How to Make Chloroform: A Simple Guide

This article is a summary of the YouTube video ‘Making Chloroform’ by NileRed

Written by: Recapz Bot

Written by: Recapz Bot

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How does it work?
Chloroform, historically an anesthetic, now primarily used as a solvent, synthesized from household products.

Key Insights

  • Chloroform was historically used as an anesthetic but is now mostly used as a solvent.
  • Chloroform can be easily made from household products like concentrated bleach and acetone.
  • The concentration of sodium hypochlorite in the bleach can be determined by reacting it with hydrogen peroxide.
  • The concentration of bleach used in the experiment was approximately 1.28 molar, with a density of about 8.6%.
  • The reaction between bleach and acetone is exothermic, requiring cooling to at least 0 degrees Celsius before adding acetone.
  • An excess of bleach (around 11%) is used to ensure complete consumption of acetone and prevent the formation of azeotrope.
  • After adding acetone, the mixture is shaken and left overnight to allow for complete separation of chloroform from the aqueous layer.
  • Chloroform, sodium hydroxide, and sodium acetate are formed when acetone reacts with sodium hypochlorite.
  • The aqueous layer is carefully decanted multiple times, while chloroform settles at the bottom.
  • The remaining liquid is poured into a beaker, allowing chloroform to settle further.
  • The chloroform layer is separated using a separatory funnel and washed with sodium chloride.
  • The chloroform is distilled using a hot water bath, discarding the cloudy distillate below 60 degrees Celsius.
  • A clear liquid is collected as the distillate at around 60 degrees Celsius, yielding approximately 58 milliliters of chloroform.
  • Ethanol is added to stabilize the chloroform and prevent the formation of phosgene.
  • The final yield of chloroform is approximately 53%.

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Transcript

[Transcript]

Historically, chloroform was widely used as an anesthetic, but nowadays it’s mostly used just as a solvent.

Interestingly, it can be easily made from common household products. In this experiment, the major chemicals I used were 3.6 liters of concentrated bleach and 100 milliliters of acetone.

The first thing that must be done is to determine the concentration of sodium hypochlorite in the bleach. This is done by reacting about 5 milliliters of bleach with 3% hydrogen peroxide. As shown in the equation above, the hydrogen peroxide reacts with the sodium hypochlorite to form water, sodium chloride, and oxygen gas. Hydrogen peroxide is added until no more bubbling occurs and the reaction is complete. The level of the water in the graduated cylinder is measured before and after the addition of the gas. By calculating the amount of gas that has evolved and on the assumption that one mole of gas occupies a volume of 24 liters, we can calculate the concentration of the bleach. The equation that I used is shown above and the result I obtained was that the sodium hypochlorite concentration was about 1.28 molar.

This isn’t necessary, but I used a hydrometer to measure the density of the bleach and I determined that the concentration was about 8.6%.

The bleach was chilled to about -2 degrees Celsius and 150 milliliters was poured out. 150 milliliters is removed to make sure that it has enough space to add the acetone as well as to shake it.

The reaction of bleach with acetone is extremely exothermic and it’s absolutely necessary to cool it to at least 0 degrees Celsius before the addition. I added about a hundred milliliters of acetone to the bleach, which represents an excess of bleach at around 11%. I think an excess between three to five percent is better and 11% is much too high.

We use an excess of bleach because we want to make sure that all of the acetone is consumed. Any leftover acetone could form a difficult to separate azeotrope with the chloroform.

After adding the acetone, the bottle is capped and shaken. The cap is then removed and placed lightly on top to allow any gases to escape. I left the bottle overnight to allow for a complete separation of the chloroform from the aqueous layer. Chloroform is denser than water and immiscible, so it should form a layer on the bottom.

After five minutes the temperature is already at around 30 degrees Celsius. The temperature peaked at around 45 degrees Celsius. For the purpose of the video, I will visually demonstrate the reaction between the acetone and the bleach. When the acetone is added, it reacts with three equivalents of sodium hypochlorite to form chloroform, sodium hydroxide, and sodium acetate. After allowing the solution to sit undisturbed for a short period of time, it’s possible to see chloroform in a separate layer on the bottom. The solution is still yellow due to the presence of unreacted sodium hypochlorite.

Carefully decant the upper aqueous layer. Due to the large amount of water, you’re going to need to do this several times. You should empty the aqueous layer into a waste container labeled bleach and chloroform waste.

Eventually, the remaining liquid of the bleach bottle is poured into the beaker and the chloroform layer is allowed to settle on the bottom. You might notice that the solution is much less yellow than the previous example that I showed. This is because it was allowed to react overnight and the concentration of sodium hypochlorite in the solution is much less.

Leave it for several minutes until the chloroform layer fully separates. Decant off as much of the aqueous layer as possible and then add the rest to a separatory funnel. Allow the two phases to separate and then drain the lower chloroform layer. Add the upper aqueous layer to your waste container.

The chloroform was washed once with saturated sodium chloride and then it was added to a distillation flask containing calcium chloride. The simple distillation of the chloroform was carried out using a hot water bath. The distillate that came over below 60 degrees Celsius was cloudy and it was discarded. The temperature then remained constant at around 60 degrees and the distillate was collected as a clear liquid.

The total volume of chloroform obtained was about 58 milliliters. The chloroform was transferred to a bottle that was wrapped in foil to protect it from light. About one milliliter of absolute ethanol was added to stabilize the chloroform and prevent the formation of phosgene. Again, the final yield was about 58 milliliters, which represents a final yield of about 53 percent.

This article is a summary of the YouTube video ‘Making Chloroform’ by NileRed