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
Nuclear magnetic resonance (NMR) spectroscopyVK VIKRAM VARMA
SPECTROSCOPY
NMR SPECTROSCOPY
HISTORY
THEORY
PRINCIPLE
INSTRUMENTATION
SOLVENTS USED IN NMR(PROTON NMR)
CHEMICAL SHIFT
FACTORS AFFECTING CHEMICAL SHIFT
RELAXATION PROCESS
SPIN-SPIN COUPLING
푛+1 RULE
NMR SIGNALS IN VARIOUS COMPOUNDS
COUPLING CONSTANT
NUCLEAR MAGNETIC DOUBLE RESONANCE/ SPIN DECOUPLING
FT-NMR
ADVANTAGES & DISADVANTAGES
APPLICATIONS
REFERENCE
Quadrupole and Time of Flight Mass analysers.Gagangowda58
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
Nuclear magnetic resonance (NMR) spectroscopyVK VIKRAM VARMA
SPECTROSCOPY
NMR SPECTROSCOPY
HISTORY
THEORY
PRINCIPLE
INSTRUMENTATION
SOLVENTS USED IN NMR(PROTON NMR)
CHEMICAL SHIFT
FACTORS AFFECTING CHEMICAL SHIFT
RELAXATION PROCESS
SPIN-SPIN COUPLING
푛+1 RULE
NMR SIGNALS IN VARIOUS COMPOUNDS
COUPLING CONSTANT
NUCLEAR MAGNETIC DOUBLE RESONANCE/ SPIN DECOUPLING
FT-NMR
ADVANTAGES & DISADVANTAGES
APPLICATIONS
REFERENCE
Quadrupole and Time of Flight Mass analysers.Gagangowda58
Description about important mass analysers Quadrupole and TOF: Principle, Construction and Working, Advantages and Disadvantages and their Applications.
It would be use full to All Needy People. It involve information about NMR Spectroscopy ( a spectroscopic techniques), factors influencing , proton NMR and their applications of NMR as well as Nuclear magnetic imaging.
For UG/PG students of All Engineering (B Tech/B E) branches, Chemistry, Food Technology, Biochemistry, Biotechnology.
The video lecture link of the presentation is
https://www.youtube.com/watch?v=bFPhvnW8T18&t=99s
CHAPTER 1 SEMESTER V PREVENTIVE-PEDIATRICS.pdfSachin Sharma
This content provides an overview of preventive pediatrics. It defines preventive pediatrics as preventing disease and promoting children's physical, mental, and social well-being to achieve positive health. It discusses antenatal, postnatal, and social preventive pediatrics. It also covers various child health programs like immunization, breastfeeding, ICDS, and the roles of organizations like WHO, UNICEF, and nurses in preventive pediatrics.
How many patients does case series should have In comparison to case reports.pdfpubrica101
Pubrica’s team of researchers and writers create scientific and medical research articles, which may be important resources for authors and practitioners. Pubrica medical writers assist you in creating and revising the introduction by alerting the reader to gaps in the chosen study subject. Our professionals understand the order in which the hypothesis topic is followed by the broad subject, the issue, and the backdrop.
https://pubrica.com/academy/case-study-or-series/how-many-patients-does-case-series-should-have-in-comparison-to-case-reports/
Navigating the Health Insurance Market_ Understanding Trends and Options.pdfEnterprise Wired
From navigating policy options to staying informed about industry trends, this comprehensive guide explores everything you need to know about the health insurance market.
Antibiotic Stewardship by Anushri Srivastava.pptxAnushriSrivastav
Stewardship is the act of taking good care of something.
Antimicrobial stewardship is a coordinated program that promotes the appropriate use of antimicrobials (including antibiotics), improves patient outcomes, reduces microbial resistance, and decreases the spread of infections caused by multidrug-resistant organisms.
WHO launched the Global Antimicrobial Resistance and Use Surveillance System (GLASS) in 2015 to fill knowledge gaps and inform strategies at all levels.
ACCORDING TO apic.org,
Antimicrobial stewardship is a coordinated program that promotes the appropriate use of antimicrobials (including antibiotics), improves patient outcomes, reduces microbial resistance, and decreases the spread of infections caused by multidrug-resistant organisms.
ACCORDING TO pewtrusts.org,
Antibiotic stewardship refers to efforts in doctors’ offices, hospitals, long term care facilities, and other health care settings to ensure that antibiotics are used only when necessary and appropriate
According to WHO,
Antimicrobial stewardship is a systematic approach to educate and support health care professionals to follow evidence-based guidelines for prescribing and administering antimicrobials
In 1996, John McGowan and Dale Gerding first applied the term antimicrobial stewardship, where they suggested a causal association between antimicrobial agent use and resistance. They also focused on the urgency of large-scale controlled trials of antimicrobial-use regulation employing sophisticated epidemiologic methods, molecular typing, and precise resistance mechanism analysis.
Antimicrobial Stewardship(AMS) refers to the optimal selection, dosing, and duration of antimicrobial treatment resulting in the best clinical outcome with minimal side effects to the patients and minimal impact on subsequent resistance.
According to the 2019 report, in the US, more than 2.8 million antibiotic-resistant infections occur each year, and more than 35000 people die. In addition to this, it also mentioned that 223,900 cases of Clostridoides difficile occurred in 2017, of which 12800 people died. The report did not include viruses or parasites
VISION
Being proactive
Supporting optimal animal and human health
Exploring ways to reduce overall use of antimicrobials
Using the drugs that prevent and treat disease by killing microscopic organisms in a responsible way
GOAL
to prevent the generation and spread of antimicrobial resistance (AMR). Doing so will preserve the effectiveness of these drugs in animals and humans for years to come.
being to preserve human and animal health and the effectiveness of antimicrobial medications.
to implement a multidisciplinary approach in assembling a stewardship team to include an infectious disease physician, a clinical pharmacist with infectious diseases training, infection preventionist, and a close collaboration with the staff in the clinical microbiology laboratory
to prevent antimicrobial overuse, misuse and abuse.
to minimize the developme
We understand the unique challenges pickleball players face and are committed to helping you stay healthy and active. In this presentation, we’ll explore the three most common pickleball injuries and provide strategies for prevention and treatment.
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QA Paediatric dentistry department, Hospital Melaka 2020Azreen Aj
QA study - To improve the 6th monthly recall rate post-comprehensive dental treatment under general anaesthesia in paediatric dentistry department, Hospital Melaka
Global launch of the Healthy Ageing and Prevention Index 2nd wave – alongside...ILC- UK
The Healthy Ageing and Prevention Index is an online tool created by ILC that ranks countries on six metrics including, life span, health span, work span, income, environmental performance, and happiness. The Index helps us understand how well countries have adapted to longevity and inform decision makers on what must be done to maximise the economic benefits that comes with living well for longer.
Alongside the 77th World Health Assembly in Geneva on 28 May 2024, we launched the second version of our Index, allowing us to track progress and give new insights into what needs to be done to keep populations healthier for longer.
The speakers included:
Professor Orazio Schillaci, Minister of Health, Italy
Dr Hans Groth, Chairman of the Board, World Demographic & Ageing Forum
Professor Ilona Kickbusch, Founder and Chair, Global Health Centre, Geneva Graduate Institute and co-chair, World Health Summit Council
Dr Natasha Azzopardi Muscat, Director, Country Health Policies and Systems Division, World Health Organisation EURO
Dr Marta Lomazzi, Executive Manager, World Federation of Public Health Associations
Dr Shyam Bishen, Head, Centre for Health and Healthcare and Member of the Executive Committee, World Economic Forum
Dr Karin Tegmark Wisell, Director General, Public Health Agency of Sweden
CHAPTER 1 SEMESTER V - ROLE OF PEADIATRIC NURSE.pdfSachin Sharma
Pediatric nurses play a vital role in the health and well-being of children. Their responsibilities are wide-ranging, and their objectives can be categorized into several key areas:
1. Direct Patient Care:
Objective: Provide comprehensive and compassionate care to infants, children, and adolescents in various healthcare settings (hospitals, clinics, etc.).
This includes tasks like:
Monitoring vital signs and physical condition.
Administering medications and treatments.
Performing procedures as directed by doctors.
Assisting with daily living activities (bathing, feeding).
Providing emotional support and pain management.
2. Health Promotion and Education:
Objective: Promote healthy behaviors and educate children, families, and communities about preventive healthcare.
This includes tasks like:
Administering vaccinations.
Providing education on nutrition, hygiene, and development.
Offering breastfeeding and childbirth support.
Counseling families on safety and injury prevention.
3. Collaboration and Advocacy:
Objective: Collaborate effectively with doctors, social workers, therapists, and other healthcare professionals to ensure coordinated care for children.
Objective: Advocate for the rights and best interests of their patients, especially when children cannot speak for themselves.
This includes tasks like:
Communicating effectively with healthcare teams.
Identifying and addressing potential risks to child welfare.
Educating families about their child's condition and treatment options.
4. Professional Development and Research:
Objective: Stay up-to-date on the latest advancements in pediatric healthcare through continuing education and research.
Objective: Contribute to improving the quality of care for children by participating in research initiatives.
This includes tasks like:
Attending workshops and conferences on pediatric nursing.
Participating in clinical trials related to child health.
Implementing evidence-based practices into their daily routines.
By fulfilling these objectives, pediatric nurses play a crucial role in ensuring the optimal health and well-being of children throughout all stages of their development.
Defecation
Normal defecation begins with movement in the left colon, moving stool toward the anus. When stool reaches the rectum, the distention causes relaxation of the internal sphincter and an awareness of the need to defecate. At the time of defecation, the external sphincter relaxes, and abdominal muscles contract, increasing intrarectal pressure and forcing the stool out
The Valsalva maneuver exerts pressure to expel faeces through a voluntary contraction of the abdominal muscles while maintaining forced expiration against a closed airway. Patients with cardiovascular disease, glaucoma, increased intracranial pressure, or a new surgical wound are at greater risk for cardiac dysrhythmias and elevated blood pressure with the Valsalva maneuver and need to avoid straining to pass the stool.
Normal defecation is painless, resulting in passage of soft, formed stool
CONSTIPATION
Constipation is a symptom, not a disease. Improper diet, reduced fluid intake, lack of exercise, and certain medications can cause constipation. For example, patients receiving opiates for pain after surgery often require a stool softener or laxative to prevent constipation. The signs of constipation include infrequent bowel movements (less than every 3 days), difficulty passing stools, excessive straining, inability to defecate at will, and hard feaces
IMPACTION
Fecal impaction results from unrelieved constipation. It is a collection of hardened feces wedged in the rectum that a person cannot expel. In cases of severe impaction the mass extends up into the sigmoid colon.
DIARRHEA
Diarrhea is an increase in the number of stools and the passage of liquid, unformed feces. It is associated with disorders affecting digestion, absorption, and secretion in the GI tract. Intestinal contents pass through the small and large intestine too quickly to allow for the usual absorption of fluid and nutrients. Irritation within the colon results in increased mucus secretion. As a result, feces become watery, and the patient is unable to control the urge to defecate. Normally an anal bag is safe and effective in long-term treatment of patients with fecal incontinence at home, in hospice, or in the hospital. Fecal incontinence is expensive and a potentially dangerous condition in terms of contamination and risk of skin ulceration
HEMORRHOIDS
Hemorrhoids are dilated, engorged veins in the lining of the rectum. They are either external or internal.
FLATULENCE
As gas accumulates in the lumen of the intestines, the bowel wall stretches and distends (flatulence). It is a common cause of abdominal fullness, pain, and cramping. Normally intestinal gas escapes through the mouth (belching) or the anus (passing of flatus)
FECAL INCONTINENCE
Fecal incontinence is the inability to control passage of feces and gas from the anus. Incontinence harms a patient’s body image
PREPARATION AND GIVING OF LAXATIVESACCORDING TO POTTER AND PERRY,
An enema is the instillation of a solution into the rectum and sig
2. INTRODUCTION – NMR SPECTROSCOPY.
INSTRUMENTATION
SOLVENT REQUIREMENT IN NMR.
RELAXATION PROCESS IN NMR.
CHEMICAL SHIFT.
FACTORS AFFECTING CHEMICAL SHIFT.
NMR SIGNALS IN VARIOUS COMPOUNDS.
3. • This spectroscopic technique gives us information about the number and types of atoms in a
molecule.
• Nuclear magnetic spectroscopy is a powerful analytical technique used to organize organic
molecules by identifying carbon hydrogen frameworks within molecules.
Principle :
• The principle behind NMR is that many nuclei have spin and all nuclei are electrically charged. If
an external magnetic field is applied, an energy transfer is possible between the base energy to a
higher energy level.
4.
5. A NMR spectrophotometer consists of following components :
• A Magnet
• Sample and Sample holder
• Radio frequency generator
• Detector
• Reader
WORKING : In NMR spectrometer, the sample is dissolved
in CDCL3 and placed in magnetic field. Then radio frequency
generator irradiates the sample with short pulse of radiation
causing resonance. When nuclei fall back to their lower energy
state, detector measures the energy released and the spectrum
is recorded. The super conducting magnet in modern NMR
spectrometers have coils that are cooled in liquid Helium and
conduct electricity.
6.
7. The solvents used in NMR spectroscopy should be chemically inert, magnetically isotropic, devoid of hydrogen
atom and should dissolve the sample to a reasonable extent.
• Eg : CCl4, CS2, CDCl3, DMSO etc.
When selecting a solvent for running Nuclear Magnetic Resonance Spectroscopy (NMR) analysis, typically a
deuterated solvent is used in order to minimize background signals and provide a lock signal to compensate for
drifts in the magnetic field.
NMR solvents are distinctly different from other spectroscopic solvents as the majority of hydrogen nuclei are
replaced with deuterium so as to minimize the interference due to protons.
Though deuterium also has a nuclear spin, it does not operate on the same frequency as protons in the given
magnetic field. Therefore, it serves the purpose of NMR spectroscopy.
8. • It is crucial to remember that the price increases with the degree of deuteration. Deuterated chloroform, is most
commonly used because of its low price. Plus, the NMR peak is observed with the minimal chemical shift.
• A reference standard such as tetramethylsilane is commonly added (around 0.03%) to most commercially
available solvent grades to serve as zero ppm chemical shift reference for NMR studies.
• However, there are several other factors to consider for NMR solvent selection:
1. Solubility
2. Interfering peaks
3. Price
4. Isotopic purity
5. Ease of NMR sample recovery.
• Common spectroscopic solvents are available commercially in different degrees of deuteration. Apart from
CDCl3 other deuterated solvents in common use are:
9. • Deuterated water-(D_2O)
• DMSO (There is no ???? NMR peak, making this one of the best solvents)
• Methanol
• Methylene chloride
• Pyridine
• Acetic acid
• Acetone
For Example :
1. CDCL3 :
This solvent is the deuterated form of chloroform ,since it is relatively in expensive with isotopic purity, dissolves
many compounds, and is easy to evaporate after analysis for NMR sample recovery.
Since no solvent is 100% deuterated there will always be an observed ¹H peak for the solvent, which may interfere
with the compound of interest.
2. DMSO :
Compounds like DMSO have benefits to use as an NMR solvent as they are relatively inexpensive and can
solubilize many compounds that are difficult to solubilize.
10. Relaxation Process In
NMR
Relaxation is the process by which the spins in the
sample come to equilibrium with the surroundings.
The rate of relaxation determines how fast an
experiment can be repeated. The rate of relaxation
is influenced by the physical properties of the
molecule and the sample.
11. An understanding of relaxation processes is important for the proper measurement and interpretation of
NMR spectra.
There are three important considerations.
• 1. The very small energy difference between α and β states of a nuclear spin orientation in a magnetic
field results in a very small excess population of nuclei in the ground vs the excited states. For many
nuclei, relaxation is a very slow process. It is thus very easy to saturate an NMR transitions, with the
resultant loss in signal quality, and failure to obtain correct peak areas.
• 2. NMR lines are extraordinarily sharp, and close compared to higher energy spectroscopic methods.
When relaxation is very fast, NMR lines are broad, J-coupling may not be resolved or the signal may
even be difficult or impossible to detect.
• 3. The success of many multipulse experiments, especially 2D and 3D spectra, depends crucially on
proper consideration of relaxation times.
12. NMR Relaxation is of two types :
1. Spin-Lattice or Longitudinal Relaxation.
2. Spin-spin or Transverse Relaxation.
13. • Relaxation process occurs along z-axis.
• Transfer of the energy to the lattice or the solvent material.
• Coupling of the nuclei magnetic field with the magnetic field of the ensemble of the vibrational and rotational
motion of the lattice or the solvent.
• Results in a minimal temperature increase in sample.
• Relaxation time (T1) → Exponential decay.
o Spin-Lattice or Longitudinal Relaxation
14. • Relaxation process in the X-Y plane.
• Exchange of energy between excited nucleus and low energy state nucleus.
• Randomization of spins or magnetic moment in X-Y plane.
• Related to NMR peak line-width.
• Relaxation time T2.
• T2 may be equal to T1.
• No energy change Mx = My = M0 [1- e(- t/T2]
o Spin-spin or Transverse Relaxation
15. The shift in the position of the NMR region resulting from the shielding and deshielding by electrons is called
chemical shift.
When a proton is present inside the magnetic field more close to an electro positive atom more applied magnetic
field is required to cause excitation. This effect is called shielding effect.
When a proton is present outside the magnetic field close to a electronegative atom less applied magnetic field is
required to cause excitation . This effect is called deshielding effect.
Greater the electron density around the proton greater will be the induced secondary magnetic field [ local
diamagnetic effect].
Currents induced by fixed magnetic field result in secondary fields which can either enhance or decrease the field
to given a proton responds.
16. • Under the influence of the magnetic field electrons bonding the protons tends to process
around the nucleus in a plain perpendicular to magnetic field
• The position of the peaks in an NMR spectrum relative to the reference peak is expressed in terms of the
chemical shift
ᵟ = H0(reference) - H0(sample) X 106PPM
H0(reference)
17. • The value of H0 for the reference is usually greater than H0 for the sample, so subtraction in the
direction indicated gives a positive ᵟ.In terms of frequency unit ᵟ takes the form
ᵟ = ѵ(sample)- ѵ(reference) X 106ppm
ѵ(reference)
• Chemical shift is dimension less and expressed in parts per million (ppm ).
• Alternative system used is tau scale.
• τ=10-ᵟ scale the position of TMS signal is taken as 0.0 ppm
• Most chemical shifts value ranges from 0-10.
• A small value in tau represents low field absorption.
• High value represents high field absorption.
• Greater the deshielding of protons larger the value of delta.
18. Reasons for Chemical Shift
Positive shielding: Resonance position moves upfield.
Negative shielding: Resonance position moves downfield.
19. In order to measure the magnitude of chemical shifts of
different kinds of protons,
There must be some standard signal .
0.5%Tetra methylsilane (TMS)(ch3)4si is used as reference or
standard compound.
Chemical shift is represented by δ.
Δ scale: 0 to 10 scale.
TMS is taken as zero markers.
Dimensionless expression; negative for most protons
Measurement of
Chemical Shift
20. Accepted internal standard.
TMS has 12 equivalent protons and gives an intense single
signal.
Electro negativity of silicon is very low so the shielding of
equivalent protons in TMS is more than other compound so all
the signal arrives in a down field direction.
Chemically inert
Low boiling point
So it can be easily removed by evaporation after the spectrum
has been recorded
So the sample can easily recovered.
TMS is not suitable in aqueous solution so DSS ( 2,2- dimethyl-
2silapentane-5 sulphate) used as reference.
Protons in the methyl group of DSS gives a strong line.
TMS – As Internal
Standard
22. 1. Electronegativity and Inductive effect.
The proton is said to be deshielded if its attached with an electronegative atom/group. Greater the electro
negativity of atom greater is the deshielding caused to proton. If the deshielding is more, then δ value also more.
Electronegative atoms like Halogens Oxygen and Nitrogen deshield the protons. There for the absorption occurs
downfield.
The deshielding is directly proportional to the halogens oxygen or nitrogen.
+I effect : An electron releasing group increase the electron density around the proton and give rise to its
shielding.
-I effect : An electron withdrawing group is able to reduce electron density around the proton and Deshields the
proton.
23. 2. Anisotropic Effect (Space Effect)
In this Shielding and deshielding can be determined by location of proton in space.
It is also called as Space effect.
Downfield or paramagnetic shift of protons attached to C = C, aldehydic or aromatic, proton is experienced by
the molecular magnetic field induced by an action of applied field Ho on pi electrons, this magnetic field
induced by pi electrons are directional or unsymmetrical and this directional measurement is called
ANISOTROPY.
24. Anisotropic effect in Alkanes
o Alkanes do not possess the same degree of electron circulation as alkynes but do not exert nonlocal fields on
adjacent nuclei.
o The c-c σ bond shields a proton on its side more than its end.
25. Anisotropy in Alkynes
• In a magnetic field, the pi-electrons of a carbon-carbon triple bond are induced to circulate, but in this case the
induced magnetic field opposes the applied magnetic field (B॰).
• Thus, the proton feels a weaker magnetic field, so a lower frequency is needed for resonance. The nucleus is
shielded and the absorption is upfield.
26. Anisotropy In Benzene
• In a magnetic field, the six electrons in a benzene ring circulate around the ring creating a ring current.
• The magnetic field induced by these moving electrons reinforces the applied magnetic field in the vicinity
of the protons.
• The protons feel a stronger magnetic field and thus are deshielded. A higher frequency is needed for
resonance.
27. 3. Vanderwaals Deshielding
The electron cloud of a bulkier group will tend to repel the electron cloud surrounding the proton.
Thus such a proton will be deshielded will resonate at slightly higher value of δ than expected in the absence
of this effect.
The presence of bulky groups in a molecule cause deshielding due to weak VanderWaals force and give higher
δ value.
28. 4. Hydrogen Bonding
Intra-molecular hydrogen bonding does not show any change in absorption due to change in concentration.
While hydrogen atom involved in the intermolecular H-bonding shares its electrons with two electronegative
elements and as a result it itself deshielded and get higher δ value.
• E.g. Carboxylic acid dimer and β-diketones.
29. NMR Signal in Various Compounds
The number of NMR signals represent the number of protons in a molecule.
30. • For example,
let’s start with the simplest hydrocarbon; how many signals would you expect to see on the NMR
spectrum of methane?
Even though methane has four protons, they are all connected to the same atoms and have the same
neighbors on all sides – in other words, they are equivalent because they are in the same
environment.
Remember, equivalent protons give one NMR signal:
31. • It is the same with ethane (CH3-CH3); six protons – all equivalent, therefore one NMR signal:
32. For example:
• Bromoethane gives two NMR signals because the protons of the CH2 groups, being closer to the
bromine, are different from those in the CH3 group:
33. • Propane and butane give two signals.
• One because the protons of the CH2 group are different from those in the CH3 group, and the other,
because despite having four carbon atoms, the molecule is a combination of two identical CH2 and CH3
groups:
34. • Butane also gives 2 NMR signals.
• Because protons a are different from protons b. Each type gives one NMR signal.
35. Introduction to spectroscopy-5th edition- NMR Spectroscopy
by Donald Pavia, Pg no: 215 – 262.
Spectrometric Identification of Organic Compounds-6th
Edition-- Robert Silverstein, Pg No: 222 - 245.
www.slideshare.net/chemicalshift
https://www.sciencedirect.com/science/nuclear-magnetic-
resonance
http://chem.ch.huji.ac.il/nmr/whatisnmr/whatisnmr.html
Images – Internet search
REFERENC
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