F The boiling point and C-H analysis for the unknown are listed in Live Data. If the unknown is a solid, the melting point can be measured by clicking on the melting point apparatus to the left of the lab bench and dragging the melting point tube to the unknown in the flask. The melting point will be displayed on the machine, which can be enlarged by hovering over the apparatus or it will also be posted in Live Data. It will also be useful to know the polarity of the unknown by performing a TLC measurement (if you have not previously completed the activity Using Thin Layer Chromatography, please see the note at the bottom of that assignment regarding TLC in Beyond Labz). Record all of this information below. C-H Analysis Melting Point
◻
\deg C
Boiling Point
\deg C
R_(f)=
To collect an FTIR spectrum of your unknown, click on the FTIR spectrometer located to the left of the lab bench and drag the salt plate icon to the flask on the lab bench. A window containing the FTIR spectrum for your product should now open. Identify the relevant peaks in the FTIR spectrum and record the position and associated functional group for each in the FTIR table below. The FTIR spectrum can also be saved to the lab book for later analysis. When entering values for the FTIR please enter them in order from left to right on the spectrum to ensure they match the grading rubric. FTIR List position/ Funtional Group To collect a
^(1)H
NMR spectrum of your unknown, click on the NMR magnet and drag the NMR sample tube to the flask on the lab bench. A window containing the NMR spectrum for your unknown should now open. You can zoom into various portions of the NMR spectrum by clicking and dragging over the desired area. The Zoom Out button is used to zoom back out to view the full spectrum. Identify all of the peaks in the NMR spectrum and record the chemical shift, the splitting, and the number of hydrogens for each peak in the NMR table. The NMR spectrum can also be saved to the lab book for later analysis.
^(13)C
NMR and Mass Spectrometry are also available in the laboratory to help you determine the structure of your unknown.
†
Specify the multiplicity as a singlet
(s)
, doublet
(d)
, triplet
(t)
, quartet
(q)
, or multiplet
(m)
.
$
Specify the number of hydrogens associated with each peak. To perform the functional group tests, click on the unknown and drag a test tube containing the unknown to the clamp over the stir plate. You should see a picture of your unknown in Live Data. Now perform the bromine test by clicking on the reagent bottle labeled
Br_(2)
and dragging the pipet to the test tube (or double click the
Br_(2)
bottle). The results of the test are shown in Live Data with either a picture or a short video clip. Record the results of the test as either positive or negative in the table below. (See your textbook for a description of the functional group tests.) Discard the test tube by dragging it to the red disposal bucket and repeat the procedure for the other functional group tests. Make sure to record all of your results in the table below. Results for Functional Group Tests To perform the functional group tests, click on the unknown and drag a test tube containing the unknown to the clamp over the stir plate. You should see a picture of your unknown in Live Data. Now perform the bromine test by clicking on the reagent bottle labeled
Br_(2)
and dragging the pipet to the test tube (or double click the
Br_(2)
bottle). The results of the test are shown in Live Data with either a picture or a short video clip. Record the results of the test as either positive or negative in the table below. (See your textbook for a description of the functional group tests.)