Summary
In our latest post, we introduce something that should be known before doing H NMR experiment. Now here we are going to describe the steps of this experiment.
Steps and details
Requirements of sample tube
NMR sample tube is a kind of dedicated sample tube, which is made of good-quality glass temperature and also the use of quartz or polytetrafluoroethylene (PTFE) material. Requirements of the sample tube are non-magnetic, wall straight and uniform thickness.
The sample tube is cylindrical shape, the diameter of the sample tube depends on the type of spectrometer probe. Its outer diameter can be as small as 1mm or as large as 25mm. Common sample tube’s diameter are 5mm, 10mm, 2.5mm. Length is more than 150mm.
The sample tube used here is 5mm.
Sample preparation and requirements
Since NMR is a method of qualitative analysis, the amount of the sample’s drift amount has no strict requirement. The principle is: In the case of analysis requirement, few samples should be much better. Sample with large concentration and the spectrum with spinning side bands or large satellite peak and poor spectral resolution are not conducive to spectra analysis.
5mg solid samples; 0.05ml liquid sample
Putting sample into a sample tube with 0.5ml CDCL3 and making sample dissolve completely. Mixing the sample with a reagent, generating a clear solution, transparent, no suspended solids or other impurities.
Turn on the machine
Turning on the computer and entering the appropriate power-on password.
Running CPU monitoring program.
Open cabinet power, total power→BSMS/2 power supply→BLAX300/1 Power→BLAX300/2 power supply→AQS
Entering into NMR program: Double-click: Desktop TOPSPIN 3.1.
Initialization: Type: CF↙
Instrument’s self-test and initial state settings.
Standard sample is placed in a magnetic field and in magnets.
Transferred spectrum done before, type: ii↙. Initializatiing sampling parameters
Adjustment of instrument status
These are the main steps and some details of the H NMR experiments.
In our latest post, we introduce something that should be known before doing H NMR experiment. Now here we are going to describe the steps of this experiment.
Steps and details
Requirements of sample tube
NMR sample tube is a kind of dedicated sample tube, which is made of good-quality glass temperature and also the use of quartz or polytetrafluoroethylene (PTFE) material. Requirements of the sample tube are non-magnetic, wall straight and uniform thickness.
The sample tube is cylindrical shape, the diameter of the sample tube depends on the type of spectrometer probe. Its outer diameter can be as small as 1mm or as large as 25mm. Common sample tube’s diameter are 5mm, 10mm, 2.5mm. Length is more than 150mm.
The sample tube used here is 5mm.
Sample preparation and requirements
Since NMR is a method of qualitative analysis, the amount of the sample’s drift amount has no strict requirement. The principle is: In the case of analysis requirement, few samples should be much better. Sample with large concentration and the spectrum with spinning side bands or large satellite peak and poor spectral resolution are not conducive to spectra analysis.
5mg solid samples; 0.05ml liquid sample
Putting sample into a sample tube with 0.5ml CDCL3 and making sample dissolve completely. Mixing the sample with a reagent, generating a clear solution, transparent, no suspended solids or other impurities.
Turn on the machine
Turning on the computer and entering the appropriate power-on password.
Running CPU monitoring program.
Open cabinet power, total power→BSMS/2 power supply→BLAX300/1 Power→BLAX300/2 power supply→AQS
Entering into NMR program: Double-click: Desktop TOPSPIN 3.1.
Initialization: Type: CF↙
Instrument’s self-test and initial state settings.
Standard sample is placed in a magnetic field and in magnets.
Transferred spectrum done before, type: ii↙. Initializatiing sampling parameters
Adjustment of instrument status
These are the main steps and some details of the H NMR experiments.