Undergraduate chemistry education with Spinsolve benchtop NMR
Spinsolve is the perfect way to provide high throughput NMR as part of an undergraduate teaching program. The high sensitivity and advanced capability means it is fast and informative, critically important for a busy class. Spinsolve provides convenient, high performance NMR at a fraction of the cost of traditional NMR systems. The small footprint of the instrument means that it can be placed on the bench in the lab, right next to where students prepare their samples. The stray magnetic field is completely contained within the instrument case, so there is no risk of wiping credit cards or damaging watches.
Thanks to the exceptional sensitivity, students can obtain informative spectra within a minute of sample preparation. This is important for large laboratory classes, where often hundreds of samples need to measured by students. The operating costs are very low, as no liquid cryogens are required. Deuterated solvents are not necessary, and low-cost budget NMR tubes can be used.
Spinsolve software is beautiful and intuitive which means it can be easily operated by anyone in the chemistry lab with minimal training. Most experiments can be run with a single click of a button. Switching between experiments also involves a single click. This simple, easy to use operation reduces time spent learning how to operate the system and increases throughput.
When first being exposed to NMR, many students find it difficult to understand and distinguish between chemical shift and j-coupling. Two-dimensional NMR experiments project additional information into a second dimension, which tremendously facilitates the interpretation of NMR spectra. Spinsolve supports 2D COSY and homonuclear j-resolved experiments.
Getting NMR into the hands of students at an early stage is just part of the evolution in the world of NMR. The launch of the benchtop NMR spectrometers like the Spinsolve series of instruments has changed the face of education in chemistry with institutes around the world being able to adopt a low-cost, low-maintenance system to bring practical teaching into undergraduate teaching laboratories.
“Now the students are able to acquire their own NMR spectra as well as carry out the analysis of the compounds they have made. This makes their undergraduate experiment more applicable to both research and industry settings and increases their enthusiasm for chemistry.” -Professor Frances Separovic, Head of Chemistry at the University of Melbourne
The following lab manuals are available for download:
– Identification of the Isomers of C4H8O2: This is a laboratory where students acquire their own spectra and utilise basic concepts of NMR. The lab involves analysis of 1H NMR spectra in order to identify the structure of different isomers with the chemical formula C4H8O2.
– Distinguishing Between the Isomers of C4H8O2: This laboratory involves analysis of 1H NMR spectra in order to distinguish between ethyl acetate, butyric acid and isobutyric acid, the structural isomers of C4H8O2. This experiment is aimed at students interpreting real NMR spectra for the first time.
– Composition of Some Common Household Products: This experiment is an adaptation of an experiment carried out at RMIT in Melbourne by final-year high school students. The aim of the experiment is to introduce 1H-NMR spectroscopy to students as a tool to identify the organic compounds in some common household products, such as nail polish remover and vinegar. This experiment can be adapted for slightly more advanced students by introducing percent composition by NMR.
– Introduction to 13C-NMR and DEPT – Identification of an Alcohol: This experiment utilises the identification of alcohols by 13C-NMR spectroscopy as a means to introduce students to NMR spectroscopy for the first time. 1H-decoupled 13C-NMR spectra are simple to interpret and the use of alcohols, with well separated peaks in the 13C-NMR spectrum, allows students to acquire their own spectra, correlate chemical shift with electronegativity and apply nomenclature for naming organic compounds.
– Synthesis and Reactions of Ferrocene: This experiment aims to provide experience in the synthesis, isolation, purification and characterisation of organometallic compounds. Purification techniques include distillation, sublimation, chromatography and crystallisation. Students will also develop their synthetic skills using inert atmosphere techniques.
– Synthesis of p-Nitroaniline via a Multi-Step Sequence: Here students gain experience in the synthesis, isolation, purification and characterisation of simple aromatic compounds. In particular, they will study aromatic substitution reactions in which functional groups greatly influence further substitution of monosubstituted benzenes. The main characterisation technique utilised in these experiments is 1H NMR spectroscopy using the Spinsolve benchtop NMR spectrometer.
– Extraction of Essential Oils from Spices using Steam Distillation: Students will isolate and purify the key chemical compounds that contribute to the aroma and flavour of the spices. The compounds will then be characterised by 1D and 2D NMR spectroscopy.
– Separation of Acidic, Basic and Neutral Compounds: Students will gain practical experience in the separation and purification of simple organic compounds using liquid/liquid extraction and acid/base extraction techniques. The various separation steps will be followed by 1H NMR spectroscopy to determine and characterise the compounds present.
– Measuring Lipophilicity with NMR: In this experiment the 1-octanol/water partition coefficient (Pow) of some common solvents will be measured. Students will quantify the amount of the chosen analyte in water before and after the addition of 1-octanol layer by NMR spectroscopy. This information will allow the calculation of the Pow and log(Pow) of the analytes.
– The Aldol Condensation: The objective of this experiment is to understand aspects of carbonyl chemistry and carbon-carbon bond formations using the classical, well-known aldol condensation reaction as an example. One- and two-dimensional NMR spectra will be used to characterise the reaction products and evaluate their chemical structure and geometry.
– Synthesis of Aspirin: The synthesis of aspirin is a common undergraduate laboratory experiment that introduces students to the synthesis of a pharmaceutical product and the importance and assessment of purity. In this laboratory an additional step in the synthesis has been added to introduce students to multi-step synthesis and the idea of converting a naturally occurring substance to one of therapeutic value. 1H NMR spectroscopy is used to assess the purity of their product and intermediates and give students experience in reporting the structures.
– Preparation and Characterisation of Metal Acetylacetonate Complexes: The aim of this experiment is for students to synthesise a metal acetylacetonate complex, understand the ketol-enol tautomerisation of acetylacetone and determine the electronic structure of their compound using Evans method and the Spinsolve NMR spectrometer.
– Determination of Lewis Acidity using 31P NMR: The aim of this experiment is to use NMR to evaluate Lewis acidity of solvents using the Gutmann-Beckett Acceptor Number. Triethylphosphine oxide is used as a 31P NMR probe. The acceptor number of classic Lewis acids such as boron trihalides may be determined by advanced chemistry students or as ademonstration.