CN106908405A - A kind of hypersensitive sulfate radical nephelometric analysis method and detection means - Google Patents
A kind of hypersensitive sulfate radical nephelometric analysis method and detection means Download PDFInfo
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Abstract
The invention discloses a kind of hypersensitive sulfate radical nephelometric analysis method and detection means, belong to sulfate radical detection and analysis technical field.The method is that sulfate sample to be detected is delivered in threeway blender through sample current-carrying；The glycerine ethanol barium chloride solution system that hydrochloric acid is acidified is delivered in threeway blender and carries out on-line mixing with sulfate sample to be detected, reaction ring reaction is flowed through after mixing, generate barium sulfate emulsion；Barium sulfate emulsion is first flowed through be connected with light emitting diode optical fiber, flow into liquid core waveguide pipe again, then flow through photodiode after enter waste liquid pool, the change of light intensity when finally flowing through liquid core waveguide pipe to barium sulfate emulsion using photodiode is detected.Overlength light path liquid core waveguide pipe of the invention significantly improves the sensitivity that barium sulfate turbidimetry determines sulfate radical, detected using light emitting diode and photodiode, instrument is simple, easy to operate, is suitable to the super sensitivity detection of sulfate radical in environmental water sample and trace analysis.
Description
Technical field
The present invention relates to a kind of hypersensitive sulfate radical nephelometric analysis method and detection means, belong to sulfate radical detection and analysis skill
Art field.
Background technology
Sulfate radical is one of common anion in water body, puritan filler salt mineral dissolution and sulfur-containing compound production and application
It is the main source of sulfate radical in water body.Additionally, the sulfurous gas such as sulfur dioxide using generation of coal and oil is in an atmosphere
Conversion and sedimentation are also the important sources of sulfate radical in water body.The concentration of sulfate radical directly affects water quality and aquatic dynamic plant in water body
The metabolism of thing, so that influence ecological environment.Human body largely takes in sulfate radical can be caused to suffer from diarrhoea, be dehydrated and gastrointestinal disturbance.
Therefore, detection water body in sulfate ion content for grasp water quality condition and avoid sulfate radical harmful effect have it is important
Meaning.At present, the chromatography of ions, titration, gravimetric method, atomic spectroscopy, ultraviolet-visible spectrophotometry, fluorescence method and electrification
Method is used equally to the detection and analysis of sulfate radical.Wherein, in acid condition, surfactant and excessive barium ions and sulphur are introduced
Acid ion forms barium sulfate precipitate and carries out nephelometric analysis, is one of conventional vis spectroscopy spectrographic technique of sulfate radical detection.Should
Method possesses convenience, simple, good selective, using quite varied in micro sulfate radical detection and analysis.
Generally, sulfate ion is analyzed using nephelometry, it is necessary to select good surfactant as dispersant, dispersion
Agent can be adsorbed in liquid-solid boundary reduction interfacial free energy, precipitation is uniformly dispersed.To ensure the reappearance of turbidimetric analysis turbidimetry and accurate
Property, it is necessary to strict control adds order, mixing time, stir speed (S.S.) and the standing time of reagent.But the efficiency of this method compared with
It is low, it is difficult to realize precise control, while the sensitivity of this method detection sulfate radical is poor, it is unsuitable for trace and ultra trace sulfate radical
Accurate analysis.
The content of the invention
The parameters such as mixing time, speed, standing time for the existing sulfate radical nephelometric analysis of solution are difficult to precise control, examine
Sulfate radical precision and the poor problem of sensitivity are surveyed, the invention provides a kind of hypersensitive sulfate radical nephelometric analysis method and inspection
Device is surveyed, the technical scheme of use is as follows：
It is an object of the invention to provide a kind of hypersensitive sulfate radical nephelometric analysis method, the method is to include following step
Suddenly：
1) using ultra-pure water as sample current-carrying, ultra-pure water is delivered to sampling valve 4 by pump 3, by sulfate radical sample to be detected
Product inject sampling valve 4, and sulfate sample to be detected is delivered in threeway blender 6 through sample current-carrying；
2) while the glycerin-ethanol that will be acidified through hydrochloric acid-barium chloride solution system is conveyed by pump 3 or another pump
On-line mixing is carried out in threeway blender 6 into threeway blender 6 and with sulfate sample to be detected, is flowed through after mixing anti-
Answer ring 7 to react, generate barium sulfate emulsion；
3) the barium sulfate emulsion for generating step 2 first flow through be connected with light emitting diode 10 optical fiber 8, flow into wick-containing again
In waveguide 9, then flow through photodiode 11 after enter waste liquid pool 14, finally using photodiode 11 to barium sulfate milkiness
Light intensity change when liquid flows through liquid core waveguide pipe 9 is detected.
Preferably, barium chloride solution in the glycerin-ethanol-barium chloride solution system through hydrochloric acid acidifying described in step 2
Concentration be 20g/L.
Preferably, described in step 2 through hydrochloric acid be acidified glycerin-ethanol-barium chloride solution system in glycerine body
Product percentage is 4%.
Preferably, described in step 2 through hydrochloric acid be acidified glycerin-ethanol-barium chloride solution system in ethanol volume
Percentage is 4%.
Preferably, the sampling volume of sulfate sample to be detected described in step 1 is 200 μ L.
Preferably, the length of liquid core waveguide pipe 9 described in step 3 is 2.5m, and volume is 500 μ L.
Preferably, the length that ring 7 is reacted described in step 2 is 80cm, and internal diameter is 1mm；The reaction ring 7 is to twine PTFE tube
Coiled, a diameter of 15mm of spiral, promotes solution to be sufficiently mixed.
Preferably, the voltage signal that photodiode 11 described in step 3 is produced is converted to digital letter by data collecting card 12
Number.
Preferably, the connection of the data collecting card 12 computer 13 carries out data record and treatment.
The glycerin-ethanol-barium chloride solution system is pre-mixed and prepares.
Preferably, step 1) pump 3 is peristaltic pump, two passages of first passage I and the equal peristaltic pumps of second channel II.
Preferably, step 1) sampling valve 4 be six-way injection valve.
Present invention also offers a kind of device for realizing above-mentioned hypersensitive sulfate radical nephelometric analysis method, including the
One sample introduction pipeline 1, the second sample introduction pipeline 2, pump 3, sampling valve 4, mixing tee 6 reacts ring 7, optical fiber 8, liquid core waveguide pipe 9, hair
Optical diode 10, photodiode 11, data collecting card 12 and computer 13, waste liquid pool 14；Wherein：First sample introduction pipeline 1 passes through
Glycerin-ethanol-barium chloride solution the system of the conveying hydrochloric acid acidifying of pump 3；Second sample introduction pipeline 2 passes through pump 3 or another pump
Conveying sample current-carrying；Sampling valve 4 is additionally provided with the second sample introduction pipeline 2；The first sample introduction pipeline 1 and the second sample introduction pipeline
2 liquid outlet is connected with mixing tee 6 respectively, and the remaining one end of mixing tee 6 is connected with reaction ring 7, reacts ring 7
The other end be connected with liquid core waveguide pipe 9；The two ends of the liquid core waveguide pipe 9 also respectively by optical fiber 8 and light emitting diode 10 and
Photodiode 11 is connected, and the liquid outlet of liquid core waveguide pipe 9 is also associated with waste liquid pool 14；The data collecting card 12 is by light
The voltage signal that electric diode 11 is produced is converted to data signal；The connection data collecting card 12 of the computer 13 carries out data record
And treatment.
Preferably, the pump 3 is two passages of peristaltic pump, first passage I and the equal peristaltic pumps of second channel II.
First sample introduction pipeline 1 conveys glycerin-ethanol-barium chloride solution body that hydrochloric acid is acidified by the first passage I of pump 3
It is A；Second sample introduction pipeline 2 conveys sample current-carrying B by the second channel II or another pump of pump 3.
Preferably, step 3) photodiode 11 produce voltage signal digital letter is converted to by data collecting card 12
Number, and recorded.
Preferably, the connection of the data collecting card 12 computer 13 carries out data record and treatment.
The inventive method is under acid ethanol-glycerol-aqueous systems, sulfate ion and barium ions to be generated into sulfuric acid
Barium emulsion, into overlength light path detect flow cell, by the use of light emitting diode as light source, photodiode as detector,
Light intensity change under detection current system, realizes the detection of sulfate radical.
The characteristics of the inventive method is：
1) glycerine and ethanol are used in the present invention, its effect is to prevent barium sulfate from forming precipitation, can form dispersiveness
Preferable barium sulfate emulsion
2) glycerin-ethanol-barium chloride solution system 1 uses the percent by volume of glycerine to be 4%, second in the present invention
The percent by volume 4% of alcohol, barium chloride concentration 20g/L.
The characteristics of apparatus of the present invention is：
1) present invention uses peristaltic pump, the glycerin-ethanol-barium chloride solution and sample current-carrying of conveying hydrochloric acid acidifying, behaviour
Make easy, with low cost, sample and barium chloride solution on-line mixing effectively improve the efficiency and stability to form emulsion.
2) present invention uses six-way injection valve, carries out sample loading and sample introduction operation, realizes accurate quantitative analysis sample introduction, effectively carries
Sample feeding efficiency high.
3) present invention can realize that signal is changed by using data collecting card 12, and computer processing data is convenient and swift；
4) present invention effectively improves detection light path using overlength light path liquid core waveguide pipe as optical detecting channel, improves
Sensitivity for analysis；
5) present invention uses light emitting diode and photodiode as light source and detection means, with low cost, effectively drop
Low installation cost.
Beneficial effect of the present invention：
The invention provides one kind based on light emitting diode-overlength light path detection flow cell-photodiode-flow injection
The method of sulfate concentration in analysis Sensitive Determination water sample, the method passes through to use overlength light path liquid core waveguide pipe, significantly
The sensitivity that barium sulfate turbidimetry determines sulfate radical is improve, sensitivity is low up to 7.5 μ g L-1, while using light emitting diode and
Photodiode is detected that instrument is simple, easy to operate, is suitable to the super sensitivity detection of sulfate radical in environmental water sample and trace point
Analysis, the method controls reagent order of addition and mixing time, on-line operation energy without adding reagent and stirring manually without artificial
Enough height are repeated, overlength liquid core waveguide detection device but also with detection sensitivity it is high the characteristics of, can be adapted to trace in water sample
With the accurate detection of ultra trace sulfate radical.
The present invention by adding glycerine and ethanol in the barium chloride solution that is acidified hydrochloric acid, then using flow injection body
System is capable of achieving the on-line mixing of the sulfate radical and barium chloride in water sample, can form dispersed preferably barium sulfate precipitate.Shape
Into precipitation, detected by the liquid core waveguide of overlength light path, be capable of achieving the accurate detection of trace and ultra trace sulfate radical in water body.
Brief description of the drawings
Fig. 1 is the hypersensitive sulfate radical nephelometric analysis square law device schematic diagram of present invention analysis sulfate radical；
(A, the glycerin-ethanol-barium chloride solution system of hydrochloric acid acidifying；B, sample current-carrying；1, the first sample introduction pipeline；2,
Second sample introduction pipeline；3, pump；I, first passage；II, second channel；4, sampling valve；5, sulfate sample to be detected；6, mixing three
It is logical；7, react ring；8, optical fiber；9, liquid core waveguide pipe；10, light emitting diode；11, photodiode；12, data collecting card；13,
Computer；14, waste liquid pool).
Fig. 2 is the datagram analyzed various concentrations sulfate radical using the method for the present invention.
Fig. 3 is that the standard curve for determining sulfate radical is obtained using the method for the present invention.
Specific embodiment
With reference to specific embodiment, the present invention will be further described, but the present invention should not be limited by the examples.
Embodiment 1：
Present embodiments provide a kind of hypersensitive sulfate radical nephelometric analysis method and auxiliary realizes the device of the method, tool
Body is as follows：
A kind of device for realizing above-mentioned hypersensitive sulfate radical nephelometric analysis method, the device includes the first sample introduction
Pipeline 1, the second sample introduction pipeline 2, pump 3, sampling valve 4, mixing tee 6 reacts ring 7, optical fiber 8, liquid core waveguide pipe 9, light-emitting diodes
Pipe 10, photodiode 11, data collecting card 12 and computer 13, waste liquid pool 14；
Wherein：Pump 3 includes two passes, respectively first passage I and second channel II；First sample introduction pipeline 1 passes through pump 3
First passage I conveying through hydrochloric acid be acidified glycerin-ethanol-barium chloride solution system A；Second sample introduction pipeline 2 is by pump 3
Second channel II conveying sample current-carrying B；Sampling valve 4 is additionally provided with second sample introduction pipeline 2；First sample introduction pipeline 1 and the second sample introduction
The liquid outlet of pipeline 2 is connected with mixing tee 6 respectively, and the remaining one end of mixing tee 6 is connected with reaction ring 7, instead
The other end of ring 7 is answered to be connected with liquid core waveguide pipe 9；The two ends of liquid core waveguide pipe 9 also respectively by optical fiber 8 and light emitting diode 10 and
Photodiode 11 is connected, and the liquid outlet of liquid core waveguide pipe 9 is also associated with waste liquid pool 14；Data collecting card 12 is by photoelectricity two
The voltage signal that pole pipe 11 is produced is converted to data signal；The connection data collecting card 12 of computer 13 carries out data record and treatment.
Pump 3 is two passages of peristaltic pump, first passage I and the equal peristaltic pumps of second channel II.The present invention can also be used
Two pumps convey the glycerin-ethanol-barium chloride solution system A and sample current-carrying B being acidified through hydrochloric acid respectively, for result without shadow
Ring, cost may be increased.
Sampling valve 4 is six-way injection valve.
The length of liquid core waveguide pipe 9 is 2.5m, and volume is 500 μ L.
The length for reacting ring 7 is 80cm, and internal diameter is 1mm；The reaction ring 7 is that PTFE tube is wound into curl, spiral
A diameter of 15mm, promote solution to be sufficiently mixed.
Liquid line is connected with each other by the hand-tight joint of 1/16 inch of PEEK, device 7, T-shaped threeway is utilized between 8 and 9,
It is using the hand-tight joint connections of PEEK.Optical fiber and light source, and optical fiber and detector (photodiode) are directly consolidated using AB glue
Fixed, then friction tape wraps up lucifuge.
Apparatus of the present invention structural representation is as shown in Figure 1.
The present embodiment additionally provides a kind of method that hypersensitive sulfate radical nephelometric analysis is carried out using said apparatus, the method
It is to comprise the following steps：
1) using ultra-pure water as sample current-carrying B, ultra-pure water is delivered to sampling valve 4 by the second channel II passages of pump 3,
Sulfate sample to be detected 5 is injected into sampling valve 4, sulfate sample to be detected is delivered to threeway blender 6 through sample current-carrying B
In；
2) while the glycerin-ethanol that will be acidified through hydrochloric acid-barium chloride solution system A passes through the passage first passage I of pump 3
It is delivered in threeway blender 6 and on-line mixing is carried out in threeway blender 6 with sulfate sample to be detected 5, is flowed after mixing
Reacted ring 7 reacts, and generates barium sulfate emulsion；
3) the barium sulfate emulsion for generating step 2 first flow through be connected with light emitting diode 10 optical fiber 8, flow into wick-containing again
In waveguide 9, then flow through photodiode 11 after enter waste liquid pool 14, finally using photodiode 11 to barium sulfate milkiness
Light intensity change when liquid flows through liquid core waveguide pipe 9 is detected.
4) after detection is finished, successively using hydrochloric acid and ultrapure water whole system.
Glycerin-ethanol-barium chloride solution the system being acidified through hydrochloric acid is pre-mixed and prepares, and wherein barium chloride is molten
The concentration of liquid is 20g/L, and the percent by volume of glycerine is 4%, and the percent by volume of ethanol is 4%.
The sampling volume of sulfate sample to be detected is 200 μ L.
The inventive method is under acid ethanol-glycerol-aqueous systems, sulfate ion and barium ions to be generated into sulfuric acid
Barium emulsion, into overlength light path detect flow cell, by the use of light emitting diode as light source, photodiode as detector,
Light intensity change under detection current system, realizes the detection of sulfate radical.
The principles of chemistry of the inventive method are reacted with sulfate radical to be measured using the barium chloride of acidifying, in surfactant
In the presence of form emulsion, detect the change of solution absorbance, the concentration for calculating sulfate radical can be quantified.
The physical principle of apparatus of the present invention is：Light emitting diode 10 sends light and enters the pole of photoelectricity two by 9 liquid core waveguide pipes
Pipe 11, solution changes in liquid core waveguide pipe, and photodiode signal changes, and realizes detection.
Concrete operating principle of the present invention is：The water sample of containing sulfate radicals enters Flow-injection System by sampling valve, pure
The barium chloride solution on-line mixing being acidified with addition glycerine and ethanol under the promotion of water and with hydrochloric acid forms favorable dispersibility
Barium sulfate precipitate turbid solution, into the liquid core waveguide detection cell of overlength light path, the luminous intensity for causing liquid core waveguide pipe to pass through occurs
Change, so as to realize the measure of sulfate concentration.
The present invention, can using Flow-injection System by adding glycerine and ethanol in the barium chloride solution that is acidified in hydrochloric acid
The on-line mixing of the sulfate radical and barium chloride in water sample is realized, dispersed preferably barium sulfate precipitate can be formed.Formed
Precipitation, is detected by the liquid core waveguide of overlength light path, is capable of achieving the accurate detection of trace and ultra trace sulfate radical in water body.
Embodiment 2：The measure of sulfate radical in running water and bottled pure water
Its step is：
(1) sample filtering：
Filter method：10mL running water and certain brand drinking pure water are drawn respectively using plastic injector, using 0.22 μ
M apertures syringe filters are filtered, and it is standby that the water sample after filtering is positioned over plastic centrifuge tube.
(2) determine：
Addition glycerine and ethanol and the barium chloride solution being acidified with hydrochloric acid are prepared, sulfate radical concentration of standard solution point is prepared
It is not：50,500,1000,2000,3000μg L-1。
Instrument measuring condition is shown in Table 1.The analytical performance of apparatus of the present invention is shown in Table 2.Fig. 2 is using the method for the present invention pair
The datagram of Trace Sulfur acid group analysis in water sample.Fig. 3 carries out quantitative standard curve for this method by external standard method.To originally
Sulfate radical in water and bottled pure water is determined and is determined with mark-on reclaims.The measurement result of sulfate radical is shown in Table 3.Using this
Inventive method, the recovery of standard addition detected to sulfate radical in running water and pure water is between 97.4~101.4%, it was demonstrated that method
It is accurate feasible.
Table 1 determines the flow injection overlength light path wick-containing analysis of waveguide method operating condition of sulfate concentration in water sample
The analytical performance of 2 flow injections of table-overlength light path wick-containing analysis of waveguide sulfate radical
The measurement result of sulfate radical in the running water of table 3 and bottled pure water
In the operating condition, the indices to this method are tested repeatedly.In certain concentration range, sulfuric acid
The linearly dependent coefficient of root is 0.9976, and detection is limited to 7.5 μ g L-1。
Although the present invention is disclosed as above with preferred embodiment, it is not limited to the present invention, any to be familiar with this
The people of technology, without departing from the spirit and scope of the present invention, can do various changes and modification, therefore protection of the invention
What scope should be defined by claims is defined.
Claims (10)
1. a kind of hypersensitive sulfate radical nephelometric analysis method, it is characterised in that comprise the following steps：
1) using ultra-pure water as sample current-carrying, ultra-pure water is delivered to sampling valve (4) by pump (3), by sulfate radical sample to be detected
Product inject sampling valve (4), and sulfate sample to be detected is delivered in threeway blender (6) through sample current-carrying；
2) while the glycerin-ethanol that will be acidified through hydrochloric acid-barium chloride solution system is delivered to by pump (3) or another pump
On-line mixing is carried out in threeway blender (6) in threeway blender (6) and with sulfate sample to be detected, is flowed through after mixing
Reaction ring (7) reaction, generates barium sulfate emulsion；
3) by step 2) the barium sulfate emulsion of generation first flows through optical fiber (8), the influent again being connected with light emitting diode (10)
In core waveguide (9), then flow through photodiode (11) after enter waste liquid pool (14), it is finally right using photodiode (11)
Light intensity change when barium sulfate emulsion flows through liquid core waveguide pipe (9) is detected.
2. method according to claim 1, it is characterised in that step 2) described in the glycerin-ethanol being acidified through hydrochloric acid-
The concentration of barium chloride solution is 20g/L in barium chloride solution system.
3. method according to claim 1, it is characterised in that step 2) described in the glycerin-ethanol being acidified through hydrochloric acid-
The percent by volume of glycerine is 4% in barium chloride solution system.
4. method according to claim 1, it is characterised in that step 2) described in the glycerin-ethanol being acidified through hydrochloric acid-
The percent by volume of ethanol is 4% in barium chloride solution system.
5. method according to claim 1, it is characterised in that step 1) sulfate sample to be detected sampling volume
It is 200 μ L.
6. method according to claim 1, it is characterised in that step 3) length of the liquid core waveguide pipe (9) is 2.5m,
Volume is 500 μ L.
7. method according to claim 1, it is characterised in that step 2) length of reaction ring (7) is 80cm, internal diameter
It is 1mm；Reaction ring (7) is that PTFE tube is wound into curl, a diameter of 15mm of spiral.
8. method according to claim 1, it is characterised in that step 3) the voltage letter that produces of the photodiode (11)
Number data signal is converted to by data collecting card (12).
9. method according to claim 7, it is characterised in that the data collecting card (12) connects computer (13) and enters line number
According to record and treatment.
10. a kind of device for realizing the hypersensitive sulfate radical nephelometric analysis method described in claim 1, it is characterised in that
Including the first sample introduction pipeline (1), the second sample introduction pipeline (2), pump (3), sampling valve (4), mixing tee (6), reaction ring (7), light
Fine (8), liquid core waveguide pipe (9), light emitting diode (10), photodiode (11), data collecting card (12) and computer (13), give up
Liquid pool (14)；Wherein：First sample introduction pipeline (1) conveys glycerin-ethanol-barium chloride solution body that hydrochloric acid is acidified by pump (3)
System；Second sample introduction pipeline (2) conveys sample current-carrying by pump (3) or another pump；Also set on the second sample introduction pipeline (2)
There is sampling valve (4)；The liquid outlet of the first sample introduction pipeline (1) and the second sample introduction pipeline (2) respectively with mixing tee (6)
It is connected, mixing tee (6) remaining one end is connected with reaction ring (7), the other end and liquid core waveguide pipe of reaction ring (7)
(9) it is connected；Liquid core waveguide pipe (9) two ends are also respectively by optical fiber (8) and light emitting diode (10) and photodiode
(11) it is connected, the liquid outlet of liquid core waveguide pipe (9) is also associated with waste liquid pool (14)；The data collecting card (12) is by photoelectricity
The voltage signal that diode (11) is produced is converted to data signal；The computer (13) connects data collecting card (12) and carries out data
Record and treatment.
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| CN113008818A (en) * | 2021-02-25 | 2021-06-22 | 河北冀衡集团有限公司蓝天分公司 | Method for measuring acid mist content in sulfuric acid production tail gas |
| CN113720834A (en) * | 2021-08-25 | 2021-11-30 | 中国科学院南海海洋研究所 | Micro-fluidic chip, system and method for detecting biochemical elements of water body |
| CN113720834B (en) * | 2021-08-25 | 2023-08-18 | 中国科学院南海海洋研究所 | Microfluidic chip, system and method for detecting biochemical elements of water body |
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