DRC-2018-006022 - 0901a068808508be

Div of Waste Management
and Radiation Control
CLIVE SITE JUN 1 9 2018
LETTER OF TRANSMITTAL D12L-200-00b0Z2-
DATE: 06/18/2018
ATTN: Don Verbica — DWMRC
CC; Treesa Parker
Karen Kirkwood
RE: Transmittal 18025
Description of Documents Transmitted Qty
See attached for an update to Chem Lab;
CL-LB-PR-133 Rev 2 Liquid Scintillation 1
Please replace your current procedure revisions with the documents with in this
Transmittal.
You are not required to sign any documents to verify receipt of this distribution.
However, you should make every effort to ensure that your copy of the License is
current.
FROM: EnergySolutions
Document Control
Clive Facility
Sam Stanley, Gamma-Spectroscopy Specialist Date
Sam Stanley
Jun 14 2018 12:40 PM Authored By:
ENERGYSOLUTIONS CL-LB-PR-133
Liquid Scintillation
Revision 2
Reviewed By:
Jerrod T. Andresen Jun 14 2018 12:42 PM

Jerrod Andresen, Sample Control Officer Date
Approved By
Jared Stark
Jun 18 2018 9:03 AM

Jared Stark, Lead, Laboratory Date
Approved By
Thomas Brown
9-larm."4/ Jun 18 2018 9:05 AM cosign

Thomas A. Brown, Radiation Safety Officer Date
[s] Non-Proprietary
Proprietary EI Restricted Information
Safeguards Information II Sensitive Security Information
CI New El Title Change E Revision I=1 Rewrite
Cancellation
Electronic documents, once printed, are uncontrolled and may become outdated. Refer to the Intranet or the Document Control authority for the correct revision.
CL-LB-PR-133
Liquid Scintillation Revision 2
Table of Contents
1 PURPOSE AND SCOPE 3

1.1 Purpose 3

1.2 Scope 3
2 REFERENCES 3
3 GENERAL 3

3.2 Definitions 4

3.3 Responsibilities 5

3.4 Precautions and Limitations 5

3.5 Records 9
4 REQUIRMENTS AND GUIDANCE 9

4.1 Equipment and Supplies 9

4.2 Reagents and Standards 10

4.3 Calibration and Standardization 10

4.4 Procedure 11

4.5 Quality control 21

4.6 Corrective Actions for Out-of-Control Data 21
5 ATTACHMENTS AND FORMS 22
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1 PURPOSE AND SCOPE
1.1 Purpose
To provide guidelines for the routine operation, calibration, and maintenance of
the Packard Tricarb 2900TR and the Perkin Elmer Tricarb 4910TR Liquid
Scintillation Analyzer and detection of tritium using these instruments.
1.2 Scope
This procedure covers self nonnalization calibration (SNC), the establishment of
quench curves, typical operational functions, and steps for performing
preventative maintenance of the Packard Tricarb 2900TR and the Perkin Elmer
Tricarb 4910TR, as well as methods for the determination of tritium in a given
sample matrix using these instruments.
2 REFERENCES
2.1 CL-SH-PR-150, Laboratory Chemical Hygiene Plan
2.2 CL-TN-PR-030, Qualification Procedure
2.3 Liquid Scintillation Analysis Science and Technology. Editor Michael J. Kessler,
Ph.D. Published by Packard Instrument Company 1989, Meriden CT.
2.4 QuantiSmartTM for the Tricarb® Liquid Scintillation Analyzer Reference Manual.
Published by Packard Instrument Company 1999, Meriden CT
2.5 Handbook of Environmental Liquid Scintillation Spectrometry. Charles J. Passo,
Jr. and Gordon T. Cook, Ph.D. Published by Packard Instrument Company 1996.
Meriden, Ct.
2.6 QuantaSmart Preventative Maintenance Procedure. PerkinElmer.
2.7 QuantaSmart Preventative Maintenance Check List. PerkinElmer
2.8 EPA 906.0, section 10 of EPA report no. EPA-600/4-80-032, Prescribed
Procedures for Measurement of Radioactivity in Drinking Water. Krieger,
Herman L. and Whittaker, Earl L., August 1980.
2.9 1985 Annual Book of ASTM Standards, Vol. 11.01; Standard Specification for
Reagent Water; ASTM: Philadelphia, PA, 1985; D1193-77.
3 GENERAL
3.1 Summary
3.1.1 Self Nonnalization and Calibration (SNC) is performed daily or prior to
counting samples. The baseline values for acceptance on this measurement
are established upon receipt of the instrument and when the SNC source
set being used expires and is replaced with a new source set.
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3.1.2 If quench curves are to be used to report activity for an isotope, the
associated quenched standard set is to be recounted and re-plotted at least
annually. A minimum of five standards of varying quench shall be used to
plot quench curves.
3.1.3 This procedure covers preventative maintenance functions of the Packard
Tricarb 2900TR and the Perkin Elmer Tricarb 4910TR, which are to be
performed at a minimum of annually while the instrument is in use at the
EnergySolutions Clive Facility. Preventative maintenance on the Packard
Tricarb 2900TR and the Perkin Elmer Tricarb 4910TR serves to optimize
the instruments performance and reduce the likelihood of instrument
breakdown.
3.1.4 Filter paper swipes are counted as received after the addition of Liquid
Scintillation Counting (LSC) cocktail to the counting vial.
3.1.5 Water samples are treated with sodium hydroxide and potassium
permanganate and distilled prior to counting, based on the guidelines in
EPA 906.0. The alkaline treatment prevents other radionuclides such as
radioiodine and radiocarbon from distilling over with the tritium. The
permanganate treatment oxidizes trace organics in the aliquot which could
distill over and cause quenching interferences. This applies to the
detection of tritium as T20 and HTO.
3.2 Definitions
3.2.1 Cassettes - Rack for holding counting vials within the liquid scintillation
counter. A standard cassette holds twelve counting vials and enables
movement of counting vials on the sample changer deck.
3.2.2 Counting Vials - 20 mL super polyethylene vial used to contain the sample
and added cocktail for counting within the liquid scintillation counting
instrument.
3.2.3 Figure of Merit (Efficiency2/Background) - A term applied to a numerical
value used to characterize the performance of a system. In liquid
scintillation counting, specific formulas have been derived for
quantitatively comparing certain aspects of counter performance and
cocktail performance.
3.2.4 LSC Cocktail - A solution containing solvent, scintillators, and emulsifiers
that is added to samples in preparation for analysis by liquid scintillation
counting.
3.2.5 Protocol Flags - numbered, plastic devices that contain an enclosed,
reflective metal that the instrument uses to identify the appropriate assay
counting parameters for a set of samples.
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3.2.6 Quench Curve - a mathematical graph which correlates the counting
efficiency to a quench indicating parameter (QIP). The QIP for a sample is
determined during sample counting. This value is used to interpolate the
counting efficiency for a sample from the quench curve (where %
Efficiency is plotted vs. the QIP). The interpolated efficiency value is use
to calculate the dpm.
3.2.7 Self Normalization and Calibration (SNC) - The normal calibration
functions of the liquid scintillation counting instrument. It is performed
daily or prior to counting any samples - See Attachment 5.1, SNC Protocol
Printout, Example.
3.2.8 Detector Enclosure Area — The counting chamber in which samples drop
into for counting.
3.2.9 Reagent Water - Reagent water for tritium analysis shall be free of
detectable interferences and shall meet or exceed ASTM Type II
requirements in accordance with reference 2.9.

3.3 Responsibilities
3.3.1 Lead, Laboratory or designee, is responsible for the overall
implementation of this procedure and reviews all documents associated
with sample analysis and instrument calibration and maintenance.
3.3.2 Gamma Spectroscopy Specialist or designee, oversees the daily operations
of the onsite Radiological Laboratory, ensuring personnel coverage and
proper sample management and scheduling. In addition, the Gamma
Spectroscopy Specialist supervises the Gamma Spectroscopy Technician
in all sample prep performance as well as the analysis of samples prepped
for Radiological Analysis. Performs calibration and maintenance
operations on the Liquid Scintillation Analyzer. Provides technical
knowledge and assistance for ongoing site operations. Shall be responsible
for monitoring standards of performance and monitoring the validity of
analysis and the data generated to assure reliable data. This responsibility
will include technical direction and support for the day to day performance
of the laboratory operations described in this procedure.
3.3.3 Gamma Spectroscopy Technician performs sample preparation for
Radiological Analysis, documenting thoroughly the process. Assists the
Gamma Spectroscopy Specialist in calibration and maintenance operations
for the Liquid Scintillation Analyzer.

3.4 Precautions and Limitations
3.4.1 Compliance
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3.4.1.1 Personnel performing this procedure shall be qualified on
the tasks or activities contained in this procedure according
to CL-TN-PR-100, Clive Facility Training Procedure.
Those individuals not qualified according to CL-TN-PR-
100 may perform tasks within this procedure provided they
are operating under the direction of a qualified individual.

3.4.1.2 Annually a single blind sample should be evaluated using
the Packard Tricarb 2900TR or Perkin Elmer Tricarb
4910TR Liquid Scintillation Analyzer to verify the proper
functioning of the instrument.

3.4.1.3 Packard Tricarb 2900TR or Perkin Elmer Tricarb 4910TR
Liquid Scintillation Analyzer shall not be used to analyze
1 1 e. (2) Waste.
3.4.2 Safety

3.4.2.1 All personnel performing tasks within the Chemistry
Laboratory shall comply with the applicable requirements
of CL-SH-PR-150, Laboratory Chemical Hygiene Plan.

3.4.2.2 The methods and procedures described in this and other
documents related to the operation of the Packard Tricarb
2900TR and Perkin Elmer Tricarb 4910TR Liquid
Scintillation,Analyzer are designed to be performed by
trained personnel in a suitable workplace. Lab procedures
may involve hazardous materials and substances of
unknown toxicity. In order to safely and correctly perform
these activities, all standard safety procedures for sample
handling must be observed.

3.4.2.3 All unknown samples shall be considered both hazardous
and radioactive and shall be handled accordingly.

3.4.2.4 Beware of moveable parts and pinch points while
performing this procedure.

3.4.2.5 Instrument power supply shall be turned off during
maintenance

3.4.2.6 The appropriate PPE shall be employed when handling the
LSC cocktail. Follow the MSDS and manufacturers
guidelines for the handling and safety precautions of each
LSC cocktail used in accordance with this procedure.
3.4.3 Preservation and handling

3.4.3.1 The SNC Standard Set is stored within the Liquid
Scintillation Analyzer for ease of use for daily calibration
of the instrument.
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3.4.3.2 Quenched standard sets should be refrigerated to 4°C±2°C
for storage
3.4.3.3 Standards Solutions and LSC Cocktail should be stored
within appropriately marked chemical storage cabinet(s).
Note: LSC cocktail in current use may stay on countertop
within appropriate secondary containment, and
pipettor device.
3.4.3.4 See individual methods of detection for specific sample
collection, preservation and handling instructions.
3.4.3.5 Water samples should be collected in their natural state,
and should not be acidified. Since tritium in water is very
much apt to be in the form of T20 or HTO, there is no need
for special handling or preservation.
3.4.4 Scope of Matrices
3.4.4.1 This procedure applies to the detection of tritium on filter
paper and tritium within water and aqueous liquids.
3.4.5 Detection Limits
3.4.5.1 Refer to individual methods for the determination of
applicable detection limits of different nuclides.
3.4.5.2 Detection limits vary individually with each sample,
background, and counting time. Some of these parameters
may be altered to facilitate the needs of the requisitioning
department, with regards to detection limit.
3.4.6 Interferences
3.4.6.1 External background radiation: Although the counting
chamber is shielded, background gamma and x-ray
radiation can interfere with the instrument. Sources of
radiation should be stored at an appropriate distance from
the instrument or shielded.
3.4.6.2 Quenching: Quenching is anything which interferes with
the conversion of decay energy to photons emitted from the
sample vial. Quenching is the most prevalent interference
in liquid scintillation counting. The two types of quench are
color quench and chemical quench, and both types of
quench result in lowered efficiencies. Quenching is
corrected by the use of quench curves and other calibration
methods.
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3.4.6.3 Electrostatic discharge: A static charge can build up on
plastic vials when handled with gloves. This static
discharge can cause false pulse events during counting,
thereby increasing the reported activity. Electrostatic
discharge is corrected by using the Electrostatic Controller
option within counting parameters
3.4.6.4 Luminescence: The emission of light that is not attributed
to the temperature of the source is luminescence.
Luminescence is typically either chemiluminesence or
photoluminescence, and both of these cause false counts
when counting a sample. The Tricarb analyzer corrects for
most luminescence using the coincidence circuit, but the
user should be aware that very high incidences of
luminescence can cause false counts because of limitations
in the resolving time of the coincidence circuit.
3.4.6.5 Scintillation volume variation: Energy detection of
photons by the photomultiplier is decreased with a decrease
in fill volume of the cocktail. This is because efficiencies
vary across the face of the photomultiplier. As a minimum,
enough cocktail should be added to the vial to entirely
submerge the sample.
3.4.6.6 Writing on counting vial sides can block light that is
generated by decay events within the vial from getting to
the photomultipliers. A sample shall not be counted if there
is writing on the vial sides or bottom. The vial lid is the
only acceptable place to label a counting vial.
3.4.6.7 Slightly elevated levels are present in surface waters, so
deep well sources for background water should be used
when analyzing water samples.
3.4.6.8 All fluors (and LSC Cocktails) should be checked for
excitation under lighting conditions being used and if
necessary they should only be exposed to red light.
Dioxane-base scintillators exposed to fluorescent lighting
should be dark-adapted for 24-hours. All other cocktails
should be dark adapted as necessary.
3.4.7 Method Performance
3.4.7.1 Precision and accuracy for the detection of tritium in water
can be found in EPA 906 (See references for more
information).
3.4.8 Pollution prevention
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3.4.8.1 Solutions, standards and samples should be prepared in the
smallest volumes appropriate to the procedure and
consistent with the expected usage.

3.4.8.2 Waste disposal will be preceded by the segregation of
hazardous and non-hazardous materials.
3.4.9 Waste management

3.4.9.1 Contact waste is accumulated in marked containers and
periodically sent to the onsite mixed waste disposal facility
for treatment and disposal.

3.4.9.2 Non-contact waste is accumulated and sent to the onsite
waste disposal facility.

3.4.9.3 The handling and disposal of samples and waste materials
generated by the laboratory shall be performed in
accordance with CL-LB-PR-003, Sample control.
3.5 Records
3.5.1 The SNC documentation shall be reviewed (initial and dated) to ensure the
instrument is functioning properly. Quarterly, these documents shall be
transmitted to Document Control for storage and maintenance.
3.5.2 A Packard Tricarb 2900TR and Perkin Elmer Tricarb 4910TR
Preventative Maintenance Checklist, Example in Attachment 5.1, shall be
used to document the preventative maintenance operations performed on
the Packard Tricarb 2900TR and Perkin Elmer Tricarb 4910TR Liquid
Scintillation Analyzer.
3.5.3 Analytical data produced by the Packard Trcarb 2900TR and Perkin Elmer
Tricarb 4910TR shall be evaluated by the gamma spec specialist and
turned over to the requisitioning department for interpretation and use.
4 REQUIRMENTS AND GUIDANCE
4.1 Equipment and Supplies
4.1.1 Packard Tricarb 2900TR Liquid Scintillation Analyzer
4.1.2 Perkin Elmer Tricarb 4910TR
4.1.3 Counting vials
4.1.4 Cassettes
4.1.5 Protocol flags
4.1.6 Manufacturer recommended tools, to include Eye bolts and T-handles
4.1.7 Soapy water — mild detergent (i.e. Dawn®, etc.) and standard tap water
4.1.8 Static control solution (i.e. Windex®, Staticide®, etc.)
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4.1.9 Bottle Brush, dry, optional
4.1.10 Canned Air — specific for equipment cleaning
4.1.11 Lint free cloth or tissue
4.1.12 Distillation apparatus for aqueous liquid analysis

4.2 Reagents and Standards
4.2.1 Unless otherwise indicated, it is intended that all reagents shall conform to
the specifications of the Committee on Analytical Reagents of the
American Chemical Society, where such specifications are available.
Other grades may be used, provided it is first ascertained that the reagent
is of sufficiently high purity.
4.2.2 NIST traceable Self Normalization and Calibration set containing H-3, C-
14, and a background standard.
4.2.3 NIST traceable Quenched Standard Set.
4.2.4 NIST traceable Standards Solutions for target analytes (e.g. tritium).
4.2.5 LSC Cocktail (e.g. UltimaGold LLT, or equivalent).
4.2.6 Alcohol, methanol or ethanol, ACS grade, preferably anhydrous.
4.2.7 Reagent water.

4.3 Calibration and Standardization
4.3.1 The instrument manufacturer's guidelines and specifications for
calibration should be referenced when calibrating the Packard Tricarb
2900TR and Perkin Elmer Tricarb 4910TR.
4.3.2 When analyzing tritium activity in aqueous liquids, the following
calibration steps will be performed specific to this method:
4.3.2.1 Prepare the control standard
4.3.2.1.1 Combine reagent water and a tritium standard
solution in a glass beaker of sufficient volume to
generate 100m1 of 100dpm/m1 control stock
solution.
NOTE: Volumes and activity concentrations in
the control stock solutions are subject to
change at the discretion of the gamma
spec specialist.
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4.3.2.1.2
4.3.2.1.3
4.3.2.1.4
The control stock solution is then run through the
distillation process described in section 4.4.2 of this
procedure.
The distillate produced from the control stock
solution shall be counted as a set of at least four
separate vials.
The data produced by the set of four control stock
solution distillate samples shall be used to calculate
a distillation collection efficiency. This efficiency
shall be applied subsequent to the instruments
counting efficiency to the following batch of
samples.
NOTE: A distillation collection efficiency shall
be obtained for every batch of samples
being analyzed. Sample batch not to
exceed 10 samples.
4.4 Procedure
4.4.1 Calibration and operation
4.4.1.1 Calibration baseline establishment.
4.4.1.1.1
4.4.1.1.2
4.4.1.1.3
4.4.1.1.4
4.4.1.1.5
Baseline values shall be established for Self
Normalization and Calibration (SNC) before SNC
can be performed on the instrument - This needs to
be performed to determine acceptance criteria on all
SNC parameters.
Baseline values are typically only acquired when a
SNC source set expires and is replaced with a new
set or when other conditions change that would
warrant a change in SNC values (e.g. major
maintenance/repair, instrument location change,
natural decay of H-3 activity that causes too large of
a drop in observed H-3 efficiency etc.).
If the baseline values have already been determined
skip to step 4.4.2, otherwise proceed as follows:
Click the IPA tab and choose IPA definitions.
Ensure that the IPA parameters are correct and the
SNC is in the correct cassette carriers and position
within the instrument.
4.4.1.1.6 Click the reset baselines button.
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4.4.1.1.7 After all of the baseline data points have been
collected, the instrument will automatically set
limits on the efficiency and background. The only
parameter limit that the user will need to calculate is
the Figure of Merit threshold, FT. Calculated as
follows:
E FT = BL
Where:
EL=Efficiency limit (in IPA definition window)
BL=Background limit (in IPA definition window)

4.4.1.1.8 Once the figure of merit threshold has been
determined for both H-3 and C-14, enter these
values into the IPA Definition window.

4.4.1.1.9 The instrument is now ready for Self Normalization
and Calibration
4.4.1.2 Calibration self normalization calibration (SNC).

4.4.1.2.1 SNC shall be performed daily or with each use,
whicheveris less frequent.

4.4.1.2.2 Ensure that the working life on the SNC standards
has not expired.

4.4.1.2.3 Verify that the SNC standards are in the correct
position within the SNC cassette (The cassette is
labeled with these positions).

4.4.1.2.4 Reset the SNC protocol flag to the start position by
sliding the flag tab to the left.

4.4.1.2.5 Place the SNC cassette on the right side of the
sample changing deck and to the back.

4.4.1.2.6 Click the green flag start button with the mouse
cursor to start the count.

4.4.1.2.7 When the SNC has finished, review the SNC
protocol report to ensure the following parameters
have been met:
Parameter Acceptable Value
H-3 Efficiency > Mean baseline Eff. minus 3% _
C-14 Efficiency > Mean baseline Eff. minus 3% _
H-3 Background < Mean baseline BKG plus 4a
C-14 Background < Mean baseline BKG plus 4a
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H- 3 FOM (E2/B) As calculated in step 4.4.1.1.7
C-14 FOM (E2/B) As calculated in step 4.4.1.1.7
H-3 Chi2 7.63-36.19
C-14 C hi2 7.63-36.19
4.4.1.2.8 When the above items have been reviewed, initial
and date the SNC Protocol printout.
4.4.1.3 Calibration, establishment of quench curves
4.4.1.3.1
4.4.1.3.2
4.4.1.3.3
4.4.1.3.4
4.4.1.3.5
Perform quench curves at least annually for each
radionuclide that is quantified using them. To
establish a quench curve, proceed as follows:
Perform the SNC procedure, as outlined above.
Verify that the working life on the quench set has
not expired and load the cassette(s) with vials and
place the loaded cassette into the instrument.
NOTE: If the appropriate counting assay has not
been assigned to the protocol flag,
proceed as follows. Otherwise skip to
step 4.4.1.3.6.
Create a new assay, choosing Quench Standards as
the assay type and define the new parameters.
Associate (link) the assay parameters with a
protocol and attach the corresponding protocol flag
to the first cassette to be counted.
4.4.1.3.6 Ensure the flag has been activated and start the
count.
4.4.1.3.7 When count has finished and quench curves have
been plotted, review for accuracy and validity, then
proceed to associate the quench set curve to the
appropriate nuclide.
NOTE: If using an assay that was previously
created, verify that the quench curve has
been updated for associated nuclides.
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4.4.1.3.8 Select the 'Libraries-Sample Nuclides' Main menu
item. The sample nuclides window is displayed.

4.4.1.3.9 Click one of the Quench Set buttons to display the
Quench Standards window.

4.4.1.3.10 Select the Quench Set Low if you are counting one
nuclide in one counting region, the Quench Set
Medium if you are counting a second nuclide in a
separate region, and Quench Set High if you are
counting a third nuclide in a third region.

4.4.1.3.11 Select the name of the quench set you would like to
link to the sample nuclide.

4.4.1.3.12 Click OK and the name of the quench set(s) you
selected should appear in the Sample Nuclides
Library window on the Quench Set buttons.
4.4.1.4 Operate the Packard Tricarb 2900TR and 4910TR for
sample counting.

4.4.1.4.1 Perform the SNC as outlined in step 4.4.1.2.

4.4.1.4.2 Ensure appropriate volumes of liquid scintillation
cocktail have been added to each sample and place
samples in correct order into a cassette carrier.
4.4.1.4.2.1 If counting a filter paper enough
cocktail to completely submerge the
filter paper at a minimum is required.

4.4.1.4.3 If no assay exists for desired counting parameters,
proceed as •follows, otherwise skip to step 4.4.1.4.6.

4.4.1.4.4 Click FILE, NEW ASSAY and proceed to defme
the new assays counting parameters to align to those
needed for the sample analysis.

4.4.1.4.5 Associate assay to a vacant or unused protocol flag.

4.4.1.4.6 Attach appropriate protocol flag to the sample
cassette carriers and activate flag by sliding it to the
right.

4.4.1.4.7 Place loaded sample cassette carriers on the right
and to the back of instrument sample deck.

4.4.1.4.8 Close the lid of the instrument and, if necessary,
allow for dark adapt period.

4.4.1.4.9 Start the count by clicking the green flag on the
spectra view screen of the quantasmart® software.
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ter out
distillation head .--- te r in
0+=1
distillation flask ---_____------1°.
of-i--1-1
FT II-
tillation adaptor
1---1--c
rec eiving flask e. 1 J
c ordenser
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Liquid Scintillation Revision 2
4.4.1.4.10 Upon completion of the count, review the data for
accuracy and validity before turning over to the
requisitioning department.
NOTE: All used counting vials containing liquid
scintillation cocktail shall be
appropriately disposed of in the contact
waste receptacle.
4.4.2 Detection of tritium in aqueous liquids by distillation.

4.4.2.1 Add 0.5 g sodium hydroxide, 0.1 g potassium
permanganate, and a boiling chip to a 100-mL aliquot of
the sample and place into a boiling flask of sufficient
volume.

4.4.2.2 Assemble the distillation apparatus see below.
the nnometer
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4.4.2.3 Heat the sample to boiling to distill and discard the first 10-
mL of distillate as a separate fraction. (It is important that
the first 10 mL fraction for samples and standards alike be
discarded, since there is a gradient in the tritium
concentration of the distillate).

4.4.2.4 Collect the next 50 mL of distillate for tritium analysis and
mix thoroughly.

4.4.2.5 In 10-12m1 aliquots, distribute the mixed sample distillate
amongst at least four counting vials.

4.4.2.6 A laboratory control spike (LCS) shall be made and
counted with each sample batch.

4.4.2.6.1 An additional vial labeled "LCS" shall be filled
with a ratio of reagent water and liquid scintillation
cocktail matching that of the samples. A known
amount of activity of the target analyte shall be
added to this vial for QA purposes.

4.4.2.6.2 The LCS shall be loaded with the sample batch and
counted as an extra sample at the end of the sample
string.

4.4.2.7 If using PerkinElmer UltimaGold LLT as the LSC cocktail,
combine up to 12 mL distillate with up to 10 mL of cocktail
— adjust this ratio as necessary to keep counting conditions
optimum. If using another type of LSC cocktail,
manufacturer guidelines shall be followed.

4.4.2.8 Place samples into sample cassette carriers and into the
instrument to the back and right of the sample deck and
start the count in accordance with step 4.4.1.4.

4.4.2.9 Upon completion of the count(s), and before data is turned
over to the requisitioning department, the distillation
collection efficiency obtained from step 4.3.2.1.4 must be
applied to each samples activity value to correct for any
potential loss of the target analyte during distillation.
4.4.3 Maintenance of Packard Tricarb 2900tr and 4910TR.
NOTE: Maintenance may be performed by
Perkin Elmer personnel as service
contracts are in place.

4.4.3.1 Login as the Technical Service Engineer (TSE) user to
obtain access to diagnostic mode:

4.4.3.1.1 On the windows taskbar, click Start, Shutdown, and
then Restart.
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4.4.3.1.2 When the Windows startup screen appears, press
ctrl, alt, delete to bring up the login window.

4.4.3.1.3 Enter TSE' as the login and 'meriden' as the
password (both fields are case sensitive).

4.4.3.2 Run the SNC as outlined in step 4.4.1.2.

4.4.3.3 Review the H-3 and C-14 Efficiencies, Backgrounds, and
Figure of Merit values and record these values on the
Preventative Maintenance Checklist.

4.4.3.4 Record the DAC Values found in TSE diagnostics on the
Preventative Maintenance Checklist.

4.4.3.5 View the error log in TSE diagnostics.
4.4.3.5.1
4.4.3.5.2
4.4.3.5.3
Examine the log for potential problems with the
instrument. Contact the manufacturer for repair
guidelines if necessary to resolve errors.
Record the number of elevator cycles.
Reset the cycle counter and the error log.

4.4.3.6 Check the functionality of the cassette sensors from within
the TSE diagnostics by depressing each of eight levers and
ensuring the corresponding light on the monitor is
activated.

4.4.3.7 Shutdown windows, power the instrument off, and unplug
all power sources and components.

4.4.3.8 Open and remove instrument lid
4.4.3.8.1
4.4.3.8.2
Disconnect the lift struts from the lid by popping
them off the ball studs that hold them on.
Remove the screws that hold the lid hinges to the
instrument rear and lift and remove lid from the
instrument.

4.4.3.9 Clean both sides of the instrument lid with a static control
solution.

4.4.3.10 Lift the sample changer deck.

4.4.3.10.1 Ensure the sample elevator is in the full down
position.

4.4.3.10.2 Remove the ball studs and brackets located at the
rear of the sample changer deck.

4.4.3.10.3 Remove the plastic vial storage tray from the center
of the sample changer deck.
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4.4.3.10.4 Ensure that the shipping screw securing the front of
the sample changer deck has been removed.

4.4.3.10.5 Obtain T-handles and thread them clock-wise into
the holes in the sample changer deck
simultaneously until the deck begins to rise (These
are the two holes, located about three-quarters to the
rear of the sample changer deck).

4.4.3.10.6 Manually lift the sample changer deck with the T-
Handles until the underside of the deck will clear
the front of the instrument body. Move the deck
forward, and allow it to rest on the front of the
instrument body and on the rear drive motor
brackets.

4.4.3.10.7 Clean the sample changer deck with static control
solution.
4.4.3.11 Clean and inspect the counting Chamber.
4.4.3.11.1
4.4.3.11.2
Thread eyebolts into the lead shield lids and lift
them out of the instrument.
Carefully lift the counting chamber out of the lead
base. As this is done, the springs that hold the tubes
in the chamber should come out.

4.4.3.11.3 Disconnect the photomultiplier tube ground strap
from the mounting stud.

4.4.3.11.4 Slide the photomultiplier tubes out of the housing
and place them in a safe location.

4.4.3.11.5 Slide the Reflectors out and clean them with soapy
water.

4.4.3.11.6 Clean the lead base.

4.4.3.11.7 Clean the faces of the photomultipliers with alcohol
and a lint-free cloth or tissue.
4.4.3.12 Elevator assembly inspection

4.4.3.12.1 Remove the front panel of the instrument.

4.4.3.12.2 Adjust the elevator until the elevator is accessible
by using the brass counter-weight.

4.4.3.12.3 Inspect, clean or replace the elevator spring,
pedestal, light seal rings, elevator body, the detector
enclosure area, and the fan filter
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4.4.3.13 Clean the static-controller with a dry bottle brush or canned
air.

4.4.3.14 Clean the sample load area and inspect the shutter light
seal.

4.4.3.15 Clean the optical readers with alcohol and a lint-free cloth
or tissue.

4.4.3.16 Inspect the barium source.

4.4.3.16.1 Remove the front of the elevator drive assembly and
turn the elevator drive clock-wise to release the
source.

4.4.3.16.2 Pull the source from the elevator.

4.4.3.16.3 Because the source moves in and out of the
counting chamber, uneven wear can occur over time
- rotate the source if necessary.

4.4.3.16.4 Reinsert the source into the back of the drive using
a fold of paper as a channel. This will keep the
spring straight in order to feed it into the brass tube.
Replace the front elevator drive assembly and lock
the elevator spring in position.

4.4.3.17 Check mechanical adjustments within the sample changer
deck.

4.4.3.17.1 Inspect hardware, ensuring that nothing is loose or
out of place.

4.4.3.17.2 Obtain a 15 ml cassette with a protocol plug
inserted into the end.

4.4.3.17.3 Manually move the cassette across the transfer end
(front) of the sample changer deck, verifying that
the cassette does not bind up.

4.4.3.17.4 Move the flag to the count position and repeat this
check on the load-end (rear) of the instrument.
Verify that the flag actuator changes the flag to the
off position and that the transfer of the cassette is
bind-free.

4.4.3.17.5 Visually inspect the shutter, ensuring that the
shutter sensors are not in contact with the shutter
when the shutter closes. This can be done by
manually moving the shutter from underneath.
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Revision 2

4.4.3.17.6 Turn the elevator to the full load position and verify
that a slight resistance is felt as the drive pin is
released from the fork.
4.4.3.18 Reassembly.

4.4.3.18.1 Reinsert the reflectors into the chamber while lining
the pins and holes up.

4.4.3.18.2 Slide the photomultiplier tubes into the housing.

4.4.3.18.3 Place the housing into the lead base. Ensure that the
cables are in the slot so they are not pinched when
the shield lid is replaced.

4.4.3.18.4 Reattach the ground cable.

4.4.3.18.5 The springs should be replaced so that the small end
is pointed toward the lead base.

4.4.3.18.6 Reinstall the lead, starting with the two outside
pieces.

4.4.3.18.7 Ensure that the cables will not obstruct the sample
changer deck when it is lowered.

4.4.3.18.8 Move the sample changer deck over the load hole.

4.4.3.18.9 Carefully lower the deck by twisting the T-Handles
counter-clockwise. As this is done, monitor the
alignment of the load hole.
4.4.3.18.10 The deck will not rock when lowered properly.
Rocking usually is caused by the deck resting on a
misplaced cable.

4.4.3.18.11 Reinstall the brackets that secure the sample
changer deck at the rear of the instrument.

4.4.3.18.12 Replace the lid and secure the hinges to the rear of
the instrument.

4.4.3.18.13 Reinstall the lift struts with the widest part of the
shaft connected to the lid.

4.4.3.18.14 Inspect the sample cassettes and replace any that are
broken. Broken cassettes can damage the
instrument.
4.4.4 Power the instrument up and login using 'TSE' as the login.
4.4.5 Using TSE diagnostics, verify that each cassette sensor around the sample
changer deck is functional by pressing each sensor and viewing the
response on the Sample Changer Tab.
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4.4.6 Use the Sample Changer Action option to check mechanical operations of
the sample changer. Cycle a cassette clockwise then counter clockwise to
ensure that the sample changer is mechanically operational.
4.4.7 Verify that the optical reader is operational.
4.4.8 Restart the computer and login using appropriate credentials.
4.4.9 Perform the SNC calibration function, and review the data in accordance
with step 4.4.1.2 of this procedure.
4.4.10 Review the H-3 and C-14 Efficiencies, Backgrounds, and Figure of Merit
and record these values on the Preventative Maintenance Checklist.
4.4.11 Complete the remainder of the Preventative Maintenance Checklist, attach
a copy of the before and after SNC Protocol sheets and forward
documentation to the Gamma Spec Specialist for review and approval.

4.5 Quality control
4.5.1 The distillation collection efficiency is designed to calculate and correct
for potential loss of target analyte during the distillation process. As such,
there is no acceptance range for the values these standards produce.
4.5.1.1 Due to the variance of matrix in which an aqueous liquid
may manifest, care should be taken to mimic the sample
matrix as much as feasible when building the control stock
solution set.
4.5.2 The observed activity of the LCS shall fall within ±10% of the NIST
traceable activity.

4.6 Corrective Actions for Out-of-Control Data.
4.6.1 Instrument warnings should be investigated and corrected using
manufacturer guidelines and specifications. The appropriate recalibration
steps shall be performed if correcting instrument warnings justifies doing
so.
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4.6.2 Out of control LCS/quenched standard activities shall be recounted. If the
recount fails, a new LCS/ quenched standard will be obtained or made.
The instrument shall be recalibrated as necessary if the new LCS fails to
fall within +/- 10% of the NIST traceable activity.
4.6.3 Data gathered during an out-of-control analytical sequence will not be
reported without clearly indicating that the analysis was out-of-control and
that the results should be considered as estimated.
5 ATTACHMENTS AND FORMS.
5.1 CL-LB-PR-133 F1 Packard Tricarb 2900TR and 4910TR Preventative
Maintenance Checklist, Example.
5.2 SNC Protocol Printout, Example.
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Attachment 5.1 - CL-LB-PR-133-F1,
Packard Tricarb 2900TR Preventative Maintenance Checklist, Example

CL-LB-PR-004-F1
Rev 0 ENERGYSOLUTIONS
PACKARD TRICARB 2900TR AND 4910TR MAINTENANCE
DOCUMENTATION SHEET
Serial number Cycles Logged Date
Self Normalization and Calibration Information
(Attach Printouts)
Before Maintenance After Maintenance
Efficiency 3H 3H
14C 14C
Background 3H 3H
14C 14C
Figure of Merit 3H 3H
14C 14C
DAC # L L R R
Inspected and cleaned (if applicabk):
Instrument lid
Sample changer deck
Photomultiplier faces
Reflectors
Lead shielding and base
Elevator spring assembly
Light seal rings (elevator body) Barium Standard
Detector enclosure area
Optical readers
Cassettes
Fan filter
Static controller
Elevator pedestal
Instrument exterior

Mechanical Operation checks Load-end cassette movement All hardware for tightness
Transfer-end cassette movement Shutters
Protocol plug and flag actuators _Sample changer Belt tension Elevator
All sensors
Notes
Next Maintenance Due:
Perfonned by Date.
Reviewed by Date:
Page 1 of 1
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Attachment 5.2 - SNC Protocol Printout, Example
11/10/06 8:47:59 AM Qaaategaart erbel - 1.31 - Serial* 422422 Page # 1
WC Protocol
Calibration Information Software Version IC: 2.11 Software Version EC: 1.31
Instrument Model: A250000 Instrument Serial Number: 422422
3H Chi Square: 18.97 Date Processed: 11/10/06 8:47:59 AM 14C Chi Square: 26.09 Date Processed: 11/10/06 8:47:59 AM 3H E'2/H (1-18.6 keV): 235.43 Date Processed: 11/10/06 8:47:59 AM 14C EA2/13 (4-156 keV): 390.48 Date Processed: 11/10/06 8:47:59 AM 3H Efficiency (0-18.6 keV): 68.11 Date Processed: 11/10/06 8:47:59 AM 14C Efficiency (0-156 keV): 96.40 Date Processed: 11/10/06 8:47:59 AM IPA Background Date Processed: 11/10/06 8:47:59 AM 3H Background CPM (0-18.6 keV): 19.17 Date Processed: 11/10/06 8:47:59 AM 14C Background CPM (0-156 keV): 29.68 Date Processed: 11/10/06 8:47:59 AM 3H Calibration DPM: 279000 3H Reference Date: 3/9/06 14C Calibration DPM: 143100
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DOCUMENT SUMMARY FORM
Please provide the following information for newlrevised documents.
Forward the completed form, approved document, and electronic file, to Document Control.
Document No.: CL-LR-PR-133 Revision No.: 2

Title: Liquid Sdntrtllation
Special Status (i.e. Restricted; SSI; etc.): N/A
If special status is applicable, please note any special distribution/handling requirements:
Summary of changes (if this is a revision):.
Addition of new instnunent reference, various formatting changes.
Yes El No
E] Yes El No
This document requires evaluation per the requirements of a license. If yes,
attach evaluation results.
This document requires regulatory agency approval before implementation. If
yes, contact Document Control.
Distribution (or changes to distribution) for controlled copies of this document.
Source: ES-AD-PR-001, Rev.7, Document Preparation [Attachment 5.4]
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