US5638172A
Expired / Lapsed
US
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On-line quantitative analysis of chemical compositions by raman spectrometry
Assignee: Rosemount Inc
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Filing: 1995-05-25
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Granted: 1997-06-10
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Expires: 2015-05-25
Abstract
Abstract A method for quantitatively monitoring in situ by Raman spectrometry one or more selected constituents of a chemical composition comprises: simultaneously irradiating with a substantially monochromatic radiation source a reference material and a chemical composition containing one or more constituents, the radiation being transmitted from the source to the chemical composition by an excitation conduit connecting the source to an optical probe that interfaces with the composition; simultaneously acquiring at more than one wavelength convolved Raman spectra of the reference material and the chemical composition by means of a spectrograph, which is connected to the optical probe by a collection conduit; choosing the standard Raman spectrum of the reference material; determining the convolution function of the convolved spectra from the convolved Raman spectrum and the standard Raman spectrum of the reference material; applying the convolution function to adjust the convolved Raman spectrum of the composition to produce the standard Raman spectrum of the chemical composition; and applying predetermined calibration means to the standard Raman spectrum of the chemical composition, by which the chemical constitution of the composition at the time of acquisition of the convolved Raman spectra can be ascertained.
Inventors
- 👤 Daniel C. Alsmeyer
- 👤 Michael J. Pearce
- 👤 Vincent A. Nicely
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-08 11:16
CPC Classifications
G; G01; G01J; G01J3/00; G01J3/28; G01J3/44; G01N; G01N21/00; G01N21/62; G01N21/63; G01N21/65; C; C08; C08F; C08F2400/00; C08F2400/02; G01J2003/2866
Claims Analysis
Total Claims: 26
Claim 1
Independent Claim
233 words
A method for quantitatively monitoring in situ by Raman spectrometry one or more selected constituents of a chemical composition, which comprises: (a) simultaneously irradiating with a substantially monochromatic radiation source a reference material and a chemical composition comprising one or more chemical constituents, said radiation being transmitted from said source to an optical probe that interfaces with said chemical composition, said source being connected to said probe by means of an excitation conduit; (b) simultaneously acquiring at more than one wavelength a convolved Raman spectrum of said reference material and a convolved Raman spectrum of said chemical composition by means of a spectrograph remotely situated from said chemical composition, said spectrograph being connected to said optical probe by means of a collection conduit; (c) choosing the standard Raman spectrum of said reference material; (d) from the convolved Raman spectrum and the standard Raman spectrum of said reference material, determining the convolution function; (e) applying said convolution function to adjust the convolved Raman spectrum of said chemical composition to produce thereby the standard Raman spectrum of said chemical composition; (f) applying predetermined calibration means to said standard Raman spectrum of said chemical composition; whereby the quantity of one or more selected constituents of said chemical composition at the time of the acquiring of said convolved Raman spectra can be ascertained; and wherein said excitation conduit and said collection conduit each comprises an optical waveguide.
Claim 2
Independent Claim
233 words
A method for quantitatively monitoring in situ by Raman spectrometry one or more selected constituents of a chemical composition, which comprises: (a) simultaneously irradiating with a substantially monochromatic radiation source a reference material and a chemical composition comprising one or more chemical constituents, said radiation being transmitted from said source to an optical probe that interfaces with said chemical composition, said source being connected to said probe by means of an excitation conduit; (b) simultaneously acquiring at more than one wavelength a convolved Raman spectrum of said reference material and a convolved Raman spectrum of said chemical composition by means of a spectrograph remotely situated from said chemical composition, said spectrograph being connected to said optical probe by means of a collection conduit; (c) choosing the standard Raman spectrum of said reference material; (d) from the convolved Raman spectrum and the standard Raman spectrum of said reference material, determining the convolution function; (e) applying said convolution function to adjust the convolved Raman spectrum of said chemical composition to produce thereby the standard Raman spectrum of said chemical composition; (f) applying predetermined calibration means to said standard Raman spectrum of said chemical composition; whereby the quantity of one or more selected constituents of said chemical composition at the time of the acquiring of said convolved Raman spectra can be ascertained; and wherein said excitation conduit and said collection conduit each comprises an optical waveguide.
Claim 3
Dependent Claim
14 words
A method according to claim 1 wherein said source of radiation is a laser.
Claim 4
Dependent Claim
13 words
A method according to claim 2 wherein said laser is a diode laser.
Claim 5
Dependent Claim
15 words
A method according to claim 3 wherein said diode laser is a multi-mode diode laser.
Claim 6
Dependent Claim
20 words
A method according to claim 1 wherein said excitation conduit and said collection conduit each further comprises a radiation filter.
Claim 7
Dependent Claim
16 words
A method according to claim 1 wherein said spectrograph is a dispersion spectrograph or a FT-interferometer.
Claim 8
Dependent Claim
12 words
A method according to claim 1 wherein said reference material comprises diamond.
Claim 9
Independent Claim
230 words
A method for quantitatively monitoring in situ by Raman spectrometry one or more selected constituents of a chemical composition, which comprises: (a) simultaneously irradiating with a substantially monochromatic radiation source a reference material and a chemical composition comprising one or more chemical constituents, said radiation being transmitted from said source to an optical probe that interfaces with said chemical composition, said source being connected to said probe by means of an excitation conduit; (b) simultaneously acquiring at more than one wavelength a convolved Raman spectrum of said reference material and a convolved Raman spectrum of said chemical composition by means of a spectrograph remotely situated from said chemical composition, said spectrograph being connected to said optical probe by means of a collection conduit; (c) choosing the standard Raman spectrum of said reference material; (d) from the convolved Raman spectrum and the standard Raman spectrum of said reference material, determining the convolution function; (e) applying said convolution function to adjust the convolved Raman spectrum of said chemical composition to produce thereby the standard Raman spectrum of said chemical composition; (f) applying predetermined calibration means to said standard Raman spectrum of said chemical composition; whereby the quantity of one or more selected constituents of said chemical composition at the time of the acquiring of said convolved Raman spectra can be ascertained; and wherein said optical probe comprises at least two optical fibers.
Claim 10
Independent Claim
230 words
A method for quantitatively monitoring in situ by Raman spectrometry one or more selected constituents of a chemical composition, which comprises: (a) simultaneously irradiating with a substantially monochromatic radiation source a reference material and a chemical composition comprising one or more chemical constituents, said radiation being transmitted from said source to an optical probe that interfaces with said chemical composition, said source being connected to said probe by means of an excitation conduit; (b) simultaneously acquiring at more than one wavelength a convolved Raman spectrum of said reference material and a convolved Raman spectrum of said chemical composition by means of a spectrograph remotely situated from said chemical composition, said spectrograph being connected to said optical probe by means of a collection conduit; (c) choosing the standard Raman spectrum of said reference material; (d) from the convolved Raman spectrum and the standard Raman spectrum of said reference material, determining the convolution function; (e) applying said convolution function to adjust the convolved Raman spectrum of said chemical composition to produce thereby the standard Raman spectrum of said chemical composition; (f) applying predetermined calibration means to said standard Raman spectrum of said chemical composition; whereby the quantity of one or more selected constituents of said chemical composition at the time of the acquiring of said convolved Raman spectra can be ascertained; and wherein said optical probe comprises at least two optical fibers.
Claim 11
Independent Claim
248 words
A method for quantitatively monitoring in situ by Raman spectrometry one or more selected constituents of a chemical composition, which comprises: (a) simultaneously irradiating with a substantially monochromatic radiation source a reference material and a chemical composition comprising one or more chemical constituents, said radiation being transmitted from said source to an optical probe that interfaces with said chemical composition, said source being connected to said probe by means of an excitation conduit; (b) simultaneously acquiring at more than one wavelength a convolved Raman spectrum of said reference material and a convolved Raman spectrum of said chemical composition by means of a spectrograph remotely situated from said chemical composition, said spectrograph being connected to said optical probe by means of a collection conduit; (c) choosing the standard Raman spectrum of said reference material; (d) from the convolved Raman spectrum and the standard Raman spectrum of said reference material, determining the convolution function; (e) applying said convolution function to adjust the convolved Raman spectrum of said chemical composition to produce thereby the standard Raman spectrum of said chemical composition; (f) applying predetermined calibration means to said standard Raman spectrum of said chemical composition; whereby the quantity of one or more selected constituents of said chemical composition at the time of the acquiring of said convolved Raman spectra can be ascertained; and wherein said calibration means comprises a concentration-intensity correlation (CIC) multivariate calibration, said concentration-intensity correlation calibration being determined from Raman spectra of mixtures of chemical components having known concentrations.
Claim 12
Independent Claim
248 words
A method for quantitatively monitoring in situ by Raman spectrometry one or more selected constituents of a chemical composition, which comprises: (a) simultaneously irradiating with a substantially monochromatic radiation source a reference material and a chemical composition comprising one or more chemical constituents, said radiation being transmitted from said source to an optical probe that interfaces with said chemical composition, said source being connected to said probe by means of an excitation conduit; (b) simultaneously acquiring at more than one wavelength a convolved Raman spectrum of said reference material and a convolved Raman spectrum of said chemical composition by means of a spectrograph remotely situated from said chemical composition, said spectrograph being connected to said optical probe by means of a collection conduit; (c) choosing the standard Raman spectrum of said reference material; (d) from the convolved Raman spectrum and the standard Raman spectrum of said reference material, determining the convolution function; (e) applying said convolution function to adjust the convolved Raman spectrum of said chemical composition to produce thereby the standard Raman spectrum of said chemical composition; (f) applying predetermined calibration means to said standard Raman spectrum of said chemical composition; whereby the quantity of one or more selected constituents of said chemical composition at the time of the acquiring of said convolved Raman spectra can be ascertained; and wherein said calibration means comprises a concentration-intensity correlation (CIC) multivariate calibration, said concentration-intensity correlation calibration being determined from Raman spectra of mixtures of chemical components having known concentrations.
Claim 13
Dependent Claim
17 words
A method according to claim 9 wherein said Raman spectra of said mixtures comprise standard Raman spectra.
Claim 14
Independent Claim
238 words
A method for quantitatively monitoring in situ by Raman spectrometry one or more selected constituents of a chemical composition, which comprises: (a) simultaneously irradiating with a substantially monochromatic radiation source a reference material and a chemical composition comprising one or more chemical constituents, said radiation being transmitted from said source to an optical probe that interfaces with said chemical composition, said source being connected to said probe by means of an excitation conduit; (b) simultaneously acquiring at more than one wavelength a convolved Raman spectrum of said reference material and a convolved Raman spectrum of said chemical composition by means of a spectrograph remotely situated from said chemical composition, said spectrograph being connected to said optical probe by means of a collection conduit; (c) choosing the standard Raman spectrum of said reference material; (d) from the convolved Raman spectrum and the standard Raman spectrum of said reference material, determining the convolution function; (e) applying said convolution function to adjust the convolved Raman spectrum of said chemical composition to produce thereby the standard Raman spectrum of said chemical composition; (f) applying predetermined calibration means to said standard Raman spectrum of said chemical composition; whereby the quantity of one or more selected constituents of said chemical composition at the time of the acquiring of said convolved Raman spectra can be ascertained; and wherein said chemical composition comprises a polymer-forming composition produced by the reaction of lower molecular weight reactant compounds.
Claim 15
Independent Claim
238 words
A method for quantitatively monitoring in situ by Raman spectrometry one or more selected constituents of a chemical composition, which comprises: (a) simultaneously irradiating with a substantially monochromatic radiation source a reference material and a chemical composition comprising one or more chemical constituents, said radiation being transmitted from said source to an optical probe that interfaces with said chemical composition, said source being connected to said probe by means of an excitation conduit; (b) simultaneously acquiring at more than one wavelength a convolved Raman spectrum of said reference material and a convolved Raman spectrum of said chemical composition by means of a spectrograph remotely situated from said chemical composition, said spectrograph being connected to said optical probe by means of a collection conduit; (c) choosing the standard Raman spectrum of said reference material; (d) from the convolved Raman spectrum and the standard Raman spectrum of said reference material, determining the convolution function; (e) applying said convolution function to adjust the convolved Raman spectrum of said chemical composition to produce thereby the standard Raman spectrum of said chemical composition; (f) applying predetermined calibration means to said standard Raman spectrum of said chemical composition; whereby the quantity of one or more selected constituents of said chemical composition at the time of the acquiring of said convolved Raman spectra can be ascertained; and wherein said chemical composition comprises a polymer-forming composition produced by the reaction of lower molecular weight reactant compounds.
Claim 16
Dependent Claim
27 words
A method according to claim 11 wherein said lower molecular weight reactant compounds comprise a diol compound and a dicarboxylic acid compound or a dicarboxylic ester compound.
Claim 17
Dependent Claim
30 words
A method according to claim 12 wherein said diol compound comprises ethylene glycol, 1,4-cyclohexanedimethanol, 1,4-butanediol, diethylene glycol, triethylene glycol, polyethylene glycol, polypropylene glycol, bis(2-hydroxyethyl) terephthalate, bis(4-hydroxymethylcyclohexylmethyl) terephthalate, or (2-hydroxyethyl)-(4-hydroxyethylcyclohexylmethyl) terephthalate.
Claim 18
Dependent Claim
25 words
A method according to claim 12 wherein said dicarboxylic acid compound comprises terephthalic acid, isophthalic acid, 1,4-naphthalenedicarboxylic acid, 2,6-naphthalenedicarboxylic acid, 1,4-cyclohexanedicarboxylic acid, or adipic acid.
Claim 19
Dependent Claim
31 words
A method according to claim 12 wherein said dicarboxylic ester compound comprises dimethyl terephthalate, dimethyl isophthalate, dimethyl 2,6-naphthalenedicarboxylate, dimethyl 2,6-naphthalenedicarboxylate, dimethyl 1,4-cyclohexanedicarboxylate, dimethyl adipate, bis(2-hydroxyethyl) terephthalate, bis(4-hydroxymethylcyclohexylmethyl) terephthalate, or (2-hydroxyethyl)-(4-hydroxymethylcyclohexylmethyl) terephthalate.
Claim 20
Dependent Claim
19 words
A method according to claim 12 wherein said lower molecular weight reactant compounds comprise ethylene glycol and terephthalic acid.
Claim 21
Dependent Claim
13 words
A method according to claim 16 wherein said reactant compounds further comprises cyclohexanedimethanol.
Claim 22
Dependent Claim
19 words
A method according to claim 12 wherein said lower molecular weight reactant compounds comprise ethylene glycol and dimethyl terephthalate.
Claim 23
Dependent Claim
13 words
A method according to claim 18 wherein said reactant compounds further comprises cyclohexanedimethanol.
Claim 24
Dependent Claim
14 words
A method according to claim 11 wherein said chemical composition further comprises poly(ethylene terephthalate).
Claim 25
Independent Claim
231 words
A method for quantitatively monitoring in situ by Raman spectrometry one or more selected constituents of a chemical composition, which comprises: (a) simultaneously irradiating with a substantially monochromatic radiation source a reference material and a chemical composition comprising one or more chemical constituents, said radiation being transmitted from said source to an optical probe that interfaces with said chemical composition, said source being connected to said probe by means of an excitation conduit; (b) simultaneously acquiring at more than one wavelength a convolved Raman spectrum of said reference material and a convolved Raman spectrum of said chemical composition by means of a spectrograph remotely situated from said chemical composition, said spectrograph being connected to said optical probe by means of a collection conduit; (c) choosing the standard Raman spectrum of said reference material; (d) from the convolved Raman spectrum and the standard Raman spectrum of said reference material, determining the convolution function; (e) applying said convolution function to adjust the convolved Raman spectrum of said chemical composition to produce thereby the standard Raman spectrum of said chemical composition; (f) applying predetermined calibration means to paid standard Raman spectrum of said chemical composition; whereby the quantity of one or more selected constituents of said chemical composition at the time of the acquiring of said convolved Raman spectra can be ascertained; and wherein said chemical composition comprises volatile material at a distillation head.
Claim 26
Independent Claim
231 words
A method for quantitatively monitoring in situ by Raman spectrometry one or more selected constituents of a chemical composition, which comprises: (a) simultaneously irradiating with a substantially monochromatic radiation source a reference material and a chemical composition comprising one or more chemical constituents, said radiation being transmitted from said source to an optical probe that interfaces with said chemical composition, said source being connected to said probe by means of an excitation conduit; (b) simultaneously acquiring at more than one wavelength a convolved Raman spectrum of said reference material and a convolved Raman spectrum of said chemical composition by means of a spectrograph remotely situated from said chemical composition, said spectrograph being connected to said optical probe by means of a collection conduit; (c) choosing the standard Raman spectrum of said reference material; (d) from the convolved Raman spectrum and the standard Raman spectrum of said reference material, determining the convolution function; (e) applying said convolution function to adjust the convolved Raman spectrum of said chemical composition to produce thereby the standard Raman spectrum of said chemical composition; (f) applying predetermined calibration means to paid standard Raman spectrum of said chemical composition; whereby the quantity of one or more selected constituents of said chemical composition at the time of the acquiring of said convolved Raman spectra can be ascertained; and wherein said chemical composition comprises volatile material at a distillation head.
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