CN103398961A - Microfluidic glass chip used for detecting chemical oxygen demand, and preparation method thereof - Google Patents
Microfluidic glass chip used for detecting chemical oxygen demand, and preparation method thereof Download PDFInfo
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- CN103398961A CN103398961A CN2013103418202A CN201310341820A CN103398961A CN 103398961 A CN103398961 A CN 103398961A CN 2013103418202 A CN2013103418202 A CN 2013103418202A CN 201310341820 A CN201310341820 A CN 201310341820A CN 103398961 A CN103398961 A CN 103398961A
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Abstract
The invention relates to a microfluidic glass chip used for detecting chemical oxygen demand, and a preparation method thereof. A microstructure and a micro channel are provided on the surface of the disc-shaped microfluidic chip; under the driving of centrifugal force generated by the rotation of a centrifuge, mixing, reaction, and separation processes of a sample to be detected and a reagent pack are realized; and the chemical oxygen demand of the sample on the detection chip can be quantitatively or qualitatively detected with an ultraviolet-visible spectrophotometer. With the microfluidic chip, a plurality of samples can be simultaneously treated and detected. Reagent and sample doses are low. Such that chemical oxygen demand detection integration, miniaturization, and automation are realized. The chip is economical, fast, and convenient. With the chip, a novel analysis technology is provided for the detection of chemical oxygen demand in water body. The microfluidic glass chip is mainly used in fields such as environment protection, water quality detection, and the like.
Description
Technical field
the present invention relates to a kind of micro-fluidic glass-chip that detects chemical oxygen demand (COD) in water body and preparation method thereof, there are microstructure and microchannel in this discoid micro-fluidic glass-chip surface, under the centrifugal force that the hydro-extractor rotation produces drives, realize mixing of testing sample and pack, the reaction and separation processes process, with ultraviolet-visible spectrophotometer content of chemical oxygen demand (COD) in sample quantitatively or on the qualitative detection chip, a plurality of samples can be processed and detect to this micro-fluidic glass-chip and method simultaneously, reagent and amount of samples are few, realized the integrated of chemical oxygen demand detection, microminiaturized, robotization, has economy, fast, portable characteristics, for the detection of chemical oxygen demand (COD) in water body provides a kind of brand-new analytical technology.Be mainly used in the fields such as environmental protection, water quality detection.
Background technology
Chemical oxygen demand COD (Chemical Oxygen Demand) is chemically to measure in water sample the amount that needs oxidized reducing substances.It has reflected the degree that polluted by reducing substances.This index is also as one of overall target of organism relative content.High meaning in water of chemical oxygen demand (COD) contained a large amount of reducing substanceses, is mainly wherein organic contaminant.Chemical oxygen demand (COD) is higher, just represents that the Organic Pollution of river is more serious, and the source of these Organic Pollutions may be agricultural chemicals, chemical plant, organic fertilizer etc.If do not process, many organic contaminants can adsorbed by bed mud at the bottom of river and, under depositing, within the several years from now on, hydrobiont caused to lasting toxic action.After the hydrobiont mass mortality, the ecosystem of korneforos is namely destroyed.If the people, take the biology in water as food, can absorb the toxin in these biosomes in a large number, in vivo, that these poisonous substances often have is carcinogenic, teratogenesis shape, mutagenic effect, extremely dangerous to the people in accumulation.Therefore, foundation simply, Development for Determination of COD is very necessary fast and effectively.The chemical oxygen demand (COD) content detection is of great significance at tool aspect environmental protection, water quality detection.
Traditional assay method of chemical oxygen demand (COD) has had relevant national standard, but the disadvantage of the method is that amount of samples is large, the sample pretreatment process time is long, cost is higher, and the sample separation process is separately independently carried out with detecting, easily cause sample loss and pollution, be not suitable for the integrated of on-the-spot Fast Measurement and micro-analysis system, can not meet the needs of micro-total analysis system development.
Therefore, in the urgent need to developing a kind of quick, efficient, convenient, low-cost, robotization, collection sample pretreatment and detecting the detection method of one.In recent years, micro-fluidic glass-chip is as a kind of novel analysis platform, has microminiaturization, robotization, the advantage such as integrated, convenient and quick, in the environment measuring association area, obtains a wide range of applications.Yet, adopt the disc-shaped chip, in its surface preparation microstructure and microchannel, be used for analyzing, rely on centrifugal force to drive microstream, complete simultaneously the centrifugal type microfludic glass-chip technology of several sample analysis, the fast detecting application in chemical oxygen demand (COD) not yet has substantial breakthrough at present.
Summary of the invention
the purpose of this invention is to provide a kind of centrifugal type microfludic glass-chip that detects chemical oxygen demand (COD) and preparation method thereof, it is characterized in that this chip is the centrifugal type microfludic glass-chip of disc-shaped band microstructure and microchannel, substrate by the microstructure that is carved with micron level and microchannel, blank substrate thermocompression bonding forms, under the centrifugal force that the hydro-extractor rotation produces drives, complete testing sample and detect mixing of pack, the reaction and separation processes process, with the ultraviolet-visible spectrophotometer pick-up unit, the content of chemical oxygen demand (COD) in sample on detection chip quantitatively or qualitatively.
For achieving the above object, the present invention adopts following operation steps:
1) by microstructure and the microchannel of micro-processing technology at micro-fluidic glass-chip substrate surface machining need, comprise micro-sample cell, detection cell, microchannel and micropore.
2) testing sample is put into to micro-sample cell.
3) by the thermocompression bonding method, microstructure substrate and the blank substrate thermocompression bonding of being carved with micron level are formed to the centrifugal type microfludic glass-chip.
4) after involution, in sample cell, add pack.
5) chip is put into to hydro-extractor, set centrifugal speed, testing sample and pack are mixed under centrifugal action, reaction and separation processes is to detection cell.
6) chip is put into to baking oven, heating, after 15 minutes, is taken out chip and is cooled to room temperature under 150 ℃;
7) test wavelength 600nm place absorbance on ultraviolet-visible spectrophotometer, thus testing sample chemical oxygen demand (COD) content calculated.
In the present invention, the chip substrates that detects the centrifugal type microfludic glass-chip of chemical oxygen demand (COD) can be to be quartz glass or simple glass disk.
In the present invention, microstructure and the microchannel of detecting the centrifugal type microfludic glass-chip of chemical oxygen demand (COD) can be by chemical etching method in the preparations of chip substrates surface.
In the present invention, between the chip of the centrifugal type microfludic glass-chip of detection chemical oxygen demand (COD), with the pressure sintering bonding, form.
In the present invention, detect the width and the degree of depth that between sample and the detection cell of centrifugal type microfludic glass-chip of chemical oxygen demand (COD), are connected microchannel and be 380 μ m, insert external diameter 375 μ m, the quartz capillary of internal diameter 25,50,75 or 100 μ m, as passive valve, the internal diameter of quartz capillary is less, and microfluid is larger by the required centrifugal force of quartz capillary, and required centrifugal rotational speed is just higher.
In the present invention, the length of quartz ampoule reserved 0.5-1mm in micro-sample cell, play the effect of holding back solid particle in micro-sample cell.
In the present invention, when the pack of the centrifugal type microfludic glass-chip of detection chemical oxygen demand (COD) and sample mix reaction, centrifuge speed is 150～300 rev/mins, and it is 700～1000 rev/mins by centrifugal rotational speed capillaceous that mixed reaction solution liquid separates.
In the present invention, the pack that detects the centrifugal type microfludic glass-chip of chemical oxygen demand (COD) is potassium dichromate digestion solution, sulfuric acid-silver sulfate catalyzer and mercuric sulfate screening agent.
In the present invention, the collocation method of potassium dichromate digestion solution is: take the 4.9g potassium dichromate, 25.0g aluminium potassium sulfate, 5.0g ammonium molybdate.Be dissolved in about 250ml water, add the 100ml concentrated sulphuric acid, be transferred to the 500ml volumetric flask after cooling, add water to graticule.
In the present invention, the collocation method of sulfuric acid-silver sulfate catalyst solution is: take silver sulfate 5.0g, be dissolved in the 500mL concentrated sulphuric acid, and cooling rear stand-by.
In the present invention, the collocation method of screening agent is: take mercuric sulfate 10.0g, be dissolved in 100mL10% sulfuric acid, and cooling rear stand-by.
This analyzing and testing chip is furnished with special-purpose centrifugal and optical detection integrated module, and the step that simplifies the operation improves detection efficiency.
The centrifugal type microfludic glass-chip of the detection chemical oxygen demand (COD) that the present invention proposes, can realize the Parallel testing of a plurality of samples, reduced the consumption of reagent and sample size, reduced the time that testing sample is processed and detected, have portable, economic, characteristics fast and efficiently, in the analyzing and testing of chemical oxygen demand (COD), have a good application prospect.
The accompanying drawing explanation
Fig. 1 is the schematic layout pattern that detects the centrifugal type microfludic glass-chip of chemical oxygen demand (COD).
Fig. 2 is the structural representation of one group of sample analysis detecting unit: 1) sample cell, 2) detection cell, 3) kapillary, 4) air hole, 5) the kapillary length in reserve.
Fig. 3 is centrifugal for this chip and detects one platform schematic diagram.1) light source, 2) optical fiber, 3) collimation lens, 4) integrated detection cell, 5) condenser lens, 6) optical fiber, 7) the photodiode array spectrometer.
Specific embodiments
By chemical corrosion method in the required microstructure of glass baseplate surface working and microchannel, comprise micro-sample cell, detection cell, microchannel and micropore, finally with tap water, distilled water, clean substrate respectively, and with spots such as the residual fingerprint of ethanol substrate surface, oil stains.To be carved with the substrate of micro-pattern, blank substrate Heat Sealing, make the centrifugal type microfludic detection chip that detects chemical oxygen demand (COD).The 5ml testing sample is positioned over respectively in each sample cell, the centrifugal type microfludic glass-chip is fixed in to the hydro-extractor rotation and detects on the one platform, at each sample filling orifice place, add potassium dichromate digestion solution, sulfuric acid-silver sulfate catalyzer and each 1ml of mercuric sulfate screening agent, after the rotating speeds mixing of 300 rev/mins, reaction 10min, improve rotating speed to 1000 rev/min, reaction mixture in sample cell is all moved to detection cell, chip is put into to baking oven, under 150 ℃, heating, after 15 minutes, is taken out chip and is cooled to room temperature; At the 600nm place, carry out absorbance detection, finally obtain the content of chemical oxygen demand (COD) in sample.
Claims (10)
1. one kind is detected micro-fluidic glass-chip of chemical oxygen demand (COD) and preparation method thereof, it is characterized in that, this chip is the micro-fluidic glass-chip of disc-shaped band microstructure and microchannel, microstructure substrate and the blank substrate thermocompression bonding of by a slice, being carved with micron level form, centrifugal driving force by hydro-extractor, complete the mixing of testing sample and pack, reaction and separation processes process, take ultraviolet-visible spectrophotometer as pick-up unit, the content of chemical oxygen demand (COD) in sample on detection chip quantitatively or qualitatively.Prepared by micro-processing technology by microstructure, comprise micro-sample cell, detection cell, microchannel and micropore.
2. press micro-fluidic glass-chip of detection chemical oxygen demand (COD) claimed in claim 1 and preparation method thereof, it is characterized in that, its making step is as follows:
1) by microstructure and the microchannel of micro-processing technology at micro-fluidic glass-chip substrate surface machining need, comprise micro-sample cell, detection cell, microchannel and micropore;
2) testing sample is put into to micro-sample cell;
3) by the thermocompression bonding method, microstructure substrate and the blank substrate thermocompression bonding of being carved with micron level are formed to the centrifugal type microfludic glass-chip;
4) after involution, in sample cell, add pack;
5) chip is put into to hydro-extractor, set centrifugal speed, testing sample and pack are mixed under centrifugal action, reaction and separation processes is to detection cell;
6) chip is put into to baking oven, heating, after 15 minutes, is taken out chip and is cooled to room temperature under 150 ℃;
7) test wavelength 600nm place absorbance on ultraviolet-visible spectrophotometer, thus testing sample chemical oxygen demand (COD) content calculated.
3. by right, ask micro-fluidic glass-chip of 1 or 2 described detection chemical oxygen demand (COD) and preparation method thereof, it is characterized in that, the base material of this detection chip can be quartz glass or simple glass.
4. by right, ask micro-fluidic glass-chip of 1 or 2 described detection chemical oxygen demand (COD) and preparation method thereof, it is characterized in that, this detection chip can directly complete sample pretreatment and detection on chip.
5. press micro-fluidic glass-chip of the described detection chemical oxygen demand (COD) of claim 1 or 2 and preparation method thereof, it is characterized in that, this detection chip can, at chip piece by becoming many group sample analysis detecting units form, improve the Parallel testing ability of unit interval.
6. press micro-fluidic glass-chip of the described detection chemical oxygen demand (COD) of claim 1 or 2 and preparation method thereof, it is characterized in that, micro-valve of the detection chip of this chemical oxygen demand (COD) is embedded in microchannel and is formed by quartz capillary, by controlling internal diameter capillaceous, regulate and control the minimum flow velocity capillaceous that passes through of microfluid, the internal diameter of quartz capillary is less, microfluid is larger by the required centrifugal force of this quartz capillary, and centrifugal rotational speed is just higher.
7. press micro-fluidic glass-chip of the described detection chemical oxygen demand (COD) of claim 1 or 2 and preparation method thereof, it is characterized in that, the length of quartz ampoule reserved 0.5-1mm in micro-sample cell, play the effect of holding back solid particle in micro-sample cell.
8. press micro-fluidic glass-chip of the described detection chemical oxygen demand (COD) of claim 1 or 2 and preparation method thereof, it is characterized in that, pack is potassium dichromate digestion solution, sulfuric acid-silver sulfate catalyzer and mercuric sulfate screening agent.
9. press micro-fluidic glass-chip of the described detection chemical oxygen demand (COD) of claim 1 or 2 and preparation method thereof, it is characterized in that, the chip substrates that detects the centrifugal type microfludic glass-chip of chemical oxygen demand (COD) can be to be quartz glass or simple glass disk.
10. press micro-fluidic glass-chip of the described detection chemical oxygen demand (COD) of claim 1 or 2 and preparation method thereof, it is characterized in that, this analyzing and testing chip is furnished with special-purpose centrifugal and optical detection integrated module, and the step that simplifies the operation improves detection efficiency.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104001562A (en) * | 2014-06-09 | 2014-08-27 | 南京大学 | Disc centrifugation type micro-fluidic chip and device for rapid chromium form separation |
| CN104928163A (en) * | 2015-05-29 | 2015-09-23 | 河北工业大学 | Micro-fluidic chip used for raw milk body cell counting |
| CN105964313A (en) * | 2016-01-22 | 2016-09-28 | 上海快灵生物科技有限公司 | Centrifugal type multi-channel microfluidic chip |
| CN106596877A (en) * | 2015-10-14 | 2017-04-26 | 孙诗文 | Method and reagent composition for measuring chemical oxygen consumption in water |
| CN107064216A (en) * | 2017-04-19 | 2017-08-18 | 哈尔滨工业大学 | A kind of portable COD detection means based on microfluidic chip technology |
| CN107643411A (en) * | 2017-08-11 | 2018-01-30 | 深圳市芯思微生物科技有限公司 | Micro-fluidic chip, its preparation method and application method |
| CN108982824A (en) * | 2018-05-11 | 2018-12-11 | 石家庄禾柏生物技术股份有限公司 | A kind of reagent disc test device |
| CN109441754A (en) * | 2018-11-09 | 2019-03-08 | 中国科学院长春光学精密机械与物理研究所 | A kind of microfluidic system and its micro-fluidic fluid drive apparatus |
| TWI665439B (en) * | 2017-10-12 | 2019-07-11 | 保生國際生醫股份有限公司 | A method for determining chemical oxygen demand of a water sample |
| CN110411963A (en) * | 2019-08-08 | 2019-11-05 | 重庆科技学院 | A kind of portable spectrophotometer of Heavy Metals in Waters ion detection |
| CN110426347A (en) * | 2019-09-04 | 2019-11-08 | 中绿环保科技股份有限公司 | Anti-attenuation photoelectricity regulating water quality monitor |
| CN110470617A (en) * | 2018-05-11 | 2019-11-19 | 中国石油化工股份有限公司 | It can recognize chip and detection method and its application |
| CN110691651A (en) * | 2017-01-09 | 2020-01-14 | Gsg科技有限公司 | Fluid handling cartridge and control mechanism |
| CN113155588A (en) * | 2021-05-13 | 2021-07-23 | 武汉新烽光电股份有限公司 | Rapid automatic water quality detection system and method based on micro-fluidic |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104001562A (en) * | 2014-06-09 | 2014-08-27 | 南京大学 | Disc centrifugation type micro-fluidic chip and device for rapid chromium form separation |
| CN104928163A (en) * | 2015-05-29 | 2015-09-23 | 河北工业大学 | Micro-fluidic chip used for raw milk body cell counting |
| CN106596877A (en) * | 2015-10-14 | 2017-04-26 | 孙诗文 | Method and reagent composition for measuring chemical oxygen consumption in water |
| CN105964313B (en) * | 2016-01-22 | 2019-04-09 | 上海快灵生物科技有限公司 | A kind of centrifugal multi-channel fluid chip |
| CN105964313A (en) * | 2016-01-22 | 2016-09-28 | 上海快灵生物科技有限公司 | Centrifugal type multi-channel microfluidic chip |
| CN110691651A (en) * | 2017-01-09 | 2020-01-14 | Gsg科技有限公司 | Fluid handling cartridge and control mechanism |
| CN107064216A (en) * | 2017-04-19 | 2017-08-18 | 哈尔滨工业大学 | A kind of portable COD detection means based on microfluidic chip technology |
| CN107643411A (en) * | 2017-08-11 | 2018-01-30 | 深圳市芯思微生物科技有限公司 | Micro-fluidic chip, its preparation method and application method |
| TWI665439B (en) * | 2017-10-12 | 2019-07-11 | 保生國際生醫股份有限公司 | A method for determining chemical oxygen demand of a water sample |
| CN108982824A (en) * | 2018-05-11 | 2018-12-11 | 石家庄禾柏生物技术股份有限公司 | A kind of reagent disc test device |
| CN110470617A (en) * | 2018-05-11 | 2019-11-19 | 中国石油化工股份有限公司 | It can recognize chip and detection method and its application |
| CN108982824B (en) * | 2018-05-11 | 2023-11-10 | 石家庄禾柏生物技术股份有限公司 | Reagent disk testing device |
| CN109441754A (en) * | 2018-11-09 | 2019-03-08 | 中国科学院长春光学精密机械与物理研究所 | A kind of microfluidic system and its micro-fluidic fluid drive apparatus |
| CN110411963A (en) * | 2019-08-08 | 2019-11-05 | 重庆科技学院 | A kind of portable spectrophotometer of Heavy Metals in Waters ion detection |
| CN110426347A (en) * | 2019-09-04 | 2019-11-08 | 中绿环保科技股份有限公司 | Anti-attenuation photoelectricity regulating water quality monitor |
| CN113155588A (en) * | 2021-05-13 | 2021-07-23 | 武汉新烽光电股份有限公司 | Rapid automatic water quality detection system and method based on micro-fluidic |
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Application publication date: 20131120 |