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1 Calibration of the Thermometer:
Objective:
Determine the melting points of standard substances to calibrate the thermometer.
Find the difference between the observed values and the expected values for future correction.
1.
Ex) Naphthalene (a): Expected melting point = 80°C, Observed melting point = 82°C
2.
Urea (b): Expected melting point = 133°C, Observed melting point = 135°C
3.
4-Toluic acid (d): Expected melting point = 182°C, Observed melting point = 180°C
For each substance, calculate the correction by subtracting the observed melting point from the expected melting point:
1.
Naphthalene (a):
Correction = 80°C - 82°C = -2°C
2.
Urea (b):
Correction = 133°C - 135°C = -2°C
3.
4-Toluic acid (d):
Correction = 182°C - 180°C = +2°C
Now, calculate the average correction:
Average Correction=(−2)+(−2)+23=−0.67 °CAverage Correction=3(−2)+(−2)+2=−0.67°C (means our thermometer reads temperatures .67 C higher than normal.)
Procedure:
1.
Use the provided standards (Naphthalene, Urea, Sulfanilamide, 4-Toluic acid, Anthracene, and Caffeine) with known melting points.
2.
Determine the melting points over the temperature range of interest.
3.
Calculate the differences between the observed and expected melting points.
4.
Apply corrections to future temperature readings if needed.
5.
If the thermometer has been calibrated previously, determine one or more melting points for further familiarization.
6.
If determinations do not agree within 1°C, repeat the calibration process.
Calibration of the Thermometer (Step 1 in Experimental Procedures):
1.
Select Standard Substances:
Choose standard substances with known melting points from Table 3.1.
2.
Determine Melting Points:
Crush the sample to a fine powder.
Fill a melting point capillary with the powdered sample.
Heat the bath, and note the temperature range where the sample melts.
3.
Calibration:
Record the observed melting points and compare them with the expected values.
Determine the correction that must be applied to future temperature readings.
Note:
Both mercury-in-glass and digital thermometers need to be calibrated.
Non-mercury thermometers are typically not used for melting point determination.
2. Melting Points of Pure Urea and Cinnamic Acid:
Objective:
Determine the melting points of pure Urea and Cinnamic Acid.
Procedure:
1.
Crush the sample to a fine powder using a metal spatula on a hard surface (watch glass).
2.
Insert the open end of a melting point capillary into the powder.
3.
Force the powder down the capillary by tapping or dropping it through a long glass tube held vertically on a hard surface.
4.
Ensure the column of solid is no more than 2–3 mm in height and is tightly packed.
5.
If the approximate melting temperature is known, heat the bath rapidly until 20°C below this point.
6.
Slow down heating during the last 15–20°C, ensuring the rate of heating at the melting point is no more than 1°C per minute.
7.
Observe the melting process, starting from the appearance of the first drops of liquid in the capillary until the last trace of solid disappears.
8.
Repeat the determination for either Urea or Cinnamic Acid.
9.
If the two determinations do not check within 1°C, repeat a third time.
3. Melting Points of Urea—Cinnamic Acid Mixtures:
Objective:
Observe melting point depression and prepare a phase diagram.
Procedure:
1.
Make mixtures of Urea and Cinnamic Acid in proportions 1:4, 1:1, and 4:1.
2.
Place equal-sized small piles of the two substances side by side and mix them.
3.
Grind the mixture thoroughly for at least a minute on a watch glass using a metal spatula.
4.
Note the ranges of melting for the three mixtures.
5.
Use temperatures of complete liquefaction to construct a rough diagram of melting point versus composition, similar to Figure 3.5.
Note:
Pay attention to the dramatic evidence of melting point depression in the mixtures.
Lab Work Overview:
1.
Calibrate the Thermometer:
Use standard substances with known melting points.
Apply corrections for future readings.
2.
Determine Melting Points of Pure Substances:
Crush, fill, and determine the melting points of either Urea or Cinnamic Acid.
3.
Observe Melting Point Depression:
Create mixtures of Urea and Cinnamic Acid.
Record melting points for each mixture.
Construct a rough diagram of melting point versus composition.
4. Unknowns:
Objective:
Determine the melting point of one or more unknown substances selected by the instructor.
Identify the substance based on its melting point using the provided table (Table 3.2).
Procedure:
1.
Select one or more unknown substances as instructed by your instructor.
2.
Prepare two capillaries for each unknown.
3.
Run a fast determination on the first sample to ascertain the approximate melting point.
4.
Quickly cool the melting point bath to just below the melting point.
5.
Conduct a slow and careful determination using the second capillary.
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Note:
The goal is to identify the unknown substance based on its melting point, which should match one of the values in Table 3.2.
5. Investigation: Determination of Molecular Weight Using Melting Point Depression:
Objective:
Determine the molecular weight of an unknown substance using the molal freezing point depression of camphor.
Procedure:
1.
Background:
Mass spectrometers were not commonly used for determining molecular weights in the past.
Molal freezing point depression of camphor was used for this purpose.
2.
Relationship:
A 1% solid solution of urea in cinnamic acid causes a relatively small melting point depression.
A 1%-by-weight solid solution in camphor of any organic compound with a molecular weight of 100 will cause a 4.0°C depression in the melting point of camphor.
3.
Quantitative Use:
Prepare a 1% by weight solid solution of the unknown substance in camphor.
Measure the melting point depression of camphor caused by the addition of the unknown substance.
Use the relationship to determine the molecular weight of the unknown substance.
Note:
Utilize the provided information about the melting points of unknown compounds in Table 3.2 to
identify the substance selected for this investigation.
Table 3.2 Melting Point Unknowns:
Use the melting point of the unknown substance to identify it in the context of the investigation.
Lab Work Overview:
1.
Unknowns Determination:
Identify the melting point of unknown substances and match them with the values in Table 3.2.
Run both fast and slow determinations to confirm the accuracy of the results.
2.
Molecular Weight Investigation:
Understand the background and rationale for determining molecular weight using melting point depression.
Prepare a 1% by weight solid solution of the unknown substance in camphor.
Measure the melting point depression and use the relationship to determine the molecular weight of the unknown.
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