Measuring Crystals in Food
The major sugar in milk is lactose. Lactose is less soluble in water than table sugar so if you concentrate milk, the lactose can crystallize out. This is a problem in products like condensed milk (some of the water has been evaporated off) or in ice cream (some of the water is frozen as ice) where lactose crystallization leads to a gritty or sandy texture in the mouth. The process of crystallization is often slow and can be hard to predict so it can be a challenge to work out if a new formulation is going to give problems. If there is no reliable theory you have to experimentally measure the progression of crystallization.

Measuring the kinetics of crystallization in a solution is relatively easy; just filter off the crystals and weigh them. Measuring the kinetics of crystallization in a more complex solid food it is more challenging. This was the motivation behind some work my graduate student Umut Yucel did as part of his MS, and which was recently published in the Journal of Food Science. This work was supported by a grant from the Center for Food Manufacturing, an industry consortium at Penn State.
Our idea was that ultrasonic waves would be a useful tool to measure the process of lactose crystallization. Ultrasound is high frequency sound, beyond the range of human hearing. We can easily measure how fast the sound moves through a sample or how effectively the sample absorbs the sound energy. We had to design an experiment to see if the ultrasonic measurements would be sensitive to the formation of lactose crystals in a solid matrix.
We dissolved lactose and gelatin in hot water then cooled the solutions to allow the gelatin to solidify. Initially the gel was clear, but over the next several hours the lactose began to crystallize and the gel became more and more turbid. Initially the gel absorbed very little sound energy,but over the next several hours the lactose began to crystallize and the gel became more and more attenuating. Lactose crystals scatter the sound waves leading to high acoustic losses while lactose in solution absorbs much less sound energy. Ultrasonic attenuation measurements are an effective way to measure the presence and amount of crystals.
Ultrasonic measurements are particularly useful for sensing application, as the waves pass easily through opaque foods or through glass or plastic packaging. Ultrasonic waves are also very low-energy so don’t damage or otherwise affect the sample. You can also use them on intact foods so there is no need to separate the crystals for analysis. Our work demonstrates the potential for ultrasonic sensors as tools to study sugar crystallization in complex foods.
The main practical challenges in this work were to determine appropriate concentrations of gelatin and lactose so that the gelatin would solidify before the lactose began to crystallize but the lactose would crystallize fast enough that the experiment wasn’t impractical. Our methods tied up the instruments for long periods of time so if the crystallization took weeks then the other students would be left waiting. We also had to be careful that the amount of lactose crystals formed was not so large that all the sound was absorbed and no measurements could be made. Once we had those details were sorted out the body of the published work only took perhaps six weeks.
Umut wrote up a version of the work for use in his MS thesis, which we later adapted for the Journal of Food Science paper. The review process was fast and constructive – we had a statistical error in our first version I’m glad was pointed out. At the moment this thread of work is on hiatus. I’d like to bring in a new student to look at real products or perhaps build a quantitative relationship between the amount of crystals and the ultrasonic measurements but all of this will have to wait on a suitable grant.