R-08/009).
3. EPA. 2012. Lead in Drinking Water. Available at:
http://water.epa.gov/drink/info/lead/index. cfm.
4. World Health Organization. 2012. Water Sanitation Health. Available at:
http://www.who.int/water_sanitation_health/diseases/lead/en/.
5. Touring Ohio Magazine. 2012. Scioto River. Available at: http://www.touring-
ohio.com/central/columbus/scioto-river.html.
6. SOP ENV-ADM-009, Standard Operating Procedure for Sample Chain-of-Custody
Battelle, September 2007.
7. Standard Methods for the Examination of Water and Wastewater, 22nd Edition, American
Public Heath Association/American Water Works Association, Rice, E.W., Baird, R.B.,
Eaton, A.D. and Clesceri, L.S. (ed.)
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