CN105865892A - Anion synthetic detergent extracting and analyzing method and device - Google Patents
Anion synthetic detergent extracting and analyzing method and device Download PDFInfo
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- CN105865892A CN105865892A CN201610362655.2A CN201610362655A CN105865892A CN 105865892 A CN105865892 A CN 105865892A CN 201610362655 A CN201610362655 A CN 201610362655A CN 105865892 A CN105865892 A CN 105865892A
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- chloroform
- back extraction
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- synthetic detergent
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4055—Concentrating samples by solubility techniques
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4055—Concentrating samples by solubility techniques
- G01N2001/4061—Solvent extraction
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
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Abstract
The invention relates to an extracting method, in particular to an anion synthetic detergent extracting and analyzing method and device. The method includes the steps of firstly, injecting a sample into a sample bottle, then injecting a methylene blue reagent to be stirred and mixed, slowly adding a certain amount of chloroform in the stirring process to continue to be evenly stirred for stirring extraction, and then conducting standing; secondly, extracting chloroform and part of residual solution out of the sample bottle, injecting chloroform and part of residual solution into a back extraction bottle to be evenly stirred, sealing the back extraction bottle, discharging residual solution and chloroform into a waste liquid bucket through pressure, and injecting detergent into the rest certain amount of chloroform for back extraction; thirdly, making back extraction chloroform enter a water filter, and injecting filtered chloroform into a cuvette for test detection. The detection method is simple, the method is high in accuracy and precision and can be controlled, and detection sensitivity is improved. Automatic continuous sampling can be achieved in the extraction process, and the extracted sample can meet the requirement for batched analysis and real-time monitoring of water samples.
Description
Technical field
The present invention relates to a kind of filter method, particularly to anion synthetic detergent extractive analysis method
And device.
Background technology
Water sample pre-treatment is the important step analyzing detection, when carrying out water analysis mensuration, and tradition water sample
After pre-treatment uses manual extraction, stratification separates.Using separatory funnel, manually concussion extraction is to be measured
Thing, after candidate agent stratification, accesses object.Adopt and process water sample in this way, labor intensity
Greatly, operator directly contact reagent, and toxicity extract easily produces harm, and manual behaviour to human body
Making error big, precision is low, it is impossible to meet water sample batch quantity analysis and the requirement of monitoring in real time.
Summary of the invention
The technical problem to be solved in the present invention is how to overcome the deficiencies in the prior art, it is provided that anion is closed
Become detergent extractive analysis method.
The present invention the technical scheme is that anion synthetic detergent extraction point for achieving the above object
Analysis method: (1) injects 5-150mL sample in sample bottle, then injects 10-50mL methylene blue reagent,
It is stirred mixing, whipping process is slowly added to the chloroform of 5-30mL, continues to stir, it is achieved
Stirring extraction, stratification afterwards；(2) from sample bottle, extract the chloroform layer of excess, be injected into
In back extraction bottle, then repeating extraction 1-5 time with 5-30mL chloroform respectively, chloroform layer is fully transferred to instead
In extraction flask, stir, seal back extraction bottle, redundant solution in back extraction bottle and chloroform are utilized
Pressure enters in waste liquid barrel, injects 10-100mL cleaning mixture and carry out back extraction in residue 10-50mL chloroform；
(3) the chloroform 3-6mL after extraction back extraction enters water filter, and the chloroform after filtering injects colorimetric
Ware, is analyzed detection.
Further, the invention provides the anion synthetic detergent extractive analysis dress of above method
Putting, it comprises at least one water sample and processes detector unit, and described water sample processes detector unit and includes injection
Pump, automatic sampling apparatus, back extraction device, filter and detection device, described syringe pump passes through
Multiple-way valve is connected with described automatic sampling apparatus, back extraction device, filter.
Further, described syringe pump connects at least one reagent sample storage bottle by multiple-way valve.
Further, described syringe pump connects filter by multiple-way valve, and described filter passes through pipeline
Connect monitoring device.
Further, present invention additionally comprises sample bottle, described automatic sampling apparatus is arranged on sample bottle,
Described automatic sampling apparatus is connected with described syringe pump by multiple-way valve.
Further, described back extraction device being provided with relief valve, described back extraction device is by pipe
Road connects waste liquid barrel, and described waste liquid barrel connects multiple-way valve by pipeline.
Further, described sample bottle is provided with mechanical stirring device, and described back extraction device is provided with magnetic force
Agitating device, described automatic sampling apparatus, back extraction device are installed in constant temperature system.
Further, described reagent sample storage bottle includes that methylene blue sample storage bottle, chloroform sample storage bottle, pure water store up
Sample bottle, cleaning mixture sample storage bottle, cleanout fluid sample storage bottle, isopropanol sample storage bottle.
Further, described syringe pump one end is directly connected to back extraction device, and described back extraction device is another
One end connects syringe pump by multiple-way valve.
Water sample detection method of the present invention is simple, and veracity and precision is higher, can control, improve inspection
The sensitivity surveyed.Water sample extraction process of the present invention can realize automatic continuous sampling, and after extraction, sample can
To meet water sample batch quantity analysis and real-time detection requirement.The present invention designs uniqueness, modern design, science
Rationally, using effect is good, has good market popularization value, has huge economic outlook.
Accompanying drawing explanation
Fig. 1 is apparatus of the present invention structural representation.
Fig. 2 is apparatus of the present invention canonical plotting.
Fig. 3 is for manually extracting canonical plotting.
Detailed description of the invention
Describe the present invention below in conjunction with the accompanying drawings in detail.
Anion synthetic detergent extractive analysis method comprises the following steps: (1) injects in sample bottle
100mL sample, then inject 25mL methylene blue reagent, it is stirred mixing, whipping process slowly adds
Enter the chloroform of 10mL, continue to stir, it is achieved stirring extraction, stratification afterwards；(2) from
Sample bottle extracts enough chloroform layers, is injected in back extraction bottle, more respectively with 10mL chloroform weight
Extraction 2 times again, chloroform layer is fully transferred in back extraction bottle, stirs, and keeps constant voltage, will be anti-
In extraction flask, redundant solution and chloroform utilize pressure to enter in waste liquid barrel, note in residue 15-30mL chloroform
Enter 25-50mL cleaning mixture and carry out back extraction；(3) the chloroform 3-6mL after extraction back extraction enters water mistake
Filter, the chloroform after filtering injects cuvette, is analyzed detection.
According to above step, described anion synthetic detergent extractive analysis device as it is shown in figure 1,
Comprising a water sample and process detector unit 1, one water sample processes detector unit 1 and includes syringe pump
11, automatic sampling apparatus 12, back extraction device 13, filter 14 and detection device 15, described
Syringe pump 11 is by multiple-way valve 16 and described automatic sampling apparatus 12, back extraction device 13, filter
14 connect.Extracting reagent for convenience, described syringe pump 11 connects methylene blue respectively by multiple-way valve 16
Sample storage liquid bottle, chloroform sample storage bottle, pure water sample storage bottle, isopropanol sample storage bottle and cleaning mixture sample storage bottle.
Described syringe pump 11 one end is directly connected to back extraction device 13, and described back extraction device 13 other end leads to
Cross multiple-way valve 16 and connect syringe pump 11.Described automatic sampling apparatus 12, back extraction device 13 are respectively mounted
In constant temperature system 3, in the case of preventing temperature relatively low, extract is difficult to be layered.
For convenience of filtering and detection water sample, described syringe pump 11 connects filter by multiple-way valve 16
14, described filter 14 connects monitoring device 15 by pipeline, and the water sample conveniently carrying out filtering is timely
Entrance detection device detect.For convenience of auto injection, this device also includes sample bottle 17, institute
State automatic sampling apparatus 12 to be arranged on sample bottle 17, the convenient timely collection to sample.Described from
Dynamic sampling device 12 is connected with described syringe pump 11 by multiple-way valve 16, facilitates automatic sampling apparatus
12 samples gathered, by multiple-way valve 16, in the operation through syringe pump 11, timely enter back extraction
Device 13.
In order to protect the balance of back extraction device 13 internal gas pressure, described back extraction device 13 is provided with
Relief valve 131, facilitates equilibrium air pressure, described back extraction device 13 to install waste liquid barrel 132, described useless
Liquid bucket 132 connects multiple-way valve 16, the collection of waste liquid when facilitating back extraction by pipeline, and design science is closed
Reason.Furthermore, back extraction device 13 connects waste liquid barrel 132 by two pipe pipelines, and it plays quantitative work
With, facilitate the back extraction of chloroform.
For ensureing mixing homogeneously of sample and chloroform, described sample bottle 17 is provided with mechanical stirring device 171,
Simultaneously work as sealing process, prevent the leakage of chloroform, described back extraction device 13 to be provided with magnetic agitation dress
Put.
The present invention uses process: moved by straight line module, driven stirring rod and sample feeding pipe is inserted into
The bottom of sample bottle 17, syringe pump 11 extracts quantitative methylene blue solution, manifold by multiple-way valve 16
Vavle switching pipeline, is expelled to the methylene blue solution of extraction in sample bottle 17, and then syringe pump 11 is taken out
Take quantitative chloroform, be injected into equally in sample bottle 17, stirring rod electric machine rotation, be stirred extracting
Journey, stands after having stirred, and the chloroform and a part of unnecessary solution that add with syringe pump 11 extraction (are
Guarantee chloroform is all taken away), by the switching of multiple-way valve 16, it is expelled to back extraction device 13
In, for convenience of equilibrium air pressure, the relief valve 131 of back extraction device 13 can be opened.
In above-mentioned sample bottle 17, extraction can be carried out repeatedly.Finally, by the chloroform after repeatedly extraction instead
In extraction equipment 13, stir by magnetic stir bar, utilize syringe pump 11, inject in sample bottle 17
Air, opens the relief valve 131 in sample bottle 17 simultaneously, is pressed into useless by unnecessary solution and chloroform
In liquid bucket 132, remaining quantitative chloroform, recycling syringe pump 11 and multiple-way valve 16, to back extraction
Device 13 injects quantitative cleaning mixture, opens magnetic stirring apparatus and carry out back extraction process.
Afterwards, syringe pump 11 extracts pure water and carries out oneself's cleaning, then extracts in back extraction device 13
Chloroform, is expelled to contrast color ware in the cuvette of detection device 15 after water filter 14 and carries out clearly
Wash.
Again take the chloroform after a certain amount of back extraction by injection pumping 11, be injected in cuvette survey
Amount absorbance.After instrument reads data, the chloroform in cuvette is passed through multiple-way valve 16 by syringe pump 11
Taking away and be discharged into waste liquid barrel 132, then syringe pump 11 extracts air and is injected in back extraction device 13,
Simultaneously close off multiple-way valve 16, open end opening electromagnetic valve, the liquid in back extraction device 13 is pressed into useless
Liquid bucket 132.Finally, syringe pump 11 extracts after clear water is injected into and is carried out in back extraction device 13
Discharge opeing, repeatable cleaning is repeatedly to ensure to clean up.
For ensureing the accuracy of experiment, being also carried out sample bottle 17 cleaning, syringe pump 11 extracts clear water
Rear injection injects sample bottle 17 by multiple-way valve 16, water from the overhead stream of sample feeding pipe and stirring rod,
Being then turned on stirring and washing, automatic sampling apparatus 12 can take waste liquid away.
When carrying out the operation of next group, driven stirring rod and sample feeding pipe are inserted into another sample bottle
Bottom, process and analyze another sample, it is achieved that to automatization's pre-treatment of batch sample and point
Analysis.
With manual extraction mode, the application device is carried out contrast draw: as shown in Fig. 2 and accompanying drawing 3,
Compared with manual extracting process, the application device standard curve the most more stable, linear correlation system
Base instinct reaches more than 0.999, and recovery of standard addition is less than 5% in 82%-96%, relative standard deviation,
Accuracy ± 4%, instrumental resolution 0.001mg/L.The application device more can save organic solvent trichlorine
Methane, the airtight volatilization not resulting in toxic and volatile gas of whole process.
Manual extraction comparatively speaking, its linearly dependent coefficient is only capable of reaching more than 0.99 substantially, organic
Solvent chloroform is easier to volatilization in whole operation is constituted.Furthermore, manually extraction needs artificial clear
Washing, waste time and energy, accuracy is the highest with recovery of standard addition, the precision of impact experiment.
Above-described embodiment, simply to illustrate that the technology design of the present invention and feature, its objective is to be to allow
One of ordinary skilled in the art will appreciate that present disclosure and implements according to this, can not be with this
Limit the scope of the invention.The change of every equivalence made according to the essence of present invention
Or modify, all should contain within the scope of the present invention.
Claims (10)
1. anion synthetic detergent extractive analysis method, it is characterised in that: (1) is in sample bottle
Injection 5-150mL sample, then inject 10-50mL methylene blue reagent, it is stirred mixing, stirred
Journey is slowly added to the chloroform of 5-30mL, continues to stir, it is achieved stirring extraction, stand afterwards and divide
Layer；(2) from sample bottle, extract the chloroform layer of excess, be injected in back extraction bottle, then use respectively
5-30mL chloroform repeats extraction 1-5 time, and chloroform layer is fully transferred in back extraction bottle, stirs,
Seal back extraction bottle, utilize pressure to enter in waste liquid barrel redundant solution and chloroform in back extraction bottle, surplus
Remaining 10-50mL chloroform injects 10-100mL cleaning mixture and carries out back extraction；(3) after extraction back extraction
Chloroform 3-6mL enter water filter, will filter after chloroform inject cuvette, be analyzed detection.
2. comprise the moon that anion synthetic detergent extractive analysis method as claimed in claim 1 uses
Nonionic synthetic detergent extractive analysis device.
Anion synthetic detergent extractive analysis device the most according to claim 2, its feature exists
In: comprise at least one water sample process detector unit, described water sample process detector unit include syringe pump,
Automatic sampling apparatus, back extraction device, filter and detection device, described syringe pump passes through manifold
Valve is connected with described automatic sampling apparatus, back extraction device, filter.
Anion synthetic detergent extractive analysis device the most according to claim 2, its feature exists
In: described syringe pump connects at least one reagent sample storage bottle by multiple-way valve.
Anion synthetic detergent extractive analysis device the most according to claim 2, its feature exists
In: described syringe pump connects filter by multiple-way valve, and described filter connects detection dress by pipeline
Put.
Anion synthetic detergent extractive analysis device the most according to claim 2, its feature exists
In: also including that sample bottle, described automatic sampling apparatus are arranged on sample bottle, described auto injection fills
Put and be connected with described syringe pump by multiple-way valve.
Anion synthetic detergent extractive analysis device the most according to claim 2, its feature exists
In: being provided with relief valve on described back extraction device, described back extraction device connects waste liquid by pipeline
Bucket, described waste liquid barrel connects multiple-way valve by pipeline.
Anion synthetic detergent extractive analysis device the most according to claim 6, its feature exists
In: described sample bottle is provided with mechanical stirring device, and described back extraction device is provided with magnetic stirring apparatus,
Described automatic sampling apparatus, back extraction device are installed in constant temperature system.
Anion synthetic detergent extractive analysis device the most according to claim 4, its feature exists
In: described reagent sample storage bottle includes methylene blue sample storage bottle, chloroform sample storage bottle, pure water sample storage bottle, washing
Liquid sample storage bottle, cleanout fluid sample storage bottle, isopropanol sample storage bottle.
Anion synthetic detergent extractive analysis device the most according to claim 2, its feature
Being: described syringe pump one end is directly connected to back extraction device, the described back extraction device other end passes through
Multiple-way valve connects syringe pump.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610362655.2A CN105865892A (en) | 2016-05-27 | 2016-05-27 | Anion synthetic detergent extracting and analyzing method and device |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610362655.2A CN105865892A (en) | 2016-05-27 | 2016-05-27 | Anion synthetic detergent extracting and analyzing method and device |
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| CN105865892A true CN105865892A (en) | 2016-08-17 |
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| CN201610362655.2A Pending CN105865892A (en) | 2016-05-27 | 2016-05-27 | Anion synthetic detergent extracting and analyzing method and device |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106501061A (en) * | 2016-12-06 | 2017-03-15 | 王占辉 | Anion surfactant online auto monitoring system and method in water |
| CN106770257A (en) * | 2017-01-13 | 2017-05-31 | 北京瑞升特科技有限公司 | A kind of anionic detergent detecting system |
| CN109110856A (en) * | 2018-11-02 | 2019-01-01 | 上海昂林科学仪器股份有限公司 | Oils auto extractive system and analysis system in a kind of water |
| CN109507180A (en) * | 2018-12-26 | 2019-03-22 | 江苏赫尔斯检测技术有限公司 | It is a kind of to measure the detection device and method for drinking ABS in drinking water |
| CN109876494A (en) * | 2019-04-10 | 2019-06-14 | 青岛励德仪器有限公司 | A kind of device and method taking out upper layer solvent from de-laminating solvent |
| CN110274886A (en) * | 2019-06-13 | 2019-09-24 | 广东化一环境科技有限公司 | A kind of oil smoke on-line measuring device and method |
| CN112704909A (en) * | 2020-12-24 | 2021-04-27 | 涡阳县华腾日用化学品有限公司 | Extraction device for synthesizing detergent by anions in water and preparation method |
| CN112903612A (en) * | 2021-01-26 | 2021-06-04 | 杭州绿洁环境科技股份有限公司 | Online analyzer for anionic surfactant |
| CN114062292A (en) * | 2021-11-17 | 2022-02-18 | 江苏省环境监测中心 | Extractor for oil measurement, full-automatic ultraviolet oil measurement device and oil measurement method thereof |
| CN117619215A (en) * | 2023-12-21 | 2024-03-01 | 北京欧仕科技有限公司 | Quantitative mixer |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106501061A (en) * | 2016-12-06 | 2017-03-15 | 王占辉 | Anion surfactant online auto monitoring system and method in water |
| CN106501061B (en) * | 2016-12-06 | 2023-05-19 | 王占辉 | On-line automatic monitoring system and method for anionic surfactant in water |
| CN106770257B (en) * | 2017-01-13 | 2023-04-25 | 北京瑞升特科技有限公司 | Anionic detergent detecting system |
| CN106770257A (en) * | 2017-01-13 | 2017-05-31 | 北京瑞升特科技有限公司 | A kind of anionic detergent detecting system |
| CN109110856A (en) * | 2018-11-02 | 2019-01-01 | 上海昂林科学仪器股份有限公司 | Oils auto extractive system and analysis system in a kind of water |
| CN109110856B (en) * | 2018-11-02 | 2023-07-21 | 上海昂林科学仪器股份有限公司 | Automatic extraction system and analysis system for oil in water |
| CN109507180A (en) * | 2018-12-26 | 2019-03-22 | 江苏赫尔斯检测技术有限公司 | It is a kind of to measure the detection device and method for drinking ABS in drinking water |
| CN109876494A (en) * | 2019-04-10 | 2019-06-14 | 青岛励德仪器有限公司 | A kind of device and method taking out upper layer solvent from de-laminating solvent |
| CN110274886A (en) * | 2019-06-13 | 2019-09-24 | 广东化一环境科技有限公司 | A kind of oil smoke on-line measuring device and method |
| CN112704909A (en) * | 2020-12-24 | 2021-04-27 | 涡阳县华腾日用化学品有限公司 | Extraction device for synthesizing detergent by anions in water and preparation method |
| CN112903612A (en) * | 2021-01-26 | 2021-06-04 | 杭州绿洁环境科技股份有限公司 | Online analyzer for anionic surfactant |
| CN114062292A (en) * | 2021-11-17 | 2022-02-18 | 江苏省环境监测中心 | Extractor for oil measurement, full-automatic ultraviolet oil measurement device and oil measurement method thereof |
| CN117619215A (en) * | 2023-12-21 | 2024-03-01 | 北京欧仕科技有限公司 | Quantitative mixer |
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Application publication date: 20160817 |