CN203479695U - Instrument for on-line measurement of concentration of TMC (trimesoyl chloride) in organic solution - Google Patents
Instrument for on-line measurement of concentration of TMC (trimesoyl chloride) in organic solution Download PDFInfo
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- CN203479695U CN203479695U CN201320511392.9U CN201320511392U CN203479695U CN 203479695 U CN203479695 U CN 203479695U CN 201320511392 U CN201320511392 U CN 201320511392U CN 203479695 U CN203479695 U CN 203479695U
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Abstract
The utility model discloses an instrument for online measurement, and in particular relates to an instrument for online measurement of the concentration of TMC (trimesoyl chloride) in an organic solution. The instrument comprises a computer, a power supply and a fiber-optic probe, wherein the instrument is provided with a main circuit which is connected with the power supply and is also connected with an attached circuit of a mainframe of a spectrograph; meanwhile, the main circuit is connected with a flashing xenon lamp which is connected with the fiber-optic probe through optical fibers; the fiber-optic probe is connected with a slit in the mainframe of the spectrograph by energizing a flow cell; the spectrograph is connected with the computer. The instrument can be conveniently used for the on-line measurement of the concentration of the TMC in the organic solution, and is convenient to operate and relatively accurate. Thus, the human cost is saved.
Description
Technical field
The utility model relates to a kind of measurement mechanism, specifically refers to a kind of instrument that utilizes 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 producing, TMC concentration in organic solvent can constantly decline, for TMC concentration is remained in the scope of normal production, must often detect the concentration of TMC in organic solvent, and according to testing result, add a certain amount of TMC and meet the requirement of production to guarantee its concentration, and this sampling detection mode inconvenience and workload are large.Spectrophotometric method is set up based on Lambert-Beer's law a kind of by measuring absorbance or the luminous intensity of measured matter light in certain wave strong point or certain wavelength coverage, the method for this material being carried out to quantitative test.
In order the concentration of TMC in organic solution to be detected effectively, in time, preferably can find a kind of device that can detect online, rather than by intermittent mensuration of method of manual analysis.
Utility model content
The utility model is for 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 good linearity, the most online detection fiber spectrometer is applied in the actual production process of reverse osmosis membrane, and performance is good.
The utility model is achieved by following proposal:
The instrument of TMC concentration in a kind of on-line determination organic solution, comprise computing machine, power supply, fibre-optical probe, it is characterized in that the main circuit that has to be connected with power supply, main circuit is connected with the attached circuit for spectrometer unit, main circuit is connected with flicker xenon lamp simultaneously, and flicker xenon lamp is connected with fibre-optical probe by optical fiber; Fibre-optical probe is connected with the slit in spectrometer unit by open flow cell; Spectrometer is connected with computing machine again.In the utility model, those of ordinary skill in industry can be made the concrete technology contents that draws main circuit, attached circuit according to existence conditions;
As preferably, in above-mentioned a kind of on-line determination organic solution, in the instrument of TMC concentration, in spectrometer unit, there is successively slit to be connected with concave grating, concave grating is connected with photodiode array, and photodiode array is connected with core data chip, by core data chip, is connected with computing machine.Core data chip in spectrometer unit is prior art;
As preferably, in above-mentioned a kind of on-line determination organic solution, in the instrument of TMC concentration, between open flow cell and slit, also has a specular reflector.
As preferably, in above-mentioned a kind of on-line determination organic solution, in the instrument of TMC concentration, the light path of open flow cell is 1mm.
As preferably, the computing module in above-mentioned a kind of on-line determination organic solution in the instrument Computer of TMC concentration according to being: TMC concentration (g/L)=2.90126 * A-0.03397, wherein A is the absorbance of the organic solution containing TMC.Computing module in the utility model is very important technical characterictic, according to above-mentioned formula, can design, produce corresponding module;
In the utility model, 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 certain absorption to the light of specific wavelength, 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 is more weak.The TMC standard solution of the concentration preparation variable concentrations requiring according to production, measures the absorbance of each standard solution, and the absorbance data getting 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: by the utility model, can facilitate the TMC concentration detecting online in organic solution, easy to operate, and also more accurate, saved labor cost.
Accompanying drawing explanation
In Fig. 1 the utility model, utilize Lambert-Beer's law schematic diagram
The spectrogram of the sample to be tested in Fig. 2 embodiment
In Fig. 3 embodiment, scan neat solvent background, and the impact of removing 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 matching
Fig. 5 structural representation of the present utility model
Embodiment
Below enforcement of the present utility model is illustrated:
Embodiment 1
Make the instrument of TMC concentration in an on-line determination organic solution, comprise computing machine, power supply, fibre-optical probe, wherein there is a main circuit being connected with power supply, main circuit is connected with the attached circuit for spectrometer unit, main circuit is connected with flicker xenon lamp simultaneously, and flicker xenon lamp is connected with fibre-optical probe by optical fiber; Fibre-optical probe is connected with the slit in spectrometer unit by open flow cell; Spectrometer is connected with computing machine again; In spectrometer unit, have successively slit to be connected with concave grating, concave grating is connected with photodiode array, and photodiode array is connected with core data chip, by core data chip, is connected with computing machine; Computing module in computing machine according to being: TMC concentration (g/L)=2.90126 * A-0.03397, wherein A is the absorbance containing the organic solution of TMC.
Embodiment 2
Make the instrument of TMC concentration in an on-line determination organic solution, comprise computing machine, power supply, fibre-optical probe, wherein there is a main circuit being connected with power supply, main circuit is connected with the attached circuit for spectrometer unit, main circuit is connected with flicker xenon lamp simultaneously, and flicker xenon lamp is connected with fibre-optical probe by optical fiber; Fibre-optical probe is connected with the slit in spectrometer unit by open flow cell; Spectrometer is connected with computing machine again; In spectrometer unit, have successively slit to be connected with concave grating, concave grating is connected with photodiode array, and photodiode array is connected with core data chip, by core data chip, is connected with computing machine; Between open flow cell and slit, also has a specular reflector; Computing module in computing machine according to being: TMC concentration (g/L)=2.90126 * A-0.03397, wherein A is the absorbance containing the organic solution of TMC.
Embodiment 3-14
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 the instrument in the utility model, using neat solvent as 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 absorbance spectrogram as shown in Figure 3.From spectrogram, can find out, TMC solution has two very significantly characteristic absorption peaks at 247nm and 291nm place, and very little at 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 matching linear equation is TMC concentration (g/L)=2.90126 * A-0.03397, r
2=0.998, show that the two has highly linear correlationship, r wherein
2the effect that more approaches 1 expression matching is better.Can by the linear Solving Equations of matching, obtain the concentration of detected solution with the absorbance (A) that records unknown TMC solution on production line.
Embodiment 15-26
Online detection fiber spectrometer is applied in reverse osmosis membrane production run, the production in 8 hours of take is example, the TMC concentration that is applicable 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 the Data Comparison recording with fiber spectrometer, as shown in the table:
And in above-described embodiment, operation in the steps below
(1) organic solvent that contains TMC is placed in to 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; The light path of open flow cell is 1mm.
(3) light that sees through open flow cell is again after mirror-reflection, then the light in the slit of spectrometer, after slit enters the concave grating monochromator of spectrometer by Optical Fiber Transmission; The wavelength coverage of spectrometer is 290nm;
(4) from the concave grating monochromator of spectrometer light out, enter the photodiode array of spectrometer, light signal is changed into electric signal, after processing, the core data chip of spectrometer enters into computing machine, computing machine basis: TMC concentration (g/L)=2.90126 * A-0.03397 formula draw program, gets final product to obtain the concentration value of TMC in organic solution; Wherein A is the absorbance of the organic solution containing TMC.
Ultraviolet spectrophotometer records slightly large that TMC concentration all records than fiber spectrum instrument, and the maximum difference of the TMC concentration that two kinds of methods record is 0.006g/L, and relative difference is in 0.82%.In conjunction with Fig. 5 and upper table, can find out, online detection fiber spectrometer is in whole production run, stable; From experimental data, analyze, 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 reverse osmosis membrane production run voluntarily.
The utility model utilizes the ultimate principle of spectrophotometric method, by related experiment, has been verified that this spectrometer measurement precision is higher, good stability, has greatly been simplified TMC and add process.This spectrometer can be widely used in the online detection of TMC concentration in organic solvent.
Claims (4)
1. the instrument of TMC concentration in an on-line determination organic solution, comprise computing machine, power supply, fibre-optical probe, it is characterized in that the main circuit that has to be connected with power supply, main circuit is directly the power supply of flicker xenon lamp, the attached circuit that spectrometer separates with main circuit is connected, and flicker xenon lamp is connected with fibre-optical probe by optical fiber; In fibre-optical probe, comprise an open flow cell, fibre-optical probe is connected with the slit in spectrometer unit by optical fiber; Spectrometer is connected with computing machine again.
2. the instrument of TMC concentration in a kind of on-line determination organic solution according to claim 1, it is characterized in that having successively slit to be connected with concave grating in spectrometer unit, concave grating is connected with photodiode array, photodiode array is connected with core data chip, by core data chip, is connected with computing machine.
3. the instrument of TMC concentration in a kind of on-line determination organic solution according to claim 1, is characterized in that also having a specular reflector between open flow cell and slit.
4. the instrument of TMC concentration in a kind of on-line determination organic solution according to claim 1, is characterized in that the light path of open flow cell is 1mm.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320511392.9U CN203479695U (en) | 2013-08-20 | 2013-08-20 | Instrument for on-line measurement of concentration of TMC (trimesoyl chloride) in organic solution |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201320511392.9U CN203479695U (en) | 2013-08-20 | 2013-08-20 | Instrument for on-line measurement of concentration of TMC (trimesoyl chloride) in organic solution |
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| CN203479695U true CN203479695U (en) | 2014-03-12 |
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| CN201320511392.9U Withdrawn - After Issue CN203479695U (en) | 2013-08-20 | 2013-08-20 | Instrument for on-line measurement of concentration of TMC (trimesoyl chloride) in organic solution |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103398967A (en) * | 2013-08-20 | 2013-11-20 | 杭州北斗星膜制品有限公司 | Apparatus for online determining TMC concentration in organic solution |
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2013
- 2013-08-20 CN CN201320511392.9U patent/CN203479695U/en not_active Withdrawn - After Issue
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103398967A (en) * | 2013-08-20 | 2013-11-20 | 杭州北斗星膜制品有限公司 | Apparatus for online determining TMC concentration in organic solution |
| CN103398967B (en) * | 2013-08-20 | 2016-02-24 | 蓝星（杭州）膜工业有限公司 | The instrument of TMC concentration in a kind of on-line determination organic solution |
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| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| AV01 | Patent right actively abandoned |
Granted publication date: 20140312 Effective date of abandoning: 20160224 |
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| AV01 | Patent right actively abandoned |
Granted publication date: 20140312 Effective date of abandoning: 20160224 |
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| C25 | Abandonment of patent right or utility model to avoid double patenting |