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Title Standard Operation Procedure for Canberra Alpha Spectrometer Revision No. Revision date:

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Standard Operation Procedure for Canberra Alpha Spectrometer

Approvals: Prepared by: _Tianmin Xie_______________ Date: ________________ Reviewed by: _________________________ Date: ________________ Approved by: _________________________ Date: ________________

Document ID Approval

Title Standard Operation Procedure for Canberra Alpha Spectrometer Revision No. Revision date:

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1.0 Scope and Application 1.1 This SOP is for operating Canberra alpha spectrometer to acquire and analyze alpha spectra. 1.2 This SOP is to ensure correctly and safely using the Canberra Alpha spectrometer for providing alpha radiation measurement with stated quality. 2.0 Summary of Method and Interferences 2.1 Principal of alpha spectrometer: Alpha emitting sample sources are placed on the sample holders in the alpha spectrometer and a vacuum is pulled on the spectrometer vacuum 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. 2.2 Operation summary: The alpha spectrometer is set-up and ready for operation. The pulser check and background check were performed, and the instrument is calibrated. The instrument is then ready for counting sample. For continuing operation of the instrument perform the continuing quality control testing before sample counting. 2.3 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 must be checked and removed before sample analysis. 3.0 Reagent and supplies 3.1 NIST traceable standard sources, Echert & Ziegler 78127-251 containing 234U, 238U, 239Pu, and 241Am. 3.2 NIST traceable standard sources, Echert & Ziegler 78541-121 containing 234U, 238U, 239 Pu, and 241Am. . 4.0 Equipment 4.1 4.2 4.3 Dell PC Workstations or equivalent. Canberra Alpha Spectrometers with multi-chamber detectors. Vacuum pump. 2

Document ID Approval

Title Standard Operation Procedure for Canberra Alpha Spectrometer Revision No. Revision date:

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5.0 Standardization, Calibration and Quality Assurance 5.1 The analyst must be trained before operate the alpha spectrometer. The training consists of: study of this operation procedure, general instruction of the instrument and the software, instruction of basic instrument operation and sample analysis. 5.2 Initial calibration Perform calibration upon initial set-up, after major repair or service, or when QC results indicate the need to reestablish operating parameters for each chamber of the instrument. The calibration is performed on each shelf of each detector chamber. The energy range of the spectrometry system should at least include the region between 3 and 8 MeV. Before initial calibration, perform pulser check and detector background check to ensure the instrument is normal.
Note: make sure vacuum pump is on and working properly before start operating the instrument.

5.2.1 Pulser check and detector background check: 5.2.1.1 Pulser check 5.2.1.1.1 Click on the Sample Assigner tab. Select detectors for pulser. check. 5.2.1.1,2 Click on the Pulser Check button. 5.2.1.1.3 Click on the Load Samples button. A screen with the list of detectors will appear. Click on OK. The pulsers 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. 5.2.1.1.4 In the Reports window, click on the QA Summary Report tab. 5.2.1.1.5 Select the Pulser button then click on the Check All button. 5.2.1.1.6 Click on the View button to get the pulser report on the screen. 5.2.1.1.7 If needed, print the pulser report and complete the required approval. 5.2.1.2 Detector background check 5.2.1.2.1 Click Sample Assigner tab, select detectors for background check. 5.2.1.2.2 Click on the Background Check button. 5.2.1.2.3 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. 5.2.1,2.4 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 3

Document ID Approval

Title Standard Operation Procedure for Canberra Alpha Spectrometer Revision No. Revision date:

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are out of control limits, investigate the reason, take correction action and documented it. 5.2.1.2.5 Print out the check results and file it.
Note: Every control chart has a warning limit (2) and an action limit (3). An investment should be taken when the data are out of warning limit, while a corrective action should be taken when the data are out of control limit. The control chart is established based on all data accumulated from an assigned date to present.

5.2.2 Initial calibration 5.2.2.1 Use NIST traceable sources, Echert & Ziegler 78127-251 and 78541-121 to calibrate. Note, the 78127-251 source is used exclusively for all A chambers (up row chambers), and the 78541-121 source is used exclusively for all B chambers (low row chambers). Both sources contain 234U, 238U, 239 Pu, and 241Am. 5.2.2.2 Click Sample Assigner tab. Select Calibration and choose combined calibration. Drag source 78127-251 into the A chambers and source 78541121 into the B chambers. Choose Geometry shelf 2, Place the standard source in the chamber at the required shelf. Start counting. The count time is 60 minutes. Calibration can also be performed from Calibration table. 5.2.2.3 Upon completing the calibration a calibration report will be printed out. File it to the document holder. 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% to 25%. 5.3 Continuing instrument quality check After calibration the instrument is routinely checked using standard source 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. The continuing instrument quality control results are compared to control charts and tolerance limits. Data out of control limits should be investigated, documented and corrective action may be needed. The continuing instrument quality control checks include calibration check and background subtraction count. The calibration check is performed not less than once every three months or QC results indicate there is a potential instrument calibration problem. The background subtraction count is performed every three months, or background check (5.2.1.2) indicates that there is a potential instrument contamination existing. Before continuing instrument quality check, perform pulser check and detector background check to ensure the instrument is normal. 5.3.1 Pulser check and detector background check: See 5.2.1. 5.3.2 Calibration check 4

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5.3.2.1 Click Sample Assigner tab, select detectors to be checked for calibration. 5.3.2.2 Click on the Calibration Check button. Drag source 78127-251 into the A chambers and source 78541-121 into the B chambers. 5.3.2.3 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. 5.3.2.4 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. Data are out of warning limits should be investigated; while corrective action should be taken when data are out control limits. Special attention should be paid to instrument efficiency data (CPM, the element activity) which directly influent the analytical data accuracy. The corrective action should be documented. 5.3.2.5 Print out the check results and file it. 5.3.3 Background subtraction count Background subtraction count, or the system background count, is used for sample analysis data correction. Use blank planchet that is used for making sample test source for counting. The geometry of background subtraction count must be the same as that used for counting sample test source. Before start, check the system background procedure in the QA procedure, it should use "ROI directed" count mode and the ROI should be the same as that of the target analystes. 5.3.3.1 5.3.3.2 5.3.2.3 Click Sample Assigner tab, select detectors to be checked for background subtraction count. Click on the System Background Count button. Click on the Load Samples button. Choose Geometry shelf 2, Place the blank planchet in the chamber at the required shelf. 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 minute. 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 documented it. 5

5.3.3.4

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5.3.3.5
Note: 1. 2. 3.

Print out the check results and file it. The data are used for sample count data correction.

To prevent damaging or contaminating detectors, the door of each detector must be kept closed all the time. It is only opened when loading or unloading the test sources. Any sample test source or standard test source must be removed from detector chamber after counting to prevent contamination. Any part in the detector chamber, such as test source supporter and shelf regulator, should not be left outside the chamber.

6.0 Safety precautions 6.1 Standard test sources and sample test sources are radioactive and must be handed with care. After counting the test sources must be placed in their containers. 6.2 Safety glasses, gloves, and lab coats are required personal protective equipment. 6.3 Staff members wear radiation dosimeters and a Geiger counter is available to monitor the workplace. 6.4 Annual HazCom safety training is performed. Disposal of test source waste must follow radio safety officer's instruction. 7.0 Procedure 7.1 Instrument start Start Apex software and log on. 7.2 Perform daily pulser check and detector background check (see 5.2.1) 7.3 Create analytical batch 7.3.1 Click on the Batch tab, enter Batch ID. The format of batch ID is month-dateyear-number. For example, the batch ID of the first batch created on January 14, 2010 should be Jan-14-10-001. 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. (You can choose an existing Batch and copy it, then assign a new ID for the batch and edit it) 7.3.2 Click Next, to next page. Input information of each sample including QC samples to create sample list in the Batch. When input 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.

6.5

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7.4 Load the samples and start counting 7.4.1 Click on the Sample Assigner tab, click Queued Batch, select the Batch you want to run. Assign each sample in the batch to a chamber. 7.4.2 Click Load Sample, vent cambers, load samples into the corresponding chambers. All samples are placed in shelf 2. 7.4.3 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.
Note: You must double check the sample ID and the chamber ID to ensure they agree with the run log table.

7.5 Data review 7.5.1 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. 7.5.2 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. 7.5.3 Review the regions of interest (ROI). If the ROIs are acceptable, go to step7.5.6. If the ROIs need adjusting, go to step 7.5.4. 7.5.4 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, then go to step 7.5.6. 7.5.5 If the ROIs created in step 7.5.4 are not acceptable, you may adjust the ROIs 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. You must update the ROIs by clicking on the Update ROI button. Once the ROIs have been updated, click on the Reanalyze button. 7.5.6 From "View" click on "report" button to review the report on screen. Check 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 anaytes, FWHM of each peak. The percent recoveries of lab control spike and matrix spike are also included in the reports of QC samples.

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7.5.7 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. 7.5.8 Return to step 7.5.2 to review the next sample. Repeat this process until the review of all the samples in the batch is completed. 7.5.9 Review the QC results: click on the Quality Assurance View tab and select "chemistry". Select the type of QC (spike, duplicate, unknown etc.), select sample matrix and element, and then select the report of 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 QC data chart. If the data are out of control limits, investigate the reason, take correction action and documented it. To see total QC results and control chart in a period of time, select "Full Report" and define the start and the end date.
Note: If no QC information was inputted in the batch, e.g. the QC samples are treated as normal samples, you can manually calculate the QC results.

8.0 8.0 References 8.1 User's manual of Canberra Apex-Alpha Spectroscopy Software Suite. 8.2 Operation manual of Canberra Genie 2000. 8.3 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