atomic absorption spectrometry - nptel
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1
INDUCTIVELY COUPLED PLASMA ATOMIC EMISSION SPECTROMETRY
2
When an atom is exposed to high temperature sourceenergy is transferred to the atom by collisions withenergetic particles and also by the interaction with theelectromagnetic radiation. The excited atom decays toa lower energy level with emission of its owncharacteristic electromagnetic radiation. Themeasurement of the electromagnetic radiation emittedby the atoms, ions and isotopes can be accomplishedby employing suitable optics which also permitsconcentration determination.
3
SCHEMATIC DIAGRAM OF ATOMIC EMISSION
ELEMENTCONC
READOUT
EXCITATIONSOURCE SPECTROMETER
DETECTOR
4
A. GENERATION OF EM RADIATION
ARC Discharge
Sample is mixed with a conducting material such as graphite and packed into the crator of a carbon electrode. A DC arc discharge between the sample electrode and thecounter electrode vapourizes the sample, decomposes molecular species produced in the plasma and atomizes the analyte. The atoms are excited to higher energy by the energetic particles in the plasma.
5
ARC DISCHARGE
6
The DC arc is generated from a rectified power supply which provides 5-30 A0 and 10-25 V, generating temperatures from 4000 �– 60000 k. However the arc tends towander resulting in poor analytical precision. As the arc temperature is determined by the species in the arc plasma, the composition and temperature changes with time and space. Molecular species such as cynogen etc., exist in theplasma.
Many of these limitations can be minimized or eliminated. The DC arc is more suited for qualitative analysis which finds extensive applications in foundries, steel & metallurgical industries.
7
An AC arc provides more uniform sampling of the electrode compared to DC arc. It operates at voltages ranging from 1100 �– 4400 V .The polarity of the discharge is reversed at each halfcycle and the discharge is extinguished when the voltage drops to zero. Thesampling is random, resulting in improved precision compared to the DC arc. The sensitivity is less that of the corresponding DC arc.
8
HV SPARKThe circuit consists of HV transformer used to charge anoil filled capacitor and an auxiliary control gap to initiate and control the discharge. A potential of 15000 - 45000 V develops across the analytical gap. An HV spark discharge between the metal sample and counter electrode generatessufficient energy to vapourise the sample and generate atoms and excite them. The emitted radiation is monitoredthrough a quartz window mounted on the excitation stand. A thoriated tungsten electrode is used as a counter electrode and argon is used to purge the gas chamber.
The spark technique is useful for major, minor and trace elements in metals and alloys for analysis and production control. The intensity of the emission is measured relative to iron and plotted against the concentration ratio to eliminate errors resulting from the fluctuations. Typical detection limitsare of the order of 0.001 to 0.1% by weight.
9
SPARK DISCHARGE
10
GLOW DISCHARGE
It consists of a flat sample cathode and cylindrical anode mounted in a sealed chamber filled with argon.At 600 �– 1800 V , the gas is ionized and accelerated to the cathode. Collisions with the cathode surface causes vapourization of the sample material and excitation. The emitted radiation is viewed from a quartz window.
The cathode block which is in direct contact with the sample is water cooled to remove excess heat. The sample is pressed against the open end of the cathode body and held in vacuum. After evacuation the chamber is filled with argon to 5-15 torr pressure. Standard calibration curves for the determination of trace elements in pure materials are linear over three orders of magnitude in concentration.
11
LASER INDUCED PLASMA
Pulsed laser beams have been used in AES of extremely small samples and occlusions on surfaces of metal alloys laser beam is focused on sample surface and the material is vapourized. The plasma plume formed above the target passed through an auxiliary electrode gap and is excited by a low voltage spark discharge.
Hollow cathode discharge : 0.06-10 ppm for solid samples and from 0.2-1 ppm for solutions.
12
The electromagnetic radiation is resolved with a spectrograph and the spectra are recorded photographically or measured with an array detector. Solid state Nd glass laser, a spark source, a mirror and focusing lens to direct the laser beam on to the surface of the sample constitute theinstrumentation.
A laser pulse with 0.1 �– 1.0 J and a duration of 2 secproduces a crator of 25 �– 250 µm. The detection limit is 10-9 �– 10-11 g.
13
PLASMA SOURCES
High temperature plasmas generated from electrical power sources where collisions are induced by electrical currents are useful for the analysis of solid, liquid and gaseous samples. They are Direct Current Plasma (DCP), Inductivity Coupled Plasma (ICP) and Microwave Induced Plasma (MCP).
A DC plasma source consists of a DC arc discharge between two electrodes in which argon is introduced.Gas is introduced in a tangential flow so that the resultant gas is constricted, resulting in increased current density and higher temperature. The DC plasma is operated at a current 5 - 30 A0 and gas flow rates up to 70 litres/minute. Temperatures in the plasma range from 4700-11000 K.
14
The sample is introduced as an aerosol by means of a neubulizer positioned between the electrodes (anodes).The optical measurement region is located near the base of the confluence to eliminate high background from the arc plasma.
It is useful for analysis of solutions containing 45% of thetotal dissolved solids. The advantage is that it is a low cost DC power supply. However continuous operation for longer periods is not possible because the electrodes erode. Consequently electrodeless plasma sources such as inductively coupled plasma are common in ICP �– AES.
15
PLASMA TORCH
16
INDUCTIVELY COUPLED PLASMAThe energy to form the plasma is generated by a high frequency magnetic field. It is analogous to that of a transformer in which primary winding is an induction coil with an oscillatory current from a RF generator. The secondary winding (or load) is the ionized argon gas which is coupled inductively to the radio frequency source. The plasma torch consists of two concentric quartz tubes with Ar gas flowing tangentially between the inner and outer tubes to provide cooling and a water cooled induction coil near the periphery of the outer tube. Argon gas flowing through the smaller tube interacts with the magnetic fieldwhen sufficient external energy is applied to ionize the gas. Initial ionization can be provided by a Tesla discharge and the plasma is sustained by ionized argon formed in the high temperature plasma.
17
The sample is directed into the plasma through a capillary tube mounted in the centre of the torch assembly. An RF generator of 1-5 kw at 3-100 MHz will sustain an argon plasma which produces 5000 �– 10000 K depending upon the power, gas flow rate and composition and coupling efficiency. Optimum viewing heights vary with the analyte and which is usually a compromise of 3 -10 mm range in multi-element analysis.
ICP is an extremely versatile source for AES. Sample solutions are nebulized into a chamber and the aerosol is directed into the plasma using a carrier gas. Standard calibration curves for most elements are linear over 5-6 orders of magnitude in concentration and detection limits range from 0.1 to 200 ppb.
18
MICROWAVE INDUCED PLASMA
The plasma source consists of a microwave resonator or a cavity inductively coupled to a high frequency generator by means of a coaxial waveguide. It provides 200-500 W of power at a frequency of 2 - 45 GHz. Power is transferred to the microwave cavity by means of a coupling loop.
MIP is used to determine a wide variety of gases such as C, H, N, O, F, Cl, Br, S. Detection limits range from 1 - 50 ppb and calibration curves are linear over 3 - 4 orders of magnitude.
19
B. SEPARATION OF EM RADIATION
Electromagnetic radiation can be separated into its components by a variety of instruments and techniques. Grating instruments are commonly used. For high resolution spectroscopy the incident radiation can be separated in two dimensions by an Echelle grating and separating multiple orders with a prism. Fourier transform spectroscopy has been developed that extends the wavelength range to ultraviolet region.
20
ECHELLE GRATING
21
CONCAVE GRATINGS
In Rowland mounting, the grating and the detector are attached to a rigid bar that moves relative to a fixed entrance slit. The angle of diffraction remains constant and the angle of incidence varies. The detector is always kept in a position normal to the grating. Under these conditions, the dispersion is linear over a broad wavelength range.
In Abney mounting, grating and detector are fixed and the slit moves along the axis of the Rowland circle. This is slightly cumbersome because light source and external optics also need to be repositioned when the angle of incidence is changed.
22
ROWLAND MOUNTING
23
In Eagle mounting, slit and detector are mounted on the same side of the grating normal to all components on the Rowland circle. This is a compact arrangement.
The Paschen �– Runge mounting has slit ,grating and detector at fixed positions on the Rowland circle. Most of the commercial direct reading instruments are of this type.
In Wadsworth mounting, a spherical mirror is used to collimate the incident beam which illuminates the grating with a parallel light. When the wavelength region is changed, the detector to grating distance must be changed to maintain proper focus of the diffracted light.
24
PLANE GRATINGS
The Ebert �– Fastie and Czerny turner mountings utilize a plane grating in combination with a spherical mirror to collimate the incident beam and to focus the diffracted light on the exit slit or detector. The incident beam passes over the grating and the diffracted light passes under the grating. Since the detector is near normal to the grating plane, the dispersion is approximately linear.
The Czerny �–Turner mounting differs from the Ebert �– Fastie in that the spectrometer has two spherical mirrors. These are used in combination with array detectors which have replaced photographic emulsionsfor the measurement of spectra.
25
Czerny �– Turner mounting
26
C. DETECTION OF ELECTROMAGNETIC RADIATION
The PMT is the preferred mode of measurement. It consists of a photo cathode, a series of dynodes and an anode in an evacuated tube. The amplification is nearly 1 million. The line image is focused on the slit and directed to PMT by means of a refractor plate.
27
PHOTOGRAPHIC DETECTOR
This is the most sensitive and versatile technique. A densitometer is used for measuring and identifying elements. It consists of a photoplate or film holder assembly and a light source and associated photo detector to measure the quantity of light passing through a photographic emulsion. The photoplate is moved in a direction normal to the light beam and can be positioned to measure any segment on the photoplate. The image is magnified and displayed on a screen. A reference spectrum with spectral lines of known elements is displayed adjacent to the sample spectrum.
28
THE ICP SOURCE
A typical ICP source is called a torch. It consists of threeconcentric quartz tubes through which streams of argon flow at a total rate of 5-20 L/min. the inner diameter of the tube is about 2.5 cm. The top portion of this tube is an induction coil that is powered by a radio frequency generator which radiates 0.5 �– 2 kW of power at 27.12 MHz or 40.68 MHz at this voltage a spark from the Tesla coil ionises the argon.
29
The resulting ions and their associated electrons interact with the fluctuating magnetic field produced by the induction coil. This interaction causes the ions and electrons within the coil to flow in the closed annular paths. The resistance of the ions and electrons causes ohmic heating of the plasma.
The temperature of the plasma reaches 4000-6000 K, which requires thermal isolation of the outer quartz cylinder. This is achieved by argon flowing tangentially around the walls of the tube and entering the plasma radially.
In most of the instruments the torch is positioned at 900
and aligned axially with the spectrometer system. The radiation emitted from the plasma is used for analysis.
30
TYPICAL DESIGNS OF ICP TORCHES
31
SAMPLE INTRODUCTIONThe most common means of sample introduction is through the Bernoulli effect. High velocity moving gas flowing around a capillary sucks the sample and delivers it at the tip where the liquid breaks up into fine droplets before enteringthe plasma.
Another way of introducing the sample is to pump it throughthe capillary using a peristaltic pump. At the tip, high velocity argon flows across at right angles causing the same Bernoulli effect.
It is also possible to atomize the sample in a graphite tube and introduce the vapour into the plasma.
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MEIN HARD NEBULIZER
33
A typical plasma appears as very intense white flame. It hasa non-transparent core topped by a flame like tail. The core extends a few millimeters above the tube and produces the atomic spectrum of argon superimposed on a continuum spectrum. The continuum spectrum is typical of charged ions and electrons interaction and known as �“bremstrahlung�”.
10-30 millimeters above the core the continuum fades and the plasma is optically transparent. Hence spectral observations are generally made a 15-20 millimeters above the induction coil where temperature of 6000-6500 K prevail. In this region the background radiation is remarkably free from the argon lines but those of Ca+, Cd+, Cr+, Mn+ etc., remain.
34
TEMPERATURE VARIATION IN THE PLASMA
35
ADVANTAGES OF PLASMA SOURCE
High temperatures ensure complete atomization. Hence fewer interferences are found in ICP.
Atomization occurs in a chemically inert environment.
The temperature cross section is more uniform. Therefore self absorption or self reversal do not occur. Therefore calibration curves are linear over several orders of magnitudes of concentration.
Since the plasma produces significant ionization, it is an excellent source for ICPMS.
36
PLASMA SOURCE SPECTROMETERS
High resolution 0.01 nm or / > 100,000.Rapid signal acquisition and recovery. Low stray light.Wide dynamic range (> 106).Accurate and precise wavelength identification and selection.Precise intensity readings (< 1% relative standard devn).High stability with respect to environmental changes.Computerized data handling.
37
SEQUENTIAL ICP INSTRUMENTS
Such instruments use a holographic grating monochromator of 2400 or 3600 grooves/mm. Scanning is accomplished by rotating the grating with a digitally controlled stepper motor so that precise wavelengths are focused on the exit slit.
In some designs the grating is fixed and the slit and photomultiplier tubes are moved along the focal plane. For ultraviolet and visible range, separate sets of slits and PMTs are used. The switch between the two is effected by the movement of a plane mirror located between the two transducers.
38
The scanning of spectra is controlled by a computer in a series of small steps of 0.01 to 0.001 nm. Usually whenever there is no emission, the spectra is scanned quickly and slows down near a peak. Such an arrangement is known as slew scan spectrometer.
39
OPTICAL SCHEMATIC DIAGRAM OF ICP
40
MULTICHANNEL INSTRUMENTS
In multichannel instruments the entrance slit, exit slits and the grating surface are located around the circumference of a Rowland circle which corresponds to the focal curve of the concave grating.
Radiation from each of the fixed slits impinges on the PMTs. The slits are factory configured to transmit lines for selected elements. The signals are integrated , the output is digitized and converted into concentrations.
For rapid analysis such instruments are quite useful.
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MULTICHANNEL ARRANGEMENT 1
42
MULTICHANNEL ARRANGEMENT 2
43
APPLICATIONS OF PLASMA SOURCES
Useful for qualitative and quantitative elemental analysis. The samples must be dissolved in aqueous or organic solvents.
In principle all metallic elements can be determined by ICP. For B, N, S and C, vacuum spectrometer is necessary as their emission wavelengths are less than 180 nm.
Li, K, Rb and Cs lines are located at near IR lines which lead to detection problems.
44
TYPICAL DETECTION LIMITS IN ICP
45
CHEMICAL ANALYSIS WITH ICP
Typical calibration curves in ICP consist of electrical signals in the form of counts (intensity) versus analyte concentration . More than 70 elements have been determined by ICP at various wavelengths and the data is recorded to three decimal places with appropriate intensity. The information is available in several data bases and standard publications. Thus a suitable wavelength for any element can be found easily.
46
Usually the selection of an analytical line depends upon the intensity. However other concomitant elements present in the matrix should not be emitting at the same wavelength. Calibration plots are usually linear over several orders of magnitudes of concentration.Therefore log-log plots can also be used.
47
TYPICAL CALIBRATION CURVES IN ICP-AES
48
Departures from linearity often occur especially when large concentrations are covered.
Self absorption becomes evident only at high analyte concentrations and causes the calibration curves to bend towards the horizontal axis.
Nonlinearity also arises from erroneous background correction, from ionization and from nonlinear detector responses.
49
INTERNAL STANDARD
In ICP work an internal standard is often used. In this case, the vertical axis of the calibration curve is the ratio or the log ratio of the detector signal for the analyte and that of the internal standard. Thus the intensity improves to a considerable extent.
50
INTERNAL STANDARD CALIBRATION CURVES IN ICP
yttrium 242.2 nm as internal standard
51
INTERFERENCES
Chemical and matrix interferences are significantly lower with plasma sources compared to other atomizers.However at low analyte concentrations the background emission due to recombination of argon ions with electrons is significant. For both single channel and double channel instruments, this correction is made by taking an average of the background readings on either side of the emission peak. Nowadays instrument software accomplishes this task automatically or at the discretion of the operator.
52
Spectral interferences are always possible in ICP analysis because emission spectra of many elements are rich in lines. Therefore it is preferable to have a knowledge of the other matrix elements in the sample and their emission lines to choose a noninterference analytical line.
The software for ICP instruments has powerful routinesfor wavelength selection, calibration, spectral analysis and deconvolution of overlapping lines. Additionally, integrated data bases of spectral lines of other elements make spotting and correcting for interferences an integral part of the analytical process.
53
DETECTION LIMITSIn general, detection limits in ICP-AES are comparable to or better than flame AAS and electrothermal AAS. The following table is illustrative.
54
DETECTION LIMITS OF ICP
55
Table 1. DETECTION LIMITS FOR AIR-ACETYLENEFLAME
56
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57
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58
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59
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60
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61
Table 2. DETECTION LIMITS FOR NITROUS OXIDE ACETYLENE FLAME
62
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63
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64
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65
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66
Table 2 �…