CN109827915A - A kind of bi-component detection agent measuring phosphorus content - Google Patents
A kind of bi-component detection agent measuring phosphorus content Download PDFInfo
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- CN109827915A CN109827915A CN201910186647.0A CN201910186647A CN109827915A CN 109827915 A CN109827915 A CN 109827915A CN 201910186647 A CN201910186647 A CN 201910186647A CN 109827915 A CN109827915 A CN 109827915A
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Abstract
The present invention relates to a kind of bi-component detection agents for measuring phosphorus content, belong to technical field of analysis and detection.A kind of bi-component detection agent of measurement phosphorus content of the invention is solids two-component, including detection agent component A and component B, it is simple with preparation, performance is stablized, measure it is sensitive, quick, the features such as being easy to save, be convenient for carrying and operate with, it solves the problems, such as that measurement uses liquid reagent unstable and inconvenient to carry and difficulty, is quickly measured suitable for phosphorus content.Use can be operated in layman.As long as directly carrying out phosphorus detection using spectrophotometer or optical colorimetry in use, the component A and component B of the measurement phosphorus content bi-component detection agent are successively separately added into testing sample solution.
Description
Technical field
The present invention relates to a kind of bi-component detection agents for measuring phosphorus content, belong to technical field of analysis and detection.
Background technique
Phosphorus is nutrient necessary to biological growth and development.It is not only the group of many important organic compounds in plant
At ingredient, various metabolic physiology processes in plant are participated in, and are also the limitative nutrient of water body planktonic algae growth,
Its content and water body generation eutrophication are closely related.Therefore, the measurement of phosphorus content, for water resource, soil, aquaculture etc.
It has a very important significance and application value.
The measuring method of phosphorus content mainly has gravimetric method, volumetric method and spectrophotometry etc..Gravimetric detemination phosphorus, operated
Journey is cumbersome tediously long, and not applicable low content phosphorus yield.Volumetric determination phosphorus content, because being generated by solution acidity and reaction
The unstable influence of the component of object, evaluated error are larger.Spectrophotometry measurement phosphorus content, including basic dye heteropoly acid are polynary
Associated matter spectrophotometry and molybdenum-antimony anti-spectrophotometric method.Basic dye heteropoly acid multiple association object spectrophotometry measures phosphorus,
It is to react to generate ionic associate and be measured based on phosphomolybdate and the dye of positive ion such as peacock green etc..But the measuring method needs
The measurement of phosphorus content carried out under highly acidity and permolybdic acid salt concentration conditions, and measure background value height, limit it in phosphorus
Application in content quick determination.Molybdenum-antimony anti-spectrophotometric method is a kind of common method for measuring phosphor content.The measuring method is
Under a certain concentration sulfuric acid or hydrochloric acid acidity condition, orthophosphoric acid root and ammonium molybdate and trivalent antimony ion are collectively formed P: Sb: Mo
Atomic ratio be about 1: 2: 12 the heteromeric complex compound of phosphorus antimony molybdenum.Then, a kind of molybdenum that high chroma is stable is reduced by ascorbic acid
Indigo plant is measured using spectrophotometry.Molybdenum-antimony anti-spectrophotometric method measures phosphorus, and color stability, high sensitivity is easy to operate,
It is widely used in the measurement of phosphorus content.But this method carries out the measurement of phosphorus content, needs to be added a certain concentration liquid prepared in advance
Body acid and liquid reagent carry out the measurement of phosphorus content, it has not been convenient to carry and use.Especially liquid reagent (such as ascorbic acid) is steady
Qualitative difference, Extemporaneous when needing to measure are not able to satisfy the needs of phosphorus content quickly measured.
Summary of the invention
The purpose of the present invention is to provide a kind of bi-component detection agents for measuring phosphorus content, to overcome the deficiencies of the prior art,
Quick measurement applied to phosphorus content.
To achieve the goals above, the invention adopts the following technical scheme: it is a kind of measure phosphorus content bi-component detection agent,
Increased using solids two-component, preferred composition reagent and its composition weight ratio with improving the sensitivity and accuracy of measuring method
The stability of strong detection agent is convenient for carrying and uses convenient for saving for a long time, and the quick measurement suitable for phosphorus content needs.
A kind of bi-component detection agent of measurement phosphorus content of the invention, including detection agent component A and component B.Respectively by molybdenum
Sour ammonium, potassium antimony tartrate, tartaric acid, sulfamic acid, mixing reducing agent, complexing increase steady agent, solid acid and polyvinyl alcohol, according to one
Surely the weight ratio mixed preparing for forming reagent forms.
Wherein it is preferred to which the mixing reducing agent is by ascorbic acid, thiocarbamide and sucrose, according to WAscorbic acid∶WThiocarbamide∶WSucroseFor
1: 1: 6 weight ratio is hybridly prepared into.
The complexing increase steady agent be by disodium ethylene diamine tetraacetate (referred to as EDTA-2Na) and sodium sulphate, according to
WEDTA-2Na∶WSodium sulphateIt is hybridly prepared into for 1: 40 weight ratio.
The solid acid is that sulfuric acid is added in silica gel, and reaction prepares solid acid.It reacts as follows:
SiO2-OH+HO-SO3H——SiO2-OSO3H+H2O
Wherein it is preferred to which a kind of bi-component detection agent component A of measurement phosphorus content is 1~3g ammonium molybdate, 0.15
~0.45g potassium antimony tartrate, 4~10g sulfamic acid and 8~20g solid acid；Detection agent component B is 2~4g mixing reducing agent, 1
~2g tartaric acid, 5~10g complexing increase steady agent and 0.02~0.04g polyvinyl alcohol.
Mentioned reagent is to analyze pure or its ratings above reagent.Silica gel is chromatographically pure (200~300 mesh of granularity).
A kind of application method of the bi-component detection agent of measurement phosphorus content of the invention are as follows:
20ml testing sample solution is pipetted in 25ml color-comparison tube, 0.80g bi-component detection agent component A is first added,
1min is stood after shaking up.Then, 0.10g detection agent component B is added, is dissolved, colour developing 15mim is stood, using spectrophotometer
In λ700nmOr optical colorimetry carries out phosphorus detection.
Effect of the invention is that:
A kind of bi-component detection agent of measurement phosphorus content of the invention has preparation simply, property using solid component A, B
The features such as energy is stablized, and measurement is sensitive, quick, saves and easy to carry, easily operated use.Solve measurement using liquid acid and
The problem and difficulty unstable, inconvenient to carry of liquid reagent.Use can be operated in layman, is suitable for water quality, soil
The quick measurement of the phosphorus contents such as earth, aquaculture.As long as in use, by a kind of bi-component detection agent for measuring phosphorus content of the present invention
Component A and component B are successively added separately in testing sample solution, are directly carried out using spectrophotometer or optical colorimetry
The measurement of phosphorus content.
Specific embodiment
Below by way of description the embodiment of the present invention, just a kind of bi-component detection for measuring phosphorus content provided by the present invention
Agent is described further.
A kind of embodiment 1: preparation for the bi-component detection agent measuring phosphorus content
(1) 0.25g ascorbic acid, 0.25g thiocarbamide and 1.5g sucrose are uniformly mixed by, obtain mixing reducing agent；
(2) 0.15g EDTA-2Na and 6g sodium sulphate is uniformly mixed by, is obtained complexing and is increased steady agent；
(3) 80% sulfuric acid of 60ml is added in 10g silica gel by, stirs 3h, and filtering, 110 DEG C of drying obtain solid acid；
(4) 1g ammonium molybdate, 0.15g potassium antimony tartrate, 4g sulfamic acid and 8g solid acid are uniformly mixed by, are detected
Agent component A；
(5) is uniform by 2g mixing reducing agent, 1g tartaric acid, the steady agent of 5g complexing increasing and 0.02g polyvinyl alcohol, obtains
Detection agent component B.
A kind of embodiment 2: preparation for the bi-component detection agent measuring phosphorus content
(1) 0.5g ascorbic acid, 0.5g thiocarbamide and 3g sucrose are uniformly mixed by, obtain mixing reducing agent；,
(2) 0.2g EDTA-2Na and 8g sodium sulphate is uniformly mixed by, is obtained complexing and is increased steady agent；
(3) 80% sulfuric acid of 90ml is added in 15g silica gel by, stirs 3h, and filtering, 110 DEG C of drying obtain solid acid；
(4) 2 ammonium molybdates, 0.3g potassium antimony tartrate, 7g sulfamic acid and 14g solid acid are uniformly mixed by, obtain detection agent
Component A；
(5) is uniform by 3g mixing reducing agent, 1.5g tartaric acid, the steady agent of 7.5g complexing increasing and 0.03g polyvinyl alcohol,
Obtain detection agent component B.
A kind of embodiment 3: preparation of the bi-component detection agent of phosphorus content
(1) 0.5g ascorbic acid, 0.5g thiocarbamide and 3g sucrose are uniformly mixed by, obtain mixing reducing agent；,
(2) 0.25g EDTA-2Na and 10g sodium sulphate is uniformly mixed by, is obtained complexing and is increased steady agent；
(3) 80% sulfuric acid of 120ml is added in 20g silica gel by, stirs 3h, and filtering, 110 DEG C of drying obtain solid acid；
(4) 3g ammonium molybdate, 0.45g potassium antimony tartrate, 10g sulfamic acid and 20g solid acid are uniformly mixed by, are examined
Survey agent component A；
(5) is uniform by 4g mixing reducing agent, 2g tartaric acid, the steady agent of 10g complexing increasing and 0.04g polyvinyl alcohol, is ground into
Powder obtains detection agent component B.
Embodiment 4: the measurement of water sample phosphorus content
Pretreated water sample 20ml to be measured is pipetted in 25ml color-comparison tube, according to said determination method, is successively distinguished
Bi-component detection agent component A and component B is added, using spectrophotometer in λ700nmIt is measured.Measurement result shows using this
Invention a kind of measurement phosphorus content bi-component detection agent measurement water sample in phosphorus content be 103.43 μ g/L, with use National Standard Method
103.20 μ g/L of GB11893-89 measurement result coincide.
Embodiment 5: the measurement of pedotheque phosphorus content
6 parts of each 20ml of soil testing sample solution for pipetting preprocessed extraction successively distinguish according to said determination method
Bi-component detection agent component A and component B is added, using spectrophotometer in λ700nmCarry out the measurement of pedotheque phosphorus content.And
It is measured using National Standard Method GB9837-88, the results are shown in Table 1.Show using a kind of measurement phosphorus content provided by the invention
Bi-component detection agent carry out pedotheque phosphorus content measurement, it is almost the same with National Standard Method GB9837-88 measurement result.
The measurement result (mg/kg) of pedotheque phosphorus content
Said determination carries out water sample the result shows that using a kind of bi-component detection agent for measuring phosphorus content provided by the invention
It is quick, easy with the measurement of phosphorus content in pedotheque, as a result reliably.
The above is only a preferred embodiment of the present invention, to a kind of double groups for measuring phosphorus content provided by the present invention
Divide and further illustrated made by detection agent, is not intended to limit the invention.It is noted that, not departing within the principle of the present invention
Made any modification, equivalent replacement and modification etc., should all be included in the protection scope of the present invention.
Claims (6)
1. it is a kind of measure phosphorus content bi-component detection agent, it is characterised in that: the bi-component detection agent include detection agent component A and
Component B, respectively by ammonium molybdate, potassium antimony tartrate, tartaric acid, sulfamic acid, mixing reducing agent, complexing increase steady agent, solid acid and
Polyvinyl alcohol is hybridly prepared into according to the weight ratio of definite composition reagent.As long as in use, by the detection agent component A and component B
It is successively added separately in testing sample solution, the survey of phosphorus content is directly carried out using spectrophotometer or optical colorimetry
It is fixed.
2. a kind of bi-component detection agent for measuring phosphorus content according to claim 1, it is characterised in that: the mixing reduction
Agent is by ascorbic acid, thiocarbamide and sucrose, according to WAscorbic acid∶WThiocarbamide∶WSucroseIt is hybridly prepared into for 1: 1: 6 weight ratio.
3. a kind of bi-component detection agent for measuring phosphorus content according to claim 1, it is characterised in that: the complexing increases steady
Agent is by disodium ethylene diamine tetraacetate (referred to as EDTA-2Na) and sodium sulphate, according to WEDTA-2Na∶WSodium sulphateFor 1: 40 weight ratio
It is hybridly prepared into.
4. a kind of bi-component detection agent for measuring phosphorus content according to claim 1, it is characterised in that: the solid acid is
Sulfuric acid is added in silica gel, solid acid is prepared in reaction.
5. a kind of bi-component detection agent for measuring phosphorus content according to claim 1, it is characterised in that: the detection agent group
Dividing A is 1~3g ammonium molybdate, 0.15~0.45g potassium antimony tartrate, 4~10g sulfamic acid and 8~20g solid acid；Detection agent group
Dividing B is 2~4g mixing reducing agent, 1~2g tartaric acid, the steady agent of 5~10g complexing increasing and 0.02~0.04g polyvinyl alcohol.
6. a kind of application method of bi-component detection agent for measuring phosphorus content according to claim 1, it is characterised in that: move
It takes 20ml testing sample solution in 25ml color-comparison tube, 0.80g detection agent component A is first added, stands 1min after shaking up.So
Afterwards, 0.10g detection agent component B is added, is dissolved, colour developing 15mim is stood, using spectrophotometer in λ700nmOr visual colorimetric determination
The measurement of method progress phosphorus content.
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