CN101776581A - Method for photometric analysis of trace pollutant in water sample and device thereof - Google Patents
Method for photometric analysis of trace pollutant in water sample and device thereof Download PDFInfo
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- CN101776581A CN101776581A CN200910156637A CN200910156637A CN101776581A CN 101776581 A CN101776581 A CN 101776581A CN 200910156637 A CN200910156637 A CN 200910156637A CN 200910156637 A CN200910156637 A CN 200910156637A CN 101776581 A CN101776581 A CN 101776581A
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Abstract
The invention discloses a method for photometric analysis of trace pollutants in a water sample, which comprises the following steps: a, guiding a quantified water sample to be tested and a reagent matched with pollutants to be tested into a reaction unit, thereby generating reaction products in the reaction unit through reaction of the water sample to be tested and the reagent; b, making the reaction solution with the reaction products flow through a concentration unit, so that the reaction products can be combined with a carrier in the concentration unit and can be concentrated on the carrier; c, detecting the concentration unit with a luminosity detection unit so as to obtain the content or concentration of the pollutants to be tested in the water sample. The invention also discloses an analysis device which can apply the analysis method. Moreover, the invention has the advantages of high measurement sensitivity, low requirements for the detection unit and the like.
Description
Technical field
The present invention relates to a kind of water quality detection, relate in particular to a kind of method for photometric analysis and device that can detect contaminant trace species in the water sample.
Background technology
Analytical photometry has characteristics such as analysis result accuracy height, good stability, is widely used in the water analysis field.The photometric analysis ratio juris is: under specific acid-base condition, developer optionally reacts the reaction of formation compound with the target detection thing, carry out photometric detection then, obtain the concentration or the content of target detection thing in the original solution at last according to the absorbance of reaction product.As the ammonia nitrogen analysis, standard " the mensuration nessler reagent colourimetry of water quality ammonium " (GB 7479-87) regulation, under strong alkaline condition, ammonia in the water sample and nessler reagent reaction generate the yellowish-brown complex compound, in 420nm place photometric detection, calculate the ammonia nitrogen concentration of water sample at last according to the absorbance of reactant liquor then.Automated analysis instrument based on photometry generally comprises parts compositions such as auto injection unit, reagent switch unit, reaction member, detecting unit, as shown in Figure 1.
Although analytical photometry has advantages such as good stable and accuracy, but it detects lower limit and generally can only reach about 0.1mg/L, be difficult to satisfy volatile phenol in the surface water, lead, cadmium, the isoparametric analysis of mercury (wherein surface water standard-required I class water volatile phenol content is lower than 0.002mg/L), limited photometry application aspect the contaminant trace species analysis in water sample greatly.
Summary of the invention
In order to solve the limitation problem that prior art medium sensitivity is low, be difficult to satisfy contaminant trace species analyzing and testing demand, the invention provides a kind of highly sensitive, good stability, water quality contaminant trace species analytical approach that reliability is high, a kind of highly sensitive, good stability, reliability height, productibility and maintainable good water quality contaminant trace species analytical equipment also are provided.
For achieving the above object, the present invention is by the following technical solutions:
The method for photometric analysis of contaminant trace species in a kind of water sample may further comprise the steps:
A, with quantitative water sample to be measured, import in the reaction member with the reagent of pollutant to be measured coupling;
Water sample to be measured and reagent are at reaction member reaction of formation product;
B, have reaction product reactant liquor by the enrichment unit, carrier in reaction product and enrichment unit knot is incorporated in enrichment on the carrier;
C, photometric detection unit detect described enrichment unit, thereby obtain the content or the concentration of pollutant to be measured in the water sample.
Further, also comprise elution step: use the reaction product on the eluant, eluent wash-out carrier.
As preferably, described carrier is macroporous absorbent resin, ion exchange resin, fiber, silica gel, PTFE microballon, nano material, activated charcoal, activated alumina or gel.
In above-mentioned analytical approach, detect transmitance or scattered power or the absorbance of enrichment unit to light.
As preferably, adopt the hyperchannel selection valve, the public passage on this valve connects liquid storage unit and pump;
Select water sample passage, the reagent passage of hyperchannel selection valve respectively, pump is drawn into water sample, reagent in the liquid storage unit respectively;
Select the reaction channel of hyperchannel selection valve, pump is delivered to the water sample in the liquid storage unit, reagent in the reaction member.
Further, after water sample, reagent were delivered to reaction member, pump was by the air duct extracting air;
Select the reaction channel of hyperchannel selection valve, pump is delivered to the air that extracts in the reaction member, has stirred, mixed water sample, reagent in the reaction member.
As preferably, described air duct be arranged on the hyperchannel selection valve or with pump and valve that the liquid storage unit is connected on.
In order to realize said method, the invention allows for the photometric analysis device of contaminant trace species in a kind of like this water sample, comprise switch unit, reaction member, pump and detecting unit, detecting unit comprises light source, detector and analysis module; Characteristics are: described analytical equipment also comprises:
Inside is provided with the enrichment unit of enrichment carrier, and the reaction product that is used for reactant liquor that reaction member is discharged is enriched in described carrier;
The reaction product of the rayed that light source sends on carrier, the light signal after detector reception and the reaction product effect, the signal that receives send analysis module.
As preferably, described carrier is macroporous absorbent resin, ion exchange resin, fiber silica gel, PTFE microballon, nano material, activated charcoal, activated alumina or gel.
As preferably, described switch unit adopts the hyperchannel selection valve, this hyperchannel selection valve is provided with public passage, reagent passage, water sample passage, measures passage, reaction channel, described public passage connects liquid storage unit and pump, described measurement passage connects the enrichment unit, described reaction channel connects mixing-reaction member, and described analytical equipment also comprises air duct.
As preferably, described air duct is arranged on the hyperchannel selection valve.
As preferably, described pump connects the liquid storage unit by valve, and described air duct is arranged on this valve.
Compared with prior art, the present invention has the following advantages:
1, by of the enrichment of enrichment unit, improved Sensitivity of Analytical Method, made analytical photometry become possibility the analysis of water quality contaminant trace species to the target detection thing.
2, directly enriching column is detected, to the requirement of detecting unit, make analytical equipment become stable, reliable when having reduced analytical photometry analysis contaminant trace species, improved maintainability.
Analytic process is easy, has simplified analytical equipment.
Description of drawings
Fig. 1 installs synoptic diagram in the background technology;
Fig. 2 is an analytical equipment structural representation among the embodiment 1;
Fig. 3 is an analytical equipment structural representation among the embodiment 2;
Fig. 4 is an analytical equipment structural representation among the embodiment 3.
Embodiment
Embodiment 1:
As shown in Figure 2, the photometric analysis device of a kind of face of land underwater trace phenol comprises syringe pump, liquid storage unit, hyperchannel selection valve, mixing-reaction member, enriching column, photometric detection unit composition.
The hyperchannel selection valve is provided with public passage, reagent passage, water sample passage, measures passage, reaction channel and air duct, reagent passage connects reagent bottles such as buffer solution, the potassium ferricyanide, 4-amino-antipyrine, described public passage connects liquid storage unit and syringe pump, described measurement passage connects enriching column, and described reaction channel connects mixing-reaction member.
Filled resin in the enriching column.
Described photometric detection unit comprises light source, detector and analysis module, is used to detect the reaction product of enrichment in the enriching column.Light source and detector are in the both sides of enriching column.
Present embodiment has also disclosed the method for photometric analysis of a kind of face of land underwater trace phenol, may further comprise the steps:
A, hyperchannel selection valve select the water sample passage respectively, during with reagent passage that each reagent is communicated with, syringe pump is drawn into quantitative water sample, buffer solution, the potassium ferricyanide, 4-amino-antipyrine in the liquid storage unit respectively exactly;
Hyperchannel selection valve choice reaction passage, syringe pump imports to hybrid reaction in mixing-reaction member with the water sample in the liquid storage unit, all ingredients;
The hyperchannel selection valve is selected air duct, and syringe pump extracts the air of certain volume; Hyperchannel selection valve choice reaction passage, syringe pump imports to the air in the liquid storage unit in mixing-reaction member, pneumatic blending water sample, the reagent in mixing-reaction member, water sample, reagent are fully mixed, improve the accuracy of measuring, reduced Measuring Time;
B, treat that phenol in the water sample and mentioned reagent reaction generate the bronzing reactant after, the hyperchannel selection valve selects to measure passage, syringe pump will mix-and reactant liquor in the reaction member leads enriching column and passes through from enriching column, the enrichment on resin of bronzing reactant, and cause resin generation change color;
C, light source send light and pass enriching column, and detector receives and passes the light of enriching column, and is converted into electric signal, and analysis module analytical reactions liquid passes through the variation of the forward and backward absorbance of enriching column, thereby obtain the phenol concentration in the water sample:
The hyperchannel selection valve is selected the reagent passage corresponding to ethanol, the ethanol that extracts certain volume to the liquid storage unit in, hyperchannel selection valve selection measurement passage, syringe pump imports to the ethanol in the liquid storage unit in the enriching column, enriching column is washed, enter wait after enriching column is rinsed and analyze next time.
In the present embodiment, when the sample volume of water sample was 100ml, the sensitivity for analysis of phenol can reach 0.001mg/L.
Embodiment 2:
As shown in Figure 3, the photometric analysis device of trace lead in a kind of surface water comprises the multithread road transfer valve, first peristaltic pump, mixing-reaction member, second peristaltic pump, enriching column, the photometric detection unit that connect successively.
Filled gel in the enriching column.
Described multithread road transfer valve is made up of a plurality of valves, connects water sample, each reagent (as buffer solution, dithizone solution) respectively.
Described photometric detection unit comprises light source, detector and analysis module, is used to detect the reaction product of enrichment in the enriching column.Light source and detector are in the same side of enriching column.
Present embodiment has also disclosed the method for photometric analysis of trace lead in a kind of surface water, may further comprise the steps:
When a, analysis, by the switching of multithread road transfer valve, first peristaltic pump imports to quantitative water sample, buffer solution, dithizone solution exactly respectively in mixing-reaction member and mixes, reacts;
B, treat that lead in the water sample and mentioned reagent reaction generate red reactant after, second peristaltic pump is led reactant liquor enriching column and is passed through from enriching column from mixing-reaction member, red reactant enrichment on gel, and cause gel generation change color;
The rayed that c, light source send is on enriching column, and detector detects the variation of enriching column to the scattering of light rate of 510nm wavelength, and analysis module is through obtaining the lead concentration in the water sample after calculating;
By the switching of valve, first peristaltic pump and second peristaltic pump import to methenyl choloride in the enriching column, and the flushing enriching column enters after enriching column is rinsed and waits for analysis state next time.
Embodiment 3:
As shown in Figure 4, the photometric analysis device of Trace Hg in a kind of surface water, as different from Example 1:
1, filled the PTFE microballon in the enriching column.
2, syringe pump is communicated with the liquid storage unit by valve (as T-valve), and air duct is arranged on this valve.Air duct no longer is set on the hyperchannel selection valve.
3, the reagent of Shi Yonging changes into: acetate-sodium acetate buffer solution, microemulsion solution, the adjacent nitro-azo arsine of dibromo etc.
Present embodiment has also disclosed the method for photometric analysis of Trace Hg in a kind of surface water, as different from Example 1:
1, owing to the pollutant difference of measuring, the reagent of use changes into: acetate-sodium acetate buffer solution, microemulsion solution, the adjacent nitro-azo arsine of dibromo etc.
2, in step a, after syringe pump imports to mixing-reaction member with the water sample in the liquid storage unit and reagent; Syringe pump extracts the air of certain volume by air duct, hyperchannel selection valve choice reaction passage, syringe pump imports the air that extracts in the mixing-reaction member, water sample and reagent have been stirred, make between water sample and reagent and fully mix, react, improve the accuracy of measuring, reduced Measuring Time.
Above-mentioned embodiment should not be construed as limiting the scope of the invention.As, potting resin, gel and PTFE microballon can also be nano material, activated charcoal or activated alumina certainly in the enriching column.Key of the present invention is: the reactant liquor of water sample and reagent is enriched with the reaction product that water sample and reagent generate by the enrichment unit on the carrier in the enrichment unit, the photometric detection unit directly detects the enrichment unit.Under the situation that does not break away from spirit of the present invention, any type of change that the present invention is made all should fall within protection scope of the present invention.
Claims (12)
1. the method for photometric analysis of contaminant trace species in the water sample may further comprise the steps:
A, with quantitative water sample to be measured, import in the reaction member with the reagent of pollutant to be measured coupling;
Water sample to be measured and reagent are at reaction member reaction of formation product;
B, have reaction product reactant liquor by the enrichment unit, carrier in reaction product and enrichment unit knot is incorporated in enrichment on the carrier;
C, photometric detection unit detect described enrichment unit, thereby obtain the content or the concentration of pollutant to be measured in the water sample.
2. method according to claim 1 is characterized in that: also comprise elution step: use the product on the eluant, eluent wash-out carrier.
3. method according to claim 1 is characterized in that: described carrier is macroporous absorbent resin, ion exchange resin, fiber, silica gel, PTFE microballon, nano material, activated charcoal, activated alumina or gel.
4. according to claim 1 or 2 or 3 described methods, it is characterized in that: detect transmitance or scattered power or the absorbance of enrichment unit light.
5. according to claim 1 or 2 or 3 described methods, it is characterized in that: adopt the hyperchannel selection valve, the public passage on this valve connects liquid storage unit and pump;
Select water sample passage, the reagent passage of hyperchannel selection valve respectively, pump is drawn into water sample, reagent in the liquid storage unit respectively;
Select the reaction channel of hyperchannel selection valve, pump is delivered to the water sample in the liquid storage unit, reagent in the reaction member.
6. method according to claim 5 is characterized in that: after water sample, reagent were delivered to reaction member, pump was by the air duct extracting air;
Select the reaction channel of hyperchannel selection valve, pump is delivered to the air that extracts in the reaction member, has stirred, mixed water sample, reagent in the reaction member.
7. method according to claim 6 is characterized in that: described air duct be arranged on the hyperchannel selection valve or with pump and valve that the liquid storage unit is connected on.
8. the photometric analysis device of contaminant trace species in the water sample comprises switch unit, reaction member, pump and detecting unit, and detecting unit comprises light source, detector and analysis module; It is characterized in that: described analytical equipment also comprises:
Inside is provided with the enrichment unit of enrichment carrier, and the reaction product that is used for reactant liquor that reaction member is discharged is enriched in described carrier;
The reaction product of the rayed that light source sends on carrier, the light signal after detector reception and the reaction product effect, the signal that receives send analysis module.
9. device according to claim 8 is characterized in that: described carrier is macroporous absorbent resin, ion exchange resin, fiber, silica gel, PTFE microballon, nano material, activated charcoal, activated alumina or gel.
10. according to Claim 8 or 9 described devices, it is characterized in that: described switch unit adopts the hyperchannel selection valve, this hyperchannel selection valve is provided with public passage, reagent passage, water sample passage, measures passage, reaction channel, described public passage connects liquid storage unit and pump, described measurement passage connects the enrichment unit, described reaction channel connects mixing-reaction member, and described analytical equipment also comprises air duct.
11. device according to claim 10 is characterized in that: described air duct is arranged on the hyperchannel selection valve.
12. device according to claim 10 is characterized in that: described pump connects the liquid storage unit by valve, and described air duct is arranged on this valve.
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| Application Number | Priority Date | Filing Date | Title |
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| CN200910156637A CN101776581A (en) | 2009-12-29 | 2009-12-29 | Method for photometric analysis of trace pollutant in water sample and device thereof |
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| CN200910156637A CN101776581A (en) | 2009-12-29 | 2009-12-29 | Method for photometric analysis of trace pollutant in water sample and device thereof |
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Cited By (12)
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| CN105004836A (en) * | 2014-04-21 | 2015-10-28 | 赛默飞世尔（上海）仪器有限公司 | Method and device for online water quality detection |
| CN105527147A (en) * | 2015-11-23 | 2016-04-27 | 浙江省海洋水产研究所 | Extraction apparatus for heavy metals in seawater sample |
| CN106198625A (en) * | 2016-06-02 | 2016-12-07 | 东北电力大学 | One heavy metal species on-line monitoring system device in situ |
| CN108535435A (en) * | 2018-04-19 | 2018-09-14 | 赛默飞世尔（上海）仪器有限公司 | Ammonia nitrogen water quality monitoring method and water quality on-line monitoring instrument |
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| CN110470650A (en) * | 2019-08-01 | 2019-11-19 | 广东省测试分析研究所（中国广州分析测试中心） | A kind of multi-mode water quality heavy metal on-line monitoring system |
| CN111174098A (en) * | 2019-12-19 | 2020-05-19 | 江苏国技仪器有限公司 | Flow path system of water quality analyzer and accurate quantification method |
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- 2009-12-29 CN CN200910156637A patent/CN101776581A/en active Pending
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101907599A (en) * | 2010-07-21 | 2010-12-08 | 宇星科技发展(深圳)有限公司 | All-in-one heavy metal online analyzer |
| CN101907599B (en) * | 2010-07-21 | 2013-03-27 | 宇星科技发展(深圳)有限公司 | All-in-one heavy metal online analyzer |
| CN105004836A (en) * | 2014-04-21 | 2015-10-28 | 赛默飞世尔（上海）仪器有限公司 | Method and device for online water quality detection |
| CN105527147A (en) * | 2015-11-23 | 2016-04-27 | 浙江省海洋水产研究所 | Extraction apparatus for heavy metals in seawater sample |
| CN105527147B (en) * | 2015-11-23 | 2018-05-22 | 浙江省海洋水产研究所 | A kind of seawater sample Extraction of Heavy Metals device |
| CN106198625A (en) * | 2016-06-02 | 2016-12-07 | 东北电力大学 | One heavy metal species on-line monitoring system device in situ |
| CN109580480A (en) * | 2017-09-28 | 2019-04-05 | 株式会社岛津制作所 | Total phosphorus determination device |
| CN108535435A (en) * | 2018-04-19 | 2018-09-14 | 赛默飞世尔（上海）仪器有限公司 | Ammonia nitrogen water quality monitoring method and water quality on-line monitoring instrument |
| CN109283138A (en) * | 2018-09-30 | 2019-01-29 | 宁波万泽微测环境科技股份有限公司 | A kind of quantitative sample injection system |
| CN109283138B (en) * | 2018-09-30 | 2021-08-31 | 宁波万泽微测环境科技股份有限公司 | Quantitative sample introduction system |
| CN110470650A (en) * | 2019-08-01 | 2019-11-19 | 广东省测试分析研究所（中国广州分析测试中心） | A kind of multi-mode water quality heavy metal on-line monitoring system |
| CN110470650B (en) * | 2019-08-01 | 2022-04-22 | 广东省测试分析研究所（中国广州分析测试中心） | Multi-mode quality of water heavy metal on-line monitoring system |
| CN110441291A (en) * | 2019-08-26 | 2019-11-12 | 广州伊创科技股份有限公司 | A kind of plasma atomic emission spectroscopy analyzer |
| CN111174098A (en) * | 2019-12-19 | 2020-05-19 | 江苏国技仪器有限公司 | Flow path system of water quality analyzer and accurate quantification method |
| CN111174099A (en) * | 2019-12-19 | 2020-05-19 | 江苏国技仪器有限公司 | Multi-range water quality analyzer flow path system and accurate quantification method |
| CN113567376A (en) * | 2021-07-29 | 2021-10-29 | 北京京能电力股份有限公司 | Device and method for measuring concentration of trace iron ions in water vapor of power plant |
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Effective date of registration: 20120314 Address after: Hangzhou City, Zhejiang province Binjiang District 310052 shore road 760 Applicant after: Focused Photonics (Hangzhou) Inc. Co-applicant after: Hangzhou Juguang Environmental Protection Technology Co.,Ltd. Address before: Hangzhou City, Zhejiang province Binjiang District 310052 shore road 760 Applicant before: Focused Photonics (Hangzhou) Inc. |
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