Novel Real-Time Diagnosis of the Freezing Process Using an Ultrasonic Transducer

The freezing stage governs several critical parameters of the freeze drying process and the quality of the resulting lyophilized products. This paper presents an integrated ultrasonic transducer (UT) in a stainless steel bottle and its application to real-time diagnostics of the water freezing process. The sensor was directly deposited onto the stainless steel bottle using a sol-gel spray technique. It could operate at temperature range from −100 to 400 °C and uses an ultrasonic pulse-echo technique. The progression of the freezing process, including water-in, freezing point and final phase change of water, were all clearly observed using ultrasound. The ultrasonic signals could indicate the three stages of the freezing process and evaluate the cooling and freezing periods under various processing conditions. The temperature was also adopted for evaluating the cooling and freezing periods. These periods increased with water volume and decreased with shelf temperature (i.e., speed of freezing). This study demonstrates the effectiveness of the ultrasonic sensor and technology for diagnosing and optimizing the process of water freezing to save energy.

[1]  Rymantas Kažys,et al.  High temperature ultrasonic transducers: review , 2008 .

[2]  S. J. Norton,et al.  Ultrasonic measurement of internal temperature distribution , 1986, Philosophical Transactions of the Royal Society of London. Series A, Mathematical and Physical Sciences.

[3]  Takuo Inoue,et al.  PbTiO3/Pb(Zr,Ti)O3 sol-gel composite for ultrasonic transducer applications , 2014 .

[4]  Y. Ono,et al.  Real-time diagnosis of co-injection molding using ultrasound , 2007 .

[5]  Cristina Ratti,et al.  Hot air and freeze-drying of high-value foods : a review , 2001 .

[6]  P. Coates,et al.  In-line characterization of polymer deformation in melt and solid phase processing☆ , 1994 .

[7]  Xiaolin Tang,et al.  Design of Freeze-Drying Processes for Pharmaceuticals: Practical Advice , 2004, Pharmaceutical Research.

[8]  N. Maeno Air Bubble Formation in Ice Crystals , 1967 .

[9]  M. Rahman,et al.  Analysis of cooling curve to determine the end point of freezing , 2002 .

[10]  Yuu Ono,et al.  Real‐time monitoring of injection molding for microfluidic devices using ultrasound , 2005 .

[11]  Dielectric Characteristics and Orientation of Piezoelectric (PbZrxTi1−xO3, PZT) Films Fabricated by Sol-Gel Spray and Spin Techniques , 2010 .

[12]  C. Jen,et al.  Piezoelectric thick bismuth titanate/lead zirconate titanate composite film transducers for smart NDE of metals , 2004 .

[13]  X. Peng,et al.  Force of a gas bubble on a foreign particle in front of a freezing interface. , 2004, Journal of colloid and interface science.

[14]  J. Kokini,et al.  Glass transitions in low moisture and frozen foods: effects on shelf life and quality. , 1996 .

[15]  I. Trelea,et al.  Effect of controlled ice nucleation on primary drying stage and protein recovery in vials cooled in a modified freeze-dryer. , 2009, Journal of biomechanical engineering.

[16]  M. Hageman,et al.  Effects of buffer composition and processing conditions on aggregation of bovine IgG during freeze-drying. , 1999, Journal of pharmaceutical sciences.

[17]  Jinsong Liu,et al.  A Study of the Impact of Freezing on the Lyophilization of a Concentrated Formulation with a High Fill Depth , 2005, Pharmaceutical development and technology.

[18]  Ikuo Ihara,et al.  Ultrasonic Monitoring of Internal Temperature Distribution in a Heated Material , 2008 .

[19]  J. Carpenter,et al.  The ice nucleation temperature determines the primary drying rate of lyophilization for samples frozen on a temperature-controlled shelf. , 2001, Journal of pharmaceutical sciences.

[20]  E. C. Brown,et al.  Ultrasound: A Virtual Instrument Approach for Monitoring of Polymer Melt Variables , 1999 .

[21]  Wolfgang Friess,et al.  The freezing step in lyophilization: physico-chemical fundamentals, freezing methods and consequences on process performance and quality attributes of biopharmaceuticals. , 2011, European journal of pharmaceutics and biopharmaceutics : official journal of Arbeitsgemeinschaft fur Pharmazeutische Verfahrenstechnik e.V.