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Civil Engineering Workshop - Environmental Engineering Lab: 1. Total Organic Carbon (Toc) Analyzer

The document describes various analytical techniques used in an environmental engineering lab, including: 1) Total organic carbon analysis to measure organic compounds in water samples. 2) UV-visible spectrophotometry to identify organic compounds using light absorption characteristics. 3) Fourier transform infrared spectroscopy to identify chemical bonds in molecules using infrared light absorption. 4) Gas chromatography-mass spectrometry and high performance liquid chromatography to separate and identify organic compounds in mixtures. 5) Atomic absorption spectrophotometry to quantify metals in liquid samples by absorbing light at specific wavelengths.
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0% found this document useful (0 votes)
86 views3 pages

Civil Engineering Workshop - Environmental Engineering Lab: 1. Total Organic Carbon (Toc) Analyzer

The document describes various analytical techniques used in an environmental engineering lab, including: 1) Total organic carbon analysis to measure organic compounds in water samples. 2) UV-visible spectrophotometry to identify organic compounds using light absorption characteristics. 3) Fourier transform infrared spectroscopy to identify chemical bonds in molecules using infrared light absorption. 4) Gas chromatography-mass spectrometry and high performance liquid chromatography to separate and identify organic compounds in mixtures. 5) Atomic absorption spectrophotometry to quantify metals in liquid samples by absorbing light at specific wavelengths.
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CIVIL ENGINEERING WORKSHOP - ENVIRONMENTAL ENGINEERING LAB

1. TOTAL ORGANIC CARBON (TOC) ANALYZER

Total organic carbon (TOC) is the amount of carbon found in an organic compound and is
often used as a non-specific indicator of water quality. A typical analysis for TOC measures
both the total carbon present and the so-called "inorganic carbon" (IC), the latter
representing the content of dissolved carbon dioxide and carbonic acid salts. Based on the
fact that only TC and IC can be measured directly out of these three parameters, the two
following methods can be used to measure TOC.

(1) Calculate TOC from the difference between measured TC and IC. (TOC = TC - IC)
(2) Remove IC by pretreatment, and then calculate TOC from the measured TC. (TOC = TC)

Method (1) measures IC and method (2) removes IC. When pH decreases below 3, almost
all IC is present as dissolved carbon dioxide. At this state of equilibrium, carbon dioxide is
present in water as a dissolved gas, and can be driven out of the sample simply by purging
the sample with a gas that contains no CO2. Thus, the IC of a sample can be extracted by
adding acid to reduce its pH to 3 or below, and then purging the sample with a gas that
contains no CO2. IC measurement involves measuring the amount of CO2 extracted during
purging, while IC removal involves simply disposing of the purged CO2. Method (2) of
calculating TOC is called the NPOC method, and the TOC content value measured called the
NPOC value. NPOC stands for non-purgeable organic carbon.

2. UV-VISIBLE SPECTROMETER

Ultraviolet–visible spectroscopy or ultraviolet-visible spectrophotometry (UV-Vis or UV/Vis)


refers to absorption spectroscopy or reflectance spectroscopy in the ultraviolet-visible
spectral region. This means it uses light in the visible and adjacent ranges. UV-Vis
spectroscopy has many different applications in organic and biological chemistry. One of the
most basic of these applications is the use of the Beer - Lambert Law to determine the
concentration of a chromophore. The law is simply an application of the observation that,
within certain ranges, the absorbance of a chromophore at a given wavelength varies in a
linear fashion with its concentration: the higher the concentration of the molecule, the
greater its absorbance. The instrument used in ultraviolet-visible spectroscopy is called a
UV/Vis spectrophotometer. It measures the intensity of light passing through a sample (I),
and compares it to the intensity of light before it passes through the sample (I 0). The ratio I/
I0 is called the transmittance, and is usually expressed as a percentage (%T). The basic parts
of a spectrophotometer are a light source, a holder for the sample, a prism to separate the
different wavelengths of light and a detector.
3. FOURIER TRANSFORM INFRARED SPECTROSCOPY (FTIR)

FTIR is most useful for identifying chemicals that are either organic or inorganic. It can be
utilized to quantitate some components of an unknown mixture and for the analysis of
solids and liquids. The term Fourier Transform Infrared Spectroscopy (FTIR) refers to a
development in the manner in which the data is collected and converted from an
interference pattern to a spectrum. It is a powerful tool for identifying types of chemical
bonds in a molecule by producing an infrared absorption spectrum that is like a molecular
"fingerprint". The wavelength of light absorbed is characteristic of the chemical bond
present.

Principle

FTIR relies on the fact that the most molecules absorb light in the infra-red region of the
electromagnetic spectrum. This absorption corresponds specifically to the bonds present in
the molecule. The frequency range are measured as wave numbers typically over the range
4000 – 600 cm-1.

Working

Light Source (IR Interferometer Sample Detector Interface


Beam) (Beam Splitter) Compartment (Interferogram) (IR Spectrum)

Chromatography is a laboratory technique for the separation of a mixture. The mixture is


dissolved in a fluid called the mobile phase, which carries it through a structure holding
another material called the stationary phase. Based on the physical state of the mobile
phase it is classified into i) Gas chromatography ii) Liquid chromatography.

4. GAS CHROMATOGRAPHY- MASS SPECTROSCOPY (GC-MS)

GC is a technique capable of separating, detecting and partially characterizing the organic


compounds particularly when present in small quantity. Mass spectroscopy provides some
definite structural information from in small quantity. Gas chromatography coupled to mass
spectrometry is a versatile tool to separate, quantify and identify unknown (volatile) organic
compounds and permanent gases. By combining sensitivity and a high resolving power,
complex mixtures can be analyzed. Column is the region where the separation takes place;
Column is filled with the stationary phase. Mostly organic compounds will be separated-
Vapour will be carried out by helium gas. The mass spectrometer is an instrument designed
to separate gas phase ions according to their mass to charge ratio (m/z) value.

5. HIGH PERFORMANCE LIQUID CHROMATOGRAPHY (HPLC)

It is a separation technique in which the mobile phase is a liquid. It can be carried out either
in a column or a plane. Present day liquid chromatography that generally utilizes very small
packing particles and a relatively high pressure is referred to as High performance Liquid
chromatography (HPLC).In HPLC the sample is forced by a liquid at high pressure (the mobile
phase) through a column that is packed with a stationary phase composed of irregularly or
spherically shaped particles, a porous monolithic layer, or a porous membrane. Each
component in the sample interacts slightly differently with the stationary phase, causing
different flow rates for the different components and leading to the separation of the
components as they flow out the column.

6. ATOMIC ABSORPTION SPECTROPHOTOMETER (AAS)

AAS is an instrument used to quantify many metals and some non-metals in liquid samples.
It can analyse about 70 metals in the periodic table.

Principle: Free atoms generated can absorb radiation at specific frequency. The atoms
absorb the energy and make transition to higher energy levels. The analyte concentration is
determined from the amount of absorption in either ppm or ppb ranges.

Parts:

1. Light source : Two common types of lamps are used as the light source in AAS
a. Hollow Cathode lamp (HCL)
b. Electrode-less Discharge Lamp(EDL)
Each element has a unique lamp that has to be used for the analysis.

2. Nebulizer: suck up the liquid at a controlled rate and create a fine aerosol spray for
the introduction to the flame.
3. Atomizer: where separation of particles into individual molecules and breaking
molecules into atoms occur. This is done by exposing the analyte to high
temperatures in a flame. In most cases air-acetylene flames are used.
4. Monochromator: Used to select the specific wavelength of light absorbed by the
sample, by excluding other wavelengths.
5. Detector: Convert the light signals into electrical signals proportional to the light
intensity. It is usually connected with a software which helps to display the results.

Working: The instrument is calibrated using several standard solutions of known


concentrations. Absorbance of each known solution is measured and then a calibration
curve of concentration vs absorbance is plotted. The sample solution is then fed into the
instrument and the absorbance of the solution is measured. The unknown concentration
of the element is calculated from the calibration curve.

Applications: Determination of quantities of metals in environment studies (drinking


water, soil, ocean water), food industry, pharmaceutical industries.

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