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Structure of gallium chalcogenide cubane compound, where E = S, Se, and R = CMe 3 , CMe 2 Et, CEt 2 Me, CEt 3 .

Data collection

In a typical experiment 5 - 10 mg of sample is used with a heating rate of ca. 5 °C/min up to under either a 200-300 mL/min inert (N 2 or Ar) gas flow or a dynamic vacuum ( ca . 0.2 Torr if using a typical vacuum pump). The argon flow rate was set to 90.0 mL/min and was carefully monitored to ensure a steady flow rate during runs and an identical flow rate from one set of data to the next.

Once the temperature range is defined, the TGA is run with a preprogrammed temperature profile ( [link] ). It has been found that sufficient data can be obtained if each isothermal mass loss is monitored over a period (between 7 and 10 minutes is found to be sufficient) before moving to the next temperature plateau. In all cases it is important to confirm that the mass loss at a given temperature is linear. If it is not, this can be due to either (a) temperature stabilization had not occurred and so longer times should be spent at each isotherm, or (b) decomposition is occurring along with sublimation, and lower temperature ranges must be used. The slope of each mass drop is measured and used to calculate sublimation enthalpies as discussed below.

A typical temperature profile for determination of isothermal mass loss rate.

As an illustrative example, [link] displays the data for the mass loss of Cr(acac) 3 ( [link] a, where M = Cr, n = 3) at three isothermal regions under a constant argon flow. Each isothermal data set should exhibit a linear relation. As expected for an endothermal phase change, the linear slope, equal to m sub , increases with increasing temperature.

Plot of TGA results for Cr(acac) 3 performed at different isothermal regions. Adapted from B. D. Fahlman and A. R. Barron, Adv. Mater. Optics Electron ., 2000, 10 , 223.
Samples of iron acetylacetonate ( [link] a, where M = Fe, n = 3) may be used as a calibration standard through ΔH sub determinations before each day of use. If the measured value of the sublimation enthalpy for Fe(acac) 3 is found to differ from the literature value by more than 5%, the sample is re-analyzed and the flow rates are optimized until an appropriate value is obtained. Only after such a calibration is optimized should other complexes be analyzed. It is important to note that while small amounts (<10%) of involatile impurities will not interfere with the ΔH sub analysis, competitively volatile impurities will produce higher apparent sublimation rates.

It is important to discuss at this point the various factors that must be controlled in order to obtain meaningful (useful) m sub data from TGA data.

  1. The sublimation rate is independent of the amount of material used but may exhibit some dependence on the flow rate of an inert carrier gas, since this will affect the equilibrium concentration of the cubane in the vapor phase. While little variation was observed we decided that for consistency m sub values should be derived from vacuum experiments only.
  2. The surface area of the solid in a given experiment should remain approximately constant; otherwise the sublimation rate (i.e., mass/time) at different temperatures cannot be compared, since as the relative surface area of a given crystallite decreases during the experiment the apparent sublimation rate will also decrease. To minimize this problem, data was taken over a small temperature ranges ( ca . 30 °C), and overall sublimation was kept low ( ca . 25% mass loss representing a surface area change of less than 15%). In experiments where significant surface area changes occurred the values of m sub deviated significantly from linearity on a log(m sub ) versus 1/T plot.
  3. The compound being analyzed must not decompose to any significant degree, because the mass changes due to decomposition will cause a reduction in the apparent m sub value, producing erroneous results. With a simultaneous TG/DTA system it is possible to observe exothermic events if decomposition occurs, however the clearest indication is shown by the mass loss versus time curves which are no longer linear but exhibit exponential decays characteristic of first or second order decomposition processes.

Questions & Answers

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Eke Reply
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Joseph
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Maira Reply
nanopartical of organic/inorganic / physical chemistry , pdf / thesis / review
Ali
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There are lots of products of nano chemistry... Like nano coatings.....carbon fiber.. And lots of others..
learn
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da
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Bhagvanji
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Giriraj
Preparation and Applications of Nanomaterial for Drug Delivery
Hafiz Reply
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da
Application of nanotechnology in medicine
has a lot of application modern world
Kamaluddeen
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narayan
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Crow Reply
what about nanotechnology for water purification
RAW Reply
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Damian
yes that's correct
Professor
I think
Professor
Nasa has use it in the 60's, copper as water purification in the moon travel.
Alexandre
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Alexandre
what is the stm
Brian Reply
is there industrial application of fullrenes. What is the method to prepare fullrene on large scale.?
Rafiq
industrial application...? mmm I think on the medical side as drug carrier, but you should go deeper on your research, I may be wrong
Damian
How we are making nano material?
LITNING Reply
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LITNING Reply
What is meant by 'nano scale'?
LITNING Reply
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LITNING
scanning tunneling microscope
Sahil
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Santosh
Do u think that Graphene and Fullrene fiber can be used to make Air Plane body structure the lightest and strongest. Rafiq
Rafiq
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Rafiq
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Anam
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Anam
Any one who tell me about Preparation and application of Nanomaterial for drug Delivery
Hafiz
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Bob Reply
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Bob
The nanotechnology is as new science, to scale nanometric
brayan
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Damian
how did you get the value of 2000N.What calculations are needed to arrive at it
Smarajit Reply
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Source:  OpenStax, Chemistry of electronic materials. OpenStax CNX. Aug 09, 2011 Download for free at http://cnx.org/content/col10719/1.9
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