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1220 Quantulusä

1. Type to go to the READY state Type Lx RETURN to jump to line x 03 COINCIDENCE BIAS L H L gt H BLOCK 2 Line 4 Set MCA Configuration Line 4 is the beginning of the second program block in which the MCA configuration is set This determines which analogue signal is converted in MCA 1 and which is converted in MCA2 It also includes ADC trigger conditions inhibit and MCA memory split conditions The command line enables display modification and removing or disabling of an MCA For convenient use there is a selection of 2 preset MCA configurations configuration 1 for C counting configuration 2 for H counting Configuration 3 enables free set up of the MCAs Parameters when modifying the MCA configurations are ADC INPUT Analogue pulse to be converted by the ADC A list of the choices can be obtained by the HELP function ADC TRIGGER Logical signal which enables conversion of the analogue pulse The list can be obtained by the HELP function INHIBIT Logical signal which inhibits the conversion This is usually a signal from the active guard MEMORY SPLIT Logical condition which guides the converted pulse to the first or second half of the MCA If the condition is true the pulse is guided to Half 2 otherwise to Half 1 120 Mode 6 Quasi simultaneous counting program For MCA 2 modifications the same principles apply Print MCA configurations and control order are given
2. Note printout codes are explained in Ch 4 in Printout Selection Extended List Selection Line 14 1s the last line of the short parameter list The user is given the opportunity to continue with the rest of the parameters in the extended list or to return to the Ready state If N No is answered to the Extended Parameter List question the parameter setting will be terminated the parameter group updated with the parameter values set by the user and the word READY will be displayed If Y Yes is answered to the Extended List question the remaining parameters will be listed for editing starting with line 15 57 Mode 1 CPM DPM If this is answered with Y yes then the standard points if any will be listed one by one to allow editing or if there are no points data entry See Curve Edit for more details Line 16 Curve Fitting Method This allows selection of one of the three curve fitting methods Smoothing Spline Interpolation Spline or Linear Interpolation See Curve Edit for more details Line 16A Replot with Auto Run There are two types of curve plot which differ in their scales One is a so called full size plot designed for printout and the other a reduced size scale designed to fit the display Answering Y Yes to this first question on line 16A means that a full size plot will be printed out before the results during an automatic run i e normal sample measurement Replot with Curve Edit T
3. OA PROGRAM MODE 1 gt COUN ODE D WINDOW E SINGLE LABEL POSIT Y gt 60 00 gt 1 900000 gt E QUALITY MONITOR N gt OF WINDOWS 1 gt 5 320 gt STD TIME 0 15 gt STD COUNTS 900000 gt INT 1 2 5 7 21 22 8 10 Mea Mes s RROR 1 000001 ES UuwmghuouuWWWUU ugwWOO orooorkosozznz 0 84 Mode 1 CPM DPM Results Automatic Counting Start the instrument counting by typing A followed by the correct parameter group number and then press RETURN To stop automatic counting type letter O and press RETURN The instrument then returns to the READY state Radiation Safety Protocol The total sum of CPM or DPM counted in a batch is summed together and printed out at the end of the batch If DPMs are counted the printout of total DPM will also include the DPM value transformed to nanocuries and kilo Becquerels Thus a record of the activity handled can be kept by collecting these printouts in a binder or by giving them to the person responsible for the records of radioactivity in the laboratory Result reliability The long term stability of the counter is of utmost importance when counting large amounts of samples or when results which are counted at different times are compared I
4. 177 Installation Installation of the PMTs and External Standard 178 open the lead shielding door cut the bunch holders remove the preampilfier check the serial number of the PMT on the door of the lead shielding take the same numbered PMT from the box assemble the PMT to the socket of the preamplifier only one possible position to assemble assemble the preamplifier carefully with PMT back into the instrument keep the PMT angled up 10 15 degrees when inserted into the instrument tight the screws and insert new bunch holders close the lead shielding door carefully check that no cables between push on the ear of the door when tightening the screw door gets tight against the lead Installation install the pmt as on the right side install upper part of the external standard pipe before inserting bunch holders and closing door pull the stripe out from the lower part of the external standard pipe prevents the capsule from moving during the transportation push the upper half upper end into the bottom of the hole of the guard container joint the pipes together by tightening the joint Screw push on the rubber part of the external standard pump and listen that the external standard capsule moves freely inside the pipe Reassemble the lids and connect the instrument to the mains circuit having a protective earth 179 Installation 180 Instal
5. I 125 UAL LABEL H 3 ECHANICAL TE I 125 UA PM AUTO SQE PM FIXED SQE H 3 E PM FIXED SQE H 3 HE UASI EOUS COUNTING PROGRAM ERE UASI EOUS COUNTING PROGRAM S NON GM oM Ed Ed Ed F4 Ed Ed wee ou YH mOr oaaaanaa 1 2 3 4 5 6 7 8 EADY gt Parameter group editing Quantulus is designed to present to the user only those parameters which need to be set for the particular mode of operation selected by the user In what follows a description is given of all the possible parameters that can be set by the user in the CPM DPM counting mode 51 Mode 1 CPM DPM Sometimes where the description of a parameter requires more background information it is described in its own section as can be seen by looking at the subject index Parameter Setting Selection P Parameter setting is started from the READY state by typing control letter P and pressing Return The current date and time is then printed out automatically The section entitled Clock describes how this date and time can be set or adjusted Parameter Group Selection After the date and time have been printed out the question PARAMETER GROUP will appear A parameter group comprises all the parameter values needed to count a set of samples Eight parameter groups are stored in the memory of Quantulus each with an identifying number in the range 1 8 Normally a group
6. CPM DPM Mode 1 Parameters Chemiluminescence monitoring and subtraction Standard curve fitting DPMI measurements Half life correction Printout selection Repeat and replicates Results Sample quality monitor Standardization parameter setting Window setting 49 50 Mode 1 CPM DPM Mode 1 CPM DPM Parameter setting Note In newer user interfaces such as Queue Manager and WinQ the Term inal door must be used to access the following commands Instrument control commands Instrument control commands are available by typing in the READY state refer to Ch 3 Parameter Groups A parameter group comprises all the parameter values needed to count a set of samples Eight parameter groups are stored in the memory of Quantulus each with an identifying number in the range 1 8 Normally a group consists of preset parameters but these can be edited to produce a group of parameters just suited to the need of the user Listing Stored Parameter Groups Type L and press RETURN to see the parameter groups A list will be printed out showing the group number as well as the program mode count mode and name identifier of each group The list also shows if a quench calibration curve is stored with the group of parameters EADY gt L Type L and press RETURN to get a list of the stored groups WED 18 SEP 1996 14 44 FU ROGRAM E COUNT MODE ID PM FIXED SQE PM FIXED SQE CARBON STD CU PM FIXED SOF
7. Edit notes Window 1234567 8 Sample Parameters ORD POS ID PATHIS OFF CTIMECOUNTS CUCNTSMCWREP ST STMSSTIME 1 1 14C 2 00 Nolim Nolim 1 1 Y 1 10 1 00 2 2 3H 2 00 Nolim Nolim 1 1 Y 1 10 1 00 3 5 BKG 30 00 Nolim Nolim 1 1 Y 1 10 1 00 Once the settings are the way they should be press F10 and enter for saving the protocol Highlight Queue 1 and press F4 fur running the protocol The protocol will be sent to the instrument and the measurement is started For getting the live spectrum push Alt F3 simultaneously When the measurement is finished the results and the selected spectra will be sent to the PC and can then be analyzed by the SPA program SPA The SPA program is activated with F9 from the QMGR program and with F10 gt F1 for the Old program When calculating and plotting spectra GRAPH F8 or statistical plots STAT F6 or F7 the program suggests for example C up on screen 182 Installation of the PC ORD 01 POS 01 STD N REP 01 CYC 001 SP 11 gt The path for where the files are as well as the name of the files comes from the protocol used Saving path C TEST running number for each time Protocol name PERFTEST this protocol is started The name of the files Q Quantulus O1 99 Order number P1 60 Position number 01 99 Repeat number N S Normal External Standard 001 999 Cycle number 000 cumulative file In this case 14C C TESTI PERFTEST QOIP101N 001 3H C TEST1 PER
8. NPAC Pulse amplitude comparison not met G Guard pulse G EG Guard pulse in coincidence with external guard pulse EG External guard pulse optional L R Left and right detectors in coincidence PSA Pulse Shape Analyzer and combinations of the above For example EG G PAC means any of external guard guard or PAC or any two or three of them When the criterion is met the digital pulse goes to half 2 of the MCA Note for PAC LRC left right comparator and for PSA PSD pulse shape discriminator and PSM pulse shape monitor have been used in earlier versions of the Quantulus internal software A high coincidence bias can be selected for improved background and figure of merit for counting C or other high energy beta emitters in glass vials A pulse below the bias threshold cannot trigger the coincidence unit Additional glass vial background in Ch 1 300 is caused by beta particles from 40K such as Cerenkov and fluorescence and is thus cut off by high bias with only a small loss of true events from C External standard Under certain conditions the MCA configuration is locked This is when the external standard is counted or when program mode one or two is used Program mode one is the DPM program and mode two is the spectrum plot program The locked configuration is the following MCA 1 half 2 is used for the beta spectrum The guard is active as an inhibitor When counting the external standard guard is off the
9. Normalized pulse length vs pulse height for Ra 226 by Quantulus Norm d uid pulse Rn 222 Po 218 length PSA PSA level level Ra 226 gt s Po 214 Pulse height 3 D spectrum of Ra 226 vs pulse amplitude and pulse length normalized to pulse amplitude Wallac PSA excellency Operates simultaneously with and independently of the anticoincidence guard detector from which sample detector is optically isolated Ultra low level counting mode is thus enabled in the presence of PSA Wallac PSA works well in a large variety of cocktails without need to lengthen the pulse with any additives such as naphthalene Spill over of alphas and betas into each others spectra is typically less than 0 2 in 8 ml water mixed with 12 ml safe cocktail samples Wallac PSA works very well with both fast and slow cocktails without the need to add naphthalene to make the pulse slower Wallac PSA saves alpha and beta spectra Automatic scanning can be carried out with this software package to test for the optimum division of events Scanning can be made using any pure alpha and beta samples or by using a mixed alpha beta and background sample Usage of pulse shape analysis a for alpha beta separation and b extra background reduction in alpha and beta counting 23 The concept of total optimization a Most of the LSC background is composed of short pulses and thus falls into the beta spectrum while alpha background remains ve
10. Sample position number Sample count time External standard count time Counts in window 1 Counts per minute in window 1 background subtracted CPM1 corrected for half life if set and spillover if set and dual label multiplied by factor 1 Percentage error in CPM1 Disintegrations per minute DPM in window 1 multiplied by factor 1 Percentage error in DPM1 Efficiency in window 1 Counts in window 2 Counts per minute in window 2 background subtracted CPM2 corrected for half life if set and spillover if set and dual label multiplied by factor 2 Percentage error in CPM 2 Disintegrations per minute in window 2 DPM in window 2 multiplied by factor 2 Percentage error in DPM2 Efficiency in window 2 Isotope spectral quench parameter External standard spectral quench parameter Percentage error in SQP E Chemiluminescence as a percentage of window 1 CPM CPM in window 3 CPM in window 4 CPM in window 5 Corrected CPM in window 1 Corrected CPM in window 2 Percentage error in S P I Disintegrations per second in window 1 Disintegrations per second in window 2 Sample CCPM or DPM if selected in window 1 as a percentage of Reference 1 CCPM or DPM Sample CCPM or DPM if selected in window 2 as a percentage of Reference 2 CCPM or DPM Date of sample measurement ime of sample measurement Elapsed time since A or Q Return pressed unless Zero Time 1 set in which case this defines start time for S Half life secti
11. continue gt Printout codes are added to the list using the I nsert command It is possible to specify which printout which terminal 1 or 2 and the place in the printout of the inserted items By typing IB3 the codes typed in after the write mnemonic printout codes question are inserted before item number 3 in the printout list for terminal 2 B terminal The number given in the printout code is the order number for the item in the printouts set by the instrument The order number is used when inserting or removing printout codes Line 7 Send Spectra It is possible to send the spectra together with the printout to the computer on terminal 2 The spectra can then be stored together with the other information of the sample given by the printout Thus an off line data analysis of the total measured data is later possible using the Spectrum Analysis program If the Quantulus is used together with the Laboratory Computer the four spectra are sent together and stored under a unique file name created by the system The transferred spectra are determined by the following codes A All 4 spectra N No spectrum output 11 MCA 1 HALF 1 12 MCA 1 HALF 2 21 MCA 2 HALF 1 22 MCA 2 HALF 2 S External standard spectrum 125 Mode 6 Quasi simultaneous counting program The spectra output can be combinations of these i e 11 21 S gives MCA 1 HALF 1 MCA 2 HALF 1 and the external standard spectrum The preset value is all s
12. lt 34 35 36 37 38 395 40 CPM7 COUNTS7 CPM7 CPM8 COUNTS8 CPM8 Selected printout for terminal 2 B Le 2 23 4 5x 6 75 8 9 10 11 CYC POS REP TIME DTIME1 DTIME2 CUCNTS SOP SOP STIME lt 12 T3 T4 15 16 17 18 19 ID CPM1 COUNTS1 CPM1 CPM2 COUNTS2 The printout for a particular output port can be inserted selecting control character I followed by a number 1 or 2 If both output ports are selected then I alone is sufficient Selecting this control command causes the parameter line WRITE MNEMONIC PRINTOUT CODES The printout codes are typed in in mnemonic form separated by spaces A list of the printout codes is obtained with the HELP function for the line 124 Mode 6 Quasi simultaneous counting program COMMAND Display Remove Insert Preset lt ret gt continue gt I WRITE MNEMONIC PRINTOUT CODES gt Help Selectable printout codes POSITION ID CTIME CYCLE DATE TIME REPEAT STIME CPM1 CPM2 CPM3 CPM4 CPM5 CPM6 CPM7 CPM8 COUNTS1 COUNTS2 COUNTS3 COUNTS4 COUNTS5 COUNTS6 COUNTS7 COUNTS8 DTIME1 DTIME2 CUCNTS INSTR SQP SQP CPM1 CPM2 CPM3 CPM4 CPM5 CPM6 CPM7 CPM8 8SPACES 17SPACES lt lt New line Type in required codes separated by space RETURN only no insert WRITE MNEMONIC PRINTOUT CODES gt COMMAND Display Remove Insert Preset lt ret gt
13. Dx y Display orders from x to y If y omitted order x displayed If x y omitted all displayed Mx y Modify orders from x to y Ix Insert order before x If x omitted insert at the end Cx y Copy order x and insert copy before y P Path on off If path is on sample ID is added to directory path and spectra of each order will be in own directory RETURN or exit to next line Rx y Remove orders x to y Inserting an Order into the sequence of Orders This command allows a new order to be created This command must come first if the group has been cleared because then there is no Order Here order number 4 is inserted in the sequence and the parameter values are set 117 Mode 6 Quasi simultaneous counting program COMMAND Display Modify Remove Insert Copy Path lt ret gt continue gt I Modifying order 4 POSITION s 0 gt 3 6 E gt TESTRUN COUNTING TIME 60 00 gt 2 CUMULATIVE COUNTS NO LIM gt 360000 WINDOW OF COUNT LIMI gt Help Window which counts terminates counting Range 1 8 Type to exit to command line COUNTS NO LIM gt WINDOW OF COUNT LIMI gt REPEATS 1 gt 2 EXTERNAL STANDARD N gt odifying order 5 POSITION s 0 gt COMMAND Display Modify Remove Insert Copy Path lt ret gt continue gt Creating a Copy of an existing order If an Order exists then a further copy of
14. Note SQP I can only be used for single label samples SQP I is not well defined for low activity samples for which SQP E is always recommended The DPM program offers additional benefits quench curves can be edited and replotted thus different curve fitting methods can be tested to see which will give the best result The questions concerning editing and plot are in the extended parameter list A complete set of standard points can manually be typed in thus if the standard points are deleted by mistake the standards need not be counted anew Quantulus can be used as a DPM calculator DPM results can be manually counted The CPM value and quench indicator value can then be manually typed in ry Mode 1 CPM DPM Half life correction One of the characteristics of radioactive decay is the half life that is the time in which the activity has decayed to half of the original The decrease in activity is exponential and each isotope has its specific half life If the decrease in activity is noticeable when compared with the time between the first and last sample in a batch a considerable error is introduced and the results within the batch can not be directly compared with each other e g a count of P lasting 24 hours gives results 5 too low by the end of the batch Quantulus makes automatic half life correction for single or dual labelled samples if required by the user Half life corrected CPM values are obtained by giving
15. POWER FAILURE will be displayed 2 mins after power is switched on Press to go to the READY state 5 Set the clock see the section entitled Clock Instrument description The concept of total optimization Detector shielding Multiple multichannel analyser technology Pulse shape analysis Pulse amplitude comparison Program modes 10 The concept of total optimization The concept of total optimization Introduction To enhance the accuracy of low level counting all factors which affect the counting have to be considered This can be defined as total optimization The design and construction of Quantulus enable the optimization of the counting conditions and data validation for various applications This is achieved by optimized design for background reduction measurements based on multiple multichannel analyzer MCA technology random access variable time base counting electronic noise suppression and a high capacity personal computer for storage and post assay validation and optimization In addition the special teflon counting vials give a choice of the most suitable vials for different sample volumes Shielding As the detection limit is determined by the signal to background ratio or more specifically by the error in the background determination this places the following demands on instrument performance the background must be minimized the instrument must be stable during the long counting times
16. for example in radiocarbon dating and in the analysis of environmental radioactivity 15 The concept of total optimization Detector shielding The low background levels obtained with the Quantulus are comparable with those obtained with installations made underground in special laboratories This is achieved by the unique detector shielding which consists of a passive and an active shield Passive shield The Passive shield is graded first the asymmetric lead shield and a layer of copper of the active liquid scintillation guard container The lead shield total weight 630 kg is asymmetric which means that it is thickest 20 cm above the measuring position Shielding is needed most above the measuring chamber because the intensity of cosmic radiation is higher from above the earth attenuates radiation coming from below The thickness of the shielding to other directions is 7 11 cm which is sufficient for attenuation of the gamma radiation in the instrument surroundings The asymmetrical shape gives improved shielding against both cosmic radiation and radiation resulting from interactions between cosmic radiation and the shielding material The lead X rays induced by cosmic radiation are partly absorbed by the copper wall of the container of the liquid scintillator guard The signal threshold is adjusted below the thermal noise of the phototubes thus allowing the detection of the smallest signals triggered by external radiation in the
17. 1024 2 1 8 1 1024 2 2 128 Mode 6 Quasi simultaneous counting program COMMAND Display Modify Remove lt ret gt continue gt 06 SET PRINTOUT Y Selected printout for terminal 1 A 1 3 4 95 6 gie 88 9 REP CTIME DTIME1 DTIME2 CUCNTS SOP SQP STIME lt 10 11 12 19 14 15 1 6 17 ID CPM1 COUNTS1 CPM1 CPM2 COUNTS2 CPM2 lt 18 19 20 21 22 23 24 25 PM3 COUNTS3 CPM3 CPM4 COUNTS4 CPMAS lt 26 2 28 29 30 31 32 33 PM5 COUNTS5 CPM5 CPM6 COUNTS6 CPM6 lt 34 35 36 33b 38 395 40 CPM7 COUNTS7 CPM7 CPM8 COUNTS8 CPM8 Selected printout for terminal 2 B 14 5235 2 Bie 4 5 6 he 8 9 104 T4 CYC POS REP CTIME DTIME1 DTIME2 CUCNTS SOP SOP STIME lt 12 13 14 T5 16 17 18 19 ID CPM1 COUNTS1 CPM1 CPM2 COUNTS2 CPM2 lt COMMAND Display Remove Insert Preset lt ret gt continue gt 07 SPECTRA SENDING CANNOT BE EDITED This parameter cannot be edited 08 LISTING Y This parameter and the next can be edited 09 INSTRUMENT NUMBER do lt gt SAVING PARAMETER GROUP 7 EDIT Command ended by pressing R Parameters Queue List groups Clock Resume gt R Editing is COUNTING R ED E E ESUM 129 Mode 6 Quasi simultaneous counting program 130 Specifications and Routine maintenance 131 132 Specifications Spe
18. 16 gt LISTING TIMI 10 0 COUNTS 1 5000 COUNTS 2 5000 SAMPLE QUALITY MONITOR NUMBER OF WINDOWS WINDOW 1 5 30 DOW 2 100 60 RNAL STD TIME Que AL STD COUNTS 90000 1r25 13 217 227 9 200 C Oo 0 1 O1 4 WH H AUTO R H CURVE E FITTING 17 D SAMPL D SUB gt T E 18B 2 0 gt 20 PE 2 PL i gt 22 E PREP E 0 gt 26 R 1 gt 27 1 000001 gt 28 IFE 1 0 gt 29 i LIFE 2 E gt 30 ER OF CYCLI gt 3l FERENCE 1 0 gt 32 RENCE 2 0 gt Unknown dual label samples are counted POS CTIME CPM1 CPM2 S P E E DPM1 DPM1 013 10 01 39 95 98 14 868 27 1 9 12900 014 10 01 80 53 195 99 866 43 15 2 54 117 015 10 01 157 26 372 95 856 55 14 9 86 207 016 10 01 166 54 374 29 850 82 22 5 61 071 TOTAL COUNT RATE 1485 7 CPM TOTAL ACTIVITY 1180 3 DPM 5 nCi CONVEYOR CLEARING READY gt 96 Mode 1 CPM DPM Window setting The Quantulus has built in window setting for six common isotopes in both single and dual label combinations These settings give the optimal windows for unquenched samples If there is quenching the isotope spectrum will be shifted to lower energies In order to keep the spectrum within the counting window you should adj
19. 46 1996 26 The concept of total optimization Pulse amplitude comparison PAC Introduction The Pulse Amplitude Comparator provides a means for decreasing the background component produced by optical crosstalk in liquid scintillation counting Physical background A considerable amount of the background in liquid scintillation counting is produced by fluorescence and Cerenkov phenomena in the photomultiplier tubes due to cosmic rays environmental gamma radiation and residual radioactive impurities in the materials of the detectors themselves Typically the corresponding coincidence pulse comprises a relatively large amplitude component from the affected tube and a small amplitude from the other tube which may also detect some of the photons emitted so called crosstalk The sample scintillations in the vial on the other hand produce coincidences with a much smaller relative difference between the component amplitudes from the individual photomultipliers How PAC works Pulse amplitude comparison can be explained as follows The coincidence pulse consists of an output component from both individual photomultipliers Obviously then the smaller greater ratio between the amplitudes of the two components has a value ranging from nearly zero the amplitudes are highly different to unity the amplitudes are equal Due to the above reasons smaller greater ratios of sample coincidences are distributed closer to unity than those of crosst
20. 62 75 1 16 1 38 5 509 29 40 34 I 1 13 Curve replotted with five points only I y y y y y TE Oor T KOK KK KKK KK 90 0 KKKKOKKK I kkk kkk k I KORK E KKK KKK 70 0 xx I H HHH HHHH HHHH H EFFICIENCYS 550 600 650 700 750 800 850 900 USEFUL SOP E RANGE 509 904 Gl UNKNOWNS N gt L16 Jump to line 16 to change fitting method SS gt LI Smoothing Spline changed to Linear Interpolation UN Y gt Curve replotted with new method EDIT Ni Sy 173 Mode 1 CPM DPM ISOTOPI WINDOW 1 LINI ERPOLATION FITTING TABLE E EFF DEV WEIGHT There is no deviation shown in this 95 95 95 00 1 14 table because linear interpolation goes 43 88 37 00 1 17 through all the points 223 81 37 00 1422 43 62 75 00 1 38 5 40 34 00 1273 This curve is replotted using linear interpolation to fit the points EFFICIENCYS KKKKOT KKKKKKKKK KKKOK KKK KKKKKKKK KORK kkk KKK O I I I I I I Hs I ale I I I 600 650 700 750 800 EFUL SOP E RANGE 509 904 CALCULATE UNKNOWNS N gt L15 Jump to line 15 again for further editing 15 CURVE EDIT X gt ISOTOPE 1 SOP E EFF1 WEIGHT 903 95 95 95 14 gt 785 43 88 37 17 gt 37 22 700 81 37 1
21. By choosing window 4 and step 4 the plotted spectrum will be a copy of the displayed spectrum The interesting channel area can be specified When mode 2 is selected the heading SPECTRUM PLOT PARAMETERS will be printed out followed by the parameters themselves Line 01 Position As in Mode 1 the free ordering of every sample in all of the three trays is allowed Each sample is specified by its position number 1 60 so each sample will be counted in the order in which its position number is specified on parameter line 1 Each position number is separated from the next by a comma If several samples are to be counted in numeric order they can be specified by giving the first and last numbers of the sequence separated by a hyphen Line 40 Parameter Listing If answered Y Yes it provides a printout of the Spectrum plot parameters before results are printed Line 41 Spectrum Selection The user can select either to have the sample spectrum or the external standard spectrum Line 42 Counting time The time in minutes seconds S or hours H for which the spectrum is to be accumulated is specified on this line Line 43 Maximum Counts The maximum number of counts in the area of interest is specified here 101 Mode 2 Spectrum plot Line 45 Area of Interest The number of channels to be plotted out should be given on this line The range is from 1 to 1024 Line 46 Window Width This parameter allows the user to
22. C counting mode The active guard performance and the intensity of the background can be monitored during counting by the following two methods 1 MCA 2 is used for measuring the spectrum of the guard As the guard detector electronics is similar to that of the beta detector the energy spectrum caused by the background radiation in the guard can be measured Also the MCA configuration for MCA 2 can be selected so that in the second half the guard pulses coincident with pulses in the beta detector are measured and in the first half all the other or anti coincident pulses are measured The latter pulse rate is not to be expected to stay stable because it is affected by the variable cosmic flux which is dependent on the Sun s activity and on the atmospheric pressure or amount of air mass above the instrument 17 The concept of total optimization LIQUID SCINTILLATOR E UNIT fl N Tanatos TRIGGER A D CONVERTER MCA SPLIT MCA1 MCA1 HALF1 HALF2 2 If the logical guard signal is used as a memory split signal for MCA 1 then MCA 1 half 1 will contain the sample spectrum in anticoincidence with the guard and MCA 1 half 2 will contain the spectrum of the pulses in the beta detector coincident with the guard MCA1 half 1 contains therefore accepted counts from the sample half 2 contains rejected counts More details on the MCA co
23. COUNTING Y gt SE Data to be filed in PC Y N Y gt N ISOTOPE 1 STANDARDIZATION CPM1 EFF1 ERR1S CPM2 5751 93 67 67 65 4430 81 3014 48 35 46 76 1534 33 1486 92 17 49 96 475 63 520 43 6 12 1 47 91 98 159 96 1 88 2 55 22 36 CONVEYOR CLEARING ISOTOPE 1 WINDOW 1 SMOOTHING SPLINE BUSY CALCULATING S E P 00 0 0 T 00 00 The last three columns in the fitting table explain the symbols used in the plots FITTING TABLE SOP E EFF EV WEIGHT POINT CURV ERR LIMIT 906 67 00 69 783 35 00 87 692 Ld 00 215 593 6 00 70 508 L 00 07 9 Mode 1 CPM DPM ISOTOPE 1 WINDOW 2 SMOOTHING SPLINE Di BUSY CALCULATING S E P 00 0 0 FITTING TABLE WEIGHT POINT 00 92 ERR LIMIT Mode 1 CPM DPM Standard curve showing results for isotope 1 in tritium and carbon windows ISOTOPE 2 STANDARDIZATION CPM1 EFF1 ERRI1 2641 81 26 68 STO 5362 95 54 17 67 7350 60 74 25 67 6109 55 61 71 64 4040 92 40 82 71 CONVEYOR CLEARING ISOTOPE 2 WINDOW 1 SMOOTHING SPLINE BUSY CALCULATING N S E P 1 00 1 1 00 VIZ V2 00 FITTING TABLI SOP E EFF DEV WEIGHT POINT CURV ERR LIMIT 902 83 26 68 00 91 785 0
24. LABELS ARE PERMANENTLY ATTACHED TO THE EXTERIOR REAR PLATE OF THE INSTRUMENT 1 2 5 Suhde 1 4 5 1 154 1390 3693 I gt DECLARATION OF CONFORMITY FOR CE MARKING INSTRUMENTS PerkinElmer life sciences We Supplier s name WALLAC OY Address PL 10 20101 TURKU FINLAND declare under our sole responsibility that the product Name type or model lot batch or serial number possibly sources and numbers of items 1220 QUANTULUS LIQUID SCINTILLATION COUNTER Valid from serial number 2200195 to which this declaration relates is in conformity with the following standard s or other normative document s Title and or number and date of issue of the standard s or other normative document s EN 50082 1 1992 EN 50081 1 1992 EN 61000 3 2 1995 A1 1998 A14 2000 EN 61000 3 3 1995 EN 61010 1 1993 if applicable following the provisions of the following directives Electromagnetic compatibility EMC 89 336 EEC Low voltage LV 73 23 EEC Date and place of issue 16 August 2001 TURKU FINLAND Name and signature or equivalent marking of authorized person Pekka Makinen Quality Assurance Manager 155 156 Installation Low background counting requirements Installation instructions 157 158 Low background counting requirements Low background counting requirements Achieving stability The most important factor for the low level counting procedures is the stabil
25. MCA pe OTT OUT ALOIS een 33 External standard 2 ea e e ha cies 37 General features A dd 41 Ouiputde VIGES AAA AAA dis 41 Commandsinthe READY Ae eb ease eit eum eut den sd a m S Ames 42 Information control coTmmadrid e 42 Calendar ClO Ck d H 43 Help TUBellOnca incidi i A bu dtes quede ty cha a alicia Vote quie Gi dibus planet d 44 A O rM eser eo dox ea equi eue 44 Starting A ten ecce Ra 44 Display and multichannel analyser iue dts di eer dieti o neri dia 46 Error messi E Seeron pH Sc x EA I ea lau aqu a nude Rte ee 47 Mode 1 CPWDP Masas 51 Parameter selline da 51 Chemiluminescence monitoring and subtraction sssssssssseseeeeeeeeere nenne 66 EAA E EE EETA TA EE S E E c E TA 69 DEN nee ers 76 Half life esrtecton ee 78 PrIMOUN Dee 79 Repeats and qepHediel a e eaten le lo a dal to a aS 82 O 85 Sample Quality TUOBIOE di iii 86 Standardization parameter setting ins asics 87 A nennen len 97 Mode 2 AAA A A N 101 Mode 6 Quasi simultaneous counting program essssssssnsssssnnssnonnsnnnnnennnnnsnnnnnennnnnennnnnennen 113 Intr duction ar TE 113 BEOCR Vai Er A EA Re 115 BROCAS do a 120 BEOCK a RO 123 BEOCKA E n 124 Storing the parameter group sx esie eire Ener Rn 127 Editing while counting as 127 Contents Si Us PCIE T C IIT 133 Physical MEANS a 133 POWELL A ee Ud domes u tes ie Nu LS acini e 133 Connections TIPU elf DUE eos Od n 133 Rad
26. Quasi Simultaneous QS counting mode The QS mode enables the full use of the possibilities the Quantulus gives for data validation The QS mode enables random access to the sample changer individual time base for samples free setup of the multichannel analysers and most important of all Windowless Counting based on spectrum analysis The term windowless counting means that spectra are measured and then sent to a computer Even rejected count spectra can be saved if needed Optimization of the counting window can be done off line based on the information of the total spectral content Quantulus can store 8 counting protocols or parameter groups in non volatile EEPROM memory A counting protocol can be any of the three program modes modified so that it suits the application in question If CPM to DPM conversion is used the quench curve is also stored in the EEPROM together with the counting protocol The counting protocols are run in the order determined by the user by setting up a queue in which the order is specified A virtually unlimited number of mode 6 protocols parameter groups can be saved and sent to Quantulus with newer user interfaces such as Queue Manager Program mode 1 CPM DPM Program mode 1 gives the CPM results for up to 8 counting windows which can be freely set to cover any part of the spectrum In addition CPM to DPM conversion average of repeat counts or replicate samples percentage of reference sample etc is enable
27. Window 1 12External Std time 14 Print 15 2 2720524 15 Curve Edit 16Curve Fit 16A Replot with Auto Run Replot with Curve Edit 17Background sample 18A Background Sub 1 20 Repeat 20A Repeat Plot 21 Replicate 22Sample Prep 26Factor 1 28Half Life 1 30Number Cycles 31Reference 1 Error POS CTIME CPM1 T Y 0 30 900 000 N Ji 5 320 0 15 1 00000E0 SQP I SQP E Change the following memory locations see 1220 service manual section 5 EJJ MCA interface measurement configuration table READY gt T SERVICE gt PR 2A03 2A03 01 2A04 SERVICE PR 2180 2180 03 2181 00 2182 03 Test service mode Program Ram memory location 2A03 01 other memory changes will be valid back to service prompt Program Ram memory location 2180 digital pulse select 03 gt L R inhibit pulse select 00 OFF LSB select 03 gt LSB 1 186 Installation of the PC 2183 0D analogue pulse select 0D gt L R 0E 0E gt R OF OF gt L 2184 back to service prompt SERVICE gt RE back to ready prompt depended of which side is calibrated Select the spectrum of the left side 2183 OF and start the measurement with the unquenched H 3 glass vial which is supplied with the instrument Use the parameter group edited on previous page Adjust using trimmer R89 EL on FAD the SQP I to be according to the table subtracted with 4 channels on next page Sel
28. answering Y Yes 87 Mode 1 CPM DPM on the parameter line If N No is answered there will be no automatic plot of quench curve and measurement of unknowns these are subject to user control and thus allow the possibility of curve editing before unknowns are measured It also means that any of the three quench standard measurement methods including the manual one can be used When using the standardization program only certain combinations of automatic run and automatic window are allowed with particular quench calibration methods These are shown in the following table Line 03 Standardization Method There are three methods as described in the DPM section of this manual If the fixed window manual run has been selected any of these can be chosen 1 e Manual HatTrick or Series but if an automatic run has been chosen then only HatTrick and Series are allowed Note 1210 126 HatTrick kit is not available any more from Wallac Line 04 Isotope DPM The DPM s for the isotope or isotopes being used in the quench standard measurement must be given on this line Line 05 DPM percentage error The uncertainty in the DPM value given on line 04 can be given as a percentage of the isotope DPM Line 06 Starting SQP value A quench curve establishes a relationship between the efficiency of measurement of a standard and the spectral quench parameter SQP T or SQP E This parameter allows maximum SQP value to be given
29. be necessary to use an uninterruptable power supply The cooling unit may be left connected directly to power line but the computer has to be fed through the uninterruptable supply if Quantulus is connected there in order to ensure continuous operation Addition of lead or low activity steel plates around the Quantulus is another way to improve the background but leads certainly to a significant mass of material see below for surface loads The anticoincidence guard counter spectrum in its Compton continuum region reflects the changes in the environmental gamma flux although attenuated by the additional shielding 160 Low background counting requirements effect of the lead e g in the Wallac low level laboratory the continuum drops only to one half of the one seen in the normal environment Incandescent lighting is recommended and sunlight should not have access to the counting room It is recommended that only background samples are prepared and stored in the counting room One should check for the background changes of high activity gamma sources outside the counting room caused by moving the sources for instance A pulsed accelerator in the distance may be source of variable background too Other factors Humidity Quantulus is able to run in a high humidity environment but then a container should be placed under the condensed water outlet In extremely dry atmosphere less than 10 rel humidity there is a danger of static e
30. been answered thus 16A REPLOT WITH AUTO RUN gt Y After curve edit a small scale curve is plotted out after Y is answered to the second part of this parameter line 16A REPLOT WITH CURVE EDIT gt Y Due to the limitations of the matrix printer and the small area involved several asterisks may appear on one line A small scale curve can be converted to a full scale curve by following procedure 11 given above This parameter reverts back to N after a curve has been plotted 69 Mode 1 CPM DPM In the FITTING TABLE printed prior to curve plotting the WEIGHT means the initial uncertainty of each standard point The larger the weight the bigger the uncertainty If Smoothing Spline is chosen the following list is an explanation of the characters printed prior to the fitting table N number of curve fitting attempts 1 6 S smoothing factor measures the ease of smoothing the fitted curve The larger this is the more difficult it is to make the curve fit smooth E the number of maxima and minima values of the curve these should be eliminated during curve fitting TP number of turning points of the curve F fitting factor the lower the value the better the fit T quench level value SQP T or SQP E where the curvature of the curve changes turning or inflection point Curve edit When the standard points information is being printed out after Y and RETURN have been typed in
31. consists of preset parameters but these can be edited to produce a group of parameters just suited to the need of the user The response required is to give the number of the group of parameters to be listed and if required edited Select one of these groups by typing the number and pressing Return There are a number of other possible responses to the Parameter Group question Copying Parameters Mx y This command copies parameters in one parameter group represented here by x into another group represented here by y The parameters in group x remain unchanged whereas those in group y are overwritten by the ones from group x Select parameter setting WED 18 SEP 1996 14 45 PARAMETER GROUP gt M3 4 Copy values from group 3 to group 4 SAVING PA ETER GROUP 4 Press RETURN to end the line The program goes to the READY state Copy can be helpful if a user wants a parameter group similar to an existing one without changing the existing one and without having to enter all the parameters one by one in a new group especially if a standard curve is stored in the first group Once parameters have been copied to the new group any changes can be made to that second group without affecting the first group After the copy operation the program returns to the READY state Clearing Parameters Cx Parameters in a group can be cleared and reset that is returned to the default values which are built int
32. guard detector LIQUID SCINTILLATOR FE LEAD ES COPPE 16 The concept of total optimization Active Shield The active shielding is the asymmetric liquid scintillator guard The guard is a cylinder in which the beta detector is fitted in a tube This tube is off axis thus the scintillator thickness is greatest above the measuring chamber and the photomultiplier tubes The active element in the guard is a mineral oil based scintillator Two photomultiplier tubes are used to detect scintillation in the guard Fast cosmic particles can cause Cerenkov radiation in the glass of the PM tubes To avoid this being accepted by the instrument and contributing to the background the active guard also covers the PM tubes so these pulses are inhibited The function of the active shield is the following Ionizing radiation i e gamma and cosmic radiation which moves through material leaves a trace behind this is in the form of excited atoms and molecules In the active guard the excitation creates scintillations which are detected by the photomultiplier tubes of the guard detector The pulse in the guard detector activates a logical signal If this signal is coincident with a pulse in the beta detector it can be used to inhibit the analogue to digital conversion of the pulse or to cause the converted pulse to be stored in Half 2 of the MCA
33. guard detector pulses summed lt GL GR GL Left guard detector pulse GR Right guard detector pulse EG External guard pulse optional Help Digital pulse select A D conversion TRIGGER pulse L R Left and right detectors in coincidence L R either left or right pulse or both exist L Only left detector pulse R Only right detector pulse DCOS Left and right in coincidence or delayed left in coincidence with right L R DL R G EG Guard pulse in coincidence with external guard pulse G EG Guard pulse or external guard pulse G Left and right guard pulses in coincidence GL Left guard detector pulse GR Right guard detector pulse EG External guard pulse optional Help INHIBIT SELECT conversion inhibit pulse N No inhibit pulse PAC Pulse amplitude comparison met NPAC Pulse amplitude comparison not met G Guard pulse G EG Guard pulse in coincidence with external guard pulse EG External guard pulse optional L R Left and right detectors in coincidence PSA Pulse Shape Analyzer and combinations of the above For example EG G PAC means any of external guard guard or PAC or any two or three of them When the criterion is met it causes an inhibit pulse This pulse prevents a digital pulse from being sent to MCA 36 The concept of total optimization Help MEMORY SPLIT SELECT Selection of MCA half for converted pulse N Half 1 always PAC Pulse amplitude comparison met
34. guard is off and the spectrum is stored in MCAI half 1 SQP E evaluation is done in two phases 1 the external standard is present and the sum of sample and Compton recoil electrons from gamma interaction is recorded and saved 2 the external standard is removed and only sample is counted at the same time as in phase 1 Net external standard spectrum and SQP E are calculated from the difference of the recorded spectra 37 The concept of total optimization 38 General features Output devices Commands in the READY state Information control command Calendar clock Help function Sample handling Starting counting Display and multichannel analyser Interrupting Counting Error messages 39 40 General features General features Output devices Output Ports The Quantulus has two output ports called Terminal 1 or A and Terminal 2 or B Simultaneous use of both terminals is not possible if one terminal is used the instrument will ignore all commands typed in on the other terminal The data output is freely selectable for both ports Also any or all of the possible 4 measured sample spectra and the external standard spectrum can be sent to the PC via port 2 Using the Video Terminal Optional When operated via a video terminal connected to Terminal 1 the following points must be observed The on line light must be on the light is situated on the upper left corner of the keyboard The caps lock key must be pr
35. is high 98 the observed deviation is abnormally small because there is then a 98 probability that a random sample from a correct distribution would have a larger 82 Mode 1 CPM DPM chi square value The probability should be between 5 and 95 for a good fit of the observed distribution and the theoretical one The number of observations cycles repeats must be 30 or greater before any definite conclusions can be drawn about the fit If the number of repeats or replicates is equal to or greater than 5 the additional questions REPEAT PLOT or REPLICATE PLOT are asked If answered Yes the instrument will after printing out the results print out a trend plot showing the distribution of the results around the average value in the plot the 90 and 99 confidence limits and the confidence intervals are indicated After the distribution plot a frequency plot is obtained The range between the highest and lowest result is divided in to a number of intervals depending on the number of repeats or replicates The number of results in each interval is then plotted 83 Mode 1 CPM DPM READY gt A Data to be filed in PC Y N Y gt 1 assay in queue PARAMETER GROUP NUMBER 0 gt 5 DIRECTORY PATH USRINH3TEST 2 assay in queue PARAMETER GROUP NUMBER 0 gt COMMAND Display Modify Remove Insert List groups Start counting gt S EP 1996 10 40 PARAMETER G ID REPEAT
36. light detection and the electrical parts of the photomultiplier are corrected for giving a guaranteed stability in the CPM from a sample of 0 2 per 24 hours having allowed for the normal statistical variation in the CPM value due to the nature of radioactive processes PREAMP COINCIDENC COUNTING CIRCUITS HIGH VOLTAGE E E VOLTAGE As the HV is automatically adjusted to the correct value it is possible to switch it off when not needed In Quantulus the HV is only switched on when the sample is in the measuring chamber which increases the photomultipler life time and performance 12 The concept of total optimization A further benefit is that there is no need for a complicated double light shutter to protect the detectors when the sample is being lifted into the chamber because the detector HV is off at that time The sample elevator acts as the light shutter when the sample is in the measuring chamber see the figure This makes the system mechanically much simpler and more reliable JRING CHAMBER NOU a em Em gt A a Bee SAMPLE a LEVATOR Random access counting Low level counting generally includes the counting of standard and background samples together with unknown samples The counting time is divided into several parts so that the samples are c
37. list of printout codes but these can be changed by the user like any other parameter A maximum of 33 codes or characters can be set Each printout code set on line 14 causes a preset column heading to be printed out when count results are being printed out Then the numerical values for the items selected are printed out row by row each under its own column heading Two symbols and allow the user to edit the printout selection line without retyping the whole line If printout codes are to be added the should be typed followed by the codes to be added 14 PRINT 1 2 40 6 gt 4 32 would add codes 4 and 32 to the existing list so that it becomes 14 PRINT 1 2 40 6 4 32 gt Similarly the symbol allows printouts to be deleted so 14 PRINT 1 2 40 6 4 32 gt 6 32 leads to the printout selection list 14 PRINT 1 2 40 6 gt Both these symbols can be used on the same line e g 14 PRINT 1 2 4 5 gt 12 13 4 5 which gives 14 PRINT 1 2 12 13 The order does not matter so gt 4 5 12 13 79 Mode 1 CPM DPM would give the same result Text can be added to the printout in the form of one or more extra columns E g the text could be added to the printout selection during actual printout the text would appear on every line in the position specified The effect of the printout editing can be checked by jumping back to line 14 using the L14 command 80 Mode 1 CPM DPM Printout
38. scintillation counting see the figure below The higher the sample quench is the poorer the resolution High quench as in 8 ml water mixed with 12 ml cocktail effectively merges the Ra Rn and Po peaks into a single broader one The high energy Po peak remains separated Alpha and beta particle spectrum of Ra 226 measured in a Wallac liquid scintillation counter Resolution is also affected by the vial choice translucent vials scatter light and offer better resolution Teflon is the best standard glass vials give poorer energy resolution ref 1 During long storage of a sample deterioration of energy resolution may occur because of the accumulation of alpha emitters on the surface of vial This leads to a smaller geometrical factor than unity for decays occurring on the surface The alpha particles may also be partly absorbed in the wall Poorer energy resolution and counting efficiency will result alpha peaks creating a low energy tail The aging effect can be avoided by adding acid e g HCl in 0 1 0 5 M concentrations 25 The concept of total optimization Pulse shape analysis and plastic vial effect Fast cocktails such as the ones containing toluene xylene and pseudocumene will penetrate into the plastic vial wall resulting in deterioration of the alpha spectrum and instability of the alpha count rate Plastic vials are not recommended for counting using these cocktails instead teflon coated plastic vials glass
39. specify how many channels are to be summed together to produce one line on the printout plot If the window width is very small i e one or two channels then the number of counts accumulated per channel could be quite small producing a ragged plot due to statistical variation A reasonable window width produces a clearer spectrum A width of 4 produces an identical spectrum to that on the display If the window width is too great the peaks in the spectrum can be lost A good idea of what width to select can be obtained by looking at the spectrum display Line 47 Step This parameter specifies how many channels one window starts after the start of the previous one If the step number is the same as the width then the windows follow exactly one after each other If the step is less than the width the windows overlap and if it is greater there will be channels not included in the printout Line 48 Repeat The number of times a sample is to be counted and hence the number of plots for each sample is specified here Line 49 Width of printer output This parameter allows the user to make the best use of the printer output by adjusting the size of the plot to the best width for the printer paper or display The units are printer characters Note the printout includes 23 characters of information before the plot line If 80 is selected for the print width the plot will be 57 characters wide Note Spectrum Analysis Program gives access
40. system diagram sse 1036 0835 CE CODO dI C os o o ener ne Tee 1390 3693 145 146 1099 0209 November 1995 Evaluation of the safety of the Eu 152 external standard source in Wallac 1220 Quantulus ultra low level spectrometer Isotope Europium 152 Maximum activity 37 kilo Becquerels 1 microcurie half life 13 5 years Origin of radioactive material The Eu 152 radioactive material is made by the Radiochemical Centre Amersham England Manufacturer of the standard capsules The Eu 152 standard capsules are manufactured by Wallac Oy Finland Manufacturing process The manufacturing process by which the radioactive standards are produced involves two steps the preparation of the radioactive material and the encapsulation of this material with a metal cover In the manufacturing process the active Eu 152 solution is absorbed homogeneously into crystalline synthetic zeolites in such a way that the activity of each active source is 1 uCi The construction principles of the capsule are described in document 1036 0835 ISO test The capsule has been tested by the Quality Assurance department of Wallac Oy according to the ISO 2919 standard The rating C43334 has been achieved External standard transport system The transport system is illustrated in document 1036 0835 The construction with dimensions is illustrated in document 1036 0841 Disposal of the capsule When the instrument is no longer in us
41. the stand in the centre of the front of the instrument see picture assemble the two resting legs according to the numbers on the leg and instrument Installation Unpacking the Lead Shielding cut the stripes open the Phillips screws down on the box lift the box carefully over the lead remove the wooden plates and the planks with which the lead shielding is attached to the stand 169 Installation Installation with a fork lift truck lift the lead shielding up with the truck so that the forks are only 2 5cm over the edge of the lead Note On the front of the lead shielding are the hinges for the doors and at the rear are the cables push the instrument base under the lead let the lead shielding slowly down and guide the instrument so the lead goes on the four guide pins 170 Installation Installation with Lifting Pulley disassemble the back panel Disconnect the ground cable disassemble the top cover 171 Installation upper front panel disassemble the support pillars note the numbering when assembling back open the screws of the j lift the upper front panel up on the instrument disconnect the cables numbered lift the upper front panel carefully on the floor 172 Installation disconnect all cables which goes from the lower part to the upper part disassemble the upper part by ope
42. the count time is then long enough so that the counting of every sample is terminated by this maximum count parameter the count error for every sample will be the same If there is the danger of chemiluminescence in samples causing abnormally high count rates and thus hiding the isotope contribution making it useless to continue counting the sample this parameter can be used to terminate the counting of such samples For further discussion on Chemiluminescence see the section with that name Line 07 Sample Quality Monitor This allows DPM results to be monitored to make sure that within the limits of expected uncertainty the results from the sample agree with the quench curve If the DPMI value is outside the expected limits then a change has most likely happened to the sample quality This function is describe in the section entitled Sample Quality Monitor It can only be used if SQP E is selected The default setting is No Line 08 Number of Windows This line only appears if Fixed Window is selected The number of simultaneous windows from 1 to 8 can be selected here Lines 09 10 amp 11A to 11F Windows 1 to 8 These lines only appear if Fixed Window selected The number of lines that appear depends on the number of windows specified on line 8 The preset value for the windows will be 1 1024 unless changed by the user 56 Mode 1 CPM DPM Line 12 External Standard Counting Time This and the next two lines do not appear
43. the fuses fitted in the fuse carriers on the back panel are of the correct rating for the local supply and according to the label Connect the battery cable 162 Installation Preparing Installation of Quantulus The weight of the lead shielding is almost 700 kg and is transported separately from the main instrument and has to be installed on the customers place Before the actual installation there are some points to be done Look for a place where the installation of the lead shielding can be done depended of lifting equipment The closer to the final position the better Check that the corridors and doors are wide enough and that there are no barriers on the route If an elevator is used check that it can handle the weight of the instrument and that there is space enough Check also that the floor of the operation room is strong enough for an instrument with a total weight of about 1000kg and that there is enough space for the instrument Note that there has to be at least 50 cm of empty space around the instrument for service purposes Check what kind of lifting equipment is available Remember that there has to be enough of space for doing the installation and if the installation is made in a different place than the operating room that the route for an already installed instrument is clear the easiest is to use a fork lift truck 163 Installation Total 1000kg if a truck is not possible the second altern
44. the half life in hours and zero time for the isotope or isotopes and selecting the corrected CPM CCPM 2 printouts The half life correction for DPM values is automatically done for DPM 2 if half life and zero time are given If a half life value differing from 0 is given the counter will ask for zero date and zero time This is the time back to which the activity is corrected This means also that if the batch is counted anew after e g one week the DPM results are directly comparable as they are half life corrected back to the same date and time If the half life is set to 0 or ZERO TIME is not set when half life is a non zero value the time of the start of counting will be used as the zero time If the Zero time is set in advance of the present date then the CCPM will be negative Instead of a number the text NEG ETIME will be printed and instead of the ETIME the text NEG will be printed 0 gt 340 8 Y EP 1996 gt 15 SEP 1996 8 35 gt 11 51 15 SEP 1996 11 51 1 gt 0 0 gt 78 Mode 1 CPM DPM Printout Printout selection There are 48 standard printouts available with Quantulus Each printout is identified by a number in the range 1 48 called a printout code Printout codes are set on parameter line 14 Each code is separated by a comma and after the last code RETURN must be pressed Each count mode has its own preset
45. under Instrument description program modes 121 Mode 6 Quasi simultaneous counting program BER OF CYCLES NCIDENCE BIAS L H CA CONFIGURATION RBON CONFIG 1 ITIUM CONFIG 2 EE SETUP 3 SE COMPARATOR LEVEL WINDOW CONFIGURATION HH Cp p pmocG nuAHanaOaz E E CA CONFIGURATION ARBON CONFIG 1 RITIUM CONFIG 2 REE SETUP 3 NPUT TRIGG INHIBIT MEMORY SPLIT R S N SUM L R PAC G EG U G L R D Display Modify Remove lt ret gt continue gt Display MCA configuration Display window configuration Display MCA configuration Summary of all Set MCA x Disable MCA x ETURN or exit to next line COMMAND Display Modify Remove lt ret gt continue 122 Mode 6 Quasi simultaneous counting program BLOCK 3 Line 5 Set Window configuration Window settings are done in Block 3 A total of 8 fixed counting windows can be specified For each window the window limits MCA and MCA Half have to be specified The command line enables the user to select what windows are displayed modified or removed Parameters are WINDOW order number for the window 1 8 CHANNELS lower and upper channel limit for the window MCA MCA from which the window data is collected HALF the half of the MCA from which the data is collected Note If a default MCA configuration 1 or 2 is selected the p
46. will be tested A Analyzer background efficiency B Gain stabilizer C Guard detector Make the following protocol and measure the sealed standards General Parameters MCA amp Counter Window Settings Saving path C TEST Configuration 14C high energy n Protocol name PERFTEST Send spectra All PAC 1 Number of cycles 1 Number of channels 1024 PSA N A Parameter listing YES Coincidence bias LOW Edit notes Window 12345678 Sample Parameters ORD POS ID PATHIS OFF CTIMECOUNTS CUCNTSMCWREP ST STMSSTIME 1 1 14C 1 00 Nolim Nolim 1 1 Y 1 1 0 15 2 2 3H 1 00 Nolim Nolim 1 1 Y 1 0 15 3 5 BKG 5 00 Nolim Nolim 1 1 Y 1 0 15 Check the performance and compare them to the results on the final test data sheet in the instrument manual Calculate also the efficiency for 3H SPA program 4SPCalc gt E gt DPM gt DECAY CORRECTION Y Because the PMTs has been disassembled and exposed to light during the transportation it will take 2 3 days before they are stabilized The spectrum calibration has to be checked according to the instruction on next page The same check should be done after 2 3 days 185 Installation of the PC Spectrum Adjustment Enter terminal mode and make the following protocol Parameter Group Las 00A Program mode Count Mode 1 Spectrum Adj 1 Fixed Window SQP E Single Label 3 H 01 Positions 02 Listing 03 Time 04 Counts 1 07 Sample Quality Monitor 08 Number of Windows 09
47. 0 of the total CPMs CPM1 CPM2 and adjust with trimmer M3 R90 on FAD board if needed Lower part of the spectra Set the PSA value to 1 and measure 3 H Check that the ratio of CPM1 CPM2 is 70 30 of the total CPMs CPM1 CPM2 and adjust with trimmer ZC4 on FAD board if needed 190 Performance test Performance test Measurement Make an over night run with the following protocol and measure the sealed standards General Parameters MCA amp Counter Window Settings Saving path C TEST Configuration 14C high energy B Protocol name PERFTEST Send spectra All PAC 1 Number of cycles 30 Number of channels 1024 PSA N A Parameter listing YES Coincidence bias LOW Edit notes Window 1234567 8 Sample Parameters ORD POS ID PATH IS OFF CTIME COUNTS CUCNTSMCW REP ST STMS STIME 1 14C 2 00 Nolim Nolim 1 Y 1 10 1 00 2 3H 2 00 Nolim Nolim 1 Y 10 1 00 5 BKG 30 00 Nolim Nolim 1 Y 10 1 00 Note The amount of cycles is depended on how much time is available Minimum is 20 cycles which takes about 13 hours and the more the better The cumulative counting time is visible at the bottom of the screen when using QMGR Analyzing When the counting is finished check the following things A Instrument Stability B Background amp Efficiency C Guard 191 Performance test A Stability Activate the SPA program and check the instrument stability by entering the SWSTA F7 of the STAT program Check SP11 of 14 C 3 H a
48. 5 This point and the next are moved ED 338 DD 62 175 125 34 13 gt Lr gt Mo gt N gt Y Curve replotted with points moved 74 Mode 1 CPM DPM ISOTOPI WINDOW 1 LINI INTERPOLATION FITTING TABLE SOP E EFF DEV W 903 95 95 195 00 785 43 88 37 00 700 00 81 37 00 594 00 6245 00 509 29 40 34 00 Curve plotted with points saved EFFICIENCY l l KKKKOT KKKKKKKKK KKKOK KKK KKKKKKK O kk kkk rr k I I I I ale I I I I I dE I 600 650 700 750 800 EFUL SOP E RANGE 509 904 CALCULATE UNKNOWNS N gt Y Unknown values to be entered manually UMBER OF REPLICATES gt 2 Number of replicates given EPLICAT 1 Values for first replicate required OP 1 gt 650 SQP Q for first replicate R gt 0 1 Error in SQP value PM1 gt 1500 CPM value PM1 1 gt 0 5 Error in CPM value 1 WINDOW 1 Calculated efficiency using the curve printed out previously Calculated DPM PM1 1 II Calculated DPM error EPLICAT Values for second replicate required SQP I Etc 75 Mode 1 CPM DPM DPM DPM measurements Quantulus includes the DPM program which enables efficiency corrected results to be obtained The DPM program automatically calculates an efficienc
49. 7 54 17 00 71 689 20 74 25 00 67 585 11 61 71 00 68 507 76 40 82 00 83 ISOTOPE 2 WINDOW 2 SMOOTHING SPLINE BUSY CALCULATING N S E 1 00 0 0 1 00 00 FITTING TABLE E 3 EV WEIGHT POINT CURV 83 s 00 60 07 00 62 20 00 69 LA 5 00 1 9 76 00 1 24 93 Mode 1 CPM DPM HHHHHH HHHHHHH HHHHHH HHHHHH HHHHHHH HHHHHHH vx 1 ER GROUP Di IX4E HERE E ER NF D IO HHHHHHH HHHH HI HI HH HI HI HI HL H HH HI HI HI H HF HI HI HI HI HI HI HF HI HI HI HI HI HH J o o o o Ne e EFFICIENCYS SAVING PARAME POINTS STORE 94 Mode 1 CPM DPM EFFICIENCYS HHH FEL EH ELE ELE HH HH A HA HH HH HH HH EHI EHE HE HH HH AA HAHAHAHA H FI EH EH HL HL E HF ELE EH EH EHI EHI FHHHHHH HHHHHH FE EH EIL HI HE HE ELE HL EH EHI EHI o e Sm 903 509 m RANGE SQP E 1 USEFUL ETER GROUP D B SAVING PARA POINTS STORE 95 Mode 1 CPM DPM E 24 SEP 1996 12 21 PARAMETER GROUP 1 ID DUAL 0A PROGRAM MODI 1 gt COUNT MODE FIXED WINDOWS SOP E DUAL LABEL H 3 C 14 POSITIONS 13
50. 71 Mode 1 CPM DPM EADY gt P Parameter setting selected TUE 24 SEP 1996 14 11 ER GROUP gt 2 gt E gt 15 Jump to line 15 C EDI N gt C SS REPLOT WITH AUTO R N Y Replot curve before counting unknowns R WITH CURVE N Y Printout small scale curve ISOTOPE 1 WINDOW 1 Curve fitting using the smoothing spline method SMOOTHING SPLINE selected on line 16 BUSY CALCULATING E P 2 0 FITTING TABLE Table of SQP E values versus DEV EIGHT Efficiency for each standard EFFICI 44 4 KKKKKOT SKK KKK KKK KK y 90 e HH HHH HHHH HHH HH KARKRKKRKO Q KKK KK KKK KKK xO k k k k 0O kx e e al o o w o o H HHH HHHH HHH Oo 4 4 4 4 S8QP E 550 600 650 700 750 800 850 900 USEFUL SQP E RANGE 460 904 ULATE UNKNOWNS N gt L15 Jump to line 15 EDIT N gt Y Line 15 selected to allow curve to be edited 72 Mode 1 CPM DPM ISOTOPE 1 WINDOW 1 SMOOTHING SPLIN Gl BUSY CALCULATING N S E P 1 00 0 2 1 25 0 0 un ll 1 4 29 FITTING TABLE STD S P E EFF DEV WEIGHT 903 95 95 95 02 1 14 N 2 T 1 2 785 43 88 37 49 T17 3 690 23 81437 31 1 22 4 583 43
51. 82 Limit values for workplace air 8 2 1 Limit values 8 2 2 Other information on limit values 8 3 Personal protective equipment 8 3 1 Special instructions for protection and hygiene 8 3 2 Respiratory protection 8 3 3 Hand protection Rubber or plastic gloves 8 3 4 Eye protection Safety goggles 8 3 5 Skin protection Protective clothing 9 PHYSICAL AND CHEMICAL PROPERTIES 9 1 Physical state colour and odour Clear bluish liquid fluorescent Faint hydrocarbon odour 92 pH 9 3 Information on changes in the physical state 9 3 1 Boiling point boiling ranger gt 208 C 9 3 2 Melting point melting range 198 Trade name Quantulus Guard Scintillation liquid Date 30 06 1996 Former date 9 3 3 Decomposition temperature 9 4 Flash point 81 1 C 9 5 Flammability solid gas 9 6 Autoflammability 9 7 Explosion hazard 9 8 Explosive limits a lower b upper 9 9 Oxidizing properties 9 10 Vapour pressure lt 133 Pa 20 C 9 11 Relative density 0 86 kg dm3 20 C 9 12 Solubility a water solubility Insoluble b fat solubility 9 13 Partition coefficient for ingredients n octanol water 9 14 Viscosity 9 15 Other information 10 STABILITY AND REACTIVITY 10 1 Conditions to avoid 10 2 Materials to avoid The product may react with strong oxidizers 10 3 Hazardous decomposition products Thermal decomposition may include hazardous gases for example carbon monoxide and carbon dioxide 11 TOXI
52. 826 107 Mode 2 Spectrum plot Spectrum plot of Am sample WINDOW WIDTH STE ds X Ro X FF FF FF x 108 Mode 2 Spectrum plot SAMPLE SPECTRUM Spectrum plot of a background sample POSITION 021 TIME 900 01 WINDOW WIDTH 20 STEP 20 HHHHHHHHHHHHHHHHHHHHH HHHHH 109 Mode 2 Spectrum plot 110 Mode 6 Quasi simultaneous counting Mode 6 Introduction Block 1 sample or position related data Block 2 MCA configuration Block 3 window settings Block 4 printout for both output terminals Editing while counting 111 112 Mode 6 Quasi simultaneous counting program Mode 6 Quasi simultaneous counting program Introduction Note This counting mode is supported by the Quantulus workstations such as Queue Manager and WinQ allowing creation and saving of virtually unlimited number of parameter groups on computer disk The following applies to direct control of Quantulus using the old user interfaces and Quantulus internal command language using eight parameter groups on Quantulus RAM refer to Chapter 4 These commands are accessible in Queue Manager and WinQ via the Term inal command In counting mode 6 each sample or pos
53. COLOGICAL INFORMATION 11 1 Acute toxicity Breathing vapour may cause headache nausea and dizziness 11 2 Irritancy and corrosiveness Solution may cause severe irritation redness and blurred vision 11 3 Sensitization No data available 11 4 Subacute subchronic and prolonged toxicity 11 5 Empirical data on effects on humans No data available 11 6 Other information on health effects 12 ECOLOGICAL INFORMATION 12 1 Persistence in the environment 12 1 1 Biodegradation 12 1 2 Chemical degradation 12 2 Bioaccumulation 12 3 Mobility 12 4 Toxic effects on organisms 12 4 1 Aquatic toxicity 12 4 2 Other toxicity 12 5 Other information No data available 13 DISPOSAL CONSIDERATIONS Burning in a chemical incinerator Disposal of all waste shall be in accordance with local regulations 14 TRANSPORT INFORMATION 14 1 UN number 14 2 Packaging category 199 Trade name Quantulus Guard Scintillation liquid Date 30 06 1996 Former date 14 3 Land transport 14 3 1 Transport class 14 3 2 Risk code 14 3 3 Name according to bill of freight 14 3 4 Other information 14 4 Sea transport 14 4 1 IMDG class 14 4 2 Correct technical name 14 4 3 Other information 14 5 Air transport 14 5 1 IDAO IATA class 14 5 2 Correct technical name 14 5 3 Other information This product is not a subject to transport regulations 15 REGULATORY INFORMATION 15 1 Information on the warning label 15 1 1 Letter code of the warning s
54. ERS 01 POSITIONS 1 3 gt 40 PARAMETER LISTING Mee 41 SPECTRUM SELECTION SAMPLE 1 EXTERNAL STANDARD 2 Looe 42 TIME 2 00 gt 44 COUNTS 900000 gt 45 AREA OF INTEREST 5 1024 gt 46 WINDOW WIDTH 20 gt 47 STEP 20 gt 48 REPEAT Loc 49 PRINT WIDTH 80 104 Mode 2 Spectrum plot SPECTRUM Spectrum plot for Tritium sample 001 2 01 WINDOW WIDTH 20 EL 0 HHHHHHHHHHH I I 104371 105 Mode 2 Spectrum plot SPECTRUM Spectrum plot for C sample 002 2 01 WINDOW WIDTH 20 EL 0 o Te I I I I I I I I I I I E JR I I E L I I I I I I I I I I I t I e 106 Mode 2 Spectrum plot Spectrum plot for Cl sample WINDOW WIDTH 20 STE 0 0 5 0 10 0 de I I I E I I I I E I AR E I Ag I I I I I I I I I I E I I I I AR I I de 397
55. Extended list has been selected 15 CURVE EDI N gt 16 CURVE FIT SS gt 16A REPLOT WITH AUTO RUN N gt REPLOT WITH CURVE EDIT N gt 1 BACKGROUND SAMPLE 0 0 gt 18A BACKGROUND SUB 1 0 gt 20 REPEA 1 gt 21 REPLICATE 1 gt 22 SAMPLE PREP ERROR 0 gt 26 FACTOR 1 1 00000E 0 gt 28 HALF LIFE 1 0 gt T 0 62 Mode 1 CPM DPM ER GROUP gt RAM MODE T MODE DOW 120 0 gt 900000 gt E QUALITY MONITOR N gt OF WINDOWS 1 gt 1 5 320 gt STD TIME 0 15 gt STD COUNTS 900000 gt ALA ALL By 10 D PARAMETER LIST N gt Y EDI N gt FIT gt WI gt WI E gt ROUN PLI gt ROUN 20 gt gt gt gt gt gt gt 63 Mode 1 CPM DPM 01 POSI gt 02 Y gt 03 1 00 gt 04 900000 gt 07 PLE QUALITY MONITOR N gt 08 OF WINDOWS 1 gt 8 09 5 320 gt 10 1 1024 gt 11A T T02A4 11B 1 1024 gt TTC 1 1024 gt 11D 1 1024 gt 11E 1 1024 gt 11F 1 1024 gt STD
56. FTEST QO2P201N 001 BKG C V TESTIS PERFTEST Q03P501N 001 The SP xx spectra value comes from the MCA configuration In this case 14 C configuration is used MCA INPUT TRIGG INHIBIT MEMORY SPLIT 1 LRSUM L R PAC G 2 GSUM G L R This means that the normal beta coincidence LRSUM amp L R goes into SP11 MCA 1 half one and when the PAC pulse amplitude comparator and G guard is activated the pulses goes into SP12 MCA 1 half 2 The guard pulses GSUM amp G goes into SP21 MCA 2 half 1 and when L R coincidence is activated the pulses goes into SP22 MCA 2 hold 2 For changing an order or a position ORD 01 POS 01 STD N REP 01 CYC 001 SP 11 gt O2P2 enter ORD 02 POS 02 STD N REP 01 CYC 001 SP 11 gt 183 Installation of the PC Type H or for help or see Quantulus PC Spectrum Analysis Program User Manual for more specific information Mechanical check Enter with F8 the terminal mode of the QMGR program and type Ready Tandenter entering service mode Service gt MO motor and sensor test At this point the conveyor can be controlled with the following commands XL XR YI and YO Conveyor table check Disconnect the HV cables Insert a tray and pick it up with the transporter with the commands xl and yi Run the tray into measuring position and switch the instrument off Run the elevator up manually by rotating the cogwheels Check that the elevator shaft goes smoothly up and th
57. H11 1 166 28080 388 400 5808 688 708 INTEGR 5 326 A1121824 422 CPM B 9 579 CPM BUNCH 3 FM 187998 46 DPMco FM I 1 LB13 438 E 64 88 7 A Q018101N 001 11 B Q038501N 001 11 Read 14 C into array A plot A and B bkg calculate FM dpms no decay correction and set the window to 5 650 Max deviation E 1 unit BKG 3cpm 193 Performance test 396 152 CPM ch 2 93 min A NSTEFANSNQ626261N 661 SPH11 8 189 CPM ch 493 57 min A NSTEFANS Q636561N 661 SPH11 188 288 388 488 588 688 788 INTEGR 1 658 A 98833 898 CPM B 11 133 CPM BUNCH 3 FM 181188 88 DPM FM_X A1 B13 gt 844 E 96 96 7 CA Q8280281N 001 11 CB Q630561N 661 11 C Guard Plot the background spectra of SP 21 and SP 22 SP 21 gt Pulse GSUM trigger G SP 22 gt memory split L R SP 21 are the guard pulses Window 1 200 shows the coincidence tube noise which could be decreased by adjusting the threshold level higher but then the cosmic peak and the detection of the environmental radiation would also decrease The noise peak is usually quite high in the beginning of the installation This is because the scintillation liquid in the guard container is unstable after of the transportation Window 200 800 is the background radiation from the environment This varies between 200 1200 cpm depended on the building material around the instrument Typical value is around 800 cpm Window 800 1024 is the cosmic p
58. Hz to 400 Hz 10G Puncture 50 g from 1 m Leakage tests according to ISO TR 4826 have been performed after the classification tests The tests show no significant leakage The source fullfils ISO 2919 tests and is therefore classified as C43334 Date 26 Oct 1994 Signature of controller um Ku j Raimo Kananen M Sc Physicist Quality Assurance Department Instruments 151 152 per This document must not be copied without our written imparted nor be used for any unauthorized purpose lontravention w thereof must not be contents ard the mission rty de prosecuted CAPTIVE DEVICE FOR THE CAPSULE IF THE NUTS WERE OPENED LZ STEEL RIVET PRESSED WITH THE HOLES ON THE NUTS STAINLESS STEEL AISI 321 POLYURE THAN SHOCK ABSORBER STEEL RIVET LEAD SHIELD THICKNESS 40mm STAINLESS STEEL AIS 321 POLYURETHANE SHOCK ABSORBER STAINLESS STEEL Als 321 STAINLESS STEEL ACTIVE SOURCE ABSORBED IN CRYSTALLINE SYNTHETIC ZEOLITE 5 1 CAUTION RADIOACTIVE MATERIAL SATEILYVAARA When this instrument is no longer in use the gt Eu 152 standard capsule must be removed and sent to the eppr opriate radiation safety authorities or to the instrument manufacturer for safe disposal Kun tama laite poistetaan lopullisesti k yt st onEu 152 standard kapseli irroitettava ja toimitettava sateilyturvallisuusviranomaisille tai laitteen valmistajalle THE ABOVE
59. INSTRUMENT MANUAL September 2002 5731220 Quantulus Ultra Low Level Liquid Scintillation Spectrometer gt PerkinElmer life sciences Wallac 1220 Quantulus Ultra Low Level Liquid Scintillation Spectrometer Internal software version 1 D gt PerkinElmer life sciences PerkinElmer Life Sciences Wallac Oy P O Box 10 FIN 20101 Turku Finland Tel 358 2 2678111 Fax 358 2 2678 357 Website www perkinelmer com lifesciences Warning This equipment must be installed and used in accordance with the manufacturer s recommendations Installation and service must be performed by personnel properly trained and authorized by PerkinElmer Life Sciences Failure to follow these instructions may invalidate your warranty and or impair the safe functioning of your equipment Il PerkinElmer life sciences Contents Contents Introduction eec D 3 Introduction to the instrument manual eisen 3 Introduction to the instrument operation enne enne enne entere 3 SS GA EHUD e 7 Power Requirements ran 7 Coo ee esse Seinen 7 SWITCH OM proced re aeos vein br A ld T The concept of total optimization essoesssesssecssooesoossooesssesssoessooesoosssossssesesoessoossoossssssssesssosse 11 EEO CIC ION real se ee 11 Shieklins tennis Ci E MK Sc M E or alee 11 Multichannel analyser 5 ere eret ei 11 Automatic continuous spectru
60. S 2 5000 gt gt 2 gt 08 NUMBER OF WINDOWS 09 5 240 gt 5 300 10 200 650 gt 100 600 12 STD TIME 0 15 gt 13 STD COUNTS 900000 gt 14 E 120 fp 137 15 21 22 87 10 16 18 gt Y 0 0 0 07 SAMPLE QUALITY MONITOR N gt 2 0 0 L5 d iD PARAMETER LIST N gt Y 15 QE N gt 16 SS gt 16A PL H AU UN N gt PL H CU EDIT N gt 17 D SAMPLI gt 18A D SUB gt 18B gt 20 IPE gt 2 PL e 22 E PREP E E gt 26 gt 27 gt 28 N IFE A gt 29 IFE gt 30 gt Sl FERE A 32 FERE gt 90 Mode 1 CPM DPM READY gt S EP 1996 10 26 STANDARDIZATION PROGRAM PARAMETER GROUP gt 1 COUNT MODE FIXED WINDOWS SOP E DUAL LABEL H 3 C 14 01A NO OF STAN ISOTOPE 1 10 gt 5 POSITION OF FIRST STAND 1 gt 01B NO OF STAN ISOTOPE 2 10 gt 5 POSITION OF FIRST STAND 11 gt 7 02 AUTOMATIC RUN Y 03A METHOD 2 3 3 gt 04A ISOTOPE 1 0 gt 8500 04B ISOTOP 0 gt 9900 O5A ISOTOPE 1 ERRORS QD gt 5 05B ISOTOPI ERRORS 00D 06B START SOP 1 1024 gt 07 TIME FACTO 1 0 gt 3 08 START
61. T WITH CU gt KGROUND SAME gt KGROUND SUB 32 KGROUND SUB EA gt ICATE gt PLE P gt TOR 1 gt TOR 2 gt IFE gt IFE gt ER OF gt ERENCE gt ERENCE gt Ss y f 1 f HW GOO AOR a un SAVING PARAME 65 Mode 1 CPM DPM Chemiluminescence monitoring and subtraction Chemical reactions can result in the emission of photons under certain conditions e g when during sample preparation solubilizers or H202 have been used Several types of sample have to be solubilized before counting Generally some quaternary ammonium hydroxide compounds are used as solubilizers H20 is added as a bleaching agent for sample types which are strongly coloured The sample preparation then results in an alkaline solution which because it is water based is counted in a liquid scintillation cocktail of emulsifying type The emulsifier chemicals combined with the alkaline oxygen rich compound can result in a high rate of chemiluminescence reactions Chemiluminescence is a single photon reaction consequently one chemiluminescence reaction is not enough to trigger the fast coincidence discriminator of Quantulus but the higher the chemiluminescence reaction rate the bigger the probability that two reactions happen so close to each other that the fast coincidence discr
62. TIME 0315 gt STD COUNTS 900000 gt NP da 22 8 0 ED PARAMETER LIS X gt gt gt gt gt gt gt gt Um gt gt gt gt gt gt gt gt gt gt gt 16A i H AU H CU SAM SUB SUB SUB SUB SUB SUB SUB SUB UN EDIT 0 ve lt eo les 17 18A 18B 19A 19B 19C 19D 19E 19F 20 21 22 VUUUUUUUU 00 3010145 CO PO RA 28 oroocoorroo00o00o00o0o0o00o0o0ZZNZZ SAVING P READY gt 64 Mode 1 CPM DPM ER GROUP gt 5 P RAM MODE T MODE SELE ED WINDOW I E SINGL SINGLE E DUAL RM CHANGE 1 125 C 14 35 Ca 45 P 32 C 14 35 Ca 45 P 32 Ca 45 P 32 Ca 45 P 32 P 32 DE ED WINDOWS E DUAL LABEL H 3 C 14 TIONS 5 I Y NRO 00 1 OY O1 iS CO DN 2 gt gSSSUSSISSISSISSISNNS O G Y gt 1 00 gt 1 900000 gt 2 900000 gt QUALITY MONITOR N gt OF WINDOWS 2 gt 1 5 240 gt 2 200 650 gt F AL STD TIME 015 gt ERNAL STD COUNTS 900000 gt E1725 ip io 2 22857 107 L618 ENDED PARAMETER LIST N gt Y EDI gt ESELI gt OT WITH AU gt O
63. UOES ne nal 161 Edteratutes sc aom ue sd md EM d serie Met 161 iii Contents A 162 ENVIO MEN A re 162 Elegtric PONE ao 162 Checking the mains voltage settine anne ee 162 Preparing Installation of QUIN ii ia 163 Unpacking the Lead MO e ais 169 Installation with a Tort RR 170 Installation with Lifting Poll t 171 Installation of the PMT s and External Standard sse 178 Installation of the PC ee ei Bee 181 General Information of the SPA and QMGR program esssessseenseensenennnsnennnsennnennnnan nn 181 Mechanical Check nun unse is 184 A 185 Spectrum Adjustment u ee rare setzen 186 PSA amp PAC Check anne Ein 189 Performance irc dpt 191 Measurement ri aaa tete Into teed Saad essai li iaa 191 ANNIE 191 Material data safety SHEGt 9 5515 lt ccsccccosnssscsctesees edsosuscccsoonssesdsbescuctosuts sense ssuassauesesbobscsecsosseseas ous 197 iv Introduction Introduction to the instrument manual Introduction to the instrument operation Introduction Introduction Introduction to the instrument manual The Instrument manual forms the second level of the Quantulus Operating System The first level is the built in HELP feature which is a constantly available aid to the operator and can be called on at any point where a decision has to be made to clarify the possibilities Then secondly there is this instrument manual This describes the basic operational details of the instrument as the
64. a replacement for normal sand The ceiling and the floor are also of the low activity material In this environment the gamma flux is about 1 20th of the flux in our normal environment resulting in halving of background count rate We maintain overpressure in the room to flush out radon underneath the door air exchange is about 3 times hr The outside air inlet should be located well above the ground level since otherwise a small variation of radon concentration will result due to diurnal variation close to ground level Filters in the air inlet maintain dust free air no dust nor cigarette smoke should be allowed in the counting room It is also important to avoid great temperature changes in the counting room air conditioning and temperature control is recommended to reduce humidity as well The instrument cooling unit is able to maintain a 12 degree centigrade difference between the instrument interior and ambient air temperature If cooling is boosted by running water through the cooling fringes a 12 degree difference is maintained between the water and interior The mass of the instrument presents a thermal inertia which considerably slows down the temperature variation due to power failure The Wallac low level room is a Faraday cage When the power line is dependable and not noisy it is not necessary to have Faraday cage Quantulus contains an aerial in anticoincidence to filter electromagnetic interference With noisy power lines it may
65. ading is from 2 5 to 12 5 The cooling unit contains copper tubing to circulate the cooling water By cooling Quantulus it boosts the performance In this case the reference is the water temperature instead of air temperature At the rear of the instrument is an outlet for condenser water Take care when putting the cover on the instrument because it is necessary to prevent leakage of warm air into it Switch on procedure 1 Switch on the computer or video terminal check that it is on line shown by the red light on the keyboard If you have a video terminal check that the CAPS LOCK key is down 2 Switch on the printer In the case of the video terminal if you do not want printout press CTRL PRINT 3 Switch on Quantulus When the instrument is turned on the first time or when the duration of the power failure is too long more than 100 hours for one memory board and half that time for 2 boards etc the software types Start up MASTER CLEAR 1220 QUANTULUS MAIN PROGRAM V 1 D Copyright C 1986 by LKB Wallac OPTION PROGRAMS PSA V 1 C UE 10 APR 1984 0 00 NOT SE YPE C RETUR O SE IHE CORREC MAKE SURE HAT THE POSITION E TRAY ONE IS EMPTY AND AFTER THA E ETURN CONVEYOR CLEARING READY gt 4 If power has been off but not long enough to drain the standby power supply the message
66. alk coincidences This is the basis of the PAC operation The user adjustable PAC level from 1 to 256 corresponds to the smaller greater ratios ranging from nearly zero to about 0 8 27 The concept of total optimization Access to the PAC is in counting mode 6 after selection of PAC as a part of the trigger inhibit or MCA split condition Software then asks for a PAC level which can be set by the user 1 255 1 no PAC PAC acts as a discriminator so that the higher the level the closer the amplitudes from the individual photomultipliers must be for the detected coincidence pulse to be accepted see the figure An optimum setting is found by measuring an isotopic standard and a background sample at different PAC levels The best settings may be e g that which gives the maximum figure of merit in the counting window PAC is particularly effective in glass vials when low quench C sample is measured PAC levels above 180 have effect on the figure of merit in these samples Set PAC level gt Pulses not Pulses accepted accepted Sample y A Crosstalk SMALLER GREATER 1 28 The concept of total optimization Program modes Introduction The instrument software is organized in three program modes having the numbers 1 2 and 6 Program mode 1 gives access to the CPM DPM program and program mode 2 is a spectrum printer plot program 80 character resolution Program mode 6 1s also called the
67. aracters preset counting time 1 s to 277 hrs count limit cycle 1 9 9E99 counts or no limit cumulative limit 1 9 9E99 counts or no limit count limit for window definition repeats for a sample 1 99 external standard yes no SQP E ext std on each sample cycle or every Nth cycle N 1 99 139 Specifications ext std counting time 1 s 2 hrs cycles of batch 1 999 preset windows 1 8 printout selection and definition for 2 printers spectrum save selection max 4 spectra ext std spectrum resolution on save 16 32 64 128 256 512 1024 140 Routine maintenance Routine maintenance Keeping the instrument clean The conveyor surface should be kept clean to avoid dust and dirt entering into the optics at the measuring position The conveyor surface should be cleaned using a soft cloth or tissue paper soaked in a mild detergent solution or alcohol Power supply fan Check that the cooling fan in the power supply unit is working by listening for its sound Cables Check that the power cable and the cables to the peripherals are tightly connected and that the cables and connectors are not damaged Any damaged cable should be replaced immediately 141 142 Quality control information 143 144 QC Contents Safety evaluation of the Eu 152 ext std source 1099 0209 Construction with dimensions AA 1036 0841 Quality control report es essen 1096 1061 External standard transport
68. at the light shield core does not hit against the lead shielding on the way up and that it does not hit against the sample tray on the way down If this is the case the conveyor table has to be aligned see mechanical adjustments in service manual When o k switch instrument on and re enter the motor and sensor test and run pos 1 5 16 and 20 to be sure the mechanical alignments are o k For the final mechanical test make a protocol with 1s measuring time and for the positions 1 21 41 5 25 45 16 36 56 20 40 60 Insert a sample tray in each position and push the tray as much as possible to the left Check that the sample tray is picked up smoothly and that the elevator goes up and down smoothly without the core hitting against the lead or the tray Push the tray each time it is returned from the instrument to the left This is done for all corner positions Make a rerun of the protocol and now with the sample tray to the most right position If problems check alignments When o k reconnect the HV cables and reassemble the lids except for the back panel Assemble the cooling unit and set the temperature to be about 5 degrees of Celsius below the room temperature 18 degrees of Celsius is normal temperature 184 Installation of the PC Electronic check First step is to run a short performance test similar to the one on the final test data sheet but with shorter counting time for the background With this test the following circuits
69. ation If possible a separate room should be provided for Quantulus as this allows the best control over the immediate environment Ventilation in the room should be adequate for all conditions of use the temperature should be reasonably constant at about 220C relative humidity should not be excessive and direct sunlight should not be able to reach the instrument It is also important that the various isotopes are stored well away from the instrument in another room Only those radioactive samples that are actually measured should be in the laboratory at any time in order to keep the background at a low level Electric power Three electrical outlets each with a protective earth should be available with if possible a separate power line for the instrument itself having an isolation switch and a fuse box If excessive fluctuations in the mains voltage are anticipated a mains stabilizer may be necessary Checking the mains voltage setting Measure and note the mains voltage at the outlets to be used Note the instrument is provided with two mains electrical inlets the instrument itself and the cooling unit Fuses T4A Mains 100 120 V T2A Mains 220 240 V More than one live circuit see the diagram Locate the mains selector switches If necessary adjust the mains selector switches to correspond with the measured supply For supplies with a nominal voltage of 230 V it is recommended that the selector be set to 220 V Check that
70. ative is to disassemble the upper part of the instrument and to use a lifting pulley Check where to hook it 700 kg Total 1000kg 164 Installation When the lead shielding is installed it is easiest to move the instrument to the operation place with a jack Normal service tools are needed and it would be good from service training point of view for the local service engineer to be present all the time The installation and the checking of the instrument takes in normal condition about 4 5 days including the training of the local service engineer and the basic training of the customer Note The instrument has to be connected to a mains circuit having a protective earth Installation 165 Installation Unpacking the Main Instrument cut the stripes open the Phillips screws down on the box lift the box carefully over the instrument remove the plastic around the instrument Note Break the box if there is not enough of space to lift the box Disassemble first the side lids and then the front lid 166 Installation Disassemble the cooling unit Disassemble the rails with which the instrument is attached to the stand Pull the instrument see arrow about 20 cm over the stand install the legs the legs are in the lead shielding box Note The legs are numbered and the according numbers are typed on the instrument 167 Installation 168 put the corner of
71. cial problems Pulse selection and additional conditions of analysis are set by logic commands in MCA INPUT TRIGGER INHIBIT and MEMORY SPLIT In MCA INPUT the analogue pulse is selected this is normally the combined total pulse train from left and right PMT s L R 33 The concept of total optimization The trigger condition is normally coincidence condition L R which eliminates the random noise of phototubes and is the first requisite for low level counting A D conversion can further be inhibited with a logic condition which quite often activates the anti coincidence guard counter for more background reduction Finally the pulses may be directed into two separate MCA halves by using logic split condition If the condition is true the pulse will end up in the second half else in the first one The configurations are the following 1 C 14 or other high energy beta emitters MCA INPUT TRIGG INHIBIT MEMORY SPLIT 1 LRSUM L R PAC G EG 2 GSUM G L R MCA 1 is used for analysis of the combined left and right PM tube pulses Using the Coincidence condition as a trigger select reduces random coincidence of thermal noise Split by pulse amplitude comparator guard and external guard leaves in SP11 all events which were detected by the guard or external guard or were not accepted by the comparator or by any combination of these Detection by the guard means that the event was caused by an external source cosmic or other environme
72. cifications Physical dimensions Width 1010 mm Height 1560 mm Depth 920 mm Weight approx 1000 kg Stands on four feet each 28 square cm 90 cm apart Power Mains voltage selectable 100 115 120 220 240 V 10 50 60 Hz In the case of the mains voltage being 230V select 220 V on Quantulus Power consumption 200 VA Cooling unit consumes approximately 350 VA voltage rating as above Connections input output Serial ASCII interface RS 232C two output terminals terminal 1 for data input output to a display printer and terminal 2 for data input output to an external microcomputer Also temperature sensor connector in cooling unit Radiation shield Asymmetric passive radiation shield made of low radioactivity lead around the detector assembly maximum thickness of 200 mm on top 100 mm on side walls and 150 mm below the counting chamber Head of the piston made of copper and is part of passive shielding Active shielding against cosmic particles and environmental gamma radiation is enforced by an asymmetric guard counter which operates in anticoincidence with the sample detector The guard s OFHC copper container offers extra passive attenuation against environmental radiation i e is part of the so called graded shield The guard length is 350 mm diameter 160 mm and it is monitored with two 2 PMTs operating in summed coincidence Filling is scintillation liquid Space is provided above the shield for an optional flat cosmic
73. cktail are not adequately mixed some of the beta particles will be absorbed in the sample phase and thus not reach the scintillation liquid phase This will appear as a reduced counting efficiency for the sample This happens because the external standard spectrum which is produced by the Compton electrons resulting from the gamma radiation from the external standard is not affected by the inhomogeneity of the sample and cocktail mixture This is because the Compton electrons are generated throughout the whole volume and thus will effectively produce scintillations The counting efficiency might even be improved for the external standard as the quenching agents are in the sample phase Thus the counting efficiency obtained from the measurement of the external standard is not correct if sample and cocktail mixture is two phased The sample and liquid scintillator mixture can be homogeneous when the counting starts but as time goes the last samples can be inhomogeneous if the samples are close to the sample holding capacity of the cocktail When using an emulsifying cocktail the sample is suspended in drops micelles in the cocktail The micelles are small compared to the range of the beta particle energy so that absorption in the micelles is minimized However if the sample amount is big close to the sample holding capacity the micelle will start to grow which will affect the counting efficiency The Sample Quality Monitor will detect this ty
74. correction calculations of averages of repeat measurements or replicate samples calculations of standard deviation observed and theoretical error and probability test for results of repeat or replicate counts user selectable printout factorization of results by multiplying the result with a factor they can be transformed from CPM DPM to wished units for example to Becquerels The quench calibration curve can be made by using the external standard or a quench parameter calculated from the sample spectrum The external standard is Ra in Quantulus models up to 2200166 after which Eu is used This source is located in its own storage shield and is moved by compressed air along a stainless steel tube to the measuring position when a measurement is to be made Full details of the external standard system are given in the Quality Control Report The Spectral Quench Parameter of the External Standard SQP E is then calculated from the external standard spectrum The SQP E is the endpoint of the net external standard spectrum i e a channel below which reside 99 of the counts generated by the gamma radiation from the external standard Usage of an external standard provides a non destructive fast method to measure sample quench no addition of known extra activity in the sample is needed 30 The concept of total optimization R SQP E 949 7 1 108 28080 388 466 S66 666 766 866 98080 1888 SOP E based on Ra 226 external sta
75. counter external guard to act as a cosmic umbrella Guard operation is sample independent i e light from the sample and guard do not pass through each other and are detected with their dedicated PM tubes External standard source is enclosed in an asymmetric lead shield with maximum attenuation towards the counting chamber 133 Specifications Operating conditions Temperature 15 to 35 C Humidity max 75 Air conditioning of the counting laboratory with stabilized temperature is recommended in conditions where temperature rises above 30 C and or humidity is above 75 Electrical safety The design of the instrument is based on the following electrical safety requirements EN61010 1 CAN CSA C22 2 No 1010 1 92 Electrical compatibility the instrument fulfils EMC standards EN 50082 1 1992 and EN50081 1 1992 Temperature control Four Peltier elements of the cooling unit are able to maintain the temperature ofthe main instrument body 12 C below the ambient temperature electronics is not cooled The cooling unit fins contain a water inlet to boost cooling so that 12 C below water temperature may be reached for the instrument temperature The large amount of lead provides effective inertia for temperature changes and therefore several hours of power failure will not cause major temperature increase of the instrument The cooling unit is always recommended for Quantulus Sample changer and conveyor 60
76. cy and the quench parameter value is recorded Quantulus uses two parameters 1 SQP E spectral quench parameter of the external standard 2 SQP D spectral quench parameter of the isotope this is the centre of gravity of the spectrum 76 Mode 1 CPM DPM Both parameters are based on spectrum analysis the SQP E on analysis of the external standard spectrum the SQP I on analysis of the isotope spectrum Characteristic for both is the good dynamic range and small statistical error A curve is fitted to the standard points using either linear interpolation interpolation spline or smoothing spline Linear interpolation fits straight lines between the standard points the interpolation spline fits a third degree polynomial function between each point subject to the condition that the curve must be continuous The smoothing spline has an additional smoothing function which decreases the influence on the curve of bad points outliers The curve fit method is specific to the parameter group to which the quench curve will be dedicated The information concerning the standards such as activity and calibration method is given in the Standardization program which is activated with the S command The quench calibration results in a plot of the quench curve The standard points are saved in EEPROM non volatile memory together with the other parameter group information and are thereafter called into use when the parameter group is selected
77. d for two windows or two isotopes simultaneously When the program mode 1 is used the spectrum is measured in one half of MCA 1 The other half of MCA 1 can be used to measure the Random Coincidence spectrum which is used to correct the CPM values for chemiluminescence The Active Guard is used in anticoincidence with the analogue to digital converter A D converter for MCA 1 This means that if the guard registers a signal simultaneously with a coincidence signal in the beta detector the guard detector will inhibit the A D conversion The sample detector with one phototube pair and the guard detector with another one are two entities which are independent of each other Therefore background caused by external 29 The concept of total optimization radiation is rejected by true event detection which guarantees sample independent improved sensitivity in the measurement Due to the construction of the sample changer it is necessary to specify which position is used in the measurement This enables also the positions to be measured in a random fashion the positions do not necessarily have to be in numerical order Program mode 1 enables CPM results for 8 counting windows DPM results for 2 counting windows or two isotopes chemiluminescence correction background correction by measurement of a background sample or by typing in background CPM value CPM results for two isotopes given as a percentage of reference samples half life
78. dar clock which gives a printout of date and time at the beginning of each batch of samples In the READY state the date and time can be displayed using the command D The time can also be selected as a part of the printout using printout code TIME will cause a printout of the current time for each sample The clock is a 24 hour clock The memorized calendar clock is valid up to year 2099 taking into account the leap years The date can be printed out by selecting DATE in printout selection The calendar clock is set in the Ready state by typing the command C and pressing Return The date and time is requested and should be entered as shown in the printout example The clock is started after typing Y and pressing Return in response to the instruction TYPE Y RETURN TO START CALENDAR CLOCK The clock has to be reset after a power failure or a Master Clear If the clock is not set after Master Clear the text NOT SET is printed out after the time printout EADY gt C ER DAY MONTH YEAR 10 APR 1984 gt lp Enter day month and year separated with a space and press ETURN ange 1 JAN 1901 31 DEC 2099 P ER DAY MONTH YEAR 10 APR 1984 gt 18 SEP 1996 UR MIN 0 08 gt 13 35 ETURN TO START CALENDAR CLOCK gt Y EP 1996 13 35 43 General features Help function Quantulus incorporates a HELP function This is a facility by which extra informat
79. date and time display program version numbers display information about parameter groups display this information edit parameters start counting enter the standardization program N PUEHHUOO Commands while editing parameters on any line display more information about the parameter no RETURN save parameters and go to the READY state n program mode 6 on main parameter lines only x Jump to line number x WHAM vw ETURN jump to the next line BACKSPACE correct typing errors Press RETURN for more information or type any READY state command gt edit while counting going on O stop counting and go to the READY state Dx no RETURN display function x is from 1 to 8 type D9 to scan again Note this command is no longer available HET while counting READY gt Information control command When the Quantulus is in the READY state control command I can be typed and RETURN pressed to give a printout of software version number and application software present in the instrument This also tests that the CPU can read the software stored in ROM memory Failure to obtain a printout after typing I indicates software error 42 General features READY gt I 1220 QUANTULUS MAIN PROGRAM V 1 D Copyright C 1986 by LKB Wallac OPTION PROGRAMS PSA V 1 C READY gt Calendar clock Quantulus includes a calen
80. dentification of the manufacturer importer or other undertaking 1 2 1 Manufacturer importer other undertaking Wallac Oy 1 2 2 Street address Mustionkatu 6 Postcode and post office FIN 20750 Turku Finland Post office box 10 Postcode and post office FIN 20101 Turku Finland Telephone number 358 2 2678 111 Telefax 358 2 2678 357 LY code 0937168 4 1 2 3 Name and address of the informant in emergency cases Emergency telephone number 1 2 4 Information on foreign manufacturer 2 COMPOSITION AND INFORMATION ON INGREDIENTS 2 1 Description Liquid containing alkylbenzene 2 2 Hazardous ingredients 2 2 1 CAS number 2 2 2 Name of the 2 2 2 4 Warning symbol R phrases or other code ingredient Concentra and other data on the ingredient 1 2 4 Trimethylbenzene X R 10 20 36 37 38 LD 5000 mg kg orl rat Mineral oil LD 22 g kg orl rat 2 2 5 Full chemical name of the ingredient CAS number name Confidential 2 2 6 Other information Product also contains other fluorescent compounds lt 0 3 3 HAZARDS IDENTIFICATION Product is irritating 4 FIRST AID MEASURES 4 1 Special instructions 197 Trade name Quantulus Guard Scintillation liquid Date 30 06 1996 Former date 4 2 Inhalation If inhaled remove to fresh air If breathing is difficult give oxygen and seek medical advice 4 3 Skin Rinse immediately with copious amount of water and wash with mild soap solution 4 4 Splashes in eyes R
81. dition for coincidence will not be fulfilled For chemiluminescence reactions there exists no time correlation between the scintillations Thus the probability for random coincidence is the same even if one of the signals is delayed In Quantulus when the chemiluminescence correction is selected the delayed coincidence spectrum is measured in MCAI Halfl 66 Mode 1 CPM DPM The normal or prompt coincidence spectrum consists of both true coincidence events and random coincidence events whereas the delayed coincidence spectrum consists of random coincidences due to chemiluminescence tube noise and depending on the sample activity random coincidences between beta decay events The delayed coincidence spectrum is used to correct the normal coincidence spectrum by subtracting it channel by channel The CLM chemiluminescence percentage is also calculated based on the delayed coincidence spectrum CLM can be printed out by selecting printout code 36 on line 14 in the parameter program If CLM is not selected and the chemiluminescence percentage is higher than 10 the instrument will give a flag warning CLM 10 Note Chemiluminescence is only subtracted if the CLM printout is selected 67 Mode 1 CPM DPM Counting started with parameters from group 6 WED 24 OCT 1984 15 31 PARAMETER GROUP 6 ID CHEM LUM TRIAL STD CURVE FITTING Standardization has already been made Thirty repeat counts of the same sampl
82. e the Eu 152 standard capsule must be removed and sent to the appropriate radiation safety authorities or to Wallac for disposal This procedure must be performed only by a qualified PerkinElmer Life Sciences service engineer 147 148 core wo oare fom PO want QUANTULUS 1220 EXTERNAL STANDARD _____ wallac OY SYSTEM CONSTRUCTION WITH DIMENSIONS 10360841 AOL er 940930 AS Tem e GUIDO kou LEFT SIDE REAR VIEW 730 MORE DETAILED INFORMATION ON THE DOC NO 10 36 0835 This document must not be opi PO without Our written per missin ne the ten hereof must not de imparted to A ird party ane ye used for any s authoritded pul po kontraventson will he prosecuted 149 150 gt PerkinElmer 1096 1061 life sciences Quality Control Report Name of Product Quantulus Product Type No 1220 Manufacturer Wallac Oy Turku Finland Function Tested Classification of External Standard Capsule Eu 152 according to ISO 2919 Activity of the capsule 37 kBq ___CERTIFICATION Eu 152 External standard source has been tested according to ISO 2919 Sealed Radioactive Sources Classification The tests are Test Short definition Temperature 40 C 20 min 400 C 1 h and thermal shock to 20 C Ext pressure 25 kPa abs to 2 MPa abs Impact 200 g from 1 m Vibration 2 times 10 min two axes 25 Hz to 50 Hz SG 50 Hz to 90 Hz 0 635 mm amplitude 90
83. e are shown below with chemiluminescence decaying from 70 to 2 POS CTIME CPM1 DPM1 DPM1 CLM SaP E 001 00030 88270 97 192121 1 905 71 271 455 85 Chemiluminescence gt 10 very high and the 00030 83119 37 180979 923 63 108 55 76 detectors are close to gt 10 saturation 00030 78762 72 171567 946 52 408 55 67 gt 10 00030 74617 76 162490 920 41 598 554 773 10 00030 72369 14 159032 932 30 524 53 76 Chemiluminescence gt 10 corrected DPMs are 1 00030 71908 83 158775 954 20 813 en now stable gt 100 00030 10525 155580 918 257 CPMs are now also gt 10 stable with over 10 00030 68681 152256 930 816 chemiluminescence 00030 69831 156230 938 693 00030 69400 155398 910 354 00030 69681 155609 930 330 00030 69477 155789 941 677 00030 70341 158175 2923 229 00030 70472 158134 918 466 00030 70257 158049 906 619 00030 69587 156732 939 650 00030 69087 156251 943 565 00030 69751 157538 919 762 00030 69244 157861 945 2331 00030 69437 158140 929 052 00030 67869 155927 933 819 00030 68379 156185 932 335 00030 69171 158099 297 00030 68552 156651 937 00030 68671 158938 27 0 00030 68447 158335 540 00030 68065 151278 376 00030 67805 157175 00030 68059 156889 00030 67488 156493 Hr N ns 1S C 0 c 0 C 0 E 0 C 0 el 0 0 oOporpororor orocotE 950 941 949 980 947 Q Ui O
84. e directed into SP11 When the PSA level is correctly set SP12 contains pure alpha events and SP11 contains beta events see also help on PSA and PSASETUP in the Spectrum analysis program In the above configurations MCA2 has been dedicated for monitoring the guard performance The SP22 contains the counts from the guard detector which are in coincidence with the signal from the sample detector typically of the order of 20 CPM most from cosmic muon passage through the lead and guard SP21 contains the rest of the guard pulses the ones in anticoincidence with the sample This spectrum shows clearly a high energy muon peak of the order of 300 400 CPM It also shows a Compton recoil electron continuum from 100 to 800 channels scattered by gamma photons which entered the guard through the lead The low energy end of the spectrum is the phototube noise spectrum see instrument performance data MCA2 may however be used for other types of analyses of the sample input signal LRSUM by combining the conditions for instance in alpha counting mode one could set the MCA2 to monitor chemiluminescence by adding there the H counting mode and denote Boolean AND and OR respectively 35 The concept of total optimization Logic signals and their combinations Help Analogue pulse select lt INPUT signal L Left detector analogue pulse R Right detector analogue pulse LRSUM Left and right pulses summed L R GSUM Left and right
85. e external standard capsule moves properly check that the SQP E values are close the table values 8 channels 188 PSA amp PAC check PSA amp PAC Check Enter terminal mode and make the following protocol PARAMETER GROUP 1 ID PSA PAC 00A PROGRAM MODE 6 ORDER POS ID CTIME COUNTS CUCNTS MCW REP STD STMS STIME 1 1 PSA PAC 0 30 NOLIM NO LIM 1 99 N NUMBER OF CYCLES 1 COINCIDENCE BIAS L H MCA INPUT TRIGG INHIBIT MEMORY SPLIT 1 LRSUM L R PSA 2 LRSUM L R PAC PSA LEVEL PAC WINDOW CHANNELS MCA HALF 1 1 1024 1 1 2 1 1024 1 2 3 1 1024 2 1 4 1 1024 2 2 Selected Printout for terminal 1 A 1 2 3 4 5 6 CTIME CPMI CPM2 CPM3 CPM4 Selected Printout for terminal 2 B 1 2 3 4 5 6 CTIME CPM1 CPM2 CPM3 CPM4 SEND SPECTRA None LISTING Y INSTRUMENT NUMBER 1 CTIME CPM1 CPM2 CPM3 CPM4 depends on what is checked see the next page 189 PSA amp PAC check PAC Check amp Adjustment Set the PAC value to 256 and measure 14 C Check that the ratio of CPM3 CPM4 is 75 25 of the total CPMs CPM3 CPM4 and adjust with trimmer R44 on EBL board if needed PSA Check amp Adjustment Upper part of the spectra Set the PSA value to 190 and measure 241 Am Check that the ratio of CPM1 CPM2 is 50 50 of the total CPMs CPM1 CPM2 and adjust with trimmer M3 R90 on FAD board if needed Note If no 241 Am available Set the PSA value to 10 and measure 14 C Check that the ratio of CPM1 CPM2 50 5
86. e only way to be able to monitor and control the above mentioned factors is to use a technology based on multiple programmable multichannel analysers The term programmable means that the user can select the analogue pulses which will be converted by the analogue to digital converter The logical signals trigger inhibit etc which guide the conversion can also be user selected by simple software commands The use of a programmable multichannel analyser gives possibilities for enhanced data validation not possible with a traditional static multichannel analyser The multichannel analysers Quantulus incorporates 2 dual programmable MCAs This enables simultaneous measurement of 4 spectra each with 1024 channel resolution The pulse amplifiers yield a linear pulse height spectrum The analogue to digital conversion is logarithmic The logarithmic presentation of the spectra gives the benefits of constant relative energy resolution and for low energy isotopes CH enhanced possibilities for the optimization of the signal to noise ratio 19 The concept of total optimization 32p Sample spectra 3H 14c after linear amplification Logarithmic A D conversion 14C Sample spectra after A D conversion l l 1 2 3 4 5 6 7 8 9 10 x 100 1 1024 MCA channels The user interface software WinQ includes a function called auto scaling the vertical scale is automatica
87. eak This varies between 50 500 cpm depended on the location of the instrument The more material above the instrument the more it is protected against the cosmic radiation Note The cosmic peak is not stable It varies depended on the weather conditions air pressure and humidity 194 Performance test A 5 824 CPM ch 493 49 min A NSTEFANS Q636561N 661 SPHZ1 200 1200 cpm 50 500 cpm Typical 800 Typical 400 1 188 288 388 488 588 688 788 888 988 INTEGR C 1 1824 A 1263 534 CPM 38 4 8880 8 4 x BUNCH 1 CA Q8380581N 001 21 B1 SP 22 is the guard in coincidence with the sample In other words these are the events subtracted from the actual sample Depending on the intensity of the cosmic peak and the sample volume the value varies between 5 25 cpm Typical value is 20 25 cpm 195 Performance test A 8 283 CPM ch 493 49 min A NSTEFANS Q636561N 661 SPH22 1 188 200 388 488 988 1888 INTEGR 1 1824 Al 16 963 CPM BUNCH 3 _ 3S 556 3 3 y CA Q838581N 881 22 B 196 Trade name Quantulus Guard Scintillation liquid Date 30 06 1996 Former date x MATERIAL SAFETY DATA INFORMATION FORM FOR CHEMICALS SHEET DATA Date 30 06 1996 Former date 1 IDENTIFICATION OF THE CHEMICAL AND OF THE MANUFACTURER IMPORTER OR OTHER UNDERTAKING 1 1 Identification of the substance or preparation Trade name Quantulus Guard Scintillation Liquid Code of the preparation 1 2 I
88. eared Note there must be a sample defined before proceeding beyond this point If you answer Y es the present state of the block will be printed out If the block has been cleared then only the headings will appear If parameters have been set then the value will appear beneath the heading ER POS ID CTIME COUNTS CUCNTS MCW REP STD STMS STIME d 6 CL36 30 00 NO LIM NO LIM 1 Hu N The headings are defined as follows 115 Mode 6 Quasi simultaneous counting program The position parameter program block has the following parameters ORDER The running line number of the sample information The increasing order is set by the instrument The instrument counts the positions following the order number A maximum of 24 order numbers is allowed POSITION Sample position to be counted If several positions are counted with the same counting time the first and last positions can be typed in Le 2 10 means that positions 2 to 10 can be counted with the same settings The positions can be typed in in any order A maximum of 60 positions is allowed ID An identification can be given to the sample s or the position using up to 16 characters CTIME Counting time for the positions Time is given in minutes It is also possible to give time in hours or seconds by following the value by space then H or S respectively COUNTS Stops counting when the number of counts set here has been reached Note this parameter a
89. ect the spectrum of the right side 2183 OE and resume counting Adjust using trimmer R86 ER on FAD the SQP I to be according to the table subtracted with 4 channels Select the spectrum of both sides 2183 0D and resume counting Check that the SQP I is according to the table CAUTION DO NOT ADJUST TEMPERATURE COMPENSATION TRIMMERS R1 AND R3 ON THE FAD BOARD After the calibration go to the SERVICE PROGRAM by pressing T when in the READY state and in the service program press MC to make MASTER CLEAR to restore the original MCA configuration EE 745 201 99 705 185 1973 665 171 o48 74 io 995 70 183 1970 e6 170 945 73 5 197 992 695 fisi 1966 es5 168 942 73 ios 199 s 19 oo es 167 939 7255 193 1985 6 amp 5 177 o60 645 166 936 72 191 982 s 176 1957 ea 165 933 187 Installation of the PC E 71 0 70 5 70 0 69 5 69 0 68 5 68 0 67 5 SQP I 187 185 183 181 SQP E table for EU 152 SQP E E SQP SQP E 932 67 0 173 913 929 66 5 171 910 927 66 0 170 908 925 65 5 168 906 922 65 0 167 903 920 64 5 166 901 918 64 0 165 899 915 SQP E within 25 channels SERVICE gt PR PR 2A03 2180 2181 2182 2183 01 0D L R table value 1 channel OFL table value 4ch 1 channel OER table value 4ch 1 channel To be sure that th
90. ect the standardization parameters control letter S must be typed and Return pressed The current date and time will be printed out and the title Standardization Program Parameter Group Selection The results of a standardization measurement i e the quench curve become part of a parameter group therefore it is necessary to specify what this group is before beginning the standardization routine Once the group number is given and Return pressed the summary of the group count mode will be printed out and then parameter setting can begin Two lines appear for parameter lines 1 4 and 5 if the dual label counting mode is selected The standard samples can be placed in any order the instrument automatically records the results in decreasing order of quench level Line 01 Positions of Standards The number of standard points to be obtained for the quench curve must be given by giving the positions of the standards a maximum of ten is allowed If correction has been selected in the P program then the vial type glass or plastic will be asked after the positions of standards Line 02 Automatic Run Selection There are two modes manual and automatic The latter mode allows a quench standard to be measured and then unknowns evaluated using the resulting quench curve without any further user intervention It also place restrictions on the methods of quench measurement Only the two automatic methods 2 and 3 can be used Automatic run is selected by
91. essed down The video terminal printer can be on line or off line the latter is often used during editing of a counting protocol The backspace key can be used for correcting typing errors before the return key is pressed The printer must be on line Take care that there is sufficient paper and that the paper runs freely Using the computer If Quantulus is operated with the computer connected to Terminal 2 the following must be observed The computer will automatically boot up the Quantulus software after power up Take care that the caps lock key is pressed down this is indicated by the signal on the caps lock key newer user interfaces do not require CAPS LOCK on see the software manual For communication with the counter the communication program must be selected by pressing function key 3 When the computer is in communication with Quantulus the READY prompt 41 General features will appear on the screen in response to the RETURN key for newer user interfaces see the software manual Commands in the READY state When the instrument is idle or when the power has been connected the message READY followed by an arrow READY gt can be seen on the screen The instrument is now ready to be operated By typing a question mark the HELP function will give a listing of possible actions READY gt Help Commands in the READY state press RETURN after a command set date and time display
92. esults are given in decimal or exponential form Lines 28 amp 29 Half Life For fast decaying isotopes it is necessary to correct for the reduction in sample activity over the period of measurement of a batch of samples The half life in hours can be entered on these lines for both single or dual labelled samples the range is 0 1 to 99000 hr See the Half Life section for more information 59 Mode 1 CPM DPM Line 30 Number of Cycles Samples on the conveyor will be passed through the counting position for the number of times specified by this parameter range 1 to 99 This parameter acts as a sort of repeat count for a batch of samples This process will continue until the number of cycles has been completed then counting of the next batch will begin Lines 31 8 32 Reference Samples The results for the samples in a batch can be compared to reference samples and the result of the comparison is printed out as a percentage of the reference The positions of the reference samples are coded by giving the lowest and highest positions One set of reference samples can be given for each isotope if dual labelled Reference 1 samples must be measured after background samples and before reference 2 samples The average of the results for the reference samples is calculated and used for the comparison When counting repeats or replicates if REF1 and REF2 have been selected the average percentage is calculated when the statistical analys
93. f high beta activity It also allows a great reduction in beta background particularly in glass vials further reducing the already low background achieved 14 The concept of total optimization by the active anticoincidence guard detector In this software the PSA level can also be set based on the figure of merit For more details of this feature see the separate chapter on PSA Pulse amplitude comparison PAC Another feature of Quantulus is the Pulse Amplitude Comparator This provides a means for decreasing the background component produced by optical crosstalk in liquid scintillation counting See the separate chapter for more details Computer The data output from the instrument can be large For each sample measurement CPM from up to 8 counting windows up to 5 x 1024 channel spectra and position count time sample ID or other selected information regarding the sample To be able to fully use all possible data validation a computer is necessary Quantulus is combined with a personal computer with a hard drive a floppy disc drive and a printer Separate manuals exist for additional computer software such as the user interface and spectrum analysis program The computer can also act as a terminal then the Quantulus is operated using the computer keyboard The concept of total optimization realized as it is in the design and construction of the Quantulus enables the accurate measurement of the low levels of radioactivity found
94. gradable cocktails are slow as those based on di isopropylnaphthalene DIN Wallac PSA principle Integrates the tail of the pulse for long enough time to enable differentiation between short and long pulses see the figure below Norm d light intensity 0 100 200 300 Time ns Pulse shape for events caused by beta and alpha particles 21 The concept of total optimization Normalizes the pulse length information to the pulse height to achieve amplitude independence The alpha beta pulse amplitude energy spectrum is transformed in the process to a three dimensional counts vs pulse amplitude and pulse spectrum see the following two figures Electronic division of pulses into alpha and beta spectra is carried out by dividing the pulse amplitude length plane in two parts by a straight user adjustable line pulses above it are directed into the long pulse spectrum pulses below it into a short pulse spectrum When the dividing line is correctly set the former spectrum is the pure alpha spectrum and the latter one is the beta spectrum The position of the dividing line is controlled by PSA level adjustment This feature allows setting to conform with various solvents fluors and quench levels Pulse length vs pulse height for Ra 226 by Quantulus Pulse length PSA level N Pulse height 3 D spectrum of Ra 226 vs Pulse amplitude total signal and pulse length tail signal 22 The concept of total optimization
95. his is the second question on line 16A If it is answered Y Yes then a small scale plot of the stored curve will be displayed immediately after Return is pressed Then another parameter line will appear with the question Lines 17 amp 18 19 Background Sample and Background Subtraction The CPM in the counting window s can be corrected for the background contribution This contribution can be an experimental background and or the natural background in the laboratory The experimental background can be for example background radiation from the counter lane when counting samples are labelled with both a beta and a gamma emitter The natural background is cosmic radiation and naturally occurring radiation in the laboratory building material The contribution of this background has to be corrected for when counting low activity samples Quantulus automatically corrects the CPM in the counting windows using either a measured background for background samples or estimated background CPM values these can also be experimental values In both cases it should be remembered that the background is dependent on the sample and cocktail volume and the background counting efficiency 58 Mode 1 CPM DPM If background samples are used the position of these samples are coded in answer to line number 17 The average background CPM in the counting windows is automatically used to correct the unknown sample CPMs If background samples are no
96. iation shield i e ken tere venio ved va e A edet a RON FORI 133 Operating O fs Sese es ipee eei aee ib pastel Ses ee 134 Temp rature Controls coo mE 134 Sample changer and cony6yOt ice edite asco ia 134 ALI rc pM ELM 135 Detector assembly esce ce oa eere betae tu een acm eorr tc rr d i eo eL Dru 135 A dana utu ig C ot e orem uv 135 Stability T ee saat sans 135 Electronic Ward Wate a a da 135 jr qc EE 135 Automatic continuous spectrum stabilizet eoe e eec ep cr bt qe ena Re 135 Stand by power supply eus ace Gr eerte eor a stre e Y Hi e rtu e ge Y daas qua 136 Static electricity eliminati os easet eed Pu eate eet bate maradona Bars 136 Electromagnetic interference eliminator u a niall dos en 136 Multiuser counting CONS id 136 Externalstandard sos eod ira eisen 136 Counting conditions nen een ae Gs Ad d a TO E 136 CODO parameters seco dae ee Pe dece ne er lee 139 Routine MAIDEN CO ssia 141 Keeping the Instrumental di AA A RA 141 PONES o ate ds seres E uie ctun e o ae Saleh cael 141 O 141 AAA AA 145 Evaluation of the safety of the Eu 152 external standard source in sss 147 Low background counting requirements sssosssssnssssnnssnsnnssnsnnssnsnnsnnnnnnnnnnnsnnnnnsnnnnnennnnnennen 159 Achieving stabllity see sense ia 159 Sources of back Ground a rin 159 Wallac low level background room irrita nennt non Render deed darias 160 Other EXO
97. ich parameters can be set Some of the main types of parameter list are shown at the end of the Parameters section The first time a count mode is selected parameters will be assigned preset values the count mode will select counting windows limits and determine the printout selection preset values for the sample and external standard count times This will also occur if the Clear command is given If the mode has been previously selected and parameters edited then other values than the default ones will be shown Whichever is the case the used can edit the parameters until they are what is required If any parameter line is changed which would mean a fundamental change to the parameter group invalidating the results if used as such a warning is given If such a change is made a hard copy of standard points dedicated to the parameter group is printed out then these points are deleted Window selection This choice assumes that option 1220 114 is included in the instrument If it is not then only Fixed window can be used For a full discussion on window setting see the section entitled Windows Spectral Quench Parameter If Fixed window has been selected there are three choices of Spectral Quench parameter two for single label and one for dual label In the former the SQP can be based either on the isotope spectrum SQP I or on the external standard spectrum SQP E In the latter only SQP E can be selected SQP is described further in i
98. ied for counting If the green LED is on then no samples from that tray have been specified and the tray can be removed for loading other samples Example If sample positions 1 25 are specified then the red LEDs will be on above tray loading positions 1 and 2 but above position 3 will be the green LED If positions 1 and 2 are specified then there will be a red LED only above tray loading position 1 Starting counting The Counting Protocol Queue Quantulus activates the counting protocols in the order they are specified in a queue The setting of the queue is based on the use of a command line which allows 44 General features D isplay of the queue M odification of the queue R emove to remove items from the queue I nsert a parameter group into the queue S tart counting The queue determines in which order the parameter groups are counted When command A with RETURN is typed in READY state the setting of the queue is started The first question is Data to be filed in PC Y N Y gt If this is answered Y es the Quantulus will check if the computer is ready to accept data If the computer is using a dedicated communication routine Quantulus then asks for the first parameter group to be counted by printing on the screen 1 assay in queue PARAMETER GROUP NUMBER 0 gt If a slash is typed in it will return to the command line If there is no queue present type in the parameter group number which i
99. if SQP is selected The external standard has an activity of 37 KBq it is normally sufficient to count it for 2 min to get adequate statistics However other counting times can be set if required by entering the value in minutes or seconds using S or hours using H here The range is 1 to 9999 sec 2 hours Line 13 External Standard Maximum Counts This acts like the maximum counts for samples on line 4 except that it is now for the external standard Line 14 Printout Selection Printout selection determines what will be printed out the heading of each printout column and the order of columns There are 48 printout codes each of which is a number specifying one type of printout Up to 33 codes can be selected for print out Text can also be included as described in the section entitled Printout 1 2 55 4 r215225 9 1L0 nt coding CPM1 CPM1 SQP E E DPM1 DPM1 EFF1 21 P E 31 DPS2 CPM6 COUNTS2 22 P E 32 SREF1 CPM7 CPM2 23 33 SREF2 CPM8 FCCPM2 24 34 DATE CPM1 CPM2 CPM2 25 35 E CPM2 CPM1 DPM2 26 36 E E DPM1 DPM2 FDPM2 27 F 37 E E DPM2 DPM1 DPM2 28 PM2 38 DTIMES 19 EFF2 29 SQP I 39 E EXT 20 SOP I 30 DPS1 40 NE INE Range 1 33 codes Type x y z t to add codes x and y and to subtract codes z and t Type to go to the READY state Type Lx RETURN to jump to line number x oO 10 01 CO ho S 1 2 3 4 5 6 8 9 10
100. igurations or to be freely set The preset configurations are given below To set the MCA configuration means the following the analogue signal can be selected this is the pulse which will be converted the logic trigger pulse for conversion can be selected the anticoincidence pulse or inhibit pulse can be selected the MCA split pulse can be selected this is the pulse which determines in which half of the dual MCA the converted analogue signal is stored Both MCAs are programmable in the way described above An MCA configuration is then the combination of the selected analogue and logical signals which are determined for the assay As the MCA configurations are set by the counter software and not by hardware the 32 The concept of total optimization configuration can vary between the 8 counting parameter groups When a new parameter group in the queue is started the MCA configuration specified in the parameter group is set and counting is started The possibility to freely set the MCA configuration enables total monitoring of the instrument performance and measuring conditions to be set so that maximal data validation can be obtained The two preset conditions will however offer a powerful choice for most applications Configuration 1 for low energy isotopes H and configuration 2 for high energy isotopes C A third configuration is available as the default in the windowed workstation the Queue Manager alpha beta sepa
101. iminator is triggered and they will be accepted as a pulse and counted At very high count rates the contributions of these random coincidences can make a considerable contribution to the counted spectra As the random coincidence is the sum of two single photons the chemiluminescence spectrum is in the low energy end in channels 5 100 and a problem only when counting H or some other low energy isotope The chemiluminescence reaction rate decays with time so that after keeping the samples in a dark cupboard at room temperature overnight the rate is so low that it does not normally disturb the counting The reaction rate can be speeded up by increasing the temperature of the samples or by stirring Other methods to reduce chemiluminescence are to add some acid HCI or ascorbic acid to the samples to return the pH value to below 7 Quantulus has a built in monitor for the detection of random coincidences this is called the chemiluminescence monitor Its function is the following the radioactive decay gives rise to multiple photon reactions as one disintegration releases energy sufficient for many photons to be produced in the scintillation cocktail Characteristic for a multi photon event is that both PM tubes see the scintillations inside a very short time a few nanoseconds If the signal from one of the PM tubes is delayed longer than the time of the scintillations then there will be no signal from the tube whose signal was delayed and the con
102. inse immediately with copious amount of water at least 15 minutes and seek medical advice 4 5 Ingestion If swallowed do not induce vomiting Give patient milk or water to drink keep warm Call a physician 4 6 Information to doctor or other trained persons giving first aid 5 FIRE FIGHTING MEASURES 5 1 Suitable extinguishing media Foam carbon dioxide 5 2 Extinguishing media which must not be used for safety reasons 5 3 Special exposure hazards in a fire 5 4 Special protective equipment for a fire 5 5 Other instructions 6 ACCIDENTAL RELEASE MEASURES 6 1 Personal precautions See section 7 1 6 2 Environmental precautions Do not allow run off to sewer waterway or ground 6 3 Methods for cleaning up Absorb on sand paper vermiculite or other appropriate material and place in a closed container for disposal Wash the area with water and detergent 6 4 Other instructions 7 HANDLING AND STORAGE 7 4 Handling Wear splash proof eye goggles and gloves Avoid contact with the product NOTICE These measures are not normally needed as the liquid is in a sealed place inside the device 7 2 Storage Store at moderate temperatures in dry well ventilated place Keep tightly closed 8 EXPOSURE CONTROLS PERSONAL PROTECTION 8 1 Technical measures for exposure controls Proper ventilation in working areas Take precautionary measures against static discharge NOTICE Empty containers may contain reactive residues Handle with care
103. ints is 10 137 Specifications Plot of standard curve and edit possibility DMP results for single and dual labelled samples Chemiluminescence monitor based on delayed coincidence The random coincidence spectrum is measured in one half of the MCA and subtracted from normal beta coincidence spectrum The contribution as percent of result CPM is given CLM gt 10 causes a warning to be printed Calendar clock Instrument contains calendar clock giving date and time Printout of time in READY state Printout of time in count result is also possible using printout code for time The instrument software is Y2K compliant Help function Ease of instrument operation is ensured by the Help Function giving information about operating possibilities in READY state and in parameter editing Mode 2 spectrum plot program Plot of the isotope spectrum or ext std spectrum from multichannel memory High resolution graphics plots are available in mode 6 with the aid of Spectrum Analyzer Software see below Mode 6 quasi simultaneous or low background counting mode This count mode offers the full control of two MCAs by Boolean logic commands There are hundreds of combinations to control measurement MCA is a sophisticated device capable of collecting up to four spectra external std spectrum from the sample simultaneously The four spectra may all be from sample under different conditions The spectra can be saved on hard disk or d
104. ion can be obtained from the instrument to help in operating it At any point where a user instruction is needed the HELP function can be activated by typing and pressing Return An explanation of what the possibilities are including the range of values allowed for a parameter if it is a parameter help in question will appear on the display and then again the command line or parameter line will be presented for the user s choice to be entered Sample handling Quantulus takes up to three sample trays each with a maximum of twenty samples Sample positions 1 20 are found on tray 1 21 40 on tray 2 and 41 60 on tray 3 The following table shows the order of samples 1 2 3 4 5 21 22 23 24 25 41 42 43 44 45 6 7 8 9 10 26 27 28 29 30 46 47 48 49 50 T2 G3 14 T5 Sd 632 33 0345 235 5L 252 253 D4 59 16 IT 189 19 20 36 37 38 39 40 56 57 58 59 60 When trays are loaded tray 1 occupies the leftmost position tray 2 the middle and tray 3 the rightmost position If possible samples should be loaded so as to fill one tray before putting samples into the next This releases the other trays for others to use When trays are loaded onto the counter check that the tray is not placed in the position of a tray under measurement as it will be returned to the empty space Above each loading position there are two LEDs one red and one green If the red LED is on it shows that during parameter setting samples from the tray in that position were specif
105. irculated and counted several times the average results are then used Traditional LSC counters have the limitation that the order in which samples are counted is fixed once the samples are loaded on to the counter This is not the case for the Quantulus The unique sample changer mechanism and the counting protocol give total freedom to determine in which order samples are counted 13 The concept of total optimization In addition the counting time can be individually determined for each sample This random access counting with a variable time base has advantages when reaching for the extreme limits of counter performance The fact that the efficiency and the background count rate are determined several times during the counting of the unknowns enables the monitoring of sample stability instrument stability and possible background variations Electronic noise suppression The modern laboratory has many types of electrical and electronic equipment Deep freezes refrigerators heating equipment equipped with thermostats and similar equipment switch on and off throughout the day This switching can cause disturbances to an LSC counter both as radio frequency noise picked up by the electronics or noise on the mains power lines The disturbances can be seen as short bursts of high count rates The use of polyethene vials can cause problems with static electricity because the vials are charged during sample preparation or during the mo
106. irection To go back to some item inside a block it is necessary to return to the command line 114 Mode 6 Quasi simultaneous counting program and start again The item in question is quickly reached by advancing through the questions by pressing RETURN Identifier The first information to be given in Mode 6 is the parameter group identifier In response to the prompt ID gt type in an identification for the parameter group with a maximum of 20 characters Line selection By typing in a line number the program will jump directly to the line specified By typing L a listing of the program is obtained By typing RETURN the program goes to the first line zero BLOCK 1 Line 1 Set position parameters In this block it is possible to specify the sample positions to be counted the order in which they are counted the counting time and counts termination limits for each position Further position specific parameters are the external standard and position repeat counts but in this program version external standard is not used for automatic quench correction however its value can be generated The command line gives possibilities to display modify remove insert and copy The format and use of these functions can be learned from the HELP for the command line 01 SET POSITION PARA TERS Y gt ER POS ID CTIME COUNTS CUCNTS MCW REP STD STMS STIME This is the order line when the block has been cl
107. is is made If reference samples for two isotopes are coded the question Dual Label CPM counting will be asked and needs to be replied Y or N By answering Y Yes to this question coefficients will be calculated using the reference samples which enables spillover corrections to be made for the two isotopes in the respective counting windows Saving Parameters After the Return has been pressed on line 31 or 32 if it appears the program will show the message SAVING PARAMETER GROUP x where x is the group number selected at the beginning of parameter setting This message will also appear after line 14 if only the shorter list has been selected or if parameter setting is terminated using the slash command This means that all the changes made to the parameters will be stored under group number x and the values there previously will be lost After parameters have been stored the program will return to the Ready state Parameter editing functions There are three instructions in addition to the Help function which simplify parameter setting and editing 60 Mode 1 CPM DPM Jump to another line Lx To jump to another parameter line before or after the one you are on type L then the line number you want to go to and press RETURN e g if you are on line 10 and want to go to line 5 type L5 and press RETURN Jump to READY Anytime you want to leave parameter setting and go to the READY state type Correct
108. iskette see SPA below Modes available are for instance default 3H and 14C MCA modes coincidence sample counts with guard counter active or low background counting sample in anticoincidence with the guard coincidence sample counts with guard counter inactive can be used for high activity samples 138 Specifications Cerenkov counting in noncoincident mode with without guard monitoring facilities are available for the user to look at any PMT noise random coincidence signal guard performance vs time can be monitored 1 e coincident active and anticoincident inactive guard pulses can be saved pulse amplitude comparison PAC can be forced with user adjustable level of rejection to reduce cross talk pulse shape analyser PSA is user adjustable to allow optimum separation of alpha particle spectra from other kinds of radiation in environmental samples like 222Rn or 226Ra water samples PSA leads to extremely low background count rates in liquid scintillation counting of alpha particles which is not achievable in standard LSC guard PAC PSA rejected sample pulses can be saved two state High Low coincidence bias operating before left right pulse summation High is tuned for low background 14C counting Low enables low energy beta counting Counting parameters 24 sample input lines parameter group each line may contain one position or a range of positions max 1 60 sample s ID max 16 ch
109. it can be created using the Copy command in the form Cx y where x is the number of the order to be copied and y is the order before which the copy is to be inserted All the order numbers after the new order will increase by one In the example here a copy of Order 4 becomes Order 5 COMMAND Display Modify Remove Insert Copy Path lt ret gt continue gt C4 5 Modifying an existing order The parameters in an existing order can be modified using the Modify command in the form Mx where x is the order number to be modified Here Order 5 is modified COMMAND Display Modify Remove Insert Copy Path lt ret gt continue gt M5 Modifying order 5 POSITION s 3 6 gt 1 2 ID TESTRUN gt FIRST COUNTING TIME 2 00 gt 5 COUNTS NO LIM gt 1E5 COUNTS NO LIM gt 100000 CUMULATIVE COUNTS 3 6605 gt WINDOW OF COUNT LIMIT 1 gt 2 REPEATS 2 EXTERNAL STANDARD Ne gt Displaying the parameter values in an order Type Dx where x is the number of an Order This will cause the contents of an Order i e the parameter values to be printed out as the example shows 118 Mode 6 Quasi simultaneous counting program COMMAND Display Modify Remove Insert Copy Path lt ret gt continue gt D4 ID CTIME COUNTS CUCNTS MCW REP STD STMS STIME 4 3 6 TESTRUN 2 00 NO LIM 3 6E05 1 2 N ORDER POS Removing an Order from the sequence Any exi
110. ition can have its own counting conditions the MCA configuration can be different for each parameter group and in the setting of count windows it is necessary to determine from which spectrum MCA and MCA Half the CPMs are collected The printouts from output ports Terminal 1 and Terminal 2 are determined independently from each other and are customized for each counting program by selecting the necessary items from a printout code list The measured spectra can also be transmitted via the Terminal 2 output port to the computer EP 1996 13 23 PARAMETER GROUP gt 7 ID CERENKOV gt LINE gt 00A PROGRAM MODE Help Program modes 1 CPM DP 2 spectrum plot 6 quasi simultaneous counting Type to go to the READY state Type Lx RETURN to jump to line number x 00A PROGRAM MODE gt Program mode 6 is built up in 4 main blocks Block 1 sample or position related data Block 2 MCA configuration Block 3 window settings Block 4 printout for both output terminals 113 Mode 6 Quasi simultaneous counting program Counting program editing is started by pressing P when the instrument is in the READY state When the parameter group number has been typed in editing can be started The HELP function is activated at any point by the question mark and RETURN Setting standard parameters If the parameter group number is preceded by the letter C i e C2 the parame
111. ity of the counter background Thus an elevated stable background is far better than a low variable background To achieve stability one must have a stable instrument environment and sample The sample should not change its composition as a function of time such as separating into two phases this can be monitored visually looking at the spectra and their statistics and by SQP E Generally it is recommended to let the samples cool down before counting Quantulus is stable in stable environmental conditions Below some hints are given about how to achieve as good a laboratory environment as possible Sources of background The background count rate of an instrument is a function of several environmental conditions Background is introduced by the inherent radioactivity of the instrument and sample containers cosmic particles and their secondaries and by environmental gamma radiation Wallac 1220 Quantulus is carefully constructed by using ultra low activity materials to minimize the inherent background of the instrument Selected phototubes are the only radioactive components in the close vicinity of the counting chamber The 40K of glass presents a stable background contribution and is reduced by using quartz in the tubes In liquid scintillation counting considerable background increase is introduced especially in the low energy region 3H if glass vials always containing some 40K are used Plastic and teflon vials can very well be u
112. lation of the PC Installation of the PC Install the SPA Spectrum Analysis Program and the QMGR QueueManaGeR to the computer according to the instructions followed with the programs Connect the cable 1221 459 for 25 pin or 1221 470 503 with shielding for 9 pin to COM1 of the computer and to port 2 of the instrument and switch it on General Information of the SPA and QMGR program QMGR In the QMGR different users can edit and save different protocols for the 1220 When the measurement is started the protocol s are queued and the one being measured is sent to the instrument During the measurement the live spectrum can be displayed on the screen of the monitor The programming is done by jumping between Queue 1 the Users and the Protocol with the arrows keys on the keyboard 181 Installation of the PC For creating a protocol you have to create a new user and a new protocol for that user Use the arrows and highlight Users on the screen Push F4 and type a user name i e TEST and then press enter Then highlight Protocol push F4 and type the saving path i e C perftest Jump through the protocol with the keyboard arrows and set the protocol you want to run Le General Parameters MCA amp Counter Window Settings Saving path C TEST Configuration 14C high energy B Protocol name PERFTEST Send spectra All PAC 1 Number of cycles 30 Number of channels 1024 PSA N A Parameter listing YES Coincidence bias LOW
113. lay Modify Remove Insert List groups Start counting gt S EP 1996 11 30 PARAMETER G ID C14 0A PROGRAM MODI COUNT MODE FIXED WINDOW SOP I SINGLE C 14 POSITIONS 1 10 gt LISTING Y TIME 1 00 COUNTS 1 900000 gt NUMBER OF WINDOWS qw DOW 1 195 645 gt DL 1 2 5 7 20 29 POS CTIME CPM1 CPM1 SOP I SOP 1 001 1 01 36553 10 919 169 54 1 13 CONVEYOR CLEARING TOTAL COUNT RATE 36553 1 CPM COUNTING INTERRUPTED PARAMETER GROUP 05 POS 002 EADY gt 98 Mode 2 Spectrum plot Mode 2 Parameters 99 100 Mode 2 Spectrum plot Mode 2 Spectrum plot A copy of the spectrum accumulated in the multichannel analyser memory can be printed in 57 characters resolution using the spectrum plot program which is obtained by selecting Program Mode 2 in parameter setting This mode has its own set of parameters beginning with line 40 Both the isotope spectrum and the external standard spectrum can be plotted The plot can be formatted using the window width and step functions Window width determines the number of channels which are summed together for the plot The step function determines how many channels there are between the lower limits of two successive windows If the number of step channels is less than window channels the spectrum will be smoothed
114. lectricity building up with some plastic vials in the most cases Quantulus deionizer and metal vial holders light shutters will remove the problem Static loading The maximum static load by the instrument is 1 tn sq meter One may distribute the load on a larger surface A 2x2 meter reinforcement would reduce the load by the instrument to 250 kp sq meter On steel reinforced concrete floors only small plates under the feet are normally necessary there is little advantage in using e g steel plate since a 200x200x2 cm plate would weigh some 600 kg by itself One might consider a thick plywood plate instead Anticoincidence guard Quantulus is run with an anticoincidence guard counter activated for low activity samples The minimum requirements to be considered for samples and counting room are then the ones printed in italics above Literature Numerous low level counting labs have been introduced in the Proc of the 3rd Int Conf on Low Level Counting Bratislava Czechoslovakia 21 25 Oct 1985 Nucl Instr amp Methods in Phys Res B17 5 6 1986 L Kaihola H Kojola and R Kananen Low Level Liquid Scintillation Counter Performance in a Low Level Surface Laboratory Nucl Instr Meth Phys Res B17 5 6 509 1986 161 Installation Installation Environment Although normal clean laboratory conditions are usually quite satisfactory as an operational environment it is useful to take the following points into consider
115. ll channels the energy distribution is shown by the content of each channel The multichannel analyser opens new possibilities the spectra can be stored and analysed possibilities for spectrum analysis and spectrum display are enhanced With the whole spectrum stored the number of counting windows can easily be increased Quantulus offers 8 independently usable counting windows e g for optimization of windows in low level counting As a consequence of the MCA approach Quantulus offers two alternatives for visualizing the counted spectra With the spectrum display it is possible to follow the growth of the spectrum during counting after the end of counting a hard copy of the spectrum can be obtained with the Spectrum Plot program mode 2 Indicator lights There are two LEDs on the upper front panel Stable spectrum stabilizer working correctly ON OFF shows the status of the instrument whether it is ON or OFF Error messages Power Failure If the mains power goes off during operation stored parameters will remain in the EEPROM indefinitely and the standby power supply comes into operation If a power failure occurs there will be a delay of 2 mins after which POWER FAILURE will be printed Use of the following commands without RETURN is possible during the delay period C this enters the Master Clear program the instrument returns to the READY state parameters are retained in the EEPROM 47 General features RETURN bypa
116. lly adjusted according to the number of counts collected during the counting The counting window limits for Windows 1 and 2 are marked by cursors You can change these limits in WinQ The logarithmic presentation spreads the spectra out over a larger channel range than the linear MCA spectra thus when the optimization of the measuring conditions are done the counting window limits can be set in smaller steps giving better resolution The setting of the MCA configuration is done by simple Boolean logic commands in the counter software For easy use preset configurations can be selected See the WinQ user manual for further information 20 The concept of total optimization Pulse shape analysis PSA Introduction Pulse Shape Analysis PSA was introduced first by Wallac for 1220 Quantulus in 1986 and since then it has been a standard feature in many Wallac liquid scintillation counters Physical background Alpha particles emit 5 MeV or more energy which is able to create triplet states in solvent which de excite to ground state slower than singlet states produced by beta particles Measurement of the pulse decay time or length allows identification of the particle which caused it and enables simultaneous recording of pure alpha and beta spectra respectively Pulse length depends also on the solvent and fluors used There are fast cocktails containing volatile solvents such as xylene pseudocumene toluene and dioxane Safe biode
117. m stabilization essere 12 Random ACCESS AU a e o es uae e 13 Electronic noise SODDIOSSEOTI sale 14 Pulse shape analysis TPSA o ee 14 Pulse amplitude comparison TIPA CA a A ao aes 15 o cc CU RUE 15 Detector shielding uiia eto ES Rapt E Nen e e NE bRe P eue EE e PRe ER kann 16 Passive shield eise iecore vii Eee aan 16 Multiple multichannel analyser technology 2000000000000000000000000000000000000000000000 0000000000000 19 Why multiple multichannel analyser techno Es 19 Howisitachieved Soon oe eor eh Ui ue ed y ah ttu d a em c esa oak 19 The multichannel analysers is 19 Pulse shape analysis PSA east 21 A O eee ew a aoa 21 Physical background asus e e a th teats t ein Stal aa 21 Wallac PSA prinemple meer Eros enden 21 Wallac PSA xl lesen 23 Lsage of pulse shape analysis see iin 23 Advantages of alpha counting by LSC e Casse esent rend ren ens sut eae nega Cot tegat ene ede aee eee en 24 P lse shape analysis and Quelie hioc a 24 A NR NIME 26 Pulse amplitude comparison PAQ eere eese eese ee eene eren eee en nest tn seen seta setas etna seo 27 Entroductoti oon cov uti ss M SM e Sanat a MEM ME MI de MD MEUS 27 Physical back strong nennen essen 27 llo aora c0 c NR 21 Contents Program MO di 29 O A CMS 29 Program mode 1 CP IV DPM didas 29 Program mode 2 Spectrum plot progr Mii a V rag ra a Eas 31 Program mode 6 Quasi simultaneous program mode seen 32 Preset
118. mance Typical counting efficiency for sealed nitrogen flushed organic samples 3H 66 14C 95 Stability Count variation less than 0 2 24 hours not including random statistics Electronic hardware Microprocessor controlled counting and data reduction Separate microprocessor control of display functions Memory configuration ROM 128 k RAM 642 k and EEPROM 16 k Logarithmic A D converter energy range 1 2000 keV beta Two dual 2 x 1024 channel programmable multichannel analyzers enable acquisition of up to 5 spectra per sample Built in dead time correction compensates for lost counts to high activity samples Up to 8 preprogrammable counting windows Display Any of the four spectra produced by the two MCAs can be selected for display on external computer screen using user interface software 1220 305 Queue Manager or 1220 307 WinQ Automatic continuous spectrum stabilizer The performance of the PM tubes and pulse amplifiers is automatically checked 62 times second using green GaP LEDs as reference light sources and the high voltage is adjusted automatically to keep the signal output constant 135 Specifications Stand by power supply Battery support for RAM memory to give automatic restart after power failure maximum 50 h Parameter group data stored indefinitely in EEPROM memory Static electricity eliminator Ionizer unit to protect against static electricity created during sample preparation and rack moveme
119. n a Liquid Scintillation Counter the most important part is the photomultiplier tube section including the pulse amplifiers the instability of whose components can be seen immediately as a spread in the results Factors such as temperature variations drift in the high voltage aging of the PM tubes can cause errors if not corrected for Quantulus as all Wallac counters incorporates the Automatic Continuous Spectrum Stabilizer which will check counter performance automatically 63 times per second and correct if any drift is observed The basic principle for the ACSS is the following Reference light sources light emitting diodes emit a light pulse of constant intensity The responses of the PM tubes and amplifiers to the light pulses are compared to a reference voltage and if they differ from it the high voltage is corrected 85 Mode 1 CPM DPM The light emitting diodes of the ACSS unit are used at a very low intensity thus the life time of the LEDs are ensured to be longer than the life time of the PM tubes The temperature dependence of the circuitry driving the LEDs is made to be the same as that of the counter so that the LED output and thus counter stability is independent of temperature variations in the range 15 35 C Sample quality monitor One problem in liquid scintillation counting is inhomogeneity of the mixture composed of the sample being analysed and the liquid scintillation cocktail If sample and co
120. nch Pulse length Pulse length is a function of sample quench the higher the quench the shorter the pulse length This is a physical phenomenon not introduced by the instrument When the sample quench level is fairly consistent there is no need to adjust the PSA level from sample to sample the counting efficiency remains constant If the quench variation is large 50 Ch or more there may be need to readjust the level for variable quench or leave the PSA level at the optimum value for the lowest quench sample and let alpha efficiency drop at higher quench Compensation for quench can be carried out by using a linear fit to the efficiency vs external quench parameter SQP E programmed as an output function In Quantulus the PSA level for the optimum alpha beta separation is the lower the higher the quench 24 The concept of total optimization Counting efficiency Alpha particle counting efficiency remains close to 100 up to very high quench levels provided that the PSA level is set accordingly This is due to the fact that the number of emitted photons per decay is several thousands and there is thus room for loss of photons and decay events are still observed The alpha spectrum will shift to a lower channel at increasing quench and therefore the counting window needs to cover the range of alpha channels under variable quench Energy resolution for alpha particles Alpha energy resolution is about 300 keV FWHM at best in liquid
121. nd BKG The program suggests some windows and asks if o k Answer N and type 5 320 for W1 and 5 650 for W2 and then enter until the statistic plot is plotted Check from the plot that there are lt 1 outliers and that the probability is between 5 95 ord 2 pos 2 rep 1 Cycles 1 38 window 2 ch 5 656 MCA 1 half 1 4c 1 6 1 6 6 1 1 ak E 2 6 1 1 6 ad 8 40 MEAN COUNT RATE 2 794 8 848 cpm Theor st dev 8 217 Obs st dev 8 264 cpm 1 outliers beyond 2 48 sigma 23 B Background amp Efficiency Read the 3 H spectra into array A and the background into array B ORD 02 POS 02 STD N REP 01 CYC 001 SP 11 gt enter Name of the array to read in A B C A gt A ORD 02 POS 02 STD N REP 01 CYC 001 SP 11 gt O3P5 Name of the array to read in A B C A gt B ORD 03 POS 05 STD N REP 01 CYC 001 SP 11 gt 192 Performance test F6 PLOT SPECTRA Name of the array to plot gt AB Auto scale gt Y Set windows to 5 320 with the arrows and push F4 for spectrum calculations Calculate FM and type 3 H dpms on the sample and in the instrument manual enable decay correction 12 43y type sample preparation date and measuring date Compare the results to the results on the final test data sheet in instrument manual Max deviation E 1 unit BKG 3cpm Al 763 678 CPM ch 2 93 min A NSTEFAN4SNQ616161N 661 SPH11 B1 8 189 CPM ch 493 57 min A NSTEFAN4SNQ636561N 661 SP
122. nd the next one require a numerical input not using exponential notation although the program will show the number in exponential notation CUCNTS Cumulative counts When the cumulative counts limit is exceeded the position will not be counted any more during the remaining cycles or repeats One cycle is defined as the time during which the counting of all positions programmed takes place MCW Maximum counts window If the COUNTS terminator or CUCNTS terminator are used the window whose counts are used for termination must be specified REP Number of repeats of the order per cycle STD Control of the external standard N no external standard Y external standard If the external standard is counted a quench parameter value can be obtained by selecting the SQP printout STMS Format 1 x Determines how often the external standard is counted E g 1 4 means that the external standard is counted every fourth cycle the 1st cycle then the 5th cycle then the 9th etc STIME Count time for the external standard Time in minutes hours or seconds See CTIME 116 Mode 6 Quasi simultaneous counting program Note for these last two parameters only appear if STD is selected After the existing parameter values have been listed the command line will appear Pressing cause the Help information to be displayed as the example shows COMMAND Display Modify Remove Insert Copy Path lt ret gt continue gt Help
123. ndard unquenched sample If the quench parameter is calculated from the sample spectrum the quench parameter is called Spectral Quench Parameter of isotope SOP I The SQP I is the centre of gravity of the measured isotope spectrum Quantulus includes a special program which measures the standard samples calculates efficiencies and quench parameter calculates the quench curve and assigns the curve to the specified counting parameter group The Quench curve can the be edited if needed and used to convert the CPM results to DPM results Program mode 2 Spectrum plot program The spectrum plot program plots the contents of the MCA on the printer The same MCA configuration is used as for program mode 1 It is possible to plot the sample spectrum or the external standard spectrum To modify the plot the following is possible determine the channel region which will be plotted add MCA channels together for the plot to select smoothing of the plot The spectrum plot program can be used for window optimization if Quantulus is used without the personal computer and the Quantulus PC software Then the spectrum plot program should be used to measure and plot spectra of standard and background samples from which the window which gives the best counting conditions can be selected For the actual measurement of the assay program mode or 6 can be used 31 The concept of total optimization Spectrum Analysis Program gives access to high
124. needed for low level samples The low background is achieved by the massive asymmetrical lead shield and the active shield The active shield can be used to give anticoincidence signals to the analogue to digital converter or to give a multichannel analyser split signal The split signal guides the converted pulse to the second half of the dual multichannel analyser Multichannel analyser The dual multichannel analyser mentioned above is a part of the multiple multichannel analyser technology Quantulus incorporates two dual multichannel analysers They are programmable in the sense that logical signals from the coincidence unit pulse analyser electronics active shield or guard pulses to mention just a few can be selected to trigger or inhibit analogue to digital conversion or to select the MCA memory half For ease of use preset MCA configurations can be selected for H and C analysis which gives optimized information about the samples with maximized shielding 11 The concept of total optimization Automatic continuous spectrum stabilization The Automatic Continuous Spectrum Stabilizer is a unique patented feature of Wallac instruments It comprises a GaAsP LED and a feedback loop to the HV supply for the photomultipliers the LED flashes 60 times per second The output from the photomultiplier is compared with a preset reference level and the HV is adjusted if any drift has occurred see the figure In this way changes in both the
125. nfiguration are given later in the Multichannel Analyser Technology INHIBIT l The following figure is the background spectrum of Quantulus It shows the high efficiency of the active anticoincidence shield Plot 1 shows the count rate with the shield inactive and plot 2 shows the much reduced background with the shield active our Channel C Counts per Channel number 18 The concept of total optimization Multiple multichannel analyser technology Why multiple multichannel analyser technology To achieve such high accuracy as in the Quantulus a rigorous approach to data evaluation is necessary Such an approach must encompass not only parameters relating to counting statistics but also those relating to the environment of the instrument such as variations in the cosmic flux contamination due to sample handling or radon build up During the long counting times needed for low level counting sample stability and counting efficiency variations must be monitored Disturbing phenomena such as chemiluminescence and static electricity must be detected and corrected for The active shielding adds to the instrument one more unit whose efficiency will affect the results consequently the active shielding performance must be monitored How is it achieved To accomplish this rigorous approach it is necessary to abandon pulse height discrimination based counting or the single static multichannel analyser technology Th
126. ning the four screw which attach the upper part to the lower see picture and then lift the upper part up put the upper part carefully down on the floor wrap a strong rope lead shielding is about 700kg around the lead like in the picture lift the lead shielding up 173 Installation 174 push the instrument base under the lead let the lead shielding slowly down and guide the instrument so the lead goes on the four guide pins Installation remove the support pieces for the lead shielding doors assemble the blocking piece that prevents the door from opening too much note numbers tight the screws for the lead shielding install the removed support pieces note numbers assemble the temperature sensing unit for the cooling unit according to the picture assemble the traffic lights according to the picture Note the cables 175 Installation guide the HV cables and a rmm ionizer and cooling unit cable through the left hole seen from the back see picture guide the analogue cables through the right hole separate the HV and analogue cables at the rear of the lead shielding PEN connect the cables according to the picture assemble the cables so the extra length goes like in the picture 176 Installation connect the cables according to the picture
127. nt on the conveyor lane Conveyor base and vial holders are metal for reduction of static electricity Electromagnetic interference eliminator An antenna operates in anticoincidence with the sample detector to reject electromagnetic noise interference from power lines and radiofrequency sources Multiuser counting conditions User interface is a menu driven software package called WinQ 1220 307 It also provides live display of selected spectra on computer screen Number of parameter groups or protocols is limited by the hard disk size of the computer Each user has their own area for the protocols WinQ can control four Quantuluses simultaneously External standard 1 uCi 37 kBq Eu 152 source in sealed stainless steel capsule Source is pneumatically transported to the vicinity of the sample vial for standardization Counting conditions Mode 1 CPM DPM Count mode selection of preset time counting windows quench monitor SQP and printout selection for 3H 14C 35S 45Ca 32P 1251 single labels and in dual label combinations All parameters are user programmable Sample position 1 60 Count time 1 999999 s approx 277 h or no limit Ext standard time 1 9999 s approx 2 7 hrs Ext standard count limit 900 000 or no limit 8 counting windows 1 1024 in one channel steps 136 Specifications Count termination after reached preset counts range 1 900000 This enables counting with same statistical error e g cou
128. ntal The rest of the events are from the sample its true activity or residual background SP11 By leaving the main background reduction device the guard in the memory split state one is able to record both the rejected events and the net signal 2 H 3 or other low energy beta emitters MCA INPUT TRIGG INHIBIT MEMORY SPLIT 1 LRSUM DCOS G EG L R 2 GSUM G L R Here a delayed coincidence circuitry combines another pulse stream with the prompt coincidence one see the logic below The aim is to monitor the random coincidence signal which may create problems in the energy range of e g H Using the guard as inhibit rejects pulses from external sources SP12 will contain the prompt coincidence events 1 e sample 34 The concept of total optimization background random coincidence like chemiluminescence SP11 contains only delayed coincidence events i e random coincidence 3 Free setup allows free configuration of MCA s by user selection of any control signal 4 Separation of alpha and beta particle spectra available as default in the newest windowed Quantulus workstations MCA INPUT TRIGG INHIBIT MEMORY SPLIT 1 LRSUM L R G PSA 2 GSUM G L R Here only true coincidence events from the sample are analysed and the pulse stream is divided by the pulse shape analyser see below The pulses that are longer than the PSA level set by the user will be directed into the second half of MCA1 SP12 The shorter pulses ar
129. nts limit 10 000 gives 2 standard deviations 2 Sample preparation error 0 99 5 Sample quality monitor quench curve validity for samples is monitored when counting in DPM mode Full user selectable printout format Printout can be formatted using the printout edit function and printout codes Automatic background correction using a preset background CPM or background sample Factorization of results in counting windows 1 and 2 multiplying the count rates with an input factor range 0 00001E 9 9 99999E9 Factor input in decimal or exponential form Automatic half life correction For dual label both results for both isotopes are corrected to their respective zero time Sample repeat 1 99 Sample batch cycling cycle repeat range 1 99 Sample replicates 1 99 Comparison of results in counting windows and 2 to reference sample Results are given as percent of reference 1 and reference 2 Sum of batch activity CPM or DPM are summed for all samples in the counted batch Sum is printed out at the end of the batch DPM program enables efficiency corrected results Automatic calculation of quench curves using spectral quench parameter of the isotope SQP or spectral quench parameter of external standard SQP E as quench indicators Two methods for counting of standard points Hat Trick and standard series Quench curve fit using Linear Interpolation Interpolating Spline or Smoothing Spline Maximum number of standard po
130. o the READY state Type Lx RETURN to jump to line x 126 Mode 6 Quasi simultaneous counting program Storing the parameter group Line 9 is the final line After the following message the instrument automatically stores the program and is ready for use SAVING PARAMETER GROUP 7 Editing while counting If control command E followed by Return are pressed during counting editing can be started as described below In the meantime counting of the sample in the measuring chamber will continue but no data is sent out When this sample has been counted the next one will be counted also While these two samples are being counted editing can be done without disturbing the counting Only if the duration of editing exceeds the time when the counting of the second sample ends will counting actually be suspended As the example shows either parameters or the queue can be edited by electing P or Q respectively After the end of editing R must be pressed to resume counting During editing you may not edit certain parameters These are indicated in the parameter listing by the text CANNOT BE EDITED Note the control character E will not be printed out when it is pressed but the bell will sound to show the command has been accepted Editing has been selected by pressing E although this does not show on the printout The first printout item is the command line shown next 127 Mode 6 Quasi simultaneous co
131. o the program The command C followed by the group number is used to perform this 52 Mode 1 CPM DPM operation To avoid accidental clearing of a group the user is asked to confirm the choice both to clear and the number of the group to be cleared If the choice is confirmed by typing Y Yes the clearing will occur but if N No is selected the group will not be cleared This command is useful if for example the user only wants to use the short list of parameters but is not sure if any of the extended list parameters have been changed by a previous user of the group Instead of checking every single parameter the Cx command can be given and then only those parameters the user is interested in need be selected After the clearing operation the program goes to edit the next parameter line identifier EP 1996 14 49 PARAMETER GROUP gt Help Type x or Ex RETURN to edit a parameter group number x Range Ex allows extended parameter listing in program mode 1 Type Mx y RETURN to copy a parameter group number x to group number y pe Cx RETURN to clear a parameter group number x Type to go to the READY state PARAMETER GROUP gt C4 This sets the default parameters CONFIRM CLEAR PARAMETER GROUP 4 N gt Y Confirm your choice with Yes CLEARING PARAMETER GROUP 4 ID TRITIUM Parameters can be edited as normal with
132. on Elapsed time since A or Q Return pressed unless Zero Time 2 set in which case this defines start time for S Half life section Sample channels ratio External standard channels ratio Start remaining printout on a new line CPM in window 6 CPM in window 7 CPM in window 8 Ratio of CPM in window 1 to that in window 2 Ratio of CPM in window 2 to that in window 1 Ratio of isotope 1 activity to isotope 2 activity Ratio of isotope 2 activity to isotope 1 activity Ratio of isotope 2 activity to isotope 1 activity Text can be added between quotation marks KOS GPS GPS GPS GPS GPS BS uS W CO Hj 0 1 OY O1 4 CQ IO HOW 81 Mode 1 CPM DPM Repeats and replicates Repeat Samples can be counted repeatedly maximum 99 times to check sample stability or instrument performance or to see the possible effect of chemiluminescence on the result Replicate samples can be used as a method to evaluate sample preparation errors e g standards can be counted as replicates before quenching for the evaluation of the spread and error in the standard DPM The number of repeats or replicate samples should be typed in on lines 20 or 21 The counter will count and print out the results After the last repeat or replicate the average values of various quantities see exam
133. ose summed time equals the total counting time The statistical reliability is the same but the instrument performance during the counting can be monitored by comparing the individual results for the cycles The sample stability can also be monitored by looking at spectrum shifts or variations in SQP values Ll gt 7 Range 1 999 Type Lx RETURN to jump to line x S l S2 02 NUMBER OF CYCLES Help Number of cycles Type to go to the READY state 02 NUMBER OF CYCL Line 3 Coincidence Bias L H This allows the adjustment of the coincidence trigger threshold level Low bias is suitable for low energy isotopes i e Tritium High bias is suitable for high energy isotopes i e C The high bias prevents a low pulse and a high pulse from being accepted and summed together 119 Mode 6 Quasi simultaneous counting program Such pulses can contribute to the background in the low energy channels below Ch 300 particularly in glass vials where Cerenkov radiation and fluorescence signal induced mainly by inherent K activity reside A small loss results in C signal from high bias but an improved background and figure of merit is achieved Since high bias threshold is applied to both phototube signals it has in principle the same effect in low energy region as the Pulse Amplitude Comparator has in the higher energy range 03 COINCIDENCE BIAS L H L gt Help Discrimination level L low H high
134. pe of changes in the samples when DPM data reduction is used If inhomogeneity is detected the information CHECK SAMPLE will be printed out after the results The same warning can be obtained for some other reason for example due to large volume differences between standards and unknown samples The Sample Quality Monitor functions as follows 86 Mode 1 CPM DPM If this function is to be used a standard curve must first be obtained During standardization a relationship is established between the SQP E value and the isotope spectrum endpoint This will automatically be stored together with the standard points It is assumed that the standards making up the standard curve are homogeneous and that these define the envelope of acceptable homogeneity If the Sample Quality Monitor prompt is answered Y yes then when the parameter group is used the SQP E and isotope spectrum endpoint are calculated for each sample The values obtained are compared against the stored Sample Quality curve If it is found that the values fall outside the standard homogeneity envelope then the sample is flagged as inhomogeneous As the Sample Quality Monitor is based on a relationship between the isotope spectrum and the quench indicating parameter a blank sample will naturally be flagged as inhomogeneous However the homogeneity of a background sample is of lesser importance Standardization parameter setting Selecting standardization S To sel
135. pectra sent 07 END SPECTRA 11 12 21 22 gt Help Select spectra for output on terminal 2 Alternatives Any combination of 11 12 21 22 and S stand all N none For example 11 means spectrum of MCA 1 half 1 Type to go to the READY state Type Lx RETURN to jump to line x Further the resolution of the spectra has to be determined This is done when answering the question RESOLUTION OF SPECTRA gt The resolution can be 16 32 64 128 256 512 or 1024 channels The resolution during the measurement is always 1024 channels 07 SEND SPECTRA LE p12 21 20 gt RESOLUTION OF SPECTRA 512 gt Help Resolution of spectra sent to terminal 2 Alternatives 16 32 64 128 256 512 or 1024 channels Type to go to the READY state Type Lx RETURN to jump to line x RESOLUTION OF SPECTRA 512 gt 1024 Line 8 Listing If answered Y ES a list of the counting program parameters is printed and or saved before the results 08 LISTING Ya gt Help List parameters before counting Y yes N no Type to go to the READY state Type Lx RETURN to jump to line x Line 9 Instrument Number This information is printed saved in the parameter list This is useful when several instruments send the same type of information to the same computer 09 INSTRUMENT NUMBER 1 gt Help Number of instrument Range 1 9 Type to go t
136. ple are calculated The following statistical evaluations are made The theoretical and observed errors are calculated The theoretical error is the total error expected due to the statistical nature of nuclear radiation for each sample plus the sample preparation error The theoretical error is given as a percentage of the mean The observed error is the standard deviation of the mean as a percentage of the average for repeats and replicates The chi square test is done for the observed and theoretical error The reduced chi square value is printed out for n observations X n 1 Observed error Theoretical error If the results obtained have a statistical spread which can be expected for the radioactive decay the theoretical and observed error should be about the same and the chi square value should be close to one refer to the chi square table Additional information about the quality of the results is obtained by the probability factor which is calculated This gives the percentage probability that a random sample from a true Poisson distribution of the same number of samples as the number of repeats or replicates will have a greater chi square value than the observed For example if the probability is low 2 it can be concluded that the observed deviation is abnormally large because there is only a 2 probability that a random sample from a correct distribution would have a larger chi square value If the probability
137. queue PARAME ER GROUP NUMBER 0 gt 7 YOURDIR ASSAY1 4 assay in queue PARAMETER GROUP NUMBER 0 gt COMMAND Display Modify Remove Insert List groups Start counting gt D ORDER PGROUP DIRECTORY PATH 1 3 MYDIR ASSAY1 2 5 MYDIR ASSAY2 3 7 YOURDIR ASSAY1 Display and multichannel analyser Quantulus includes two dual multichannel analysers providing logarithmic analogue to digital conversion to four 1024 channel spectra simultaneously This process can be described as follows The analogue pulses from the PM tubes are of different pulse heights depending on the energy of the beta decay The analogue to digital converter measures the pulse heights and compares them against a scale which is the maximum pulse possible divided by the number of channels in the multichannel analyser 46 General features The multichannel analyser is in practice a memory space with as many positions as the MCA channel number so that position one corresponds to scale interval one position two corresponds to scale interval two etc When the A D converter has measured a pulse height and found the scale interval corresponding to the pulse height the respective memory position or multichannel analyser channel content is incremented Thus the multichannel analyser shows both the count rate and the energy distribution of the isotope being counted the count rate is the total number of counts in a
138. ration or usage of the Pulse Shape Analyser PSA The combination of Quantulus and the computer supplied with the low level dedicated software offers unequalled possibilities for both measurements and data validation The most important feature of the QS counting mode is that it supports the PC software The spectra can after the measurement be sent to the PC together with the sample related information such as measuring time CPM and all other information selected to be sent to output port 2 The numerical data are stored ina REGISTRY TXT file in the directory specified for the assay For the spectra a unique file name for each sample is generated by the system based on the order number position repeat and the number of the cycle for the assay This file name convention enables convenient and easy file manipulations for the off line spectrum analysis Preset MCA configurations Quantulus MCA can be controlled by logic commands which are listed by on line 4 in Quantulus terminal communication see also help screen on SPECTRA There are two default modes in Quantulus internal software 1 CARBON CONFIGURATION Carbon 14 counting mode which may be used for any other higher spectrum that does not interfere with chemiluminescence 2 TRITIUM CONFIGURATION a counting mode which may be used for any other low energy beta emitter whose spectrum interferes with chemiluminescence 3 FREE SETUP for low level alpha particle counting and other spe
139. reset windows will be set automatically 05 SET WINDOW CONFIGURATION Y gt WINDOW CHANNELS MCA HALF 50 650 1 1 70 500 300 640 50 650 70 500 300 640 1 1024 1 1024 COMMAND Display Modify Remove lt ret gt continue gt Help Display window configuration Display window configuration Display MCA configuration Summary of all Set window s from x to y Disable window x ETURN or exit to next line COMMAND Display Modify Remove lt ret gt continue gt I lt ow ow 123 Mode 6 Quasi simultaneous counting program BLOCK 4 Line 6 Set Printout Line 6 starts the fourth major program block Here the printout selection is set for both terminal 1 optional VDU Terminal and or printer and terminal 2 The data sent out to terminal 2 is for a computer and will accompany the spectra which are also sent out The command line allows items to be removed and inserted into the printout list Alternatively preset printout can then be chosen 06 SET PRINTOUT Yoo Selected printout for terminal 1 A T 2 3 4 5 6 Ta 8 9 REP CTIME DTIMEI DTIME2 CUCNTS SOP SQP STIME lt 10 Td 12 13 14 15 IRS ve ID CPM1 COUNTS1 CPM1 CPM2 COUNTS2 CPM2 lt 18 19 20 2 225 23 24 25 CPM3 COUNTS3 CPM3 CPM4 COUNTS4 CPMAS lt 26 27 28 29 30 Salk 32 39 CPM5 COUNTS5 CPM5 CPM6 COUNTS6 CPM6
140. resolution printouts in mode 6 see the software manual Program mode 6 Quasi simultaneous program mode Program mode 6 is the main program mode in the Quantulus This allows optimization and measurement of all factors which affect the validation of the results Program mode 6 is also supported by PC software for off line data analysis spectrum storage communication with the Quantulus and windowless counting based on spectrum analysis see the software manual Program mode 6 offers free access to the sample conveyor the samples can be counted in any order individual time base for each sample position if wished the counting time and count terminator can be determined separately for each sample position user selectable printout for both output ports 8 counting windows program control of coincidence bias bias can be selected low or high high bias will reduce the background for high energy isotopes programmable control of the multichannel analysers by Boolean logic commands spectra output on output port 2 to computer for off line evaluation the external standard quench parameter the SQP E value can be determined for specified samples Unique for the quasi simultaneous counting mode is the possibility to set the MCA configurations Quantulus comprises 2 dual MCAs which enable the measurement of 4 spectra with 1024 channel resolution simultaneously It is possible to select the configuration to be one of two preset conf
141. response to line 15 CURVE EDIT there are three ways of altering the points These are Adding standard points Type the letter I after any of the standard point information lines and press RETURN An additional point can be added at the end of the table for each I typed Only one I can be typed per line After all the standard points have been listed blank lines are printed corresponding to the number of additional points chosen Changing points Type in the necessary information at the end of the relevant line and press RETURN Leave a space by pressing the space bar comma or dashed line between the figures typed in for the SQP EFF and WEIGHT Deleting points Type a hatch mark at the end of the line you want to delete and press RETURN Note A maximum of 10 standard points is allowed 70 Mode 1 CPM DPM Editing dual label curves When editing dual label quench curves it must be remembered that four fitting tables are printed out These are for Isotope 1 Window 1 Isotope 1 Window 2 Isotope 2 Window 1 Isotope 2 Window 2 If points are altered for one of the isotopes then the appropriate values must be given in both fitting tables relevant to that isotope The SQP value must be the same in both tables for the same point but the efficiency deviation and weight percentage values can differ The number of standards can differ between isotopes but must remain the same for one of the isotopes in both windows
142. ry small typically much less than 0 1 CPM One may therefore count natural decay series radionuclides with greater sensitivity by measuring their alpha emissions only than by counting the total alpha beta activity Another application is to count very small alpha activity in the presence of high beta activity Wallac counters can detect less than 1 DPM of alpha activity in the presence of 60000 times more beta activity b One may set the PSA to cut beta counting efficiency by 5 for instance resulting in a great reduction in the of beta background particularly in glass vials further reducing the already low background achieved by the active anticoincidence guard detector In this software the PSA level can also be set based on the figure of merit Alpha background may be reduced analogously by cutting some alpha counting efficiency Advantages of alpha counting by LSC 1 4n counting geometry equivalent to geometrical factor 1 2 No sample self absorption as in the case of planchet counting 3 Virtually 100 counting efficiency less than 50 in planchet counting and solid state alpha spectrometry 4 Simple sample preparation by mixing with a commercial cocktail 5 High throughput automatic multiple sample counting 6 Large sample capacity 7 Simultaneous alpha beta counting with separation of each spectrum using pulse shape analysis 8 Low backgrounds and great sensitivity for alpha counting Pulse shape analysis and que
143. s to be counted If a terminal program is used such as GENTERM ULTROTERM or Windows Terminal an error will result if there is an attempt to save spectral data that would be printed on screen instead Data to be filed in PC Y N Y gt Y PC not on line With terminal programs one should select N at this point If DATA TO PC is selected Yes then the next question is the directory path The name of the directory where the results are to be stored should now be typed in Quantulus will then cause the PC to make the directory If the directory already exists a warning is given Are you sure Directory Exists It is also possible to make a sub directory i e 45 General features DIRECTORY PATH MYDIR ASSAY1 causes a sub directory ASSAY to be established under the directory MY DIR If the DATA TO PC is selected as No the directory question is omitted When the last parameter group to be counted is typed in the slash returns to the command line If counting is started by typing S the queue is memorized and can be edited later If the command line is left by typing slash the instrument returns to the READY state and the queue is cleared The queue can take a maximum of 8 parameter groups READY gt A Data to be filed in PC Y N Y gt Y 1 assay in queue PARA ETER GROUP NUMBER 0 gt 3 Bee 2 assay in queue PARAMETER GROUP NUMBER 0 gt 5 MYDIR ASSAY2 3 assay in
144. samples in 3 racks 20 each can be accessed in random pre programmed order Standard 20 ml vials as well as copper teflon vials may be used Other sizes can be measured in adapters of 20 ml vial size 0 3 ml teflon for instance Lift piston may be modified on request for adapters that do not allow axial rotation The modification does not prevent counting of normal vials Rack transport is by friction belt drive system transverse movement by toothed chain driven by electric motors Sample lifted up to measuring chamber by elevator driven by electric motor Vial holder act as light shutter Sample change time is 45 s for the first sample and 20 s 134 Specifications for samples in the same rack Rack and sample position and movements are controlled by electro optical sensors Vials Maximum acceptable sample vial diameter is 28 mm and maximum height 62 mm Special Wallac copper teflon vials are available in sizes 20 15 7 and 3 ml The body of the vial has been raised to the centre of the PM tube and environmental radiation is attenuated by copper tops and bases which also reduce cross talk Any other sizes can be counted in adapters of 20 ml vial size Detector assembly There are two low noise selected PM tubes working in the detector assembly Assembly includes also light emitting diodes for the automatic spectrum stabilizer Coincidence resolution time 15 ns The PM tube high voltage is switched off between sample changes Perfor
145. sed for this purpose today since modern biodegradable cocktails will not create a plastic vial effect If a glass vial is preferred one has a means of electronic background reduction in Quantulus the so called Pulse Shape Analyser A major background component in liquid scintillation counting is the high energy cosmic radiation whose intensity varies with the atmospheric pressure and humidity Quantulus contains however an extra detector to identify external radiation and block its background contribution The detector anticoicident guard counter is external to the counting chamber and very effectively detects the high energy cosmic particles and most of other environmental radiation leading to stable sample background It is an advantage to have the laboratory built underground where cosmic radiation is attenuated by floor masses on top It is not however a necessary requirement 159 Low background counting requirements The most important factor in terms of Quantulus background is the gamma photon flux from the counting environment Wallac low level background room The Wallac low background counting room is an example of an inexpensive room with considerably reduced gamma background It has 1 m thick walls the inner halves of which are low activity concrete composed of iron ore pellets from the Finnish Outokumpu mine to replace sand not available any more plus white cement Aalborg Portland from Denmark Quartz sand can serve as
146. sses the delay and continues program execution After about ten minutes delay the program automatically goes back to the READY state if the program was in the READY state EDIT state listing parameters or editing If the instrument was counting a sample then the same sample will be recounted Mechanical Obstruction If the conveyor is mechanically obstructed after a period of one minute the instrument will stop and CONVEYOR ERROR will be printed followed by READY The obstruction should be removed and operation can then continue High Voltage Failure If the high voltage to the detectors goes off during counting the message COUNTING ERROR will be printed File Error If a parameter group is not properly initialized when the Ax command is used then the message FILE ERROR will be printed and the instrument returns to the READY state If this continues after repeating the Ax command then a fault in the EEPROMs is indicated Memory Storage Fault The error message PARAMETER SAVING FAILURE is printed out and the instrument returns to the READY state if the memorization procedure fails during any operation that requires transfer of information into the EEPROMs for storage This indicates a fault in the EEPROMs Too few counts The error message NOT ENOUGH COUNTS FOR SQP E will appear if too few counts are accumulated to allow a meaningful SQP E calculation SQP E and SQP E values will not be printed out for the sample 48 Mode 1
147. sting order can be deleted using the R command in the form Rx where x is the Order number to be removed from the sequence In the following example the orders are displayed to show that there are three of them then number 3 is deleted Display is used again to show there are only two of them Note When an order is deleted the others are renumbered COMMAND Display Modify Remove Insert Copy Path lt ret gt continue gt D ORDER POS ID CTIME COUNTS CUCNTS MCW REP STD STMS STIME 1 5 CL36 30 00 NO LIM NO LIM dl 1 N 2 7 H20 BKG 60 00 NO LIM NO LIM 1 1 N 3 8 RN 60 00 NO LIM NO LIM 1 1 N 4 3 6 TESTRUN 2 00 NO LIM 3 6E05 1 2 N D X2 HIRST 5 00 1 0E05 3 6E05 2 2 N COMMAND Display Modify Remove Insert Copy Path lt ret gt continue gt R3 COMMAND Display Modify Remove Insert Copy Path lt ret gt continue gt D ORDER POS LD CTIME COUNTS CUCNTS MCW REP STD STMS STIME 1 5 CL36 30 00 NO LIM NO LIM 1 T N 2 7 H20 BKG 60 00 NO LIM NO LIM 1 1 N 3 3 6 TESTRUN 2 00 NO LIM 3 6E05 al 2 N 4 1 2 FIRST 5 00 1 0E05 3 6E05 2 2 N COMMAND Display Modify Remove Insert Copy Path lt ret gt continue gt Line 2 Number of Cycles One Cycle is the counting of all the programmed positions Number of cycles determines how many times the sample sequence are to be counted For data evaluation it is more beneficial to divide a long counting time in shorter cycles wh
148. t coded background the CPM line 18 and 19 if more than 2 windows have been selected will be asked for each of the counting windows given on line 8 Note Background sample only applies to Window 1 for single and dual label and Window 2 for dual label but not any other windows whereas background subtraction applies to the windows for which it is set Line 20 Repeat Each sample can be counted as many times as specified by this parameter See the Repeat and Replicate section for more details about this parameter and the next Line 21 Replicate Samples The number of replicate samples can be specified with this parameter Line 22 Sample Preparation Error When samples are prepared a certain error is involved which contributes to the total error in the final result An estimate of this uncertainty can be obtained from the differences between replicates but this parameter allows the user make sure that this uncertainty is taken into account even if only single samples are being measured Lines 26 amp 27 Multiplying by a factor The CPM or DPM for windows one and two can be multiplied with the factors typed in as answers to lines 26 and 27 The corrected CPM or the DPM results for windows one and two are multiplied with the respective factors and the results are obtained by selecting the factorized CPM or DPM FCCPM 1 2 or FDPM 1 2 in the printout selection The factor limits are 0 00001 E 9 0 9999E9 or 0 00001 to 999999 R
149. t first sample 2 on tray 1 is counted then samples 41 to 50 on tray 3 are counted followed by samples 22 and 23 on tray 2 and finally sample 5 on tray 1 Line 02 Listing If a listing of the parameters in this group is required before results are printed out when measurements are taking place then answer Y Yes to this question otherwise answer N No 55 Mode 1 CPM DPM Line 03 Counting Time Give here the length of time for which each sample is to be counted The normal units are minutes and the default is 1 min The range is 1 900 000 counts 999 999 means no limitation However the units can be given in seconds or hours by following the number by S or H respectively e g 30S or 5H It is important that the time given here is long enough for enough counts to be accumulated even for the most quenched sample so that the statistical error square root of the number of counts is within the range required for the measurement Lines 04 amp 05 Maximum Counts The maximum number of counts to be accumulated can be set on these two lines For fixed window single label counting maximum counts for window 1 need to be specified on line 04 For fixed window dual label maximum counts for both window 1 and 2 need to be given using lines 04 and 05 and then during counting when both of the two maximum values are exceeded counting stops This parameter enables the user to decide on the uncertainty error level required Providing
150. ter of this counting program will be set to the default values Parameter Editing The instrument will ask for the needed data line by line New input data is entered by typing the new data and RETURN If no change is needed only RETURN need be typed to give the next question It is possible to jump from one line to any other backwards or forwards by typing in L and the line number i e L9 causes a jump to line 9 A slash given on a main command line terminates editing and returns the instrument to the Ready state after saving the parameter group Program Block Structure The main program blocks have a common structure as far as editing is concerned If the settings in any of the 4 blocks are modified the steps are the following Answer the line Y ES i e 04 set MCA configuration N gt Y the instrument responds with a listing of current settings and prints out the command line The command line gives the following possibilities by typing D the settings are displayed by typing M the settings can be modified M is generally followed by an index showing which item can be specified by typing R items can be removed i e printout codes or counting windows by typing I items can be inserted by typing C items can be copied Pressing only RETURN will cause a jump to the following item in the block Typing slash will return the program to the command line Inside a block the steps in editing are only in one d
151. the character typed BACKSPACE If you want to change what you have just typed you can do this as long as you have not pressed RETURN by using the BACKSPACE key on the keyboard Each time you press it one character will be deleted When you have got rid of all the characters you want type the new ones and then press RETURN If you have pressed RETURN and then notice something needs to be changed in the parameter value use the Lx instruction to go back to the line and give the whole parameter value again 61 Mode 1 CPM DPM EADY gt PARAME TDs LINE ER GROUP gt 00A PROGRAM MODE 1 gt 00B COUNT MODE SELECTION FIXED WINDOW 1 1 gt SOP 1 SINGLE LABEL 1 SQP E SINGLE LABEL 2 SOP E DUAL LABEL 3 2 gt H 3 Ip I I25 2 C 14 3 S 35 4 Ca 45 5 P 32 6 1 gt COUNT MODE FIXED WINDOW SOP E SINGLE LABEI H 3 01 POSITIONS 5 gt 5 02 LISTING Re 03 TIME 100 00 gt 1 04 COUNTS 1 900000 gt 07 SAMPLE QUALITY MONITOR N gt 08 NUMBER OF WINDOWS 1 gt 09 WINDOW 1 5 320 gt 12 EXTERNAL STD TIME 0 15 gt 13 EXTERNAL STD COUNTS 900000 gt i4 PRINT 1 2 8 7 21 22 8 10 gt EXTENDED PARAMETER LIST N gt Y
152. the default values Identifier The identifier is an identifying name for the group which can be set by the user if required It is purely optional but helps to identify the group in parameter group listing and can be used to give an idea of the function of the group Up to 20 alphanumeric characters can be used If no identifier is to be given or if the existing one is not to be changed only Return need be pressed Line Selection The next parameter gives the user a choice of starting at any particular parameter line by giving the line number 0 32 or of only listing the existing parameters by typing L and pressing Return The program returns to the READY state after the listing If however a line number was given then the parameter line selected will be displayed next Line 00A Program Modes There are three standard program modes The program mode determines the type of data reduction intended to be used The program modes are 1 CPM DPM counting 33 Mode 1 CPM DPM 2 Spectrum plot 6 Quasi simultaneous counting mode The rest of this section describes the Mode 1 parameter Mode 2 and Mode 6 are described in their own sections Line 00B Count modes A count mode determines the general details of the counting protocols such as windows quench indicating parameter single or dual label and isotopes One count mode is the combination chosen in each specific case The selection of the count mode automatically determines wh
153. thus eliminating the plotting of points outside the range that is significant for the unknown samples to be measured When the Repeat or Replicate mode is in operation when using the extended list if some of the repeat or replicate values of the unknown samples are outside the limits of the standard curve then OUT OF RANGE is printed if a single sample is out of range Line 07 Time Factor The time factor multiplies both standard parameters line 03 Time and line 11 External Standard Time A time factor of 1 means that the counting time will be the same as that for the unknowns 2 means twice as long etc 88 Mode 1 CPM DPM Line 08 Start Counting Counting is started by typing Y Yes and pressing Return The name of the method of producing the quench curve is printed out then the title Standardization after which counting begins The example shown on the following pages is of a dual label standardization First the parameters are set for counting dual label samples then the standardization parameters One quench series for each isotope is measured and two standard curves plotted 89 Mode 1 CPM DPM EP 1996 10 24 2 gt WINDOWS DUAL LABEL C 14 mEC CN CN SS SO SM MS O Bl OU 4S QN IP O t0 O0 2 0 UT iS COO PER E 01 POSITIONS 13 gt 02 LISTING 03 TIME 10 0 04 COUNTS 1 5000 05 COUNT
154. to high resolution printouts in mode 6 see the software manual 102 PARAMETER GROUP gt 3 ID PLOT gt LINI E gt 00A PROGRAM MODE CONFIRM CHANG Gl P MODE N 1 Mode 2 Spectrum plot READY gt P THU 19 SEP 1996 11 50 gt 2 Program Mode 2 Spectrum plot selected gt Y SPECTRUM PLOT PARAMETERS Sample positions specified ple p p 01 POSITIONS gt 1 3 40 PARAMETER LISTING 41 SPECTRUM SELECTION SAMPLE EXTERNAL STANDARD 42 TIME 44 COUNTS 45 AREA OF INTEREST 46 WINDOW WIDTH 47 STEP 48 REPEAT 49 PRINT WIDTH SAVING PARAMETER GROUP Y 1 2 1 1 00 900000 5 1024 20 20 1 80 3 gt Parameter listing before plots gt Only sample spectrum required gt 2 Count time 2 mins gt gt gt gt Other parameters unchanged 103 Mode 2 Spectrum plot EADY gt A ta to be filed in PC Y N Y gt N assay in queue RAMETER GROUP NUMBER 0 gt 3 assay in queue RAMETER GROUP NUMBER 0 gt MAND Display Modify Remove Insert List groups Start counting gt S THU 19 SEP 1996 11 52 PARAMETER GROUP 3 Parameters listed before results plotted ID PLOT 00A PROGRAM MODE 2 gt SPECTRUM PLOT PARAMET
155. ts own section If option 1220 114 is selected only SQP E can be used Isotope selection The are six single label isotopes and fourteen dual label preset isotope counting windows These are shown in the following table 54 Mode 1 CPM DPM Single label H 3 1 125 1 H 3 C 14 2 H 3 S 35 3 H 3 Ca 45 4 H 3 P 32 5 I 125 c 14 6 I 125 S 35 7 I 125 Ca 45 8 I 125 P 32 9 C 14 Ca 45 10 C 14 P 32 11 S 35 Ca 45 12 S 35 P 32 13 Ca 45 P 32 14 When the isotope has been selected the count mode specification is complete Quantulus displays a summary of the mode giving the type of window the window setting the SQP selected the number of labels and the name of the isotope s If an isotope is required which is not in the list select fixed window and an isotope with the closest window setting to that required then give the correct window on line 8 in parameter setting Line 01 Position Quantulus allows free ordering of every sample in all of the three trays Each sample is specified by its position number 1 60 so each sample will be counted in the order in which its position number is specified on parameter line 1 Each position number is separated from the next by a comma If several samples are to be counted in numeric order they can be specified by giving the first and last numbers of the sequence separated by a hyphen E g POSITIONS gt 2 41 50 22 23 5 means tha
156. unting program EDIT while COUNTING EDIT Command Parameters Queue List groups Clock Resume gt P Parameter editing selecting THU 19 SEP 1996 14 34 ETER GROUP gt 7 Group 7 is to be edited L7 gt gt POSITION PARAMETERS Y gt POS ID CTIME COUNTS CUCNTS MCW REP STD STMS 5 30 00 NO LIM NO LIM 1 1 N Display Modify Remove Back Insert lt ret gt continue gt M1 Modifying order 1 COUNTING TIME 30 00 gt COUNTS NO LIM gt CUMULATIVE COUNTS NO LIM gt These parameters can be edited REPEATS 1 gt COMMAND Display Modify Remove Back Insert lt ret gt continue gt 02 NUMBER OF CYCLES 2 This parameter can be edited 03 COINCIDENCE BIAS L H L WARNING If changed only restart allowed gt This parameter should not be edited 04 SET MCA CONFIGURATION Y WARNING If changed only restart allowed gt This parameter should not be edited CARBON CONFIG 1 TRITIUM CONFIG 2 FREE SETUP 3 3 gt MCA INPUT TRIGG INHIBIT MEMORY SPLIT 1 LRSU L R PAC G EG 2 GSU G L R COMMAND Display Modify Remove lt ret gt continue gt PULSE COMPARATOR LEVEL poss 05 SET WINDOW CONFIGURATION Y gt WINDOW CHANNELS CA HALF 1 50 650 1 1 2 70 500 1 1 3 300 640 1 1 4 50 650 1 2 5 70 500 1 2 6 300 640 1 2 7 1
157. ust the window to fit the spectrum Quantulus allows you to do this in two ways Using the spectrum display to help you adjust your window settings until the spectrum falls visually within the windows Using option 1220 114 This works by measuring first the sample with the external standard in place Then the sample spectrum alone is measured over the complete energy range The two spectra are subtracted to give the external standard spectrum From this the spectral quench parameter is obtained This is then used to calculate the optimum window setting for the sample This optimum setting is then imposed on the stored spectrum and the amount of the sample spectrum in that window is calculated and the final result printed out The spectral quench parameter guarantees a precise window setting If the status of this mode is changed e g going from fixed to automatic or vice versa the quench curve must be rerun If BATCH WINDOW is selected the results of counting the first sample of the batch are used by the instrument to select the window setting for the remaining samples This should only be used for counting a batch of samples that are similarly quenched Note The Batch Window parameter only appears if option 1220 114 is included 97 Mode 1 CPM DPM READY gt A Data to be filed in PC Y N Y gt N 1 assay in queue PARAMETER GROUP NUMBER 0 gt 5 2 assay in queue PARAMETER GROUP NUMBER 0 gt COMMAND Disp
158. vement in the counter Static electricity is also seen as random bursts of high count rates The lower the activity levels the more clearly even small disturbances can be seen in the results This has been taken into account in the construction of the Quantulus as follows the cooling device is a noise free Peltier cooling unit The lower temperature reduces thermal noise in phototubes the pulse electronics preamplifier and pulse amplifier are designed to maximize the signal to noise ratio High bias pulse amplitude comparison and pulse shape analysis can be used to boost the signal to noise ratio a radio frequency noise suppressor unit detects disturbances of this kind and inhibits the counting while they last an AC HV ionizer neutralizes static charge on the vial surface while it is raised into the counting chamber the sample changer mechanism is constructed so as to cause minimal friction between the samples and their trays and the changing mechanism Vials are contained in metal light shutters which further assists in elimination of static charge high coincidence bias can be selected for improved background and figure of merit for counting C or other high energy beta emitters in glass vials Pulse shape analysis PSA Pulse shape analysis allows identification of the particle which caused it and enables simultaneous recording of pure alpha and beta spectra and counting of very small alpha activity in the presence o
159. vials or teflon vials should be used Identification of alpha emitters Identification is always based on comparison with known samples It is possible to create calibration curves for various alpha emitters by measuring the external standard quench parameter SQP E and emission peak position Various alpha emitters will set on different lines and can then be identified by measuring the quench parameter References 1 Product News Letter Pulse Shape Analysis Wallac Oy February 1987 November 1991 2 Oikari T Kojola H Nurmi J and Kaihola L Simultaneous counting of low alpha and beta particle activities with liquid scintillation spectrometry and pulse shape analysis Int J Appl Radiat Isot 38 875 1987 3 Kaihola L Oikari T and Suontausta J Ultra sensitive alpha particle detection in the presence of high beta activity by low level liquid scintillation spectrometry Int Conf on Advances in Liquid Scintillation Spectrometry LSC94 Glasgow Scotland Aug 8 12 1994 4 Suontausta J Oikari T and Kaihola L Liquid scintillation counting with high water content cocktails Int Conf on Advances in Liquid Scintillation Spectrometry LSC94 Glasgow Scotland Aug 8 12 1994 5 DeVol T A Brown D D Leyba J D and Fjeld R A A Comparison of Four Aqueous Miscible Liquid Scintillation Cocktails with an Alpha Beta Discriminating Wallac 1415 Liquid Scintillation Counter Health Physics Journal 70 1 41
160. xecuted The instrument will continue with the next protocols in the queue after the previous one has been finished The multiple MCA technology allows an MCA configuration to be specified for each counting protocol An MCA configuration comprises parameters such as analogue signal to be converted anticoincidence conditions spectrum split signals etc A detailed discussion of MCA configurations can be found in the chapter Program modes Start up Power requirements Cooling unit Switch on Start up Start up Power Requirements Two electrical outlets each with a protective earth should be available if possible with a separate power line having an isolation switch and a fuse box for the instrument itself The power requirements are 200 VA for the instrument and 350 VA for the cooling unit If excessive disturbances to the mains voltage are anticipated a mains stabilizer may be necessary Note the cooling unit may be left connected to the normal power line because Quantulus great thermal inertia allows fairly long power shortages without major changes in temperature Cooling unit The cooling unit allows the temperature to be set to a maximum of 12 C below room temperature The temperature setting can be set by the potentiometer which is on the left side of the cooling unit The actual temperature set is twice the number on the potentiometer i e the allowed temperature setting is from 5 C to 25 C whereas the potentiometer re
161. y P2 xo Po hN2 O1 ND A DN iS OY OY XO 1 00 ON NNNNDNDNDNO CO CO 4S Hs Hs O1 O1 NOW to XO O1 O1 Nod BRB BA BA KR BA KR BA KR BA ID BWA KIA NO 4 ND CO CO CO O1 O1 O1 4S OY Oy OO 000010 010 OOO HP 68 Mode 1 CPM DPM Curve Standard curve fitting In the standardization program the standard points can be plotted out and fitted automatically by curves based on three different calculation methods Linear Interpolation LI Smoothing Spline SS Interpolation Spline IS Smoothing Spline is the standard method it fits a continuous curve to all the standard points using a different third degree polynomial to fit each pair of points It also imposes the additional restrictions that the curve has only one turning point and is as smooth as possible Interpolation Spline is similar to the smoothing spline except that no restriction is placed on the shape of the curve other than that it must be continuous Linear Interpolation fits a straight line between each pair of points In the case of dual label operation the symbols used on the quench curves are listed in the efficiency listing before the curves are plotted out Two types of curve plots are possible A full scale curve is plotted out i during a standardization run after the curve fitting information has been printed out ii when Ax is typed when the instrument has returned to the READY state after curve editing provided that the following parameter of the extended list has
162. y are visible to the user via direct control of the instrument either with DOS based data acquisition software using a line editor or menu driven Queue Manager or with the Windows user interface WinQ via the Term key However it is recommended that instead of the approach described above you use the Windows user interface You can use the protocol editor define a protocol on the three editor pages This protocol is then queued to the instrument and started with Start button WinQ usage is described in the user manual 1220 924 Data can be processed with the off line spectrum analysis program called EASY View This runs under Windows See its user manual 1224 945 for more details In this Instrument manual the material is arranged in subject blocks e g Chemiluminescence Clock etc and these blocks are in alphabetical order The key section is entitled Parameters this describes briefly all the Mode 1 parameters in the order they are found in the parameter listing Where a parameter requires a fuller treatment it is then described in its own section Introduction to the instrument operation For a specific measurement the counting parameters such as count time counting windows MCA configuration printout etc can be set by the user Eight such protocols can be stored in the instrument Counting of samples can be interrupted for editing of counting protocols or adding protocols to the queue which consists of counting protocols waiting to be e
163. y correction curve or quench curve for single labelled samples and the two efficiency curves and spillover correction curves needed for dual labelled samples Each of the 8 parameter groups can be supplied with quench curves A maximum of 10 standard points can be used to calculate the quench curve There are three methods of quench curve calculation Method 1 Single sample incremental quench Quenching agent is added progressively after each measurement The sample may be measured up to ten times Each quenched sample can be counted when START COUNTING is printed Method 2 Single sample using HatTrick calibration Quenching agent CC14 is diffused into the cocktail from a special cap Eleven measurements are made automatically when using external standardization and the mean values of each pair of measurements are calculated and stored giving ten calibration points The starting SQP D or SQP E may be used to define the starting quench level for which quench points are stored Note the HatTrick kit has been discontinued in 1996 Method 3 Standard Series A series of up to ten quenched samples per isotope is made up and measured automatically Note For single labelled samples calibration is carried out once for the single isotope For double labelled samples calibration is carried out automatically twice once for each isotope the low energy isotope being counted first For each quench or efficiency level the counting efficien
164. ymbol and indications of danger for the preparation X irritating 15 1 2 Names of the ingredients given on the warning label 1 2 4 Trimethylbenzene 15 1 3 R phrases 36 37 38 Irritating to eyes respiratory system and skin 20 Harmful by inhalation 15 1 4 S phrases 36 Wear suitable protective clothing 15 1 5 Special regulations on certain preparations 15 2 National regulations 16 OTHER INFORMATION 16 1 Purpose of use 16 1 1 Expressed in writing Scintillation liquid for liquid scintillation counting 16 1 2 Code for the purpose of use SICI KTl SIC2 KT2 SIC3 KT3 SIC4 KT4 SIC TOL Standard industrial classification KT Desired effect of the chemical 16 2 Directions for use 16 3 Other information The above information is believed to be correct but does not purport to be all inclusive and shall be used only as a guide Wallac shall not be held liable for any damage resulting from handling or from contact with the above product 16 4 Additional information available from 16 5 Sources of information used in the compilation of the safety data sheet Information given by manufacturer Hazardous Substances Databank The Sigma Aldrich MSDS on CD ROM Reasons for the confidentiality of the information 200

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