CN105277552A - Device for online detection of azo coloring agents and using method of device - Google Patents
Device for online detection of azo coloring agents and using method of device Download PDFInfo
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Abstract
The invention relates to a device for online detection of azo coloring agents and a using method of the device. The device comprises a constant flow pump conveying system, a reduction reaction system, a diazotization reaction system, a chromogenic reaction system and a detection system. According to the device, the adding sequence of equivalent weight of reagents are adjusted on line, reactions are accurately controlled, and the online heat reduction, diazotization and a chromogenic reactions of azo reagents are achieved, direction detection in a amaranth spectrum section can be achieved through the reaction systems, operation is simple and sensitive, the analyzing efficiency is high, results are stable, the limitation that the detection sensitivity of light color coloring agents such as the basic orange in coloring agents is low due to small light absorbing coefficients is broken through, and the device can be applied to automatic analysis of the total amount of the azo coloring agent in samples to be detected.
Description
Technical field
The present invention relates to a kind of device for azo colouring agent on-line checkingi and using method thereof.
Background technology
Azo colouring agent carcinogenicity is strong, toxicity large, and harm is large, for countries in the world are classified as key monitoring object.In recent years, the non-edible industrial dye/pigment such as tonyred, para red, Basic Orange adds that green azo dyes etc. is frequent to be occurred in process of production in Misuse, tealeaves in violation of rules and regulations.How to monitor the azo colouring agent that may exist in market circulation food quickly and efficiently, become the focal issue that the whole society pays close attention to.
The assay method of azo colouring agent mainly contains spectrophotometric method, chromatography.In single azo colouring agent context of detection, utilize colorimetric determination, analyze simple and fast.Adopt high performance liquid chromatography, GC-MS(gas chromatography-mass spectrography), liquid chromatography-mass spectrography/mass spectroscopy, method accuracy is high, involved apparatus expensive and operation requirements is high, and sample preparation is comparatively complicated, is difficult to effectively be applied in the quick circulation systems in market.In colorimetric detection, mainly carry out visual analysis based on pigment self color, apply more method and have polycaprolactam method, liquid-liquid apportion design, simple to operate, extraction ratio is high, can detect the colorants such as lemon yellow, erythrosine amaranth and famille rose, but operating process is loaded down with trivial details, the time is tediously long, is difficult to obtain high throughput automated application in practice.Need the azo colouring agent on-line measuring device that research and development are simple and practical badly.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of device for azo colouring agent on-line checkingi and using method thereof, achieve the automated analysis of azo colouring agent total amount in testing sample.
For achieving the above object, the present invention adopts following technical scheme: a kind of device for azo colouring agent on-line checkingi, is characterized in that: comprise the constant flow pump induction system, reduction reaction system, diazo-reaction system, chromogenic reaction system and the colorimetric assay system that connect successively.
Further, described constant flow pump induction system comprises the reagent bottle, that a reagent bottle, that distilled water is housed is equipped with buffering agent the reagent bottle that the reagent bottle and going back original reagent is equipped with testing sample is housed; Described distilled water is housed reagent bottle, the reagent bottle that buffering agent is housed, the reagent bottle going back original reagent is housed and the reagent bottle that testing sample is housed is connected with a four-way valve through a pump housing respectively.
Further, described reduction reaction system comprises an electronic temperature control device and and is arranged at reduction reactor in described electronic temperature control device, and the input end of described reduction reactor is connected with described four-way valve.
Further, described diazo-reaction system comprises a refrigeratory, described refrigeratory is connected with the output terminal of described reduction reactor and a diazo-reaction device respectively, and the reagent bottle that the reagent bottle and that described diazo-reaction device is also equipped with acid reagent through a pump housing and is respectively equipped with diazo reagent is connected.
Further, described chromogenic reaction system comprises a chromogenic reaction device, described chromogenic reaction device is connected with described diazo-reaction device, and the reagent bottle that the reagent bottle and that described chromogenic reaction device is also equipped with masking reagent through a pump housing and is respectively equipped with chromogenic reagent is connected.
Further, described colorimetric assay system comprises a detection cell, is provided with a colorimetric detector in described detection cell, and described colorimetric detector is connected with a signal acquisition process terminal.
For a detection method for the device of azo colouring agent on-line checkingi, it is characterized in that comprising the following steps:
Step S1: configure buffer reagent, go back original reagent, acid reagent, diazo reagent, masking reagent and chromogenic reagent;
Step S2: each reagent of distilled water, testing sample, step S1 configuration is injected corresponding reagent bottle;
Step S3: start the corresponding pump housing with the flow velocity of 1.0mL/min by described buffer solution, go back original reagent and testing sample input four-way valve mix, stop the pump housing after 10 seconds;
Step S4: control described electronic temperature control device heating-up temperature to 70 degree Celsius, sends into the mixed liquor in four-way valve in described reduction reactor simultaneously and reacts 10min;
Step S5: start the pump housing be connected with the reagent bottle that distilled water is housed, the mixed liquor promoted in reduction reactor enters fast after described diazo-reaction device through described refrigeratory and stops the pump housing; Then start the pump housing be connected with the reagent bottle that acid reagent is housed and reagent bottle that diazo reagent is housed respectively, in described diazo-reaction device, inject sulphate reagent and diazo reagent with the flow velocity of 1.0mL/min, within 10 seconds, stop the pump housing afterwards and react 3min;
Step S6: start the pump housing be connected with the reagent bottle that distilled water is housed, stops the pump housing after the mixed liquor promoted in diazo-reaction device enters described chromogenic reaction device fast; Then start the pump housing be connected with the reagent bottle that masking reagent is housed, in described chromogenic reaction device, inject masking reagent with the flow velocity of 1.0mL/min, within 10 seconds, stop the pump housing afterwards and react 3min; Then start the pump housing be connected with the reagent bottle that chromogenic reagent is housed, in described chromogenic reaction device, inject chromogenic reagent with the flow velocity of 1.0mL/min, within 10 seconds, stop the pump housing afterwards and react 15min;
Step S7: start the pump housing be connected with the reagent bottle that distilled water is housed, mixed liquor in chromogenic reaction device is delivered into detection cell, by colorimetric detector and signal acquisition process terminal, the content that online colorimetric analysis draws azo colouring agent in testing sample is carried out to mixed liquor.
Further, described buffer reagent is the citrate solution of pH=6.0, describedly go back the hydrogensulfite solution that original reagent is 0.20mol/L, described acid reagent is the sulfuric acid solution of 0.10mol/L, described diazo reagent to be mass content be 5% nitrite natrium solution, described masking reagent to be mass content be 2.5% sulfaminic acid amine aqueous solution, described chromogenic reagent to be mass content be 2% N-(1-naphthyl) ethylenediamine-hydrochloride solution.
The present invention compared with prior art has following beneficial effect: the present invention robotization can carry out online thermocatalysis sodium dithionate reduction azo colouring agent, the control inputs pump housing makes to react the reactant liquor acquired a certain degree and enters diazotising and chromogenic reaction system successively fast, improve the molar absorptivity of azo colouring agent, realization response system is at the direct sensitive analysis of aubergine spectrum range, the present invention is based on online conveying and online RCS, by on-line control reaction reagent addition sequence and equivalent, the reaction of accurate control differential responses system, simple to operate, efficiently, avoid sample heating in conventional colorimetric analysis, cooling, the factors such as reagent interpolation cause the problems such as reaction instability, improve analysis efficiency high, result is stablized, it also avoid in colorant if the light color such as Basic Orange are the restriction that colorant causes detection sensitivity on the low side because self absorptivity is little, analysis efficiency is high, detect sensitive, can be applicable to the automated analysis of azo colouring agent total amount in testing sample.
Accompanying drawing explanation
Fig. 1 is the apparatus structure schematic diagram of one embodiment of the invention.
In figure: 1-is equipped with the reagent bottle of distilled water; 2-is equipped with the reagent bottle of buffer reagent; 3-is equipped with the reagent bottle going back original reagent; 4-is equipped with the reagent bottle of testing sample; 5-contains the reagent bottle of acid reagent; 6-contains the reagent bottle of diazo reagent; 7-contains the reagent bottle of masking reagent; 8-contains the reagent bottle of chromogenic reagent; The 9-pump housing; 10-four-way valve; 11-electronic temperature control device; 12-reduction reactor; 13-refrigeratory; 14,15,17, the 18-pump housing; 16-diazo-reaction device; 19-chromogenic reaction device; 20-colorimetric assay system.
Embodiment
Below in conjunction with drawings and Examples, the present invention will be further described.
Please refer to Fig. 1, the present embodiment provides a kind of device for azo colouring agent on-line checkingi, comprises the constant flow pump induction system, reduction reaction system, diazo-reaction system, chromogenic reaction system and the colorimetric assay system 20 that connect successively.
In the present embodiment, described constant flow pump induction system comprises reagent bottle 2, that a reagent bottle 1, that distilled water is housed is equipped with buffering agent and the reagent bottle 4 that the reagent bottle 3 and going back original reagent is equipped with testing sample is housed; Described distilled water is housed reagent bottle 1, the reagent bottle 2 that buffering agent is housed, the reagent bottle 3 going back original reagent is housed and the reagent bottle 4 that testing sample is housed is connected with a four-way valve 10 through a pump housing 9 respectively.
In the present embodiment, described reduction reaction system comprises an electronic temperature control device 11 and and is arranged at reduction reactor 12 in described electronic temperature control device 11, and the input end of described reduction reactor 12 is connected with described four-way valve 10.
In the present embodiment, described diazo-reaction system comprises a refrigeratory 13, described refrigeratory 13 is connected with the output terminal of described reduction reactor 12 and a diazo-reaction device 16 respectively, the reagent bottle 5 that described diazo-reaction device 16 is equipped with acid reagent through the pump housing 14 and is connected, and the reagent bottle 6 that described diazo-reaction device 16 is equipped with diazo reagent through the pump housing 15 and is connected.
In the present embodiment, described chromogenic reaction system comprises a chromogenic reaction device 19, described chromogenic reaction device 19 is connected with described diazo-reaction device 16, the reagent bottle 7 that described chromogenic reaction device 19 is equipped with masking reagent through the pump housing 17 and is connected, and the reagent bottle 8 that described chromogenic reaction device 19 is equipped with chromogenic reagent through the pump housing 18 and is connected.
In the present embodiment, described colorimetric assay system comprises a detection cell, a colorimetric detector is provided with in described detection cell, described colorimetric detector is connected with a signal acquisition process terminal, described signal acquisition process terminal is the terminal handler of integrated electro signals collecting, process, comprises control chip, display and Data Control button.
The present embodiment also provides a kind of detection method of the device for azo colouring agent on-line checkingi, it is characterized in that comprising the following steps:
Step S1: configure buffer reagent, go back original reagent, acid reagent, diazo reagent, masking reagent and chromogenic reagent; Wherein said buffer reagent is the citrate solution of pH=6.0, describedly go back the hydrogensulfite solution that original reagent is 0.20mol/L, described acid reagent is the sulfuric acid solution of 0.10mol/L, described diazo reagent to be mass content be 5% nitrite natrium solution, described masking reagent to be mass content be 2.5% sulfaminic acid amine aqueous solution, described chromogenic reagent to be mass content be 2% N-(1-naphthyl) ethylenediamine-hydrochloride solution;
Step S2: each reagent of distilled water, testing sample, step S1 configuration is injected corresponding reagent bottle;
Step S3: start the corresponding pump housing with the flow velocity of 1.0mL/min by described buffer solution, go back original reagent and testing sample input four-way valve 10 mix, stop the pump housing after 10 seconds;
Step S4: control described electronic temperature control device 11 heating-up temperature to 70 degree Celsius, sent in described reduction reactor 12 by the mixed liquor in four-way valve 10 simultaneously and react 10min, described reduction reactor 12 is the type reactor that spirals;
Step S5: start the pump housing 9 be connected with the reagent bottle 1 that distilled water is housed, the mixed liquor promoted in reduction reactor 12 enters fast after described diazo-reaction device 16 through described refrigeratory 13 and stops the pump housing 9; Then the pump housing 15 be connected with the pump housing 14 of the reagent bottle 5 that acid reagent is housed and reagent bottle that diazo reagent 6 is housed is started respectively, in described diazo-reaction device 16, inject sulphate reagent and diazo reagent with the flow velocity of 1.0mL/min, within 10 seconds, stop the pump housing afterwards and react 3min;
Step S6: start the pump housing 9 be connected with the reagent bottle 1 that distilled water is housed, the mixed liquor promoted in diazo-reaction device 16 stops the pump housing 9 after entering described chromogenic reaction device 19 fast; Then start the pump housing 17 be connected with the reagent bottle 7 that masking reagent is housed, in described chromogenic reaction device 19, inject masking reagent with the flow velocity of 1.0mL/min, within 10 seconds, stop the pump housing 17 afterwards and react 3min; Then start the pump housing 18 be connected with the reagent bottle 8 that chromogenic reagent is housed, in described chromogenic reaction device 19, inject chromogenic reagent with the flow velocity of 1.0mL/min, within 10 seconds, stop the pump housing 18 afterwards and react 15min;
Step S7: start the pump housing 9 be connected with the reagent bottle that distilled water 1 is housed, mixed liquor in chromogenic reaction device 19 is delivered into detection cell, by colorimetric detector and signal acquisition process terminal, the content that online colorimetric analysis draws azo colouring agent in testing sample is carried out to mixed liquor.
The foregoing is only preferred embodiment of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (8)
1. for a device for azo colouring agent on-line checkingi, it is characterized in that: comprise the constant flow pump induction system, reduction reaction system, diazo-reaction system, chromogenic reaction system and the colorimetric assay system that connect successively.
2. the device for azo colouring agent on-line checkingi according to claim 1, is characterized in that: described constant flow pump induction system comprises the reagent bottle, that a reagent bottle, that distilled water is housed is equipped with buffering agent and the reagent bottle that the reagent bottle and going back original reagent is equipped with testing sample is housed; Described distilled water is housed reagent bottle, the reagent bottle that buffering agent is housed, the reagent bottle going back original reagent is housed and the reagent bottle that testing sample is housed is connected with a four-way valve through a pump housing respectively.
3. the device for azo colouring agent on-line checkingi according to claim 2, it is characterized in that: described reduction reaction system comprises an electronic temperature control device and and is arranged at reduction reactor in described electronic temperature control device, and the input end of described reduction reactor is connected with described four-way valve.
4. the device for azo colouring agent on-line checkingi according to claim 3, it is characterized in that: described diazo-reaction system comprises a refrigeratory, described refrigeratory is connected with the output terminal of described reduction reactor and a diazo-reaction device respectively, and the reagent bottle that the reagent bottle and that described diazo-reaction device is also equipped with acid reagent through a pump housing and is respectively equipped with diazo reagent is connected.
5. the device for azo colouring agent on-line checkingi according to claim 4, it is characterized in that: described chromogenic reaction system comprises a chromogenic reaction device, described chromogenic reaction device is connected with described diazo-reaction device, and the reagent bottle that the reagent bottle and that described chromogenic reaction device is also equipped with masking reagent through a pump housing and is respectively equipped with chromogenic reagent is connected.
6. the device for azo colouring agent on-line checkingi according to claim 5, it is characterized in that: described colorimetric assay system comprises a detection cell, be provided with a colorimetric detector in described detection cell, described colorimetric detector is connected with a signal acquisition process terminal.
7., based on a detection method for the device for azo colouring agent on-line checkingi described in any one of claim 1-6, it is characterized in that comprising the following steps:
Step S1: configure buffer reagent, go back original reagent, acid reagent, diazo reagent, masking reagent and chromogenic reagent;
Step S2: each reagent of distilled water, testing sample, step S1 configuration is injected corresponding reagent bottle;
Step S3: start the corresponding pump housing with the flow velocity of 1.0mL/min by described buffer solution, go back original reagent and testing sample input four-way valve mix, stop the pump housing after 10 seconds;
Step S4: control described electronic temperature control device heating-up temperature to 70 degree Celsius, sends into the mixed liquor in four-way valve in described reduction reactor simultaneously and reacts 10min;
Step S5: start the pump housing be connected with the reagent bottle that distilled water is housed, the mixed liquor promoted in reduction reactor enters fast after described diazo-reaction device through described refrigeratory and stops the pump housing; Then start the pump housing be connected with the reagent bottle that acid reagent is housed and reagent bottle that diazo reagent is housed respectively, in described diazo-reaction device, inject sulphate reagent and diazo reagent with the flow velocity of 1.0mL/min, within 10 seconds, stop the pump housing afterwards and react 3min;
Step S6: start the pump housing be connected with the reagent bottle that distilled water is housed, stops the pump housing after the mixed liquor promoted in diazo-reaction device enters described chromogenic reaction device fast; Then start the pump housing be connected with the reagent bottle that masking reagent is housed, in described chromogenic reaction device, inject masking reagent with the flow velocity of 1.0mL/min, within 10 seconds, stop the pump housing afterwards and react 3min; Then start the pump housing be connected with the reagent bottle that chromogenic reagent is housed, in described chromogenic reaction device, inject chromogenic reagent with the flow velocity of 1.0mL/min, within 10 seconds, stop the pump housing afterwards and react 15min;
Step S7: start the pump housing be connected with the reagent bottle that distilled water is housed, mixed liquor in chromogenic reaction device is delivered into detection cell, by colorimetric detector and signal acquisition process terminal, the content that online colorimetric analysis draws azo colouring agent in testing sample is carried out to mixed liquor.
8. the detection method of the device for azo colouring agent on-line checkingi according to claim 7, it is characterized in that: described buffer reagent is the citrate solution of pH=6.0, describedly go back the hydrogensulfite solution that original reagent is 0.20mol/L, described acid reagent is the sulfuric acid solution of 0.10mol/L, described diazo reagent to be mass content be 5% nitrite natrium solution, described masking reagent to be mass content be 2.5% sulfaminic acid amine aqueous solution, described chromogenic reagent to be mass content be 2% N-(1-naphthyl) ethylenediamine-hydrochloride solution.
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