CN107102102A - A kind of detection method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid - Google Patents
A kind of detection method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid Download PDFInfo
- Publication number
- CN107102102A CN107102102A CN201710308753.2A CN201710308753A CN107102102A CN 107102102 A CN107102102 A CN 107102102A CN 201710308753 A CN201710308753 A CN 201710308753A CN 107102102 A CN107102102 A CN 107102102A
- Authority
- CN
- China
- Prior art keywords
- ethephon
- cepha
- chloroethyl
- phosphonic acid
- measured
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
-
- 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
- G01N21/29—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands using visual detection
-
- 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
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
-
- 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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
Landscapes
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Molecular Biology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The present invention discloses a kind of detection method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid, including：(1) take ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample to be dissolved in water, obtain the first solution to be measured, determine the first Chlorine in Solution ion concentration to be measured；(2) take after another identical ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample is dissolved in water, plus alkali is adjusted to alkalescence, reaction obtains intermediate product, heats, until the intermediate product is decomposed completely, cools down, obtains the second solution to be measured；Determine the Chlorine in Solution ion concentration to be measured；(3) the second Chlorine in Solution ion concentration to be measured that content of dissociative chlorine ion and the step (2) are obtained in the described first solution to be measured obtained according to the step (1), calculating obtains ethephon (CEPHA),2-(chloroethyl) phosphonic acid content in the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample.Methods described can be used for ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample of the detection containing interfering material, and measurement range is wide, and available for detection ethephon (CEPHA),2-(chloroethyl) phosphonic acid active compound, single dose and complex preparation, and the rate of recovery, accuracy are high.
Description
Technical field
The present invention relates to detection technique field, and in particular to a kind of detection method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid.
Background technology
Ethephon (CEPHA),2-(chloroethyl) phosphonic acid (ISO adopted names：Ethephon, chemical name：The chloro- ethylphosphonic acids of 2-), it is a kind of high-quality and efficient plant
Thing growth regulator, empirical formula is C2H6ClO3P, structural formula isEthephon (CEPHA),2-(chloroethyl) phosphonic acid is easily absorbed by plants, in plant body
It is interior to discharge ethene rapidly, strengthen the peroxidase activity of plant, so as to reduce apical dominance, increase effective tillering, make plant
Stalwartness is downgraded, lodging is prevented；Also plant male sterility can be made, ahead of time result, promotes fruit early-maturing, neat ripe；Also having makes cotton
Fallen leaves, tea tree take off flower bud effect；It can also be used as accelerating ripening of fruit agent.Ethephon (CEPHA),2-(chloroethyl) phosphonic acid be widely used in paddy rice, wheat, sorghum, cotton,
In the plurality of cereals of rape, melon, tomato, banana, apple, pineapple, rubber tree, tobacco leaf etc. 50 and industrial crops, ethephon (CEPHA),2-(chloroethyl) phosphonic acid should
It is rapid with research and development, there is facilitation to China's agricultural production.
The detection method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid plays an important role to the application study of ethephon (CEPHA),2-(chloroethyl) phosphonic acid.At present, ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample ethene
The content of profit is typically used, and ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample is neutralized into alkalescence, generates ethephon (CEPHA),2-(chloroethyl) phosphonic acid disodium salt, and ethene and phosphoric acid are generated after heating
Sodium dihydrogen, biphosphate sodium content is determined with sodium hydroxide titration, thus seeks calculation ethephon (CEPHA),2-(chloroethyl) phosphonic acid mass fraction.The method is only capable of determining
Ethephon (CEPHA),2-(chloroethyl) phosphonic acid content in ethephon (CEPHA),2-(chloroethyl) phosphonic acid active compound or single dose, when in ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample contain interfering material, such as potassium dihydrogen phosphate, di(2-ethylhexyl)phosphate
When hydrogen ammonium, ammonium hydrogen phosphate, phosphoric acid, ammonium sulfate and the ion precipitated with alkali reaction generation, the measure of ethephon (CEPHA),2-(chloroethyl) phosphonic acid content can be by dry
Disturb, determine incorrect.
The content of the invention
In view of this, it can be used for ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample of the detection containing interfering material this application provides a kind of methods described, survey
Determine scope wide, available for detection ethephon (CEPHA),2-(chloroethyl) phosphonic acid active compound, single dose and complex preparation, and the rate of recovery, accuracy are high.
To solve above technical problem, the technical scheme that the present invention is provided is a kind of detection method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid, including：
(1) take ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample to be dissolved in water, obtain the first solution to be measured, determine the first Chlorine in Solution ion to be measured
Content；
(2) take after another identical ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample is dissolved in water, plus alkali is adjusted to alkalescence, reaction obtains intermediate product, plus
Heat, until the intermediate product is decomposed completely, cools down, obtains the second solution to be measured；The Chlorine in Solution ion to be measured is determined to contain
Amount；
(3) content of dissociative chlorine ion and the step (2) in the described first solution to be measured obtained according to the step (1)
The second obtained Chlorine in Solution ion concentration to be measured, calculating obtains ethephon (CEPHA),2-(chloroethyl) phosphonic acid content in the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample.
It is preferred that, ethephon (CEPHA),2-(chloroethyl) phosphonic acid content is calculated as follows in the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample：
In formula：
X is ethephon (CEPHA),2-(chloroethyl) phosphonic acid content in the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample represented with mass fraction, and numerical value is represented with %；M1For chlorion
Molal weight, M1=35.45g/mol；M2For ethephon (CEPHA),2-(chloroethyl) phosphonic acid molal weight, M2=144.5g/mol；X1Represented with mass fraction
The first Chlorine in Solution ion concentration to be measured, numerical value represents with %, X2It is described second to be measured molten for what is represented with mass fraction
Chloride ion content in liquid, numerical value is represented with %.
It is preferred that, second solution to be measured includes：Ethene, chlorate, dihydric phosphate.
It is preferred that, alkali described in the step (2) is potassium hydroxide or sodium hydroxide, and the intermediate product is ethephon (CEPHA),2-(chloroethyl) phosphonic acid two
Sodium salt or ethephon (CEPHA),2-(chloroethyl) phosphonic acid di-potassium.
It is preferred that, heating-up temperature is 90~110 DEG C in the step (2).
It is preferred that, using a mole method, potentiometric titration, Enrichment AAS, mercury salt titration, mercuric thiocyanate
AAS, the chromatography of ions, visual turbidimetry, ion selective electrode method, atomic absorption spectrphotometry indirect method, silver nitrate
First Chlorine in Solution ion concentration to be measured and described second described in volumetric method, mercuric nitrate volumetric method or rhodan ammonium titration measuring
Chlorine in Solution ion concentration to be measured.
It is preferred that, using the described in potentiometric determination first Chlorine in Solution ion concentration to be measured and described second to be measured molten
Chloride ion content in liquid.
It is preferred that, the step (1) is specially to take ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample to be dissolved in water, and obtains the first solution to be measured, adds nitre
Acid solution is adjusted in acidity, is titrated with silver nitrate standard titration solution, is terminal to potential break, is determined described first to be measured
Chlorine in Solution ion concentration.
It is preferred that, the first Chlorine in Solution ion concentration to be measured is calculated as follows：In formula：
X1For the described first Chlorine in Solution ion concentration to be measured represented with mass fraction, numerical value is represented with %；M1For chlorion mole matter
Amount, M1=35.45g/mol；V1To determine step (1) consumption nitric acid silver label described in the first Chlorine in Solution ion concentration to be measured
Quasi- volumetric soiutions volume, Unit/mL；m1Ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample quality, unit g are taken by the step (1)；C drips for silver nitrate standard
Determine solution concentration, unit mol/L.
It is preferred that, the step (2) is specially to take after another identical ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample is dissolved in water, plus alkali is adjusted to alkali
Property, reaction obtains intermediate product, heated, until the intermediate product is decomposed completely, cools down, and obtains the second solution to be measured, adds
Salpeter solution is adjusted in acidity, is titrated with silver nitrate standard titration solution, be terminal to potential break, determine described in obtain
Second Chlorine in Solution ion concentration to be measured.
It is preferred that, the second Chlorine in Solution ion concentration to be measured is calculated as follows：In formula：
X2For the described second Chlorine in Solution ion concentration to be measured represented with mass fraction, numerical value is represented with %；M1For chlorion mole matter
Amount, M1=35.45g/mol；V2To determine step (2) consumption nitric acid silver label described in the second Chlorine in Solution ion concentration to be measured
Quasi- volumetric soiutions volume, Unit/mL；m2To take ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample quality, unit g by the step (2)；C is silver nitrate standard
Volumetric soiutions concentration, unit mol/L.
It is preferred that, the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample include interfering material, the interfering material be phosphate anion, hydrogen phosphate from
It is one or more in son, dihydrogen phosphate ions and the ion precipitated with alkali reaction generation.
It is preferred that, the foreign ion is potassium dihydrogen phosphate, ammonium dihydrogen phosphate, ammonium hydrogen phosphate, phosphoric acid, ammonium sulfate and and alkali
Reaction produces one or more in the ion precipitated.
It is preferred that, reacted with alkali and produce the ion of precipitation for calcium ion, magnesium ion or aluminium ion.
It is preferred that, the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample is ethephon (CEPHA),2-(chloroethyl) phosphonic acid active compound, ethephon (CEPHA),2-(chloroethyl) phosphonic acid preparation, and the ethephon (CEPHA),2-(chloroethyl) phosphonic acid preparation is ethephon (CEPHA),2-(chloroethyl) phosphonic acid list
Agent or ethephon (CEPHA),2-(chloroethyl) phosphonic acid complex preparation.
It is preferred that, the ethephon (CEPHA),2-(chloroethyl) phosphonic acid preparation formulation is water dispersible granules, wettable powder, soluble powder or aqua..
It is preferred that, the ethephon (CEPHA),2-(chloroethyl) phosphonic acid preparation formulation is solvable pulvis.
It is preferred that, the first Chlorine in Solution ion concentration to be measured is content of dissociative chlorine ion in the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample.
It is preferred that, the second Chlorine in Solution ion concentration to be measured is total chloridion content in the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample.
Compared with prior art, its detailed description is as follows by the application：
The chlorine ions fraction that the present invention is decomposited by determining ethephon (CEPHA),2-(chloroethyl) phosphonic acid in ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample calculates ethephon (CEPHA),2-(chloroethyl) phosphonic acid indirectly
The content of ethephon (CEPHA),2-(chloroethyl) phosphonic acid in sample；It is adaptable to determine ethephon (CEPHA),2-(chloroethyl) phosphonic acid in ethephon (CEPHA),2-(chloroethyl) phosphonic acid active compound, ethephon (CEPHA),2-(chloroethyl) phosphonic acid single dose or ethephon (CEPHA),2-(chloroethyl) phosphonic acid complex preparation
Content, ethephon (CEPHA),2-(chloroethyl) phosphonic acid content can accurately be also determined to the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample containing interfering material, and detection accuracy, the rate of recovery are high；
Determine chloride test method maturation various, different accuracy of detection requirements and different chloride ion content ranges can be met
Detection, so as to ensure that the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample of the sharp content of differing ethylene determines demand, it is easy to commercial application；
Heat resolve intermediate product process in continuous mode of the present invention, the ethene and ethephon (CEPHA),2-(chloroethyl) phosphonic acid compound probability for making generation reacts
Generate monochlorethane and/or dichloroethanes, heating volatilization, it is ensured that ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample determines the accuracy of ethephon (CEPHA),2-(chloroethyl) phosphonic acid content.
Embodiment
In order that those skilled in the art more fully understands technical scheme, with reference to specific embodiment pair
The present invention is described in further detail.
Embodiment 1
1st, test example
A kind of detection method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid, including：
(1) take 1.5g ethephon (CEPHA),2-(chloroethyl) phosphonic acids sample plus 100ml water to dissolve, obtain the first solution to be measured, determine described first to be measured molten
Chloride ion content in liquid；The ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample is the ethephon (CEPHA),2-(chloroethyl) phosphonic acid active compound of 0.25~0.35wt% containing free chloro ion；
(2) take after another identical 0.1g ethephon (CEPHA),2-(chloroethyl) phosphonic acids sample plus the dissolving of 100mL water, plus alkali is adjusted to alkalescence, during reaction is obtained
Between product, 90~110 DEG C of heating 30min, until the intermediate decomposes completely, being cooled to 15~30 DEG C, to obtain second to be measured molten
Liquid, determine described in obtained the second Chlorine in Solution ion concentration to be measured；The alkali is sodium hydroxide, and the intermediate product is ethene
Sharp disodium；Second solution to be measured includes：Ethene, sodium chloride, sodium dihydrogen phosphate.
(3) content of dissociative chlorine ion and the step (2) in the described first solution to be measured obtained according to the step (1)
The second obtained Chlorine in Solution ion concentration to be measured, calculating obtains ethephon (CEPHA),2-(chloroethyl) phosphonic acid content in the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample, numbering test group
1, experimental result is shown in Table 1.
Wherein, the measure first Chlorine in Solution ion concentration process to be measured is specially：Add 3~4 drop nitric acid molten
Liquid is adjusted in acidity, is titrated with silver nitrate standard titration solution, is terminal to potential break, is determined first solution to be measured
Middle chloride ion content；The the second Chlorine in Solution ion concentration process to be measured obtained described in the measure is specially：Add nitric acid molten
Liquid is adjusted in acidity, is titrated with silver nitrate standard titration solution, is terminal to potential break, determine described in obtain second treat
Survey Chlorine in Solution ion concentration；
The first Chlorine in Solution ion concentration to be measured is calculated as follows：
The second Chlorine in Solution ion concentration to be measured is calculated as follows：
Ethephon (CEPHA),2-(chloroethyl) phosphonic acid content is calculated as follows in the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample：
In formula：
X is ethephon (CEPHA),2-(chloroethyl) phosphonic acid content in the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample represented with mass fraction, and numerical value is represented with %；M1For chlorion
Molal weight, M1=35.45g/mol；M2For ethephon (CEPHA),2-(chloroethyl) phosphonic acid molal weight, M2=144.5g/mol；X1Represented with mass fraction
The first Chlorine in Solution ion concentration to be measured, numerical value represents with %, X2It is described second to be measured molten for what is represented with mass fraction
Chloride ion content in liquid, numerical value is represented with %；V1The step (1) described in determining the first Chlorine in Solution ion concentration to be measured disappears
Consume silver nitrate standard titration solution volume, Unit/mL；V2To determine step described in the second Chlorine in Solution ion concentration to be measured
(2) silver nitrate standard titration solution volume, Unit/mL are consumed；m1Ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample quality, unit g are taken by the step (1)；
m2To take ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample quality, unit g by the step (2)；C is silver nitrate standard titration solution concentration, unit mol/
L。
The above-mentioned step of test group 1 of repetition, numbering test group 2~5, experimental result is shown in Table 1.
2nd, reference examples
With reference to GB 24750-2009, the same batch ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample of test example plus 0.5mol/L sodium hydroxides, thyme are taken
Phenol indigo plant is indicator, is neutralized to alkalescence, and solution is changed into blueness from yellow；Boiling water bath heating generation ethene and sodium dihydrogen phosphate, it is cold
But, it is terminal to be changed into blueness from yellow with 0.1mol/L sodium hydroxide titrations sodium dihydrogen phosphate to solution, obtains the matter of ethephon (CEPHA),2-(chloroethyl) phosphonic acid
Amount fraction, numbering control group group 1, experimental result is shown in Table 1.
The above-mentioned step of control group 1 of repetition, numbering control group 2~5, experimental result is shown in Table 1.
The ethephon (CEPHA),2-(chloroethyl) phosphonic acid active compound measurement result of table 1
As shown in Table 1, with a collection of ethephon (CEPHA),2-(chloroethyl) phosphonic acid active compound, using detection method of the present invention, ethephon (CEPHA),2-(chloroethyl) phosphonic acid mass fraction exists
74.5%-74.6%, reference examples testing result is 74.2%-74.4%, the data fluctuations scope of detection method than
Reference examples are small by 0.1%, therefore detection method more accurate stable.
Embodiment 2
1st, test example
A kind of detection method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid, including：
(1) take 3.75g ethephon (CEPHA),2-(chloroethyl) phosphonic acids sample plus 100ml water to dissolve, obtain the first solution to be measured, determine described first to be measured molten
Chloride ion content in liquid；The ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample is 40% ethephon agent of 0.25~0.35wt% containing free chloro ion；
(2) take after another identical 0.19g ethephon (CEPHA),2-(chloroethyl) phosphonic acids sample plus the dissolving of 100mL water, plus alkali is adjusted to alkalescence, during reaction is obtained
Between product, 90~110 DEG C of heating 30min, until the intermediate decomposes completely, being cooled to 15~30 DEG C, to obtain second to be measured molten
Liquid, determines the second Chlorine in Solution ion concentration to be measured；The alkali is potassium hydroxide, and the intermediate product is ethephon (CEPHA),2-(chloroethyl) phosphonic acid two
Potassium；Second solution to be measured includes：Ethene, potassium chloride, potassium dihydrogen phosphate.
(3) content of dissociative chlorine ion and the step (2) in the described first solution to be measured obtained according to the step (1)
The second obtained Chlorine in Solution ion concentration to be measured, calculating obtains ethephon (CEPHA),2-(chloroethyl) phosphonic acid content in the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample, numbering test group
A, experimental result is shown in Table 2.
Wherein, the measure first Chlorine in Solution ion concentration process to be measured is specially：Add 3~4 drop nitric acid molten
Liquid is adjusted in acidity, is titrated with silver nitrate standard titration solution, is terminal to potential break, is determined first solution to be measured
Middle chloride ion content；The the second Chlorine in Solution ion concentration process to be measured obtained described in the measure is specially：Add nitric acid molten
Liquid is adjusted in acidity, is titrated with silver nitrate standard titration solution, is terminal to potential break, determine described in obtain second treat
Survey Chlorine in Solution ion concentration；
The first Chlorine in Solution ion concentration to be measured is calculated as follows：
The second Chlorine in Solution ion concentration to be measured is calculated as follows：
Ethephon (CEPHA),2-(chloroethyl) phosphonic acid content is calculated as follows in the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample：
In formula：
X is ethephon (CEPHA),2-(chloroethyl) phosphonic acid content in the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample represented with mass fraction, and numerical value is represented with %；M1For chlorion
Molal weight, M1=35.45g/mol；M2For ethephon (CEPHA),2-(chloroethyl) phosphonic acid molal weight, M2=144.5g/mol；X1Represented with mass fraction
The first Chlorine in Solution ion concentration to be measured, numerical value represents with %, X2It is described second to be measured molten for what is represented with mass fraction
Chloride ion content in liquid, numerical value is represented with %；V1The step (1) described in determining the first Chlorine in Solution ion concentration to be measured disappears
Consume silver nitrate standard titration solution volume, Unit/mL；V2To determine step described in the second Chlorine in Solution ion concentration to be measured
(2) silver nitrate standard titration solution volume, Unit/mL are consumed；m1Ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample quality, unit g are taken by the step (1)；
m2To take ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample quality, unit g by the step (2)；C is silver nitrate standard titration solution concentration, unit mol/
L。
Above-mentioned test group step A is repeated, numbering B~E, experimental result is shown in Table 2.
2nd, reference examples
With reference to GB 23554-2009, it is ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample to take the same ethephon agent of batch 40% of test example, adds 10 and drips
Thymol blue is indicator, plus 0.5mol/L sodium hydroxides, is neutralized to alkalescence, and solution is changed into blueness from yellow；Boiling water bath adds
Ethene and sodium dihydrogen phosphate are thermally generated, cools down, is changed into 0.1mol/L sodium hydroxide titration sodium dihydrogen phosphates to solution from yellow
Blueness is terminal, obtains the mass fraction of ethephon (CEPHA),2-(chloroethyl) phosphonic acid, numbering control group group A, experimental result is shown in Table 2.
Above-mentioned control group A step is repeated, numbering control group B~E, experimental result is shown in Table 2.
The ethephon agent measurement result of table 2 40%
As shown in Table 2, with a collection of 40% ethephon agent, using detection method of the present invention, ethephon (CEPHA),2-(chloroethyl) phosphonic acid mass fraction
In 40.2%-40.4%, reference examples testing result is 39.7%-40.5%, and the data fluctuations scope of detection method will
It is smaller than reference examples, therefore detection method more accurate stable.
Embodiment 3
1st, test example
A kind of detection method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid is differed only in embodiment 1, takes the sample preparation first of 5g ethephon (CEPHA),2-(chloroethyl) phosphonic acids to be measured
Solution, takes another identical 0.75g ethephon (CEPHA),2-(chloroethyl) phosphonic acids sample preparation second solution to be measured, and the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample is that magnesium sulfate is filler
The solvable pulvis of 10% ethephon (CEPHA),2-(chloroethyl) phosphonic acid, numbering test group a, experimental result is shown in Table 3.Repetition test group a steps, numbering test group b~e,
Experimental result is shown in Table 3.
2nd, reference examples and embodiment 2 are differed only in, take that the same batch magnesium sulfate of test group a~e is filler 10%
The solvable pulvis of ethephon (CEPHA),2-(chloroethyl) phosphonic acid is ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample, and numbering control group a, experimental result is shown in Table 3, repeats control group a steps, numbering control
Group b~e, experimental result is shown in Table 3.
The magnesium sulfate of table 3 is the solvable pulvis measurement result of 10% ethephon (CEPHA),2-(chloroethyl) phosphonic acid of filler
By table 3, with the solvable pulvis of 10% ethephon (CEPHA),2-(chloroethyl) phosphonic acid that a collection of magnesium sulfate is filler, using detection method of the present invention,
Ethephon (CEPHA),2-(chloroethyl) phosphonic acid mass fraction is in 10.1%-10.3%, and reference examples testing result is 27.5%-38.0%, reference examples testing result ripple
Dynamic scope is larger and substantial deviation theoretical value, and reason is that magnesium sulfate can produce precipitation with sodium hydroxide reaction, wraps up and be passivated
Electrode, therefore detection method more accurate stable.
Embodiment 4
A kind of detection method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid is differed only in the test example of embodiment 1, takes 5g ethephon (CEPHA),2-(chloroethyl) phosphonic acid samples, the second
Alkene profit sample is containing 2wt%KH2PO410% ethephon (CEPHA),2-(chloroethyl) phosphonic acid wettable powder, calculating obtains ethephon (CEPHA),2-(chloroethyl) phosphonic acid in the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample and contains
Amount, repeats 5 detections of experiment, carries out precision test, the results are shown in Table 4.
The solvable pulvis Precision test result of the ethephon (CEPHA),2-(chloroethyl) phosphonic acid of table 4 10%
As shown in Table 4, the examination criteria deviation that the present invention is provided is small, and the degree of accuracy is high.
Embodiment 5
A kind of detection method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid is differed only in the test example of embodiment 1, takes 5g ethephon (CEPHA),2-(chloroethyl) phosphonic acid samples, the second
Alkene profit sample is containing 1wt%CaSO410% ethephon (CEPHA),2-(chloroethyl) phosphonic acid water dispersible granules, calculating obtains ethephon (CEPHA),2-(chloroethyl) phosphonic acid in the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample and contains
Amount, carries out mark-on reclaims experiment, is added into standard specimen, the gap of quality of the actual quality measured of contrast with adding sample, to return
Yield is represented, is repeated 5 detections of experiment, be the results are shown in Table 5 and table 6, wherein, quality is the ethephon (CEPHA),2-(chloroethyl) phosphonic acid product of known content in sample
Middle chlorine ions, it is chloride ion-containing quality in known ethephon (CEPHA),2-(chloroethyl) phosphonic acid standard specimen to add standard specimen quality.
The ethephon (CEPHA),2-(chloroethyl) phosphonic acid water dispersible granules free chlorine recovery test result of table 5 10%
The total chlorine recovery test result of the ethephon (CEPHA),2-(chloroethyl) phosphonic acid water dispersible granules of table 6 10%
Known by table 5, table 6, the free chlorine rate of recovery 100.31%, total chlorine rate of recovery 99.83%, detection method is reclaimed
Rate is high.
Embodiment 6
1st, test example
A kind of detection method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid is differed only in the test example of embodiment 1, takes 1.8g ethephon (CEPHA),2-(chloroethyl) phosphonic acid samples, described
Ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample is the 30% diethyl aminoethyl hexanoate ethephon agent using potassium dihydrogen phosphate as pH buffer, and calculating obtains the ethephon (CEPHA),2-(chloroethyl) phosphonic acid
Ethephon (CEPHA),2-(chloroethyl) phosphonic acid content in sample, numbering test group 6, and the repetition step of test group 6, numbering test group 7~10, experimental result is shown in Table 7.
2nd, reference examples and the reference examples of embodiment 2 are differed only in, and take the same batch of test example using potassium dihydrogen phosphate as pH
30% diethyl aminoethyl hexanoate ethephon agent of buffer is ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample, obtains the mass fraction of ethephon (CEPHA),2-(chloroethyl) phosphonic acid, numbering control group group
6, and the repetition step of control group 6, numbering control group 7~10, experimental result is shown in Table 7.
The diethyl aminoethyl hexanoate ethephon agent measurement result of table 7 30%
As shown in Table 7, it is ethene with a collection of 30% diethyl aminoethyl hexanoate ethephon agent using potassium dihydrogen phosphate as pH buffer
Sharp sample, using detection method of the present invention, ethephon (CEPHA),2-(chloroethyl) phosphonic acid mass fraction is in 27.2%-27.4%, reference examples testing result
37.0%-37.6%, the data and theoretical content of detection method are more identical, and reference examples testing result substantial deviation
Theoretical value, it may be possible to because phosphatic buffer capacity causes result higher, therefore detection method more accurate stable.
Embodiment 7
A kind of detection method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid is differed only in the test example of embodiment 1, takes 1.8g ethephon (CEPHA),2-(chloroethyl) phosphonic acid samples, described
Ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample is the 30% diethyl aminoethyl hexanoate ethephon agent using potassium dihydrogen phosphate as pH buffer, and calculating obtains the ethephon (CEPHA),2-(chloroethyl) phosphonic acid
Ethephon (CEPHA),2-(chloroethyl) phosphonic acid content in sample, repeats 5 detections of experiment, carries out precision test, the results are shown in Table 8.
The diethyl aminoethyl hexanoate ethephon agent Precision test result of table 8 30%
As shown in Table 8, the examination criteria deviation that the present invention is provided is small, and the degree of accuracy is high.
Embodiment 8
A kind of detection method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid is differed only in the test example of embodiment 1, takes 1.8g ethephon (CEPHA),2-(chloroethyl) phosphonic acid samples, described
Ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample is that, containing the 30% diethyl aminoethyl hexanoate ethephon agent using potassium dihydrogen phosphate as pH buffer, calculating obtains the ethene
Ethephon (CEPHA),2-(chloroethyl) phosphonic acid content in sharp sample, carries out mark-on reclaims experiment, is added into standard specimen, the quality of the actual measurement of contrast is with adding sample
The gap of quality, is represented with the rate of recovery, is repeated 5 detections of experiment, be the results are shown in Table 9 and table 10, wherein, quality is known in sample
Chlorine ions in the ethephon (CEPHA),2-(chloroethyl) phosphonic acid product of content, it is chloride ion-containing quality in known ethephon (CEPHA),2-(chloroethyl) phosphonic acid standard specimen to add standard specimen quality.
The diethyl aminoethyl hexanoate ethephon agent free chlorine recovery test result of table 9 30%
The total chlorine recovery test result of the diethyl aminoethyl hexanoate ethephon agent of table 10 30%
Known by table 9, table 10, the free chlorine rate of recovery 100.36%, total chlorine rate of recovery 99.81%, detection method is returned
High income.
Embodiment 9
Mole method
The difference of a kind of detection method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid and the test example of embodiment 1 is：
1st, 5g ethephon (CEPHA),2-(chloroethyl) phosphonic acid samples are taken, the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample is 10% ethephon (CEPHA),2-(chloroethyl) phosphonic acid water dispersible granules of phosphoric acid ammonium dihydrogen,
Calculating obtains ethephon (CEPHA),2-(chloroethyl) phosphonic acid content in the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample, and numbering test group 11 the results are shown in Table 11；
2nd, the measure first Chlorine in Solution ion concentration process to be measured is specially：Into the first solution to be measured, plus
People 2 drips phenolphthalein indicator, and the pH of the aqueous solution is adjusted with sodium hydroxide solution or salpeter solution, red is just become colorless.Plus
People's 1.0mL potassium chromate indicator, in the case of continuous shake, preferably uses silver nitrate standard titration solution under the conditions of white background
Titration, untill appearance is brick-red.Make blank test simultaneously, determine the first Chlorine in Solution ion concentration to be measured；It is described
Obtained the second Chlorine in Solution ion concentration process to be measured described in determining is specially：With determine first Chlorine in Solution to be measured from
Sub- content process is identical, the second Chlorine in Solution ion concentration to be measured obtained described in measure.
The Chlorine in Solution ion concentration to be measured is calculated as follows：
In formula：
X --- the Chlorine in Solution ion concentration to be measured represented with mass fraction, %；
M1--- chlorion molal weight, M1=35.45g/mol；
V --- determine the Chlorine in Solution ion concentration to be measured and consume silver nitrate standard titration solution volume, mL；
V0--- determine the numerical value of the volume of the solution blank test consumption silver nitrate standard titration solution to be measured, mL；
M --- prepare ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample quality, g used in the solution to be measured.
Embodiment 10
Precipitation enrichment AAS
The difference of a kind of detection method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid and the test example of embodiment 1 is：
1st, take and dissolve simultaneously constant volume in 100mL volumetric flasks for 8.0~80mg sample containing ethephon (CEPHA),2-(chloroethyl) phosphonic acid and, to 100mL, obtain the
One solution to be measured, the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample is 40% ethephon (CEPHA),2-(chloroethyl) phosphonic acid water dispersible granules of phosphoric acid hydrogen ammonium, and calculating obtains the ethene
Ethephon (CEPHA),2-(chloroethyl) phosphonic acid content in sharp sample, numbering test group 12 the results are shown in Table 11；
2nd, the drafting of calibration curve：0mL (blank), 0.20mL, 0.40mL, 0.60mL, 1.00mL are pipetted respectively,
In 1.50mL, 2.00mL chloride standard liquid, injection 250mL polyethylene centrifuge tubes, about 200mL, phase are diluted to without chlorine water
The C1 answered-Content is respectively 0 μ g, 2.0 μ g, 4.0 μ g, 6.0 μ g, 10.0 μ g, 15.0 μ g and 20.0 μ g.Then in the steps below 3
Measure its absorbance.With C1-Content is abscissa, and the corresponding absorbance measured is ordinate, draws calibration curve.
3rd, determining the first Chlorine in Solution ion concentration process to be measured is specially：(1) solution to be measured of 1.5mL first is pipetted
It is placed in 250mL polyethylene centrifuge tubes, plus people's 4mL lead nitrate solution, shake up.Plus people 4mL disodium hydrogen phosphates-potassium dihydrogen phosphate is mixed
Solution is closed, is fully shaken up, 5min is stood.(2) centrifuge tube is placed in centrifuge base, centrifuged with 5 000r/min rotating speed
5min, confides all centrifugal clear liquid, allows sediment to stay in centrifuge tube.Add ferric nitrate-perchloric acid solution 10rnL in toward centrifuge tube, make
Sediment is completely dissolved.(3) people 1mL mercuric thiocyanates-methanol solution is added.Develop the color after 5min, under 460nm wavelength, inhaled with 30mm
Receives pond, as blank, to measure its absorbance without chlorine water.Corresponding chloride content is found (with C1 from calibration curve-Meter), determine
The first Chlorine in Solution ion concentration to be measured；The the second Chlorine in Solution ion concentration process tool to be measured obtained described in the measure
Body is：The solution to be measured of 0.1mL first is pipetted to be placed in 250mL polyethylene centrifuge tubes as the second solution to be measured, plus people's 4mL nitric acid
Lead solution, shakes up.Identical with determining the first Chlorine in Solution ion concentration process to be measured afterwards, being obtained described in measure second
Chlorine in Solution ion concentration to be measured.Wherein, chlorine ion concentration measurement range is the μ g/L of 10 μ g/L~100.
Embodiment 11
Mercury salt titration
The difference of a kind of detection method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid and the test example of embodiment 1 is：
1st, take and dissolve simultaneously constant volume in 50mL volumetric flasks for 20mg~2000mg sample containing ethephon (CEPHA),2-(chloroethyl) phosphonic acid and, to 50mL, obtain the
One solution to be measured, the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample is 10% ethephon (CEPHA),2-(chloroethyl) phosphonic acid water dispersible granules of phosphoric acid, and calculating obtains the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample
Ethephon (CEPHA),2-(chloroethyl) phosphonic acid content in product, numbering test group 13, the results are shown in Table 11；
2nd, the measure first Chlorine in Solution ion concentration process to be measured is specially：(1) 15mL first is pipetted to be measured
Solution is in 250mL triangular flasks, plus 85mL water, plus 5 and drips mixed indicator (mixed indicator：Weigh 0.5g diphenylcarbazones,
0.05g bromophenol blues, 0.12g xylene blue-FF, are dissolved with 100mL95% ethanol, are stored in standby in brown drop bottle.), dropwise
Add salpeter solution (1+65) and adjust liquid acidity to be measured, until solution becomes yellow green from purple through green, after amount 1mL.
(2) under continuous shake, titrated, should slowly be dripped close to (solution colour turns dark green by yellowish green) during terminal with nitric acid mercury standard solution
It is fixed, the as terminal when solution colour is changed into purple.(3) while doing blank test, determine first Chlorine in Solution to be measured from
Sub- content；The the second Chlorine in Solution ion concentration process to be measured obtained described in the measure is specially：Pipette 1.0mL first to be measured
Solution is used as the second solution to be measured, plus 85mL water in 250mL triangular flasks.Afterwards with determine first Chlorine in Solution to be measured from
Sub- content process is identical, the second Chlorine in Solution ion concentration to be measured obtained described in measure.Wherein, determination of chloride ion concentration range
For 1~100mg/L.
Chloride ion content X is calculated in the prepare liquid：
In formula：
X --- the Chlorine in Solution ion concentration to be measured represented with mass fraction, %；
A --- titration prepare liquid consumes the volume of nitric acid mercury standard solution, ml；
B --- blank test consumes the volume of nitric acid mercury standard solution, ml；
T --- nitric acid mercury standard solution is to the titer of chloride, mg/ml；
M --- prepare solution specimen in use quality to be measured, g.
Embodiment 13
Mercuric thiocyanate AAS
The difference of a kind of detection method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid and the test example of embodiment 1 is：
1st, take containing ethephon (CEPHA),2-(chloroethyl) phosphonic acid for 0.75mg~250mg sample dissolve in 100mL volumetric flasks simultaneously constant volume to 100mL, obtain
To the first solution to be measured, the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample is the ethephon (CEPHA),2-(chloroethyl) phosphonic acid water dispersible granules of liquid containing ammonium sulfate 1%, and calculating obtains the ethephon (CEPHA),2-(chloroethyl) phosphonic acid
Ethephon (CEPHA),2-(chloroethyl) phosphonic acid content in sample, numbering test group 14, the results are shown in Table 11；
2nd, the drafting of standard working curve：Take 1 group of chlorion standard liquid, be separately added into pipette 5.0mL perchloric acid-
Iron nitrate solution, shakes up, and adds 0.2% mercuric thiocyanates of 2.0mL-methanol solution, shakes up, and places 5min.With 721-100 points
Light photometer, wavelength is 460nm, and cuvette is 100mm, and reference is made with high purity water, measures absorbance.According to measure absorbance and
Corresponding chloride ion content, calculates regression equation.
3rd, the measure first Chlorine in Solution ion concentration process to be measured is specially：Pipette 15mL first to be measured molten
Liquid, adds 5.0ml perchloric acid-iron nitrate solution, shakes up, add 0.2% mercuric thiocyanates of 2.0ml-methanol solution, shake up, quiet
5min is put, with 721-100 spectrophotometers are used, wavelength is 460nm, and cuvette is 100mm, reference is made with high purity water, measurement is inhaled
Luminosity.Chloride ion content is calculated from regression equation, the first Chlorine in Solution ion concentration to be measured is determined；The measure institute
Stating second obtained Chlorine in Solution ion concentration process to be measured is specially：Pipette the solution to be measured of 1mL first to be measured molten as second
Liquid, identical with determining the first Chlorine in Solution ion concentration process to be measured afterwards, the second solution to be measured obtained described in measure
Middle chloride ion content.Wherein, determination of chloride ion concentration range is 0.018mg/L~6mg/L.
Embodiment 14
The chromatography of ions
The difference of a kind of detection method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid and the test example of embodiment 1 is：
1st, take containing ethephon (CEPHA),2-(chloroethyl) phosphonic acid for 8mg sample dissolve in 100mL volumetric flasks simultaneously constant volume to 100mL, obtain first to be measured
Solution, the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample is the 25% ethephon (CEPHA),2-(chloroethyl) phosphonic acid suspending agent containing magnesium nitrate, and calculating obtains ethene in the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample
Sharp content, numbering test group 15, the results are shown in Table 11；
2nd, the drafting of standard working curve：
The preparation of hybrid standard working solution：Hybrid standard working solution liquid should day preparation, hybrid standard working solution
Concentration range should include sample in chlorion concentration.Prepare a blank solution, the mixing of at least five concentration level
Standard working solution.Using reagent water as blank solution, the concentration level of chlorion is respectively 5,10 in hybrid standard working solution,
15,20,25μg/L。
Appearance time on analysis margin solution, hybrid standard working solution, record spectrogram, when determining the reservation of chlorion
Between, using peak height or peak area as ordinate, using chlorine ion concentration as abscissa, draw standard working curve or obtain recurrence side
Journey, linearly dependent coefficient should be greater than 0.995.
3rd, the measure first Chlorine in Solution ion concentration process to be measured is specially：Pipette 1.5mL first and survey solution
100mL is diluted to, with point folding standard working solution identical test condition, analysis measure being carried out to sample, according to tested
The peak height or peak area of anion determine that chlorine, from concentration, is determined in first solution to be measured by corresponding standard working curve
Chloride ion content；The the second Chlorine in Solution ion concentration process to be measured obtained described in the measure is specially：Pipette 0.1mL first
Solution is surveyed as ibid being operated after the second solution to be measured, determine described in obtained the second Chlorine in Solution ion concentration to be measured.Its
In, test limit μ g/L meters.
Embodiment 15
Visual turbidimetry
The difference of a kind of detection method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid and the test example of embodiment 1 is：
1st, the sample of the ethephon (CEPHA),2-(chloroethyl) phosphonic acid containing 2.0~40mg is taken to be diluted to 100mL, the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample is phosphoric acid hydrogen dipotassium
1% ethephon agent, calculating obtains ethephon (CEPHA),2-(chloroethyl) phosphonic acid content in the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample, and numbering test group 16 the results are shown in Table 11；
2nd, preparation of the standard than turbid solution：Prepare 0.5 μ g/ml, 1.0 μ g/ml, 1.5 μ g/ml, 2.0 μ g/ml, 2.5 μ g/ml
Chlorion standard liquid, take the chlorion standard liquid of each concentration gradients of 1ml, with 1ml salpeter solutions (25%) be acidified, plus
1ml silver nitrate solutiones (17g/L), are diluted to 25ml, shake up, and 10min are placed in dark place, as standard than turbid solution.
3rd, the measure first Chlorine in Solution ion concentration process to be measured is specially：Take and chlorion standard liquid phase
First solution to be measured of same volume, while same processing, solution is compared into turbidity with standard than turbid solution, determines described first
Chlorine in Solution ion concentration to be measured；The the second Chlorine in Solution ion concentration process to be measured obtained described in the measure is specially：With
Determine that the described first Chlorine in Solution ion concentration process to be measured is identical, determine described in obtained the second Chlorine in Solution ion to be measured contain
Amount.Wherein, determination of chloride ion concentration range is the μ g/ml of 0.2 μ g/ml~4.
The testing result of statistical test group 11~21, is shown in Table 11.
Table 11
| Group | Ethephon (CEPHA),2-(chloroethyl) phosphonic acid content (%) |
| Test group 11 | 10.1 |
| Test group 12 | 40.2 |
| Test group 13 | 10.2 |
| Test group 14 | 1.0 |
| Test group 15 | 24.9 |
| Test group 16 | 1.0 |
As shown in Table 11, detection range of the present invention is wide, you can for detect ethephon (CEPHA),2-(chloroethyl) phosphonic acid content range be 1~40% ethene
Sharp preparation.
It the above is only the preferred embodiment of the present invention, it is noted that above-mentioned preferred embodiment is not construed as pair
The limitation of the present invention, protection scope of the present invention should be defined by claim limited range.For the art
For those of ordinary skill, without departing from the spirit and scope of the present invention, some improvements and modifications can also be made, these change
Enter and retouch and also should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of detection method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid, it is characterised in that including：
(1) take ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample to be dissolved in water, obtain the first solution to be measured, determine the first Chlorine in Solution ion to be measured and contain
Amount；
(2) take after another identical ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample is dissolved in water, plus alkali is adjusted to alkalescence, reaction obtains intermediate product, heats, directly
Decomposed completely to the intermediate product, cool down, obtain the second solution to be measured；Determine the Chlorine in Solution ion concentration to be measured；
(3) content of dissociative chlorine ion and the step (2) are obtained in the described first solution to be measured obtained according to the step (1)
The second Chlorine in Solution ion concentration to be measured, calculating obtain ethephon (CEPHA),2-(chloroethyl) phosphonic acid content in the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample.
2. detection method according to claim 1, it is characterised in that ethephon (CEPHA),2-(chloroethyl) phosphonic acid content is as the following formula in the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample
Calculate：
<mrow>
<mi>X</mi>
<mo>=</mo>
<mfrac>
<msub>
<mi>M</mi>
<mn>2</mn>
</msub>
<msub>
<mi>M</mi>
<mn>1</mn>
</msub>
</mfrac>
<mrow>
<mo>(</mo>
<msub>
<mi>X</mi>
<mn>2</mn>
</msub>
<mo>-</mo>
<msub>
<mi>X</mi>
<mn>1</mn>
</msub>
<mo>)</mo>
</mrow>
<mo>;</mo>
</mrow>
In formula：
X is ethephon (CEPHA),2-(chloroethyl) phosphonic acid content in the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample represented with mass fraction, and numerical value is represented with %；M1For chlorion mole
Quality, M1=35.45g/mol；M2For ethephon (CEPHA),2-(chloroethyl) phosphonic acid molal weight, M2=144.5g/mol；X1Described in being represented with mass fraction
First Chlorine in Solution ion concentration to be measured, numerical value represents with %, X2For in the described second solution to be measured for being represented with mass fraction
Chloride ion content, numerical value is represented with %.
3. detection method according to claim 1, it is characterised in that alkali described in the step (2) be potassium hydroxide or
Sodium hydroxide, the intermediate product is ethephon (CEPHA),2-(chloroethyl) phosphonic acid disodium salt or ethephon (CEPHA),2-(chloroethyl) phosphonic acid di-potassium.
4. detection method according to claim 1, it is characterised in that heating-up temperature is 90~110 in the step (2)
℃。
5. detection method according to claim 1, it is characterised in that using mole method, potentiometric titration, Enrichment
AAS, mercury salt titration, mercuric thiocyanate AAS, the chromatography of ions, visual turbidimetry, ion-selective electrode
Described in method, atomic absorption spectrphotometry indirect method, silver nitrate volumetric method, mercuric nitrate volumetric method or rhodan ammonium titration measuring
One Chlorine in Solution ion concentration to be measured and the second Chlorine in Solution ion concentration to be measured.
6. detection method according to claim 5, it is characterised in that to be measured molten using described in potentiometric determination first
Chloride ion content and the second Chlorine in Solution ion concentration to be measured in liquid.
7. detection method according to claim 1, it is characterised in that the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample includes interfering material, described
Interfering material is phosphate anion, phosphoric acid hydrogen radical ion, dihydrogen phosphate ions and the ion for producing precipitation is reacted with the alkali
Middle one or more.
8. detection method according to claim 7, it is characterised in that the foreign ion is potassium dihydrogen phosphate, di(2-ethylhexyl)phosphate
Hydrogen ammonium, ammonium hydrogen phosphate, phosphoric acid, ammonium sulfate and react one or more in the ion for producing precipitation with alkali.
9. detection method according to claim 1, it is characterised in that the ethephon (CEPHA),2-(chloroethyl) phosphonic acid sample is ethephon (CEPHA),2-(chloroethyl) phosphonic acid active compound, ethene
Sharp preparation, the ethephon (CEPHA),2-(chloroethyl) phosphonic acid preparation is ethephon (CEPHA),2-(chloroethyl) phosphonic acid single dose or ethephon (CEPHA),2-(chloroethyl) phosphonic acid complex preparation.
10. detection method according to claim 9, it is characterised in that the ethephon (CEPHA),2-(chloroethyl) phosphonic acid preparation formulation be water dispersible granules,
Wettable powder, soluble powder or aqua.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710308753.2A CN107102102A (en) | 2017-05-04 | 2017-05-04 | A kind of detection method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710308753.2A CN107102102A (en) | 2017-05-04 | 2017-05-04 | A kind of detection method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107102102A true CN107102102A (en) | 2017-08-29 |
Family
ID=59657395
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710308753.2A Pending CN107102102A (en) | 2017-05-04 | 2017-05-04 | A kind of detection method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107102102A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112362653A (en) * | 2020-10-29 | 2021-02-12 | 湖南久日新材料有限公司 | Method for detecting low chlorine content of photoinitiator |
| CN112661607A (en) * | 2020-12-28 | 2021-04-16 | 安道麦安邦(江苏)有限公司 | Method and device for recycling organic waste liquid generated in ethephon production |
-
2017
- 2017-05-04 CN CN201710308753.2A patent/CN107102102A/en active Pending
Non-Patent Citations (3)
| Title |
|---|
| 江涛等: "自动电位滴定法测定乙烯利含量", 《理化检验-化学分册》 * |
| 袁月莲等: "快速分析乙烯利含量方法的研究", 《莱阳农学院学报》 * |
| 陆益民等: "离子选择性电极法测定乙烯利的含量", 《韶关学院学报·自然科学》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112362653A (en) * | 2020-10-29 | 2021-02-12 | 湖南久日新材料有限公司 | Method for detecting low chlorine content of photoinitiator |
| CN112362653B (en) * | 2020-10-29 | 2024-02-27 | 湖南久日新材料有限公司 | Method for detecting low chlorine content of photoinitiator |
| CN112661607A (en) * | 2020-12-28 | 2021-04-16 | 安道麦安邦(江苏)有限公司 | Method and device for recycling organic waste liquid generated in ethephon production |
| CN112661607B (en) * | 2020-12-28 | 2023-04-07 | 安道麦安邦(江苏)有限公司 | Method and device for recycling organic waste liquid generated in ethephon production |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Boltz et al. | Determination of phosphorus, germanium, silicon, and arsenic | |
| Brupbacher | Analytical methods and procedures used in the soil testing laboratory | |
| CN101334365B (en) | Determination method for chloride ion content of temper rolling liquor for steel plate rolling | |
| CN101294896A (en) | Method for measuring cadmium content in smoke tipping paper | |
| CN105758927A (en) | Method for simultaneously measuring iodine, boron, tin and germanium elements in soil | |
| CN103954596A (en) | Method for indirectly measuring content of uranium in soil through atomic fluorescence spectroscopy | |
| CN107102102A (en) | A kind of detection method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid | |
| CN108872223A (en) | A kind of method of phosphorus content in measurement molybdenum compound | |
| CN109541128B (en) | Method for measuring manganese content in basic manganese chloride | |
| CN112540115A (en) | Internal standard combined solution for detecting 6 single elements in whole blood | |
| CN112540116A (en) | Method for detecting six trace elements in whole blood by using internal standard combined solution | |
| CN112557492A (en) | Method for calibrating ICP-MS (inductively coupled plasma-mass spectrometry) trace element analyzer by using internal standard combined solution | |
| CN104914093B (en) | The method of testing of constant cadmium and zinc in tellurium-zincium-cadmium crystal | |
| CN104914083B (en) | A kind of fluorescence silver nanoclusters detect I simultaneously‑And Br‑Method and utilization | |
| CN109633079A (en) | A method of vanadium and ammonium content in detection metavanadate solution | |
| CN102435560B (en) | Method for testing nitrification inhibition rate of stabilized fertilizer | |
| White et al. | Fluorometric determination of microgram quantities of boron | |
| CN104089958B (en) | The assay method of phosphorus content in steel containing niobium | |
| CN103808708A (en) | Method for detecting components of industrial ammonium sulfate product | |
| CN112595710A (en) | Rapid detection kit and detection method for iodide ions in serum sample | |
| CN106092935A (en) | Method For Nitrate Content and application thereof in soil microorganism toxicity test | |
| CN111122465A (en) | Arsenic-free detection kit for iodide ions in trace serum sample | |
| Waldo et al. | The determination of fluoride in drinking water and biological materials | |
| CN105866324A (en) | A method of measuring a content of citric acid or a citrate in a solution | |
| CN104360008B (en) | Detection method for concentration of iodine in polyethylene glycol-potassium iodide-cyclic carbonate mixed system |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170829 |