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Related Concept Videos

Solvents01:12

Solvents

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A solvent is a substance, most often a liquid, that can dissolve other substances. Here, the substance being dissolved is called a solute. When a solvent and a solute combine, they form a solution - a homogenous mixture of both the solvent and the solute. Water is a universal biological solvent. Its polar structure allows it to dissolve many other polar compounds. The ability of water to dissolve is governed by a balance between water molecules binding to each other and binding to the solute.
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Sublimation01:03

Sublimation

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Sublimation is the direct transformation of a solid to a gaseous state. For instance, at standard pressure and room temperature, solid carbon dioxide sublimes to gaseous carbon dioxide. The phase diagram depicts the conditions required for sublimation. This process occurs at the solid-gas phase boundary and is not observed above the triple point of the substance. The reverse of sublimation is called deposition, where a gaseous substance condenses directly into a solid. Sublimation and...
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High-Performance Liquid Chromatography: Elution Process01:05

High-Performance Liquid Chromatography: Elution Process

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In High-Performance Liquid Chromatography (HPLC), the elution process is critical to the separation of analytes and the quality of chromatographic results. Elution describes how compounds move through the column and separate based on their interactions with the mobile and stationary phases. This process determines the resolution, peak shape, and retention times in the chromatogram, which are essential for identifying and quantifying components in complex mixtures. Understanding the elution...
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Sample Preparation for Analysis: Advanced Techniques01:08

Sample Preparation for Analysis: Advanced Techniques

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Accurate analysis of complex samples often requires advanced preparation techniques to achieve reliable and reproducible results. Samples containing inorganic or organic materials can be challenging to dissolve or decompose effectively. Standard sample preparation methods include acid digestion, fusion, dry ashing, and wet digestion.
Acid digestion with strong acids is commonly used to dissolve inorganic materials that are insoluble (do not dissolve) in water. This method can be useful for...
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Volatilization01:10

Volatilization

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Volatilization gravimetry is an analytical technique that measures the mass lost due to the volatilization of the substance. This technique is used to estimate the amount of volatile material in a sample. To perform this method, heat a known amount of the sample to a high temperature in a crucible or other suitable vessel. The volatile substance in the sample evaporates, and the vapor is completely expelled from the crucible either by heating the sample or bubbling a stream of inert gas through...
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Recrystallization: Solid–Solution Equilibria01:10

Recrystallization: Solid–Solution Equilibria

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Recrystallization is a purification technique used to separate impurities from solid compounds. In this technique, no chemical reactions occur. Instead, it exploits physical properties only, specifically, the solubility differences between the desired compound and impurities, either at a single temperature or at different temperatures, and under other selected conditions. The solid-solution equilibrium (solubility equilibrium) of each component in the solution represents a binary phase...
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Related Experiment Video

Updated: Nov 3, 2025

Separation of Aldehydes and Reactive Ketones from Mixtures Using a Bisulfite Extraction Protocol
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A Versatile Method of Ambient-Temperature Solvent Removal.

Igor V Kolesnichenko1, Galina Z Goloverda2, Vladimir L Kolesnichenko2

  • 1Sandia National Laboratories, Albuquerque, New Mexico.

Organic Process Research & Development
|June 7, 2021
PubMed
Summary
This summary is machine-generated.

A new "cryovap" method uses a pressure gradient and low temperatures to efficiently remove heat-sensitive solvents like DMSO and NMP. This technique is practical for bench-scale chemistry and can be adapted for recovering water-soluble compounds.

Keywords:
distillationevaporationfreeze-dryinghigh-boiling solventreaction product isolationsynthesis workup

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Area of Science:

  • Organic Chemistry
  • Chemical Engineering
  • Materials Science

Background:

  • Isolation of heat-sensitive compounds often requires low-temperature solvent removal.
  • Conventional methods can be time-consuming or inefficient for delicate molecules.

Purpose of the Study:

  • To introduce a novel, low-temperature solvent evaporation technique called "cryovap".
  • To demonstrate the method's effectiveness for heat-sensitive solvents and its adaptability for compound recovery.

Main Methods:

  • Solvent evaporation driven by a pressure gradient in an evacuated closed system.
  • Utilizing an all-glass apparatus with a water bath (18-28 °C) and a liquid nitrogen-chilled receiver.
  • Bench-scale application for removing dimethyl sulfoxide (DMSO) and N-methylpyrrolidone (NMP) from benzophenone solutions.

Main Results:

  • Successful evaporation of 50 mL of dimethylformamide, DMSO, and NMP within 90-140 minutes.
  • Gravimetric and 1H NMR analyses confirmed efficient solvent removal from benzophenone solutions.
  • Demonstrated potential for recovering water-soluble compounds, including polymers and biopolymers, by mimicking freeze-drying.

Conclusions:

  • The "cryovap" method offers an efficient and practical approach for low-temperature solvent removal.
  • This technique is suitable for isolating heat-sensitive reaction products and recovering valuable compounds.
  • The cryovap method provides a versatile alternative to traditional solvent evaporation techniques.