Calibration Copy Working - TIAERtiaer.tarleton.edu/transfer/Shepherd/QAM-RI-107rev... · QAM-RI-107...

QAM-RI-107

Operation and Calibration of the

Canberra Alpha Analyst Spectrometer

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QAM-RI-107 Operation and Calibration of the Canberra Alpha Analyst Spectrometer

Rev.0 of 12 TIEAR

1.0 Applicability and Purpose

A. This procedure applies to the operation and calibration of the

Canberra Alpha Analyst Spectroscopy system using Apex

Alpha and Genie 2000 software in the TIAER Laboratory at

Tarleton State University, Stephenville, Texas. The procedure

outlined in this text ensures that there is consistency between

trained analysts to produce accurate and precise data of high

quality. In performing these calibration and confirmation steps

the analyst reduces anomalies caused by instrument sensitivity,

interference and fluctuations.

B. Principals of alpha spectroscopy: Alpha emitting sample

sources are placed on the sample holders arranged in certain

geometries in the alpha spectrometer and a vacuum is pulled

on the spectrometer chambers. When alpha particles are

emitted by the sample, the alpha detectors produce electronic

signals that are analyzed by the MCA (multi-channel analyzer)

to generate a digital spectrum equivalent to the energy of the

alpha particles. The spectrum is then analyzed by computer

software that identifies and quantifies the alpha energies.

C. Operation summary: The alpha spectrometer is set-up and

ready for operation. The pulser and background checks are

performed, and the instrument is calibrated on a continuing

basis. For operation of the instrument performance

measurements of the continuing quality control standards,

spikes, duplicates and blanks are analyzed with each sample

batch.

D. Alpha-emitting radionuclides (or their short-lived decay

progeny) on the sample test sources may contaminate analyzer

chambers. The contaminants may emit alpha rays with peaks

at energies that cannot be adequately resolved from the tracers

or analytes of following sample test sources. The contaminants

are checked and removed before sample analysis with proper

instrument maintenance and sample preparation steps.

2.0 Definitions

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A. Refer to QAM-R-100, “TIAER Laboratory Radiochemistry

Program” for general radiological terms

B. FWHM- Full Width Half Maximum- the point on a spectral peak

where the surrounding area is most effectively calculated

C. ROI- Range of Interest- viewing area for energy peaks

D. MDC- Minimum Detectable Concentration

3.0 Equipment and Reagents

A. Computer with Apex Alpha and Genie 2000 software B. Alpha Analyst Spectroscopy system with multiple chambers C. Vacuum pump D. NIST traceable standard sources, Echert & Ziegler 7400-SRC

containing 234U, 238U, 239Pu, and 241Am, or equivalent

4.0 Procedure

A. The analyst is trained in accordance with QAM-Q-107 and approved by the RSO and LM to operate the instrument. All other aspects of the Quality Assurance Manual are followed.

B. Instrument start

1. Power on the instrument and computer.

2. Start Apex software and log on.

3. Make sure vacuum pump is on and working properly before

starting operation of the instrument.

C. Pulser check and detector background check:

1. Pulser check

a. Click on the “Sample Assigner” tab. Select detectors for

pulser check.

b. Click on the “Pulser Check” button.

c. Click on the “Load Samples” button. A screen with the list

of detectors will appear. Click on “OK”. The pulser count

will start for each available detector. The count time is 5

minutes. To view the pulsers, click on the “Main” tab. After

the pulsers have finished counting, click on the “Reports”

tab.

d. In the “Reports” window, click on the “QA Summary

Report” tab.

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e. Select the Pulser button then click on the “Check All”

button.

f. Click on the “View” button to get the pulser report on the

screen.

g. If needed, print the pulser report, or export to an electronic

file and obtain the required approval.

2. Detector background check

a. Click “Sample Assigner” tab, select detectors for

background check.

b. Click on the “Background Check” button.

c. Click on the “Load Samples” button. A screen with the list

of detectors will appear. Click on “OK”. The background

check count will start for each available detector. The

count time is 30 minutes.

d. After the background check has finished counting, click on

the “Quality Assurance View” tab and click on "Charts and

Reports". Select chamber and geometry, select

“Background Check”, and select the report of “Last

Measurement” to see the last check, or “Control Chart” to

see the chart graph. If the data are out of control limits,

investigate the reason, take correction action and

documented it.

e. Print out or save the check results and file.

f. Record results on the control chart for the detector and

geometry used.

g. Every control chart has a warning limit (2σ) and an action

limit (3σ). The LM is notified when the data are out of

warning limit, and a Corrective Action Report generated

when the data are out of control limit. The control chart is

established based on all data accumulated from an

assigned date to present (See QAM-Q-100).

D. Initial calibration 1. Calibration is performed upon initial set-up, after major

repair or service, or when QC results indicate the need to

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reestablish operating parameters for each chamber of the instrument. The calibration is performed on each shelf of each detector chamber that is used. These geometries are recorded in the Alpha Spec Log (attachment 1). The energy range of the spectrometry system is set to at least include the region between 3 and 8 MeV. Before initial calibration, the analyst performs a pulser check and detector background check to ensure the instrument is operating normally.

2. Use the NIST traceable source, Echert & Ziegler 7400-SRC to calibrate.

3. Click “Sample Assigner” tab. Select Calibration and choose combined calibration. Drag source 7400-SRC into the assigned chamber. Choose the appropriate geometry shelf. Place the standard source in the chamber and double check to ensure the computer file assignment matches the geometry. Start counting. The count time is 60 minutes. Calibration can also be performed from “Calibration” table.

4. Upon completing the calibration a calibration report is printed out and stored electronically. For geometry at shelf 2 the centroid error for energy calibration should be less than 2 (6 KeV) channel, the FWHM should be less than 33 channels (100 KeV), and the efficiency should be between 17% and 25%.

E. Continuing calibration check

1. After calibration the instrument is routinely checked before and after each batch using standard sources to ensure the instrument operating conditions are (1) acceptable for analysis of sample test sources and (2) equivalent to those to be established during calibration.

2. The continuing calibration check results are compared to control charts and tolerance limits. Data out of control limits are investigated, documented and corrective action may be needed. The continuing calibration checks include calibration check and background subtraction count. The background subtraction count is performed daily. Before continuing instrument quality check, perform pulser check and detector background check to ensure the instrument is operating normally.

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3. Calibration check

a. Click “Sample Assigner” tab, select detectors to be checked for calibration.

b. Click on the “Calibration Check” button. Drag the 7400-SRC source to the appropriate chamber and geometry described on the screen.

c. Click on the “Load Samples” button. A screen with the list of detectors will appear. Place the standard source in the corresponding chamber and shelf. Click on “OK”. The calibration check count will start for the loaded detectors.

d. After the calibration check has finished counting, click on the “Quality Assurance View” tab and click on "Charts and Reports". Select chamber and geometry, select “Calibration Check”, and then select the report of “Last Measurement” to see the last check, or “Control Chart” to see the chart graph.

e. Data that are out of warning limits are investigated and the LM is notified. A CAR is generated when data are out of control limits.

f. Special attention is paid to instrument efficiency data

(CPM, the element activity) which directly influences the analytical data accuracy. Any corrective actions are documented with a CAR.

g. Print out and electronically store the check results and file.

F. Background subtraction count 1. The background subtraction count, or the system

background count, is used for sample analysis data correction.

2. Use a blank planchet of the same type that is used for making samples or test sources for counting. The geometry of a background subtraction count is the same as that used for counting samples or sources.

3. Before starting, ensure the system background procedure is set to the "ROI directed" count mode and the ROI should be the same as that of the target analytes.

4. Click “Sample Assigner” tab, select detectors to be checked for background subtraction count.

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5. Click on the “System Background Count” button. 6. Click on the “Load Samples” button. Choose the

appropriate geometry (i.e. “Shelf 2”, “Detector 1”), Place the blank planchet in the chamber at the required shelf.

7. A screen with the list of detectors to be counted will appear. Click on “OK”. The system background check count will start. The count time is 1000 minutes.

8. After the background subtraction count has finished counting, click on the “Quality Assurance View” tab and click on "Charts and Reports". Select chamber and geometry. Select “System background count”, and then

select the report of “Last Measurement” to see the last background subtraction count results, or “Control Chart” to see the chart graph. If the data are out of control limits, investigate the reason, take correction action and document and/or notify the LM.

9. Print out the check results and store electronically. The data are

used for sample count data correction.

G. Creating an analytical batch

1. Click on the “Batch” tab, enter Batch ID. The format of batch

ID is month-date-year-number. For example, the batch ID of

the first batch created on January 14, 2017 should be Jan-14-

17-001. Input batch description, select sample matrix, input

sample number (unknowns), select QC samples included,

select procedure (for Uranium, select Uranium 60 or Uranium

120; for Americium, select Americium 60 or Americium 120,

etc.), input sample amount, tracer amount, and QC spike

amount etc. An existing Batch may be copied, then assigned a

new ID for the batch and edited.

2. Click “Next”, to next page. Input information of each sample

including QC samples to create sample list in the Batch.

When inputting duplicate and spike samples, right click the

mouse to assign the sample to be spiked or duplicated. After

input each sample, click “Update Sample” to save it. After all

samples are inputted, click “Save” to save the Batch.

H. Sample analysis

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1. Load samples (or background planchets) for counting in

calibrated detectors.

2. Click on the “Sample Assigner” tab, click “Queued Batch”, and

select the Batch to run. Assign each sample in the batch to a

chamber.

3. Click “Load Sample”, vent chambers, and load samples into

the corresponding chambers with calibrated geometries.

4. Click “OK”, a sample run log table will show up. Print the

sample run log table for filing. Carefully review the sample run

log to ensure each sample is placed in correct chamber and

geometry. Press “OK” to start counting.

5. Double check the sample ID and the chamber ID to ensure

they agree with the run log table.

I. Data review

1. Click on the “Data Review” tab, Click “Batch ID” on the search

type box. Type the batch number for samples to be reviewed,

select procedure used by the batch, click "search now" to get

the batch. You can use procedure to find batch ID from

procedure too. To do so, select procedure, assign the date

filter (date start and date end), click "search now" to list the

batches associated with this procedure, select the one you

want.

2. Check the batch number in the search results window to list

the samples to be reviewed, click the “Next” button located on

the bottom right of the data review page. A spectrum of the

highlighted data file (on the up-right box) is shown.

3. Review the regions of interest (ROI) to determine if they are

within specification.

4. The ROIs associated for each isotope may be adjusted at one

time using the “Shift All ROIs” slide bar or the left marker may

be adjusted using the “Shift only Left Markers” slide bar. If the

ROIs are acceptable, click on the “Update ROI”, and

“Reanalyze”.

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5. If the ROIs created are not acceptable, they may be adjusted

manually in the review box. If this approach is taken, each ROI

that requires adjustment must first be deleted by clicking on the

“delete ROI” button. Then the new ROI is set by adjusting the

left and right markers and clicking on the “Add ROI” button.

The ROIs are updated by clicking on the “Update ROI” button.

Once the ROIs have been updated, click on the “Reanalyze”

button.

6. From "View" click on the "report" button to review the report on

screen. Check the chemical recovery factor. It should be >

75% and <125%. If the data are acceptable, add any

comments on this sample by click on "Enter comments" button

when needed, then click on the “Approved” button. The

following important items are reported in the report: sample

and count information, chemical recovery factor, sample

activities of tracer and analytes and their relative errors

(uncertainty), MDCs and their errors of analytes, FWHM of

each peak. The percent recoveries of lab control spike and

matrix spike are also included in the reports of QC samples.

7. Click on the “Print Report” button. A print option screen will

appear. Select "Print Report" option, click "OK". A hard copy

of the report will be printed. Save a copy electronically in the

assigned folder.

8. Repeat the above steps to review the next sample. Repeat

this process until the review of all the samples in the batch is

completed.

9. Review the QC results: click on the “Quality Assurance View”

tab and select "chemistry". Select the type of QC (spike,

duplicate, unknown etc.), then select sample matrix and

element. Select the report of the “Last Measurement” to see

the "RPD" (relative percent difference) of last duplicate, or

"RPR" (relative percent recovery) of last spike, or chemical

recovery of last unknowns. Select "control chart" to see the

QC data chart. If the data are out of control limits, investigate

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the reason, take correction action and document with a CAR.

To see total QC results and control chart in a period of time,

select "Full Report" and define the start and the end dates.

10. If no QC information was entered in the batch, e.g. the QC

samples are treated as normal samples, the QC results may

be manually calculated.

5.0 Quality Control and Safety Aspects

A. All aspects of this procedure comply with QAM-Q-101,

“Laboratory Quality Control”, QAM-S-101, “Laboratory Safety”,

and QAM-R-100, “TIAER Laboratory Radiochemistry Program”.

Only personnel properly trained and authorized by the LM and

RSO are allowed to perform this procedure. Area swipes for

loose surface contamination are performed per S-101 and R-100.

B. All data are documented and maintained in accordance with,

QAM-A-102, “Document and Data Control”. All raw data are

recorded in the appropriate logbook or E-log.

C. Waste is handled and disposed of in accordance with QAM-W-

101, “Disposal of Laboratory Waste”. All waste from this

procedure should initially be considered radioactive.

D. Any sample or standard test source is removed from detector

chamber after counting to prevent contamination.

E. Any part in the detector chamber, such as test source supporter

and shelf regulator, should not be left outside the chamber.

F. To prevent damaging or contaminating detectors, the door of

each detector is kept closed at all times except when loading or

unloading the test sources or samples.

G. Current activities for source checks are found in the Calibration

Source Log, Q-102-4. Document source ID and source dates.

H. Ensure that the instrument has been calibrated prior to use.

I. Always take into account background radiation levels and record

the most recent with all data. Measure and record background

radiation levels in the appropriate logbook or E-log. Background

values must be within +/- 20% of the initial background average

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used for calibration. Measurements must fall within +/- 20% of the

initial average used for Quality Control.

J. During operation internal components contain live voltage. Turn

the instrument OFF, unplug coax cable and allow it to sit for one

minute before accessing internal components.

K. The connector contains voltage exceeding 1kV. Contacting it

during operation may result in electric shock.

L. Follow all safety precautions outlined in QAM-S-101 when

working with radioactive samples.

M. System background checks for each tray and geometry used are

performed at least weekly and recorded in the log.

N. Perform alpha and beta source Calibration Source check

measurements daily using a consistent location and geometry.

O. Standard test sources and sample test sources are radioactive

and must be handled with care. After counting the test sources

must be placed in their containers.

P. Safety glasses, gloves, and lab coats are recommended personal

protective equipment when handling samples.

Q. Staff members wear radiation dosimeters and a Geiger counter is

available to monitor the workplace.

R. Annual HazCom and safety training is performed in accordance

S-101 and R-100.

6.0 References

A. User's manual of Canberra Apex-Alpha Spectroscopy Software Suite.

B. Operation manual of Canberra Genie 2000.

C. ASTM D7282 “Standard Practice for Set-up, Calibration, and Quality Control of Instruments Used for Radioactivity Measurements,” ASTM Book of Standards 11.02, current version, ASTM International, West Conshohocken, PA

7.0 Attachments

A. Alpha Spectrometer Log, RI-107-1 (example)

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Attachment A

Alpha Spectrometer Log (example)

Instrument ID

Analysis Date

Analyst Source ID Background Date

Background Results

Tracer ID Prep Date Batch ID Comments

Attach printed copies of QC Analytical Batches and QC results

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