CN103398966A - Method for detecting TMC concentration in organic solution by using spectrometer - Google Patents
Method for detecting TMC concentration in organic solution by using spectrometer Download PDFInfo
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- CN103398966A CN103398966A CN2013103641188A CN201310364118A CN103398966A CN 103398966 A CN103398966 A CN 103398966A CN 2013103641188 A CN2013103641188 A CN 2013103641188A CN 201310364118 A CN201310364118 A CN 201310364118A CN 103398966 A CN103398966 A CN 103398966A
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Abstract
The invention discloses a measuring method, and specifically relates to a method for detecting TMC concentration in an organic solution by using a spectrometer. The method comprises: an organic solvent containing TMC is placed in an open circulating pool; then compound light emitted by a xenon lamp is transmitted to a fiber probe via a fiber, and the light emitted by the fiber probe enters into the open circulating pool; the light penetrating the open circulating pool is subjected to specular reflection, then is transmitted to a slit of the spectrometer by the fiber, and the light passing through the slit enters into the concave grating monochromator of the spectrometer; the light coming from the concave grating monochromator of the spectrometer enters into the photodiode array of the spectrometer, and the light signal is converted into an electric signal; and the electric signal is processed by the core data chip of the spectrometer and transmitted to the computer, and the concentration value of TMC in the organic solution is obtained. The method is capable of conveniently online determining TMC concentration in the organic solution, and the method has the advantages of convenient operation, better accuracy and saved labor cost.
Description
Technical field
The present invention relates to a kind of measuring method, specifically refer to a kind of method of utilizing spectrometer to measure the TMC concentration in organic solution.
Technical background
Pyromellitic trimethylsilyl chloride (hereinafter to be referred as TMC) is the important source material that NF membrane, reverse osmosis membrane are produced, and its concentration in organic solvent directly determines the performance of product.In counter-infiltration diaphragm production run, along with the carrying out that produces, TMC concentration in organic solvent can constantly descend, for TMC concentration is remained in the scope of normal production, must often detect the concentration of TMC in organic solvent, and according to a certain amount of TMC of testing result interpolation, to guarantee its concentration, meet the requirement of production, and this sampling detection mode inconvenience and workload are large.Spectrophotometric method is based on a kind of absorbance or the luminous intensity by mensuration measured matter light in certain wave strong point or certain wavelength coverage that Lambert-Beer's law is set up, the method for this material being carried out quantitative test.
, in order the concentration of TMC in organic solution effectively, in time to be detected, preferably can find a kind of method that can detect online, rather than by the method for manual analysis is intermittent, measure.
Summary of the invention
The present invention is directed to deficiency of the prior art, proposing a kind utilizes spectrometer to measure the method for TMC concentration in organic solution, the absorbance test of detection fiber spectrometer to the TMC concentration of variable concentrations online, and absorbance and TMC concentration standard curve have been drawn, obtain the linearity preferably, the most online detection fiber spectrometer is applied in the actual production process of reverse osmosis membrane, and performance is good.
The present invention is achieved by following proposal:
Spectrometer is measured the method for TMC concentration in organic solution, it is characterized in that comprising the steps:
The organic solvent that (1) will contain TMC is placed in open flow cell;
(2) complex light of xenon lamp being sent arrives fibre-optical probe by Optical Fiber Transmission, and the light that fibre-optical probe sends enters into open flow cell again;
(3) light that sees through open flow cell again after mirror-reflection, then is entered the concave grating monochromator of spectrometer by the light of Optical Fiber Transmission in the slit of spectrometer, after slit;
(4) enter the photodiode array of spectrometer from the concave grating monochromator light out of spectrometer, light signal is changed into electric signal, enter into computing machine after the core data chip of spectrometer is processed, get final product to obtain the concentration value of TMC in organic solution.
As preferably, above-mentioned spectrometer is measured open flow cell in the method for TMC concentration in organic solution light path is 1mm.
As preferably, above-mentioned spectrometer is measured spectrometer in the method for TMC concentration in organic solution wavelength coverage is 200nm-800nm, and wavelength accuracy is ± 0.3nm that the wavelength reappearance is ± 0.1nm.As better selection, the wavelength coverage of spectrometer is 240nm-320nm.
In the present invention, Lambert-Beer's law is the most basic principle of fiber spectrometer, as shown in Figure 1, when a branch of directional light is vertically injected the solution of stable homogeneous, solution can have to the light of specific wavelength certain absorption, in the situation that light path is constant, the concentration of solution is directly proportional to absorbance, can use formula (1) to describe:
In formula: A is absorbance; I
oFor incident intensity; I is transmitted intensity; K is molar absorptivity, and unit is L/ (molcm); B is light path, and unit is cm; C is the concentration of extinction material, and unit is mol/L.
When the concentration of test substance is larger, light path is thicker, solution light more to the absorption of light, that see through are more weak.The TMC standard solution of the concentration preparation variable concentrations that requires according to production, measure the absorbance of each standard solution, and the absorbance data that gets standard samples is made the typical curve of TMC concentration and absorbance.Under identical operating conditions, measure the absorbance of TMC solution on unknown certain moment production line, can draw fast TMC concentration by typical curve.
Beneficial effect: can facilitate by the present invention the TMC concentration that detects online in organic solution, easy to operate, and also more accurate, saved labor cost.
Description of drawings
Utilize the Lambert-Beer's law schematic diagram in Fig. 1 the present invention
The spectrogram of the sample to be tested in Fig. 2 embodiment
Scanning neat solvent background in Fig. 3 embodiment, and the impact of removal background obtains the absorbance spectrogram of the TMC solution of 6 kinds of variable concentrations
The canonical plotting (290nm) of the TMC solution after Fig. 4 match
In Fig. 5 reverse osmosis membrane production run, TMC concentration is with the variation of working time
Embodiment
Below enforcement of the present invention is illustrated:
Embodiment 1-12
The TMC standard solution is measured
The solution of 6 kinds of variable concentrations of TMC concentration preparation during according to actual production, solvent is IsoparG.Concentration is respectively: 0.25g/L, 0.49g/L, 0.72g/L, 1.01g/L, 1.25g/L, 1.53g/L.TMC and IsoparG are the raw material that production is used.
Use online detection fiber spectrometer in the present invention, use neat solvent as the reference sample, obtain the UV-VIS spectrogram of TMC standard solution, as shown in Figure 2, show that TMC solution has obvious absorbing phenomenon in the ultraviolet region of 240-320nm.TMC concentration is larger, and the absorption in the ultraviolet region of 240-320nm is more obvious.
Scanning neat solvent background, and the impact of removing background obtain 6 kinds of variable concentrations TMC solution the absorbance spectrogram as shown in Figure 3.Can find out from spectrogram, TMC solution has two very significantly characteristic absorption peaks at 247nm and 291nm place, and very little at the visible region absorbance.
Choosing TMC solution is the absorbance at 290nm place at wavelength, and analyzes the absorbance at 290nm place and the linear relationship of TMC solution, and as shown in Figure 4, ordinate is TMC concentration, and the match linear equation is TMC concentration (g/L)=2.90126 * A-0.03397, r
2=0.998, show and both have the highly linear correlationship, r wherein
2More the effect near 1 expression match is better.Can obtain with the absorbance that records unknown TMC solution on production line (A) concentration of detected solution by the linear Solving Equations of match.
Embodiment 13-24
Online detection fiber spectrometer is applied in the reverse osmosis membrane production run, produced as example take 8 hours, the TMC concentration that is fit to reverse osmosis membrane production is a concentration interval (0.72g/L-0.86g/L), the initial concentration that TMC produces is 0.82g/L, record in production run TMC concentration with the variation of working time, as shown in Figure 5.Production line organic solvent solution when getting TMC and adding, the normal analysis ultra-violet and visible spectrophotometer (model: UV-2802CP of using when in the past producing, producer: carry out concentration determination UNICO(Shanghai) Instruments Co., Ltd.), test data and the Data Comparison that records with fiber spectrometer, as shown in the table:
And in above-described embodiment, operation in the steps below
(1) will open flow cell is immersed in the organic solution that contains TMC;
(2) complex light of xenon lamp being sent arrives fibre-optical probe by Optical Fiber Transmission, and the light that fibre-optical probe sends enters into open flow cell again; The light path of open flow cell is 1mm.
(3) light that sees through open flow cell again after mirror-reflection, then is entered the concave grating monochromator of spectrometer by the light of Optical Fiber Transmission in the slit of spectrometer, after slit; The wavelength coverage of spectrometer is 290nm;
(4) enter the photodiode array of spectrometer from the concave grating monochromator light out of spectrometer, light signal is changed into electric signal, be converted into digital signal and show on computers absorbance after the core data chip of spectrometer is processed, mensuration by the absorbance A to the TMC standard solution, and simulate the typical curve of TMC concentration and A: TMC concentration (g/L)=2.90126 * A-0.03397, r
2=0.998, both have the height correlation relation., by measuring solution absorbance value A to be measured, get final product to obtain the concentration value of TMC in organic solution.
Ultraviolet spectrophotometer record TMC concentration all than fiber spectrum instrument record slightly large, and the maximum difference of the TMC concentration that two kinds of methods record is 0.006g/L, relative difference is in 0.82%.Can find out in conjunction with Fig. 5 and upper table, online detection fiber spectrometer is in whole production run, and is stable; Analyze from experimental data, with always for the production of the measurement data of ultra-violet and visible spectrophotometer differ less.Illustrate, the online detection fiber spectrometer of research and development is applicable to the online detection of the organic solvent concentration in the reverse osmosis membrane production run voluntarily.
The present invention utilizes the ultimate principle of spectrophotometric method, by related experiment, has verified that this spectrometer measurement precision is higher, good stability, has greatly simplified TMC and add process.This spectrometer can be widely used in the online detection of TMC concentration in organic solvent.
Claims (4)
1. spectrometer is measured the method for TMC concentration in organic solution, it is characterized in that comprising the steps:
(1) will open flow cell is immersed in the organic solution that contains TMC;
(2) complex light of xenon lamp being sent arrives fibre-optical probe by Optical Fiber Transmission, and the light that fibre-optical probe sends enters into open flow cell again;
(3) light that sees through open flow cell again after mirror-reflection, then is entered the concave grating monochromator of spectrometer by the light of Optical Fiber Transmission in the slit of spectrometer, after slit;
(4) enter the photodiode array of spectrometer from the concave grating monochromator light out of spectrometer, light signal is changed into electric signal, be converted into digital signal and show on computers absorbance after the core data chip of spectrometer is processed, according to TMC concentration (g/L)=2.90126 * A-0.03397 relation,, by measuring solution absorbance value A to be measured, get final product to obtain the concentration value of TMC in organic solution.
2. spectrometer according to claim 1 is measured the method for TMC concentration in organic solution, it is characterized in that the light path of open flow cell is 1mm.
3. spectrometer according to claim 1 is measured the method for TMC concentration in organic solution, and the wavelength coverage that it is characterized in that spectrometer is 200nm-800nm, and wavelength accuracy is ± 0.3nm that the wavelength reappearance is ± 0.1nm.
4. spectrometer according to claim 3 is measured the method for TMC concentration in organic solution, and the wavelength coverage that it is characterized in that spectrometer is 240nm-320nm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105973886A (en) * | 2016-05-30 | 2016-09-28 | 田发益 | Method and device for determining concentration value based on visible light spectrum |
| CN106370613A (en) * | 2016-11-10 | 2017-02-01 | 广东电网有限责任公司电力科学研究院 | Spectrum system and method for directly measuring concentration of furfural in transformer oil |
| CN112763436A (en) * | 2020-12-24 | 2021-05-07 | 中国原子能科学研究院 | Spectrum measuring system |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105973886A (en) * | 2016-05-30 | 2016-09-28 | 田发益 | Method and device for determining concentration value based on visible light spectrum |
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| CN106370613B (en) * | 2016-11-10 | 2024-01-19 | 广东电网有限责任公司电力科学研究院 | Spectrum system and method for directly measuring concentration of furfural in transformer oil |
| CN112763436A (en) * | 2020-12-24 | 2021-05-07 | 中国原子能科学研究院 | Spectrum measuring system |
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Owner name: LANXING (HANGZHOU) FILM INDUSTRY CO., LTD. Free format text: FORMER OWNER: HANGZHOU BEIDOUXING MEMBRANE CO., LTD. Effective date: 20140929 |
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