Abstract:

This report includes The CHNS-O Analyzers utility in determining the percentages of
Carbon, Hydrogen, Nitrogen, Sulphur and Oxygen of organic compounds, based on the principle
of combustion. The combustion products are separated by a chromatographic column and
detected by the thermal conductivity detector (T.C.D.), which gives an output signal proportional
to the concentration of the individual components of the mixture.

Introduction:
CHNS-O elemental analysers provide a means for the rapid determination of carbon,
hydrogen, nitrogen and sulphur in organic matrices and other types of materials. They are
capable of handling a wide variety of sample types, including solids, liquids, volatile and viscous
samples, in the fields of pharmaceuticals, polymers, chemicals, environment, food and energy.
The analysers are often constructed in modular form such that they can be set up in a number of
different configurations to determine, for example, CHN, CHNS, CNS or N depending on the
application. This adaptability allows not only flexibility of operation but also the use of a wide
range of sample weights from a fraction of a milligram to several grams (macro-systems.) In its
simplest form, simultaneous CHNS analysis requires high temperature combustion in an oxygenrich environment and is based on the classical Pregl-Dumas method. This combustion can be
carried out under both static conditions i.e. introduction of a set volume of oxygen or dynamic
conditions i.e. a constant flow of oxygen for a set period of time. Often, catalysts are also added
to the combustion tube in order to aid conversion.

Figure 1. CHNS-O Analyzer

Basic Principle:
In the combustion process (furnace at ca. 1000oC), carbon is converted to carbon dioxide;
hydrogen to water; nitrogen to nitrogen gas/ oxides of nitrogen and sulphur to sulphur dioxide. If
other elements such as chlorine are present, they will also be converted to combustion products,
such as hydrogen chloride. A variety of absorbents are used to remove these additional
combustion products as well as some of the principal elements, sulphur for example, if no
determination of these additional elements is required.
The combustion products are swept out of the combustion chamber by inert carrier gas
such as helium and passed over heated (about 600oC) high purity copper. This copper can be
situated at the base of the combustion chamber or in a separate furnace. The function of this
copper is to remove any oxygen not consumed in the initial combustion and to convert any
oxides of nitrogen to nitrogen gas. The gases are then passed through the absorbent traps in order
to leave only carbon dioxide, water, nitrogen and sulphur dioxide.
Detection of the gases can be carried out in a variety of ways including
1. A GC separation followed by quantification using thermal conductivity detection
2. A partial separation by GC (frontal chromatography) followed by thermal conductivity
detection (CHN but not S)
3. A series of separate infra-red and thermal conductivity cells for detection of individual
compounds. Quantification of the elements requires calibration for each element by using
high puritymicro-analytical standard compounds such as acetanilide and benzoic acid.

Comparison with Other Different Techniques:

1. X-RAY FLOURESCENCE SPECTROSCOPY
This technique is used for direct analysis of metal samples, coal, cement and many other
materials in solid form. It is a fast techniques and non-destructive to sample. But this technique is
less accurate technique for low mass number elements.
2. ENERGY DISPERSIVE SPECTROSCOPY (EDX)
In this technique the energy of each x-ray and the number of x-rays for each are
measured. The EDX is usually installed with SEM. Its limitation is in case of lighter elements
peaks will overlap which result in inaccurate results.

3. WET CHEMISTRY
In Wet chemistry either the volume of a known reagent called volumetric analysis or
mass of the reagent called gravimetric analysis required to complete a reaction with analyte is
measured. From this volume or mass and stiochiometry of the reaction, we calculate how much
analyte is present in the unknown sample. These techniques are labor intensive and time
consuming, and sometimes less accurate than the current instrumental methods.

EXPERIMENTAL PROCEDURE:
Samples are weight by using mettle Toledo machine. The sample was wrapped in a tin
small crucible.
O2 and He gas valves were open, turned the equipment started the software E300.
The pressure was kept about 250 psi.
Voltage difference was set at 1000 micro volts between carrier helium gas and reference
gas.
Turned on furnace 1 and set at temperature of about 900 C and oven at temperature of
about 60 C.
Some tests like leak, blank tests are performed to check whether the equipment works
properly or not.
In order to completely remover the previous combustion product usually gases by pass
test is done.
Then four standards samples (BBOT, cystine, methionine and Sulphanileamide) were run
in the instrument and their results were compared with known standard result.
Standard samples results are also serve in calibration purpose. Finally unknown charcoal
sample is run and its constituents elements were calculated.

Results and Discussion:

The results of standard samples are found to be:
C

Cystine

29.94

5.02

11.64

26.67

26.62

Methionine

40.26

7.43

9.38

21.47

21.44

Sulfanilamide

41.85

4.69

16.26

18.63

18.59

BBOT

72.52

6.08

6.52

7.45

7.44

The reactivity time versus count plots for standard sample are as follows:
1. For Cystine:

Figure 2. Reactivity time vs. count plot for Cystine

2. For Methionine:

Figure 3.Reactivity time vs. count plot for Methionine

3. For Sulfanilamide:

Figure 4. Reactivity time vs. count plot for SULFANILAMIDE

4. For BBOT

Figure 5. Reactivity time vs. count plot for BBOT

The results of standard samples are compared with standard known results. Finally, the unknown
charcoal sample of weight 2.02mg is run through the analyzer. The results of unknown charcoal
sample are as follows:

Figure 6. Reactivity time vs. count plot for unknown charcoal

sample

Areas of Applications:

Organic compounds
Pharmaceuticals
Food & Agricultural Industries
Chemistry & Chemical Engineering
Geological & Environmental samples
Organometallics
Gasoline and fuels
Coal and coke
Graphite and carbides
Metals and alloys
Polymers and explosives
Building materials and your samples...

Conclusion:
The unknown charcoal sample was successfully analyzed through CHNS-O analyzer. The concentration
of different elements(C, N, S and H) was calculated by using equipment software. There is slight
difference found between manual calculated and automated calculated results.

References:
http://www-odp.tamu.edu/publications/tnotes/tn30/tn30_10.htm
http://departments.agri.huji.ac.il/zabam/EA.html
Instrumental Criteria Subcommittee (2005). Evaluation of Analytical Instrumentation Part
XIX: CHNS Elemental Analysers.