Name: steam distillation and low-boiling separation
Uploaded: 2020-03-26T07:22:28.000Z
Duration: 3 min 54 s
Channel: JoVE

두 개의 혼합 가능한 액체의 이상적인 혼합물을 가열하여 끓이면 용액은 각 구성 요소의 끓는점 사이의 온도에서 끓습니다. 이러한 액체의 끓는점이 매우 다른 경우 혼합물이 끓기 시작하면 증기에 휘발성 성분의 분자가 풍부해집니다. 이 현상은 종종 두 개의 혼합성 액체의 혼합물을 가열하고 증기를 액체로 다시 응축하여 수집하는 간단한 증류를 사용하여 혼합물을 분리하는 데 사용됩니다.
휘발성 성분이 더 풍부한 증기가 증류액으로 수집됨에 따라 액상은 휘발성이 적은 성분의 분자로 부유해집니다. 그러나, 이 기술은 용액이 적어도 더 휘발성이 높은 화합물의 끓는점까지, 그리고 종종 그 이상으로 가열되어야 합니다.
온도에 민감한 유기 화합물의 경우, 이 고온으로 인해 유기 분자가 다른 것으로 분해될 수 있습니다. 그렇다면 이러한 유형의 화합물을 어떻게 분리할 수 있습니까? 먼저 한 걸음 물러서겠습니다.
응축 된 위상과 평형 상태에있는 증기의 압력을 증기압이라고합니다. 액체 혼합물의 구성 요소는 각각 자체 증기압을 가지고 있으며, 이를 분압이라고 합니다. 우리는 용액의 총 증기압이 대기압과 같을 때 용액이 끓는다는 것을 알고 있습니다. 총 증기압은 구성 요소의 분압의 합과 같습니다.
혼화성 액체의 혼합물, 즉 액체의 모든 조합이 균일한 용액을 형성한다는 것을 의미하는 경우, 분압은 순수한 화합물의 증기압에 용액의 몰 분율을 곱한 값으로 계산됩니다. 그러나 비혼화성 액체의 이질적인 혼합물, 즉 액체가 서로 불용성임을 의미하는 경우 분압은 단순히 순수 화합물의 증기압입니다.
이종 혼합물의 각 성분은 다른 성분과 독립적으로 총 증기압에 기여하기 때문에 분압의 합인 총 증기압이 대기압과 같을 때 혼합물이 끓습니다. 이는 각 구성 요소의 개별 끓는점보다 낮은 온도에서 발생하는데, 이는 총 증기압이 가장 휘발성이 높은 구성 요소에 대해 예상하는 것보다 훨씬 빠르게 온도에 따라 증가하기 때문입니다.
우리는 이 현상을 활용하여 고열에서 분해되고 물에 불용성인 온도에 민감한 유기 화합물을 비휘발성 물질로부터 분리하는 데 사용되는 증기 증류를 수행할 수 있습니다. 증기 증류 설정은 공정 전반에 걸쳐 물을 보충하기 위해 물 저장고를 추가하는 간단한 증류 설정과 유사합니다.
혼합물이 끓으면 물과 관심 유기 화합물이 모두 기화됩니다. 물과 유기 화합물 증기는 응축기로 이동하여 액체로 응축되어 수집됩니다. 혼합되지 않는 액체는 나중에 분리됩니다. 플라스크의 혼합물에는 물과 비휘발성 물질만 남습니다.
이 실험실에서는 오렌지 껍질의 비휘발성 성분에서 에센셜 오일을 추출하기 위한 증기 증류 실험을 설정하고 수행합니다. 그런 다음 액체-액체 추출을 사용하여 물에서 에센셜 오일을 유기 용매로 추출합니다.

증기 증류법

Steam Distillation

<h4>증기 증류법 </h4>
증기 증류는 혼합되지 않는 혼합물의 낮은 끓는점 특성을 활용하는 분리 기술입니다. 주로 온도에 민감한 유기 분자를 비휘발성 오염 물질로부터 분리하는 데 사용됩니다. 유기 분자는 물과 섞이지 않아야 합니다.
증기 증류에서는 비혼화성 혼합물이 가열되어 끓어오르게 되어 물과 휘발성 유기 화합물을 모두 증류합니다. 이것은 기체 혼합물이 응축기로 위쪽으로 이동한 다음 증기를 액체로 응축하여 포집할 수 있음을 의미합니다. 단순 증류와 달리 증기 증류는 물 저장소를 사용하여 공정 전반에 걸쳐 가열된 혼합물에 물을 보충합니다. 비혼화성 유기 성분은 물과 함께 천천히 증류되는 반면, 비휘발성 성분은 가열된 혼합물에 남아 있습니다. 유기 성분이 증류되면 액체-액체 추출을 사용하여 물과 분리할 수 있습니다.
<h4>혼합물의 증기압</h4>
균질 해결책을 형성하는 혼화성 혼합물을 위해, 각 분대의 증기압은 Raoult 법률에 따라 액체 혼합물에 있는 순수한 분대 그리고 그것의 두더지 분율의 증기압에 달려 있습니다.
pA = pA*xA
여기서,p A는 혼화성 액체 혼합물에서 한 액체 성분의 증기압이고, pA*는 순수한 액체의 증기압이며, xA는 혼합물에서 해당 액체의 몰 분율이며, 이는 nA/nt와 같습니다. nA는 혼합물 내 개별 액체의 몰 수입니다. 그리고 nt는 혼합물에 있는 모든 액체의 총 몰 수입니다.
혼화성 액체 혼합물 위의 총 증기압은 그 안에 있는 각 성분의 부분 증기압의 합과 같으며, 이를 Dalton의 법칙이라고 합니다. 액체의 증기압은 더 많은 분자가 액체 상태에서 기체 상태로 탈출하기 위해 운동 에너지를 얻음에 따라 온도에 따라 증가합니다. 두 개의 액체를 포함하는 혼합성 혼합물에서 총 압력은 다음과 같이 설명될 수 있습니다.
P = pA + pB
여기서, p, A 및 p, B는 각각 혼합물 위의 액체 A 액체 B의 증기압입니다. P는 혼합물 위의 두 액체의 총 증기압입니다. 방정식을 결합하면 용액의 총 증기압과 개별 구성 요소의 몰 분율 사이의 관계가 설명됩니다.
P = pA*xA + pB*xB
성분이 이질적인 혼합물을 형성하는 혼합되지 않는 혼합물에서 각 성분의 증기압은 총 증기압에 독립적으로 기여합니다. 따라서 총 증기압은 개별 순수 증기압의 합과 같습니다. 두 개의 액체로 구성된 혼합되지 않는 혼합물에서 총 압력은 첫 번째 액체의 증기압에 두 번째 액체의 증기압을 더한 값으로 정의됩니다.
P = pA* + pB*
<h4>비혼합성 혼합물의 끓는점</h4>
액체가 가열되면 증기압이 증가합니다. 혼합물의 각 성분에는 자체 끓는점이 있습니다. 혼화성 액체의 혼합물에서 끓는 것은 구성 액체의 끓는점 사이의 온도에서 발생합니다.
혼합되지 않는 혼합물의 경우, 끓는 것은 개별 구성 요소의 끓는점보다 훨씬 낮은 온도에서 발생합니다. 각 개별 구성 요소가 독립적으로 기여하기 때문에 총 증기압을 대기압으로 증가시키는 데 더 적은 열이 필요합니다.
예를 들어, 벤젠과 물의 혼합되지 않는 혼합물을 생각해 보십시오. 정상 대기압에서 벤젠의 끓는점은 80.1 °C이고 정상 대기압에서 물의 끓는점은 100 °C입니다. 용액은 총 증기압이 760mm Hg (정상 대기압)에 도달하면 끓습니다. 69.3 ° C에서 물의 증기압은 227 mm Hg이고 벤젠 증기압은 533 mm Hg이며, 이는 총 끓는 데 필요한 760 mm Hg와 같습니다. 이것은 개별 구성 요소의 끓는점보다 훨씬 낮습니다.
<h4>참조</h4>
<ol>
	<li style="font-size:17px">Kotz, J.C., Treichel Jr, P.M., Townsend, J.R. (2012). 화학 및 화학 반응성. 캘리포니아 벨몬트 : Brooks / Cole, Cengage Learning.</li>
	<li style="font-size:17px">Silderberg, M.S. (2009). 화학: 물질과 변화의 분자적 성질. 매사추세츠주 보스턴: 맥그로 힐.</li>
</ol>

증기 증류법 
증기 증류는 혼합되지 않는 혼합물의 낮은 끓는점 특성을 활용하는 분리 기술입니다. 그것은 주로 ...

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JoVE Lab Manual

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화학

steam distillation and low-boiling separation

Steam distillation is a separation method for temperature-sensitive organic compounds. It works best when the organic compound is immiscible in water, meaning the two liquids do not mix. The method helps remove the organic molecule from a non-volatile contaminant without using the higher temperatures needed for many other separations.

In steam distillation, the immiscible mixture is heated until both water and the volatile organic compound distill together. The vapor rises to a condenser, where it cools and becomes a liquid that can be collected. Unlike simple distillation, this setup uses a water reservoir to keep replacing water in the heated mixture during the process.

The organic component is carried over slowly with the water, while the non-volatile component stays behind in the heated flask. After distillation, the organic product can be separated from the water by liquid-liquid extraction. This makes steam distillation useful for isolating sensitive organic materials from unwanted impurities.

The same low-boiling behavior can be explained by vapor pressure. For a miscible mixture, each liquid follows Raoult’s law, so its vapor pressure depends on the pure liquid vapor pressure and its mole fraction. The mole fraction is the number of moles of one liquid divided by the total number of moles in the mixture. The total vapor pressure above a miscible mixture follows Dalton’s law and equals the sum of the partial vapor pressures.

As temperature rises, vapor pressure increases because more molecules gain enough kinetic energy to escape into the gas phase. In a two-liquid miscible mixture, the total pressure can be written as P = pA + pB, or as P = pA*xA + pB*xB when Raoult’s law is included. In an immiscible mixture, the components act independently, so the total pressure is the sum of the vapor pressure of the first liquid and the vapor pressure of the second liquid.

This independent vapor-pressure behavior is why immiscible mixtures boil at lower temperatures than either pure liquid. In a miscible mixture, boiling usually happens between the boiling points of the components. In an immiscible mixture, less heat is needed to reach atmospheric pressure, so the boiling point drops well below the boiling points of the individual liquids.

A benzene-water mixture shows this effect clearly. Benzene boils at 80.1 °C, and water boils at 100 °C at normal atmospheric pressure. The mixture boils when the total vapor pressure reaches 760 mm Hg. At 69.3 °C, water contributes 227 mm Hg and benzene contributes 533 mm Hg, which adds up to 760 mm Hg. That means the mixture boils at a temperature below either pure component.

Steam Distillation and Low-Boiling Separation

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Separating liquids by boiling point is the goal of distillation. A miscible mixture contains liquids that mix evenly, and it can be heated so that the more volatile liquid evaporates first. Volatility is a liquid’s tendency to vaporize, and boiling begins when bubbles form in the liquid phase. In a closed container, liquid and vapor can reach equilibrium, which means the rate of vaporization equals the rate of condensation. The pressure from the vapor above the liquid is called vapor pressure.

steam distillation

Steam distillation is a separation method for temperature-sensitive organic compounds. It works best when the organic compound is immiscible in water, meaning the two liquids do not mix. The method helps remove the organic molecule from a non-volatile contaminant without using the higher temperatures needed for many other separations. In steam distillation, the immiscible mixture is heated until both water and the volatile organic compound distill together. The vapor rises to a condenser,...

thin-layer chromatography

TLC Separation by Polarity

Thin-layer chromatography (TLC) separates compounds in a mixture by polarity. It uses the same basic parts as other chromatography methods: a stationary phase, a mobile phase, and the solute. In TLC, the stationary phase is a thin coating on a plate instead of material packed into a column. The stationary phase in most TLC systems is polar silica gel, a form of silicon dioxide. Its surface has OH groups that can form hydrogen bonds. The sample is first spotted on a pencil start line with a...

column chromatography

Separating Mixtures by Polarity

Column chromatography separates compounds in an organic chemistry lab by using differences in physical properties. It is especially useful for microscale separations when less than 10 grams of material is available for analysis. The method can separate a mixture based on solubility, polarity, hydrophobicity, size, and charge. Any chromatography system has three main parts: the stationary phase, the mobile phase, and the sample mixture. In column chromatography, the stationary phase is usually...

hydrolysis of an ester

Soap Formation from Triglycerides

Triglycerides are lipids made of a glycerol backbone linked to three fatty acids. They are common in vegetable oils and animal fats. Plant lipids are the basis of vegetable oils, while animal lipids are used as lard or general sources of fats. A fatty acid has a long carbon chain, usually between 12 and 20 carbons, with a weak organic acid at one end. Some fatty acids contain double bonds. These are unsaturated fats. The double bond usually gives the chain a bent, cis shape. As a result,...

synthesis of luminol

Luminol Chemiluminescence in Forensics

Luminol chemiluminescence shows how a chemical reaction can produce light and help with blood detection. Chemical reactions may be endothermic or exothermic, depending on whether they absorb or release heat as reactants become products. The enthalpy of a reaction is the energy difference between reactants and products, or ΔH. A positive ΔH means the reaction is endothermic. A negative ΔH means it is exothermic. Many reactions do not happen in a single step. They can pass through intermediates...

esterification

Ester Formation and Everyday Fragrances

Esters are organic compounds with a carbonyl group attached to an oxygen that connects to another alkyl or aryl group. Their general formula is RCOOR'. They are often made by reacting a carboxylic acid with an alcohol in an esterification reaction. In this process, the hydroxyl group of the acid is replaced by an alkyl or aryl group. Many simple esters have familiar fruit and flower smells because their structures are small and less complex. Formic acid and methanol can combine to form methyl...

identification of unknown aldehydes and ketones

identification-of-unknown-aldehydes-and-ketones

Carbonyl Tests for Aldehydes and Ketones

Aldehydes and ketones are carbonyl compounds, which means they contain a C=O functional group. A ketone has two alkyl or aryl groups attached to the carbonyl carbon. Acetone is the simplest ketone, with two methyl groups. An aldehyde is similar, but it has at least one hydrogen attached to the carbonyl carbon. Formaldehyde is the simplest aldehyde, and acetaldehyde has one hydrogen and one methyl group. The carbonyl carbon in both aldehydes and ketones is electrophilic because the oxygen atom...

uv-vis spectroscopy of dyes

How Dyes Absorb Visible Light

Dyes absorb visible light because their molecular structure lets them interact with specific wavelengths. When light hits a substance, some light is absorbed and the rest is reflected or transmitted. The color we see depends on the wavelength that is reflected. A blue substance reflects blue light, around 430 to 480 nm, and absorbs the complementary orange region, around 590 to 630 nm. Compounds that do not absorb in the visible range appear colorless to the human eye. Light also has energy and...

identifying alcohols

Alcohol Tests for Primary, Secondary, and Tertiary

Alcohol tests can help sort alcohols by structure and reactivity. Alcohols are organic molecules with a hydroxyl group attached to an alkyl or aryl group, written as ROH. If the carbon with the hydroxyl group has one R group, the alcohol is primary. If it has two R groups, it is secondary. If it has three R groups, it is tertiary. Alcohols can also be aromatic when they contain a benzene ring. Phenol is the simplest aromatic alcohol. To identify an alcohol, chemists can use its chemical...

chemistry

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Learn how steam distillation separates temperature-sensitive organic compounds from water-insoluble mixtures using vapor pressure and low boiling points.

Steam Distillation and Low-Boiling Separation | JoVE K12

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Steam Distillation and Low-Boiling Separation

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