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Che 216: Lab 1B / 2A Notes

This document provides information about two chemistry lab experiments: 1) Melting point determination of purified benzil to determine its purity. The procedure involves heating samples in a sealed capillary tube and recording the melting point range. 2) Analysis of mixtures using gas-liquid chromatography (GC). The GC separates components using a stationary and mobile phase. Factors like component structure and column properties affect retention times. For the lab, student groups will analyze unknown mixtures on one of four GCs and use retention times and response ratios to identify the components and calculate their percentages.

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43 views3 pages

Che 216: Lab 1B / 2A Notes

This document provides information about two chemistry lab experiments: 1) Melting point determination of purified benzil to determine its purity. The procedure involves heating samples in a sealed capillary tube and recording the melting point range. 2) Analysis of mixtures using gas-liquid chromatography (GC). The GC separates components using a stationary and mobile phase. Factors like component structure and column properties affect retention times. For the lab, student groups will analyze unknown mixtures on one of four GCs and use retention times and response ratios to identify the components and calculate their percentages.

Uploaded by

patelp4026
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© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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CHE 216: LAB 1B / 2A NOTES

LAB 1B (WEEK 2): Melting Point Determination (Benzil)


LAB 2A (WEEK 1): Analysis of Mixture by Gas-Liquid
Chromatography
A. Melting Point Determination (Purified Benzil)
1. Melting Point (Mohring, pp. 212-220)
a. objective: determine purity of solid compounds
b. melting point range
1) temperature when solid begins to liquefy to temperature when solid
has completely liquefied
2) 0.50 C 2.00 C for relatively pure compound
3) impurities increase range / depress m.p. of pure compound
2. Lab Procedure (Mel-Temp apparatus: Fig 14.3, p. 215)
a. heating rate curves: Course Information Sheet
1) depends directly on voltage setting
2) ideally, 20 C/min rate
c. sample preparation (pp. 215-216)
1) use of sealed-end capillary tube
2) solid should be dry and pulverized; ~2 mm length in capillary tube
d. procedure summary: pp. 217-218 , Mel-Temp file (to be demonstrated by
instructor)
e. Note: published (literature) m.p. values are usually higher due to higher purity
of samples

B. Gas-Liquid Chromatography (GC) (Mohring, pp. 293-308)


1. Basic Components ( Fig. 20.4, p. 294)
a. stationary phase (column): high b.p. liquid coated on inert solid or to
column wall
b. mobile phase (gas): carries vaporized liquid sample through column
2. Column Separation (resolution of component peaks) (Fig. 20.10, p. 299)
a. base-line separation a must
b. sharp , narrow peaks early / broader, wider peaks later
3. Component Retention Time (RT) Factors
a. component structure / polarity / b.p.: low b.p. (more volatile), less polar
compounds elute first
b. column length / diameter / packing polarity: usually, a direct relationship to
RT
c. column T: a indirect relationship to RT
d. carrier gas flow rate: an indirect relationship to R T
Caveat: shorter RT may not always provide optimum resolution

C. Lab Procedure (GC)


1. The GC assignment you will submit at the pre-lab lecture next week will be
returned during the lab.
2. Students work in groups of two. Each group gets one unknown mixture (~4 mL);
record unknown # in lab notebook; unknown has 2 of the possible 4 compounds.
3. GCs: 4 instruments (A-D) ; operation will be demonstrated by instructor.

a. Inject 1 microliter of unknown mixture + 1 microliter of air and obtain


chromatogram print-out (one copy for each group member). Keep this as it will be
submitted with the lab report.
b. Compare retention times of each component peak with those posted for
your specific GC. This will give a tentative indication of the identity of your
unknown mixture components.
c. Using the peak area data along with the calculated response ratios for your
GC, determine the corresponding % values for each mixture component.

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