Dramatically reduce experiment time using feedback control software

  • Article
  • August 1, 2023

When time matters

In research and development, time is one of the most valuable resources. Therefore, tools that can reduce the time needed to complete experiments can be invaluable.

The Crystal16 and CrystalBreeder instruments are already used to collect solubility information in as little as 4 hours. This can be reduced further using the feedback control software, automatically detecting clear and cloud points to trigger the next process steps and thus eliminating wasted time. Additionally, the feedback software is vital for using the nucleation rate analysis, reducing experiments from weeks to a few days.

Feedback Control

Within the pharmaceutical sector, 80% of the active ingredients are used in their crystalline form, and 40% of all industrial crystallization processes are “cooling crystallization”.

In the designing of a crystallization process, solubility is key. The feedback control functionality of the Technobis Crystallization Systems software allows automatic detection of clear and cloud point, allowing the significant reduction of solubility experiment run times. The Crystal16 or CrystalBreeder instruments with the feedback control functionality enable you to easily detect when the compound is completely dissolved (clear point) and controls crystallization by triggering the next temperature controlled step (cloud point). By making use of the feedback control functionality, the experiment time can be reduced dramatically. This means you can increase your R&D output and productivity to maintain the competitive edge of your company.

Solubility case study

Upon heating a suspension of known composition, the temperature at which all crystals are dissolved marks a point on the solubility line. After a recrystallization step through cooling, the measurement can be repeated.

With the Crystal16, one can perform 16 solubility measurements at 1 mL scale. Measuring multiple samples simultaneously gives a dataset of saturation temperatures at different concentrations that represent the solubility line. Typical measurements for a full solubility line may take up to 8 hours. By making use of the feedback control functionality offered by the Technobis Crystallization Systems software, the time can be reduced to just 5 hours.

Induction time case study

Nucleation rate is information that can be used in modeling crystallization process, and the Crystal16 offers the first commercially available instrument for measuring induction time and calculating nucleation rate. However, it has been shown that it requires at least 80 datapoints to capture the randomness of nucleation, which can make the experiment run for several days.

Making use of the feedback control strategy will help you to reduce significantly the time spent making and optimizing your crystallization process by triggering the next temperature-controlled step once the first crystals are detected. The experiment time can be significantly reduced by making use of the new software options for feedback control.

For example, crystallization experiments may take up to 70 hours. By making use of the feedback control options offered by the Technobis Crystallization Systems software, the time can cut down to only 15 hours. Growth of single crystals also benefit hugely from the feedback control options. Once the crystal is detected, the next temperature step is triggered to allow growth. Feedback control will finally help you reduce the time to market of your product.

Curious to learn more?

Download the Application Note on "New software options for Feedback control"