Questions tagged [distillation]

For questions about the process of distillation. For the distillation process used in metal refining, also use the [metallurgy] tag.

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Distilling milligram quantities of oil like it's late 1970s

In a currently retracted* manuscript by Tomas Hudlicky [1, Retraction Watch] the following has been noted: Fifty years ago professors took an active part in all laboratory instructions and they ...
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386 views

Why is ethanol distilled off before adding water in the first step of a malonic synthesis?

I am doing a malonic synthesis shown below, and I wonder why I should distill ethanol off before adding water in the first step of the reaction (First I add absolute ethanol and solid sodium).
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Do theoretical plates required to obtain a pure product decrease under vacuum distillation?

For this question I am using Ethanol as an example. The following is the vapor-liquid equilibrium diagram for Ethanol under atmospheric pressures. Under reduced pressures do the number of theoretical ...
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Is there a way to form only ortho product without using fractional distillation?

Using benzene and ethane as your only source of carbon in the final molecule, synthesize the following using any useful reagents. Reaction must form pure ortho compound. I have to form the product ...
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Is it possible to fractionally distill a compound made up of substances with very similar boiling points?

Let's say I have a solution that is made up of substances that have very similar boiling points, say less than 5 degrees apart. Is it even possible to fractionally distill those substances, say, using ...
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How concentrated does sulfuric acid need to be for nitric acid synthesis (H2SO4 + nitrate salt distillation)?

So I have a home lab setup and recently found myself in need of some nitric acid. I could just buy some, but I thought it would be a useful exercise to make my own. I have plenty of nitrate salts ...
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29 views

Strange Distillation Behavior

I was attempting a fractional distillation with 1mL water and 1mL propylene glycol, and I’ve been encountering strange behavior with the heating of the mixture. The heating curve shows strange “spikes”...
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24 views

Is the width of a Soxhlet Condenser Inherent to its Function?

Soxhlet extractors are often coupled to a specifically designed condenser with a very large lower joint. Is this inherent to it's function as a condenser in the apparatus or only because the Soxhlet ...
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31 views

Reason for rounded fitting at the top end of Allihn Condenser

I am purchasing an essential oil distillation setup. The Allihn Condenser at the top end, and the attached glassware, are rounded. It is supposedly 24/40. I have never seen this. If one of them broke, ...
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37 views

How to handle CO2 being evolved during vacuum distillation?

Setup: vacuum aspirator pump, distillation apparatus with stirring (instead of a bubbler). Partial vacuum around 5" Hg. What would you suggest to hold the vacuum set-point?
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Azeotropic Distillation - Am I interpreting this VLE diagram correctly?

I've been looking at ways to re-concentrate a formic acid-water binary mixture with the VLE diagram below. Am I correct in saying that to concentrate a solution of say , 40% formic acid by weight I ...
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76 views

Distillation of oxalyl chloride

May I use water as a condensing medium while distilling out oxalyl chloride? As oxalyl chloride reacts with water and the products are $\ce{HCl},$ $\ce{CO}$ and $\ce{CO2},$ when there is a leak or ...
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84 views

What causes both components of a binary gas mix to condensate at the same time for a given composition

Okay, so recently I encountered the temperature - mole fraction diagrams for binary vapour-liquid equilibrium. For now, I only consider two-component systems where the components are very similar and ...
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Distillery Transfer Hoses

I was hoping an actual person could offer me some advice. I work in a craft distillery and I'm getting a lot of mixed information on how compatible PVC is with high-proof alcohol. It definitely seems ...
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753 views

How to get anhydrous triflic acid from triflic anhydride?

I require a small amount of triflic acid, and while other research groups do not have any, I did locate some trflic anhydride. Does anyone have a published protocol for obtaining the anhydrous acid ...
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Distillation for separating very close boiling components

When components of a mixture have very similar Boiling Points, say 2 C is distillation ever a viable separation procedure at industrial scale? Assuming one were willing to install a very tall column,...
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200 views

Can I use a Liebig condenser for condensing sulfuric acid?

I have a Liebig condenser but I read that the air cooled condenser is preferred for high temperature boiling points. My question is whether I can still use my Liebig with minimal risk... Should I just ...
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1answer
72 views

Laboratory setup for the distillation of sulfuric acid

Purification of Laboratory Chemicals, 5th Edition, by Armarego, reads (p. 53): Reagents such as water, ammonia, hydrochloric acid, nitric acid, perchloric acid, and sulfuric acid can be purified via ...
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When exactly does the first drop of distillate appear in a distillation?

The below image (source: here) is from a fractional distillation of a mixture of two liquids, one with a boiling point of 69 degrees celsius and the other with a boiling point of 98 degrees celsius. ...
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1answer
64 views

When to use chromatographic separation vs vacuum-assisted rectification distillation?

I'm trying to understand a bit more about industrial scale separation processes. One particular element I'm interested in is the question as to when chromatography (HPLC or Simulated Moving Bed) may ...
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388 views

Column pressure control in distillation

In the industry , it's important to maintain the column pressure control in the distillation column . " Pressure alterations will alter column vapour loads and temperature profiles. . So when using ...
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1answer
42 views

Why is the temperature graph sigmoidal in simple distillation of components with very different bps?

I'm writing an organic chemistry lab report on distillation and I thought I understood this, but the more I look at my lab textbook, I realize I don't. My textbook 1 explains that the temperature of ...
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123 views

Will there be some ethanol evaporating before the boiling point of azeotrope? And will it bring some water with it because of the hydrogen bond?

Before the specific temperature, even if the temperature doesn't reach the boiling point of azeotrope or ethanol or water, we know that there are still some ethanol evaporate. In this time(before the ...