CN112485316A - Electrochemical titration method for testing total chlorine in industrial monobutyl tin oxide - Google Patents
Electrochemical titration method for testing total chlorine in industrial monobutyl tin oxide Download PDFInfo
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- CN112485316A CN112485316A CN202011286698.XA CN202011286698A CN112485316A CN 112485316 A CN112485316 A CN 112485316A CN 202011286698 A CN202011286698 A CN 202011286698A CN 112485316 A CN112485316 A CN 112485316A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/42—Measuring deposition or liberation of materials from an electrolyte; Coulometry, i.e. measuring coulomb-equivalent of material in an electrolyte
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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
Abstract
The invention provides an electrochemical titration method for testing total chlorine in industrial monobutyltin oxide, which reduces space by adopting a silver composite electrode, thereby being capable of carrying out titration by using a smaller reactor, simultaneously reducing the collision probability of a stirring device to a precious silver electrode to zero in the titration process, improving the experimental safety and prolonging the service life of consumables, carrying out automatic titration and drawing by adopting a potentiometric titrator, not needing to continuously record the change of a potential value in the dripping process, then drawing, and automatically judging a titration end point by setting the potential change value in unit time by adopting the potentiometric titrator. The titration end point is judged without recording potential value change, the weighed mass of the monobutyltin oxide sample is input in the titration process, the titration method is adjusted, the start button is clicked, the total chlorine content in the monobutyltin oxide sample is obtained through automatic titration, and the possibility of difficult judgment of the end point and calculation error in manual testing is reduced.
Description
Technical Field
The invention relates to the field of chemical precipitation titration, in particular to an electrochemical titration method for testing total chlorine in industrial monobutyltin oxide.
Background
Monobutyl tin oxide is a widely used chemical raw material. The use of monobutyl tin oxide has the following advantages: 1. the esterification reaction time can be shortened; 2. the reaction temperature is reduced, the energy is saved, and the equipment utilization rate is improved; 3. the side reactions in the reaction, especially the dehydration condensation reaction and the oxidative decomposition reaction of the polyhydric alcohol and the secondary alcohol are reduced; 4. can be used with other reaction materials without special treatment, and only needs to be careful to avoid excessive moisture contact; 5. the finished product does not need neutralization or filtration, thereby saving time and cost. Because of the advantages, the utility model has the following purposes: 1. a plastic stabilizer raw material; 2. an esterification catalyst; 3. an organotin intermediate; 4. electrophoretic electrodeposition coating catalysts, and the like.
The raw materials in the production process of the monobutyl tin oxide are monobutyl magnesium chloride, tin chloride and an intermediate product of monobutyl tin chloride, and then the monobutyl tin oxide is generated by the reaction of the monobutyl magnesium chloride, the tin chloride and sodium hydroxide. Each reaction step cannot be completed, so that the product contains chlorine. And the purity of the indirect reaction monobutyl tin oxide is high and low due to the high and low chlorine content of the monobutyl tin oxide product.
At present, the principle of the method for testing total chlorine in monobutyltin oxide is precipitation reaction, i.e. silver ions react with chloride ions to generate silver chloride precipitate. However, the testing methods of many enterprises are not very complete at present. An enterprise tests total chlorine by adopting a chemical precipitation titration method, silver chloride precipitation can be generated quickly in the titration process, and the final finishing time is extremely difficult to judge. There is a potential titration with the help of electrochemical method, using PHS-3C acidimeter, saturated calomel electrode as reference electrode, and silver electrode as indicator electrode. Titrate with silver nitrate standard solution to the end of the jump. The end point judgment is as follows: in the titration process, 0.1ml of recording potential value is added to each drop, and the point with the largest potential difference value change is selected through the two drops before and after the drop. This method is time consuming and labor intensive. It is therefore important to solve the above problems.
Disclosure of Invention
In order to solve the problems, the invention provides an electrochemical titration method for testing total chlorine in industrial monobutyltin oxide, which reduces the space by adopting a silver composite electrode, thereby being capable of carrying out titration by using a smaller reactor, simultaneously, the collision probability of a stirring device to a noble silver electrode is reduced to zero in the titration process, the experimental safety is improved, the service life of consumables is prolonged, a potentiometric titrator is adopted for carrying out automatic titration and drawing, the change of a potential value is not required to be continuously recorded in the dripping process, then drawing is carried out, and the potentiometric titrator is adopted for automatically judging a titration endpoint by setting the potential change value in unit time. The titration end point is judged without recording the potential value change, the weighed mass of the monobutyltin oxide sample is input in the titration process, the titration method is adjusted, the start button is clicked, the total chlorine content in the monobutyltin oxide sample is obtained through automatic titration, the possibility of difficult end point judgment and calculation error in manual testing is reduced, and the problems in the background technology are solved.
The invention aims to provide an electrochemical titration method for testing total chlorine in industrial monobutyltin oxide, which comprises the following steps:
step 1: firstly, accurately weighing a sample into a beaker;
step 2: adding absolute ethyl alcohol into the mixture, and magnetically stirring until the sample is dispersed;
and step 3: adding concentrated nitric acid into the solution, and magnetically stirring until the solution is clear and transparent;
and 4, step 4: cooling the water to room temperature;
and 5: performing potentiometric titration, namely performing automatic titration drawing by adopting a silver composite electrode and a potentiometric titrator, and automatically judging a titration end point by setting the magnitude of a potential change value in unit time by adopting the potentiometric titrator; in the titration process, the mass of the weighed monobutyl tin oxide sample is input, the titration method is called, the start button is clicked, and the total chlorine content in the monobutyl tin oxide sample is obtained through automatic titration.
The further improvement lies in that: comprises the following steps:
step 1: accurately weighing 10g of sample (accurate to 0.0001 g) into a 100ml beaker;
step 2: measuring 50ml of absolute ethyl alcohol by using a measuring cylinder, adding the absolute ethyl alcohol into the measuring cylinder, and magnetically stirring until a sample is dispersed;
and step 3: measuring 20ml of concentrated nitric acid by using a measuring cylinder, adding the concentrated nitric acid into the measuring cylinder, and magnetically stirring the mixture until the mixture is clear and transparent;
and 4, step 4: cooling the water to room temperature;
and 5: performing potentiometric titration, namely performing automatic titration drawing by adopting a potentiometric titrator by adopting a silver composite electrode;
5.1 method (S-1 Cl) editing:
5.1.1 DET U Dynamic U titration:
and (3) balance is started: starting volume: 0.0000 mL; liquid adding speed: maximum; pausing: 0 s;
titration parameters: titration speed: optimizing; temperature: 25 ℃;
stopping conditions are as follows: number of stop equivalence points: 1; volume after equivalence point: 5 mL; liquid suction speed: maximum; the rest are all set as: closing;
potential evaluation: equivalence point criterion standard: 30, of a nitrogen-containing gas; and (3) equivalent point confirmation: all; setting a window: closing;
a sensor: measurement input: 1; a sensor: an Ag electrode;
liquid feeding device: liquid feeding device: 1; titrant: ag standard solution;
a stirrer: a stirrer: 1; stirring speed: and 8, automatically closing.
5.1.2 CAL C Calculation:
Calculating the formula: EP1 0.1003 0.03545/C00 100
5.1.3 preservation method, named S-1 Cl;
5.2, the method S-1 Cl is added, and the weighed mass of the monobutyl tin oxide is input;
5.3, starting a button, automatically titrating to an end point, automatically calculating to obtain a result,
the chlorine content is calculated by the formula
In the formula: v- - -titration of sample consumption silver nitrate standard solution volume, ml; c- - -concentration of silver nitrate standard solution (and 0.1003mol/L silver nitrate standard solution is adopted in the experiment), mol/L; m-sample mass, g; 0.03545- -mass of chlorine expressed in grams equivalent to 1.0ml of 1.000mol/L silver nitrate standard solution.
The invention has the beneficial effects that: the invention reduces the space by adopting the silver composite electrode, thereby being capable of carrying out titration by using a smaller reactor, simultaneously reducing the collision probability of a stirring device to the precious silver electrode to zero in the titration process, improving the experimental safety and prolonging the service life of consumable materials, carrying out automatic titration and drawing by adopting a potentiometric titrator, not needing to continuously record the change of the potential value in the dripping process, then drawing, and automatically judging the titration end point by setting the potential change value in unit time by adopting the potentiometric titrator. The titration end point is judged without recording potential value change, the weighed mass of the monobutyltin oxide sample is input in the titration process, the titration method is adjusted, the start button is clicked, the total chlorine content in the monobutyltin oxide sample is obtained through automatic titration, and the possibility of difficult judgment of the end point and calculation error in manual testing is reduced.
Detailed Description
For the purpose of enhancing understanding of the present invention, the present invention will be further described in detail with reference to the following examples, which are provided for illustration only and are not to be construed as limiting the scope of the present invention.
The embodiment provides an electrochemical titration method for testing total chlorine in industrial monobutyltin oxide, which comprises the following steps:
step 1: accurately weighing 10g of sample (accurate to 0.0001 g) into a 100ml beaker;
step 2: measuring 50ml of absolute ethyl alcohol by using a measuring cylinder, adding the absolute ethyl alcohol into the measuring cylinder, and magnetically stirring until a sample is dispersed;
and step 3: measuring 20ml of concentrated nitric acid by using a measuring cylinder, adding the concentrated nitric acid into the measuring cylinder, and magnetically stirring the mixture until the mixture is clear and transparent;
and 4, step 4: cooling the water to room temperature;
and 5: performing potentiometric titration, namely performing automatic titration drawing by adopting a potentiometric titrator by adopting a silver composite electrode;
5.1 method (S-1 Cl) editing:
5.1.1 DET U Dynamic U titration:
and (3) balance is started: starting volume: 0.0000 mL; liquid adding speed: maximum; pausing: 0 s;
titration parameters: titration speed: optimizing; temperature: 25 ℃;
stopping conditions are as follows: number of stop equivalence points: 1; volume after equivalence point: 5 mL; liquid suction speed: maximum; the rest are all set as: closing;
potential evaluation: equivalence point criterion standard: 30, of a nitrogen-containing gas; and (3) equivalent point confirmation: all; setting a window: closing;
a sensor: measurement input: 1; a sensor: an Ag electrode;
liquid feeding device: liquid feeding device: 1; titrant: ag standard solution;
a stirrer: a stirrer: 1; stirring speed: and 8, automatically closing.
5.1.2 CAL C Calculation:
Calculating the formula: EP1 0.1003 0.03545/C00 100
5.1.3 preservation method, named S-1 Cl;
5.2, the method S-1 Cl is added, and the weighed mass of the monobutyl tin oxide is input;
5.3, starting a button, automatically titrating to an end point, automatically calculating to obtain a result,
the chlorine content is calculated by the formula
In the formula: v- - -titration of sample consumption silver nitrate standard solution volume, ml; c- - -concentration of silver nitrate standard solution (and 0.1003mol/L silver nitrate standard solution is adopted in the experiment), mol/L; m-sample mass, g; 0.03545- -mass of chlorine expressed in grams equivalent to 1.0ml of 1.000mol/L silver nitrate standard solution.
Through adopting silver combined electrode, the space has been reduced to can titrate with littleer reactor, simultaneously, the probability of titrating the collision of in-process agitating unit to noble silver electrode falls to zero, improve experimental security and prolonged the consumptive material life-span, adopt potentiometric titrator to carry out the autotitration and draw, needn't drip the in-process and constantly take notes the potentiometric value and change, then draw again, adopt potentiometric titrator, through setting up the potentiometric value size automatic judgement titration terminal point in the unit interval. The titration end point is judged without recording potential value change, the weighed mass of the monobutyltin oxide sample is input in the titration process, the titration method is adjusted, the start button is clicked, the total chlorine content in the monobutyltin oxide sample is obtained through automatic titration, and the possibility of difficult judgment of the end point and calculation error in manual testing is reduced.
Claims (2)
1. An electrochemical titration method for testing total chlorine in industrial monobutyl tin oxide is characterized in that: the method comprises the following steps:
step 1: firstly, accurately weighing a sample into a beaker;
step 2: adding absolute ethyl alcohol into the mixture, and magnetically stirring until the sample is dispersed;
and step 3: adding concentrated nitric acid into the solution, and magnetically stirring until the solution is clear and transparent;
and 4, step 4: cooling the water to room temperature;
and 5: performing potentiometric titration, namely performing automatic titration drawing by adopting a silver composite electrode and a potentiometric titrator, and automatically judging a titration end point by setting the magnitude of a potential change value in unit time by adopting the potentiometric titrator; in the titration process, the mass of the weighed monobutyl tin oxide sample is input, the titration method is called, the start button is clicked, and the total chlorine content in the monobutyl tin oxide sample is obtained through automatic titration.
2. The method for electrochemical titration of total chlorine in monobutyltin oxide for industrial use according to claim 1, wherein: comprises the following steps:
step 1: accurately weighing 10g of sample (accurate to 0.0001 g) into a 100ml beaker;
step 2: measuring 50ml of absolute ethyl alcohol by using a measuring cylinder, adding the absolute ethyl alcohol into the measuring cylinder, and magnetically stirring until a sample is dispersed;
and step 3: measuring 20ml of concentrated nitric acid by using a measuring cylinder, adding the concentrated nitric acid into the measuring cylinder, and magnetically stirring the mixture until the mixture is clear and transparent;
and 4, step 4: cooling the water to room temperature;
and 5: performing potentiometric titration, namely performing automatic titration drawing by adopting a potentiometric titrator by adopting a silver composite electrode;
5.1 method (S-1 Cl) editing:
5.1.1 DET U Dynamic U titration:
and (3) balance is started: starting volume: 0.0000 mL; liquid adding speed: maximum; pausing: 0 s;
titration parameters: titration speed: optimizing; temperature: 25 ℃;
stopping conditions are as follows: number of stop equivalence points: 1; volume after equivalence point: 5 mL; liquid suction speed: maximum; the rest are all set as: closing;
potential evaluation: equivalence point criterion standard: 30, of a nitrogen-containing gas; and (3) equivalent point confirmation: all; setting a window: closing;
a sensor: measurement input: 1; a sensor: an Ag electrode;
liquid feeding device: liquid feeding device: 1; titrant: ag standard solution;
a stirrer: a stirrer: 1; stirring speed: 8, automatically closing;
5.1.2 CAL C Calculation:
calculating the formula: EP1 0.1003 0.03545/C00 100
5.1.3 preservation method, named S-1 Cl;
5.2, the method S-1 Cl is added, and the weighed mass of the monobutyl tin oxide is input;
5.3, starting a button, automatically titrating to an end point, automatically calculating to obtain a result,
the chlorine content is calculated by the formula
In the formula: v- - -titration of sample consumption silver nitrate standard solution volume, ml; c- - -concentration of silver nitrate standard solution (and 0.1003mol/L silver nitrate standard solution is adopted in the experiment), mol/L; m-sample mass, g; 0.03545- -mass of chlorine expressed in grams equivalent to 1.0ml of 1.000mol/L silver nitrate standard solution.
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| CN110726803A (en) * | 2019-11-01 | 2020-01-24 | 江苏扬农化工集团有限公司 | Method for determining amino value by automatic potentiometric titration |
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2020
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Application publication date: 20210312 |