CN106323939A - Method for directly determining components in multicomponent system adopting raman spectrum - Google Patents
Method for directly determining components in multicomponent system adopting raman spectrum Download PDFInfo
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- CN106323939A CN106323939A CN201610667791.2A CN201610667791A CN106323939A CN 106323939 A CN106323939 A CN 106323939A CN 201610667791 A CN201610667791 A CN 201610667791A CN 106323939 A CN106323939 A CN 106323939A
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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]
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Abstract
The invention discloses a method for directly determining components in a multicomponent system adopting a raman spectrum, and relates to a measuring method of the components in the multicomponent system. The method comprises the steps that 1, the raman spectrums is measured, wherein the raman spectrum of a pure solution of each component in the multicomponent system to be tested and the raman spectrum of a homogeneous solution M of the unknown-content multicomponent system to be tested are respectively measured; 2, each raman spectrum is converted to an integral spectrum through a computer, wherein the integral spectrum of the component to be quantified is recorded as SI, the matrix formed by the integral spectrums of the other components is recorded as SJ, and the integral spectrum of the homogeneous solution M is recorded as SPI; 3, the vector quantity-space included angle theta between SI and SJ is calculated, and the vector quantity-space included angle beta between SPI and SJ is also calculated; 4, the content of the component to be quantified in the homogeneous solution M is obtained through calculating the ratio of beta and theta. According to the method, direct measurement of each phase in the multicomponent system can be realized conveniently, the operation is simple and the data is real, moreover, the method can be used for the phase equilibrium study on a liquid-liquid multicomponent system and process condition control of a series of separation unit operations such as extraction and rectification.
Description
Technical field
The present invention relates to the measuring method of a kind of multicomponent system component, particularly a kind of employing Raman spectrum directly determines many
The method of unit's system component.
Background technology
In Multiple liquid phase system, when balancing each other, the assay of each middle component mutually, is in chemical teaching and research
The drafting of common and important work, such as Multicomponent Phase Equilibria, extractant condition selection etc..Current existing method, or
Chromatography or use index of refraction and material component relationship or utilize system turbidity change etc. to characterize after using sampling, this
There is complex operation or the shortcoming such as accuracy is low in a little methods；Additionally due to the sensitivity balanced each other, the contact operation such as sampling can
Interference can balance each other, thus affect the verity of data.
Summary of the invention
The technical problem to be solved in the present invention is: provide a kind of side using Raman spectrum directly to determine multicomponent system component
Method, to solve, the aforesaid operations of prior art existence is loaded down with trivial details, accuracy is low, affect the weak point of data validity.
The technical scheme solving above-mentioned technical problem is: a kind of side using Raman spectrum directly to determine multicomponent system component
Method, the method comprises the following steps:
1. Raman spectrum is measured: measure 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. by computer, each Raman spectrum is converted to integration spectrum；Wherein, the integration spectrum treating quantitative component is designated as SI,
The matrix that other component integration spectrum is constituted is designated as the integration spectrum of SJ, homogeneous phase solution M and is designated as SPI；
Vector-space angle the β of the vector of calculating SI and SJ-space angle θ, SPI and SJ the most respectively；
4. the content treating quantitative component in homogeneous phase solution M is obtained by calculating β/θ.
The further technical scheme of the present invention is: step 1. in, also need to measure series for the known content demarcated
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 designated as
SBI；Step 3. in, the most respectively calculate SBI and SJ vector-space angle α；And step 3. and step 4. between, also
Include step 3.-1: demarcate measurement result: calculate the content of component to be measured in homogeneous phase solution N by α/θ, this all mixed
In liquid N, the content of component to be measured compares with known content, if error is relatively big, adjusts spectral wavelength point range, reduces predictive value
Linear deviation degree.
The further technical scheme of the present invention is: step 1. in, described series is for the known content demarcated
The homogeneous phase solution N of multicomponent system to be measured, is in the content range of system not split-phase, all mixing of preparation series known content
Liquid.
The further technical scheme of the present invention is: step 1. in, measure Raman spectrum be use LR laser raman probe, point
Do not measure the pure solution of each component of multicomponent system to be measured, unknown the homogeneous phase solution M of multicomponent system to be measured of content, known content
The Raman spectrum of homogeneous phase solution N of multicomponent system to be measured.
The further technical scheme of the present invention is: step 2. in, it is respectively that Raman spectrum is converted to integration spectrum
The Raman spectrum point-by-point integration that will record, is converted to integration spectrum.
Owing to using said structure, the employing Raman spectrum of the present invention directly determines that the method for multicomponent system component is with existing
Technology is compared, and has the advantages that
1. can conveniently realize the direct mensuration of each phase of multicomponent system
Owing to the present invention includes that 1. step measures Raman spectrum；2. by computer, Raman spectrum is converted to integration spectrum；Its
In, the integration spectrum treating quantitative component is designated as SI, the matrix that other component integration spectrum is constituted is designated as SJ, treating of unknown content
The integration spectrum of the homogeneous phase solution M surveying multicomponent system is designated as SPI；Calculate the most respectively SI and SJ vector-space angle θ, SPI and
The vector of SJ-space angle β；4. the content treating quantitative component in homogeneous phase solution M is calculated by β/θ.Therefore, the present invention be
On the premise of system composition determines, utilize the feature of Raman spectrum non-cpntact measurement, by the space-vectorial angle of spectrum, directly
The quantitatively content of component, can conveniently realize the direct mensuration of each phase of multicomponent system.
The most easy and simple to handle, can easily and accurately carry out quantitatively
Due to the multicomponent system for determining composition, the present invention is without modeling and complicated demarcation, easy and simple to handle, can facilitate accurately
Ground is carried out quantitatively.
3. can ensure data validity
Owing to the present invention uses non-cpntact measurement, system will not be produced interference, thus ensure that the verity of data, it is accurate
Rate is higher, and the dynamic system research for actual chemistry and chemical industry provides great convenience.
The most 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 operations such as extraction, rectification
Process regulation.
Below, the method in conjunction with the accompanying drawings and embodiments the employing Raman spectrum of the present invention directly being determined multicomponent system component
Technical characteristic be further described.
Accompanying drawing explanation
Component A, the Raman spectrogram of B, C in Fig. 1: embodiment one, two；
The Raman spectrogram of the ternary system of mixing in Fig. 2: embodiment one, two；
Fig. 3: embodiment one, two medium wave band is 1100-1400cm-1Component A, the Raman spectrogram of B, C；
Component A volumn concentration and the graph of a relation of angle value in Fig. 4: embodiment one.
Component B volumn concentration and the graph of a relation of angle value in Fig. 5: embodiment two.
Detailed description of the invention
A kind of method using Raman spectrum directly to determine multicomponent system component, the method comprises the following steps:
1. measuring Raman spectrum: in the content range of multicomponent system not split-phase, in volumetric flask or conical flask, preparation the unknown contains
The homogeneous phase solution M of the multicomponent system to be measured of amount, the homogeneous phase solution N of the multicomponent system to be measured of preparation series known content, all mix
Liquid N is used for the data scaling that predicts the outcome；Employing LR laser raman is popped one's head in, and measures the pure molten of each component of multicomponent system to be measured respectively
Liquid, the unknown homogeneous phase solution M of multicomponent system to be measured of content, the Raman of homogeneous phase solution N of multicomponent system to be measured of known content
Spectrum；
2. by computer, each Raman spectrum is converted to integration spectrum；Wherein, the integration spectrum treating quantitative component is designated as SI,
The matrix that the integration spectrum of other components is constituted is designated as the integration spectrum of SJ, homogeneous phase solution M and is designated as SPI；Also will be used for demarcation
The integration spectrum of homogeneous phase solution N is designated as SBI；
Calculate the most respectively the vector of the vector of the vector-space angle θ, SBI and SJ of SI and SJ-space angle α, SPI and SJ-
Space angle β；
3.-1: demarcate measurement result: calculate the content of component to be measured in homogeneous phase solution N by α/θ, by this homogeneous phase solution N
The content of component to be measured compares with known content, if error is relatively big, adjusts spectral wavelength point range, reduces the linear of predictive value
Departure degree；
4. the content treating quantitative component in homogeneous phase solution M is calculated by β/θ.
The following is the specific embodiment of the present invention:
Embodiment one
The present embodiment one is determined by the body of a kind of component hexamethylene in a kind of hexamethylene-normal hexane-ethanol ternary liquid phase system
The process of long-pending percentage ratio, the method proposing the present invention illustrates.
A kind of method using Raman spectrum directly to determine multicomponent system component, wherein, multicomponent system be hexamethylene-just oneself
The ternary liquid phase system of alkane-ethanol, treats that quantitative component is hexamethylene, and the method comprises the following steps:
1. in volumetric flask, the homogeneous phase solution of the ternary liquid phase system of the hexamethylene-normal hexane-ethanol of preparation series known content
N: according to treat the percent by volume of quantitative component A hexamethylene in the range of 0-100% (8.0%, 16.0%, 30.0%, 50.0%,
70.0%, 90.0%) preparing the homogeneous phase solution N of 6 samples, remaining component B normal hexane, component C ethanol are constituted with random proportioning；Again
The homogeneous phase solution M of the hexamethylene-normal hexane-ethanol ternary system of the unknown content of preparation.
Employing LR laser raman is popped one's head in, and measures the pure solution of each component (hexamethylene, normal hexane, ethanol), known content respectively
Homogeneous phase solution N, the Raman spectrum of homogeneous phase solution M of unknown content；
Fig. 1 is the Raman spectrogram of component A, B, C, treats that quantitative component A spectrally has overlapping with component B, C as seen from the figure,
Cannot directly use peak quantitative.
Fig. 2 is the ternary liquid phase system Raman spectrum of the hexamethylene-normal hexane-ethanol of mixing, due to joining that remaining forms
Than random, so the concentration change situation treating quantitative component also cannot be directly obtained on figure.
2. for reducing amount of calculation, the present invention selects the spectral band 1100-1400cm that component response is concentrated-1For calculating,
Such as Fig. 3, by computer respectively to 6 samples, the Ramans of homogeneous phase solution M in component A, the pure solution of B, C and homogeneous phase solution N
Spectrum is converted to integration spectrum；The integration spectrum of wherein component A is designated as SI, the matrix note that component B, the integration spectrum of C are constituted
For SJ, the integration spectrum of 6 sample homogeneous phase solution N is designated as SBI, the integration spectrum of homogeneous phase solution M is designated as SPI；
Calculate the most respectively the vector of the vector of the vector-space angle θ, SBI and SJ of SI and SJ-space angle α, SPI and SJ-
Space angle β；
3.-1 measurement result is demarcated: calculate the percent by volume of component A in 6 sample homogeneous phase solution N by α/θ, with known
Value compares.Calculated result is as shown in table 1 and Fig. 4, it was predicted that result has good linear relationship and accuracy.
4. by calculate β/θ the volume of component A hexamethylene in hexamethylene-normal hexane-ethanol ternary liquid phase system
Degree.
In order to verify this method, embodiment one has also been made checking and has been tested by present inventor:
Preparation hexamethylene-normal hexane-ethanol ternary system homogeneous phase solution 5 parts, wherein component A content be respectively 12.0%, 20.0%,
40.0%, 60.0% and 80.0% as the homogeneous phase solution M of multicomponent system to be measured.Measure the Raman spectrum of homogeneous phase solution M, by meter
The spectral band 1100-1400cm that component response is concentrated by calculation machine-1The spectrum point-by-point integration of corresponding wavelength point position, by integral light
Spectrum is designated as SPI；Calculate the vector-space angle β of SPI and SJ, obtained by calculating β/θ and homogeneous phase solution M1 treats quantitative component A
Volume percent content is shown in Table 2, and from this table 2, the volume percent content value of component A that employing this method records is with known
Content value is compared, and relative error magnitudes is between-2.00～+2.83%, and its accuracy rate is higher.
Embodiment two
The present embodiment two is determined by the matter of a kind of component normal hexane in a kind of hexamethylene-normal hexane-ethanol ternary liquid phase system
The process of amount percentage ratio, the method proposing the present invention illustrates.
A kind of method using Raman spectrum directly to determine multicomponent system component, wherein, multicomponent system be hexamethylene-just oneself
The ternary liquid phase system of alkane-ethanol, treats that quantitative component is normal hexane, and the method comprises the following steps:
1. in volumetric flask, the homogeneous phase solution of the ternary liquid phase system of the hexamethylene-normal hexane-ethanol of preparation series known content
N: according to treat the percent by volume of quantitative component B normal hexane in the range of 0-100% (8.0%, 16.0%, 30.0%, 50.0%,
70.0%, 90.0%) preparing the homogeneous phase solution N of 6 samples, remaining component A hexamethylene, component C ethanol are constituted with random proportioning；Again
The homogeneous phase solution M of the hexamethylene-normal hexane-ethanol ternary system of the unknown content of preparation.
Employing LR laser raman is popped one's head in, and measures the pure solution of each component (hexamethylene, normal hexane, ethanol), known content respectively
Homogeneous phase solution N, the Raman spectrum of homogeneous phase solution M of unknown content；
Fig. 1 is the Raman spectrogram of component A, B, C, treats that quantitative component B spectrally has overlapping with component A, C as seen from the figure,
Cannot directly use peak quantitative.
Fig. 2 is the ternary liquid phase system Raman spectrum of the hexamethylene-normal hexane-ethanol of mixing, due to joining that remaining forms
Than random, so the concentration change situation treating quantitative component also cannot be directly obtained on figure.
2. for reducing amount of calculation, the present invention selects the spectral band 1100-1400cm that component response is concentrated-1For calculating,
Such as Fig. 3, by computer respectively to 6 samples, the Ramans of homogeneous phase solution M in component A, the pure solution of B, C and homogeneous phase solution N
Spectrum is converted to integration spectrum；The integration spectrum of wherein component B is designated as SI, the matrix note that component A, the integration spectrum of C are constituted
For SJ, the integration spectrum of 6 sample homogeneous phase solution N is designated as SBI, the integration spectrum of homogeneous phase solution M is designated as SPI；
Calculate the most respectively the vector of the vector of the vector-space angle θ, SBI and SJ of SI and SJ-space angle α, SPI and SJ-
Space angle β；
3.-1 measurement result is demarcated: calculate the percent by volume of component B in 6 sample homogeneous phase solution N by α/θ, with known
Value compares.Calculated result is as shown in table 3 and Fig. 5, it was predicted that result has good linear relationship and accuracy.
4. by calculate β/θ the volume of component B normal hexane in hexamethylene-normal hexane-ethanol ternary liquid phase system
Degree.
In order to verify this method, embodiment two has also been made checking and has been tested by present inventor:
Preparation hexamethylene-normal hexane-ethanol ternary system homogeneous phase solution 5 parts, wherein component B content be respectively 12.0%, 20.0%,
40.0%, 60.0% and 80.0% as the homogeneous phase solution M of multicomponent system to be measured.Measure the Raman spectrum of homogeneous phase solution M, by meter
The spectral band 1100-1400cm that component response is concentrated by calculation machine-1The spectrum point-by-point integration of corresponding wavelength point position, by integral light
Spectrum is designated as SPI；Calculate the vector-space angle β of SPI and SJ, calculated by β/θ and homogeneous phase solution M2 treats quantitative component B
Percent by volume is shown in Table 4.From this table 4, the volume percent content value of component B that employing this method records and known content
Value is compared, and relative error magnitudes is between-5.33～+2.80%, and its accuracy rate is higher.
In the homogeneous phase solution N of table 1 embodiment one, the percent by volume predictive value of component A compares catalog with given value
In the homogeneous phase solution M of table 2 embodiment one, the percent by volume predictive value of component A compares catalog with given value
In the homogeneous phase solution N of table 3 embodiment two, the percent by volume predictive value of component B compares catalog with given value
In the homogeneous phase solution M of table 4 embodiment two, the percent by volume predictive value of component B compares catalog with given value
Claims (5)
1. one kind uses the method that Raman spectrum directly determines multicomponent system component, it is characterised in that: the method includes following step
Rapid:
1. Raman spectrum is measured: measure 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. by computer, each Raman spectrum is converted to integration spectrum；Wherein, the integration spectrum treating quantitative component is designated as SI,
The matrix that other component integration spectrum is constituted is designated as the integration spectrum of SJ, homogeneous phase solution M and is designated as SPI；
Vector-space angle the β of the vector of calculating SI and SJ-space angle θ, SPI and SJ the most respectively；
4. the content treating quantitative component in homogeneous phase solution M is obtained by calculating β/θ.
The method that employing Raman spectrum the most according to claim 1 directly determines multicomponent system component, it is characterised in that:
Step 1. in, also need to measure the Raman spectrum of homogeneous phase solution N of the series multicomponent system to be measured of known content for demarcating；?
Step 2. in, also by be used for demarcate homogeneous phase solution N spectrum be designated as SBI；Step 3. in, the most respectively calculate SBI and SJ to
Amount-space angle α；And step 3. and step 4. between, also include step 3.-1: demarcate measurement result: counted by α/θ
Calculate to obtain the content of component to be measured in homogeneous phase solution N, the content of component to be measured in this homogeneous phase solution N is compared with known content, as
Really error is relatively big, adjusts spectral wavelength point range, reduces the linear deviation degree of predictive value.
The method that employing Raman spectrum the most according to claim 2 directly determines multicomponent system component, it is characterised in that:
Step 1. in, the homogeneous phase solution N of multicomponent system to be measured of the described series known content for demarcating, is in system not split-phase
Content range in, preparation series known content homogeneous phase solution.
The method that employing Raman spectrum the most according to claim 2 directly determines multicomponent system component, it is characterised in that:
Step 1. in, measure Raman spectrum be use LR laser raman probe, measure respectively each component of multicomponent system to be measured pure solution,
The unknown homogeneous phase solution M of multicomponent system to be measured of content, the Raman light of homogeneous phase solution N of multicomponent system to be measured of known content
Spectrum.
The method that employing Raman spectrum the most according to claim 2 directly determines multicomponent system component, it is characterised in that:
Step 2. in, it is the Raman spectrum point-by-point integration that will record respectively that Raman spectrum is converted to integration spectrum, is converted to integral light
Spectrum.
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