CN109142450B - Method based on electrical conductivity method measurement sugar alcohol fertilizer of chelated calcium chelation percent - Google Patents
Method based on electrical conductivity method measurement sugar alcohol fertilizer of chelated calcium chelation percent Download PDFInfo
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Abstract
The invention discloses a kind of methods based on electrical conductivity method measurement sugar alcohol fertilizer of chelated calcium chelation percent, first under the frequency of oscillation of 100r/min-350r/min, it is extracted repeatedly using acetone as extractant, by the separation of sugar alcohol chelating calcium Chelating state calcium and free state calcium in sugar alcohol fertilizer of chelated calcium, sugar alcohol chelating calcium and supernatant are obtained；Then any two in appropriate sugar alcohol chelating calcium, sugar alcohol fertilizer of chelated calcium and supernatant are taken, same amount of water is added, measures electrical conductivity of solution respectively under the same conditions --- DSubstrate、DChelate mother liquorAnd DSupernatant, chelation percent is finally calculated according to formula.Electrical conductivity method experiment requires equipment and personnel low, suitable enterprise and common lab measurement；Compared with common method, and without calculating calcium ion content, and complicated calculating process, only need conductance measurement that chelation percent can be obtained, treatment process is simplified, by the measurement of calcium ion concentration, is converted into the measurement of electrical conductivity of solution, measuring method is simpler, at low cost, easy to accomplish.
Description
Technical field:
The invention belongs to chelate rate determination techniques fields, and in particular to the chelated calcium chelation percent measurement side of sugar alcohol
Method measures the conductivity that sugar alcohol chelates calcium and sugar alcohol fertilizer of chelated calcium stoste by electrical conductivity method, calculates chelation percent.
Background technique:
Sugar alcohol calcium chelate be occur that chelatropic reaction generates after the hydroxyl dehydrogenation by sugar alcohol with calcium ion there is five-membered ring
Or the isostructural substance of hexatomic ring, have the advantages that stability is good, utilization rate is high, has been widely used in the neck such as food, medicine, chemical industry
Domain.Sugar alcohol is photosynthetic head product as polyol, and conveying capacity is strong, and conveying effect is good.Sugar alcohol is in plant
Stress resistance of plant inside can be improved, reinforce the differentiation and power of regeneration of callus, the multiple tooth property in structure, so that chelate products
Stablize, enters easy degradation in plant body and release nutrient, promote being absorbed and utilized for plant.Many mechanisms and enterprise in the market
Sugar alcohol chelate fertilizer all is being produced and sold, but is illustrating the quantity or matter of chelate in chelate fertilizer without exact technical indicator
Amount, is primarily due to the deficiency of analysis detection means.The chelation percent of sugar alcohol chelate is the detection of such material mass and Analysis on Mechanism
Important evidence, but at present there is no sugar alcohol chelate rate detect national standard method.Current existing national standard side
Method is mainly used in the detection of amino-acid chelate chelation percent, such as gel filtration chromatography, organic solvent extractionprocess；In addition,
There is granted patent to be also mainly used in the detection of amino-acid chelate chelation percent, such as: infra-red sepectrometry, ultraviolet spectroscopy, modification
Electrode method, spectrophotometry and XRD are combined method.So far, there is not yet the relevant report of " sugar alcohol chelates the detection of calcium chelation percent ".
Patent CN101368903A discloses a kind of detection method for measuring amino acid micro-element chelate rate,
It is middle to utilize UV-Vis spectra analysis absorbance and wavelength and then the chelating for measuring amino-acid chelate (Cu, Fe, Mn, Zn)
Rate, because the metal ion of amino-acid chelate applied by this method is all the one kind for itself having color characteristic, and sugar alcohol chelates
Ionic calcium soln in calcium is colorless and transparent, this leads to that absorbance can not be measured in spectrophotometer, though using color developing agent with
Calcium ion carry out chromogenic reaction, due to color developing agent with the ability to function of metal ion it is stronger, the chelated calcium knot of sugar alcohol can be destroyed
Structure, therefore can not directly carry out the measurement of sugar alcohol chelating calcium chelation percent.Patent CN105004774A discloses a kind of modified electrode
Preparation method and feed addictive Copper lysinate in free copper ion measurement application method, the crucial of patent application exist
In modified electrode to Copper lysinate be not present electrochemical response, thus using differential pulse voltammetry measurement GOLD FROM PLATING SOLUTION category copper from
Sub- content calculates the chelation percent of Copper lysinate, and sugar alcohol chelating calcium is to belong to electrically charged one kind with electrochemical signals itself
The calcium ion of chelate, free state is also conductive, thus the method can not do not separate sugar alcohol chelating calcium Chelating state calcium and
Chelation percent is accurately measured in the case of free state calcium.Patent CN107286219A discloses a kind of spectrophotometry and XRD combination is true
Determine microelement compound amino acid/small-peptide chelated object synthetic ratio and the quick estimating and measuring method of chelation percent, the patented method are mainly answered
Premise is by how much estimation chelation percents of appearance in XRD spectrum, and can only to estimate chelating to the measurement of chelating proportion
The higher chelating stoste of degree, the system more for free state metal ion in system are not suitable for measurement chelation percent.
The detection method of sugar alcohol chelate fertilizer chelation percent is constantly in the process of discussion, finds suitable chelation percent detection side
Method has great importance for the fertilizer efficiency and quality evaluation of sugar alcohol chelate fertilizer.Based on there is presently no chelate calcium about sugar alcohol
The chelation percent detection method of fertilizer establishes the standard of sugar alcohol fertilizer product to push the further investigation of sugar alcohol chelate fertilizer, formulates
A kind of effective detection method to the production of sugar alcohol chelate fertilizer, popularization, using having important practical significance.In measurement sugar alcohol
When chelating fertilizer chelation percent, since calcium ion is divided into free state and Chelating state in sugar alcohol chelating fertilizer mother liquor, it is necessary first to by sugar alcohol chela
It closes calcium to separate from sugar alcohol chelating fertilizer mother liquor, then measurement sugar alcohol chelates the calcium ion in calcium and solution respectively.However sugar alcohol chela
Unstable, the conventional separation method of calcium is closed, is such as centrifuged, is easily destroyed its chelate structure, leads to the measurement inaccuracy of chelation percent.And
According to the concentration of EDTA titration determination calcium ion after separation, workload certainly will be increased, measured according to ICP-AES, sugar alcohol chela
Closing calcium is that a kind of its standard curve of chelate is difficult to draw, how simply, quickly, measure the chelated calcium chelating of sugar alcohol at low cost
Rate becomes urgent problem.The present invention establishes organic solvent extractionprocess and electrical conductivity method combination detection sugar alcohol chelating calcium chela
The method of conjunction rate, has the advantages that simple, efficient, at low cost, can quickly measure sugar alcohol chelate accounting in chelate fertilizer
The amount of having.
Summary of the invention:
It is an object of the invention to seek a kind of method for quickly detecting sugar alcohol fertilizer of chelated calcium chelation percent based on electrical conductivity method,
Solve existing method free state and when Chelating state calcium ion content in measuring sugar alcohol chelating liquid fertilizer, there are complicated for operation,
The problems such as being difficult to realize.
To achieve the goals above, the present invention is based on a kind of electrical conductivity method measurement sugar alcohol fertilizer of chelated calcium chelation percent method,
Specifically includes the following steps:
(1) sugar alcohol fertilizer of chelated calcium free state and Chelating state separation
Proper amount of acetone is added in sugar alcohol fertilizer of chelated calcium, is placed in oscillator, in the oscillation frequency of 100r/min-350r/min
Under rate, 10min-40min, isolated white gum bottom sediment object and supernatant are vibrated；It is added in bottom sediment object suitable
Acetone is measured, is placed in oscillator, under the frequency of oscillation of 100r/min-350r/min, is separated after vibrating 10min-40min, then
It is secondary to obtain bottom sediment object and supernatant, above-mentioned separating step is repeated until nitrate radical content is constant in supernatant, is finally obtained
Bottom sediment object be sugar alcohol chelating calcium；
(2) electrical conductivity method measures chelation percent
Merge the supernatant that step (1) generates, the supernatant after taking appropriate sugar alcohol chelating calcium, sugar alcohol fertilizer of chelated calcium and merging
Any two in liquid, same amount of water is added, measures electrical conductivity of solution respectively under the same conditions --- DSubstrate、DChelate mother liquorWith
DSupernatant, the usage amount of supernatant and sugar alcohol chelating fertilizer three after the sugar alcohol chelating calcium, merging is corresponding, according to the following formula
Calculate chelation percent: chelation percent=1-DSupernatant/DChelate mother liquor=DSubstrate/DChelate mother liquor=DSubstrate/(DSubstrate+DSupernatant)。
Sugar alcohol chelating calcium is that chelate not exclusively exists in the solution with ionic forms, to improve the accurate of conductivity
Property, preferably D in determination step (2)SubstrateAnd DChelate mother liquor, chelation percent=DSubstrate/DChelate mother liquor。
Further, the sugar alcohol fertilizer of chelated calcium is prepared by sugar alcohol, water and excessive calcium nitrate, and wherein sugar alcohol includes
But one of it is not limited to sorbierite, mannitol and xylitol or a variety of.
Compared with prior art, the present invention it is low to have the advantage that the experiment of (1) electrical conductivity method requires equipment and personnel,
It is suitble to enterprise and common lab measurement；Compared with common method, and without calculating calcium ion content, and complicated calculating
Process only needs conductance measurement that chelation percent can be obtained, and simplifies treatment process.(2) it by the measurement of calcium ion concentration, is converted into
The measurement of electrical conductivity of solution, measuring method is simpler, at low cost, easy to accomplish, and (3) provide a kind of convenient for enterprise and mechanism measurement
Sugar alcohol chelates the technology of calcium chelation percent, measures chelation percent in a manner of most simple direct, fills up national standard detection method vacancy,
Meet industry needs.
Specific embodiment:
The present invention is described further below by specific embodiment.
Embodiment 1:
It is the accuracy for verifying electrical conductivity method measurement chelation percent involved in the present embodiment, specifically includes the following steps:
(1) by 16 parts of sorbierite, 18 parts and 45 parts of calcium nitrate of water are added in wide-mouth bottle, are stirred in magnetic force water-bath,
It under 65 DEG C and 1000r/min of revolving speed, reacts and continues 35min, obtain sugar alcohol chelating mother liquor of calcium；
(2) it weighs the sugar alcohol chelating mother liquor of calcium prepared in 1g above-mentioned (1) and 10mL acetone is added in centrifuge tube, after sealing
It is placed in oscillator, under the frequency of oscillation of 300r/min, duration of oscillation 30min collects supernatant Ai, i=1；
(3) 10ml acetone is added in the centrifuge tube of removal supernatant, is again placed in oscillator, in the vibration of 300r/min
It swings under frequency, vibrates 30min, collect supernatant Ai, i=2；
(4) it repeats above-mentioned (3) four times, centrifuge tube bottom white gum sediment is sugar alcohol chelating calcium；
(5) above-mentioned (1)-(4) are repeated, and collects the supernatant A generated in front (2)-(4)i, i=1,2,3,4,5；It will
Five solution, which pour into same volumetric flask, is diluted with water to 100mL, and constant volume shakes up, and measures its conductivity D at 25 DEG CSupernatant；
It collects the bottom white gum sediment sugar alcohol generated in (4) and chelates calcium, sugar alcohol chelating calcium is diluted with water, until 100mL, constant volume
It shakes up, measures its conductivity D at 25 DEG CSubstrate；It takes 1g sugar alcohol to chelate mother liquor of calcium, is diluted with water, until 100mL, constant volume is shaken up,
Measure its conductivity D at 25 DEG CChelate mother liquor。
(6) chelation percent is calculated according to the following formula: chelation percent=1-DSupernatant/DChelate mother liquor=DSubstrate/DChelate mother liquor=DSubstrate/(DSubstrate+
DSupernatant), as shown in table 1.
1 conductivity readings of table and chelation percent data
Conclusion: as it can be seen from table 1 three parallel laboratory test acquired results elementary errors of setting between 0-1%, are reappeared
Property is good.
Embodiment 2:
Different sugar alcohol chelating calcium utilization electrical conductivity methods involved in the present embodiment measure chelation percent, specifically include following step
It is rapid:
(1) by 8 parts of sorbierite, 18 parts and 40 parts of calcium nitrate of water are added in wide-mouth bottle, are stirred in magnetic force water-bath,
It under 65 DEG C and 1000r/min of revolving speed, reacts and continues 35min, obtain sugar alcohol chelating mother liquor of calcium；
(2) it weighs the sugar alcohol chelating mother liquor of calcium prepared in 1g above-mentioned (1) and 10mL acetone is added in centrifuge tube, after sealing
It is placed in oscillator, under the adjustment frequency of oscillation of 300r/min, duration of oscillation 30min collects supernatant Ai, i=1；
(3) 10mL acetone is added in the centrifuge tube of removal supernatant, is again placed in oscillator, in the vibration of 300r/min
It swings under frequency, vibrates 30min, collect supernatant Ai, i=2,3,4,5；
(4) it repeats step (3) four times, measurement centrifuge tube bottom white gum sediment is sugar alcohol chelating calcium；
(5) electrical conductivity method measures chelation percent: collecting the supernatant A that front (1)-(4) step generatesi, i=1,2,3,4,5；
Five solution are poured into same volumetric flask and are diluted with water to 100mL, constant volume shakes up, and measures its conductivity at 25 DEG C
DSupernatant；The bottom white gum sediment sugar alcohol that collection step (4) generates chelates calcium, and sugar alcohol chelating calcium is diluted with water, until
100mL, constant volume shake up, and measure its conductivity D at 25 DEG CSubstrate；It takes 1g sugar alcohol to chelate mother liquor of calcium, is diluted with water, until 100mL,
Constant volume shakes up, and measures its conductivity D at 25 DEG CChelate mother liquor；
(6) chelation percent η is calculated, electrical conductivity method measures chelation percent η=1-DSupernatant/DChelate mother liquor=DSubstrate/DChelate mother liquor.With conductivity
On the basis of the conductivity that instrument measures at 25 DEG C, table 2 is is surveyed the different chelated calcium chelation percents of sugar alcohol using electrical conductivity method.
The surveyed chelation percent % of 2 electrical conductivity method of table
Conclusion: three groups of parallel tests illustrate the chelating fertilizer that electrical conductivity method is suitble to sorbierite to synthesize as chelating agent with calcium nitrate
The measurement of the chelation percent of material.
Embodiment 3:
Different sugar alcohol chelating calcium utilization electrical conductivity methods involved in the present embodiment measure chelation percent, specifically include following step
It is rapid:
(1) by 8 parts of mannitol, 18 parts and 50 parts of calcium nitrate of water are added in wide-mouth bottle, are stirred in magnetic force water-bath,
At specific temperature and revolving speed, the specific time is reacted, obtains sugar alcohol chelating mother liquor of calcium；
In addition to step (1), other steps are same as Example 2.
Table 2 is the chelated calcium chelation percent of different sugar alcohols measured at 25 DEG C using electrical conductivity method.Electrical conductivity method measures chela
Conjunction rate η=1-DSupernatant/DChelate mother liquor=DSubstrate/DChelate mother liquor；Illustrate that electrical conductivity method is suitble to mannitol to synthesize as chelating agent with calcium nitrate
The chelation percent of chelate fertilizer measures.
Embodiment 4:
Different sugar alcohol chelating calcium utilization electrical conductivity methods involved in the present embodiment measure chelation percent, specifically include following step
It is rapid:
(1) by 4 parts of xylitol, 17 parts and 40 parts of calcium nitrate of water are added in wide-mouth bottle, are stirred, are obtained in magnetic force water-bath
Mother liquor of calcium is chelated to sugar alcohol；
In addition to step (1), other steps are same as Example 2.
Table 2 is the chelated calcium chelation percent of different sugar alcohols measured at 25 DEG C using electrical conductivity method.Electrical conductivity method measures chela
Conjunction rate η=1-DSupernatant/DChelate mother liquor=DSubstrate/DChelate mother liquor；Illustrate that electrical conductivity method is suitble to xylitol to synthesize as chelating agent with calcium nitrate
The chelation percent of chelate fertilizer measures.
Embodiment 5:
Different sugar alcohol chelating calcium utilization electrical conductivity methods involved in the present embodiment measure chelation percent, specifically include following step
It is rapid:
(1) by 4 parts of sorbierite, 4 parts of mannitol, 17 parts and 40 parts of calcium nitrate of water are added in wide-mouth bottle, in magnetic force water-bath
It is stirred in pot, obtains sugar alcohol chelating mother liquor of calcium；
In addition to step (1), other steps are same as Example 2.
Table 2 is the chelated calcium chelation percent of different sugar alcohols measured at 25 DEG C using electrical conductivity method.Electrical conductivity method measures chela
Conjunction rate η=1-DSupernatant/DChelate mother liquor=DSubstrate/DChelate mother liquor；Illustrate that electrical conductivity method is suitble to sorbierite, mannitol as chelating agent and nitric acid
The chelation percent measurement of the chelate fertilizer of calcium synthesis.
Embodiment 6:
Different sugar alcohol chelating calcium utilization electrical conductivity methods involved in the present embodiment measure chelation percent, specifically include following step
It is rapid:
(1) by 8 parts of sorbierite, 8 parts of xylitol, 18 parts and 50 parts of calcium nitrate of water are added in wide-mouth bottle, in magnetic force water-bath
It is stirred in pot, obtains sugar alcohol chelating mother liquor of calcium；
In addition to step (1), other steps are same as Example 2.
Table 2 is the chelated calcium chelation percent of different sugar alcohols measured at 25 DEG C using electrical conductivity method.Electrical conductivity method measures chela
Conjunction rate η=1-DSupernatant/DChelate mother liquor=DSubstrate/DChelate mother liquor；Illustrate that electrical conductivity method is suitble to sorbierite and xylitol as chelating agent and nitric acid
The chelation percent measurement of the chelate fertilizer of calcium synthesis.
Embodiment 7:
Different sugar alcohol chelating calcium utilization electrical conductivity methods involved in the present embodiment measure chelation percent, specifically include following step
It is rapid:
(1) by 4 parts of mannitol, 4 parts of xylitol, 17 parts and 40 parts of calcium nitrate of water are added in wide-mouth bottle, in magnetic force water-bath
It is stirred in pot, obtains sugar alcohol chelating mother liquor of calcium；
In addition to step (1), other steps are same as Example 2.
Table 2 is the chelated calcium chelation percent of different sugar alcohols measured at 25 DEG C using electrical conductivity method.Electrical conductivity method measures chela
Conjunction rate η=1-DSupernatant/DChelate mother liquor=DSubstrate/DChelate mother liquor；Illustrate that electrical conductivity method is suitble to mannitol and xylitol as chelating agent and nitric acid
The chelation percent measurement of the chelate fertilizer of calcium synthesis.
Embodiment 8:
Different sugar alcohol chelating calcium utilization electrical conductivity methods involved in the present embodiment measure chelation percent, specifically include following step
It is rapid:
Table 2 is the chelated calcium chelation percent of different sugar alcohols measured at 25 DEG C using electrical conductivity method.Electrical conductivity method measures chela
Conjunction rate η=1-DSupernatant/DChelate mother liquor=DSubstrate/DChelate mother liquor；Illustrate that electrical conductivity method is suitble to sorbierite, mannitol and xylitol as chelating
The chelation percent for the chelate fertilizer that agent is synthesized with calcium nitrate measures.
Embodiment 9:
Two kinds of measuring methods of sugar alcohol chelating calcium chelation percent, are respectively as follows: conductance in organic fertilizer involved in the present embodiment
Rate method, EDTA complexometry, specifically includes the following steps:
(1) by 5 parts of sorbierite, 17 parts of water, 20 parts of calcium nitrate are added in wide-mouth bottle, are stirred, are obtained in magnetic force water-bath
Mother liquor of calcium is chelated to sugar alcohol；
In addition to step (1), step (2)-(6) are same as Example 2.
(7) using eriochrome black T as calcium color developing agent, using ammonium chloride and ammonium hydroxide alkalinity as buffer solution under conditions of, matched using EDTA
Calcium in sugar alcohol chelating calcium obtained in the chelating mother liquor of calcium of sugar alcohol obtained in position titration difference determination step (1) and step (4)
The quality of ion --- LChelate mother liquorAnd LSubstrate(LSubstrateCalcium ion content (g) in calcium is chelated for sugar alcohol；LChelate mother liquorFor in sugar alcohol fertilizer of chelated calcium
Calcium ion content (g)), calculate chelation percent: η=LSubstrate/LChelate mother liquor, as shown in table 3.
3 two methods of table measure chelation percent %
Conclusion: two kinds of chelation percent measuring methods all have high accuracy and repeatability.
Claims (2)
1. the method based on electrical conductivity method measurement sugar alcohol fertilizer of chelated calcium chelation percent, which is characterized in that specifically includes the following steps:
(1) sugar alcohol fertilizer of chelated calcium free state and Chelating state separation
Proper amount of acetone is added in sugar alcohol fertilizer of chelated calcium, is placed in oscillator, in the frequency of oscillation of 100r/min-350r/min
Under, vibrate 10min-40min, isolated white gum bottom sediment object and supernatant；It is added in bottom sediment object appropriate
Acetone is placed in oscillator, under the frequency of oscillation of 100r/min-350r/min, is separated after vibrating 10min-40min, again
It obtains bottom sediment object and supernatant, repeats above-mentioned separating step until nitrate radical content is constant in supernatant, finally obtain
Bottom sediment object is sugar alcohol chelating calcium；
(2) electrical conductivity method measures chelation percent
Merge the supernatant that step (1) generates, sugar alcohol the chelating calcium, the identical sugar alcohol of step (1) amount used for taking step (1) to obtain
Any two in supernatant after fertilizer of chelated calcium and merging, are diluted with water to identical volume, distinguish under the same conditions
Measure electrical conductivity of solution --- DSubstrate、DChelate mother liquorAnd DSupernatant, supernatant and sugar alcohol chelating fertilizer three after the sugar alcohol chelating calcium, merging
The usage amount of person is corresponding, calculates chelation percent according to the following formula: chelation percent=1-DSupernatant/DChelate mother liquor=DSubstrate/DChelate mother liquor=DSubstrate/
(DSubstrate+DSupernatant)；
The sugar alcohol fertilizer of chelated calcium is prepared by sugar alcohol, water and excessive calcium nitrate, the sugar alcohol be sorbierite, mannitol and
One of xylitol is a variety of.
2. the method according to claim 1 based on electrical conductivity method measurement sugar alcohol fertilizer of chelated calcium chelation percent, which is characterized in that
Specifically includes the following steps: D in determination step (2)SubstrateAnd DChelate mother liquor, according to formula chelation percent=DSubstrate/DChelate mother liquor, calculate chelating
Rate.
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