CN106323939B - The method that multicomponent system component is directly determined using Raman spectrum - Google Patents
The method that multicomponent system component is directly determined using Raman spectrum Download PDFInfo
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- CN106323939B CN106323939B CN201610667791.2A CN201610667791A CN106323939B CN 106323939 B CN106323939 B CN 106323939B CN 201610667791 A CN201610667791 A CN 201610667791A CN 106323939 B CN106323939 B CN 106323939B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N2021/653—Coherent methods [CARS]
Abstract
A method of multicomponent system component is directly determined using Raman spectrum, be related to the measurement method of multicomponent system component, comprising steps of 1. measuring Raman spectrum: measure respectively the pure solution of each component of multicomponent system to be measured, the multicomponent system to be measured of unknown content homogeneous phase solution M Raman spectrum；2. each Raman spectrum is converted to integral spectrum by computer；Wherein, the integral spectrum to quantitative component is denoted as SI, the matrix that other components integral spectrum is constituted is denoted as SJ, and the integral spectrum of homogeneous phase solution M is denoted as SPI；3. calculating separately vector-space angle θ, SPI and SJ vector-space angle β of SI and SJ；4. obtaining the content in homogeneous phase solution M to quantitative component by calculating β/θ.The present invention can facilitate the direct measurement for realizing each phase of multicomponent system, and easy to operate, data are true, can be used for the process regulation of the series of separate unit such as research and extraction, the rectifying operation that balances each other of liquid-liquid multicomponent system.
Description
Technical field
The present invention relates to a kind of measurement method of multicomponent system component, especially a kind of use Raman spectrum directly determines more
The method of first system component.
Background technique
In Multiple liquid phase system, when balancing each other in each phase component assay, be chemical teaching and research in
Common and important work, for example, Multicomponent Phase Equilibria drafting, extractant condition selection etc..Existing method at present, or
It is characterized using chromatography after sampling or using index of refraction with material composition relationship or using system turbidity variation etc., this
There are the disadvantages such as cumbersome or accuracy is low for a little methods；Additionally due to the sensibility to balance each other, the contacts operation such as sampling can
It can interfere and balance each other, to influence the authenticity of data.
Summary of the invention
The technical problem to be solved by the present invention is providing a kind of side for directly determining multicomponent system component using Raman spectrum
Method, to solve the shortcoming that aforesaid operations of the existing technology are cumbersome, accuracy is low, influence data validity.
The technical solution for solving above-mentioned technical problem is: a kind of side directly determining multicomponent system component using Raman spectrum
Method, method includes the following steps:
1. measuring Raman spectrum: measure respectively the pure solution of each component of multicomponent system to be measured, unknown content it is to be measured more
The Raman spectrum of the homogeneous phase solution M of first system；
2. each Raman spectrum is converted to integral spectrum by computer；Wherein, the integral spectrum to quantitative component is remembered
For SI, the matrix that other components integral spectrum is constituted is denoted as SJ, and the integral spectrum of homogeneous phase solution M is denoted as SPI；
3. calculating separately vector-space angle θ, SPI and SJ vector-space angle β of SI and SJ；
4. obtaining the content in homogeneous phase solution M to quantitative component by calculating β/θ.
A further technical solution of the present invention is: step 1. in, also need known content of the measurement series for calibration
The Raman spectrum of the homogeneous phase solution N of multicomponent system to be measured；Step 2. in, also by be used for demarcate homogeneous phase solution N spectrum be denoted as
SBI；Step 3. in, also calculate separately vector-space angle α of SBI and SJ；And step 3. with step 4. between, also
Include step 3. -1: calibration measurement result: the content of component to be measured in homogeneous phase solution N being calculated to obtain by α/θ, this is mixed
The content of component to be measured is compared with known content in liquid N, if error is larger, adjusts spectral wavelength point range, reduces predicted value
Linear deviation degree.
The further technical solution of the present invention is: step 1. in, the known content of the series for calibration
The homogeneous phase solution N of multicomponent system to be measured is to prepare mixing for serial known content in the system not content range of split-phase
Liquid.
A further technical solution of the present invention is: step 1. in, measurement Raman spectrum be using LR laser raman pop one's head in, point
The pure solution of each component of multicomponent system to be measured, the homogeneous phase solution M of the multicomponent system to be measured of unknown content, known content are not measured
Multicomponent system to be measured homogeneous phase solution N Raman spectrum.
The further technical solution of the present invention is: step 2. in, by Raman spectrum be converted to integral spectrum be difference
The Raman spectrum point-by-point integration that will be measured, is converted to integral spectrum.
Due to using the above structure, the present invention using Raman spectrum directly determine the method for multicomponent system component with it is existing
Technology is compared, and is had the advantages that
1. can be convenient the direct measurement for realizing each phase of multicomponent system
Since the present invention includes 1. step measures Raman spectrum；2. Raman spectrum is converted to integral light by computer
Spectrum；Wherein, the integral spectrum to quantitative component is denoted as SI, the matrix that other components integral spectrum is constituted is denoted as SJ, unknown to contain
The integral spectrum of the homogeneous phase solution M of the multicomponent system to be measured of amount is denoted as SPI；3. calculating separately vector-space angle of SI and SJ
The vector of θ, SPI and SJ-space angle β；4. calculating to obtain content in homogeneous phase solution M to quantitative component by β/θ.Therefore, originally
Invention is the characteristics of using Raman spectrum non-cpntact measurement, to pass through space-vector of spectrum under the premise of system is formed and determined
Angle, the content of direct quantitative component can be convenient the direct measurement for realizing each phase of multicomponent system.
2. it is easy to operate, it can be convenient and accurately quantified
Due to the multicomponent system for determining composition, the present invention is not necessarily to modeling and complicated calibration, easy to operate, can be convenient
Accurately quantified.
3. certifiable data validity
Since the present invention uses non-cpntact measurement, interference will not be generated to system, thus ensure that the authenticity of data,
Accuracy rate is higher, and the dynamic system research for practical chemistry and chemical industry provides great convenience.
4. applied widely
The present invention can be used for the research that balances each other of liquid-liquid multicomponent system, it may also be used for the series of separate unit such as extraction, rectifying
The process regulation of operation.
In the following, in conjunction with the accompanying drawings and embodiments to the method for directly determining multicomponent system component using Raman spectrum of the present invention
Technical characteristic be further described.
Detailed description of the invention
Fig. 1: the Raman spectrogram of component A, B, C in embodiment one, two；
Fig. 2: the Raman spectrogram of the ternary system mixed in embodiment one, two；
Fig. 3: embodiment one, two medium wave bands are 1100-1400cm-1Component A, B, C Raman spectrogram；
Fig. 4: the relational graph of component A volumn concentration and angle value in embodiment one.
Fig. 5: the relational graph of component B volumn concentration and angle value in embodiment two.
Specific embodiment
A method of multicomponent system component is directly determined using Raman spectrum, method includes the following steps:
1. measuring Raman spectrum: in the multicomponent system not content range of split-phase, in volumetric flask or conical flask, preparing not
Know the homogeneous phase solution M of the multicomponent system to be measured of content, prepares the homogeneous phase solution N of the multicomponent system to be measured of serial known content,
Phase solution N is used for prediction result data scaling；It is popped one's head in using LR laser raman, measures the pure of each component of multicomponent system to be measured respectively
Solution, the homogeneous phase solution M of the multicomponent system to be measured of unknown content, known content multicomponent system to be measured homogeneous phase solution N drawing
Graceful spectrum；
2. each Raman spectrum is converted to integral spectrum by computer；Wherein, the integral spectrum to quantitative component is remembered
For SI, the matrix that the integral spectrum of other components is constituted is denoted as SJ, and the integral spectrum of homogeneous phase solution M is denoted as SPI；It will also be used to mark
The integral spectrum of fixed homogeneous phase solution N is denoted as SBI；
3. calculate separately vector-space angle θ, SBI and SJ vector-space angle α, SPI and SJ of SI and SJ to
Amount-space angle β；
3. -1: calibration measurement result: the content of component to be measured in homogeneous phase solution N is calculated to obtain by α/θ, by the homogeneous phase solution
The content of component to be measured is compared with known content in N, if error is larger, adjusts spectral wavelength point range, reduces predicted value
Linear deviation degree；
4. calculating to obtain content in homogeneous phase solution M to quantitative component by β/θ.
The following is specific embodiments of the present invention:
Embodiment one
The present embodiment one passes through a kind of component hexamethylene in a kind of determining hexamethylene-n-hexane-ethyl alcohol ternary liquid phase system
Percent by volume process, method proposed by the present invention is illustrated.
A method of multicomponent system component is directly determined using Raman spectrum, wherein multicomponent system be hexamethylene-just oneself
Alkane-ethyl alcohol ternary liquid phase system is hexamethylene to quantitative component, method includes the following steps:
1. hexamethylene-n-hexane-ethyl alcohol ternary liquid phase the system for preparing serial known content is homogeneous in volumetric flask
Solution N: according to the percent by volume to quantitative component A hexamethylene within the scope of 0-100% (8.0%, 16.0%, 30.0%, 50.0%,
70.0%, 90.0%) the homogeneous phase solution N of 6 samples is prepared, remaining component B n-hexane, component C ethyl alcohol are constituted with random proportion；Again
Prepare hexamethylene-n-hexane-ethyl alcohol ternary system homogeneous phase solution M of unknown content.
It is popped one's head in using LR laser raman, measures pure solution, the known content of each component (hexamethylene, n-hexane, ethyl alcohol) respectively
Homogeneous phase solution N, unknown content homogeneous phase solution M Raman spectrum；
Fig. 1 is the Raman spectrogram of component A, B, C, spectrally has friendship with component B, C to quantitative component A as seen from the figure
It is folded, it is quantitative that peak can not be directlyed adopt.
Fig. 2 is mixed hexamethylene-n-hexane-ethyl alcohol ternary liquid phase system Raman spectrum, due to matching for remaining composition
Than random, so can not also directly obtain the concentration situation of change to quantitative component on the diagram.
2. to reduce calculation amount, the spectral band 1100-1400cm that the present invention selects component response to concentrate-1For calculating,
Such as Fig. 3, by computer respectively to the Raman of 6 samples, homogeneous phase solution M in the pure solution and homogeneous phase solution N of component A, B, C
Spectrum is converted to integral spectrum；The integral spectrum of wherein component A is denoted as SI, the matrix note that the integral spectrum of component B, C is constituted
For SJ, the integral spectrum of 6 sample homogeneous phase solution N is denoted as SBI, the integral spectrum of homogeneous phase solution M is denoted as SPI；
3. calculate separately vector-space angle θ, SBI and SJ vector-space angle α, SPI and SJ of SI and SJ to
Amount-space angle β；
3. -1 calibration measurement result: the percent by volume of component A in 6 sample homogeneous phase solution N is calculated to obtain by α/θ, with
Given value compares.For the result being calculated as shown in table 1 and Fig. 4, prediction result has good linear relationship and accuracy.
4. the volume of component A hexamethylene in hexamethylene-n-hexane-ethyl alcohol ternary liquid phase system can be obtained by calculating β/θ
Degree.
In order to verify this method, present inventor has also made verification test to embodiment one:
With preparing cyclohexane-n-hexane -5 parts of ethyl alcohol ternary system homogeneous phase solution, wherein component A content be respectively 12.0%,
20.0%, 40.0%, the 60.0% and 80.0% homogeneous phase solution M as multicomponent system to be measured.The Raman spectrum of homogeneous phase solution M is measured,
The spectral band 1100-1400cm that component response is concentrated by computer-1The spectrum point-by-point integration of corresponding wavelength point position, will
Integral spectrum is denoted as SPI；It calculates vector-space angle β of SPI and SJ, obtained in homogeneous phase solution M1 by calculating β/θ to quantitative group
The volume percent content of A is divided to be shown in Table 2, by the table 2 as it can be seen that the volume percent content value of the component A measured using this method
Compared with known content value, for relative error magnitudes between -2.00~+2.83%, accuracy rate is higher.
Embodiment two
The present embodiment two passes through a kind of component n-hexane in a kind of determining hexamethylene-n-hexane-ethyl alcohol ternary liquid phase system
Mass percent process, method proposed by the present invention is illustrated.
A method of multicomponent system component is directly determined using Raman spectrum, wherein multicomponent system be hexamethylene-just oneself
Alkane-ethyl alcohol ternary liquid phase system is n-hexane to quantitative component, method includes the following steps:
1. hexamethylene-n-hexane-ethyl alcohol ternary liquid phase the system for preparing serial known content is homogeneous in volumetric flask
Solution N: according to the percent by volume to quantitative component B n-hexane within the scope of 0-100% (8.0%, 16.0%, 30.0%, 50.0%,
70.0%, 90.0%) the homogeneous phase solution N of 6 samples is prepared, remaining component A hexamethylene, component C ethyl alcohol are constituted with random proportion；Again
Prepare hexamethylene-n-hexane-ethyl alcohol ternary system homogeneous phase solution M of unknown content.
It is popped one's head in using LR laser raman, measures pure solution, the known content of each component (hexamethylene, n-hexane, ethyl alcohol) respectively
Homogeneous phase solution N, unknown content homogeneous phase solution M Raman spectrum；
Fig. 1 is the Raman spectrogram of component A, B, C, spectrally has friendship with component A, C to quantitative component B as seen from the figure
It is folded, it is quantitative that peak can not be directlyed adopt.
Fig. 2 is mixed hexamethylene-n-hexane-ethyl alcohol ternary liquid phase system Raman spectrum, due to matching for remaining composition
Than random, so can not also directly obtain the concentration situation of change to quantitative component on the diagram.
2. to reduce calculation amount, the spectral band 1100-1400cm that the present invention selects component response to concentrate-1For calculating,
Such as Fig. 3, by computer respectively to the Raman of 6 samples, homogeneous phase solution M in the pure solution and homogeneous phase solution N of component A, B, C
Spectrum is converted to integral spectrum；The integral spectrum of wherein component B is denoted as SI, the matrix note that the integral spectrum of component A, C is constituted
For SJ, the integral spectrum of 6 sample homogeneous phase solution N is denoted as SBI, the integral spectrum of homogeneous phase solution M is denoted as SPI；
3. calculate separately vector-space angle θ, SBI and SJ vector-space angle α, SPI and SJ of SI and SJ to
Amount-space angle β；
3. -1 calibration measurement result: the percent by volume of component B in 6 sample homogeneous phase solution N is calculated to obtain by α/θ, with
Given value compares.For the result being calculated as shown in table 3 and Fig. 5, prediction result has good linear relationship and accuracy.
4. the volume of component B n-hexane in hexamethylene-n-hexane-ethyl alcohol ternary liquid phase system can be obtained by calculating β/θ
Degree.
In order to verify this method, present inventor has also made verification test to embodiment two:
With preparing cyclohexane-n-hexane -5 parts of ethyl alcohol ternary system homogeneous phase solution, wherein component B content be respectively 12.0%,
20.0%, 40.0%, the 60.0% and 80.0% homogeneous phase solution M as multicomponent system to be measured.The Raman spectrum of homogeneous phase solution M is measured,
The spectral band 1100-1400cm that component response is concentrated by computer-1The spectrum point-by-point integration of corresponding wavelength point position, will
Integral spectrum is denoted as SPI；Calculate SPI and SJ vector-space angle β, by β/θ calculate in homogeneous phase solution M2 to quantitative group
The percent by volume of B is divided to be shown in Table 4.By the table 4 as it can be seen that the volume percent content value of the component B measured using this method with
Know that content value is compared, for relative error magnitudes between -5.33~+2.80%, accuracy rate is higher.
The percent by volume predicted value of component A list compared with given value in the homogeneous phase solution N of table 1 --- embodiment one
The percent by volume predicted value of component A list compared with given value in the homogeneous phase solution M of table 2 --- embodiment one
The percent by volume predicted value of component B list compared with given value in the homogeneous phase solution N of table 3 --- embodiment two
The percent by volume predicted value of component B list compared with given value in the homogeneous phase solution M of table 4 --- embodiment two
Claims (4)
1. a kind of method for directly determining multicomponent system component using Raman spectrum, it is characterised in that: this method includes following step
It is rapid:
1. measuring Raman spectrum: measuring the pure solution of each component of multicomponent system to be measured, the polyploid to be measured of unknown content respectively
The Raman spectrum of the homogeneous phase solution M of system；
2. each Raman spectrum is converted to integral spectrum by computer；Wherein, the integral spectrum to quantitative component is denoted as SI,
The matrix that other components integral spectrum is constituted is denoted as SJ, and the integral spectrum of homogeneous phase solution M is denoted as SPI；
3. calculating separately vector-space angle θ, SPI and SJ vector-space angle β of SI and SJ；
4. obtaining the content in homogeneous phase solution M to quantitative component by calculating β/θ；
Step 1. in, also need measurement series for calibration known content multicomponent system to be measured homogeneous phase solution N Raman
Spectrum；Step 2. in, also by be used for demarcate homogeneous phase solution N spectrum be denoted as SBI；Step 3. in, also calculate separately SBI and
The vector of SJ-space angle α；And step 3. with step 4. between, further include having step 3. -1: calibration measurement result: logical
It crosses α/θ and calculates to obtain the content of component to be measured in homogeneous phase solution N, by the content and known content of component to be measured in homogeneous phase solution N
Compare, if error is larger, adjusts spectral wavelength point range, reduce the linear deviation degree of predicted value.
2. the method according to claim 1 for directly determining multicomponent system component using Raman spectrum, it is characterised in that:
Step 1. in, homogeneous phase solution N of the series for the multicomponent system to be measured of the known content of calibration is in system not split-phase
Content range in, prepare the homogeneous phase solution of serial known content.
3. the method according to claim 1 for directly determining multicomponent system component using Raman spectrum, it is characterised in that:
Step 1. in, measurement Raman spectrum be using LR laser raman pop one's head in, measure respectively each component of multicomponent system to be measured pure solution,
The Raman light of the homogeneous phase solution M of the multicomponent system to be measured of unknown content, the homogeneous phase solution N of the multicomponent system to be measured of known content
Spectrum.
4. the method according to claim 1 for directly determining multicomponent system component using Raman spectrum, it is characterised in that:
Step 2. in, by Raman spectrum be converted to integral spectrum be the Raman spectrum point-by-point integration that will be measured respectively, be converted to integral light
Spectrum.
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| CN102262054B (en) * | 2011-07-06 | 2014-05-28 | 广西工学院 | Combined spectrum pattern recognition method based on subspace coincidence judgment |
| CN103592251A (en) * | 2013-11-14 | 2014-02-19 | 广西科技大学 | Method for directly measuring potassium sorbate in soybean sauce |
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| CN104950060B (en) * | 2015-04-01 | 2016-10-26 | 广西科技大学 | Based on chromatograph-spectrogrph combination and the analysis method of the paeonol content of subspace angle criterion |
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