PART II LABORATORY 12 GAMMA RAY SPECTROSCOPY 12.1 MOTIVATION This practical is primarily about detector characterisation. An ideal detector will give you just the signal you want and nothing else, but in the real world detectors have finite resolution and pick up all sorts of other signals including noise. The purpose of this lab is to give you experience in characterising a detector, and in sifting out which features are due to the signal, which are due to other interactions in the detector, and which are properties of the detection system. As well as characterising the detector you will also see how characteristic gamma ray spectra can be used to identify the radioactive elements present in an unknown sample. The plan for this experiment is thus as follows. First the detector must be characterised, which involves determining the relationship between incident gamma ray energy and channel number on the multi-channel analyser using a set of known calibration samples (don’t panic - more about the equipment later!). We will notice that there are more features on the collected spectra than can be accounted for from the known gamma ray energies - these are due to secondary detection events which you will have to characterise in order to interpret the spectra. Armed with this information we then go on to analyse the spectra of two unknown sources in order to determine their composition. Remember that the primary concern is showing an understanding of what is going on. Getting the right results is nice, but we are more concerned with developing a mature understanding of the detector interactions and showing an understanding of what is going on with the equipment, and your report should reflect this. 12.2 THE DETECTOR SYSTEM The purpose of this section is to provide an overview of the detection system, plus some information about the way in which gamma rays interact with matter necessary for interpreting the spectra. 12.2.1 OVERVIEW The basic idea of the detection process is relatively simple: in order to measure the gamma ray spectrum it is necessary to convert the gamma rays emitted by the source into a signal which can be used to produce a quantitative graph of the energy spectrum. The conceptual layout of the equipment used to do this is illustrated in Figure 12.1. Gamma rays are incident on a sodium iodide (NaI) scintillator crystal which produces flashes of visible light in response to gamma rays 1. The light output of the scintillator is directly proportional to the energy of the incident gamma ray so that a 1 MeV photon will produce twice the light of a 0.5MeV photon, provided that all of the incident photon energy is deposited in the crystal (more about this later). This flash of light is converted into a pulse of electrons by a photomultiplier tube located immediately behind the scintillator crystal. The photomultiplier tube used in this setup consists of a series of 10 plates (dynodes) in an evacuated glass tube held at approximately 100V between each plate. Photons incident on the front of the photomultiplier release electrons through the photoelectric effect, and these free electrons are accelerated from plate to plate gaining energy from the voltage applied between the plates. Each time an electron hits one of the dynodes it releases a number of electrons, all of which are accelerated to the next dynode by the potential difference between the dynodes, where each of the incident electrons releases a number of further electrons. Thus an electron cascade is formed resulting in a detectable pulse of charge on the final dynode in response to the incident photon2. This charge pulse is converted into a voltage pulse by the preamplifier, which produces a voltage spike proportional to the amount of charge in the input pulse, and 1 The term scintillator comes from scintillation, which refers to the flashes of light produced by the crystal when it is hit by high-energy radiation. 2 This is a fairly sketch description - a more detailed description of the way in which a photomultiplier tube works can be found in the appendix to this chapter. 110 GAMMA RAY SPECTROSCOPY Radioactive source NaI Scintillator Photomultiplier tube (Gamma ray to visible photons) (converts visible photons to charge pulse using the photoelectric effect and an electron cascade) High energy photon (gamma ray) Charge pulse CRO (to directly observe the pulses from the amplifier) Voltage pulse Preamplifier Voltage pulse (charge pulse to voltage pulse) Amplifier (amplifies voltage pulse) Multi-channel analysier card in PC (converts voltage pulses into a spectrum to analyse) Figure 12.1 Schematic layout of the measurement system Gamma rays are incident on a NaI scintillator crystal which produces flashes of light in response to incident gamma rays, with the light output directly proportional to the incident gamma energy. These flashes of visible light are converted into a charge pulse by a photomultiplier tube, with this charge pulse being converted into a voltage pulse suitable for input into the multi-channel analyser card in a desktop PC by a preamplifier and amplifier pair. the voltage pulse from the pre-amp is then further amplified by a voltage amplifier into a signal suitable for detection using the multi-channel analyser (MCA) in the PC. The MCA card looks at the magnitude of each pulse arriving at the input and increments an internal counter according the voltage of the incoming pulse. The MCA we are using has 1024 channels (pigeon holes) ranging from 0 volts to 10V input, with the width of each channel being approximately 10mv. Each time a pulse arrives at the input the MCA determines its magnitude and increments the counter corresponding to that voltage by one, thus the number of counts in any channel represents the number of events detected within the voltage range of that channel - the greater the number of events, the greater the height of that channel on the display. In order to interpret this spectrum, which really displays the useless information about counts in each channel, it is necessary to determine the relationship between channel number and incident gamma ray energy. In other words it is necessary to calibrate the detector, and this is the purpose of the first part of this lab session3, section 12.4. 12.2.2 THE DETECTION OF GAMMA RAYS The incident gamma rays are converted into flashes of light by the sodium iodide (NaI) scintillator crystal, thus it is necessary to understand something about the way in which gamma rays interact with the scintillator in order to interpret the spectrum data. A -ray can interact with matter via a number of atomic processes but by far the most probable are the photoelectric 3 Ideally the relationship between channel number and incident gamma ray energy will be a liner one, with the channel number being directly proportional to incident energy. For this to be the case all of the elements in the detection system shown in Figure 12.1- scintillator, photomultiplier tube and amplifiers must be linear in their response. Fortunately this is pretty well the case for the equipment in use here, but if it were not the case this would show up in the calibration and could be corrected for using a non-linear calibration of energy to channel number. 111 PART II LABORATORY effect, Compton scattering and pair production 4. Each of these processes produce a slightly different energy at the detector for a given incident gamma ray, giving rise to a peaks at different locations on the spectrum. It is therefore necessary to understand these interaction processes in order to interpret the spectra collected. a) Photoelectric effect In the photoelectric effect a -ray of energy E interacts with an atomic electron with binding energy b , with the energy of the -ray being completely absorbed by the electron5 which is then ejected from the atom. To balance momentum, the nucleus also recoils taking with it some of the photon momentum, whilst it’s mass means that it has very little recoil energy. By energy conservation the ejected electron has a kinetic energy of Ee E b Eq. 12.1 which is carried off by the free electron. Another electron then replaces the free electron with the binding energy of b released as an x-ray, which is in turn absorbed by further photoelectric interactions and all of the incident -ray energy is absorbed. If the ejected electron comes from the innermost shell of the atom the x-ray produced is called a K x-ray, so called because it results from a transition into the K-shell of the atom. The energy of this K x-ray is a function of the binding energy of the atom, which in turn is a function of atomic number: the higher the atomic number the higher the energy of the K x-ray. A plot of the relationship between atomic number and K x-ray energy is shown in Figure 12.2. The probability of the photoelectric effect increases with atomic number Z as Z 4 , thus detector efficiency is improved through the use of heavy elements. b) Compton scattering In Compton scattering the -ray undergoes an elastic collision with an electron which is so loosely bound to the atom that it can be considered to be a free electron. Without the much heavier nucleus to carry off the recoil momentum the full energy of the -ray can not be absorbed, thus the -ray is scattered off the electron with reduced energy, the electron taking the balance of the energy with it as kintetic energy. The energy of the recoil electron, referred to as the Compton electron, depends upon the angle of scattering and is given by 1 cos Ee E 1 1 cos Eq. 12.2 where E = energy of the incident -ray, Ee = energy of the recoil electron, = photon scattering angle, = E mo c2 , mo c2 = electron rest mass (511keV). This reaction produces a distribution of electron energies from zero up to some maximum value depending on the scattering angle with the maximum energy of the recoil electron being when the scattering angle is 180 . As with the photoelectric effect the recoil electrons ultimately convert their kinetic energy into optical photons through subsequent atomic interactions. c) Pair production 4 All of these processes produce an energetic electron as a result of the interaction. This energetic electron is rapidly stopped by matter and is converted into a large number of low energy (visible) photons by ionisation and atomic excitation, thereby producing the flashes of light detected by the photomultiplier tube with the intensity of the light directly proportional to the energy of the electron produced by interaction of the -ray with the crystal. 5 The nucleus is capable of accepting some of the momentum of the photon, enabling both momentum and energy to balance. 112 GAMMA RAY SPECTROSCOPY Figure 12.2 K x-ray energy as a function of atomic number. If the -ray has sufficient energy pair production may occur when the -ray passes within the field of the nucleus. In pair production the -ray energy is converted into the rest mass and kinetic energy of an electron-positron pair; the positron then annihilates with an electron producing two annihilation photons of energy 511keV (the rest mass of an electron) which can then further interact by either Compton scattering, the photoelectric effect, or can be lost from the detector altogether. By energy conservation, pair production can not occur unless the -ray energy is greater than 1022keV, E 2me c2 . d) Combined effect of all three interaction processes When a -ray source is placed in front of the detector, the detector is bathed in a continuous flux of -rays, each of which can interact with the scintillator by any of the above processes. The relative probability of each of these processes is a function of -ray energy, and the form of this relationship is shown in Figure 12.3. The final spectrum recorded by the detector is simply the probability weighted sum of the above three processes, that is to say the actual spectrum recorded is a combination of all energetically possible events for every -ray the source produces. Note that it is possible for the -ray or x-ray produced in any of these processes to further interact: for example, the recoil gamma ray from Compton scattering may further interact via the photoelectric effect. However, the probability of two interactions is much lower than the probability of a single interaction, thus for the purposes of the analysis here only single processes will be considered. 113 PART II LABORATORY Figure 12.3 Interaction probability for an NaI detector. The relative probability of photoelectric, Compton and pair production interactions as a function of incident Gamma ray energy for an NaI scintillator crystal. 12.3 INTRODUCTORY EXERCISES These calculations are designed to help you interpret the spectra and should be done before you start the first days’ work. Pre-lab Question (a) Calculate the maximum energy imparted to the recoil electron in the case of Compton scattering of a -ray of energy E. What scattering angle does this maximum energy correspond to? Calculate the energy of the electron for the case of a 622keV -ray, and at what energies do the events for other scattering angles appear? Pre-lab Question (b) Now consider what happens when the scattered photon escapes from the detector: what is the maximum energy deposited in the detector when the scattered photon escapes? Draw a diagram of this process, including the scintillator crystal, indicating where all of the reaction products end up. How much energy would be deposited in the detector if the scattered photon were also absorbed within the detector? Pre-lab Question (c) Calculate the energy of the scattered photon for an incident -ray of energy E when the scattering angle is 180 , and then calculate the energy of the scattered photon for an incident 622keV -ray. Once again draw a simple diagram of this and suggest a process by which only the scattered photon could be measured by the detector. Hint: Could the -ray scatter from anything behind the scintillator so that only the scattered photon is measured by the scintillator crystal? Pre-lab Question (d) Show that for high energy -rays, E , the energy of the photons scattered through 180 approaches 255keV, and that this result becomes independent of ray energy as E . Pre-lab Question (e) Consider pair production by a -ray of energy E 1022 keV . How much energy is deposited in the detector if both the electron and positron deposit all of their energy in the scintillator? How much energy is deposited if one of the annihilation photons escapes from the detector, and how much is deposited if both annihilation photons escape? Once again diagrams may help you here. What does this say about the nature of the peaks you expect to see from pair production? Pre-lab Question (f) Consider a mono-energetic -ray source. In the light of your calculations above draw on a calibrated scale the spectrum you would expect to see for a 114 GAMMA RAY SPECTROSCOPY 622keV -ray. Remember that the total spectrum is simply the sum of all possible processes weighted according the probability of that process so it might be useful to draw separate sketches of the contribution of each process first. See Figure 12.3 for the relative probabilities of different events at different energies. Similarly draw separate sketches of the spectrum you would expect to see for a mono-energetic -ray source of 50keV and 2000keV, taking into account the relative probability of detection events in each case. 12.4 DETECTOR CALIBRATION 12.4.1 SETTING UP THE EQUIPMENT First of all look around the bench. Identify all the pieces of equipment, Caesium 137 (137Cs) 32 keV and follow the cables to see what is 662 keV connected to what. Sodium 22 (22Na) 511 keV Then turn on the power supplies to the 1275 keV equipment one by one: this includes Cobalt 60 (60Co) 1173 keV the NIM bin containing the amplifier 1332 keV modules, the HV supply (which should Table 12.1 Energies of the calibration read 100V once turned on), the CRO sources and the PC. Let the equipment stand as is for about 5 minutes to warm up (this enables the electronics to stabilise and helps make sure your readings don’t drift during the experiment), during which time you should find the 137Cs source and place it in front of the scintillator so that it is roughly in line with the detector’s central axis. Whilst doing this also locate the two other calibration sources, 22Na and 60Co, but leave them some distance from the detector so that they don’t contaminate the 132Cs spectrum. Slowly increase the voltage on the EHT supply to 800V (EHT means Extra High Tension and is a 1950s term for High Voltage (HV)) and view the output of the preamplifier on the CRO to make sure that you are getting some signal from the photomultiplier. Then reconnect the preamplifier output to the amplifier input and view the output of the amplifier on the CRO. If you are having trouble finding any pulses at all try adjusting the triggering and Y-scale on the CRO, and if you are unsure about what you are seeing talk to your demonstrator after first thinking about what you’d expect to see. Question (a) Do you notice anything interesting about the pulses? For example, are all the pulses of the same height and shape? We now have to set the gain on the amplifier so that the amplifier output falls within a useful detection range of the MCA card. Recall that the MCA card digitises voltages in the range from 0 volts to 10V into 1024 channels and that we want to be able to measure gamma rays of at least 1800 keV (but no more than 2000 keV) in order to identify the unknown sources. Question (b) Given that the highest energy gamma emitted by 137Cs is 662 keV (see Table 12.2) and assuming that the relationship between incident gamma ray energy and voltage is linear and that 0keV=0V, at what voltage should this peak appear in order to allow detection of 1800 keV gamma rays by the MCA, and in what channel number should the peak corresponding to the 662 keV gamma ray appear? Now adjust the amplifier gain so that the maximum peak height on the CRO trace is at this calculated voltage, which should be around 3.5V. Note your final amplifier settings. The detector output is highly sensitive to variations in EHT voltage supplied to the photomultiplier tube. To investigate this, gradually increase the EHT voltage until the output voltage displayed on the CRO has doubled. Note the change in EHT required to do this and comment on the sensitivity of the output to EHT fluctuations. Question (c) What demands does this place on the stability of the EHT supply, and what will be the effect of small drifts (eg: 5V) in EHT voltage on the output pulses and, hence, on the spectrum measured by the MCA? 115 PART II LABORATORY Figure 12.4 Summary of MCA commands Question (d) What precautions can you take to minimise the effect of EHT drift on your measurements? For bonus points, try to explain why the photomultiplier might be so sensitive to variations in supply voltage (think about the design of your photomultiplier tube, which has 10 dynodes, and about how electron cascade is amplified). Return the EHT voltage to 800V and let it stabilise for at least 10 minutes before collecting any real data, readjusting the supply if necessary. Remember to note the final (stable) voltage at which your actual data is collected. 12.4.2 SETTING UP THE DATA ACQUISITION SOFTWARE Make sure the PC with the MCA card is switched on and start the MCA program by typing ‘mca’ at the command prompt. (yes, this is a DOS based program but it works as well as its modern counterparts. Who needs a graphical interface anyway?) Review the MCA command list (see box) and try the following: Start collecting a test spectrum (Alt-1). You should see a series of dots creeping up on the screen - let this run for about a minute or so. Stop acquisition (Alt-2) and transfer your data from the MCA card into the computer’s buffer memory (Alt-5), then save the data (Alt-F, Alt-S) into a temporary file. You can only save data in the buffer, but can only acquire data from the MCA card, thus you must always transfer the data from the MCA to the buffer (Alt-5) before saving. Many a student has wasted hours by saving the wrong spectrum in the wrong file, so be careful. Move the cursor using the left and right arrow keys. Note that a counter at the bottom of the screen changes as you do this: this indicates which channel number the central line is located over. Note that Page-up and Page-down move the cursor quickly from one place to another. Adjust the vertical scale from logarithmic to linear (Up arrow): at first the spectrum will disappear, but keep going until the spectrum reappears. To return to a logarithmic scale keep hitting the down arrow key. 116 GAMMA RAY SPECTROSCOPY Change to expanded view (F3) and move the cursor around again. Now change the size of the expansion region using Keypad +/- and note that you can get the cursor resolution down to single channel units. Note the counter on the left indicating the detector dead time. It takes the MCA card a few milliseconds to digitise the incoming pulse during which time no further incoming pulses can be measured. The dead time measures the amount of time the MCA is digitising data relative to the amount of time it is waiting for incoming data. We want to measure as many counts as possible, but if the dead time is too high many pulses will be missed and the quality of the spectrum will decrease. A good compromise is to have a dead time of less than 10%, which can be achieved by adjusting the source to detector distance. Check that your dead time is less than 10%, adjust the source if necessary, and record your final dead time value for all spectra. If you are at all unsure about whether your spectrum looks OK check with your demonstrator now. 12.4.3 COLLECTING KNOWN SPECTRA We are now in a position to collect spectra of all the known sources. First check that the EHT supply is still set to 800V and, if necessary, readjust it. Then start the MCA program counting for approximately 10 minutes. There is nothing magical about this figure: the longer the count time the better the spectrum, but more time you have to spend waiting for data collection. 10 minutes is a reasonable compromise between the two, but feel free to chose some other time if you think it is appropriate. Make sure only the 137Cs source is infront of the detector and collect a spectrum for the time you have determined. Save this file, print one copy for each partner by pressing <Print screen>, and record the channel numbers of all features using the MCA program 6. Repeat this procedure for both the 22Na and 60Co sources, remembering to check the dead time and EHT voltage before starting each collection run. 12.4.4 ANALYSIS a) Feature identification Each calibration source gives out only two -rays, but there are many more features than this on each of your spectra. Identify the origin of all features on all of your spectra, noting which ones are in the same position for all spectra and which are in different locations. Remember from your calculations in section 12.3 above that a gamma ray of a single energy incident on the detector can produce peaks at a number of positions. Use the results of these calculations to identify all of the peaks on your three spectra, including uncertainties, and comment on how well the peak location agrees with the result of your calculations (you may need to do the energy calibration before being able to determine whether all the features are at the energy you expect). One of the peaks present in all graphs is hard to identify on the basis of gamma ray-detector interactions alone: it is due to the interaction of a gamma ray with the lead blocks around the detector. b) Energy calibration We are now in a position to determine the relationship between channel number and energy for the detector operating with your particular electronic settings. From Table 12.2 we know the energies of the two gamma rays given off by each source, that is six known gamma rays in total, and from the results in section 12.4.4(a) we know the channel number corresponding to each of these energies. One useful feature of the scintillation detector is that the output voltage is proportional to the energy deposited in the detector, thus we can calibrate the MCA channel numbers in terms of energy by performing a linear fit to the data. Do this calibration now, including the uncertainties in measured channel number, and comment on the shape of the graph. Question (e) Does it appear to be linear? Does it pass through the origin? Does it appear to be what you expect? 6 Remember that you can analyse one data set in the PC memory whilst collecting the next data set in the MCA buffer. 117 PART II LABORATORY Using your calibration data work out the energies of all other features on your graph and compare them to the expected energies of secondary features such as Compton edges, pair production and backscatter peaks. Comment on the extent to which the measured values agree with the calculated values. Question (f) Do these results indicate that you have correctly identified all of the features on the spectrum? 12.5 IDENTIFICATION OF UNKNOWN SOURCES Armed with the calibration graph we are now in a position to use the spectrometer to identify unknown sources. Using the same electronics settings as used in section 12.4.3 (why?) collect spectra of the two unknown sources and, using your calibration data from section 12.4.4(b) above, measure the energy of all features across the full range of the spectrum including uncertainties. Using the table of known gamma ray energies in Table 12.2 identify the unknown sources. Question (g) Which peaks can be dismissed as properties of the system, which are secondary features such as Compton edges and pair production (amongst others), and which can be attributed to the sources? Remember that it’s not so much a correct identification as a good description of your reasoning that we are after here, so think carefully about what you’re doing. Fully justify your reasoning, and don’t forget to refer to the ratio column in Table 12.2 which indicates the proportion of events from a given nucleus which give rise to a gamma ray of that particular energy: the higher the ratio the higher the peak should be. 12.6 ENERGY RESOLUTION The amount of detail that can be observed in the spectra is governed by the resolution of the detector, which essentially measures the width of the peak produced by the equipment for an incident gamma ray of a single energy. The poorer the resolution, the broader the peak will be and the harder it will become to distinguish two gamma rays of closely spaced energy. There are a number of ways to measure resolution depending on how you wish to characterise the breadth of the peaks, but a standard, commonly used measure of resolution is given by Resolution FWHM E Eq. 12.3 where FWHM is the full width at half maximum of an isolated peak and E is the energy of that peak. Thus this measure of resolution expresses resolution as the ratio of the width of the peak to the energy represented by that peak. Return to your calibration spectra, 132Cs, 60Co and 22Na, and measure the full width at half maximum (FWHM) for the two characteristic peaks in each spectrum and, thence, calculate the resolution for this set of six peaks (remembering to include uncertainties). Plot this measure of resolution as a function of gamma ray energy and comment on its shape. Given that the gamma rays in a full energy peak have all lost an identical amount of energy in the scintillator suggest a cause for the finite peak width. (Hint: Think about what is happening in the detector chain and where the most likely causes of variations in peak height might occur. It is unlikely that the amplifiers and MCA card contribute significantly to the peak broadening.) 118 GAMMA RAY SPECTROSCOPY Energy (keV) 32 35 53 53 77 80 81 97 121 122 136 176 186 232 242 245 225 265 270 273 280 284 295 Source 137Ba 125Sb 133Ba Ratio (%) 7.0 4.5 2.2 226Ra 142Ba 131I 133Ba 75Se 75Se 152Eu 75Se 125Sb 226Ra 142Ba 226Ra 152Eu 142Ba 75Se 56Ni 133Ba 75Se 131I 226Ra 54.0 2.4 33.9 3.5 17.3 28.2 59.0 6.8 3.4 57.2 6.7 7.4 100.0 59.1 35.6 7.1 25.2 5.9 16.9 Energy (keV) 303 344 353 356 364 364 381 401 425 428 463 511 570 600 601 607 609 636 637 622 723 750 769 Source 133Ba 152Eu 226Ra 133Ba 142Ba 131I 125Sb 75Se 142Ba 125Sb 125Sb e+ ann 207Bi 142Ba 125Sb 125Sb 226Ra 125Sb 131I 137Cs 131I 56Ni 226Ra Table 12.2 Known gamma ray energies 119 Ratio (%) 18.4 26.3 32.0 62.2 22.2 81.1 1.5 11.6 27.5 29.8 10.4 99.7 9.0 17.8 4.9 41.7 11.4 7.2 85.1 1.8 47.8 5.3 Energy (keV) 779 812 894 898 949 964 1001 1064 1078 1086 1120 1173 1204 1238 1277 1333 1378 1408 1562 1764 1770 1836 Source 152Eu 56Ni 142Ba 88Y 142Ba 152Eu 142Ba 207Bi 142Ba 152Eu 226Ra 60Co 142Ba 226Ra 22Na 60Co 226Ra 152Eu 56Ni 226Ra 207Bi 88Y Ratio (%) 12.8 74.1 61.5 93.2 50.0 14.4 44.0 75.5 52.2 10.0 14.3 99.86 76.6 5.0 99.95 99.98 4.8 20.6 13.1 15.9 7.0 99.4 Gamma ray spectroscopy 1