Description about important mass analysers Quadrupole and TOF: Principle, Construction and Working, Advantages and Disadvantages and their Applications.
PRINCIPLES of FT-NMR & 13C NMR
Fourier Transform
FOURIER TRANSFORM NMR SPECTROSCOPY
THEORY OF FT-NMR
13C NMR SPECTROSCOPY
Principle
Why C13-NMR is required though we have H1-NMR?
CHARACTERISTIC FEATURES OF 13 C NMR
Chemical Shifts
NUCLEAR OVERHAUSER ENHANCEMENT
Short-Comings of 13C-NMR Spectra
spectrofluorometer is the instrument for recording fluorescence emission and absorption spectra When a beam of light is incident on certain substances they emit visible light or radiations. This is known as fluorescence. Fluorescence starts immediately after the absorption of light and stops as soon as the incident light is cut off. The substances showing this phenomenon are known as flourescent substances.
PRINCIPLES of FT-NMR & 13C NMR
Fourier Transform
FOURIER TRANSFORM NMR SPECTROSCOPY
THEORY OF FT-NMR
13C NMR SPECTROSCOPY
Principle
Why C13-NMR is required though we have H1-NMR?
CHARACTERISTIC FEATURES OF 13 C NMR
Chemical Shifts
NUCLEAR OVERHAUSER ENHANCEMENT
Short-Comings of 13C-NMR Spectra
spectrofluorometer is the instrument for recording fluorescence emission and absorption spectra When a beam of light is incident on certain substances they emit visible light or radiations. This is known as fluorescence. Fluorescence starts immediately after the absorption of light and stops as soon as the incident light is cut off. The substances showing this phenomenon are known as flourescent substances.
Introduction
working principle
fragmentation process
general rules for fragmentation
general modes of fragmentation
metastable ions
isotopic peaks
applications
Types of crystals & Application of x raykajal pradhan
some basic information:-
A crystal lattice is a 3-D arrangement of unit cells.
Unit cell is the smallest unit of a crystal, By stacking identical unit cells, the entire lattice can be constructed
A crystal’s unit cell dimensions are defined by six numbers, the lengths of the 3 axes, a, b, and c, and the three interaxial angles, α, β and γ.
If a unit cell has the same type of atom at the corners of the unit cell but not also in the middle of the faces nor in the centre of the cell, it is called primitive and given by symbol P
7 types of crystal system details
14 bravis lattice
APPLICATION X-RAY CRYSTALLOGRAPHY
1. Structure of crystals
2. Polymer characterisation
3. State of anneal in metals
4. Particle size determination
a) Spot counting method
b) Broadening of diffraction lines
c) Low-angle scattering
5.Applications of diffraction methods to complexes
a) Determination of cis- trans isomerism
b) Determination of linkage isomerism
6.Miscellaneous applications
a type of an analyzer used in mass spectrometer. separates the ions based on mass to charge ratios. useful for the detection of ions present in the sample
Analyser of Quadrupole and time of flight.Mass Analysers.
Summary of Mass Analyser.
Quadrupole mass spectrometer.
Factors Affecting Function Of Quadrupole.
Principal, Construction & Working.
Linear Time of flight mass spectrometer.
Time Of Flight Mass Spectrometry, Need For Variant Type Of Time of Flight Analyser.
Variant Of Linear TOF Analyser.
Ion mirror / ion reflectron / reflectron. Time-lag focussing.
Advantages, Disadvantage, Application.
Introduction
working principle
fragmentation process
general rules for fragmentation
general modes of fragmentation
metastable ions
isotopic peaks
applications
Types of crystals & Application of x raykajal pradhan
some basic information:-
A crystal lattice is a 3-D arrangement of unit cells.
Unit cell is the smallest unit of a crystal, By stacking identical unit cells, the entire lattice can be constructed
A crystal’s unit cell dimensions are defined by six numbers, the lengths of the 3 axes, a, b, and c, and the three interaxial angles, α, β and γ.
If a unit cell has the same type of atom at the corners of the unit cell but not also in the middle of the faces nor in the centre of the cell, it is called primitive and given by symbol P
7 types of crystal system details
14 bravis lattice
APPLICATION X-RAY CRYSTALLOGRAPHY
1. Structure of crystals
2. Polymer characterisation
3. State of anneal in metals
4. Particle size determination
a) Spot counting method
b) Broadening of diffraction lines
c) Low-angle scattering
5.Applications of diffraction methods to complexes
a) Determination of cis- trans isomerism
b) Determination of linkage isomerism
6.Miscellaneous applications
a type of an analyzer used in mass spectrometer. separates the ions based on mass to charge ratios. useful for the detection of ions present in the sample
Analyser of Quadrupole and time of flight.Mass Analysers.
Summary of Mass Analyser.
Quadrupole mass spectrometer.
Factors Affecting Function Of Quadrupole.
Principal, Construction & Working.
Linear Time of flight mass spectrometer.
Time Of Flight Mass Spectrometry, Need For Variant Type Of Time of Flight Analyser.
Variant Of Linear TOF Analyser.
Ion mirror / ion reflectron / reflectron. Time-lag focussing.
Advantages, Disadvantage, Application.
mass spectrometry for pesticides residue analysis- L4sherif Taha
This is the fourth and the last lecture in series of lectures on mass spectrometry for pesticides residue analysis. this lecture present the commonly used mass to charge analyzer for pesticides residue analysis.
Localising Charged Particles by Electric and Magnetic Fields
the trapping of charged particles
Prepared By : Mohamed Fayed Mohamed Ali
Email : M10513fayed@gmail.com
IMS is a sensitive analytical technique that is used for detection, identification and monitoring of chemicals, mainly explosives, highly toxic gases and drug interdiction. Thus making it a powerful tool to counter terrorism.
A brief information about the SCOP protein database used in bioinformatics.
The Structural Classification of Proteins (SCOP) database is a comprehensive and authoritative resource for the structural and evolutionary relationships of proteins. It provides a detailed and curated classification of protein structures, grouping them into families, superfamilies, and folds based on their structural and sequence similarities.
Observation of Io’s Resurfacing via Plume Deposition Using Ground-based Adapt...Sérgio Sacani
Since volcanic activity was first discovered on Io from Voyager images in 1979, changes
on Io’s surface have been monitored from both spacecraft and ground-based telescopes.
Here, we present the highest spatial resolution images of Io ever obtained from a groundbased telescope. These images, acquired by the SHARK-VIS instrument on the Large
Binocular Telescope, show evidence of a major resurfacing event on Io’s trailing hemisphere. When compared to the most recent spacecraft images, the SHARK-VIS images
show that a plume deposit from a powerful eruption at Pillan Patera has covered part
of the long-lived Pele plume deposit. Although this type of resurfacing event may be common on Io, few have been detected due to the rarity of spacecraft visits and the previously low spatial resolution available from Earth-based telescopes. The SHARK-VIS instrument ushers in a new era of high resolution imaging of Io’s surface using adaptive
optics at visible wavelengths.
Richard's entangled aventures in wonderlandRichard Gill
Since the loophole-free Bell experiments of 2020 and the Nobel prizes in physics of 2022, critics of Bell's work have retreated to the fortress of super-determinism. Now, super-determinism is a derogatory word - it just means "determinism". Palmer, Hance and Hossenfelder argue that quantum mechanics and determinism are not incompatible, using a sophisticated mathematical construction based on a subtle thinning of allowed states and measurements in quantum mechanics, such that what is left appears to make Bell's argument fail, without altering the empirical predictions of quantum mechanics. I think however that it is a smoke screen, and the slogan "lost in math" comes to my mind. I will discuss some other recent disproofs of Bell's theorem using the language of causality based on causal graphs. Causal thinking is also central to law and justice. I will mention surprising connections to my work on serial killer nurse cases, in particular the Dutch case of Lucia de Berk and the current UK case of Lucy Letby.
Multi-source connectivity as the driver of solar wind variability in the heli...Sérgio Sacani
The ambient solar wind that flls the heliosphere originates from multiple
sources in the solar corona and is highly structured. It is often described
as high-speed, relatively homogeneous, plasma streams from coronal
holes and slow-speed, highly variable, streams whose source regions are
under debate. A key goal of ESA/NASA’s Solar Orbiter mission is to identify
solar wind sources and understand what drives the complexity seen in the
heliosphere. By combining magnetic feld modelling and spectroscopic
techniques with high-resolution observations and measurements, we show
that the solar wind variability detected in situ by Solar Orbiter in March
2022 is driven by spatio-temporal changes in the magnetic connectivity to
multiple sources in the solar atmosphere. The magnetic feld footpoints
connected to the spacecraft moved from the boundaries of a coronal hole
to one active region (12961) and then across to another region (12957). This
is refected in the in situ measurements, which show the transition from fast
to highly Alfvénic then to slow solar wind that is disrupted by the arrival of
a coronal mass ejection. Our results describe solar wind variability at 0.5 au
but are applicable to near-Earth observatories.
Richard's aventures in two entangled wonderlandsRichard Gill
Since the loophole-free Bell experiments of 2020 and the Nobel prizes in physics of 2022, critics of Bell's work have retreated to the fortress of super-determinism. Now, super-determinism is a derogatory word - it just means "determinism". Palmer, Hance and Hossenfelder argue that quantum mechanics and determinism are not incompatible, using a sophisticated mathematical construction based on a subtle thinning of allowed states and measurements in quantum mechanics, such that what is left appears to make Bell's argument fail, without altering the empirical predictions of quantum mechanics. I think however that it is a smoke screen, and the slogan "lost in math" comes to my mind. I will discuss some other recent disproofs of Bell's theorem using the language of causality based on causal graphs. Causal thinking is also central to law and justice. I will mention surprising connections to my work on serial killer nurse cases, in particular the Dutch case of Lucia de Berk and the current UK case of Lucy Letby.
Comparative structure of adrenal gland in vertebrates
Quadrupole and Time of Flight Mass analysers.
1. Topic: Quadrupole and Time Of Flight mass
analyzers
Presented by:
Ramesh S. Gagan S.
Dept. of Pharmacology. Dept. of Pharmaceutical
Chemistry
Government college of Pharmacy, Bengaluru.
Mass spectroscopy
3. INTRODUCTION
Mass spectrometry is an analytical chemistry technique that helps
identifying the amount and type of chemicals present in a sample
by measuring the mass-to-charge ratio and abundance of gas
phase ions.
5. MASS ANALYSERS
Mass analysers are called heart of mass
spectrometer .
These are the instruments which separates
the mixtures of ions that are generated
during the ionization step by m/z in order to
obtain a spectrum.
6. Types of mass analysers
Magnet sector mass spectrometer.
Quadrupole mass spectrometer.
Ion trap mass spectrometer.
Time of flight mass spectrometer.
Fourier transform mass spectrometer.
7. Table : Summary of mass analysers.
MASSS MASS RANGE RESOLUTION SENSITIVITY
MAGNETIC
SECTOR
1-15,000 m/z 0.0001 Low
QUADRUPOLE 1-5000 m/z Unit High
ION TRAP 1-5000 m/z Unit High
TIME OF FLIGHT Unlimited 0.0001 High
FOURIER
TRANSFORM
Up to 70 k Da 0.0001 High
8. QUADRUPOLE MASS SPECTROMETER
Quadrupole mass analysers concept was first reported
by Paul and Steinwedel in the 1950s.
Quadrupole consists of four rods which are arranged
parallelly.
Rods opposite to one another are electrically
connected.
Ions are separated based on m/z at a particular DC and
Radiofrequency voltage.
9. PRINCIPLE:
. IONS FROM THE IONS SOURCE
QUADRUPOLE ANALYSER WITH A
CONSTANT DC AND RF VOLTAGE
AT GIVEN COMBINATION OF DC AND RF
VOLTAGE
IONS WITH CERTAIN m/z
VALUES REACH THE
DETECTOR
IONS WITH DIFFERENT m/z
VALUES TRAVEL UNSTABLE
PATH
11. It consists of four electrically conducting parallel rods.
One diagonally opposite pair of rods is held at +Udc
volts and the other pair at –Udc volts.
A radiofrequency oscillator supplies +Vcosωt to the first
pair and –Vcosωt to the second pair.
Ions enter to the quadrupole through a circular aperture.
12. WORKING:
When ions enter into the quadrupole ions get deflected by
the positive and negative electrodes and ion with a certain
m/z value will reach the detector.
This can be explained by taking individual pair of rods.
17. FACTORS AFFECTING FUNCTION OF QUADRUPOLE:
Focussing slits
Rod length
Rod diameter
Increased rf frequency
18. ADVANTAGES:
High sensitivity.
They can operate close to ground potential.
Ideal for interfacing to LC system and for atmospheric
pressure ionization (API) techniques such as electrospray.
Well suited for the negative ions ,since the analyser does not
discriminate between the polarity of the ions.
Economic, robust and scanning is very fast.
19. DISADVANTAGES:
Quadrupole is generally inferior to magnetic sector
analyser with respect to resolution and mass range.
Peak height variable as a function of mass.
Not well suited for pulsed ionization methods.
20. APPLICATIONS:
In liquid chromatography-Mass spectrometry.
In Gas chromatography-Mass spectrometry.
To measure the relative amounts of different gases in
a mixture.
Proteomics.
21. TIME OF FLIGHT MASS SPECTROMETR
Introduction:
Stephens first described the concept of time of flight in 1946.
As the name implies, time of flight mass spectrometer
separates ions and measure their m/z based on the time they
take to pass ( “fly” ) from the ion source to the detector.
22. PRINCIPLE:
Ions with different masses and same kinetic energy
travel when accelerated and the ions with smaller
masses (less m/z value)reaches early to the detector
than the bigger masses .
23. THEORY:
The kinetic energy of ions of mass (m), charge (z) and accelerating potential (V) is given by
KE = zV = ½ mv2 (1)
Where (v) is velocity of the ions which is given by
v = l/t
where, l = length of the tube
t = time taken by the ions to pass the length of the tube
Therefore, equation 1 becomes
zV = ½ ml2/t2
m/z = 2Vt2/l2
2V/l2 = k (constant)
therefore, m/z = kt2
m/z α t2
25. Working:
.
IONS FROM THE ION
SOURCE
TOF
ACCELERATION OF
IONS
ACQUIRES
DIFFERENT
VELOCITIES
SPATIAL
SEPARATION OF
IONS
IONS WITH HIGHER
VELOCITY REACH
THE DETECTOR
FIRST
26. VARIANTS OF LINEAR TOF ANALYSER
1.Ion mirror / ion reflectron / reflectron.
2.Time-lag focussing
27. NEED FOR VARIANT TYPE OF TOF ANALYSER
Ions with very similar m/z ratio may have relatively poor
mass resolutions .
This is due to the spatial distribution in the ion source and
their proximity to the applied electric field, not all the ions
receive the same kinetic energy.
This leads to components in mixtures being unresolved
from one another and large errors in molecular weight
measurements.
28.
29. ION MIRROR / ION REFLECTRON / REFLECTRON
Construction and working:
30. .
It consists of stack of donut shaped lens connected by a
series of resistors across which voltage is applied.
These lenses repell the ions entered.
These ions are reflected down at second flight tube to a
second detector.
Mass resolution is achieved as ions of different kinetic
energies penetrate the mirror to differing degrees.
31. .
For example consider two ions of the same m/z ratio that
have slightly different kinetic energies.
32. TIME-LAG FOCUSSING / PULSED ION EXTRACTION /
DELAYED EXTRACTION
Construction and working:
33. .
In time-lag focusing TOF applying accelerating potential is
delayed.
Ions from the ion source will have some kinetic energy and
moves with different velocities
Application of potential gives more energy to the ions which
are away from the detector than closer to it.
The amplitude is adjusted in such a way that all the ions
reach the detector at the same time.
34. ADVANTAGES OF TOF MASS ANALYSER
Mass range is unlimited.
Excellent sensitivity due to lack of resolving slits.
35. DISADVANTAGES OF TOF MASS ANALYSER
Limited use in case of pulsed ionization techniques.
Mass resolution is usually less than 20000.
Fast electronics are necessary for adequate resolution.
36. APPLICATION OF TOF MASS ANALYSER
Due to its fast scanning capability it is increasingly being
used in LC-MS instrumentation.
Generally it is used in case of fast analysis or in high
chromatographic resolution techniques.
37. REFERENCE:
1. Spectrometric identification of organic compounds by Robert M Silverstein
and Francis X Webster,pg. no. 10-12.
2. Instrumental methods of analysis ,7th edition by Willard Merrit Dean Settle,
pg. no. 480-483.
3. Instrumental analysis by Skoog, Holler, Crouch, India edition pg. no. 627.
4. Mass spectroscopy, A foundation course by K.Downard, pg. no. 40-43.
5. Organic spectroscopy, William Kemp, Third edition, pg. no.286-288
6. An introduction to Quadrupole Time of flight mass spectroscopy ,Journal of
mass spectroscopy, Willey analytical science.
