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Experiment No.

Determination of Molar Refraction of a Given Sample

Refractometry

A Research Study Presented to the

Faculty of the Department of the Chemical Engineering

School of Engineering and Architecture

Saint Louis University

In Partial Fulfilment of the Requirements for the Degree

Bachelor of Science in Chemical Engineering

By:

Bullago, Joshua G.

Domalanta, Marcel Roy B.

Caw-is, Imee A.

February 2017
ACKNOWLEDGEMENT

The researchers would like to extend their warmest gratitude to everyone who

contributed for the success of this experiment:

To Engr. Genevieve De Vera, for providing deeper understanding of the topic to the

researchers by explaining the theory and principles related to the experiment, as well as the

different procedures that must be carried out.

To the laboratory custodians, for supervising and assisting the researchers in using the

instruments needed for the experiment.

To God, for giving the researchers the strength and patience to perform the

experiment as best they could.


TABLE OF CONTENTS

TITLE PAGE i

ACKNOWLEDGEMENT ii

TABLE OF CONTENTS iii

LIST OF TABLES iv

LIST OF FIGURES v

ABSTRACT vi

Chapter 1: INTRODUCTION 1

Chapter 2: DESIGN AND METHODOLOGY 5

Chapter 3: RESULTS AND DISCUSSION 6

Chapter 4: CONCLUSION AND RECOMMENDATION 10

REFERENCES 11

APPENDICES 12
LIST OF TABLES

Table 3.1: Molar refraction of samples


LIST OF FIGURES

Figure 2.1: Schematic diagram of procedures

Figure D.1: The refractometer used for the experiment

Figure D.2: Some reagents used for the experiment

Figure D.3: Looking through the refractometer

Figure D.4: Displaying the index of refraction reading


ABSTRACT
Chapter 1

INTRODUCTION

The speed of light in a vacuum is always the same, but when light moves through any

other medium it travels more slowly since it is constantly being absorbed and reemitted by

the atoms in the material. The ratio of the speed of light in a vacuum to the speed of light in

another substance is defined as the index of refraction (aka refractive index or n) for the

substance.

Whenever light changes speed as it crosses a boundary from one medium into another

its direction of travel also changes, i.e., it is refracted (Figure 1). (In the special case of the

light traveling perpendicular to the boundary there is no change in direction upon entering the

new medium.) The relationship between light's speed in the two mediums (vA and vB), the

angles of incidence (qA) and refraction (qB) and the refractive indexes of the two mediums

(nA and nB) is shown below:

Thus, it is not necessary to measure the speed of light in a sample in order to

determine its index of refraction. Instead, by measuring the angle of refraction, and knowing

the index of refraction of the layer that is in contact with the sample, it is possible to

determine the refractive index of the sample quite accurately. The refractive index of

different substrates measures with refractometers. There are four main types of

refractometers: traditional handheld refractometers, digital handheld refractometers,

laboratory or Abbe refractometers, and inline process refractometers. There is also the
Rayleigh Refractometer used (typically) for measuring the refractive indices of gases.A

sodium lamp may be used to provide the light source at a known wave-length (589.6 nm)

although many instruments are corrected for daylight use. Nearly all refractometers utilize

this principle, but may differ in their optical design. In the Abbe' refractometer the liquid

sample is sandwiched into a thin layer between an illuminating prism and a refracting prism

(Figure 2). The refracting prism is made of a glass with a high refractive index (e.g., 1.75)

and the refractometer is designed to be used with samples having a refractive index smaller

than that of the refracting prism. A light source is projected through the illuminating prism,

the bottom surface of which is ground (i.e., roughened like a ground-glass joint), so each

point on this surface can be thought of as generating light rays traveling in all directions.

Inspection of Figure 2 shows that light traveling from point A to point B will have the largest

angle of incidence (qi) and hence the largest possible angle of refraction (qr) for that sample.

All other rays of light entering the refracting prism will have smaller qr and hence lie to the

left of point C. Thus, a detector placed on the back side of the refracting prism would show a

light region to the left and a dark region to the right.

Samples with different refractive indexes will produce different angles of refraction

(see Equation 2 above and recall that the angle of incidence and the refractive index of the

prism are fixed) and this will be reflected in a change in the position of the borderline

between the light and dark regions. By appropriately calibrating the scale, the position of the

borderline can be used to determine the refractive index of any sample. In an actual Abbe'

refractometer there is not a detector on the back of the refracting prism, and there are

additional optics, but this is the essential principle. (It is also possible to design a

refractometer based on the reflection of light from the boundary between the prism and the

sample. These types of refractometers are often used for continuous monitoring of industrial

processes.)
In most liquids and solids the speed of light, and hence the index of refraction, varies

significantly with wavelength. (This variation is referred to as dispersion, and it is what

causes white light moving through a prism to be refracted into a rainbow. Shorter

wavelengths are normally refracted more than longer ones.) Thus, for the most accurate

measurements it is necessary to use monochromatic light. The most widely used wavelength

of light for refractometry is the sodium D line at 589 nm. If white light were used in the

simple Abbe' refractometer optics shown in Figure 2, dispersion would result in the light and

dark borderline being in different places for different wavelengths of light. The resulting

"fuzziness" of the borderline would make precise work impossible. However, many Abbe'

refractometers are able to operate satisfactorily with white light by introducing a set of

"compensating prisms" into the optical path after the refracting prism. These compensating

prisms are designed so that they can be adjusted to correct (i.e., compensate for) the

dispersion of the sample in such a way that they reproduce the refractive index that would be

obtained with monochromatic light of 589 nm, the sodium D line.

As mentioned earlier, the speed of light in a substance is slower than in a vacuum

since the light is being absorbed and reemitted by the atoms in the sample. Since the density

of a liquid usually decreases with temperature, it is not surprising that the speed of light in a

liquid will normally increase as the temperature increases. Thus, the index of refraction

normally decreases as the temperature increases for a liquid (Table 1). For many organic

liquids the index of refraction decreases by approximately 0.0005 for every 1 °C increase in

temperature. However for water the variation is only about -0.0001/°C.

Many refractometers are equipped with a thermometer and a means of circulating

water through the refractometer to maintain a given temperature. Most of the refractive index

measurements reported in the literature are determined at 20 or 25 °C.


The study aims to identify the different refractive indices of each of the following

substance at particular temperature: chloroform, ethyl acetate, butanol, benzene, sugar

solution and carbon tetrachloride.

Refractive index has the large number of applications. It is mostly applied to identify

a particular substance, confirm its purity, or measure its concentration. Generally it is used to

measure the concentration of a solute in an aqueous solution. For a solution of sugar, the

refractive index can be used to determine the sugar content (Brix degree). It can be used also

in determination of drug concentration in pharmaceutical industry. It is used to calculate the

focusing power of lenses, and the dispersive power of prisms. Also it is applied for estimation

of thermophysical properties of hydrocarbons and petroleum mixtures. As can be seen in the

above rows, the study on refractive index of substrates can be useful in various fields (both

industry and academic).


Chapter 2

DESIGN AND METHODOLOGY

The following sets of apparatus were used in the experiment: Abbe

refractometer, medicine droppers, small beaker. On the other hand, the following reagents

and materials were used: cotton, ethyl acetate, benzene, chloroform, butanol, sugar solution,

ethyl alcohol and carbon tetrachloride.

Calibration with distilled water was first done by the laboratory supervisor. Distilled

water using glass dropper was placed on the prism surface of the refractometer. It remained to

stand for at least three to five minutes for temperature stability. The turn mode selector was

shifted to refractive index option. The eyepiece is then focused until crosshair is clear. The

adjustment control was rotated counterclockwise so that the shadow line an crosshair meet.

The dispersion correction wheel is also rotated until a possible color free shadow line is

produced. Then the shadowline is adjusted to meet the crosshair. The red button and

temperature button were pressed.

To calibrate further, the mode selector is turned to BX-TC position. The “read” display

button was pressed. An LED reading of 000.0 or 0.1 is normal. A negative sign and decimal

point however will indicate no reading. If this persists, the adjustment control unit must bte

turned until a normal reading can be displayed. Only slight adjustment is required. Reading

through the reticle crosshair to shadowline, should measure 000.0. The process is repeated

until persistent normal readings occur.

Determining the refractive index of the substance has now been made possible. The

prism assemble cover is then opened and the protective lens tissue removed. The measuring

prism surface is cleaned with cotton and alcohol before any sample has been placed. The

mode selector is put to desired position. Adjustment control was turned counterclockwise to
position the shadowline at bottom of field of view. The shadowline is in center and is in

center to crosshair for accurate reading. The eyepiece is also adjusted to focused on crosshair.

The shadowline is moved to crosshair reticle through coarse adjustment knob. The dispersion

correction wheel has been rotated to eliminate any red or green color at edge of shadownline.

After such conditions are met, the molar refraction was calculated.

Proper laboratory guidelines were followed on disposing some excess samples and on

handling the excess unknown liquid. The sets of apparatus were cleaned thoroughly with

water and detergent.

FIGURE 2.1 Schematic diagram of procedures


Chapter 3

RESULTS AND DISCUSSION

A. RESULTS

Table 3.1. Molar refraction of samples

Sample n = Index of M= ρ = Density T= Rm = Molar


refraction Molecular (g/cm3) Temperature refraction
weight (0C) (cm3/mol)
(g/mol)
Chloroform 1.4439 119.378 1.4968 20.3 21.813
Ethyl Acetate 1.3718 88.105 0.8999 20.3 22.2411
Butanol 1.3980 74.122 0.8089 21.1 22.1158
Benzene 1.4991 78.112 0.8768 21.9 26.1622
Sugar Solution 1.3367 342 1.02 23.0 69.6632
Carbon 1.4581 153.82 1.59 22.7 26.4022
Tetrachloride

B. DISCUSSION

The Abbe Refractometer used was very precise, accurate and fast in acquiring the

respective indexes of refraction of the solutions to be analyzed. Using the equipment, the

values needed for the computation for the molar refraction was easily taken. When adjusting

the eyepiece, there is a dependence on the clarity and focus of the sample with the eyes of the

person manipulating the refractometer because what is clear to one person may not on the

other. When adjusting the dispersion correction wheel, there is a great deal to make sure the

crosshair is adjusted properly. The refractive index of a liquid varies with temperature that is

why there is a must for the researchers to make use of the proper density of the liquid to be

analyzed in the proper temperature scale. These values were calculated given the constants

given in the Perry’s Chemical Engineers’ Handbook. The molar mass values were also taken

in the handbook.

The molar refraction was then computed given the formula and the following solution

and calculations can be seen in the Appendix Section C.


Chapter 4

CONCLUSION AND RECOMMENDATION

Refractometry is a technique that measures how light is refracted when it passes

through a given substance. The amount by which the light is refracted determines the

refractive index. Refractive index can be used to identify an unknown liquid compound.

Refractive index is defined as the ratio of the velocity of light in air to the velocity of light in

the medium being measured. In the experiment the refractometer used was able to determine

the index of refraction of Chloroform, Benzene, Ethyl acetate, Sugar solution, Butanol, and

Carbon tetrachloride as well as its temperature. The mode in the refractometer was already

settled and was ready to use. The sample solution was placed to the prism using a dropper

and the prism was closed. Adjustments in both the dispersion correction wheel and the

eyepiece was needed primary to the control knob before reading the output value. Since the

index of refraction depends on the temperature and the pressure the density at a given

temperature was used to correct and achieve the molar refraction of the samples. Combining

refractive index and substance density it is possible to define a quantity that is temperature

independent. It is called specific refraction and multiplying it with the molar mass gave the

molar refraction results in the experiment. The experiment enabled the researchers to

successfully manipulate and operate the refractometer as well as determining the molar

refraction of different samples while critically capturing the underlying principles of

refractometry.

To limit the errors in determining the molar refraction by means of the refractometer,

the following should be observed; the prism must be wiped properly and cleaned with alcohol

followed by distilled water to avoid contaminants in the sample, do not wipe the prism dry to

avoid any residue in the prism that can affect the accuracy of the reading, when rotating the
eyepiece to focus the crosshair, one person can see the crosshair more clearly than another

because of human error and visible clarity and it is suggested that only one should operate per

liquid, and the shadow line must also be made sure to be below the field of view. When

proper care and correct procedure is followed and exercised using the refractometer, this

equipment can be used for highly accurate and precise determination of the refractive index

of materials that can help to determine the specific refraction and molar refraction of a

sample.
REFERENCES

Hanson, J. (2006). Refractometry.

Koohyar F (2013) Refractive Index and Its Applications. Journal of

Thermodynamics and Catalysis


APPENDIX A

List and Uses of Apparatus

Abbe Refractometer - is a highly reliable instrument with high precision that is used to

measure the refractive index of liquid samples.

Medicine Dropper- a laboratory apparatus used to transfer samples through suction of the

liquids in and out of the dropper.

Small Beaker- a laboratory apparatus used mainly as containers for the liquid samples and

cleaning agent
APPENDIX B

Definition of Terms

Refraction- is the bending of a wave when it enters a medium where its speed is different.

Refractometry- is a technique that measures how light is refracted when it passes through a

given substance.

Refractometer- is an instrument that measures the extent to which light is bent, or refracted,

when it moves from air into a sample and is typically used to determine the index of

refraction of a sample.

Refractive index- also known as the index of refraction, this is defined as the speed of light in

vacuum divided by the speed of light in the medium.

Specific Refraction- is a parameter characterizing the electronic polarizability of a unit mass

of a substance in the high-frequency electromagnetic field of a light wave.

Molar Refraction- indicates the manner in which a molecule interacts with light. This is a

function of the density of the medium.


APPENDIX C

Computations

Molar refraction, Rm, is calculated by the formula:

(𝑛2 − 1)𝑀
𝑅𝑚 =
(𝑛2 + 2)𝜌

Where: M = molecular weight; ρ = density of the substance; n = index of refraction

For Chloroform:

𝑔
(1.44392 − 1)(119.378 ) 𝑐𝑚3
𝑅𝑚 = 𝑚𝑜𝑙 = 21.8130
𝑔 𝑚𝑜𝑙
(1.44392 + 2)(1.4968 3 )
𝑐𝑚

For Ethyl Acetate:

𝑔
(1.37182 − 1)(88.105 ) 𝑐𝑚3
𝑅𝑚 = 𝑚𝑜𝑙 = 22.2411
𝑔 𝑚𝑜𝑙
(1.37182 + 2)(0.8999 )
𝑐𝑚3

For Butanol:

𝑔
(1.39802 − 1)(74.122 ) 𝑐𝑚3
𝑅𝑚 = 𝑚𝑜𝑙
𝑔 = 22.1158 𝑚𝑜𝑙
(1.39802 + 2)(0.8089 )
𝑐𝑚3

For Benzene:

𝑔
(1.49912 − 1)(78.112 ) 𝑐𝑚3
𝑅𝑚 = 𝑚𝑜𝑙 = 26.1622
𝑔 𝑚𝑜𝑙
(1.49912 + 2)(0.8768 )
𝑐𝑚3

For Sugar Solution:

𝑔
(1.33672 − 1)(342 ) 3
𝑅𝑚 = 𝑚𝑜𝑙 = 69.6632 𝑐𝑚
𝑔 𝑚𝑜𝑙
(1.33672 + 2)(1.0200 )
𝑐𝑚3

For Carbon Tetrachloride:

𝑔
(1.45812 − 1)(153.82 ) 𝑐𝑚3
𝑅𝑚 = 𝑚𝑜𝑙 = 26.4022
𝑔 𝑚𝑜𝑙
(1.45812 + 2)(1.59 )
𝑐𝑚3
APPENDIX D

Documentation

Figure D.1: The refractometer used for the experiment

Figure D.2: Some reagents used for the experiment


Figure D.3: Looking through the refractometer

Figure D.4: Displaying the index of refraction reading