Detectors 1.

Introduction: The detector for an HPLC is the component that emits a response due to the eluting sample compound and subsequently signals a peak on the chromatogram. It is positioned immediately posterior to the stationary phase in order to detect the compounds as they elute from the column. The bandwidth and height of the peaks may usually be adjusted using the coarse and fine tuning controls, and the detection and sensitivity parameters may also be controlled (in most cases). There are many types of detectors that can be used with HPLC. Some of the more common detectors include: Refractive Index (RI), Ultra-Violet (UV), Fluorescent, Radiochemical, Electrochemical, Near-Infra Red (NearIR), Mass Spectroscopy (MS), Nuclear Magnetic Resonance (NMR), and Light Scattering (LS). [1] 1.1 Refractive Index (RI): detectors measure the ability of sample molecules to bend or refract light. This property for each molecule or compound is called its refractive index. For most RI detectors, light proceeds through a bi-modular flow-cell to a photo detector. One channel of the flow-cell directs the mobile phase passing through the column while the other directs only the mobile phase. Detection occurs when the light is bent due to samples eluting from the column, and this is read as a disparity between the two channels. 1.2 Ultra-Violet (UV) detectors measure the ability of a sample to absorb light. This can be accomplished at one or several wavelengths: A) Fixed Wavelength measures at one wavelength, usually 254 nm B) Variable Wavelength measures at one wavelength at a time, but can detect over a wide range of wavelengths C) Diode Array measures a spectrum of wavelengths simultaneously. UV detectors have sensitivity to approximately 10-8 or 10 -9 gm/ml. [2]

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Detectors 1.3 Fluorescent detectors measure the ability of a compound to absorb then re-emit light at given wavelengths. Each compound has a characteristic fluorescence. The excitation source passes through the flow-cell to a photo detector while a monochromator measures the emission wavelengths. Has sensitivity limit of 10-9 to 10-11 gm/ml. 1.4 Radiochemical detection involves the use of radio labeled material, usually tritium (3H) or carbon-14 (14C). It operates by detection of fluorescence associated with betaparticle ionization, and it is most popular in metabolite research. Two detector types: A) Homogeneous- Where addition of scintillation fluid to column effluent causes fluorescence. B) Heterogeneous- Where lithium silicate and fluorescence caused by beta-particle emission interact with the detector cell. Has sensitivity limit up to 10-9 to 10-10 gm/ml. 1.5 Electrochemical detectors measure compounds that undergo oxidation or reduction reactions. Usually accomplished by measuring gain or loss of electrons from migrating samples as they pass between electrodes at a given difference in electrical potential. Has sensitivity of 10-12 to 10-13 gm/ml 1.6 Mass Spectroscopy (MS) Detectors- The sample compound or molecule is ionized, it is passed through a mass analyzer, and the ion current is detected. There are various methods for ionization: A) Electron Impact (EI)- An electron current or beam created under high electric potential is used to ionize the sample migrating off the column. B) Chemical Ionization- A less aggressive method which utilizes ionized gas to remove electrons from the compounds eluting from the column.

Smt. R.B.P.M.P.C. 21

Detectors C) Fast Atom Bombardment (FAB) - Xenon atoms are propelled at high speed in order to ionize the eluents from the column. Has detection limit of 10-8 to 10-10 gm/ml. [3] 1.7 Nuclear Magnetic Resonance (NMR) Detectors- Certain nuclei with oddnumbered masses, including H and 13C, spin about an axis in a random fashion. However, when placed between poles of a strong magnet, the spins are aligned either parallel or anti-parallel to the magnetic field, with the parallel orientation favored since it is slightly lower in energy. The nuclei are then irradiated with electromagnetic radiation which is absorbed and places the parallel nuclei into a higher energy state; consequently, they are now in "resonance" with the radiation. Each H or C will produce different spectra depending on their location and adjacent molecules, or elements in the compound, because all nuclei in molecules are surrounded by electron clouds which change the encompassing magnetic field and thereby alter the absorption frequency. 1.8 Light-Scattering (LS) Detectors- When a source emits a parallel beam of light which strikes particles in solution, some light is reflected, absorbed, transmitted, or scattered. Two forms of LS detection may be used to measure the two latter occurrences: A) Nephelometry- This is defined as the measurement of light scattered by a particulate solution. This method enables the detection of the portion of light scattered at a multitude of angles. The sensitivity depends on the absence of background light or scatters since the detection occurs at a black or null background. B) Turbidimetry- This is defined as the measure of the reduction of light transmitted due to particles in solution. It measures the light scatter as a decrease in the light that is transmitted through the particulate solution. Therefore, it quantifies the residual light transmitted. Sensitivity of this method depends on the sensitivity of the machine employed, which can range from a simple spectrophotometer to a sophisticated discrete analyzer. Thus, the measurement of a decrease in transmitted light from a large signal of transmitted light is limited to the photometric accuracy and limitations of the instrument employed.

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Detectors

1.9 Near-Infrared Detectors Operates by scanning compounds in a spectrum from 700 to 1100 nm. Stretching and bending vibrations of particular chemical bonds in each molecule are detected at certain wavelengths. This is a fast growing method which offers several advantages: speed (sometimes less than 1 second), simplicity of preparation of sample, multiple analyses from single spectrum, and no consumption of the sample. [4]

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Detectors

2. Classification of Detectors: Detectors can be classified into two types, bulk property detectors and solute property detectors. The bulk property detector measures some bulk physical property of the eluent (such as dielectric constant or refractive index) and the solvent property detector, measures some physical or chemical property that is unique to the solute (such as heat of combustion or fluoresce Detectors can also be classified as concentration sensitive devices such as the katharometer or mass sensitive devices such as the flame ionization detector (FID). Another method of classification is to define detectors as specific or non-specific. An example of a specific detector would be the nitrogen phosphorous detector (NPD), which as its name implies detects only those substances that contain nitrogen or phosphorous. A non-specific detector would be the katharometer detector which senses all vapors that have specific heats or thermal conductivities different from those of the carrier gas. In general (though not always), non specific detectors have lower sensitivities than the specific detectors, the reasons for which will be discussed in due course. In this treatment of GC detectors the classification of bulk property detector and solute property detectors will be used. [5], [6]

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Detectors

3. Laser-Based Detectors: Detectors that utilize lasers have been developing and some laser-based detectors are available commercially, but they are not widely used in routine chromatographic practice. Lasers offer several beneficial properties relevant to the chromatographer. In most cases, they offer improved sensitivity and selectivity than other detectors. Improved signal-tonoise ratios (S/N) and deletion of background disturbances are observed. Lasers are capable of better resolution than most liquid chromatographic needs, and they are well suited for pulsed- detection. On the other hand, they are not only costly, but the instrumentation can be complex. High energies of lasers can cause thermal distortions, and sensitivity can decrease due to scattering at the optical sections of the system. Listed below are some of the types of laser-based detectors used: 3.1 Laser-Induced Absorption: In most cases, this system is limited to trace concentrations due to difficulties in comparing the laser source signal from the altered signal. 3.2 Laser-induced photo acoustic (PA): detection has been shown where a 488 nm argon laser source is emitted through an effluent cell. A PA detector measures pressure changes resulting from absorbed radiation. The data is sensed by a piezoelectric transducer (PZT) positioned posterior to a foil-covered slit. The signal is subsequently detected by an amplifier. Compared to a typical UV detector, the PA offers 25 times more sensitivity 3.3 Laser-Induced Fluorescence: Offers increased sensitivity but Rayleigh light scattering at optical sections and in the eluents can present a problem to certain detectors. Detection can proceed through one- or two-photon excited fluorescence (OPEF or TPEF). TPEF results in absorption of a pair of photons that occupy a certain molecular energy level; it is feasible due to availability of high-powered lasers and absence of noise levels often seen in OPEF. There are several detector types:

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Detectors 3.3.1 Flowing Droplet Cell: Four l of eluent is kept between the end of an HPLC column and a solid probe. A laser is emitted perpendicular to this flow channel. The fluorescence is measured using an amplifier. Rayleigh scattering of the radiation source is mostly avoided 3.3.2 Laminar-Flow Cell: Effluent is confined in the cell by one- way, laminar flow. The cell utilizes a submicroliter flow-through cuvette whose windows are 5mm from the stream which minimizes scattering. The laser beam and effluent are perpendicular to the optical component-C 3.3.3 Optical-Fiber Cell: A capillary tube cell is connected to an optical fiber, which conducts light rays to the detector flow. The fluorescence collection optics is placed at a 30 degree angle in relation to the capillary in order to minimize scattering. 3.4 Laser-Based Refractive Index Detector: Differences in RI's are accomplished by using interferometer. A monochromatic laser measures changes in RI for a sample contained in a Fabry-Perot interferometer. A photo amplifier senses the light when the interferometer is scanned. A computer calculates the likely position of maximum interference and converts this data into a signal that represents a change in RI. 3.5 Laser Light Scattering: Considered the most "mature" of the laser-based techniques, this process involves the detection of Rayleigh scattering. This approach utilizes a lowangle laser light scattering (LALLS) photometer and a gel permeation chromatograph (GPC). GPC, otherwise known as size-exclusion chromatography (SEC), separates compounds based on molecular weight. The LALLS focuses a laser beam on the sample placed between two quartz windows separated by a Teflon spacer that reduces background noise: .The scattered light can be measured at scattering angles as little as 2 degrees. In series, the GPC/LALLS can provide on-line molecular weight distributions; consequently, this technique is well-suited for polymer characterization 3.6 Laser-Induced Raman Scattering: Raman scattering is directly proportional to intensity of the source. Visible or UV lasers can therefore be useful in this technique. When the laser wavelength corresponds to the energetic vibrational level in an "excited" Smt. R.B.P.M.P.C. 21

Detectors state, a phenomenon known as resonance Raman scattering (RRS) occurs. Resonance enhancement of the normal Raman scattering (NRS) results in increased intensity of RRS bands, as well as improved efficiency since an increase is observed in the number of scattered photons-to-number of incident photons ratio. 3.7 Laser-Based Optical Activity: By coupling a laser-based micropolarimeter with a HPLC, a system is devised which is both selective and it improves the extinction coefficient of the polarimeter up to 4 orders of magnitude. The important components of this system include the Glan prism, the air-based Faraday rotators, and the cell-window. Also important to note is that many of the mobile phase eluents are not optically active and this, in turn, helps facilitate the detection of optically active samples. [7]

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Detectors

4. Chromatographic detector 4.1 Definition: A chromatography detector is a device that locates in the dimensions of space and time, the positions of the components of a mixture that has been subjected to a chromatographic process and thus permits the senses to appreciate the nature of the separation 4.2 Various Types of chromatographic Detectors: 4.2.1 Gas chromatographic: The development of GC there has been a continuous interaction between improved detector performance and improved column performance. Separations monitored by detectors with improved sensitivity permitted a precise column theory to be developed and experimentally substantiated. This allowed new columns to be designed with reduced dispersion and higher efficiencies. The improved efficiencies, produced small volume peaks, small, that is, compared with the volume of the detector sensor and the dispersion that took place in the conduits of the detector system, the ultimate efficiency obtainable from the column was determined by the geometry of the fluid conduits of the detector and not its sensitivity. This provoked detector redesign, with smaller sensor volumes, different geometry and shorter connecting tubes between the column and sensor. In turn, these modifications allowed much smaller particles to be used in the column resulting in even lower column dispersion and higher efficiencies. In this way, just as in GC, detector design and column design have interacted over the years to a point where the performance of LC columns are now commensurate with those of GC columns. [8] [Link] Detector Specifications Detector specifications are like those for GC detectors and are listed as follows, 1. Dynamic Range

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Detectors 2. Response Index or Linearity 3. Linear Dynamic range 4. Detector Response 5. Detector Noise Level 6. Detector Sensitivity or Minimum Detectable Concentration 7. Total System Dispersion 8. Sensor Dimensions 9. Detector Time Constant 10. Pressure Sensitivity 11. Flow Sensitivity 12. Operating Temperature Range In general, the specifications are the same for both GC and LC detectors with the exception of detector dispersion. Although, detector dispersion has a minimal effect on the resolution in GC separations, detector dispersion can actually destroy a separation achieved in an LC column if the system is not designed correctly. [9] The dynamic range and linear dynamic range are the same. The response index, the measure of detector linearity, can also be determined in exactly the same way, either by the incremental method of calibration, or the logarithmic dilution method. In the logarithmic method of calibration, mobile phase, now a liquid is passed continuously through an enclosed stirred vessel containing a known mass of solute, the eluent passing directly into the detector. The logarithm of the detector output is plotted against the logarithm of the calculated solute concentration and the magnitude of the response index determined from the slope of the curve. The response, noise and sensitivity are measured in exactly the same way as for GC detectors. Pressure sensitivity and pressure tolerance have a more important significance in LC as in multidimensional. LC; the detector may be situated between two or more columns and thus must tolerate pressures up to the input pressure (e.g., several thousand p.s.i). Pressure sensitivity and flow sensitivity are also more important in LC due to the relatively high pressures involved and the sensitivity of many sensors to pressure changes. LC columns have a

Smt. R.B.P.M.P.C. 21

Detectors high impedance to flow and so pressure pulses are often smoothed out in the column and do not reach the detector. Dispersion that takes place in a column is very important and will be dealt with in some detail. [9] 4.3 Katharometer: The first alternative GC detector to be devised was the katharometer introduced by Ray (hot wire detector -HWD). 4.3.1 Principle It consists of two heated filaments, situated in the arms of a Wheatstone bridge, one suspended in the eluent gas from the column and the other in a pure reference stream of gas. In the presence of a solute, both the thermal conductivity and the heat capacity of the gas change changing the heat loss and, thus, the temperature of the filament and, consequently, its resistance The bridge is unbalanced and the out-of-balance signal is passed to a suitable monitoring device. This detector is relatively insensitive but responds to all solutes that differ in heat capacity and thermal conductivity from those of the carrier gas. 4.3.2 Use: This detector was used extensively in the early days of GC for the analysis of hydrocarbon gases. There was much discourse and dissent with regards to the exact mechanism of detection involved in the katharometer and even today it is considered to respond to a number of different physical properties of the eluent gas with no one property playing a major role.[10] 4.4. Flame Thermocouple: The "flame thermocouple detector" is the forerunner to the flame ionization detector FID.

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Detectors

Fig.: 01 flame thermocouple 4.4.1 Principle: Hydrogen or a mixture of hydrogen and nitrogen was used as the carrier gas which after passing through the column was burnt at a small jet. A thermocouple was placed above the jet and was heated by the flame. In the presence of a solute, the heat of combustion of the gas increased, raising the flame temperature and the output from the thermocouple. The electronic circuit consisted of a simple backing off circuit to offset the output from the hydrogen flame alone and an attenuating circuit, the output from which passed to a potentiometer recorder. The detector had a linear response over about three orders of magnitude of concentration and a sensitivity of about 1 x 10-6 g/ml (n-heptane). Its response was proportional to the heat of combustion of the solute. This detector was also made commercially but enjoyed a very short life as it was quickly supplanted by the FID. [11] 4.5 Emissivity: This is an interesting and innovative extension of the flame thermocouple detector.

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Detectors

Figure: 3 Emissivity Detectors A, draught proof Sindanyo top. B, double layer of 40 meshes copper gauze. C, Sindanyo front for photo-cell mounting. D, metal stops for draught top. E, selenium photo-cell. F, glass condensing lens. G, column inlet. H, column. I, column heating jacket. J, supports for reflector. L, metal reflector. M, stainless steel jet. N, 2 cm deep layer of porcelain beads. O, coal gas inlet. P, air inlet. It did not prove particularly popular at the time, but in recent years the concept has been revived and commercial detectors based on the emissivity concept of are now available.
[12]

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Detectors

5. Ionization: The first ionization detector to be developed was the cross-section detector of which, competitive at the time, has limited sensitivity (e.g. 10-6 g/ml, about that of the katharometer or the flame thermocouple detector). An ionization detector functioned on an entirely different principle. The argon type detectors utilize noble gases to produce metastable argon atoms which have sufficient energy to ionize most organic compounds. 5.1 Principle Noble gases have their outer octet of electrons complete and, thus, collisions between argon atoms and electrons are perfectly elastic. If a high potential is set up between two electrodes in argon, and ionization is initiated (for example by a suitable radioactive source) electrons will be accelerated towards the anode and will not be impeded by energy absorbed from collisions with argon atoms. If the potential of the anode is high enough, the electrons will develop sufficient kinetic energy that on collision with an argon atom, energy can be absorbed, and a metastable atom can be produced. A metastable atom carries no charge but adsorbs its energy from collision with a high energy electron by the displacement of an electron into an outer orbit. As a result, the metastable atom, on collision with a molecule of an organic compound, can release energy of about 11.6 electron volts as the electron returns to its original orbit. Energy of 11.6 electron volts is sufficient to ionize most organic molecules. Collision between a metastable argon atom and an organic molecule will result in the outer electron of the metastable atom collapsing back to its original orbit, followed by the expulsion of an electron from the organic molecule. The electrons produced by this process are collected at the anode, generating a large increase in anode current. 5.2 Limitations: There are some complications to this apparently simple sensing system; when an ion is produced by collision between a metastable atom and an organic molecule, the electron,

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Detectors simultaneously produced, is immediately accelerated toward the anode. This results in a further increase in metastable atoms and a consequent increase in the ionization of the organic molecules. The resulting cascade effect, unless controlled, results in an exponential increase in ion current. The control of this cascade production of ions involves a negative feed back control on the ion production. [13] 5.3 -Ray Ionization:

Figure: 2 -Rays Ionization Detector This was the first ionization detector that utilized a radioactive source and the design of the detor. 5.3.1Construction It consisted of a reference cell, through which pure carrier gas passed, and a sensor cell, which carried the column eluent. Each cell contained a 90strontium emitting source that the three stage fission terminating in the stable atom of 90zirconium. [15]

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Detectors

5.3.2 Principle: The ionization currents formed (collected by appropriate electrode potentials) are arranged to oppose one another and consequently any variation in pressure or temperature of the two cells will be balanced out. The differential signal resulting from the presence of a solute in the column eluent sensor cell is amplified and recorded. The sensitivity of the detector was similar to that of the katharometer i.e. about 1 x 10-6 g/ml. The practical lifetime of this detector was also relatively short as it was eclipsed by both the FID and the argon ionization. [16]

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Detectors 6. Argon detector: 6.1 Simple OR Macro Argon:

Figure: 4 Macro Argon Detectors The cylindrical body can be made of stainless steel and the insulator made of PTFE or, for high temperature operation, a suitable ceramic. The very first argon detector sensors used an automobile sparking plug as the electrode, the ceramic seal being a very efficient insulator at very conditions. The decay of 90strontium occurs in two stages, each stage emitting a particle producing the stable atom of 90zirconium.

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Detectors The electrons produced by the radioactive source were accelerated under a potential that ranged from 500 to 2000 volts depending on the dimensions of the sensor and the geometry of the electrodes. As an example, the main body had an I.D. of about 2 cm, a length of about 5 cm and a sparking plug was used as the electrode. This sensor geometry was shown to function well with an electrode potential of about 1200 volts.

Figure: 5 Power Supply Circuit for the Argon Detector The signal is taken across the 1 x 108 ohm resistor and as the standing current from the ionization of the argon (with the type of sensor geometry described above) is about 2 x 10-8 amp. There is a standing voltage of about 2 volts across it that requires 'backing off' The cascade effect is controlled by the linearizing resistance. As the current increases due to the presence of organic vapor, the voltage drop across the linearizing resistance is also increased this reduces the voltage applied across the electrodes. For example, if 1300 volts is applied to the detector and when a solute is eluted, the current increases to 10 -7 amp, this will cause a 300 volt drop across the linearizing resistance of 3 x 109 (10-7x 3 x 109 = 300) and consequently reduce the voltage across the electrodes to 1000 volts. In this way the natural exponential response of the detector can be made sensibly linear. [17], [18]

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Detectors The primary current consists of about 1011 electrons per second. Taking the charge on the electron as 1.6 x 10-19 coulombs this gives a current of 1.6 x 10-8 amp. If each of these electrons can generate 10,000 metastables on the way to the electrode, the steady state concentration of metastables will be about 10 10 per ml (this assumes a life span for the metastables of about 10 - 5 seconds at NTP). From the kinetic theory of gases it can be calculated that the probability of collision between a metastable atom and an o organic molecule will be about 1.6: 1. This would lead to very high ionization efficiency and with sensors of more advanced sensors design; ionization efficiencies of 10% could be achieved. Ionization efficiencies of at least 0.5 % are readily obtainable, which, compared with that of the FID, is very large indeed. The implied higher sensitivity is not always realized in many sensors the sensitivity of the macro argon detector is about 10 times less than the FID (the minimum detectable concentration is an order of magnitude higher). This is because the large primary current carries a high noise level compared with the FID (more than two orders of magnitude greater) and thus the signal to noise (which determines the sensitivity) is ten times less.[19] The argon detector is a very sensitive it was not popular, largely because its linearity did not extend over more than two orders of magnitude of concentration (0.98 < r > 1.02) and its response was not predictable. In addition, the early detectors employed a "hot radioactive source" to provide the ionization (90strontium) which was also unacceptable. Less active sources are now available that work perfectly well with the argon detector and are acceptable from the point of view of safety. In addition, modern solid state electronic linearizing circuits might well give the detector a much wider linear dynamic range. Nearly all organic vapors and most inorganic vapors have ionization potentials of less than 11.6 electron volts and thus are detected. The short list of substances that are not detected include H2, N2, O2, CO2, (CN)2, H2O and fluorocarbons. The compounds methane, ethane, acetonitrile and propionitrile have ionization potentials well above 11.6 electron volts, but, in fact, do provide a slight response. The sensitivity of the macro argon detector is 4 x 10-11 g/ml.

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Detectors 6.1.1 Disadvantage The main technical disadvantage of the argon detector was its large sensor volume which precluded its use with capillary columns. [20] 6.2 Micro Argon: This sensor is designed to have a very small "effective" sensing volume to facilitate its use with capillary columns where the flow rate may be as low as 0.1 ml/min or less. In the micro argon detector sensor, the anode is withdrawn into a small cavity about 2.5 mm in diameter. This ensures that the electrons can only reach the anode along a restricted path and the electric field around the electrode resides within a few diameters of the anode tip. The anode is tubular in form and the capillary column can slide up inside the anode until it is within a millimeter or so of the electric field. Metastable argon atoms are formed as a cloud of around the anode tip and any solute molecules eluted from the column immediately pass through this cloud and are ionized. [21]

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Detectors

Figure: 6 Micro Argon Detectors At the other end of the sensor is another inlet that provides a scavenger flow of argon that rapidly removes the solute from the cell through two holes at the bottom of the anode cavity. This procedure reduces the effective sensor volume to less than a micro liter and thus allows the efficient use of a capillary column. The radioactive source originally used was about 25 micro-curies of radium (a particle source). The radioactive source was very small. It was subsequently recognized that exposure to particles could cause a health problem. Eventually radium was replaced by tritium (a very weak ray emitter) which, although a fairly strong source (sometimes as much as one curie was used), it was relatively harmless from the point of view of radiation energy. It is somewhat unstable at high temperatures causing loss of tritium to the air and consequent atmospheric contamination.

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Detectors

Figure: 7 Separation of a Hydrocarbon Mixture on a Nylon Capillary Column Using the Micro Argon Detector Column: 1000 ft of Nylon tubing 0.020 in I.D. Temperature 23oC. Column efficiency for butane eluted at 65 minutes 0.75 x 106 theoretical plates. In due course the tritium was replaced by Ni63 (another, more energetic ray source) but a fairly safe source that can be operated at relatively high temperatures without fear of contamination. Employing radium as the active source, the micro argon detector was used with long Nylon capillary columns for the separation of hydrocarbon mixtures. The column was 1000 ft long giving 0.75 x 106 theoretical plates. It is seen that the sensor volume has no effect on the column performance and the detector is now very suitable for use with capillary columns. The modifications carried out to reduce the effective sensor volume did not improve its linearity nor increase its linear range. However, the noise level was reduced by about two orders of magnitude and thus the sensitivity was commensurably increased by the same amount making it 10 times more sensitive than the FID. [23] 6.3 Thermal Argon: The argon detector could be made to function without a radioactive source or other electron producing device providing the argon and sensor system was operated at

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Detectors temperatures above 150oC. Glass becomes conducting at temperatures of 150oC and above, and so glass could be employed as one of the electrodes.

Figure: 8 Thermal Argon Detector Sensors The column eluent (argon) passes through a stainless steel tube, which acts as the anode, into a cylindrical glass tube held at 150oC or above. The tube is insulated from the glass tube by a PTFE sleeve. The argon exits from the sensor by a length of PTFE tube. A metal band round the glass acts as an electrical connection to the amplifier, the other input of the amplifier being connected to the ve side of the power supply. The +ve side of the power supply is connected to the metal tubular anode. Electrons, thermally emitted from the glass surface, are accelerated under the high potential and on collision with argon atoms produce metastable atoms in the usual manner which collect round the anode. Organic vapors are sensed in the same way as the normal argon detector, i.e., by collision between the organic molecules and the metastable argon atoms. The electrons and organic ions produced are collected and the resulting current is monitored by a high impedance amplifier. The performance of the detector using potentials ranging from about600Vto 1500 V and sensor temperatures of 150oC, 200oC and 250oC were reported. The authors claimed sensitivities at least as good as those of the FID and a linear range of three orders of magnitude or more (0.98 < r < 1.02). Employing the propensity for glass

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Detectors to conduct at elevated temperatures they also designed a sensor completely free of metal and demonstrated it worked effectively.

Figure: 9 Sensor of the MetalFree Argon Detector It is seen that a very inert type of sensor can be constructed having no radioactive source or other separate electron generator and yet provide a high sensitivity to all compounds that have ionization potentials of less than 11.5 electron volts. The system was found to work equally effectively using helium as the carrier and sensor gases, showing that metastable helium atoms could also be produced in the same manner.[24]

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Detectors

Figure: 10 Separation of a Mixture of Hydrocarbons Monitored by the Thermal Argon Detector and the FID

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Detectors

7. UV Detectors: Although over the years a large number of LC detectors have been developed and described, the vast majority of all contemporary LC analyses are carried out using one of four detectors, the UV detector in one of its forms, the electrical conductivity detector, the fluorescence detector and the refractive index detector. In addition, some form of the UV detector probably accounts for 80% of those analyses. 7.1 UV Absorption Detectors: UV absorption detectors respond to those substances that absorb light in the range 180 to 350 nm. Many substances absorb light in this wavelength range, including those substances having one or more double bonds and substances having unshared (unbounded) electrons, e.g. all olefins, all aromatics and compounds, for example, containing > C = O , > C = S , N = N groups. UV light is arranged to pass through the cell and fall on a photoelectric cell (or array). The output from the photocell passes to a modifying amplifier and then to a recorder or data acquisition system. [25] The relationship between the intensity of UV light transmitted through a cell (IT) and Beers Law gives the concentration of solute contained by it (c). Or ln (IT) = ln (Io) - kcl Where (Io) = Intensity of the light entering the cell, (l) = path length of the cell, K = molar extinction coefficient of the solute for the specific wavelength of the UV light. Differentiating,

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Detectors

The sensitivity of the detector, as measured by the transmitted light, will be directly proportional to the extinction coefficient (k) and the path length of the cell (l). To increase the sensitivity of the system, (l) must be extended but there is a limit to which (l) can be increased as the cell volume and, in particular, the length of the cell must be restricted. This is necessary to minimize peak dispersion in the sensor and to avoid more than a small fraction of a peak existing in the cell at any one time this problem has already been discussed. [26] To restrict peak dispersion, the radius of the cell must also be reduced as (l) is increased. Thus, less light will fall on the photocell, the signaltonoise ratio will be reduced and u to restrict peak dispersion, the radius of the cell must also be reduced as (l) is increased. Thus, less light will fall on the photocell, the signaltonoise ratio will be reduced and s the detector sensitivity or minimum detectable concentration denigrated. Thus, increasing the detector sensitivity by increasing the path length has limitations and a welldesigned cell involves a careful compromise between cell radius and length to provide the maximum sensitivity. Most modern UV detector sensors have path lengths that range between 1 and 10 mm and internal radii that range from about 0.5 to 2 mm

Now, Where (A) is termed the absorbance Now ( is sometimes employed to define the detector sensitivity where the value of A) (A) is the change in absorbance that provides a signal-to-noise ratio of two. A = k' l c

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Detectors Where c is the detector concentration sensitivity or minimum detectable concentration.

7.2 Fixed Wavelength UV Detector: The fixed wavelength UV detector uses light of a single wavelength (or nearly so) which is produced by a specific type of discharge lamp. The most popular lamp is the lowpressure mercury vapor lamp, which generates most of its light at a wavelength of 254 nm. Other lamps that could be used are the low-pressure cadmium lamp, which generates the majority of its light at 225 nm, and the low-pressure zinc lamp that emits largely at 214 nm. None of the lamps are strictly monochromatic and light of other wavelengths is always present but usually at a significantly lower intensity. The emission spectra of the mercury, cadmium and zinc lamps are shown in figure 24. It is seen that to obtain monochromatic light an appropriate filter would be needed. The low pressure mercury light source (wavelength 253.7 nm) provides the closest to true monochromatic light of all three lamps. However, there is light present of significant intensity below 200 nm, but light of such wavelengths is generally absorbed by the mobile phase. [28] Light from the UV source is collimated by a suitable lens and passed through both the sample cell and the reference cell and then on to two photocells. The cells are cylindrical with quartz windows at either end. The reference cell compensates for any absorption that mobile phase might have at the sensing wavelength. The outputs from the two photocells are passed to a signal-modifying amplifier so that output is linearly related to the concentration of solute being detected.

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Detectors

Figure: 11 the Fixed Wavelength UV Detector

Modern sensor cells have angular conduits that form a 'Z' shape to reduce dispersion. The UV sensor can be sensitive to both flow rate and pressure changes but this instability can be greatly reduced if the sensor is well thermo stated. The fixed wavelength UV detector is one of the most commonly used LC detectors; it is sensitive, linear and relatively inexpensive. Sensitivity (minimum detectable concentration) can be expected to be about 5 x 108 g/ml with a linear dynamic range of about three orders of magnitude for 0.98 < r < 1.02. [29], [30]

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Detectors

8. Refractive Index Detector: Despite its limited sensitivity, this detector can be very useful for detecting those compounds that are nonionic, do not adsorb in the UV, and do not fluoresce. 8.1 Angle of Deviation Method: When a monochromatic ray of light passes from one isotropic medium (A), to another, (B), it changes its wave velocity and direction. The change in direction is called the refraction and the relationship between the angle of incidence and the angle of refraction is given by Snell's law, namely,

Where (i) is the angle of incident light in medium (A), (r) Is the angle of refractive light in medium (B), (nA) is the refractive index of medium (A), (nB) is the refractive index of medium (B), And (n'B) is the refractive index of medium (B) relative to that of medium (A). [31] 8.2 Principle: Refractive index is a dimensionless constant that normally decreases with increasing temperature. The reported values are usually taken at 20o or 25oC and are mean values measured for the two sodium lines. If the mobile phase is allowed to flow through a hollow prism and a ray of light passes through the prism it will be diverged from its original path and can be focused onto a photocell. If the refractive index of the mobile phase changes, due to the presence of a solute, the angle of deviation of the transmitted light will also alter and the amount of light falling on the photocell will change. A

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Detectors number of manufacturers have employed the angle of deviation method in refractive index detector design. The differential refractometer monitors the deflection of a light beam caused by the difference in refractive index between the contents of the sample cell and those of the reference cell. A light beam from an incandescent lamp is confined to the region of the cell by an optical mask. A lens collimates the light beam through both the sample and reference cells to a plane mirror. The mirror reflects the beam back through the sample and reference cells to a lens which focuses it onto a photocell.

Figure: 12 Refractive Index Detectors It is the location of the beam, rather than its intensity, that changes with the refractive index difference between the contents of the two cells. As the position of focus of the beam on the photoelectric cell changes, the electrical output changes which are electronically modified to provide a signal proportional to the concentration of solute in the cell. [32]

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Detectors

Figure: 13Chromatogram from a RI Detector 8.3 Christiansen Effect Detector: 8.3.1 Principle: This procedure for measuring refractive index arose from the work on crystal filters. Consider a cell packed with particulate material having the same refractive index as the mobile phase passing through. If a beam of light passes through the cell there will be little of no refraction or scattering, if the refractive index of the mobile phase changes, there will now be a refractive index difference between the mobile phase and that of the packing. As a consequence some light will be refracted away from the incident beam and the intensity of the transmitted light will be attenuated. If the transmitted light is focused onto an appropriate photocell, then any change in refractive index caused by the elution of a solute will produce scattering and a consequent change in electrical output The optical dispersions of the media are likely to differ, and consequently the refractive index will only match at one particular wavelength. As a result the fully transmitted light will be largely monochromatic. Light of different wavelengths will be proportionally dispersed depending on the wavelength at which the two media have the same optical dispersion. Thus, a change in mobile phase refractive will change both the intensity of the transmitted light and its wavelength.

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Detectors

Figure: 14 Christiansen Effect Detector In the optical unit there is a pre focused lamp having an adjustable voltage supply to allow low energy operation when the maximum sensitivity is not required. The condensing lens, aperture, achromatic and beam splitting prisms are mounted in a single tube which permitted easy optical alignment prevented contamination from dust. The device contains two identical and interchangeable cells. 8.3.2 Disadvantage: The cells must be changed each time a different mobile phase is chosen in order to match the refractive index of the packing to that of the new mobile phase. The refractive indices of the cell packing can be closely matched to that of the mobile phase by using appropriate solvent mixtures. In most cases solvent mixing can be achieved without affecting the chromatographic resolution significantly (e.g. by replacing a small amount of n-heptanes in a mixture with either n-hexane or n-octane depending on whether the refractive index needs to be increased or decreased. However a considerable knowledge of the effect of different solvents on solute retention is necessary to accomplish this procedure successfully. As a result of limitations inherent in his type of detector combined with the general disadvantages of the RI detector has not made the Christiansen Effect Detector very popular. [33]

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Detectors 8.4 The Interferometer Detector 8.4.1 Principle: The response of the detector depends on the change in the effective path length of a beam of light passing through a cell when the refractive index of its contents changes due to the presence of an eluted solute. Light that has passed through the cell is focused on a photocell. Coincidentally a reference beam of light from the same source is focused on the photocell, interference fringes are produced. The fringes change as the path length of one light beam changes with reference to the other, thus, as the concentration of solute increases in the sensor cell during an elution of a peak, a series of electrical pulses will be generated as each fringe passes the photocell. The optical path length (d) of light through the cell depends on the change in refractive index (n), and the path length (l), thus, d = n l In addition, the number of fringes (N) which move past a given point on the photo cell (or the number of cyclic changes of the central portion of the fringe pattern) is given by,

Where n is the wavelength of the light employed. The larger the value of (N) for a given (n), the more sensitive the detector will be. It follows that; (l) should be made as large as possible. This procedure for increasing the sensitivity is limited by the dead volume of the column and the dispersion that can be tolerated before chromatographic resolution is impaired. [34]

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Detectors

Figure: 15 Original Optical Systems Used in the Interferometer Detector Light from an appropriate source strikes a half silvered mirror and is divided into two paths. Part of the beam is reflected by a plane mirror back along the same path and onto a photocell. The other part of the beam passes through the sensor cell to a plane mirror, where it is reflected back again through the sensor cell to the half silvered mirror that reflects it onto the photocell. Interference takes place with the other half of the light beam on the surface of the photocell.

Figure: 16 Chromatogram from the Interferometer Detector Each peak represents the passage of a fringe across the surface of the photocell. The four interference peaks represents a single chromatographic peak. The number of fringes will be directly proportional to the total change in refractive index, which, in turn, will be Smt. R.B.P.M.P.C. 21

Detectors proportional to the total amount of solute present. In this form the detector has limited use, but has been developed into a commercially viable instrument called the Optilab. Light from the source is linearly polarized at -45o to the horizontal plane. Horizontal and vertical polarized light beams are produced and after passing through the Wollaston prism, one beam passes through the sample cell and the other beam through the reference cell. The sample cell beam is horizontally polarized and the reference cell beam is vertically polarized. After passing through the cells, the beams are focused onto a second Wollaston prism and then through a quarter-wave plate which has its fast axis set -45o to the horizontal plane. A beam that is linearly polarized in the fast axis plane after passing through the plate will lead another linearly polarized but orthogonal beam by a quarter of a wavelength. The phase difference results in a circularly polarized beam. [35]

Figure 17 Optilab Interference Refractometer Detectors Each of the beams focused on the Wollaston prism consists of two such perpendicular beams which, after the quarter wave plate, result in two circularly polarized beams of opposite rotation. These beams will interfere with each other to yield the original linearly polarized beam. A second polarizer is placed at an angle (90) to the first, allowing

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Detectors about 35% of the signal to reach the photocell. A filter transmitting light at 546 nm precedes the photocell. If the sample cell contains a higher concentration of solute than the reference cell the refractive index will be higher and the interfering beams will be out of phase. The refractive index difference (n) and the phase difference (p) are related by

Where (L) is the length of the cell, And (l) is the wavelength of the light The circularly polarized beams will, therefore, interfere to yield a linearly polarized beam

which is rotated will be given by

radians, and the amplitude of the light striking the photocell (Ap)

An extremely high sensitivity is claimed for this system but it is difficult to interpret the data in terms of minimum detectable concentration The smallest cell is reported to give a sensitivity of about 2 x 10-7 RI units at a signal-to-noise ratio of two. For benzene (RI = 1.501) sensed as a solute in n-heptanes (RI=1.388) this sensitivity would represent a minimum detectable concentration of 5.6 x 10-5 g/ml. The alternative cell would decrease the minimum detectable concentration to about 1 x 10-6 g/ml, similar to that obtained for other refractive index detectors. A number of LC detectors have been developed that are either based on refractive index measurement or function on some physical property of the mobile phase system that is related to the refractive index. Although most are not commercially available, they

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Detectors demonstrate the range of sensing techniques that have been investigated as possible methods of detection. [36]

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Detectors

9. Radio detector: 9.1 Amplitude modulation detectors: 9.1.1 Envelope detector: One major technique is known as envelope detection. The simplest form of envelope detector is the diode detector that consists of a diode connected between the input and output of the circuit, with a resistor and capacitor in parallel from the output of the circuit to the ground. If the resistor and capacitor are correctly chosen, the output of this circuit will approximate a voltage-shifted version of the original signal. [37] 9.1.2 Product detector: A product detector is a type of demodulator used for AM and SSB signals. Rather than converting the envelope of the signal into the decoded waveform like an envelope detector, the product detector takes the product of the modulated signal and a local oscillator, hence the name. This can be accomplished by heterodyning. The received signal is mixed, in some type of nonlinear device, with a signal from the local oscillator, to produce an intermediate frequency, referred to as the beat frequency, from which the modulating signal is detected and recovered. [38] 9.2 Frequency and phase modulation detectors: AM detectors cannot demodulate FM and PM signals because both have constant amplitude. However an AM radio may detect the sound of an FM broadcast by the phenomenon of slope detection which occurs when the radio is tuned slightly above or below the nominal broadcast frequency. Frequency variation on one sloping side of the radio tuning curve gives the amplified signal a corresponding local amplitude variation, to which the AM detector is sensitive. Slope detection gives inferior distortion and noise rejection compared to the following dedicated FM detectors that are normally used.

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Detectors 9.2.1 Phase detector A phase detector is a nonlinear device whose output represents the phase difference between the two oscillating input signals. It has two inputs and one output: a reference signal is applied to one input and the phase or frequency modulated signal is applied to the other. The output is a signal that is proportional to the phase difference between the two [Link] phase demodulation the information is contained in the amount and rate of phase shift in the carrier wave. [39] 9.3 The Foster-Seeley discriminator: The Foster-Seeley discriminator is a widely used FM detector. The detector consists of a special center-tapped transformer feeding two diodes in a full wave DC rectifier circuit. When the input transformer is tuned to the signal frequency, the output of the discriminator is zero. When there is no deviation of the carrier, both halves of the center tapped transformer are balanced. As the FM signal swings in frequency above and below the carrier frequency, the balance between the two halves of the center-tapped secondary are destroyed and there is an output voltage proportional to the frequency deviation. [40] 9.4 Ratio detector The ratio detector is a variant of the Foster-Seeley discriminator, but one diode conducts in an opposite direction. The output in this case is taken between the sum of the diode voltages and the center tap. The output across the diodes is connected to a large value capacitor, which eliminates AM noise in the ratio detector output. While distinct from the Foster-Seeley discriminator, the ratio detector will similarly not respond to AM signals, however the output is only 50% of the output of a discriminator for the same input signal.
[40]

9.5 Quadrature detector In quadrature detectors, the received FM signal is split into two signals. One of the two signals is then passed through a high-reactance capacitor, which shifts the phase of that

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Detectors signal by 90 degrees. This phase-shifted signal is then applied to an LC circuit, which is resonant at the FM signal's unmodulated, "center," or "carrier" frequency. If the received FM signal's frequency equals the center frequency, then the two signals will have a 90degree phase difference and they are said to be in "phase quadrature" hence the name of this method.[41] The two signals are then multiplied together in an analog or digital device, which serves as a phase detector; that is, a device whose output is proportional to the phase difference between two signals. In the case of an unmodulated FM signal, the phase detector's output is after the output has been filtered; that is, averaged over time constant; namely, zero. f the received FM signal has been modulated, then its frequency will vary from the center frequency. In this case, the resonant LC circuit will further shift the phase of the signal from the capacitor, so that the signal's total phase shift will be the sum of the 90 degrees that's imposed by the capacitor and the positive or negative phase change that's imposed by the LC circuit. Now the output from the phase detector will differ from zero, and in this way, one recovers the original signal that was used to modulate the FM carrier. [42] This detection process can also be accomplished by combining, in an exclusive-OR (XOR) logic gate, the original FM signal and a square wave whose frequency equals the FM signal's center frequency. The XOR gate produces an output pulse whose duration equals the difference between the times at which the square wave and the received FM signal pass through zero volts. As the FM signal's frequency varies from its unmodulated center frequency (which is also the frequency of the square wave), the output pulses from the XOR gate become longer or shorter. (In essence, this quadrature detector converts an FM signal into a pulse-width modulated (PWM) signal.) When these pulses are filtered, the filter's output rises as the pulses grow longer and its output falls as the pulses grow shorter. In this way, one recovers the original signal that was used to modulate the FM carrier. 9.6 Other FM detectors Specialized, or obsolescent types of detectors includes

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Detectors

Travis or double tuned circuit discriminator using two non-interacting tuned circuits above and below the nominal center frequency Weiss discriminator which uses a single LC tuned circuit or crystal Pulse count discriminator which converts the frequency to a train of constant amplitude pulses, producing a voltage directly proportional to the frequency. [43]

9.7 Phase-locked loop detector: The phase-locked loop detector requires no frequency-selective LC network to accomplish demodulation. In this system, a voltage controlled oscillator (VCO) is phase locked by a feedback loop, which forces the VCO to follow the frequency variations of the incoming FM signal. The low-frequency error voltage that forces the VCO's frequency to track the frequency of the modulated FM signal is the demodulated audio output. In experimental and applied particle physics and nuclear engineering, a particle detector, also known as a radiation detector, is a device used to detect, track, and/or identify highenergy particles, such as those produced by nuclear decay, cosmic radiation, or reactions in a particle accelerator. Modern detectors are also used as calorimeters to measure the energy of the detected radiation. They may also be used to measure other attributes such as momentum, spin, charge etc. of the particles. [44]

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Detectors 10. Infrared detector: Infrared radiation consists of electromagnetic waves in the wavelength region from 0.75 m to 1000 m; lying between visible light and microwave light. In order to cover this broad spectrum of wavelengths, a variety of infrared detectors have been developed and produced. This manual describes major characteristics and applications of infrared detectors, including InGaAs PIN photodiodes, PBS and PbSe photoconductive detectors, 10.1 Infrared radiation Characteristics: (1) Invisible to human eyes, this is useful for security applications, but sometimes makes measurements and optical system design difficult. (2) Small energy Infrared radiation energy is equal to the vibration or rotational energy of a molecule, this phenomenon makes it possible to identify molecules. (4) Emitted from all kinds of objects. All objects with an absolute temperature of over 0 K emit infrared radiation. Infrared radiant energy is determined by the temperature and surface condition of an object. Suppose there is an object that absorbs all radiant energy and appears completely black at wavelengths. This object is called "blackbody. The following formula and laws can be established with regard to blackbodies. M = C1-5 [exp (C2/T) -1]-1 T: Absolute temperature C1: 1st radiation constant C2: 2nd radiation constant 10.2 Infrared detection: Infrared radiation is used in a wide variety of applications, and new applications are constantly being developed. A typical system for detecting infrared radiation is usually configured as shown below.
Infrared Source Transmission System Optical System Detectors Signal Processing

10.2.1 Infrared sources

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Detectors All objects with an absolute temperature of over 0 K radiate infrared energy. For example, a human body at a temperature of 310 K (37C) radiates infrared energy with a peak wavelength of close to 10 m. Infrared sources include blackbody radiators, tungsten lamps, silicon carbide, and other substances. Infrared lasers that emit infrared energy of a specific wavelength are used. In addition to the infrared source to be measured, there is background radiation from the ground at a temperature of 300K. If the measurement system is required for a wavelength region over 3 m, noise due to fluctuations in the background radiation will not be ignored. To reduce this type of noise, cold shields and cold filters are used in most cases. 10.2.2 Transmission media Typical examples of infrared transmission media include a vacuum, the atmosphere, and optical fibers, in the atmosphere. Absorption by H2O, CO2, and other elements take place at specific wavelengths. The bandwidths from 3 m to 5 m and from 8 m to 12 m, where the rate of absorption is lower, are sometimes called "atmospheric Windows" and are often used for remote sensing applications, optical fibers made of quartz with an attenuation factor that almost reaches the theoretical value has been developed, but other infrared fibers are still under improvement. [45] 10.2.3 Optical materials To converge or focus infrared radiation, optical lenses made of quartz, CaF2, Ge and Si, polyethylene Fresnel lenses and mirrors made of Al, Au or a similar material are used according to the wavelengths. In some applications, band-pass filters may be needed to utilize a specific wavelength, as well as choppers for passing and interrupting a beam of infrared addition, when designing a band-pass filter, it is necessary to consider the center wavelength, half width (FWHM) and a 5% transmittance width, in addition, the side bands, meaning secondary transmission wavelengths other than the target wavelength, must also be considered, along with the transmittance at extraneous wavelengths, this is called blocking output signals from photovoltaic detectors are usually extracted as photocurrent, so the photo sensitivity is expressed in units of A/W. When light at a given wavelength enters a photovoltaic detector, the photocurrent flows through the circuit for effectiveness. Output signals from photoconductive detectors are extracted as voltage by

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Detectors using a circuit like that shown below; the photo sensitivity is expressed in units of V/W.
[48]

10.2.4 Detector elements There are two types of major used infrared detectors: a thermal type that has no wavelength dependence, and a quantum type that is wavelength-dependent. The characteristics of the Detector Elements are as follows, a) Photo sensitivity (Responsivity) Photo sensitivity is the output voltage (or output current) per watt of incident energy when noise sensitivity. This represents the magnitude of photo sensitivity (voltage or current) per watt of incident light. The photo sensitivity of photoconductive type detectors is expressed in V/W, and the photo sensitivity of photovoltaic type detectors is expressed in A/[Link] not a consideration. b) Noise equivalent power: NEP This is the quantity of incident light equal to the intrinsic noise level of a detector. In other words, this is the quantity of incident light when the signal-to-noise ratio (S/N) is 1. This represents the detection ability of a detector and is expressed in the quantity of incident light equal to the quantity of noise, i.e., the quantity of the incident light in which its S/N becomes unity. c) Detectivity: D* (D-star) D* is the photo sensitivity per unit active area of a detector, which makes it easier to compare the characteristics of different detectors. In many detectors, NEP is proper square root of the detector active area. In general, the measurement conditions of D* are expressed in the format of D* (A, B, C), where A is the temperature [K] or wavelength [m] of a radiant source, B is the chopping frequency and C is the bandwidth. It can be said that a larger value of D* indicates a better detector element. When selecting infrared detectors for your applications, it is necessary to consider wavelength, response time, cooling method, active area and shape, number of elements (single element, onedimensional array, two-dimensional array, etc.) in addition to the above characteristics. d) D* and peak sensitivity wavelength

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Detectors When measuring infrared detector characteristics, a 500 K blackbody is often used as a radiant source. Between D* (500, f, 1) of this blackbody used as a radiant source and D* (p, f, 1) At the peak sensitivity wavelength of a detector. e) Theoretical limit of D* Some noise occurs when detecting infrared radiation. This noise may come from the infrared detector itself, from its operating circuits or from background fluctuation. Suppose that noise from an infrared detector and its circuits can be ignored in comparison with the noise caused by background fluctuation. The detection limit is determined by only the noise from the background fluctuation. This is called "Background Limited Infrared photo detection (BLIP)". D* is a measure of the S/N of a detector when infrared radiation of 1 W is input through an optical chopper. Since D* is independent of the active area and shape of the detector element, it is convenient when comparing characteristics of the detector element materials. D* is usually measured by normalizing the detector active areas to 1 cm2 and setting the amplifier bandwidth to 1 Hz. Measurement conditions of D* are expressed in the form of D* (A, B, C), where A is the temperature of a light source (K) or wavelength (m), B is the chopping frequency (Hz), and C is the noise bandwidth (Hz). The units are cmHz1/2/W. The higher the value of D*, the better the detection capability. [46] 10.2.5 Signal processing The signal output from a detector is generally quite small and needs to be amplified. When designing a preamplifier, it is necessary to consider impedance that matches the detector, low noise and bandwidth. if the incident light is modulated by a chopper, use of a tuned amplifier is effective in reducing the noise. If the detector is cooled, it is also practical to cool. the amplifier. Figure 1-10 shows an example of a very low-light measurement circuit Incorporating an InSb photovoltaic detector. [50] 10.3 Applications using infrared radiation Infrared radiation is used in a number of applications in the fields of industry, agriculture, medicine, science, communications, and remote sensing from space. 10.4 Types of Infrared Detectors Infrared detectors are classified into thermal types and quantum types. Thermal detectors use the infrared energy as heat and their photo sensitivity is independent of wavelength..

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Detectors Thermal detectors do not require cooling, but have disadvantages that response times slow and detection capability is low. In contrast, quantum detectors offer higher detection performance and a faster response speed, although their photo sensitivity is dependent on wavelength. In general, quantum detectors must be cooled for accurate measurement, except for detectors used in the near infrared region. 10.5 Selection procedure of the IR Detectors There are approximately 100 different types of infrared detectors which are available in the market the selection of them is based on the application where it will be used. To select infrared detectors that suit your applications, please refer to the following selection guides. (1) Wavelength region or temperature of the object to be measured Temperature limits of the application plays an important role in the selection of the infrared detectors. (2) Photo sensitivity and S/N (Signal-to-Noise) Depending on the intensity of light signals and the type of information to be obtained, photo sensitivity and S/N required of infrared detectors differ, so the NEP and D* are used as guides to select the optimum infrared detectors. To improve the S/N, cooling the infrared detector will be necessary. There are several cooling methods: thermoelectric cooling, cryogenic cooling such as dry ice and liquid nitrogen, and mechanical cooling such as stirling coolers. See 11. cooling techniques for how to cool the detectors. As you may notice from Figure 2-1, cooling changes the spectral response. The spectral response curves of PbS, PbSe and MCT photoconductive detectors shift to the longer wavelength side, while those of InGaAs PIN photodiodes, InAs and InSb photovoltaic detectors shift to the shorter wavelength side. The response time of PbS and PbSe photoconductive detectors becomes slower when cooled, so take precautions when cooling these detectors. As stated previously, the spectral response can chiefly be evaluated in terms of the following three characteristics. (3) Response speed and chopping frequency Response speeds required of infrared detectors depend on their applications. For example, optical communications require a response speed of 1 GHz, and intrusion detection alarms require a response speed of 0.1 Hz. It is essential to select an appropriate

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Detectors infrared detector with the response speed and chopping frequency that suits your applications. (4) Active area size and the number of elements Depending on the optical systems in your application, you may need to determine the size and geometry of an active area and also use a single detector, linear array or 2-D array. InGaAs PIN photodiodes, PbS and PbSe photoconductive detectors, InSb photovoltaic detectors and MCT photoconductive detectors are relatively flexible in terms of geometry, size and the number of elements. (5) Package Packages used for infrared detectors are divided into metal can package, ceramic package, DIP types and Dewar types (glass or metal). Also, depending on the application, the linearity, Stability, temperature characteristics, price and other elements become important factors for Selection. [47] 10.6 InGaAs Photodiode InGaAs PIN photodiodes are photovoltaic detectors having p-n junctions just like Si Photodiodes. Since InGaAs PIN photodiodes have a smaller energy gap than Si photodiodes, they have sensitivity in the longer wavelength range than Si photodiodes. The energy gap of InGaAs PIN photodiodes varies as shown in Figure 4-1 depending on the composition ratio of In and Ga. By changing the composition ratio, it is possible to manufacture infrared detectors with various spectral response ranges In addition to the standard type having a long wavelength cut-Off at 1.7 m, also provides longer wavelength types having cutoffs at 1.9 m, 2.1 Amplifier. Supposing the open loop gain of the operational amplifier is "A", the equivalent input Resistance expressed as Rf/A due to the negative feedback circuit becomes several digits Smaller. Thus, an ideal Isc measurement is possible with this method. When measuring Isc over A wider range, change the Rf value as necessary. m and 2.6 m. 10.6.1 Linearity Linearity of InGaAs PIN photodiodes is determined by noise, while the upper limit is determined by the detector active area and the electrode structure. To expand the upper limit, it is sometimes practical to apply a bias voltage. Where only the linearity is a

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Detectors consideration, applying 1 V is Sufficient. The InGaAs PIN photodiode is used as a photoconductive detector. Applying a bias Voltage is effective in improving the linearity and response speed, but this also increases the Dark current and noise level. An excessive bias voltage may damage InGaAs PIN photodiodes and deteriorate their performance. Always use them within the Maximum rating voltage and set so that the cathode has a positive potential with respect to the Anode. [48] 10.6.2 Feedback resistance The output of photocurrent becomes the voltage of Isc Rf (current-voltage conversion). The feedback resistance Rf is determined by Isc and the required output voltage Vo. When it Becomes larger than the shunt resistance, the input noise voltage and input offset voltage of the operational amplifier are multiplied by (1+ Rf/Rsh) and the result is superimposed over the output voltage. As the bias current error of the operational amplifier also becomes Large, the feedback resistance should not be allowed to increase without limit. The feedback Capacitance Cf is sometimes called the damping capacitance and is used mainly for oscillation Protection. In some cases, a few pF is sufficient for this protection. This feedback circuit has a Time constant of Cf Rf and serves as a noise filter. At the same time it constrains the response speed, and so it is necessary to select values that suit your applications. The error Caused by offset voltage can be reduced to below 1 mV by connecting a variable resistor to the Offset adjustment terminal of the operational amplifier. 10.6.3 The operational amplifier The actual input resistance of the operational amplifier is not infinite and some bias current flows into and out of the input terminal, potentially causing an error, depending on the level of the Detection current. Such bias current ranges from several nA to several hundred nA in the case of A bipolar operational amplifier and is below several 0.1 pA in the case of an FET input type Operational amplifier. The bias current of the FET type operational amplifiers doubled when the temperature rises by 10 C, but it decreases with a bipolar operational Amplifier. When designing a high-temperature circuit, use of a bipolar type Operational amplifier should be considered. Like offset voltage, the error voltage caused by the bias current can be fine-adjusted by connecting a variable resistor to the offset adjustment Terminal of the operational amplifier. [49]

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Detectors 10.6.4 Feedback resistance The feedback resistance Rf is determined by Isc and the required output voltage Vo. When it becomes larger than the shunt resistance, the input noise voltage and input offset voltage of the operational amplifier are multiplied by (1+ Rf/Rsh) and the result is superimposed over the output voltage. As the bias current error of the operational amplifier also becomes large, the feedback resistance should not be allowed to increase without limit. The feedback Capacitance Cf is sometimes called the damping capacitance and is used mainly for oscillation Protection. In some cases, a few pF is sufficient for this protection. This feedback circuit has a Time constant of Cf Rf and serves as a noise filter. However, at the same time it con-strains the Response speed, and so it is necessary to select values that suit your applications. Also, the error Caused by offset voltage can be reduced to below 1 mV by connecting a variable resistor to the Offset adjustment terminal of the operational amplifier. [50] 10.6.5 The operational amplifier The actual input resistance of the operational amplifier is not infinite and some bias current flows into and out of the input terminal, potentially causing an error, depending on the level of the Detection current. Such bias current ranges from several nA to several hundred nA in the case of A bipolar operational amplifier and is below several 0.1 pA in the case of an FET input Type operational amplifier. Generally, the bias current of the FET type operational amplifier is doubled when the temperature rises by 10 C, but it decreases with a bipolar operational Amplifier. For this reason, when designing a hightemperature circuit, use of a bipolar type Operational amplifier should be considered. Like offset voltage, the error voltage caused by the bias current can be fine-adjusted by connecting a variable resistor to the offset adjustment Terminal of the operational amplifier. [51] 10.6.6 InGaAS Image Sensors The InGaAs linear image sensor is a self-scanning photodiode array designed specifically for Detectors in multichannel spectroscopy. The InGaAs PIN linear image sensor offers a number of features necessary for detectors in multichannel sectors copy, for example a large Photosensitive area, high quantum efficiency, wide dynamic range due to low dark current and High saturation charge, excellent output linearity and low power

Smt. R.B.P.M.P.C. 21

Detectors Consumption. The standard types use a sapphire window that has superior infrared transmission. Applications include not only spectroscopy but also a wide range of image readout systems. (A)The charge integration method in which the InGaAs active area is handled simply as a Current source. This allows the InGaAs photodiodes in the active area to operate at low Bias, resulting in outstanding performance as an image sensor. (B) Wavelength ranges of 0.9 to 1.7 m and 0.9 to 2.6 m are provided. (C) G InGaAs active area fabricated in a highly stable production. (D) Process allows an extremely small dark current level and a long exposure time, making it ideal for low-light-level detection. (E) Thermoelectric coolers make temperature control and cooling easy. [52] 10.7 PbS, PbSe Photoconductive detector PbS and PbSe photoconductive detectors are infrared detectors making use of the Photoconductive effect that resistance is reduced when infrared radiation enters the detecting Elements. Compared with other detectors in the same wavelength region, the PbS and PbSe have Superior features, such as higher detection capability, faster response speed, and they also Operate at room temperatures. However, the dark resistance, photosensitivity and response Characteristics change depending on the ambient temperature. Therefore, care is required to Ensure the best results. 10.7.1 Spectral response Unlike other semiconductors, the temperature characteristics of PbS and PbSe band gaps have a Negative coefficient. Because of this, the spectral response characteristics shift to the long Wavelength region when cooled. 10.7.2 Bias voltage dependence The noises levels in the PbS and PbSe suddenly increase when the voltage applied to the detector Elements exceed a certain threshold level. Since the signal level increases in proportion to the voltage, it is recommended that the detectors be used at as low a voltage as possible within the rated maximum applied voltage described in the catalog. Active area With respect to the S/N, it is much more efficient to use PbS and PbSe with a small active area And introduce a converged light to the detector elements, rather than using detector

Smt. R.B.P.M.P.C. 21

Detectors elements With a large active area. Incident light may falls on the outside of the active area or extraneous Light may enter the active area causing the S/N to drop. Take precautions against the optical path Of the incident light. [53] 10.8 Pyroelectric Detector: The pyroelectric detector is a thermal type infrared detector that operates at room temperatures. The pyroelectric detector consists of a PZT having the pyroelectric effect, a high resistor and a low-noise FET, hermetically sealed in a metal package to protect against external noise. The pyroelectric detector itself does not have wavelength dependence, but the combination of various window materials makes it usable for various applications, such as human body Detection and gas analysis. 10.8.1 Pyroelectric effect The PZT is spontaneously polarized in the dark state. The element surface is always electrified, but it is neutralized by ions in the air. When light enters the element and is absorbed, the element Temperature increases, resulting in a change in the spontaneous polarization state. These changes are outputted as a voltage change. Since the pyroelectric detector detects is necessary to use an Optical chopper for measurement of still objects. 10.8.2 Pyroelectric materials By changing the compositional ratio of PZT, various pyroelectric materials can be produced with a dielectric constant of 200 to 400 and a Curie temperature of 250 to 450 C. Since PZT has a Polycrystalline composition structure, it features high resistance to mechanical distortion caused by sudden temperature changes and offers extremely high stability against temperature Fluctuations, allowing highly reliable operation as pyroelectric detectors. 10.8.3 Operating principle There are two methods for extracting a surface charge: using voltage, and using current. Ordinarily, voltage output type pyroelectric detectors are used. The voltage type offers a simple Circuit configuration and less noise, and has a sensitivity peak at a relatively low frequency. Advantage of these features, it can be used in applications such as sensors to detect Human bodies The current type features high gain and a constant sensitivity ranging from low to High, and is often used in laser detectors and other similar

Smt. R.B.P.M.P.C. 21

Detectors applications. The frequency limit is determined by the constant of the amplifier, so the frequency response can be improved by adjusting the circuit configuration of the amplifier. 10.8.4 Features of voltage output type: Pyroelectric detectors (voltage output type) have the following features. Operation at room temperature. Flat spectral response. Output signal obtained only when there is a change in Incident energy built-in impedance-conversion FET Low cost. Long life High sensitivity compared to other thermal type detector. [54]

10.9 Applications Infrared Radiations: 10.9.1 Optical power meters: Optical power meters are used for measuring light intensity and find a wide variety of Applications, such as in optical fiber communications and lasers. Optical fiber communications are classified into short, middle and long distance communications systems. For long distance Optical communications systems, infrared beams in the wavelength region from 1.3 m to 1.5 m that provide less optical fiber transmission loss are employed. InGaAs PIN photodiodes, etc. are used for optical power meters to measure optical fiber transmission loss, relay quality, laser Power, etc. The characteristics particularly required for the optical power meter are linearity and Uniformity. Cooledtype detector is used to reduce the noise level so that Low power light can be measured with low noise. 10.9.2 LD monitors: The output level and the emission wavelength of a laser diode (LD) vary with the temperature. To stabilize the LD, automatic power control (APC) is performed. The APC includes two Methods: one is to monitor the integrated amount of light pulses from the LD and the other is to monitor the peak value of light pulses. With the development of high power LD, high linearity has become essential for monitoring light pulses. In the

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Detectors method for monitoring the peak value of Light pulses; faster response is also required. 10.9.3 Radiation thermometers: Objects emit infrared radiation based on their own temperatures if they are above the absolute zero degree temperature. The radiant energy of a black body actually, the quantity of infrared rays emitted from an object is not necessarily determined based on the temperature. The emissivity must be compensated for. In the case of a black body, e = 1, the emissivity of various objects. Since the emissivity e is determined by the temperature and wavelength of an object, care should be taken when measuring the absolute temperature of an object. The noise equivalent temperature differential (NET) is used as an index to express the thermal resolution. 10.9.4 Flame monitors (flame detection): The flame monitor is used for detecting light emitted from flames and for observing how the Flames are burning. Light emitted from flames is distributed widely From the UV region to the infrared region. Detection methods include using a PbS Photoconductive detector to detect infrared light, using a two-color detector (K1713-01) to detect a broad spectrum from the UV region to the infrared region, and using PbSe and pyroelectric Detectors to detect a wavelength of 4.3 m. [55]

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Detectors

11. Conclusion: A detector is a photodiode, the core of which is a p-n-junction created during the wafer processing. The Fermi-levels of the p- and n-type materials, i.e. the highest occupied energy state of the electron gas within the semiconductor material, must match, which effectively creates an electric field across the junction. The incident infrared photons free electron-hole pairs into the conductance band at or near the junction, which are immediately separated by the electric field. The accumulated charge carriers cause a voltage change across the junction, which can be detected and used as a measure of the incident light. The dark current strongly depends on whether the "bump" anomaly will be observed or not (see next section) when NICMOS will be cooled down to operating temperatures with the NCS. The quoted readout noise is the realized noise from a pair of readouts (i.e., the quadrative sum of a single initial and final readout). The following sections will give more information for each of the quantities of this table. Saturation is defined as 2% deviation from quadratic non-linearity. The NICMOS arrays exhibit a noiseless signal gradient orthogonal to the direction of primary clocking, which is commonly referred to as shading. The final element of the mass spectrometer is the detector. The detector records either the charge induced or the current produced when an ion passes by or hits a surface. In a scanning instrument, the signal produced in the detector during the course of the scan versus where the instrument is in the scan. The mass resolving power is the measure of the ability to distinguish two peaks of slightly different m/z. The mass range is the range of m/z amenable to analysis by a given analyzer. The linear dynamic range is the range over which ion signal is linear with analyze concentration. Speed refers to the time frame of the experiment and ultimately is used to determine the number of spectra per unit time that can be generated. A tandem mass spectrometer is one capable of multiple rounds of mass spectrometry, usually separated by some form of molecule fragmentation. For example, one mass analyzer can isolate one peptide from many entering a mass spectrometer. A second mass analyzer then stabilizes the peptide ions while they collide with a gas, causing them to fragment by Collision Induced dissociation. The development of radiation detectors in the field of Smt. R.B.P.M.P.C. 21

Detectors nuclear and particle physics has had a terrific impact in medical imaging since this latter. The accelerated scientific progression in genetics and molecular biology has finally generated what it is now called Molecular Imaging. The use of gas, scintillation and solid-state detectors in digital radiology and digital mammography, clinical CT and small animal CT.

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Detectors

References:
1. I. A. Fowlis and R. P. W. Scott, J. Chromatogr.,vol -11 1963 P-11. 2. J. E. Lovelock, "Gas Chromatography 1960"P- 26 3. A. T. James and A. J. P. Martin, Biochem. J. VOL-50 1952 P-679. 4. A. T. James, The Times Science Review, VOL-1955 P-8. 5. C. W. Munday and G. R. Primavesi, "Vapor Phase Chromatography",1957 P-146. 6. N. H. Ray, J. Appl. Chem.,vol 4 1954 P-21. 7. R. P. W. Scott, "Vapor Phase Chromatography" 1957 P-131. 8. H. Boer, "Vapor Phase Chromatography" 19571 P-69. 9. D. W. Grant, "Gas Chromatography 1957 P-153. 10. 1. J. Harley,W. Neland V. Pretorious,,vol-181 1958 P-177. 11. I. G. McWilliams and R. A. Dewer, "Gas Chromatography 1958 12. S. A. Beres, C. D. Halfmann, E. D. Katz and R. P. W. Scott, Analyst, vol-112 1987 P-91. 13. L. Ongkiehong, "Gas Chromatography" 1958 P-9. 14. D. H. Desty, A. Goldup and C. J. Geach, "Gas Chromatograph 1958 P-156. 15. H, F. Calcote and I. R. King, "The Fifth Symposium on Combustion",1955.P-23 16. K. E. Schuler and J. J. Weber, J. Chem. Phys.,vol-22 1994 P-49 17. J. E. Lovelock and S. R. Lipsky, J. Amer. Chem. [Link]-82 1960 P-431. 18. E. Lovelock, J. Chromatography. VOL-1 1958 P-35. 19. J. E. Lovelock, Nature, Lond. VOL-181 1958 P-1460. 20. R. P. W. Scott, Nature, Lond, VOL-183 1959 P-1753. 21. S. A. Beres, C. D. Halfman, E. D. Katz and R. P. W. Scott, VOL-112 1987 P-91. 22. J. E. Lovelock and S. R. Lipsky, J. Amer. Chem. [Link]- 82 1960 P-431. 23. A.J.P. Martin and R.L.M. Synge, Biochem. J. VOL- 35 1941 P-1358. 24. A. T. James and E. A. Piper, J. Chromatogrphy. VOL-5 1961 P-265. 25. A. T. James and E. A. Piper, Anal. [Link]-35 1963 P-515. 26. S. A. Ryce and W. A. Bryce, NatureVOL-179 1957 P-541. 27. S. A. Ryce and W. A. Bryce, Can. J. Chem., VOL-35 1957 P-1293.

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Detectors 28. L. V. Guild, M. I. Lloyd and F. Aul, "Gas Chromatograph, 2nd International I. S. A. Symposium, June, 1969" 1961 P-91. 29. E. A. Hinkle, H. C. Tucker, R. F. Wall and J. F. Combs, "Gas Chromatograph, 2 nd International I. S. A. Symposium, June, 1969" P-432 30. J. Harley and V. Pretorious, Nature, VOL-178 1957 P-1244. 31. R. C. Pitkethly, Anal. [Link]- 30 1958 P-1460. 32. J. E. Lovelock, J. Chromatography., VOL-1 1958 P-35 33. A. Karman and R. L. Bowman, Ann. N. Y. Acad. Sci., vol-72 1959 p-714. 34. W. L. Nyborg, C. L. Woodbridge and A. K. Schilling, Acoust. vol-25 1953 p138. 35. M. K. Testerman and P. C. McLeod, "Gas Chromatography" 1957 p-765 36. J. D. Winefordner, D. Steinbrecher and W. E. Lear, Anal. [Link]-33 1961 P515. 37. U.S. patent 2,121,103 (inventor: Stuart William Seeley); issued 21 June 1938. 38. D.E. Foster and S.W. Seeley, "Automatic tuning, simplified circuits, and design practice," Proceedings of the Institute of Radio Engineers, vol. 25, no. 3, part 1, pages 289-313 (March 1937). 39. See: U.S. patent 2,497,840 (inventor: Stuart William Seeley); issued: 14 February 1950. 40. See also: U.S. patent 2,561,089 (inventor: Earl I. Anderson); issued: 17 July 1951. 41. Report L.B.-645: "Ratio detectors for FM receivers" (15 September 1945) issued by the Radio Corporation of America, RCA Laboratories Industry Service Division, 711 Fifth Avenue, N.Y., N.Y. Reprinted in Radio, pages 18-20 (October 1945). 42. Stuart W. Seeley and Jack Avins, "The ratio detector," RCA Review, vol. 8, no. 2, pages 201-236 (June 1947). 43. D. S. Evans and G. R. Jessup, VHF-UHF Manual (3rd Edition), Radio Society of Great Britain,London, 1976 pages 4-48 through 4-51 44. Charles Travis, "Automatic oscillator frequency control system" U.S. patent: 2,294,100, vol. 23, no. 10, pages 1125-1141,1935.

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Detectors 45. R. A. Wood, Uncoiled thermal imaging with monolithic silicon focal planes, SPFE Vol. 2020,993, pp. 322-329. 46. [Link],.Uncoiled thermal imagin vo l 2020,1993, pp. 330-339 47. .[Link], H.Y a s h i r o and [Link]`An Integrated Thermal InfraredSensing Array Vol 14,1988 pp 191-201 48. I. H. Choiand ,K. D. Wise, A Silicon-Thermophile-based Infrared Sensing Array for Use in Automated Manufacturing,IEEE Transactions. Electron Devices, vol. ED-33, pp. 72-79, Jan. 1986. 49. [Link],K.D Wise and [Link] A 32-Element Thermophile With On- Chip Multiplexing Vol-48 1995,Pp47-54 50. T. Kanno, M. Saga, S. M a s u m o t o S. T o t h A. Vol-22 1984 P-23 51. A. W. van Herwaarden, The Effect in Silicon ICs, vol. 6, pp. 245254, 1984 52. R. Lenggenhager, H. B a l t e s J. Peer and M. Forster,Thermoelectric Infrared Sensors by CMOS Technology, vol. 13, pp. 454-456, Sept. 1992. 53. M. von A r x O. Paul, and H. B a l t e s , Test Structures to Measure The Coefficient of C M O S technology Vol-43 P-768 1967. 54. R. Lenggenhagger, H. B a l t e s and T. E l b e l , Thermoelectric Infrared sensors in CMOS technology, vol. 37-38, pp. 216-220, 1993 55. D. F. Floring and B. J. OKeefe, The Design of Fast Thermophiles and the Ultimate Sensitivity of Thermal Detectors,vol. 18, pp. 474-482 1947. [Link] [Link]

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Detectors

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