Thermo 334610 Refractometer

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Purpose:
To learn techniques for measuring the melting point, boiling point, and refractive indexes of a substance and use these measurements to identify an unknown sample.
Theory and Background: The melting point (mp) of a substance is the temperature range, which can be measured in celsius, Kelvin or Fahrenheit, where said substance moves from the solid to liquid state. If held within that range, the substance could exist in both of these states at once. If the sample is a pure solid it has a sharp mp because of the small temperature range. The new Melt-Temp apparatus was used in this experiment to measure mps. For this apparatus, the capillary tube with the sample is inserted from the side and warmed quickly until it reaches the set plateau. …show more content…

This measurement is quite sensitive to impurities and temperature because every difference within the sample will alter the path of light, effectively slowing or increasing the speed. In this experiment a Thermo 334610 Refractometer was used to find the ri of the same unknown sample used in the bp measurement. Typically ri is measured at 20℃ with the wavelength of the sodium D line. This refractometer maintains this temperature with circulating water through the upper prism. To use the refractometer, a few drops, 1-2, of the unknown should be placed on the lower prism and the upper prism then closed onto the lower one. The lamp is then fully lifted and turned on. Looking through the eyepiece, the hand wheel should be moved so that an image with a light top and a dark bottom can be seen. The compensation dial then brings the line between the 2 colors into focus and the hand wheel used to bring the crosshairs on top of the image onto the focused line. Pushing the switch down, the ri scale will be shown with the crosshairs on the ri of the …show more content…

(Structures from MedLibrary, Illustrated Glossary of Organic Chemistry, Sigma-Alderich, Wikimedia, and Wikipedia)
Summary of Key Data:
Table 1: Melting Points (mp) of the Possible Unknown Samples
(Organic Chemistry 321 & 322 Laboratory Manual)
Name of Compound
Known mp (℃)
Name of Compound
Known mp (℃)
Acetamide
80
Maleic Acid
135
Vanillin
81
Urea
134
M-toluic Acid
113
4-acetamidophenol (or acetaminophen)
171
Benzoic Acid
122
Hydroquinone
172
Benzamide
128

Table 2: Collected Melting Point (mp) Data
Sample
Temperature (℃) at
1st Sign of Melting
Temperature (℃) when
Fully Melted
Known: m-toluic acid
106
109
Unknown # 26
130
134
Unknown #26 + Urea
132
134
Table 3: Boiling Points (bp) and Refractive Indexes (RI) of the Possible Unknowns
(Organic Chemistry 321 & 322 Laboratory Manual)
Name of Compound
Known bp (℃)
Known Refractive Index
Ethanol
78
1.3611
2-Butanol
99
1.3978
1-Butanol
117
1.3988
2-Methyl-1-butanol
131
1.4053
2-Ethyl-1-butanol
147
1.4220
Cyclohexanol
161
1.4641
Table 4: Collected Boiling Point (bp) Data
Reflux Method
Dennis-Thiele Tube Method
Sample
Bp (℃)
Sample
Bp (℃)
Known: Ethanol
79
Known: Ethanol
77
Unknown #15
105

Table 5: Collected Refractive Index (RI) Data
Sample
RI
Unknown # 15

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