Resonance Spin Mate User manual

NMR Analyzer “Spin Mate”
Operation manual
RESONANCE
SYSTEMS

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Content
1. General safety information ................................................................................................................... 3
2. Spin Mate Overview .............................................................................................................................. 5
2.1. NMR Analyzer components................................................................................................................ 5
2.2. Connecting Hardware to PC and Drivers Installation......................................................................... 8
2.3. Technical Characteristics and Service Conditions ............................................................................ 11
2.4. Preparation of Spin Mate for measurements................................................................................... 12
3. Software Overview .............................................................................................................................. 13
3.1. Software Installation ................................................................................................................... 13
3.2. Menu and Control Board............................................................................................................. 16
3.3. Measuring System Settings ......................................................................................................... 23
4. Software Start-up ................................................................................................................................ 31
4.1. Preparation of Validation Sample................................................................................................ 31
4.2. First Start-up and Daily Check ..................................................................................................... 31
4.3. Applications Test ......................................................................................................................... 37
5. Relaxation Time Measurements.......................................................................................................... 39
5.1. Spin-lattice Relaxation Time T1.................................................................................................... 39
5.1.1. Inversion-Recovery experiment .............................................................................................. 39
5.1.2. Saturation-Recovery experiment ............................................................................................ 39
5.1.3. Utilizing applications for measuring Spin-lattice Relaxation Time.......................................... 40
5.2. Spin-spin Relaxation Time T2....................................................................................................... 44
5.2.1. Free Induction Decay (FID) ...................................................................................................... 44
5.2.2. Solid Echo (SE) ......................................................................................................................... 44
5.2.3. Magic Sandwich Echo (MSE).................................................................................................... 45
5.2.4. Utilizing applications for measuring Spin-spin Relaxation Time ............................................. 46
5.2.5. Hahn Echo (HE). Main information and applying.................................................................... 46
5.2.6. Carr-Purcell-Meiboom-Gill (CPMG). Main information and applying ..................................... 48
6. Diffusion Measurements ..................................................................................................................... 51
6.1. Calibrating of Gradient Multiplier ............................................................................................... 52
6.2. Measurements of Self-Diffusion Coefficients.............................................................................. 54
7. Spectrum Construction.................................................................................................................... 56
8. Development Applications for Software Relax8.............................................................................. 58
8.1. Syntax of Inline Programming Language of Relax8 ..................................................................... 58
8.2. Comments to Examples of Applications...................................................................................... 69

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1. General safety information
The chapter describes the general safety precautions and precautionary measures that must
be observed when operating the TD-NMR analyzer (Spin Mate). The instructions are intended to
supplement, but not replace, the normal safety regulations in your region. The information provided
does not cover all safety precautions that must be observed in a laboratory. Ultimately, the
responsibility for a well-maintained and safe laboratory environment rests with the user and his
organization.
DANGER:
For the safety of the user, all safety instructions and safety information must be taken into account
and strictly followed. Therefore, these operating instructions must be available to all users at all
times. Read all manuals supplied with the Spin Mate system (including manuals available online)
before setting up and operating the system. Read the safety instructions in this chapter and those
in the other manuals with particular care. When assembling, commissioning the SpinMate system
and performing analyzes, strictly adhere to the specifications in the manuals and the Relax8
operating software.
1.1 Important precautions
The Spin Mate system was developed in accordance with a large number of international
standards, which are decisive for the safety of laboratory equipment. Routine use is not dangerous.
With simple and sensible precautionary measures, you can ensure the safe operation of your system
in the long term.
• Make sure that the system is placed securely and stably on a sufficiently stable surface (e.g.
table with a load capacity of 100 kg/m2).
• Do not place the Spin Mate system near any heat sources, such as radiators.
• Do not block the ventilation openings on the sides, top or bottom of the housing.
• Do not cover the top of the cases
• Make sure that all devices are properly connected to the mains, i.e. connect the devices to a
power supply that has either a switch or some other device for interrupting the power supply.
• Only plug the power cord into sockets that have a grounded protective conductor connection
• In particular, make sure that all devices are securely grounded.
• Do not open any housings. They serve to protect against strong magnetic fields and electrical
hazards. There are no user-serviceable components. Otherwise there is a risk of strong magnetic
fields (e.g. influence on pacemakers) and mechanical injuries.
• Keep the system dry, especially the magnet and the sample volume.
• Do not use flammable gases to purge the device. Use dry, oil-free nitrogen or air to purge the
device.
• Only operate the spectrometer system indoors under the following conditions:

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- Ambient temperature range: 293±5 K (from 15 to 25 °C);
- Relative humidity 90% maximum (non-condensing)
1.2. Requirements for the user
The systems may only be set up and used by laboratory personnel and persons who, due to
their training and professional experience, are familiar with the possible dangers that can arise
during operation. Personnel without relevant training or persons who are in training require careful
supervision by a qualified person.
1.3. Location and ventilation
Do not place the spectrometer in a poorly ventilated area of the laboratory when using
nitrogen as the purge gas.
1.4. Risk of fire and explosion
The Spin Mate system with heating and its contact with flammable vapors can trigger an
explosion. Therefore, flammable solvents and samples should not be kept near the system. During
sample preparation, such materials must be handled in a safe area away from the system, such as
in a fume hood.
1.5. Improper use
Any use other than those mentioned and any application that does not correspond to the
technical data is deemed to be improper use. Improper use can result in dangerous situations for
operators and / or devices and damage to property. The user bears the sole risk for any damage or
dangers that can be attributed to improper use. In particular, the following applications are not
permitted:
Carrying out repair and maintenance work that is not explained in these operating
instructions by the user.
Opening houses / cases, dismantel moduls, components, subsystems.
If the Spin Mate system is used in a manner not described by the manufacturer, the safe
functioning of the system may be impaired. No modifications of any kind may be made to the system
without prior consultation with the manufacturer and without written approval. Modifications and
upgrades may only be carried out by service technicians authorized by Resonance Systems. The
manufacturer rejects claims for damages based on unapproved modifications without exception. If
the system is operated in a way that is not specified here, its safety may be impaired and the user
may be endangered.

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2. Spin Mate Overview
2.1. NMR Analyzer components
Compact TD-NMR analyzer Spin Mate is an ideal instrument for such applications as Relaxation
times measurement, Surface Area and Wettability of nanoparticles and colloidal systems,
Crystallinity and Domain Sizes in Polymers and many others. Observable nuclei: 1H (basic
configuration).
Pic. 2.1. Spin Mate.
Front and back panels of Spin Mate are shown schematically in Pic. 2.2-2.3.

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Pic. 2.2. Front panel of Spin Mate.
POWER –power LED. Switched to 100 % of brightness if temperature of magnet stable,
otherwise flashes at 50 % of brightness;
MAGNET –indicates magnet heating;
MEASUREMENT –indicates active measurement process;
1–OLED display. It shows set up temperature of the magnet, actual magnet temperature,
temperature of air inside the system and current consuming power (in %%);
2–sensitive power button. This button switches on the power analog part of NMR analyser.
In standby mode its brightness and brightness of OLED display is 50 % and 100 % when the
analyser is fully switched on. Caution –measurement is not possible if this button is
switched off.
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2

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Pic. 2.3. Back panel of Spin Mate.
AC Input –power input with integrated switcher. This switcher switches on digital part of
the analyser and magnet heater. The temperature is stored in the internal memory and the
factory preset is +35 °C;
USB –USB connector.

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2.2. Connecting Hardware to PC and Drivers Installation
2.2.1. The power switches on back panel units must be in position “O” – turned off.
2.2.2. Connect the Spin Mate to the PC by USB cable through USB port.
2.2.3. Connect the power supply cables to the Spin Mate.
2.2.4. Turn on the PC. Turn on the power of NMR Analyzer by pressing the power switch on the
back panel of the analyzer to the position “I”.
2.2.5. The “Installing device driver software” MS Windows 7 message will appear (Pic. 2.5).
Pic. 2.5. MS Windows message.
2.2.6. For the drivers installation you should open Device Manager. In the next window you will
see the following –see Pic. 2.6.
Pic. 2.6. Device Manager window.
2.2.7. The right click on Spin Mate 4.0 and choose Properties (Pic. 2.7).
Pic. 2.7. Drivers installation.

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2.2.8. The Spin Mate 4.0 Properties window will appear (Pic. 2.8), in which you should push on
Update Driver button.
Pic. 2.8. Spin Mate 4.0 Properties window.
2.2.9. The Update Driver Software –Spin Mate 4.0 window will appear (Pic. 2.9), in which you
should click on Browse my computer for driver software.
Pic. 2.9. Update Driver Software –Spin Mate 4.0 window.
2.2.10. Choose the Drivers folder where Relax8 was installed by the Browse... button as it is
shown at the Pic. 2.10. Click on Next.
Pic. 2.10. Search of the appropriate drivers.

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2.2.11. The result of drivers installation is shown in Pic. 2.11 a and b.
a
b
Pic. 2.11. Result of installation drivers.
2.2.12. Push on Close button.