Process and apparatus for the determination of the concentration of a substance dissolved in a solvent by means of an osmometer

• US 5,005,403 A
• Filed: 07/25/1989
• Issued: 04/09/1991
• Est. Priority Date: 07/25/1988
• Status: Expired due to Fees

• Current Assignee: Ernst Steudle
• Original Assignee: Ernst Steudle
• Inventors: Steudle, Ernst, Stumpf, Burkhard
• Primary Examiner(s): Williams, Hezron E.
• Application Number:
  US07/385,324
• Time in Patent Office: 623 Days
• Field of Search: 73/64.3
• US Class Current: 73/61.71
• CPC Class Codes: G01N 13/04 Investigating osmotic effects

Abstract

In a process for the determination of the concentration of a substance dissolved in a solvent by means of an osmometer, comprising a two-chamber system with a first chamber having an osmosis cell and a second chamber for the measurement solution, to shorten the measurement time and to improve the separation of permeating components during the measurement of the concentration of the substances in the measurement solution, the pressure in the osmosis cell is held constant with an incompressible membrane arrangement, whereby with a pressure measurement apparatus in the second chamber after the replacement of a solvent, a reference solution or a calibration solution by a measurement solution, a pressure curve which corresponds to the concentrations of the nonpermeating substance and permeating substances or to the flows of the permeating substances between the osmosis cell and the second chamber is measured, and by analysis of the curve, the concentration of the nonpermeating and permeating substances in the measurement solution is determined. In one embodiment, the volume of the chamber containing the osmotic cell is varied in response to the pressure vs. time curve so as to maintain the volume flow of solvent through the membrane at substantially zero.

Claims

1. A process for testing a test solution, said test solution comprising a solvent and at least one solute dissolved in said solvent, said process employing a first chamber defining a first volume, a second chamber defining a second volume, said first volume being less than said second volume and a membrane interposed between said first and second chambers, said process comprising the steps of:

(a) introducing an osmometer solution into said first chamber;

(b) introducing a reference solution into said second chamber;

(c) determining a reference pressure P₀ established in one of said first and second chambers;

(d) replacing said reference solution in said second chamber with said test solution;

(e) limiting the amount of fluid exchange between said first and second chambers to a value equalling approximately zero;

(f) limiting the amount of deflection of said membrane to a preselected value;

(g) maintaining a constant fluid pressure in one of said first and second chambers;

(h) determining at least one pressure change characteristic occurring in the other of said first and second chambers; and

(i) using said at least one determined pressure change characteristic to determine the concentration of said at least one solute dissolved in said solvent.

2. The process according to claim 1, wherein said one of said first and second chambers in which said fluid pressure is maintained constant in said first chamber containing said osmometer solution, and wherein the other of said first and second chambers in which said at least one pressure change characteristic is determined in said second chamber containing said test solution.

3. The process according to claim 2, wherein said membrane is maintained in a substantially nondeflectable configuration.

4. The process according to claim 2, wherein said at least one pressure change characteristic comprises a maximum pressure change Δ

P_max which substantially corresponds to the difference between said reference pressure P₀ in said second chamber when said second chamber contains said reference solution and the fluid pressure in said second chamber substantially immediately following the replacement of said reference solution with said test solution.

5. The process according to claim 4, wherein said solute dissolved in said solvent comprises at least one of:

(1) a nonpermeating substance;

(2) a permeating substance;

(3) a mixture of a nonpermeating substance and a permeating substance; and

(4) at least two permeating substances; and

wherein said nonpermeating substances are substances which have relatively low degree of permeability with respect to said membrane, as compared to said permeating substances which are substances having a relatively high degreee of permeability with respect to said membrane.

6. The process according to claim 5, wherein said solute consists of said mixture of said nonpermeating substance and said permeating substance 3, and;

wherein said determination of concentration in step (i) comprises at least one of;

(a) determining the combined concentration of said nonpermeating substance and said permeating substance through a relationship wherein said combined concentration is proportional to said maximum pressure change Δ

P_max ; and

(b) determining a substantially stable final pressure in said second chamber and determining the individual concentration of said nonpermeating substance through a relationship wherein said individual concentration of said nonpermeating substance is proportional to the difference between said substantially stable final pressure and said reference pressure P₀.

7. The process according to claim 5, wherein said determination of concentration in step (i) comprises at least one of:

(a) determining the concentration of said nonpermeating substance according to the relationship;

space="preserve" listing-type="equation">Δ

P=π

=R·

T·

C, )Equation

     1)

wherein

π

is the osmotic pressure,

C is the concentration,

R=8,31434 J/°

K mol, and

T is the absolute temperature; and

(b) determining the concentration of said permeating substance according to the relationship;

space="preserve" listing-type="equation">Δ

P=σ

·

π

, (Equation

     2)

wherein σ

is the coefficient of reflection of said permeating substance.

8. The process according to claim 7, wherein said solute consists of said mixture of permeating substances in item (4), wherein a first of said at least two permeating substance has a relatively higher degree of permeability with respect to said membrane than a second of said at least two permeating substances, and wherein said determination of concentration in step (i) further comprises at least one of:

(a) determining a pressure change Δ

P^S associated with the passage of said first permeating substance through said membrane;

(b) determining the concentration of said first permeating substance according to Equation 2;

(c) determining a pressure change Δ

P^F associated with the passage of said second permeating substance through said membrane; and

(d) determining the concentration of said second permeating substance according to Equation 2.

9. The process according to claim 8, wherein:

at least one of said first chamber and said second chamber employs at least one rigid wall;

said membrane is generally incompressible;

pressure P_O is a constant hydrostatic working pressure;

said maintaining of constant fluid pressure in step (g) adjusts the propulsion force for the volume of flow through said membrane; and

at least one of said Δ

P^S and Δ

P^F occurs at an exponential rate.

10. The process according to claim 2, wherein said maintaining of a constant fluid pressure in said first chamber in step (e) is carried out by varying at least one of:

(a) the fluid pressure in said second chamber, and (b) the volume of said second chamber.

11. The process according to claim 2, wherein said solute comprises a substance with respect to which said membrane is relatively permeable, and wherein said concentration determination in step (i) comprises:

(a) determining at least an approximate value of the rate of change of the fluid pressure in said second chamber with respect to time (dP/dt) at substantially the time of replacement of said reference solution in said second chamber with said test solution (t=0); and

(b) determining the concentration of said substance through a relationship wherein the concentration of said substance is proportional to said rate of change (dP/dt) at said time (t=0).

12. The process according to claim 2, further comprising the additional step of inducing, in said first chamber, a fluid pressure which is one of a negative pressure and a pressure which is less than the ambient atmospheric pressure prior to the replacement of said reference solution in said second chamber with said test solution.

13. The process according to claim 2, further comprising the additional step of inducing, in said first chamber, a fluid pressure which is less than the fluid pressure in said second chamber prior to the replacement of said reference solution in said second chamber with said test solution.

14. The process according to claim 2, wherein said pressure change characteristic determination in step (h) comprises sensing, digitizing and storing in memory values representative of the fluid pressure in said second chamber for a period of time following the replacement of said reference solution in said second chamber with said test solution, and wherein said concentration determination in step (i) comprises comparing said sensed, digitized and stored values with determination criteria previously stored in memory.

15. The process according to claim 14, wherein said determination criteria comprise sensed, digitized and stored values representative of the fluid pressure in said second chamber following replacement of said reference solution with at least one solution having a known concentration of said solute.

16. The process according to claim 2, wherein said first and second chambers are maintained at a constant temperature.

17. The process according to claim 2, wherein said reference solution consists of at least one of said solvent and said solvent having said solute dissolved therein, and wherein said osmometer solution consists of at least one of said solvent and said solvent having said solute dissolved therein.

18. A process for the determination of the concentration of a solution to be tested comprising at least one substance dissolved in a solvent, said process comprising the steps of:

(a) providing a first chamber defining a first volume and a second chamber defining a second volume, said first volume being less than said second volume;

(b) interfacing said first and second chambers through a membrane;

(c) introducing an osmometer solution into said first chamber;

(d) introducing the solution to be tested into said second chamber;

(e) limiting the amount of fluid exchange between said first and second chambers to a value equalling approximately zero;

(f) limiting the amount of deflection of said membrane to a preselected value;

(g) maintaining a constant fluid pressure in one of said first and second chambers;

(h) determining at least one pressure change characteristic occurring in the other of said first and second chambers; and

(i) using said at least one determined pressure change characteristic to determine the concentration of the at least one substance dissolved in the solvent.

19. The process according to claim 18, further comprising the additional steps of calibrating the process by introducing a calibration solution into said second chamber, and determining at least one pressure change characteristic occurring in the other of said first and second chambers in response thereto.

20. The process according to claim 19, wherein:

at least one of said first chamber and said second chamber employs at least one rigid wall; and

said maintaining of constant fluid pressure in step (g) adjusts the propulsion force for the volume of flow through said membrane.

21. An apparatus for the determination of the concentration of a solute dissolved in a solvent, said apparatus comprising:

a first chamber defining a first volume;

a second chamber defining a second volume, said first volume being less than said second volume;

a membrane interposed between said first and second chambers;

means for introducing an osmometer solution into said first chamber;

means for introducing, selectively, into said second chamber, a reference solution and said solute dissolved in said solvent;

means for limiting the amount of fluid exchange between said first and second chambers to a value equalling approximately zero;

means for limiting the amount of deflection of said membrane to a preselected value;

pressure maintenance means for maintaining a constant pressure in one of said first and second chambers; and

pressure sensor means for sensing the fluid pressure in the other of said first and second chambers.

22. The apparatus according to claim 21, wherein said pressure sensor means senses the fluid pressure in said second chamber, wherein said pressure maintenance means maintains a constant pressure in said first chamber, and further comprising another pressure sensor means for sensing the fluid pressure in said first chamber and deflection prevention means for preventing any substantial deflection of said membrane.

23. The apparatus according to claim 22, wherein said pressure maintenance means comprises:

pressure/volume varying means for varying at least one of;

the pressure of said second chamber and the volume of said second chamber; and

control means for receiving signals from said another pressure sensor means indicative of the fluid pressure in said first chamber, and for activating said pressure/volume varying means in response thereto.

24. The apparatus according to claim 23, wherein said means for introducing, selectively, into said second chamber, said reference solution and said solute dissolved in said solvent comprises a feed line, a discharge line, pump means disposed in one of said feed line and said discharge line, and valve means disposed in the other of said feed line and said discharge line.

25. The apparatus according to claim 24, wherein said pressure sensor means comprises means for generating digitized signals representative of the fluid pressure in said second chamber, and wherein said control means comprises a computer, said computer including means for receiving and storing said digitized signals in a time ordered sequence.

26. The apparatus according to claim 25, further comprising display means for displaying said digitized signals.

27. The apparatus according to claim 26, wherein:

at least one of said first chamber and said second chamber employs at least one rigid wall; and

said maintaining of constant fluid pressure adjusts the propulsion force for the volume of flow through said membrane.

28. The apparatus according to claim 21, wherein said membrane comprises at least one of:

a substantially incompressible porous body saturated with solution; and

glass sinter material;

a solution film interposed between at least two support grids;

a hyperfiltration membrane; and

a wood membrane.

29. The apparatus according to claim 28, further comprising an osmosis cell located within said first chamber, said osmosis cell having a layer thickness of 0.2 mm.

30. A process for the determination of the concentration of a test solution, said test solution comprising at least one solute dissolved in a solvent, said process employing a first chamber defining a first volume, a second chamber defining a second volume, said first volume being less than said second volume, a membrane interposed between said first and second chambers, compensation means for compensating for the volume flow of at least said solvent through said membrane and between said first and second chambers, and pressure sensing means for sensing at least one pressure existing in said first chamber, said process comprising the steps of:

introducing an osmometer solution into said first chamber;

introducing a reference solution into said second chamber;

determining a reference pressure P₀ established in one of s aid first and second chambers;

replacing said reference solution in said second chamber with said test solution;

limiting the amount of fluid exchange between said first and second chambers to a value equalling approximately zero;

limiting the amount of deflection of said membrane to a preselected value;

employing said compensation means for compensating for the volume flow of at least said solvent through said membrane;

employing said pressure sensing means for determining at least one pressure change characteristic occurring in said first chamber; and

using said at least one determined pressure change characteristic occurring in said first chamber to determine the concentration of said at least one solute dissolved in said solvent.

31. A process according to claim 30, wherein said compensation means comprises means for varying the volume of said first chamber and wherein said step of employing said compensation means comprises varying the volume of said first chamber to compensate for the volume flow of at least said solvent through said membrane.

32. A process according to claim 30, wherein said compensation means comprises means for varying the hydrostatic pressure existing in said first chamber and wherein said step of employing said compensation means comprises varying the hydrostatic pressure existing in said first chamber to compensate for the volume flow of at least said solvent through said membrane.

33. The process according to claim 30, wherein said at least one solute comprises a substance with respect to which said membrane is relatively nonpermeable, and wherein said at least one determined pressure change characteristic occurring in said first chamber comprises a maximum pressure change differential (P_O -P_E) between the pressure in said first chamber when said second chamber contains said reference solution (P_O) and the pressure in said first chamber when said second chamber contains said test solution (P_E).

34. The process according to claim 30, wherein said at least one solute comprises a substance with respect to which said membrane is relatively permeable, and wherein said at least one determined pressure change characteristic occurring in said first chamber comprises a maximum pressure change differential (P_O -P_min) between the pressure in said first chamber when said second chamber contains said reference solution (P_O) and the peak pressure in said first chamber when said second chamber contains said test solution (P_min).

35. The process according to claim 30, wherein:

at least one of said first chamber and said second chamber employs at least one rigid wall; and

said pressure P_O is a constant hydrostatic working pressure.

36. An apparatus for the determination of the concentration of a test solution, said test solution comprising a solute dissolved in a solvent, said apparatus comprising:

a first chamber defining a first volume;

a second chamber defining a second volume, said first volume being less than said second volume;

a membrane interposed between said first and second chambers;

means for introducing an osmometer solution into said first chamber;

means for introducing, selectively, into said second chamber, a reference solution and said test solution;

means for limiting the amount of fluid exchange between said first and second chambers to a value equalling approximately zero;

means for limiting the amount of deflection of said membrane to a preselected value;

pressure sensing means for sensing the pressure existing in said first chamber and for generating signals representative thereof; and

compensation means for compensating for the volume flow of at least said solvent through said membrane and between said first and second chambers.

37. An apparatus according to claim 36, wherein said compensation means comprises means for varying the hydrostatic pressure existing in said first chamber.

38. An apparatus according to claim 36, wherein said compensation means comprises means for varying the volume of said first chamber.

39. An apparatus according to claim 36, wherein said compensation means comprises a reciprocally translatable piston which can be extended into and withdrawn from said first chamber, and means for translating said piston in response to said pressure representative signals generated by said pressure sensing means.

40. The apparatus according to claim 36, wherein:

at least one of said first chamber and said second chamber employs at least one rigid wall.