The Manufacture of Sodium Cyanide (Notes courtesy Bert Tucker) Sodium cyanide can be manufactured in a number of ways. Two relatively simple methods are described in the scientific literature. The first involves the use of the readily available dye, Prussian Blue (Iron III Ferro cyanide). A second uses the common swimming pool chlorine stabiliser, cyanuric acid. In the first process the Prussian Blue is first converted to sodium ferrocyanide. This is done by allowing it to react with caustic soda in water. Iron oxide is precipitated and sodium ferro cyanide obtained. This sodium ferrocyanide (Yellow Prussate of Soda) is then converted to sodium cyanide by allowing it to react with concentrated sulphuric acid. Fig7.1: Forge reduces sodium cyanate with carbon
The very toxic HCN produced is passed into caustic soda to form the desired salt. There is considerable information available on this process but it was abandoned after initial experiments, considering it too dangerous for the inexperienced home chemist - some of whom may be readers of this book. A more suitable method of safe, small-scale home manufacture of sodium cyanide involves the two stage conversion of the common swimming pool chemical cyanuric acid. Cyanide 95 The first step is carried out by heating powdered cyanuric acid with sodium carbonate. Sodium carbonate is obtained directly as washing soda (or by converting sodium bicarbonate, baking soda). In the second stage, the sodium cyanate produced is reduced to sodium cyanide by heating it with powdered charcoal in a covered crucible (Fig 7.1). It is important that this stage is undertaken outside. In this process, carbon monoxide is given off. The resultant glassy mass is cooled, crushed and filtered with water to remove the soluble sodium cyanide from the remaining insoluble carbon (Fig 7.2). Careful drying produces solid sodium cyanide powder. As with all home manufacture there is a need for great care in carrying out this process. Contaminated items need to be disposed of carefully after traces of cyanide are removed. This is best achieved using chlorine bleach to oxidise any unwanted cyanide and to prevent it contaminating the equipment. The product also needs to be tested by analytic means to determine its concentration and purity. Quantitative tests are available and Exit offers such a service for supporters. Further information that details the manufacturing process can be found in most university and public libraries. The Peaceful Pill Handbook
How to Make Cyanide
Here is a complete recipe on how to make sodium cyanide.
First, 100 g of sodium hydroxide is mixed with 43g of cyanuric acid and 12g of carbon. This is heated to 600 Celsius with occasional stirring for at least an hour. If the bubbling goes out of control, turn down the temperature and let it come back under control before raising it again.
After the mixture is cooled, it is broken up and dissolved in methanol. After all the large chunks are converted to a powder, 100g of sodium bicarbonate is added to convert the excess sodium hydroxide into sodium carbonate. The solution is allowed to stir for 30 minutes and then filtered.
The filtrate maybe tested for cyanide by reacting a few drops with a solution of ferrous sulfate. A deep blue color of Prussian blue indicates cyanide ions are present.
The filtrate is then dried to obtain crude sodium cyanide. Approximate yield 19g.
Cyanide Manufacturing The various processes for the manufacture of cyanide may be classified according to the source from which the nitrogen is derived. The principal methods in use are:
(a) Those in which refuse animal matter is used as the nitrogenous raw material, ferrocyanide being generally produced as an intermediate product. (b) Those in which atmospheric nitrogen is employed to form cyanide compounds, directly or indirectly. (c) Those in which ammonia or ammonium compounds form the nitrogenous raw material, including methods which utilize residues from gas-works.
PRODUCTION OF CYANIDES FROM REFUSE ANIMAL MATTER Until about the year 1890, this was the method almost universally used. The raw materials required are: (1) Nitrogenous animal matter, such as horns, hoofs, dried blood, wool, woollen
rags, hair, feathers, leather-clippings, etc. (2) An alkaline carbonate, such as pearl-ash, sodaash, etc. (3) Iron filings or borings.
The alkali and the iron are first fused together at a moderate heat in an iron pan, or other suitable vessel, contained in a reverberatory furnace. The well-dried animal matter is then introduced in small quantities at a time and stirred in. The heat is then raised and the furnace closed so as to maintain a reducing atmosphere. The hard black mass which forms is then taken out and lixiviated with nearly boiling water. The crude ferrocyanide containing sulphides, sulphates, carbonates and thiocyanates, is crystallized out and purified by recrystallization. The ferrocyanide was formerly converted into cyanide by first dehydrating and then fusing, either alone or with alkaline carbonate:
K4Fe(CN)6+K2CO3 = 5KCN+KCNO+Fe+CO2
The cyanide so formed is always contaminated with cyanates and carbonates, and generally with small amounts of other salts (sulphides, chlorides, thiocyanates, etc.). The procedure frequently adopted at present is to fuse with metallic sodium:
K4FeCy6 + 2Na = 4KCy + 2NaCy + Fe;
thus yielding a mixture of potassium and sodium cyanides free from cyanates, etc. The presence of sulphides and thiocyanates in the product is due chiefly to the sulphur contained in the organic matter. These compounds are partially decomposed and removed by metallic iron during the fusion. When the cyanide is made by direct fusion of ferrocyanide, the product contains carbide of iron, some nitrogen being given off in the process. Most of the volatile organic nitrogen is lost in the form of ammonia or nitrogen gas during the fusion for ferrocyanides, in the first stage of the process.
PRODUCTION OF CYANIDES FROM ATMOSPHERIC NITROGEN It was observed by Scheele that when nitrogen is passed over a mixture of K2CO3 and charcoal heated to redness, a cyanide of potassium is formed. Many attempts were made throughout the nineteenth century to utilize this reaction for industrial purposes. One of the earliest was that of Possoz and Boissiere, who used a mixture of charcoal with 30 per cent. of potassium carbonate. This was kept at a red heat in fire-clay cylinders, through which a mixture of N and CO, produced by passing air over red-hot alkalized carbon, was allowed to pass for about 10
hours. The product was then lixiviated with water in presence of ferrous carbonate (spathic iron ore) to give a ferrocyanide.
4444
It was also observed at an early date (by Clark, in 1837), that cyanides are formed as an efflorescence in blast-furnaces, and that the gases of these furnaces contain cyanogen. Bunsen proposed a special blast-furnace for the production of cyanide, in which coke and potash in alternate layers were to be heated by a strong blast, the fused cyanide running off at the bottom of the furnace. It was found, however, that a very high temperature was necessary, as the potassium compound must be reduced to metallic potassium before combination with atmospheric nitrogen takes place.
Better results were obtained by substituting barium carbonate for K2CO3, as in the process of Margueritte and DeSourdeval (1861). Air (deoxygenated by hot carbon) was passed over a previously ignited mixture of BaCO3, iron-filings, coal tar, and sawdust, whereby barium cyanide is produced. This is converted into sodium cyanide by fusion with sodium carbonate. The BaCO3 is first reduced to barium carbide (BaC2):
BaCO2 + 4C = BaC2 + 3CO.
This then combines with nitrogen to form Ba(CN)2. It has been found, however, that only about 30 per cent, of the barium is converted to cyanide, the remainder forming barium cyanamide by a secondary reaction:
Ba(CN)2 = C + BaCN2.
When calcium is substituted for barium in this process, practically the whole is converted into calcium cyanamide:
CaC2 + N2 = C + CaCN2.
Calcium cyanamide is also formed in the electric resistance furnace by passing nitrogen over a mixture of lime and charcoal:
CaO + 2C + N2 = CaCN2 + CO.
By heating the product at a high temperature with a further quantity of carbon, with the addition of salt-to prevent frothing and facilitate the reaction, the cyanamide is converted into cyanide as follows:
CaCN2 + C = Ca(CN)2.
The crude mixture so formed has been used as a substitute for potassium cyanide under the name of “ Cyankalium surrogat,” and is equivalent in cyanogen contents to about 30 per cent. KCN. [See Erlwein and Frank, U. S. patent, 708,333.]
An improved method more recently introduced is to convert the calcium cyanamide into sodium cyanide by the following series of reactions:
(1) By leaching with water, a crystallizable, easily purified salt is obtained, known as dicyandiamide:
2CaCN2 + 4H2O = (CN · NH2)2 + 2Ca(OH)2.
(2) This, when fused with sodium carbonate and carbon, is largely converted into sodium cyanide:
(CN · NH2)2 + Na2CO3 + 2C = 2NaCN + NH3 + N + H + 3CO
A portion of the dicyan-diamide sublimes and polymerizes; this is recovered and re-treated with Na2CO3 in a subsequent operation. The cyanamide and dicyan-diamide are also utilized as sources of products valuable as manures, as they can be readily converted into ammonia, ammonium carbonate, urea, etc.
Cyanides may also be formed by the action of metallic sodium and carbon on atmospheric nitrogen (Castner); but it is preferable to use ammonia as the source of nitrogen in this reaction (see below).
PRODUCTION OF CYANIDES FROM AMMONIA OR AMMONIUM COMPOUNDS When ammonia is passed over mixtures of heated alkali and carbon, only small quantities are converted into cyanide; better results are obtained by passing CO and NH3 through a molten mixture of KOH and carbon, but even by this means much of the ammonia is dissociated into N and H, owing to the great heat which is necessary. It is supposed that potassamide is an intermediate product:
cyanide-productcyanide-product
In Castner’s process (Brit, patents, 12,218, 12,219, of 1894), molten sodium is allowed to flow through a mass of heated coke while ammonia gas is passed upward, the reaction being
2NH3 + 2C + 2Na = 2NaCN + 3H2.
The reaction takes place at a much lower temperature than in the previous process with KOH, and the losses by dissociation of NH3 and volatilization of the cyanide are consequently smaller. It probably takes place in two stages, forming sodamide as an intermediate product:
(1) NH3 + Na = NaNH3 + H (at 300° to 400° C). (2) NaNH2 + C = NaCN + H2 (at dull red heat).
In a modification of this method used by the Deutsche Gold Silber Scheide-Anstalt, metallic sodium is melted with carbonaceous matter in a crucible, and then ammonia is led in at 400° C. — 600° O.; this forms disodium cyanamide:
Na2 + C + 2NH3 = Na2CN2 + 3H2.
By then raising the temperature to 700-800° C., the excess of C. interacts, forming sodium cyanide:
Na2CN2 + C = 2NaCN;
the whole operation being conducted in the same crucible.
Methods have also been proposed by J. Mactear, H. C. Woltereck, and others, in which cyanogen compounds are produced by the action of ammonia gas on gaseous carbon compounds at a high temperature.
In Mactear’s method (Brit, patent, No. 5037, of 1899) the reaction
2NH3 + CO = NH4CN + H2O
is supposed to take place in a closed chamber at 1800° to 2000° F., the products being condensed and absorbed in alkali hydrate and the ammonia liberated for reuse. Instead of CO, a mixture of CO with N and H (producer gas) may be used.
In Woltereck’s method (Brit, patent, No. 19,804, of 1902) “ perfectly dry ammonia and a volatilized or gaseous carbon compound, also perfectly dry, are passed together with hydrogen, in equal volumes, over a strongly heated catalytic agent, such as platinized pumice. One volume of NH3 and two volumes of ‘water-gas’ (CO + H2) make a convenient mixture. The HCN produced is absorbed in an alkaline solution.”
Cyanide has also been made from the trimethylamine (CH3)3N obtained by the distillation of beet-root molasses at a high temperature. This, at a red heat, decomposes, giving NH3, HCN, and H.
Another source of cyanogen compounds is the crude illuminating gas from the distillation of coal. In Knublauch’s method (Brit. patent, No. 15,164, of 1887) the gas is passed through a solution of an alkali or alkaline earth containing ferrous hydrate in suspension. The gas carries
with it ammonium cyanide and thiocyanate, which are absorbed by the mixture and converted into ferrocyanide.
In Rowland’s process (U. S. patent, No. 465,600, of 1891) the gas is passed through a solution of an iron salt, thus forming ammonium ferrocyanide. This is converted into the calcium salt by boiling with lime. The calcium ferrocyanide may then be converted into the required alkali ferrocyanide by decomposing with an alkaline carbonate.
Bueb’s process (Brit, patent, No. 9075, of 1898) is a modification of the above, in which the cyanogen is separated in the form of an insoluble double compound by using a concentrated iron solution (FeSO4); the reactions said to take place are:
FeSO4 + H2S + 2NH3 = FeS + (NH4)2SO4. 2FeS + 6NH4CN = (NH4)2Fe2(CN)6 + 2(NH4)2S.
The insoluble product, known as ” cyanide mud,” is then treated to obtain marketable cyanogen compounds. Many other modifications have been suggested. Cyanides may also be obtained by desulphurizing thiocyanates by means of iron, or by zinc and carbon.
Manufacture of Cyanide from Beet-sugar Residues C. A. Browne describes this process in Columbia School of Mines Quarterly (Ab3. Mining Magazine, Sept. 1913, p. 226).
The residue, containing 12 to 15 per cent, of potassium and 4 per cent, of nitrogen, is heated in retorts and yields a number of volatile products, including ammonia and methylamine. These gases are further heated in tubes to a temperature of 1000° C. whereby the nitrogenous compounds are converted into ammonium cyanide. After cooling and purifying, the gases are passed through sulphuric acid, thus yielding ammonium sulphate and hydrocyanic acid. The latter is absorbed in water, redistilled and collected in sodium hydroxide. This solution is evaporated and crystallized to obtain sodium cyanide.
The remaining combustible gases are led back to the furnace for heating the retorts. About three fourths of the nitrogen in the residues is recovered as ammonium sulphate and sodium cyanide, the remainder escaping as nitrogen gas.
About 5000 tons of sodium cyanide are produced annually by this process by two factories in Germany, the product being exported to the Transvaal.
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How To Make Chloroform For Survival You’ve likely watched many movies where chloroform is used to knock people out in order to kidnap them or disable them for some other reason. It’s definitely good for that, but subversive maneuvers isn’t what it was originally made for. Originally it was used as an anesthetic to knock people out for surgery. Sounds like a handy thing to have in your supplies, right? The problem is that you can’t just walk into your local superstore and pick up a gallon of it from the shelf beside the milk. You can, however, make your own. Chloroform, whether pharmaceutical grade or homemade, is lethal in the wrong hands. Don’t use it without training! That being said, if you have a medically-trained person in your group, knowing how to make it can come in handy in a variety of ways. You can use it to anesthetize people for surgical procedures, or to operate on animals for procedures such as castration. It’s also used in pesticides, disinfectants, dry cleaning solutions, photography development and refrigerators.
This is the Best Natural Painkiller, and Grows in Your Backyard! So, how can you make chloroform at home? Actually, it’s not that difficult – it involves two common household items – but it is a bit dangerous for both the patient and anybody within several feet of it. There are actually a few different ways to make it, but keep in mind that this can very well kill the patient you are trying to save. Yes, I’ve already said that, but it bears repeating. Now, on to it.
Gather Your Ingredients You know all those warnings you’ve heard about mixing your cleaning products? Well there’s a good reason for them. When combined, certain chemicals such as bleach create toxic fumes such as chloroform (yes, I said TOXIC), hydrochloric acid, chloroacetone and other things you really don’t want to breathe. Since we’re actually trying to make one of those chemicals, let’s proceed with it. Household bleach is your first ingredient. It needs to be at least 6 percent without any added ingredients. If you use a higher concentration, you’re going to need more ice, which I’ll explain in a second.
The second ingredient is used by most women for cosmetic purposes and by many men (and women) to shine their rides with an awesome paint job. Acetone, also known as finger nail polish remover or paint reducer. Be careful to read labels though, because these products aren’t always pure acetone, or even acetone at all. You can buy acetone in the cosmetics section of your local superstore and you can also buy it at most paint stores where it will probably be labeled simply as acetone. The final ingredient is one that’s really tricky. You’ll actually have to walk all your way to the freezer for it. It’s ice. So to recap, the ingredients you will need are: household bleach, acetone, ice.
Gather Your Equipment • • • •
You’re going to need a large glass container. HDPE buckets will work because the reagents won’t attack it, but you won’t be able to see the chloroform forming as well. A separation funnel will be needed to separate the chloroform from the other ingredients. You can do it with other tools such as an eye dropper, but that’s a long row to hoe. You can get a separation funnel online for about $25. A gas mask is highly recommended because of the risk of inhaling the fumes. You should make the chloroform in a well-ventilated area even if you’re using the mask. The vapors alone can make you nauseated, give you a headache or even make you pass out. A stir stick will be necessary. Glass is, of course, the best tool for this job.
Make the Chloroform I feel the need to warn you again to be careful. This isn’t something you should use as a family science experiment. If you’re ready to move ahead, gather your ingredients and equipment together in a wellventilated area. It’s best to start with the bleach and acetone chilled even if you’re using ice because the reaction will cause the mixture to heat up by at least 85 degrees. The higher concentrate bleach you use, the hotter it gets. The
ratio for making chloroform needs to be 1 part acetone to 50 parts bleach. That’s 1 teaspoon of acetone per cup of bleach.
• •
• •
Place the bleach in the container, then add several ice cubes. Add the acetone and stir the mixture, or swirl it around if you’re using a vessel that allows you to do that without sloshing it out. If you’re using a high concentrate of bleach, i.e. 12 percent, add more ice. Leave the mixture alone for 30 minutes to an hour so that the chemical reaction can develop and the mixture can cool. First you’ll notice a white cloud of vapor coming from the solution and the solution itself will become cloudy. You don’t want to breathe this! You’ll also be able to see a white residue, powder, or bubble forming on the bottom. That’s the chloroform. After the hour is up and the mixture is cool, gently pour most of the liquid off the top. Be careful to leave the chloroform on the bottom. Once you’ve gotten most of the liquid out, transfer the rest to your separation funnel. Let it settle, then drain the chloroform out, leaving behind the water. You’ll yield around 50-70 percent of your starting material volume in chloroform. At this point, the chloroform is created but if you’re going to use it on people, or animals for that matter, it needs to be distilled in order to purify it. Obviously, you’ll need a distiller for that.
Other Ingredients to Combine If you have a copper still (and who doesn’t?) laying around, this is the way to distill your chloroform into liquid. You can use the ingredients listed above or you can use 4 parts of bleaching powder (32.5-34.5 percent), 3 parts 96% alcohol, and 13 parts water. The actual distillation process for this is lengthy and requires several different steps. It’s not particularly viable for the average person, but I wanted to make you aware of it. Because chloroform, either pharmaceutical grade or homemade, is thought to be carcinogenic, is dangerous to use and make, and doesn’t have much of a shelf life, it may not be your best option for use in a survival situation. Topical analgesics or oral pain meds may be the better option. Shoot, even doing it like they did in the Wild West is a better option – take a shot of liquor til you feel no pain. Seriously, chloroform is nothing to fool around with. If you want to make it at home, now you know how but do so with care. Your life, or the life of the person you administer it to, will depend upon it. Being skilled is the only asset that you can really count on if things are going South. Be prepared and train your medical skills to face disaster!
https://www.survivopedia.com/diy-chloroform-for-survival/
How to make chloroform
Hello readers, In this post we will talk about “how to make chloroform”. To begin with,i must say this: This is not for everybody. You need special equipment, hard to get chemicals and most of all specialized safety gear. This is not a game, making chloroform is dangerous, as is the chloroform itself. It can cause serious diseases and can even kill if not handled correctly. SO BE CAREFUL WITH IT. Only qualified people should handle this chemical. This should be made in a laboratory, for security reason, even though it can be made at home as well. Chemicals required for the process: – most important a separation funnel – pure acetone (hard to get) – bleach (this can be purchased easily) – ice (normal ice) – glassware (you will need to use glass for the process, plastic or metal containers are not good) Once you have those ingredients, you will need to procure the safety equipment, a gas mask and some gloves. When you have it all follow the steps i wrote here: 1. step: You will need the bleach (half a liter). Take the glass container (make sure it is a clear container, with no residues in it, and you can see clearly through/in it. Now add ice to the mix (you need to keep the bleach at a low temperature). 2. Step: You need 1:50 ratio here, so we need to add the acetone to the mixture. Add only 10ml of it since we have half a liter of bleach. We need to add ice again(if you don’t add the ice fumes will raise and that is bad). 3. Step: Now we leave the mixture to react (leave it around 20-30 minutes). After it reacted fully (you can tell this by just watching , fumes will raise in the glass container, or by touching the container, the temperature will raise a lot) leave it to settle. We need the fog to go away, if it doesn’t go away in like half an hour steer it away. 4. Step: After all is done, you will see a white, blueish mixture at the bottom of the glass (that is your chloroform). Pour away the still liquid part as best as you can, but care not to mix the powder with it. The remaining chloroform now needs to be placed in the separation funnel for extraction. Take care and be careful not to inhale anything. Using chloroform on people is illegal, and will come with serious consequences. If you have more questions, feel free to address us at mailto: know_it_all_now@yahoo.com
https://knowitallnowblog.wordpress.com/2014/06/05/how-to-make-chloroform/
How do I prepare chloroform at home? You would proceed by using the haloform reaction of hypochlorite bleach and acetone. Please proceed with caution and note the caveats: Buy acetone and a gallon of 6% sodium hypochlorite bleach. Make sure to get bleach without other additives. In a well ventilated space, measure out sixty grams of acetone. Pour the bleach in to either a large glass container (so that you can see the reagents), or, if that is not available, an HDPE bucket. The reagents will not attack HDPE, but you will be less able to see the chloroform as it forms. Pour the acetone in to the bleach. Mix gently, either by stirring or swirling the mixture. The temperature will rise by about 30C as the reaction proceeds, so be aware that if you want to do this with any more concentrated reagents (for example, 8.25% or 10% bleach), you will need to prechill the reagents in a freezer to avoid boiling off the chloroform and causing a hazardous condition. At 6% concentration, it is still practical to begin with reagents at room temperature, but the reaction vessel may become too hot to hold with bare hands. Leave the mixture to separate and cool for an hour. If working in glass, you should now be able to see a small, separate blob of denser liquid at the bottom of your flask or container. Decant off the large amount of other liquid above it. If you have a separatory funnel, separate it that way; otherwise, you may have to use an eye dropper or some other finicky technique to capture the denser chloroform while leaving the aqueous phase behind. Crude yield from this proceeding is typically 50-70%, around 75g. You may find the small volume disappointing given the gallon of starting material. That's chemistry for you ;-). IMPORTANT: the resulting material is still far too impure for human consumption. If you're using it to kill insects, or for home TLC, or as a solvent, this doesn't matter. But if you plan for whatever reason to ingest some of it, you should purify it by distillation over sulfuric acid (the 19th century method) or else by more modern means.
https://www.quora.com/How-do-I-prepare-chloroform-at-home 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13.
take sodium hypochlorite (a disinfectant) take acetone ( nail remover ) 200 ml of sodium hypochlorite + 10ml of acetone take a flask and keep it in a ice jar mix acetone slowly make sure the temperature is below 20 degree Celsius you will notice that the solution is cloudy after 1 hour you will see that the solution becomes clear two layers will be formed in the flask chloroform gets settle down ( the lower layer is chloroform) as it is not that clear collect it from the dropper store it in brown bottle and in water
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Historicamente, o Clorofórmio foi utilizado como anestésico, mas hoje em diaé usado principalmente como solventeCuriosamente pode ser feito facilmente a partir de produtos domésticos comuns.Neste experimento, os principais produtos químicos que usei foram 3,6 litros deágua sanitária concentrada e cem mililitros de acetona.Primeiramente deve determinar a concentração de hipoclorito de sódiono alvejante.Isso é feito reagindo cerca de cinco mililitros de alvejantes com três por centode Peróxido de HidrogênioConforme mostra a equação acima, o Peróxido de Hidrogênio reage com o Hipocloritode sódio para formar água, cloreto de sódio e gás oxigênioO peróxido é adicionado até não ocorrer mais borbulhas e a reação estar completa.O nível de água no cilindro graduado é medido antes e depois daadição do gás. Ao calcular a quantidade de gás que aumentou epartindo do pressuposto de um mol de gás ocupa um volume de 24 litros, podemoscalcular a concentração do alvejante. A equação que usei, como está mstrandoacima, e o resultado que obtive, foi que a concentração de hipoclorito de sódio erade cerca de 1,28 molar.Isso não é necessário, mas usei o hidrogênio para medir a densidade doalvejante e determinei que a concentração era cerca de 8,6%o alvejante foi resfriado até cerca de menos 2 graus Celsius e150 mililitros foram descartados.Para que tenha espaço suficiente para acetona, e também para agitar.A reação do cloro com a acetona é extremamente exotérmica e absolutamentesendo necessário resfriar para alcançar pelo menos zero graus Celsius antes de adicionarEu adicionei cerca de 100 mililitros de acetona ao alvejante que representamm excesso de alvejante em torno de 11%. Eu acho um acesso entre trêse cinco pro cento é melhor e 11% alto demais. Usamos um excesso dealvejante porque queremos garantir que toda acetona seja consumidaQualquer acetona restante poderia formar um azeótropo com o clorofórmio dificílde separarDepois de adicionar a acetona, a garrafa deve ser tampada e agitada. A tampa é entãoremovida lentamente na parte superior para permitir que alguns gases escapem.Deixe o frasco durante uma noite para permitir uma separação completa do clorofórmioda camada aquosa. O clorofórmio é mais denso que a água e é imiscível.então deve formar uma camada na parte inferior. Após cinco minutos a temperatura estáem cera de 30 graus Celsius. A temperatura alcançou cerca de 45 grausCelsiusPara este vídeo vou demonstrar visualmente a reação entre aacetona e o alvejante. Quando a acetona é adicionada ele reage com trêsequivalentes de hipoclorito de sódio para formar clorofórmio, hidróxido de sódio eacetato de sódio.Depois de permitir que a solução permaneça sem pertubação por um curto período de tempo.é possível ver o clorofórmio em uma camada separada na parte inferior.A solução ainda está amarela devido à presença do hipoclorito de sodioque não reagiuDecante cuidadosamente a camada aquosa superior. Para uma grande quantidade de água vocêPrecisa fazer isso várias vezes.Você deve decantar a camada aquosa em recipiente de descarte marcado rotulado como alvejante eresíduos de clorofórmio.Eventualmente, o liquido restante do frasco alvejante é vertido no bequere as camadas de clorofórmio permitidas decantar mo fundo. Você pode notarque a solução é menos amarela no exemplo anterior que mostrei. Istoocorre porque foi permitido reagir de um dia para o outro e a concentração dehipoclorito de sódio na solução é muito menor. Deixe-o por vários minutosate que a camada de clorofórmio se separe completamente. Decante o máximo decamada aquosa possível e depois adicione o resto a um funil se separação.Permita que as duas fases se separem e depois drene a camada inferior de clorofórmio.Adicione a camada aquosa superior ao seu recipiente de descarte. O clorofórmio foi lavado uma vezcom cloreto de sódio saturado e depois foi adicionado a um balão de destilaçãocontendo coreto de cálcio. A destilação simples do clorofórmio foifoi realizada no banho mariaO destilado que passou abaixo de 60 graus Celsius estava nublado e foidescartadoA temperatura permanece constante em torno de 60 graus e o destilado foicoletado como um liquido transparente.O volume total de clorofórmio obtido foi de cerca de 58 mililitrosO clorofórmio é transferido para uma garrafa que foi enrolada em papel alumínio para proteger.da luzCerca de 1 mililitro de etanol absoluto foi adicionado para estabilizar o clorofórmioe evitar a formação de fosgênio. Novamente, o rendimento final foi cerca de58 ml, o que representa um rendimento final de cerca de 53%
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