The start of an experimental section usually comprises a general experimental procedure. The general experimental provides detailed information which contextualises information subsequently provided in the rest of the experimental section. These typically provide information on the instrumentation used to record data, how solvents have been purified and/or dried as appropriate and where chemicals have been procured from.
Often research groups maintain a general experimental which can be used by all their researchers in publications and theses, removing any sections which are not relevant to the work being reported. Below is an example general experimental for Teaching Labs which can be used as a starting point.
Unless otherwise indicated, all reagents listed have been obtained from commercial chemical suppliers or have been prepared via methods included or referenced in the experimental without additional purification. Solvents have been obtained from commercial suppliers, and where indicated as having been dried this refers to purification using a Puresolve solvent purification system. For dried solvents, residual water levels were checked weekly using a Mettler Toledo C20S Karl-Fisher instrument to ensure levels were less than ## ppm for diethyl either, tetrahydrofuran (THF), dichloromethane, toluene, acetonitrile and N,N-dimethylformamide (DMF). If indicated as degassed, the solvents were sparged by the bubbling of nitrogen gas through flasks containing the solvent for at least 15 minutes prior to use. Petrol refers to light petroleum ether fractions with a boiling point range of 40 - 60 °C unless otherwise indicated. Thin layer chromatography (TLC) was carried out using aluminium sheets pre-coated with Merck silica gel 60 F254, and visualised with ultraviolet light (254 nm), and where indicated with alcoholic p-anisaldehyde, alcoholic vanillin or aqueous potassium permanganate stains. Retention factors (Rf) values are reported to two decimal places with measurements having been recorded to the nearest mm. Nuclear magnetic resonance (NMR) spectra were recorded on a Bruker AVIII300NB UltraShield spectrometer operating at 7.04925 Tesla with nuclei recorded at the follow frequencies: ¹H 300 MHz; ¹³C 100 MHz; ¹⁹F 282 MHz; ³¹P 121 MHz. Deuterated NMR solvents were obtained from commercial suppliers. Proton (¹H) NMR was referenced using the residual protic solvent peak to 7.27 ppm (CDCl₃) and using the values from Fulmer et al.¹ for all other solvents. Carbon (¹³C) NMR was referenced for CDCl₃ for the centre peak of the triplet to 77.0 ppm and using the values from Fulmer et al.¹ for all other solvents. Chemical shifts are reported in parts per million (ppm) to the nearest 0.01 ppm for ¹H, or to 0.1 ppm for ¹³C, ¹⁹F and ³¹P nuclei. NMR resonances are reported as follows: chemical shift δ (ppm) (number of protons, multiplicity, coupling constant J (Hz), assignment). The following abbreviations are used for multiplicities: s (singlet); d (doublet); t (triplet); q (quartet). Where multiplicities are unclear, a range is reported for the signals with m indicating a multiplet. Where signals are significantly broadened, this is indicated with br (broad). The coupling constants are quoted as matched coupling constants, averaged where necessary, to the nearest 0.1 Hz and are reported as measured splittings on each individual resonance. ¹³C were verified using Distortionless Enhancement by Polarization Transfer experiments (DEPT-135) to confirm carbon environments. The use of 2D NMR experiments including correlation spectroscopy (¹H-¹H COSY), Heteronuclear single quantum coherence spectroscopy (¹H - ¹³C HSQC) and Heteronuclear multiple-bond correlation spectroscopy (¹H - ¹³C HMBC) were used to aid spectral assignments. Where numbering or text labels are used to assign data to structures this is to aid assignment and does not necessarily follow IUPAC numbering conventions. Infrared spectra were recorded on Bruker Alpha II spectrometers fitted with Platinum Diamond Attenuated Total Reflectance (ATR) QuickSnap Sampling Modules. Data has been recorded and analysed in transmission mode unless otherwise indicated. The frequency of selected absorbance bands is reported in cm⁻¹. Bands for key functional groups are assigned where possible and broad absorbances are indicated (br). Scanning UV-vis spectra were recorded using Thermo Genesis 180 Spectrometers at ambient temperature unless indicated otherwise. Melting point ranges were determined using Digimelt MPA161 or Stuart SMP20 melting point apparatus with values rounded to the nearest °C. Electrospray Ionisation (ESI) and Atmospheric Pressure Chemical Ionisation (APCI) mass spectrometry measurements were recorded using a Bruker Compact Time of Flight (TOF) mass spectrometer and Gas-Chromatography Electrospray Ionisation (GC-EI) measurements were recorded on a JEOL AccuTOF GCx plus mass spectrometer. Gas chromatography (GC) measurements were recorded using Thermo Trace 1300 instruments and High Performance Liquid Chromatography (HPLC) measurements using Agilent 1260 Infinity II Quaternary Pump instruments. Where chromatography has been used, methods are provided within the experimental. X-ray crystal structures were recorded on a Rigaku XtaLAB Synergy or Oxford Diffraction SuperNova diffractometer, with structures deposited in the Cambridge Crystallographic Data Centre (CCDC) with the reference number shown. Detailed information for the data collection and refinement method can be obtained by viewing the CCDC deposition. All novel products or products without fully reported literature data were fully characterised, unless sufficient material was not available and/or decomposition had occurred. Compounds which are known in the literature were confirmed by a minimum of three pieces of characterisation data which were concordant with those reported in the referenced literature source.
¹G. R. Fulmer, A. J. M. Miller, N. H. Sherden, H. E. Gottlieb, A. Nudelman, B. M. Stoltz, J. E. Bercaw, K. I. Goldberg Orgmet., 2010, 29, 2176-2179. DOI:10.1021/om100106e.