Gamma Spectroscopy Principles

9.
NUCE604 Revision: Gamma Spectrometry Principles
Gamma Spectrometry Principles

Aim
To introduce course members to the practical application of high-resolution gamma ray spectrometry and to explain the processes of detector calibration and of spectral interpretation.
Objectives
At the end of this session the course members should be able to: 1 Draw a diagram showing the main components of a high-resolution gamma ray spectrometry system.
Explain the concepts of live time, dead time and real-time in a counting system.
Explain the function of pole zero compensation.
Explain what is meant by pulse pile-up.
List five types of interference in gamma ray spectrometry.
Explain the effects of increasing count rates on a spectrum.
List five factors to be considered in selecting a counting geometry.
Explain the steps involved in calculating a sample activity from a gamma ray spectrum.
List the criteria for accepting or rejecting a provisional nuclide identification.
Gamma Spectroscopy Principles
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Gamma Spectrometry Principles

1 Introduction
Whatever type of detector is used for gamma spectrometry the detector output pulse height contains information on the gamma ray spectrum incident on the detector. To maintain the best possible spectral resolution this information must be collected, displayed and analysed with the minimum of noise added to the signal by the processing electronics. This lecture describes typical signal processing units used in high-resolution gamma ray spectrometry in todays radiochemistry laboratory. The first wide energy range high-resolution gamma ray detectors were fabricated from lithium drifted germanium and were known as Ge(Li) detectors. These detectors have now been largely superseded by high purity germanium detectors (HPGe) also known as intrinsic or hyperpure germanium detectors. Regardless of whether a Ge(Li) or HPGe detector is used very similar electronics is used to process the data.
2 Detector Selection
When selecting a detector for a gamma ray spectrometer a philosophy of the bigger the better is not necessarily appropriate. If the detector is required for general-purpose spectrometry then a detector with a good efficiency above 1 MeV or higher is always required. The critical decision is the lowest energy gamma ray that will be required to be detected. If the lower limit is about 60 keV (suitable for Am-241) then the conventional HPGe detector (a p-type coaxial germanium crystal) is probably suitable. If it is required to extend the available energy range too much below 50 keV then a thin detector end cap and a thin detector dead layer (or entrance window) is necessary. This will normally require a reverse electrode n-type coaxial germanium crystal, although some p-type coaxial detectors with special thin entrance windows are available. Both these types of detectors have very thin electrical contacts on the front surface facing the incoming radiation, and so have a very low attenuation of low energy gamma rays before the gamma rays reach the active volume. For specifically low energy gamma ray or x-ray spectrometry a planar detector would be more suitable to cover the range 5 keV to 500 keV, however this region is not being separately covered. A comparison of the efficiency curves for the various types of detector is shown in Figure 1.
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Figure 1
Typical Efficiency Curves for Ge Detectors
The other main consideration is the energy resolution required. For general purpose spectrometry the highest available resolution is not usually required; however, it must be remembered that good resolution implies a good peak-to-Compton ratio, and thus small peaks are easier to locate and measure. A resolution of 1.9 to 2.1 keV at 1332 keV is normally adequate. Another useful parameter relating to the peak shape is the ratio of the peak width at one tenth of the maximum peak height (FWTM) to the peak width at one half of the maximum peak height (FWHM) and similarly the ratio at one fiftieth of the maximum peak height (FWFM) to FWHM. For a purely Gaussian peak shape these ratios would be 1.82 and 2.38 respectively. For many computer based spectrometers, the program fits a Gaussian function to the measured peak to determine the peak position and area, thus a true Gaussian peak shape would produce a good mathematical fit. For typical modern detectors of 30% relative efficiency, values for these parameters should be about 1.95 and 2.8, although for bigger detectors (~100% relative efficiency) the values may be 2.0 and 3.0 and for smaller detectors (10% relative efficiency) about 1.90 and 2.65. For radiochemical measurements the most convenient geometry for the detector and cryostat would probably be a vertical dipstick geometry with the detector placed vertically above the liquid nitrogen Dewar. This allows samples to be placed vertically above the detector at suitably predefined positions on a jig either inside a lead shielded enclosure or with no external shielding. This would allow a wide range of activities to be measured with the same detector.
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Any shield used should allow at least a 10 cm air gap between the shield wall and the detector and source. The usual shield material is 10 or 20 cm of lead, and the characteristic lead X-rays at 75 and 85 keV will be observed in any spectrum. To overcome this the shield must be lined with a lower Z material to prevent the excitation of the X-rays and to absorb any that are generated. The usual liner is a combination of 0.5 mm and 1.5 mm copper; this combination will produce Cu X-rays at 8 keV, which should not be a problem for most gamma spectrometry applications. Detectors have traditionally been cooled by being mounted on a cryostat that is cooled by liquid nitrogen. It is now possible to cool the detector without liquid nitrogen by using a closed cycle helium refrigerator. These are claimed to be reliable in operation and only require a maintenance period of 1 hour every 10,000 hours (less than 1 hour per year). The experience of these devices within Nuclear Electric has not been encouraging so far.
3 Electronics
The basic electronic components of all conventional high-resolution gamma spectrometers are very similar. This section of the report gives details of the electronic building blocks shown in Figure 2 of a typical system. The main signal path is emphasised in the figure. The signal from the detector is amplified and shaped in the preamplifier and main amplifier to give an output pulse whose height is proportional to the energy deposited by each gamma ray in the detector. These pulses are then converted to digital form in an analogue-to-digital converter (ADC) and stored in a multi-channel analyser (MCA). The MCA sums the number of pulses of each height coming from the amplifier to produce a histogram of the number of events against pulse height (or energy); this is the gamma spectrum.
Figure 2
Typical Electronic Configuration for High Resolution Gamma Spectrometer
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4 Preamplifiers
Modern germanium detector systems use a charge sensitive preamplifier, which normally comes as an integral part of the detector assembly. The low noise input stage is usually a field effect transistor (FET) that is sometimes mounted with the detector inside the detector cap to keep it cool. This reduces he electrical noise but is more difficult to repair or replace if it fails.
Figure 3
RC Feedback Preamplifier
This first stage of the preamplifier has an RC feedback (resistor, capacitor) network that provides an output pulse with an amplitude proportional to the integrated charge output from the detector (see Figure 3). The pulse risetime (20 200 ns) is a measure of the charge collection time in the detector and the fall time (~ 1 ms) is controlled by the RC time constant. The second stage is a differentiating circuit which produces output pulses with a rise time of about 10 ns and a fall time of ~50 s. A simple differentiating circuit would produce an output pulse with a long undershoot below the baseline (see Figure 4). To maintain a steady baseline a pole zero compensation network is used with the differentiating circuit to eliminate this undershoot. It consists of a variable resistor across the differentiating capacitor. This circuit is usually factory adjusted and requires no further attention.
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Figure 4
Preamplifier Behaviour RC Coupled
The sawtooth waveform of the input signal means that even at low count rates (~ 1000 cps) most pulses will be sitting on the tail of the previous pulse, causing the mean DC Level to rise slightly. As long as the peak of the second pulse does not exceed the dynamic range of the preamplifier the output pulse is still a true representation of the input gamma energy. At higher count rates some pulses may saturate the preamplifier, see Figure 5, and the output pulse will be distorted. At even higher count rates the mean DC level may exceed the dynamic range and then there will be no output until the count rate drops. This lack of output is the shutdown effect.
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Figure 5
High Count Rate Effects in RC Coupled Preamplifier
The shutdown effect is controlled by the energy rate limitation of the preamplifier, or the product of the gamma ray energy and the input count rate. 5 A typical value for the energy rate capability is 2 x 10 MeV/s. Higher count rates can be accommodated by having a shorter time constant in the RC feedback circuit and thus having a shorter decay time. However, the penalty is an increase in the noise, which results in an increase in the spectral peak width. The energy rate product could be increased tenfold for an increase of ~ 20% in the peak width. This may be acceptable if very high count rates are expected.
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An alternative solution to preamplifier shutdown is to use a transistor reset preamplifier (TRP). In this type of preamplifier the feedback resistor in the first stage is replaced by a transistor (shown as a switch in Figure 3) that discharges (or resets) the feedback capacitor when the DC level starts to approach saturation. As there is no decay of charge via the resistor, the signal on the capacitor builds up in a series of steps and there is no need for a second stage differentiator with pole zero compensation. This type of preamplifier never saturates and so does not shutdown, however there is a small time period associated with each reset pulse during which it is not able to accept any input pulses. This dead time must be taken into account when calculating the input pulse count reset rate. This reset also affects the main amplifier, the negative reset signal drives the amplifier into overload and the amplifier may be out of action for about 3 pulse widths, i.e. for the time it takes to process 3 pulses.
Figure 6
Signal Behaviour with TRP
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A TR preamplifier gives a better resolution as there is no feedback resistor, and for the same reason it has a higher count rate performance. There is one other important consideration; as the output is a step function rather than a tail pulse, there is no need for pole zero cancellation in the main amplifier, simplifying the amplifier set up procedure.
5 Main Amplifier
The main amplifier has to be a signal processor as well as a signal amplifier. The output from a preamplifier either has a long tail pulse (from a RC preamplifier) or a staircase ramp (from a TRP); both of these outputs have floating baselines. The first stage of the amplifier has to clip the signal to produce a pulse with a fast fall time and block the DC signal to bring the baseline rapidly back to the reference potential. As with the RC preamplifier a differentiating circuit with pole zero cancellation is used to return the pulse quickly to the baseline with little or no overshoot. The first stage is usually followed by an integrator to recover the energy information from the signal that is contained in the pulse height. In these first two stages compromises must be made between short time constants (to return the signal rapidly to the baseline), which allow too much noise, and long time constants (to improve resolution by reducing noise), which increases the possibility of pulse pile-up and consequent baseline shifts. A typical optimum time constant for low count rates is 2-6 s, tending to the longer time constants for larger detectors and TR preamplifiers. To ensure good energy resolution and peak position stability at higher count rates (>10,000 cps) the various stages of the amplifier are DC coupled. Thus any DC offsets in the early stages can cause large offsets at the output. A baseline restorer is required to remove these offsets and ensure a steady reference base line at ground potential. This is usually carried out with a gated baseline restorer, which is a CR (capacitor, resistor) differentiating circuit with an open/close switch in the resistive leg to ground. This switch is open whenever a pulse is detected and closed otherwise. Thus the differentiator is only active between pulses and keeps the baseline close to ground potential. This method can keep the 5 baseline steady at input count rates up to 10 cps with 2 s shaping time constants. At high input count rates two gamma rays may arrive at the detector within the resolution time of the amplifier. The two pulses will be piled-up and they will create a summed peak that looks like a single gamma pulse. For detectors with a short charge collection time, i.e. having a short rise time, it is possible to reject these pile-up peaks using a pile-up rejecter (see Figure 7).
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Figure 7
Operation of Pile-Up Rejecter Circuit
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Each time an incoming pulse is detected a fast logic pulse is produced which triggers an inspection interval that covers the amplified pulse. If a second fast logic pulse from a second event occurs during the inspection interval a signal rejection pulse is generated. This signal rejection is used in the ADC to reject analysis of this signal and the dead time of this system is extended to cover this second signal. In order to count at very high count rates (input count rate >50,000 cps) it is usual to reduce the shaping time constant no less than 2 s. However, with large detectors the charge collection time can be long (up to ~500 ns) and variable. This results in a long and variable rise time in the preamplifier pulses and causes lower amplitude main amplifier pulses because not all charge will be collected in the pulse processing time. This effect is known as ballistic deficit. The ballistic deficit causes an increase in the width of spectral peaks and may be significant as the shaping time constants are reduced below 2 s. A gated-integrator amplifier can overcome this ballistic deficit problem. Instead of a RC shaping integrator in the second stage of the amplifier there is a circuit that integrates the total charge from the detector for each pulse from the first stage. When the input pulse signal returns to the base line the integrating circuit is discharged, ready for the next pulse. This process gives a slow rising pulse with a sharp cut-off whose peak is much later in the pulse than in a Gaussian pulse with the same time constant. This enables pulses of variable risetimes to be accurately processed and avoids the problems of ballistic deficit. Figure 8 shows how the gated integrator output pulse produces good results for slow rise time input pulses that would give problems of ballistic deficit with a conventional gaussian amplifier. The gated integrator amplifier can give good results at time constants as short 5 as 0.25 s with input could rates up to 5 x 10 cps. The amplifier must be able to accept the inhibit signal from a TRP during the reset interval to prevent the processing of any pulses in this period and add to the total system busy time. As well as the amplified output signal, there are two output logic signals from the amplifier one to indicate the presence of pulse pile-up and another to indicate the time the amplifier was busy and not able to process other pulses; these signals were indicated on Figure 7.
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Figure 8
Improved Performance Using a Gated Integrator
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6 ADC
An analogue to digital converter (ADC) measures the maximum amplitude if an analogue pulse and converts it to a digital (or channel) value. The digital output is proportional to the pulse amplitude and thus proportional to the energy of the initiating gamma ray. For a series of pulses the digital outputs are stored in a multi-channel array that gives the cumulative number of counts observed in each channel. This is done by adding one to the contents of the channel corresponding to the pulse height measured. The resulting histogram represents the spectrum of input pulse heights. If the input pulses come from an energy spectroscopy amplifier the histogram corresponds to the energy spectrum observed by the detector connected to the amplifier. The histogram storage device can be a dedicated memory, or part of a computer memory. With the addition of a histogram display device the combination of ADC, memory and display is known as a multi-channel analyser. These are two major types of ADC used in high-resolution gamma ray spectroscopy, the Wilkinson type ADC and the successive approximation ADC.
7 Wilkinson ADC
The operation of a Wilkinson ADC is shown in Figure 9. A pulse is detected when the signal level exceeds the pre-set lower level discriminator (LLD). The LLD is usually set just above the noise level of the amplifier to prevent the ADC permanently analysing noise. The LLD triggers the linear gate and peak detection circuit, during this time period a special capacitor, the rundown capacitor, is connected to the input signal. This capacitor is forced to charge up so that its voltage follows the amplitude of the input pulse. When the peak of the signal is detected the linear gate is closed and the rundown capacitor is disconnected from the signal input. At this time, the capacitor has the same voltage as the maximum voltage of the signal pulse. When the linear gate is closed a constant current source is connected to the rundown capacitor to discharge it, at he same time a clock (the conversion clock) is started and the clock pulses are counted until the capacitor voltage reaches zero. The number of clock pulses is proportional to the pulse amplitude and represents the channel number where the event is to be stored during the memory write cycle. During the time the pulse is being processed, the ADC cannot process another pulse and so it produces a so-called busy signal equal to the processing time period. The busy signal indicates that the ADC is dead to any further pulses while it is analysing any single pulse. In order to measure the true detector event rate these dead time losses must be corrected.
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The correction is usually done by counting clock pulses from an oscillator. Only when the ADC is not busy are these clock pulses stored, this time is known as the live time. If this live time is used as the count duration period (rather than the actual count duration or real time) the dead time losses are accounted for. The ADC dead time depends on the conversion clock frequency, (the higher then frequency the faster the rundown capacitor can be discharged), the amplifier pulse height (or storage channel number) and the memory write cycle time.
DT =
N + TM F
DT is the dead time. N is the channel number. F is the conversion clock frequency. TM is the memory write cycle time. For modern ADCs conversion clock frequencies of 50 to 450 MHz are typical and memory write cycle times carry from 0.5 to 2 s. Table 1 gives the conversion times for several clock rates for a differing number of ADC storage channels. As can be seen from the table, for a typical high resolution gamma ray spectrometer with a 100 MHz ADC and 4096 storage channels the conversion time of 43 s for a pulse in the highest channel is longer than other times involved in pulse processing. Typical pulse processing times for an amplifier are about 8 times the shaping time constant or 16 to 32 s for a conventional gaussian amplifier or down to 4 s for a gated integrator amplifier used at high count rates. However the amplifier busy times are not significant and these dead times have to be summed with the ADC dead time to obtain the overall system dead time. Most ADCs have a facility for accepting the amplifier dead time and logically Or-ing this with the ADC dead time.
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Figure 9
Operation of a Wilkinson Type ADC
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8 Successive Approximation or Fixed Conversion Time ADC

The major part of the process in this type of ADC is similar to a Wilkinson ADC. A capacitor is charged up by the incoming signal, but instead of being discharged when it reaches its maximum voltage, it is held at this voltage. A voltage comparator then measures the voltage on the capacitor. The voltage comparator is a successive approximation device. The most significant bit of a digital to analogue converter (DAC) is set, the comparator determines if the DAC voltage is greater than the capacitor voltage, if so the most significant bit is reset to zero, if not the bit is left set. Subsequently the same test is made by setting the next significant bit. This process is repeated until all the bits have been tested. The bit pattern at the end of the process is the channel number to store the input pulse. If the ADC has n bits (i.e. 2 channels) n test cycles are required, which is the same for all pulse amplitudes. This type of ADC has a short conversion time that is independent of pulse amplitude, but the linearity may not be as food as a Wilkinson type. Conversion times of 1.5 s to 10 s are available. Table 2 gives a range of conversion to compare with Table 1. Clock Rate MHz 50 100 450 Conversion Time s including memory Cycle 0.02 x N + 2 0.01 x N + 2 0.0022 x N + 2 Number of Channels, N 1024 22.48 12.24 4.28 4096 83.92 42.96 11.10 8192 165.84 83.92 20.20
n
Table 1 Conversion Times for Wilkinson ADCs Nominal Conversion time s 8 5 1.5 Actual Conversion Time with Memory Cycle s 9.5 + 2 6.5 + 2 2.4 + 2 Number of Channels, N 1024 11.5 8.5 4.4 4096 11.5 8.5 4.4 8192 8.5
Table 2 Conversion Times for Successive Approximation ADCs For a typical 4096-channel gamma spectrometer the 5 s fixed conversion time (FCT) ADC would be faster than a 100 MHz Wilkinson type, but would only be faster than a 450 ADC at the top of the range. To compare the conversion times of the various ADCs see Figure 10.
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For most spectra the majority of the events are of low energy due to the large number of Compton events, which contribute to the low energy continuum, and the efficiency of HPGe detectors being much higher at low energies (~100keV) than at high energies (~1 MeV). To obtain the highest pulse throughout a 1.5 s FCT ADC should be used with a 4096-channel spectrometer.
Figure 10 Comparison of Conversion Times for Wilkinson and Fixed Conversion Time ADC
9 High Voltage Power Supply

All germanium gamma ray selectors require a high voltage bias supply. A variable 0-5 kV supply with a low current capacity (< 1 mA) is sufficient. The detector performance will not vary with small changes in bias voltage so voltage stability and ripple requirements are not stringent. As detectors and preamplifier FETs can be damaged if a detector warms up with the detector bias still applied there should be a remote shutdown feature on the unit that can be driven by the detector bias shutdown signal developed by most integral preamplifiers.
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10 Liquid Nitrogen Level Monitor

This is not essential, but it is a useful accessory. The monitor will inform the user, via an audible alarm that the liquid nitrogen level in the Dewar is low and needs refilling, before the detector warms up. The unit will also turn off the EHT. The nitrogen level is monitored by a thermistor probe in the Dewar, which is connected directly to the monitor. When the Dewar is approximately full the nitrogen level is below the thermistor and it warms up creating the audible alarm.
11 Digital Spectrum Stabiliser

It is often suggested that it is necessary to stabilise spectra to prevent zero intercept and gain variation in the spectrometer, which may degrade a spectrum, collected over a long time. In most simple gamma spectrometry measurements, where the half life of the isotopes are long compared with the counting time, the system count rate will not vary significantly during the count period, and the gas in unlikely to change. This may not be the case in neutron activation analysis measurements where there may be gain shifts due to count rate variation. There may be long term zero and gain drift bit this can be corrected by the system operator manually recalibrating the system as required. For a temperature controlled counting laboratory the energy calibration should be sufficiently stable for periods of days or weeks. Spectrum stabilisers rely on the presence of two peaks in the spectrum, one at a low energy and the other at a high energy, these peaks are then maintained in fixed channel positions by small variations in the system zero offset and gain. These two peaks can be provided in two ways. 1. A source or sources are placed close to the detector to provide suitable peaks (they may in fact be part of the measured spectra itself, an internal energy calibration). 2. Inject pulses of the required height into the preamplifier. Both these solutions have problems, the first method means that the added sources will always be present, increasing the background count rate and so decreasing the minimum detectable activity of all isotopes. The isotopes that have been added will also be difficult to determine if they occur in the sample to be measured. The second solution is only as good as the stability of the pulsar, and difficulties with pole zero cancellation of the pulsar tails may lead to some broadening of all peaks. In the special case of continuous monitoring of an industrial process where known isotopes are being measured, (such as the on-line coolant monitor on AGR) there may be some advantage in using a digital spectrum stabiliser.
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12 Setting Up a Gamma Spectrometer

In summary, the setting up procedure consists of adjusting the main amplifier gain to give a maximum pulse height suitable for the full range of the ADC. The pole-zero of the amplifier is adjusted to minimise the spectral peaks widths, and the baseline restorer optimised for the maximum count rate expected. The ADC is switched to the desired conversion range and adjusted to minimise any DC offset from the amplifier. The controls may then all be slightly readjusted in turn to improve the system performance. It is important that the adjustments are made in a logical sequence; otherwise the full capability of the system may not be achieved. A detail description is given in the rest of this section. This section will describe how to set up a typical high-resolution gamma spectrometer to cover an energy range 0-2.4 MeV with a 4096 channel ADC and multi-channel analyser. This is a common arrangement, and minor changes to the procedure can be made to cover energy ranges.
13 Connecting the Electronic Units

The electronic units should be placed into a single electronics rack and powered from a single clean mains power supply. The units should be interconnected as shown in Figure 2 or as indicated in the manufactures instruction manual. All signal cables should be of the same impedance to minimise signal reflection, preferably they should be: 93 cable (RG-62A/U) as this is a common output impedance from preamplifiers. The system should be dc-coupled from the preamplifier to the MCA. If any modules have options, select dc-coupling rather than ac-coupling. Apply power to the electronics to allow them to temperature stabilise, but do not apply bias to the detector. The detector Dewar should be filled with liquid nitrogen and left for at least six hours to allow the detector to cool.
14 Applying Detector Bias

The first time a new detector is used care should be taken to check it is performing correctly. Connect the unipolar output from the main amplifier to an oscilloscope and adjust the gain to display the system noise. Any 50 Hz sine wave indicates a ground loop or other mains pick-up, the source should be tracked down and eliminated.
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Apply about 100 V of bias of the correct polarity as indicated by the detector manufacturer, (usually indicated on the detector end cap). The noise amplitude on the oscilloscope should decrease; sometimes the noise disappears completely to several seconds before reappearing. Increase the bias in steps of 100 to 200 V while observing the system noise. Allowing for the amplifier gain the system noise should reduce to less than 1 mV. When the bias voltage has been raised to the value given in the manufacturers data sheet the noise may have marginally increased. Inspect the oscilloscope trace for any further problems due to ground loops, pickup or microphonics and eliminate these as much as possible before processing any further. On subsequent occasions the full bias voltage may be switched on without risk of damage as most detectors have a HV filter with a long time constant.
15 Preamplifier Set-Up
With RC feedback preamplifiers no adjustment is required; the pole-zero compensation is factory set and should not normally be adjusted. Some preamplifiers have two gain settings, the higher gain is usually only used for low energy gamma ray or X-ray application and the low gain setting should be selected for the current set-up. The transistor reset preamplifier has an associated circuit for producing the inhibit pulse to fate (or reject) any signal pulses during the reset period. The length of this inhibit pulse must be adjusted to suit the gain setting on the main amplifier as directed in the manufacturers handbook. The inhibit pulse is of the order of 50 to 200 s wide.
16 Main Amplifier Set-Up

To provide suitable pulses to allow the amplifier to be set up adjust the coarse gain to 50 and the fine gain to 1.0, final adjustments can be made when all the units are set up. Set the shaping time constants for both the unipolar and gated integrator output (if applicable) to 2 s. Set the input polarity switch to the correct polarity, normally positive for p-type detectors with positive bias. If a TRP is used the amplifier pole-zero compensation potentiometer should be adjusted completely out. For a RC feedback preamplifier the pole-zero potentiometer must be correctly adjusted. The operators manual for the amplifier should give the front panel switch positions to give the best pole-zero set up conditions. Place a Co source close to the detector to give a count rate of about 1000 cps, connect the unipolar output of the amplifier to the input of the oscilloscope. Adjust the pole-zero potentiometer to bring the long tail component of the trailing edge of the amplifier pulses to a flat baseline with no long negative or positive tail (Figure 11). Remove the source from the detector.
60
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If there is a dc-level adjustment keep the oscilloscope on the unipolar output and adjust the dc-level to 0 1mV. The base line restorer (BLR) must finally be adjusted. There may be an automatic position and this can be selected, but for optimum performance at higher count rates select the variable BLR setting. There is normally an LED or other indicator associated with the BLR adjustment; alter the BLR potentiometer until the LED is on full, then back off the potentiometer until the LED noticeably dims and flickers. The BLR is now in about the best position. If a counter-timer is available the BLR can be adjusted while monitoring the Busy output with the counter timer. A count rate of about 200 cps gives the correct BLR setting. Some amplifiers have a pile-up rejecter discriminator setting; this can be adjusted in a similar manner to the BLR using the LED method.
17 ADC Set-Up
In order to have channel zero corresponding to 0.0 MeV it is necessary to ensure the dc-level of the ADC input is at zero volts. In some ADCs the input dc-level can be adjusted, in others it is fixed at a nominal zero volts. This section will describe setting up an ADC with a variable dc-level. Set the conversion gain to 4096, remove the signal input cable and insert a shorting plug into the ADC input. Set any coincidence/anti-coincidence switch to coincidence or, off, as all input pulses are to be accepted and sample the input signal (0.0 v) either with the strobe switch or the sample voltage analysis (SVA) switch, dependent on the manufacturer. Set the lower level discriminator (LLD) to its minimum value. Expand the region of display to about the first 100 channels so that the contents of each channel can be easily seen and initialise data acquisition. Adjust the ADC zero level control until data is accumulating in only the first channel. Remove the shorting plug and reconnect the signal input cable. Reinitialise data acquisition and check that data are still being acquired in the first channel. At this stage the signal may have noise associated with it and the data may appear in several channels, but the peak should be in the first channel. If the noise peak is not in the lowest channel adjust the amplifier dc-offset or the zero control of the ADC if necessary. Place an Am and Co source close to the detector to give a count rate of about 1000 cps and return the strobe or SVA switch to its normal position. Adjust the LLD control so that any noise peak in the lowest channel is 241 Am at 60 keV is detected. The LLD eliminated but the peak due to the control should be as low as possible, preferably giving a cut-off at about channel 20 to 40. The upper level discriminator (ULD) can be set to its maximum value. The amplifier gain can now be adjusted so that the Co 1332 keV peak is in 241 Am peak at channel 2220 and the ADC zero level adjusted so that the 59.5 keV is in Channel 100. These steps may have to be repeated several times until both conditions are satisfied. If the amplifier gain is altered significantly then the BLR may have to be reset.
60 241 60
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Figure 11 Pole Zero Compensation
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18 System Resolution Determination

Unless high count rates are to be routinely measured the shaping time constant of the amplifier should be adjusted to give the best resolution. Optimum performance at high count rates and best resolution at lower count rates will usually not occur at identical shaping time constant settings and some trade-off in performance may be necessary to find a suitable compromise for all count rates. Place a Co source on the detector to give a count rate of about 1000 cps and acquire a spectrum with at least 3000 counts in the peak channel of the 122 keV line (at least 10,000 total count in the peak). Analyse the spectrum and 60 record the FWHM for the 122 keV peak. Repeat this process for a Co source and the 1332 keV peak. Determine the FWHM for both peaks for all shaping time constants (or as many as seems appropriate) but check the main amplifier (in particular the pole-zero settings) and ADC settings are satisfactory between each change in time constants. A plot of FWHM as a function of shaping time constant should give a graph with a minimum value for the FWHM in agreement with the manufacturers data or test sheet. The FWHM should increase rapidly at small time constants and increase more slowly at longer time constants. Normally the FWHM minimum value will be at a shaping time constant of 4 to 6 s. The resolution should only deteriorate by about 10% at 2 s and less than 25% at 1 s. For counting at rates of less than 1000 cps the optimum shaping time constant will be satisfactory, but if routine is at rates in excess of this then shorter time constants should be used. For count rates up to 10,000 cps a shaping time of 2 s will probably be adequate, and 1 s would probably be advisable for count 4 rates up to 5 x 10 cps. At this time constant a gated integrator amplifier would 4 probably give equivalent or better results. At input count rates above 5 x 10 cps a gated integrator with a 0.5 s or smaller time constant would probably be the best option. It is probably best to set the time constant to suit the most commonly used count rate and then calibrate other counting geometries at greater source to detector distances to reduce the count rate to the usual value rather than change amplifier settings from count to count.
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19 Pile Up Correction
If more than one gamma ray is detected within the resolution time of the amplifier then the pulses are summed. This summed peak would appear in the spectrum in a higher channel than the two individual gamma rays, this is pulse pile-up. The effect is to produce extra peaks in the spectrum and remove counts from the contributing peaks. These summed pulses should be rejected by a suitably fast pile-up rejection circuit, but there will be some pulses that are sufficiently close in time that they cannot be rejected. The spectrometer should be checked to determine the upper count rate at which the pile-up rejection circuit works adequately.
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Place an Am and a Y source close to the detector to produce a count rate 4 of about 1000 cps. Acquire a spectrum with at least 10 counts in the 59.5 keV, 898 keV and 1836 keV gamma ray peaks. Analyse the spectrum and determine the peak areas and the spectrum live time and real time. Am and Y sources in the same fixed position bring up a Keeping the 137 Cs and record spectra over a wide range of input count rates. source of Analyse the spectra and determine the peak areas and system times.
241 88
241
88
Figure 12 Pulse Pile-Up Correction Calibration
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Plot the ratio of the observed peak count rate to the actual peak count rate as a function of log (real time/live time) for all three peaks (Figure 12). The actual peak count rate is defined as the count rate at the lowest count rate used i.e. 137 without the Cs present. The points should form a straight line for each gamma ray peak with a small value for the slope. The slope should be similar for each peak and the mean slope can be used to correct spectra for high count rate losses from a knowledge of the system live and real time. In some computer based spectrometers a function identical to or similar to this model is built in to automatically correct all spectra. At very high count rates the relationship may become non-linear and the spectrometer should not be used at count rates greater than this limit as the accuracy will be reduced.
20 Count Rate Effects

The time that a detector is running is called the Real Time. The time that the ADC was unable to accept signals as it was processing another pulse is called the Dead Time. The time the system was waiting to accept a signal is called the Live Time. If the same isotope is counted on the same detector then the spectrum observed will vary with the sample activity and the presence of other isotopes. At the lowest sample count rates, the rates normally encountered with environmental samples, the spectrum will be dominated by the detector background count rate. The sample and detector should be in a low background facility, preferably in a laboratory away from any source of high activity. The background spectrum inside a typical low background lead shield is 238 232 U and Th decay. normally a combination of daughter products from 228 212 208 40 These daughters include Ac, Pb and Tl. There will also be K from any 226 Ra that are transported via concrete nearby and probably daughters of 222 Rn released into the atmosphere. The latter component can be gaseous reduced by venting the detector shield with the nitrogen gas boiling off from the Dewar thereby keeping a flow of gas out of the shield. Low count rate spectra will probably have been collected for a long time so there will be a possibility of gain drift; the peaks could be both small and broad, making them difficult to locate and quantify. If only a few known isotopes are to be determined it would be best to look for these isotopes using a library directed peak search program that forces a fit to any peaked feature in the spectrum close to the location of the known isotope peak. At normal count rates there will be little or no environmental background interference, the background for most peaks will be the Compton continuum from higher energy peaks. The peaks should be well defined and simple to detect except for minor constituents in a mixed isotope source. Any peak search program should be able to find all the peaks. To minimise analysis time the nuclide library used to identify the isotopes present should match the sample, i.e. if activation products only are being measured then the library need not contain fission products.
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As count rates increase above about 1000 cps the system dead time increases and good live time correction is required to give accurate quantitative results. At count rates above 5000 cps or so the spectral peaks start to broaden and shift due to baseline variations, the random coincidence summing (pulse pile-up) will start to increase and extra pile-up peaks will occur in the spectrum. There will initially be pile-up between two identical gamma rays of the highest intensity, giving a pile-up peak at twice the energy, subsequently there will be a pile-up between other intense peaks. If activities need to be determined to better than 5% corrections will have to be made for pile-up losses. At higher count rates, say above 20,000 cps, peak broadening and peak shifting can be significant, depending very much on the set up of the individual spectrometer. The longer the shaping time constant, for either a unipolar amplifier or gated integrator, the earlier the effects will occur at increasing count rates. At the highest input count rates of 100,000 cps or more the output count rate will drop, the system throughput being limited by the amplifier time constant and pulse pile-up in the amplifier. At some input count rate a RC feedback preamplifier will lock up completely due to its energy rate saturation and the output count rate will drop to zero. This effect does not happen with a TR preamplifier, the output count rate just becomes smaller. At these highest count rates the pile-up effects are very noticeable, the peaks may become very broad with pile-up between peaks and Compton continuum pulses giving decreased peak to Compton ratios.
21 Interferences in Gamma Ray Spectrometry

The major advantage of the HPGe spectrometer over a NaI spectrometer is the very much-improved resolution (~2 keV at 1332 keV for HPGe and about 60 keV for NaI). At first sight this resolution improvement may suggest that there should not be any problems with differentiating one gamma ray energy from another in a well set up spectrometer. However, as many isotopes emit several gamma rays a multi-isotope source may have gamma rays from one isotope that are not resolved from the gamma rays of other isotopes. There are several ways in which one isotope may suffer interference to one or more of its gamma rays. 1. Background In low count rate environmental samples the largest source of interference is usually the presence of the isotope to be measured in the detector and shield background or in the blank sample. Typical problems here are the presence 60 137 Cs in the background due to contamination and nuclear of Co and 238 234 U and Th and their daughters weapons fallout. Other problems arise if are to be measured. These isotopes are nearly always present as impurities in lead shields. In all cases care must be taken to subtract the correct background component. With large volume high-density samples the shielding effect of the sample may be significant and the background count must be determined with an equivalent blank sample.
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2. Compton continuum At normal count rates the biggest source of interference is probably the presence of other more active isotopes giving a large Compton continuum in the region of the peaks of the isotope of interest. This problem can be improved by counting for a longer time so that the Compton continuum becomes better defined and smoother so that any small peak will be more significant. The only other solution is chemical separation of the isotopes. 3. Escape peaks At any energy E greater than 1 MeV it is possible for an incident gamma ray to interact with the detector to produce two annihilation gamma rays of 511 keV each. If either or both of these gamma rays are not fully absorbed in the detector then extra escape peaks are created in the spectrum. These peaks appear at energies of E-511 keV (the single escape peak) and E-1022 keV (the double escape peak). The escape peaks may be confused with energies of interest. A typical 60 example is the single escape peak of the Co 1173 keV peak at 662.2 being 137 Cs. All spectra with one or more confused with the 661.6 keV peak of isotopes having a high activity with a gamma ray greater than 1 MeV should be checked for escape peaks. The annihilation gamma ray at 511 keV is of course not a reliable indicator of any particular isotope as it is observed in spectra of many isotopes. A bigger problem is that this peak interferes with other gamma rays such as 514 keV 85 85 106 from Sr and Kr and the 511.9 keV peak of Ru. 4. Random Summing A problem at high count rates is random summing of two main lines in a spectrum. This can lead to two problems, creation of additional lines in the spectrum (which will not normally be in the nuclide library) and loss of counts from the peaks concerned, which leads to undervaluation of these isotopes. This type of interference can be reduced by counting at a lower count rate, by either using a smaller mass of sample or counting at a greater distance from the detector. 5. True Coincident Summing With close counting geometries, true coincident summing can be significant, any gamma rays emitted in cascade from an isotope could in principle be detected simultaneously and produce a sum peak. With a reverse electrode HPGe detector which will be sensitive to low energy X-rays, coincident summing peaks can be seen between gamma rays and X-rays for internal transition and electron capture decays. Again there will be extra peaks produced which will not appear in nuclide libraries and consequent loss of counts from the summing peaks. This interference can only be reduced by reducing the solid angle presented by the source to the detector and so making it unlikely that two radiations emitted at the same time from a single atom or nucleus are both detected. This is usually accomplished by moving the source to at least 10 cm from the detector.
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6. Gamma Interference The final form of interference is due to gamma rays of similar energy from different isotopes being misidentified or of identical energy and the peak area not being correctly split between the two isotopes. This type of interference can be best overcome by a matrix inversion technique that takes into account all the peaks in the spectrum and all possible isotope energies. Usually a unique combination of isotopes can be determined. This process is sometimes simplified by calculating the activity of one isotope from only the non-interfered peaks and then back calculating the expected contribution to the interfered peak, the remaining area of the interfered peak may then be associated with another isotope. This type of direct interference is quite common and some well-known examples are listed in Table 3. Energy 59.54 122.06 129.7 136.47 197.15 243.4 249.3 279.5 344.7 402.58 511.01 511.01 563.25 795.85 810.75 832.0 1115.52 1120.49 1293.64 1332.51 Isotope Am-241 Co-57 Kr-77 Co-57 O-19 Xe-125 Kr-90 Se-75 Kr-79 Kr-87 Annihilation Annihilation Cs-134 Cs-134 Co-58 Kr-79 Zn-65 Sc-46 Ar-41 Co-60 Energy 59.32 121.1 129.85 135.9 196.32 242.56 249.79 279.18 345.03 400.70 513.99 511.80 564.24 795.07 810.46 834.83 1115.1 1120.28 1291.56 1332.1 Isotope Ta-182 Se-75 m Kr-85 Se-75 Kr-88 Xe-138 Xe-135 Hg-203 Kr-89 Se-75 Sr-85 Ru-106 Sb-122 Ac-228 Eu-152 Kr-88 Kr-79 Bi-214 Fe-59 Kr-79 Energy 121.82 136.0 196.56 Isotope Kr-90 Kr-79 m Xe-129
344.27 513.99
Eu-152 Kr-85
811.77 834.8
Eu-156 Mn-54
Table 3 Table of some Interfering Isotopes and their Gamma Ray Energies
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Selecting a Counting Geometry 1. Ideally every detector should be efficiency calibrated with a source made of the same material and in the same shape as the samples and counted at the same distance from the detector. Unless the samples are in liquid form this requirement is rarely met. Compromises must then be made and suitable corrections applied for any variation between the sample and the calibration source. The most common radioactivity standards that are readily available are in the form of standardised liquids or gases and reference point sources deposited on Mylar film. With care suitable gas and liquid calibration standards may be prepared from the standardised gases or solution, and spiked soil, and or other granular calibration sources may be generated for volume sources of variable density. A common procedure for efficiency calibration is to prepare sources for the commonly used geometries in the laboratory (e.g. 10 ml vial of liquid or 1000 ml Marinelli beaker) and determine the efficiency function for these frequently used geometries. The point sources are also often used to generate efficiency curves at various distances from the detector (say 10 cm and 30 cm), which can then be used as the basis for determining the activity of less often used counting geometries. 2. Before choosing any particular counting geometry the accuracy required for the analysis must be decided. If it is only necessary to identify the isotopes present, then any geometry would be provided the spectrometers count rate limit was not exceeded. Conversely if an accuracy of much better than 5% is required then there would probably have to be an extensive check on the whole system to ensure that such accuracy was possible. If an accuracy of 5% is adequate then most well set up systems should satisfy this criterion if an identical geometry to the sample has been calibrated. The next thing to consider is the sample count rate; is the sample of such a low activity that it needs to be counted in a low background shield, or is it so active that it must be counted at some distance from the detector? At both ends of the count rate scale the accuracy available will most probably be reduced. At low count rates the accuracy will be limited by the background count rate and at high count rates the pile up correction will be limiting. These two problems can be eased by ensuring that a suitable mass or volume of sample is counted. For a low specific activity source, such as an environmental sample, a large volume could be counted in a Marinelli beaker. Conversely for a high activity source a small aliquot could be counted, assuming the sample is homogeneous and a representative sample can be taken.
3.
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4.
Assuming a suitable counting geometry exists it is best to count the sample at least 10 cm away from the detector to minimise true coincident summing. The exact distance from the detector may be limited by the sample count rate. If a relative accuracy of 1% is 4 required between samples than a minimum peak area of 10 counts is necessary. For a low sample activity this would require a long count time, it may be necessary to sacrifice some accuracy to enable a series of samples to be counted within the available time. The true coincident summing effect may be significant at close geometries, i.e. for a point source or disc source in contact with the detector end cap. For distributed sources such as a Marinelli beaker, or a small source at some distance from the detector the coincident summing can be small and in many cases, ignored.
5.
If a suitable geometry does not exist for the sample being counted then the best procedure is to find an efficiency calibration that approximates to the sample and subsequently make suitable correction to the results. Thus large samples can be counted at a distance and a point source efficiency used, alternatively a liquid volume geometry could be used to simulate an activation sample of graphite for example and suitable self-absorption correction factors applied to the calculated results.
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Calculation of Sample Activity In modern computer based gamma spectrometers most of the calculations necessary to determine a sample activity are carried out automatically and the results printed out for the user. However some final corrections to these results may still be necessary for non-standard sources or counting geometries and for correction for true coincidence summing. The complete analysis process can be briefly summarised: (i) (ii) (iii) (iv) (v) (vi) (vii) (viii) (ix) (x) (xi) Locate all the peaks. Determine the peak areas (counts). Determine the peak positions and calculate their energies. Calculate for count rate for each peak. Correct for random summing (if available). Subtract known background peak count rates (if available). Calculate the gamma ray emission rates using the detector efficiency table or function. Match the peaks found with the nuclide library to identify all possible isotopes present. Correct the emission rates for radioactive decay and gamma ray abundance. Calculate the activity of the provisionally identified isotopes. Check whether the identified isotopes are realistic and reject those that are unlikely.
The gamma spectrometer analysis computer will handle most of the calculation with minimal user intervention with the possible exception of the last stage where some knowledge and experience will be needed. The above steps are now described in more detail. The first step in the analysis after the spectrum has been collected and stored is to locate all the peaks in the spectrum and to determine their areas. This can be a two-stage process but with some programs it is done in a single pass. The peak location process can be complex but basically it consists of smoothing the background continuum and finding significant deviations above the background. This can be done either by looking at the second difference of the spectrum or by convoluting the spectrum with a peak shaped function. Whatever method is used the peak area is normally determined by fitting a combination of a Gaussian shaped peak and a smooth background function. Some programs incorporate extra refinements to account for low and high energy tailing. Once the peak positions and peak areas are determined the peak energies and peak count rates can be calculated using the energy calibration and the system live time. If the system has a method of correcting for random summing (pulse pile-up correction) this can be done now. The correction is applied through a function derived either from the system total count rate or the system dead time. The correction is normally a simple multiplier used on all the peak count rates.
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For low sample count rates a correction is applied to subtract known background peak count rates from the measured peaks in the system. In some systems the background activity may be subtracted from the calculated activity at the end of the analysis. The former method is preferred to retain the system counting statistics. The next stage for all samples is to determine the sample gamma ray emission rate from all the peaks. This is done by dividing the net peak count rate by the detector efficiency at the relevant peak energy. The efficiency may be determined either directly from an algebraic function describing the detector energy-efficiency response, or from interpolation of an energy-efficiency lookup table. The detector efficiency table or function is usually measured using either single gamma ray emitting isotopes with no coincident summing or in a geometry such that coincident summing corrections are small. Any corrections to isotopes for coincident summing must be carried out manually at the end of the analysis. The gamma ray energies and emission rates from the sample are now known; these must be correlated with possible isotopes. This is usually done by comparing the measured gamma ray energies one by one with the gamma rays listed in isotope name in a nuclide library; a nuclide identification program. Any gamma ray in the spectrum matching in energy with a gamma ray in the library within a specified energy difference range is provisionally presumed to have been emitted by that isotope. This is carried out for all the gamma rays in the spectrum. Some gamma rays in the spectrum may not match with the library; they may be due to summing peaks or escape peaks or isotopes that are not in the library. Some gamma rays may match more than one isotope. When the gamma rays have been provisionally identified corrections are made for the gamma ray abundance (emission per decay) and for half-life dependent decay processes. There are two major processes that occur in most samples and the corrections are usually carried out in the computer. The two decay corrections that are calculated are: 1. Decay during the sample counting time. 2. Decay during the period between sample collection and the start of the sample count time. There is a third decay process that has sometimes to be applied and that is for decay during the sample collection time, e.g. for decay to a short-lived isotope that is being collected on a filter over a long collection time. A diagram of these corrections is given in Figure 13.
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Figure 13 Decay Corrections to Sample Activity The calculated activity for every measured gamma ray has now been calculated. Some gamma rays may have been provisionally allocated to more than one isotope as the isotopes may emit gamma rays of similar energy. This interference effect can be resolved in two ways. The most elegant method is to construct a matrix of all the measured gamma rays and all the possible isotopes during the nuclide identification process and then to solve the matrix to allocate the relevant components of the interfering peaks to each isotope. The alternative is to determine the mean activity of each isotope using the noninterfering peaks and from this mean calculate the relevant contribution for the interfered peaks; the remainder may then be allocated to alternative isotopes. The provisional allocation of peaks to isotopes and the consequent activities are then tested to see if they are probable. Two tests are commonly used, the first checks if the cooling time was large compared with the isotope half-life; if the ratio is larger than some preset value the provisional allocation is rejected as unlikely. The second test checks that for those isotopes that emit several gamma rays most of the gamma rays have been identified. This check may just be a numerical check e.g. more than 75% of all lines are present, or the program may use the gamma ray abundance and look for several rays contributing a total of more than a specified fraction of the total number of gamma rays emitted. This test will never reject a single gamma ray emitting isotope but will reject those isotopes identified with only one or a few gamma rays that are provisionally allocated due to coincident or close energy gamma rays.
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Once all the provisional allocations have been confirmed or rejected the program may compute a final activity for each isotope by one of three ways: Either or (1) (2) The activity is determined from one specified gamma ray. The best-fit activity for all isotopes is calculated using the matrix inversion method. The weighted mean is calculated from all the lines identified for each isotope.
or
(3)
At the end of this process some correction may have to be applied manually dependant upon the precision of the required answer and the precise calculational route. If no pulse pile-up corrections were made this correction will have to be calculated and applied to all isotopes. If the efficiency curve is derived from essentially coincidence free isotopes then corrections will have to be applied on an isotope-by-isotope, gamma ray by gamma ray basis to correct for the coincident summing. If the sample was counted at a distance or more than 10 cm from the detector and the accuracy precision is 5% or less this correction will not be necessary. If the sample density and shape does not conform to the calibration source then corrections will have to be made for self-absorption. As described earlier in this section most computer based gamma spectrometers are able to test the provisional allocation of gamma rays to specific isotopes. The tests, if carried out with appropriate criteria, will eliminate most misidentified isotopes. However there are two other tests that are important. The first is for programmes that do not correct or test for gamma ray interference. If one gamma ray could be associated with two or more isotopes check that the peak count rate is not fully accounted for by one isotope. The second and most important check is the experience and skill of the operator; are the samples being counted likely to contain the identified isotopes? In some cases isotopes can simply be ruled out as unlikely to be present in that type of sample. If a sample of steel is being counted for activation products, it is unlikely to contain fission gases, etc.
Reference Material Radiation Detection and Measurement, Knoll, 2 Edition, Wiley. Nuclear and Radiochemistry, Friedlander, 3 Edition, Wiley-Interscience.
rd nd
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Gamma Spectroscopy Principles

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9.

NUCE604 Revision: Gamma Spectrometry Principles

Gamma Spectrometry Principles

Explain the function of pole zero compensation.

Explain what is meant by pulse pile-up.

List five types of interference in gamma ray spectrometry.

Explain the effects of increasing count rates on a spectrum.

List five factors to be considered in selecting a counting geometry.

List the criteria for accepting or rejecting a provisional nuclide identification.