Download as pdf or txt
Download as pdf or txt
You are on page 1of 62

GROUP 2

Quality Control 2: Laboratory

Baxter || Catalan || Dela Rosa || Mariñas || Señoron || Yulo

ACTIVITY 3
REFRACTIVE INDEX-
REFRACTOMETER
ACTIVITY 3: REFRACTIVE INDEX-
REFRACTOMETER
OBJECTTVE:
To be able to determine the refractive index of a substance using a
handheld refractometer.

APPARATUS / GLASSWARE:
Refractometer

MATERIAL/ SAMPLE:
Distilled water,
any liquid flavor or any liquid sample
ACTIVITY 3: REFRACTIVE INDEX-
REFRACTOMETER
PROCEDURE:
1. Open the illuminator flap.
ACTIVITY 3: REFRACTIVE INDEX-
REFRACTOMETER
PROCEDURE:
2. Put a sample on the measurement prism surface, using
dropper or pipette.
ACTIVITY 3: REFRACTIVE INDEX-
REFRACTOMETER
PROCEDURE:
3. Close the flap.
ACTIVITY 3: REFRACTIVE INDEX-
REFRACTOMETER
PROCEDURE:
4. Look through the
eyepiece.
ACTIVITY 3: REFRACTIVE INDEX-
REFRACTOMETER
PROCEDURE:
5. Read result from the scale, if necessary place the
refractometer in the direction of light.
ACTIVITY 3: REFRACTIVE INDEX-
REFRACTOMETER
PROCEDURE:
6. Wipe dry the prism and flap with a clean, soft cloth.
ACTIVITY 3: REFRACTIVE INDEX-
REFRACTOMETER
PROCEDURE:
7. Perform in two trials.
ACTIVITY 3: REFRACTIVE INDEX-
REFRACTOMETER
Determine the Refractive Index:

Substance Refractive Index

Salicylic Acid 1.565 @25 °C/D

Peppermint Oil 1.460-1.464 @ 20 °C/D


Menthol 1.458 @ 25°C/D

Acetic Acid 1.3720 @25° C/D

1.4758 @ 15°C/D;
Glycerol 1.4746@ 20° C/D;
1.4730 @ 25° C/D.
ACTIVITY 3: REFRACTIVE INDEX-REFRACTOMETER

Questions:
1. What are the specific use/s of a refractometer in
pharmacy?
(1)Identifies a pure substance,
(2) Establish the purity of some substances
(3) Determines the concentration of some simple solutions
alcohol solutions,
sugar solutions [percent of sugar in syrup]
(4) Determines the uniformity of final compounded
preparations
ACTIVITY 3: REFRACTIVE INDEX-REFRACTOMETER

Questions:
2. Draw the handheld refractometer and label its parts.
Handheld Refractometer
ACTIVITY 3: REFRACTIVE INDEX-REFRACTOMETER

Questions:
3. What is an Abbe refractometer? Draw and label the
parts.
A refractometer in which the critical angle for total reflection
at the interface of a film of a liquid between two similar glass
prisms is utilized in determining the index of refraction.
Eyepiece
Abbe refractometer
Prism
adjust drum

ling light into


the lens holder Adustable knob

thermometer in casting
Rotating
Illuminated dial
Shaft
concentrator

Base
ACTIVITY 4: OPTICAL
ROTATION - POLARIMETER
ACTIVITY 4: OPTICAL ROTATION -
POLARIMETER
OBJECTIVE
To be able to identify the parts of a polarimeter and
determine the specific rotation of a sugar solution

APPARATUS/GLASSWARES MATERIAL/SAMPLE
volumetric flask sucrose solution
weighing balance
polarimeters
others (as needed)
Other Needed Apparatus Other Needed Reagents

Beaker
Spatula HCl 5mL
Wash bottle NaOH solution
Funnel Phenolphthalein
Stirring rod
Pipette
Volumetric stopper
Water bath
Dropper
Dry cloth
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER

PROCEDURE:
SAMPLE PREPARATION (The Specific Rotation Of Sucrose)
1. Weigh as accurately as possible about 52 grams of sucrose.

52.0000 g
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER

PROCEDURE:
SAMPLE PREPARATION (The Specific Rotation Of Sucrose)
2. Dissolve it in enough distilled water to make a 100mL solution.
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER

PROCEDURE:
SAMPLE PREPARATION (The Specific Rotation Of Sucrose)
3. Transfer 50mL of the solution into a 100mL volumetric flask, and
dilute to the mark with distilled water. Mix the solution well. Cool.
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER

PROCEDURE:
SAMPLE PREPARATION (The Specific Rotation Of Sucrose)
4. Optical rotation is determined within 30 minutes after the
preparation at 250 ± 0.5°C
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER

PROCEDURE:
SAMPLE PREPARATION (The Specific Rotation Of Sucrose)
5. Carefully rinse the sample tube twice with this solution.
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER

PROCEDURE:
SAMPLE PREPARATION (The Specific Rotation Of Sucrose)
6. Obtain 3 readings of this solution and get the average. Average
optical rotation of sucrose:______
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER

PROCEDURE:
SAMPLE PREPARATION (The Specific Rotation Of Sucrose)
7. Calculate the specific rotation of sucrose.
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER

PROCEDURE:
SAMPLE PREPARATION (The Inversion of Sucrose)
1. Clean and rinse well the volumetric flask used above.
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER

PROCEDURE:
SAMPLE PREPARATION (The Inversion of Sucrose)
2. Place the other 50ml portion of the prepared sucrose solution in
the clean volumetric flask.
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER

PROCEDURE:
SAMPLE PREPARATION (The Inversion of Sucrose)
3. Add 25mL of distilled water and 5mL of conc. HCl
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER

PROCEDURE:
SAMPLE PREPARATION (The Inversion of Sucrose)
4. Heat in a water bath for 15 minutes, keeping the temperature
constant at 70°C
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER

PROCEDURE:
SAMPLE PREPARATION (The Inversion of Sucrose)
5. Cool thoroughly under running water.
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER

PROCEDURE:
SAMPLE PREPARATION (The Inversion of Sucrose)
6. Add drop by drop saturated NaOH solution, shaking after each addition
until a drop of the solution gives a pink color to phenolphthalein which is
used as an outside indicator.
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER

PROCEDURE:
SAMPLE PREPARATION (The Inversion of Sucrose)
7. Dilute to the mark with distilled water and mix thoroughly.
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER

PROCEDURE:
SAMPLE PREPARATION (The Inversion of Sucrose)
8. Rinse the sample tube twice.
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER

PROCEDURE:
SAMPLE PREPARATION (The Inversion of Sucrose)
9. Obtain 3 readings of this solution and get the average. Average
optical rotation of sucrose:_______
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER

PROCEDURE:
SAMPLE PREPARATION (The Inversion of Sucrose)
10. Calculate the specific rotation of sucrose.
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER
PROCEDURE:

2. USING THE APPARATUS

1. Pour the solution


to be measured
into the test tube
for measurement
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER
PROCEDURE:

2. USING THE APPARATUS

Caution:
the screws at the
both ends of the test
tube should not to be
tightened more than
necessary
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER
PROCEDURE:

2. USING THE APPARATUS

2. Connect the power


source and switch on
the sodium lamp.
Wait for about
10minutes until the
lamp emits yellow
sodium light.
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER
PROCEDURE:

2. USING THE APPARATUS

3. Rotate the scale


knob until the
illumination of the
viewing field have
equal intensity
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER
PROCEDURE:

2. USING THE APPARATUS

4. Check the zero-


position of the Vernier
scale. If the position is
not in zero adjustment
can be made or adjust
to zero position
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER
PROCEDURE:

2. USING THE APPARATUS

5. Open the cover of the


sample chamber, and
put the test tube into
the chamber, the bulb
part of the test tube is in
upward position.
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER
PROCEDURE:

2. USING THE APPARATUS

6. Adjust the viewing


field screw until the
triplex viewing aspect
becomes distinct.
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER
PROCEDURE:

2. USING THE APPARATUS

7. Rotate the scale


knob until illumination
of the viewing field
becomes identical.
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER
PROCEDURE:

2. USING THE APPARATUS

8. Read on the dial,


thru a magnifying
glass, the angle of
rotation.
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER
PROCEDURE:

2. USING THE APPARATUS

9. After using, clean


the apparatus.
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER

Optical Rotation Computation


Given:
1. A sample of pure 2-butanol was placed in a 10cm polarimeter tube. Using
the D-line of a sodium lamp, the observed rotation at 20°C was a= +104°.
The conc. of the compound is 0.805 g/ mL.

What is the specific rotation of 2-butanol?


ACTIVITY 4: OPTICAL ROTATION - POLARIMETER

Optical
Rotation
Computation
#1
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER

Optical Rotation Computation


Given:
2. Calculate the observed rotation of a solution of 5.245 g of 1- ammonium-
1-phenylethane diluted to a volume of 100 mL w/ a methanol at 20°C using
the D-line of a sodium lamp and a 1 dm tube.

Specific rotation of this material=(-30°)


Sample concentration is 5.245 g in 100mL
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER

Optical
Rotation
Computation
#2
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER

Optical Rotation Computation


Given:
3. Calculate the specific rotation of 2,3-tartaric acid based on the ff
observation: A 0.856 g sample of pure acid was diluted to 10 mL w/water
and observed in a 1.00 dm polarimeter tube. The observed rotation using
the 589 nm line of a sodium lamp at 20°C was a=+1.06.
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER

Optical
Rotation
Computation
#3
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER

1. What is meant by specific rotation?

Specific rotation is defined as the angle of


rotation in degrees of the plane of
polarization of monochromatic light passing
through a 100 ml long tube containing an
optical active substance in solution at a
concentration of 1 g/ml.
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER

2. Enumerate and differentiate the type of polarimeter.

Laurent's half-shade polarimeter


A device used to determine the direction of
polarization of plane polarized light; it consists
of a quartz plate of special thickness that
covers half of the plane polarized beam,
followed by a plane polarization analyzer.
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER

2. Enumerate and differentiate the type of polarimeter.


Biquartz polarimeter

In biquartz polarimeters, a biquartz plate is used.


Biquartz plate consists of two semi circular plates


of quartz each of thickness 3.75mm. One half
consists of right-handed optically active quartz,
while the other is left-handed optically active
quartz.
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER

2. Enumerate and differentiate the type of polarimeter.


Lippich polarimeter

The Lippich polarimeter differs from the


Laurent form only in the method of producing


the half-shadow. Laurent’s polarimeter suffers
from the defect that it can be used only for
light of a particular wavelength for which the
half wave plate has been constructed. To
overcome this difficulty, Lippich constructed a
polarimeter, that can be used for light of any
wavelength.
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER

2. Enumerate and differentiate the type of polarimeter.


Quartz-wedge Polarimeter
The quartz wedge is a simple, semi-quantitative compensator designed
around a crystalline block of quartz cut with an elongated wedge angle so

that the optical axis of the quartz is oriented either parallel or perpendicular
to the edge of the birefringent crystal.
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER

2. Enumerate and differentiate the type of polarimeter.


Manual
Ideal for determining concentration levels of
samples for applications in educational,

pharmaceutical, and cosmetic industries. Operation


is simple—line up the vernier and scale to the zero
position, place the sample-filled tube into the
measuring field chamber, and close the light shield.
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER

2. Enumerate and differentiate the type of polarimeter.

Semi-automatic
Suitable for measuring the proportion, purity,
concentration and content of rotatory organic

material. Some of applications are: Agricultural


Industry: For analyzing the element of
agricultural antibiotic, microbial pesticide and
the starch content of farm produce.
ACTIVITY 4: OPTICAL ROTATION - POLARIMETER

2. Enumerate and differentiate the type of polarimeter.

Fully-automatic
This digital polarimeter is
designed to
measure optically
active liquids. The measuring
time is one second, regardless
of the rotation angle of the
sample.
THANK

YOU!!!

You might also like