tag:blogger.com,1999:blog-32957821011913883042024-02-18T18:40:53.775-08:00Experimentos para Taller NanoAndes 2012Este es un espacio para intercambio de información respecto al taller experimental de NanoAndes 2012Cesar Costa Verahttp://www.blogger.com/profile/08593067130012155534noreply@blogger.comBlogger5125tag:blogger.com,1999:blog-3295782101191388304.post-79747906898888436372012-02-03T06:43:00.000-08:002012-02-03T06:43:54.220-08:00Fabrication of Nanosized Cuprous Oxide Using Fehling's Solution<br />
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<span lang="EN-US">A facile
method for the synthesis of Cu</span><span lang="EN-US" style="font-family: "F9","sans-serif"; font-size: 6.0pt; line-height: 115%; mso-ansi-language: EN-US; mso-bidi-font-family: F9;">2</span><span lang="EN-US">O nanoparticles by reduction of Fehling's solution, using glucose as
reducing agent. Copper sulfate is used as a precursor with potassium sodium
tartarate in an alkaline media to produce Fehling's solution. The precipitation
of Cu</span><span lang="EN-US" style="font-family: "F9","sans-serif"; font-size: 6.0pt; line-height: 115%; mso-ansi-language: EN-US; mso-bidi-font-family: F9;">2</span><span lang="EN-US">O nanoparticles from this solution
in the presence of glucose was controlled by addition of SLES or Triton-X 100
as surfactants. The reactions have been carried out at 60</span><span lang="EN-US" style="font-family: "F10","sans-serif"; font-size: 6.0pt; line-height: 115%; mso-ansi-language: EN-US; mso-bidi-font-family: F10;">_</span><span lang="EN-US">C with high repeatability. The purification
process of the Cu</span><span lang="EN-US" style="font-family: "F9","sans-serif"; font-size: 6.0pt; line-height: 115%; mso-ansi-language: EN-US; mso-bidi-font-family: F9;">2</span><span lang="EN-US">O product does
not require expensive methods, since a solid product isobtained from a reaction
in liquid phase.<o:p></o:p></span></div>
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<b><span lang="EN-US" style="font-family: "F7","sans-serif"; font-size: 10.0pt; mso-ansi-language: EN-US; mso-bidi-font-family: F7;">Materials<o:p></o:p></span></b></div>
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<li><span lang="EN-US" style="font-family: F12, sans-serif; text-indent: -0.25in;"><span style="font-size: x-small;">1</span><span style="font: normal normal normal 7pt/normal 'Times New Roman';"><span style="font-size: small;"> </span></span></span><span lang="EN-US" style="font-family: F12, sans-serif; text-indent: -0.25in;">CuSO</span><span lang="EN-US" style="font-family: F13, sans-serif; text-indent: -0.25in;">4</span><span lang="EN-US" style="font-family: F12, sans-serif; text-indent: -0.25in;">.5H</span><span lang="EN-US" style="font-family: F13, sans-serif; text-indent: -0.25in;">2</span><span lang="EN-US" style="font-family: F12, sans-serif; text-indent: -0.25in;">O,</span></li>
<li><span lang="EN-US" style="font-family: F12, sans-serif; text-indent: -0.25in;">2<span style="font: 7.0pt "Times New Roman";"> </span></span><span lang="EN-US" style="font-family: F12, sans-serif; text-indent: -0.25in;">Potassium sodium tartarate tetrahydrate,</span></li>
<li><span lang="EN-US" style="font-family: F12, sans-serif; text-indent: -0.25in;">3<span style="font: 7.0pt "Times New Roman";"> </span></span><span lang="EN-US" style="font-family: F12, sans-serif; text-indent: -0.25in;">Triton-X 100,</span></li>
<li><span lang="EN-US" style="font-family: F12, sans-serif; text-indent: -0.25in;">4<span style="font: 7.0pt "Times New Roman";"> </span></span><span lang="EN-US" style="font-family: F12, sans-serif; text-indent: -0.25in;">Sodium laureth sulfate</span></li>
<li><span lang="EN-US" style="font-family: F12, sans-serif; text-indent: -0.25in;">5<span style="font: 7.0pt "Times New Roman";"> </span></span><span lang="EN-US" style="font-family: F12, sans-serif; text-indent: -0.25in;">NaOH analytical grade</span></li>
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<b><span lang="EN-US" style="font-family: "F12","sans-serif"; font-size: 10.0pt; mso-ansi-language: EN-US; mso-bidi-font-family: F12;">Preparation of Cu2O Nanoparticles<o:p></o:p></span></b></div>
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<span lang="EN-US">Fehling's
solution which is comprised of equal parts of the following solutions was first
made:<o:p></o:p></span></div>
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<i><span lang="EN-US">Solution 1:</span></i><span lang="EN-US"> Was made by dissolving of copper (II) sulfate
pentahydrate (6.9 g 0.02 mol) in distilled water (100 mL).<o:p></o:p></span></div>
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<i><span lang="EN-US">Solution 2:</span></i><span lang="EN-US"> Was made by dissolving of potassium sodium
tartarate tetrahydrate (34.6 g) and sodium hydroxide (12 g) in distilled water
(100 mL).<o:p></o:p></span></div>
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<span lang="EN-US">50 mL of
each of the above solutions were mixed together in a beaker and Triton X-100 or
SLES (2 g) was added to the mixture and vigorously stirred for 15 m. To this
mixture, aqueous solution containing 5 g of glucose in 50 mL water was added
and the whole content was then heated at 60° under continuous stirring. A
brick-red solid of Cu2O precipitated after a short period of reaction time. The
solid was filtered off, washed with deionized water (3 times) and ethanol (2
times) and it was dried in an oven at 80</span><span lang="EN-US" style="font-family: "F16","sans-serif"; font-size: 7.0pt; line-height: 115%; mso-ansi-language: EN-US; mso-bidi-font-family: F16;">°</span><span lang="EN-US">C for 3 h to afford nanosized Cu</span><span lang="EN-US" style="font-family: "F13","sans-serif"; font-size: 7.0pt; line-height: 115%; mso-ansi-language: EN-US; mso-bidi-font-family: F13;">2</span><span lang="EN-US">O, 1.38 g (97% yield based n the used copper
sulfate; each mole of copper sulfate produces 0.5 mole of Cu</span><span lang="EN-US" style="font-family: "F13","sans-serif"; font-size: 7.0pt; line-height: 115%; mso-ansi-language: EN-US; mso-bidi-font-family: F13;">2</span><span lang="EN-US">O).<o:p></o:p></span></div>
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<span lang="EN-US"><br /></span></div>
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<span lang="EN-US">Tomado de :</span></div>
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<span lang="EN-US"><br /></span></div>
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<span lang="EN-US"></span></div>
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<b><span lang="EN-US" style="font-size: 12.0pt; line-height: 115%; mso-ansi-language: EN-US; mso-bidi-font-size: 11.0pt;">Fabrication of Nanosized Cuprous Oxide Using Fehling's Solution<o:p></o:p></span></b></div>
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M. Kooti <span style="font-family: "F2","sans-serif"; font-size: 8.0pt; line-height: 115%; mso-bidi-font-family: F2;"> </span>and L. Matouri</div>
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<span lang="EN-US" style="font-family: "F1","sans-serif"; font-size: 8.0pt; mso-ansi-language: EN-US; mso-bidi-font-family: F1;">Transaction F: Nanotechnology<o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "F1","sans-serif"; font-size: 8.0pt; mso-ansi-language: EN-US; mso-bidi-font-family: F1;">Vol. 17, No. 1, pp. 73-78<o:p></o:p></span></div>
<br />
<br />Cesar Costa Verahttp://www.blogger.com/profile/08593067130012155534noreply@blogger.com0tag:blogger.com,1999:blog-3295782101191388304.post-45539121979443436572012-02-03T06:29:00.000-08:002012-02-03T06:29:10.363-08:00Facile preparation of water-soluble fluorescent gold nanoclusters<br />
A simple one-pot strategy of preparing small fluorescent AuNCs using a mild reductant, tetrakis-<br />
(hydroxymethyl)phosphonium chloride (THPC). For biological imaging applications, a zwitterionic functional ligand, D-penicillamine (DPA), was chosen as a capping agent to endow the gold clusters with good stability in aqueous solvent.<br />
<br />
Materiales<br />
<br />
<br />
1. Tetrakis(hydroxymethyl) phosphonium chloride (THPC, P(CH2OH)4Cl, 80% aqueous solution),<br />
2. D-penicillamine (DPA),<br />
3. Rhodamine 6G<br />
4. Gold(III) chloride trihydrate (HAuCl4.3H2O)<br />
5. Sodium borohydride (NaBH4)<br />
6. High purity deionized water<br />
<br />
Síntesis<br />
<br />
<br />
12 ml THPC (80%) was added to 47 ml NaOH solution (6 mM) at 37 C. The mixture was stirred for 3<br />
min, followed by rapid addition of a solution of HAuCl4 (0.67ml, 2% by mass) and DPA (2.5 ml, 0.1 M). The reaction, during which the colorless solution slowly turned light yellow, was stopped after stirring for 15 h.<br />
<br />
<br />
As-prepared AuNCs were purified by triple centrifugation filtration, using Nanosep filters (PallNanosep, Ann Arbor, MI) with a molecular weight cut-off of 3 kDa to remove impurities. The yellowish DPA–AuNCs<br />
remaining on the filter could be re-suspended readily in water,and the solution was stored at 4 C for later use<br />
<br />
Tomado de:<br />
<br />
<br />
Facile preparation of water-soluble fluorescent gold nanoclusters for cellular imaging applications<br />
<br />
Li Shang,a Ren e M. D€orlich,a Stefan Brandholt,a Reinhard Schneider,b Vanessa Trouillet,c Michael Bruns,c<br />
Dagmar Gerthsenb and G. Ulrich Nienhaus<br />
<br />
Nanoscale, 2011, 3, 2009<br />
<br />
http://dx.doi.org/10.1039/c0nr00947d<br />
<br />
<br />
<br />
<br />
<br />
<br />Cesar Costa Verahttp://www.blogger.com/profile/08593067130012155534noreply@blogger.com0tag:blogger.com,1999:blog-3295782101191388304.post-45934195058934345852012-02-03T06:21:00.000-08:002012-02-03T06:21:03.602-08:00Preparation of Silver Nanoparticles<br />
Uniform silver nano particles can be obtained through the reduction of silver ions by ethanol at a temperature of<br />
80°C to 100°C under atmospheric conditions [4]. In this synthesis process, 20 ml of aqueous solution containing silver nitrate (0.5g of AgNO3), 1.5 g sodium linoleate (C18H32ONa), 8 ml ethanol and 2 ml linoleic acid (C18H32O2) are added in a capped tube under agitation. The system is sealed and treated at the temperatures between 80°C to100°C for 6 hours.<br />
<br />
<br />
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<b>Materiales<o:p></o:p></b></div>
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<!--[if !supportLists]-->1.<span style="font: 7.0pt "Times New Roman";">
</span><!--[endif]--><b><span style="color: #333333; font-family: "Verdana","sans-serif"; font-size: 8.5pt; line-height: 115%; mso-bidi-font-family: Verdana;">silver nitrate </span></b><b><span style="color: #333333; font-family: Wingdings; font-size: 8.5pt; line-height: 115%; mso-ascii-font-family: Verdana; mso-bidi-font-family: Verdana; mso-char-type: symbol; mso-hansi-font-family: Verdana; mso-symbol-font-family: Wingdings;">à</span></b><b><span style="color: #333333; font-family: "Verdana","sans-serif"; font-size: 8.5pt; line-height: 115%; mso-bidi-font-family: Verdana;"> 5g</span></b></div>
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<!--[if !supportLists]-->2.<span style="font: 7.0pt "Times New Roman";">
</span><!--[endif]--><b><span style="color: #333333; font-family: "Verdana","sans-serif"; font-size: 8.5pt; line-height: 115%; mso-bidi-font-family: Verdana;">sodium linoleate </span></b><b><span style="color: #333333; font-family: Wingdings; font-size: 8.5pt; line-height: 115%; mso-ascii-font-family: Verdana; mso-bidi-font-family: Verdana; mso-char-type: symbol; mso-hansi-font-family: Verdana; mso-symbol-font-family: Wingdings;">à</span></b><b><span style="color: #333333; font-family: "Verdana","sans-serif"; font-size: 8.5pt; line-height: 115%; mso-bidi-font-family: Verdana;"> 15 g</span></b></div>
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<!--[if !supportLists]-->3.<span style="font: 7.0pt "Times New Roman";">
</span><!--[endif]--><b><span style="color: #333333; font-family: "Verdana","sans-serif"; font-size: 8.5pt; line-height: 115%; mso-bidi-font-family: Verdana;">Ethanol </span></b><b><span style="color: #333333; font-family: Wingdings; font-size: 8.5pt; line-height: 115%; mso-ascii-font-family: Verdana; mso-bidi-font-family: Verdana; mso-char-type: symbol; mso-hansi-font-family: Verdana; mso-symbol-font-family: Wingdings;">à</span></b><b><span style="color: #333333; font-family: "Verdana","sans-serif"; font-size: 8.5pt; line-height: 115%; mso-bidi-font-family: Verdana;">
50 mL</span></b></div>
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<!--[if !supportLists]-->4.<span style="font: 7.0pt "Times New Roman";">
</span><!--[endif]--><b><span style="color: #333333; font-family: "Verdana","sans-serif"; font-size: 8.5pt; line-height: 115%; mso-bidi-font-family: Verdana;">linoleic acid </span></b><b><span style="color: #333333; font-family: Wingdings; font-size: 8.5pt; line-height: 115%; mso-ascii-font-family: Verdana; mso-bidi-font-family: Verdana; mso-char-type: symbol; mso-hansi-font-family: Verdana; mso-symbol-font-family: Wingdings;">à</span></b><b><span style="color: #333333; font-family: "Verdana","sans-serif"; font-size: 8.5pt; line-height: 115%; mso-bidi-font-family: Verdana;"> 50 mL</span></b></div>
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<b><span style="color: #333333; font-family: "Verdana","sans-serif"; font-size: 8.5pt; line-height: 115%; mso-bidi-font-family: Verdana;"><br /></span></b></div>
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<span style="color: #333333; font-family: Verdana, sans-serif;"><span style="font-size: 11px; line-height: 12px;"><b><br /></b></span></span></div>
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<span style="color: #333333; font-family: Verdana, sans-serif;"><span style="font-size: 11px; line-height: 12px;"><b>TTomado de:</b></span></span></div>
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<span style="color: #333333; font-family: Verdana, sans-serif;"><span style="font-size: 11px; line-height: 12px;"><b><br /></b></span></span></div>
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<span style="color: #333333; font-family: Verdana, sans-serif;"><span style="font-size: 11px; line-height: 12px;"><b></b></span></span></div>
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<span style="color: #333333; font-family: Verdana, sans-serif;"><b>PPreparation of Silver Nanoparticles and <b style="text-indent: -0.25in;"></b></b></span></div>
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<span style="color: #333333; font-family: Verdana, sans-serif;"><b><b style="text-indent: -0.25in;">Their Characterization</b></b></span></div>
<br />
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<span style="color: #333333; font-family: Verdana, sans-serif;"><b>R. Das, S. S. Nath, D. Chakdar, G. Gope, R. Bhattacharjee</b></span></div>
<br />
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<span style="color: #333333; font-family: Verdana, sans-serif;"><span style="font-size: 11px; line-height: 12px;"><b><br /></b></span></span></div>
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<span style="color: #333333; font-family: Verdana, sans-serif;"><span style="font-size: 11px; line-height: 12px;"><b>www.azonano.com/oars.asp</b></span></span></div>
<br />Cesar Costa Verahttp://www.blogger.com/profile/08593067130012155534noreply@blogger.com0tag:blogger.com,1999:blog-3295782101191388304.post-60325313894972573552011-11-24T14:25:00.001-08:002011-11-24T14:29:47.867-08:00Preparation and Properties of Colloidal CdSe Quantum Dots<br />
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<b><u><span lang="EN-US" style="font-family: "Times New Roman","serif"; font-size: 12.0pt;">Objective:<o:p></o:p></span></u></b></div>
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<span lang="EN-US" style="font-family: "Times New Roman","serif"; font-size: 12.0pt; line-height: 200%;"> CdSe quantum dots will be synthesized anaerobically
from elemental selenium and cadmium oxide.
The resulting quantum dots will be characterized by their emission
properties.<o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman","serif"; font-size: 12.0pt; line-height: 200%;"></span></div>
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<b><u><span lang="EN-US" style="font-size: 12pt;">Experimental:</span></u></b><span lang="EN-US" style="font-size: 12pt;"> <o:p></o:p></span></div>
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<span lang="EN-US" style="font-size: 12pt; line-height: 200%;"> The synthesis of quantum dots
requires a nucleation step, separate from dot growth. To achieve a complete nucleation, solutions
of Se and CdO are prepared separately and then combined. <b>Preparation
of CdO solution:</b> A 25mL 3-neck round
bottom flask is equipped with a stir bar and a septum in all three ports. The top port is used to purge and vent the
system with Ar, the left port is equipped with a temperature probe attached to
a digital thermometer, and the right port is used for addition of
reagents. 0.100mmol (0.0127g) of CdO and
0.400mmol (0.1140g) of stearic acid are added to the round bottom flask and
heated, with a heating mantle, to 150°C until the CdO has fully dissolved. Reaction is cooled to about room temperature
and 5.017mmol (1.9400g) of trioctylphosphine oxide (TOPO) and 8.035mmol
(1.9400g) of hexadecylamine (HDA) are added to the flask. Reaction is heated to 320°C and becomes
optically clear. <b>Preparation of Se Solution: </b>To
a 15mL side arm pear shaped flask equipped with a stir bar, 1.000mmol (0.0790g)
of selenium powder, and 2.10mL of dioctylamine are added. The side arm is equipped with a screw top cap
and Teflon seal facing the inside of the flask, so as to keep material from
clumping in the side arm. The top of the
flask is equipped with a septum and an Argon inlet-needle, and a vent needle. The reaction flask is purged for 10min with
Ar. A 1mL syringe with a 4” stainless
steel needle is purged with Ar and then used to remove 0.290mL of tributylphosphine
(TBP) from a sure seal bottle. The TBP
is then injected into the flask via the Teflon coated disk on the side arm. <b>Combination of Solutions: </b>Once the CdO solution has reached 320°C
the entire Se solution is added using a 5mL glass syringe with a 4” stainless
steel needle. The reaction temperature
is reduced to 290°C and ≈5µL aliquots are removed at 2sec, 40sec, 90sec, 130
sec, 310sec, and 600sec; each aliquot is diluted to 3mL with chloroform in a
microfuge tube. After ten minutes the
reaction is cooled to room temperature and 15mL of chloroform is added to the
reaction. <b>Reaction purification and data collection: </b>The final reaction mixture is transferred
equally into two 15mL centrifuge tubes and centrifuged at max speed for
20min. The supernatant is collected and
centrifugation is repeated until the resulting supernatant is clear. Once optically clear the QD’s were
precipitated by adding methanol into the chloroform solution and isolated by
centrifugation and decantation. The
aliquots collected and diluted in microfuge tubes are used without further
purification and UV-Vis data is obtained from 350-700nm. Samples are
diluted so that they have an optical density at the first excition absorption
peak below .1 in order to avoid any signicant reabsorption; fluorescence
emission data is obtained.<o:p></o:p></span></div>
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<span lang="EN-US" style="font-size: 12pt; line-height: 200%;"></span></div>
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<b><u><span lang="EN-US" style="font-size: 12pt; line-height: 200%;">References:<o:p></o:p></span></u></b></div>
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<a href="https://blogger.googleusercontent.com/img/b/R29vZ2xl/AVvXsEjI9oVoApoysHtbxb4AVAj2dcA3hnOBfo9kVt_DgMn-pwFs99mPB-fSsxLul8sPd724pT5MjCPi9F2WodrWZVkW7iCLtg_W6FfAPfQ5RXIDWuC-Q5HCV0DrM077q-dJgUfAYVjVdHTCMG3v/s1600/UVVIS+QD+CdSe.jpg" imageanchor="1" style="margin-left: 1em; margin-right: 1em;"><img border="0" src="https://blogger.googleusercontent.com/img/b/R29vZ2xl/AVvXsEjI9oVoApoysHtbxb4AVAj2dcA3hnOBfo9kVt_DgMn-pwFs99mPB-fSsxLul8sPd724pT5MjCPi9F2WodrWZVkW7iCLtg_W6FfAPfQ5RXIDWuC-Q5HCV0DrM077q-dJgUfAYVjVdHTCMG3v/s1600/UVVIS+QD+CdSe.jpg" /></a></div>
<div class="MsoListParagraphCxSpMiddle" style="line-height: normal;">
<span lang="EN-US" style="font-size: 12pt; text-indent: -24px;">Qu, L.; Peng, X. <i>J. Am.
Chem. Soc.</i> <b>2002,</b> <i>124</i>, 2049.</span></div>
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<br />
<br />Cesar Costa Verahttp://www.blogger.com/profile/08593067130012155534noreply@blogger.com0tag:blogger.com,1999:blog-3295782101191388304.post-76823484534860508992011-10-19T07:02:00.000-07:002011-10-19T07:03:16.041-07:00PropósitoPodemos usar este blog para organizar la discusión de los posibles experimentos que se realizarían en el <span class="Apple-style-span" style="color: #cc0000;"><b>Taller Práctico Experimental </b></span> de la escuela de <span class="Apple-style-span" style="color: cyan; font-size: large;"><i>NanoAndes 2012</i></span>. Todos los participantes pueden:<br />
<br />
<ul><li>Crear entradas y comentar sobre otras. </li>
<li>Proponer recetas, métodos y procedimientos </li>
<li>Añadir links, documentos y otros recursos relevantes</li>
<li>Plantear preguntas y respuestas </li>
<li>Reunir los resultados, tanto preliminares de las pruebas y tests, como los que eventualmente obtengan los participantes</li>
</ul>En esta plataforma trataremos de compilar la información y dar seguimiento al proceso de definición de los temas, los experimentos, las tareas y demás aspectos necesarios.Cesar Costa Verahttp://www.blogger.com/profile/08593067130012155534noreply@blogger.com0