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Phase Rule: Ternary Liquid System: Save The Titrated Mixtures

1. This document outlines the procedure for determining the solubility curve and tie lines for a ternary liquid system using isopropyl alcohol, benzene, and water. 2. The procedure involves preparing mixtures of varying compositions and determining the cloud point with added water. Refractive indices are measured to plot the solubility curve. Conjugate solutions are formed and refractive indices are measured to determine tie line compositions. 3. Safety precautions when working with chemicals include understanding hazards, treating all chemicals as dangerous, relying on instructor suggestions for chemical pairs, being trained on equipment, and calibrating equipment.

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Marthy Dayag
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55 views

Phase Rule: Ternary Liquid System: Save The Titrated Mixtures

1. This document outlines the procedure for determining the solubility curve and tie lines for a ternary liquid system using isopropyl alcohol, benzene, and water. 2. The procedure involves preparing mixtures of varying compositions and determining the cloud point with added water. Refractive indices are measured to plot the solubility curve. Conjugate solutions are formed and refractive indices are measured to determine tie line compositions. 3. Safety precautions when working with chemicals include understanding hazards, treating all chemicals as dangerous, relying on instructor suggestions for chemical pairs, being trained on equipment, and calibrating equipment.

Uploaded by

Marthy Dayag
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as DOCX, PDF, TXT or read online on Scribd
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1.

Laboratory experimental procedure and safety issues

PHASE RULE: TERNARY LIQUID SYSTEM

Chemicals:

Iso-propyl alcohol, benzene.


Other pairs of liquids suitable for the experiment, may be suggested by the instructor.

Apparatus:

Stoppered Erlenmeyer flasks (125 ml)


Constant temperature water bath (25.0 + 0.1oC)
Refractometer

Procedure:

I. Determination of the solubility limits.

1) Prepare eleven mixtures of benzene and anhydrous iso-propyl alcohol, of a wide


range of composition. Deliver the necessary amounts into clean dry stoppered
Erlenmeyer flasks from burets.

2) Place the flasks and one containing distilled water in a constant temperature
water bath (25.0 + 0.1oC) and allow enough time to establish thermal equilibrium
(15 to 20 minutes).

3) Titrate each mixture, carefully and slowly, with distilled water (at 25.0 + 0.1 oC)
until the first permanent turbidity appears. The composition of this cloud point is
on or near the solubility curve.
It is important to shake the mixture vigorously after each addition with
water. Air bubbles formed by shaking must not be confused with a cloud
point.
To expedite the titration, withhold about 1-2 mL of the alcohol from the
initial mixture; titrate rapidly with distilled water until the cloud point is
reached, then add the remaining alcohol and continue titration to the
cloud point.

4) Measure the refractive index of each titrated mixture.


• Save the titrated mixtures.

II. Determination of the tie lines.


1) After completion of step I add excess distilled water, (about 2 ml) delivered by a
burette, to at least six or seven of the titrated mixtures. Allow sufficient time, in a
constant temperature water bath, for the two conjugate phases to separate into two
layers (one hour and preferably longer).

NOTE: The volumes of each layer must be large enough to sample for analysis,
thus do not use the mixture with the smallest benzene amount.

Alternately, prepare conjugate solutions of a wide range of composition.

2) Analyze each layer of each solution by measuring the refractive index.

Samples may be removed from the conjugate solutions for refractive index
measurements as follows:

Upper layer - use a disposable pipet. Don't insert the dropper tip too close to the
interface between the two layers.

Lower layer - when inserting the pipet through the upper layer squeeze the bulb
gently to prevent liquid from entering the dropper. Upon
withdrawing likewise squeeze gently so that a small amount
of the sample is lost into the upper layer.

Transfer the samples into small vials and stopper the vials immediately.

Treatment of results:

I. Determination of the solubility curve

1) Calculate the composition, in


weight percent, of each mixture at the cloud point.

2) Tabulate data including


refractive index, volume and weight percent of each component in each mixture.

3) Construct the solubility curve


on a triangular coordinate graph paper.

5) Interpret the meaning of the areas


bounded by the curve and of various selected points marked clearly on the
diagram. This would include points in the two regions, on the solubility curve and
at the plait point. Apply the phase rule in your interpretation.

AI. Refractive Index - Composition Calibration Curve


1. Fasten a sheet of rectangular coordinate graph paper to the triangular graph
paper with the long side parallel and level with to the triangle base line.

2. Construct a refractive index scale on the y-axis of the rectangular paper.


Maximize its range, but use only about half of the length of the vertical axis.

3. Plot the calibration curve points at the intersection of a vertical projection from
each cloud point composition and its refractive index.

4. To determine the composition of a given solution, locate its refractive index on


the calibration curve, and project downward to the solubility curve.

III. The tie lines

1. Use the refractive index calibration curve and the refractive indices of the
conjugate solutions to determine the intersection of the tie lines with the
solubility curve. Follow the projection procedure in step II (4) and mark the
compositions on the solubility curve.

2. Connect the two points of each conjugate pair of solutions to obtain the
corresponding tie line.

3. On a separate graph paper plot the weight percent of alcohol in the benzene-rich
layer as ordinate vs. the weight percent of alcohol in the water-rich layer as
abscissa, for the conjugate solutions. Draw 45o line through the origin, it
represents equal distribution. Comment on the distribution ratio in this system.

Safety issues:
 Before you start an experiment, make sure you are fully aware of the hazards of
the materials you will be using.
 Every chemical should be treated as though it were dangerous.
 Pairs of liquids suitable for experiment must rely on the suggestion of your
instructor.
 Never use lab equipment that you are not approved or trained by your
instructor.
 Familiarity in the equipment that will be utilized is a MUST.
 Calibration of equipment is a MUST.

2. Examples of the three systems discussed. Identify which liquids are miscible and which
are not miscible.
a. One partially miscible pair
Water and benzene + ethanol (water is miscible with ethanol but
immiscible with benzene, likewise benzene is miscible with ethanol but
immiscible with water)
b. Two partially miscible pairs
Water, phenol, aniline ( water is miscible with phenol but immiscible with
aniline)
c. Three partially miscible pairs
Trichloroethane, water, acetone (Trichloroethane dissolves completely in
acetone but immiscible in water, likewise water dissolves in acetone but
immiscible with Trichloroethane)

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