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ANALYTICAL 
INSTRUMENT 
Presented by :- Pranjit Sharmah 
2013-2014 
M.Sc Sem I
ANALYTICAL 
INSTRUMENTS 
In mineral science, there are several analytical 
instruments used for various purpose, viz… 
 Scanning electron microscopy 
 X-ray diffraction 
 Transmission electron microscopy 
 X-ray fluorescence 
 Flame atomic absorption spectroscopy 
 Electron microprobe analysis 
 Secondary ion mass spectrometry 
 Atomic force microscopy 2
SCANNING ELECTRON MICROSCOPY (SEM) 
The scanning electron microscope has an electron 
optical column in which a finely focused electron beam 
can be scanned over a specified area of the specimen. 
3
FUNDAMENTAL PRINCIPLES OF SCANNING 
ELECTRON MICROSCOPY (SEM) 
Accelerated electrons in an SEM carry significant 
amounts of kinetic energy, and this energy is 
dissipated as a variety of signals produced by 
electron-sample interactions when the incident 
electrons are decelerated in the solid sample. These 
signals include secondary electrons (that produce 
SEM images), backscattered electrons (BSE), 
diffracted backscattered electrons (EBSD) that are 
used to determine crystal structures and 
orientations of minerals. 
4
SCHEMATIC DRAWING OF FINELY FOCUS ELECTRON 
BEAM IMPINGING ON A MATERIAL SURFACE : 
5
APPLICATIONS OF SEM 
The SEM is routinely used to – 
 To generate high-resolution images of shapes of objects. 
 Identify phases based on qualitative chemical analysis 
and/or crystalline structure. 
 SEMs equipped with diffracted backscattered electron 
detectors can be used to examine microfabric and 
crystallographic orientation in many materials. 
6
STRENGTHS AND LIMITATIONS OF SEM 
Strength:- 
 Most SEM are comparatively easy to operate. 
 Modern SEMs generate data in digital format which are highly 
portable. 
 For many applications, data acquisition is rapid. 
Limitations- 
 . Samples must be solid and they must fit into the microscope 
chamber 
 An electrically conductive coating must be applied to electrically 
insulating samples for study in conventional SEM. 7
X-RAY DIFFRACTION TECHNIQUES (XRD) 
The first application of an X-ray experiment to 
the study of crystalline material in 1912 by 
Max Von Lou. There are two different X-ray 
diffraction techniques – 
i) Single crystal techniques 
ii)X-ray powder diffraction techniques 
8
SINGLE CRYSTAL TECHNIQUES…… 
What is Single-crystal X-ray Diffraction??? 
Single-crystal X-ray Diffraction is a non-destructive 
analytical technique which provides detailed 
information about the internal lattice of crystalline 
substances, including unit cell dimensions, bond-lengths, 
bond-angles, and details of site-ordering. 
9
FUNDAMENTAL PRINCIPLES OF SINGLE-CRYSTAL X-RAY 
DIFFRACTION 
Single crystal X-ray diffraction concern with the interaction of an 
X-ray beam with a very small single crystal. 
The X-ray beam and the crystalline structure produce that can be 
recorded on film or measured by electronic device called X-ray 
counter. 
The most commonly used single crystal method is precession 
method. 
The modern approach to data acquisition by “single crystal 
diffractometer” . 
The most commonly used automated technique in structure analysis 
is four circle diffractometer. 10
APPLICATIONS 
Specific applications of single-crystal diffraction include: 
 For precise determination of a unit cell, including cell 
dimensions and positions of atoms within the lattice. 
 New mineral identification, crystal solution and 
refinement. 
 Determination of crystal-chemical vs. environmental 
control on mineral chemistry etc. 
11
STRENGTHS AND LIMITATIONS OF SINGLE-CRYSTAL 
X-RAY DIFFRACTION 
Strengths:- 
 Non-destructive. 
 Detailed crystal structure, including unit cell dimensions, bond-lengths, 
bond-angles and site-ordering information 
Limitations 
 Must have a single, stable sample, generally between 50—250 
microns in size. 
 Optically clear sample. 
 Data collection generally requires between 24 and 72 hours 12
X-RAY POWDER DIFFRACTION (XRD) 
X-ray powder diffraction (XRD) is a rapid analytical 
technique primarily used for phase identification of a 
crystalline material. 
13
FUNDAMENTAL PRINCIPLES OF X-RAY POWDER 
DIFFRACTION (XRD) 
The sample of powder diffrractometer analysis spread uniformly 
over a surface of a glass slide. The instrument is so constructed that 
the sample, when clamped in place, rotates in the path of a 
collimated X-ray beam, an X-ray detector, mounted on a arm 
rotates about it to pick up the diffracted X-ray signals. X-ray 
detector maintains the appropriate geometrical relationship to 
receive each diffraction separately. Once the diffractometer tracing 
is obtained and various diffraction peaks have been tabulated in 
sequence of decreasing interplanar spacing together with their 
relative intensities. 
14
SCHEMATIC ILLUSTRATION OF A SINGLE-CRYSTAL 
DIFFRACTOMETER 
15
APPLICATIONS 
X-ray powder diffraction is most widely used for:- 
 Characterization of crystalline materials 
 Identification of fine-grained minerals that are 
difficult to determine optically. 
 Measurement of sample purity. 
16
STRENGTHS AND LIMITATIONS OF X-RAY POWDER 
DIFFRACTION (XRD)? 
Strength :- 
 Powerful and rapid (< 20 min) technique for 
identification of an unknown mineral. 
 Minimal sample preparation is required. 
Limitation :- 
 Requires tenths of a gram of material which must be 
ground into a powder. 
 For mixed materials, detection limit is ~ 2% of sample 
 For unit cell determinations, indexing of patterns for 
non-isometric crystal systems is complicated. 
17
X-RAY FLUORESCENCE(XRF) 
An X-ray fluorescence (XRF) spectrometer is an x-ray 
instrument used for routine, relatively non-destructive 
chemical analyses of rocks, minerals, sediments and fluids. 
18
FUNDAMENTAL PRINCIPLES OF X-RAY FLUORESCENCE 
(XRF) 
An XRF spectrometer works if a sample is illuminated by 
an intense X-ray beam, known as the incident beam, some 
of the energy is scattered, but some is also absorbed within 
the sample in a manner that depends on its chemistry. 
When the primary X-ray beam illuminates the sample, 
excited sample in turn emits X-rays along a spectrum of 
wavelengths characteristic of the types of atoms present in 
the sample. Various types of detector are used to measure 
the intensity of the emitted beam. The intensity of the 
energy measured by these detectors is proportional to the 
abundance of the element in the sample. 19
SCHEMATIC CROSS SECTION OF XRF 
20
APPLICATION 
X-Ray fluorescence is used in a wide range of 
applications, including:- 
 Research in igneous, sedimentary, and 
metamorphic petrology 
 Mining (e.g., measuring the grade of ore) 
 Metallurgy (e.g., quality control) 
21
STRENGTHS AND LIMITATIONS…….. 
Strengths:- 
 Bulk chemical analyses of major elements (Si, Ti, Al, Fe, 
Mn, Mg, Ca, Na, K, P) in rock and sediment. 
Limitations:- 
 XRF analyses cannot distinguish variations among isotopes 
of an element. 
22
ELECTRON MICROPROBE ANALYSIS(EMPA) 
An electron probe micro-analyzer is a micro beam instrument used 
primarily for thein situ non-destructive chemical analysis of minute 
solid samples. EPMA is also informally called an electron microprobe, 
or just probe. It is fundamentally the same as an SEM, with the added 
capability of chemical analysis. 
23
FUNDAMENTAL PRINCIPLES OF ELECTRON PROBE 
MICRO-ANALYZER (EMPA) 
An electron microprobe operates under the principle that if a solid 
material is bombarded by an accelerated and focused electron 
beam, the incident electron beam has sufficient energy to liberate 
both matter and energy from the sample. These electron-sample 
interactions mainly liberate heat, but they also yield both 
derivative electrons and x-rays. These quantized x-rays are 
characteristic of the element. EPMA analysis is considered to be 
"non-destructive" so it is possible to re-analyze the same materials 
more than one time. 
24
APPLICATIONS OF EMPA 
 Quantitative EMPA analysis is the most commonly used 
method for chemical analysis of geological materials at 
small scale. 
 EPMA is also widely used for analysis of synthetic 
materials such as optical wafers, thin films, 
microcircuits, semi-conductors, and superconducting 
ceramics. 
25
STRENGTHS AND LIMITATIONS OF ELECTRON 
PROBE MICRO-ANALYZER (EPMA) 
Strength's:- 
 An electron probe is the primary tool for chemical analysis of solid 
materials at small spatial scales . 
 Spot chemical analyses can be obtained in situ , which allows the 
user to detect even small compositional variations within textural 
context or within chemically zoned materials. 
Limitations:- 
 Electron probe unable to detect the lightest elements (H, He and Li). 
 Probe analysis also cannot distinguish between the different 
valence states of Fe. 26
TRANSMISSION ELECTRON MICROSCOPY 
(TEM) 
Transmission electron microscopy (TEM) is 
a microscopy technique in which a beam of electrons is 
transmitted through an ultra-thin specimen, interacting 
with the specimen as it passes through. 
27
FUNDAMENTAL PRINCIPLES OF TEM 
A transmissions electron microscope consist of a finely focused 
electron beam that impinges on a very thin foil of an object. 
Transmission through the object, can be used to display electron 
diffraction patterns, and high resolution transmission electron 
microscope images. The thin foil is produced by ion bombardment 
or sputter-etching method for non conducting materials and 
conducting material is done by electrochemical methods. The thin 
foil is held n place with a sample holder centered in a electron 
beam. 
28
APPLICATIONS OF TEM 
Transmission electron microscope provide information 
about symmetry, distance among indexed diffraction 
provide information about unit cell size. This in turns 
allows for phase identification. 
29
STRENGTHS AND LIMITATIONS OF TEM 
Strength:- 
 The TEM technique is especially powerful in elucidating structural 
features that range in size from 100 to 10,000 Ao . 
 TEM studies allow for phase identification of extremely small 
particles or intergrowths of minerals. 
Limitation:- 
 TEMs are large and very expensive. 
 TEMs require special housing and maintenance. 
 Images are black and white. 30
FLAME ATOMIC ABSORPTION MICROSCOPY 
This analytical technique is commonly considered a “wet” analytical 
procedure because the original sample must be completely 
dissolved in a solution before it can be analysed. 
31
FUNDAMENTAL PRINCIPLES OF FAA 
The energy source in this technique is a light source. When the light 
energy is equivalent to the energy required to raise the atom from 
its low energy level to high energy levels, it is absorbed and causes 
excitation of atom. In order to determine element concentrations by 
this method, the atoms must be completely free of any of the 
bonding. The amount of light radiation that is measured by 
spectrometer is expressed by – 
A= log lo 
/ l, where A is absorbance, l0 is the 
incident light intensity and l the transmitted light intensity. 
The incident light intensity is supplied by hollow cathode 
lamp. The reduction in intensity is measured by the photomutiplier. 
32
STRENGTH AND LIMITATION OF FAA 
Strength:- 
 Greater sensitivity and detection limits than other methods. 
 Direct analysis of some types of liquid samples. 
 Very small sample size. 
Limitation:- 
 The method cannot be used to detect non-metallic elements. 
 It also suffers from ionic interference. 
33
SECONDARY ION MASS SPECTROMETRY(SIMS) 
Secondary ion mass spectrometry (SIMS) is a technique 
used to analyse the composition of solid surfaces 
and thin films by sputtering the surface of the specimen 
with a focused primary ion beam. 
34
FUNDAMENTAL PRINCIPLE OF SIMS 
The instruments employs a focused beam of ions that impinges on 
the solid surface of the sample. These atoms of the surface are 
extracted as secondary ions for analysis by mass spectrometer. In 
this method particles are ejected in ionized state. The instruments 
consists of a source of bombarding primary ions that are focused 
onto the specimen sample by lens systems. In most of the 
instruments used for mineralogical analysis the extracted 
secondary ions focused into a double focusing mass spectrometer 
which separates ions on the basis of energy and mass. 
35
SCHEMATIC DEPICTION OF SIMS SOURCE 
36
APPLICATIONS OF SIMS 
 It is commonly applied to the determination of the abundance and 
distribution of the rare earth material. 
 The SIMS technique also allows collecting isotropic composition 
for age dating and diffusion studies. 
 Instrument can be used to determine the concentration of any 
chemical element. 
37
STRENGTH AND LIMITATIONS OF SIMS 
Strength :- 
 This technique offers very high sensitive quantitative elemental 
analysis with detection limits in the parts per million to parts per 
billion range. 
 It can analyze most chemical elements from H to U. 
Limitations:- 
 Not all elements in all substrates (matrices) can be 
analysed quantitatively. 
 SIMS instrumentation tends be expensive. 38
39

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Analytical instrument

  • 1. ANALYTICAL INSTRUMENT Presented by :- Pranjit Sharmah 2013-2014 M.Sc Sem I
  • 2. ANALYTICAL INSTRUMENTS In mineral science, there are several analytical instruments used for various purpose, viz…  Scanning electron microscopy  X-ray diffraction  Transmission electron microscopy  X-ray fluorescence  Flame atomic absorption spectroscopy  Electron microprobe analysis  Secondary ion mass spectrometry  Atomic force microscopy 2
  • 3. SCANNING ELECTRON MICROSCOPY (SEM) The scanning electron microscope has an electron optical column in which a finely focused electron beam can be scanned over a specified area of the specimen. 3
  • 4. FUNDAMENTAL PRINCIPLES OF SCANNING ELECTRON MICROSCOPY (SEM) Accelerated electrons in an SEM carry significant amounts of kinetic energy, and this energy is dissipated as a variety of signals produced by electron-sample interactions when the incident electrons are decelerated in the solid sample. These signals include secondary electrons (that produce SEM images), backscattered electrons (BSE), diffracted backscattered electrons (EBSD) that are used to determine crystal structures and orientations of minerals. 4
  • 5. SCHEMATIC DRAWING OF FINELY FOCUS ELECTRON BEAM IMPINGING ON A MATERIAL SURFACE : 5
  • 6. APPLICATIONS OF SEM The SEM is routinely used to –  To generate high-resolution images of shapes of objects.  Identify phases based on qualitative chemical analysis and/or crystalline structure.  SEMs equipped with diffracted backscattered electron detectors can be used to examine microfabric and crystallographic orientation in many materials. 6
  • 7. STRENGTHS AND LIMITATIONS OF SEM Strength:-  Most SEM are comparatively easy to operate.  Modern SEMs generate data in digital format which are highly portable.  For many applications, data acquisition is rapid. Limitations-  . Samples must be solid and they must fit into the microscope chamber  An electrically conductive coating must be applied to electrically insulating samples for study in conventional SEM. 7
  • 8. X-RAY DIFFRACTION TECHNIQUES (XRD) The first application of an X-ray experiment to the study of crystalline material in 1912 by Max Von Lou. There are two different X-ray diffraction techniques – i) Single crystal techniques ii)X-ray powder diffraction techniques 8
  • 9. SINGLE CRYSTAL TECHNIQUES…… What is Single-crystal X-ray Diffraction??? Single-crystal X-ray Diffraction is a non-destructive analytical technique which provides detailed information about the internal lattice of crystalline substances, including unit cell dimensions, bond-lengths, bond-angles, and details of site-ordering. 9
  • 10. FUNDAMENTAL PRINCIPLES OF SINGLE-CRYSTAL X-RAY DIFFRACTION Single crystal X-ray diffraction concern with the interaction of an X-ray beam with a very small single crystal. The X-ray beam and the crystalline structure produce that can be recorded on film or measured by electronic device called X-ray counter. The most commonly used single crystal method is precession method. The modern approach to data acquisition by “single crystal diffractometer” . The most commonly used automated technique in structure analysis is four circle diffractometer. 10
  • 11. APPLICATIONS Specific applications of single-crystal diffraction include:  For precise determination of a unit cell, including cell dimensions and positions of atoms within the lattice.  New mineral identification, crystal solution and refinement.  Determination of crystal-chemical vs. environmental control on mineral chemistry etc. 11
  • 12. STRENGTHS AND LIMITATIONS OF SINGLE-CRYSTAL X-RAY DIFFRACTION Strengths:-  Non-destructive.  Detailed crystal structure, including unit cell dimensions, bond-lengths, bond-angles and site-ordering information Limitations  Must have a single, stable sample, generally between 50—250 microns in size.  Optically clear sample.  Data collection generally requires between 24 and 72 hours 12
  • 13. X-RAY POWDER DIFFRACTION (XRD) X-ray powder diffraction (XRD) is a rapid analytical technique primarily used for phase identification of a crystalline material. 13
  • 14. FUNDAMENTAL PRINCIPLES OF X-RAY POWDER DIFFRACTION (XRD) The sample of powder diffrractometer analysis spread uniformly over a surface of a glass slide. The instrument is so constructed that the sample, when clamped in place, rotates in the path of a collimated X-ray beam, an X-ray detector, mounted on a arm rotates about it to pick up the diffracted X-ray signals. X-ray detector maintains the appropriate geometrical relationship to receive each diffraction separately. Once the diffractometer tracing is obtained and various diffraction peaks have been tabulated in sequence of decreasing interplanar spacing together with their relative intensities. 14
  • 15. SCHEMATIC ILLUSTRATION OF A SINGLE-CRYSTAL DIFFRACTOMETER 15
  • 16. APPLICATIONS X-ray powder diffraction is most widely used for:-  Characterization of crystalline materials  Identification of fine-grained minerals that are difficult to determine optically.  Measurement of sample purity. 16
  • 17. STRENGTHS AND LIMITATIONS OF X-RAY POWDER DIFFRACTION (XRD)? Strength :-  Powerful and rapid (< 20 min) technique for identification of an unknown mineral.  Minimal sample preparation is required. Limitation :-  Requires tenths of a gram of material which must be ground into a powder.  For mixed materials, detection limit is ~ 2% of sample  For unit cell determinations, indexing of patterns for non-isometric crystal systems is complicated. 17
  • 18. X-RAY FLUORESCENCE(XRF) An X-ray fluorescence (XRF) spectrometer is an x-ray instrument used for routine, relatively non-destructive chemical analyses of rocks, minerals, sediments and fluids. 18
  • 19. FUNDAMENTAL PRINCIPLES OF X-RAY FLUORESCENCE (XRF) An XRF spectrometer works if a sample is illuminated by an intense X-ray beam, known as the incident beam, some of the energy is scattered, but some is also absorbed within the sample in a manner that depends on its chemistry. When the primary X-ray beam illuminates the sample, excited sample in turn emits X-rays along a spectrum of wavelengths characteristic of the types of atoms present in the sample. Various types of detector are used to measure the intensity of the emitted beam. The intensity of the energy measured by these detectors is proportional to the abundance of the element in the sample. 19
  • 21. APPLICATION X-Ray fluorescence is used in a wide range of applications, including:-  Research in igneous, sedimentary, and metamorphic petrology  Mining (e.g., measuring the grade of ore)  Metallurgy (e.g., quality control) 21
  • 22. STRENGTHS AND LIMITATIONS…….. Strengths:-  Bulk chemical analyses of major elements (Si, Ti, Al, Fe, Mn, Mg, Ca, Na, K, P) in rock and sediment. Limitations:-  XRF analyses cannot distinguish variations among isotopes of an element. 22
  • 23. ELECTRON MICROPROBE ANALYSIS(EMPA) An electron probe micro-analyzer is a micro beam instrument used primarily for thein situ non-destructive chemical analysis of minute solid samples. EPMA is also informally called an electron microprobe, or just probe. It is fundamentally the same as an SEM, with the added capability of chemical analysis. 23
  • 24. FUNDAMENTAL PRINCIPLES OF ELECTRON PROBE MICRO-ANALYZER (EMPA) An electron microprobe operates under the principle that if a solid material is bombarded by an accelerated and focused electron beam, the incident electron beam has sufficient energy to liberate both matter and energy from the sample. These electron-sample interactions mainly liberate heat, but they also yield both derivative electrons and x-rays. These quantized x-rays are characteristic of the element. EPMA analysis is considered to be "non-destructive" so it is possible to re-analyze the same materials more than one time. 24
  • 25. APPLICATIONS OF EMPA  Quantitative EMPA analysis is the most commonly used method for chemical analysis of geological materials at small scale.  EPMA is also widely used for analysis of synthetic materials such as optical wafers, thin films, microcircuits, semi-conductors, and superconducting ceramics. 25
  • 26. STRENGTHS AND LIMITATIONS OF ELECTRON PROBE MICRO-ANALYZER (EPMA) Strength's:-  An electron probe is the primary tool for chemical analysis of solid materials at small spatial scales .  Spot chemical analyses can be obtained in situ , which allows the user to detect even small compositional variations within textural context or within chemically zoned materials. Limitations:-  Electron probe unable to detect the lightest elements (H, He and Li).  Probe analysis also cannot distinguish between the different valence states of Fe. 26
  • 27. TRANSMISSION ELECTRON MICROSCOPY (TEM) Transmission electron microscopy (TEM) is a microscopy technique in which a beam of electrons is transmitted through an ultra-thin specimen, interacting with the specimen as it passes through. 27
  • 28. FUNDAMENTAL PRINCIPLES OF TEM A transmissions electron microscope consist of a finely focused electron beam that impinges on a very thin foil of an object. Transmission through the object, can be used to display electron diffraction patterns, and high resolution transmission electron microscope images. The thin foil is produced by ion bombardment or sputter-etching method for non conducting materials and conducting material is done by electrochemical methods. The thin foil is held n place with a sample holder centered in a electron beam. 28
  • 29. APPLICATIONS OF TEM Transmission electron microscope provide information about symmetry, distance among indexed diffraction provide information about unit cell size. This in turns allows for phase identification. 29
  • 30. STRENGTHS AND LIMITATIONS OF TEM Strength:-  The TEM technique is especially powerful in elucidating structural features that range in size from 100 to 10,000 Ao .  TEM studies allow for phase identification of extremely small particles or intergrowths of minerals. Limitation:-  TEMs are large and very expensive.  TEMs require special housing and maintenance.  Images are black and white. 30
  • 31. FLAME ATOMIC ABSORPTION MICROSCOPY This analytical technique is commonly considered a “wet” analytical procedure because the original sample must be completely dissolved in a solution before it can be analysed. 31
  • 32. FUNDAMENTAL PRINCIPLES OF FAA The energy source in this technique is a light source. When the light energy is equivalent to the energy required to raise the atom from its low energy level to high energy levels, it is absorbed and causes excitation of atom. In order to determine element concentrations by this method, the atoms must be completely free of any of the bonding. The amount of light radiation that is measured by spectrometer is expressed by – A= log lo / l, where A is absorbance, l0 is the incident light intensity and l the transmitted light intensity. The incident light intensity is supplied by hollow cathode lamp. The reduction in intensity is measured by the photomutiplier. 32
  • 33. STRENGTH AND LIMITATION OF FAA Strength:-  Greater sensitivity and detection limits than other methods.  Direct analysis of some types of liquid samples.  Very small sample size. Limitation:-  The method cannot be used to detect non-metallic elements.  It also suffers from ionic interference. 33
  • 34. SECONDARY ION MASS SPECTROMETRY(SIMS) Secondary ion mass spectrometry (SIMS) is a technique used to analyse the composition of solid surfaces and thin films by sputtering the surface of the specimen with a focused primary ion beam. 34
  • 35. FUNDAMENTAL PRINCIPLE OF SIMS The instruments employs a focused beam of ions that impinges on the solid surface of the sample. These atoms of the surface are extracted as secondary ions for analysis by mass spectrometer. In this method particles are ejected in ionized state. The instruments consists of a source of bombarding primary ions that are focused onto the specimen sample by lens systems. In most of the instruments used for mineralogical analysis the extracted secondary ions focused into a double focusing mass spectrometer which separates ions on the basis of energy and mass. 35
  • 36. SCHEMATIC DEPICTION OF SIMS SOURCE 36
  • 37. APPLICATIONS OF SIMS  It is commonly applied to the determination of the abundance and distribution of the rare earth material.  The SIMS technique also allows collecting isotropic composition for age dating and diffusion studies.  Instrument can be used to determine the concentration of any chemical element. 37
  • 38. STRENGTH AND LIMITATIONS OF SIMS Strength :-  This technique offers very high sensitive quantitative elemental analysis with detection limits in the parts per million to parts per billion range.  It can analyze most chemical elements from H to U. Limitations:-  Not all elements in all substrates (matrices) can be analysed quantitatively.  SIMS instrumentation tends be expensive. 38
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