CN101793839A - Colorimetric detection method and device of sugar content of water - Google Patents
Colorimetric detection method and device of sugar content of water Download PDFInfo
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Abstract
The invention relates to a colorimetric detection method of sugar content of water, which comprises the steps of: under the condition of concentrated sulfuric acid, taking alpha-naphthol as a color-developing agent to prepare furfuraldehyde and derivatives thereof under the action of sugar and the concentrated sulfuric acid, and further performing condensation of the furfuraldehyde and the derivatives thereof and the alpha-naphthol to obtain purple complex compounds; and measuring reactant and recording change of intensity of transmitted light of aubergine condensation compounds absorbing absorb light with wavelength of 595 nanometers by a photoelectric colorimeter to obtain a response curve with corresponding peak height and peak width, and comparing the peak height of the curve with that of a light absorption curve of master standard water with a known sugar concentration to obtain sugar content values in water samples through calculation. The method has the advantages that: the on-line detection of the content of sugar with low content in water or solution can be performed; the process is simple, convenient and short; the detection data is accurate and reliable; the sample injected for one time of detection is only 50mu m to 1ml; only a very small amount of reagent is consumed each time; the operation cost is low; and the reagent is safe and nontoxic.
Description
Technical field
The present invention relates to the colorimetric detection method of sugared content in a kind of water and be particularly related to sugared colorimetric detection method that can measure micro-sugar in the aqueous solution or on-line monitoring, belong to chemical analysis and monitoring water environment analysis field.
Background technology
Sugar is divided into monose, disaccharide and polysaccharide usually.When sugar was water-soluble, tautomerism can take place in monose and the disaccharide that contains the hemiacetal hydroxyl in aqueous solution, and open-chain structure and ring texture have certain balance, therefore have reductibility, are also referred to as reducing sugar.Polysaccharide such as sucrose, starch, cellulose all are non-reducing sugars, but their hydrolyzables under the effect of acid or enzyme are monose, so its hydrolyzate has reductibility.
Sugar content is excessive in the water, can make boiler produce the sugar dirt, and why sugared dirt is called the source of hundred evils, and key is that it is hot poor conductor, has the sugar dirt on the boiler evaporating face, and heat conductivility reduces, and has reduced exerting oneself of boiler, makes evaporation of water amount minimizing in the boiler.For improving fire box temperature, increase exerting oneself of boiler, must increase fuel consumption, cause energy dissipation.Therefore, need at any time the industrial discharge water body to be carried out express-analysis, the data of the instant content of sugar in the water are provided, implement to carry out in the industrial discharge water body to sugar refinery the on-line monitoring of sugared content,, guarantee the normal safe operation of enterprise's boiler in time to take corresponding measure.
At present, measure the main anthracene copper of the method colourimetry of low content sugar, the Fei Linshi volumetric method.
Anthracene copper colourimetry is that sugar generates hydroxymethylfurans formaldehyde with the sulfuric acid reaction dehydration, produces thing and is condensed into blue look compound with anthracene copper again, and its shade is directly proportional with the concentration of sugar in the solution, but colorimetric assay.But it has certain concentration range restriction to tested liquid glucose, and requires detected liquid clarification, in most of the cases, requires not contain starch and dextrin, and this will be with starch before mensuration, and dextrin removes, so complicated operation, has limited its widespread use.Fei Linshi volumetric method colourimetry sample solution needn't transform, and carries out titration but directly get filtrate, and the suitable detectable concentration of reducing sugar is 0.2-0.5%.The reaction of valgar Fei Linshi volumetric method is complicated, and influence factor is more, and the result is inaccurate, operate loaded down with trivial detailsly, and slowly, reagent stability is poor rapidly.
Summary of the invention
The purpose of this invention is to provide the method for sugar in a kind of simple to operate, quick reliable, reagent is nontoxic and operating cost is cheap detection water and be exclusively used in the low content sugar pick-up unit of this method, to overcome traditional anthracene copper colourimetry, poisonous or the reagent of complex operation, the reagent that low contents such as Fei Linshi volumetric method sugar detection method exists can not long preservation etc. shortcoming, and realize that the automatic on-line of sugar in the water detects.
The method that the present invention detects sugared content is as follows:
With the concentrated sulfuric acid solution is oxygenant, alpha-Naphthol is a developer, in quantitative water sample injecting reactor to be measured, with the reagent concentrated sulphuric acid and alphanaphthol reaction, sugar generates furfural and derivant thereof with concentrated sulphuric acid effect, further generate the purple condensation product with the alpha-Naphthol condensation, the changing value that sees through light intensity after the aubergine condensation product that reacts in the liquid stream absorbs the 595nm wavelength light is measured and write down to reactant through photolometer, acquisition has the response curve of corresponding peak height and peak width, the peak height of the absorption curves that the standard specimen water of the peak height of curve and known sugars concentration is recorded contrasts, and obtains sugared content value in the water sample by relatively calculating.
The change reaction that this method relates to is as follows:
As oxygenant, saccharide compound in the sample and concentrated sulphuric acid effect generate furfural and derivant thereof with concentrated sulfuric acid solution:
Furfural that is generated and derivant thereof generate the purple condensation product with alphanaphthol reaction under the condition of the concentrated sulphuric acid.
The growing amount of furfural and derivant thereof is along with the concentration of sugar increases and increases, reaction generates the purple condensation product and increases, the depth of color and the sugared concentration that are purple are linear, so available 595nm wavelength light irradiation, record the photovoltage value by photoelectric commutator, acquisition has the response curve of corresponding peak height, by comparing with the measured value of known standard specimen, calculates the sugared concentration in the water sample.
The present invention has designed the pick-up unit of the special use of implementing above-mentioned detection method to sugar content in the water.
Sugar content pick-up unit in the said water comprises reactor, discharge pump, photoelectricity flow cell, two way selected valve, 5 way valve, six-way transfer valve and first~5th totally five three-way solenoid valves, is linked to be system by capillary pipeline therebetween;
Be on-off between said two way selected valve interface 1 and the interface 2, wherein, the 1st interface links to each other with reactor, and the 2nd interface is connected with the 2nd interface of 5 way valve is individual;
Said 5 way valve is provided with the 1st of circumferential arrangement~the 5th interface; Be on-off between the 1st interface and the 2nd interface, the 4th interface communicates with the 3rd or the 5th interface convertiblely; When the 4th interface and the 5th interface when logical, the 1st interface and the 2nd interface are for leading to; When the 4th interface and the 3rd interface when logical, the 1st interface and the 2nd interface are for breaking; Wherein, the 1st interface links to each other with reactor with the photoelectricity flow cell respectively with the 3rd interface;
Said six-way transfer valve is provided with the 1st of circumferential arrangement~the 6th interface, and the 1st interface communicates with the 2nd or the 6th interface convertiblely, and the 4th interface communicates with the 3rd or the 5th liang of interface convertiblely, when the 1st interface communicates with the 2nd interface; The 4th interface communicates with the 3rd interface; When the 1st interface communicated with the 6th interface, the 4th interface communicated with the 5th interface; Wherein, be connected with reagent between the 1st interface and the 4th interface and quantitatively encircle, the 2nd interface links to each other with reagent bottle, and the 3rd interface reclaims the liquid bottle with reagent and links to each other, and the 5th interface communicates with atmosphere, and the 6th interface links to each other with reactor;
Said five solenoid valves are equipped with three interfaces, and the 2nd interface in each solenoid valve communicates with separately the 1st interface or the 3rd interface all convertiblely;
Wherein, the 1st interface, the 3rd interface of first solenoid valve communicate with distilled water, water sample respectively, and the 2nd interface links to each other with the 3rd interface of second solenoid valve; The 1st interface of second solenoid valve communicates with second standard specimen, and the 2nd interface links to each other with the 3rd interface of the 3rd solenoid valve; The 1st interface of the 3rd solenoid valve communicates with first standard specimen, and the 2nd interface links to each other with the 3rd interface of the 4th solenoid valve; The 1st interface of the 4th solenoid valve communicates with atmosphere, is connected with sample between the 4th interface of the 2nd interface and 5 way valve and quantitatively encircles; The 1st interface of the 5th solenoid valve links to each other with reactor, and the 2nd interface links to each other with discharge pump, and the 3rd interface links to each other with the 5th interface of 5 way valve.
Said discharge pump is a peristaltic pump.
Be provided with a photoelectric alarm between the 2nd interface of said the 3rd solenoid valve and the 3rd interface of the 4th solenoid valve.
Said water sample import is equipped with and can be differed from separation vessel.
The orderly switching of each valve of this device may command and change system's capillary passage makes the sugar content of sample detect step and carries out in order.Discharge pump is earlier sent into water sample in the quantitative sampling ring between five-way valve reversal valve and the 4th solenoid valve; The mix reagent of alpha-Naphthol and sulfuric acid quantitatively encircles by the reagent that high-order transfusion bottle freely is full of six-way transfer valve; Quantitative reagent in gauge water in peristaltic pump quantitatively encircles water sample then and reagent quantitatively encircle is delivered in the reactor respectively, hybrid reaction is after a period of time, start discharge pump, reactant liquor after the variable color is sent into flow cell, measure the photovoltage value by photoelectric commutator, obtain to have the response curve of corresponding peak height.By comparing, calculate the sugared concentration in the water sample with the measured value of known standard specimen.
The present invention adopts under the effect of concentrated sulphuric acid oxygen, with alpha-Naphthol as developer, carry out the detection of sugared content in the water by photoelectric colorimetry, method is simple, the degree of accuracy height, can detect the water of low sugar contents, overcome anthracene copper colourimetry, the poisonous or reagent of complex operation, the reagent that methods such as Fei Linshi volumetric method exist can not long preservation, the expensive shortcoming of instrument.The pick-up unit of this method special use is linked to be system with kapillary and a plurality of cross-over valve, by orderly switching to each valve, water sample and reagent are carried by peristaltic pump and kapillary, under flow state, finish testing process, simple and efficient to handle, and can realize robotization control, be particularly useful for automatic on-line monitoring to sugar content in the recycle-water of sugar refinery.Water sample and reagent are quantitatively correct by the fixing kapillary of length (promptly quantitatively encircling) respectively, and it is accurately reliable to detect data, applicable to the detection to low content sugar in the water.The water sample of this device one-time detection is 1ml only, reagent 2ml, and consumption is minimum, and operating cost is cheap, and reagent is nontoxic, no exhaust emission.
Description of drawings
Fig. 1~Fig. 3 is the system architecture synoptic diagram of the colour comparison detection apparatus of sugared content, wherein:
Fig. 1 is that the expression system is in the sampling state,
Fig. 2 represents that system is in the sample introduction state,
Fig. 3 represents that system is in the measurement state.
Fig. 4 (1) and Fig. 4 (2) are respectively the transition state of five-way cross-over valve V4.
Fig. 5 (1) and Fig. 5 (2) are respectively the transition state of six cross valve V5.
Fig. 6 (1) and Fig. 6 (2) are respectively the transition state of two cross valve V4.
Mark is expressed as among the figure: P-peristaltic pump, M-reactor, H-reagent bottle, S-water sample, B1-first standard specimen, B2-second standard specimen, the K-photoelectric alarm, F-can differ from separation vessel, the L1-sample quantitatively encircles, and L2-reagent quantitatively encircles, W1-first waste liquid outlet, W2-second waste liquid outlet, N-reagent solution returnable bottle, V1-first solenoid valve, V2-second solenoid valve, V3-the 3rd solenoid valve, V7-the 4th solenoid valve, V8-the 5th solenoid valve, V4-two cross valves, V5-five-way cross-over valve, V6-six cross valves.
Embodiment
The structure of present embodiment accompanying drawings low content of the present invention sugar pick-up unit and detect the method for sugared content in water with its.
As Fig. 1, this pick-up unit comprises reactor M, peristaltic pump P, photoelectricity flow cell, two way selected valve V6,5 way valve V4, six-way transfer valve V5 and the first solenoid valve V1, the second solenoid valve V2, the 3rd solenoid valve V3, the 4th solenoid valve V7, the 5th solenoid valve V8, is that the polytetrafluoroethylene capillary of 0.5~1mm is linked to be system by internal diameter all therebetween.Each solenoid valve is T-valve.
Fig. 4 (1), Fig. 4 (2) are under two kinds of transition status: Fig. 4 (1) state of 5 way valve V4, and interface 4 is logical with interface 5, and interface 1 is logical (being the V4A attitude) with interface 2; Under Fig. 4 (2) state, interface 4 is logical with interface 3, and interface 1 is disconnected (being the V4B attitude) with interface 2.
Fig. 5 (1), Fig. 5 (2) are that interface 1 communicates with interface 2 under two kinds of transition status: Fig. 5 (1) state of six-way transfer valve V5, interface 4 communicate with interface 3 (being the V5A attitude); Under Fig. 5 (2) state, interface 1 communicates with interface 6, interface 4 communicate with interface 5 (being the V5B attitude).
Fig. 6 (1), Fig. 6 (2) are two kinds of transition statuses of two way selected valve V6, under Fig. 6 (1) state, are between interface 1 and the interface 2 logical (being the V6A attitude), under Fig. 6 (2) state, are between interface 1 and the interface 2 disconnected (being the V6B attitude).
Above cross-over valve V6, V4 and V5 all contain spool and valve seat, and the on/off relation between the valve inner joint is changed by the rotation of spool.
Implementing procedure and operating process below in conjunction with this pick-up unit of description of drawings.
One. sampling routine:
Solenoid valve V8, V7, V3, V2 and V1 all are adjusted to interface 2 communicate, reversal valve V4 is gone to the state A of Fig. 4 (1), simultaneously six-way valve V5 is gone to the state A of Fig. 5 (1) with 3.Start peristaltic pump P turn clockwise (pump is in suction condition).See Fig. 1, under the effect of peristaltic pump P, sample water S is by following flow path: S → V1 interface 3 → 2 → V2 interface 3 → 2 → V3 interface 3 → 2 → alarm K → V7 interface 3 → 2 → quantitatively encircle L1 → V4 interface 4 → 5 → V8 interface 3 → 2 → peristaltic pump → W1.Be sample water S under peristaltic pump P effect, flow out from wastewater outlet W1 at last by above-mentioned path flows.In this process, quantitatively encircle and be full of sample water in the L1.Simultaneously, the reagent (mixed liquor of sulfuric acid and alpha-Naphthol) in the reagent bottle H flows freely into valve V5 with a high position, and stream is: H → V5 interface 2 → 1 → quantitatively encircle L2 → 4 → 3 → N.Reagent flows into returnable bottle N by above-mentioned stream, in this process, quantitatively encircles and has been full of reagent in the L2.Finish the sampling process of water sample and reagent.
Alarm K contains flow cell, utilize in this flow cell have, n.s. (water) and the different principle of photovoltage that produces when not adopting sample mouth product, because of voltage is low, promptly can be reported to the police automatically.
For prevent>the 0.8mm granule foreign enters detection system, can granule foreign bigger in the water be moved downward because of gravity with water sample by differing from separation vessel F (patent No. 011082496), avoid entering among the water sample S.
Two. the sample introduction program
After sampling routine is finished, promptly change V5 to Fig. 4 (2) state, V5 is converted to Fig. 5 (2) state, the interface 2 of solenoid valve V8 and V7 all is transformed to interface 1 communicate, and at this moment, the terminal vigour of L1 and L2 communicates with air.System such as Fig. 2 state, peristaltic pump P turn clockwise (pump is in suction condition).
See Fig. 2, under peristaltic pump P effect, the water sample that quantitatively encircles L1 is by stream: L1 → V4 interface 4 → interface 3 → M, and water sample is inhaled into reactor M; Meanwhile, reagent H presses stream: L2 → V5 interface 1 → interface 6 → M, developer are also gone into reactor M.Sample introduction finishes, termination of pumping P.
Three. process of measurement
Water sample and reagent go to Fig. 4 (1) state with valve V4 behind the reactor internal reaction, with valve V5 go to Fig. 5 (2) state, valve V6 goes to Fig. 6 (2) state, the interface 2 of solenoid valve V8 communicates with interface 1, makes the measurement state of system such as Fig. 3.Starting peristaltic pump P is rotated counterclockwise.
As Fig. 3, under peristaltic pump P effect, reactant liquor in the reactor M is pushed to flow cell R, record the changing value that the aubergine condensation product sees through light intensity after to wavelength 595nm light absorption by photolometer, acquisition has the response curve of corresponding peak height and peak width, warp compares with the response curve that standard specimen B1 and B2 under equal conditions record, and calculates the value that obtains sugar in the water sample.
This device needed system is cleaned before each test.Promptly by to the conversion of each valve, by means of the effect of peristaltic pump with distilled water by predetermined pipeline inflow reactor M or flow cell R, then as the waste liquid outflow system, make reactor M, flow cell R, sample quantitatively encircle L1 and pipeline therebetween and obtain distilled water and clean; In addition, valve V5 is gone to Fig. 5 (1) attitude, make reagent H cross reagent and quantitatively encircle L2 and flow into returnable bottle N, make cleaning reagent quantitatively encircle the cleaning that L2 obtains fresh reagent from high-order free flow.
1. configuration reagent
Preparation contains the syrup sample: sugared concentration is 30mg/L: formulated with pure sucrose and distilled water.
The preparation developer: methyl naphthol-concentrated sulphuric acid, 10g/L solution: get the 10g methyl naphthol, be settled to 1000L with the concentrated sulphuric acid,
The preparation standard specimen: prepare one group of standard specimen, every group of two standard specimens, sugared content (mg/l) is respectively:
First group:
Standard specimen B1:0mg/l (the steaming water that does not contain sugar), standard specimen B2:80mg/l.
2. experiment
After earlier pick-up unit being cleaned, carry out sample introduction, sample incision, reaction, process of measurement successively and carry out the check of sugar.Reaction time: 120 seconds.
With first group of standard specimen is contrast, carries out the mensuration of standard specimen and sample 1, data such as following table:
From above test data as seen, this method is minimum to the error between the actual concentrations value of the sugared concentration detected value of low sugar water sample and sample, illustrates that to detect degree of accuracy very high.
Claims (5)
1. the colorimetric detection method of sugared content in the water, it is characterized in that with the concentrated sulfuric acid solution being oxygenant, alpha-Naphthol is a developer, in quantitative water sample injecting reactor to be measured, with the reagent concentrated sulphuric acid and alphanaphthol reaction, sugar generates furfural and derivant thereof with concentrated sulphuric acid effect, further generate the purple condensation product with the alpha-Naphthol condensation, the changing value that sees through light intensity after the aubergine condensation product that reacts in the liquid stream absorbs the 595nm wavelength light is measured and write down to reactant through photolometer, acquisition has the response curve of corresponding peak height and peak width, the peak height of the absorption curves that the standard specimen water of the peak height of curve and known sugars concentration is recorded contrasts, and obtains sugared content value in the water sample by relatively calculating.
2. the isolated plant of claim 1 detection method is characterized in that comprising reactor, discharge pump, photoelectricity flow cell, two way selected valve, 5 way valve, six-way transfer valve and first~5th totally five three-way solenoid valves, is linked to be system by capillary pipeline therebetween;
Be on-off between said two way selected valve interface 1 and the interface 2, wherein, the 1st interface links to each other with reactor, and the 2nd interface is connected with the 2nd interface of 5 way valve is individual;
Said 5 way valve is provided with the 1st of circumferential arrangement~the 5th interface; Be on-off between the 1st interface and the 2nd interface, the 4th interface communicates with the 3rd or the 5th interface convertiblely; When the 4th interface and the 5th interface when logical, the 1st interface and the 2nd interface are for leading to; When the 4th interface and the 3rd interface when logical, the 1st interface and the 2nd interface are for breaking; Wherein, the 1st interface links to each other with reactor with the photoelectricity flow cell respectively with the 3rd interface;
Said six-way transfer valve is provided with the 1st of circumferential arrangement~the 6th interface, and the 1st interface communicates with the 2nd or the 6th interface convertiblely, and the 4th interface communicates with the 3rd or the 5th liang of interface convertiblely, when the 1st interface communicates with the 2nd interface; The 4th interface communicates with the 3rd interface; When the 1st interface communicated with the 6th interface, the 4th interface communicated with the 5th interface; Wherein, be connected with reagent between the 1st interface and the 4th interface and quantitatively encircle, the 2nd interface links to each other with reagent bottle, and the 3rd interface reclaims the liquid bottle with reagent and links to each other, and the 5th interface communicates with atmosphere, and the 6th interface links to each other with reactor;
Said five solenoid valves are equipped with three interfaces, and the 2nd interface in each solenoid valve communicates with separately the 1st interface or the 3rd interface all convertiblely;
Wherein, the 1st interface, the 3rd interface of first solenoid valve communicate with distilled water, water sample respectively, and the 2nd interface links to each other with the 3rd interface of second solenoid valve; The 1st interface of second solenoid valve communicates with second standard specimen, and the 2nd interface links to each other with the 3rd interface of the 3rd solenoid valve; The 1st interface of the 3rd solenoid valve communicates with first standard specimen, and the 2nd interface links to each other with the 3rd interface of the 4th solenoid valve; The 1st interface of the 4th solenoid valve communicates with atmosphere, is connected with sample between the 4th interface of the 2nd interface and 5 way valve and quantitatively encircles; The 1st interface of the 5th solenoid valve links to each other with reactor, and the 2nd interface links to each other with discharge pump, and the 3rd interface links to each other with the 5th interface of 5 way valve.
3. device according to claim 2, the said discharge pump of its feature is a peristaltic pump.
4. device according to claim 3 is provided with a photoelectric alarm device between the 2nd interface of said the 3rd solenoid valve of its feature and the 3rd interface of the 4th solenoid valve.
5. device according to claim 2, the said water sample import of its feature is equipped with and can be differed from separation vessel.
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CN102830117A (en) * | 2012-09-18 | 2012-12-19 | 国家海洋局天津海水淡化与综合利用研究所 | Device and method for carrying out continuous flow detection on bicarbonates in water |
CN103645180A (en) * | 2013-12-02 | 2014-03-19 | 中国烟草总公司重庆市公司烟草科学研究所 | Method for determining content of reducing sugars in flue-cured tobacco leaves |
CN107064121A (en) * | 2016-12-29 | 2017-08-18 | 核工业北京化工冶金研究院 | The device of uranium concentration in a kind of application colorimetric method on-line checking adsorption tail liquid |
WO2020098229A1 (en) * | 2018-11-15 | 2020-05-22 | 微山宏瑞电力科技有限公司 | Cooking sweetness measurement device and manufacturing method therefor |
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