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Paci Report Assignment

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Assignment 3

Principles of analytical & characterization


Instruments

Research paper review


By
Mahima Baid (220CH1630)
Sharmistha Bhatt (220CH1161)

Department of Chemical Engineering


National Institute of Technology
Rourkela
Acknowledgement

We express our sincere thanks to our guide Prof. (Dr.) Biswajit Saha for
his inspiring guidance and for his exemplary perseverance and hospitality.
We would like to admit our deep sense of gratitude for his constant
support and cooperation throughout the work. We sincerely acknowledge
him for extending his valuable supervision.
Research Paper under Review:

Corrosion Study of Iron and Copper Metals


and Brass Alloy in Different Medium
(No of citations=11)
This is a review report on the above paper which studies the corrosion in iron, copper
and brass alloys.

An outline of the research paper


This paper presents an investigation on the corrosion of iron, copper and brass alloy
in different medium i.e. strong and weak acids of different concentrations viz 0.1 N,
0.5 N, 1 N, 4 N and similarly bases like NaOH, KOH and NH4OH have been used
in different concentrations.

Small rectangular size metal–alloy plates of the size 8 x 6 x 0.3 cm were used and
were dipped in the different solutions for different timings viz 1 to 5 h. The weight
loss in different solutions and the emf was measured for each metal. From the weight
loss and the emf observed, a correlative study of the corrosion rate has been done.
The summary of the results prsesnted in the paper are:
 The rate of corrosion increases with increasing the concentration of the acid.
 The rate of corrosion increases with increase in time.
 The order of corrosion activity on the acids was HNO3 > H3PO4 > H2SO4
> HCl > CH3COOH > oxalic acid > benzoic acid > succinic acid> salicylic
acid > KOH > NaOH.
For inorganic acids which show more corrosion, the emf was found to be less, and
for bases, the emf was found to be more. The potential studies on Fe showed the
following order bases > neutral > organic acids > inorganic acids. This is related to
the electrochemical behavior of metals under different concentrations.
Similar weight loss and potential studies have also been carried out for Cu and brass
alloy. The order of reactivity was found to be Fe > Cu > brass.
Propositions :
The author could demonstrate how the result obtained using the present method are
consistent with results obtained using different techniques. Therefore our
recommendation is as follows:
1.Xray Diffraction
Ferrous corrosion and rust are some of the most common forms of corrosion
analyzed. To better understand the corrosion process, the identification of phase
compositions is crucial. Different phases build under different conditions and in
different environments. Not only is the information about the chemical phases
helpful to explain the corrosion process, but can help to locate the origin of corrosion
and provide solutions to the problem.
X-ray powder diffraction (XRD) is a rapid analytical technique primarily used for
phase identification of a crystalline material and can provide information on unit cell
dimensions. The analyzed material is finely ground, homogenized, and average bulk
composition is determined. As we know, XRD analysis provides quantitative
evidence and can readily distinguish between different crystallographic
modifications of phases that have the same chemical formula.
The authors have studied the corrosion of iron using five different concentrations for
different timings. The results were obtained by weight loss method.
By performing XRD analysis of the samples at different conditions used in the
experiment, could have confirmed the presence of different phases in the samples at
different timings. As we know that formation of different phases in corrosive layer
on iron takes place with changing surrounding conditions. Not only is change in
surrounding a factor but time variation also affects the composition of corrosion
layers which could be confirmed by the XRD. Thus results provided by the authors
could be better presented by giving information of how the surrounding and time
factors determine the presence of different phases in corrosive layers and would have
added to the credibility of the results.
2.Scanning electron Microscope
The scanning electron microscope (SEM) uses a focused beam of high-energy
electrons to generate a variety of signals at the surface of solid specimens. The
signals that derive from electron-sample interactions reveal information about the
sample including external morphology by generating high-resolution images.
The SEM images of the iron sample before and after the experiment could easily
show the changes in the morphology of the samples thus confirming the presence of
corrosion layer on the iron sample subjected to different concentrations and different
timings.
Also as discussed earlier, different concentrations of medium used would create
different phases on corrosion layer which could be well supported by the SEM
images of samples as SEM micrographs can show morphologies typical to a
particular type of phase present in the corrosion layer as each phase has different
surface features.
The order of reactivity presented by the author which is: Fe > Cu > brass could also
have been verified by SEM images.

3. Xray Photoelectron Spectroscopy-


Through ion etching and a detailed XPS analysis, it could have been possible to
identify the exact amount of each corrosive product at a given depth. Based on the
amount of each corrosion and its etch rate, the character of the corrosion layer in a
specific corrosion environment can be derived.
These recommendations can give results consistent with the results presented by the
authors and also could give additional information which the authors can interpret
accordingly and utilize it for better presentation with added results or it can be
utilized for future researches.

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