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Representative sampling of powders

Representative Sampling of Powders
In contrast to liquids, which typically form a continuous flow, powders exhibit non-uniform behavior when subjected to motion. Consequently, obtaining a small, representative sample from a larger batch for subsequent analysis poses a significant challenge and can easily result in experimental errors. Even when employing highly accurate analysis techniques on a non-representative sample, the resulting data often proves to be unreliable. Therefore, at Delft Solids Solutions, we prioritize meticulous attention to the sampling process when investigating our customers’ powder materials.

Powder materials with good flow characteristics can be segregated based on differences in particle size, shape, and density. While cohesive powder materials exhibit less segregation, agglomeration can still significantly affect the sampling procedure. So, how can we obtain a truly representative sample, especially when dealing with a small fraction of the total sample volume? Well, the solution lies in the use of rotating or spinning rifflers, which address this issue and enable the extraction of smaller sub-lots from a larger batch.

This can be done on various scales, from kilograms (or liters) to grams (or milliliters), down to milligrams (or sub-milliliters). Statistical analysis demonstrates that the error associated with sampling when using rotary rifflers is just 0.1% in relative standard deviation, in contrast to approximately 5% when employing simple scoop sampling( image 1). A chute sampler, which divides the sample into roughly equal portions, displays an error of approximately 1%, but struggles with small sample volumes.

A spinning riffler comprises a feeder that continuously supplies the original sample to a rotor. The rotor then divides the sample over a cone into typically 8 or 10 sub-fractions, each retaining the same characteristics as the original sample.

If the volume of one sub-sample remains too large for the intended analysis, one can select one or more sub-samples and repeat the process to further reduce the sample volume. However, it’s essential to use the total volume of a sub-sample to maintain the low statistical error mentioned earlier.

Differently-sized spinning rifflers, as utilized at Delft Solids Solutions, further facilitate the transition from large to smaller sample volumes.

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Delft Solids Solutions
12 November 2023|Insights|

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20 do’s & don’ts Rheology and Dispersion

10 DO’s
Powder Rheology and Dispersion

  1. Understand Particle Size Distribution:

Analyze and comprehend the particle size distribution for effective powder dispersion.

2. Use Suitable Dispersing Agents:

Select appropriate dispersing agents to enhance the dispersion process and stability.

3. Control Environmental Factors:

Manage humidity and temperature to prevent agglomeration and ensure consistent powder behavior.

4. Optimize Mixing Speed and Time:

Adjust mixing parameters to achieve optimal dispersion without causing excess energy input.

5. Regular Equipment Calibration:

Calibrate equipment regularly to maintain accuracy and precision in powder processing.

6. Thorough Powder Characterization:

Conduct comprehensive characterization of powder properties to tailor dispersion methods.

7. Consider Powder Wetting:

Ensure proper wetting of powders by liquids to enhance dispersion efficiency.

8. Monitor Rheological Properties:

Continuously monitor rheological behavior to adapt processing conditions as needed.

9. Utilize Advanced Measurement Techniques:

Employ advanced techniques like laser diffraction for precise particle size analysis.

10. Document Process Parameters:

Keep detailed records of process parameters to facilitate troubleshooting and optimization.

10 DON’TS
Powder Rheology and Dispersion

  1. Avoid Overmixing:

Overmixing can lead to particle damage and affect the overall performance of the powder.

2. Don’t Neglect Environmental Conditions:

Inconsistent environmental conditions can result in unpredictable powder behavior.

3. Avoid Using Incompatible Dispersing Agents:

Incompatible dispersing agents may lead to poor dispersion and stability issues.

4. Don’t Disregard Safety Protocols:

Follow safety guidelines when handling powders, considering potential health hazards.

5. Avoid Excessive Shear Forces:

High shear forces can cause particle breakage and alter the powder’s rheological properties.

6. Don’t Skip Powder Characterization:

Neglecting comprehensive powder characterization can lead to inefficient dispersion strategies.

7. Avoid Rapid Temperature Changes:

Sudden temperature changes can impact powder stability and rheological behavior.

8. Don’t Mix Incompatible Powder Types:

Mixing incompatible powders may lead to undesirable reactions or poor dispersion.

9. Avoid Contaminated Equipment:

Contaminated equipment can introduce impurities and compromise powder quality.

10. Don’t Ignore Equipment Maintenance:

Regular maintenance is crucial to prevent equipment malfunctions and ensure consistent performance.

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Events

Particle Size Characterization 2024

November 26 - November 27

Delft Solids Solutions presents a comprehensive 2-day Particle Characterization course, intricately linked with a 1-day Porosity and Surface Area Characterization program. Designed for industries dealing with diverse materials, the course explores fundamental principles, definitions, and techniques for particle size and shape characterization. Key topics include sampling, sieving, sedimentation, microscopy, and quality control, with practical demonstrations reinforcing theoretical knowledge in the well-equipped laboratory. Scheduled for November 26-27, 2024, in Wateringen, The Netherlands, the course offers participants a profound understanding of particle characterization techniques, enabling them to interpret results and ensure measurement reliability. Upon completion, a certificate of participation is awarded. For inquiries or registration, contact Delft Solids Solutions at +31 174 271 460 or info@solids-solutions.com.

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