Abstract

NMR Relaxation (NMRR) is an extremely useful quantitative technique for material science, particularly for studying polymers and porous materials. NMR Cryoporometry (NMRC) is a powerful technique for the measurement of pore-size distributions and total porosities. This paper discusses the use, capabilities and application of a newly available compact NMR time-domain relaxation spectrometer, the Lab-Tools Mk3 NMR Relaxometer & Cryoporometer [Lab-Tools (nano-science), Ramsgate, Kent, UK (2019)]. Being Field Programmable Gate Array based means that it is unusually compact, which makes it particularly suitable for the lab bench-top, in the field and also mobile use. Its use with a variable-temperature NMR probe such as the Lab-Tools Peltier thermo-electrically cooled variable-temperature (V-T) probe is also discussed. This enables the NMRC measurement of pore-size distributions in porous materials, from sub-nano- to over 1 micron sized pores. These techniques are suitable for a wide range of porous materials and also polymers. This instrument comes with a Graphical User Interface (GUI) for control, which also enables both online and offline analysis of the measured data. This makes it is easy to use for material science studies both in the field and in university, research institute, company and even school laboratories. The Peltier cooling gives the precision temperature control and smoothness needed by NMR Cryoporometry, particularly near the probe liquid bulk melting point. Results from example NMR Relaxation and NMR Cryoporometric measurements are given.

Highlights

  • NMR Relaxation (NMRR) is an extremely useful quantitative technique for material science, for studying polymers and porous materials [1,2,3,4,5,6,7,8,9,10,11,12,13]

  • A sample of Barnett shale was measured by NMR Relaxation (NMRR) to obtain an estimate of the quantity and mobility of the hydrocarbons in the pores

  • The NMR Cryoporometry measurements were performed on a purpose built NMR Scanning

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Summary

Introduction

NMR Relaxation (NMRR) is an extremely useful quantitative technique for material science, for studying polymers and porous materials [1,2,3,4,5,6,7,8,9,10,11,12,13]. This paper discusses the use and application of the Lab-Tools Mk3 precision compact NMR time-domain spectrometer for both NMRR, Sections 3.1 and 4, and NMRC, Sections 3.2 and 5 This NMR spectrometer is based on a Field Programmable Gate Array (FPGA). A particular feature of this spectrometer is that it is fast recovery and so can measure NMR Relaxation both in the bulk and in sub-nano-meter and upward sized pores, for materials that may be liquid, gel, waxy, tarry . Progressive changes to the quantity and mobility of hydrocarbons, as well as changes in pore-blocking, as a function of preparation temperature, have been demonstrated [27] All these measurement techniques can be implemented using this recently developed highly compact Spectrometer, based on a Field Programmable Gate array (FPGA) module and custom surface mount low-noise NMR receiver and NMR linear transmitter. Complete with a Graphical User Interface (GUI) for control and online and offline analysis, this instrument has been found to be suitable for material science studies

Apparatus
Temperature Measurement and Control
Key Time-Domain NMR Methods
NMRC History
NMRC Theory
NMRC Protocol
Bulk Ice T2 Measurement
NMR Cryoporometric Measurement on a Sol-Gel Silica
NMR Cryoporometric Measurements on Three Porous Rocks
Measured Instrument Parameters and Capabilities
Conclusions and Suggestions
Diffusion and Controlled Magnetic Field Gradient Experiments
Portability
Patents

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