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[link] can have E substituted for hν, leading to [link] , which can solve for the NMR resonance frequency (v).

Using the frequency (v), the δ, or expected chemical shift may be computed using [link] .

Delta (δ) is observed in ppm and gives the distance from a set reference. Delta is directly related to the chemical environment of the particular atom. For a low field, or high delta, an atom is in an environment which produces induces less shielding than in a high field, or low delta.

Nmr instrument

An NMR can be divided into three main components: the workstation computer where one operates the NMR instrument, the NMR spectrometer console, and the NMR magnet. A standard sample is inserted through the bore tube and pneumatically lowered into the magnet and NMR probe ( [link] ).

Standard NMR instrument, with main components labeled: (A) bore tube, (B) outer magnet shell, (C) NMR probe.

The first layer inside the NMR ( [link] ) is the liquid nitrogen jacket. Normally, this space is filled with liquid nitrogen at 77 K. The liquid nitrogen reservoir space is mostly above the magnet so that it can act as a less expensive refrigerant to block infrared radiation from reaching the liquid helium jacket.

Diagram of the main layers inside an NMR machine.

The layer following the liquid nitrogen jacket is a 20 K radiation shield made of aluminum wrapped with alternating layers of aluminum foil and open weave gauze. Its purpose is to block infrared radiation which the 77 K liquid nitrogen vessel was unable to eliminate, which increases the ability for liquid helium to remain in the liquid phase due to its very low boiling point. The liquid helium vessel itself, the next layer, is made of stainless steel wrapped in a single layer of aluminum foil, acting once again as an infrared radiation shield. It is about 1.6 mm thick and kept at 4.2 K.

Inside the vessel and around the magnet is the aluminum baffle, which acts as another degree of infrared radiation protection as well as a layer of protection for the superconducting magnet from liquid helium reservoir fluctuations, especially during liquid helium refills. The significance is that superconducting magnets at low fields are not fully submerged in liquid helium, but higher field superconducting magnets must maintain the superconducting solenoid fully immersed in liquid helium The vapor above the liquid itself is actually enough to maintain superconductivity of most magnets, but if it reaches a temperature above 10 K, the magnet quenches. During a quench, the solenoid exceeds its critical temperature for superconductivity and becomes resistive, generating heat. This heat, in turn, boils off the liquid helium. Therefore, a small opening at the very base of the baffle exists as a path for the liquid helium to reach the magnet surface so that during refills the magnet is protected from accidental quenching.

Problems with solid state nmr

The most notable difference between solid samples and solution/gas in terms of NMR spectroscopy is that molecules in solution rotate rapidly while those in a solid are fixed in a lattice. Different peak readings will be produced depending on how the molecules are oriented in the magnetic field because chemical shielding depends upon the orientation of a molecule, causing chemical shift anisotropy. Therefore, the effect of chemical shielding also depends upon the orientation of the molecule with respect to the spectrometer. These counteracting forces are balanced out in gases and solutions because of their randomized molecular movement, but become a serious issue with fixed molecules observed in solid samples. If the chemical shielding isn’t determined accurately, neither will the chemical shifts (δ).

Another issue with solid samples are dipolar interactions which can be very large in solid samples causing linewidths of tens to hundreds of kilohertz to be generated. Dipolar interactions are tensor quantities, which demonstrate values dependent on the orientation and placement of a molecule in reference to its surroundings. Once again the issue goes back to the lattice structure of solids, which are in a fixed location. Even though the molecules are fixed, this does not mean that nuclei are evenly spread apart. Closer nuclei display greater dipolar interactions and vice versa, creating the noise seen in spectra of NMR not adapted for solid samples. Dipolar interactions are averaged out in solution states because of randomized movement. Spin state repulsions are averaged out by molecular motion of solutions and gases. However, in solid state, these interactions are not averaged and become a third source of line broadening.

Magic angle spinning

In order to counteract chemical shift anisotropy and dipolar interactions, magic angle spinning was developed. As discussed above, describing dipolar splitting and chemical shift aniostoropy interactions respectively, it becomes evident that both depend on the geometric factor (3cos 2 θ-1).

If this factor is decreased to 0, then line broadening due to chemical shift anisotropy and dipolar interactions will disappear. Therefore, solid samples are rotated at an angle of 54.74˚, effectively allowing solid samples to behave similarly to solutions/gases in NMR spectroscopy. Standard spinning rates range from 12 kHz to an upper limit of 35 kHz, where higher spin rates are necessary to remove higher intermolecular interactions.

Application of solid state nmr

The development of solid state NMR is a technique necessary to understand and classify compounds that would not work well in solutions, such as powders and complex proteins, or study crystals too small for a different characterization method.

Solid state NMR gives information about local environment of silicon, aluminum, phosphorus, etc. in the structures, and is therefore an important tool in determining structure of molecular sieves. The main issue frequently encountered is that crystals large enough for X-Ray crystallography cannot be grown, so NMR is used since it determines the local environments of these elements. Additionally, by using 13 C and 15 N, solid state NMR helps study amyloid fibrils, filamentous insoluble protein aggregates related to neurodegenerative diseases such as Alzheimer’s disease, type II diabetes, Huntington’s disease, and prion diseases.

Bibliography

  • J. W. Akitt, NMR and Chemistry , 3 rd Edn., Chapman&Hall, London (1992).
  • A. R. Grimmer and B. Blümich, Introduction to Solid-State NMR , Springer-Verlag, Berlin(1994).
  • J. A. Iggo, NMR Spectroscopy in Inorganic Chemistry , Oxford University Press, New York (1999).
  • J. C. C. Chan, Top. Curr. Chem. , 2011, 306 , 47.
  • R. Freeman, Chem Heterocyc Compd , 1995, 31 , 1004-1005.
  • Jeol USA, JEOL Delta-GSX 270 NMR Magnet Destruction ,<http://www.jeolusa.com>
  • University of Pittsburgh, Magnet Safety ,<http://www.ehs.pitt.edu/assets/docs/magnet-safety.pdf>, 2008, (accessed 15 February 2012).

Questions & Answers

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Sanjika
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Sanjika
ology means a study of
SharaAmor Reply
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SharaAmor
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Tina
a branch of knowledge
Kanchan
psych means soul and ology means to study.
Wajid
Can someone help me with tha latent functions of different social institutions
Usman
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Interestingly Reply
Factors that affect learning?
Ofentse Reply
I am struggling with survivors guilt and complicated grief after traumatic death of spouse. how to cope.
Rowdy Reply
Try to talk with someone you trust and join people who makes you feel worthy. try to help someone. Helping someone makes you feel better
sherlock
I think you must seek professional help.
Swarada
I am extremely sorry for your loss...I know that the pain of your loss is overwhelming and that you are experiencing all kinds of difficult and unexpected emotions. please don't get me wrong but the best way to cope is to move on..i know its hard..but that's the only way..(continued.)
Princess
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Princess
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Princess
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Princess
First and foremost -- Wow Rowdy! You have been through a highly difficult situation in your life, hands down. As a wife, I simply cannot phathom nor imagine slightly the feelings and thoughts you bare and I'm sure as these words do not help and hit rewind; my heart and prayers are going out to you-
Stephanie
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Stephanie
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Stephanie
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Stephanie
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Stephanie
to guide you through; keep an your senses wide open so that you can learn when she is trying to communicate.
Stephanie
What is meant by politics of intelligence? Please guide about this article.
Ali Reply
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Angela
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Ali
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Ali
Information about child psychology
Mohammed Reply
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Maryam
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Geo
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Geo
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Maryam
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Geo
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Mohammed
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Jobin
branches of psychology
QSN Reply
neuropsychology
jeddy
behaviorism
Mira
Legal psychology
Miljana
Developmental psychology, Sports psychology , Clinical psychology , Marketing psychology , counseling psychology , Biological psychology, Educational psychology , Positive psychology etc.
Swarada
child.psychology
Nss
social, occupational psychology
jeddy
what does it mean when the temporal lobe is anterior to occipital lobe
John Reply
the cortex refers to what part of the brain
John
the cortex refers to what part of the brain
John
cerebral cortex
jeddy
behind?
jeddy
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marjelee Reply
during bad experience
Nyakuei
i think its not about suitation, its about the thing tatz need training.
gokul
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rhoda
I would think that training should be an ungoing thing. That's before, during and after. just in case there's a reoccurrence
Angela
any time
Aaronz
what is Karma
ana Reply
I think the summation of good and bad deeds you do in your life. Accidentally or otherwise.
Swarada
Yes. I totally agree.
ana
And if it is bad then the root must have been too.
ana
Yes , In Hinduism we also believe that our parent's Karma also applies to us ! Don't know about that , but it kept people in check .
Swarada
Adding to Swarada point. karma can be good or bad. both will have consequences. karma is biasedness you have shown in your life. like a king could not have two rules for normal man and his son, that comes under karma.
Sujeet
Oh perfectly said!
Swarada
Ok. It is also said that when one does something... bad or good..it will come back to you 10 folds of the same.
ana
yea that too ! I remember my mother always said if u stole someone's 10 rupees ur 100 will be stolen ( excuse my English ! I'm a non - English speaking person)
Swarada
karma is nothing but what one usually mean when they say- what you sow, so shall you reap.
Alisha
certainly
Crazy
more important.. this concept was told by lord Krishna as part of spirituality, to focus on your good deed ,the purpose you are born for and your responsibilities. Not for hoping that bad will happen with people who made you feel bad. just giving example ;)
Sujeet
karma is the boomerang of your actions. what u put out in the universe u get back
David
Who is the founder of psychology
Daryl Reply
Wilhelm wundt
Amanda
Wilhelm Wundt
Sneha
William wundth
Ihrar
Wilhelm Wundt
Megha
and William James
Amanda
Wilhelm Wundt
adam
Wilhelm Wundt is the founder of structuralism
Angela
Yes and also the "Father of Psychology" I think the correct word is Father not Founder.
Swarada
oh ok. noted
Angela
i believe it goes beyond him I believe it is Ancient but un formalized
David
I like your answer Swarada
David
Oh thanks! But u summarised it well!
Swarada
what is up my fellow psych peeps!!
what are some academic research on developmental psychology
Chezy
Sawrada Founder of Psychology is W.Wundt but Father of Psychology is Sigmund Freud...
Wajid
what are some good schools to study psychology?
Enjoy Reply
George Mason, Penn State, UVA, university of Michigan
Jasmine
Hi I'm currently doing my experimental psychology research can you suggest a topic or research topic for my research thank you and please see 😊
Jerico Reply
Hello Jerico. I could help you out with some ideas if you're interested!
Yasmine
can u give me some ideas too?
Geo
For sure. It depends if you're trying to do an experiment (using statistics probably) or a case study what are you aiming for?
Yasmine
Hello Jerico. Try to opt for something simple and easy to do. I wouls say perhaps study the effects of color on concentration? You could get a group of people and have them take a memory test (you can find some online) in a white room for example. Then have them take another memory test
Yasmine
similar to the first one but in a different room and then you check the responses if the performance is better
Yasmine
but you have to know that a lot of factors will interfere in the performance such as mental state etc so make sure to choose a certain specific population. that's very important
Yasmine
you could be a bit more specific about it , to isolate the variables that can mess it up like age, sex, etc... you gotta take that into account
Yasmine
so that the results get somewhat accurate
Yasmine
that is very detailed information I really like it thank you very much 😊 your so very kind
Jerico
You're very welcome
Yasmine
what are your interests in general?
Yasmine
Althogh I'm persuing botany and engineering.... but I also want to study human behaviour and psychology.... I would like if anyone can share their knowledge with me !!!!
Crazy
I'm interested on effect of electroconvulsive therapy on people having a depression
Jerico
What is Electroconvulsive therapy?
Pixeled
Astral Projection
Mansi
Electroconvulsive therapy (ECT) is a medical treatment that is most commonly used in patients with severe major depression.
Jerico
What are the expected dutties functions and responsibilities of a head of an agency based on the principles, Practice of industrial psychology?
Paul Reply
what are the psychological characteristics expected from an employee wether regular or occupying a position?
Paul
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Source:  OpenStax, Basic knowledge of nuclear magnetic resonance spectroscopy ( nmr ). OpenStax CNX. Jun 07, 2012 Download for free at http://cnx.org/content/col11429/1.1
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