CN103823019B - For detecting the pack of zinc ion in water quality - Google Patents
For detecting the pack of zinc ion in water quality Download PDFInfo
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- CN103823019B CN103823019B CN201410072187.6A CN201410072187A CN103823019B CN 103823019 B CN103823019 B CN 103823019B CN 201410072187 A CN201410072187 A CN 201410072187A CN 103823019 B CN103823019 B CN 103823019B
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Abstract
The invention provides a kind of preparation method of the pack for detecting zinc ion in water quality, described pack is made up of correctives solution, chromogenic reagent solution and damping fluid, in described correctives solution, the volume ratio of correctives and water is (0.5 ~ 5): (500 ~ 3000), and described correctives is any one in anionic surfactant, cationic surfactant, non-ionic surfactant.According to the pack of the embodiment of the present invention, owing to employing correctives, sensitization can be produced to system well, thus effectively can improve the sensitivity that zinc ion is detected.
Description
Technical field
The present invention relates to on-line monitoring technique field, more particularly, relate to a kind of monitoring of zinc ion.
Background technology
Zinc is one of main vital activity element, and be the activity centre of various active enzyme in body, the metabolism for human body has a very important role.When zinc concentration in alkaline water is more than 5mg/L, water has bitter taste, and occurs milky.Time in water containing zinc 1mg/L, there is slight inhibiting effect to the biological oxidation process of water body.The main pollution source of zinc is the waste discharge of the departments such as plating, metallurgy, pigment and chemical industry.Therefore, accurate measurements water quality zinc ion content is significant.
Measure the common method of zinc to have and directly suck atomic absorption spectrophotometry, dithizone spectrophotometry, anodic stripping voltammetry etc.A kind of front method measures zinc and has higher sensitivity, and interference is few, but instrument has high input.Dithizone method sensitivity is higher, applies also more extensive.But dithizone and Zn
2+the complex compound formed is water insoluble, and the organic solvent such as benzene, methenyl choloride must be adopted to extract, and detachment process is complicated, and the organic solvents such as benzene also can bring harm to human body.
Summary of the invention
The present invention one of is intended to solve the problems of the technologies described above at least to a certain extent or at least provides a kind of useful business to select.
For this reason, one object of the present invention is to propose a kind of pack for detecting zinc ion in water quality.
According to the pack for detecting zinc ion in water quality of the embodiment of the present invention, described pack is made up of correctives solution, chromogenic reagent solution and damping fluid, in described correctives solution, the volume ratio of correctives and water is (0.5 ~ 5): (500 ~ 3000), described correctives is any one in anionic surfactant, cationic surfactant, non-ionic surfactant, is preferably non-ionic surfactant
According to the pack of the embodiment of the present invention, owing to employing correctives, sensitization can be produced to system well, thus effectively can improve the sensitivity that zinc ion is detected.
Wherein, described anionic surfactant comprises at least one in dodecyl phenenyl sulfate, neopelex.
Described cationic surfactant comprises at least one in hexadecyl trimethylamine, tetradecyl chloride base benzyl dimethylamine, cetylpyridinium chloride.
Described non-ionic surfactant comprises at least one in Tween-80, OP, triton x-100 ,-cyclodextrin.
In described correctives solution, the volume ratio of correctives and water is (0.5 ~ 3): (500 ~ 2000).
According to some embodiments of the present invention, in described chromogenic reagent solution, the volume ratio of developer and water is (0.05 ~ 5g): 1L, and described developer is that 1-(2-pyridylazo)-beta naphthal (PAN), trihydroxy fluorones developer and 2-carboxyl-2 ' hydroxyl-5 ' sulfo group are together with any one in benzene-azo-benzene sodium salt.
According to some embodiments of the present invention, described damping fluid is borate buffer solution.
According to some embodiments of the present invention, the volume ratio of described chromogenic reagent solution, correctives solution and damping fluid is (0.5 ~ 2): (0.5 ~ 2): (1 ~ 3).
Additional aspect of the present invention and advantage will part provide in the following description, and part will become obvious from the following description, or be recognized by practice of the present invention.
Embodiment
Embodiments of the invention are described below in detail.It should be noted that, embodiment described below is exemplary, is intended to for explaining the present invention, and can not be interpreted as limitation of the present invention.
first, pack correctives solution and preparation method thereof is described.
According to the embodiment of the present invention for detect zinc ion in water quality pack correctives solution in containing correctives and water.
Wherein, described correctives can such as, for being anionic surfactant, dodecyl phenenyl sulfate, neopelex; Cationic surfactant, such as hexadecyl trimethylamine, tetradecyl chloride base benzyl dimethylamine, cetylpyridinium chloride; Non-ionic surfactant, such as, in Tween-80, OP, triton x-100 ,-cyclodextrin any one or multiple, especially preferred nonionic surfactants.Large quantity research through the present inventor finds, these correctivess can produce sensitization to system well, thus effectively can improve the sensitivity detected zinc ion.
In addition, preferably, in described pack regulator solution, the volume ratio of correctives and water is (0.5 ~ 5): (500 ~ 3000); Further preferably, in described pack regulator solution, the volume ratio of correctives and water is (0.5 ~ 3): (500 ~ 2000); Especially preferably, in described pack regulator solution, the volume ratio of correctives and water is 2:1000.
According to the pack of embodiment of the present invention correctives solution, its preparation method comprises the steps:
A) correctives is taken;
B) described correctives is dissolved in pure water, obtains described correctives solution.
Preferably, in described pack regulator solution, the volume ratio of correctives and water is (0.5 ~ 5): (500 ~ 3000); Further preferably, in described pack regulator solution, the volume ratio of correctives and water is (0.5 ~ 3): (500 ~ 2000); Especially preferably, in described pack regulator solution, the volume ratio of correctives and water is 2:1000.
secondly, chromogenic reagent solution and preparation method thereof is described.
In addition, the correctives solution of the embodiment of the present invention is suitable for combining with xylenol orange chromogenic reagent solution, porphin series solution, Fluorone reagent series chromogenic reagent solution, peacock green chromogenic reagent solution and azo chromogenic reagent solution, for zinc ion in detection water quality.
The regulator solution of the embodiment of the present invention is suitable for combining with 1-(2-pyridylazo)-beta naphthal (PAN) chromogenic reagent solution, SAF chromogenic reagent solution, zincon solution, for zinc ion in detection water quality.
Below, for different chromogenic reagent solution, its composition and configuration method is described respectively.
pyridylazo)-beta naphthal (PAN) chromogenic reagent solution
1-(2-pyridylazo)-beta naphthal (PAN) is orange red crystalline powder, is tridentate ligand body structure, can react generate ML with zinc ion
2the chelate that type is stable, has larger absorbance between 550 ~ 570nm, can go out zinc ion concentration by monitor.
The preparation of chromogenic reagent solution: take PAN0.50g in 500mL volumetric flask, to add after ethanol with supersonic oscillations process and constant volume, is made into the PAN nitrite ion mother liquor that mass concentration is 1.00g/L, is diluted to desired concn as required during experiment.
developer
SAF is a kind of trihydroxy fluorones developer, reagent is containing chromophore (quinonyl) and auxochrome (hydroxyl), and there is the large bond structure of rigidity, plane and conjugation, easy absorption visible ray, ultraviolet light, under suitable surfactant exists, its water-soluble increase, absorption peak red shift, mole increase, it is usually at 105 ~ 106L.mol
-1.cm
-1between, be the highly sensitive developer of metallic ion.
In examples more of the present invention, employing SAF is developer, utilizes reverse automatic reference FIA method to determine trace zinc in seawater, sensitivity is higher, accuracy is good, and detecting of the method is limited to 1.5 μ g/L, and the range of linearity is 5 ~ 400 μ g/L relative standard deviations is 1.85%.
zincon developer
Zincon is organic compound, and it consists of 2-carboxyl-2 ' hydroxyl-5 ' sulfo group together with benzene-azo-benzene sodium salt, is the azo-compound generated by phenol and aromatic diazo salt action.Phenol as coupling component has acidity, therefore zincon can be dissolved in sodium hydrate aqueous solution.Because the color acidity of the method is in pH8.5 ~ 9.5, so the concentration of sodium hydroxide solution should not be selected excessive, the general sodium hydroxide solution of 2mol/L of selecting is dissolved.Color development system is stablized, and adds surfactant and have stronger sensitization to system.
finally, the method for detecting zinc ion in water is described.
Use the pack of above-mentioned any embodiment, the content of the zinc ion in water quality can be detected.
According to the method for detecting zinc ion in water of the embodiment of the present invention, comprise the following steps:
Measure correctives solution, chromogenic reagent solution and damping fluid;
In water to be detected, add described correctives solution, chromogenic reagent solution and damping fluid successively and mix, obtaining test samples; And
Use the absorbance of test samples described in spectrophotometer measurement, and calculate the Zn content in described water sample to be detected, wherein,
In described test samples, the volume ratio of described water to be detected and chromogenic reagent solution, correctives solution liquid and damping fluid is (3 ~ 15): (0.5 ~ 3): (0.5 ~ 3): (1 ~ 4),
In described correctives solution, the volume ratio of correctives and water is (0.5 ~ 5): (500 ~ 3000), and described correctives is any one in anionic surfactant, cationic surfactant, non-ionic surfactant.
In examples more of the present invention, zinc standard aqueous solution and described correctives solution, chromogenic reagent solution and damping fluid is used to mix and measure absorbance, to draw zinc solution standard absorbance curve, and by the absorbance of described test samples and described standard absorbance curve are compared the Zn content calculated in described water sample to be detected.
Preferably, the volume ratio of described water sample to be detected and correctives solution, chromogenic reagent solution and damping fluid is (3 ~ 15): (0.5 ~ 3): (0.5 ~ 3): (1 ~ 4).
With must with compared with abstraction technique in prior art, according to detection method of the present invention, avoid and use methenyl choloride contour toxic organic solvent extract the harm and environmental pollution that bring, fast easy, measurement result is accurately, more friendly to environment.
Below, described in detail according to the pack of the embodiment of the present invention and the detection method using this pack by preferred embodiment.
Wherein, with developer be zincon, regulator solution for OP solution, damping fluid for borate buffer solution for example is described detection method.For the situation of the pack of other embodiments of use, except the composition difference of pack, identical method can be adopted to detect, and description is omitted herein.
Embodiment 1
For monitoring the raw materials of the pack of zinc ion be: potassium chloride, boric acid, NaOH and pure water that the OP that the ethanol that the zincon that purity is AR, purity are AR, purity are AR, purity are AR.
The preparation of chromogenic reagent solution: take a certain amount of zincon, adds a certain amount of ethanol and dissolves, as in 1000ml volumetric flask, use ethanol constant volume, mix for subsequent use.Wherein, in described chromogenic reagent solution, the mass volume ratio of developer and water is 0.08g:1L.
The preparation of regulator solution: accurately measured amounts OP is dissolved in pure water, is stirred to and dissolves completely, then add pure water, be settled to 1000ml, mixing, be kept in brown volumetric flask for subsequent use, the mass volume ratio of described correctives and pure water is 10ml:1L.
The preparation of damping fluid: take a certain amount of potassium chloride-boric acid-NaOH and be dissolved in pure water, shake up, then add pure water, be settled to 1000ml, shake up, for subsequent use.
The drafting of typical curve: accurately pipette 0,5,10,15,20,25,30,35,40,45,50ml concentration is that the plumbous standard solution of 20mg/L is in 100ml volumetric flask, add 1ml screening agent, solution is fully mixed, after adding 1ml developer, solution is fully mixed, add 1ml damping fluid again, fully shake up, after a few minutes, take reagent blank as reference, 30mm cuvette, a given wavelength measures absorbance, and drawing standard curve.
Embodiment 2
Target actual water sample is added with Tianrui's online water quality zinc ion monitor automatic sucking is a certain amount of, automatic sucking chromogenic reagent solution, correctives solution, damping fluid successively again, by automatic mixing, after 5 minutes, take reagent blank as the cuvette of reference, 30mm light path, measure absorbance at 620nm wavelength place, it is 1.7% that the result measured for six times is respectively 1.548,1.597,1.604,1.626,1.580,1.615, relative standard deviation RSD.
From the present embodiment, the pack monitoring zinc ion of the monitoring zinc ion adopting the present invention to prepare, measured result precision, accuracy are all fine, solve because auto injection pipeline remains brought error.
Embodiment 3
By a certain amount of actual water sample of Tianrui's online water quality lead ion monitor automatic sucking, automatic sucking chromogenic reagent solution, correctives solution, damping fluid successively again, by automatic mixing, after 5 minutes, take reagent blank as the cuvette of reference, 30mm light path, measure absorbance at 620nm wavelength place, the result measured for six times is respectively 0.092,0.086,0.088,0.084,0.084,0.088,0.088, and relative standard deviation is 0.0028.
From the present embodiment, adopt agents useful for same of the present invention and water sample that proportioning is surveyed to detect lower limit and be low to moderate 0.1mg/L, reach Standard.
In the description of this instructions, specific features, structure, material or feature that the description of reference term " embodiment ", " some embodiments ", " example ", " concrete example " or " some examples " etc. means to describe in conjunction with this embodiment or example are contained at least one embodiment of the present invention or example.In this manual, identical embodiment or example are not necessarily referred to the schematic representation of above-mentioned term.And the specific features of description, structure, material or feature can combine in an appropriate manner in any one or more embodiment or example.
Although illustrate and describe embodiments of the invention above, be understandable that, above-described embodiment is exemplary, can not be interpreted as limitation of the present invention, those of ordinary skill in the art can change above-described embodiment within the scope of the invention when not departing from principle of the present invention and aim, revising, replacing and modification.
Claims (2)
1. for detecting a pack for zinc ion in water quality, it is characterized in that, described pack is made up of correctives solution, chromogenic reagent solution and damping fluid,
In described correctives solution, the volume ratio of correctives and water is 10ml:1L, and described correctives is OP,
In described chromogenic reagent solution, the volume ratio of developer and water is 0.08g:1L, described developer be 2-carboxyl-2 ' hydroxyl-5 ' sulfo group together with benzene-azo-benzene sodium salt,
The volume ratio of described chromogenic reagent solution, correctives solution and damping fluid is 1:1:1.
2. pack as claimed in claim 1, it is characterized in that, described damping fluid is borate buffer solution.
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| CN103529114B (en) * | 2013-10-18 | 2015-10-14 | 山东理工大学 | A kind of household garden stuff pesticide residue fast detector |
| CN104297240A (en) * | 2014-10-24 | 2015-01-21 | 中国人民解放军国防科学技术大学 | Method and device applied to detection of toxic metal ions in water |
| CN104535564A (en) * | 2014-12-26 | 2015-04-22 | 四川大学 | Concentration pillar filling, concentration pillar and application of concentration pillar in analysis of trace metal elements |
| CN104597045B (en) * | 2015-01-09 | 2017-07-21 | 上海绿帝环保科技有限公司 | A kind of preparation and application of water quality total heavy metal detection agent |
| CN105548177B (en) * | 2016-02-19 | 2019-02-22 | 常州罗盘星检测科技有限公司 | One kind is for anionic polymer concentration quick detection reagent packet and detection method in aqueous systems |
| CN112557317A (en) * | 2020-11-20 | 2021-03-26 | 上海仪电科学仪器股份有限公司 | Method for measuring zinc ion content |
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| WO2004109256A3 (en) * | 2003-06-06 | 2005-01-13 | Univ Case Western Reserve | Deposition and detection of zinc and other metals in solution |
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| WO2008078641A1 (en) * | 2006-12-27 | 2008-07-03 | Keio University | Method for electrochemically measuring zinc ion |
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| CN1137117A (en) * | 1995-05-29 | 1996-12-04 | 朱建安 | Method for measuring Zn content in urine |
| WO2004109256A3 (en) * | 2003-06-06 | 2005-01-13 | Univ Case Western Reserve | Deposition and detection of zinc and other metals in solution |
| CN101173931A (en) * | 2006-10-30 | 2008-05-07 | 苏州艾杰生物科技有限公司 | Zinc diagnosis/measuring reagent kit and method for measuring zinc concentration |
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