nmr across the periodic table• nmr periodic table nmr active nuclei spin receptivity multiple...
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Innovation with Integrity
NMR Across The Periodic TableSpectroscopy beyond H, C, N, P and FENC WorkshopBaltimore, March 7. 2020Clemens Anklin
@canklin
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Overview• NMR periodic table
NMR active nuclei Spin Receptivity Multiple Isotopes Referencing
General trends in Multinuclear NMR
• Instrument preparation
Pulse calibration
• Examples
Platinum-195
Boron-11
Arsenic-75
Selenium- 77
Rubidium 85/87
Chlorine 35/37
Sodium-23
Oxygen-17
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NMR Periodic table
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NMR Periodic TableBasics
• Spin
Known spins = 0, 1/2, 1, 3/2, 5/2, 7/2, 9/2, 5, 6, 7Spin = 0 is not observable by NMRSpin = 1/2 nuclei typically provide narrow lines and often easy to observeSpin > 1/2 nuclei are more difficult and sometimes impossible to observe
• Isotopes
Some elements have multiple NMR active isotopes, some have active and inactive isotopes
NMR is typically not done on radioactive nuclei. Exceptions: 99Tc, 235U, 239Pu
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NMR Periodic TableProperties of NMR active nuclei
• Frequency
The NMR frequency of an isotope is determined by its gyromagnetic ratio
• Sensitivity and receptivity
Sensitivity = Sensitivity at equal number of spins
Receptivity = Sensitivity * natural abundance, often relative to 13C.
• Referencing
There are accepted references for almost all isotopes
Referencing to the 1H resonance of TMS is known as Ξ “Chi”
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NMR Frequency
𝝂𝝂 =𝜸𝜸𝟐𝟐𝝅𝝅
𝑩𝑩𝟎𝟎
• Frequency
The NMR frequency of an isotope is determined by its gyromagnetic ratio
• The gyromagnetic ratio is a property of every nucleus with a spin ≠ 0
• The actual values can be found in the CRC Handbook for Chemistry and Physics or the derived NMR frequencies in Harris et. Al. Pure Appl.Chem., Vol. 80, No. 1, pp. 59–84, 2008.doi:10.1351/pac200880010059
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NMR Frequency• Frequency
NMR active nuclei are well spread over the frequency range.
0
20
40
60
80
100
120
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NMR Frequency• Frequency
NMR active nuclei are well spread over the frequency range.
More than half of pairwise differences are less then 1 MHz
0.001
0.01
0.1
1
10
100
19F
203T
l11
9Sn
115S
n14
1Pr
129X
e23
Na
27Al
151E
u45
Sc12
1Sb
185R
e11
5In
165H
o12
7I19
9Hg
209B
i13
9La
138L
a18
1Ta
153E
u50
V85
Rb
169T
m17
6Lu
33S
97M
o67
Zn49
Ti79
Se17
3Yb
109A
g87
Sr10
7Ag
83Kr
149S
m57
Fe16
7Er
187O
s19
7Au
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NMR Sensitivity and Receptivity• The NMR sensitivity is defined as
the relative sensitivity of one nucleus when compared to another nucleus at equal number of spins. It is determined by the gyromagnetic ratio and the spin.
• High spin increases sensitivity
0 100 200 300 400 500
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0 100 200 300 400 500
NMR Sensitivity and Receptivity• The NMR sensitivity is defined as
the relative sensitivity of one nucleus when compared to another nucleus at equal number of spins. It is determined by the gyromagnetic ratio and the spin.
• Scaled for spin
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NMR Sensitivity and Receptivity• The NMR receptivity also takes
into account the natural abundance of a nucleus.
• Receptivity = Sensitivity * natural abundance
1H19F
31P
13C
93Nb
15N
0 100 200 300 400 500
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NMR Periodic Table
H He
Li Be B C N O F Ne
Na Mg Al Si P S Cl Ar
K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br Kr
Rb Sr Y Zr Nb Mo Tc Ru Rh Pd Ag Cd In Sn Sb Te I Xe
Cs Ba La Hf Ta W Re Os Ir Pt Au Hg Tl Pb Bi Po At Rn
Fr Ra Ac Rf Db Sg Bh Hs Mt Ds Rg Cn Nh Fl Mc Lv Ts Og
Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu
Th Pa U Np Pu Am Cm Bk Cf Es F Md No Lr
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NMR Periodic Table
H He
Li Be B C N O F Ne
Na Mg Al Si P S Cl Ar
K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br Kr
Rb Sr Y Zr Nb Mo Tc Ru Rh Pd Ag Cd In Sn Sb Te I Xe
Cs Ba La Hf Ta W Re Os Ir Pt Au Hg Tl Pb Bi Po At Rn
Fr Ra Ac Rf Db Sg Bh Hs Mt Ds Rg Cn Nh Fl Mc Lv Ts Og
Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu
Th Pa U Np Pu Am Cm Bk Cf Es Fm Md No Lr
Unobservable
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NMR Periodic Table
H He
Li Be B C N O F Ne
Na Mg Al Si P S Cl Ar
K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br Kr
Rb Sr Y Zr Nb Mo Tc Ru Rh Pd Ag Cd In Sn Sb Te I Xe
Cs Ba La Hf Ta W Re Os Ir Pt Au Hg Tl Pb Bi Po At Rn
Fr Ra Ac Rf Db Sg Bh Hs Mt Ds Rg Cn Nh Fl Mc Lv Ts Og
Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu
Th Pa U Np Pu Am Cm Bk Cf Es Fm Md No Lr
The easy ones: Spin = 1/2
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NMR Periodic Table
H He
Li Be B C N O F Ne
Na Mg Al Si P S Cl Ar
K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br Kr
Rb Sr Y Zr Nb Mo Tc Ru Rh Pd Ag Cd In Sn Sb Te I Xe
Cs Ba La Hf Ta W Re Os Ir Pt Au Hg Tl Pb Bi Po At Rn
Fr Ra Ac Rf Db Sg Bh Hs Mt Ds Rg Cn Nh Fl Mc Lv Ts Og
Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu
Th Pa U Np Pu Am Cm Bk Cf Es Fm Md No Lr
Spin = ½, Spin > ½,
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NMR Periodic Table
H He
Li Be B C N O F Ne
Na Mg Al Si P S Cl Ar
K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br Kr
Rb Sr Y Zr Nb Mo Tc Ru Rh Pd Ag Cd In Sn Sb Te I Xe
Cs Ba La Hf Ta W Re Os Ir Pt Au Hg Tl Pb Bi Po At Rn
Fr Ra Ac Rf Db Sg Bh Hs Mt Ds Rg Cn Nh Fl Mc Lv Ts Og
Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu
Th Pa U Np Pu Am Cm Bk Cf Es Fm Md No Lr
Spin = ½, Spin > ½, Multiple Isotopes
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Multiple Isotopes• Many elements have multiple NMR active isotopes
• Examples: 1H, 2H and 3H , 115Sn, 117Sn and 119Sn, 39K and 41K, 6Li and 7Li
• Which one to choose:
• Spin ½ over anything else
• Natural Abundance the higher the better
• Frequency the higher the better
• Quadrupole Moment the lower the better
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Multiple Isotopes• Examples:
Vanadium
Isotope 50 V 51 VFrequency 9.97 26.3Spin 6 7/2Natural Abundance
0.24 % 99.76 %
QuadrupoleMoment
0.21 -5.2x10-2
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Multiple Isotopes• Examples:
Molybdenum
Isotope 95 Mo 97 MoFrequency 6.51 6.65Spin 5/2 5/2Natural Abundance
15.9 % 9.55 %
QuadrupoleMoment
-0.015 0.17 From NMR periodic table athttp://chem.ch.huji.ac.il/nmr/techniques/1d/multi.html
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NMR Periodic Table
H He
Li Be B C N O F Ne
Na Mg Al Si P S Cl Ar
K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br Kr
Rb Sr Y Zr Nb Mo Tc Ru Rh Pd Ag Cd In Sn Sb Te I Xe
Cs Ba La Hf Ta W Re Os Ir Pt Au Hg Tl Pb Bi Po At Rn
Fr Ra Ac Rf Db Sg Bh Hs Mt Ds Rg Cn Nh Fl Mc Lv Ts Og
Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu
Th Pa U Np Pu Am Cm Bk Cf Es Fm Md No Lr
Paramagnetic nuclei, Difficult nuclei
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ReferencingThere are accepted references for almost all isotopes Harris et. Al: Pure Appl.Chem., Vol. 80, No. 1, pp. 59–84, 2008.doi:10.1351/pac200880010059
In many cases it is not possible to add an internal reference to the sample or it is not even possible to acquire a spectrum of the reference compound.
In such cases referencing to the 1H resonance of TMS can be used and is known as Ξ Chi – reference.
AU program = xiref
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ReferencingTwo problematic nuclei
13C and 15N
Both have two accepted references
13C uses TMS for organic solvents and DSS/TSP in aqueous solutions
The difference is ~ 2.66 ppm
For 15N the difference is much larger. The references are CH3NO2 and NH3 (liquid).
CH3NO2 is 380.44 ppm from NH3
NH3 is -380.298 ppm from CH3NO2
𝛿𝛿 =𝜈𝜈 𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠 − 𝜈𝜈(𝑟𝑟𝑠𝑠𝑟𝑟)
𝜈𝜈(𝑟𝑟𝑠𝑠𝑟𝑟)
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General trends in multinuclear NMRChemical Shifts
Many nuclei have very large chemical shift ranges. Transition metals can exceed 10’000 ppm
Major influences on chemical shift are:
inner coordination sphere
Oxidation state
Chemical shift (ppm)
hard ligands (O, Cl) soft ligands (C, P)
high oxidation state low oxidation state
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The Spectrometer
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Hardware requirements
• Many spectrometers are capable of acquiring multinuclear NMR data.
• The range of nuclei accessible will be determined by the probe used.
• When direct observe is of importance multinuclear probes will be the primary choices over inverse detection probes for conventional probes
• Multinculear spectroscopy can also be conducted with cryogenically cooled probes. The limiting factor might be the reduced VT range
• Most of the work can be done in 5mm probes. For direct observation of low receptivity nuclei a 10 mm probe might be helpful
• For many applications a variable temperature accessory is recommended. Some nuclei show very large temperature dependent shifts.
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Probes
• BBO, BBFO, SmartProbe and iProbe BBFO
• All these probes have a tuning range from (19F) 31P to 15N or 109 Ag.
• 203/205 Tl is not necessarily included
• For nuclei with a resonance frequency below that of 109Ag, special low range probes are offered.
• For some nuclei such as 27Al, 29Si, 11B, 10B special probes are offered where minimal amounts of these elements are used in the construction of the probe.
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Conventional probe range 31P to 109Ag
H He
Li Be B C N O F Ne
Na Mg Al Si P S Cl Ar
K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br Kr
Rb Sr Y Zr Nb Mo Tc Ru Rh Pd Ag Cd In Sn Sb Te I Xe
Cs Ba La Hf Ta W Re Os Ir Pt Au Hg Tl Pb Bi Po At Rn
Fr Ra Ac Rf Db Sg Bh Hs Mt Ds Rg Cn Nh Fl Mc Lv Ts Og
Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu
Th Pa U Np Pu Am Cm Bk Cf Es Fm Md No Lr
Spin = ½, Spin > ½,
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Cryogenic probe range 31P to 15N
H He
Li Be B C N O F Ne
Na Mg Al Si P S Cl Ar
K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br Kr
Rb Sr Y Zr Nb Mo Tc Ru Rh Pd Ag Cd In Sn Sb Te I Xe
Cs Ba La Hf Ta W Re Os Ir Pt Au Hg Tl Pb Bi Po At Rn
Fr Ra Ac Rf Db Sg Bh Hs Mt Ds Rg Cn Nh Fl Mc Lv Ts Og
Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu
Th Pa U Np Pu Am Cm Bk Cf Es Fm Md No Lr
Spin = ½, Spin > ½,
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Pulse calibration
• Pulse calibration: a bit more complicated than 1H or 13C
• Easy cases:
• A signal is observable in one or a few scans and the relaxation times are not too long.
• Use your standard method of pulse calibration
• Look for the null at 360 degrees
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Pulse calibration
• Pulse calibration: a bit more complicated than 1H or 13C
• More complex cases:
• Direct observation is hard but satellite signals in 1H spectrum are resolved and reasonably narrow.
• Use “inverse” calibration with decp901H U$lUUNX UUUU&UU
Signal is null at 90 degree X pulse
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Pulse calibration
• Pulse calibration: a bit more complicated than 1H or 13C
• More complex cases:
• Direct observation is hard and satellite signals in 1H spectrum are not resolved and somewhat broad. Use the HMQC experiment to determine the 90 degree pulse.
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Pulse calibration
• Pulse calibration: a bit more complicated than 1H or 13C
• More complex cases:
• Direct observation is not easy, no coupling to 1H.
• Amplifier power and probe response are continuous over the frequency range. Find a easier nucleus nearby to calibrate the pulse or extrapolate from a known nucleus. For example use 39K to calibrate the pulse for 109Ag, 37Cl can be used for 131Xe etc.
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Setting up a new nucleus
• Ready to measure:
• If possible prepare a concentrated sample of the reference compound or another simple, stable well known sample. Harris et. Al: Pure Appl.Chem., Vol. 80, No. 1, pp. 59–84, 2008.
• Try not to use your research sample for set up
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And now Examples
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Application examples
• NMR of nuclei outside the ones used for organic molecules are used in
• Organometallic and inorganic chemistry
• Material sciences
• Pharma
• Food
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Application examples
• Organometallic and inorganic chemistry
• Nuclei measured: 195Pt, 103Rh, 57Fe, 119Sn, 31P, 183W, 109Ag, 199Hg etc
• Coordination chemistry
• Homogeneous catalysis
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Application examples
• Organometallic and inorganic chemistry
• Chemical shifts provide information about coordination sphere.
• Coupling constants give information about geometry
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Application examples
• Materials sciences
• Nuclei measured: 29Si, 27Al, 57Fe, 119Sn, 31P, 51V, 7Li, etc
• Lithium has gained a lot of attention for battery research.
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Application examples
• Biomolecules
• Nuclei measured: 113Cd, 109Ag, 199Hg etc
• Metal complexes
• Non active or quadrupolar metals in metallo-proteins can be replaced by spin ½ NMR active nuclei.
• For example Zn can be replaced by Cd
• 1H – 113Cd correlation experiments can be measured,
From S. Forsen FEBS Letters, 1979
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Application examples
• Pharma and Medicine
• Nuclei measured: 23Na, 25Mg, 35Cl, 39K,
• Quality control
• Electrolytes
• Quantification of Na, Cl, K and Mg in infusion solutions.
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Application examples
• Food
• Nuclei measured: 23Na, 25Mg, 31P, 35Cl, 39K,
• Quality control
• Concentration measurements of various salts.
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NMR Periodic Table
H He
Li Be B C N O F Ne
Na Mg Al Si P S Cl Ar
K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br Kr
Rb Sr Y Zr Nb Mo Tc Ru Rh Pd Ag Cd In Sn Sb Te I Xe
Cs Ba La Hf Ta W Re Os Ir Pt Au Hg Tl Pb Bi Po At Rn
Fr Ra Ac Rf Db Sg Bh Hs Mt Ds Rg Cn Nh Fl Mc Lv Ts Og
Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu
Th Pa U Np Pu Am Cm Bk Cf Es Fm Md No Lr
Spin = ½, Spin > ½,
Pt
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195Pt - Platinum
• Spin = ½
• Nat Abundance = 33.83 %
• Receptivity (rel 13C) = 19.1
• Shift range > 15,000 ppm
• Reference = 1.2 M Na2PtCl 6 in D2O
![Page 44: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/44.jpg)
195Pt - Platinum
• Main problem: Finding the peak
• Literature can help
![Page 45: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/45.jpg)
195Pt - Platinum
• Main problem: Finding the peak
• Is there coupling with 1H ?
• If yes use inverse experiments to
• find the peak
• Calibrate the pulse
![Page 46: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/46.jpg)
195Pt - Platinum
• Main problem: Finding the peak
• Is there coupling with 1H ?
![Page 47: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/47.jpg)
195Pt - Platinum
• Main problem: Finding the peak
• Run a HMQC, with wide sweep in indirect dimension and small flip-angle. Here 8000 ppm and 2 usec pulse.
• Set gradients with gradratio
•
![Page 48: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/48.jpg)
195Pt - Platinum
• Main problem: Finding the peak
• Run a HMQC, with wide sweep in indirect dimension and small flip-angle. Here 8000 ppm and 2 usec pulse.
![Page 49: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/49.jpg)
195Pt - Platinum
• Main problem: Finding the peak
• Center the signal and reduce sweep in f1
![Page 50: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/50.jpg)
195Pt - Platinum
• Pulse Calibration
• Optimize pulse on HMQC experiment
![Page 51: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/51.jpg)
195Pt - Platinum
• Ready for direct detect 195Pt experiment
• Ca 10 mg, 400 MHz Prodigy Probe
![Page 52: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/52.jpg)
195Pt - Platinum• Multinuclear NMR to characterize metal complexes
• Chemical shifts provide information about the direct environment of the metal
• Coupling constants can proivde information about the configuraitonof the complex.
![Page 53: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/53.jpg)
195Pt - Platinum• Multinuclear NMR to characterize metal complexes
• 31P spectra provide J(31P,195Pt)
• Cis coupling larger than Trans
3518 Hz
2392 Hz
![Page 54: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/54.jpg)
195Pt – Platinum and 119Sn Tin NMR• Multinuclear NMR to follow reactions
• This platinum complex reacts with SnCl2
• The proton spectrum shows a second species forming
![Page 55: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/55.jpg)
195Pt – Platinum and 119Sn Tin NMR• Multinuclear NMR to follow reactions
• This platinum complex reacts with SnCl2
• The 31P spectrum shows at least 3 species
3518 Hz2392 Hz
2088 Hz
![Page 56: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/56.jpg)
195Pt – Platinum and 119Sn Tin NMR• Multinuclear NMR to follow reactions
• The new signal show additional peaks
• Ratio of J = = ratio of γ 119Sn and γ 117Sn
• Area matches as well
223.8 Hz
234.7 Hz
![Page 57: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/57.jpg)
195Pt – Platinum and 119Sn Tin NMR• Multinuclear NMR to follow reactions
• 195Pt NMR confirms the coordination of Sn
• J(119Sn/195Pt) ~ 28000 Hz
![Page 58: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/58.jpg)
195Pt – Platinum and 119Sn Tin NMR• Multinuclear NMR to follow reactions
• 195Pt NMR confirms the coordination of Sn
• J(119Sn/195Pt) ~ 28000 Hz
![Page 59: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/59.jpg)
195Pt – Platinum and 119Sn Tin NMR• Multinuclear NMR to follow reactions
• And finally the 119Sn NMR spectrum
![Page 60: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/60.jpg)
NMR Periodic Table
H He
Li Be B C N O F Ne
Na Mg Al Si P S Cl Ar
K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br Kr
Rb Sr Y Zr Nb Mo Tc Ru Rh Pd Ag Cd In Sn Sb Te I Xe
Cs Ba La Hf Ta W Re Os Ir Pt Au Hg Tl Pb Bi Po At Rn
Fr Ra Ac Rf Db Sg Bh Hs Mt Ds Rg Cn Nh Fl Mc Lv Ts Og
Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu
Th Pa U Np Pu Am Cm Bk Cf Es Fm Md No Lr
Spin = ½, Spin > ½,
B
![Page 61: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/61.jpg)
11/10B - Boron
• Boron - 11
• Spin = 3/2
• Nat Abundance = 80.1 %
• Receptivity (rel 13C) = 754
• Shift range > 200 ppm
• Reference = BF3 Et2O in CDCl3 15%
• Quadrupolar moment = 4.059*10-2
• Boron - 10
• Spin = 3
• Nat Abundance = 19.9 %
• Receptivity (rel 13C) = 22.1
• Shift range > 200 ppm
• Reference = BF3 Et2O in CDCl3 15%
• Quadrupolar moment = 8.459*10-2
![Page 62: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/62.jpg)
11/10B - Boron
• Boron - 11
• NaBH4 in D2O BH4 BH3D
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11/10B - Boron
• 1H Spectrum
• NaBH4 in D2O
![Page 64: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/64.jpg)
11/10B - Boron
• 1H Spectrum
• NaBH4 in D2O
• 4 x ~ 20= 80
7 x ~ 2.8 = 19.8
![Page 65: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/65.jpg)
11/10B - Boron
• 1H Spectrum
• NaBH4 in D2O
Na11BH4
Na10BH4Na11BH3DNa10BH4
![Page 66: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/66.jpg)
NMR Periodic Table
H He
Li Be B C N O F Ne
Na Mg Al Si P S Cl Ar
K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br Kr
Rb Sr Y Zr Nb Mo Tc Ru Rh Pd Ag Cd In Sn Sb Te I Xe
Cs Ba La Hf Ta W Re Os Ir Pt Au Hg Tl Pb Bi Po At Rn
Fr Ra Ac Rf Db Sg Bh Hs Mt Ds Rg Cn Nh Fl Mc Lv Ts Og
Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu
Th Pa U Np Pu Am Cm Bk Cf Es Fm Md No Lr
Spin = ½, Spin > ½,
As
![Page 67: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/67.jpg)
75As - Arsenic
• Spin = 3/2
• Nat Abundance = 100 %
• Receptivity (rel 13C) = 143
• Shift range ? ppm
• Reference = 0.5 M NaAsF6 in CD3CN
• Quadrupolar moment = 0.314
![Page 68: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/68.jpg)
75As - Arsenic
• Only highly symmetric molecules give observable lines
• AsO4 or NaAsF6
![Page 69: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/69.jpg)
NMR Periodic Table
H He
Li Be B C N O F Ne
Na Mg Al Si P S Cl Ar
K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br Kr
Rb Sr Y Zr Nb Mo Tc Ru Rh Pd Ag Cd In Sn Sb Te I Xe
Cs Ba La Hf Ta W Re Os Ir Pt Au Hg Tl Pb Bi Po At Rn
Fr Ra Ac Rf Db Sg Bh Hs Mt Ds Rg Cn Nh Fl Mc Lv Ts Og
Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu
Th Pa U Np Pu Am Cm Bk Cf Es Fm Md No Lr
Spin = ½, Spin > ½,
Se
![Page 70: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/70.jpg)
77Se - Selenium
• Spin = 1/2
• Nat Abundance = 7.63 %
• Receptivity (rel 13C) = 2.98
• Shift range + 2400 to -900 ppm
• Reference = neat (CH3)2Se with trace of C6D6 for lock.
![Page 71: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/71.jpg)
77Se - Selenium
• Relatively easy to measure.
• Most organo-selenium compounds will show nJ(H,Se)
![Page 72: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/72.jpg)
77Se - Selenium
• Relatively easy to measure.
• Most organo-selenium compounds will show nJ(H,Se)
• We can again use the strategy outlined for 195Pt to set up the parameters.
![Page 73: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/73.jpg)
77Se - Selenium
• Relatively easy to measure.
• Most organo-selenium compounds will show nJ(H,Se)
• Proton decoupling is essential for good S/N and sharp lines
without with
![Page 74: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/74.jpg)
77Se - Selenium
• Selenium satellites will also show in experiments such as H,C HSQC
J(C, Se)
J(H, Se)
![Page 75: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/75.jpg)
NMR Periodic Table
H He
Li Be B C N O F Ne
Na Mg Al Si P S Cl Ar
K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br Kr
Rb Sr Y Zr Nb Mo Tc Ru Rh Pd Ag Cd In Sn Sb Te I Xe
Cs Ba La Hf Ta W Re Os Ir Pt Au Hg Tl Pb Bi Po At Rn
Fr Ra Ac Rf Db Sg Bh Hs Mt Ds Rg Cn Nh Fl Mc Lv Ts Og
Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu
Th Pa U Np Pu Am Cm Bk Cf Es Fm Md No Lr
Spin = ½, Spin > ½,
Rb
![Page 76: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/76.jpg)
85/87Rb - Rubidium
• 85Rb
• Spin = 5/2
• Nat Abundance = 72.15 %
• Frequency = 9.655 MHz
• Receptivity (rel 13C) = 43.4
• Quadrupole mom = 0.26
• Shift range = 30 - -80 ppm
• Reference = RbCl 0.01 M in D2O
• 87Rb
• Spin = 3/2
• Nat Abundance = 27.83 %
• Frequency = 32.72 MHz
• Receptivity (rel 13C) = 277
• Quadrupole mom = 0.13
• Shift range = 30 - -80 ppm
• Reference = RbCl 0.01 M in D2O
![Page 77: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/77.jpg)
85/87Rb - Rubidium
• 85Rb Spectrum • 87Rb Spectrum
![Page 78: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/78.jpg)
NMR Periodic Table
H He
Li Be B C N O F Ne
Na Mg Al Si P S Cl Ar
K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br Kr
Rb Sr Y Zr Nb Mo Tc Ru Rh Pd Ag Cd In Sn Sb Te I Xe
Cs Ba La Hf Ta W Re Os Ir Pt Au Hg Tl Pb Bi Po At Rn
Fr Ra Ac Rf Db Sg Bh Hs Mt Ds Rg Cn Nh Fl Mc Lv Ts Og
Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu
Th Pa U Np Pu Am Cm Bk Cf Es Fm Md No Lr
Spin = ½, Spin > ½,
Cl
![Page 79: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/79.jpg)
35/37Cl - Chlorine
• 35Cl
• Spin = 3/2
• Nat Abundance = 75.53 %
• Frequency = 9.798 MHz
• Receptivity (rel 13C) = 21
• Quadrupole mom = -0.1
• Shift range = 1000 - 0 ppm
• Reference = NaCl 0.1 M in D2O
• 37Cl
• Spin = 3/2
• Nat Abundance = 24.47 %
• Frequency = 8.156 MHz
• Receptivity (rel 13C) = 3.87
• Quadrupole mom = -0.079
• Shift range = 1000 - 0 ppm
• Reference = NaCl 0.1 M in D2O
![Page 80: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/80.jpg)
35/37Cl - Chlorine
• 35Cl Spectrum • 37Cl Spectrum
![Page 81: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/81.jpg)
35/37Cl - Chlorine
• 35Cl
• Spin = 3/2
• Nat Abundance = 75.53 %
• Frequency = 9.798 MHz
• Receptivity (rel 13C) = 21
• Quadrupole mom = -0.1
• Shift range = 1000 - 0 ppm
• Reference = NaCl 0.1 M in D2O
• 37Cl
• Spin = 3/2
• Nat Abundance = 24.47 %
• Frequency = 8.156 MHz
• Receptivity (rel 13C) = 3.87
• Quadrupole mom = -0.079
• Shift range = 1000 - 0 ppm
• Reference = NaCl 0.1 M in D2O
• 85Rb
• Spin = 5/2
• Nat Abundance = 72.15 %
• Frequency = 9.655 MHz
• Receptivity (rel 13C) = 43.4
• Quadrupole mom = 0.26
• Shift range = 30 - -80 ppm
• Reference = RbCl 0.01 M in D2O
![Page 82: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/82.jpg)
35/37Cl - Chlorine
• 35Cl
• Spin = 3/2
• Nat Abundance = 75.53 %
• Frequency = 9.798 MHz
• Receptivity (rel 13C) = 21
• Quadrupole mom = -0.1
• Shift range = 1000 - 0 ppm
• Reference = NaCl 0.1 M in D2O
• 85Rb
• Spin = 5/2
• Nat Abundance = 72.15 %
• Frequency = 9.655 MHz
• Receptivity (rel 13C) = 43.4
• Quadrupole mom = 0.26
• Shift range = 30 - -80 ppm
• Reference = RbCl 0.01 M in D2O
![Page 83: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/83.jpg)
35Cl – Chlorine\85Rb - Rubidium
• 35Cl
• Frequency = 9.798 MHz
• 85Rb
• Frequency = 9.655 MHzAt 400 MHz the two signals are only 572 kHz apart. This is a true heteronuclear spectrum
35Cl Signal 85Rb Signal
![Page 84: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/84.jpg)
And now some fun
![Page 85: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/85.jpg)
Soy Sauce NMR
• There are a number of nuclei you can measure in soy sauce but lets focus on one.
![Page 86: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/86.jpg)
Soy Sauce NMR
![Page 87: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/87.jpg)
Soy Sauce NMR
Kikkoman Bragg
EtOH
• Not this one
![Page 88: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/88.jpg)
Soy Sauce NMR
![Page 89: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/89.jpg)
NMR Periodic Table
H He
Li Be B C N O F Ne
Na Mg Al Si P S Cl Ar
K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br Kr
Rb Sr Y Zr Nb Mo Tc Ru Rh Pd Ag Cd In Sn Sb Te I Xe
Cs Ba La Hf Ta W Re Os Ir Pt Au Hg Tl Pb Bi Po At Rn
Fr Ra Ac Rf Db Sg Bh Hs Mt Ds Rg Cn Nh Fl Mc Lv Ts Og
Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu
Th Pa U Np Pu Am Cm Bk Cf Es Fm Md No Lr
Spin = ½, Spin > ½,
Na
![Page 90: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/90.jpg)
23Na - Sodium
• Spin = 3/2
• Nat Abundance = 100 %
• Receptivity (rel 13C) = 525
• Shift range ~ 110 ppm
• Reference = 0.1 M NaCl in D2O
![Page 91: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/91.jpg)
23Na - Sodium
• Easy Nucleus
• 0.125M NaCl in D2O
![Page 92: NMR Across The Periodic Table• NMR periodic table NMR active nuclei Spin Receptivity Multiple Isotopes Referencing General trends in Multinuclear NMR • Instrument preparation Pulse](https://reader030.vdocuments.mx/reader030/viewer/2022013010/5f0b84e57e708231d430eaf5/html5/thumbnails/92.jpg)
23Na - Sodium
• How salty is?
• Unknown Na concentration
• Quantification vs 0.125M NaClsolution
Reference Kikkoman 90% + 10% D200.125 M 1.7 M (1.666M label)
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23Na - Sodium
• How salty is?
• Unknown Na concentration
• Quantification vs 0.125M NaClsolution
Reference Bragg 90% + 10% D200.125 M 3.28 M (2.78M label)
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Soy Sauce NMR
Do not forget to read the serving size too
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And now some more fun
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Water NMR
• There are two nuclei you can measure in water, Hydrogen and Oxygen.
• Let’s look at Oxygen
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NMR Periodic Table
H He
Li Be B C N O F Ne
Na Mg Al Si P S Cl Ar
K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br Kr
Rb Sr Y Zr Nb Mo Tc Ru Rh Pd Ag Cd In Sn Sb Te I Xe
Cs Ba La Hf Ta W Re Os Ir Pt Au Hg Tl Pb Bi Po At Rn
Fr Ra Ac Rf Db Sg Bh Hs Mt Ds Rg Cn Nh Fl Mc Lv Ts Og
Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu
Th Pa U Np Pu Am Cm Bk Cf Es Fm Md No Lr
Spin = ½, Spin > ½,
O
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17O - Oxygen
• Spin = 5/2
• Nat Abundance = 0.038 %
• Receptivity (rel 13C) = 0.0611 %
• Shift range - 50 to + 1600 ppm
• Reference = Tap Water
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17O - Oxygen
• Different types of Oxygen show large chemical shift differences
• Hydroxyl ~ 0 – 50 ppm
• Carboxylic acids > 200 ppm
• Carbonyls > 500 – 600 ppm
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17O - Oxygen
• Some people claim that there is a special healthy form of water called hexagonal water.
• Unhealthy water forms “larger” clusters
• This water can be made with various expensive devices. Or it can be purchased in bottles
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17O - Oxygen
• There are claims that Oxygen 17 NMR line width gives information about “structured” or “hexagonal” water.
• Evidence are O17 NMR spectra of water before and after treatment
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17O - Oxygen
• So I took a whole bunch of samples that consisted mostly of water and ran O17 NMR.
• Billerica Tap water = 45Hz
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17O - Oxygen
• So I took a whole bunch of samples that consisted mostly of water and ran O17 NMR.
• Buffer solution pH 7.4 = 53 Hz
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17O - Oxygen
• So I took a whole bunch of samples that consisted mostly of water and ran O17 NMR.
• White wine = 80 Hz
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17O - Oxygen
• So I took a whole bunch of samples that consisted mostly of water and ran O17 NMR.
• Diet Coke= 44 Hz
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17O - Oxygen
• So I took a whole bunch of samples that consisted mostly of water and ran O17 NMR.
• Soy Sauce = 200 Hz
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17O - Oxygen
• What primarily determines the linewidth of the O17 signal ?
• pH• David L. Turner (1980) Proton and deuteron
exchange rates in water measured by oxygen-17 N.M.R., Molecular Physics, 40:4, 949-957,
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Conclusion
• There are a lot of interesting nuclei in the periodic table
• Some are easy, some are hard
• Using a standard for preparation is helpful
• Do not be afraid to try something new
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Acknowledgement
• The engineers and scientists who build the probes
• My applications colleagues who provided me with material and let me use their instruments
• And all of you for listening
• Check out #IYPT2019 #NMRPT
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My NMR Periodic Table
H He
Li Be B C N O F Ne
Na Mg Al Si P S Cl Ar
K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br Kr
Rb Sr Y Zr Nb Mo Tc Ru Rh Pd Ag Cd In Sn Sb Te I Xe
Cs Ba La Hf Ta W Re Os Ir Pt Au Hg Tl Pb Bi Po At Rn
Fr Ra Ac Rf Db Sg Bh Hs Mt Ds Rg Cn Nh Fl Mc Lv Ts Og
Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu
Th Pa U Np Pu Am Cm Bk Cf Es Fm Md No Lr
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Innovation with Integrity