CN109541127A - The method that a kind of pair of saturated potassium chloride solution carries out assay - Google Patents
The method that a kind of pair of saturated potassium chloride solution carries out assay Download PDFInfo
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- CN109541127A CN109541127A CN201811559986.0A CN201811559986A CN109541127A CN 109541127 A CN109541127 A CN 109541127A CN 201811559986 A CN201811559986 A CN 201811559986A CN 109541127 A CN109541127 A CN 109541127A
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- 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
- G01N31/162—Determining the equivalent point by means of a discontinuity
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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- 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
- G01N21/79—Photometric titration
Abstract
The invention discloses the methods that a kind of pair of saturated potassium chloride solution carries out assay, comprising: step S1: taking out a certain amount of saturated potassium chloride solution, carries out quantitative dilution, obtains potassium chloride weak solution；Step S2: taking out a certain amount of potassium chloride weak solution, carries out assay, calculates the content of each component in potassium chloride weak solution, then converse the content of each component in saturated potassium chloride solution.The method that a kind of pair of saturated potassium chloride solution provided by the invention carries out assay, not only high to the accuracy of each component assay in saturated potassium chloride solution, evaluated error is small, and convenience simple to operation, is with a wide range of applications.
Description
Technical field
The invention belongs to inorganic chemicals industry manufacture fields, contain more particularly, to a kind of pair of saturated potassium chloride solution
Measure method for measuring.
Background technique
In the prior art, potassium chloride is produced frequently with thermosol-cold junction crystallization, thermosol process, which refers to, heats sylvite
Dissolution makes potassium chloride in sylvite rising temperature for dissolving step by step, is finally warming up to 90 DEG C -95 DEG C and is just able to satisfy process requirements.
In thermosol process, changes relatively small principle using the solubility with temperature of sodium chloride, keep the potassium chloride in sylvite complete
Fully dissolved obtains potassium chloride high temperature saturated solution, and sodium chloride is retained in solid phase, then is separated by solid-liquid separation, thus by solid phase
Sodium chloride is separated with Klorvess Liquid.
Thermosol process carries out in thermosol slot, passes through the ginsengs such as control water temperature, water mine proportion, dissolution time and stirring intensity
Number achievees the effect that dissolve sylvite rate controlling, and obtained heat of solution liquid is potassium chloride high temperature saturated solution.Potassium chloride high temperature
The accuracy of measurement of each component content is directly related to the examination of the indexs such as the potassium chloride rate of recovery, thermosol effect in saturated solution,
If the accuracy of measurement of each component content is high, technical staff can learn potassium chloride and insatiable hunger in undissolved complete sylvite
Specific difference between solution and saturated solution, then by way of calculating, it is accurate to determine sylvite and the additional amount of water etc.
Parameter ensures the continuous-stable of production to reduce technique adjustment number, avoids unnecessary discharge, reduces KCl production
The loss of middle chlorination potassium resource and the loss of energy.If the accuracy of measurement of each component content is not high, there are error, then technology
Personnel will be unable to accurately adjust water mine proportion, and then the potassium chloride in sylvite can not be made to be completely dissolved, or obtained chlorination
Saturation state is not achieved in potassium solution, in any case as a result, can all lead to the rate of recovery of potassium chloride reduces.Therefore, in potassium chloride
In production, the accuracy of measurement of each component content in strict guarantee potassium chloride high temperature saturated solution.
Currently, direct sample method for measuring is used to the measurement of each component content in potassium chloride high temperature saturated solution, but
It is, since the sample is that saturated potassium chloride solution of the temperature at 90 DEG C -95 DEG C not can avoid temperature in sampling and continuous mode
Drop has a large amount of potassium chloride nucleus once cooling and is precipitated, causes evaluated error bigger than normal.There are what moisture evaporated to ask for hot solution
Topic, moisture evaporate the accuracy for directly influencing whether measurement result.In addition, if brilliant with the mode potassium chloride dissolving to heat up again
Core though avoiding nucleus is precipitated the error generated, but has partial moisture evaporation, can equally cause the bigger error of measurement.
Therefore, it is badly in need of a kind of method that can be improved to the accuracy of each component assay in potassium chloride high temperature saturated solution.
Summary of the invention
The purpose of the present invention is to provide the methods that a kind of pair of saturated potassium chloride solution carries out assay, full to potassium chloride
With carry out quantitative dilution after solution sampling, measure again, assay in saturated potassium chloride solution is deposited to solve the prior art
The bigger error the problem of, the accuracy to each component assay in saturated potassium chloride solution is improved.
The invention provides the following technical scheme: the method that a kind of pair of saturated potassium chloride solution carries out assay, wherein wrapping
It includes:
Step S1: taking out a certain amount of saturated potassium chloride solution, carries out quantitative dilution, obtains potassium chloride weak solution.
Step S2: taking out a certain amount of potassium chloride weak solution, carries out assay, calculates each group in potassium chloride weak solution
The content divided, then converse the content of each component in saturated potassium chloride solution.
According to embodiment of the present invention, wherein assay is carried out to the saturated potassium chloride solution, is at least wrapped
It includes: assay is carried out to potassium ion, calcium ion, magnesium ion and the chloride ion in saturated potassium chloride solution.
According to embodiment of the present invention, wherein the saturated potassium chloride solution is potassium chloride high temperature saturated solution,
Its temperature is between 90 DEG C -95 DEG C.
According to embodiment of the present invention, wherein described in step S1 is quantitatively diluted to take a certain amount of chlorination
Potassium high temperature saturated solution is added in the distilled water of specified weight.
According to embodiment of the present invention, wherein take a certain amount of potassium chloride high temperature saturated solution to be added to specific
In the distilled water of weight, include the following steps: that a. prepares a clean glassware, weigh m1 grams, distilled water is added, and it is described
Glassware is weighed as m2 grams together；B. the potassium chloride high temperature saturated solution is added into the glassware for fill distilled water,
M3 grams is weighed as together with the glassware for filling distilled water.
According to embodiment of the present invention, wherein the assay in step S2 is included at least to potassium chloride
Potassium ion, calcium ion, magnesium ion and chloride ion in weak solution carry out assay.
According to embodiment of the present invention, wherein using analysis by titration to the potassium in the potassium chloride weak solution
Ion, calcium ion, magnesium ion and chloride ion carry out assay.
According to embodiment of the present invention, wherein when carrying out assay to the potassium ion in potassium chloride weak solution,
It needs in advance to demarcate the standard solution of sodium tetraphenylborate and quaternary ammonium salt.
According to embodiment of the present invention, wherein in potassium chloride weak solution calcium ion and magnesium ion contain
Timing is measured, selects EDTA standard solution as titrating solution.
According to embodiment of the present invention, wherein when carrying out assay to the chloride ion in potassium chloride weak solution,
Select potassium chromate as indicator.
The method that a kind of pair of saturated potassium chloride solution provided by the invention carries out assay has the advantage that chlorination
Potassium high temperature saturated solution measures again after carrying out quantitative dilution, avoids the problem of cooling afterchlorinate potassium nucleus is precipitated, improves chlorine
Change the accuracy of potassium ion and chlorine ion content determination in potassium saturated solution；A certain amount of potassium chloride high temperature saturated solution is taken to be added
Into the distilled water of specified weight, not only reached quantitatively diluted effect, but also achieve the effect that cooling, and had avoided the evaporation of moisture,
Improve the accuracy of measurement；Analysis by titration is a kind of easy, quick quantitative analysis method, using analysis by titration to chlorine
Change potassium solution and carry out assay, there is higher accuracy, therefore, a kind of pair of saturated potassium chloride solution provided by the invention carries out
The method of assay, not only high to the accuracy of each component assay in saturated potassium chloride solution, evaluated error is small, and
Convenience simple to operation, is with a wide range of applications.
Specific embodiment
The preferred embodiments of the present invention will be described in detail below, and reference label refers to component in the present invention, technology,
Realizing under appropriate circumstances so as to advantages and features of the invention can be easier to be understood.Following description is weighed to the present invention
The materialization that benefit requires, and other specific implementations not clearly stated relevant to claim also belong to claim
Range.
The present invention provides the method that a kind of pair of saturated potassium chloride solution carries out assay, comprising:
Step S1: taking out a certain amount of saturated potassium chloride solution, carries out quantitative dilution, obtains potassium chloride weak solution.
Step S2: taking out a certain amount of potassium chloride weak solution, carries out assay, calculates each group in potassium chloride weak solution
The content divided, then converse the content of each component in saturated potassium chloride solution.
General chemical analysis is all operated at normal temperature, is sampled survey to the saturated potassium chloride solution of high temperature
Periodically, it is necessarily accompanied with the cooling of test sample and the evaporation of moisture, cooling will lead to the precipitation of potassium chloride nucleus, moisture evaporation
The concentration that will lead to test sample is bigger than normal, to influence the accuracy of measurement.
The present invention uses for reference most common double dilution method in pesticide industry, carries out quantitative dilution to saturated potassium chloride solution,
So that saturated solution is become unsaturated solution, then measure, rather than directly measured after traditional sampling, so as to avoid chlorine after cooling
Change the problem of potassium nucleus is precipitated, improves the accuracy of potassium ion and chlorine ion content determination in saturated potassium chloride solution；Meanwhile
The temperature for being diluted rear solution to saturated potassium chloride solution reduces, and reduces the evaporation of moisture, also improves the accurate of measurement
Property.
Method provided by the invention, wherein assay is carried out to the saturated potassium chloride solution, is included at least: to chlorine
Potassium ion, calcium ion, magnesium ion and the chloride ion changed in potassium saturated solution carry out assay.
In thermosol process, except containing in addition to a large amount of potassium chloride in the saturated potassium chloride solution of generation, also containing sodium chloride,
The impurity such as magnesium chloride and calcium sulfate can learn that potassium chloride is saturated by carrying out assay to the saturated potassium chloride solution
The content of each component in solution to further determine whether the solution is saturated potassium chloride solution, and by calculating, is learnt
The specific difference between potassium chloride and unsaturated solution and saturated solution in undissolved complete sylvite, it is accurate to adjust thermosol work
The parameters of sequence ensure the continuous-stable of production to reduce technique adjustment number, avoid unnecessary discharge, reduce chlorine
Change the loss of chlorination potassium resource and the loss of energy in potassium production.
Method provided by the invention, wherein the saturated potassium chloride solution is potassium chloride high temperature saturated solution, and temperature exists
Between 90 DEG C -95 DEG C.
In thermosol process, sylvite need to dissolve at a temperature of 90 DEG C -95 DEG C, therefore, obtained saturated potassium chloride solution is
High temperature saturated solution of the temperature between 90 DEG C -95 DEG C.
Method provided by the invention, wherein described in step S1 is quantitatively diluted to that a certain amount of potassium chloride height is taken to have enough to eat and wear
It is added in the distilled water of specified weight with solution.
It evaporates to reduce potassium chloride high temperature saturated solution nucleus during sampling and diluting and be precipitated with moisture, uses in advance
Glassware weighs up the weight of the distilled water of dilution, then fast sampling, is added in distilled water, completes dilution,
The sampling weight and thinner ratio of potassium chloride high temperature saturated solution are calculated with the method for weighing again.
Dilution process in the present invention is referred from common double dilution method in pesticide industry, but operating procedure is completely not
Together.Common double dilution method is that pesticidal preparations are first diluted to mother liquor or mother with a small amount of water or dilution carrier in pesticide industry
Then powder is diluted to required concentration again, to guarantee medicament evenly dispersed in water, accurate medication and the danger for reducing pesticide poisoning
Danger.And diluted purpose is crystallization in order to prevent and moisture evaporation in the present invention, it is therefore desirable to first by the distilled water of dilution
Weight weighs up, and sampling is added, and is re-weighed the weight and thinner ratio for calculating sampling, and does not want specifically to the concentration after dilution
It asks.
Method provided by the invention, wherein a certain amount of potassium chloride high temperature saturated solution is taken to be added to the steaming of specified weight
In distilled water, include the following steps:
A. prepare a clean glassware, weigh m1 grams, distilled water is added, is weighed as m2 together with the glassware
Gram.
B. the potassium chloride high temperature saturated solution is added into the glassware for fill distilled water, fills distilled water with described
Glassware be weighed as m3 grams together.
According to above-mentioned steps, the sampling weight of potassium chloride high temperature saturated solution can be calculated are as follows: m3-m2 grams, thinner ratio A
Are as follows:
A=(m3-m2)/(m3-m1)
Method provided by the invention, wherein the assay in step S2 is included at least in potassium chloride weak solution
Potassium ion, calcium ion, magnesium ion and chloride ion carry out assay.
Step S2 is to carry out assay to potassium chloride weak solution, by measurement, calculates each group in potassium chloride weak solution
The content divided converses the content of each component in saturated potassium chloride solution further according to thinner ratio A.
Method provided by the invention, wherein using analysis by titration in the potassium chloride weak solution potassium ion, calcium from
Son, magnesium ion and chloride ion carry out assay.
Analysis by titration is a kind of easy, quick quantitative analysis method, using analysis by titration to Klorvess Liquid into
Row assay has higher accuracy.
Method provided by the invention, wherein when carrying out assay to the potassium ion in potassium chloride weak solution, it is right in advance to need
The standard solution of sodium tetraphenylborate and quaternary ammonium salt is demarcated.
According to sodium tetraphenylborate-quaternary ammonium salt volumetric determination potassium ion content, potassium ion and sodium tetraphenylborate are generated surely
Fixed potassium tetraphenylborate precipitating, superfluous sodium tetraphenylborate titrates the tetraphenylboron quaternary ammonium salt for generating indissoluble with quaternary ammonium salt, thus between
It connects volumetric determination and goes out potassium content.The standard solution of sodium tetraphenylborate and quaternary ammonium salt is demarcated in advance, it can be further
Evaluated error is reduced, the accuracy of K+ determination is improved.
Method provided by the invention, wherein in potassium chloride weak solution calcium ion and magnesium ion carry out assay when,
Select EDTA standard solution as titrating solution.
EDTA is a kind of important complexing agent, can use the content of EDTA complexometry measurement calcium ion and magnesium ion.
Method provided by the invention, wherein when carrying out assay to the chloride ion in potassium chloride weak solution, select chromic acid
Potassium is as indicator.
Potassium ion, calcium ion, magnesium ion and the chloride ion conductor method in potassium chloride weak solution are done specifically below
It is bright:
1, the measurement of potassium content
1.1, the calibration of sodium tetraphenylborate and quaternary ammonium salt
A, the calibration of sodium tetraphenylborate concentration of standard solution:
5.00ml potassium chloride standard solution is drawn in triangular flask, 2ml magnesium sulfate-acetic acid solution is added, is stirred continuously down
10.00ml tetraphenyl borate sodium standard solution is instilled dropwise, is placed 5 minutes, and 4 0.1% bromophenol blue indicators of drop are added, are added
0.5ml sodium acetate buffer solution and 15 drop turpentine oil, sufficiently shake, and continue to be titrated to quaternary ammonium salt standard solution and blue are
Only.
Calculation formula are as follows: N(KCl)·V(KCl)=NsT·VsT1―NcT·VcT1
That is: N(KCl)5=NsT·10―NcT·VcT1 (1)
B, the calibration of quaternary ammonium salt concentration of standard solution:
5.00ml tetraphenyl borate sodium standard solution is drawn in triangular flask, 1ml NaAC-HAC buffer solution, 4 drops are added
0.1% bromophenol blue indicator, until being then titrated to blue with quaternary ammonium salt standard solution.
Calculation formula are as follows: NsT·VsT2=NcT·VcT2
That is: NsT5=NcT·VcT2 (2)
The measured concentration N of sodium tetraphenylborate and quaternary ammonium salt standard solution is calculated by above-mentioned formula (1) and formula (2)sTWith
NcT。
1.2, operating procedure
2ml magnesium sulfate-acetic acid solution is added in triangular flask in potassium chloride weak solution 5.00g obtained in aspiration step S1,
It instills 10.00ml tetraphenyl borate sodium solution dropwise under constant stirring, places 5 minutes, add 2ml NaAc_HAc buffer solution
About 15 drop turpentine oil, then plus 2 0.1% bromophenol blue indicators of drop, sufficiently shake, be then titrated to quaternary ammonium salt standard solution and be in
Until blue.
1.3, result calculates
In formula:
CK +The content of potassium ion in (%)-saturated potassium chloride solution；
NsTThe measured concentration of-tetraphenyl borate sodium standard solution；
NcTThe measured concentration of-quaternary ammonium salt standard solution；
VcT3The volume (ml) of-consumption quaternary ammonium salt standard solution；
A-thinner ratio.
2, the measurement of calcium ion content
2.1, principle
Calcon-carboxylic acid is dark brown powder, and being dissolved in water is purple, it can form red complex with calcium ion, in PH=12
When, can be used for calcium catalyst in calcium and magnesium mixture, terminal becomes blue from red, and color change is sharp, with this condition magnesium from
Son generates magnesium hydrate precipitate, does not react with titrant.
2.2, operating procedure
Potassium chloride weak solution 5.00g obtained in aspiration step S1 is titrated to PH with sodium hydroxide solution in triangular flask
12 or more, add calcium carboxylate indicator a little, shake up, is titrated to solution with EDTA standard solution and pure blue is become as extremely by red.
2.3, result calculates
In formula:
CCa 2+The content of calcium ion in (%)-saturated potassium chloride solution；
N(EDTA)The concentration of-EDTA standard solution；
V1The volume (ml) of-titration of calcium ions consumption EDTA standard solution；
A-thinner ratio.
3, the measurement of magnesium ion content
3.1, principle
As addition eriochrome black T (H3It In is blue in the buffer solution of PH=10) when indicator, with life after magnesium ion cooperation
At red complex, react as follows:
When being titrated with EDTA standard solution, H2Y2-Gradually capture the Mg in complex2+And it generates more stable
Complex MgY2-, it reacts as follows:
Work as MgIn-It is fully converted to MgY2-Blue HIn out free simultaneously2-, when solution becomes blue from red, as titrate
Terminal.
3.2, operating procedure
10.00ml ammonium hydroxide-ammonium chloride is added in triangular flask in potassium chloride weak solution 5.00g obtained in aspiration step S1
Buffer solution and 2 drop chromium black T indicators, shake up, and being titrated to solution to become blue by red with EDTA standard solution is to titrate eventually
Point.
3.3, result calculates
In formula:
CMg 2+The content of magnesium ion in (%)-saturated potassium chloride solution；
N(EDTA)The concentration of-EDTA standard solution；
V2The volume (ml) of-titration magnesium ion consumption EDTA standard solution；
A-thinner ratio.
4, the measurement of chloride ion content
4.1, principle
In weakly acidic pH chloride solution, titrated with silver nitrate standard solution, potassium chromate is indicator, due to chromate with
Silver ion reaction, generate siliver chromate, therefore, after Chlorine in Solution ionic reaction is complete, excessive silver nitrate immediately with chromate
Stable salmon pink siliver chromate precipitating is formed, to judge titration end-point.
Ag++Cl-→ AgCl ↓ (white)
Ag++CrO4 2-→Ag2CrO4↓ (salmon pink)
4.2, operating procedure
Potassium chloride weak solution 5.00g obtained in aspiration step S1 adds 1 drop potassium chromate indicator, is filling in triangular flask
Divide to be titrated under shaking with silver nitrate standard solution and stable salmon pink suspension, as titration end-point is presented.
4.3, result calculates
In formula:
CCl -The content of chloride ion in (%)-saturated potassium chloride solution；
N(AgNO3)—AgNO3The concentration of standard solution；
V(AgNO3)- consumption AgNO3The volume (ml) of standard solution；
A-thinner ratio.
Assay is that us is instructed to produce control " eyes ", and the present invention is by carrying out potassium chloride high temperature saturated solution
It is measured again after quantitative dilution, substantially increases the accuracy of assay, reduce the error of sampling and measurement, solve chlorination
Potassium high temperature saturated solution evaporates the problem for causing evaluated error excessive with moisture because crystallizing.
The method provided according to the present invention, by it is long-term it is on probation after, the analytical error of potassium chloride high temperature saturated solution can
It is maintained within 0.2%, the method can be applied to the measurement analysis of each component content in all high temperature saturated solutions.
It should be noted that the above-mentioned embodiments illustrate rather than limit the invention, and this
Field technical staff can be designed alternative embodiment without departing from the scope of the appended claims.In claim
In, any reference symbol between parentheses should not be configured to limitations on claims.
Claims (10)
1. the method that a kind of pair of saturated potassium chloride solution carries out assay, including:
Step S1: taking out a certain amount of saturated potassium chloride solution, carries out quantitative dilution, obtains potassium chloride weak solution；
Step S2: taking out a certain amount of potassium chloride weak solution, carries out assay, calculates each component in potassium chloride weak solution
Content, then converse the content of each component in saturated potassium chloride solution.
2. according to the method described in claim 1, wherein, carrying out assay to the saturated potassium chloride solution, including at least:
Assay is carried out to potassium ion, calcium ion, magnesium ion and the chloride ion in saturated potassium chloride solution.
3. the saturated potassium chloride solution is potassium chloride high temperature saturated solution according to the method described in claim 2, wherein,
Temperature is between 90 DEG C -95 DEG C.
4. according to the method described in claim 3, wherein, described in step S1 is quantitatively diluted to take a certain amount of potassium chloride high
Warm saturated solution is added in the distilled water of specified weight.
5. according to the method described in claim 4, wherein, a certain amount of potassium chloride high temperature saturated solution is taken to be added to specified weight
Distilled water in, include the following steps:
A. prepare a clean glassware, weigh m1 grams, distilled water is added, is weighed as m2 grams together with the glassware；
B. the potassium chloride high temperature saturated solution is added into the glassware for fill distilled water, with the glass for filling distilled water
Glass vessel are weighed as m3 grams together.
6. according to the method described in claim 1, wherein, the assay in step S2 includes at least dilute to potassium chloride molten
Potassium ion, calcium ion, magnesium ion and chloride ion in liquid carry out assay.
7. according to the method described in claim 6, wherein, using analysis by titration to the potassium in the potassium chloride weak solution from
Son, calcium ion, magnesium ion and chloride ion carry out assay.
8. according to the method described in claim 7, wherein, when carrying out assay to the potassium ion in potassium chloride weak solution, needing
The standard solution of sodium tetraphenylborate and quaternary ammonium salt is demarcated in advance.
9. according to the method described in claim 7, wherein, in potassium chloride weak solution calcium ion and magnesium ion carry out containing measuring
Periodically, select EDTA standard solution as titrating solution.
10. according to the method described in claim 7, wherein, when carrying out assay to the chloride ion in potassium chloride weak solution, selecting
Use potassium chromate as indicator.
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