<a href="https://www.the-hive.ws/forum/showflat.pl?Number=463236&page=23&view=&sb=&Search=&vc=&new=&start=0&xrated=y&&URLForums=" title="Click here to show this downrated post">Nitroethane from Sodium Ethyl Sulfate</a> (Rated as: waste of space) </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post463259"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> Rhodium (Chief Bee) 10-07-03 23:18 No 463259 </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> Waste of space </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> First, you have obviously shown that you are capable of linking to documents at my site, so why are you then copying 10-15 kilobytes of irrelevant text from that document anyway? The only section pertinent to your question is the small section below the "Nitroethane from Sodium Ethyl Sulfate" header, not the entire section on how to prepare Sodium Ethyl Sulfate... Second, to answer your question, I believe that I have read that sodium carbonate works too, but gives a somewhat lowered yield. </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post463272"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> psyloxy (Hive Addict) 10-08-03 00:12 No 463272 </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> a rant from Mr.Unsatisfied </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> Uhm, to add a naive question: why is the use of oleum in sodium ethylsulphate preparation so discouraged around here ? Well, I could answer that question myself in telling me that: SO3 is no fun to play around with. BUT: we have people here handling Cl2, KCN, HgCl2, DMS and all kinds of really nasty chemicals, wouldn't EtNO2 be a worthy enough target to try and handle SO3 ? Both the synth of SO3 and NaEtSO4 with oleum look so damn straight forward and give good yields, that I don't know why everybody avoids it. The opposite is true for the 'state-of-the-art' way IMO, which can be reviewed at: <a href="../novel/000251119.html#Post251119">Post 251119</a> (Bandil: "Nitroethane ala Antoncho succes", Novel Discourse). Now, I know I haven't come up with anything better but this looks like a not-so-much-fun way to get 3mL of nitroethane. anyway: here are my collected notes concerning SO3 / oleum preparation, surely taken somewhere from Rh.ws and the Hive: A simple method for SO3 could be heating NaHSO4 or KHSO4. The reaction will be in two stages, one at 200-300°C, when the alkali pyrosulfate is formed, and then the other at 500°C when SO3 is formed because of the thermal decomposition of the pyrosulfate (those temps seem to be correct for KHSO4 ??). The reactions are: 1: 2 NaHSO4 __> Na2S2O7 + H2O 2: Na2S2O7 ___> Na2SO4 + SO3 To produce sulfur trioxide, sodium bisulfate is first dried in a thin layer on a pan in an oven set at 300°F. Let it dry for at least an hour. The sodium bisulfate is then placed in a flask set for distillation. Heat this under a gas flame. The bisulfate will melt and convert to sodium pyrosulfate and water. Try to control the heat to where water is just being produced. Collect the water and discard. When no more water is produced heat the flask more vigorously and the sodium pyrosulfate that was previously formed will decompose into sulfur trioxide and sodium sulfate. Collect this gas in a cooled flask. It will liquify and then solidify if the temperature is low enough. If fuming sulfuric acid is the goal, collect the gas in chilled concentrated sulfuric acid. --psyloxy-- </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post463311"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> Vitus_Verdegast (Hive Bee) 10-08-03 04:54 No 463311 </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> More suggestions... </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> Pyrosulfuric acid, or H2S2O7 corresponds to H2SO4 + SO3, and is in fact oleum containing ~40-45% SO3. It has a melting point of 36°, and is easily prepared by the addition of 2 molar equivalents of sulfuric acid to one mol equiv. of sodium pyrosulfate (Na2S2O7). Sodium pyrosulfate itself is easily prepared by heating sodium bisulfate above its melting point. <center>2NaHSO4 __> Na2S2O7 + H2O Na2S2O7 + 2H2SO4 __> H2S2O7 + 2NaHSO4 </center> Sulfur trioxide can be readily prepared by the oxidation of sulfur dioxide with Caro's acid (permonosulfuric acid). If potassium persulfate is digested with 40% sulfuric acid in a freezing mixture so that there is no rise in temperature; or if conc. H2SO4 and 5% H2O2 are mixed together, permonosulfuric acid is obtained. The pure acid forms a white crystalline mass which melts at about 45° and is relatively stable. <center> H2SO4 + H2O2 <__> H2O + H2SO5 </center> The solid acid is best obtained by the action of chlorosulfonic acid on anhydrous hydrogen peroxide <img src="../forum/images/icons_lightgrey/crazy.gif" alt="crazy" title="Crazy" heigth="15" width="15">: <center> ClSO3H + H2O2 <__> HCl + H2SO5 </center> Source: Mellor's Modern Inorganic Chemistry, rev. ed. 1963 <hr><a href="http://www.poedecoder.com/Qrisse/works/dreamw.html" target="_blank" title="Jump to this external site">A Dream Within A Dream</a> (http://www.poedecoder.com/Qrisse/works/dreamw.html) </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post463595"></a><a name="last"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> wolfram (Newbee) 10-09-03 17:46 No 463595 </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> Sorry </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> I humbly appollogise Grand Master Rhodium for my offence. <img src="../forum/images/icons_lightgrey/blush.gif" alt="blush" title="Blush" heigth="15" width="15"><img src="../forum/images/icons_lightgrey/blush.gif" alt="blush" title="Blush" heigth="15" width="15"><img src="../forum/images/icons_lightgrey/blush.gif" alt="blush" title="Blush" heigth="15" width="15"> </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> </body> </html>

Nitroethane from Sodium Ethyl Sulfate , Hive Chemistry Discourse


		wolfram 10-07-03 21:06				<a href="https://www.the-hive.ws/forum/showflat.pl?Number=463236&page=23&view=&sb=&Search=&vc=&new=&start=0&xrated=y&&URLForums=" title="Click here to show this downrated post">Nitroethane from Sodium Ethyl Sulfate</a> <br> <i title="This post has been downrated by the moderators">(Rated as: waste of space)</i> </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post463259"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> <font color="#FF0033">Rhodium</font><br> <i>(<span title="The user's title at the time of posting">Chief Bee</span>)</i><br> <span title="Posting date">10-07-03 23:18</span><br> <span title="Link to this post by using the markup [463259]">No 463259</span><br> </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Waste of space</b> </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> First, you have obviously shown that you are capable of linking to documents at my site, so why are you then copying 10-15 kilobytes of irrelevant text from that document <b>anyway</b>? The only section pertinent to your question is the small section below the "Nitroethane from Sodium Ethyl Sulfate" header, not the entire section on how to prepare Sodium Ethyl Sulfate...<br><br>Second, to answer your question, I believe that I have read that sodium carbonate works too, but gives a somewhat lowered yield. </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post463272"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> psyloxy<br> <i>(<span title="The user's title at the time of posting">Hive Addict</span>)</i><br> <span title="Posting date">10-08-03 00:12</span><br> <span title="Link to this post by using the markup [463272]">No 463272</span><br> </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">a rant from Mr.Unsatisfied</b> </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> Uhm, to add a naive question: why is the use of oleum in sodium ethylsulphate preparation so discouraged around here ? Well, I could answer that question myself in telling me that: SO<sub>3</sub> is no fun to play around with. BUT: we have people here handling Cl<sub>2</sub>, KCN, HgCl<sub>2</sub>, DMS and all kinds of really nasty chemicals, wouldn't EtNO<sub>2</sub> be a worthy enough target to try and handle SO<sub>3</sub> ? Both the synth of SO<sub>3</sub> and NaEtSO<sub>4</sub> with oleum look so damn straight forward and give good yields, that I don't know why everybody avoids it. The opposite is true for the 'state-of-the-art' way IMO, which can be reviewed at: <span title="Jump to this post"><a href="../novel/000251119.html#Post251119">Post 251119</a> <i>(Bandil: "Nitroethane ala Antoncho succes", Novel Discourse)</i></span>. Now, I know I haven't come up with anything better but this looks like a not-so-much-fun way to get 3mL of nitroethane.<br><br><b>anyway: here are my collected notes concerning SO<sub>3</sub> / oleum preparation</b>, surely taken somewhere from Rh.ws and the Hive:<br><br>A simple method for SO<sub>3</sub> could be heating NaHSO<sub>4</sub> or KHSO<sub>4</sub>. The reaction will be in two stages, one at 200-300°C, when the alkali pyrosulfate is formed, and then the other at 500°C when SO<sub>3</sub> is formed because of the thermal decomposition of the pyrosulfate (those temps seem to be correct for KHSO<sub>4</sub> ??). The reactions are: <br><br>1: 2 NaHSO<sub>4</sub> <sup>__</sup>> Na<sub>2</sub>S<sub>2</sub>O<sub>7</sub> + H<sub>2</sub>O <br><br>2: Na<sub>2</sub>S<sub>2</sub>O<sub>7</sub> <sup>___</sup>> Na<sub>2</sub>SO<sub>4</sub> + SO<sub>3</sub> <br><br>To produce sulfur trioxide, sodium bisulfate is first dried in a thin layer on a pan in an oven set at 300°F. Let it dry for at least an hour. The sodium bisulfate is then placed in a flask set for distillation. Heat this under a gas flame. The bisulfate will melt and convert to sodium pyrosulfate and water. Try to control the heat to where water is just being produced. Collect the water and discard. When no more water is produced heat the flask more vigorously and the sodium pyrosulfate that was previously formed will decompose into sulfur trioxide and sodium sulfate. Collect this gas in a cooled flask. It will liquify and then solidify if the temperature is low enough. If fuming sulfuric acid is the goal, collect the gas in chilled concentrated sulfuric acid.<br><br>--<b>psyloxy</b>-- </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post463311"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> Vitus_Verdegast<br> <i>(<span title="The user's title at the time of posting">Hive Bee</span>)</i><br> <span title="Posting date">10-08-03 04:54</span><br> <span title="Link to this post by using the markup [463311]">No 463311</span><br> </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">More suggestions...</b> </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> Pyrosulfuric acid, or H<sub>2</sub>S<sub>2</sub>O<sub>7</sub> corresponds to H<sub>2</sub>SO<sub>4</sub> + SO<sub>3</sub>, and is in fact oleum containing ~40-45% SO<sub>3</sub>. It has a melting point of 36°, and is easily prepared by the addition of 2 molar equivalents of sulfuric acid to one mol equiv. of sodium pyrosulfate (Na<sub>2</sub>S<sub>2</sub>O<sub>7</sub>).<br>Sodium pyrosulfate itself is easily prepared by heating sodium bisulfate above its melting point.<br><br><center>2NaHSO<sub>4</sub> <sup>__</sup>> Na<sub>2</sub>S<sub>2</sub>O<sub>7</sub> + H<sub>2</sub>O<br>Na<sub>2</sub>S<sub>2</sub>O<sub>7</sub> + 2H<sub>2</sub>SO<sub>4</sub> <sup>__</sup>> H<sub>2</sub>S<sub>2</sub>O<sub>7</sub> + 2NaHSO<sub>4</sub><br></center><br><br><br><br>Sulfur trioxide can be readily prepared by the oxidation of sulfur dioxide with Caro's acid (permonosulfuric acid).<br>If potassium persulfate is digested with 40% sulfuric acid in a freezing mixture so that there is no rise in temperature; or if conc. H<sub>2</sub>SO<sub>4</sub> and 5% H<sub>2</sub>O<sub>2</sub> are mixed together, permonosulfuric acid is obtained. The pure acid forms a white crystalline mass which melts at about 45° and is relatively stable.<br><br><center><br>H<sub>2</sub>SO<sub>4</sub> + H<sub>2</sub>O<sub>2</sub> <<sup>__</sup>> H<sub>2</sub>O + H<sub>2</sub>SO<sub>5</sub><br></center><br><br>The solid acid is best obtained by the action of chlorosulfonic acid on anhydrous hydrogen peroxide <img src="../forum/images/icons_lightgrey/crazy.gif" alt="crazy" title="Crazy" heigth="15" width="15">:<br><br><center><br>ClSO<sub>3</sub>H + H<sub>2</sub>O<sub>2</sub> <<sup>__</sup>> HCl + H<sub>2</sub>SO<sub>5</sub><br></center><br><br>Source: <font color="blue">Mellor's Modern Inorganic Chemistry, rev. ed. 1963</font color="blue"> <br> <span title="The signature"><hr><a href="http://www.poedecoder.com/Qrisse/works/dreamw.html" target="_blank" title="Jump to this external site">A Dream Within A Dream</a> (http://www.poedecoder.com/Qrisse/works/<wbr>dreamw.h<wbr>tml)</span> </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post463595"></a><a name="last"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> wolfram<br> <i>(<span title="The user's title at the time of posting">Newbee</span>)</i><br> <span title="Posting date">10-09-03 17:46</span><br> <span title="Link to this post by using the markup [463595]">No 463595</span><br> </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Sorry</b> </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> I humbly appollogise Grand Master Rhodium for my offence.<br><img src="../forum/images/icons_lightgrey/blush.gif" alt="blush" title="Blush" heigth="15" width="15"><img src="../forum/images/icons_lightgrey/blush.gif" alt="blush" title="Blush" heigth="15" width="15"><img src="../forum/images/icons_lightgrey/blush.gif" alt="blush" title="Blush" heigth="15" width="15"> </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> </body> </html>