Measuring the Melting Point

Measuring Melting Point

Measuring the Melting Point

Posted on the 8th of May 2023 by Westlab

Melting point analysis is a crucial technique used in the laboratory for the identification of pure substances and the determination of sample purity. The melting point of the substance is the temperature at which it changes from a solid to a liquid state and is determined by its molecular structure and the strength of intermolecular bonds. Meanwhile, this guide covers the importance of melting point analysis, what determines melting points, sample preparation, and tips for conducting melting point experiments.

What Determines Melting Point? 

The determination of a melting point of a sample is a standard laboratory procedure and is relatively straightforward. It is used to identify a sample, establish its purity, and determine the thermal stability of the sample. When measuring a melting point, you will generally find that it is recorded as a melting range rather than the exact melting point. This is due to most samples appearing to melt over a small temperature range. A melting range is a difference between the temperature at which the sample begins to melt and the temperature at which the sample has actually melted.

Melting Point Determination Principle

The melting point of a substance is determined by its molecular structure and the strength of the bonds between its atoms. In general, substances with strong intermolecular bonds have higher melting points, as more energy is required to break these bonds and cause the substance to change from a solid to a liquid state.

The principle of melting point determination is simple: a sample of the substance is heated at a controlled rate, and the temperature at which the substance changes from a solid to a liquid is recorded. This temperature is the melting point of the substance.

Melting point determination can be performed using a variety of methods, including the capillary tube method and differential scanning calorimetry. In the capillary tube method, a small amount of the substance is placed in a capillary tube and heated, and the temperature at which the substance begins to melt is recorded. In differential scanning calorimetry, the sample is placed in a sealed chamber and heated while its temperature is monitored, and the temperature at which the substance begins to melt is recorded.

It is important to note that the melting point of a substance can be affected by impurities and other factors, such as pressure and humidity. This highlights the importance of accurate and precise melting point determination in the laboratory, as it can provide valuable information about the purity and identity of a substance.

Why Measure Melting Point? 

Melting point analysis is a crucial technique used in the laboratory for the identification of pure substances and the determination of the purity of a sample. This technique involves the measurement of the temperature at which a solid substance changes from a solid to a liquid state, known as its melting point.

  • In the field of pharmaceuticals, melting point analysis is used to determine the purity of active pharmaceutical ingredients (API) and to ensure that they meet the required specifications. This helps to ensure the quality and efficacy of the final drug product.
  • In materials science, melting point analysis is used to identify and characterize materials, including polymers and ceramics. The melting point of a material can provide information about its molecular structure and its suitability for various applications.
  • In forensics, melting point analysis is used to identify unknown substances and to determine the purity of seized drugs. This information is used in court as evidence to support criminal investigations.

Overall, melting point analysis plays a vital role in many different fields and helps to ensure the accuracy and reliability of laboratory results. Westlab Canada is committed to providing high-quality laboratory equipment and support to customers, including melting point apparatus, to aid in the effective and efficient completion of melting point analysis in the laboratory.

Methods of Measuring Melting Point

There are a variety of methods that you can use to determine the melting point of a sample. The following are some measuring methods:

Capillary Method

The most common and basic method of determination is the capillary method. This method involves placing the sample in a capillary tube and running an experiment that will heat the sample until it reaches the melting point. The melting point can then be recorded.
There are a few ways in which you can set up an experiment with the capillary method. 

  1. The first is a manual apparatus set up with the aim of heating up a sample inside a capillary tube whilst visually looking for when the sample has melted. The concept involves placing a small amount of the substance in a capillary tube and joining this to a thermometer.
  2. The capillary tube is then placed into a heating bath and the experiment is conducted. If you don’t have a heating bath, you can use Mineral Oil in a Thiele Tube.
  3. Heat the tube with a Bunsen Burner. It is important to heat the sample slowly using this method so that a thermal equilibrium can be established.

A more modern way of using the capillary method is to use a device called a Melting Point Apparatus. This device uses the same concept of heating a sample in a capillary tube but makes the process far simpler and quicker. There are many different types of Melting Point Apparatus machines and they range in functionality and accuracy. At a basic level, the machine is designed so that a capillary tube with the sample can be inserted into the device and rapidly heated to a set temperature. Generally, you will heat the capillary tube to near melting point and then decrease the speed of the temperature increase so that you can observe when the sample melts. Observation is generally conducted through a viewing eyepiece. A Melting Point Apparatus will more than likely have the temperature displayed in digital format for easy recording of data.

Differential Scanning Calorimetry

The following are some steps for measuring melting point using differential scanning calorimetry:

  • Place the sample in a sealed chamber
  • Heat the sample
  • Monitor the temperature of the sample
  • Record the temperature at which the substance begins to melt, which is the melting point

Steps for Measuring Melting Point Using a Modern Melting Point Apparatus:

  • Prepare the sample by ensuring it is fully dry and in powdered form
  • Place the sample in a capillary tube
  • Insert the capillary tube into the melting point apparatus
  • Rapidly heat the sample to a set temperature
  • Decrease the speed of the temperature increase to observe when the sample melts
  • Observe the melting point through a viewing eyepiece
  • Record the melting point digitally

Sample Preparation

Firstly, you must ensure that the sample is fully dry and in powdered form. Then with your capillary tube, use the open end of the tube to press down gently on the sample several times. You then need to get the powder all the way to the bottom of the capillary tube by tapping the closed-end multiple times on a hard surface so that the sample is compacted down at the closed end of the tube (you could also use a method where you drop the tube multiple times through a glass tube approx. 1m in length). For further accuracy, you can use a packing wire to further compact the sample. Note that the sample height should be between 2 and 3mm to ensure the best results.

Melting Point Tips

Here are a few helpful tips to assist with melting point experiments.

  • Never re-melt a sample! Always use a fresh sample and a new capillary tube.
  • Always use the same batch of capillary tubes for routine measurements. Not all capillary tubes are equal and using the same batch will ensure repeatable results.
  • Always clean the tube before running the melting point experiment. Failure to do so can result in a low melting point or a wide melting range.
  • Don’t heat the sample too fast. It is recommended only 1-2°C per minute.

In conclusion, melting point analysis is a vital technique used in various fields, including pharmaceuticals, materials science, and forensics, to identify pure substances, determine sample purity, and provide valuable information about the purity and identity of a substance. Westlab Canada, as a leading provider of laboratory equipment, is committed to providing high-quality products and support to customers, including melting point apparatus, to aid in the effective and efficient completion of melting point analysis in the laboratory. By utilizing accurate and precise melting point determination techniques, researchers and scientists can ensure the reliability and validity of their results, making a significant contribution to their respective fields.

FAQs

What is a melting point?

It is the temperature at which a substance changes from a solid to a liquid state. It is defined as the temperature at which the liquid and solid phases exist in equilibrium and the substance can change from one phase to the other without further heating or cooling. The melting point is a characteristic physical property of a substance and is used to identify and characterize materials, as well as to determine their purity.

What is the melting and boiling point?

The melting point is the temperature at which a solid substance changes to a liquid state, while the boiling point is the temperature at which a liquid substance changes to a gaseous state. Both the melting point and boiling point are important physical properties of a substance and are used in various applications, including material identification and characterization, quality control, and process optimization.

What is the difference between temperature and melting point?

Temperature is an estimate of the average kinetic energy of a substance and can be used to describe the heat content of a material. The melting point, on the other hand, is a specific temperature that marks the transition from a solid to a liquid state. The temperature of a substance can change over a range of values, while the melting point is a unique and fixed value for a given substance.

What is the difference between the boiling point and a melting point of a substance?

The boiling point of a substance is the temperature at which it changes from a liquid to a gaseous state, while the melting point is the temperature at which it changes from a solid to a liquid state. These two physical properties are related but distinct, as the boiling point is dependent on the pressure at which the substance is heated, while the melting point is not.

What is the melting point of water?

The melting point of water, also known as ice, is 0 °C (32 °F) at normal atmospheric pressure. This means that water will change from a solid (ice) to a liquid (water) at 0 °C, and will change from a liquid to a gas (steam) at 100 °C (212 °F) under normal conditions. The melting point of water is an important property that plays a role in various natural and industrial processes, including climate and weather patterns, food processing, and energy production.

 

2023-05-08 13:03:00
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