REFRACTOMETRY

Refractometry is the analytical method of measuring substances' refractive index (one of their
fundamental physical properties) in order to, for example, assess their composition or purity.
When a light ray passes from a less dense medium to a more dense medium (e.g., from air to
glass), it bends towards the normal and when it passes from a denser medium to a less dense
medium (e.g., from glass to air) it bends away from the normal. This phenomenon of deviation of
light rays from their original path, when they pass from one medium to another, is called
refraction of light.

The speed of light in different substances varies. Therefore, different substances have different
abilities to bend or refract light. We call this bending ability of a material as the index of
refraction or refractive index of that material.The refractive index (ηi) of a material is defined
as the ratio of the speed of light in vacuum to that in the material medium. Therefore refractive
index of a medium;
(ηi) = speed of light in vacuum / speed of light in medium= c / vi
where vi is the velocity of the propagation of the radiation in the medium and c is the velocity in
a vacuum; c is a constant under all conditions.
A refractometer is the instrument used to measure refractive index ("RI").
Although refractometers are best known for measuring liquids, they are also used to measure
gases and solids; such as glass and gemstones.
The RI of a substance is strongly influenced by temperature and the wavelength of light used to
measure it, therefore, care must be taken to control or compensate for temperature differences
and wavelength. RI measurements are usually reported at a reference temperature of 20
degrees Celsius, which is equal to 68 degrees Fahrenheit, and considered to be room
temperature. A reference wavelength of 589.3 nm is most often used. Though RI is a
dimensionless quantity, it is typically reported as nD20 (or n20

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D ), where the "n" represents refractive index, the "D" denotes the wavelength, and the 20
denotes the reference temperature. Therefore, the refractive index of water at 20 degrees Celsius,
taken at the Sodium D Line, would be reported as 1.3330 nD20.
Refractometers are frequently used by grape growers and kiwifruit growers for Brix testing
of sucrose levels in their fruit. Refractometry is also used in the gelatin industry. To convert the
RI of a gelatin sol (reported in Brix) to a gelatin concentration, one need only multiply by eight-
tenths (0.8). A sol with a 10.0 RI would therefore be 8% gelatin by weight. This is known to be a
reliable conversion for gelatin sols as low as 1% up to over 50%.
Types of refractometers
A traditional handheld refractometer is an analog instrument for measuring a
liquid's refractive index. It works on the critical angle principle by which lenses and prisms
project a shadow line onto a small glass reticle inside the instrument, which is then viewed by the
user through a magnifying eyepiece.
In use, a sample is placed between a measuring prism and a small cover plate. Light traveling
through the sample is either passed through to the reticle or totally internally reflected. The net
effect is that a shadow line forms between the illuminated area and the dark area. It is where this
shadow line crosses the scale that a reading is taken. Because refractive index is very
temperature dependent, it is important to use a refractometer with automatic temperature
compensation. Compensation is accomplished through the use of a small bi-metallic strip that
moves a lens or prism in response to temperature changes. This design was invented by Emanuel
Goldberg. There are many types of refractometers and the most common types are Abbe's
refractometer, Pulfrich refractometer, Immersion refractometer.

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Digital handheld refractometer
This is an instrument for measuring the refractive index of materials. Digital handheld
refractometers are generally more precise than traditional handheld refractometers, but less
precise than most benchtop refractometers. They also may require a slightly larger amount of
sample to read from since the sample is not spread thinly against the prism.
The result may be displayed in one of various units of measurement: Brix, freezing point, boiling
point, concentration, etc. Nearly all digital refractometers feature Automatic Temperature
Compensation.
Most have a metal sample well around the prism, which makes it easier to clean sticky samples,
and some instruments offer software to prevent extreme ambient light from interfering with
readings (you can also shade the prism area to prevent this as well). Some instruments are
available with multiple scales, or the ability to input a special scale using known conversion
information. There are some digital handheld refractometers that are IP65 (IP Code) water-
resistant, and thus washable under a running faucet.

Principle of operation
Most operate on the same general critical angle principle as a traditional handheld refractometer.
The difference is that light from an LED light source is focused on the underside or a prism
element. When a liquid sample is applied to the measuring surface of the prism, some of the light
is transmitted through the solution and lost, while the remaining light is reflected onto a linear
array of photodiodes creating a shadow line. The refractive index is directly related to the
position of the shadow line on the photodiodes. Once the position of the shadow line has been
automatically determined by the instrument, the internal software will correlate the position to
refractive index, or to another unit of measure related to refractive index, and display a digital
readout on an LCD or LED scale.
The more elements there are in the photodiode array, the more precise the readings will be, and
the easier it will be to obtain readings for emulsions and other difficult-to-read fluids that form
fuzzy shadow lines.
In the Abbe' refractometer the liquid sample is sandwiched into a thin layer between an
illuminating prism and a refracting prism. 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. A detector placed on the back side of the refracting prism would show a light and a
dark region.
Over a century after Abbe's work, the usefulness and precision of refractometers has improved,
although their principle of operation has changed very little. They are also possibly the easiest
device to use for measuring the refractive index of solid samples, such as glass, plastics,
and polymer films. Some modern Abbe refractometers use a digital display for measurement,
eliminating the need for discerning between small graduations. However, the user still has to
adjust the view to get a final reading.

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The first truly digital laboratory refractometers began appearing in the late 1970s and early
1980s, and no longer depended on the user's eye to determine the reading. They still required the
use of circulating water baths to control instrument and fluid temperature. They did, however,
have the ability to electronically compensate for the temperature differences of many fluids
where there is a known concentration-to-refractive-index conversion. Most digital laboratory
refractometers, while much more accurate and versatile than their analog Abbe counterparts, are
incapable of readings on solid samples.
In the late 1990s, Abbe refractometers became available with the capability of measurements at
wavelengths other than the standard 589 nanometers. These instruments use special filters to
reach the desired wavelength, and can extend measurements well into the near infrared (though a
special viewer is required to see the infrared rays). Multi-wavelength Abbe refractometers can be
used to easily determine a sample's Abbe number.

The most advanced instruments of today use solid-state Peltier effect devices to heat and cool the
instrument and the sample, eliminating the need for an external water bath. The software on most
of current instruments offers features such as programmable user-defined scales and a history
function that recalls the last several measurements. Several manufacturers offer easily usable
controls, with the ability to use from and export readings to a linked computer.

Inline process refractometers are a type of refractometer designed for the continuous
measurement of a fluid flowing through a pipe or inside a tank. These refractometers typically
consist of a sensor, placed in line with the fluid flow, coupled to a control box. The control box
usually provides a digital readout as well as 4-20 mA analog outputs and relay outputs for
controlling pumps and valves. Instead of placing the sensor inline of the process, it can be placed
in a bypass, attached by a thin tube.
This measurement has been an important element in the process control of the chemical and
refining, pulp and paper, food, sugar and pharmaceutical industries for more than a century. For
instance, the in-line concentration measurement can be used as a real-time predictive tool for the
final concentration. A quick and accurate response is needed to optimize production. Cost
reduction is possible by reducing the variation of mean average of the product concentration. The
cost saving is related to the value of the component being measured.

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A digital inline process refractometer sensor measures the refractive index and
the temperature of the processing medium. The measurement is based on the refraction of light in
the process medium, i.e. the critical angle of refraction using a light source. The measured
refractive index and temperature of the process medium are sent to the control box. It calculates
the concentration of the process liquid based on the refractive index and temperature, taking pre-
defined process conditions into account. The output is typically a 4 to 20mA DC output or,
increasingly, an Ethernet signal proportional to process solution concentration, liquid density,
Brix or other scale that has been selected for the instrument.[1]
The inline process refractometer consists of three primary components: the inline sensing head,
the electronics console, and the process adapter. The inline sensing head is mounted on the
adapter and contains a prism that scans the process solution through a transparent window and
outputs a value relative to the refractive index of the solution. The electronics console houses all
control circuitry, microprocessors, digital displays and calibration points and conditions the
sensing head signal. The process adapter is the mechanical connection between the inline sensing
head and the process piping, and is designed specifically to accommodate the pipe size and
application.
Inline process refractometers are used primarily in the pulp and paper industry; the food and
beverage industry, the pharmaceutical industry, and the chemical industry as a means to assure
consistency and quality. In the pulp and paper industry, inline process refractometers are used in
the energy recovery from black liquor recovery boilers by accurately measuring solids in the
black liquor. In the food and beverage industry, inline process refractometers are used to measure
dissolved solids, most often as sugar content, measured in degrees Brix. In the pharmaceutical
industry they are used to monitor and control concentration levels during supersaturation, a
critical process in crystallization. In the chemical industry they are used in Hydrochloric
Acid applications, Sulphuric Acid applications, and boiler cleaning chemicals processes.

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