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1. Gross Beta Analysis SOP 1259 112 September 8 2009 Page 1 of 65 Standard Operating Procedure for Gross Beta Analysis Using the Canberra Tennelec XLB Gas Proportional Counter with Eclipse LB Software Please Note The official version of this document is maintained on the LDEQ Intranet and on the Laboratory Information Management System Copies whether in electronic or printed form unless issued by the LSD QAO and stamped controlled are not official and should be verified by the LSD QAO The Control Header of the SOP will be used for comparison to the official document d 0 Developer David L Boucher Ph D Environmental Scientist III Date UL 4 0 07 Approved By Donna B Haydel Environmental Scientist Manager Date i 2 Jof Approved By Elaine S Sorbet Quality Assurance Officer Date Approved By J H Brent Ph D Lab Division Administrator Date Gross Beta Analysis SOP 1259 r12 September 8 2009 Page 2 of 65 Annual Document Reviews Changes made if any 1 Review Made some minor changes throughout the document 2 Review 8 6 08 Major changes made regarding upgrading instrument to computer operating software Eclipse LB software 3 Review 10 6 08 Changes made to incorporate second source run time for samples LSC changed and appendix for spreadsheets 4 Review 9 8 09 Minor changes made throughout the document Changes Reviewed and Approved by
2. Enter key action None Right Print Save Cancel User Info AniCode GBETA GBETACAL LIGBETA L2GBETA_ LPGBETA an Name Gross Beta count Calibration for LCS Result LCSD Result LCS LCSD Precision MethRef pEQINRC DEQ NRC DEQINRC pEGiNRC Lits au im fpciicum we L0E 02 L 0E02 efm L0E02 O AL15512 result degsampid 08196R2 Resut2 jali5514 fresule deqsampid 08196R4 Resutz jalis6s6 fresule degsampid 08196W2 Resutz jaLi5688 resule degsampid 08196W4 Resut2 iL15837 fresat deqsampid 0819762 Resutz j 15839 fresat leqsampid 08197G4 Resut2 AL15840 leqsampid AL15849 leqsampid 7 23 2008 Detailed edit Standard results Left click result cell to enter data headers to display user test or Select the Labshares Radfiles network drive from the Drives pull down menu and select the folder Alpha Beta Select the subfolder for the current year Data Objects Sample AL15840 Analysis GBETACAL Load object from file Open Move Copy Link Close File Name Directories la talpha beta 20081ab_qcs_2008_data xls gi Alpha Beta 2008 A Ca JJAlpha Beta j OCS 2008 Data xls Object File type Drives a Pa Labshares Radfiles v C Alpha Beta 2008 Data Previously stored objects Sample A
3. 2 8 654 04 Feb WED 0 cpm cm ERN 8 653 06 Feb FRI Q cpm cpm NE 8 652 09 Feb MON 0 cpm cpm TN 8 650 11 Feb WED Q cpm cpm oa 8 649 13 Feb FRI 0 cpm cpm ER 8 648 16 Feb MON 0 cpm cm NES 20 8 647 18 Feb WED Q cpm cpm T 8 645 20 Feb FRI 0 cpm cpm ER 8 644 23 Feb MON 0 cpm cpm HD 8 643 25 Feb WED 0 cpm cm un 8 642 27 Feb FRI 9 cpm cpm s 9 641 02 Mar MON 0 cpm cm i 8 639 04 Mar WED 0 cpm cpm VE 8 638 06 Mar FRI Q cpm cpm TN 8637 09 Mar MON 0 cpm cpm TN 8635 11 Mar ED Q cpm cpm XN 2 8 634 13 Mar FRI Q cpm cpm UM 2 8 633 16 Mar MON 0 cpm cpm HN 861 18 Mar WED 0 cpm cym TN 8 630 20 Mar FRI Q cpm cm a 8 629 23 Mar MON 0 cpm cpm E 8 627 25 Mar WED 0 cpm cpm A 8 626 27 Mar FRI Q cpm cpm EE 8 625 30 Mar MON 0 cpm cpm EN 2 8 624 NODA oroo gt s Bo C 10 gg l VON IDD OOo dots a 2 o o o 5 op Appendix D Alpha Beta Quality Control Data Spreadsheet PONE enit Soo EV OD vido oq ee mee Qui 68 z SPGE 86707 LIA SFI 6I R6TOT seco o 4 Isr 6l s6COC LEO 4 sm 6t ROT OT 6str 0 f 86707 LL F6 0 7 groz 6K r6 0 T 86707 ToFFG 0 S961 86C0C 6Mrr60 T 89161 gerot rro 0 z OLGE 86707 EPA f UA YA 86707 oorr 4 9LI 6I 86COC TLIPGO 4 SLI 6I 86707 FEE Tsgol gerot zosr
4. degsampid 0819764 Resut2 AL15840 result ET EDI Resuk2 Standard results AL15849 result deqsampid Resut2 sis Analysis comments Left click result cell to enter data headers to display use Analysis special info LoadjView object for analysis GBETACAL Calculati A3 6 Type the Start and End dates and times in the appropriate fields and make sure analyst initials are correct Also type the start date into the field labeled Result When all fields are correct click Save Results Entry Sample AL15840 Analysis GBETACAL Calibration for Gross Beta counter Sample ID AL15840 Location QAGBETA Gru E Location Description QA for Gross Beta counter Method reference Audit Trai Units E DEOSAMPID History REGION Current objects 0 display SOP Validated No Analysis Comment Analysis GBETACAL Calibration For Gross Beta counter Result 7 23 2008 Qualifier Sample Comments Secondary result TES Analysis Spec Info MDL Analysis data Due date 07 16 2008 23 59 Start date 7232008 start time 15 06 4 End date 7izaj2o08 End time 06 08 s Analyst initials DLB Gross Beta Analysis SOP_1259 112 September 8 2009 Page 40 of 65 A3 7 Atthe resulting screen right click on the cell for GBETACAL to bring up the menu Choose LoadWiew analysis objects A3 8 Result Entry
5. 0 4 FSI GE 86C0C risr t 4 LSV6L 86707 9csr o f 166 R6TOT prow 4 6l 6l 86COC 9ssr 0 4 Sorel groz B960 66161 86707 9Ssr6 0 t Loot 86707 S6Sh 0 T vores R6T0T 01960 S7960 4 6 9r60 z ira 86707 19960 9IT6L 86707 69960 4 s1761 S6T OT Is9r 0 z TC 60 86707 6960 PEE 86707 nire 4 Lite 86COC fcLr6 0 T 67761 gror SELPOW T61 S6T 07 fsLF6 0 1 SET secoc soLr60 7 BEGE 867OC LLLF6 0 f UKU 6707 SOLFOD T Prol 86C C LoSF6 0 4 9FC6l S6TOT 6ISF 0 f 05761 B6TOT LESF6 0 waa pounaou ALIALLOV vd X3 60 ssor ssor ssoi ssor Es sso Lor iso Lor iso sor aor iso wor 9500 9s0 t soir 9s00 950 ISI ssor ssor sso ssir ssor sso t ssor ror tw LL o tr rsot ka Est fso t for Mt JAVTATVH Iom Lt H6 6 076 L6 Sle 16 016 906 06 sava w S HEND PON JO 14015 MOLA EOLA ADO Aro EJ S MEO ao sw wo www wm AWO A LI S E vo wwo m ww gt gt vo wo m ow LI IS 0 ww S L 1 1 A a gt gt vo wo a a 3 a Ea Isa zi ESTA m 1 1 A 30143 97 Spey WA YA Te ane y y DOT X AH VINV LSAGH VON VLS TVINIWINA AXI NOLLVTA42 TVO MOUNT IN32H3d OLE NVHL SS3138 ISAW 32Y1VA ANVADSTHO HWA ALLALLOV QHYONV IS NOW AMA Tad
6. Analyst Supervisor Manager QAO Date 13 ond gr qth Gross Beta Analysis SOP 1259 r12 September 8 2009 Page 3 of 65 Table of Contents Link to Table of Appendices Section Description Page 1 0 Identification of Test Method 6 2 0 Applicable Matrices 6 3 0 Detection And Quantitation Limits 6 4 0 Scope And Application 6 5 0 Summary Of Method 6 6 0 Definition Of Terms 7 7 0 Interferences and Pretreatments 7 8 0 Safety 8 9 0 Equipment And Supplies 8 10 0 Reagents And Standards 8 Sample Collection Preservation Shipment Storage and 11 0 a 9 Sample Rejection Policy 12 0 Quality Control 10 13 0 Calibration 12 14 0 Procedure 12 15 0 Evaluation of Data Reporting Results and Calculations 20 16 0 Method Performance 25 17 0 Pollution Prevention 26 18 0 Data Assessment and Acceptance Criteria 26 Section 19 0 20 0 21 0 22 0 23 0 24 0 Description Corrective Action for Out of Control Data Contingencies for Handling Unacceptable Data Waste Management Data and Records Management Tables Diagrams Flowcharts and Validation Data References Link to Table of Appendices Gross Beta Analysis SOP 1259 r12 September 8 2009 Page 4 of 65 Page 27 27 27 27 28 28 Gross Beta Analysis SOP 1259 r12 September 8 2009 Page 5 of 65 Table of Appendices Link to Table of Contents Appendix Description Page A Batching Samples Into LIMS and Entering Data 29 B Air Particulate Filter Gross Beta
7. and click OK Analyses to Add to Sample GBETA AJ23852 Special analyses for O4 OC sample r Y LIGBETA LCS Result For Gross Beta count Air Pa M L2GBETA LCSD Result for Gross Beta count Air P LPGBETA LCS LCSD Precision for Gross Beta count Gross Beta Analysis SOP 1259 112 September 8 2009 Page 35 of 65 A2 16 At the QA Batch Sample specification screen select the instrument on which the tests will be run by right clicking next to the cell Assigned Instrument Click on Assign instrument for batch GBETA Batch QA Sample Specification OBS Number of batches 1 Samples in largest batch 10 OK Cancel 139527 4323851 Assign instrument For batch GBETA 139527 LABWORKS Instrument Selection Instrument Selection Ok Cancel f Instrument Code Instrument Name Hewlett Packard 6890 Single FID Hewlett Packard 6890 Single FID Hewlett Packard 5890 5971 HP4 HP GCMS Optima 3300DV ICP Spectrometer Quik Chem 8000 FIA Autoanalyzer MAN TECH Man Tech Autotitrator System M7500 Mercury Analyzer Specific Ion Meter Model 9204 Packard 2900 TR pH 5 pi Meter Model AP 61 pH Meter Model AP 61 pH Meter PH4 BOD pH meter BOD room Spectrophotometer Model 21D Tennelec Series 5E Gross Beta counter A2 18 Repeat Step A2 16 on the second batch Gross Beta Analysis SOP 1259 112 September 8 2009 Page 36 of 65 A2 19 After adding the Special Samples and selectin
8. particulate matter the gray area on the APF 14 1 7 4 Place the APF onto the planchet gray side up Use the glassine envelope to lightly press the APF onto the tape inside the planchet Use just enough pressure to make the tape stick Be careful not to remove any particulate matter 14 1 7 5 When the APF is in the properly numbered planchet discard the glassine envelope 14 1 7 6 Place each planchet into the planchet carrier of the same number 14 1 7 7 Batch samples to be run in LIMS according to the procedure described in Appendix A 14 2 Operation of the Canberra Tennelec XLB Gas Proportional Counter 14 2 1 The Canberra Tennelec XLB Gas Proportional Counter is a computer driven instrument operated by Eclipse LB software 14 2 2 Double click the Eclipse Icon on the Desktop e H Eclipse 14 2 3 Login as Administrator no password Enter Login Information Name mmm Password Cancel Gross Beta Analysis SOP 1259 112 September 8 2009 Page 15 of 65 14 2 4 The Eclipse main screen will appear The Main screen includes a Title bar a Menu bar a Tool bar and at the bottom of the screen the Status bar The Eclipse LB Menu bar and Tool bar control all of the functions of the Canberra Tennelec XLB Gas Proportional Counter Eclipse AB BKG lbd XLB fd rie View Manage Count Reports QC System DB Utilities Window Help DB a E dal 7 Samples Status Plateau Attenuation La See ee
9. that you created when the samples were batched See Section 14 1 and Appendix B The results of the sample counts are listed in the 6 column on the sample report The column is labeled Beta pCi There are three results for each sample one result for each of the three counts Calculate the average and standard deviation of the three counts for each sample and write the results of your calculations on the Sample Report printout For each sample copy the calculated average results for each sample to the column labeled ACTIVITY pico Curies on the spreadsheet Copy the calculated standard deviation for each sample to the column labeled ERROR 1S on the spreadsheet As you enter results into the Air Particulate Filter Gross Beta Data spreadsheet the spread sheet will calculate the sample activities per unit volume and sample statistics 2 sigma error in pico Curie m See Appendix B Measuremert Activity pCi TotalVolume m Sample Activity Gross Beta Analysis SOP 1259 r12 September 8 2009 Page 25 of 65 1 Sigma Error pCi zi Total Volume m 2 Sigma Error 2s Where Sample Activity Calculated Activity in pCi m Measurement Activity Activity measured from the instrument in pCi 2 Sigma Error 2 Sigma Calculated Activity uncertainty 1Sigma Error 1 Sigma Error from the instrument Total Volume m Total Volume of sample in m 15 10 The post analysis LCS beta count serves a
10. with pull down menus labeled Format and Destination Gross Beta Analysis SOP 1259 r12 September 8 2009 Page 60 of 65 G11 0 For Format select MS Excel 97 2000 data only For Destination select Disk File Click OK G12 0 The Excel Format Options window will appear Don t change any of the format options just click OK to continue G12 1 The Excel Format Options window for the MS Excel 97 2000 data only format always opens with the following settings These are the default settings Don t change them G12 1 1 Column Width in points 2 36 0 G12 1 2 Export Page Header and Footer box checked G12 1 3 Simplify Page Footers box checked G13 0 After you click OK the Select Export File window will appear with a default name for saving the file G14 0 In order to uniquely identify the file it is necessary to modify the default name before saving the file G15 0 The default name for saving the export file is the same as the name of the report template used G16 0 In the header of the pdf report file there is a number with the label Batch Key The batch key is a unique sequential number that is assigned to each run by the Eclipse software Append that number on the end of the default name for the export file as described below G17 0 For example G17 1 The default name for an efficiency report is Efficiency Report To save an eff
11. Data Sheet 45 C Alpha Beta Quality Control Worksheet 46 D Alpha Beta Quality Control Data Sheet 47 E Reports 48 F Control Charts and QC Profiles 53 G How to extract data from Eclipse to an Excel 59 Spreadsheet H Excel Spreadsheet Calculations 62 2 0 3 0 4 0 5 0 Gross Beta Analysis SOP 1259 r12 September 8 2009 Page 6 of 65 Identification of Test Method The procedure described in this SOP has been developed by the LDEQ Environmental Radiation Laboratory in accordance with the requirements of the Louisiana Department of Environmental Quality This SOP describes in detail the essential elements of the procedure for performing Gross Beta analysis for Air Particulate Filters APF using the Canberra Tennelec XLB Gas Proportional Counter Applicable Matrices 2 1 Air Particulate Filters Detection and Quantitation Limits 3 1 The Limit of Detection LOD for this procedure is calculated as two standard deviations above the mean value for the beta background counts divided by the average beta efficiency for the set of measurements used to calculate the current QC acceptance criteria for the method See Section 16 1 The current LOD is 4 79 DPM 2 16 pCi per filter The LOD per unit volume is obtained by dividing the LOD per filter by the sample volume 3 2 The Limit of Quantitation LOO reporting limit for this procedure is defined being equal to the LOD 3 38 The LOD and acceptance criteria shall be recalculated
12. FP2 0 purchased from Specialty Products Inc P O Box 2888 Ocala FL 34478 2888 9 8 Glassine envelopes and small ziplock bags with labels Reagents and Standards 10 1 All standard information shall be entered into an appropriate logbook All standards are traceable to the National Institute of Standards and Technology NIST Calibration standards must be low level but with sufficient activity in the range of 10 000 40 000 DPM so as to make measurement count times for the QC procedure is less than five minutes per count 10 2 Beta Standard Cs 137 supplied by Analytics Inc of Atlanta Georgia Serial No 73654 65 Assay Date 09 15 2006 11 00 AM CT Activity 20298 00 dpm 3 3 95 conf interval sigma 33 49 dpm 11 0 Gross Beta Analysis SOP 1259 r12 September 8 2009 Page 9 of 65 10 3 Alpha Standard Th 230 supplied by Eberline Instruments Santa Fe New Mexico now Thermo Electron Corporation Serial No 11889 Assay Date 04 21 2008 Activity 22900 687 dpm 9996 conf interval sigma 229 dpm 10 4 Laboratory Control Standard Cs 137 supplied by Analytics Inc of Atlanta Georgia Serial No 78248A 65 Assay Date 09 24 2008 11 00 AM CT Activity 6720 dpm 112 0 Bq 3 3 95 conf interval sigma 111 dpm 10 5 Background Sample One Air Particulate Filter Model No FP2 0 Sample Collection Preservation Shipment Storage and Sample Rejection Policy 11 1 The procedure for air samp
13. Gross Beta Analysis SOP 1259 112 September 8 2009 Page 49 of 65 Batch ID ALPHA EFFICIENCY 200807230738 Count Date 7 23 2008 12 39 58P Group Count Minutes 1 00 Device Count Mode Simultaneous Batch Key Operating Volts 1380 Selected Geometry 1 8 Stainless Steel Selected Standard 11588 Alpha Background cpm 0 66 0 06 Average Alpha Efficiency 21 14 0 36 Average Alpha Spillover 25 50 0 62 Sample ID Alpha Source d Alpha Unc Alpha Spillover nc ncpm Decay Corrected 6l 20080723073 49 A48 7 071 34 22 899 00 30 88 0 48 25 05 0 68 2008072312401 1 A48 7 118 34 22 899 99 31 08 0 48 26 20 0 68 20080723124121 A48 7 250 34 22 899 00 31 66 0 49 26 58 0 68 20080723124221 A48 7 025 34 22 899 99 30 68 0 48 24 84 0 66 20080723124321 A48 7 157 34 22 899 99 31 25 0 48 25 60 0 67 20080723124431 A48 7 003 34 22 899 98 30 58 0 48 25 85 0 68 20080723124531 A48 7 154 34 22 890 08 31 24 0 48 26 43 0 68 20080723124631 A48 7 243 34 22 899 99 31 63 0 49 25 72 0 67 20080723124731 A48 7 110 34 22 890 08 31 05 0 48 25 88 0 68 20080723 124841 448 7 100 34 22 899 99 31 01 0 48 24 87 0 66 20080723124041 A48 7 055 34 22 890 00 30 81 0 48 26 65 0 89 20080723125041 A48 7 093 34 22 898 08 30 98 0 48 25 45 0 67 20080723125151 A48 7 029 34 22 899 00 30 74 0 48 25 23 0 67 20080723125251 A48 7 125 34 22 899 90 31 12 0 48 25 43 0 67 20080723125351 A48 7 263 34 22 899 99 31 72 0 49 25 20 0 66 20080723125501 A48 7 104 34 22 899 99 31 02 0 42 24 80 0
14. activity of the standard relative to the calculated decay corrected activity shall be within 3 3 of the decay corrected activity This parameter is an indicator of the accuracy of the method 15 3 Decay corrected activity of the standard is calculated by this formula in the Alpha Beta Quality Control Spreadsheet Appendix D A Ae Where A Decay corrected activity Ao Standard activity at the time of calibration In2 Ty Ty Half life of Cs 137 in days t time from the calibration date to the date of activity calculation in days A 15 4 The chi square value for Beta Efficiency is calculated by the formula shown below The Chi square must be less than 37 6 The warning limit for Chi square is 31 4 nus 2 X E Where Jf is the chi square value X is the average value of n beta counts Gross Beta Analysis SOP 1259 r12 September 8 2009 Page 23 of 65 n is the number of measurements i e the number of times the standard was counted In this case n 21 Xi is the itt measurement 15 5 The reduced chi square value is the chi square value divided by the degrees of freedom as shown below The number of degrees of freedom is the number of measurements taken minus one 2 Reduced chi square x n 1 Where J is the chi square value n is the number of measurements i e the number of times the standard was counted For Efficiency Counts n 21 15 6 The average values of the Sample and LCS b
15. graph and is located immediately to the left of the Go Icon DE c1 ed 8 F1 3 The QC Chart menu will appear Select Create a QC Chart and click the OK button QC Chart Create a QC Chart Create Edit a OC Profile r Cancel F1 4 The Create a QC Chart menu will appear Select a date range for the chart In the Select a QC Profile panel on the right select one or more parameters Create a OC Chart Display Select a QC Profile C All Data Points for Chart C5 137 Efficiency Date Range for Chart Alpha Background From 77 9 2008 Beta Background Ta 7 29 2008 v Print Chart Automatically Create E dit a QC Profile Gsm Exit Gross Beta Analysis SOP 1259 112 September 8 2009 Page 54 of 65 F1 5 A QC chart wil appear for the date range and parameter you selected Click the Print button to print the control chart Units Efficiency TH 230 Efficiency Individuals 32 063 UCL 30941 Ala ih T MER de ex Ara R ii W Tt y v ly igh Td Li i i ig n 29 818 LCL H H 07 09 0710 07 14 0715 0718 07 21 07 22 07 23 07 25 2008 2008 2008 2008 2008 2008 2008 2008 2008 Profile Settings Data Point Value 0 UCL amp LCL 3 sigma Sample Driven Test Active CE 1 Sigma 0 374 Comment Mean 30 941 Print Back F1 6 If you selected more than one parameter on the Create a QC Chart menu Section F1 3 click the Next
16. of ten If there are more than ten samples type the number of actual samples into the cell under batch size to keep all samples together as a single analytical batch Batch Size Specification Cancel Anl Code Analysis Name Number Samples GBETA Gross Beta count Air Particulates fio 10 A2 6 The Batch QA Sample Specification window will appear Batch QA Sample Specification Number of batches 1 Samples in largest batch 10 Cancel omplete Pend Unbatched Pending Batched GBETA Batch Name IGBETA 139527 Batch Number 139527 OA Sample ID OA Group Added A Tests Added ESA E 00 ES gt o B3 P D ssigned Instr ssigned Analyst Sample 01 Sample 02 4322528 Sample 03 A323231 Sample 04 323233 ample 05 Sample 06 Sample 07 Sample 08 Sample 09 Sample 10 23497 Specify QA QC batch name Select QA sample and QA analyses to add Gross Beta Analysis SOP_1259 112 September 8 2009 Page 32 of 65 A2 7 By right click on Batch Name choose Clone GBETA Batch QA Sample Specification Number of batches 1 Samples in largest batch 10 Pend Unbatched Pending Batched plete d Cancel Batch Name n Batch Number Es gt GA Sample ID Assign instrument For batch GBETA 139527 A Group Added Assign analyst For batch GBETA 139527 Tests Added ll Assigned Instr ya Assigned Analyst Login special GA sample Sample 01 AS A2 8 Right click on
17. the empty cell designated Special Sample in the first column and choose Login special QA sample Batch QA Sample Specification DER Number of batches 1 Samples in largest batch 10 T Cancel Pend Unbatched Pending Batched Batch Name IGBETA 139527 GBETA 139527A Batch Number 139527 139528 ka a Nons y o k ka jm2526 lao A322526 A322528 4323235 4123237 coin special QA sample Left click on batch sample to select QA sample Right click on OA sample to deselect Gross Beta Analysis SOP 1259 112 September 8 2009 Page 33 of 65 A2 9 LABWORKS QA Batching screen will show up with available Location codes Highlight QAGBETA and click OK LABWORKS QA Batching Location Cancel Available entries For QA sample login Laboratory Blank Calibration Verification Data E HP 6890 Single FID WA For Gross Beta counter QA For Gamma Spec NORM analysis A2 10 The Batch QA Sample Specification window will reappear and there will be a LIMS Sample ID for the QA Sample in the Special Sample cell Write the Special Sample LIMS ID number on the air sample data work sheet that you had previously printed out for this sample batch See Section 14 1 of this SOP A2 11 Right click on Special Sample on second batch column and repeat steps A2 8 and A2 9 for the second column Write the Special Sample LIMS ID number from the second column on the a
18. the standard Error calculated as a percentage of the calculated decay corrected activity as shown in Sections 15 2 and 15 8 16 3 2 The precision of this method is evaluated as the relative percent difference between the pre and post analysis LCS beta counts calculated by LIMS as described in Sections 12 4 and 15 10 16 4 Documentation of the initial DOC must be kept in the analyst s training file Training files are kept by the section supervisor 16 5 Continuing Demonstration of Capability 16 5 1 Once initial laboratory and analyst capability are verified and established a program of continued verification of data quality must be maintained This requires 16 5 1 1 Ongoing analysis of LCS beta counts as described in Section 12 16 5 1 2 Regular calibration and maintenance of laboratory instrumentation 16 5 1 3 Maintenance of quality control records 16 5 2 Annual performance of at least one of the following is required 16 5 2 1 Performance of four consecutive of LCS beta counts with acceptable recovery and precision or 16 5 2 2 An initial DOC study 17 0 Pollution Prevention 17 1 Pollution prevention encompasses any technique that reduces or eliminates the quantity or toxicity of waste at the point of generation There is no waste associated with this method other than the samples collected See Section 21 0 of this SOP 18 0 Data Assessment and Acceptance Criteria 18 1 All data collected in the XLB Quali
19. would not give a reliable estimate of precision Control charts for alpha and beta background counts and efficiencies shall be generated monthly The procedure for generating control charts is described in detail in Appendix F Gross Beta Analysis SOP 1259 r12 September 8 2009 Page 12 of 65 13 0 Calibration 13 1 13 2 Instrument Calibration and LCS beta counts of the Canberra Tennelec XLB are performed on Monday Wednesday and Friday of each week except when one of those days falls on a holiday Instrument Calibration and an LCS beta count shall be performed less than 24 hours prior to sample analysis Additionally an LCS beta count shall be performed immediately after sample analysis The calibration procedure takes approximately 5 75 hours to complete An LCS beta count takes approximately one hour The instrument is programmed to perform specific functions by reading a Group label on the side of the planchet holder The following labels are currently in use 13 4 1 CAL QC Performs the Calibration and QC functions 13 4 2 Group A Performs an Alpha Efficiency Calibration Count 13 4 3 Group B Performs a Beta Efficiency Calibration Count 13 4 4 Group C Performs a Background Calibration Count 13 4 5 Group J Performs an LCS beta count 13 4 6 Group G Performs a sample analysis 13 4 7 END Completes analysis sequence and return all planchet holders to their initial position If the END carrier is no
20. 105014 G1 Unknown 0 52 0 27 0 66 200807 16114014 G1 Unknown 0 73 0 28 0 66 200807 16123024 G2 Unknown 0 41 0 28 0 65 200807 16132034 G2 Unknown 0 79 0 23 0 66 200807 16141044 G2 Unknown 0 76 0 28 0 66 200807 16150044 G5 Unknown 1 25 0 30 0 66 200807 16155054 G5 Unknown 1 11 0 30 0 66 200807 16164104 G5 Unknown 1 14 0 30 0 66 20080716173104 G6 Unknown 0 87 0 28 0 66 200807 16182114 G6 Unknown 0 76 0 28 0 66 20080716191124 G6 Unknown 0 96 0 29 0 66 Reviewed by Page 1 of 1 Gross Beta Analysis SOP 1259 r12 September 8 2009 Page 52 of 65 Count Date 7 18 2008 9 59 43AM Count Minutes 50 00 Count Mode Simultaneous Operating Volts 1380 Beta nc Beta MDA pci ipCi 7 19 0 44 0 72 7 58 0 45 0 72 7 85 0 46 0 72 7 58 0 45 0 72 7 52 0 45 0 72 721 0 44 0 72 17 54 0 65 0 72 17 52 0 65 0 72 17 33 0 65 0 72 12 52 0 56 0 72 13 43 0 57 0 72 12 95 0 57 0 72 Print Date 7 23 2008 Print TIme 2 33 57PM CAProgram FilesiTennelec SystemsiEcllpseisample report rpt Gross Beta Analysis SOP 1259 112 September 8 2009 Page 53 of 65 Appendix F Control Charts and QC Profiles F1 0 Control Charts F1 1 Control charts for alpha and beta background counts and efficiency counts shall be generated monthly Printed copies of the charts shall be kept in the same folder as the Background and Efficiency Report printouts F1 2 To generate a control chart first click on the QC icon on the Eclipse LB Tool bar The QC icon has a picture of a
21. 14 3 Pre Analysis Background Efficiency and LCS Beta Counts 14 3 1 Before beginning a count confirm that the printer has been loaded with paper a E E 14 3 2 Make a stack of planchets in holders as shown in the diagram below No 47 LCS No 49 beta std Planchet Stack Diagram No 48 alpha std No 50 blank sample CAL QC 14 3 3 Load the stack of planchet holders onto the sample tower on the right hand side of the instrument The upright prongs on the tower fit into the indents on the sides of the planchet holders 14 3 4 Click on the Go icon on the Eclipse LB Tool bar The Go button has a picture of a green hand pointing to the right T c1 ei 8 Gross Beta Analysis SOP 1259 112 September 8 2009 Page 16 of 65 14 3 5 The Start a Count window will appear Check the two pull down menus to ensure that XLB is selected for Device and C is selected for Group Select AB BKG and click OK to start the alpha beta background count Start a Count ALPHA EFFICIENCY BETA EFFICIENCY a Air Filters Ta Swipes Percent Err a delay a delay 9 hours Device More Info XLB Group E y wen 14 3 6 As soon as the Start a Count window closes click the Go button on the Eclipse LB Tool bar again The Start a Count window will reappear This time Select ALPHA EFFICIENCY with Group A and click OK This will put
22. 66 20080723125601 A48 7 240 34 22 898 08 31 62 0 49 24 83 0 65 20080723125701 A48 7 191 34 22 899 98 31 40 0 49 24 79 0 66 20080723125801 A48 7 258 34 22 890 08 31 70 0 48 25 27 0 66 2008072312591 1 A48 7 130 34 22 899 99 31 14 0 48 24 57 0 66 2008072313001 1 A48 7 023 34 22 899 99 30 67 0 48 25 94 0 68 Reviewed by Page 1 of 1 Print Date 7 23 2003 C Program FlesiTenneiec SystemsiEcilpseie iciency report rpt Print Time 2 31 50PM Batch ID Group Device Batch Key Selected Geometry Selected Standard Beta Background cpm Sample ID 20080723073700 B49 20080723130231 849 20080723130331 B49 20080723130431 849 20080723130541 B49 20080723130641 B40 20080723130741 B49 20080723130851 849 20080723130951 849 20080723131051 849 20080723131151 849 20080723131301 849 20080723131401 849 20080723131501 849 20080723131611 849 20080723131711 849 20080723131811 849 20080723131921 B40 20080723132021 B49 20080723132121 B40 20080723132221 849 Reviewed by Beta Efficiency Report BETA EFFICIENCY 200807230737 1 8 Stainless Steel CS137 73854 85 1 98 0 25 Beta Source d ncpm Decay Corrected 9 270 04 19 449 00 9 035 04 19 449 00 9 103 04 19 440 00 9 168 04 19 449 00 9 025 04 19 449 00 9 008 04 19 449 00 9 172 04 19 449 00 9 100 04 19 449 00 9 109 04 19 449 00 9 023 04 19 449 00 9 068 04 19 448 90 9 168 04 19 448 00 9 107 04 19 448 00 9 030 04 19 448 00 9 192 04 19 448 00 9 091 04 19 448 99 9 222 04 19 448
23. 8 849 Unknown 5 80 20080723141129 849 Unknown 5 80 2008072314 1429 849 Unknown 8 21 20080723141739 849 Unknown 12 07 20080723142039 849 Unknown 4 24 20080723142339 849 Unknown 7 73 20080723142849 849 Unknown 10 14 20080723142049 849 Unknown 12 55 20080723142248 849 Unknown 12 07 20080723143550 B40 Unknown 8 21 20080723142850 849 Unknown 7 25 20080723144159 849 Unknown 7 73 Reviewed by Count Date Count Minutes Count Mode Operating Volts Efficiency Alpha 31 14 0 36 Beta 46 81 0 38 Unc Alpha MDA Beta pci pCi 1 99 3 54 8777 94 1 74 3 54 8752 28 2 11 3 54 8776 65 2 05 354 8778 90 2 51 354 8784 35 2 65 354 8693 25 2 10 354 B673 37 1 81 354 8641 93 1 81 354 8685 56 1 81 3 54 8746 50 2 11 354 8715 29 2 51 3 54 8805 52 1 07 354 8624 93 2 05 354 8660 84 2 32 3 54 8604 08 2 56 354 8704 94 2 51 354 8815 47 2 11 3 54 8774 09 1 99 3 54 8757 73 2 05 354 8703 34 Page 1 of 1 C Program FilesiTennelec SystemsiEclipseisampie report rpt Gross Beta Analysis SOP 1259 r12 September 8 2009 Page 51 of 65 7 23 2008 1 43 28PM 3 00 Simultaneous 1380 Print Date 7 23 2008 Print TIme 3 01 00PM Sample Report Batch ID Air Filters 200807160959 Group G Device XLB Batch Key 76 Selected 1 8 Stainless Steel Background cpm Efficiency Alpha Rate 0 62 0 12 Alpha E Beta Rate 1 87 0 13 Beta Sample ID Sample Type Alpha nc Alpha MDA pci pci 20080716095043 G 1 Unknown 0 55 0 27 0 66 200807 16
24. 98 8 103 04 19 448 00 9 037 04 19 448 00 9 016 04 19 448 00 9 136 04 19 448 08 C Program FiesiTenneiec SystemsiEcilpseietticiency report rpt Gross Beta Analysis SOP 1259 r12 September 8 2009 Page 50 of 65 Count Date 7 23 2008 1 02 13P Count Minutes 1 00 Count Mode Simultaneous Operating Volts 1380 Average Beta Efficiency 4881 t 0 38 Average Beta Spillover 0 06 0 03 Beta Unc Beta Spillover Unc Ls pi 47 66 0 50 0 01 0 02 46 46 0 49 0 06 0 03 46 80 0 50 0 08 0 03 47 14 0 50 0 01 0 02 46 40 0 49 0 11 0 04 46 31 0 49 0 08 0 03 47 16 0 50 0 04 0 02 46 79 0 50 0 11 0 04 46 84 0 50 0 08 0 03 46 39 0 49 0 08 0 03 46 62 0 50 0 07 0 03 47 14 0 50 0 06 0 03 46 83 0 50 0 06 0 03 46 43 0 49 0 08 0 03 47 28 0 50 0 08 0 03 46 74 0 50 0 06 0 03 47 42 0 50 0 05 0 02 46 80 0 50 0 06 0 03 46 47 0 49 0 06 0 03 46 36 0 49 0 06 0 03 46 97 0 50 0 03 0 02 Page 1 of 1 Print Date 7 23 2008 Print Time 2 30 43PM Sample Report Laboratory Control Standard 200807231343 Batch ID Group B Device XLB Batch Key 94 Selected 1 8 Stainless Steel Background cpm Alpha Rate 0 66 0 06 Beta Rate 198 025 Sample ID Sample Type Alpha pCi 20080723124328 849 Unknown 7 25 20080723134650 B49 Unknown 5 32 20080723124958 849 Unknown 8 21 20080723135308 B40 Unknown 7 73 20080723135609 849 Unknown 12 07 20080723135909 849 Unknown 13 51 20080723140219 849 Unknown 8 09 20080723140519 849 Unknown 5 80 2008072314082
25. AVIN LT dam AMIA EST NOW avt T AMAT dam AVWCSIE NOW wW Tad AMIA EL cam av NOW AVIW 60 i4 AMA aiu avro NOW AA ra au dam WASI NOW PACT Tad Paor dain PASI NOW Pav T Pret dam Part NOW Pron Tua 494 90 dam Paro NOW Pazo Tad wfe can wepi NOW Uefa Tad wrez ain ad ia NOM uer 61 Tad wepo aw aver NOM wea T wp qi weza NOM uvf su ALVA NOLLVHSTTVO HV ONY LS GIS 3LL3HON Vid YALTA ALVINOLLAVd YIV LEIS SOLLATVNV ONISA viva TOHINOD ALVIVAO WALSAS ONLIN200 VL38 VHd TV ISS DITINNAL VAJAANV O Gross Beta Analysis SOP 1259 112 September 8 2009 Page 48 of 65 Appendix E Reports Background Report Batch ID AB BKG 200807230736 Count Date 7 23 2008 7 36 40AM Group c Count Minutes 60 00 Device XLB Count Mode Simultaneous Batch Key 91 Operating Volts 1380 Selected 1 8 Stainless Steel Background cpm Alpha Rate 0 66 0 06 Beta Rate 1 96 0 25 Sample ID Alpha Unc Beta Unc Guard cpm cpm cpm 20080723073640 C50 0 63 0 10 2 30 0 20 209 73 20080723082841 C50 0 57 0 10 2 05 0 18 211 43 20080723083851 C50 0 65 0 10 1 63 0 16 211 03 20080723103851 C50 0 70 0 11 2 00 0 18 209 92 20080723113851 C50 0 73 0 11 1 80 0 17 206 32 Guard Avg Rate 209 69 Reviewed by Page 1 of 1 Print Date 7 23 2003 C iProgram Files Tennelec SystemsiEclipseibackground report rpt PrintTime 2 32 35PM Alpha Efficiency Report
26. At the Results entry screen choose the Batched Analyses under QA QC Batches folder under Search for samples by Check GBETA under select one or more batched analyses Click Find button LABWORKS Result Entry File Help zr ml Available templates RAD y Batched Analyses Search For samples by Sample IDs E Location FWTTDS Final Weight TDS Deqsampid FWTTS Final weight Total Solids Sample Delivery Group GBETA Gross Beta count Air Particulates Last selected samples E HARD Hardness Cross Reference Search HG245 Mercury by 245 1 External Files HG7470 Mercury by 7470A Stepped Query HG7471 Mercury in Sediment 2 4 QAQC Batches Y Batched Analyses Batch Creation Dates Z3 Batch Numbers 3 Batch Names Uncheck All Sample ro status Location pEOsaMero Submitted collect Analyses Awaiting Results 3 Analyses Awaiting Validation Select one or more batched analyses No samples are currently selected Gross Beta Analysis SOP 1259 112 September 8 2009 Page 38 of 65 A3 3 Check the batches for which you want to enter results You can identify the batch by the date in the Date Created column There will be two Batch Names for each set of samples the original and the cloned batch that you created See Section A2 7 of this SOP Check both Batch Names and click View Selections LABWORKS Result Entry File Help Bi amp I Available templates RAD Batched Analyses Search for sampl
27. BETA 187939 GBETA 187599 GBETA 187598 GBETA 187447 GBETA 187446 GBETA Z3 Batch Creation Dates Batch Numbers Batch Names Analyses Awaiting Results E Analyses Awaiting Validation METOWAR ZACRYAP APFOLAP APESOAP STJOEAP NEWLTAP QAGBETA QAGBETA 08196R2 08196R4 08196W2 08196wW4 08197G2 08197G4 Pending Pending Pending Pending Pending Pending Pending Pending 07 14 2008 13 14 07 14 2008 13 14 07 15 2008 11 24 07 15 2008 11 24 07 16 2008 11 50 07 16 2008 11 50 07 16 2008 15 16 07 16 2008 15 17 Number of samples Found 8 Gross Beta Analysis SOP 1259 112 September 8 2009 Page 39 of 65 A3 5 The Results Entry screen will appear Right click on the cell for GBETACAL to bring up the menu Choose Detailed Edit Result Entry Enter key action None Right Down Print Save Cancel User Info anicode GBETA cBEracat LiGBErA L2GBETA LPGBETA pnt Name Gross Beta count Calibration for LCS Result for LCSD Result ALCS LCSD Precision J Meth Ref pegic DEQ NRC projec peoiec L mts jpicuM acum jpC CUuM w Der MOL toeo joe ioeoz ioe02 ALISSI2 result degsampid O8196R2_ Resut2 laLis5i4 result degsampid 08196R4 Resut2 aL15636 result degsampid osi96w2 Resut2 AL15638 result degsampid 08196W4 Resut2 AL15837 result deqsampid 08197G2 Resut2 AL15839 result
28. L15840 Analysis GBETACAL Gross Beta Analysis SOP 1259 112 September 8 2009 Page 41 of 65 A3 9 Choose the current Alpha Beta Quality Control Spreadsheet See Section 15 2 and click Link Data Objects Sample AL15840 Analysis GBETACAL Load object from file Open Move Copy Link Close File Name Directories q alpha beta 2008 ab_qcs_2008_data xls q Alpha Beta 2008 Cal CS 21 a AB OCS 2008 Data xls CAlpha Beta 3 Alpha Beta 2008 Data Object file type Drives v Pa Labshares Radfiles y C Previously stored objects Sample AL15840 Analysis GBETACAL Open Remove A3 10 The Description for Analysis Object box appears Click Ok to accept the file description Description for Analysis Object Sample AJ23851 Analysis GBETACAL Description of object iradfilesiab _qc_2006_data xls Gross Beta Analysis SOP 1259 112 September 8 2009 Page 42 of 65 A3 11 Once file has been linked the name will appear in the Previously stored objects box Click Close to finish The Results Entry screen will reappear Data Objects Sample AL15840 Analysis GBETACAL Load object from file Oper Move Cor Link File Name Directories q Alpha Beta 2008 Cua Alpha Beta Alpha Beta 2008 Data Object file type Drives or 2 q Labshares Radfiles y q alpha beta 2008 ab_qcs_2008_data xls Q ALPHA BETA1200814B_QC5_2008_DATA XLS A3 12 Type in the results fo
29. LCL 3 sigma Sample Driven Test Active 1 Sigma 0 180 Comment gt Mean 1 870 Print Back Next Gross Beta Analysis SOP 1259 112 September 8 2009 F2 0 QC Profiles Page 56 of 65 F2 1 The Eclipse LB software uses QC Profiles to determine and store Quality Control limits Quality control limits are redetermined by selecting a new date range for the Sample Driven test To edit a QC Profile first click on the QC icon on the Eclipse LB Tool bar The QC Chart menu will appear Select Create Edit a QC Profile and click the OK button QC Chart C Create a QC Chart Create Edit a QC Profile v List active profiles only Cancel F2 2 The QC Profile menu will appear OC Profile Data Parameters QC Profile Name Activate Trend Test TH 230 Efficiency z Length 3 to 20 pts M Is Active Chart Parameters Activate Run Test Device Length 3to 20 pts XLB EE Upper amp Lower 3 MES Data Channel Count Mode Control Limits sigma C Alpha Data in Alpha Only Sample Driven Test Alpha Data in Simultaneous 7 9 2008 Beta Data in Simultaneous zie Alpha Data in Alpha then Beta End 7 23 2008 v Beta Data in Alpha then Beta C User Driven Test Data Type 30 94056 C Background eua Efficiency Sigma 0 374252 Boundary Test Upper P Geometry 1 8 Stainless Steel y pee Lower Limit fo New Save As Print Cancel Stan
30. act the other Select the batch that you want to extract and click OK Data from the selected batch will appear on the screen Click File on the menu bar and select Print Preview from the pop up menu A list of Report Templates will appear Report Templates are files with the extension rpt NOTE If the batch selected is same as the most recent batch previously displayed the Eclipse program automatically uses the report template previously used and goes directly from Step G3 0 to step G8 0 The following report template types are used G6 1 Background Report Used for background counts G6 2 Efficiency Report Used for efficiency counts G6 3 Sample Report Used for Air Filter samples and Laboratory Control Samples Select the report template that corresponds to the type of sample batch that you are opening and click Open to open the Eclipse Report Server The Eclipse Report Server will open to display a pdf file of the selected batch in the center of the screen NOTE The report server sometimes does not display but instead appears as an orange rectangle at the bottom of the display screen If this happen click on the orange rectangle to display the pdf file in the center of the screen In the task bar of the Eclipse Report Server click on the Export Report icon This is the third icon from the left with a picture of an open envelope with an arrow pointing into it G10 0 The Export window will appear
31. age header Canberra Tennelec Calibration QC Printout Data Parameter Location on printout a Bkgd cpm Alpha Background cpm 8 Bkgd cpm Beta Background cpm Calculated from the data in the Beta ncpm e column on the Beta Efficiency Report using the formula in Section 15 4 p 96e Eff Beta Efficiency 96 8 Count The average value of the data in the Beta pCi Activity column of the LCS Sample Report The difference between the measured beta count activity of the standard and the calculated decay corrected activity of the standard calculated as a Error percentage of the calculated decay corrected activity This value is calculated by the Alpha Beta Quality Control Spreadsheet using the formula in Section 15 4 Gross Beta Analysis SOP 1259 r12 September 8 2009 Page 22 of 65 15 2 8 The alpha background count must fall within the range of 0 287 1 013 counts per minute sigma 0 121 Warning limits are 0 408 0 892 cpm 15 2 9 The beta background count must fall within the range of 1 331 2 409 counts per minute sigma 0 180 Warning limits are 1 511 2 229 cpm 15 2 10 The Chi square value must be less than 37 6 The warning limit is 31 4 This parameter is an indicator of the reproducibility of the method 15 2 11 The beta efficiency must fall within the range of 45 062 48 054 sigma 0 499 Warning limits are 45 561 47 555 15 2 12 The measured beta count
32. button to see the next chart F1 7 Generate and print a control chart for each of the four QC Parameters Th 230 Efficiency alpha efficiency Cs 137 Efficiency beta efficiency Alpha Background and Beta Background Initial and date and store the charts in the designated folder Units Efficiency CS 137 Efficiency Individuals 48 054 UCL mE 5 y PA i it Ali i ith ith f Ag Jj Mn i CL Al M Meni ia E 07 10 0744 0715 0718 07 21 07 22 07 23 07 25 2008 2008 2008 2008 2008 2008 2008 2008 2008 Profile Settings Data Point Value 0 UCL amp LCL 3 sigma Sample Driven Test Active 1 Sigma 0 499 Comment AA Mean 46 558 Print Back N Exit Gross Beta Analysis SOP 1259 112 September 8 2009 Page 55 of 65 F1 8 Example of Alpha Background control chart QC Chart Units CPM Alpha Background Individuals 1 013 0 287 i i E 1 07 09 0710 07 14 07 15 07 17 07 21 07 22 07 23 07 25 2008 2008 2008 2008 2008 2008 2008 2008 2008 Profile Settings 1 Data Point 0 Value o Fiemove UCL amp LCL 3 sigma Sample Driven Test Active EL Data Point 1 Sigma 0 121 Comment Mean 0 650 Print Back Next Exit F1 9 Example of Beta Background control chart QC Chart Units CPM Beta Background Individuals 0710 07 14 0715 0717 07 21 07 22 07 23 2008 2008 2008 2008 2008 2008 2008 2008 2008 Profile Setti i Data Point 0 Value 0 UCL amp
33. dard 11883 X Gross Beta Analysis SOP 1259 112 September 8 2009 Page 57 of 65 F2 3 Select the Profile that you wish to edit from the pull down menu OC Profile Data Parameters QC Profile Name TH 230 Efficiency v CS 137 Efficiency Alpha Background Beta Background XLB Y Data Channel Count Mode C Alpha Data in Alpha Only Alpha Data in Simultaneous C Beta Data in Simultaneous C Alpha Data in Alpha then Beta C Beta Data in Alpha then Beta Chart Parameters Activate Trend Test Length 3 to 20 pts Activate Run Test Length 3 to 20 pts Upper amp Lower 3 1 3 Control Limits sigma Sample Driven Test Stat 7 9 2008 End 7 23 2008 Data Type Background Efficiency Standard 11889 Upper Geometry 1 8 Stainless Steel X it Lower Limit C User Driven Test Mean 20 94056 Sigma 0 374252 v C Boundary Test New Save s Print Cancel F2 4 The Data Parameters left panel shall be set according to the following table QC Profile Data Parameters QC Profile Name Data Channel Count Mode Data Type Th 230 Efficiency Alpha Data in Simultaneous Efficiency Cs 137 Efficiency Beta Data in Simultaneous Efficiency Alpha Background Alpha Data in Simultaneous Background Beta Background Beta Data in Simultaneous Background F2 5 Set the new date range for the Sample Driven test using the pull down menus for the start a
34. er 22 6 Raw data for samples and quality controls are stored in binders 22 7 Data generated during sample analysis must be reviewed by the laboratory When the data is approved as acceptable the analysis data must then be filed in the designated location Data generated on the nuclear power plants must be included in the laboratory s report data file for the respective power plant 22 8 The analyst shall maintain performance records that define the quality of the data that are generated 23 0 Tables Diagrams Flowcharts and Validation Data 23 1 Data is validated after it has been entered into the LIMS system 24 0 References 24 1 S550 Eclipse LB User s Manual V3 1 2 2004 Canberra Industries Inc 800 Research Parkway Meriden CT 06450 24 2 S550 Eclipse LB Technical Manual V3 1 2 2004 Canberra Industries Inc 800 Research Parkway Meriden CT 06450 Gross Beta Analysis SOP 1259 112 September 8 2009 Page 29 of 65 Appendix A Batching Samples into LIMS and Entering Data A1 0 Logging on to the System A1 1 Click on Labworks icon on the desktop A1 2 Enter user name and password LABWORKS User Logon Enter user information For LABWORKS logon PerkinElmer User ID Password OK Cancel 5 8 311 3896 393588 svrlabsvcsilabworkses LWEXES SYSTEM Serv A2 0 QA QC Batching for Gross Beta analysis A2 1 Access QA Batching from QA QC option of file menu LABWORKS ES Desktop Ji Wiley File Log
35. es by x A Sample IDs Location Deqsampid Select one or more batches Sample Delivery Group Last selected samples Cross Reference Search GBETA 1879394 GBETA 187939 GBETA 1875984 187940 GBETA 187939 GBETA 187599 GBETA 07 16 2008 15 07 16 2008 15 07 11 2008 11 GBETA 187598 GBETA 1874464 View Selections Cancel Uncheck All Sample ID status Location DEOSAmMPID submitted 187598 GBETA 187447 GBETA 07 11 2008 11 07 10 2008 11 y External Files Stepped Query H E QAQC Batches y Batched Analyses Batch Creation Dates Batch Numbers Batch Names Analyses Awaiting Results Analyses Awaiting Validation A3 4 List of samples will show up Confirm that the sample numbers and the QAGBETA sample numbers match the numbers on the Air Particulate Filters Worksheet for the results you want to enter then click Enter Selection gt LABWORKS Result Entry File Help 3 18 e Batched Analyses Search for samples by Sample IDs E Location Y Degsampid Sample Delivery Group E Last selected samples Cross Reference Search External Files Stepped Query QAQC Batches Available templates RAD m Select one or more batches Reselect Batches Date Created 07 16 2008 15 18 07 16 2008 15 18 07 11 2008 11 32 07 11 2008 11 32 07 10 2008 11 18 07 10 2008 11 18 GBETA 187939A GBETA 187939 GBETA 187598A GBETA 187598 GBETA 187446A GBETA 187446 187940 G
36. eta counts are calculated by the following formula ixi n x Where X is the average value of n beta counts n is the number of measurements i e the number of times the sample or standard was counted For the LCS and test samples 2 5 Xi is the it measurement 15 7 The standard deviation of the test sample counts is calculated by the following formula Where S is the standard deviation X is the average value of 7 beta counts Gross Beta Analysis SOP 1259 r12 September 8 2009 Page 24 of 65 n is the number of measurements i e the number of times the sample or standard was counted For test samples 2 5 Xi is the it measurement 15 8 The Alpha Beta Quality Control Spreadsheet calculates the Yo error by the formula Beta Count Net Activity Decay Corrected Activity x100 Decay Corrected Activity Error 15 9 Procedure for Calculating Sample Results 15 9 1 15 9 2 15 9 3 15 9 4 15 9 5 The Eclipse LB software produces a single page printout of results for the count of a sample batch The first column on the report labeled Sample ID gives a code for each sample count performed The code is a 14 digit number representing the date and time followed by a letter and a number representing the sample group and the planchet ID number A second page is produced by the post analysis LCS beta count Open the Excel spreadsheet Air Particulate Filters Worksheet ddMONyy xls
37. from i3 through i23 Copy or type the following formula into Cell j3 of the excel spreadsheet Be sure that the formula is entered exactly as shown below then press Enter i3 b3 42 i3 Copy cell j3 and paste the formula into cells j4 through j23 This formula gives the square of the difference between each individual 3 minute beta count and the average value of twenty one beta counts divided by the average value of the beta counts Copy or type the following formula into Cell j24 of the excel spreadsheet Be sure that the formula is entered exactly as shown below then press Enter The chi square value for the 21 efficiency counts will appear in the cell sum j3 j23 Enter or copy the following formula into Cell k24 of the excel spreadsheet Be sure that the formula is entered exactly as shown below then press Enter The reduced Chi Square value for the 21 efficiency counts will appear in the cell j24 20 Gross Beta Analysis SOP 1259 r12 September 8 2009 Page 64 of 65 H3 9 Copy or type the word Average into cell a24 of the spreadsheet then press Enter Copy or type the letters chi sq into cell j25 of the spreadsheet then press Enter Copy or type the letters red chi sq into cell k25 of the spreadsheet then press Enter Save the spreadsheet H3 10 Write the Average the Chi Square value and the Reduced Chi Square value rounded off to two decimal places on the printout for
38. g the Assigned Instrument the Batch QA Sample Specification screen will show all the information Click OK Batch QA Sample Specification Number of batches 1 Samples in largest batch 10 ok Cancel plete GBETA 139527 QA Tests Added 1 3 Assigned Instr TENNELEC TENNELEC Assigned Analyst e Sample 01 AJ22526 AJ22526 A123233 A123233 Sample 05 Sample 06 323235 323235 323237 A323237 A123292 A123292 Specify QA QC batch name Select QA sample and QA analyses to add A2 19 The program will return to the LABWORKS QA Analysis Batching Screen gt LABWORKS QA Analysis Batching File Filters Help Aja 21x e a ms cafes es elm New batch by sample details Analyses to include Analyses from selected department Selected samples None selected Selected analyses None selected Analysis status to batch Unbatched pending Yes Batched pending No Completed No Gross Beta Analysis SOP 1259 112 September 8 2009 Page 37 of 65 A 3 Result data entry and linking QA Excel file A 3 1 To link the QA Excel spreadsheet to the new GBETACAL test code go to Results Entry LABWORKS ES Desktop David Boucher DER File Login Results Reports QA QC Search Maintenance Utilities Options Help o Sample and Analysis Validation 4 57 Thursday July 24 2008 Retiesh ES Multicomponent Transfer 1 Instrument Results Conversion Ay MC Select Ay MC Select OLD A3 2
39. he file will be located in the folder C000 Reports with the file name sample report xls where is the Batch Key number for the report The data file and sample printout for an LCS Sample Report shows the results of five counts with the result of each count on a separate row The analyst must calculate the average and standard deviation for the LCS Sample Counts Copy or type the following formula into cell f8 of the excel spreadsheet Be sure that the formula is entered exactly as shown below then press Enter The average value of the sample activity for 5 LCS sample counts will appear in the cell average f3 f7 Copy or type the following formula into cell i8 of the excel spreadsheet Be sure that the formula is entered exactly as shown below then press Enter then press Enter The standard deviation of the sample activity for 20 LCS sample counts will appear in the cell zstdev f3 f7 Copy or type the word Average into cell e8 of the spreadsheet then press Enter Copy or type the letters SD into cell h8 of the spreadsheet then press Enter Save the spreadsheet Write the Average and Standard Deviation rounded off to two decimal places on the printout for the batch immediately below the column labeled Beta pCi Write the words Average and Std Dev next to the corresponding numbers If this calculation has been performed for the Pre Analysis LCS beta count e
40. iciency report that had a batch key number of 221 you would change the file name to Efficiency Report 221 G17 2 For an LCS Sample Report the default file name would be Sample Report To save a sample report that had a batch key number of 122 you would change the file name to Sample Report 122 G17 3 For an Air Filters Sample Report the default file name would also be Sample Report In order to distinguish Air Filters data files from Data files for the LCS name these files with the format Sample Run Report where HH is the batch key number To save an Air Filters sample report that had a batch key number Gross Beta Analysis SOP 1259 r12 September 8 2009 Page 61 of 65 of 131 you would change the file name to Sample Run Report 131 G18 0 After you have entered the file name save the data file in the folder C000 Reports Gross Beta Analysis SOP 1259 r12 September 8 2009 Page 62 of 65 Appendix H Excel Spreadsheet Calculations H1 0 Average sample activities and chi square values are calculated using the data in the Excel spreadsheet files created by data export The formulas are different for each type of file H2 0 LCS Sample Report data file H2 1 H2 2 H2 3 H2 4 H2 5 H2 6 H2 7 Go to Microsoft Excel and open the file you created using the procedure described in Appendix G for the Laboratory Control Standard Sample Report If you followed Appendix G correctly t
41. in Results Reports QA QC Search Maintenance Utilities Options Help ensure E Setup Display SQC Charts Friday August 11 2006 Refresh A2 2 Click the second icon which is selecting batches by analysis LABWORKS QA Analysis Batching File Filters Help Aja 21x 2 fa usi 38 em Gross Beta Analysis SOP 1259 112 September 8 2009 Page 30 of 65 A2 3 By default the option Unbatched samples with selected analysis pending is selected Type GBETA test code in the blank field to select GBETA analyses then click OK Sample selection options E Cancel C Al samples with selected analyses pending Unbatched samples wth selected analyses pending ses available for batching CAL Calibe tion for Gross Beta counter Gil Coast Analytica Labs A2 4 If all samples are to be batched click Ok to continue If not unclick the arrow in the top cell next to Batch which will then remove the check marks from all samples Click the individual samples to put check marks on the samples to be batched Batch Selections zz Pending unbatched Su Analysis complete Pending batched Not ordered Samom locaton Gera po Batch merowae 0 0 0 0 0 Zi Cancel A322526 METOWAP J23235 STJOEAP 4 Pending Gross Beta Analysis SOP 1259 112 September 8 2009 Page 31 of 65 A2 5 Atthe next screen click Ok to accept the batch size and continue By default LIMS is setup to have a maximum batch size
42. in the same manner as ordinary waste After a sample has been analyzed if it is determined that the total sample activity is lower than 200 pCi the sample can be handled and disposed of as non radioactive material 21 1 1 Solid samples and leftovers are put into a trash can that has been lined with a plastic bag If necessary put the sample in a plastic bag and then secure the bag before discarding 21 2 Samples that are determined to have radioactive levels unsuitable for regular disposal will be disposed in a safe way and by an NRC approved method 22 0 Data and Records Management 22 1 Procedures for data and records management must adhere to the Quality Manual and subordinate documents covering record keeping and the document control plan Records documenting all laboratory activities shall be retained permanently All records shall be stored in such a way as to be secure and accessible 22 2 All data entries must be initialed and dated by the analyst Gross Beta Analysis SOP 1259 r12 September 8 2009 Page 28 of 65 22 3 Certificates of analysis for standards used are kept in the designated binder by the analyst 22 4 A file with all Calibration and Quality Control data must be kept to document the performance of the instrument Also all ongoing maintenance and preventative maintenance must be documented in the Maintenance log for the Canberra Tennelec instrument 22 5 Permanent electronic records are stored on the LIMS Serv
43. ir sample data work sheet A2 12 Right next to the field for QA Tests Added click on number 4 in the first batch Batch QA Sample Specification Number of batches 1 Samples in largest batch 10 Pend Unbatched Pending Batched Analysis Batch Name GBETA 139527 GBETA 139527A Batch Number 139527 139528 OA Sample ID AJ23851 4123852 OA Group Added OGBETA w OGBETA OA Tests Added 4 Assigned Instr Assigned Analyst e Sample 01 AJ22526 Sample 02 AJ22528 Sample 03 AJ23231 Sample 04 AJ23233 Sample 05 AJ23235 Sample 06 AJ23237 Sample 07 AJ23292 Sample 08 AJ23294 Sample 09 AJ23495 Sample 10 AJ23497 Specify QA QC batch name Select QA sample and QA analyses to add Gross Beta Analysis SOP 1259 112 September 8 2009 Page 34 of 65 A2 13 The Analyses to Add screen will appear Analyses to Add to Sample GBETA AJ23851 Special analyses for QA OC sample LIGBETA LCS Result for Gross Beta count Air Pa L2GBETA LCSD Result for Gross Beta count Air P LM LPGBETA LCS LCSD Precision for Gross Beta count A2 14 Uncheck the last 3 analyses and click OK Analyses to Add to Sample GBETA AJ23851 M GBETACAL Calibration For Gross Beta counter J LIGBETA LCS Result For Gross Beta count Air Pa 4 L2GBETA LCSD Result for Gross Beta count Air P A2 15 Repeat Step A2 12 on the second batch Uncheck the first analysis
44. le collection is described in Section 11 of ERL SOP 1023 Preparation of Samples for Gamma Spectroscopy and Gross Beta Analysis 11 2 Air filter samples received by the DEQ Environmental Radiation Laboratory must meet the following acceptance criteria 11 2 1 The filters must be intact dry and contained in a labeled glassine envelope 11 2 2 The envelope containing the filters must be labeled with identification of the collection site identification of the sample collector and the beginning and ending dates and time of collection 11 2 3 The filters must be accompanied by a completed chain of custody form 11 3 Samples received by Laboratory Services Division must be logged into the LIMS The procedure for logging in samples is described in Appendix A of ERL SOP 1023 Preparation of Samples for Gamma Spectroscopy and Gross Beta Analysis 11 4 After samples have been properly logged in they must be stored in the designated location for a minimum of four days to allow the decay of Radon daughters 11 5 In case of samples with incomplete chain of custody contact the person s submitting the sample to obtain the missing information Document the contact and how the information was obtained in the comment section of the chain of custody form 11 6 For policy on chain of custody usage see Section 11 5 of the QAM Gross Beta Analysis SOP 1259 r12 September 8 2009 Page 10 of 65 12 0 Quality Control 12 1 A quality contr
45. lt 8733 8739 esE02 deasampid Result D S T Left click result cell to enter data headers to display user test or sample info Right click For context menu A3 15 The abbreviated LABWORKS Result Entry screen appears and the data has been saved in LIMS gt LABWORKS Result Entry File Help alls el Available templates OIM Number of selected samples 12 Gross Beta Analysis SOP_1259 112 September 8 2009 Page 44 of 65 A3 16 Click on the file menu for further options If you need to enter results for other samples select Reselect samples to return to the full Results Entry menu as shown in Section A3 2 If you are finished select Exit LABWORKS Result Entry SE Reselect samples Available templates Rap y Edit results for selected samples Import instrument results A3 17 The program will return to the LABWORKS ES Desktop window Close the window and exit LABWORKS LABWORKS ES Desktop David Boucher File Login Results Reports QA QC Search Maintenance Utilities Options Help emm Labworks Today 5 7 Tuesday July 22 2008 Rehesh AN Oo 10 T OOO gt IS Toyo C LO nO IA omo o LL 93 6SzLdOS ZOEL 26 ON SAS SS LH PUSS Jauno guotiodod seo gx S seues 2epuue esque oa dD on e mo 5 a a a o 5 09 o0 x4000 00 300 0 SN55 00000 00 3000 SN55 ooo Lem T ER 1 ev 3989 A St Sunod s
46. m the sixth and seventh columns of the Air Particulate Filter Gross Beta Data Sheet into the LIMS column labeled GBETA There are two results for each sample The first result is the Activity in picoCuries m The second result result2 is the Error 2S Note The LIMS sample numbers may not be listed in the same order as they appear on the Air Particulate Filter Gross Beta Data Sheet Check and compare the order of the LIMS sample numbers before entering data A3 14 After all the results have been entered check to ensure that the data has been entered correctly then click Print and click Save gt Result Entry Enter key action C None e Right Print Save Cancel ano aa nera ITA JEE LZeNEA ues DP jAnName Gross Beta coulCalibration For GraLCS Result for GLCSD Result for Gr LCS LCSD Precision esse peamac pegwc pegwc pegwc oo mts pium pci cum pcifcum e poo fpefmo noce Pez roeo2 i oeoz result 1 39 02 musi degsampid 08196R2 1 48E 03 jALI5514 result 1456 02 deqsampid 08196R4 Resuk2 6 50E 04 JALIS636 result deqsampid 08196W2 l 5 79E 04 result 1 64E 02 AL15638 deqsampid 08196W4 IResuk2 1 31E 03 jAL15837 result 213E 02 deqsampid 08197G2 Resuk2 1 40E 03 jL15839 result 141 02 AL15839 deqsampid 0819764 Result2__ 2 19E 03 ALi5e40 result AL15849 resu
47. nd end dates After you select a new date range the mean and sigma values for the control limits will F2 6 F2 7 Gross Beta Analysis SOP 1259 r12 September 8 2009 Page 58 of 65 not change automatically In order to reset the control limits to the new range do the following F2 5 1 Click to change the Data Channel Count Mode in the left panel to one of the alternate options This will clear out the old control limits F2 5 2 Click again to change the Data Channel Count Mode back to the correct mode as shown in the table above Be sure all of the Data Parameters have been returned to the correct settings This will reset the control limits to the new date range The upper and lower control limits shall be set to 3 sigma Click the Save button to save the new settings then click the OK button to exit Gross Beta Analysis SOP 1259 r12 September 8 2009 Page 59 of 65 Appendix G How to extract data from Eclipse to an Excel Spreadsheet G1 0 G2 0 G3 0 G4 0 G5 0 G6 0 G7 0 G8 0 G9 0 Click on the Recall Batch icon on the Eclipse task bar The icon is a picture of an open folder and is the first icon on the left side of the task bar A list of previously run batches will appear The batches you will need to extract are the Beta Efficiency the Laboratory Control Standard and Air Filters You can only extract one batch at a time so you will have to choose one to extract then go back and extr
48. nter the Average sample count in the designated fields on the Alpha Beta Quality Control Worksheet Appendix C and the Alpha Beta Quality Control Data Spreadsheet Appendix D Gross Beta Analysis SOP 1259 r12 September 8 2009 Page 63 of 65 H3 0 Beta Efficiency Report data file H3 1 H3 2 H3 3 H3 4 H3 5 H3 6 H3 7 H3 8 Go to Microsoft Excel and open the file you created using the procedure described in Appendix G for the Beta Efficiency Report If you followed Appendix G correctly the file will be located in the folder C 000 Reports with the file name efficiency report xls where is the Batch Key number for the report The data file and sample printout for a Beta Efficiency Report shows the results of 21 counts with the result of each count on a separate row The analyst must calculate the Average of the counts and from that result the analyst must calculate the Chi Square and Reduced Chi square values Copy or type the following formula into cell b24 of the excel spreadsheet Be sure that the formula is entered exactly as shown below then press Enter The average value of the 21 beta efficiency counts will appear in the cell average b3 b23 Select Cell b24 and click copy Then highlight the cells i3 i23 Click the down arrow at the bottom of the Paste icon and then click Paste Values on the pull down menu The same number from Cell b24 will appear in each cell
49. ol program is required for this method The requirements of this program consist of demonstration of capability and the continuing analysis of a NIST traceable standard of known activity as an ongoing demonstration of performance All Demonstrations of Capability DOCs must be documented using the appropriate Certification Statement Form The analyst shall maintain performance records that define the quality of the data that are generated 12 2 Demonstration of Capability 12 2 1 12 2 2 A demonstration of capability for this method requires the acceptable performance of four 4 Instrument Calibration and Laboratory Control Standard LCS Beta Count procedures Acceptable performance is attained when the results meet the acceptance criteria defined in Section 15 2 of this SOP Additionally the standard deviation of the four measurements must be within the designated control limits Calibration requirements are described in Section 13 0 of this SOP Step by step descriptions of the calibration and sample count procedures are found in Section 14 0 of this SOP 12 3 During the calibration procedure the following counts are performed 12 3 1 12 3 2 12 3 3 Background Count Planchet carrier No 50 background filter is counted for five 5 consecutive 40 minute counts to determine the system alpha and beta backgrounds Acceptance Criteria for alpha and beta background counts are given in Section 15 2 Values outside of the acce
50. on an annual basis Scope and Application This SOP describes in detail the essential elements of the procedure for performing Gross Beta analysis for Air Particulate Filters APF using the Canberra Tennelec XLB Gas Proportional Counter Summary of Method 5 1 X Airborne particulate matter is collected on air particulate filters using RADeCO Model No HD 28A Air Samplers over a period of one or two weeks These samples are collected concurrently with charcoal cartridge samples for gamma analysis of lodine 131 Prior to analysis the filters are stored for at least one week to allow the decay of short lived radon daughters 5 2 Samples are analyzed for Gross Beta using a Canberra Tennelec XLB Gas Proportional Counter with Eclipse LB software The instrument is 5 3 5 4 Gross Beta Analysis SOP 1259 r12 September 8 2009 Page 7 of 65 calibrated less than 24 hours prior to analysis of each sample batch and a Laboratory Control Standard LCS Beta Count is performed immediately before and after each sample batch Each air particulate filter is counted for three consecutive 50 minute counts to measure the Gross Beta activity of each sample After gross beta analysis has been completed the air particulate filters are composited by site and location and saved for quarterly gamma analysis 6 0 Definition of Terms 6 1 6 2 6 3 Duplicate Measurement A second measurement made on the same or identical sample of mate
51. ptable range would indicate problems with the detector and actions must be taken to correct any problem s before continuing with sample analysis Alpha Efficiency Calibration Count Planchet carrier No 48 Th 230 Alpha standard is counted for 21 consecutive one minute counts to determine the system alpha efficiency Beta Efficiency Calibration Count Planchet carrier No 49 Cs 137 Beta standard is counted for 21 consecutive one minute counts to determine the system beta efficiency Acceptance Criteria for beta efficiency are given in Section 15 2 Values outside of the acceptable range would indicate problems with the detector and actions must be taken to correct any problem s before continuing sample analysis 12 4 AnLCS beta count is performed immediately before and after the analysis of a sample batch 12 5 12 6 12 7 Gross Beta Analysis SOP 1259 r12 September 8 2009 Page 11 of 65 12 4 1 Pre Analysis LCS beta count 12 4 1 1 Planchet No 47 Cs 137 Laboratory Control Standard is counted for five 5 consecutive 20 minute counts The summary beta count of the standard is compared to the expected value of the count calculated from the initial calibration value and date of the standard These calculations are performed using the Alpha Beta Quality Control Data Sheet See Appendix D 12 4 2 Post Analysis LCS beta count 12 4 2 1 Planchet No 47 Cs 137 Laboratory Control Standard is counted for five 5 consecuti
52. ptember 8 2009 Page 18 of 65 count will take 100 minutes A one page report will print for each count After all counts have completed the planchets will restack on the right hand side of the instrument 14 4 See Section 15 2 of this SOP for a description of how the Pre Analysis Background counts Efficiency counts and the LCS beta count results are documented and evaluated 14 5 Sample Counting 14 5 1 Before beginning a count confirm that the printer has been loaded with paper 14 5 2 Place each sample on a planchet in a numbered planchet carrier according to the procedure described in Section 14 1 14 5 3 Carefully load sample planchet carriers onto the right side tower beginning with the Group G planchet carrier followed by the lowest number at the bottom and progressing to the highest number at the top Once all sample planchet carriers have been loaded into the system place the planchet carrier labeled Group J 47 and END at the top of the sample stack 14 5 4 The complete planchet stack for a sample run will resemble the diagram below No 47 LCS Group J Sample 6 Planchet Stack Diagram Sample 4 14 5 1 After the planchet stack has been loaded into the sample changer mechanism click on the Go button the green hand on the Eclipse LB Tool bar DB T WEE 7 14 5 2 The Start a Count window will appear Select Air Filters Check the two pull down menus to ensure that XLB is selected for De
53. r LI GBETA and L2GBETA L1GBETA is the average value of the Beta activity pCi for the pre analysis LCS beta counts L2GBETA is the average value of the Beta activity pCi for the post analysis LCS beta counts LPGBETA is calculated automatically by the LIMS when the other two values are entered Result Entry Enter key action None Right C Down Print Save Cancel userinfo anicode peta cBEracat LiGBErA i2GBerA ieGBETA nt Name Gross Beta co Calibration for GraLCS Result for qLCSD Result for Gr LCS LCSD Precision MehRe foege jpeorec bromec psomrc L mts ptum paum pcifcum w gt pewo Lo f fiomoz Loro Leg result AL15512 O 8 Ss deqsampid 08196R2 Resut2 ALISSIS C RET O deqsampid 08196R4 Resutz A c EE CN degsampid 08196W2 Resutz EE result leqsampid 08196W4 Resulez laL15e37 resulte legsampid 08197G2 Resulez AL15839 resulte deqsampid 0819764 Resutz ALI5840 result deqsampid Resul2 IE aL15849 result 6733 8739 6902 deqsampid jResutz SEEN NENNEN Left click result cell to enter data headers to display user test or sample info Right click For context menu Gross Beta Analysis SOP 1259 112 September 8 2009 Page 43 of 65 A3 13 Enter the calculated sample results fro
54. rial to assist in the evaluation of measurement variance Minimum Detectable Activity MDA The minimum level of activity that can be measured counted with a defined level of confidence that the measurement is not the result of random fluctuations in the background count i e noise 6 2 1 The DEQ Environmental Radiation Laboratory defines the level of confidence for the MDA at 95 This means that for an observed sample count that appears to indicate that the sample activity is equal to the MDA there is only a 5 probability that the sample might actually be free of activity 6 2 2 The MDA is also referred to as the detection limit or lower limit of detection The counting rate from a sample at the MDA is called the determination level 6 2 3 Radon Daughters Elements produced by the radioactive decay of radon gas These include a number of radioactive isotopes Radon is a gas but radon daughters are all solids at ambient temperatures and so may be trapped on particulate filters See QA Manual Appendix B for additional definitions 7 0 Interferences and Pretreatments 7 1 Beta emissions from short lived radon daughters may cause the sample count to be artificially high Radon and its decay products are not produced by nuclear reactors and so should not be included in the beta count Because they decay rapidly radioactive isotopes with short half lives exhibit a high level of activity relative to their concen
55. rol samples must be within designated control limits Quality control acceptance criteria for this method were established by a statistical analysis of 55 one hour background counts and 231 one minute alpha and beta efficiency counts performed over a two week period from 07 09 2008 through 07 23 2008 Acceptance criteria shall be recalculated annually in the same manner from data collected during the first quarter of the calendar year 15 2 Procedure for Recording and Evaluating Calibration Data 15 2 1 The Eclipse LB software produces a one page report for each procedure it performs Examples of the different report formats are shown in Appendix E There are three report formats that are used 15 2 1 1 Background Report used for background counts 15 2 1 2 Efficiency Report used for alpha and beta efficiency counts 15 2 1 3 Sample Report used for test sample counts and LCS beta counts 15 2 2 A summary of the data is recorded by the analyst on the Alpha Beta Quality Control Worksheet Appendix C The Beta Efficiency is evaluated using the Alpha Beta Quality Control Spreadsheet Appendix D This spreadsheet is a protected spreadsheet that includes the formulas necessary to compare the beta activity measured by the LCS beta count to the decay corrected activity calculated from the initial activity and calibration date of the beta standard 15 2 3 The electronic copy of the Alpha Beta Quality Control Spreadsheet Appendi
56. s ending QC for the batch The relative percent difference RPD between the pre and post analysis LCS beta counts must be less than 1 15 10 1 The LIMS calculates the relative percent difference between the pre and post analysis LCS beta counts by the following formula 2X A A RPD before after x 100 Abefore Aafter Where Abefore Pre Analysis LCS Beta Count Aafter Post Analysis LCS Beta Count 15 11 Results will be reported to two decimal places 15 12 Data will be entered into LIMS See Appendix A 16 0 Method Performance 16 1 16 2 Quality control acceptance criteria for this method were established by a statistical analysis of 55 one hour background counts and 231 one minute alpha and beta efficiency counts performed over a two week period from 07 09 2008 through 07 23 2008 Acceptance criteria shall be recalculated annually in the same manner from data collected during the first quarter of the calendar year All demonstrations of capability accuracy and precision must be determined at least annually or whenever there is a significant change in background or instrument response or when a new operator begins work 16 3 Determination of Accuracy and Precision Gross Beta Analysis SOP 1259 r12 September 8 2009 Page 26 of 65 16 3 1 The accuracy of this method is evaluated as the difference between the measured beta count activity of the standard and the calculated decay corrected activity of
57. t placed at the top of the stack the sample program will run continuously until manually stopped NOTE The XLB is designed to have a planchet carrier labeled END at the beginning and end of the system s sample changer One END planchet carrier must always remain in the counting system while the second END planchet carrier must be positioned at the top of any sample stack There are also two empty planchet holders that always remain in the instrument these function solely as place holders 14 0 Procedure 14 1 Air Particulate Filter APF data sheet preparation 14 1 1 Each APF will be in a glassine envelope with the collection date LIMS Sample ID and Sample Volume volume of air that had passed through the filter written on the label The filters are batched by the week in which the filters were collected Samples are scheduled to be analyzed on the second Friday after collection Gross Beta Analysis SOP 1259 r12 September 8 2009 Page 13 of 65 14 1 2 Open the spreadsheet Air Particulate Filters Worksheet xls The 14 1 3 14 1 4 14 1 5 14 1 6 14 1 7 spreadsheet is located in the network folder labshares Radfiles This folder is mapped as the Q V drive on the computers in Room R02 The spreadsheet is a protected spreadsheet that includes the necessary formulas to calculate the sample results from the raw data The format is shown in Appendix B Record the LIMS Sample ID Sample Date collection da
58. te and Sample Volume in the appropriate fields The worksheet is divided into groups of six rows By convention the rows within a group are assigned to specific sites as shown in the following table Air Sample Collection Sites Row Number Site Location Code 1 RBS METOW 2 RBS ZACRY 3 W 3 APFO01 4 W 3 APE30 5 GGNS STJOE 6 GGNS NEWLT If in a given week there are no samples from a specific site leave the rows for that site blank on the worksheet After the sample information has been filled in use the Save As function to save the spreadsheet with a new filename in the format Air Particulate Filters Worksheet ddMONyy xls where ddMONyy represent the day month and year of the sample count Ignore the last two columns activity and uncertainty for the time being Print the air sample data work sheet to use as a work sheet until results are obtained Prepare the APF s for Gross Beta analysis 14 1 7 1 With a Sharpie or similar permanent marker put the LIMS sample ID sample location code and sample date on the bottom of each planchet 14 1 7 2 Put a small piece of double stick cellophane tape in the planchet Use about 0 5 or less of tape any more will make it hard to remove the APF later Gross Beta Analysis SOP 1259 112 September 8 2009 Page 14 of 65 14 1 7 3 With tweezers grasp the APF by the edge and carefully remove it from the glassine envelope Do not touch the
59. the Alpha Efficiency count in the queue to start as soon as the alpha beta background count is completed Start a Count Ta AB BKG ALPHA EFFICIENCY Ta delay 9 hours XLB Group A hd E More Info Gross Beta Analysis SOP 1259 112 September 8 2009 Page 17 of 65 14 3 7 When the Start a Count window closes click the Go button for the third time When the Start a Count window reappears select BETA EFFICIENCY with Group B and click OK This will put the Beta Efficiency count in the queue to start as soon as the other two counts have completed Start a Count Ta AB BKG Ta ALPHA EFFICIENCY a BETA EFFICIENCY Ta Air Filters Ta Swipes f Percent Err Ya delay Ta delay 9 hours Device More Info XLE y Group B Caes 14 3 8 When the Start a Count window closes click the Go button for the fourth time When the Start a Count window reappears select Laboratory Control Standard with Group J and click OK This will put the LCS beta count in the queue to start as soon as the other counts have completed Start a Count Ta AB BKG Ta ALPHA EFFICIENCY a BETA EFFICIENCY a Air Filters a Swipes Ta Percent Err Ta delay Ta delay 9 hours 3 Laboratory Control Standard More Info Cancel 14 3 9 The Background and Efficiency calibration counts will take a total of approximately 5 5 hours to complete The LCS beta Gross Beta Analysis SOP 1259 r12 Se
60. the batch immediately below the Beta Counts column Write the words Average Chi Square and Reduced Chi Square next to the corresponding numbers H3 11 Enter the Chi square value in the designated fields on the Alpha Beta Quality Control Worksheet Appendix C and the Alpha Beta Quality Control Data Spreadsheet Appendix D H4 0 Air Filters Sample Report data file H4 1 Go to Microsoft Excel and open the file you created using the procedure described in Appendix G for the Air Filters Sample Report If you followed Appendix G correctly the file will be located in the folder C 000 Reports with the file name sample run report xls where is the Batch Key number for the report H4 2 The data file and sample printout for an Air Filters Sample Report shows the results of five counts for each sample with the result of each count on a separate row The analyst must calculate the average and standard deviation for each sample H4 3 Copy or type the following formula into cell j3 of the excel spreadsheet Be sure that the formula is entered exactly as shown below then press Enter The average value of the sample activity for 3 sample counts will appear in the cell average f3 f7 H4 4 Copy or type the following formula into cell k3 of the excel spreadsheet Be sure that the formula is entered exactly as shown below then press Enter The average value of the sample activity for 3 sample coun
61. tration For this reason samples are aged for a minimum of four days to allow any short lived radon daughters to decay to negligible levels 8 0 9 0 10 0 Gross Beta Analysis SOP 1259 r12 September 8 2009 Page 8 of 65 Safety 8 1 Standard laboratory clothing lab coat or apron eye covering safety glasses or goggles and radiation badges shall be worn 8 2 Care should be taken when working around the sample changer while the changer is in motion Possible finger injuries can occur Fingers should remain clear of sample changer while XLB is in use 8 3 Material safety data sheets MSDS of all chemicals used in the DEQ Environmental Radiation Laboratory are kept in a yellow binder in Room R 02 Additionally MSDS are available at a web site maintained by Cornell University The link is http hazard com msds index php NOTE Radioactive materials are not included in the notification requirements of the OSHA Hazard Communication Standard 29CFR1910 1200 Equipment and Supplies 9 1 Canberra Tennelec XLB Gas Proportional Counter Serial No 67455 9 2 Dell Computer Model GX270 running Windows XP Professional 9 3 Canberra Eclipse LB v 3 1 2b interface software for Tennelec Series 5 and LB550 Gas Proportional Counters 9 4 RADeCO Model No HD 28A Air Samplers 9 5 P 10 counting gas 10 methane 90 argon supplied by AirGas 9 6 Stainless steel planchet sample holders 9 7 2 inch Air Particulate Filters Model No
62. ts will appear in the cell zstdev f3 f7 H4 5 If the sample batch contains 4 samples H4 5 1 Copy cell j3 and paste into cells j8 j13 and j18 H4 5 2 Copy cell k3 and paste into cells k8 k13 and k18 H4 6 If the sample batch contains 6 samples H4 7 H4 8 H4 9 Gross Beta Analysis SOP 1259 r12 September 8 2009 Page 65 of 65 H4 6 1 Copy cell j3 and paste into cells j8 j13 j18 j23 and j28 H4 6 2 Copy cell k3 and paste into cells k8 k13 k18 k23 and k28 After you have done the above the cells that you pasted in column J will show the average values for the sample counts The cells you have pasted in column K will show the standard deviations for the sample counts Copy or type the word Average into cell j2 of the spreadsheet then press Enter Copy or type the letters stdev into cell k2 of the spreadsheet then press Enter Save the spreadsheet On the printout for the Air Filters Sample Report label two columns on the right hand side of the page next to the printed results Label one column Average Beta pCi Label the second column Std Dev Write the average values and standard deviations from the spreadsheet rounded off to two decimal places on the printout in the designated columns next to the sample results H4 10 Enter the Average Beta pCi and Std Dev values in the designated fields on the Air Particulate Filter Gross Beta Data Sheet See Appendix B
63. ty Control procedure are reviewed by the analyst to ensure that all acceptance criteria have been met Refer to Section 15 for acceptance criteria Instrument printouts are initialed and dated by the analyst and kept in designated files in reverse chronological order Spreadsheets used for calculations are printed out initialed and dated and kept in designated binders LIMS entries Gross Beta Analysis SOP 1259 r12 September 8 2009 Page 27 of 65 are reviewed by the analyst for accuracy and are reviewed by the Manager 19 0 Corrective Action for Out of Control Data 19 1 If the QC data is out of acceptance criteria QC procedure will be repeated once 19 2 Ifthe QC fails for a second time the instrument must not be used until diagnostics have been completed and the problem resolved The assistance of Canberra Tennelec System Service Engineer s shall be utilized to determine the cause of out of control data 20 0 Contingencies for Handling Unacceptable Data 20 1 Data will be considered unacceptable if the acceptance criteria for Quality Control measures are not met Continual or persistent QC failures will result in the XLB counting system being unavailable for use until the cause of the failures has been identified and corrected 21 0 Waste Management 21 1 Samples with an exposure rate less than or equal to 200 uR h or that upon analysis are shown to have activity equivalent to background or control samples can be disposed of
64. ve 20 minute counts The summary beta count is compared to the previous count obtained from the same standard immediately prior to analysis of the sample batch This calculation is performed automatically by the LIMS when the count values are entered A decay correction is not necessary because the elapsed time between counts is negligible relative to the half life of the standard 12 4 3 The relative percent difference between the pre and post analysis LCS beta counts as calculated by LIMS must fall within the range of 3 3 This parameter is an indicator of the precision of the method 12 4 3 1 Acceptance criteria for the Error of LCS beta counts are given in Section 15 2 Values outside of the acceptable range would indicate problems with the detector and actions must be taken to correct any problem s before continuing sample analysis The background count is performed as a negative control The post analysis efficiency check serves as a positive control Because these are not aqueous samples and no chemical separation occurs a matrix spike is not required or performed Precision is evaluated by the pre and post analysis LCS beta counts Duplicate sample analysis is not performed because only one air particulate filter sample is collected in each sampling event Additionally because the vast majority of the samples tested exhibit a very low level of activity near or below the MDA repeated analysis of a single sample
65. vice and G is selected for Group start the sample count Start a Count Ta AB BKG Ta ALPHA EFFICIENCY BETA EFFICIENCY e TE Ta Swipes Ta Percent Err Ta delay Ta delay 9 hours Device XLB z Group G hd Cancel Start a Count 2 AB BKG Ta ALPHA EFFICIENCY Gross Beta Analysis SOP_1259 112 September 8 2009 Page 19 of 65 Click OK to More Info 14 5 3 As soon as the Start a Count window closes click the Go button on the Eclipse LB Tool bar again The Start a Count window will reappear This time Select Laboratory Control Standard with Group J and click OK This will put the LCS beta count in the queue to start as soon as the sample run is completed More Info 14 5 4 Each test sample will be counted for five 5 consecutive 20 minute counts The Laboratory Control Standard will also be counted for five 5 consecutive 20 minute counts Gross Beta Analysis SOP 1259 r12 September 8 2009 Page 20 of 65 14 5 5 Atthe conclusion of the counts two one page reports will print out a report for the test samples and a report for the LCS beta count 14 5 6 Perform the necessary calculations and enter the data into the LIMS according to the procedures described in Section 15 and Appendix A of this SOP 15 0 Evaluation of Data Reporting Results and Calculations 15 1 All data must be evaluated before reporting All quality cont
66. x D is saved in the folder for the current year in the network folder Labshares Radfiles Alpha Beta The spreadsheet is linked to the associated sample batch in the LIMS See Appendix A3 8 for a description of how the spreadsheet is linked 15 2 4 15 2 5 15 2 6 15 2 7 Gross Beta Analysis SOP 1259 r12 September 8 2009 Page 21 of 65 The fields for data entry on the Alpha Beta Quality Control Worksheet Appendix C and the Alpha Beta Quality Control Spreadsheet Appendix D are the same The analyst shall enter the data from the instrument printout for alpha and beta background counts the reduced chi square of the beta efficiency counts the beta 96 efficiency and the average LCS beta count activity on the paper worksheet then enter the same data in the electronic spreadsheet The reduced chi square and the average LCS beta count activity must be calculated manually by the analyst Write the reduced chi square of the beta efficiency counts on the Beta Efficiency report Write the average LCS beta count activity on the LCS Sample Report The other data are calculated automatically by the Eclipse LB software Values for the column labeled 96 Error are calculated automatically by the spreadsheet Write those values on the worksheet and initial The relevant data for completion of the worksheet are described in the table below Except where noted this information is printed on the Sample Report Immediately below the p
67. z wsonnj onid NOLLV OO NUSINON YONYAJALIALLOV YONA ALALLOV ALEHOVA 3I4N VS 3 I4INVS HIV 1VI01 WIAIA VS AG CALYVLS LNIOD ULEVO LNN09 VLITI VLADNI JOYS vjeq LPY sso 1 IYJ NVEMONILd ATW A10 8 108 UONBIPe Y pjuouruo mAu UOISIAI SIDALIS amp 10 U IOqU T Aypengd eu uro uz jo juourn redo q VUBISINO T JO 938 S Wig Appendix B Air Particulate Filter Gross Beta Data Sheet Gross Beta Analysis SOP 1259 112 September 8 2009 Page 46 of 65 Appendix C Alpha Beta Quality Control Worksheet CANBERRA TENNELEC S5E ALPHA BETA COUNTING SYSTEM QUALITY CONTROL DATA USING ANALYTICS CS 137 AIR PARTICULATE FILTER PLANCHETTE STD SRS 72654 1 STANDARD CALIBRATION DATE 09 15 06 STANDARD ACTIVITY DPM 20 298 CHI SQUARE VALUE MUST BE LESS THAN 37 6 PERCENT ERROR CALCULATION EXPERIMENTAL STANDARD STANDARD X 10 Date Day of a Bxga B erga p 8 count 2009 Week cpm Err Activity Error FRI 0 cpm cpm E o2 9 671 05 Jan MON Q cpm com NN 8 670 07 Jan WED Q cpm cpm E 8 668 09 Jan RI 0 cpm cpm EN 8 667 12 Jan MON Q cpm _ cpm E 8 666 14 Jan ED 0 cpm com 8 665 16 Jan FRI Q 8 663 59 700 roo O e lt lt 21 Jan ED 0 cpm cyn 8 661 23 Jan FRI Q cpm cpm TM 8 660 26 Jan MON 0 cpm cpm a 8 658 28 Jan WED 0 cpm cpm a 8 657 30 Jan FRI Q cpm cpm en 8 656 02 Feb MON Q cpm cpm pc

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