CN103018393B - Method for measuring content of components in mixed dye solution - Google Patents

Method for measuring content of components in mixed dye solution Download PDF

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CN103018393B
CN103018393B CN201210523883.5A CN201210523883A CN103018393B CN 103018393 B CN103018393 B CN 103018393B CN 201210523883 A CN201210523883 A CN 201210523883A CN 103018393 B CN103018393 B CN 103018393B
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component
data
dye solution
mixed dye
value
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CN103018393A (en
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葛军
姚志湘
粟晖
刘柳
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Guangxi University of Science and Technology
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Guangxi University of Science and Technology
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Abstract

The invention discloses a method for measuring the content of components in a mixed dye solution and relates to the method for measuring the dye components. The method comprises the steps as follows: obtaining a linear equation of sample application amount and SKS value of a single component of a dye by using the single-component sample dye firstly, applying the mixed dye solution to be measured onto a silicon rubber plate, scanning and collecting data by adopting a multi-wavelength thin layer scanner, and carrying out signal separation and analysis on the collected data in combination with an oblique projection operator on an Matlab platform to finish quantitative analysis of the measured component in the mixed dye solution. According to the method, the mixed dye solution to be measured does not need to be developed in a developing solvent, the developing solvent is not required, the cost is saved, the collected data is rich, the quantitative analysis error is small, and the measured component is convenient and quick to analyze.

Description

The assay method of component concentration in a kind of mixed dye solution
Technical field
The present invention relates to a kind of assay method of dye component, particularly a kind of utilization does not launch the assay method that multi-wavelength thin layer scanning is measured the content of tested component in mixed dye simultaneously.
Background technology
In dye liquor, dye strength variable effect is to the variation of dyeing course dyestuff dye-uptake, and then has influence on Color.Real-Time Monitoring to dyeing course dye liquor concentration, reflects colored state in time, to formulate more rational workflow and formula.There is no at present the method for real-time of dye strength in dye liquor, this is also that the textile difficulty that precisely dyes has the one of the main reasons of breakthrough for many years.
In mixed dye solution, the assay method of concentration of component mainly contains spectrophotometric method, thin-layer developing scanning method, high performance liquid chromatography etc.Thin-layer chromatography (Thin Layer Chromatography, TLC) is a kind of quick, easy, efficient, economic, widely used chromatogram analysis method.TLC application is more because thin-layer chromatography has advantages of cheapness, quick, micro-, sensitive and easy and simple to handle.For the research of the thin-layer chromatography of mixed dye, external existing many reports, from the initial stage in the sixties, are just applied to thin-layer chromatography the analysis of synthetic dyestuffs abroad.Traditional thin layer chromatography quantitative analysis be mainly by potpourri point sample on silica gel plate, through developping agent, launch, the measured object spot launching is carried out to scanning analysis with single wavelength or dual-wavelength lamellar scanning instrument.Then traditional thin layer scanning need to be separated the tested component in potpourri completely measured matter is carried out to thin layer scanning quantitative test, a difficult point that is selected to traditional thin layer quantitative test of developping agent; Adopt the thin layer scanning of single wavelength or dual wavelength to collect the less quantitative test error that caused of data message amount larger.
The nonoverlapping mensuration of absorption spectrum between the applicable tested component of spectrophotometric method is larger for recording error in the overlapped situation of each component absorption spectrum.There is long, the shortcoming such as instrument is expensive, analysis cost is higher analysis time in high performance liquid chromatography, in mixed dye solution analysis, is subject to certain restrictions.
Summary of the invention
The technical problem to be solved in the present invention is: provide that a kind of accuracy is high, cost is low, conveniently mixed dye solution does not launch multi-wavelength thin layer chromatography quantitative analysis method.
The technical scheme solving the problems of the technologies described above is: the assay method of component concentration in a kind of mixed dye solution, is characterized in that: comprise the following steps:
A. make the linear equation of each one-component point sample amount of dyestuff and SKS value:
A1. each one-component standard dyes solution of preparing variable concentrations: each one-component dyestuff is mixed with to variable concentrations b 1, b 2, b 3... b yone-component standard dyes solution;
A2. obtain the spectroscopic data of each one-component standard dyes solution: each one-component standard dyes solution point sample preparing in steps A 1, on silica gel plate, with the scanning of multi-wavelength thin-layer chromatogram scanner, is gathered to the spectroscopic data of each one-component dyestuff;
A3. translation data form: the spectroscopic data of each one-component dyestuff gathering in above-mentioned steps A2 is become to KS function data by the Data Format Transform of light intensity;
A4. the SKS value of suing for peace to obtain: the KS value summation by under each wavelength of gained in steps A 3, obtains SKS value;
A5. make the linear equation of point sample amount and the SKS value of each one-component of dyestuff: according to the point sample amount of each one-component dyestuff and SKS value, make the point sample amount of each one-component of dyestuff and the linear equation of SKS value; This linear equation is y=ax+b, and wherein, x is point sample amount, and y is SKS value, and a and b are constant.
B. the mensuration of each one-component content in mixed dye solution:
B1. obtain the spectroscopic data of mixed dye solution: by mixed dye solution point sample on silica gel plate, application multi-wavelength thin-layer chromatogram scanner scanning mixed dye solution, the light intensity data that scanning is preserved converts KS function data to, and the data after conversion are as the spectroscopic data Z of mixed dye solution;
B2. obtain background spectrum data and the spectroscopic data of each one-component: by the KS function data mapping of each one-component dyestuff obtaining in steps A 3, obtain the background spectrum data Y of each one-component dyestuff and the spectroscopic data X of each one-component dyestuff;
B3. calculate the SKS value of each one-component in mixed dye solution: in conjunction with oblique projection operator, the data that gather are carried out to signal compartment analysis, the spectroscopic data X of gained in the spectroscopic data Z of gained in step B1 and step B2 and background spectrum data Y are imported in oblique projection Operators Algorithm program, calculate the SKS value of each one-component in mixed dye solution;
B4. calculate the content of each one-component in mixed dye solution: the content of each one-component in mixed dye will be tried to achieve in the point sample amount of resulting each one-component of dyestuff and the linear equation of SKS value in the SKS value substitution steps A respectively of each one-component in the mixed dye solution obtaining in step B3.
Further technical scheme of the present invention is: each one-component standard dyes solution of preparing variable concentrations described in steps A 1 is: to containing measured object component a 1and a 2mixed dye solution, will only contain tested component a respectively 1or a 2one-component dyestuff be mixed with variable concentrations b 1, b 2, b 3, b 4, b 5one-component standard dyes solution.
The spectroscopic data that obtains mixed dye solution described in step B1 is: will contain tested component a 1and a 2mixed dye solution I point sample on silica gel plate, application multi-wavelength thin-layer chromatogram scanner scans the spectroscopic data Z that mixed dye solution I to be measured obtains mixed dye solution i.
The spectroscopic data of the background extraction spectroscopic data described in step B2 and tested component is: tested component a 1background spectrum data Y 2with tested component a 2background spectrum data Y 1, obtain tested component a 1spectroscopic data X 1with tested component a 2spectroscopic data X 2.
The background spectrum data Y of each one-component dyestuff described in step B2 refers to the spectroscopic data that does not contain tested component in selected spectroscopic data.
The obtaining step of the background spectrum data Y of each one-component dyestuff described in step B2 is: to the KS value mapping under the respective wavelength in the KS function data of the arbitrary one-component beyond tested component, choose the data of those row of peak on figure as the background spectrum data Y of tested component, this column data does not contain tested component.
The spectroscopic data X of each one-component dyestuff described in step B2 refers to the spectroscopic data that only contains tested component in selected spectroscopic data and do not contain other components.
the obtaining step of the spectroscopic data X of each one-component dyestuff described in step B2 is: to the KS value mapping under the respective wavelength in the KS function data of tested component, on figure the tested component purity of the data representation of those row of peak the highest, do not contain other components, choose this column data as tested component spectra data X.
Steps A 3 with described in step B1, convert KS function data to for application KS=(ones(sizeab)-Refe) .^2./(2*Refe) becomes spectroscopic data the data layout of KS functional form by the Data Format Transform of light intensity, wherein, the reflective light intensity data of Refe for adopting multi-wavelength scanning instrument to gather; Sizeab is the dimension from the data of the reflective light intensity data acquisition of collection according to the absorbing wavelength of tested component; It is 1 matrix that ones helps the reflective light intensity data-switching of collection according to absorbing wavelength scope.
Oblique projection operator described in step B3 is E s|H=S(S tp h s) -1s tp h , P h =I-P h=I-H(H th) -1h t, wherein, subscript T represents transpose of a matrix; I is and P hthe unit matrix that dimension is identical; E s|Hfor oblique projection operator; S is the subspace that the vector of measured variable is opened; The adjacent subspace of H for not opening containing the vector of measured variable; P hfor the projection operator along subspace H to subspace S.
Owing to adopting technique scheme, in a kind of mixed dye solution of the present invention, the assay method of component concentration is compared with the assay method of concentration of component in existing mixed dye solution, has following beneficial effect:
1. quantitative test error is little, accuracy is high:
The present invention directly by mixed dye solution point sample to be measured on silica gel plate, application multi-wavelength thin-layer chromatogram scanner carries out thin layer scanning acquisition scans data to the mixed dye spot to be measured not launching, the data that gather are carried out data computing to obtain the content of tested component in mixed dye to be measured in conjunction with oblique projection operator basic theories and the application in signal separation thereof on Matlab platform, complete the quantitative test of tested component in mixed dye solution, the data volume gathering is abundant, each component absorption spectrum is without overlapped phenomenon, quantitative test error of the present invention is little, accuracy is high.
2. cost is low, convenient and swift:
The present invention adopts multi-wavelength thin-layer chromatogram scanner directly to carry out scanning collection data to mixed dye solution to be measured, and then by data computing to obtain the content of tested component in mixed dye to be measured, without mixed dye solution to be measured is launched in developping agent, having solved needs in classic method that the tested component in potpourri is separated to rear ability completely and measured matter is carried out to the problem of thin layer scanning quantitative test, the data that record are accurate compared with the result of the tlc analysis of classic method, this method is convenient for thin layer quantitative test simultaneously, fast, the present invention is without developping agent, shortened analysis time, saved cost.
Method simple, be convenient to promote the use of:
The present invention first prepares the linear equation of dyestuff one-component concentration and SKS with pure sample product dye liquor, with multi-wavelength thin-layer chromatogram scanner, mixed dye solution to be measured is directly carried out to scanning collection data again, carry out the quantitative test that data computing completes tested component in mixed dye solution, without the long complex operations of process, the present invention can in printing and dyeing industry for the fast quantitative analysis of dye solution, method is simple, easy to operate, is convenient to promote the use of.
Below, in conjunction with Figure of description and specific embodiment, the technical characterictic of the assay method of component concentration in a kind of mixed dye solution of the present invention is further described.
accompanying drawing explanation:
Fig. 1: flow chart of steps of the present invention,
Fig. 2: the oblique projection schematic diagram in the present invention,
Fig. 3: the spectrogram of the cationic yellow X-5GL in the present embodiment,
Fig. 4: the spectrogram of the cationic yellow x-8gl in the present embodiment.
In Fig. 2, each label is: 1-measured object spectrum, 2-oblique projection output, 3-biased sample spectrum.
Horizontal ordinate in Fig. 3 and Fig. 4 represents that wavelength (nm), ordinate represent absorbance, is 1. the spectrogram of cationic yellow X-5GL, is 2. the spectrogram of cationic yellow x-8gl.
embodiment:
The assay method of component concentration in a kind of mixed dye solution, in described mixed dye solution, contain cationic yellow X-5GL and cationic yellow x-8gl, the content that now needs to measure respectively cationic yellow X-5GL and cationic yellow x-8gl in mixed dye solution, comprises the following steps:
A. make the linear equation of each one-component point sample amount of dyestuff and SKS value:
A1. each one-component standard dyes solution of preparing variable concentrations:
A11. accurately take the cationic yellow X-5GL of 0.1250g, after dissolving with distilled water, move in 250mL volumetric flask, use distilled water constant volume, being mixed with concentration is the cationic yellow X-5GL standard mother liquor of 0.5g/L, accurately pipette cationic yellow X-5GL standard mother liquor 2.0mL, 4.0mL, 6.0mL, 8.0mL, 10.0mL and be placed in respectively 10mL volumetric flask, use distilled water constant volume, being mixed with respectively concentration is the one-component standard dyes solution of the cationic yellow X-5GL of 0.1g/L, 0.2g/L, 0.3g/L, 0.4g/L, 0.5g/L.
A12. accurately take the cationic yellow x-8gl of 0.1250g, after dissolving with distilled water, move in 250mL volumetric flask, use distilled water constant volume, being mixed with concentration is the cationic yellow x-8gl standard mother liquor of 0.5g/L, accurately pipette cationic yellow x-8gl standard mother liquor 2.0mL, 4.0mL, 6.0mL, 8.0mL, 10.0mL and be placed in respectively 10mL volumetric flask, use distilled water constant volume, being mixed with respectively concentration is the one-component standard dyes solution of the cationic yellow x-8gl of 0.1g/L, 0.2g/L, 0.3g/L, 0.4g/L, 0.5g/L.
A2. obtain the spectroscopic data of each one-component standard dyes solution:
A21. prepare multi-wavelength thin-layer chromatogram scanner: this multi-wavelength thin-layer chromatogram scanner comprises light source, fibre-optical probe, spectrometer, electric displacement platform, and the parameter that multi-wavelength thin-layer chromatogram scanner is set is: the spectrum integral time is that 50ms, average time are 4, scanning integration interval time 200ms, sweep velocity are 200step/s.
A22. with microsyringe respectively in removing step A11 the concentration of gained be that the one-component standard solution 5uL point sample of cationic yellow X-5GL of 0.1g/L, 0.2g/L, 0.3g/L, 0.4g/L, 0.5g/L is on G type high-efficient silica gel plate, dry and form point sample spot, multi-wavelength thin-layer chromatogram scanner fibre-optical probe is placed in and on the point sample spot of cationic yellow X-5GL on G type high-efficient silica gel plate, carries out " bow " shape two-dimensional movement mode and scan, obtain the spectroscopic data of cationic yellow X-5GL, determine absorbing wavelength scope, referring to Fig. 3.
A23. with microsyringe respectively in removing step A12 the concentration of gained be that the one-component standard solution 5uL point sample of cationic yellow x-8gl of 0.1g/L, 0.2g/L, 0.3g/L, 0.4g/L, 0.5g/L is on G type high-efficient silica gel plate, dry and form point sample spot, multi-wavelength thin-layer chromatogram scanner fibre-optical probe is placed in and on the point sample spot of cationic yellow x-8gl on G type high-efficient silica gel plate, carries out " bow " shape two-dimensional movement mode and scan, obtain the spectroscopic data of cationic yellow x-8gl, determine absorbing wavelength scope, referring to Fig. 4.
Wherein, in the above-mentioned data that obtain with the scanning of multi-wavelength thin-layer chromatogram scanner, some data is clear datas, according to wavelength coverage, can in scan-data, select needed data, and data volume just reduces calculated amount is reduced like this.
A3. translation data form:
A31. the data layout that the spectroscopic data gathering in above-mentioned steps A2 is light intensity, application KS=(ones(sizeab)-Refe) .^2./(2*Refe) spectroscopic data of the cationic yellow X-5GL gathering in steps A 22 is converted to the data layout of KS functional form, obtains the KS value of cationic yellow X-5GL.
A32. the data layout that the spectroscopic data gathering in above-mentioned steps A2 is light intensity, application KS=(ones(sizeab)-Refe) .^2./(2*Refe) spectroscopic data of the cationic yellow x-8gl gathering in steps A 22 is converted to the data layout of KS functional form, obtains the KS value of cationic yellow x-8gl.
Described KS=(ones(sizeab)-Refe) in .^2./(2*Refe): the reflective light intensity data of Refe for adopting multi-wavelength scanning instrument to gather; Sizeab is the dimension from the data of the reflective light intensity data acquisition of collection according to the absorbing wavelength of tested component; It is 1 matrix that ones helps the reflective light intensity data-switching of collection according to absorbing wavelength scope.
A4. the SKS value of suing for peace to obtain:
A41. apply the SKS value that sum (sum (KS)) tries to achieve cationic yellow X-5GL point sample spot, the soon KS value summation of the cationic yellow X-5GL under each wavelength of gained in steps A 31, try to achieve the SKS value of the point sample amount of each point sample spot of cationic yellow X-5GL, referring to table 1.
A42. apply the SKS value that sum (sum (KS)) tries to achieve cationic yellow x-8gl point sample spot, the soon KS value summation of the cationic yellow x-8gl under each wavelength of gained in steps A 32, the SKS value of the point sample amount of each point sample spot of cationic yellow x-8gl, referring to table 1.
A5. make the linear equation of point sample amount and the SKS value of each one-component of dyestuff:
A51. according to the different point sample amounts of the one-component standard solution of cationic yellow X-5GL and the SKS value of the cationic yellow X-5GL trying to achieve, do the linear equation of point sample amount and the SKS value of cationic yellow X-5GL, this linear equation is y=ax+b, referring to table 2.
A52. according to the different point sample amounts of the one-component standard solution of cationic yellow x-8gl and the SKS value of the cationic yellow x-8gl of trying to achieve, do the linear equation of point sample amount and the SKS value of cationic yellow x-8gl, this linear equation is y=ax+b, referring to table 2.
In described this linear equation y=ax+b: x is point sample amount, y is SKS value, and a and b are constant.
B. the mensuration of each one-component content in mixed dye solution:
B1. obtain the spectroscopic data of mixed dye solution:
For effect and the accuracy of the quantitative test of the quantitative analysis method that adopts in can more effective explanation the present invention, the mixed dye solution in the present embodiment be the mixed dye solution of known each component theoretical content value of oneself preparing.
B11. the preparation of mixed dye solution I: accurately pipette concentration and be the cationic yellow X-5GL standard mother liquor 5mL of 0.5g/L and cationic yellow x-8gl standard mother liquor 4mL that concentration is 0.5g/L in 10mL volumetric flask, use distilled water constant volume, the concentration of cationic yellow X-5GL after constant volume is that the concentration of 0.25g/L, cationic yellow x-8gl is 0.20g/L, stores and uses as mixed dye solution I.
B12. the preparation of mixed dye solution II: accurately pipette concentration and be the cationic yellow X-5GL standard mother liquor 4mL of 0.5g/L and cationic yellow x-8gl standard mother liquor 5mL that concentration is 0.5g/L in 10mL volumetric flask, use distilled water constant volume, the concentration of cationic yellow X-5GL after constant volume is that the concentration of 0.20g/L, cationic yellow x-8gl is 0.25g/L, stores and uses as mixed dye solution II.
B13. obtaining of the spectroscopic data of mixed dye solution I and mixed dye solution II: the mixed dye solution I preparing and mixed dye solution II are pipetted respectively to 5uL point sample on G type high-efficient silica gel plate with microsyringe, dry and form point sample spot, point sample spot on G type high-efficient silica gel plate is placed under fibre-optical probe, set thin layer scanning parameter, with fibre-optical probe, point sample spot is carried out to the scanning of " bow " type, preserve the data of scanning collection, the data of preservation are applied on matlab platform to KS=(ones (sizeab)-Refe) .^2./(2*Refe) data-switching of light intensity the is become data of KS function, data after conversion are as the spectroscopic data of mixed dye solution, after conversion, obtain the spectroscopic data Z of mixed dye solution I i, mixed dye solution II spectrum count Z iI.
B2. obtain background spectrum data and the spectroscopic data of surveying each one-component in mixed dye solution I or mixed dye solution II:
The background spectrum data of each one-component refer to the spectroscopic data that does not contain tested component, as the content that need to survey cationic yellow X-5GL in mixed dye solution I or mixed dye solution II only need be by the spectroscopic data of cationic yellow x-8gl spectroscopic data as a setting, as the content that need to survey cationic yellow x-8gl in mixed dye solution I or mixed dye solution II only need be by the spectroscopic data of cationic yellow X-5GL spectroscopic data as a setting.
The spectroscopic data of each one-component refers to the spectroscopic data that only contains the spectroscopic data of tested component in selected spectroscopic data and do not contain other components.
B21. the background spectrum data Y of cationic yellow X-5GL (X-8GL)obtain: by the KS value of the cationic yellow x-8gl of gained in steps A 32, what the data mapping in KS value was obtained is the spectral curve of cationic yellow x-8gl, on figure, peak row mean and do not contain component cationic yellow X-5GL, select the data of these row as the data Y of the background spectrum of cationic yellow X-5GL (X-8GL).
B22. the spectroscopic data X of cationic yellow X-5GL (X-5GL)obtain: by the KS value of the cationic yellow X-5GL obtaining in A31, what the data mapping in KS value was obtained is the wavelength of cationic yellow X-5GL and the spectral curve of KS value, on figure corresponding peak row mean component cationic yellow X-5GL the purest, do not contain component cationic yellow x-8gl, the data of these row are selected the spectroscopic data X as cationic yellow X-5GL (X-5GL).
B23. the background spectrum data Y of cationic yellow x-8gl (X-5GL)obtain: adopt the same procedure with step B21, the KS value of the cationic yellow X-5GL obtaining in A31 mapped and obtained the background spectrum data Y of cationic yellow x-8gl (X-5GL).
B24. the spectroscopic data X of cationic yellow x-8gl (X-8GL)obtain: adopt the same procedure with step B22, the KS value of the cationic yellow x-8gl of gained in steps A 32 mapped and obtained the spectroscopic data X of cationic yellow x-8gl (X-8GL).
B3. calculate the SKS value of each one-component in mixed dye solution I or mixed dye solution II:
B31. calculate the SKS value of cationic yellow X-5GL in mixed dye solution I: by the spectroscopic data Z of the mixed dye solution I of gained in step B13 ibackground spectrum data Y with the cationic yellow X-5GL of gained in step B21 (X-8GL)and the spectroscopic data X of the cationic yellow X-5GL of gained in step B22 (X-5GL)bring the SKS value of obtaining cationic yellow X-5GL in mixed dye solution in oblique projection Operators Algorithm program into.
B32. calculate the SKS value of cationic yellow x-8gl in mixed dye solution I: by the spectroscopic data Z of the mixed dye solution I of gained in step B13 ibackground spectrum data Y with the cationic yellow x-8gl of gained in step B23 (X-5GL)and the spectroscopic data X of the cationic yellow x-8gl of gained in step B24 (X-8GL)bring the SKS value of obtaining cationic yellow x-8gl in mixed dye solution in oblique projection Operators Algorithm program into.
B33. calculate the SKS value of cationic yellow X-5GL in mixed dye solution II: by the spectroscopic data Z of the mixed dye solution II of gained in step B13 iIbackground spectrum data Y with the cationic yellow X-5GL of gained in step B21 (X-8GL)and the spectroscopic data X of the cationic yellow X-5GL of gained in step B22 (X-5GL)bring the SKS value of obtaining cationic yellow X-5GL in mixed dye solution in oblique projection Operators Algorithm program into.
B34. calculate the SKS value of cationic yellow x-8gl in mixed dye solution II: by the spectroscopic data Z of the mixed dye solution II of gained in step B13 iIbackground spectrum data Y with the cationic yellow x-8gl of gained in step B23 (X-5GL)and the spectroscopic data X of the cationic yellow x-8gl of gained in step B24 (X-8GL)bring the SKS value of obtaining cationic yellow x-8gl in mixed dye solution in oblique projection Operators Algorithm program into.
Oblique projection operator described above is E s|H=S(S tp h s) -1s tp h , P h =I-P h=I-H(H th) -1h t, wherein, subscript T represents transpose of a matrix; I is and P hthe unit matrix that dimension is identical; E s|Hfor oblique projection operator; S is the subspace that the vector of measured variable is opened; The adjacent subspace of H for not opening containing the vector of measured variable; P hfor the projection operator along subspace H to subspace S.
B4. calculate the content of each one-component in mixed dye solution:
B41. calculate the content of cationic yellow X-5GL in mixed dye solution I: the SKS value of cationic yellow X-5GL in the mixed dye solution I calculating in step B31 is brought in the point sample amount of cationic yellow X-5GL and the linear equation y=ax+b of SKS value of gained in steps A 51, calculate the content of cationic yellow X-5GL in mixed dye solution I, referring to table 3.
B42. calculate the content of cationic yellow x-8gl in mixed dye solution I: the SKS value of cationic yellow x-8gl in the mixed dye solution I calculating in step B32 is brought in the point sample amount of cationic yellow x-8gl and the linear equation y=ax+b of SKS value of gained in steps A 52, calculate the content of cationic yellow x-8gl in mixed dye solution I, referring to table 3.
B43. calculate the content of cationic yellow X-5GL in mixed dye solution II: the SKS value of cationic yellow X-5GL in the mixed dye solution II calculating in step B33 is brought in the point sample amount of cationic yellow X-5GL and the linear equation y=ax+b of SKS value of gained in steps A 51, calculate the content of cationic yellow X-5GL in mixed dye solution II, referring to table 3.
B44. calculate the content of cationic yellow x-8gl in mixed dye solution II: the SKS value of cationic yellow x-8gl in the mixed dye solution II calculating in step B34 is brought in the point sample amount of cationic yellow x-8gl and the linear equation y=ax+b of SKS value of gained in steps A 52, calculate the content of cationic yellow x-8gl in mixed dye solution II, referring to table 3.
Table 1: the SKS value of the point sample amount of cationic yellow X-5GL and cationic yellow x-8gl
Table 2: the point sample amount of cationic yellow X-5GL and cationic yellow x-8gl and the linear equation of SKS value
Dyestuff Linear equation Correlation coefficient r
Cationic yellow X-5GL y=12101x+1588.1 0.9997
Cationic yellow x-8gl y=11921x-225.64 0.9998
Table 3: the content of each component recording
A kind of conversion as the present embodiment: in the mixed dye solution that contains two or more components, the method for measuring of each component concentration and the present embodiment are basic identical, background extraction spectroscopic data is for needing only the KS value mapping under the respective wavelength in the KS function data of the arbitrary one-component beyond tested component.

Claims (8)

1. an assay method for component concentration in mixed dye solution, is characterized in that: comprise the following steps:
A. make the linear equation of each one-component point sample amount of dyestuff and SKS value:
A1. each one-component standard dyes solution of preparing variable concentrations: each one-component dyestuff is mixed with to variable concentrations b 1, b 2, b 3... b yone-component standard dyes solution;
A2. obtain the spectroscopic data of each one-component standard dyes solution: each one-component standard dyes solution point sample preparing in steps A 1, on silica gel plate, with the scanning of multi-wavelength thin-layer chromatogram scanner, is gathered to the spectroscopic data of each one-component dyestuff;
A3. translation data form: the spectroscopic data of each one-component dyestuff gathering in above-mentioned steps A2 is become to KS function data by the Data Format Transform of light intensity;
A4. the SKS value of suing for peace to obtain: the KS value summation by under each wavelength of gained in steps A 3, obtains SKS value;
A5. make the linear equation of point sample amount and the SKS value of each one-component of dyestuff: according to the point sample amount of each one-component dyestuff and SKS value, make the point sample amount of each one-component of dyestuff and the linear equation of SKS value; This linear equation is y=ax+b, and wherein, x is point sample amount, and y is SKS value, and a and b are constant;
B. the mensuration of each one-component content in mixed dye solution:
B1. obtain the spectroscopic data of mixed dye solution: by mixed dye solution point sample on silica gel plate, application multi-wavelength thin-layer chromatogram scanner scanning mixed dye solution, the light intensity data that scanning is preserved converts KS function data to, and the data after conversion are as the spectroscopic data Z of mixed dye solution;
B2. obtain background spectrum data and the spectroscopic data of each one-component: by the KS function data mapping of each one-component dyestuff obtaining in steps A 3, obtain the background spectrum data Y of each one-component dyestuff and the spectroscopic data X of each one-component dyestuff;
B3. calculate the SKS value of each one-component in mixed dye solution: in conjunction with oblique projection operator, the data that gather are carried out to signal compartment analysis, the spectroscopic data X of gained in the spectroscopic data Z of gained in step B1 and step B2 and background spectrum data Y are imported in oblique projection Operators Algorithm program, calculate the SKS value of each one-component in mixed dye solution;
B4. calculate the content of each one-component in mixed dye solution: the content of each one-component in mixed dye will be tried to achieve in the point sample amount of resulting each one-component of dyestuff and the linear equation of SKS value in the SKS value substitution steps A respectively of each one-component in the mixed dye solution obtaining in step B3;
Steps A 3 is become spectroscopic data the data layout of KS functional form with the KS function data that converts to described in step B1 for application KS=(ones (sizeab)-Refe) .^2./(2*Refe) by the Data Format Transform of light intensity, wherein, the reflective light intensity data of Refe for adopting multi-wavelength scanning instrument to gather; Sizeab is the dimension from the data of the reflective light intensity data acquisition of collection according to the absorbing wavelength of tested component; It is 1 matrix that ones helps the reflective light intensity data-switching of collection according to absorbing wavelength scope;
Oblique projection operator described in step B3 is E s|H=S (S tp h s) -1s tp h , P h =I-PH=I-H (H th) -1h t, wherein, subscript T represents transpose of a matrix; I is and P hthe unit matrix that dimension is identical; E s|Hfor oblique projection operator; S is the subspace that the vector of measured variable is opened; The adjacent subspace of H for not opening containing the vector of measured variable; P hfor the projection operator along subspace H to subspace S.
2. the assay method of component concentration in a kind of mixed dye solution according to claim 1, is characterized in that: each one-component standard dyes solution of preparing variable concentrations described in steps A 1 is: to containing measured object component a 1and a 2mixed dye solution, will only contain tested component a respectively 1or a 2one-component dyestuff be mixed with variable concentrations b 1, b 2, b 3, b 4, b 5one-component standard dyes solution.
3. the assay method of component concentration in a kind of mixed dye solution according to claim 2, is characterized in that: the spectroscopic data that obtains mixed dye solution described in step B1 is: will contain tested component a 1and a 2mixed dye solution I point sample on silica gel plate, application multi-wavelength thin-layer chromatogram scanner scans the spectroscopic data Z that mixed dye solution I to be measured obtains mixed dye solution i.
4. the assay method of component concentration in a kind of mixed dye solution according to claim 2, is characterized in that: the spectroscopic data of the background extraction spectroscopic data described in step B2 and tested component is: tested component a 1background spectrum data Y 2with tested component a 2background spectrum data Y 1, obtain tested component a 1spectroscopic data X 1with tested component a 2spectroscopic data X 2.
5. the assay method of component concentration in a kind of mixed dye solution according to claim 1, is characterized in that: the background spectrum data Y of each one-component dyestuff described in step B2 refers to the spectroscopic data that does not contain tested component in selected spectroscopic data.
6. the assay method of component concentration in a kind of mixed dye solution according to claim 5, it is characterized in that: the obtaining step of the background spectrum data Y of each one-component dyestuff described in step B2 is: to the KS value mapping under the respective wavelength in the KS function data of the arbitrary one-component beyond tested component, choose the data of those row of peak on figure as the background spectrum data Y of tested component, this column data does not contain tested component.
7. the assay method of component concentration in a kind of mixed dye solution according to claim 1, is characterized in that: the spectroscopic data X of each one-component dyestuff described in step B2 refers to the spectroscopic data that only contains tested component in selected spectroscopic data and do not contain other components.
8. the assay method of component concentration in a kind of mixed dye solution according to claim 7, it is characterized in that: the obtaining step of the spectroscopic data X of each one-component dyestuff described in step B2 is: to the KS value mapping under the respective wavelength in the KS function data of tested component, on figure the tested component purity of the data representation of those row of peak the highest, do not contain other components, choose this column data as tested component spectra data X.
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偏最小二乘-分光光度法同时测定染液中直接染料组分的浓度;粟晖等;《广西工学院学报》;20120630;第23卷(第2期);85-87,91 *
粟晖等.偏最小二乘-分光光度法同时测定染液中直接染料组分的浓度.《广西工学院学报》.2012,第23卷(第2期),85-87,91.

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