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NMR Hardware - Global NMR Discussion Meeting
14 September, 2021
Mark S. Conradi
ABQMR, Inc.
Albuquerque, NM 87108 USA
msc@wuphys.wustl.edu
ABQMR – contract NMR research and specialty equipment, to the
government and industry. Lately, MRI of sorghum plant roots
undisturbed, in the ground (and greenhouse).
1
Target Audience
 Solid state NMR scientists
 < mid-career
 Now in research group with technically-
knowledgable people
 Thinking “what do I do when I am my own
assistant professor?”
 Curious “how does it work?”
2
Today’s topics
 Diagnosis of
Spectrometer
Probe
 Test gear – scopes, signal generators …
 Build a simple probe
Most of us will not build our own spectrometer. But
we will need to de-bug it when there is
No More Resonance. So:
3
Simple Spectrometer
Plus computer-
controlled signal
digitizer and
pulse sequence
controller
4
No signal – Is it Tx? Rcvr? Probe?
 If it does not pulse and run, suspect computer control.
 Check that magnet is ON, with a steel tool.
 Transmitter – look for rf pulse with an oscilloscope.
 Receiver – check that Rcvr noise looks normal. Turn off Tx power amp,
inject signal at resonance freq where probe normally connects. Use
1 mWt level and 60 dB atten. Look for signal.
Check triggering of scope
5
Looking at the High Power Tx
 Usual Attenuators (½ watt, 20, 30, 40 dB) are OK.
 Except at first position. Use attenuator built for high peak power.
20 dB atten if each R is
½ watt, 120 ohm,
carbon composition
(Stackpole, from
DigiKey), in small alum
box.
►If you look directly at rf, need rf scope ($$$).
►Or, insert a diode detector in front of scope (at “here”), so you see
pulse envelope.
►Can also look at input to Tx power amp (level is ≅ 1 mW, no
attenuators needed). 6
Testing the Receiver
 NMR receivers can be narrow-band (1-100 kHz
wide).
Get signal generator onto desired frequency
 1 mW = 0 dBm = 0.22 Vrms = 0.63 VP-P
You should be able to “see” 1 µV rms (= -107 dB
from 1 mW)
 Can check “after” T-R switch.
 Can check “after” preamp.
7
What is dB?
dB Power Ratio Volt Ratio
0 1 1
3 2 1.41
6 4 2
10 10 3.2
20 100 10
40 10,000 100
60 1M 1000
8
Testing the Probe
 Check tuning with tune-up bridge. Maybe coil is open?
This is low power.
 If you have in-line forward / reflected power meter, what
does it say? A big reflection suggests bad arcing
(breakdown) or other.
 Put in big signal sample (water, D2O, 13C-labelled ethylene
glycol). Even if probe arcs, will see a signal.
 Listen (ear) for breakdown (snap, snap, …). Use dark
room and look (eye) for blue light. Go to 200 µs pulse,
every 0.1 sec.
 Note – probe will de-tune if you remove cover. Need to
re-tune. 9
Replace Probe with a Crystal
Turn power down to 1 watt and look for “FID” from crystal. No
echoes! See Sam Emery and MSC, JMR 242, 1-3 (2014).
Again, crystals are narrow-band but are usually within 500 ppm of the
frequency stamped on the case.
OR build a simple test probe. Use it to check Tx (is 90o length
changed?) and Rcvr (is received FID same as it was when everything
was working?)
10
In-line
Wattmeter
A large reflection
(reflected amplitude
almost as large as
forward amplitude) says
“bad probe”.
11
What and Where to Buy – Test Equipment
 Borrow what you can
 Try eBay or equivalent. Remember, you will only use occasionally.
 Oscilloscopes
 If you need to see 500 MHz, ≥ $10,000
 If you only need to see diode detected envelope, ≤$600.
 Tektronix, Rhode-Schwarz, Rigol, …
 Diode detectors, SMA connecters = zero-bias Schottky,
 Pasternack PE8012 $550
 Fairview Microwave SMD 0102 $550
 Digikey CPDETLS-4000 $34
 Careful, diode detectors need peak inputs of around 10 mW, = +10 dBm
12
13
14
 Signal generators. HP, Tektronix, Agilent, Keysight, Rhode-Schwarz …
Try eBay
 Most VNA (vector network analyzers) can be put into CW signal generator
mode. My $60 VNA-H4 is CW if you reduce SPAN to 1K (1 kHz) or less.
 VNA Can be pricy
 Or, try VNWA 3 from SDRKits.com $500. Needs a computer (Windows) to
drive it.
 Or, Nano VNA (VNA-H4) from AURSINCO $60 from Amazon
 Take the VNA to an rf-person to set yours up! Keep the NanoVNA flow
chart to help you change it later.
 VNWA 3 uses computer keyboard, needs computer.
 NanoVNA is battery-operated, hand held, but has awkward touch screen
15
16
17
18
Attenuators, Filters
 Mini Circuits Laboratories
 JFW
 Crystek, sold by DigiKey
 Cinch, sold by DigiKey
 Bird
 EME Precisions 7020/30 A, needs diode detectors
and scope
In-line Directional Wattmeters
19
20
Old Man Advice: Try it first
(when it is all working)!!
Don’t wait until you need it to get used to your
oscilloscope, VNA, signal generator, …
“Why can’t I get this ___ ___ scope to trigger?”
Always use external trigger
Write it All Down
As you disconnect cables, change settings, lengthen rf
pulses, make a record so you can get back to start
21
Build a Simple Probe – not rocket science
 The only way to learn is to do.
 Keep it simple (not triple resonance)
 Read Wheeler and Conradi, Concepts in Magnetic
Resonance, part A, 40A, pp1-13 (2012).
I can send you a copy.
 You need a shielding aluminum enclosure, a box or old
probe body.
Figure out the mechanical aspects first.
Find a small permanent magnet (5 cm3) to look at all
parts for magnetism.
22
A Suitable Coil, Resonating it.
 Resonance: ω2LC = 1, ω = 2πf
 Estimate solenoidℒ =
𝑛2𝑟2
9𝑟+10𝑙
ℒ in μH, r and l in inches (sorry).
Typical ℒ has ZL = ωℒ = 50-100 Ω
So C obeys 𝑍𝐶 =
1
𝜔𝐶
= 𝑍𝐿, too.
23
Finding L-C Resonance Frequency
Adjust C to desired freq.
Kong – good way to
bench-tune a trap for a
new freq, in double or
triple-resonance probe
24
What is Tuning and Matching for?
Typically 𝑍𝑐𝑜𝑖𝑙 = 𝑖100 + 1
So 𝑄 =
𝜔𝐿
𝑟
= 100
𝑍𝑐𝑜𝑖𝑙 = 𝑖𝜔𝐿 + 𝑟
* You want to transform this Zcoil to i0+50 (50 ohms
resistive).
So you add C to cancel i𝜔L, leaving r alone, provided:
𝑖𝜔𝐿 +
−𝑖
𝜔𝐶
= 0, or 𝜔2𝐿𝐶 = 1
Then you need to step-up the impedance to 50 ohm.
25
Transformers
26
𝑉
𝑠𝑒𝑐
𝑉𝑝𝑟𝑖
= 𝑛
𝐼𝑠𝑒𝑐
𝐼𝑝𝑟𝑖
=
1
𝑛
V I = Power = Conserved
𝑍 =
𝑉
𝐼
⇒
𝑍𝑠𝑒𝑐
𝑍𝑝𝑟𝑖
=
𝑛
1
𝑛
= 𝑛2
This is a Current Divider
to 50 Ω
spectr.
Impedance matched iff dissipation internally (in r) matches dissipation
externally (in 50 Ω ext)
𝐼𝐿
2
∙ 𝑟 = 𝐼50
2
∙ 50 =>
𝐼50
𝐼𝐿
2
=
𝑟
50
or I stepdown
𝐼50
𝐼𝐿
=
C𝑐
𝐶𝑐+𝐶𝑡
=
𝑟
50
*You could just add the impedances of L, Ct, Cc in series and parallel,
following the usual rules. But it is a mess and will carry no take-home
meaning.
Instead, use 𝜔2𝐿(𝐶𝑐 + 𝐶𝑡)=1 and
C𝑐
𝐶𝑐+𝐶𝑡
=
𝑟
50
=
1
7 27
Voltage Step-down
is equiv to
is equiv to
Iff L′=L
and Rr = (ωL)2
𝑅 =
ω𝐿
𝑟
∙ ω𝐿,
Q =
ω𝐿
𝑟
=
𝑅
𝜔𝐿
28
Here you step-down from 10k to 50Ω, so you step-down voltage by
10𝑘
50
= 14
𝐶𝑠𝑒𝑟𝑖𝑒𝑠 =
1
1
𝐶𝑡
+
1
𝐶𝑀
𝜔2ℒ𝐶𝑠𝑒𝑟𝑖𝑒𝑠 = 1
𝐶𝑆
𝐶𝑀
≃
𝐶𝑡
𝐶𝑀
=
50
10𝑘
29
𝑍𝑐 =
1
𝜔𝑐
Lots of Ways to Match …
30
31
32
33
Buying Non-magnetic Capacitors
 Polyflon, teflon-insulated piston trimmers
 Digikey sells Sprague-Goodman and other piston trimmers
 Digikey sells chip caps, non-magnetic, easy to solder, high
voltage from Knowles-Seyfer
34

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NMR Hardware3.pptx

  • 1. NMR Hardware - Global NMR Discussion Meeting 14 September, 2021 Mark S. Conradi ABQMR, Inc. Albuquerque, NM 87108 USA msc@wuphys.wustl.edu ABQMR – contract NMR research and specialty equipment, to the government and industry. Lately, MRI of sorghum plant roots undisturbed, in the ground (and greenhouse). 1
  • 2. Target Audience  Solid state NMR scientists  < mid-career  Now in research group with technically- knowledgable people  Thinking “what do I do when I am my own assistant professor?”  Curious “how does it work?” 2
  • 3. Today’s topics  Diagnosis of Spectrometer Probe  Test gear – scopes, signal generators …  Build a simple probe Most of us will not build our own spectrometer. But we will need to de-bug it when there is No More Resonance. So: 3
  • 4. Simple Spectrometer Plus computer- controlled signal digitizer and pulse sequence controller 4
  • 5. No signal – Is it Tx? Rcvr? Probe?  If it does not pulse and run, suspect computer control.  Check that magnet is ON, with a steel tool.  Transmitter – look for rf pulse with an oscilloscope.  Receiver – check that Rcvr noise looks normal. Turn off Tx power amp, inject signal at resonance freq where probe normally connects. Use 1 mWt level and 60 dB atten. Look for signal. Check triggering of scope 5
  • 6. Looking at the High Power Tx  Usual Attenuators (½ watt, 20, 30, 40 dB) are OK.  Except at first position. Use attenuator built for high peak power. 20 dB atten if each R is ½ watt, 120 ohm, carbon composition (Stackpole, from DigiKey), in small alum box. ►If you look directly at rf, need rf scope ($$$). ►Or, insert a diode detector in front of scope (at “here”), so you see pulse envelope. ►Can also look at input to Tx power amp (level is ≅ 1 mW, no attenuators needed). 6
  • 7. Testing the Receiver  NMR receivers can be narrow-band (1-100 kHz wide). Get signal generator onto desired frequency  1 mW = 0 dBm = 0.22 Vrms = 0.63 VP-P You should be able to “see” 1 µV rms (= -107 dB from 1 mW)  Can check “after” T-R switch.  Can check “after” preamp. 7
  • 8. What is dB? dB Power Ratio Volt Ratio 0 1 1 3 2 1.41 6 4 2 10 10 3.2 20 100 10 40 10,000 100 60 1M 1000 8
  • 9. Testing the Probe  Check tuning with tune-up bridge. Maybe coil is open? This is low power.  If you have in-line forward / reflected power meter, what does it say? A big reflection suggests bad arcing (breakdown) or other.  Put in big signal sample (water, D2O, 13C-labelled ethylene glycol). Even if probe arcs, will see a signal.  Listen (ear) for breakdown (snap, snap, …). Use dark room and look (eye) for blue light. Go to 200 µs pulse, every 0.1 sec.  Note – probe will de-tune if you remove cover. Need to re-tune. 9
  • 10. Replace Probe with a Crystal Turn power down to 1 watt and look for “FID” from crystal. No echoes! See Sam Emery and MSC, JMR 242, 1-3 (2014). Again, crystals are narrow-band but are usually within 500 ppm of the frequency stamped on the case. OR build a simple test probe. Use it to check Tx (is 90o length changed?) and Rcvr (is received FID same as it was when everything was working?) 10
  • 11. In-line Wattmeter A large reflection (reflected amplitude almost as large as forward amplitude) says “bad probe”. 11
  • 12. What and Where to Buy – Test Equipment  Borrow what you can  Try eBay or equivalent. Remember, you will only use occasionally.  Oscilloscopes  If you need to see 500 MHz, ≥ $10,000  If you only need to see diode detected envelope, ≤$600.  Tektronix, Rhode-Schwarz, Rigol, …  Diode detectors, SMA connecters = zero-bias Schottky,  Pasternack PE8012 $550  Fairview Microwave SMD 0102 $550  Digikey CPDETLS-4000 $34  Careful, diode detectors need peak inputs of around 10 mW, = +10 dBm 12
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  • 15.  Signal generators. HP, Tektronix, Agilent, Keysight, Rhode-Schwarz … Try eBay  Most VNA (vector network analyzers) can be put into CW signal generator mode. My $60 VNA-H4 is CW if you reduce SPAN to 1K (1 kHz) or less.  VNA Can be pricy  Or, try VNWA 3 from SDRKits.com $500. Needs a computer (Windows) to drive it.  Or, Nano VNA (VNA-H4) from AURSINCO $60 from Amazon  Take the VNA to an rf-person to set yours up! Keep the NanoVNA flow chart to help you change it later.  VNWA 3 uses computer keyboard, needs computer.  NanoVNA is battery-operated, hand held, but has awkward touch screen 15
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  • 19. Attenuators, Filters  Mini Circuits Laboratories  JFW  Crystek, sold by DigiKey  Cinch, sold by DigiKey  Bird  EME Precisions 7020/30 A, needs diode detectors and scope In-line Directional Wattmeters 19
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  • 21. Old Man Advice: Try it first (when it is all working)!! Don’t wait until you need it to get used to your oscilloscope, VNA, signal generator, … “Why can’t I get this ___ ___ scope to trigger?” Always use external trigger Write it All Down As you disconnect cables, change settings, lengthen rf pulses, make a record so you can get back to start 21
  • 22. Build a Simple Probe – not rocket science  The only way to learn is to do.  Keep it simple (not triple resonance)  Read Wheeler and Conradi, Concepts in Magnetic Resonance, part A, 40A, pp1-13 (2012). I can send you a copy.  You need a shielding aluminum enclosure, a box or old probe body. Figure out the mechanical aspects first. Find a small permanent magnet (5 cm3) to look at all parts for magnetism. 22
  • 23. A Suitable Coil, Resonating it.  Resonance: ω2LC = 1, ω = 2πf  Estimate solenoidℒ = 𝑛2𝑟2 9𝑟+10𝑙 ℒ in μH, r and l in inches (sorry). Typical ℒ has ZL = ωℒ = 50-100 Ω So C obeys 𝑍𝐶 = 1 𝜔𝐶 = 𝑍𝐿, too. 23
  • 24. Finding L-C Resonance Frequency Adjust C to desired freq. Kong – good way to bench-tune a trap for a new freq, in double or triple-resonance probe 24
  • 25. What is Tuning and Matching for? Typically 𝑍𝑐𝑜𝑖𝑙 = 𝑖100 + 1 So 𝑄 = 𝜔𝐿 𝑟 = 100 𝑍𝑐𝑜𝑖𝑙 = 𝑖𝜔𝐿 + 𝑟 * You want to transform this Zcoil to i0+50 (50 ohms resistive). So you add C to cancel i𝜔L, leaving r alone, provided: 𝑖𝜔𝐿 + −𝑖 𝜔𝐶 = 0, or 𝜔2𝐿𝐶 = 1 Then you need to step-up the impedance to 50 ohm. 25
  • 26. Transformers 26 𝑉 𝑠𝑒𝑐 𝑉𝑝𝑟𝑖 = 𝑛 𝐼𝑠𝑒𝑐 𝐼𝑝𝑟𝑖 = 1 𝑛 V I = Power = Conserved 𝑍 = 𝑉 𝐼 ⇒ 𝑍𝑠𝑒𝑐 𝑍𝑝𝑟𝑖 = 𝑛 1 𝑛 = 𝑛2
  • 27. This is a Current Divider to 50 Ω spectr. Impedance matched iff dissipation internally (in r) matches dissipation externally (in 50 Ω ext) 𝐼𝐿 2 ∙ 𝑟 = 𝐼50 2 ∙ 50 => 𝐼50 𝐼𝐿 2 = 𝑟 50 or I stepdown 𝐼50 𝐼𝐿 = C𝑐 𝐶𝑐+𝐶𝑡 = 𝑟 50 *You could just add the impedances of L, Ct, Cc in series and parallel, following the usual rules. But it is a mess and will carry no take-home meaning. Instead, use 𝜔2𝐿(𝐶𝑐 + 𝐶𝑡)=1 and C𝑐 𝐶𝑐+𝐶𝑡 = 𝑟 50 = 1 7 27
  • 28. Voltage Step-down is equiv to is equiv to Iff L′=L and Rr = (ωL)2 𝑅 = ω𝐿 𝑟 ∙ ω𝐿, Q = ω𝐿 𝑟 = 𝑅 𝜔𝐿 28
  • 29. Here you step-down from 10k to 50Ω, so you step-down voltage by 10𝑘 50 = 14 𝐶𝑠𝑒𝑟𝑖𝑒𝑠 = 1 1 𝐶𝑡 + 1 𝐶𝑀 𝜔2ℒ𝐶𝑠𝑒𝑟𝑖𝑒𝑠 = 1 𝐶𝑆 𝐶𝑀 ≃ 𝐶𝑡 𝐶𝑀 = 50 10𝑘 29 𝑍𝑐 = 1 𝜔𝑐
  • 30. Lots of Ways to Match … 30
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  • 34. Buying Non-magnetic Capacitors  Polyflon, teflon-insulated piston trimmers  Digikey sells Sprague-Goodman and other piston trimmers  Digikey sells chip caps, non-magnetic, easy to solder, high voltage from Knowles-Seyfer 34