DISTRIBUTION LIST To be filled out by Document Author or person requesting document deletion

Transcription

1

2

3

4 DISTRIBUTION LIST To be filled out by Document Author or person requesting document deletion: Once approved, the new or revised document or the notice of deleted document(s) should be distributed to all persons identified below: ( ) All RP staff members ( X ) All holders of the following manual(s): SLAC Radioanalysis Laboratory Procedures ( ) The following individuals: November 27, 2006 SLAC-I-7602A39C-004-R-01 Page 3

5 TABLE OF REVISIONS REVISION DATE SECTION(S) REASON FOR REVISION # 001 June 2, 2005 All Update Data Entry procedures. Addition of Sample Analysis and Data Entry checklists. November 27, 2006 SLAC-I-7602A39C-004-R-01 Page 4

6 TABLE OF CONTENTS General Sample Analysis Procedure 1 PURPOSE REFERENCES RESPONSIBILITIES Rad Lab Operator REP Manager PREREQUISITES PROCEDURES Sample Receiving Analysis Determination Perform Operational Check Count the sample Determine the results Data Entry and Distribution Sample Disposal RECORDS ATTACHMENTS/FORMS Attachment 1: Sample Analysis Flow chart Attachment 2: General Sample Analysis Checklist Attachment 3: Chain of Custody Form Attachment 4: Radioactivity Analysis Form Attachment 5: Data Entry and Reporting Checklist June 2, 2005 SLAC-I-7602A39C-004-R-01 Page 5

7 General Sample Analysis Procedure 1 PURPOSE This procedure outlines the steps for general sample analysis. The procedure applies to anyone characterizing samples for the Radioanalysis Laboratory (Rad Lab). Following this procedure will ensure the completion of the necessary protocols and documentation. A flowchart (Attachment 1) is attached to provide an overview of the Sample analysis procedure. Sample Analysis checklist (Attachment 2) is attached to the appendix to provide detailed steps for routine analysis. 2 REFERENCES 2.1 SLAC Rad Lab Manual, Quality Assurance Plan 3 RESPONSIBILITIES 3.1 Rad Lab Operator The Rad Lab Operator assigned to perform activities described in this chapter is responsible for: ensuring that prerequisites are met as required, maintenance of the laboratory equipment and performing daily quality control checks, reporting any problems or unexpected events to the Radiological Environmental Protection (REP) Manager, routine sample analysis counting, providing the data to the REP Manager for analysis and approval, and Performing other duties assigned by the REP Manager. 3.2 REP Manager The REP Manager is responsible for: ensuring that the activities in this chapter are conducted in accordance with this written procedure, June 2, 2005 SLAC-I-7602A39C-004-R-01 Page 6

8 General Sample Analysis Procedure assigning the tasks in this procedure to a qualified Rad Lab Operator, and providing final approval or disapproval of all data and submittals. 4 PREREQUISITES 4.1 Must be familiar with Windows, Microsoft Access and Notepad. 4.2 Must be familiar with general laboratory equipment (pipettes, scales, etc.) 4.3 Must have a basic understanding of Liquid Scintillation Counting and Gamma Spectroscopy theory 5 PROCEDURES 5.1 Sample Receiving Samples may be received in person or they may be left in the sample drop off location in Room 185 of Building 24. The person delivering the sample shall enter the sample number, date and time of delivery and a signature on the Chain of Custody Log Sheet (Attachment 3). A Radioactivity analysis form (Attachment 4) is also filled out by the customer. This form must accompany the sample. The Rad Lab Operator receiving the sample shall enter the date and time of sample receipt, sign the Chain of Custody Log Sheet, and enter the sample information into the Sample Database. 5.2 Analysis Determination The customer should indicate which analysis he or she desires. The customer may not know which analysis is appropriate. In this case the procedure used shall be decided by the customer in consult with the Rad Lab Operator. If there is any question about the desired analysis, the Rad Lab Operator shall contact and assist the customer. 5.3 Perform Operational Check Before analyzing samples, the Rad Lab Operator shall determine the status of the required periodic quality control checks. An operational source check should be performed on a system daily when in use. A source check procedure is outlined in the instrument system counting procedure. Follow the steps appropriate for the applicable instrument. June 2, 2005 SLAC-I-7602A39C-004-R-01 Page 7

9 General Sample Analysis Procedure 5.4 Count the sample See the appropriate chapter for the desired analysis. To ensure integrity of the samples during the analysis process, samples shall be stored in an area with restricted access. 5.5 Determine the results The Rad Lab Operator shall review all data for any discrepancies. The following are examples of results that should be further investigated. They may be indications of a machine failure or inappropriate use of the software. Background measurements that are unusually high or low Extreme departure from the expected result of the analysis Isotopes that are not usually found at SLAC Isotopes having relatively short half lives which should preclude their presence in the sample 5.6 Data Entry and Distribution The Rad Lab Operator shall enter the sample results into the Sample Database and print the results. The Rad Lab Operator shall prepare the analysis results for distribution. A Data Entry checklist is attached (Attachment 5) to provide the steps for routine data entry and file distribution. The printed report should be reviewed for data entry errors by comparing it to the analysis printouts. When the accuracy of the report has been verified, the Rad Lab Operator shall sign the report, make a copy, and attach the original analyzer printouts and the Radioactivity Analysis Form to the report. The signed Radioactivity Analysis Form indicating release of the sample will be returned to the customer. File a copy of the report, analyzer printout, and Analysis Form for each sample in the Rad Lab cabinet in Building Sample Disposal Upon completion of analysis the sample, container, and release documentation are returned to the customer. Samples vials are to be placed in the appropriate Rad Lab waste container. June 2, 2005 SLAC-I-7602A39C-004-R-01 Page 8

10 General Sample Analysis Procedure 6 RECORDS 6.1 All analysis results generated from this procedure must be entered into the REP Rad Lab database on the network drive to ensure data access, security control, and backup. 6.2 All hardcopies of the Analysis reports generated from this procedure should also be provided and stored in the Rad Lab archives. 7 ATTACHMENTS/FORMS 7.1 Attachment 1: Sample Analysis Flow chart 7.2 Attachment 2: General Sample Analysis Checklist 7.3 Attachment 3: Chain of Custody Form 7.4 Attachment 4: Radioactivity Analysis Form 7.5 Attachment 5: Data Entry and Reporting Checklist June 2, 2005 SLAC-I-7602A39C-004-R-01 Page 9

11 General Sample Analysis Procedure 7.1 Attachment 1: Sample Analysis Flow chart Receive sample & SIS (info/release sheet) [SAC Steps 1-4] LSC required for sample? [SAC Step 5] REP or DOS No personnel complete GS Process analysis [RGS Steps 2-28] Cited Procedures SAC = Sample Analysis Checklist RGS = Routine Gamma Spec RLSC = Routine Liquid Scintillation Counting DER = Data Entry & Reporting Cited Forms/Reports SIS = Sample Information Sheet Yes (release authorization form) RA Report = Radioanalysis Report Complete LSC analysis, vial disposition [RLSC Steps 2-31] Determine radioactivity, etc. [SAC 9-12] Gamma Spec required for sample & not yet done? [SAC 5] Yes No Is water or item release approval needed? [SAC 22] No Continue next page [B] Yes Continue next page [A] June 2, 2005 SLAC-I-7602A39C-004-R-01 Page 10

12 General Sample Analysis Procedure [A] Does sample contain radioactivity OR any hazmat? Yes Is request to release water No to sanitary sewer? FO Mgr signs SIS if authorizing release of item (or REP, DREP or DOS Mgr) No Sign SIS to authorize release Yes REP mgr signs SIS if authorizing release of water (or FO, DREP & DOS. Mgr ) Notify requestor whether release approved or disapproved (if approved, provide signed copy of SIS. [B] Enter results into database, print report, attach LSC or GS print-out [DER 1-31] Did sample analysis include Gamma Spec? Yes REP Mgr reviews RA Report & signs or requests corrections (or FO, DREP or DOS Mgr) No DOS Mgr reviews RA Report & signs or requests corrections (or REP, DREP or DOS Mgr) Continue next page [C] Cited Procedures SAC = Sample Analysis Checklist RGS = Routine Gamma Spec Process RLSC = Routine Liquid Scintillation Counting DER = Data Entry & Reporting Cited Forms/Reports SIS = Sample Information Sheet (release authorization form) RA Report = Radioanalysis Report June 2, 2005 SLAC-I-7602A39C-004-R-01 Page 11

13 General Sample Analysis Procedure [C] Distribute RA Report (if appliacable). File RA Report & LSC/GS print-out [SAC 26] Assure sample handled per procedure (labeled, stored, returned, disposed) per procedure [SAC 27-28] Cited Procedures SAC = Sample Analysis Checklist RGS = Routine Gamma Spec Process RLSC = Routine Liquid Scintillation Counting DER = Data Entry & Reporting Cited Forms/Reports SIS = Sample Information Sheet (release authorization form) RA Report = Radioanalysis Report June 2, 2005 SLAC-I-7602A39C-004-R-01 Page 12

14 General Sample Analysis Procedure 7.2 Attachment 2: General Sample Analysis Checklist Done? Step No. Item Additional Information Sample Receiving [ ] 1. When picking up a sample for analysis from drop location (normally Room 185), check for sample no. on chain of custody log sheet. Sign sheet as Receiving Person & enter date & time. (If sample no. & other info not recorded in C-of-C Log, enter info immediately.) SLAC-I-7602A39C-004 (general analysis procedure) SLAC-I-7602A39C-014 (cof-c log sheet) [ ] 2. Confirm that a completed RP Analysis Form was submitted for the sample. Don t proceed w/o a completed copy of this form. Verify that RP Analysis Form and Sample Label are in agreement. Contact the sample collector if the RP Analysis Form was not submitted, or if the information on the RP Analysis Form and Sample Label are inconsistent. [ ] 3. Check sample with survey meter notify REP or FO mgr if detect radiation. [ ] 4. If the RP Analysis From indicates a hazardous substance in the sample, label the sample bottle with the details. Determine Analysis [ ] 5. Confirm type of analysis to be done. Consult person requesting analysis or REP mgr, if unclear. Also note that samples from EP, RAMSY, BDE, Storm water and wells EXW-4, MW-30, MW-81, & MW-94 must be analyzed using LSC & GS. SLAC-I-7602A39C-004 (general analysis procedure) Perform Operational Check [ ] 6. Confirm applicable QA checks have been completed (LSC: source check recorded completed w/in past 24 hrs in LSC log; GS: source check recorded completed w/in past 24 hrs in GS log] SLAC-I-7602A39C-004 (general analysis procedure) June 2, 2005 SLAC-I-7602A39C-004-R-01 Page 13

15 Done? Step No. Item General Sample Analysis Procedure [ ] 7. If required source check(s) not completed, set up for check (source checks are required within 24 hours sample count OK before or after). Count the Sample Additional Information See applicable procedure: Routine Liquid Scintillation Counting or Routine Gamma Spec Process SLAC-I-7602A39C-008 SLAC-I-7602A39C-009 [ ] 8. Prepare & count sample per LSC &/or GS counting/analysis procedure. See applicable procedure: Routine Liquid Scintillation Counting or Routine Gamma Spec Process SLAC-I-7602A39C-008- R-002 SLAC-I-7602A39C-009 Determine the Results [ ] 9. Determine the whether radioactivity was detected in the sample: a. For GS, a sample is NDA if the only radioactivity detected was naturally-occurring & in concentrations normal for the material. b. For LSC (H-3) swipes, a swipe is NDA if <1000 DPM c. For LSC environmental samples counted on Protocol 13, a sample is NDA if the calculated H-3 concentration is < 500 pci/l d. For all other LSC samples counted on Protocol 1 or 13, a sample is NDA if the calculated H-3 concentration is < 1000 pci/l [ ] 10. If the sample is not NDA put a rad mat l label on sample bottle & mark radionuclide(s) detected. June 2, 2005 SLAC-I-7602A39C-004-R-01 Page 14

16 Done? Step No. Item General Sample Analysis Procedure [ ] 11. If the sample is one that was run on the GS only, proceed to Step 16; otherwise continue with Step 12. [ ] 12. If the sample was determined to be NDA in Step 9, mark the LSC print-out to clearly indicate this. [ ] 13. Determine whether sample is one that may require GS analysis in addition to LSC. Review: Steps 25 & 26 of Routine Liquid Scintillation Counting procedure, and List in Step 5 of this procedure. [ ] 14. If GS analysis is required & hasn t been completed, attach the LSC print-out to the sample bottle & place it on the top shelf of the bookcase by the door to the GS lab. DON T DO DATA ENTRY UNTIL ALL ANALYSES ARE COMPLETE! [ ] 15. Proceed to Step 18. [ ] 16. Determine whether this sample is one that requires LSC in addition to GS (generally all water samples). [ ] 17. If LSC is required & hasn t been completed, attach the GS print-out & RP Analysis Form to the sample bottle & place it in the bin for incoming samples in Room 185. [ ] 18. Double-check to assure that all required LSC (correct protocol) & GS analyses have been completed. Make sure all results are clearly stated. (For GS results, list any nuclides detected & their activities. Normally, positive GS results should be converted to pci & be listed on paperwork with units pci GS.) [ ] 19. Put sample bottle in holding location until all data entry for the sample is completed. [ ] 20. Wash hands! Additional Information June 2, 2005 SLAC-I-7602A39C-004-R-01 Page 15

17 Done? Step No. General Sample Analysis Procedure Item Additional Information Data Entry [ ] 21. Either continue with Step 22 or turn over all sample paperwork (RP Analysis Form, SC &/or GS reports) to person responsible for data entry. [ ] 22. Proceed with entering results into database (see Data Entry checklist). Print report of results using sample database. Check that report(s) matches analysis print-outs. See procedure Data Entry & Reporting SLAC-I-7602A39C-004 (general analysis procedure) Prepare for Distribution [ ] 23. If the sample was submitted requesting RP approval for the release of the material (e.g. approval to release water to the sanitary sewer, resin for off-site treatment, or a sample or item for shipment), proceed to Step 24, otherwise skip to Step 25. [ ] 24. If the sample contains a hazardous substance OR if it contains radioactivity (per Step 9), one of the following must sign (or disapprove) the Sample Log Sheet to authorize the release: the REP mgr, the FO mgr, or the DREP mgr. SLAC-I-760-2A39Z-001 (REP water release policy draft as of 7/04) SBSA permit SLAC-I-760-xxxx-00x (FO resin procedure) SLAC-I-760-2A39Z-001 (FO release criteria) [ ] 25. If the sample contains no hazardous substances and no radioactivity (per Step 9), the person who did the radioanalysis may sign RP Analysis Form to authorize the release. [ ] 26. Notify person/group requesting approval to release of outcome if approval has been refused, follow-up as necessary (e.g. notify RP, SEM mgmt. of circumstances & alternatives). [ ] 27. Obtain signature the REP mgr, the FO mgr, or the DREP mgr on radioanalysis report. SLAC-I-7602A39C-004 (general analysis procedure) June 2, 2005 SLAC-I-7602A39C-004-R-01 Page 16

18 Done? Step No. Item General Sample Analysis Procedure [ ] 28. File the Radioanalysis report, LSC/& or Gamma Spec printout, and a copy of the RP Analysis Form in the Rad Lab file cabinet. Return the RP Analysis Form to the sample requestor. Sample Disposal Additional Information SLAC-I-7602A39C-004 (general analysis procedure) [ ] 29. For the following types of samples, alert the responsible employees to retrieve the sample: solid samples (including resins) samples containing a hazardous material samples that are unusually radioactive [ ] 30. If water sample has not been returned (Step 29), assure it is labeled per Step 10. Store it in location specified by REP or FO mgr. [ ] 31. Dispose of the sample vial in the appropriate Rad Lab waste drum. June 2, 2005 SLAC-I-7602A39C-004-R-01 Page 17

19 General Sample Analysis Procedure 7.3 Attachment 3: Chain of Custody Form June 2, 2005 SLAC-I-7602A39C-004-R-01 Page 18

20 General Sample Analysis Procedure 7.4 Attachment 4: Radioactivity Analysis Form June 2, 2005 SLAC-I-7602A39C-004-R-01 Page 19

21 General Sample Analysis Procedure Done? Step No. 7.5 Attachment 5: Data Entry and Reporting Checklist Item [ ] 1 Open the Microsoft Access database: V:\ESH\OHP\REP\Rad Lab\sample.mdb [ ] 2. Opening this database should bring you to a gray start-up form labeled Slac Environmental & showing six buttons. (If this screen does not appear, move the cursor to the left sidebar. Under Objects click on [Forms] & then double click on the icon for the form named StartUp ). [ ] 3. Before entering the results of counting, you must enter information on the sample. Proceed to Step 13 if you have already done that & want to enter LSC &/or Gamma Spec results or to Step 26 if you want to view or print out an analysis report for a known sample number. Initial Data Entry [ ] 4. Click on the button labeled Data Entry for Taken Sample. This will bring you to the Taken Samples screen. Do not enter any information if data is displayed in any field. [ ] 5. Move the cursor to the bottom left corner of the display. To the right of the box showing that you are at record 1, click on the >* button. This moves you to an empty record at the end of the table. [ ] 6. Click on the Sample Id box & enter the sample ID that is in the upper right corner of the sample label & on the RP Analysis Form. Swipes, resin, and liquid samples should to be labeled with an ID that starts with L; solids start with S0 (S-zero). [ ] 7. Use the Tab-key to get to the Taken Date box. Enter the date the sample was collected (listed on the sample label & on the RP Analysis Form using the form mmddyy. [ ] 8. Tab to the Sample Type box & select the appropriate sample description from the drop-down menu. For water samples submitted with paperwork asking approval for release of water to the sanitary sewer, select Water (sewer) do this even if the water is storm water or LCW. For water samples from any well, select Water (well). Otherwise, select the most appropriate description. June 2, 2005 SLAC-I-7602A39C-004-R-01 Page 20

22 Done? Step No. Item General Sample Analysis Procedure [ ] 9. Tab to the System Name box &, based on the sample label (& RP Analysis Form), select the appropriate description from the dropdown menu there are many choices, take a moment to select the most appropriate. Note that the wells EXW-4, MW-94, MW-30, & MW-81 are individually listed please be sure to identify samples from them correctly! (Samples from any other wells should be identified as GROUND H2O WELLS.) [ ] 10. Tab to the Taken by box &, based on the sample label (or accompanying paperwork), select the appropriate name from the drop-down menu. [ ] 11. Tab to the Sample Description and Comments box & enter any further description that might help identify the sample. For the wells EXW-4, MW-94, MW-30, & MW-81, enter the measured distance to the top of the water, if that information appears on the sample label or RP Analysis Form. [ ] 12. To save the entered record for the sample, move the cursor to the bottom left corner of the display. To the right of the box showing the record number, click on the >* button. To do initial data entry for additional samples, repeat Steps Entering Analysis Results [ ] 13. Before proceeding, assure that all analyses have been completed & have results available for entry. If not, don t start entering results. Note: There are some samples for which both LSC & Gamma Spec analysis are required (e.g. samples from EXW-4, MW-94, MW-30, & MW-81, BDE LCW, BDE sump, storm water, etc.). [ ] 14. If necessary to report the specific activity (pci/g or pci/l) from Gamma Spec (GS) analysis, determine the sample weight or volume and calculate the specific activity from the activity determined by GS before proceeding with data entry. [Note: The output from GS provides radionuclide identities and activities. The activities reported by the GS system assume the sample had the same volume, shape, composition, density, counting geometry, etc. as the applicable standard did at the time the calibration was done. The accuracy of the activity reported by the system for a sample will decrease if this is not the case.] June 2, 2005 SLAC-I-7602A39C-004-R-01 Page 21

23 Done? Step No. Item General Sample Analysis Procedure [ ] 15. In the start-up screen, click on the button labeled Data Entry for Released Sample. If you are in another screen (e.g. the Taken Sample screen), move to a blank record, then use the innermost x in the upper right corner of the display to close that window this should bring you to the start-up screen. (If elsewhere in the database, move the cursor to the left sidebar. Under Objects click on [Forms] & then click on the icon for the form named StartUp ). [ ] 16. Before entering any data, move the cursor to the bottom left corner of the display. To the right of the box showing that you are at record 1, click on the >* button. This moves you to an empty record at the end of the table (>4600 as of July 2004). [ ] 17. Enter the sample ID in the box labeled SAMPLE ID #. [ ] 18. Tab to the Released_Date box and enter the date the sample was analyzed, using the form mmddyy. [ ] 19. Proceed to Step 22 unless the sample is water. [ ] 20. If the sample is from water that is to be released to the sanitary sewer, tab to the Amount box and enter the volume for release (in gallons). In most cases, this volume will be listed on the RP Analysis Form. Water from the four wells EXW-4, MW-94, MW- 30, or MW-81 (unlike all other wells at SLAC) is always released to the sewer, but if you have no information on the volume that will go to the sewer, enter 1 (gallon) this will be noted & corrected later. [ ] 21. If the sample is from water that is to be released to the sanitary sewer, tab to the To box & select SS sanitary sewer from the drop down menu. [ ] 22. Using the cursor, move to field labeled Nuclide. If no radioactivity was detected using the Liquid Scintillation counter, press the * key. If no radioactivity was detected using the Gamma Spectrometer, use the. key. This will fill-in the field with *NDA or.nda, indicating no detected activity. Otherwise start typing the radionuclide symbol &/or select from the choices on the drop-down menu. [ ] 23. If radioactivity was detected, enter the applicable activity or specific activity (by volume or weight), in the field labeled Concentration. Note that for all liquid samples, results are normally recorded as a concentration (pci/l); for solids, they are recorded as a sample activity (pci), unless there is a specific request. June 2, 2005 SLAC-I-7602A39C-004-R-01 Page 22

24 Done? Step No. Item General Sample Analysis Procedure [ ] 24. Select the units that apply to the info entered in the Concentration field, even if the sample is NDA: For LSC For GS For swipes pci/liter pci GS pci/swipe pci/gram - LS pci/gram - GS DPM/swipe Qualitative pci/liter - GS [ ] 25. If more than one radionuclide was detected for this sample, use the >* button at the bottom of the dark gray box to move to add a record to the table of radionuclides. Repeat Steps until all detected radionuclides and quantities have been entered for this sample. [ ] 26. To save the entered information for the sample, move the cursor to the bottom left corner of the display. To the right of the box showing the record number, click on the >* button. To record results for additional samples, repeat Steps Print the Analysis Report [ ] 27. Viewing or printing an analysis report: before proceeding, assure you have the sample ID(s) for the sample(s) of interest. [ ] 28. In the start-up screen, click on one of the buttons labeled Analysis Report. (See instructions in Step 15 if you are in another screen.) [ ] 29. Enter the sample ID of interest & [OK]. [ ] 30. Before printing the report, make sure it has the relevant info report may be blank if the sample ID is not in the database. [ ] 31. Follow steps in procedure Sample Analysis Checklist for signatures, distribution, & filing of the report(s). June 2, 2005 SLAC-I-7602A39C-004-R-01 Page 23