US 12,352,741 B2
Apparatus and method for measuring degradation kinetics of a biomaterial in aqueous solution below the normal freezing temperature
Andreia Filipa Silvestre Duarte, Sacavém (PT); Pedro Gil Sena Rego, Lisbon (PT); and Rui De Brito Estrela, Lisbon (PT)
Assigned to SMARTFREEZ, LDA, Porto Salvo (PT)
Appl. No. 16/980,115
Filed by SMARTFREEZ, LDA, Porto Salvo (PT)
PCT Filed Mar. 12, 2019, PCT No. PCT/IB2019/051995
§ 371(c)(1), (2) Date Sep. 11, 2020,
PCT Pub. No. WO2019/175767, PCT Pub. Date Sep. 19, 2019.
Claims priority of application No. 110619 (PT), filed on Mar. 12, 2018.
Prior Publication US 2021/0018485 A1, Jan. 21, 2021
Int. Cl. G01N 33/48 (2006.01); G01N 21/25 (2006.01); G01N 31/22 (2006.01); G01N 33/15 (2006.01)
CPC G01N 33/48 (2013.01) [G01N 21/25 (2013.01); G01N 31/22 (2013.01); G01N 33/15 (2013.01)] 15 Claims
OG exemplary drawing
 
1. A method for preparation of a sample for measuring degradation kinetics of a biomaterial in aqueous solution, comprising the steps of:
filling a high-pressure container with the biomaterial in aqueous solution and submitting said biomaterial to a temperature below the freezing temperature of the biomaterial at atmospheric pressure;
closing the high-pressure container with a nucleating-lock, wherein the nucleating-lock comprises a compressing-lid and a plug with a retainer, wherein the retainer prevents detachment of the plug from the high-pressure container, and wherein the retainer insulates the plug from the compressing-lid at a temperature below the freezing temperature of the biomaterial at atmospheric pressure;
allowing the high-pressure container to reach a pre-determined temperature different from the freezing temperature of the biomaterial at atmospheric pressure;
wherein the tip of the plug of the nucleating-lock contacts the surface of the biomaterial solution inducing the nucleation whereby an ice layer is formed acting as a natural piston and ensuring isochoric conditions;
removing the high-pressure container at a selected time and placing it at a temperature higher than the freezing temperature of the biomaterial at atmospheric pressure; and
opening the high-pressure container and recovering the biomaterial in aqueous solution.