H TETRATECH
May 27, 2014
Mr. James Johnson
On-Scene Coordinator
U.S. Environmental Protection Agency, Region 7
11201 Renner Boulevard
Lenexa, Kansas 66219
Subject: Quality Assurance Project Plan for Baseline Off-Site Air Monitoring and Sampling
West Lake Landfill Site, Bridgeton, Missouri
CERCLIS fi>: MOD079900932
EPA Region 7, START 4, Contract No. EP-S7-13-06, Task Order No. 0058
Task Monitor: James Johnson, On-Scene Coordinator
Dear Mr. Johnson:
Tetra Tech, Inc. is submitting the attached Quality Assurance Project Plan regarding air monitoring and
sampling at locations off-site of the West Lake Landfill Site (WLLS) in Bridgeton, Missouri. This
monitoring will be conducted during a baseline period prior to start of construction of an isolation barrier
at the WLLS. If you have any questions or comments, please contact me at (816) 412-1775.
Sincerely,
Ted Faile, PG, CHM;
® START Program Ma
START Program Manager
Enclosures
>inA7n100
I.D
OW
Superfund
X9025.14.0058.000
0W0D
Tel 816.412.1741
41S Oak Street, Kansas City, MO 64106
Fax 816.410.1748 www.tetratech.com
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QUALITY ASSURANCE PROJECT PLAN FOR BASELINE OFF-SITE AIR MONITORING
WEST LAKE LANDFILL SITE
Superfund Technical Assessment and Response Team (START) 4
Contract No. EP-S7-13-06, Task Order No. 0058
Prepared For:
U.S. Environmental Protection Agency
Region 7
Superfund Division
11201 Renner Blvd.
Lenexa, Kansas 66219
May 27, 2014
Prepared By:
Tetra Tech, Inc.
415 Oak Street
Kansas City, Missouri 64106
(816)412-1741
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CONTENTS
Section/Table Page
QUALITY ASSURANCE PROJECT PLAN FORM 1
TABLE 1A: SAMPLE SUMMARY - RADIOLOGICAL PARAMETERS 5
TABLE IB: SAMPLE SUMMARY - CHEMICAL AND PARTICULATE PARAMETERS 6
TABLE 2: DATA QUALITY OBJECTIVE SUMMARY 7
Appendix
A SITE-SPECIFIC INFORMATION REGARDING BASELINE OFF-SITE AIR MONITORING
AND SAMPLING IN SUPPORT OF A REMOVAL ASSESSMENT AT THE WEST LAKE
LANDFILL SITE BRIDGETON, MISSOURI
B FIGURE
C ANALYTICAL LABORATORY STANDARD OPERATING PROCEDURES
X9025.14.0058.000
1
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1,4 Project'I afk Dticiiplion:
~ i" f'Ri I A r*<\
[~1 Uliior iik-st ripiU'ii 1
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O Pre-CERCL1S Site Sunrninr
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[3 RL-mnv,il A>-.ksmtrn» (hscrl.rf iTnijjiuig;
i.iiiL\iuk- Biistlmc st mpling is jiuiKipuli'd frjic June ill 14 through fhc .star, oi isnl.itii>r hami*r co:K;ruvi'hir. Prc-samplr i n referenced report:
Title
Dale
1.5 (Jujility Objectives ami Criteria for Measurement Bain;
Accuracy:
PmvisHjfi:
Reptesentativetiess:
CompteWtiess*:
Coxupaiability:
Identified la aached table.
Identified in aachri labte.
Identified in afctdhsi able.
Identified in attached table.
Identified in uttaelwi lafcle.
Other - 'u I'l'i t
C'Kn.i MuV oT Hh• jx'i-.jmT hj? ^S'ahli.chc\1 in avrvrT i ?h * i . yx I 5 if 1 .n, EPA -l 1;. 1,_iii be „bk w
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Region 7 Superfund Program
Addendum for the Generic QAPP for Superfund Site Assessment and Targeted Brownfields Assessment Activities (October 2012) for the
West Lake Landfill Site
1.7 Documentation and Records:
Field Sheets
Chain of Custody
Site Log
Health and Safety Plan
~ Trip Report
13 Letter Report
Site Maps
Photos
~ Video
Sample documentation will follow EPA Region 7 SOP 2420.05.
Other: Analytical information will be handled according to procedures identified in Table 2.
2.0 Measurement and Data Acquisition:
2.1 Sampling Process Design:
~ Random Sampling Q Transect Sampling
~ Search Sampling Q Systematic Grid
I~1 Screening w/o Definitive Confirmation
153 Sample Map Attached
153 Biased/Judgmental Sampling Q Stratified Random Sampling
I~1 Systematic Random Sampling £3 Definitive Sampling
153 Screening w/ Definitive Confirmation
The proposed sampling scheme will be biased/judgmental with definitive laboratory analysis, in accordance with procedures included in the
Guidance for Performing Site Inspections Under CERCLA, Office of Solid Waste and Emergency Response (OSWER) Directive #9345.1-05,
September 1992, and Removal Program Representative Sampling Guidance, Volume 1: Soil, OSWER Directive 9360.4-10, November 1991.
Samples will be submitted for analysis by a START-contracted laboratory. See Appendices A and B for additional site-specific information.
Sample Summaiy I maliim
Matrix
of Sample-
\nal\-
Off-site Air Monitoring Stations
(see Appendix B, Figure 1)
Air
Continuous/weekly/monthly
monitoring and sampling
(see Tables 1A & IB)
Radionuclides, radon, gamma exposure rate,
carbon monoxide, sulfur dioxide, hydrogen
sulfide, volatile organic compounds, and
particulates
*NOTE: Quality Control (QC) samples are not included with these totals. See Table 1 for a complete sample summary.
2.2 Sample Methods Requirements:
Maliix
Sampling Mrllinil
I P \ SOI'IM Method-
Air
various (see Tables 1A & IB)
various (see Tables 1A & IB)
2.3 Sample Handling and Custody Requirements:
I~1 Samples will be packaged and preserved in accordance with procedures defined in Region 7 EPA SOP 2420.06.
13 COC will be maintained as directed by Region 7 EPA SOP 2420.04.
~ Samples will be accepted according to Region 7 EPA SOP 2420.01.
153 Other (Describe): Samples will be packaged and accepted according to procedures established by the START-contracted laboratory.
2.4 Analytical Methods Requirements:
153 Identified in attached table.
153 Rationale: The requested analyses have been selected based on the historical information on the site and program experience with similar types
of sites.
~ Other (Describe):
2.5 Quality Control Requirements:
~ Not Applicable
153 Identified in attached table.
153 In accordance with the Generic QAPP for Superfund Site Assessment and Targeted Brownfields Assessment Programs (updated October 2012).
153 Describe Field QC Samples: Field blanks, trip blanks, and field duplicate samples are specified in Tables 1A and IB. Trip blanks will be used
to evaluate contamination introduced during transportation of the containers/samples. Field blanks will be collected to evaluate contamination of
sampling containers and to assess contamination potentially introduced during the sampling and laboratory procedure(s). Evaluation of blank
samples depends on the levels of contamination found in environmental samples to determine whether the environmental samples are representative.
Analytical results from blank samples will be evaluated qualitatively by the EPA Project Manager and EPA contractor(s) to determine a general
indication of field-introduced and/or lab-introduced contamination. Field duplicate samples will be collected to evaluate total method precision.
~ Other (Describe):
X9025.14.0058.000
2
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Region 7 Superfund Program
Addendum for the Generic QAPP for Superfund Site Assessment and Targeted Brownfields Assessment Activities (October 2012) for the
West Lake Landfill Site
2.6 Instrument/Equipment Testing, Inspection, and Maintenance Requirements:
~ Not Applicable
153 In accordance with the Generic QAPP for Superfund Site Assessment and Targeted Brownfields Assessment Programs (updated October 2012).
153 Other (Describe): Testing, inspection, and maintenance of instrumentation will accord with the SOPs and/or manufacturers' recommendations
referenced in Tables 1A and IB.
2.7 Instrument Calibration and Frequency:
~ Not Applicable
153 Inspection/acceptance requirements accord with the Generic QAPP for Superfund Site Assessment and Targeted Brownfields Assessment
Programs (updated October 2012).
153 Calibration of laboratory equipment will be performed as described in the SOPs and/or manufacturers' recommendations referenced in
Tables lAand IB.
153 Other (Describe): Calibration of field instruments will be performed as described in the SOPs and equipment operating guides referenced in
Tables lAand IB.
2.8 Inspection/Acceptance Requirements for Supplies and Consumables:
~ Not Applicable
153 In accordance with the Generic QAPP for Superfund Site Assessment and Targeted Brownfields Assessment Programs (updated October 2012).
~ All sample containers will meet EPA criteria for cleaning procedures for low-level chemical analysis. Sample containers will have Level II
certifications provided by the manufacturer in accordance with pre-cleaning criteria established by EPA in Specifications and Guidelines for
Obtaining Contaminant-Free Containers.
153 Other (Describe): Air filter media will meet criteria in Code of Federal Regulations (CFR) Title 21, Part 177.2260. Summa canisters for VOC
analysis will be certified clean by the START-contracted laboratory per the laboratory's SOP referenced in Table IB.
2.9 Data Acquisition Requirements:
~ Not Applicable
153 In accordance with the Generic QAPP for Superfund Site Assessment and Targeted Brownfields Assessment Programs (updated October 2012).
~ Previous data/information pertaining to the site (including other analytical data, reports, photos, maps, etc., which are referenced in this QAPP)
have been compiled by EPA and/or its contractor(s) from other sources. Some of that data has not been verified by EPA and/or its contractor(s);
however, the information will not be used for decision-making purposes by EPA without verification by an independent professional qualified to
verify such data/information.
~ Other (Describe):
2.10 Data Management:
~ All laboratory data acquired will be managed in accordance with Region 7 EPA SOP 2410.01.
153 Other (Describe): All laboratory data acquired will be managed according to procedures established by the START-contracted laboratory.
3.0 Assessment and Oversight:
3.1 Assessment and Response Actions:
153 Peer Review £3 Management Review Q Field Audit ~ Lab Audit
~ Assessment and response actions pertaining to analytical phases of the project are addressed in Region 7 EPA SOPs 2430.06 and 2430.12.
~ Other (Describe):
3.1A Corrective Action:
153 Corrective actions will be taken at the discretion of the EPA Project Manager whenever there appear to be problems that could adversely affect
data quality and/or resulting decisions affecting future response actions pertaining to the site.
~ Other (Describe):
3.2 Reports to Management:
~ Audit Report E3 Data Validation Report ~ Project Status Report ~ None Required
153 A letter report describing the sampling techniques, locations, problems encountered (with resolutions to those problems), and interpretation of
analytical results will be prepared by Tetra Tech START and submitted to the EPA.
153 Reports will be prepared in accordance with the Generic QAPP for Superfund Site Assessment and Targeted Brownfields Assessment Programs
(updated October 2012).
~ Other (Describe):
X9025.14.0058.000
3
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Region 7 Superfund Program
Addendum for the Generic QAPP for Superfund Site Assessment and Targeted Brownfields Assessment Activities (October 2012) for the
West Lake Landfill Site
4.0 Data Validation and Usability:
4.1 Data Review, Validation, and Verification Requirements:
~ Identified in attached table:
M Data review and verification will accord with the Generic QAPP for Superfund Site Assessment and Targeted Brownfields Assessment
Programs (updated October 2012).
~ Data review and verification will be performed by a qualified analyst and the laboratory's section manager as described in Region 7 EPA SOPs
2430.06, 2410.10, and 2430.12.
153 Other (Describe): The analytical data package from the START-contracted laboratory will be validated internally by the contracted laboratory
in accordance with the laboratory's established SOPs. A START chemist will conduct an external verification and validation of the laboratory data
package.
4.2 V alidation and V erification Methods:
~ Identified in attached table:
~ The data will be validated in accordance with Region 7 EPA SOPs 2430.06, 2410.10, and 2430.12.
M Other (Describe): The data will be validated using methods consistent with a Stage 2B validation, as described in the EPA Contract Laboratory
Program (CLP) Guidance for Labeling Externally Validated Laboratory Analytical Data for Superfund Use (EPA 2009). A Stage 2B validation
includes verification and validation based on a completeness and compliance check of sample receipt conditions and sample-related and instrument-
related QC results. The EPA Project Manager will be responsible for overall validation and final approval of the data, in accordance with the
projected use of the results.
4.3 Reconciliation with User Requirements:
~ Identified in attached table:
153 If data quality indicators do not meet the project's requirements as outlined in this QAPP, the data may be discarded and re-sampling or re-
analysis of the subject samples may be required by the EPA Project Manager.
~ Other (Describe):
X9025.14.0058.000
4
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Region 7 Superfund Program
Addendum for the Generic QAPP for Superfund Site Assessment and Targeted Brownfields Assessment Activities (October 2012) for the
West Lake Landfill Site
Table 1A: Sample Summary - Radiological Parameters
Site Name: West Lake Landfill Site
Location: Bridgeton, Missouri
START Project Manager: Dave Kinroth
Activity/ASR #: NA
Date: May 2014
No. of
Samples
Matrix
Location
Purpose
Requested Analysis
Sampling Method
Analytical Method/SOP
Samples Submitted for Laboratory Analysis
1 sample per
station per
week
Radionuclides in
airborne
particulates
5 off-site
monitoring
stations
Assess
concentrations of
radionuclides
present on airborne
particulates
Isotopic Th (including
Th-230)
EPA NCRFO SOP
RPR-250:
Operation of Air
Samplers without
Flow Measurement
Capability
Alpha spec, per lab SOP1
Total alpha-emitting
Ra
EPA 903.0 &SW-846 9315
as modified by lab SOP1
Isotopic U
Alpha spec, per lab SOP1
Gross alpha/beta
Low background GFPC per
lab SOP1
Gamma spectroscopy
Gamma spec, per lab SOP1
Ra-2262
EPA 903.0 &SW-846 9315
as modified by lab SOP1
preceded by 21-day in-
growth of Ra-226 progeny
3 badges per
station,
submitted
monthly
Gamma exposure
rate by
environmental TLD
5 off-site
monitoring
stations
Assess gamma
exposure rates
Gamma exposure rate
Per vendor-provided
instructions and
Service Guide4
NRC Regulatory Guide 4.13
Field Measurements
3 E-Perms per
station, read
weekly
Radon in ambient
air
5 off-site
monitoring
stations
Assess
concentrations of
radon in air
Radon
EPA Region 7
E-PERM Radon
Detection System
Equipment Guide
NA
(field measurement only)
1 continuous
real-time
instrument per
station
Gamma exposure
rate by Saphymo
GammaTRACER
(G-M tube)
5 off-site
monitoring
stations
Assess gamma
exposure rates
Gamma exposure rate
Per EPA ERT
procedures
NA
(field measurement only)
1 real-time
sensor per
station
Gamma exposure
rate by RAE
Systems AreaRAE
sensor
5 off-site
monitoring
stations
Assess gamma
exposure rates
Gamma exposure rate
EPA Region 7
AreaRAE EOG
NA
(field measurement only)
QC Samples/Measurements
1 per weekly
field blank
submittal
Radionuclides on
filter media
Field blank
Assess
contamination of
the filter from field
handling
Same as the requested
analyses for filter
samples
Filter will be
handled in the field2
Same as the analyses for
filter samples
1 each per
batch of TLDs
Gamma exposure
rate by
environmental TLD
Transit/control
badge
Assess
contributions to
gamma exposure
rates related to
background and
badge transit
Gamma exposure rate
Per vendor-provided
instructions and
Service Guide4
NRC Regulatory Guide 4.13
2 replicates per
station5
Radon in ambient
air
5 off-site
monitoring
stations
Assess total
method precision
Radon
EPA Region 7
E-PERM EOG
NA
(field measurement only)
2 replicates5
Gamma exposure
rate by
environmental TLD
5 off-site
monitoring
stations
Assess total
method precision
Gamma exposure rate
Per vendor-provided
instructions and
Service Guide
NRC Regulatory Guide 4.13
Alpha spec. = alpha spectroscopy; EPA = U.S. Environmental Protection Agency; EOG = Equipment Operating Guide; ERT = Environmental
Response Team; gamma spec. = gamma spectroscopy; GFPC = gas flow proportional counting; G-M = Geiger-Mueller; NA = not applicable; lab
= laboratory; NCRFO = National Center for Radiation Field Operations; NRC = U.S. Nuclear Regulatory Commission; Ra = radium; SOP =
Standard Operating Procedure; TLD = thermoluminescence dosimeters; Th = thorium; U = uranium
Notes: 1 See Appendix C
2 Analyzed only if total alpha-emitting radium is greater than 5 picoCuries/filter
3 A filter will be handled in the field in a manner similar to that for the primary filter samples, except no sampling onto the filter will
occur
4 See http://www.landauer.com/uploadedFiles/About_Us/LDR%20Service%20Guide%20-%20012013.pdf
5 These replicates are included in the per station number of samples
X9025.14.0058.000
5
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Region 7 Superfund Program
Addendum for the Generic QAPP for Superfund Site Assessment and Targeted Brownfields Assessment Activities (October 2012) for the
West Lake Landfill Site
Table IB: Sample Summary - Chemical and Particulate Parameters
Site Name: West Lake Landfill Site
Location: Bridgeton, Missouri
START Project Manager: Dave Kinroth
Activity/ASR #: NA
Date: May 2014
No. of
Samples
Matrix
Location
Purpose
Requested Analysis
Sampling Method
Analytical Method/SOP
Samples Submitted for Laboratory Analysis
1 sample per
station per
week
Outdoor air
5 off-site
monitoring
stations
Assess VOCs
VOCs
EPA ERT SOP
4231.1704 and EPA
Region 7 SOP
2313.04
EPA Method TO-15 and lab
SOP1
Field Measurements
1 real-time
sensor per
station
Outdoor air
5 off-site
monitoring
stations
Assess for typical
landfill gasses of
concern
CO, S02.H2S, VOCs2
EPA Region 7
AreaRAE EOG
NA
(field measurement only)
1 real-time
sensor per
station
Outdoor air
5 off-site
monitoring
stations
Assess for airborne
particulate
concentrations
PM2.5and PM10
EPA Region 7
DataRAM EOG
NA
(field measurement only)
QC Samples
1 per week
Outdoor air
Trip blank
Assess
contamination of
the Summa
canister from field
handling
VOCs
Trip blank will be
handled in the field3
EPA Method TO-15 and lab
SOP1
1 per week
Outdoor air
Field
duplicate
Assess total
method precision
VOCs
Field duplicate will
be co-located with a
primary Summa
canister and will be
sampled concurrent
with the primary
Summa canister
EPA Method TO-15 and lab
SOP1
CO = carbon monoxide; EPA = U.S. Environmental Protection Agency; EOG = Equipment Operating Guide; ERT = Environmental Response
Team; H2S = hydrogen sulfide; NA = not applicable; lab = laboratory; PM2 5 = particulates less than 2.5 micrometers in diameter; PMi0 =
particulates less than 10 micrometers in diameter; SOP = Standard Operating Procedure; VOC = volatile organic compound
Notes: 1 See Appendix C
2 Measures VOCs as a relative instrument response to a 10.6 electron volt lamp calibrated to isobutylene
3 A Summa canister will be handled in the field in a manner similar to that for the sampled Summa canisters, except no sampling with
the trip blank canister will occur
X9025.14.0058.000
6
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Region 7 Superfund Program
Addendum for the Generic QAPP for Superfund Site Assessment and Targeted Brownfields Assessment Activities (October 2012) for the
West Lake Landfill Site
Table 2: Data Quality Objective Summary
Site Name: West Lake Landfill Site
Location: Bridgeton, Missouri
START Project Manager: Dave Kinroth
Activity/ASR #: N/A (START-contracted laboratory)
Date: May 2014
Analysis
Analytical
Method
Data Quality Measurements
Sample
Handling
Procedures
Data
Management
Procedures
Accuracy
Precision
Representativeness
Completeness
Comparability
Radionuclides
in airborne
particulates
collected on
filters
see
Table 1A
per
analytical
method
per
analytical
method
Biased/judgmental
sampling based on
professional
judgment of the
sampling team
The completeness
goal is 100%;
however, no
individual
samples have
been identified as
critical samples.
Standardized
procedures for
sample
collection and
analysis will be
used.
See Section
2.3 of
QAPP
form.
See Section
2.10 of QAPP
form.
Gamma
exposure rate
by
environmental
TLD
see
Table 1A
per
analytical
method
per
analytical
method
Biased/judgmental
sampling based on
professional
judgment of the
sampling team
The completeness
goal is 100%;
however, no
individual
samples have
been identified as
critical samples.
Standardized
procedures for
sample
collection and
analysis will be
used.
See Section
2.3 of
QAPP
form.
See Section
2.10 of QAPP
form.
VOCs by
EPA Method
TO-15
see
Table IB
per
analytical
method
per
analytical
method
Biased/judgmental
sampling based on
professional
judgment of the
sampling team
The completeness
goal is 100%;
however, no
individual
samples have
been identified as
critical samples.
Standardized
procedures for
sample
collection and
analysis will be
used.
See Section
2.3 of
QAPP
form.
See Section
2.10 of QAPP
form.
X9025.14.0058.000
7
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APPENDIX A
SITE-SPECIFIC INFORMATION REGARDING BASELINE OFF-SITE AIR MONITORING
AND SAMPLING IN SUPPORT OF A REMOVAL ASSESSMENT AT THE
WEST LAKE LANDFILL SITE
BRIDGETON, MISSOURI
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INTRODUCTION
The Tetra Tech, Inc. (Tetra Tech) Superfund Technical Assessment and Response Team (START) has
been tasked by the U.S. Environmental Protection Agency (EPA) to assist with baseline monitoring at
off-site locations around the West Lake Landfill site (WLSS) in Bridgeton, Missouri. Dave Kinroth of
Seagull Environmental Technologies, Inc. (SETI) will serve as the START Project Manager. He will be
responsible for ensuring that air monitoring and sampling proceeds as described in this Quality Assurance
Project Plan (QAPP), and for providing periodic updates to the client concerning the status of the project,
as needed. James Johnson will be the EPA Project Manager for this activity.
START'S tasks will include, but are not limited to: (1) assembling and maintaining a network of off-site
air monitoring stations with instrumentation and sampling devices to measure radiological and chemical
parameters of concern, (2) collecting samples and coordinating laboratory analysis, (3) assisting EPA
with data acquisition and management, and (4) documenting the off-site air monitoring efforts. The Tetra
Tech START quality assurance (QA) manager will provide technical assistance, as needed, to ensure that
necessary QA issues are adequately addressed.
START will adhere to this QAPP as much as possible, but may alter proposed activities in the field if
warranted by site-specific conditions and unforeseen hindrances that prevent implementation of any
aspect of this QAPP in a feasible manner. Such deviations will be recorded in the site logbook, as
necessary. This QAPP will be available to the field team at all times during sampling activities to serve
as a key reference for the proposed activities described herein.
PROBLEM DEFINITION, BACKGROUND, AND SITE DESCRIPTION
EPA will conduct air monitoring to address concerns that operations at WLLS could impact human health
and the environment via release to ambient air of solid waste landfill gases of concern or of particulates
with radiologically-impacted materials (RIM). This QAPP was prepared by Tetra Tech START to
support the off-site air monitoring program during a baseline monitoring period prior to initiation of
construction of a planned isolation barrier at WLLS. Air monitoring will be conducted during the
baseline period to provide data that will be used to (1) evaluate pre-construction concentrations of
chemical and radiological parameters of potential concern in outdoor air, and (2) provide data that will be
used to optimize the sampling and monitoring plan for the off-site air monitoring to occur during
construction of the isolation barrier.
X9025.14.0058.000
1
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West Lake Landfill is an approximately 200-acre property that includes several closed solid waste landfill
units that accepted wastes for landfilling from the 1940s or 1950s through 2004, plus a solid waste
transfer station, a concrete plant, and an asphalt batch plant. The WLLS is at 13570 St. Charles Rock
Road in Bridgeton, St. Louis County, Missouri, approximately 1 mile north of the intersection of
Interstate 70 and Interstate 270 (see Appendix B, Figure 1). The WLLS was used for limestone quarrying
and crushing operations from 1939 through 1988. Beginning in the late 1940s or early 1950s, portions of
the quarried areas and adjacent areas were used for landfilling municipal refuse, industrial solid wastes,
and construction/demolition debris. In 1973, approximately 8,700 tons of leached barium sulfate residues
(a remnant from the Manhattan Engineer District/Atomic Energy Commission project) were reportedly
mixed with approximately 39,000 tons of soil from the 9200 Latty Avenue site in Hazelwood, Missouri,
transported to the WLLS, and used as daily or intermediate cover material. In December 2004, the
Bridgeton Sanitary Landfill—the last landfill unit to receive solid waste—stopped receiving waste
pursuant to an agreement with the City of St. Louis to reduce potential for birds to interfere with Lambert
Field International Airport operations. In December 2010, Bridgeton Landfill detected changes—
elevated temperatures and elevated carbon monoxide levels—in its landfill gas extraction system in use at
the South Quarry of the Bridgeton Sanitary Landfill portion of the Site (a landfill portion not associated
with known RIM). Further investigation indicated that the South Quarry Pit landfill was undergoing an
exothermic subsurface smoldering event (SSE). In 2013, potentially responsible parties committed to
constructing an isolation barrier that would separate the Bridgeton Landfill undergoing the SSE from the
RIM-containing WLLS (EPA 2014).
Before construction of the isolation barrier and during construction activities, START will assist EPA
with air monitoring at locations off-site of the WLSS to determine if any releases with contaminant levels
above health-based benchmarks are migrating into ambient air within areas surrounding the WLLS.
Monitoring will be conducted for radiological parameters (including alpha-, beta-, and gamma-emitting
radionuclides on particulates; radon; and external gamma exposure), as well as typical solid waste landfill
gases (including sulfur dioxide [S02], hydrogen sulfide [H2S], carbon monoxide [CO], and volatile
organic compounds [VOC]). The potentially responsible parties will complement off-site monitoring by
EPA with ongoing on-site air monitoring.
EPA has arranged for placement of the air monitoring stations at the following locations (see Appendix B,
Figure 1):
Station 1 - Robertson Fire Protection District Station 2, 3820 Taussig Rd., Bridgeton, Missouri
Station 2 - Pattonville Fire Department District, 13900 St Charles Rock Rd., Bridgeton, Missouri
X9025.14.0058.000
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Station 3 - Pattonville Fire Department District Station 2, 3365 McKelvey Rd., Bridgeton, Missouri
Station 4 - Spanish Village Park, 12827 Spanish Village Dr., Bridgeton, Missouri
Station 5 - St. Charles Fire Department Station #2, 1550 S. Main St., St. Charles, Missouri.
Combined on-site air monitoring by the potentially responsible parties and off-site air monitoring by EPA
and START will constitute an air monitoring network helping to ensure that work on the isolation barrier
does not pose a threat to those living in the areas around the landfill.
SAMPLING STRATEGY AND METHODOLOGY
EPA and START began setup of the five off-site monitoring stations in April 2014; these activities
included installation of electrical service, instrument weather housings, monitoring and sampling devices
(including particulate air samplers, RAE Systems AreaRAEs, Saphymo GammaTRACERs, E-Perm radon
detectors, and thermoluminescence dosimeters), and a real-time remote monitoring network. The
baseline sampling period is anticipated to begin in early June 2014, and will end prior to initiation of the
isolation barrier construction anticipated to start in September 2014, when a second phase of air
monitoring and sampling will begin.
Baseline period off-site air monitoring and sampling will proceed according to the following sampling
process design, including selection of parameters of interest and associated sampling procedures:
Parameters of Interest
The following radiological and chemical parameters of potential concern were identified based on
historical information regarding the site and program experience with similar types of sites:
Radiological Parameters of Concern
Presence of naturally occurring alpha-, beta-, and gamma-emitting radionuclides on airborne particulates
will be assessed. The radionuclides of potential concern based on the characteristics of the West Lake
RIM that will be assessed are thorium-230, radium-226, and radon. Gross gamma activity at each of the
monitoring stations will also be assessed.
Chemical Parameters of Concern
Chemical parameters of concern selected for assessment include CO, H2S, S02, and VOCs.
X9025.14.0058.000
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Airborne Particulate Matter
Because the isolation barrier construction activities could release airborne particulate matter, PM2 5 and
PM10 (particulates less than 2.5 and 10 micrometers in diameter, respectively) have been identified as
contaminants of potential concern.
Sampling Procedures
Samples will be collected in a manner consistent with EPA methods and standard operating procedures
(SOP). The following are summaries of the project-specific sampling methods. Tables 1A and IB
summarize the sampling method requirements.
Radionuclides in Airborne Particulates
To determine airborne concentrations of radionuclides transported via airborne particulates, airborne
particulates will be collected onto borosilicate glass fiber filter media using high-volume air samplers.
One air sampler will be operated at each off-site monitoring station and will collect airborne particulates
continuously onto the filter media for durations of 7 days. At the end of the sampling period, the sampled
filter will be submitted for laboratory analysis, a new filter will be installed, and a new 7-day sampling
period will begin. The air samplers will be operated at a flow rate of at least 2.0 cubic feet per minute to
yield a minimum air sample volume of 20,160 cubic feet (571 cubic meters [m3]). With an anticipated
laboratory detection limit of 1 picoCurie (pCi) per filter for thorium-230 and radium-226, this sample
volume corresponds to a detection limit, in terms of an air concentration, of 1.75E-2 pCi/m3 for those
radionuclides. Calibration and operation of the high-volume air samplers will accord with the EPA
National Center for Radiation Field Operations (NCRFO) SOP RPR -250: Operation of Air Samplers
without Flow Measurement Capability.
Radon
Electret ion chamber radon detectors (E-PERM®) equipped with a high-volume chamber ("H-chamber")
short-term ("ST") electrets will be used to assess radon levels at each off-site monitoring station.
E-PERM® measurements are performed by use of an Electret Voltage Reader to measure a beginning and
final electrical charge on the electret that is exposed for a specified time period. The E-PERM® will be
read weekly to yield a radon measurement that is continuously integrated (averaged) over the week-long
exposure duration. Three E-PERMs® will be deployed per off-site monitoring station to provide
redundant measurements in case of a device failure, and to provide an indication of total method
precision.
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Gross Gamma Activity
Real-time gross gamma activity at each off-site monitoring station will be assessed using Saphymo
GammaTRACER and RAE Systems AreaRAE instruments. The real-time gross gamma measurements
from these instruments will be remotely transmitted via Safe Environment Engineering's Lifeline remote
telemetry system and logged by EPA's Viper data management software.
Thermoluminescence dosimeters (TLD) will also record gross gamma activity at the off-site monitoring
stations. TLDs are passive detection devices that require analysis by the dosimeter provider. The TLDs
will be deployed for continuous periods of approximately 30 days. Three TLDs will be deployed per
off-site monitoring station to provide redundant measurements allowing determination of total method
precision.
Real-time Monitoring for CO. H2S. S02. and VOCs
RAE Systems AreaRAEs equipped with CO, H2S, S02, and photo-ionization (for VOC detection) sensors
will be deployed at each off-site air monitoring station for continuous air monitoring. These AreaRAE
measurements will be remotely transmitted via Safe Environment Engineering's Lifeline remote
telemetry system and logged by EPA's Viper data management software.
Air Sampling for VOCs
Sampling for VOCs via Summa® canisters will occur each week at the air monitoring stations. The
Summa® canister will be fitted with a passive flow regulator to enable collection of an air sample for a
continuous 24-hour period. The sampled Summa canisters will be submitted to a START-contracted
laboratory for VOC analysis. All Summa® sampling will accord with EPA Environmental Response
Team SOP 4231.1704 - Summa® Canister Sampling, and with EPA Region 7 SOP 2313.04 - Air
Sampling with Stainless Steel Canisters. During the weekly sampling, a field duplicate sample will be
collected at one of the off-site air monitoring stations. In addition, an un-sampled Summa canister will be
handled in the field and will be submitted as a trip blank.
Airborne Particulate Matter
A DataRAM air particulate monitor will be deployed at each off-site air monitoring station to
continuously monitor real-time concentrations and median particle sizes of airborne dust, smoke, mist,
and fumes. The DataRAM instruments will be equipped with particle discriminators to yield
measurements correlated with PM2 5 and PM10. The real-time DataRAM measurements will be remotely
X9025.14.0058.000
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transmitted via Safe Environment Engineering's Lifeline remote telemetry system and logged by EPA's
Viper data management software.
Quality Control Samples
To evaluate sample quality control (QC), field blank, trip blank, and field duplicate samples will be
collected, as specified in Section 2.5 of the QAPP form.
ANALYTICAL METHODS
All samples will be submitted to a START-contracted laboratory for analysis. All samples will be
analyzed according to SOPs and methods referenced on the QAPP Form.
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REFERENCES
U.S. Environmental Protection Agency (EPA). 2014. Administrative Settlement Agreement and Order
on A Consent For Removal Action - Preconstruction Work. EPA Docket No.
CERCLA-07-2014-0002. April 20.
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APPENDIX B
FIGURE
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Station 2 - Pattonville Fire Protection District Headquarters
Station 1 - Robertson Fire Protection District Station 2
Station 5 - St. Charles Fire Department Station 2
Station 4 - Spanish Village Park
Station 3 - Pattonville Fire Department Station 2
Legend
Proposed off-site
— air monitoring station
Approximate site boundary
Operational Unit 1
(radiological area)
1,000 2,000
Source: ArcGIS Online Aerial Imagery, 2013
West Lake Landfill
Bridgeton, Missouri
Figure 1
Proposed Off-Site
Air Monitoring Stations
J .
Project No: X9025.14.0058.000
Date: 5/23/2014
Drawn By: Bill Spiking
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APPENDIX C
ANALYTICAL LABORATORY STANDARD OPERATING PROCEDURES
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TestAmerica
THE LEADER IN ENVIRONMENTAL TESTING
TestAmerica St. Louis
SOP No. ST-RC-G020, Rev. 18
Effective Date: 02/14/2014
Page No.: 1 of 14
Title: DETERMINATION OF GROSS ALPHA/BETA ACTIVITY
Approvals (Signature/Date):
irah Bernsen Date
ferah Bernsen
Radiochemistry Prep Supervisor
A
Marti
Quality Assurance Manager
Michael Rid^afiower Date
Health & Safety Manager / Coordinator
Ji/'*! TL, Ujtf 1/131 /*f
i Ward Date Elaine Wild ' Date
Elaine Wild
Laboratory Director
This SOP was previously identified as SOP No. ST-RC-0020 Rev. 17
Copyright Information:
This documentation has been prepared by TestAmerica Laboratories Inc. and its affiliates ("TestAmerica"), solely
for their own use and the use of their customers in evaluating their qualifications and capabilities in connection with
a particular project. The user of this document agrees by its acceptance to return it to TestAmerica upon request and
not to reproduce, copy, lend, or otherwise disclose its contents, directly or indirectly, and not to use if for any other
purpose other than that for which it was specifically provided. The user also agrees that where consultants or other
outside parties are involved in the evaluation process, access to these documents shall not be given to said parties
unless those parties also specifically agree to these conditions.
THIS DOCUMENT CONTAINS VALUABLE CONFIDENTIAL AND PROPRIETARY INFORMATION.
DISCLOSURE, USE OR REPRODUCTION OF THESE MATERIALS WITHOUT THE WRITTEN
AUTHORIZATION OF TESTAMERICA IS STRICTLY PROHIBITED. THIS UNPUBLISHED WORK
BY TESTAMERICA IS PROTECTED BY STATE AND FEDERAL LAW OF THE UNITED STATES. IF
PUBLICATION OF THIS WORK SHOULD OCCUR THE FOLLOWING NOTICE SHALL APPLY:
©COPYRIGHT 2014 TESTAMERICA LABORATORIES INC.
Facility Distribution No.:
Distributed To: See Electronic Distribution Sheet
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SOP No. ST-RC-0020, Rev. 18
Effective Date: 02/14/2014
Page No.: 2 of 14
1.0 SCOPE AND APPLICATION
1.1 This procedure applies to the preparation and analysis of samples for gross alpha and/or beta
radioactivity in air filters, water, soil/sediment, oil and vegetation samples.
1.2 This SOP is based on EPA Method 900.0, SW-846 Method 9310 and DOE RP-710.
1.3 For water samples containing high concentrations of dissolved solids (> 500 ppm), see SOP ST-
RC-0021 for analysis of gross alpha radioactivity.
1.4 The reporting limits, method detectable activities and QC limits are maintained in the Laboratory
Information Management System (LIMS).
2 J SUMMARY OF METHOD
2.1 An aliquot of aqueous sample is evaporated to dryness in a glass beaker after the addition of
concentrated nitric acid to convert any chlorides to nitrates, and transferred quantitatively to a
tared counting planchet.
2.2 For the activity of dissolved matter, an aliquot of aqueous sample is filtered through a 0.45-fim
membrane filter. The filtrate is evaporated to dryness in a glass beaker after the addition of
concentrated nitric acid to convert any chlorides to nitrates, and transferred quantitatively to a
tarred counting planchet.
2.3 For the activity of suspended matter, an aliquot of aqueous sample is filtered through a 0.45-fim
membrane filter. The filter is transferred to a counting planchet.
2.4 Air filter samples are counted for gross alpha and/or beta activity without further processing if the
filter is less than 2 inches diameter. If the filter is greater than 2-inch diameter, the sample is
digested per ST-RC-0004, "Preparation of Soil, Sludge, Filter, Biota , Oil and Grease Samples for
Actinide Analysis" and then an aliquot prepared like a liquid.
2.5 Solid samples can be analyzed for gross alpha and/or beta activity as a dry powder. If Method
RP710 (for total dissolution) is required, an acid leach is performed per ST-RC-0004, "Preparation
of Soil, Sludge and Filter Paper Samples for Radiochemical Analysis". The digestate is then
treated like a liquid.
NOTE: Total Sample Dissolution can also be done using Hydrofluoric acid, Hydrochloric acid
and Nitric acid as in section 11.8.
2.6 Oil samples are ashed in a muffle furnace, then dissolved in nitric acid and transferred to a glass
beaker where they are converted to nitrate salts using concentrated nitric acid. The sample is then
transferred to a planchet using 4 M nitric acid.
2.7 The sample residue is dried, and then counted for alpha and/or beta radioactivity using a Gas Flow
Proportional Counter
3.0 DEFINITIONS
3.1 See the T est America St. Louis Quality Assurance Manual (ST-QAM) for a glossary of common
laboratory terms and data reporting qualifiers.
3.2 There are no specific definitions for this procedure.
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4.0 INTERFERENCES
4.1 In this method for gross alpha and gross beta measurement, the radioactivity of the sample is not
separated from the solids of the sample. The solid concentration may adversely affect sensitivity of
the method.
4.2 For a 2-inch diameter counting planchet (20 cm2), an aliquot containing 100 mg of dissolved solids
would be the maximum aliquot size for that sample which should be evaporated and counted for
gross alpha or gross beta activity.
4.3 Radionuclides that are volatile under the sample preparation conditions of this method can not be
measured. Other radionuclides may also be lost during the sample evaporation and drying (such as
tritium and some chemical forms of radioiodine). Some radionuclides, such as the cesium and
technetium radioisotopes, may be lost when samples are heated to dull red color. Such losses are
limitations of the test method.
4.4 Moisture absorbed by the sample residue increases self absorption and, if uncorrected, leads to
low-biased results. Hygroscopic sample matrices may not remain at a constant weight after being
dried and exposed to the atmosphere before and during counting. Those types of water samples
need to be heated to a dull red color for a few minutes to convert the salts to oxides.
4.5 Heterogeneity of the sample residue in the counting planchet interferes with the accuracy and
precision of the method.
4.6 Gross Alpha and Gross Beta activity does not identify the radionuclide that is present. Instead, the
activity is referenced as equivalent to Th-230 for Gross Alpha and Sr-90/Y-90 for Gross Beta.
5.0 SAFETY
5.1 Employees must abide by the policies and procedures in the Corporate Environmental Health and
Safety Manual (CW-E-M-001), Radiation Safety Manual and this document. This procedure may
involve hazardous material, operations and equipment. This SOP does not purport to address all of
the safety problems associated with its use. It is the responsibility of the user of the method to
follow appropriate safety, waste disposal and health practices under the assumption that all
samples and reagents are potentially hazardous. Safety glasses, gloves, lab coats and closed-toe,
nonabsorbent shoes are a minimum.
5.2 SPECIFIC SAFETY CONCERNS OR REQUIREMENTS
None.
5.3 PRIMARY MATERIALS USED
5.3.1 The following is a list of the materials used in this method, which have a serious or
significant hazard rating. NOTE: This list does not include all materials used in the
method. The table contains a summary of the primary hazards listed in the MSDS
for each of the materials listed in the table. A complete list of materials used in the
method can be found in the reagents and materials section. Employees must review the
information in the MSDS for each material before using it for the first time or when there
are major changes to the MSDS.
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SOP No. ST-RC-0020, Rev. 18
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Page No.: 4 of 14
Material (1)
Hazards
Exposure
Limit (2)
Signs and symptoms of exposure
Nitric Acid
Corrosive
Oxidizer
Poison
2 ppm-(TWA)
4 ppm-(STEL)
Nitric acid is extremely hazardous; it is corrosive,
reactive, an oxidizer, and a poison. Inhalation of
vapors can cause breathing difficulties and lead to
pneumonia and pulmonary edema, which may be
fatal. Other symptoms may include coughing,
choking, and irritation of the nose, throat, and
respiratory tract. Can cause redness, pain, and
severe skin burns. Concentrated solutions cause
deep ulcers and stain skin a yellow or yellow-brown
color. Vapors are irritating and may cause damage
to the eyes. Contact may cause severe burns and
permanent eye damage.
Hydrochloric
Acid
Corrosive
Poison
5PPM-
(Ceiling)
Inhalation of vapors can cause coughing, choking,
inflammation of the nose, throat, and upper
respiratory tract, and in severe cases, pulmonary
edema, circulatory failure, and death. Can cause
redness, pain, and severe skin burns. Vapors are
irritating and may cause damage to the eyes.
Contact may cause severe burns and permanent eye
damage.
Hydrofluoric
Acid
Poison
Corrosive
Dehydrator
3 ppm-(TWA)
Severely corrosive to the respiratory tract. Corrosive
to the skin and eyes. Permanent eye damage may
occur. Skin contact causes serious skin burns,
which may not be immediately apparent or painful.
Symptoms may be delayed 8 hours or longer. THE
FLUORIDE ION READILY PENETRATES
THE SKIN CAUSING DESTRUCTION OF
DEEP TISSUE LAYERS AND BONE
DAMAGE.
1 - Always add acid to water to prevent violent reactions.
2 - Exposure limit refers to the OSHA regulatory exposure limit.
TWA - Time Weighted Average
STEL - Short Term Exposure Limit
Ceiling - At no time should this exposure limit be exceeded
EQUIPMENT AND SUPPLIES
6.1 Analytical Balance (4 - or 5 - place).
6.2 Beakers: Glass and Teflon, various sizes. Please consult SOP: ST-RC-5006 "Decontamination of
Laboratory Glassware, Labware, and Equiptment."
6.3 Counting planchets, stainless steel, flat and ridged, 5.0 cm (2.0"), cleaned per ST-RC-0002,
"Preparation of Stainless Steel Planchets for Radiochemistry Analyses."
6.4 Desiccator with desiccant, Dri-Rite or equivalent.
6.5 Drying oven with thermostat set at 105° C ± 5 °C.
6.6 Filter paper: ashless, Whatman #41 or ashless paper pulp, and 0.45-fim membrane.
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Page No.: 5 of 14
6.7
Hot plate
6.8
Pipettes
6.9
Muffle oven
6.10
Mod block
6.11
Tongs or forceps
6.12
Double sided tape or Self-adhesive dots
6.13
Spatula
6.14
Aluminum weighing pans
REAGENTS AND STANDARDS
7.1 All standards and reagent preparation, documentation and labeling must follow the requirements of
SOP ST-QA-0002, current revision.
7.2 Reagents are prepared from reagent grade chemicals, unless otherwise specified below, and
reagent water.
7.3 Deionized Water, obtained from the Milli-Q unit.
7.4 Nitric acid, concentrated (16N HN03)
7.4.1 4 N Nitric acid (4N HN03) - Add 250 ml of 16 N HN03 to 750 ml of reagent water and
mix well.
7.5 Hydrofluoric acid, concentrated (29 N HF)
7.6 Hydrochloric acid, concentrated (12 N HC1)
7.7 Salt Solution: NaHCO, - 22 g, KCL - 0.80 g, MgCl2 • 6H:0 - 22 g, Na2S04 - 34.2 g add to 500
mL of DI water. Stir on stir plate until dissolved. Bring final volume up to 1 L with DI.
7.8 Salt, NaCl, granular.
7.9 Thorium-230 for LCS and matrix spikes, calibrated - NIST traceable, diluted to approximately 20
dpm/mL.
7.10 Strontium-90 for LCS and matrix spikes, calibrated - NIST traceable, in equilibrium with Yttrium
90, diluted to approximately 20 dpm/ml.
7.11 Sodium Bicarbonate, NaHCO; powder.
7.12 Potassium Chloride, KC1
7.13 Sodium Sulfate, NaS04 crystals
7.14 Magnesium Chloride Hexahydrate, MgCl2 • 6H20, crystals
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8.0 SAMPLE COLLECTION, PRESERV ATION AND STORAGE
8.1 TestAmerica St. Louis supplies sample containers and chemical preservatives in accordance with
the method. TestAmerica St. Louis does not perform sample collection. Samplers should
reference the methods referenced and other applicable sample collection documents for detailed
collection procedures. Sample volumes and preservative information is given in ST-PM-0002.
8.2 Samples may be collected in glass or plastic containers.
8.3 Aqueous samples are preserved with nitric acid to a pH of less than 2.
8.3.1 The pH of aqueous samples is checked upon receipt by the Sample Control Department.
The pH does not require re-checking prior to analysis.
8.3.2 Aqueous samples acidified upon receipt (designated by label on the bottle) do require a
check of the pH prior to analysis.
9.0 QUALITY CONTROL
9.1 Batch
9.1.1 A sample batch is a maximum of 20 environmental samples, which are prepared together
using the same process and same lot(s) of reagents. Where no preparation method exists
(e.g. water sample volatile organics, water sample anion analysis ) the batch is comprised
of a maximum of 20 environmental samples which are analyzed together with the same
process, lots of reagents and personnel.
9.1.2 Instrument conditions must be the same for all standards, samples and QC samples.
9.1.3 For this analysis, batch QC consists of a method blank (MB), a Laboratory Control
Sample (LCS), and Sample Duplicate. In the event that there is insufficient sample to
analyze a sample duplicate, an LCS Duplicate (LCSD) is prepared and analyzed.
9.1.3.1 Matrix Spike (MS) and Matrix Spike Duplicate (MSD) may be performed upon
client request, and are noted in the Client Requirement Sheets and Log-in.
9.1.4 Samples having different QC codes, due to non-standard client specific QC requirements,
must be batched separately in the LIMS. A method blank and LCS may be shared across
QC codes provided the actual "sample batch" does not exceed 20 environmental samples.
Duplicates (and MS/MSD if applicable) must be performed for each separate QC code.
9.2 Method Blank (MB)
9.2.1 A method blank is a blank matrix processed simultaneously with, and under the same
conditions as, samples through all steps of the procedure.
9.2.2 A method blank must be prepared with every sample batch.
9.2.3 For Water analyses, the method blank is comprised of DI water. Prepare a method blank
of DI water equivalent to the target volume of 200 niL.
9.2.4 For Soil analyses, the method blank is comprised of salt.
9.2.5 For Oil analyses, the method blank is comprised of shredded filter paper in a crucilble.
9.2.6 For non-digested filters, a prepared method blank is provided by the count room.
9.2.7 For leached analyses, the method blank is comprised of the leaching acid.
9.3 Laboratory Control Sample (LCS)
9.3.1 A LCS is a blank matrix spiked with a known amount of analyte(s), processed
simultaneously with, and under the same conditions as, samples through all steps of the
analytical procedure.
9.3.2 An LCS must be prepared with every sample batch.
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9.3.3 For Water analyses, the LCS is comprised of DI water fortified with Strontium 90 for
beta and Thorium 230 for alpha. Add 0.7 mL of salt solution for mass.
9.3.4 For Soil analyses, the LCS is comprised of a known solid reference material :National
Bureau of Standards, SRM 4353, Rocky Flats Soil #1.
9.3.5 For Oil analyses, the LCS is comprised of shredded filter paper fortified with Strontium
90 for beta and Thorium 230 for alpha.
9.3.6 For non-digested filters, the LCS is provided by the count room.
9.4 Matrix Spike (MS)/Matrix Spike Duplicate (MSD)
9.4.1 A Matrix Spike is an aliquot of a field sample to which a known amount of target
analyte(s) is added, and is processed simultaneously with, and under the same conditions
as, samples through all steps of the analytical procedure.
9.4.2 MS/MSD samples do not count towards the 20 environmental samples in a sample batch.
9.4.3 MS/MSD samples, when requested, must be performed with every sample batch and
every LIMS batch.
9.5 Sample Duplicate (SD)
9.5.1 A Sample Duplicate is an additional aliquot of a field sample taken through the entire
analytical process to demonstrate precision.
9.5.2 If there is insufficient sample to perform a Sample Duplicate, a duplicate LCS is
analyzed. A NCM is written to document the insufficient volume and utilizing of a LCSD
for demonstration of precision.
9.6 Procedural Variations/ Nonconformance and Corrective Action
9.6.1 Any variation shall be completely documented using a Nonconformance Memo and
approved by the Supervisor and QA Manager. See SOP ST-QA-0036 for details
regarding the NCM process.
9.6.2 Any deviations from QC procedures must be documented as a nonconformance, with
applicable cause and corrective action approved by the Supervisor and QA Manager. See
SOP ST-QA-0036 for details regarding the NCM process.
10.0 CALIBRATION AND STANDARDIZATION
10.1 Balance calibration must be checked daily when used. Refer to SOP ST-QA-0005, "Calibration
and Verification Procedure for Thermometers, Balances, Weights and Pipettes Procedure.
10.2 For analytical instrumentation calibration, see SOP: ST-RD-0403, "Daily Calibration Verification
and Maintenance of the Low Background Gas Flow Proportional Counting System".
11.0 PROCEDURE
11.1 If the activity of dissolved matter in an aliquot of aqueous sample is to be determined.
11.1.1 Filter the desired aliquot through a 0.45-fim membrane filter and proceed with aqueous
sample preparation.
11.2 If the activity of suspended matter of an aliquot of aqueous sample is to be determined.
11.2.1 Filter the desired aliquot through a 0.45-fim membrane filter, and proceed with filter
sample preparation.
11.3 Aqueous Sample - Total Solid Screen
11.3.1 Record sample preparation data in Gross Alpha/Beta (GAB) Solid Screen Excel program
(RAD-0052). Weigh the empty beaker and record weight (under the tare weight header)
11.3.2 Shake the sample container thoroughly.
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11.3.2.1 If alpha and beta are to be determined simultaneously from a single aliquot, the
lowest net residue weight limit applies.
11.3.3 Measure a 20 mL aliquot into a pre-weighed beaker.
11.3.4 Add 10 mL of concentrated Nitric acid.
11.3.5 Evaporate to dryness using a hot plate, do not allow the sample to splatter.
11.3.6 Remove from heat and allow to cool to room temperature.
11.3.7 Add 10 mL concentrated Nitric acid.
11.3.8 Evaporate to dryness using a hot plate. Do not allow the sample to splatter.
11.3.9 Remove from heat and allow to cool in desicator for a minimum of 30 minutes.
11.3.10 Reweigh the beaker in GAB Solid Screen Excel (RAD-0052) program and record weight
(under the gross weight header)
11.3.10.1 By estimating the solid content of the sample, the program will provide the
target aliquot.
11.3.10.2 If GAB Solid Screen Excel program is not available use the formula found in
12.2.
11.3.10.3 From the net residue weight and sample volume used, determine the sample
volume required to meet the target residue weight using the formula given in
step 12.2, with a target weight of 80 mg alpha/beta dried residue on the
planchet (sample weights should not exceed 100 mg, if sample weights
exceed 100 mg an aliquot of the dried residue should be taken after
redissolving in 4 N nitric acid. Dilutions are noted on the worksheet. If it
is not practical to redissolve the residue the sample should be redone
using less volume. If it is not practical to redissolve or restart the sample,
check with the count room supervisor or designee to verify that the
sample weight fits on the current alpha curve before counting.). If only
Gross Beta is being performed, the target weight is to 160 mg. Compare the
calculated volume to meet the weight limitation with the volume required to
ensure that the MDA is below the Reporting Limit. The volume for analysis is
the smaller of the two volumes.
11.4 Aqueous Sample Gross Alpha/Beta
11.4.1 Initiate sample preparation worksheet.
11.4.2 Shake the sample container thoroughly.
11.4.3 Measure a volume of sample, previously determined in section 11.3, into an appropriately
sized beaker. Record volume of sample used.
11.4.3.1 If it is determined (in step 11.3) that only a small volume of sample is required,
additional volume may be added in small aliquots directly to the beaker used to
determine the volume needed to achieve the target sample weight.
11.4.4 Prepare a method blank, LCS and MS.
11.4.5 Add 10 mL of concentrated Nitric acid to all samples and QC.
11.4.6 Evaporate to near dryness using a hot plate. Do not allow the sample to splatter.
11.4.7 Remove from heat and allow to cool to room temperature.
11.4.8 Add 10 mL concentrated Nitric acid.
11.4.9 Evaporate to near dryness using a hot plate. Do not allow the sample to splatter.
NOTE: Some samples with difficult matrices may require steps 11.4.7 through
11.4.9 to be repeated until the sample residue does not change in appearance.
11.4.10 Remove from heat and allow to cool to room temperature.
11.4.11 Add 10 mL of 4 N nitric acid to wash down the sides of the beaker.
11.4.12 Heat on hot plate to dissolve sample residue and reduce volume to approximately 5-7 mL.
11.4.13 Transfer the sample to a ridged stainless steel planchet.
11.4.14 Wash down the beaker with small portions of 4 N HNO-, and add to the planchet.
11.4.15 Evaporate planchets to dryness on a hot plate. Do not allow the sample to splatter.
11.4.16 Remove sample planchets from hot plate.
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11.4.17 Dry planchets in an oven at 105 ± 5 °C for a minimum of 2 hours, if sample appears
hygroscopic. If not hygroscopic proceed to step 11.4.18.
11.4.18 Cool planchets in a desiccator for a minimum of 30 minutes.
11.4.19 Weigh the cooled planchets and record final weight(s).
11.4.19.1 If alpha and beta are to be determined simultaneously from a single aliquot,
the net residue weights for alpha apply; mass should not exceed 100 mg (2.0"
planchet).
11.4.19.2 If alpha only is to be determined simultaneously from a single aliquot, the net
residue weights for alpha apply; mass should not exceed 100 mg (2.0"
planchet).
11.4.19.3 If beta only is to be determined simultaneously from a single aliquot, the net
residue weights for beta apply; mass should not exceed 200 mg (2.0"
planchet).
11.4.20 Store dry sample in a desiccator. The sample is ready for gross alpha and/or beta activity
analysis by GFPC.
11.5 Oil Sample
11.5.1 Initiate appropriate sample worksheet for the samples to be analyzed and complete as
required.
11.5.2 Fill a 50 mL beaker % full with confetti made from Whatman No. 41 filter paper or
ashless paper pulp.
11.5.3 Place beaker on analytical balance, then record the weight in appropriate sample
worksheet.
11.5.4 Weigh to the nearest 0.0001 g, approximately 0.1-lgram of the oil sample onto the
shredded filter paper. Record the sample weight.
11.5.5 Cover with a crucible lid.
11.5.6 If the sample is a mixture of oil and water or is a sample spiked with an aqueous solution,
evaporate the water on a hot plate before muffling. Do not allow residue to "bake" on hot
plate. A programmable muffle program may also be used to dry the water before ramping
the temperature.
11.5.7 Ramp oven to approximately 600° C and hold there for four hours.
11.5.8 Turn off the muffle oven, crack open the door, and allow the sample to cool to room
temperature.
11.5.9 Add approximately 7 mL of 4 N HN03 to the residue in the beaker.
11.5.10 Transfer the sample to a glass beaker with 4 N HN03.
11.5.11 Wash down the beaker and lid with small portions of 4 N HN03 and add to beaker.
11.5.12 Evaporate to dryness on hot plate. Do not allow sample to splatter. Remove from heat and
allow to cool to room temperature.
11.5.13 Add 10 mL of concentrated nitric acid.
11.5.14 Evaporate to dryness on a hot plate. Do not allow sample to splatter.
11.5.15 Remove from heat and allow to cool to room temperature.
11.5.16 Add 10 mL of 4 N nitric acid. Heat to dissolve and then to reduce volume to
approximately 5-7 mL.
11.5.17 Transfer sample to a ridged stainless steel planchet.
11.5.18 Wash down the beaker with small portions of 4 N HN03 and add to the planchet
11.5.19 Evaporate to dryness on a hot plate, do not allow the sample to splatter.
11.5.20 Remove sample from hot plate.
11.5.21 If sample appears hygroscopic, dry planchets in an oven at 105 ± 5 °C for a minimum of 2
hours. If not hygroscopic proceed to step 11.5.22.
11.5.22 Cool planchets in a desiccator for a minimum of 30 minutes.
11.5.23 Weigh the cooled planchets and record final weight.
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11.5.23.1 If alpha and beta are to be determined simultaneously from a single aliquot, the
net residue weights for alpha apply; mass should not exceed 100 mg (2.0"
planchet).
11.5.23.2 If alpha only is to be determined simultaneously from a single aliquot, the net
residue weights for alpha apply; mass should not exceed 100 mg (2.0"
planchet).
11.5.23.3 If beta only is to be determined simultaneously from a single aliquot, the net
residue weights for beta apply; mass should not exceed 200 mg (2.0" planchet).
11.5.24 Store dry sample planchets in a desiccator. The sample is ready for gross alpha and/or
beta activity analysis by GFPC.
11.6 Filter Samples
11.6.1 Initiate appropriate sample worksheet for the samples to be analyzed and complete as
required.
11.6.2 If the filter is less than 2" diameter, secure the air filter in a stainless steel planchet with
double-sided cellophane tape such that no portion of filter extends above the lip of the
planchet. Then proceed to step 11.6.20.
11.6.3 If the filter is 2" diameter, the sample can be placed directly in the dectector.
11.6.4 If the filter is greater than 2" diameter, digest or leach the sample per ST-RC-0004 for
shared filters. Prepare a method blank and LCS from blank filters, spiked as per 9.3.3,
which are digested in the same manner as the samples.
11.6.5 Shake the digested sample thoroughly. Measure a volume of sample into an
appropriately sized teflon beaker. Record volume of sample used.
11.6.6 Add 10 mL of 16 N nitric acid.
11.6.7 Evaporate to dryness on a warm hot plate. Do not allow the sample to splatter.
11.6.8 Remove from heat and allow to cool to room temperature.
11.6.9 Add 10 mL of 16 N nitric acid.
11.6.10 Evaporate to dryness on a warm hot plate, do not allow the sample to splatter.
11.6.11 Remove from heat and allow to cool to room temperature.
11.6.12 Add 10 mL of 4 N nitric acid.
11.6.13 Heat to dissolve and then to reduce volume to approximately 5-7 mL
11.6.14 Transfer the sample to a pre-weighed, stainless steel planchet.
11.6.15 Wash down the beaker with small portions of 4 N HN03 and add to the planchet.
11.6.16 Evaporate to dryness on a warm hot plate. Do not allow the sample to splatter.
11.6.17 If sample appears hygroscopic dry planchets in an oven at 105 ± 5 °C for a minimum of 2
hours. If not hygroscopic proceed to step 11.6.18.
11.6.18 Cool planchets in a desiccator for a minimum of 30 minutes.
11.6.19 Weigh the cooled planchets and record final weight.
11.6.19.1 If alpha and beta are to be determined simultaneously from a single aliquot,
the net residue weights for alpha apply; mass should not exceed 100 mg (2.0"
planchet).
11.6.19.2 If alpha only is to be determined simultaneously from a single aliquot, the net
residue weights for alpha apply; mass should not exceed 100 mg (2.0"
planchet).
11.6.19.3 If beta only is to be determined simultaneously from a single aliquot, the net
residue weights for beta apply; mass should not exceed 200 mg (2.0"
planchet).
11.6.20 Store dry sample in a desiccator. The sample is ready for gross alpha and/or beta activity
analysis by GFPC.
11.7 Solid and/or Soil Samples by Dry, Grind Sprinkle
11.7.1 Initiate appropriate sample worksheet for the samples to be analyzed and complete as
required.
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11.7.2 If the sample has already been prepared per ST-RC-0003, "Drying and Grinding of Soil
and Solid Samples," proceed to step 11.7.8 for direct sample mounting.
11.7.3 Use table salt for the blank and a soil standard reference material, e.g. NIST Traceable
Rocky Flats Soil, for the LCS. Prepare in the same fashion as the samples.
11.7.4 Remove an aliquot (typically 1 - 5 g.) with a spatula and place into a clean, labeled
aluminum weighing pan.
11.7.5 Place sample on a hot plate or in a drying oven at approximately 105° C and evaporate
any moisture.
11.7.6 When dry, remove from hot plate or oven and allow the sample to cool.
11.7.7 If necessary, using a metal spatula, reduce the solid sample to a fine particle size.
11.7.8 Use double sided tape to secure the self-adhesive dots (adhesive side up) to a flat stainless
steel planchet. Self adhesive label dots are used to hold finely divided solid material
uniformly for gross alpha and/or beta analysis. Weigh and record the prepared planchet.
11.7.9 Distribute the sample evenly in the stainless steel planchet.
11.7.10 Record final weight. The target mass is 40-100 mg.
11.7.10.1 If alpha and beta are to be determined simultaneously from a single aliquot,
the net residue weights for alpha apply; mass should not exceed 100 mg (2.0"
planchet).
11.7.10.2 If alpha only is to be determined simultaneously from a single aliquot, the net
residue weights for alpha apply; mass should not exceed 100 mg (2.0"
planchet).
11.7.10.3 If beta only is to be determined simultaneously from a single aliquot, the net
residue weights for beta apply; mass should not exceed 200 mg (2.0"
planchet).
11.7.11 Store dry sample in a desiccator. The sample is ready for gross alpha and/or beta activity
analysis by GFPC.
11.8 Solid and/or Soil Samples by total dissolution.
11.8.1 Initiate sample preparation sheet.
11.8.2 Weigh l.Og sample into a 50 mL beaker and record weight.
11.8.3 Place in oven at 600° and allow to muffle for four hours. Allow to cool.
11.8.4 Transfer to digestion tube using 4 M HN03.
11.8.5 Carefully add 5 mL concentrated nitric acid, 5 mL concentrated hydrochloric acid and 10
mL concentrated Hydrofluoric acid.
11.8.6 Digest in mod block at > 110°C for approximately four hours or until dry.
11.8.7 Carefully add 5 mL concnetrated nitric acid, 5 mL concentrated hydrochloric acid and 10
mL concentrated Hydrofluoric acid.
11.8.8 Digest in mod block at > 110°C for approximately four hours or until dry.
11.8.9 Add 10 mL HN03 and digest in mod block at >110°C for approximately 4 hours or until
dry.
11.8.10 Reflux sample with 10 mL 4M HN03 for 20 minutes using a watchglass over digestion
vessel.
11.8.11 Bring up to 20 mL with 4M HN03 in the digestion vessel.
11.8.12 Transfer 1 mL of sample to a tared planchet and cook to dryness.
11.8.13 Cool in descicator for 30 minutes.
11.8.14 Reweigh the planchet to determine the mass of 1 mL.
11.8.15 Determine the total amount of sample needed to reach the target mass of 100 mg on the
planchet.
11.8.16 Transfer amount of sample to a 250 mL beaker.
11.8.17 Prepare blank. MS and LCS.
11.8.18 Add 10 mL of HN03 and cook to dryness. Allow to cool.
11.8.19 Add 10 mL of 4 N nitric acid.
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11.8.20 Heat on hot plate to dissolve sample residue and then to reduce volume to approximately
5-7 mL.
11.8.21 Transfer the sample to a ridged stainless steel planchet.
11.8.22 Wash down the beaker with small portions of 4 N HN03 and add to the planchet.
11.8.23 Evaporate to dryness on a warm hot plate. Do not allow liquid to splatter.
11.8.24 Remove sample from hot plate.
11.8.24.1 If sample appears hygroscopic, dry planchets in an oven at 105 ± 5 °C for a
minimum of 2 hours.
11.8.25 Weigh the cooled planchets and record final weight.
11.8.25.1 If alpha and beta are to be determined simultaneously from a single aliquot,
the net residue weights for alpha apply; mass should not exceed 100 mg (2.0"
planchet).
11.8.25.2 If alpha only is to be determined simultaneously from a single aliquot, the net
residue weights for alpha apply; mass should not exceed 100 mg (2.0"
planchet).
11.8.25.3 If beta only is to be determined simultaneously from a single aliquot, the net
residue weights for beta apply; mass should not exceed 200 mg (2.0"
planchet).
11.8.26 Store dry sample in a desiccator. The sample is ready for gross alpha and/or beta activity
analysis by GFPC.
11.9 Reprocessing planchets which are over the weight limit.
11.9.1 Rinse residue from planchet with 4 N HN03 into a beaker. Add 4 N HN03 to planchet
and heat if necessary to complete the transfer.
11.9.2 Redissolve the residue into 4 N HN03. Dilute the sample to a known volume.
11.9.3 Remove an aliquot which will keep the residue weight under the limit (100 mg) and
transfer to the pre-weighed planchet. Record information on sample worksheet.
11.9.4 Evaporate to dryness on a warm hot plate so that the sample does not boil.
11.9.5 Remove sample from hot plate. Allow to cool.
11.9.6 Weigh the cooled planchet and record final weight.
11.9.7 Store dry sample in a desiccator. The sample is ready for gross alpha and/or beta activity
analysis by GFPC.
12.0 DATA ANALYSIS AND CALCULATIONS
12.1 Commonly used calculations (e.g. % recovery and RPD) and standard instrument software
calculations are given in the T est America St. Louis ST-QAM. Specific analysis calculations are
given in the applicable analytical SOP.
12.2 To calculate the aqueous sample volume required (ml), use the following equation:
,. T. targetnet residueweight(mg)* initialaliquotvolume(mL)
volumerequired(mL) =
initialaliquotnetresidueweight(mg)
13.0 DATA ASSESSMENT AND ACCEPTANCE CRITERIA; CORRECTIV E ACTIONS FOR
OUT OF CONTROL DATA
13.1 Data assessment does not pertain to this sample preparation procedure.
13.2 Samples requiring re-preparation are submitted to the preparation lab with a NCM detailing the
issue. The NCM process is described in SOP: ST-QA-0036. Specific information is given in the
applicable analytical SOP.
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14.0 METHOD PERFORMANCE AND DEMONSTRATION OF CAPABILITY
14.1 Method performance data, Reporting Limits, and QC acceptance limits, are given in LIMS
14.2 Demonstration of Capability
14.2.1 Initial and continuing demonstrations of capability requirements are established in the ST-
QAM.
14.3 Training Qualification
14.3.1 The manager/supervisor has the responsibility to ensure that this procedure is performed
by an analyst who has been properly trained in its use and has the required experience.
14.3.2 The analyst must have successfully completed the initial demonstration capability
requirements prior to working independently. See requirements in the ST-QAM.
14.4 Annually, the analyst must successfully demonstrate proficiency to continue to perform this
analysis. See requirements in the ST-QAM.
15.0 VALIDATION
15.1 Laboratory SOPs are based on published methods (EPA, DOE, ASTM, Eichrom, Standard
Methods) and do not require validation by the laboratory. The requirements for laboratory
demonstration of capability are included in the ST-QAM. Laboratory validation data would be
appropriate for performance based measurement systems, non-standard methods and significant
modifications to published methods. Data from said validations is held in the QA department.
16.0 WASTE MANAGEMENT AND POLLUTION PREV ENTION
16.1 All waste will be disposed of in accordance with Federal, State and Local regulations. Where
reasonably feasible, technological changes have been implemented to minimize the potential for
pollution of the environment. Employees will abide by this method and the policies in the
Corporate Safety Manual for "Waste Management and Pollution Prevention."
16.2 Waste Streams Produced by the Method
16.2.1 The following waste streams are produced when this method is carried out.
16.2.1.1 Acidic sample waste generated. All acidic waste will be accumulated in the
appropriate waste accumulation container, labeled as Drum Type "A" or "B".
17.0 REFERENCES
17.1 "Prescribed Procedures for Measurement of Radioactivity in Drinking Water," Method 900.0,
August, 1980.
17.2 "Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, SW846, Method 9310,
Rev. 0, September, 1986.
17.3 DOE Method RP-710, "Laboratory Method for Gross Alpha and Beta Activity Determination,
1997
17.4 TestAmerica St. Louis Laboratory Quality Assurance Manual (ST-QAM)
17.5 Corporate Environmental Health and Safety Manual (CW-E-M-001) and Facility addendum.
17.6 Associated SOPs
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17.6.1 ST-PM-0002, Sample Receipt and Chain of Custody
17.6.2 ST-RC-0002, Preparation of Stainless Steel Planchets for Radiochemistry Analyses.
17.6.3 ST-RC-0003, Drying and Grinding of Soil and Solid Samples
17.6.4 ST-RC-0004, Preparation of Soil, Sludge and Filter Paper Samples for Radiochemical
Analysis
17.6.5 ST-RC-0021, Gross Alpha Radiation in Water Using Coprecipitation
17.6.6 ST-RD-0403, Daily Calibration Verification and Maintenance of the Low Background
Gas Flow Proportional Counting System
17.6.7 ST-RC-5006, Decontamination of Laboratory Glassware. Labware and Equipment
17.6.8 ST-QA-0002, Standards and Reagent Preparation
17.6.9 ST-QA-0005, ST-QA-0005, Calibration and Verification Procedure for Thermometers,
Balances, Weights and Pipettes
17.6.10 ST-QA-0036, Non-conformance Memorandum (NCM) Process
18.0 CLARIFICATIONS, MODIFICATIONS TO THE REFERENCE METHOD
18.1 None.
19.0 CHANGES FROM PREVIOUS REVISION
19.1 Updated section 9.2.7: added leached analyses use of a method blank that is comprised of leaching
acid.
19.2 Replaced piptte with pre-weighted beaker to measure sample aliquot in section 11.3.3.
19.3 Rev 14:
19.3.1 Updated the total dissolution procedure for solid/soil samples in Section 11.8.
19.4 Revision 15:
19.4.1 Added required pH checking for all aqueous samples prior to analysis in section 8.3.
19.5 Revision 16:
19.5.1 Added reference to DOE Method RP-710 to Sections 1 and 17
19.6 Revision 17:
19.6.1 Updated section 15.
19.6.2 Removed Structure and Analysis Codes from SOP and referenced LIMS as the new
source to recover that information in section 1.0.
19.6.3 Removed references to 'Clouseau" and "Quantims", replaced with LIMS.
19.6.4 Updated method requirements for Air Filter samples in section 2.0.
19.6.5 Updated supplies in section 6.0.
19.6.6 Updated reagents and standards in section 7.0.
19.6.7 Replaced the use of a porcelain crucible with a beaker throughout section 11.0.
19.7 Rev. 18:
19.7.1 Section 8, removed sample hold time
19.7.2 Section 11.3.1, added GAB solid screen form Rad-0052
19.7.3 Section 11.1.10, added GAB solid screen form Rad-0052
19.7.4 Grammatical errors fixed throughout
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TestAmerica
THE LEADER IN ENVIRONMENTAL TESTING
TestAmerica St. Louis
SOP No. ST-RC-0025, Rev. 15
Effective Date: 08/30/2013
Page No.: 1 of 14
Title: PREPARATION OF SAMPLES FOR GAMMA SPECTROSCOPY
[EPA 901.1 arid DOE GA-01-R]
Approvals (Signature/Date):
Sarah Bernsen
?adiochemistry Prep Supervisor
Tony L
Qualit
Marti Ward
surance Specialist
Date
'0
Terr/ Romanko for Date
Mi&Aael Ridenhower
Health & Safety Manager / Coordinator
Elaine Wild
Laboratory Director
%im3
Date
This SOP was previously identified as SOP No. ST-RC-0025 Rev. 14
Copyright Information:
This documentation has been prepared by TestAmerica Laboratories, Inc. and its affiliates ("TestAmerica"), solely
for their own use and the use of their customers in evaluating their qualifications and capabilities in connection with
a particular project. The user of this document agrees by its acceptance to return it to TestAmerica upon request and
not to reproduce, copy, lend, or otherwise disclose its contents, directly or indirectly, and not to use if for any other
purpose other than that for which it was specifically provided. The user also agrees that where consultants or other
outside parties are involved in the evaluation process, access to these documents shall not be given to said parties
unless those parties also specifically agree to these conditions.
THIS DOCUMENT CONTAINS VALUABLE CONFIDENTIAL AND PROPRIETARY INFORMATION.
DISCLOSURE, USE OR REPRODUCTION OF THESE MATERIALS WITHOUT THE WRITTEN
AUTHORIZATION OF TESTAMERICA IS STRICTLY PROHIBITED. THIS UNPUBLISHED WORK
BY TESTAMERICA IS PROTECTED BY STATE AND FEDERAL LAW OF THE UNITED STATES. IF
PUBLICATION OF THIS WORK SHOULD OCCUR THE FOLLOWING NOTICE SHALL APPLY:
©COPYRIGHT 2013 TESTAMERICA ANALYTICAL TESTING
Facility Distribution No.:
Distributed To: See Electronic Distribution Sheet
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SOP No. ST-RC-0025, Rev. 15
Effective Date: 08/30/2013
Page No.: 2 of 14
1.0 SCOPE AND APPLICATION
1.1 The purpose of this SOP is to provide detailed instructions for the preparation of samples which
require gamma spectroscopy analysis.
1.2 This SOP describes methods for the preparation of samples of liquid, soil, vegetation, air filter,
and core matrices prior to gamma spectroscopy analysis.
1.3 This SOP is based on EPA Method 901.1 and DOE Method GA-01 -R.
1.4 The laboratory target analytes supported by this method, the reporting limits, and QC limits are
maintained in the Laboratory Information Management System (LIMS).
2.0 SUMMARY OF METHOD
2.1 Samples are transferred to a standard geometry container for counting on the gamma detectors.
High purity germanium (HPGe) gamma detectors are used to detect isotopes with gamma ray
energies between 40 and 2000 KeV. Activity concentration is determined using commercially
available gamma spectral analysis software. A sample matrix which can be mounted in one of the
standard geometries may be analyzed for any of the isotopes included in the radionuclide
reference library. Detection limits may be affected by the sample size. Gamma photon energies
not identified in the reference library may be identified and evaluated manually.
3.0 DEFINITIONS
3.1 See the TestAmerica St. Louis Quality Assurance Manual (ST-QAM) for a glossary of common
laboratory terms and data reporting qualifiers.
3.2 Replicate Analyses - Two or more analysis of the same sample whose independent measurements
are used to determine the precision of equipments analytical procedure.
4.0 INTERFERENCES
4.1 Gamma energy emissions identified with scientifically measured probability by some radionuclides
are documented by multiple sources. There are some discrepancies between reference sources and
attempts are made to evaluate the reference data used in spectral analysis. Gamma emissions at
discreet energy and probability are used to identify and quantify specific radionuclides in the sample.
Gamma emissions which are completely absorbed by an HPGe detector form photo peaks which are
used for identification and quantification of gamma emitting radionuclides. When two or more
nuclides emit similar gamma energy the photo peaks cannot be resolved without using complex
algorithms. These photo peaks in close proximity can interfere with the identification or
quantification of a radionuclide. Knowing this the nuclide reference library, computer software and
analyst training are used to minimize the possibility of interference and misidentification. It is not
possible to eliminate all interferences and misidentification.
5.0 SAFETY
5.1 Employees must abide by the policies and procedures in the Corporate Environmental Health and
Safety Manual (CW-E-M-001), Radiation Safety Manual and this document. This procedure may
involve hazardous material, operations and equipment. This SOP does not purport to address all of
the safety problems associated with its use. It is the responsibility of the user of the method to
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follow appropriate safety, waste disposal and health practices under the assumption that all
samples and reagents are potentially hazardous. Safety glasses, gloves, lab coats and closed-toe,
nonabsorbent shoes are a minimum.
5.2 SPECIFIC SAFETY CONCERNS OR REQUIREMENTS
5.2.1 Wear Kevlar or MAPA Blue-Grip gloves when using knives or sharp articles.
5.3 PRIMARY MATERIALS USED
5.3.1 The following is a list of the materials used in this method, which have a serious or
significant hazard rating. NOTE: This list does not include all materials used in the
method. The table contains a summary of the primary hazards listed in the MSDS for
each of the materials listed in the table. A complete list of materials used in the method
can be found in the reagents and materials section. Employees must review the
information in the MSDS for each material before using it for the first time or when there
are major changes to the MSDS.
Material (1)
Hazards
Exposure
Limit (2)
Signs and symptoms of exposure
Nitric Acid
Corrosive
Oxidizer
Poison
2 ppm
(TWA)
4 ppm
(STEL)
Nitric acid is extremely hazardous; it is corrosive, reactive,
an oxidizer, and a poison. Inhalation of vapors can cause
breathing difficulties and lead to pneumonia and pulmonary
edema, which may be fatal. Other symptoms may include
coughing, choking, and irritation of the nose, throat, and
respiratory tract. Nitric acid can cause redness, pain, and
severe skin burns. Concentrated solutions cause deep ulcers
and stain skin a yellow or yellow-brown color. Vapors are
irritating and may cause damage to the eyes. Contact may
cause severe burns and permanent eye damage.
1- Always add acid to water to prevent violent reactions.
2 - Exposure limit refers to the OSHA regulatory exposure limit.
TWA - Time Weighted Average
STEL - Short Term Exposure Limit
EQUIPMENT AND SUPPLIES
6.1
Balance, top loader
6.2
Blender
6.3
Food chopper/grinder
6.4
Knives appropriate for food preparation
6.5
Graduated cylinder
6.6
Filter disk, 47 millimeter diameter
6.7
Plastic Tape
6.8
Marinelli beakers of various sizes (500-mL and 1000-mL)
6.9
Petri dishes, 2-inch diameter
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6.10 Can Sealer
6.11 Cans and lids (commonly referred to as tuna cans)
6.12 8 oz, straight sided polypropylene jars or equivalent; (used for 25 mL and 100 mL geometries)
6.13 Teflon® or glass beakers (250-mL, 400-mL)
6.14 Disposable digestion vessels
6.15 Muffle furnace (programmable)
6.16 TEXPEN®
6.17 Teflon® beaker covers
6.18 Watch glasses
7.0 STANDARDS AND REAGENTS
7.1 All standards and reagent preparation, documentation and labeling must follow the requirements
of SOP ST-QA-0002.
7.2 DI Water obtained from the Milli-Q® unit.
7.3 Nitric acid (16 NHN03) concentrated
7.3.1 Nitric acid (4 N HN03) - to an appropriately sized bottle containing 1500 mL of DI water;
add 500 mL of 16 N HNO3.
7.4 Hydrochloric acid (12 N HCL) - concentrated, 37.2%
7.5 Hydrofluoric acid (HF 48.52%) - concentrated
7.6 Radiacwash™ solution 10% - add 100 mL of Radiac to 1 L of water
7.7 Bleach solution 10% - add 100 mL of bleach to 1 L of water
7.8 Sodium Sulfate
8.0 SAMPLE COLLECTION, PRESERVATION AND STORAGE
8.1 TestAmerica St. Louis supplies sample containers and chemical preservatives in accordance with
the method. TestAmerica St. Louis does not perform sample collection. Samplers should
reference the methods referenced and other applicable sample collection documents for detailed
collection procedures. Sample volumes and preservative information is given in ST-PM-0002.
8.2 Samples may be collected in glass or plastic containers.
8.3 Aqueous samples are preserved with nitric acid to a pH of less than 2, unless 1-129 or 1-131 is
requested. Samples collected for 1-129 or 1-131 analysis are not preserved.
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8.3.1 The pH of aqueous samples are checked upon receipt by Sample Control, therefore, the pH
does not require checking prior to analysis
8.3.1.1 Aqueous samples acidified upon receipt (designated by a label on the bottle) do
require checking the pH prior to analysis.
8.4 Milk samples are not chemically preserved.
QUALITY CONTROL
9.1 Batch
9.1.1 A sample batch is a maximum of 20 environmental samples, which are prepared together
using the same process and same lot(s) of reagents. Where no preparation method exists
(i.e. water sample volatile organics, water sample anion analysis) the batch is comprised
of a maximum of 20 environmental samples which are analyzed together with the same
process, lots of reagents and personnel.
9.1.2 Instrument conditions must be the same for all standards, samples and QC samples.
9.1.3 For this analysis, batch QC consists of a Method Blank (MB), a Laboratory Control
Sample (LCS), and Sample Replicate.
9.1.3.1 A Sample Duplicate may be performed at the request of the client. See client
requirements.
9.2 Method Blank
9.2.1 For Water and Liquid analyses, the method blank is comprised of DI water.
9.2.2 For Soil and Solids analyses, the method blank is comprised of sodium sulfate.
9.2.3 For Filter analyses, the method blank is comprised of a Petri dish.
9.2.4 A Method Blank must be prepared with every sample batch.
9.3 Laboratory Control Sample
9.3.1 An LCS is a blank matrix spiked with a known amount of analyte(s), processed
simultaneously with, and under the same conditions as, samples through all steps of the
analytical procedure.
9.3.2 The LCS is a purchased sealed source standard in the prescribed geometry for the sample
analysis.
9.3.3 An LCS must be prepared with every sample batch.
9.4 Sample Duplicate
9.4.1 A sample duplicate is an additional aliquot of a field sample taken through the entire
analytical process to demonstrate precision (a replicate analysis of the original sample
counted on a different detector will be performed as the duplicate).
9.5 Procedural Variations/ Nonconformance and Corrective Action
9.5.1 Any variation shall be completely documented using a Nonconformance Memo and
approved by the Supervisor and QA Manager. See SOP ST-QA-0036 for details
regarding the NCM process.
9.5.2 Any deviations from QC procedures must be documented as a nonconformance, with
applicable cause and corrective action approved by the Supervisor and QA Manager. See
SOP ST-QA-0036 for details regarding the NCM process.
9.6 Decontamination of Tuna Can Sealer
9.6.1 The sealer must be wiped down with 10% Radiacwash™ solution daily
9.6.1.1 Analyst must record the information in the daily logbook.
9.6.2 Sealer will be monitored for contamination as part of the monthly contamination survey,
as per SOP ST-RP-0032
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10.0 CALIBRATION AND STANDARDIZATION
10.1 The balance must be calibrated in accordance with ST-QA-0005.
10.2 For Gamma Spectroscopy calibration requirements, see ST-RD-0102.
11.0 PROCEDURE
11.1 Liquid Sample Preparation
11.1.1 Liquid samples shall be prepared as a 25 mL, 100 mL, 500 mL, or 1000 mL geometry.
11.1.2 Determine the proper geometry.
11.1.2.1 The volume of sample used depends on the amount required to meet the detection
limits, the volume of sample supplied by the client, and whether the sample has
very high activity. The sample volume may be reduced for high activity samples
due to detector dead time considerations. Consult the count room supervisor or
radiochemistry technical director, if the sample has high activity which may
require such consideration.
11.1.3 Label the top of the container with the sample Id
11.1.4 Shake the sample to suspend any residue and to ensure that the sample is homogeneous.
11.1.5 Write sample information (i.e. ID #) on the container.
11.1.6 Measure the required sample volume (25, 100, 500 or 1000 mL) by comparing the sample
to the reference container
11.1.6.1 Reference containers are pre-made geometries comprised of DI water measured
volumetrically.
11.1.6.2 If the client does not provide sufficient sample, and the sample is near a larger
geometry, rather than reducing the volume significantly it may be preferable to
dilute an aqueous sample with DI water to the correct volume in order to achieve a
lower MDC. Consultant Supervisor/Manager to determine which action is
preferable.
11.1.6.2.1 If the sample is diluted the undiluted volume is recorded as the
sample volume. The dilution is only for fitting the calibrated
geometry.
11.1.7 Place the lid securely on the container.
11.1.7.1 Remove excess air from Marinelli.
11.1.7.2 If the density is suspected to be greater than 1.2 g/ mL or less than 0.98 g/mL,
generate a NCM. To determine the density use form RAD-0075_Density.xls
(include form with batch paper work if utilized) Attachment 1
11.1.7.2.1 Form directory: \\slsvr01\OA\FORMS\ST-LQUIS\RAD
11.1.8 Seal the lid using plastic tape. Marinelli beakers are prone to leaking liquids; the tape is
tightly wrapped around the lid and the beaker in three layers each overlapping the previous
layer with half the width of the tape. Make sure there are no creases in the tape which will
form a channel for leakage.
11.1.9 Inspect for leakage.
11.1.10 Generate a label and print proper paperwork then submit to count room for analysis by
gamma spec.
11.2 Soil Sample Preparation
11.2.1 Soil samples for 1-129 or 1-131 analysis are not dried and ground but rather inserted into
an appropriate calibrated geometry. Proceed to step 11.2.3.
11.2.2 Soil samples, which do not require 1-129 or 1-131 analyses, are prepared in accordance with
SOP ST-RC-0003 or ST-RC-0014.
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11.2.3 Soil samples shall be prepared as 200 mL sealed (tuna) can, 100 mL, or 25 mL, or 500 mL
Marinelli (marnsoil) geometry based on the amount of available sample. In both the tuna
can and marnsoil geometries, the soil should nearly fill the container.
11.2.3.1 For 1-129 analysis only a 25 mL or 100 mL straight sided poly jar geometry may
be used (check with count room analyst on which geometry I-129/I-131 is
calibrated for and prep the sample using a matching geometry).
11.2.4 Write sample information (i.e. ID #) on the sample container.
11.2.5 Pre-weigh the empty container (tare weight) and record weight in TALS and on the
container lid.
11.2.6 Fill the container with the appropriate amount of sample as described below.
11.2.6.1 Fill tuna cans to the ridge mark with sample. If there is insufficient sample to fill
the can to the ridge, reduce geometry size.
11.2.6.2 Fill 100 mL geometry to the level as denoted on the reference container. If there is
insufficient sample to fill, reduce the geometry size.
11.2.6.2.1 A 100 mL "reference" bottle is marked with the appropriate fill
level.
11.2.6.3 Fill 25 mL geometry to the level as denoted on the reference bottle. If there is
insufficient sample to fill the 25 mL geometry, write a NCM stating insufficient
sample provided for routine analysis.
11.2.6.3.1 A 25 mL "reference" container is marked with the appropriate fill
level.
11.2.6.4 Fill 500 mL Marinelli beakers to the ridge mark just below the lid with sample. If
there is insufficient sample to fill the marnsoil to the ridge, reduce geometry size.
11.2.7 Close the sample container securely.
11.2.8 Seal the container with plastic tape. For tuna cans, seal with can sealer, wipe samples clean
with paper towel and DI water.
11.2.9 Place the sample on the balance; record the weight of the sample on the gamma worksheet
(total weight of container plus sample minus the tare weight of the empty container).
11.2.10 Generate a label and proper paperwork then submit to count room for analysis by gamma
spec.
11.3 Vegetation Sample Preparation (No digestion)
11.3.1 Vegetation samples may be prepared in an appropriate calibrated geometry counted directly
as dried and chopped matrix or green unprocessed matrix (if directed to do so by the client
or if 1-131 or 1-129 is to be reported).
11.3.1.1 Green unprocessed samples can be reported on a wet or dry basis, determined by
client or Project Manager.
11.3.1.1.1 Vegetation samples for 1-129 or 1-131 analysis are not dried but
rather inserted into an appropriate calibrated geometry.
11.3.1.1.2 Dry weight can be determined on sample(s) not dried by using the
percent moisture.
11.3.1.2 Consult the client requirements, client requirement memorandums or the
Supervisor/Manager to determine proper sample handling.
11.3.2 The sample shall be counted in a 500 mL Marinelli, 100 mL, or 25 mL geometry. The
container is filled to the appropriate level with the sample.
11.3.2.1 1-129 analysis uses only a 25 mL or 100 mL straight sided poly jar geometry
(check with count room analyst on which geometry I-129/I-131 is calibrated for
and prep the sample using a matching geometry).
11.3.3 Write sample information (i.e. ID #) on the container.
11.3.4 Pre-weigh the empty container and record weight in TALS and on lid of container.
11.3.5 Place sample in the tared container.
11.3.5.1 Compress the sample when filling a 500 mL Marinelli beaker
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11.3.6 Place the sample on the balance; record the weight of the sample on the gamma worksheet
(total weight of container plus sample minus the tare weight of the empty container).
11.3.6.1 Verify with the Project Manager if sample is to be reported on a wet or dry basis.
11.3.7 Close the sample container securely, seal with plastic tape
11.3.8 Generate a label and print proper paperwork then submit to count room for analysis by
gamma spec.
11.4 Vegetation Sample Preparation (with digestion)
11.4.1 Vegetation samples may be digested and then placed into a appropriate calibrated geometry
and counted as a liquid matrix.
11.4.1.1 Green unprocessed samples can be reported on a wet or dry basis, determined by
the client or project manager.
11.4.1.1.1 Iodine isotopes (e.g. 1-125, 1-129 or 1-131) cannot be prepared
using digestion technique due to volatility.
11.4.1.2 Consult the client requirements and Supervisor/Manager to determine proper
handling.
11.4.2 Label an appropriate sized beaker with a TEXPEN® to ensure identification post muffling
11.4.3 Transfer sample into beaker and record the weight on the gamma worksheet
11.4.3.1 Check with the Project Manager to determine if sample is to be reported on a wet
or dry basis.
11.4.4 Cover sample with 8 N HN03 and allow to sit overnight.
11.4.5 Place beaker on hot plate and gently heat so that sample does not splatter. Periodically stir
sample
11.4.6 Wash down sides of the beaker with small amounts of 30% H202 and small amounts of 8M
HN03. Continue this process periodically as sample digests on hot plate.
11.4.7 Cook sample down to dryness.
11.4.7.1 Upon visual inspection if sample is orange in color, cover sample with 16M HN03
and continue to wet ash with 30% H202.
11.4.7.2 Repeat 11.4.7 and 11.4.7.1 until sample is lightyellow orwhite in color.
11.4.8 Cover beaker with a watch glass and place into the muffle oven.
11.4.9 Heat at 600° C for a minimum of 4 hours to reduce the sample
11.4.10 Allow beakers to cool to room temperature before removing from the oven.
11.4.10.1 The sample may be wet ashed again if yellow color remains.
11.4.11 Reflux samples with enough of 4 N HN03 to cover sample for approximately 30 minutes,
using a watch glass to cover the beaker.
11.4.12 Quantitatively transfer sample to a labeled digestion vessel or Teflon® beaker with a
minimal amount of 4 N HN03.
11.4.13 Add 5 mL of 16 NHN03, 5 mL of 12 NHC1 and 10 mL of concentrated HF
11.4.14 Bring sample to dryness
11.4.14.1 If using a digestion vessel, place in MOD Block
11.4.14.2 If using a Teflon® beaker, heat on a hotplate
11.4.15 Repeat steps 11.4.10 and 11.4.11
NOTE: The amount of acid will vary depending on the sample aliquot. When
increasing the aliquot, increased acid will be required
11.4.16 Reflux the sample in 10 to 20 mL of 4 N HN03. Allow to reflux with a watch glass over
the beaker for approximately 30 minutes to ensure samples goes into solution.
11.4.16.1 If sample does not go into solution additional digestions may be required
(see Supervisor/Manager/Technical Director for guidance)
11.4.17 Label appropriate size container (25 or 100 mL)
11.4.18 Quantitatively transfer sample to container by rinsing with minimal amount of 4 N HN03
11.4.19 Bring to volume to match the reference container
11.4.20 Close the sample container lid securely and seal with plastic tape.
11.4.21 Inspect for leakage.
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11.4.22 Generate a label and print proper paperwork then submit to count room for analysis by
gamma spec.
11.5 Air Filters/Swipes (no digestion)
11.5.1 Air filters may be counted as single filters or as composite filters.
11.5.1.1 Consult client requirements and Supervisor/Manager for instruction.
11.5.1.2 Air filters are reported as pCi/sample or pCi/g. The weight to the air filter is
required if the reporting units is pCi/g.
11.5.2 Write sample information (i.e. ID#) on Petri dish.
11.5.3 Filters with reporting units of
11.5.3.1 pCi/g proceed to 11.5.4
11.5.3.2 pCi/sample proceed to 11.5.5
11.5.4 Pre-weigh empty Petri dish, record the weight in TALS and then on the lid of the Petri dish.
11.5.5 Load air filter(s) directly into Petri dish
11.5.6 Place lid on Petri dish, for pCi/g record the weight of the sample (container and sample
weight minus container weight) in TALS.
11.5.7 Secure the Petri dish lid with plastic tape
11.5.8 Generate a label and print proper paperwork then submit to count room for analysis by
gamma spec.
11.6 Air Filters/Swipes (with digestion)
11.6.1 Air filters are digested and counted as a liquid.
11.6.2 Label a 250 mL beaker with a TEXPEN® to ensure identification post muffling.
11.6.3 Place sample into beaker
11.6.4 Place sample beaker in muffle oven and cover with a watch glass.
11.6.5 Ramp air filter in muffle oven
11.6.5.1 Refer to ST-RC-004 for ramping settings
11.6.6 Allow beakers to cool to room temperature
11.6.7 Digest filter in accordance with sections 11.4.9to 11.4.12
11.6.8 Label appropriate size container (25 to 100 mL)
11.6.9 Transfer sample to container with minimal amount of 4 N HN03.
11.6.10 Bring to volume using reference container as a guide
11.6.11 Place lid securely on the container
11.6.12 Seal the lid using plastic tape
11.6.13 Inspect for leakage.
11.6.14 Generate a label and proper paperwork then submit to count room for analysis by gamma
spec.
11.7 Core Samples
11.7.1 To obtain sample, cut Shelby tube or sample container into two pieces.
11.7.1.1 Using a rigid pipe cutter cut the tube completely through.
11.7.1.2 Usingawire saw, cut through the sample.
11.7.1.3 Cuts should be made at 2 inch intervals.
11.7.1.4 Remove sample from every other sliced section of the Shelby tube.
11.7.1.5 Dry and grind the sample as described in SOP ST-RC-0003.
11.7.2 Aliquot 500 g of sample
11.7.2.1 If less than 500 g of sample is available, contact Supervisor/Manager for
instruction.
11.7.2.2 Soil samples shall be prepared as 200 mL sealed (tuna) can, 100 ml, or 25 ml, or
500 mL Marinelli (marnsoil) geometry based on the amount of available sample.
In both the tuna can and marnsoil geometries, the soil should nearly fill the
container.
11.7.3 Pre-weigh the empty container and record the weight on the container lid and in TALS
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11.7.4 Writer sample information (i.e. ID#) on the sample container
11.7.5 Place the dried sample into the container for counting.
11.7.6 Weigh and record sample weight in TALS .
11.7.7 Secure the lid on the container with plastic tape.
11.7.8 Generate a label and print proper paperwork then submit to count room for analysis by
gamma spec.
11.8 Food: vegetables, produce, grain or animal feed:
11.8.1 Vegetables, produce and grain samples may be prepared in a 500 mL Marinelli beaker or 1
liter Marinelli beaker geometry depending on the requested reporting limit. These matrices
are counted directly as whole grain, chopped or blended produce or vegetable matrices
without drying unless directed by the client to dry the matrix.
11.8.1.1 Consult the client requirements and Supervisor/Manager for instruction.
11.8.2 For vegetables and produce, prepare the sample by chopping with a knife on a cutting board
or using a food processor.
11.8.3 Write sample information (i.e. ID #) on the appropriate container.
11.8.4 Pre-weigh the empty container and record weight on container and in TALS.
11.8.5 Place processed sample in the pre-weighed container.
11.8.6 Compress the sample when filling a 500 mL Marinelli beaker
11.8.7 Weigh sample and record the weight in TALS as WET weight in grams.
11.8.7.1 If the sample is dried, record the DRY weight.
11.8.8 Close the sample container securely, seal with plastic tape.
11.8.9 Generate a label and print proper paperwork then submit to count room for analysis by
gamma spec.
11.9 Food: meat and fish:
11.9.1 Meat and fish may be prepared in a 500 mL Marinelli beaker or 1 liter Marinelli beaker
geometry depending on the requested reporting limit. These matrices are counted directly
without drying.
11.9.1.1 Consult the client requirements and Supervisor/Manager for instruction.
11.9.2 For meat and edible portions of fish, prepare the sample by chopping with a knife on a
cutting board.
11.9.2.1 Fish sample are to be filleted prior to chopping.
11.9.2.2 For analysis of fish when the whole fish is required to be analyzed, remove the
head with a knife and cut the fish into pieces of appropriate size to easily fit into
the Marinelli beaker without air voids. Place the heads in the main portion of the
Marinelli and surround it with pieces to eliminate air voids or spaces.
11.9.3 Write sample information (i.e. ID #) on the container.
11.9.4 Pre-weigh the empty container and record weight on container and in TALS.
11.9.5 Place processed sample in the pre-weighed container.
11.9.6 Compress the sample evacuating any space in the geometry when filling a Marinelli beaker
11.9.7 Weigh sample and record the weight in TALS as WET weight in grams.
11.9.8 Close the sample container securely, seal with plastic tape.
11.9.9 Generate a label and print proper paperwork then submit to count room for analysis by
gamma spec.
11.10 Store unused portions of sample in appropriately sized poly containers. Food and Vegetation
samples are to be refrigerated.
12.0 DATA ANALYSIS AND CALCULATIONS
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12.1 There are no calculations pertaining to this sample preparation procedure.
12.2 Commonly used calculations (e.g. % recovery and RPD) and standard instrument software
calculations are given in the TestAmerica St. Louis ST-QAM. Specific analysis calculations are
given in the applicable analysis SOP.
12.3 Percent Moisture: Mass of original sample minus mass of dried sample divided by mass of dried
sample.
W-D
12.3.1 p =
D
p = fraction of total evaporable moisture content of sample
II' = mass of the original sample
D = mass of dried sample
12.4 Density: Sample weight divided by the volume of said sample weight
m
12.4.1 d - —
v
d = density
m = mass
v = volume
13.0 DATA ASSESSMENT AND ACCEPTANCE CRITERIA; CORRECTIVE ACTIONS FOR
OUT OF CONTROL DATA
13.1 Data assessment does not pertain to this sample preparation procedure.
13.2 Samples requiring re-preparation are submitted to the preparation lab with a NCM detailing the
issue. The NCM process is described in SOP: ST-QA-0036. Specific information is given in the
applicable analysis SOP.
14.0 METHOD PERFORMANCE AND DEMONSTRATION OF CAPABILITY
14.1 Method performance data, Reporting Limits, and QC acceptance limits, are maintained in the
LIMS.
14.2 Demonstration of Capability
14.2.1 Initial and continuing demonstrations of capability requirements are established in ST-
QAM.
14.3 Training Qualification
14.3.1 The Supervisor/Manager has the responsibility to ensure that this procedure is performed
by an analyst who has been properly trained in its use and has the required experience.
14.3.2 The analyst must have successfully completed the initial demonstration capability
requirements prior to working independently. See requirements in ST-QAM.
14.4 Annually, the analyst must successfully demonstrate proficiency to continue to perform this
analysis. See requirements in ST-QAM
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15.0 VALIDATION
15.1 Laboratory SOPs are based on standard reference EPA Methods that have been validated by the
EPA and the lab is not required to perform validation for these methods. The requirements for lab
demonstration of capability are included in ST-QAM. Lab validation data would be appropriate
for performance based measurement systems or non-standard methods. TestAmerica St. Louis will
include this information in the SOP when accreditation is sought for a performance based
measurement system or non-standard method.
16.0 WASTE MANAGEMENT AND POLLUTION PREVENTION
16.1 All waste will be disposed of in accordance with Federal, State and Local regulations. Where
feasible, technological changes have been implemented minimizing the potential for pollution to
the environment. Employees will abide by this method and the policies in section 13 of the
Corporate Safety Manual for "Waste Management and Pollution Prevention."
16.2 Waste Streams Produced by the Method
The following waste streams are produced when this method is carried out.
16.2.1 Acidic sample waste generated. All acidic waste will be accumulated in the appropriate
waste accumulation container, labeled as Drum Type "A" or "B."
16.2.2 Contaminated disposable glass or plastic materials utilized in the analysis are disposed of
in the sanitary trash. If the lab ware was used for the analysis of radioactive samples and
contains radioactivity at a level of 100 cpm over background as determined by a GM
meter, the lab ware will be collected in waste barrels designated for solid rad waste for
disposal by the EH&S Coordinator.
17.0 REFERENCES
17.1 Prescribed Procedures for Measurement of Radioactivity in Drinking Water Method EPA 901.1.
17.2 Department of Energy (DOE) Environmental Monitoring Laboratory (EML) HASL-300
Procedures Manual, GA-01-R.
17.3 TestAmerica St. Louis Quality Assurance Manual (ST-QAM), current revision.
17.4 TestAmerica Corporate Environmental Health and Safety Manual (CW-E-M-001) and St. Louis
Facility Addendum (SOP ST-HS-0002), current revision.
17.5 Associated SOPs
17.5.1 ST-RC-0003, Drying and Grinding of Soil and Solid Samples
17.5.2 ST-RC-0004, Preparation of Soil, Sludge, and Filter Paper Samples for Radiochemical
Analysis
17.5.3 ST-RD-0102, Gamma Spectroscopy Analysis
17.5.4 ST-PM-0002, Sample Receipt and Chain of Custody
17.5.5 ST-QA-0002, Standard and Reagent Preparation
17.5.6 ST-QA-0036, Non-conformance Memorandum (NCM) process
18.0 CLARIFICATIONS, MODIFICATIONS TO THE REFERENCE METHOD
18.1 None.
19.0 CHANGES FROM PREVIOUS REVISION
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19.1 No Changes, Annual Review
19.2 Rev 11:
19.2.1 Inserted instructions regarding requirements for checking the pH of samples upon receipt
and or priorto analysis in section 8.3.1.
19.2.2 Updated when sample ID's should be written on the container in section 11.0.
19.2.3 Inserted instructions for generating container ID labels throughout section 11.0.
19.2.4 Updated when weighing and recording sample weights/mass should be documented in
gamma worksheet in section 11.0.
19.2.5 Added instructions for properly cleaning tuna cans before storage in section 11.2.9.
19.3 Rev 12:
19.3.1 Extensive revision to entire procedure
19.3.2 Addition of attachment 1
19.4 Rev 13:
19.4.1 Added sodium sulfate to section 7.0.
19.4.2 Updated section 9.2 regarding the matrix of method blanks.
19.5 Rev 14:
19.5.1 Updated vegetation sample with and without digestion throughout section 11.3 and 11.4.
19.6 Rev. 15:
19.6.1 Grammatical corrections and removal of references to QuantlMS through out
19.6.2 Section 3, added definition of replicate analyses
19.6.3 Section 8, removal of 180 day holding time
19.6.4 Section 9, explained that replicate will be used as duplicate for this procedure
19.6.5 Section 9.6, added "record in daily logbook"
19.6.6 Deleted record tare weight on lid in section 11.1.2
19.6.7 Deleted record weight of sample (container and sample weight minus container weight)
on lid in section 11.1.8 , 11.2.9, 11.3.6
19.6.8 Added record weight in TAL S throughout SOP
19.6.9 Added print proper paperwork throughout SOP
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SOP No. ST-RC-0025, Rev. 15
Effective Date: 08/30/2013
Page No.: 14 of 14
Attachment 1
TestAmerica
THE LEADER IN ENVIRONMENTAL TESTING
Date:
Analyst:
DENSITY CORRECTION
DigiTube Lot#:
Balance ID:
Sample ID:
Container
Wt(g)
Sample
Volume
(mL)
Sample +
Container
Wt(g)
Density
(g/mL)
Original
Sample
Aliquot
Adjust
Sample
Aliquot
Instructions:
Record the weight of a Class A digi tube in "Container Wt(g•)"; record the volume of the sample added to the digit tube in "Sample
Volume (mL.)"; record the sample and digi tube in "Sample + Container Wt(g)." "Original Sample Aliquot" is the full sample size
used for the actual analysis.
This density is to be used for sample aliquot correction when a sample is suspected of density less than or greater than 1.
Include this document with batch papemork.
Review is to be completed by a peer (someone other than the analyst handling the samples).
Reviewed by:
Date:
WslSVr01\QA\FORMS\ST-LOUIS
RAD-0075 REV (0)
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TestAmerica
THE LEADER IN ENVIRONMENTAL TESTING
TestAmerica St. Louis
SOP No. ST-RC-0040, Rev. 12
Effective Date: 08/07/2013
Page No.: 1 of 10
Title: TOTAL ALPHA EMITTING ISOTOPES OF RADIUM (TAR)
[EPA 903.0 & SW-846 9315]
Approvals (Signature/Date):
Sarah Bernsen
Radiochemistry Prep Supervisor
Date
Marti Ward
Quality Assurance Manager
Date
Michael Ridefihower ' Date
Health & Safety Manager / Coordinator
SVv.'nji
Elaine Wild
Laboratory Director
till
'ji
te
This SOP was previously identified as SOP No. ST-RC-0040 Rev. 11
Copyright Information:
This documentation has been prepared by TestAmerica Laboratories, Inc. and its affiliates ("TestAmerica"), solely
for their own use and the use of their customers in evaluating their qualifications and capabilities in connection with
a particular project. The user of this document agrees by its acceptance to return it to TestAmerica upon request and
not to reproduce, copy, lend, or otherwise disclose its contents, directly or indirectly, and not to use if for any other
purpose other than that for which it was specifically provided. The user also agrees that where consultants or other
outside parties are involved in the evaluation process, access to these documents shall not be given to said parties
unless those parties also specifically agree to these conditions.
THIS DOCUMENT CONTAINS VALUABLE CONFIDENTIAL AND PROPRIETARY INFORMATION.
DISCLOSURE, USE OR REPRODUCTION OF THESE MATERIALS WITHOUT THE WRITTEN
AUTHORIZATION OF TESTAMERICA IS STRICTLY PROHIBITED. THIS UNPUBLISHED WORK
BY TESTAMERICA IS PROTECTED BY STATE AND FEDERAL LAW OF THE UNITED STATES. IF
PUBLICATION OF THIS WORK SHOULD OCCUR THE FOLLOWING NOTICE SHALL APPLY:
©COPYRIGHT 2013 TESTAMERICA LABORATORIES INC.
Facility Distribution No.:
Distributed To: See Electronic Distribution Sheet
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SOP No. ST-RC-0040, Rev. 12
Effective Date: 08/07/2013
Page No.: 2 of 10
1.0 SCOPE AND APPLICATION
1.1 This procedure describes the determination of total radium, for all isotopes emitting alpha radiation,
using EPA method 903.0, SW846 Method 9315.
1.2 This procedure applies to the analysis of these isotopes in liquid and in other media where dissolution
and carrier exchange are readily available in the laboratory.
1.3 The barium sulfate can be counted for total alpha radiation. The time of the last barium sulfate
precipitation should be recorded and used in calculating the in-growth factor.
1.4 The requested limits (RL), minimum detectable amount (MDA) and QC limits are maintained in the
Laboratory Information Management System (LIMS).
2.0 SUMMARY OF METHOD
2.1 Barium and lead are used to coprecipitate radium as the sulfate. Following chelation with EDTA,
barium sulfate is precipitated, purified and counted in a gas flow proportional counter, measuring
alpha radiation only. Total radium is quantified by applying correction factors for in-growth of
radium-226 progeny, gravimetric yield and counting efficiency.
3.0 DEFINITIONS
3.1 See the TestAmerica Quality Assurance Manual (ST-QAM) for a glossary of common laboratory
terms and data reporting qualifiers .
3.2 There are no specific definitions for this procedure.
4.0 INTERFERENCES
4.1. This procedure screens for radium-226 by measuring the alpha emitting radium isotopes. It follows
that if there is no detectable radium alpha activity there would be no radium-226 above the specified
detection limit.
4.2. Samples which contain natural barium cause inaccurate chemical yield determinations.
5.0 SAFETY
5.1 Employees must abide by the policies and procedures in the Corporate Environmental Health and
Safety Manual (CW-E-M-001), Radiation Safety Manual and this document. This procedure may
involve hazardous material, operations and equipment. This SOP does not purport to address all of
the safety problems associated with its use. It is the responsibility of the user of the method to
follow appropriate safety, waste disposal and health practices under the assumption that all
samples and reagents are potentially hazardous. Safety glasses, gloves, lab coats and closed-toe,
nonabsorbent shoes are a minimum.
5.2 SPECIFIC SAFETY CONCERNS OR REQUIREMENTS
None.
5.3 PRIMARY MATERIALS USED
The following is a list of the materials used in this method, which have a serious or significant
hazard rating. NOTE: This list does not include all materials used in the method. The table
contains a summary of the primary hazards listed in the MSDS for each of the materials
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listed in the table. A complete list of materials used in the method can be found in the reagents
and materials section. Employees must review the information in the MSDS for each material
before using it for the first time or when there are major changes to the MSDS.
Material (1)
Hazards
Exposure
Limit (2)
Signs and symptoms of exposure
Nitric Acid
Corrosive
Oxidizer
Poison
2 ppm
(TWA)
4ppm
(STEL)
Nitric acid is extremely hazardous; it is corrosive, reactive,
an oxidizer, and a poison. Inhalation of vapors can cause
breathing difficulties and lead to pneumonia and pulmonary
edema, which may be fatal. Other symptoms may include
coughing, choking, and irritation of the nose, throat, and
respiratory tract. Can cause redness, pain, and severe skin
burns. Concentrated solutions cause deep ulcers and stain
skin a yellow or yellow-brown color. Vapors are irritating
and may cause damage to the eyes. Contact may cause
severe burns and permanent eye damage.
Sulfuric Acid
Corrosive
Poison
Cancer
Hazard
1 mg/m3
(TWA)
Inhalation may cause irritation of the nose and throat, and
labored breathing. Skin contact symptoms include redness,
pain, and severe burning. Eye contact can cause blurred
vision, redness, pain, and severe tissue burns.
Acetic Acid,
Glacial
Corrosive
Flammable
10 ppm
(TWA)
Inhalation causes respiratory tract irritation including nasal
discharge, hoarseness, coughing, chest pain, and breathing
difficulty. Skin contact symptoms may include redness or
discoloration, swelling, itching, burning, or blistering of
skin. Eye symptoms include irritation, burning sensation,
pain, watering, and/or change of vision.
Ammonium
Hydroxide
Poison
Corrosive
50 ppm
(TWA)
Inhalation symptoms include irritation to the respiratory
tract. Ingestion symptoms include pain in the mouth, chest,
and abdomen, with coughing, vomiting and collapse. Skin
contact causes irritation and burns. Eye contact with vapors
causes irritation.
1 - Always add acid to water to prevent violent reactions.
2 - Exposure limit refers to the OSHA regulatory exposure limit.
TWA - Time Weighted Average
STEL - Short Term Exposure Limit
EQUIPMENT AND SUPPLIES
6.1
Centrifuge tubes, 50 mL
6.2
Centrifuge
6.3
Hot plate
6.4
Analytical balance
6.5
Stainless steel planchet
6.6
Syringe, 20 mL, ,45mm filter
6.7
Glassware, beakers
6.8
Water Bath
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6.9 Desiccator
7.0 REAGENTS AND STANDARDS
7.1 All standards and reagent preparation, documentation and labeling must follow the requirements
of SOP ST-QA-0002, current revision.
7.2 DI water from the Millipore unit.
7.3 Acetic acid (17.4 N, 99.8%), concentrated glacial CH3COOH, specific gravity 1.05.
7.4 Ammonium hydroxide (15 N, 56.6%), concentrated NH4OH, sp. gr. 0.90.
7.5 Ammonium sulfate (200 mg/L) - dissolve 200 grams (NH4)2S04 in 300 mL DI water. Bring to a
volume of 1000 mL.
7.6 Ammonium sulfide, 2%: Dilute 10 mL (NH4)2S, (20-24%), to 90 mL water; total volume 100 mL .
7.7 Barium carrier (standardized) - 33.9 mg/mL, NIST traceable
7.7.1 If the barium carrier is not already standardized, standardize the barium carrier solution
using the following procedure.
7.7.1.1 Pipette 1.0 mL barium carrier solution (16 mg/mL, Ba) into six separate labeled
centrifuge tubes containing 15 mL DI H20.
7.7.1.2 To each tube, add 1 mL 18 N sulfuric acid while stirring and digest precipitate in a
hot water bath for approximately 10 min.
7.7.1.3 Cool, centrifuge and decant the supernate into appropriate waste container.
7.7.1.4 Wash the precipitate with 15 mL DI water, centrifuge and decant the supernate.
7.7.1.5 Transfer the precipitate to a pre-weighed stainless steel planchet with a minimal
amount of DI water.
7.7.1.6 Dry on a heat source. Store in desiccator until cool and weigh as barium sulfate.
7.7.1.7 Record the net weights of the precipitates and calculations in the Rad Standards
Preparation Log.
7.8 Citric acid (1M) - dissolve 19.2g of C6H807H20 in water and dilute to 100 mL.
7.9 EDTA reagent basic (0.25M) - dissolve 20g NaOH in 750 mL water, heat and slowly add 93g
[ethylenedinitrilo] tetraacetic disodium salt, (CioHi408N2Na2-2H20) while stirring. Dilute to 1 liter.
7.10 Lead carrier (15 mg/mL) - dissolve 2.397g Pb(N03)2 in water, add 0.5 mL 16N HN03 and dilute to
100 mL with water.
7.11 Methyl orange indicator (0.1%) - dissolve 0.1 g methyl orange indicator in 100 mL water.
7.12 Nitric acid (16 N, 70.4%), concentrated HN03, sp. gr.
7.13 Sulfuric acid (18 N) - Cautiously mix 1 volume 36N H2S04 (concentrated) with 1 volume of water.
7.14 Radium-226, standard 20-25dpm, NIST traceable
8.0 SAMPLE COLLECTION, PRESERVATION AND STORAGE
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8.1
TestAmerica St. Louis supplies sample containers and chemical preservatives in accordance with
the method. TestAmerica St. Louis does not perform sample collection. Samplers should
reference the methods referenced and other applicable sample collection documents for detailed
collection procedures. Sample volumes and preservative information is given in ST-PM-0002.
8.2
Samples may be collected in glass or plastic containers.
8.3
Aqueous samples are preserved with nitric acid to a pH of less than 2.
8.3.1 The pH of aqueous samples is checked upon receipt by the Sample Control Department.
The pH does not require re-checking prior to analysis.
8.3.2 Aqueous samples acidified upon receipt (designated by a label on the bottle) do require a
check of the pH prior to analysis.
QUALITY CONTROL
9.1 Batch
9.1.1 A sample batch is a maximum of 20 environmental samples, which are prepared together
using the same process and same lot(s) of reagents. Where no preparation method exists
(e.g. water sample volatile organics, water sample anion analysis) the batch comprises of
a maximum of 20 environmental samples which are analyzed together with the same
process, lots of reagents and personnel.
9.1.2 Instrument conditions must be the same for all standards, samples and QC samples.
9.1.3 For this analysis, batch QC consists of a method blank, a Laboratory Control Sample
(LCS), and Sample Duplicate. In the event that there is insufficient sample to analyze a
sample duplicate, an LCS Duplicate (LCSD) is prepared and analyzed. .
9.1.4 Matrix Spike (MS) and Matrix Spike Duplicate (MSD) may be performed upon client
request, and are noted in the Client Requirement Sheets and Log-in.
9.1.5 Samples having different QC codes, due to non-standard client specific QC requirements,
must be batched separately in the LIMS. A method blank and LCS may be shared across
QC codes provided the actual "sample batch" does not exceed 20 environmental samples.
Duplicates (and MS/MSD if applicable) must be performed for each separate QC code.
9.2 Method Blank
9.2.1 A method blank is a blank matrix processed simultaneously with, and under the same
conditions as, samples through all steps of the procedure.
9.2.2 A method blank must be prepared with every sample batch.
9.2.3 For Liquid analyses, the method blank is comprised of DI water.
9.2.4 For Soil analyses, the method blank is comprised of DI water acidified with 2ml of nitric
9.3 Laboratory Control Sample
9.3.1 An LCS is a blank matrix spiked with a known amount of analyte(s), processed
simultaneously with, and under the same conditions as, samples through all steps of the
analytical procedure.
9.3.2 An LCS must be prepared with every sample batch.
9.3.3 For Liquid analyses, the LCS is comprised of DI water fortified with radium-226.
9.3.4 For Soil analyses, the LCS is comprised of radium-226.
9.4 Matrix Spike (MS) /Matrix Spike Duplicate (MSD)
9.4.1 A Matrix Spike is an aliquot of a field sample to which a known amount of target
analyte(s) is added, and is processed simultaneously with, and under the same conditions
as, samples through all steps of the analytical procedure.
9.4.2 MS/MSD samples do not count towards the 20 environmental samples in a sample batch.
acid.
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9.4.3 MS/MSD samples, when requested, must be performed with every sample batch and
every LIMS batch.
9.5 Sample Duplicate
9.5.1 A Sample Duplicate is an additional aliquot of a field sample taken through the entire
analytical process to demonstrate precision.
9.5.2 If there is insufficient sample to perform a Sample Duplicate, a duplicate LCS is
analyzed. A NCM is written to document the insufficient volume and utilizing of an
LCSD for demonstration of precision.
9.6 Procedural Variations/ Nonconformance and Corrective Action
9.6.1 Any variation shall be completely documented using a Nonconformance Memo and
approved by the Supervisor and QA Manager. See SOP ST-QA-0036 for details
regarding the NCM process.
9.6.2 Any deviations from QC procedures must be documented as a nonconformance, with
applicable cause and corrective action approved by the Supervisor and QA Manager.
See SOP ST-QA-0036 for details regarding the NCM process.
10.0 CALIBRATION AND STANDARDIZATION
10.1 Balance and thermometer calibration must be checked daily when used. Refer to SOP ST-QA-
0005, "Calibration and Verification Procedure for Thermometers, Balances, Weights and Pipettes
Procedure.
10.2 See the analytical SOP for instrument calibration; ST-RD-0403, "Daily Calibration Verification
and Maintenance of the Low Background Gas Flow Proportional Counting System."
11.0 PROCEDURE
11.1 Water Samples
11.1.1 Ensure that the sample container is capped tightly and shake it thoroughly. Transfer a
sample aliquot to a beaker.
11.1.2 Sample aliquot size is 1 liter.
11.1.2.1 For client requesting a reporting limit less than lpCi/L, a larger sample volume
may be required. Contact Radiochemistry manager/supervisor for instruction.
11.1.2.2 If less than 1 liter of sample was provided by the client, write the NCM noting
insufficient volume.
11.2 Soil Samples
11.2.1 For soil samples prepare per SOP STL-RC-003, "Drying and Grinding of Soil and Solid
Samples", and weigh 1 to 2 grams into a labeled crucible.
11.2.2 Place in oven at 600° and muffle for four hours. Allow to cool.
11.2.3 Transfer to digestion tube using 4M HN03.
11.2.4 Add 1 mL of standardized barium carrier to samples and QC. Add radium-226 spike to
LCS and MS/MSD, if applicable.
11.2.5 Carefully add 5 mL concentrated nitric acid, 5 mL concentrated hydrochloric acid and 10
mL concentrated hydrofluoric acid.
11.2.6 Digest in mod block at >110° for four hours or until dry.
11.2.7 Carefully add 10 mL concentrated nitric acid, 10 mL concentrated hydrochloric acid and 5
mL concentrated hydrofluoric acid.
11.2.8 Digest in mod block at >110° for four hours or until dry.
11.2.9 Dissolve with 10 mL HN03 and 10 mL HC1, return to mod block for 30min.
11.2.10 Transfer to 250 mL beakers with 4M HN03. Dilute to a final volume of 200 mL with DI
water.
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11.3 Precipitation
11.3.1 Add methyl orange indicator until red color persists. Add 1M citric acid in ratio of 5 mL
per liter; mix thoroughly.
11.3.2 For Waters, perform steps 11.3.2.1 through 11.3.2.3; for soil perform steps 11.3.2.1.
11.3.2.1 2.5 mL of lead carrier.
11.3.2.2 Add 1.0 mL Standardized barium carrier. (33.9 mg/mL)
11.3.2.3 Spike LCS and MS/MSD (if applicable) with radium-226. Document the spike
volume and concentration on the prep sheet.
11.3.3 Heat and stir until just beginning to boil.
11.3.4 Add ammonium hydroxide dropwise until the solution changes from pink to yellow or
the pH is > 6.5.
11.3.5 A face shield is required for this step. Add 10 mL18N sulfuric acid until the red color
reappears or the pH is < 2, and then add 5 mL ammonium sulfate.
11.3.6 Stir and heat the samples for a minimum of 15 minutes.
11.3.7 Cover the beaker and allow the precipitate to settle for at least four to six hours. Note:
the lead and barium sulfate should be clearly separate from the solution.
11.4 In-growth
11.4.1 Decant the supernate and discard into the appropriate waste container, taking care to
avoid disturbing the precipitate.
11.4.2 Transfer the precipitate to a 50 mL centrifuge tube, taking care to rinse the last particles
out of the beaker with DI water.
11.4.3 Centrifuge until precipitate appears to be compacted at the bottom of the tube. (5-10
minutes). Pour off liquid and save the BaS04 precipitate.
11.4.4 Add 10 mL 16N HN03. Cap tube and vortex to ensure complete mixing. Centrifuge for
5-10 minutes at a maximum of 2000 rpm. Pour off the liquid and save the BaS04
precipitate. Repeat this step if the precipitate visually appears larger than that in the
Blank and LCS.
11.4.5 Wash the precipitate with 10 mL DI water. Vortex, centrifuge and discard supernate.
Save the BaS04 precipitate.
11.4.6 Add 20 mL basic EDTA reagent, vortex and heat in a hot water bath until precipitate
dissolves.
11.4.6.1 If insoluble solids remain in the tube after the addition of EDTA, confirm the
pH is > 10.
11.4.6.2 If pH is >10, centrifuge and syringe filter supernatant into a clean labeled 50 mL
centrifuge tube. Discard insoluble residue.
11.4.7 Add 2 mL (NH4)2S04 (200 mg/mL) and stir thoroughly.
11.4.8 Add 3 mL 17.4N Acetic acid or until barium sulfate precipitates.
11.4.9 Digest in a hot water bath until precipitate settles. Centrifuge and discard supernatant.
11.4.10 Repeat steps 11.4.6 to 11.4.10.
11.4.11 Record date and time of the last BaS04 precipitation on the sample data sheet.
11.4.12 Add 1 mL Lead carrier (1.5 mg/mL)
11.4.13 Dissolve the precipitate in 20 mL basic EDTA.
11.4.14 Vortex, heat in hot bath until the precipitate dissolves.
11.5 Lead Scavenge Clean-up
11.5.1 Add 0.3 mL ammonium sulfide and stir well.
11.5.2 Add 10N sodium hydroxide drop-wise (approximately 0.5 mL) with vigorous stirring
until lead sulfide precipitates, then add 10 drops more. Stir intermittently. Centrifuge
11.5.3 Add 1 mL lead carrier (1.5 ng/mL), 0.1 mL ammonium sulfide, and 0.1 mL 10N sodium
hydroxide. Centrifuge and filter supernatant through 0.45 mm syringe filter into a clean
labeled tube.
11.6 Barium Yield
11.6.1 Add 2 mL Ammonium sulfate and 3 mL Acetic acid or until barium sulfate forms.
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11.6.2 Vortex.
11.6.3 Heat in hot water bath.
11.6.4 Centrifuge and decant.
11.6.4.1 If barium sulfate does not form after 2 additions; consult the radiochemistry
manager/supervisor for further instruction.
11.6.5 To the precipitate, add 20 mL basic EDTA reagent, vortex and heat in a hot water bath
until precipitate dissolves. Add a few drops 10N NaOH if precipitate does not readily
dissolve.
11.6.6 Add 2 mL Ammonium sulfate and 3 mL Acetic acid until barium sulfate forms.
11.6.7 Heat in hot water bath.
11.6.8 Centrifuge and decant.
11.6.9 Record time as "T3".
11.6.10 Wash precipitate with 10 to 20 mL DI. Centrifuge and discard supernate. Repeat this
step.
11.7
11.8
Plating
11.7.1 Transfer precipitate to a pre-weighed stainless steel cleaned planchet with a minimal
amount of water.
11.7.1.1 The cleaned planchet has been processed in accordance with SOP: ST-RC-0002.
See SOP for additional information.
11.7.2 Heat the planchet again using the hot plate, let cool in a desiccator for a minimum of 15
minutes and then weigh the planchet.
11.7.3 Record the final weight of the planchet to determine the chemical recovery for the
barium carrier solution.
Submit planchet to the count room for analysis.
12.0 DATA ANALYSIS AND CALCULATIONS
12.1 Commonly used calculations (e.g. LCS % recovery and RPD) and standard instrument software
calculations are given in the TestAmerica St. Louis ST-QAM.
12.2 There are no calculations pertaining to this sample preparation procedure.
12.3 Total Alpha Radium (TAR) by GFPC calculations are given in SOP: ST-RD-0403.
13.0 DATA ASSESSMENT AND ACCEPTANCE CRITERIA; CORRECTIVE ACTIONS FOR
OUT OF CONTROL DATA
13.1 Data assessment does not pertain to this sample preparation procedure.
13.2 Samples requiring re-preparation are submitted to the preparation lab with a NCM detailing the
issue. The NCM process is described in SOP: ST-QA-0036. Specific information is given in the
applicable analysis SOP.
14.0 METHOD PERFORMANCE AND DEMONSTRATION OF CAPABILITY
14.1 Method performance data, Reporting Limits, and QC acceptance limits, are given in the associated
analytical SOP
14.2 Demonstration of Capability
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14.2.1 Initial and continuing demonstrations of capability requirements are established in the
ST-QAM.
14.3 Training Qualification
14.3.1 The manager/supervisor has the responsibility to ensure that this procedure is performed
by an analyst who has been properly trained in its use and has the required experience.
14.3.2 The analyst must have successfully completed the initial demonstration capability
requirements prior to working independently. See requirements in the ST-QAM.
14.4 Annually, the analyst must successfully demonstrate proficiency to continue to perform this
analysis. See requirements in the ST-QAM.
15.0 VALIDATION
15.1 Laboratory SOPs are based on published methods (EPA, DOE, ASTM, Eichrom, Standard
Methods) and do not require validation by the laboratory. The requirements for laboratory
demonstration of capability are included in the ST-ST-QAM. Laboratory validation data would be
appropriate for performance based measurement systems, non-standard methods and significant
modifications to published methods. Data from said validations is held in the QA department.
16.0 WASTE MANGEMENT AND POLLUTION PREVENTION
16.1 All waste will be disposed of in accordance with Federal, State and Local regulations. Where
reasonably feasible, technological changes have been implemented to minimize the potential for
pollution of the environment. Employees will abide by this method and the policies in section 13
of the Corporate Safety Manual for "Waste Management and Pollution Prevention."
16.2 Waste Streams Produced by the Method
The following waste streams are produced when this method is carried out.
• Acidic sample waste generated. All acidic waste will be accumulated in the appropriate
waste accumulation container, labeled as Drum Type "A" or "B".
• Contaminated disposable glass or plastic materials utilized in the analysis are disposed of in the
sanitary trash. If the labware was used for the analysis of radioactive samples and contains
radioactivity at a level of 100 cpm over background as determined by a GM meter, the labware
will be collected in waste barrels designated for solid rad waste for disposal by the EH&S
Coordinator.
17.0 REFERENCES
17.1 Prescribed Procedures for Measurement of Radioactivity in Drinking Water, Section 6, Method
903.0, Alpha-Emitting Radium Isotopes in Drinking Water
17.2 SW-846,"Test Methods for Evaluating Solid Waste, Physical/Chemical Methods", Method 9315,
Alpha Emitting Radium Isotopes
17.3 TestAmerica Quality Assurance Manual (ST-QAM), current revision
17.4 TestAmerica Corporate Environmental Health and Safety Manual (CW-E-M-001) and St. Louis
Facility Addendum (SOP ST-HS-0002), current revisions.
17.5 Associated SOPs, current revisions:
17.5.1 ST-PM-0002, Sample receipt and Chain of Custody
17.5.2 ST-QA-0002, Standard and Reagent Preparation
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17.5.3 ST-QA-0005, Calibration and Verification Procedure for Thermometers, Balances,
Weights and Pipettes
17.5.4 ST-QA-0036, Non-conformance Memorandum (NCM) Process
17.5.5 ST-RC-0002, Planchet Preparation for Radiochemistry and Radiological Screening
Analysis
17.5.6 ST-RC-5006, Decontamination of Laboratory Glassware, Labware and Equipment
17.5.7 ST-RD-0403, Gas Flow Proportional Counting (GFPC) Analysis
18.0 CLARIFICATIONS, MODIFICATIONS TO THE REFERENCE METHOD
18.1 The initial precipitation of total alpha radium uses the technique cited in EPA Method 904.0
instead of 903.0 which uses straight sulfuric acid and fewer carriers to bring down the Pb/Ba
sulfate.
18.2 A lead (Pb) scavenge identical to the one found in EPA Method 904.0 has been incorporated into
this procedure. Skipping this step could artificially inflate barium yields and thus bias the result.
19.0 CHANGES TO PREVIOUS REVISION
19.1
Updated section 11.4 and 11.5 regarding amount of mL used of Acetic Acid
19.1.
Rev 10,
19.1.1.
Updated sample collection, preservation and storage times in section 8.0.
19.2.
Rev 11:
19.2.1.
Annual Review, No Changes
19.3.
Rev 12
19.3.1.
Grammatical errors fixed throughout SOP
19.3.2.
Section 11.4.6.2 added syringe filter supernate
19.3.3.
Section 11.4.8 added 3 mL
19.3.4.
Section 11.4.11 moved record date and time of last BaS04 precipitation on the sample
date sheet
19.3.5.
Section 11.5.2 Deleted "decant supernate into clean tube"
19.3.6.
Section 11.6.1 deleted "in increments"
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TestAmerica
THE LEADER IN ENVIRONMENTAL TESTING
TestAmerica St. Louis
SOP No. ST-RC-0242, Rev. 16
Effective Date: 06/20/2013
Page No.: 1 of 14
Title: ISOTOPIC THORIUM, PLUTONIUM AND URANIUM IN VARIOUS
MATRICES BY EICHROM® SEPARATION RESINS
Approvals (Signature/Date):
Sarah Berrisen
Iparations Supervisor
'AAdfA -mU
Date Michael Ridenhcwer Date
Michael
Health & Safety Manager / Coordinator
C ¦ w 13
Marti Ward
Quality Assurance Manager
Date
iw
Elaine Wild
Laboratory Director
v 'bate
This SOP was previously identified as SOP No. ST-RC-0242 Rev. 15
Copyright Information:
This documentation has been prepared by TestAmerica Laboratories Inc. and its affiliates ("TestAmerica"), solely
for their own use and the use of their customers in evaluating their qualifications and capabilities in connection with
a particular project. The user of this document agrees by its acceptance to return it to TestAmerica upon request and
not to reproduce, copy, lend, or otherwise disclose its contents, directly or indirectly, and not to use if for any other
purpose other than that for which it was specifically provided. The user also agrees that where consultants or other
outside parties are involved in the evaluation process, access to these documents shall not be given to said parties
unless those parties also specifically agree to these conditions.
THIS DOCUMENT CONTAINS VALUABLE CONFIDENTIAL AND PROPRIETARY INFORMATION.
DISCLOSURE, USE OR REPRODUCTION OF THESE MATERIALS WITHOUT THE WRITTEN
AUTHORIZATION OF TESTAMERICA IS STRICTLY PROHIBITED. THIS UNPUBLISHED WORK
BY TESTAMERICA IS PROTECTED BY STATE AND FEDERAL LAW OF THE UNITED STATES. IF
PUBLICATION OF THIS WORK SHOULD OCCUR THE FOLLOWING NOTICE SHALL APPLY:
©COPYRIGHT 2013 TESTAMERICA LABORATORIES INC.
Facility Distribution No.:
Distributed To: See Electronic Distribution Sheet
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SOP No. ST-RC-0242, Rev. 16
Effective Date: 06/20/2013
Page No.: 2 of 14
1.0 SCOPE AND APPLICATION
1.1 This SOP provides a rapid, reliable method for separation of Thorium, Plutonium and Uranium in
various matrices.
1.1.1 If only Uranium analysis is requested, see SOP: ST-RC-0238.
1.1.2 If other actinides in addition to Thorium, Plutonium and Uranium are requested, please
see SOP index to determine applicable SOP.
1.2 This SOP is based on Eichrom Technologies, Inc. Analytical Procedures "ACW13 VBS Thorium,
Plutonium and Uranium in Water (with Vacuum Box System)" and "ACW01 Uranium and
Thorium in Water".
1.3 This procedure is applicable to water, soil, filter, biota, and oil.
1.3.1 Soil, filter, biota and oils are pre-prepared in accordance with SOP, ST-RC-0004.
1.3.2 Water preparation is contained within this SOP.
1.4 The requested limits, minimum detection amounts and QC limits are maintained in the Laboratory
Information Management System (LIMS).
2.0 SUMMARY OF METHOD
2.1 This SOP describes the method for separation of Thorium, Plutonium and Uranium using Eichrom
resin prior to measurement by alpha spectrometry. A calcium phosphate precipitation technique is
used to concentrate and remove actinides from water samples. Soils, Sludge and Filters are
prepared for analysis using STL-RC-0004. Tracers are used to correct for chemical recovery and
correct results to improve precision and accuracy.
3.0 DEFINITIONS
3.1 See the TestAmerica Quality Assurance Manual (ST-QAM) for a glossary of common terms and
data qualififers.
3.2 Tracer - A known amount of 232Uranium, 229Thorium, 242Plutonium, (or 236Plutonium), added to
each sample to determine chemical yield. The tracer serves as an internal standard, which is used to
calculate the activity of the target isotopes.
4.0 INTERFERENCES
4.1 Actinides with unresolvable alpha energies, such as Americium-241 and Plutonium-238, must be
chemically separated to enable measurement of the target actinide(s). This method separates these
isotopes effectively.
4.2 Samples that are high in carbonates and phosphates, as indicated by a violent and vigorous
reaction during the initial phases of digestion, need to be loaded in a minimum of 40 mL of load
solution. The increased amount of load increases the amount of aluminum nitrate that the samples
are exposed to. The extra aluminum nitrate helps to bind phosphates which interfere with thorium
uptake.
4.3 Neptunium-237 can interfere with the Plutonium-242. This interference can be avoided by
increasing the normality of the hydrochloric acid rinse and increasing the concentration of the
titanium trichloride eluant.
5.0 SAFETY
5.1 Employees must abide by the policies and procedures in the Corporate Environmental Health and
Safety Manual (CW-E-M-001), Radiation Safety Manual and this document. This procedure may
involve hazardous material, operations and equipment. This SOP does not purport to address all of
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the safety problems associated with its use. It is the responsibility of the user of the method to
follow appropriate safety, waste disposal and health practices under the assumption that all
samples and reagents are potentially hazardous. Safety glasses, gloves, lab coats and closed-toe,
nonabsorbent shoes are a minimum.
5.1 SPECIFIC SAFETY CONCERNS OR REQUIREMENTS
5.1.1 None.
5.2 PRIMARY MATERIALS USED
5.2.1 The following is a list of the materials used in this method, which have a serious or
significant hazard rating. NOTE: This list does not include all materials used in the
method. The table contains a summary of the primary hazards listed in the MSDS
for each of the materials listed in the table. A complete list of materials used in the
method can be found in the reagents and materials section. Employees must review the
information in the MSDS for each material before using it for the first time or when there
are major changes to the MSDS.
Material'1'
Hazards
Exposure
Limit'2'
Signs and symptoms of exposure
Ammonium
Hydroxide
Poison
Corrosive
50 ppm
(TWA)
Inhalation symptoms include irritation to the respiratory tract.
Ingestion symptoms include pain in the mouth, chest, and
abdomen, with coughing, vomiting and collapse. Skin
contact causes irritation and burns. Eye contact with vapors
causes irritation.
Calcium
nitrate
Oxidizer
None
established
Inhalation symptoms include coughing and shortness of
breath. Skin contact symptoms include redness, itching, and
pain. Eye contact causes irritation, redness and pain.
Hydrochloric
Acid
Poison
Corrosive
5 ppm
(Ceiling)
Inhalation symptoms include coughing, choking,
inflammation of the nose, throat, and upper respiratory tract.
Skin contact can cause redness, pain, severe skin burns, and
discoloration. Vapors are irritating to the eyes. Contact may
cause severe burns.
Hydrofluoric
Acid
Poison
Corrosive
3 ppm
(TWA)
Inhalation symptoms may include sore throat, coughing,
labored breathing and lung congestion/inflammation. Skin
contact may cause serious burns which are not immediately
apparent or painful. Symptoms of eye contact include
redness, pain, and blurred vision.
Lead nitrate
Poison
Oxidizer
0.05 mg/m3
(TWA)
Inhalation of lead can produce local irritation of bronchia and
lungs with acute exposure causing a metallic taste in the
mouth and chest and abdominal pain. Ingestion symptoms
can include abdominal pain and spasms, nausea, vomiting,
and headache. Absorption through skin can occur causing
symptoms similar to ingestion. Skin contact may cause local
irritation, redness and pain. Absorption can also occur
through eye tissue.
Nitric Acid
Corrosive
Poison
Oxidizer
2 ppm
(TWA)
4 ppm
(STEL)
Inhalation may cause coughing, choking, and irritation of the
nose, throat, and respiratory tract. Skin contact can cause
redness, pain, and severe skin burns. Concentrated solutions
can stain the skin a yellow-brown color. Vapors are irritating
to the eyes and contact may cause severe burns.
Sulfuric Acid
Corrosive
Poison
Cancer
Hazard
1 mg/m3
(TWA)
Inhalation may cause irritation of the nose and throat, and
labored breathing. Skin contact symptoms include redness,
pain, and severe burning. Eye contact can cause blurred
vision, redness, pain, and severe tissue burns.
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Page No.: 4 of 14
1 - Always add acid to water to prevent violent reactions.
2 - Exposure limit refers to the OSHA regulatory exposure limit.
TWA - Time Weighted Average
STEL - Short term exposure limit
Ceiling - At no time should this exposure limit be exceeded.
6.0 EQUIPMENT AND SUPPLIES
6.1 Beakers, 150-2000 mL
6.2 Analytical balance - 0.0001 g sensitivity
6.3 Centrifuge
6.4 Centrifuge tubes, poly, 50 mL with cap
6.5 Pipettes, glass or plastic, disposable
6.6 Pipettes, mechanical
6.7 Fume hood
6.8 Hotplate
6.9 Vortex mixer
6.10 pH strips, narrow range
6.11 Vacuum Box, Eichrom part number AC-24-BOX, or equivalent
6.12 Syringe filter, 25 mm acrodisc, 0.45 or 0.70 |am
6.13 Cartridge reservoirs/syringe/funnel-20 mL B-D Luer Lok syringe Part Number 301625 (Fisher
part number 14-823-2B), or equivalent.
7.0 REAGENTS AND STANDARDS
7.1 All standards and reagent preparation, documentation and labeling must follow the requirements
of SOP ST-QA-0002, current revision.
7.2 DI Water, obtained from the Milli-Q unit.
7.3 Aluminum Nitrate, solid.
7.4 Ammonium hydrogen phosphate (3,2M)
7.4.1 Dissolve 104 g of (NH4)2HP04 in 200 mL of water, heat gently to dissolve, and dilute to
250 mL with water.
7.5 Ammonium hydroxide (NH40H), Reagent.
7.6 Ammonium Thiocyanate, crystals
7.6.1 Dissolve 7.6g of ammonium thiocyanate crystals in 90mL of DI water. Dilute to lOOmL.
7.7 L (+) Ascorbic Acid, reagent powder.
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7.7.1 L (+) Ascorbic Acid solution, 2.5 g dissolved in 10 mL of DI water.
7.8 Bromocresol Purple indicator solution
7.8.1 Dissolve 0.20 g of Bromocresol Purple (520.24 F.W.) in 250 mL of water, add one mL
of concentrated Ammonium Hydroxide.
7.9 Calcium nitrate (1.25M)
7.9.1 Dissolve 51 g of Ca(N03)2 in 100 mL of water and dilute to 250 mL with water.
7.10 Hydrochloric acid (12M) - concentrated HC1 (sp gr 1.19).
7.10.1 Hydrochloric acid (9M) - Add 1500 mL of concentrated HC1 (sp gr 1.19) to 200 mL of
water and dilute to 2 liters.
7.10.2 Hydrochloric acid (6M) - Add 1000 mL of concentrated HC1 (sp gr 1.19) to 200 mL of
water and dilute to 2 liters
7.10.3 Hydrochloric acid (1M) - Add 167 mL of concentrated HQ (sp gr 1.19) to 200 mL of
water and dilute to 2 liters
7.11 Hydrochloric acid (5M) - 0.05M oxalic acid solution
7.11.1 Add 12.6 grams of oxalic acid dihydrate in approximately 800 mL of water. Add 834
mL of concentrated hydrochloric acid. Dilute to 2 liters, add a stir bar, and place on stir
plate until oxalic is completely dissolved
7.12 Lead Nitrate (Reagent, crystals).
7.12.1 Lead Nitrate 1 % wt/vol. solution. Dissolve 1 g of lead nitrate crystals in 100 mL of DI
water.
7.13 Nitric acid (16M) - concentrated HNO3 (sp gr 1.42).
7.13.1 Nitric acid (3M) - Add 375mL of concentrated nitric acid to 1500mL of DI water and
dilute to 2L.
7.14 Load solution [Nitric acid (3 M) - aluminum nitrate (1 M)]
7.14.1 Weigh 1500 g A1(N03)3 • 9H20 in a 4 liter beaker. Add 800 mL of water(first) and 764
mL of concentrated nitric acid. Dilute to 4 L with water. Add stir bar, cover with watch
glass and place on stir plate until aluminum nitrate is dissolved.
7.15 Potassium Hydroxide, KOH
7.16 Potassium Sulfate (Reagent Crystals).
7.17 Oxalic Acid, reagent, crystals.
7.18 Sodium Nitrite, NaN02 reagent crystals.
7.18.1 Sodium Nitrite Solution - dissolve 1.0 grams of sodium nitrite crystals in 10 mL of DI
water.
7.19 Titanium trichloride, TiCl3, 10% solution, commercially available.
7.20 TEVA Resin - prepacked column, 100-150 micron resin, or 50-100 micron prepacked cartridges.
7.21 UTEVA Resin-prepacked column, 100-150 micron resin, or 50-100 micron prepacked cartridges.
7.22 Plutonium-242 tracer standard, 10-20 dpm/mL (Plutonium-236 can also be used).
7.23 Plutonium-238 and/or Plutonium-239.
7.24 Thorium-229, 10-20 dpm/mL.
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7.25 Natural Thorium spike standard (Thorium-232/Thorium-228), approximately 10-20 dpm/mL.
7.26 Thorium-230 spike standard, approximately 10-20 dpm/mL.
7.27 TRM solid reference material.
7.28 Uranium-232 tracer, approximatly 10-20dpm/mL.
7.28.1 Clean uranium free of Th-228 daughter, removed by lead sulfate precipitation, activity
verified prior to use. A Th-228 free Uranium-232 standard may be made as descirbed
below.
7.28.2 Dilute the appropriate aliquot of stock to about 40mL with DI water.
7.28.3 Add 3 grams of potassium sulfate.
7.28.4 Adjust the pH to 1.5 using narrow range pH strips with either 2M H2S04 or 2M KOH.
7.28.5 While mixing, slowly add 25 mL of 1% Pb(N03)2.
7.28.6 Adjust the pH to 1.5 using narrow range pH strips with either 2M H2S04 or 2M KOH.
7.28.7 Dilute to 100 mL with water, and mix well. Solution should be spun (at a rate fast
enough to form a vortex) continuously for at least 30 minutes to remove any Thorium
that maybe in solution.
7.28.8 Let stand for at least 1 hour. Centrifuge the solution for 30 minutes. Use the clean U-
232 solution as soon as possible after removing the Th-228.
7.28.9 Before each use, shake the standard at least 30 minutes (to absorb any ingrown Th-228
onto the sulfate precipitate), and let the precipitate settle (centrifuge). Do not disturb the
precipitate while using the standard.
8.0 SAMPLE COLLECTION, PRESERVATIVES AND STORAGE
8.1 TestAmerica St. Louis supplies sample containers and chemical preservatives in accordance with
the method. TestAmerica St. Louis does not perform sample collection. Samplers should
reference the methods referenced and other applicable sample collection documents for detailed
collection procedures. Sample volumes and preservative information is given in ST-PM-0002.
8.2 Samples may be collected in glass or plastic containers.
8.3 Aqueous samples are preserved with nitric acid to a pH of less than 2.
8.3.1 The pH of aqueous samples are checked upon receipt by sample control, therefore, the pH
does not require checking prior to analysis.
8.3.1.1 Aqueous samples acidified upon receipt (designated by label on the bottle) do
require checking the pH prior to analysis.
8.4 Solid sample requirements are found in SOP ST-RC-0004, "Preparation of Soil, Sludge, Filter,
Biota and Oil/Grease Samples for Actinide Analysis".
9.0 QUALITY CONTROL
9.1 Batch
9.1.1 A sample batch is a maximum of 20 environmental samples, which are prepared together
using the same process and same lot(s) of reagents. Where no preparation method exists
(e.g. water sample volatile organics, water sample anion analysis ) the batch comprises of
a maximum of 20 environmental samples which are analyzed together with the same
process, lots of reagents and personnel.
9.1.2 Instrument conditions must be the same for all standards, samples and QC samples.
9.1.3 For this analysis, batch QC consists of a method blank (MB), a Laboratory Control
Sample (LCS), and Sample Duplicate. In the event that there is insufficient sample to
analyze a sample duplicate, an LCS Duplicate (LCSD) is prepared and analyzed.
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9.1.3.1 Matrix Spike (MS) and Matrix Spike Duplicate (MSD) may be performed upon
client request, and are noted in the Client Requirement Sheets and Log-in.
9.1.4 Samples having different QC codes, due to non-standard client specific QC requirements,
must be batched separately in the LIMS. A method blank and LCS may be shared across
QC codes provided the actual "sample batch" does not exceed 20 environmental samples.
Duplicates (and MS/MSD if applicable) must be performed for each separate QC code.
9.2 Method Blank (MB)
9.2.1 A method blank is a blank matrix processed simultaneously with, and under the same
conditions as, samples through all steps of the procedure.
9.2.2 A method blank must be prepared with every sample batch.
9.2.3 For Water analyses, the method blank is comprised of DI water with Nitric Acid.
9.2.4 For non-aqueous analyses,the method blank is comprised of 1.25M Calcium Nitrate. See
the soil preparation SOP ST-RC-0004.
9.3 Laboratory Control Sample (LCS)
9.3.1 An LCS is a blank matrix spiked with a known amount of analyte(s), processed
simultaneously with, and under the same conditions as, samples through all steps of the
analytical procedure.
9.3.2 An LCS must be prepared with every sample batch.
9.3.3 For Water analyses, the LCS is comprised of DI water with Nitric acid fortified with the
isotopes of interest.
9.3.4 For non-aqueous analyses, the LCS is comprised of a TRM sold reference material or
1.25M Calcium Nitrate fortified with the isotopes of interest. See the soil prep SOP ST-
RC-0004.
9.3.4.1 For Am, Cm, Pu, Uranium only, use Calcium nitrate
9.3.4.2 For Thorium use the TRM standard.
9.4 Matrix Spike(MS)/Matrix Spike Duplicate(MSD)
9.4.1 A Matrix Spike is an aliquot of a field sample to which a known amount of target
analyte(s) is added, and is processed simultaneously with, and under the same conditions
as, samples through all steps of the analytical procedure.
9.4.2 MS/MSD samples do not count towards the 20 environmental samples in a sample batch.
9.4.3 MS/MSD samples, when requested, must be performed with every sample batch and
every LIMS batch.
9.5 Sample Duplicate (SD)
9.5.1 A Sample Duplicate is an additional aliquot of a field sample taken through the entire
analytical process to demonstrate precision.
9.5.2 If there is insufficient sample to perform a Sample Duplicate, a duplicate LCS is
analyzed. A NCM is written to document the insufficient volume and utilizing of a
LCSD for demonstration of precision.
9.6 Procedural Variations/ Nonconformance and Corrective Action
9.6.1 Any variation shall be completely documented using a Nonconformance Memo and
approved by the Supervisor and QA Manager. See SOP ST-QA-0036 for details
regarding the NCM process.
9.6.2 Any deviations from QC procedures must be documented as a nonconformance, with
applicable cause and corrective action approved by the Supervisor and QA Manager.
See SOP ST-QA-0036 for details regarding the NCM process.
10.0 CALIBRATION AND STANDARDIZATION
10.1 Balance and pipette calibrations must be checked daily when used. Refer to SOP ST-QA-0005,
"Calibration and Verification Procedure for Thermometers, Balances, Weights and Pipettes."
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11.0 PROCEDURE
11.1 For NON-AQUEOUS matrices (soil, oil, biota, etc) see SOP: ST-RC-0004 for initial sample
preparation and proceed to section 11.5 of this SOP.
11.2 Water Sample Preparation:
11.2.1 If not already pre-filtered, and the client has requested analysis on a filtered fraction,
filter the sample through a 0.45 micron filter. If the sample contains a large amount of
sediment which would not be possible to work with, contact the manager/supervisior.
11.2.2 Prepare method blank and LCS using 500ml or 1000ml DI water (match to volume of
associated samples).
11.2.2.1 Acidify with nitric acid to a pH < 2.
11.2.3 Shake the sample to suspend any residue and to ensure that the sample is homogeneous.
11.2.4 Weigh approximately 500 to lOOmL (depending on the dection limit) of sample into an
appropriate size beaker. Record weight.
11.2.4.1 Aqueous sample aliquot volumes are determined by mass and use an assumed
density of lg/mL.
11.2.4.2 If upon visual inspection a sample is suspected to have a high density
(>1.2g/mL, e.g. brine or waste) or a low density (<0.98g/mL, e.g. mixed
solvent) the sample density will be measured and the volume determined
arithemetically (sample mass divided by density equals volume).
11.2.5 Add appropriate tracers or standards. Generally 10 - 20 dpm of each of the Thorium,
Uranium and Plutonium tracers are added
11.2.5.1 Spike LCS and MS (if applicable) with isotopes of interest.
11.3 Evaporation (Alternative option to Calcium Phosphate precipitation):
11.3.1 This option may be used when large sample volumes are needed to achieve low level
reporting limits.
11.3.1.1 Consult Manager/Supervisor to determine when this option should be used.
11.3.2 Evaporate sample on a hot plate to less than 50 mL and transfer to a 100 mL beaker.
11.3.2.1 Note: For some water samples, calcium sulfate formation may occur during
evaporation. If this occurs, use the calcium phosphate precipitation option in
step 11.4
11.3.3 Gently evaporate the sample to dryness and redissolve in approximately 5 mL of
concentrated HN03 (sp gr 1.42). Repeat step two more times, evaporate to dryness and
proceed to step 11.5.
11.4 Calcium phosphate precipitation:
11.4.1 Add 0.5 mL of 1.25M Ca(N03)2 to each beaker.
11.4.2 Add 0.200 mL of 3.2 M (NH4)2HP04 solution to each beaker
11.4.3 Add 3-5 drops Bromocresol Purple indicator to each beaker.
11.4.4 Stir using the bulb of a transfer pipette and place beaker on a hot plate.
11.4.5 Allow the samples to heat to near boiling approximately 30 minutes.
11.4.6 Once the samples reach near boiling, turn the heat down to medium.
11.4.7 While stirring, add enough concentrated NH4OH with a squirt bottle to reach the
bromocresol purple indicator end point and form Ca3(P04)2 precipitate.
11.4.8 Allow the sample to heat for another 20-30 minutes.
11.4.9 Remove from the hot plate, allow sample to cool and precipitate to settle.
11.4.10 Decant.
11.4.11 Transfer the precipitate to a centrifuge tube and centrifuge the precipitate for
approximately 5 minutes at 2000 rpm.
11.4.12 Decant supernatant and discard to waste.
11.4.13 Proceed to section 11.5
11.5 Thorium/Plutonium/Uranium Separation using Eichrom resins.
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11.5.1 Dissolve calcium phosphate precipitate, soil dissolution residue or evaporated water
sample with 15 mL of Load solution. Vortex the sample.
11.5.1.1 For waters:
11.5.1.1.1 A additional 5 mL load solution aliqouts may be necessary to
dissolve the sample residue. Do not use more than 30 mL of load
solution.
NOTE: Samples that are high in carbonates and phosphates, as
indicated by a violent and /or vigorous reaction during the initial
phases of digestion, need to be loaded in a minimum of 40 mL of
load solution.
11.5.1.1.2 If particles are observed or the solution is cloudy, centrifuge the
sample at approximately 2000 rpm for 5 minutes.
NOTE: The use of filtration is also permitted, e.g. syringe filter
if the solution is still cloudy.
11.5.2 For each sample dissolved in load solution, place a UTEVA resin cartridge in the
vacuum box. Lock a TEVA Resin cartridge onto the top of the UTEVA cartridge. Attach
a plastic syringe funnel to the top of the TEVA cartidge.
11.5.2.1 If samples do not require Uranium analysis, the UTEVA cartridge is
omitted.
11.5.3 Place a waste collection reservoir inside the vacuum box to catch the column effluent.
11.5.4 Just prior to loading the sample condition the resin:
11.5.4.1 Turn on the vacuum pump.
11.5.4.2 Add 5 mL of 3M HN03 into each funnel.
11.5.4.3 Allow the solution to be pulled through the columns by adjusting the flow rate
on top of the vacuum box.
11.5.4.4 The flow rate should be approximately 3 mL per minute. Discard effluent to
waste.
NOTE: Approximately 20 drops equals 1 mL. Use the valve to adjust the
flow for each individual sample. Adjust the flow for each solution added.
11.5.5 For samples requiring Plutonium analysis (If samples do not require Plutonium, proceed
to step 11.5.8):
11.5.5.1 Add 1 drop of Ammonium Thiocyanate and 1 mL ascorbic acid solution to the
sample load solution in the centrifuge tube and heat in hot water bath for
approximately 5 minutes.
11.5.5.1.1 After heating, if samples are still red in color (indication of iron
present in sample), add ascorbic acid drop wise unitl red color
disappears. Heat in hot bath for 3 minutes.
11.5.5.2 Add lmL of NaN02 solution to the sample load solution in the centrifuge tube
and heat in hot water bath for approximately 5 minutes.
11.5.5.3 Remove samples from hot water bath and let cool in cold water bath until
samples are at or slightly below room temperature.
11.5.6 Transfer each sample load solution into the appropriate TEVA/UTEVA Resin cartridge
funnel. Allow to drain. Adjust the flow rate to approximately 1 mL per minute.
NOTE: the TEVA and the UTEVA cartridge can turn blueish green as the load
solution drains through it.
11.5.7 Rinse the funnel with 20 mL of 3M HN03 and allow to drain. Adjust flow to
approximately 3 mL per minute.
11.5.8 Separate TEVA cartridge from UTEVA cartridge. Place new syringe on the UTEVA
cartridge.
NOTE: If Uranium analysis is not requested, the UTEVA cartridge is omitted.
11.5.9 Thorium Elution
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11.5.9.1 Place a new clean labeled centrifuge tube in the rack beneath the TEVA
cartridge.
11.5.9.2 Add 20 mL of 9M HC1 into each cartridge and collect eluant. Adjust flow to
approximately 1 mL per minute.
11.5.9.3 Add 5 mL of 6M HC1 into each funnel and collect in the same centrifuge tube
as in the previous step. This 6M HC1 rinse will strip any residual traces of
Thorium from the cartridge. Adjust flow to approximately 1 mL per minute.
11.5.9.4 For Thorium analysis:
11.5.9.4.1 Transfer the Thorium HC1 solution to a clean labeled beaker (save
centrifuge tubes) and evaporate to near dryness.
11.5.9.4.2 Add 5-10mL of DI water in beaker and let sit for 15 minutes.
11.5.9.4.3 Transfer sample back to original centrifuge tube.
11.5.9.4.4 To co-precipitate the Thorium, proceed to ST-RC-0100, "Actinide
Coprecipitation."
11.5.10 Plutonium Elution (Thorium Elution step must be completed before this step- even if
Thorium is not requested)
11.5.10.1 Place a clean, labeled 50 mL centrifuge tube below each TEVA cartridge.
11.5.10.2 For samples not suspected of containing Neptunium:
11.5.10.2.1 Plutonium Elution:
11.5.10.2.1.1 Mix the HC1 and TiCl3 after closing the flow
control valve by adding 10 mL of the 1M HC1 to
the column and pipetting 0.25 mL of the TiCl3 into
the column.
11.5.10.2.1.2 Add 10 mL of 1M HC1.
11.5.10.2.1.3 Adjust the flow control valve so that the flow is
approximately 1 mL per minute.
11.5.10.2.2 Collect the plutonium eluant, and proceed to ST-RC-0100,
"Actinide Coprecipitation."
11.5.10.3 For samples suspected of containing Neptunium:
11.5.10.3.1 Plutonium Elution:
11.5.10.3.1.1 Mix the HC1 and TiCl3 after closing the flow
control valve by adding 10 mL of 9M HC1 to the
column and pipetting 0.4 mL of the TiCl3 into the
column.
11.5.10.3.1.2 Add 10 mL of 9M HC1.
11.5.10.3.1.3 Adjust the flow control valve so that the flow is
approximately 1 mL per minute.
11.5.10.3 .1.4 Collect the plutonium eluant.
11.5.10.3 .1.5 To co-precipitate the Plutonium proceed to ST-
RC-0100, "Actinide Coprecipitation."
11.5.11 Uranium Elution (if requested)
11.5.11.1 Place a waste 50 mL centrifuge tube below eachUTEVA cartridge.
11.5.11.2 Add 5 mL of 3M HN03 into each cartridge, adjust flow to approximately 3
mL per minute. Dispose to waste.
11.5.11.3 Add 5 mL of 9M HC1 into each UTEVA cartridge and allow to drain. Adjust
the flow rate to lmL per/minute.
11.5.11.4 Discard this rinse.
NOTE: This rinse converts the resin to the chloride system. Some
Neptunium may be removed here.
11.5.12 Add 20 mL of 5M HC1- 0.05M oxalic acid into each cartridge. Adjust flow rate to lmL
per/minute and allow to drain. Discard this rinse.
Note: This rinse removes neptunium and thorium from the cartridge. The 9M HC1
and the oxalic acid remove any residual ferrous ion.
11.5.13 Ensure that clean, labeled tubes are placed in the tube rack under the appropriate
cartridge.
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11.5.14 Add 15 mL of 1M HC1 into each cartridge to strip the Uranium. Adjust flow rate to
lmL per/minute and allow to drain.
11.5.15 To co-precipitate the Uranium, proceed to ST-RC-0100, "Actinide Coprecipitation."
12.0 DATA ANALYSIS AND CALCULATIONS
12.1 Density: Sample weight divided by the volume of said sample weight.
12.1.1 D=M/V D=Density, M=Mass and V=Volume
12.2 Commonly used calculations (e.g. % recovery and RPD) and standard instrument software
calculations are given in the TestAmerica St. Louis ST-QAM. Specific analysis calculations are
given in the applicable analytical SOP.
13.0 DATA ASSESSMENT AND ACCEPTANCE CRITERIA; CORRECTIVE ACTIONS FOR OUT
OF CONTROL DATA
13.1 Data assessment does not pertain to this sample preparation procedure.
13.1 Samples requiring re-preparation are submitted to the preparation lab with a NCM detailing the
issue. The NCM process is described in SOP: ST-QA-0036. Specific information is given in the
applicable analysis SOP.
14.0 METHOD PERFORMANCE
14.1 Method performance data, Reporting Limits, and QC acceptance limits, are given in the associated
analytical SOP
14.2 Demonstration of Capability
1.2.1. Initial and continuing demonstrations of capability requirements are established in the
ST-QAM.
14.3 Training Qualification
1.3.1. The manager/supervisor has the responsibility to ensure that this procedure is performed
by an analyst who has been properly trained in its use and has the required experience.
1.3.2. The analyst must have successfully completed the initial demonstration capability
requirements prior to working independently. See requirements in the ST-QAM.
14.4 Annually, the analyst must successfully demonstrate proficiency to continue to perform this
analysis. See requirements in the ST-QAM.
15.0 VALIDATION
15.1 Laboratory SOPs are based on published methods (EPA, DOE, ASTM, Eichrom, Standard
Methods) and do not require validation by the laboratory. The requirements for laboratory
demonstration of capability are included in the ST-ST-QAM. Laboratory validation data would
be appropriate for performance based measurement systems, non-standard methods and
significant modifications to published methods. Data from said validations is held in the QA
department.
16.0 WASTE MANAGEMENT AND POLLUTION PREVENTION
16.1 All waste will be disposed of in accordance with Federal, State and Local regulations. Where
reasonably feasible, technological changes have been implemented to minimize the potential for
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pollution of the environment. Employees will abide by this method and the policies in section 13
of the Corporate Safety Manual for "Waste Management and Pollution Prevention."
16.2 Waste Streams Produced by the Method
16.2.1 The following waste streams are produced when this method is carried out.
16.2.1.1 Acidic sample waste generated. All acidic waste will be accumulated in the
appropriate waste accumulation container, labeled as Drum Type "A" or "B".
16.2.1.2 Contaminated disposable glass or plastic materials utilized in the analysis are
disposed of in the sanitary trash. If the lab ware was used for the analysis of
radioactive samples and contains radioactivity at a level of 100 cpm over
background as determined by a GM meter, the lab ware will be collected in waste
barrels designated for solid rad waste for disposal by the EH&S Coordinator.
17.0 REFERENCES
17.1 Eichrom Technologies, Inc Analytical Procedure "ACW13 VBS Thorium, Plutonium and
Uranium in Water (with Vacuum Box System". January 2003
17.2 Eichrom Technologies, Inc Analytical Procedure "ACW01 Uranium and Thorium, in Water".
April, 2001
17.3 TestAmerica Quality Assurance Manual (ST-QAM), current revision
17.4 TestAmerica Corporate Environmental Health and Safety Manual (CW-E-M-001) and St. Louis
Facility Addendum (SOP ST-HS-0002), current revisions.
17.5 Associated SOPs (current revisions)
17.5.1 ST-PM-0002, Sample Receipt and Chain of Custody
17.5.2 ST-QA-0002, Standards and Reagent Preparation
17.5.3 ST-QA-0005, Calibration and Verification Procedure for Thermometers, Balances,
Weights and Pipettes
17.5.4 ST-QA-0036, Non-conformance Memorandum (NCM) Process
17.5.5 ST-RC-0004, Preparation of Soil Samples for Radiochemical Analysis
17.5.6 ST-RC-0100, Actinide Coprecipitation
17.5.7 ST-RC-5006, Decontamination of Laboratory Glassware, Labware and Equipment
17.5.8 ST-RD-0210, Daily Operations of an Alpha Spectroscopy System (using AlphaVision
Software)
18.0 CLARIFICATIONS AND MODIFICATIONS TO REFERENCED METHODS
18.1 Ascorbic acid is used in place of ferrous sulfate to do the Plutonium valance adjustment.
18.1.1 We use ascorbic acid which provides the oxidation without introducing any iron, which
is a known interference.
18.2 A 20ml rinse is done instead of a 5ml to ensure that all Uranium is rinsed from the cartridge.
18.3 The rinse steps are eliminated in the Plutonium separation step due to the larger rinse prior to the
separation of the cartridge.
18.4 Plutonium is eluted with 20ml 1M HCL to 25ml TiCl3 which serves to oxidize the Plutonium and
strip it from the column in place of 25ml Of 0.05M HN03/0.05M HF/0.02M TiCl3.
18.5 Bromocresol purple indicator is used throughout, where as the Eichrome method switches from
Bromocresol purple to phenolphthalien indicator in mid-process.
19.0 CHANGES TO PREVIOUS REVISION
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19.1 Updated to TestAmerica format.
19.2 Updated standards and reagents in section 7.0 and removed Sulfuric Acid from list.
19.3 Updated procedure in section 11.0 regarding centrifuge time length and removed "Pipet"
replacing it with "Add" throughout the section.
19.4 Rev. 13:
19.4.1 Updated the section 11.4 in reference to the amount of time sample must remain in
centrifuge.
19.5 Rev. 14:
19.5.1 Added Hydrochloric Acid to Cresol Red indicator solution in section 7.9.
19.5.2 Added a note to section 11.5.1.1.3 stipulating that samples with 5mL or more of
gel/sediment need to go though a clean-up process.
19.5.3 Added section 11.6 for Actinide Extraction from Gel/Sediment formation.
19.6 Rev. 15:
19.6.1 Updated the summary of method in section 2.0.
19.6.2 Updated equipment used in section 6.0.
19.6.3 Updated reagents & standards throughout section 7.0.
19.6.4 Removed the use of Cresol Red Indicator solution from section 7.0.
19.6.5 Updated section 8.0 regarding storage, collection, pH testing and preservatives of
samples.
19.6.6 Added uranium to the list of analytes used for laboratory control samples in section 9.3.
19.6.7 Updated section 11.0 regarding water sample prep, calcium phosphate precipitation and
thorium/plutonium/uranium separation using Eichrom resins.
19.6.8 Removed instruction for actinide extraction from gel/sediment formation in section 11.0.
19.6.9 Updated calculation for sample density in section 12.0
19.7 Rev. 16:
19.7.1 Section 7, removed reference to NIST traceable
19.7.2 Section 8, removed holding time requirement
19.7.3 Section 9, MB composition updated and LCS requirements updated.
19.7.4 Section 11.5.5 updated
19.7.5 Section 15 updated
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Sequential Thorium, Plutonium and Uranium
via TEVA/UTEVA
All rinses should flow at ImL/minute (only 3M HNO s may be done at 3ml/minute)
*only necessary when analyzing for Plutonium
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TestAmerica
THE LEADER IN ENVIRONMENTAL TESTING
TestAmerica St. Louis
SOP No. ST-RD-0102, Rev. 12
Effective Date: 04/16/2014
Page No.: 1 of 14
Title: GAMMAVISION ANALYSIS
Approvals (Signature/Date):
Chris Hough
Radiochemistry Manager
Tony L.
Quality ^surance Specialist
Mi/
Michael Ridenh^wer Date
Health & Safety Manager / Coordinator
S >5-n| VM W/S/Zf
Date Elaine Wild Date
Elaine Wild
Laboratory Director
This SOP was previously identified as SOP No. ST-RD-0102 Rev. 11
Copyright Information:
This documentation lias been prepared by TestAmerica Laboratories, Inc. and its affiliates ("TestAmerica"), solely
for their own use and the use of their customers in evaluating their qualifications and capabilities in connection
with a particular project. The user of this document agrees by its acceptance to return it to TestAmerica upon
request and not to reproduce, copy, lend, or otherwise disclose its contents, directly or indirectly, and not to use it
for any other purpose other than that for which it was specifically provided. The user also agrees that where
consultants or other outside parties are involved in the evaluation process, access to these documents shall not be
given to said parties unless those parties also specifically agree to these conditions.
THIS DOCUMENT CONTAINS VALUABLE CONFIDENTIAL AND PROPRIETARY INFORMATION.
DISCLOSURE, USE OR REPRODUCTION OF THESE MATERIALS WITHOUT THE WRITTEN
AUTHORIZATION OF TESTAMERICA IS STRICTLY PROHIBITED. THIS UNPUBLISHED WORK
BY TESTAMERICA IS PROTECTED BY STATE AND FEDERAL LAW OF THE UNITED STATES. IF
PUBLICATION OF THIS WORK SHOULD OCCUR THE FOLLOWING NOTICE SHALL APPLY:
©COPYRIGHT 2014 TESTAMERICA LABORATORIES INC.
Facility Distribution No.:
Distributed To: See Electronic Distribution Sheet
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SOP No. ST-RD-0102, Rev. 12
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1.0 SCOPE AND APPLICATION
1.1 This procedure applies to all germanium detectors and the computer assisted germanium
spectroscopy analysis system.
1.2 Due to the nature of gamma spectroscopy, once the system is calibrated to a particular geometry
a similar matrix may be run as long as it is prepared to match a calibrated geometry.
1.3 This SOP is based on EPA Method 901.1 and DOE EML HASL 300 Method GA-01-R.
1.4 The requested limits (RL), minimum detectable amount (MDA) and QC limits are maintained in
the Laboratory Information Management System (LIMS).
2.0 SUMMARY OF METHOD
2.1 This procedure provides detailed instructions for energy calibration, efficiency determination,
quality control checks, background and sample counting of the germanium spectroscopy system.
3.0 DEFINITIONS
3.1 See the TestAmerica Quality Assurance Manual (ST-QAM) for a glossary of common laboratory
terms and data reporting qualifiers.
4.0 INTERFERENCES
4.1 Germanium spectrometry has potential interference. Interferences are usually in the form of
radionuclides with unresolved photon emissions. These interferences are limited by the careful
design/construction of the gamma spectral identification and interference libraries.
5.0 SAFETY
5.1 Employees must abide by the policies and procedures in the Corporate Environmental Health and
Safety Manual (CW-E-M-001), Radiation Safety Manual and this document. This procedure
may involve hazardous material, operations and equipment. This SOP does not purport to
address all of the safety problems associated with its use. It is the responsibility of the user of the
method to follow appropriate safety, waste disposal and health practices under the assumption
that all samples and reagents are potentially hazardous. Safety glasses, gloves, lab coats and
closed-toe, nonabsorbent shoes are a minimum.
6.0 EQUIPMENT AND SUPPLIES
6.1 Germanium spectroscopy system utilizing a computer based data acquisition system
(GammaVision®-3 2).
6.2 GammaVision®-32 (know as GammaVision) is a comprehensive, all-in-one package, for the
analysis of gamma-ray spectra acquired with HPGe detectors.
6.3 Global Value software is an optimization tool for automation, custom reporting, quality
assurance and data management (GammaVision productivity add-on software).
7.0 REAGENTS AND STANDARDS
7.1 All standards and reagent preparation, documentation and labeling must follow the requirements
of SOP ST-QA-0002.
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7.2 Commercially prepared mixed gamma standards in reproducible geometries, with all appropriate
NIST Source Certificate information.
8.0 SAMPLE COLLECTION, PRESERVATION AND STORAGE
8.1 TestAmerica St. Louis supplies sample containers and chemical preservatives in accordance with
the method. TestAmerica St. Louis does not perform sample collection. Samplers should
reference the methods referenced and other applicable sample collection documents for detailed
collection procedures. Sample volumes and preservative information is given in ST-PM-0002.
Samples may be collected in glass or plastic containers.
8.2 Aqueous samples are preserved with nitric acid to a pH of less than 2.
9.0 QUALITY CONTROL
9.1 See actinide preparation SOPs for additional information regarding QC types, frequency and
preparation.
9.2 Batch
9.2.1 A sample batch is a maximum of 20 environmental samples, which are prepared
together using the same process and same lot(s) of reagents.
9.2.2 Instrument conditions must be the same for all standards, samples and QC samples.
9.2.3 For this analysis, batch QC consists of a method blank, a Laboratory Control Sample ,
and Sample Duplicate.
9.3 Method Blank (MB)
9.3.1 A method blank must be counted with every sample batch.
9.3.1.1 For soils, a method blank is sodium sulfate filled in the specified geometry.
9.3.1.2 For waters, a method blank is DI water filled in the specified geometry.
9.3.1.3 For filters, a method blank is a blank petri dish.
9.4 Laboratory Control Sample (LCS)
9.4.1 An LCS must be counted with every sample batch.
9.4.1.1 For water, a purchased mixed nuclide source in the specified geometry.
9.4.1.2 For soil, a purchased mixed nuclide source in the specified geometry.
9.4.1.3 For filters, a purchased mixed nuclide source in a petri dish.
9.5 Sample Duplicate
9.5.1 A Sample Duplicate is a recounted field sample to demonstrate instrument precision,
since there is no sample preparation (required to count on a different detector than the
sample).
9.5.1.1 If requested, the laboratory may perform a Sample Duplicate which is an
additional aliquot of a field sample.
9.6 Procedural Variations/ Nonconformance and Corrective Action
9.6.1 Any variation shall be completely documented using a Nonconformance Memo and
approved by the Supervisor and QA Manager. See SOP ST-QA-0036 for details
regarding the NCM process.
9.6.2 Any deviations from QC procedures must be documented as a nonconformance, with
applicable cause and corrective action approved by the Supervisor and QA Manager.
See SOP ST-QA-0036 for details regarding the NCM process.
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10.0 CALIBRATION AND STANDARDIZATION
10.1 There are two types of Calibrations performed for Gamma: Energy and Efficiency
10.1.1 Energy Calibrations
10.1.1.1 Frequency: the energy calibration is performed once per detector. The source
is not geometry specific.
10.1.1.2 A new calibration curve must be generated after major changes to the system
or when the continuing calibration criteria cannot be met. Major changes
include significant changes in instrument operating parameters, and major
instrument maintenance (e.g. replacing the detector)
10.1.1.3 Except in specific instances, it is NOT acceptable to remove points from a
calibration curve for the purpose of meeting criteria. Refer to the TestAmerica
Policy CA-T-P-0002, Selection of Calibration Points
10.1.1.4 Range: the energy range, is 46.54 to 1836.1 keV for air filter and solid.
10.1.1.5 Criteria:
10.1.1.5.1 The curve should have, at minimum, eight calibration points used
to determine the energy relationship of the calibration.
10.1.1.5.2 The energy difference (delta A) should be within 0.05% for all
calibration points or within 0.2 keV for the calibration points.
10.1.1.5.3 The FWHM must be less than 3.0 keV at 1332 keV.
10.1.1.5.4 FWHM difference (delta A) should be within 8% for all
calibration points.
10.1.2 Efficiency Calibrations
10.1.2.1 Frequency: the efficiency calibration is performed per geometry.
10.1.2.2 A new calibration curve must be generated after major changes to the system
or when the continuing calibration criteria cannot be met. Major changes
include significant changes in instrument operating parameters, and major
instrument maintenance (e.g. replacing the detector)
10.1.2.3 Except in specific instances, it is NOT acceptable to remove points from a
calibration curve for the purpose of meeting criteria. Refer to the TestAmerica
Policy CA-T-P-0002, Selection of Calibration Points
10.1.2.4 Range: the energy range of the calibration is dependent on the matrix that is
calibrated, i.e. 46.54 to 1836.1 keV for air filter and solid, 59.5 keV to 1836.1
keV for water.
10.1.2.5 Criteria:
10.1.2.5.1 The curve should have at least eight points to determine the
efficiency
10.1.2.5.2 The calibration source must have radionuclides that "bracket" the
intended range of calibration
10.1.2.5.3 A minimum of 10,000 counts will be accumulated for each data
point
10.1.2.5.4 The efficiency difference (delta A) should be within 8% of the true
value for each point
10.2 Initial Calibration Verification (ICV) [Frequency: Once]
10.2.1 An initial calibration verification standard must be a different standard source than the
one used for the initial calibration.
10.2.1.1 The ICV check does not include short half-life nuclides which may exist in the
purchased standard. At a minimum, the ICV will always contain Am-241
(low), Cs-137 (medium) and Co-60 (high).
10.2.2 An ICV must be performed with every initial calibration.
10.2.3 The ICV percent recovery must be within ± 10% of the true value for each nuclide.
10.2.4 Not meeting this requirement may be indicative of serious system malfunction or
inaccuracies in the standards used for the initial calibration curve or ICV standard.
Corrective action must be taken (including reanalysis of the ICV, or analysis of a
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different ICV). Any decision to proceed with analysis of samples when the ICV is out-
of-control must be taken with great care and in consultation with the QA department and
the laboratory director. Any such action must be documented in an NCM.
10.3 Annual Calibration Verification (ACV) [Frequency: Annually] not geometry specific
10.3.1 An annual calibration verification check will be performed on each detector.
10.3.2 Two verification standards (second source independent from the initial calibration
source) will be used for the verification checks.
10.3.2.1 One from a water source that surrounds the detector
10.3.2.2 One from a solid source that rests on top of the detector
10.3.3 The checks will include isotopes from the low (Am-241), medium (Cs-137) and high
(Co-60) energy range.
10.3.4 The verification can be accomplished by using LCS samples counted on each detector.
10.3.5 The ACV percent recovery must be within ± 10% of the true value for each nuclide.
10.3.6 Not meeting this requirement may be indicative of serious system malfunction or
inaccuracies in the standards used for the initial calibration curve or ICV standard.
Corrective action must be taken (including reanalysis of the ACV, or analysis of a
different ACV). Any decision to proceed with analysis of samples when the ACV is
out-of-control must be taken with great care and in consultation with the QA department
and the laboratory director. Any such action must be documented in an NCM.
10.4 Daily Checks
10.4.1 The detector background shall be checked each day that the germanium spectroscopy
system is used. Limits are set at 2 sigma and 3 sigma.
10.4.1.1 Bkgd Countrate (background count rate for entire spectrum)
Tolerance (warning) = ± 2 a
Control (out) = ± 3 a
10.4.2 The instrument Channel, Energy, FWHM (resolution) and Activity Difference
(efficiency) for a detector shall be checked each day the germanium spectroscopy
system is used (using a check source that is non-geometry specific).
10.4.2.1 Channel - (low and high energy) is monitored for channel alignment. Limits
are set around the target Channel
10.4.2.1.1 QA-60 Low Energy
Tolerance (warning) = ±1 channel
Control (out) = ±2 channels
10.4.2.1.2 QA-1332 High Energy
Tolerance (warning) = ±2 channels
Control (out) = ±3 channels
10.4.2.2 Energy - (low and high energy) is monitored for energy alignment. Limits are
set around a target energy
10.4.2.2.1 QA-60 Low Energy
Tolerance (warning) = ± 0.25 keV
Control (out) = ± 0.50 keV
10.4.2.2.2 QA-1332 High Energy
Tolerance (warning) = ±0.5 keV
Control (out) = ± 0.75 keV
10.4.2.3 Full-Width at the Half Maximum (FWHM) - (low, mid, and high energy) is
monitored for peak shape There are no limits compared to a target FWHM.
There are no lower limits (-) set for FWHM.
10.4.2.3.1
QA-60
Low Energy
Tolerance (warning)
+ 1.
.1
Control (out)
+ 1.
.2
10.4.2.3.2
QA-662
Mid Energy
Tolerance (warning)
+ 1.
.7
Control (out)
+ 1.
.8
10.4.2.3.3
QA-1332
High Energy
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Tolerance (warning) = + 2.2
Control (out) = +2.3
10.4.2.4 Activity Difference (low, mid, and high energy) - is monitored to check the
percent difference between the source activity and the reported activity. Limits
are set around the target activity.
10.4.2.4.1 QA-60/662/1332 Low/Mid/High Energy
Tolerance (warning) = ±4
Control (out) = ±5
10.4.3 If the daily check is outside of the control limits, it may be recounted or tagged out with
red tag (or with an NCM). The Daily QC check may only be recounted once without
corrective action.
10.4.3.1 If the out of control parameter is found acceptable for the rerun, the instrument
can be used for the analysis of samples. Note. No corrective action is
necessary for this situation since the uncertainty can be attributed to the
stochastic uncertainty of decay process (statistics), uncertainty of the sources,
or a known uncorrected trend.
10.4.3.2 If the instrument fails to meet the acceptance criteria for the rerun, the
instrument must be declared "Out of Service". The detector/instrument must be
"tagged out". (See ST-QA-0036 for NCM details regarding tagging out of
service).
10.4.3.3 If the QC check fails the following day for the same detector for the same
specific parameter as the day before, the instrument must be declared "Out of
Service". The detector/instrument must be "tagged out" until the detector can
be evaluated and/or maintenance can be performed.
10.4.3.4 The analyst may want to:
10.4.3.4.1 Check the expiration date of the radioactive standard to confirm
the material is current, for the isotopes being utilized.
10.4.3.4.2 Check source positioning and all instrument settings.
10.4.3.4.3 Check all cables for any apparent damage and confirm that all
cables are routed to proper connectors and are in good working
order.
10.4.3.4.4 The instrument may be returned to service once the malfunction
has been corrected and the above acceptance criteria have been
met. Corrective actions must be noted in the instrument
maintenance log.
10.4.3.4.5 If a parameter has two successive values in the warning limits, the
system will be examined for a trend and noted in the maintenance
log. Decisions will be based upon the Data Quality Objectives
(DQO) and the degree of the bias in relation to the parameter.
10.5 Background
10.5.1 Background subtraction spectrum shall be established for the germanium spectroscopy
systems monthly, or when the background quality control check indicates an
unacceptable change in the daily background parameters, or as needed per client
requirements.
10.5.1.1 Background count time is 12 hours.
10.5.1.1.1 If a client project requires a longer count time, then the background
must be performed at the longer time before initiating analysis.
10.5.1.1.2 After review of the monthly background, the analyst will mark each
detector complete on the "Monthly Background Complete" sheet
located on each gamma cave (see attachment 2)
10.5.1.2 Monthly Background limits are set at 2 sigma and 3 sigma.
10.5.1.2.1 Bkgd Countrate (background count rate for entire spectrum)
Tolerance (warning) = ± 2 a
Control (out) = ± 3 a
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10.6 Calibration Software Handling
10.6.1 Gamma Detector System Energy and Shape Calibration
10.6.1.1 Acquire a spectrum from a calibration standard in the manual mode for an
appropriate duration. Save the spectrum to the path
"C:\User\Cal\Spectra\DetX\OriginalCountfileName.spc" where:
10.6.1.1.1 X = Detector Number
10.6.1.1.2 Analysis method
10.6.1.1.3 Select library
10.6.1.1.4 Enter correct sample data.
10.6.1.1.5 Enter correct conversion time.
10.6.1.2 Close all detectors windows in the current instance of gamma vision, then
recall the appropriate calibration spectrum into the buffer window.
10.6.1.3 Select the menu "Analyze\Setting\Sample type
10.6.1.4 Select the browse button next to the "File" field and open the file. Click the
"OK" button of the window to close it.
10.6.1.5 Recall the application Calibration File from the menu "Calibration \Recall
Calibration..."
10.6.1.6 Select the menu "Calibrate\Calibration wizard..."
10.6.1.7 Select the option to create new energy calibrations. Select the next button.
10.6.1.8 On the energy calibration wizard page, select the file
"DET EnergyStandardMix Lib" or appropriate library for mixed gamma used
the browser button if desired. Select the next button.
10.6.1.9 Select the next button to perform the energy, FWHM.
10.6.1.10 Select the edit energy button to review the energy.
10.6.1.10.1 Close the energy calibration sidebar window.
10.6.1.11 Select the save calibration button and save the calibration to
"Cal\Energy\X_Energy.clb" where X is the detector.
10.6.1.12 Enter the calibration description in the format "XENERGYGEOMETRY"
where X is the detector number and Geometry is an appropriate geometry
description when prompted. Select the Finish button to close the calibration
wizard.
10.6.1.13 Print the calibration report from the menu "Calibrate \print calibration.
10.6.2 Gamma Detector System Efficiency Calibration
10.6.2.1 Acquire a spectrum from a calibration standard in the manual mode for an
appropriate duration. Save the spectrum to the path
"C:\User\Cal\Spectra\DetX\OriginalCountfileName.spc" where:
10.6.2.1.1 X = Detector Number
10.6.2.1.2 Analysis method
10.6.2.1.3 Select library
10.6.2.1.4 Enter correct sample data.
10.6.2.1.5 Enter correct conversion time.
10.6.2.2 Close all detector windows in the current instance of Gamma Vision, then
recall the appropriate calibration spectrum into the buffer window.
10.6.2.3 Select the menu "Analyze\Setting\Sample Type"
10.6.2.4 Select the browse button next to the "File", field and open the file. Click the
"OK" button at the bottom of the window to close it.
10.6.2.5 Recall the applicable calibration file from the menu "CalibrationVRecall
Calibration" (if the geometry file currently exists)
10.6.2.6 Select the menu "Calibrate\Calibration Wizard"
10.6.2.7 Select the option to create new energy and efficiency calibration. Select next
button.
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10.6.2.8 On the Energy Calibration Wizard page select the file "EnergyStandardMix
Lib" or appropriate library for mixed gamma used the browser button if
desired. Select the Next button.
10.6.2.9 On the Efficiency Calibration Wizard page, select library file,
"DETEfficiencyCalibration.Lib" for mixed gamma sources.
10.6.2.10 On the Efficiency Calibration Wizard page, select the appropriate
Certification file from the directory.
10.6.2.11 Select the next button to perform the energy FWHM and efficiency
calibration.
10.6.2.12 Select the Edit Energy button to review the energy and FWHM Calibration.
10.6.2.12.1 Close the Efficiency Calibration side window.
10.6.2.13 Select the save calibration button and save the calibration to
CalYXGeometry.clb" where X is the detector and geometry is an appropriate
geometry name.
10.6.2.14 Enter the calibration description in the format "x Geometry Source
number date counted" where X is the detector number and geometry is an
appropriate geometry description when prompted. Select the finish button to
close the calibration wizard.
10.6.2.15 Print calibration report from the menu "Calibratc\Prilit Calibration"
10.6.2.16 Select "Analyze", select "Entire spectrum in memory" and file print.
10.6.2.17 Close the spectrum Buffer window and save the spectrum when prompted.
10.6.3 Detector Long Background Counting
10.6.3.1 Remove any samples from the detector, clean the detector, close the shield lid
and start acquisition.
10.6.3.2 Select detector 1 in Global Value Quick Start
10.6.3.3 Select Monthly Background PBC under Automation Groups
10.6.3.4 Select Background PBC Long Count under Automation Jobs.
10.6.3.5 Login using name and password.
10.6.3.6 Select "OK", ensure detector cave is empty.
10.6.3.7 Repeat for each detector which background you would like to start.
10.6.3.8 After the background is complete it will save as a PBC file.
11.0 PROCEDURE
11.1 Calibration Quality Control (Daily Check)
11.
1.1
Place the calibration quality control sample on the detector, and start acquisition.
11.
1.2
Select detector from Global Value Quick Start.
11.
1.3
Select Quality Control under Automation Groups.
11.
1.4
Select Daily Quality Control Check under Automation Jobs.
11.
1.5
Login with user name and password.
11.
1.6
Select "OK", ensure source is on detector.
11.
1.7
Repeat for each detector.
11.
1.8
Record in the instrument run log.
11.2 Background Quality Control (Daily Background)
11.2.1 Remove any samples from the detector, and start acquisition.
11.2.2 Select detector global value quick start.
11.2.3 Select quality control under automation groups.
11.2.4 Select daily background check under automation jobs.
11.2.5 Login with username and password.
11.2.6 Select "OK", ensure detector cave is empty.
11.2.7 Repeat for each detector.
11.2.8 Record in the instrument run log.
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11.3 Sample Counting
11.3.1 Place the sample on the detector.
11.3.2 Select detector from GlobalValue quick start.
11.3.3 Select analyze samples under automation groups.
11.3.4 Select count sample under automation jobs.
11.3.5 Login with username and password.
11.3.6 Scan sample description from barcode report.
11.3.7 Select analysis method, sample type, geometry, library, correct date, count time,
continue.
11.3.8 Select "OK", ensure sample is on detector.
11.3.9 Record in the instrument run log.
12.0 DATA ANALYSIS AND CALCULATIONS
12.1 Commonly used calculations (e.g. % recovery and RPD) and standard instrument software
calculations are given in the Test America St. Louis ST-QAM.
12.2 All calculations are performed in GammaVision-32 software; conversions are performed in
RadCapture. Calculations are found in ST-QAM.
13.0 DATA ASSESSMENT AND ACCEPTANCE CRITERIA; CORRECTIVE ACTIONS
FOR OUT OF CONTROL DATA
13.1 The data assessment and corrective action process is detailed through the LIMS
Nonconformance Memorandum (NCM) process. The NCM process is described in SOP: ST-
QA-0036.
13.2 Method Blank (MB)
13.2.1 Acceptance Criteria:
13.2.1.1 No target analytes may be present in the method blank above the requested
limit.
13.2.1.2 Project specific requirements if more stringent than our routine procedure (e.g.
no target anlaytes present above Vi RL), will be noted on the client
requirements sheet.
13.2.2 Corrective Action for Method Blanks not meeting acceptance criteria:
13.2.2.1 Method Blank Contamination - The blank may be re-counted once to confirm
the activity (in the same detector). If the re-counted MB activity exceeds the
MDA and/or the requested limit, samples with less than 10 times the activity
found in the blank are recounted. An NCM is written to document the
excursion. Note certain analytes are common laboratory contaminants which
require special narrative comment. These compounds are so designated in
LIMS.
13.3 Laboratory Control Sample (LCS)
13.3.1 Acceptance Criteria:
13.3.1.1 All control analytes must be within the specified control limits for accuracy
(%Recovery) and precision (RPD).
13.3.2 Corrective Action for LCS not meeting acceptance criteria:
13.3.2.1 LCS Spike Recovery excursion (high) - The LCS may be re-counted once to
confirm the result. If the re-counted LCS exceeds the control limit, samples
that are non-detect may be reported with an NCM.
13.3.2.2 LCS Spike Recovery excursion (low) - The LCS may be re-counted once to
confirm the result. If the low recovery is confirmed, the batch is recounted.
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13.3.2.3 RPD/RER Duplicate excursion - The LCS is recounted if both RPD and RER
exceed criteria.
13.4 Duplicate
13.4.1 Acceptance Criteria:
13.4.1.1 All control analytes must be within the specified control limits forprecision
(RPD), max. 40% RPD, RER < 1.
13.4.2 Corrective Action for Duplicate not meeting acceptance criteria:
13.4.2.1 RPD/RER Duplicate excursion - The sample is recounted if both RPD and
RER exceed criteria.
13.5 Insufficient Sample
13.5.1 For any prescribed re-preparation corrective action, if there is insufficient sample to
repeat the analysis a narrative comment stating such is included in the report narrative.
The insufficient sample description is included in the LIMS NCM within the type
defining the excursion.
14.0 METHOD PERFORMANCE AND DEMONSTRATION OF CAPABILITY
14.1 Method performance data, Reporting Limits, and QC acceptance limits, are given in the
appendix of this SOP.
14.2 Demonstration of Capability
14.2.1 Initial and continuing demonstrations of capability requirements are established in the
ST-QAM.
14.3 Training Qualification
14.3.1 The manager/supervisor has the responsibility to ensure that this procedure is performed
by an analyst who has been properly trained in its use and has the required experience.
14.3.2 The analyst must have successfully completed the initial demonstration of capability
requirements prior to working independently. See requirements in the ST-QAM.
14.4 Annually, the analyst must successfully demonstrate proficiency to continue to perform this
analysis. See requirements in the ST-QAM.
15.0 VALIDATION
15.1 Laboratory SOPs are based on published methods (EPA, DOE, ASTM, Eichrom, Standard
Methods) and do not require validation by the laboratory. The requirements for laboratory
demonstration of capability are included in the ST-QAM. Laboratory validation data would be
appropriate for performance based measurement systems, non-standard methods and significant
modifications to published methods. Data from said validations is held in the QA department.
16.0 WASTE MANAGEMENT AND POLLUTION PREVENTION
16.1 All waste will be disposed of in accordance with Federal, State and Local regulations. Where
reasonably feasible, technological changes have been implemented to minimize the potential for
pollution of the environment. Employees will abide by this method and the policies in section 13
of the Corporate Environmental Health and Safety Manual for "Waste Management and
Pollution Prevention."
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17.0 REFERENCES
17.1 Department of Energy (DOE) Environmental Monitoring Laboratory (EML) HASL-300 28th
Edition, method GA-01-R, Gamma Radioassay
17.2 EPA Prescribed Procedures for Measurement of Radioactivity in Drinking Water Method 901.1
17.3 American National Standards Institute (ANSI) Accredited Standards Committee on Radiation
Instrumentation, N42; ANSI N42.14-1999, American National Standard for Calibration and Use
of Germanium Spectrometers for the Measurement of Gamma-Ray Emission Rates of
Radionuclides
17.4 Ortec MCB Connections-32, Hardware Property Dialogs Manual, current version
17.5 MAESTRO-3 2, MCA Emulator, current version
17.6 GammaVision-32, Gamma-Ray Spectrum Analysis and MCA Emulator, current version
17.7 Master library Source: Gerhard Erdtmann, Werner Soyka
17.8 TestAmerica Quality Assurance Manual (ST-QAM), current revision
17.9 TestAmerica Corporate Environmental Health and Safety Manual (CW-E-M-001) and St. Louis
Facility Addendum (SOP ST-HS-0002), current revisions.
17.10 TestAmerica Policy CA-T-P-0002, Selection of Calibration Points
17.11 Associated SOPs, Current Revision:
17.11.1 ST-RC-0003, Drying and Grinding of Soil and Solid Samples
17.11.2 ST-RC-0004, Preparation of Soil Samples for Radiochemical Analysis
17.11.3 ST-RC-0025, Preparation of Samples for Gamma Spectroscopy
17.11.4 ST-QA-0002, Standards and Reagent Preparation
17.11.5 ST-QA-0014, Evaluation of Analytical Accuracy and Precision Through the Use of
Control Charts
17.11.6 ST-QA-0036, Non-Conformance Memorandum (NCM) Process
18.0 CLARIFICATIONS, MODIFICATIONS TO THE REFERENCE METHOD
18.1 None.
19.0 CHANGES FROM PREVIOUS REVISION
19.1 Annual Review, No Changes.
19.2 Revision 8:
19.2.1 Increased background count times from 12 to 36 hours in section 10.3.1.1.
19.2.2 Updated the procedure for detector long background counting in section 10.5 to reflect
new software.
19.2.3 Updated daily calibration checks, daily background and sample counting procedures in
section 11.0 to reflect new software.
19.3 Revision 9:
19.3.1 Replaced quartz sand with sodium sulfate to be used for soil method blanks in section
9.2.
19.3.2 Updated section 10.4 regarding instrument daily checks.
19.3.3 Updated data assessment and acceptance criteria in section 13.0
19.3.4 Updated section 9.0 regarding batch, method blank and laboratory control samples.
19.3.5 Updated the calibation points for an internal calibation in section 10.1.
19.3.6 Updated the percent recovery regarding the ICV in section 10.2.
19.3.7 Updated software storage file name throughout section 10.5.
19.4 Revision 10:
19.4.1 Updated references to QuantlMS through out
19.4.2 Update §10.1
19.4.3 Added § 10.3 Annual Calibration Verification
19.4.4 Updated § 10.4: 36 hour background changed to 12 hour and requirement to complete
Attachment 2
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19.4.5 Added Attachment 2. "Monthly Background Complete" example
19.4.6 Updated § 13 references to Clouseau changed to LIMS
19.4.7 Added §17 reference to ANSI 42.14-1999
19.5 Revision 11:
19.5.1 Updated §1.4 with corrected termonolgy
19.5.2 Updated §6.0 software details
19.5.3 Additon/Update § 10.0 major change in calibration
19.5.4 Updated §13.0 additional corrective action steps
19.5.5 Updated § 15.0 with new verbiage
19.6 Revision 12:
19.6.1 Spelling and grammar corrections made throughout SOP.
19.6.2 Sections 10.2.3 and 10.2.5 had wording changed to common text.
19.6.3 Section 10.4.3.3 was updated to add 'for the same specific parameter as the day before'
and 'until the detector can be evaluated and/or maintenance can be performed.'.
19.6.4 Section 10.5.1.2.1 was added to provide limits for monthly backgrounds, which were
not previously provided.
19.6.5 Section 13.4.2 had 'LCS' changed to 'duplicate' since it is the duplicate section and
LCS was incorrectly referenced.
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Attachment 1
-+¦ fasared
Detector # 1 Bkgd Countrats QA Chart TofcfTOi
= ConSrol
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Attachment 2
Example of the form, actual form in use may have slight variations.
2013 Monthly Background Complete
Jan
Reveiwed bv
Initials & Date
Feb
Reveiwed by
Initials & Date
Mar
Reveiwed bv
Initials & Date
April
Reveiwed by
Initials & Date
May
Reveiwed by
Initials & Date
June
Reveiwed by
Initials & Date
July
Reveiwed by
Initials & Date
Aug
Reveiwed by
Initials & Date
Sept
Reveiwed by
Initials & Date
Oct
Reveiwed by
Initials & Date
Nov
Reveiwed bv
Initials & Date
Dec
Reveiwed by
Initials & Date
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TestAmerica
THE LEADER IN ENVIRONMENTAL TESTING
TestAmerica St. Louis
SOP No. ST-RD-0210, Rev. 11
Effective Date: 08/21/2013
Page No.: 1 of 16
Title: ALPHA SPECTROSCOPY ANALYSIS
[DOE HASL-300 A-01-R]
CnwsXough
Radiochemistry Manager
Approvals (Signature/Date):
Date
Marti ward
Quality Assurance Manager
Date
Michael Ridemower Date
Health & Safety Manager / Coordinator
\lyJ
ilaine Wild
Laboratory Director
'Date
This SOP was previously identified as SOP No. ST-RD-0210 Rev. 10
Copyright Information:
This documentation has been prepared by TestAmerica Laboratories, Inc. and its affiliates ("TestAmerica"), solely
for their own use and the use of their customers in evaluating their qualifications and capabilities in connection with
a particular project. The user of this document agrees by its acceptance to return it to TestAmerica upon request and
not to reproduce, copy, lend, or otherwise disclose its contents, directly or indirectly, and not to use if for any other
purpose other than that for which it was specifically provided. The user also agrees that where consultants or other
outside parties are involved in the evaluation process, access to these documents shall not be given to said parties
unless those parties also specifically agree to these conditions.
THIS DOCUMENT CONTAINS VALUABLE CONFIDENTIAL AND PROPRIETARY INFORMATION.
DISCLOSURE, USE OR REPRODUCTION OF THESE MATERIALS WITHOUT THE WRITTEN
AUTHORIZATION OF TESTAMERICA IS STRICTLY PROHIBITED. THIS UNPUBLISHED WORK
BY TESTAMERICA IS PROTECTED BY STATE AND FEDERAL LAW OF THE UNITED STATES. IF
PUBLICATION OF THIS WORK SHOULD OCCUR THE FOLLOWING NOTICE SHALL APPLY:
©COPYRIGHT 2013 TESTAMERICA LABORATORIES, INC
Facility Distribution No.:
Distributed To: See Electronic Distribution Sheet
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1.0 SCOPE AND APPLICATION
1.1 This procedure applies to alpha spectroscopy detectors and the computer assisted alpha
spectroscopy analysis systems, using AlphaVision software.
1.2 This SOP is based on DOE method A-01 -R
1.3 This SOP is applicable to both liquid and solid matrices.
1.4 The requested limits (RL), minimum detectable amount (MDA) and QC limits are maintained in
the Laboratory Information Management System (LIMS).
2.0 SUMMARY OF METHOD
2.1 This SOP provides detailed instructions for energy calibration, efficiency determination, quality
control checks, background and sample counting of the alpha spectroscopy system.
3.0 DEFINITIONS
3.1 See the TestAmerica St. Louis Quality Assurance Manual (ST-QAM) for glossary of common
terms and data qualifiers.
3.2 Tracer - A known amount of 232U, 242Pu or 236Pu, 243Am, 209Po, 244Cm or 229Th (depending on
analyte(s) required) added to each sample to determine chemical yield. The tracer serves as an
internal standard, which is used to calculate the activity of the target isotopes.
3.3 Region of Interest (ROI) - The keV range through which the target isotope peak signal responds.
3.4 keV - (kilo electron Volt) - electron volt is a unit of energy defined as_the amount of energy
gained (or lost) by the charge of a single electron moved across an electric potential difference of
one volt.
3.5 Tailing - Tailing is a delayed return of a peak to chromatographic baseline or continuation of
response beyond its normal response window (RT window, ROI) due to high concentration of the
analyte or matrix interference.
3.6 AlphaVision - The Alpha Spectrometer data collection and processing software.
4.0 INTERFERENCES
4.1 Alpha spectrometry has many potential interferences. These are usually in the form of radionuclides
with unresolved alpha emissions. Poorly resolved alpha peaks are often due to high alpha activity
rates or attenuation of the alpha emissions.
4.2 Isotope peak responses, when sufficiently high, may tail into other isotope ROI. Th-229 tailing
into the Th-230 region of interest is a recognized example. This interference is minimized by
maintaining low activities of the Th-229 tracer and monitoring of the separation of the ROI for
Th-229 and Th-230. The use of manual integration may be required.
4.3 Some isotopic elements are not distinguishable and are reported as an isotopic pair, unless
specifically directed by the client not to do so. These pairs may be reported separately depending
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on the client's DQO and the use-ability of the data. When reported separately, the narrative must
describe the technical aspects of how the isotopic pair was divided.
4.3.1 Recognized Isotopic Pairs:
4.3.1.1 Plutonium-23 9/240
4.3.1.2 Uranium-235/236
4.3.1.3 Uranium-233/234
4.3.1.4 Curium-245/246
4.3.1.5 Curium-247/248
5.0 SAFETY
5.1 Employees must abide by the policies and procedures in the Corporate Environmental Health and
Safety Manual (CW-E-M-001), Radiation Safety Manual and this document. This procedure may
involve hazardous material, operations and equipment. This SOP does not purport to address all of
the safety problems associated with its use. It is the responsibility of the user of the method to
follow appropriate safety, waste disposal and health practices under the assumption that all
samples and reagents are potentially hazardous. Safety glasses, gloves, lab coats and closed-toe,
nonabsorbent shoes are a minimum.
5.2 SPECIFIC SAFETY CONCERNS OR REQUIREMENTS
None.
5.3 PRIMARY MATERIALS USED
None.
6.0 EQUIPMENT AND SUPPLIES
6.1 Alpha spectroscopy system utilizing a computer based data acquisition system.
6.1.1 Hardware - Octete Plus and Alpha Ensemble
6.1.2 Software - AlphaVision and Radcapture
7.0 REAGENTS AND STANDARDS
7.1 All standards and reagent preparation, documentation and labeling must follow the requirements
of SOP ST-QA-0002, current revision.
7.2 Commercially prepared alpha standards for the isotopes Th-230, Pu-239 and Am-243.
8.0 SAMPLE COLLECTION, PRESERVATION AND STORAGE
8.1 TestAmerica St. Louis supplies sample containers and chemical preservatives in accordance with
the method. TestAmerica St. Louis does not perform sample collection. Samplers should
reference the methods referenced and other applicable sample collection documents for detailed
collection procedures. Sample volumes and preservative information is given in ST-PM-0002.
9.0 QUALITY CONTROL
9.1 See actinide preparation SOPs for additional information regarding QC types, frequency and
preparation
9.2 Batch
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9.2.1 A sample batch is a maximum of 20 environmental samples, which are prepared together
using the same process and same lot(s) of reagents.
9.2.2 Instrument conditions must be the same for all standards, samples and QC samples.
9.2.3 For this analysis, batch QC consists of a Method Blank (MB), a Laboratory Control
Sample (LCS), and Sample Duplicate (Dup). In the event that there is insufficient sample
to analyze a sample duplicate, an LCS Duplicate (LCSD) is prepared and analyzed.
9.2.3.1 Matrix Spike (MS) and Matrix Spike Duplicate (MSD) may be performed upon
client request, and are noted in the Client Requirement Sheets and Log-in.
9.3 Method Blank (MB)
9.3.1 A method blank is a blank matrix processed simultaneously with, and under the same
conditions as, samples through all steps of the procedure.
9.3.2 A method blank must be prepared with every sample batch.
9.4 Laboratory Control Sample (LCS)
9.4.1 An LCS is a blank matrix spiked with a known amount of analyte(s), processed
simultaneously with, and under the same conditions as, samples through all steps of the
analytical procedure.
9.4.2 An LCS must be prepared with every sample batch.
9.5 Matrix Spike (MS)
9.5.1 A Matrix Spike is an aliquot of a field sample to which a known amount of target
analyte(s) is added, and is processed simultaneously with, and under the same conditions
as, samples through all steps of the analytical procedure.
9.6 Sample Duplicate (Dup)
9.6.1 A Sample Duplicate is an additional aliquot of a field sample taken through the entire
analytical process to demonstrate precision.
9.7 Procedural Variations/ Nonconformance and Corrective Action
9.7.1 Any variation shall be completely documented using a Nonconformance Memo and
approved by the Supervisor and QA, see SOP ST-QA-0036 for details regarding the
NCM process.
9.7.2 Any deviations from QC procedures must be documented as a nonconformance, with
applicable cause and corrective action approved by the Supervisor and QA, see SOP ST-
QA-0036 for details regarding the NCM process.
10.0 INSTRUMENT SETUP, CALIBRATION, AND STANDARDIZATION
10.1 Initial instrument setup is performed when instrument is first installed, when a detector or
chamber is changed/replaced, when a chamber is returned from the manufacturer after servicing,
or other such circumstances. The following steps should be taken to ensure proper setup. Steps
may be accomplished either through hardware knobs/potentiometers or through software settings
(depending upon the system hardware/software). See the hardware and/or software manual to
determine further detailed instructions:
10.1.1 Set the conversion gain to 1024 channels.
10.1.2 Adjust the coarse and fine gain as well as the offset to adjust the location of the three peaks of
the alpha source such that the lower energy peak (Th-230 at 4688 keV) falls into channel
176, the mid-energy peak (Pu-239 at 5155 keV) falls into channel 239, and the higher energy
peak (Am-241 at 5486 keV) falls into channel 283. Note that this results in 107 channels
between the low energy and high energy peaks (about 7.46 keV/channel with offset of
approximately 3375 keV). Ensure each peak is within 2 channels of the desired channel
before beginning energy and efficiency calibrations.
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10.1.2.1 Gain adjustment:
10.1.2.1.1 Turning the knob counter-clockwise decreases the gain (decrease the
value in the fine gain for software adjustment), causing the spectrum
peaks to move closer to each other (smaller keV/channel slope) and
toward the lower energy.
10.1.2.1.2 Turning the knob clockwise increases the gain (increase the value in
the fine gain for software adjustment), causing the spectrum peaks to
spread apart (larger keV/channel slope) and toward higher energy.
10.1.2.2 Offset adjustment:
10.1.2.2.1 Increasing the offset moves the peak/spectra toward the the left (lower
channel number) without altering the keV/channel (slope).
10.1.2.2.2 Decreasing the offset moves the peak/spectra toward the right (higher
channel number) without altering the keV/channel (slope).
10.1.3 Adjust the pulser setting such that the pulser peak is centered at about channel 222
(approximately 5 MeV).
10.2 Calibrations, see 10.6 for procedure.
10.2.1 Energy calibrations shall be performed for the alpha spectroscopy systems yearly, or when a
calibration quality control check indicates an unacceptable change in the energy calibration
parameters.
10.1.1.1 Energy Calibrations shall be performed using at least three isotopes within
the energy range of 3-6 MeV. Typical isotopes used are Th-230, Pu-239, and Am-
241. Final peak energy positions of all observed isotopes shall be within ± 5
channels (~40 keV) of expected channel/energy (see 10.1.2). The actual energy vs.
channel and the equation with the slope is not calculated. Setting the peaks to
within 5 channels of expected will ensure calculations utilizing fixed Regions of
Interest (ROI) for each isotope will provide accurate results with minimal need for
manual adjustment of ROI. Routine pulser checks and continuing calibration
verifications (see below) will help control/monitor for drift.
10.2.2 Efficiency calibrations shall be established for the alpha spectroscopy systems yearly, or
when a calibration quality control check indicates an unacceptable change in the efficiency
calibration parameters.
10.2.2.1 Calibrated efficiency should fall between 20% and 32%. Values outside this range
do not constitute a failure. However, if the calibrated efficiency does fall outside
this range, an evaluation of the suitability of the detector for use should be
performed and documented.
10.2.3 Initial calibration verifications (ICV) shall be performed utilizing an independent second
source following the initial calibration.
10.2.3.1 The efficiency of the ICV must fall withing 95%-105% of the initial calibration
efficiency value.
10.2.3.2 A second level review will be perfomed before detectors are placed into service and
will be noted as acceptable in the electronic monthly maintenance log.
10.3 Continuing Calibration Verification (CCV)
10.3.1 A continuing calibration verification shall be performed on a monthly basis.
10.3.1.1 The Final peak energy positions for the isotopes should fall within ± 5 channels of
the expected channel/energy.
10.3.1.2 The efficiency should fall within 95%-105% of the calibrated efficiency.
10.3.1.3 A second level review will be performed before detectors are placed into service
and will be noted as accepable in the electronic monthly maintenance log.
10.4 Background subtraction spectrum shall be established for the alpha spectroscopy systems monthly, or
when the background quality control check indicates an unacceptable change in the daily background
parameters.
10.5 Daily Checks (Pulsers)
10.5.1 Routine pulser quality control verifications are performed each day of use.
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10.5.1.1 The pulser energy, peak centroid, peak resolution, peak area quality control for
a detector shall be checked each day that the alpha spectroscopy system is used.
The limits for pulser centroid and pulser energy will be as below:
10.5.1.1.1 Gross counts must be within 5% of the average (20-point minimum)
for each detector.
10.5.1.1.2 The peak resolution (FWHM) must fall within 10-20 keV.
10.5.1.1.3 The pulser centroid must fall within ± 5 channels of the average (20-
point minimum) for each detector.
10.5.1.1.4 The pulser energy must fall within ± 40 keV of the average (20-point
minimum) for each detector.
10.5.2 Routine calibration, background and pulser quality control parameters using the "Boundry"
out-of-range test will be found unacceptable if the value is outside parameter tolerance.
10.5.2.1 The routine quality control check should be rerun to determine the statistical
significance of the out of control parameter.
10.5.2.2 If the out of control parameter is found acceptable in the rerun, the investigation will
be noted in the instrument maintenance log.
10.5.2.3 Check the integrity of the radioactive standard.
10.5.2.4 Check source positioning and all instrument settings.
10.5.2.5 Check all cables for any apparent damage and to confirm that all cables are routed
to proper connectors and are in good working order.
10.5.3 If the instrument fails to meet the acceptance criteria, and the corrective actions above do not
resolve the problem, the instrument must be "tagged" out of service (OOS) for the day see
Attachment 1 for OOS tag example.
10.5.3.1 This is noted on the Alpa Spec Daily report by marking the report (The report will
display FAIL for criteria not met). The detector will be marked out of service with
the date and initials of the analyst performing the daily check.
10.5.3.2 If a detector fails three consecutive days for the same criteria, the detector will be
taken out of service until the problem is resolved. This is done by clicking on the
detector in Alphavision. Right click on the the detector, select detector properties,
check the "out of service" box and fill in the description field briefly explaining the
problem. Mark the detector with an OOS tag as a visual indicator of its status.
10.5.3.3 The instrument may be returned to service once the malfunction has been corrected
and the above acceptance criteria have been met. Note any repairs in the
maintenance log.
10.6 Calibration process in the Software
10.6.1 Alpha Detector System Energy and Efficiency Calibration
10.6.1.1 Print out the standards sheet for calibration
10.6.1.1.1 Location: Wslsvr01\rad\afoha\Calibration Sources .
10.6.1.2 Load sources into the detector
10.6.1.3 In the AlphaVision software, click on the Calibration icon.
10.6.1.4 Click on the detector to be calibrated.
10.6.1.5 Select Process and then select calibration from the dropdown menu.
10.6.1.5.1 The Calibration Explorer Window will appear.
10.6.1.6 In the General Window: Scan the source name;AV(detector)#-#_date (with year
month day format YYYYMMDD).
10.6.1.7 Choose the correct source template.
10.6.1.8 Click next
10.6.1.9 In the Acquisition window, confirm count time of 140 minutes
10.6.1.10 Click next
10.6.1.11 In the Energy/Efficiency Calibration Window, confirm the correct source is used,
and select which shelf the source is on. (This will be shelf 1) Make sure the
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'Active' box is checked so the calibratoin is put in use immediately after
calibration is processed.
10.6.1.12 Click next
10.6.1.13 In the Report Window, select print on completion
10.6.1.14 Click finish
10.6.1.15 When count is complete, the Manual Energy and Efficiency Calibration Window
will appear. In this window, select Calibration ROI, Click Calibrate, click Save.
10.6.1.16 Verify the efficiency is above 20% and below 32%
10.6.1.17 Repeat for each detector
10.6.1.18 Record the calibration in the Alpha Maintenance Log.
10.6.2 ICV Procedure
10.6.2.1 Print out the standards sheet for ICV
10.6.2.1.1 Location: \\slsvr01\rad\alpha\Calibration Sources
10.6.2.2 Place the correct source into the detector.
10.6.2.3 In The AlphaVision software, click on the Calibration Icon
10.6.2.4 Click on the detector to be calibrated
10.6.2.5 Select Process and then select calibration from the dropdown menu
10.6.2.5.2 The Calibration Explorer Window will appear.
10.6.2.6 In the General Window; Scan the source name; AV(detector)#-#_date (with year
month day format YYYYMMDD).
10.6.2.7 Chose the correct source template
10.6.2.8 Click next
10.6.2.9 In the Energy/Efficiency Calibration Window, confirm the correct source is used,
and select which shelf the source is on. (This will be shelf 1)
10.6.2.10 Click next
10.6.2.11 In the Report Window, select print on completion
10.6.2.12 Click finish
10.6.2.13 When the count is complete, the Manual Energy and Efficiency Calibration
Window will appear. In this window, select Calibration ROI, click Calibrate and
click Save.
10.6.2.14 Verify the efficiency is above 20% and below 32%
10.6.2.15 Repeat for each detector
10.6.2.16 Record the ICV in the Alpha Maintenance Log.
10.6.2.17 Open the AlphaVision Access database program on computer slradlS
10.6.2.18 Select QC main from the form tab
10.6.2.19 Enter date range
10.6.2.20 Select system 1 for AlphaVision or system 2 for AlphaVision 1
10.6.2.21 Select Get Cal Data.
10.6.2.22 Exit
10.6.2.23 Select Check Ver to run the report and verify the ICV passes criteria.
10.6.2.24 For the Intitial Calibratin (IC), the detectors must have the box checked in the Cal
Data window for that specific calibration and the previous year's IC must be
unchecked and the 'do not use' box must be checked to ensure the correct
calibration is being used.
10.6.3 CCV Procedure
10.6.3.1 Print out standards sheet for CCV on the network
10.6.3.1.1 Location: \\slsvr01\rad\alpha\Calibration Sources
10.6.3.2 Load sources into the detectors
10.6.3.3 In the AlphaVision software, click on the Calibration Icon.
10.6.3.4 Click on the detectorto be calibrated
10.6.3.5 Select process and then select calibration from the dropdown menu
10.6.3.5.1 The Calibration Explorer Window will appear.
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10.6.3.6 In the General Window: "Scan the source name;AV(detector)#-#_date (with year
month day format YYYYMMDD)."
10.6.3.7 Select correct source template
10.6.3.8 Click Next
10.6.3.9 In the Acquisition window, confirm count time of 60 mins
10.6.3.10 Click Next
10.6.3.11 In the Energy/Efficiency Calibration Window, confirm the correct source is used
and select which shelf the source is on. (This will be shelf 1)
10.6.3.12 Click next
10.6.3.13 In the Report Window, select print on completion
10.6.3.14 Click finish
10.6.3.15 When the count is complete, the Manual Energy and Efficiency Calibration
window will appear. In this window, select Calibration ROI, select Calibrate and
Save.
10.6.3.16 Verify the efficiency is above 20% and below 32%.
10.6.3.17 Repeat for each detector
10.6.3.18 Record the CCV in the Alpha Maintenace Log.Efficiency must be greater than
20% and less than 32%.
10.6.3.19 Open the AlphaVision Access database program on computer slradl8.
10.6.3.20 Select QC main from the form tab.
10.6.3.21 Enter date range.
10.6.3.22 Select system 1 for AlphaVision or system 2 for AlphaVision 1.
10.6.3.23 Select Get Cal Data.
10.6.3.24 Exit.
10.6.3.25 Select Check Ver to run the report and verify the CCV passes criteria.
10.6.4 Detector Background Process (See Section 10.4)
10.6.4.1 Select the Batch Icon
10.6.4.2 Select backgrounds from the Tool Bar
10.6.4.3 Select Process.
10.6.4.3.1 This will open the General Window in B atch Wizard
10.6.4.4 Name the background with month_year format MonthYYMMM YY (e.g.
JAN_04)
10.6.4.5 Select correct template (provided by analyst)
10.6.4.6 Click next.
10.6.4.7 In the Sample Window, add all detector names with the format:
ICB;AV(detector)#.
10.6.4.8 Click next
10.6.4.9 In the Acquisition Window, confirm count time is set at 960 minutes (or as long as
the longest sample count time)
10.6.4.10 Click next
10.6.4.11 In the Analysis Set Up Page, select Background Library and Background ROI,
check the Use ROI box.
10.6.4.12 Click next
10.6.4.13 In the Report Window, select print on completion
10.6.4.14 Click finish
10.6.4.15 The Detector Assignment worksheet will appear, assign detectors, and select start
now.
10.6.4.16 Record the backgrounds in the instrument maintenance log.
10.6.4.17 The background spectrum will be processed by the software
10.6.4.18 The detectors shall be "categorized" after each monthly background. The
detectors will be labelled as follows:
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Countsin Region of Interest (i.e. Th230. Th232. U234. U238. Pu238. Pu239):
9 0-2 counts - Blue - Ultra Low Level
0-4 counts - Yellow - Intermediate Low Level
0-20 counts - Green - Low Level
® 0-40 counts -Red - Always designated for Routine analysis when the RL=1 or
the activity is from a known radioactive site.
See Attachment 1 Detector Color Key
10.6.4.19 Detectors with backgrounds above the counts listed above are taken out of service
for cleaning.
10.6.4.20 Detectors may also be removed from service when there is a visible peak present
or at analyst judgment.
10.6.4.21 Backgrounds will be 2nd reviewed before placing into service and a notation of
acceptable will be listed in the electronic monthly maintenance log.
10.7 Detector Cleaning (This should be done before starting Backgrounds)
10.7.1 Clean detector surface with ethanol and a clean cotton ball.
10.7.2 Clean the sample tray and place a clean background planchette on the tray.
10.7.2.1 A passing background count is required before returning the detector to service.
10.6 Standard Verification Procedure
10.6.2 Receive manual batch from prep
10.6.3 Count for 960 minutes (make sure batch is set up correctly).
10.6.4 After count, open decay corrector (located in Rad Dive, LSC, decay corrector) to see if
isotope you are verifying needs to be decay corrected, (if the isotope verifying is located in
this spreadsheet, it needs to be decay corrected). Note, new activity on the prep sheet.
10.6.5 Open new spreadsheet verification folder (located in Rad Drive) and select master 3 or 6
point verification (depending on how many standards are made)
10.6.6 Enter calculated value from Decay Corrector (as True value) and value from the spectra
print outs (activity on the spectra for the Isotope you are verifying).
10.6.7 Make sure units match.
10.6.8 Standard passes if the mean value is within 5% of certified (true) value, the 1.96 sigma value
is within 10% of mean value and the standard reverification acceptablity evaluations are all
yes.
10.6.9 Sign bottom of prep sheet and calculation page.
10.6.10 Give to prep supervisior.
PROCEDURE
11.6 For sample preparation reference the applicable preparation SOP.
11.7 Initial Setup
11.7.2 Establish the normal instrument settings for all controls.
11.7.2.6 Detector specific high voltage settings and required polarity are listed in the method
software settings.
11.7.3 Pulser quality controls shall be checked before each use of the instrument.
11.8 Counting Samples
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11.8.2 In Radcapture, go to Utilities > Export>Choose 'Alphavision' or 'Alphavisionl'
depending on which instrument the samples were set up on>, enter batch # in the
window that pops up, and click ok to export to Alphavision.
11.8.3 In Alphavision, go to Process, select Batch to open the Batch Wizard.
11.8.4 Choose Load from LIMS, and pick the batch.
11.8.5 Choose proper analysis by clicking on the correct isotope
11.8.6 Select Next
11.8.7 Click on blank, and then pick blank type (Uu blank, Pu Blank, etc...)
11.8.8 Click on LCS, and then pick LCS type with correct spike number. For amount, use the
spike aliquot amount (0.1, 0.2 mL, 0.1326 g, etc) which is printed on the batch paper
work.
11.8.9 Select Next
11.8.10 Live time is count time. Enter correct count time for the batch, selectnext.
11.8.11 Select Nuclide Library, choose correct ROI and the specified tracer that is printed on the
batch paper work.
11.8.12 Selectnext
10.7.3 Select correct activity units (DPM, pCi, etc), select Activity concentration,
10.7.3.1 QuantlMS: change TPU Sigma to 2 (unless otherwise noted in client
requirements), add 5% systematic uncertainty and check the negative
activity box. .
10.7.3.2 TALS: always select TPU Sigma 1, add 5% systematic uncertainty and
check the negative activity box. .
11.8.13 Select Next, two times.
11.8.14 Select Print on Completion.
11.8.15 Select Finish.
11.8.16 Click and drag correct detectors to the correct sample ID and select Start Now.
11.8.17 The spectrum will be processed by the software.
10.7.4 For DOE:
10.7.4.1 FWHM of each tracer peak shall be < 100 keV
10.7.4.2 Tracer peak energy for each sample shall be within ± 50keV of the
expected energy.
11.8.18 Backgrounds are checked after high activity samples by counting an 180 minute
background with an empty chamber (see 11.9.2).
11.9 Samples with a count rate of greater than 1 CPS should be removed from the alpha counting
system to prevent contamination of detector(s).
11.9.2 Alpha detectors exposed to samples with count rates greater than 1 CPS should be
tagged out-of-service until an empty chamber check can be performed. To perform an
empty chamber check, place a clean stainless steel disc in the chamber, establish
vacuum, turn on bias and start acquisition for the pre-set time (180 minutes). Note this
in the instrument and maintenance log.
DATA ANALYSIS AND CALCULATIONS
12.1 Commonly used calculations (e.g. % recovery, RPD, uncertainty, MDC, tracer recovery) and
standard instrument software calculations are given in the TestAmerica St. Louis QAM.
12.2 Isotope ROI and libraries are derived from the PCNudat master nuclide library:.
12.2.1 http://www.nndc.bnl.gov/nudat2/indx dec.isp
12.3 Any manual integration of a peak or group of peaks must be documented. In all instances where
the data system report has been edited or where manual integration has been performed, the
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operator must clearly identify such edits or manual procedures. Reference SOP ST-QA-0040 for
details.
13.0 DATA ASSESSMENT AND ACCEPTANCE CRITERIA; CORRECTIVE ACTIONS FOR
OUT OF CONTROL DATA
13.1 The data assessment and corrective action process is detailed through the LIMS Nonconformance
Memorandum (NCM) module. The NCM process is described in SOP: ST-QA-0036.
13.2 Method Blank
13.2.1 Acceptance Criteria:
13.2.1.1 No target analytes may be present in the method blank above the reporting limit.
13.2.1.2 Project specific requirements if more stringent than our routine procedure (e.g.
no target anlaytes present above Vi RL), will be noted on the client requirements
sheet.
13.2.2 Corrective Action for Method Blanks not meeting acceptance criteria:
13.2.2.1 Method Blank Contamination - If the MB concentration exceeds the applicable
criteria, the batch must be re-prepped unless the concentration of all associated
samples is less than the RL or greater than ten times the concentration found in
the blank.
13.3 Laboratory Control Sample (LCS)
13.3.1 Acceptance Criteria:
13.3.1.1 All control analytes must be within the specified control limits for accuracy
(%Recovery) and precision (RPD).
13.3.2 Corrective Action for LCS not meeting acceptance criteria:
13.3.2.1 LCS Spike Recovery excursion (high) - Samples with results less than the RL
may be reported with an NCM (unless prohibited by client requirements).
Samples with detects for the isotopes with a high bias in the LCS are re-prepped
and re-analyzed.
13.3.2.2 LCS Spike Recovery excursion (low ) - The batch is re-prepped and re-
analyzed for the affected isotope.
13.3.2.3 RPD/RF.R Duplicate excursion - For the RPD/RER one or both must be within
acceptance limits. The RPD limit is 40% or less. The RER limit is 1 or less
depending on the significant digits. Not meeting the criteria requires a reprep
of the samples. If samples have a physical matrix issue (ie, nonhomogenous),
results can be reported with an NCM. If samples fail RPD/RER criteria after the
reprep and no matrix issue is observed sample may be reported with client
approval and narrated in an NCM.
13.4 Matrix Spike/Matrix Spike Duplicate (MS/MSD)
13.4.1 Analytes should be within control limits for accuracy (%Recovery) and precision (RPD).
13.4.2 Corrective Action for MS/MSD not meeting acceptance criteria:
13.4.2.1 MS/MSD Spike Rec. excursion may not necessarily warrant corrective action
other than narration
13.5 Sample Result Evaluation
13.5.1 Tracer recovery must be within specified limits. Tracer limits are 30% -110% unless
other wise specified by the client
13.5.2 Tracer/Carrier recovery (low) - Re-extract using a reduced volume or recount for
maximum count time to achieve 400 tracer counts
13.5.2.1 Note: QSAS allows for reporting results as quantitative when tracer recoveries
are below 30% if:
13.5.2.1.1 the relative uncertainty associated with the tracer recovery is less
than 10% (2 sigma)
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13.5.2.1.2 spectral resolution requirements are met and there are no
indications of spectral interferences (resolution of <100 keV).
13.5.2.1.3 detection limit requirements have been met
13.5.3 Tracer/Carrier recover/ (high) - If the blank and LCS are within limits, have the sample
logged in for native analyisis if not already logged in for native. If the blank and or LCS
has high recovery, a reprep is required.
13.5.3.1 Truncation to 100%: Truncation can be done at the clients discretion, or with
approval from manager or technical director or based on sample history.
13.5.3.2 A sample tracer recovery outside QC limits may be accepted if the sample
results are determined valid:
13.5.3.2.1 minimum number of tracer counts
13.5.3.2.2 level of uncertainty
13.5.3.2.3 client project requirements/approval
13.5.4 These expections will be documented using the NCM process. The NCM will narrate the
conditions upon which the sample results were accepted with tracer recovery excursions.
13.5.5 The following occurances require a dilution to be performed:
13.5.5.1 Dilution level is determined by taking the highest gross counts divided by the
count time divided by a factor of 2. (ie: 7200/180/2=1:20)
DL = GCtsHigh jtcount 12
DL = Dilution Level
GCtsHigh = Highest Gross Counts
tcount = Co""l Time
13.5.5.1.1 Tailing - A peak is significantly tailing out side its region of
interest (ROI)
13.5.5.1.2 The tracer recovery is low due the high activity of the sample
13.5.5.1.3 Peak Interference - A Peak is observed which is identified as an
interference
13.6 Insufficient Sample
13.6.1 For any prescribed re-preparation corrective action, if there is insufficient sample to
repeat the analysis an NCM is written and a narrative comment stating such is included
in the report narrative.
14.0 METHOD PERFORMANCE AND DEMONSTRATION OF CAPABILITY
14.1 Method performance data, Reporting Limits, and QC acceptance limits, are maintained in the
LIMS.
14.2 Demonstration of Capability
14.2.1 Initial and continuing demonstrations of capability requirements are established in ST-
QAM
14.3 Training Qualification
14.3.1 The manager/supervisor has the responsibility to ensure that this procedure is performed
by an analyst who has been properly trained in its use and has the required experience.
14.3.2 The analyst must have successfully completed the initial demonstration capability
requirements prior to working independently. See requirements in ST-QAM.
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14.1 Annually, the analyst must successfully demonstrate proficiency to continue to perform this
analysis. See requirements in ST-QAM.
15.0 VALIDATION
15.1 Laboratory SOPs are based on published methods (EPA, DOE, ASTM, Eichrom, Standard
Methods) and do not require validation by the laboratory. The requirements for laboratory
demonstration of capability are included in the ST-QAM. Laboratory validation data would be
appropriate for performance based measurement systems, non-standard methods and significant
modifications to published methods. Data from said validations is held in the QA department.
16.0 WASTE MANAGEMENT AND POLLUTION PREVENTION
16.1 All waste will be disposed of in accordance with Federal, State and Local regulations. Where
reasonably feasible, technological changes have been implemented to minimize the potential for
pollution of the environment. Employees will abide by this method and the policies in section 13
of the Corporate Safety Manual for "Waste Management and Pollution Prevention."
16.2 Waste Streams Produced by the Method
16.2.1 The following waste streams are produced when this method is carried out.
16.2.1.1 Contaminated disposable glass or plastic materials utilized in the analysis are
disposed of in the sanitary trash. If the lab ware was used for the analysis of
radioactive samples and contains radioactivity at a level of 100 cpm over
background as determined by a GM meter, the lab ware will be collected in waste
barrels designated for solid rad waste for disposal by the EH&S Coordinator.
17.0 REFERENCES
17.1 Department of Energy (DOE) Environmental Measurement Laboratory (EML) HASL 300 28th
Edition method A-01-R, Alpha Radioassay
17.2 AlphaVision-32, Alpha Particle Spectrum Acquistion and Analysis for Microsoft Windows and NT,
Software Version 5.0 Installation, User Interface and Reference Guide, Ortec (latest version)
17.3 OCTETE Plus, Integrated Alpha-Spectroscopy System Hardware Operating Manual, 777720, Ortec
(latest version)
17.4 MAESTRO-32, MCA Emulator for Microsoft Windows, A65-B32 Software User's Manual, 777800,
Ortec (latest version)
17.5 U.S. Nuclear Regulatory Commission, Quality Assurance for Radiological Monitoring Programs
(Normal Operations) - Effluent Streams and the Environment, Regulatory Guide 4.15.
17.6 "Quality Assurance Program Requirements for Nuclear Facilities", ANSI/ASME NQA-1 (latest
edition).
17.7 TestAmerica, St. Louis Quality Assurance Manual, current revision
17.8 Corporate Environmental Health and Safety Manual (CW-E-M-001) and St. Louis Facility
Addendum (SOP ST-HS-0002), current revisions.
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17.9 Decay Radiation Datebase, Version of 5/8/2013; http://www.nndc.bnl.gov/nudat2/indx dec.isp
17.10 Associated SOPs, current revisions
17.10.1 ST-PM-0002, Chain of Custody
17.10.2 ST-QA-0002, Standard and Reagent Preparation
17.10.3 ST-QA-0014, Evaluation of Analytical Accuracy and Precision Through the Use of
Control Charts
17.10.4 ST-QA-0036 Non-Conformance Memorandum (NCM) Procedure
17.10.5 ST-QA-0040, Manual Integration Procedure
17.10.6 ST-RC-0040, Total Alpha Emitting Isotopes of Radium
17.10.7 ST-RC-0238, Isotopic Uranium By Eichrom® Uteva Resin For Various Matrices
17.10.8 ST-RC-0210, Determination Of Polonium-210 By Alpha Spectrometry
17.10.9 ST-RC-0232, Isotopic Thorium And/Or Neptunium In Various Matrices By Eichrom®
Teva Separation Resin
17.10.10 ST-RC-0240, Isotopic Americium, Curium, Plutionium, Thorium, And Uranium In
Various Matrices By Eichrom® Separation Resin
17.10.11 ST-RC-0241, Americium, Plutonium, Curium, And Uranium In Various Matrices By
Eichrom® Uteva And Tru Resins (With Vacuum Box System)
17.10.12 ST-RC-0242, Isotopic Thorium, Plutonium And Uranium In Various Matrices By
Eichrom® Separation Resins
17.10.13 ST-RC-0246, Isotopic Americium, Curium, Uranium In Various Matrices By Eichrom®
Separation Resins
18.0 MODIFICATIONS TO REFERENCE METHOD
18.1 Energy calibrations checks are performed monthly. Daily pulsar checks are performed in place of
the weekly energy calibration checks.
18.2 Backgrounds are determined monthly rather weekly
18.3 CCV's are determined monthly rather that before and after each measurement.
19.0 CHANGES TO PREVIOUS REVISION
19.1 No Changes- Annual Review
19.2 Rev. 8:
19.2.1 Section 10 additions
19.2.1.1 Addition of Instrument setup as §10.1
19.2.1.2 Addition of Calibration Quality Control Check as §10.3
19.2.1.3 Addition of calibration acceptance criteria
19.3 Rev. 9:
19.3.1 Section 10.5, addition of limits for pulser centroid and pulser energy
19.4 Rev. 10:
19.4.1 Section 10:
19.4.1.1 2nd level review for ICV and CCV added to section 10
19.4.1.2 1200 minute setting for acquisition window for special projects
19.4.1.3 Upper control limits for long backgrounds
19.4.1.4 Detector cleaning
19.4.2 Section 12: addition of ROI and library reference
19.4.3 Section 13: Occurances that require dilution
19.4.4 Addition of Attachement 1
19.5 Rev. 11:
19.5.1 Grammatical corrections through out and removal of referencest to QuantlMS and
Clouseau
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19.5.2 Section 10, updated internal calibrations information in section and the calibration
process in the lab software throughout
19.5.3 Section 10, added new standards verification procedure
19.5.4 Section 13, added corrective actions and equation for dilution level
19.5.5 Section 15, updated with new verbiage
19.5.6 Attachment 1 revised
19.5.7 Section 13,removed "See Clouseau NCM for Corrective Action"and added specfic
Corrective Actions to the SOP
19.5.8 Section 18, added backgrounds will be done monthly and added CCV's will be done
monthly.
19.5.9 Section 3, Added "keV" definition
19.5.10 Section 6, Added Hardware and Software specifics
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Attachment 1
AlphaVision Detector Key
Red - Routine only 0-40 counts
Green - Low Level 0-20 counts
Yellow - Intermediate Low Level 0-4 counts
Special Projects and QC samples (Method
Blanks and Lab Control Samples) Only
Blue - Ultra Low Level (for Pu/Am/Np)
Special Projects Only
OOS Tag - Out of Service (OOS)
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TestAmerica
THE LEADER IN ENVIRONMENTAL TESTING
TestAmerica St. Louis
SOP No. ST-RD-0403, Rev. 14
Effective Date: 09/12/2013
Page No.: 1 of 19
Title: LOW BACKGROUND GAS FLOW PROPORTIONAL COUNTING
(GFPC) SYSTEM ANALYSIS
Approvals (Signature/Date):
5M
Cm4sr'Hough " / Date
Radiochemistry Department Manager
73
f///i
Marti Ward
Quality Assurance Manager
Date
Michael Ridentfower Date
Health & Safety Manager / Coordinator
tjaime VM
Elaine Wild ' Date
Laboratory Director
This SOP was previously identified as SOP No. ST-RD-0403 Rev. 13
Copyright Information:
This documentation has been prepared by TestAmerica Laboratories, Inc. and its affiliates ("TestAmerica"), solely
for their own use and the use of their customers in evaluating their qualifications and capabilities in connection with
a particular project. The user of this document agrees by its acceptance to return it to TestAmerica upon request and
not to reproduce, copy, lend, or otherwise disclose its contents, directly or indirectly, and not to use if for any other
purpose other than that for which it was specifically provided. The user also agrees that where consultants or other
outside parties are involved in the evaluation process, access to these documents shall not be given to said parties
unless those parties also specifically agree to these conditions.
THIS DOCUMENT CONTAINS VALUABLE CONFIDENTIAL AND PROPRIETARY INFORMATION.
DISCLOSURE, USE OR REPRODUCTION OF THESE MATERIALS WITHOUT THE WRITTEN
AUTHORIZATION OF TESTAMERICA IS STRICTLY PROHIBITED. THIS UNPUBLISHED WORK
BY TESTAMERICA IS PROTECTED BY STATE AND FEDERAL LAW OF THE UNITED STATES. IF
PUBLICATION OF THIS WORK SHOULD OCCUR THE FOLLOWING NOTICE SHALL APPLY:
©COPYRIGHT 2013 TESTAMERICA LABORATORIES, INC
Facility Distribution No.:
Distributed To: See Electronic Distribution Sheet
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Page No.: 2 of 19
1.0 SCOPE AND APPLICATION
1.1 This SOP is applicable to all Low Background Proportional Counting instruments. TestAmerica
St. Louis performs radium-226/228, strontium-89/90, gross alpha/beta, neptunium-36 and chlorine
36.
1.2 This SOP is based on SW846 method 9310, 9315 and 9320; EPA methods 900.0, 903.0, 904.0,
905.0; and DOE EML HASL 300 method, Ba-01-R, Sr-02 and Sr-03-RC.
1.3 The SOP applies to GFPC analysis of liquid and solid matrices.
1.4 The requested limits (RL), minimum detectable amount (MDA) and QC limits are maintained in
the Laboratory Information Management System (LIMS).
2.0 SUMMARY OF METHOD
2.1 This procedure provides instructions for the daily calibration and maintenance of the Low
Background Proportional Counting instrumentation.
3.0 DEFINITIONS
3.1 See the TestAmerica St. Louis Quality Assurance Manual (ST-QAM) for a glossary of common
terms and data qualifiers.
3.2 IOC - a computerized Quality Control Program where the counting results of Daily Radioactive
check sources and Daily Background checks are entered and compared to statistical average data.
A measurement within ± 3 standard deviations indicates the detector is operating within
acceptable parameters.
3.3 aLL - discriminator setting indicating the alpha lower voltage limit.
3.4 Alpha Voltage Only - detector voltage capable of collecting ions created by alpha radiation only.
Ion pairs created by beta radiation are not collected.
3.5 aUL - discriminator setting indicating the instruments alpha upper voltage limit.
3.6 BLL - discriminator setting indicating the beta lower voltage limit.
3.7 BUL - discriminator setting indicating the beta upper voltage limit.
3.8 Crosstalk - a measure of the amount of beta radiation that is collected in the alpha radiation
channel; it is also a measure of alpha radiation collected in the beta channel.
3.9 Plateau - a point on a graph of count rate vs. detector bias voltage where further increases in bias
will not result in an increase in measured counting rate.
3.10 LB4100 - LBPC (Low background Gas Flow Proportional Counting instrument).
4.0 INTERFERENCES
4.1 A detector contaminated with radioactive material will result in a high background and interfere
with the correct measurement of a sample.
4.1.1 If a sample "times out" reaching 10000 counts before the allotted time, and the sample
count rate is 60 cpm or greater, then another daily background check is performed on that
detector. If the detector background check is unacceptable, the detector is taken Out Of
Service until action is taken to bring the background check within acceptable limits. If
the chamber requires action to remove contamination and a new background check is
acceptable, then a 30 minute empty chamber count should be performed to determine if a
new long background needs to be performed on that detector.
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4.2 The actual counting efficiency for alpha radiation decreases greatly with a density > 6.0 mg/cm2.
Therefore, the maximum acceptable mass density is typically 5 mg/cm 2 or less that 100 mg for a
2" planchet.
4.3 For beta radiation, reliable data may be obtained counting samples with a density as high as 10
mg/cm 2 or greater.
4.4 Sample thickness as well as moisture content may impact the alpha and/or beta results.
5.0 SAFETY
5.1 Employees must abide by the policies and procedures in the Corporate Environmental Health and
Safety Manual (CW-E-M-001), Radiation Safety Manual and this document. This procedure may
involve hazardous material, operations and equipment. This SOP does not purport to address all of
the safety problems associated with its use. It is the responsibility of the user of the method to
follow appropriate safety, waste disposal and health practices under the assumption that all
samples and reagents are potentially hazardous. Safety glasses, gloves, lab coats and closed-toe,
nonabsorbent shoes are a minimum
5.2 SPECIFIC SAFETY CONCERNS OR REQUIREMENTS
5.2.1.1 None.
5.3 PRIMARY MATERIALS USED
5.3.1 The following is a list of the materials used in this method, which have a serious or
significant hazard rating. NOTE: This list does not include all materials used in the
method. The table contains a summary of the primary hazards listed in the MSDS
for each of the materials listed in the table. A complete list of materials used in the
method can be found in the reagents and materials section. Employees must review the
information in the MSDS for each material before using it for the first time or when there
are major changes to the MSDS.
Material (1)
Hazards
Exposure
Limit (2)
Signs and symptoms of exposure
Silver
Nitrate
Poison
Corrosive
Oxidizer
0.01g/m3
(TWA)
for silver,
metal dust,
and fume as
Ag
Inhalation symptoms may include burning sensation,
coughing, wheezing, laryngitis, shortness of breath,
headache, nausea, and vomiting. Skin contact may cause
redness, pain, and sever burning. Eye contact can cause
blurred vision, redness, and pain.
Ammonium
Hydroxide
Poison
Corrosive
50 ppm
(NH3)
Inhalation symptoms may include irritation to the
respiratory tract. Ingestion symptoms may include pain in
the mouth, chest, and abdomen with coughing, vomiting,
and collapse. Skin contact causes irritation and burns. Eye
contact with vapors causes irritation.
1 - Always add acid to water to prevent violent reactions.
2 - Exposure limit refers to the OSHA regulatory exposure limit.
TWA - Time Weighted Average
6.0 EQUIPMENT AND SUPPLIES
6.1 Low Background Proportional Counter, equivalent to the Canberra/Oxford/Tennelec LB4100, or
Protean MPC9604.
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6.2
Gas mixture, 90% argon, 10% Methane
6.3
Blank planchets
6.4
PC based data acquisition system, OSUM software, IQC software
6.5
Centrifuge tubes
6.6
Centrifuge
6.7
Vortex
6.8
Pipettes, Eppendorf or equivalent
6.9
Pipette, disposable
7.0 STANDARDS AND REAGENTS
7.1 All standards and reagent preparation, documentation and labeling must follow the requirements
of SOP ST-QA-0002, current revision
7.2 Radioactive sources to measure beta radiation,: Sr-90 and Ra-228 sources.
7.3 Radioactive sources to measure alpha radiation: Am-241, Th-230 and Ra-226
7.4 Deionized Water (DI), obtained from the Milli-Q unit.
7.5 Silver nitrate (AgN03), 0.5 N
7.6 Sodium chloride (NaCl), crystals
7.7 Sodium chloride (NaCl), 0.5 N
7.7.1 Add 50 mL of DI water to a 100 mL volumetric, add 5.84 g of NaCl, dilute to 100 mL,
cap and shake to dissolve. Adjust volume to 100 mL with DI water.
7.8 Ammonium hydroxide (NH4OH), concentrated, 28 N
7.9 Ammonium hydroxide (NH4OH), 5 %
7.9.1 Add 25 mL of concentrated Ammonium Hydroxide to 475 mL of DI water. CAUTION
- Ammonium hydroxide is corrosive. Mist and vapor cause burns to every area of
contact.
8.0 SAMPLE COLLECTION, PRESERVATION AND STORAGE
8.1 TestAmerica St. Louis supplies sample containers and chemical preservatives in accordance with
the method. TestAmerica St. Louis does not perform sample collection. Samplers should
reference the methods referenced and other applicable sample collection documents for detailed
collection procedures. Sample volumes and preservative information is given in ST-PM-0002.
8.2 See associated sample preparation SOPs ST-RC-0020, ST-RC -0021, ST-RC -0036, ST-RC -
0040, ST-RC -0041and ST-RC -0050, for more detailed information.
9.0 QUALITY CONTROL
9.1 See actinide preparation SOPs for additional information regarding QC types, frequency and
preparation.
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9.2 Batch
9.2.1 A sample batch is a maximum of 20 environmental samples, which are prepared together
using the same process and same lot(s) of reagents.
9.2.2 Instrument conditions must be the same for all standards, samples and QC samples.
9.2.3 For this analysis, batch QC consists of a method blank, a Laboratory Control Sample
(LCS), and Matrix Spike (MS)/ Sample Duplicate (Dup). In the event that there is
insufficient sample to analyze a sample duplicate, an LCS Duplicate (LCSD) is prepared
and analyzed.
9.2.3.1 Matrix Spike (MS) and Matrix Spike Duplicate (MSD) may be performed upon
client request, and are noted in the Client Requirement Sheets and Log-in.
9.3 Method Blank (MB)
9.3.1 A method blank is a blank matrix processed simultaneously with, and under the same
conditions as, samples through all steps of the procedure.
9.3.2 A method blank must be prepared with every sample batch.
9.4 Laboratory Control Sample (LCS)
9.4.1 An LCS is a blank matrix spiked with a known amount of analyte(s), processed
simultaneously with, and under the same conditions as, samples through all steps of the
analytical procedure.
9.4.2 An LCS must be prepared with every sample batch.
9.5 Matrix Spike
9.5.1 A Matrix Spike is an aliquot of a field sample to which a known amount of target
analyte(s) is added, and is processed simultaneously with, and under the same conditions
as, samples through all steps of the analytical procedure.
9.6 Sample Duplicate
9.6.1 A Sample Duplicate is an additional aliquot of a field sample taken through the entire
analytical process to demonstrate precision.
9.7 Procedural Variations/ Nonconformance and Corrective Action
9.7.1 Any variation shall be completely documented using a Nonconformance Memo and
approved by the Supervisor and QA Manager. See SOP ST-QA-0036 for details
regarding the NCM process.
9.7.2 Any deviations from QC procedures must be documented as a nonconformance, with
applicable cause and corrective action approved by the Supervisor and QA Manager.
See SOP ST-QA-0036 for details regarding the NCM process.
10.0 CALIBRATION AND STANDARDIZATION
10.1 Additional preventative maintenance can be found in ST-QA-0024.
10.2 Voltage Plateau Determination
10.2.1 Frequency:
10.2.1.1 Performed as a part of the Intial Calibration.
10.2.2 Voltage Plateau Determination on LB4110 Red
10.2.2.1 Place the Am-241 sources in Drawers A and B.
10.2.2.2 Select the auto-sequence file "Plateau"
10.2.2.3 Highlight the detectors in Drawers A and B
10.2.2.4 Click on 'Run"
10.2.2.5 Type 'Alpha' for the sample ID for the detectors with the alpha source
10.2.2.6 Click'Done'. The voltage plateau will begin automatically.
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10.2.2.7 When the alpha counts are complete, the highlighted detectors will flash. Click
'Unit status' and highlight the voltage plateau file name. Click on 'Re-load'.
Enter 'Beta" as the sample ID.
10.2.2.8 Place the Sr90 beta source on the detector.
10.2.2.9 Click 'Done'. The voltage plateau will complete automatically.
10.2.2.10 When the plateau is complete click on 'Data Output'. Select the plateau file.
Print the graphs and data for calibration packages. Archive the data file.
10.2.2.11 Repeat the steps above for drawers C and D.
10.2.3 Criteria for Plateaus for LB4110 Red
10.2.3.1 Voltage range used to determine the plateau is 300-1500V
10.2.3.2 Voltage increase per step is <50V per step
10.2.4 Voltage Plateau Determination on Protean MPC 9604
10.2.4.1 The manufacturer has counted plateaus and permanently set the discriminator
voltages. The manufacturer does not recommend recounting plateaus. The
detectors are manufactured to have a high dead time. However, a cross talk test
may be performed using different nuclide sources to indicate acceptable
discriminator settings. This procedure is outlined in the discriminator setting
section of this SOP.
10.2.5 Criteria for Plateaus for Protean MPC 9604
10.1.5.1 Plateaus are permanently set for this instrument from the manufactuer.
10.3 Discriminator Settings
10.3.1 Frequency:
10.3.1.1 Performed as a part of the Intial Calibration.
10.3.2 Discrimator Settings on LB4110 Red
10.3.2.1 From the unit menu, select 'Change ROI'
10.3.2.2 Place a beta source in each detector
10.3.2.3 Highligh a detector with a beta source
10.3.2.4 The alpha upper limit should be set at 100% and the beta lower limit should be
set a 0%. The alpha lower limit and the beta upperlimit should both be set at
50%.
10.3.2.5 Select 'Count'. Accumulate at least 100,000 beta counts
10.3.2.6 Reduce the beta upper limit/alpha lower limit until there is 3.5% beta into alpha
crosstalk.
10.3.2.7 Raise the alpha lower limit until there is 0.10% beta into alpha crosstalk.
10.3.2.8 Raise the beta upper limit until it is 5% less than the alpha lower limit.
10.3.2.9 Select 'Halt'.
10.3.2.10 Repeat steps above until all detectors have been set.
10.3.2.11 Select 'Close'. Discriminator settings are updated automatically.
10.3.3 Discrimator Settings on Protean MPC 9604
10.3.3.1 Collect a minimum of 10,000 counts for each of Am-241, Th-230 and Po-210
sources
10.3.3.2 Calculate the percentage of crosstalk and compare the results to historical and
expected values. Consult the Technical director if the values fall out of range.
10.4 Initial Calibration:
10.4.1 Frequency:
10.4.1.1 The Gas Flow Proportional Counter (GFPC) is calibrated initially and verified
each year thereafter. Recalibration may be required if indicated during the
operation of the instrument.
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10.4.2 The specific calibration source preparations can be found in the file containing the
previous calibration.
10.4.3 All nuclide sources shall be NIST traceable.
10.4.4 The efficiency calibration shall consist of at least seven single or dual sets of mass
attenuated calibration standards, unless a single point source efficiency is to be
determined.
10.4.5 The standards shall have enough activity to generate at least 10000 counts in 90 minutes
of count time for the most highly attenuated source. The count rate shall not exceed
5000 counts per second.
10.4.5.1 For alpha and beta analysis, separate sets of calibration sources shall be
prepared.
10.4.6 The mass attenuation is accomplished by utilization of a salt solution with comparable
make up to the majority of samples seen in the laboratory.
10.4.6.1 Alternatively, the mass attenuation may be accomplished by using the same
carrier solution used in a specific analysis.
10.4.7 Each standard shall be counted in every detector to be calibrated.
10.4.8 Criteria for a Single or Dual Set Calibration
10.4.8.1 The efficiency of the detector (the dependent variable) shall be plotted on a
single graph against the masses (the independent variable) for all data points.
10.4.8.2 The equation of the calibration curve shall be determined using polynomial
functions and be included on the plot of the curve. The curve shall be
continuous and smooth.
10.4.8.3 The degree of the polynomial shall not exceed three. The number of discreet
source pairs shall be two more than the degree of the polynomial.
10.4.8.4 The percent difference of the measured efficiency and theoretical efficiency
shall be calculated for all data points.
10.4.8.5 Points that are visual outliers or demonstrate less than 15 percent difference
between the measured efficiency and theoretical efficiency may be removed at
the analyst's discretion. Low residual mass sources and samples are difficult to
plate with acceptable duplicate precision. Therefore, high outliers may not
necessarily be removed from the calibration if they mimic live sample masses.
In any case outliers above 15 percent shall be removed from the calibration
curve. No more than 20 percent of the data points may be removed. Reasons
for removal or inclusion of outliers shall be documented in the calibration
narrative. Once outliers are removed, the percent difference between the
measured efficiency and theoretical efficiency must be recalculated using the
new polynomial coefficients generated from removal of data points. If outliers
over 15 percent difference remain between the measured efficiency and
theoretical efficiency the Radiochemistry Manager/QA must be consulted before
calibration may continue.
10.4.8.6 The coefficient of determination (r2) shall be calculated and displayed on the
plot with the equation of the trend line. An r2 greater than or equal to 0.9 is
required to proceed to counting of verification sources.
10.4.8.7 If the coefficient of determination (r2) is not greater than or equal to 0.9 on the
plot of all data points (with or without outliers removed), the data may be
plotted using the mean of the paired values for both the efficiencies and the
masses. This action is acceptable to reduce the variability caused when plating
low mass sources. Calculate the percent difference of each datum value from
the mean of the paired points. If the percent difference for any datum value is
greater than 10 percent for alpha or 7.5 percent for beta delete the data pair and
perform another statistical fit to the data. More than 20 percent of all data
points may not be removed from the curve. The coefficient of determination (r2)
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shall be calculated and displayed on the plot with the equation of the trend line.
An r2 greater than or equal to 0.9 is required to proceed to counting of
verification sources.
10.5 Independent Calibration Verification (ICV)
10.5.1 Frequency:
10.5.1.1 Performed with every intial calibration
10.5.2 GFPC initial calibrations must be verified by a second source standard.
10.5.3 The ICV standard is NIST traceable.
10.5.4 The ICV is counted to accumulate at least 5,000 counts.
10.5.5 ICV for Dual Set Calibrations:
10.5.5.1 Prepare at least one set of calibration verification sources consisting of a low,
medium and high residual mass within the calibration range of the curve.
10.5.5.2 Prepare a blank at the same time.
10.5.5.3 The sources shall contain radionuclide from a second source. Second sources
may include a second dilution from the same primary source used for the
calibration curve.
10.5.5.3.1 Alternatively, verification source nuclides may consist of different
nuclides than the calibration curve if it is customary to do so.
10.5.5.4 Count each secondary source and the blank in all detectors that were calibrated.
10.5.5.5 Calculate the results in terms of percentage recovery.
10.5.5.6 Calculate the mean results of all masses across each detector.
10.5.5.7 Criteria:
10.5.5.7.1 Individual points are within 30 percent of the true value
10.5.5.7.2 The mean result of all masses across all detectors is less than 10
percent.
10.5.5.7.3 If any detector fails the validation tests the Technical Director must
be consulted to provide corrective action.
10.5.6 ICV for Single Set Calibrations:
10.5.6.1 Prepare at least one set of verification sources varying in expected mass within
the calibration range of the curve.
10.5.6.2 Prepare a blank at the same time.
10.5.6.3 The sources shall contain radionuclide from a second source. Second sources
may include a second dilution from the same primary source used for the
calibration curve.
10.5.6.3.1 Alternatively, verification source nuclides may consist of different
nuclides than the calibration curve if it is customary to do so.
10.5.6.4 Count the secondary source and the blank in all detectors that were calibrated.
10.5.6.5 Calculate the results in terms of percentage recovery.
10.5.6.6 Calculate the mean results of all masses across each detector.
10.5.6.7 Criteria:
10.5.6.7.1 Individual points are within 30 percent of the true value
10.5.6.7.2 The mean result of all masses across all detectors is less than 10
percent.
10.5.6.7.3 If any detector fails the validation tests the Technical Director must
be consulted to provide corrective action.
10.6 Setting Performance Check Criteria After Calibration
10.6.1 Twenty background check samples are counted and used to establish quality control
limits for the daily background checks.
10.6.2 Twenty alpha/beta check sources are counted after calibration and used to establish
quality control limits for the daily source checks.
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10.6.3 The limits will be a running average of the four months post calibration.
10.6.3.1 The limits are to be documented.
10.6.3.2 The limits will be re-established monthly at the following frequency
10.6.3.2.1 1st month - take first five data points from the new month and fifteen
data points from the initial calibration.
10.6.3.2.2 2nd month - take first five points from new month, five from prior
month and ten from initial calibration.
10.6.3.2.3 3rd month - take first five points from new month, five points each
from the previous two months and five from the initial calibration.
10.6.3.2.4 4th month - take first five data points from new month and five
points each from the previous three months.
10.6.3.3 Limits are set.
10.7 Alpha to Beta Crosstalk Determination
10.7.1 The mean mass is determined for each data point used to calculate the mass attenuation
curve.
10.7.1.1 These curves are calculated and plotted and the percent of alpha into beta
crosstalk is determined. This is done by dividing the beta counts per minute as
observed in the beta channel from the alpha calibration source counts by the
sum of the alpha and beta counts per minute.
10.7.1.2 The mean percent of alpha into beta is determined for each mass point by using
the count data accumulated for two sets of alpha sources.
10.7.1.3 The crosstalk curve is plotted as mean crosstalk values relative to the mean mass
for the two sets of data.
10.7.1.3.1 In this manner the crosstalk factor can be determined for any given
mass.
10.7.1.4 The equation of the curve shall be determined using polynomial functions.
10.7.1.5 The coefficient of determination (R2) shall be calculated and displayed on the
plot as well as the equation for the trendline.
10.8 Beta to Alpha Crosstalk Determination
10.8.1 Since beta to alpha crosstalk does not vary across mass, a mean beta to alpha crosstalk
correction factor is calculated.
10.8.2 The percent of beta into alpha is determined by dividing the alpha counts per minute as
observed in the alpha channel from the beta calibration source counts by the sum of the
alpha and beta counts per minute.
10.8.3 The mean percent of beta into alpha is determined for all mass points. The mean percent
is insignificant in calculating results, therefore is not applied to the result calculation.
10.9 Long Background
10.9.1 Frequency:
10.9.1.1 Monthly or whenever instrument conditions have significantly changed since
the previous background was performed (e.g. detector replaced, etc.)
10.9.1.2 Minimum count time: 1000 minutes.
10.9.2 Wash the planchet holder and clean the drawers with a 20% radiac wash or ethyl alcohol.
10.9.2.1 Do not sprav cleaner directly onto the drawers. Sprav cleaner on a Kimwipe. a
cotton ball, or paper towel and wipe out the drawers.
10.9.3 Check that instrument settings are as specified in 11.1.
10.9.4 Red Long Background Count Set Up
10.9.4.1 Place the cursor on the red box in the upper left hand corner of the screen and
right click on the mouse.
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10.9.4.2 Select 'edit parameters'. Verily the count time on the screen is set to 1000
minutes and the iterations is set to 1. If they are different than 1000 min and
literation, change them to 1000 min and 1 iteration. Then select 'close' to exit
this window.
10.9.4.3 Place clean empty planchets in instruments.
10.9.4.4 Place the cursor on the red box in the upper left hand corner of the screen and
right click on the mouse.
10.9.4.5 Select 'create batch' from the instrument menu.
10.9.4.6 Select 'background'
10.9.4.7 Select the detectors that are to be counted by double clicking the mouse on the
drawer desired which selects all detectors in that drawer or on each individual
detector in the display.
10.9.4.8 Select 'run'
10.9.4.9 Select 'done'
10.9.4.10 When backgrounds are complete, review the printouts for acceptance.
10.9.5 Protean Long Background Count Set Up
10.9.5.1 Create Manual batch in RadCapture
10.9.5.2 Export Manual batch from RadCapture
10.9.5.3 At Protean instrument:
10.9.5.4 Select 'Detector'
10.9.5.5 Select'Sample Log'
10.9.5.6 Select appropriate Long Background (ex: Sept Lng Bkg OO) you want to start
under sample ID
10.9.5.7 Change count time to lOOOmin
10.9.5.8 Select 'Start'
10.9.5.9 Continue these steps with detectors 1-23.
10.9.5.10 Review the data for acceptance when the backgrounds are complete.
10.9.6 Printing Protean Long Backgrounds
10.9.6.1 Select 'Print Protean data icon' on the desk top
10.9.6.2 Select OK
10.9.6.3 Enter Batch#
10.9.6.4 Print
10.9.7 Protean Long Background Entry into Protean
10.9.7.1 Select Input data
10.9.7.2 Select Definitions
10.9.7.3 Select Calibrations
10.9.7.4 Select Properties
10.9.7.5 Select References 0-7 for Detectors 0 thru 7 and 8-15 for Detectors 8 thru 15
10.9.7.6 Enter Background CPM's for Alpha and Beta from printed data sheet
10.9.8 Orange and Purple Long Background Count Set-Up
10.9.8.1 Select detector 0
10.9.8.2 Select 'source log'
10.9.8.3 Select 'monthly long background' by clicking on the file list arrow.
10.9.8.4 Ensure count time is set to 1000 minutes.
10.9.8.5 Select 'start'
10.9.8.6 Continue these steps with detectors 1-23.
10.9.8.7 Review the data for acceptance when the backgrounds are complete.
10.9.9 Printing Orange and Purple Long Backgrounds
10.9.9.1 Select'Data
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10.9.9.2 Select'Source Count Data'
10.9.9.3 Select 'Source Name' Monthly Long BKG
10.9.9.4 Select 'This Range' enteryour date range that Long Backgrounds were performed.
10.9.9.5 Select'Refresh'
10.9.9.6 Select 'Source Count Summary' under Reports
10.9.9.7 Select Print'
10.9.9.8 Select 'Landscape' under Orientation
10.9.9.9 Select'OK'
10.9.10 Long Background Criteria:
10.9.10.1 The CPM for the alpha are <0.2 and the beta < 2.0, the detector may be used.
10.9.10.1.1 The data printout must include initials and date to indicate that has
been reviewed.
10.9.10.1.2 If a detector is above this limit, discard planchet.
10.9.10.1.3 Clean the planchet holder with radiac wash, ethyl alcohol or a
detergent spray cleaner and dry thoroughly.
10.9.10.1.4 Place a clean planchet in the holder and repeat steps for that detector
(s) only.
10.9.10.1.5 Performa new background.
10.9.10.1.5.1 Note: the detector is tagged out of service until a successful
background has been achieved.
10.10 Cl-36: At least four sodium chloride standards are prepared for calibration.
10.10.1.1 Add 10 mL of DI water to 4 centrifuge tubes.
10.10.1.2 Add 0.500 mL of 0.5 N sodium chloride carrier solutions to each centrifuge tube.
Swirl to mix.
10.10.1.3 Add 2 drops of 5 % ammonium hydroxide solution, swirl to mix.
10.10.1.4 Add 12 mL of 0.5 N silver nitrate solution to each centrifuge tube.
10.10.1.5 Vortex for 30 seconds.
10.10.1.6 Centrifuge and decant supernate to waste.
10.10.1.7 Proceed to section 11.4, Planchet Preparation of Silver Chloride Precipitation of
SOP ST-RC-0036.
10.10.1.8 Average the four weights for the sodium chloride carrier solution, record the
standardized weight in the log book and on the bottle.
10.10.1.9 NOTE: It may be necessary to use more than 0.500 mL of carrier in some large
water samples or calibrate a 4 N sodium chloride carrier solution. The efficiency
of the detectors will have to be calculated using the heavier sodium chloride carrier
solution.
10.10.2 Prepare four sodium chloride calibration samples as in Section 10.9 but add a known
amount of Cl-36 to each tube before the sodium chloride carrier is added. Analyze samples
by GFPC and determine detector efficiency as per Section 12, Data Analysis and
Calculations.
11.0 PROCEDURES
11.1 Initial Setup
11.1.1 Check the normal instrument settings for all controls as described below:
11.1.1.1 Tank Flow 8 psi
11.1.1.2 Flow Cells >/= 0.3 SCFH, the flow will vary, the target range is 0.15 to
0.20 SCFH.
11.1.2 The High Voltage is set as indicated in the Manuals for the LB4000/LB4100 located in
the count room file cabinet. The Protean remains as set by the manufacturer and does not
require adjustment.
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11.1.3 If counting gas has just been changed orturned on, allow a minimum purge time of 30
minutes prior to operation. Record gas tank changes on document on separate sheet.
11.2 Record date of Daily Background and Check Source Data in runlog logbook.
11.3 Maintenance
11.3.1 Change out the counting gas when the gauge reads under 500 psi. This usually occurs
every 1 to 2 weeks. Record in the instrument maintanence logbook.
11.3.2 Allow gas to purge a minimum of 30 minutes prior to operation.
11.4 Data Acquisition: Daily Background Check and Source Check
11.4.1 Daily Background Check:
11.4.1.1 Red Instrument:
11.4.1.2 Open the drawer by rotating the knob at the front of the drawer to the 'DOWN'
position and pull the sample drawer out slowly. Place clean empty planchets in
the sample holders.
11.4.1.3 Before inserting the drawer, confirm that none of the planchets
extend above the sample holder. Failure to observe this note can
result in damage to the detector.
11.4.1.4 Slowly insert sample drawer into the instrument and slowly rotate the
positioning knob into the 'UP' position.
11.4.1.5 Place the cursor on the red box in the upper left hand corner of the
screen and right click on the mouse.
11.4.1.6 Select 'create batch'
11.4.1.7 Select 'daily background check'
11.4.1.8 Select the detectors that are to be loaded by double clicking the mouse
on the drawer desired or on each individual detector in the display.
11.4.1.9 Select 'run'
11.4.1.10 Select 'done'
11.4.1.11 Measure the detector background for 200 minutes. The count time is
predetermined by the protocol selected, i.e. 'daily background check'.
11.4.1.12 The detector display will be yellow when the detector is counting.
The detector display will turn green when the count is complete.
11.4.1.13 When counting is complete, place the cursor on the red box in the
upper left hand corner of the screen and right click on the mouse.
Select 'data output' and select the data file generated by your
background counts for that instrument, "DAY- ###". Select 'ok' to
print data.
11.4.1.14 On any work station, i.e. "PC computer in the count room", double
click on the IQC icon.
11.4.1.15 Select 'import data'
11.4.1.16 Select 'Red'. Enter the current date. Click on the file list arrow.
11.4.1.17 From the file list select each file generated above individually, and then
select import data. i.e. import each "Day" or "DQC" file for that
instrument individually.
11.4.1.18 Select 'close'
11.4.1.19 Select 'reporting'. Verfiy the current date in both the 'start' and 'end'
date fields. Select 'print' to generate the report.
11.4.2 Protean Instrument:
11.4.2.1 Open each detector drawer. Place clean empty planchets into each sample
holder and slowly insert each sample drawer into the instrument.
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11.4.2.2 Double click detector 0 on the Protean computer screen.
11.4.2.3 Select'source log'
11.4.2.4 Set the time for 200 minutes.
11.4.2.5 Type 'DBO' in the sample id box. (D for daily. B for background. 0 for
detector.)
11.4.2.6 Select 'start'
11.4.2.7 Double click detector 1 on the computer screen. Repeat steps 11.4.2.3 through
11.4.2.5 for each detector, making sure to change the number to coincide with
the detector the background is counting for.
11.4.2.8 Remove planchets from detector drawers when counting is complete.
11.4.2.9 On any work station, i.e. "PC computer in the count room", double
click on the IQC icon.
11.4.2.10 Select 'import data'
11.4.2.11 Select 'Protean'. Enter the current date. Click on the file list arrow.
11.4.2.12 Select 'close'
11.4.2.13 Select 'reporting'. Verfiy the current date in both the 'start' and 'end'
date fields. Select 'print' to generate the report.
11.4.3 Orange and Purple Instrument:
11.4.3.1 Open each detector drawer. Place clean empty planchets into each sample
holder and slowly insert each sample drawer into the instrument.
11.4.3.2 Select detector 0.
11.4.3.3 Select'source log'.
11.4.3.4 Select 'DB' by clicking on the file list arrows for orange.
11.4.3.5 Select 'Daily BKG' by clicking on the file list arrows for purple.
11.4.3.6 Select 'start'
11.4.3.7 Repeat these steps with detectors 1-23.
11.4.4 Daily Background Criteria:
11.4.4.1 Review the IQC printouts for each detector.
11.4.4.1.1 If a detector fails background criteria (3 sigma), clean the detector
with radiac wash or ethyl alcohol and re-run.
11.4.4.1.2 If the detector fails a second time, but the CPM for the alpha are
<0.2 and the beta < 2.0, the detector may be used. The data
printout must include initials and date to indicate that it was
checked.
11.4.4.1.3 Circle any failed detector on the printout.
11.4.4.1.4 Place a planchet upside down in the planchet holder to indicate
that the detector is out of service for that day.
11.5 Daily Source Check
11.5.1 Red Instrument:
11.5.1.1 Open the drawer by rotating the knob at the front of the drawer to the 'DOWN'
position and pull the sample drawer out slowly.
11.5.1.2 Place alpha sources in the sample holders of the A and B drawer. Place beta
sources in the sample holders of the C and D drawer.
11.5.1.3 Place the cursor on the red box in the upper left hand corner of the screen and
right click on the mouse.
11.5.1.4 Select 'create batch'
11.5.1.5 Select 'daily source check'
11.5.1.6 Select the detectors that are loaded by double clicking the mouse on the desired
drawer or on each individual detector in the display.
11.5.1.7 Select 'run'
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11.5.1.8 Select 'done'
11.5.1.9 Measure the detector source for 2 min. The count time is predetermined by the
protocol selected, i.e. 'daily source check'
11.5.1.10 The detector display will be yellow when the detector is counting.
The detector display will turn green when the count is complete.
11.5.1.11 When counting is complete, place the cursor on the red box in the upper left
hand corner of the screen and right click on the mouse. Select 'data output' and
select the data file generated by your background counts for that instrument,
"DQC- ###". Select 'ok' to print data.
11.5.1.12 Open the drawer by rotating the knob at the front of the drawer to the 'DOWN'
position and pull the sample drawer out slowly. Place beta sources in the sample
holders of the A and B drawer. Place alpha sources in the sample holders of the
C and D drawer.
11.5.1.13 Repeat steps 11.5.1.3 to 11.5.1.11.
11.5.1.14 On any work station, i.e. "PC computer in the count room", double
click on the IQC icon.
11.5.1.15 Select 'import data'
11.5.1.16 Select 'Red'. Enter the current date. Click on the file list arrow.
11.5.1.17 From the file list select each file generated above individually, and then
select import data. i.e. import each "Day" or "DQC" file for that
instrument individually.
11.5.1.18 Select 'close'
11.5.1.19 Select 'reporting button'. Verify the current date in both the 'start' and 'end'
date fields. Select 'print'to generate the report
11.5.2 Protean Instrument:
11.5.2.1 Slowly open each detector drawer. Place alpha sources in sample holders of
detectors 0-7. Place beta sources in sample holders of detectors 8-15 and slowly
insert each drawer into the instrument.
11.5.2.2 Double click detector 0 on the Protean computer screen.
11.5.2.3 Select'source log'.
11.5.2.4 Set the time for 2 minutes.
11.5.2.5 Type "SAO" in the sample id box. (S for source. A for alpha. 0 for detector.)
11.5.2.6 Select 'start'
11.5.2.7 Double click detector 1 on the computer screen. Repeat steps 11.5.2.3 to
11.5.2.6 for each detector, making sure to change A to B when starting the beta
sources on detectors 8-15 and changing the number to coincide with the detector
the source is on.
11.5.2.8 When the counting is complete, slowly open each detector drawer. Place beta
sources in detectors 1-7. Place alpha sources in detectors 8-15.
11.5.2.9 Double click detector 0 on the Protean computer screen.
11.5.2.10 Type "SBO" in the sample id box. (S for source. B for beta. 0 for the detector.)
11.5.2.11 Double click detector 1 on the computer screen. Repeat steps 11.5.2.10 for each
detector, making sure B to A when starting the alpha sources on detectors 8-15.
11.5.3 Remove sources from detector drawers when counting is complete.
11.5.4 Orange and Purple Instrument:
11.5.4.1 Slowly open each detector drawer. Place alpha sources in sample holders of
detectors 0-7. Place beta sources in sample holders of detectors 8-15. Slowly
insert each drawer into the instrument.
11.5.4.2 Select detector 0.
11.5.4.3 Select'source log'.
11.5.4.4 Select'SAO'.
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11.5.4.5 Select 'start'
11.5.4.6 Repeat these steps for detectors 1-7 using the correlating detector number. For
detectors 8-15 select 'SB8', 'SB9', and so on for each correlating detector
number.
11.5.4.7 Slowly open each detector drawer when counting is complete. Place beta
sources in detectors 1-7 and place alpha sources in detectors 8-15.
11.5.4.8 Select detector 0.
11.5.4.9 Select 'SBO'.
11.5.4.10 Select'start'.
11.5.4.11 Repeat these steps for detectors 1-7 using the correlating detector number.
For detectors 8-15, select 'SB8', 'SB9' and so on for each correlating detector
number.
11.5.4.12 Repeat steps 11.5.4.1 to 11.5.4.11 for detectors 16-23.
11.5.4.13 Remove sources from detector drawers when counting is complete.
12.0 DATA ANALYSIS AND CALCULATIONS
12.1 Commonly used calculations (e.g. % recovery and RPD) and standard instrument software
calculations are given in the TestAmerica St. Louis ST-QAM.
12.2 Result calculations are performed by TestAmerica St. Louis' Rad Capture software program.
These calculations are found in the TestAmerica St. Louis ST-QAM.
12.3 To calculate the efficiency of the detectors for Cl-36, divide the net counts determined of the
spiked Sodium Chloride, by the known dpm of the Standard used.
Ne t Counts of Spiked Silver Chloride ,,
= Efficiency
Known dpm of Cl-36 (decay corrected to day counted)
13.0 DATA ASSESSMENT AND ACCEPTANCE CRITERIA; CORRECTIVE ACTIONS FOR
OUT OF CONTROL DATA
13.1 The data assessment and corrective action process is detailed through the LIMS Nonconformance
Memorandum (NCM) process. The NCM process is described in SOP: ST-QA-0036.
13.2 Method Blank
13.2.1 Acceptance Criteria:
13.2.1.1 No target analytes may be present in the method blank above the reporting limit.
13.2.1.2 Project specific requirements if more stringent than our routine procedure (e.g.
no target anlaytes present above Vi RL), will be noted on the client requirements
sheet.
13.2.2 Corrective Action for Method Blanks not meeting acceptance criteria:
13.2.2.1 Method Blank Contamination - (e.g. reprep/reanalysis, narration). If the
Method Blank concentration exceeds the applicable criteria, the batch must be
re-prepped unless the concentration of all associated samples is less than the RL
or greater than ten times the concentration found in the blank.
13.3 Laboratory Control Sample (LCS)
13.3.1 Acceptance Criteria:
13.3.1.1 All control analytes must be within the specified control limits for accuracy
(%Recovery) and precision (RPD).
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13.3.2 Corrective Action for LCS not meeting acceptance criteria:
13.3.2.1 LCS Spike Recovery excursion (high) - Samples with results less than the RL
may be reported with an NCM (unless prohibited by client requirements).
Samples with detects for the isotopes with a high bias in the LCS are re-prepped
and re-analyzed..
13.3.2.2 LCS Spike Recovery excursion (low) the batch is re-prepped and re-analyzed for
the affected isotope.
13.4 RPD/RER Duplicate excursion - For the RPD/RER One or both must be with in acceptance
limits. The RPD limit is 40% or less. The RER limit is 1 or less depending on the significant
digits. Not meeting the criteria requires a reprep of the samples. If samples have a physical
matrix issue (ie, nonhomogenous), results can be reported with an NCM. If samples fail
RPD/RER criteria after the reprep and no matrix issue is observed sample may be reported with
client approval and narated in an NCM.
13.5 Matrix Spike/Matrix Spike Duplicate (MS/MSD)
13.5.1 Analytes should be within control limits for accuracy (%Recovery) and precision (RPD).
13.5.2 Corrective Action for MS/MSD not meeting acceptance criteria:
13.5.2.1 MS/MSD Spike Rec. excursion may not necessarily warrant corrective action
other than narration.
13.6 Sample Result Evaluation
13.6.1 Tracer/Carrier recovery must be within specified limits.
13.6.2 Tracer/Carrier recovery low- Samples must be reextracted. Exceptions can be made and
results reported with approval from the technical director, manager, or client and
approvpriate NCM included.
13.6.3 Tracer/Carrier recovery high
13.6.3.1 A sample tracer recovery outside QC limits may be accepted if the sample
results are determined valid:
13.6.3.1.1 minimum number of tracer counts
13.6.3.1.2 level of uncertainty
13.6.3.1.3 client project requirements/approval
13.6.4 If the sample carrier recovery is significantly higher than normal, the native
concentration in the sample of the carrier analvte may be present causing a high bias to
the carrier recovery. This high bias to the carrier analvte would in turn cause a low bias
to the samples result. The laboratory defines significant to be an additional 20% above
the average LCS/MB carrier recovery (as determined from a population of LCS and MB
data), with a maximum of 110%. The table below shows the limits determined for each
carrier analvte. The analyst should ensure that the carrier analysis is requested to
determine native concentration for samples exceeding the limit.
Radium
Strontium
Chloride
110%
109%
109%
13.6.5 These expections will be documented using the NCM process. The NCM will narrate the
conditions upon which the sample results were accepted with tracer recovery excursions.
13.7 Insufficient Sample
13.7.1 For any prescribed re-preparation corrective action, if there is insufficient sample to
repeat the analysis a narrative comment stating such is included in the report narrative.
14.0 METHOD PERFORMANCE AND DEMONSTRATION OF CAPABILITY
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14.1 Method performance data, Reporting Limits, and QC acceptance limits, are given in LIMS.
14.2 Demonstration of Capability
14.2.1 Initial and continuing demonstrations of capability requirements are established in the
ST-QAM.
14.3 Training Qualification
14.3.1 The manager/supervisor has the responsibility to ensure that this procedure is performed
by an analyst who has been properly trained in its use and has the required experience.
14.3.2 The analyst must have successfully completed the initial demonstration capability
requirements prior to working independently. See requirements in the ST-QAM.
14.4 Annually, the analyst must successfully demonstrate proficiency to continue to perform this
analysis. See requirements in the ST-QAM.
15.0 VALIDATION
15.1 Laboratory SOPs are based on published methods (EPA, DOE, ASTM, Eichrom, Standard
Methods) and do not require validation by the laboratory. The requirements for laboratory
demonstration of capability are included in the ST-QAM. Laboratory validation data would be
appropriate for performance based measurement systems, non-standard methods and significant
modifications to published methods. Data from said validations is held in the QA department.
16.0 WASTE MANAGEMENT AND POLLUTION CONTROL
16.1 All waste will be disposed of in accordance with Federal, State and Local regulations. Where
reasonably feasible, technological changes have been implemented to minimize the potential for
pollution of the environment. Employees will abide by this method and the policies in section 13
of the Corporate Safety Manual for "Waste Management and Pollution Prevention."
16.2 Waste Streams Produced by the Method
16.2.1 The following waste streams are produced when this method is carried out.
16.2.1.1 Contaminated disposable glass or plastic materials utilized in the analysis are
disposed of in the sanitary trash. If the lab ware was used for the analysis of
radioactive samples and contains radioactivity at a level of 100 cpm over
background as determined by a GM meter, the lab ware will be collected in waste
barrels designated for solid rad waste for disposal by the EH&S Coordinator.
17.0 REFERENCES
17.1 Department of Energy (DOE) Environmental Monitoring Laboratory (EML) HASL-300
Procedures Manual, method Ba-01-R, Beta Radioassay, Sr-02 Strontium 90, Sr-03-RC Strontium-
90 in Environmental Samples.
17.2 Prescribed Procedures for Measurement of Radioactivity in Drinking Water, Section 1, Method
900.0 Gross Alpha and Gross Beta Radiochemistry
17.3 Prescribed Procedures for Measurement of Radioactivity in Drinking Water, Section 6, Method
903.0 Alpha-Emitting Radium Isotopes
17.4 Prescribed Procedures for Measurement of Radioactivity in Drinking Water, Section 8, Method
904.0 Radium-228
17.5 Prescribed Procedures for Measurement of Radioactivity in Drinking Water, Section 9, Method
905 Radioactive Strontium in Drinking Water
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17.6 Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, SW-846, Method 9310,
Gross Alpha and Gross Beta
17.7 Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, SW-846, Method 9315,
Alpha-Emitting Radium Isotopes
17.8 Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, SW-846, Method 9320,
Radium-228
17.9 TestAmerica St. Louis Quality Assurance Manual, current revision
17.10 Corporate Environmental Health and Safety Manual (CW-E-M-001) and St. Louis Facility
Addendum (SOP ST-HS-0002), current revisions
17.11 Associated SOPs, current revisions:
17.11.1 ST-PM-0002 "Sample Receipt and Chain of Custody"
17.11.2 ST-QA-0002, "Standards and Reagent Preparation."
17.11.3 ST-QA-0024, "Preventative Maintenance"
17.11.4 ST-QA-0036, "Non-Conformance Memorandum (NCM) Process"
17.11.5 ST-RC-0004, "Preparation of Soil, Sludge, Filter, Biota and Oil/Grease Samples for
Radiochemical Analysis".
17.11.6 ST-RC-0020, "Determination of Gross Alpha/Beta Activity"
17.11.7 ST-RC-0021, "Gross Alpha Radition in Water using Copreciptation"
17.11.8 ST-RC-0036, "Determination of Chlorine-36 in Various Matrices by GFPC"
17.11.9 ST-RC-0040, 'Total Alpha Emitting Isotopes of Radium"
17.11.10ST-RC-0041, "Radium 228 in Water"
17.11.11ST-RC-0050, "Preparation of Strontium-89 and 90"
17.11.12ST-RC-0300, "New Jersey 48-hour Gross Alpha Testing for Private Well Testing ACT
(PWTA)
18.0 MODIFICATIONS TO THE REFERENCE METHOD
18.1 TestAmerica St. Louis uses thorium-230 to calibrate the GFPC system for Ra-226. Th-230 has
similar alpha energies and a sufficiently long half life to eliminate the need for purification. The
laboratory has historically performed well on PE programs for Ra-226, demonstrating the
laboratory's ability to accurately calibrate for this isotope. Calibrating with a Ra-226 source
presents a severe bias in the quantitated result. Ra-226 can be purified and separated from all
other alpha emitting isotopes, but the moment after separation, alpha emitting daughters begin to
grow (i.e. radon-222, polonium-28 and polonium-214). As the daughter's in-growth alpha activity
changes and due to the higher alpha energies of these daughters, the measured efficiency of the
GFPC changes as well. After three weeks the alpha activity from purified Ra-226 increases by a
factor of four. Due to their short half lives, these daughters can not be isolated long enough to
mathematically correct for the bias brought on by them. Calibrating the GFPC with Ra-226 is
actually calibrating with a mix of the four isotopes and not a legitimate calibration under the cited
regulation.
18.2 Strontium-89 short half life makes it impractical to use as a calibration standard for both radium-
228 analysis, as stated in EPA method 904 and SW method 9310, and strontium-89 analysis, as
stated in EPA method 905. TestAmerica St. Louis uses a mixed strontium-90/yittrium-90 standard
for its' GFPC beta calibration used in Gross Beta, strontium-90, strontium-89, and radium-228
analyses. TestAmerica St. Louis has selected the strontium-90/yittrium-90 standard because it
produces a stable beta emission which can be reliably used for initial and continuing calibration.
By using this standard mix, we have beta emissions at the lower and upper energetic spectrum
whose average is in the middle of the beta range.
18.3 For Ra-228 analysis, TestAmerica St. Louis uses chemical separation techniques to eliminate
other potential beta emitters.
COMPANY CONFIDENTIAL AND PROPRIETARY
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SOP No. ST-RD-0403, Rev. 14
Effective Date: 09/12/2013
Page No.: 19 of 19
18.4 TestAmerica St. Louis does not perform a direct strontium-89 analysis. TestAmerica St. Louis
provides calculated results based on the difference between Total strontium and strontium-90.
19.0 CHANGES FROM PREVIOUS REVISION
19.1 Updated Section 10 to address voltage increase per step, plateau slope and QC check count
requirements (5000 counts)
19.2 Rev. 11;
19.2.1 Added instument Purple throughout section 10 and 11.
19.2.2 Adjusted procedure steps throughout section 11.
19.3 Rev. 12,
19.3.1 Added Sr-02-RC and Sr-03-RC to sections 1.0 and 17.0.
19.4 Rev. 13:
19.4.1 Added Neptunium to scope in section 1.0.
19.4.2 Updated the Quality Control Program for counting daily rad checks and daily
background checks in section 3.0.
19.4.3 Updated background count set-up, printing and entering protean data in section 10.8.
19.5 Rev. 14:
19.5.1 Removed references to Clouseau, SAC and QuantlMS
19.5.2 Section 5.0 added silver nitrate and ammonium hydroxide
19.5.3 Section 6.0 updated to include additional equipment
19.5.4 Section 7.0 updated to include addition reagents
19.5.5 Section 9.0 added reference to prep SOPs for additional information
19.5.6 Section 10.0 added sodium cloride standard preparation & reference to ST-QA-0024
19.5.7 Section 12.0 added Cl-36 detector efficiency calculation
19.5.8 Section 13.0 updated to include actual corrective actions and native concentration carrier
requirements
19.5.9 Section 13.0 updated to include corrective actions
19.5.10 Section 17.0 added reference to ST-QA-0024
COMPANY CONFIDENTIAL AND PROPRIETARY
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