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MT 322: Instrumental Analysis

Course instructor:
Dr. Praveen Sathiyamoorthi
praveen.met@iitbhu.ac.in

Lecture 18
September 27, 2022

9/27/2022 MT322; Dr. Praveen Sathiyamoorthi; IIT BHU 31


Last class recap

o FT optical spectrometer
o Multiplex instrument
o Time-domain spectroscopy
o Interferometer
𝟐𝒗𝒎
o𝒇 = 𝒗
c
1
o∆𝑣ҧ = 𝑣ҧ1 − 𝑣ҧ2 =
𝛿

9/27/2022 MT322; Dr. Praveen Sathiyamoorthi; IIT BHU 32


Fourier transform spectrometer
Advantages 299.85 nm 300.75 nm

o Throughput or Jaquinot advantage: Emission spectrum for a steel


o Few optical elements, high intensity at the detector, greater signal-
to-noise ratio

o High resolving power & wavelength reproducibility:


o Analysis of complex spectra

o Fellget or multiplex advantage:


Source: Principles of instrumental analysis, 7th edition, Douglas A.
o Significant decrease in time Skoog, F. James Holler, Stanley R. Crouch

o signal averaging ∝ 𝑛 ; Improvement in signal-to-noise ratio

Not widely used for UV/Visible – multiplex disadvantage

9/27/2022 MT322; Dr. Praveen Sathiyamoorthi; IIT BHU 33


Spectroscopy techniques
o Atomic absorption spectrometry
o Atomic emission spectroscopy
o FTIR spectroscopy
o Raman spectroscopy
o X-ray absorption spectroscopy
o X-ray fluorescence spectroscopy
9/27/2022 MT322; Dr. Praveen Sathiyamoorthi; IIT BHU 34
Atomic absorption spectrometry (AAS)
Elemental analysis technique – quantitative information
Principal advantages
o Independent of the chemical form of the element in the sample

o Determine low concentrations of most metal elements- ppb or ppm

o Given analyte can be determined in the presence of other elements – if other


elements do not interfere with absorption of analyte wavelength

Principal disadvantages
o No information on the chemical form of the analyte

o Only one element at a time-limited use of qualitative analysis.


9/27/2022 MT322; Dr. Praveen Sathiyamoorthi; IIT BHU 35
Atomic absorption spectrometry (AAS)
Basis

o Absorption of discrete wavelengths of light by the analyte


o Analyte must be converted into free atoms.
o Analyte is solution forms, converted to free atoms in the gas
phase – Atomizer
o Atomization: the process of converting an analyte to free atoms

9/27/2022 MT322; Dr. Praveen Sathiyamoorthi; IIT BHU 36


Absorption of radiant energy by atoms
Based on the absorption of radiant energy
o Atoms go from a lower energy state to a higher energy state

o No vibrational or rotational energy states

o Atomic absorption spectra – very narrow absorption lines

Electronic state
o Ground state – lowest energy electronic configuration – most
stable

o Excited state - ∆E of exactly the right magnitude – less stable

o ∆𝐸 = ℎ𝜈 = ℎ𝑐/𝜆
9/27/2022 MT322; Dr. Praveen Sathiyamoorthi; IIT BHU 37
Absorption of radiant energy by atoms
Electronic energy levels

o Resonance lines – absorption lines due to


transition from the ground state to the high
energy state.

o Only valence electrons are excited in the


AAS Source: Undergraduate instrumental analysis,7th
edition, Robinson, James W, Eileen M. Skelly Frame,
George M. Frame, M. Eileen, and Frame Skelly.
o UV/Visible radiation

9/27/2022 MT322; Dr. Praveen Sathiyamoorthi; IIT BHU 38


Absorption of radiant energy by atoms
Electronic energy levels
o Electrons can move from one excited state
to a higher excited state

o AAS – most absorptions arise from the


ground state
o amount of radiation absorbed is greatest
for absorptions from the ground state Source: Undergraduate instrumental analysis,7th
edition, Robinson, James W, Eileen M. Skelly Frame,
George M. Frame, M. Eileen, and Frame Skelly.

o restricts the number of absorption lines


9/27/2022 MT322; Dr. Praveen Sathiyamoorthi; IIT BHU 39
Absorption of radiant energy by atoms
Grotrian diagram Sodium

o Number of energy levels – quantum


theory

o Actual energy differences – atomic


spectra
1s22s22p63s1
o Energy vs energy levels
Source: Undergraduate instrumental analysis,7th
edition, Robinson, James W, Eileen M. Skelly Frame,
George M. Frame, M. Eileen, and Frame Skelly.

9/27/2022 MT322; Dr. Praveen Sathiyamoorthi; IIT BHU 40

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