Method for determining concentration in a solution using attenuated total reflectance spectrometry

• US 5,416,579 A
• Filed: 07/21/1994
• Issued: 05/16/1995
• Est. Priority Date: 07/23/1993
• Status: Expired due to Fees

• Current Assignee: NovaChem BV (Abbvie Incorporated)
• Original Assignee: Nova Chem Limited
• Inventors: Barshad, Yoav, Barshad, Yael S.
• Primary Examiner(s): EVANS, FANNIE L
• Application Number:
  US08/278,292
• Time in Patent Office: 299 Days
• Field of Search: 356/300, 356/133, 356/319, 356/326, 356/328
• US Class Current: 356/300
• CPC Class Codes: G01N 21/552 Attenuated total reflection

Abstract

A method for analyzing fluids, particularly the solute concentration in liquids which are dense or viscous and are only slightly transparent to light, which utilizes an attenuated total reflectance cell with a curved-path optical wave guide, particularly an optical fiber, the wave guide having a portion of its surface interfacing with the fluid to be analyzed. The wave guide has selected dimensions and properties including bend radius, waveguide radius, index of refraction, and effective light path which optimize the measurement. The optimum wave guide dimensions and wavelength of light are selected through calibration of the ATR device with a plurality of fluids of known composition. Light is transmitted through the wave guide and is attenuated by partial reflectance within the wave guide due to absorbance by the fluid being analyzed. The attenuated transmittance is related to optical absorbance, which is correlated directly to concentration of solute.

Claims

1. A method of using an attenuated total reflectance (ATR) spectrophotometer having an optical wave guide with a curved optical path to determine concentration of solute in a test fluid of unknown concentration, comprising the steps of:

a) providing a plurality of optical wave guides for said ATR spectrophotometer having differing values of D, where D is the ratio of the bend radius of said optical wave guide to the radius of said optical wave guide, each of said plurality of wave guides having an index of refraction greater than that of said fluid of unknown concentration, and each of said wave guides having a characteristic effective path (P_eff) and a characteristic number of internal reflections (z) for light of a given wavelength;

b) providing a plurality of calibration fluids comprising the materials of said solute and test fluid at differing known concentrations of solute (C);

c) determining values of transmittance (T) in said ATR spectrophotometer when combining each of said known concentrations with each of said optical wave guides having differing values of D;

d) calculating absorbance units (AU) for each of said combinations of C and D according to the equation;

space="preserve" listing-type="equation">AU=-log(T.sup.1/z);

e) selecting a wavelength of light (λ

) for said determination;

f) measuring the index of refraction of said test fluid at said selected wavelength of light;

g) selecting an operating range of said concentration values to be determined by said ATR spectrophotometer;

h) selecting an optical wave guide for said ATR spectrophotometer having a D value (D_test) which provides AU values in the working range of sensitivities of said ATR spectrophotometer over said operating range of said concentration values;

i) immersing said selected optical wave guide having said D_test value in said fluid of unknown concentration;

j) determining the AU value for said fluid; and

k) comparing said AU value for said fluid to said values of AU determined for said calibration fluids with said element having said D_test value to determine the value of said solute concentration in said fluid of unknown concentration.

2. The method of claim 1 wherein said working range of sensitivities is between about 0.1 and about 0.7 ABS units.

3. The method of claim 1 wherein said working range of sensitivities is between about 0.3 and about 0.5 ABS units.

4. The method of claim 1 further comprising the step of confirming said value of said solute concentration in said fluid of unknown concentration by calculating said value according to the equation:

space="preserve" listing-type="equation">ABS=-log(.sup.z √

T)=1-λ

·

P.sub.eff ·

C

wherein ABS is the measured value of said optical absorbance in absorbance units, λ

is said selected wavelength of light, P_eff is the effective path of light of said selected wavelength through said selected wave guide, z is the number of internal reflections of light of said selected wavelength in passing through said selected wave guide, T is the optical transmittance measured at the output of said selected wave guide, and C is said value of said concentration of solute in said fluid of unknown concentration.

5. The method of claim 1 wherein said step of selecting an operating range includes providing an estimated value of said unknown concentration of solute to be determined.