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LABORATORIO 3: TOTAL ORGANIC CARBON.

Yaritsa Cifuentes Molina1, Laura Geraldine Fajardo2, Daniela Guevara Barrera3.


1
Universidad Pedagógica Y Tecnológica De Colombia, Facultad De Ciencias, Escuela De Ciencias Químicas,
Programa De Química, Química Analítica II.

ABSTRACT
During the development of this laboratory experience, an analysis was performed using the
Total Organic Carbon Analytical Technique (TOC), this is a non-specific test where TOC
will not determine which specific compounds are present, and instead, the TOC shall inform
the user of the sum of all organic carbon present in the compound to be analyze. To carry out
this analysis during this laboratory practice, a total organic carbon equipment was used, with
German technology, called the ANALITIKJENA multi N/C 2100, in which the analysis of
two samples was performed, a phenol solution and another glycerol each with a concentration
of 50ppm.
KEYWORDS: TOC, Phenol, Glycerol.
INTRODUCTION
MATERIALS AND METHODOLOGY combustión and heat to temperaturas up to
750°C, the multi N/C® 2100 is equipped
Erlenmeyer
with an injection molding technology is
Pipettes perfect for samples containing particles.
The transmitter integrated sampling and
Pipettor analytical testing of solid materials make
Volumetric flask 50 mL him a constant analyzer and compact.

Phenol
Glycerol
ANALYSIS OF TOC

Perform calculations to prepare


phenol and glycerol solutions at 50
ppm, which will be your samples

Proceed to the TOC equipment

Pack approximately 100 µL the


sample you are going to read in the
glass syringe, WITHOUT THERE
ARE BUBBLES
Fig. 1: Equipment of analysis of TOC
ANALITIKJENA multi N/C 2100,
Located in the Laboratory of Catalysis
Proceed to inject the sample into the
LN-314.
equipment when requested

For the development of the practice was


used a equipment of "TOTAL ORGANIC Inject the sample and simultaneously
CARBON ANALYZER / TN / FOR order the team to perform the scan
ENVIRONMENTAL ASSESSMENTS /
BOARD MULTI N/C® 2100, MULTI
N/C® 2100 ANALYTIK JENA" , is a
parser that saves space with its strong
point in environmental analysis.In
addition to the VITA®, the Focus END OF PROCEDURE
Radiation NDIR-detector and catalytic
RESULTS AND DISCUSSION
Solution of Glycerol
Preparation:
50 ppm solución of glycerol
d=1,23g/mL Glycerol
d=m.v
v=0,00125g1,23 g/ml=0,001016 mL of
Glycerol
0,001016 mL of the glycerol=1,016 μl

Theoretical calculación of the 50-ppm


glycerol solution for the determination
of carbon present in the solution.


Solution of Phenol In graph 3 shows the inorganic carbon
present in the phenol solution, it is
Preparation:
observed that the intensity of the present
Atomic weight of the phenol:94,11 g/mol band is this graph reaches 1ppm of CO2,it
has no inorganic carbon, since phenol only
𝑥 𝑔𝑟𝑎𝑚𝑠 𝑠𝑜𝑙𝑢𝑡𝑒 possesses organic carbon , so it follows
50𝑝𝑝𝑚 = = 1,25 𝑚𝑔 that what appears in this graph is only
𝐿 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛
noise, since the ANALITIKJENA multi
1,25 mg of Phenol=0,00125 g of Phenol N/C 2100 equipment, is too robust and
Theoretical calculation of the 50-ppm sensitive, any interference such as voice,
phenol solution for the determination of knocking on the equipment door, sound
carbon present in the solution. produced by other instruments located
within the Catalysis Laboratory, are going
50𝑚𝑔 1𝑔 1𝑚𝑜𝑙 𝑃ℎ𝑒𝑛𝑜𝑙
∗ ∗ ∗ to be recorded in the TOC analysis,
1𝐿 1000𝑚𝑔 94.11𝑔
therefore, this is what is shown in this
6.022𝑥1023 6 𝑎𝑡𝑜𝑚𝑠 𝑜𝑓𝐶𝑎𝑟𝑏𝑜𝑛
∗ ∗ graph 3. In addition it is this graph should
1 𝑚𝑜𝑙 𝑃ℎ𝑒𝑛𝑜𝑙 1𝑚𝑜𝑙 𝑃ℎ𝑒𝑛𝑜𝑙
1𝐶 12𝑔 1000𝑚𝑔 start its baseline at zero but as there was an
∗ ∗ = 35,3ppm error of the analyst when injecting the
6.022𝑥1023 1𝑚𝑜𝑙 𝐶 1𝑔
sample into the equipment and giving the
order to the equipment to read the sample
since these two actions must be performed
at the same time, concurrently, this is why
the baseline of the graph does not start at
zero.
In graph 4, the total carbon measurement
present in the phenol solution is observed,
Graphic 3: Representation obtained from where a Gaussian curve is presented,
the ANALITIKJENA multi N/C 2100 of showing the total carbon concentration,
the Inorganic carbon present in phenol. which is the sum of all carbon both
inorganic and organic in the phenol
solution.

Graphic 4: Representation obtained from


the ANALITIKJENA multi N/C 2100 of
the Total carbon present in phenol.
CONCLUSIONS REFERENCES

-The ANALITIKJENA multi N/C 2100 [1]


equipment is very robust, sensible and any
external noise produced by the analyst, or [2]
the chemical noise that is present in the
team environment will be recorded in the
equipment.
-The TOC technique is supremely [3] S.N (2018) TOC in wastewater: vital
interesting and complete as it provides warnings. Recovered in:
very detailed and reliable information https://wwtonline.co.uk/features/toc-in-
about an analysis; this is why it has a lot of wastewater-vital-warnings [Consulted
applications in the analysis of materials, online 02/11/19]
water, industries among others [4] S.N (2018) The 12 principles of green
-The equipment used during this chemistry Recovered in:
laboratory experience when having https://www.sigmaaldrich.com/chemistry/gre
ener-alternatives/green-chemistry.html
German technology, complies with many
[Consulted online 02/11/19 ]
of the principles of green chemistry, for
example, during this analysis no residue is QUESTIONNAIRE
generated, the sample quantities to be
1. What is the combustion method
analyzed is in the order of µL, among
employed in the lab experience?
others.
2. What can you say about the quality
of the wastewater sample based on the
TOC measurement?

It is very important and good to perform


the TOC scan for wastewater, since it
provides great information, that is why in
most countries measuring TOC is a
mandatory requirement for those operating
in the wastewater sector. For instance,
organisations that frequently discharge
wastewater into watercourses will have to
ensure they monitor TOC levels and report
these figures to the appropriate regulatory
bodies.
They can be quite severe for humans and Atom Economy
Synthetic methods should be designed to
the environment. The TOC content of maximize the incorporation of all materials
wáter is a basic indication of the level of used in the process into the final product.
organic contamination and water purity.
As a substance, water can contain both
natural and synthetic organic matter,
which are both measured using TOC Less Hazardous Chemical Syntheses
testing. Examples of natural organic Wherever practicable, synthetic methods
should be designed to use and generate
matter include amine, urea, and in some substances that possess little or no toxicity to
cases even faecal matter. Synthetic human health and the environment.
contaminants include, but are not limited
to, pesticides, detergents, fertilisers and
herbicides.
With both of these types of matter in mind, Designing Safer Chemicals
TOC gives scientists a good idea of the Chemical products should be designed to
affect their desired function while minimizing
condition and state of the water they are their toxicity.
testing. What really concerns scientists is
that the contaminants mentioned can
interact with one another, encourage
growth of microorganisms or even become Safer Solvents and Auxiliaries
toxic for humans and animals. Discharging The use of auxiliary substances (e.g., solvents,
separation agents, etc.) should be made
contaminated water into the ecosystem can unnecessary wherever possible and innocuous
have devastating consequences in the short when used.
and long term conditions of our
ecosystem.[3]

3. How accurate was the measurement Design for Energy Efficiency


of the TOC in the Glycerol and Phenol Energy requirements of chemical processes
should be recognized for their environmental
solutions? Compare your results with and economic impacts and should be
the theoretical calculus. minimized. If possible, synthetic methods
should be conducted at ambient temperature
See in the results and discussion section. and pressure.

ANNEXES
GREEN QUIMICA PRINCIPLES
Prevention Use of Renewable Feedstocks
It is better to prevent waste than to treat or A raw material or feedstock should be
clean up waste after it has been created. renewable rather than depleting whenever
technically and economically practicable.
Reduce Derivatives
Unnecessary derivatization (use of blocking
groups, protection/ deprotection, temporary
modification of physical/chemical processes)
should be minimized or avoided if possible,
because such steps require additional
reagents and can generate waste.

Catalysis
Catalytic reagents (as selective as possible) are
superior to stoichiometric reagents.

Design for Degradation


Chemical products should be designed so that
at the end of their function they break down into
innocuous degradation products and do not
persist in the environment.

Real-time analysis for Pollution Prevention


Analytical methodologies need to be further
developed to allow for real-time, in-process
monitoring and control prior to the formation of
hazardous substances.

Inherently Safer Chemistry for Accident


Prevention
Substances and the form of a substance used
in a chemical process should be chosen to
minimize the potential for chemical accidents,
including releases, explosions, and fires.[4]

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