CN110850025A - Method for determining chloride ion content in industrial iron oxide by automatic potentiometric titration - Google Patents
Method for determining chloride ion content in industrial iron oxide by automatic potentiometric titration Download PDFInfo
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- CN110850025A CN110850025A CN201910961718.XA CN201910961718A CN110850025A CN 110850025 A CN110850025 A CN 110850025A CN 201910961718 A CN201910961718 A CN 201910961718A CN 110850025 A CN110850025 A CN 110850025A
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- iron oxide
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- industrial iron
- silver nitrate
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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
- G01N31/164—Determining the equivalent point by means of a discontinuity by electrical or electrochemical means
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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
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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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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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
- G01N1/34—Purifying; Cleaning
Abstract
A method for measuring the content of chloride ions in industrial iron oxide by an automatic potentiometric titration method comprises the following steps: (1) drying; (2) grinding; (3) dissolving and filtering; (4) calibrating; (5) titration; (6) and (4) calculating. Compared with the traditional visual turbidimetry, the method has the advantages that the implementation process is simple, the test value is more accurate, the content of chloride ions in the industrial iron oxide can be rapidly measured after the industrial iron oxide is pretreated, the measurement result is more accurate and sensitive, the required sample weight is less, the consumed reagent is less, and an indicator is not required to be added.
Description
Technical Field
The invention relates to a method for measuring the content of chloride ions in industrial ferric oxide, in particular to a method for measuring the content of chloride ions in industrial ferric oxide by an automatic potentiometric titration method.
Background
The industrial iron oxide is used as a raw material of soft magnetic ferrite, hard magnetic ferrite, polishing paste and other industrial base materials, and is widely applied; wherein, the I-type industrial ferric oxide has strict control requirements on the content of chloride, the chloride ion impurities have certain influence on the product quality, and meanwhile, in the production process, the chloride ions are easy to form HCl to corrode equipment; 3) the content determination of chloride ions in the industrial iron oxide usually adopts a silver chloride visual turbidimetry, which needs a complicated distillation process, and the leached chloride ions are taken out from the solution by using water vapor, condensed and collected, and then added with silver nitrate dropwise, and finally compared with a standard turbidimetric solution, the content range of the chloride ions is determined. The experimental equipment and process of the method are complicated, the detection period is long, and only the range of the content of the chloride ions can be given.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects in the prior art and provides a method for measuring the content of chloride ions in industrial iron oxide by an automatic potentiometric titration method, which is rapid in quantification and convenient for controlling the content of chloride from the aspect of raw materials.
The technical scheme adopted by the invention for solving the technical problems is as follows: a method for measuring the content of chloride ions in industrial iron oxide by an automatic potentiometric titration method comprises the following steps:
(1) and (3) drying: drying an industrial iron oxide sample to constant weight, and cooling;
(2) grinding: grinding the dried industrial iron oxide obtained in the step (1), and sieving;
(3) dissolving and filtering: weighing the grinded and sieved industrial iron oxide obtained in the step (2) into a beaker, adding a nitric acid solution for dissolving, filtering, and transferring the obtained filtrate into a reaction cup of an automatic potentiometric titrator to obtain a sample to be detected;
(4) calibration: except that the sample to be tested is not added in the blank test, the use amount and the processing conditions of other components are consistent with those of the sample solution to be tested, and the volume V0 of the silver nitrate standard solution consumed in the blank test at the potential jump point is recorded;
(5) titration: titrating the sample to be tested obtained in the step (3) to a terminal point by using a silver nitrate standard solution under magnetic stirring, and recording the volume V of the silver nitrate standard solution consumed in the process of potential jump point;
(6) and (3) calculating: calculating the chloride ion content according to the formula:
in the formula, omega is the content of chloride ions and the unit weight percent;
c is the concentration of the silver nitrate standard solution in the step (5), and the unit mol/L;
m is the molar mass of chlorine in the industrial iron oxide and is 35.5 g/mol;
v is the volume of the silver nitrate standard solution consumed by titrating the sample to be detected to the end point, and the unit is mL;
v0 is the volume of silver nitrate standard solution consumed by titrating a blank sample to the end point, in mL;
m is the mass of the sample to be measured, unit g.
Further, the drying temperature is 105-110 ℃.
Furthermore, the sieving is a standard sieve with the sieving mesh number not more than 120 meshes.
The invention has the beneficial effects that: 1) according to the invention, through the drying process, the moisture in the industrial iron oxide sample is removed, and the testing accuracy is improved; 2) according to the invention, through grinding and sieving, the granularity of the sample is reduced, and the leaching efficiency of chloride ions is accelerated by increasing the specific surface area of the sample; 3) the invention adopts an automatic potentiometric titration method, determines the titration end point through potential jump, can efficiently and accurately measure the chloride ion content in the industrial ferric oxide, and has the advantages of simple test method, high detection speed, low cost and convenient service production.
Drawings
FIG. 1 is a schematic view of a comparative example visual turbidimetric apparatus.
Detailed Description
The present invention will be further described with reference to the following examples.
The chemical reagents used in the examples of the present invention, unless otherwise specified, are commercially available in a conventional manner.
Examples
The embodiment comprises the following steps:
(1) taking a sample, drying the sample in a drying oven at 110 ℃ for 2-3h to constant weight, and cooling the sample in a dryer;
(2) grinding the dried sample, and sieving the ground sample by a 120-mesh standard sieve;
(3) weighing 5g of the sieved sample on an electronic balance, and accurately obtaining +/-0.002 g;
(4) solution preparation:
(1+3) nitric acid solution: taking 1 unit volume of pure water and 3 unit volumes of concentrated nitric acid (98%), slowly pouring the concentrated nitric acid into water, and continuously stirring and uniformly mixing;
silver nitrate standard solution: 8.5. + -. 0.005g of analytically pure silver nitrate is weighed, dissolved in water, transferred into a 500mL brown volumetric flask, diluted to the mark with water and shaken up.
(5) Putting the weighed sample into a 150mL beaker, adding 40mL of (1+3) nitric acid solution, frequently shaking at room temperature to fully leach out chloride ions, filtering after 20min, and washing and filtering for multiple times by using (1+3) nitric acid;
(6) transferring the filtrate into a reaction cup of an automatic potentiometric titrator, starting magnetic stirring, titrating with 0.1mol/L silver nitrate standard solution, reaching the titration end point when the potential suddenly jumps, and recording the volume V of the consumed silver nitrate standard solution;
(7) simultaneously performing a blank test, wherein the dosage and operation of other components are the same as those in the step (4) and the step (5) except that no sample is added, and recording the volume V0 of the consumed silver nitrate standard solution when the titration end point is reached;
(8) the content of chloride ions is calculated to be 0.050 percent according to a formula,
in the formula:
c- -concentration of silver nitrate standard solution, unit mol/L;
the molar mass of N-chloride ions is 35.5 g/mol;
v, titrating the volume of the silver nitrate standard solution consumed by the sample to the end point, wherein the volume is unit mL;
TABLE 1 results of measuring chloride ion content in industrial iron oxide by autopotentiometric titration
Comparative example
Visual turbidimetry, comprising the steps of:
(1) solution preparation:
(1+1) nitric acid solution: taking 1 unit volume of pure water and 1 unit volume of concentrated nitric acid (98%), slowly pouring the concentrated nitric acid into water, and continuously stirring and uniformly mixing;
silver nitrate solution (17 g/L): weighing 1.7 +/-0.005 g of analytically pure silver nitrate, dissolving the silver nitrate in water, transferring the silver nitrate into a 100mL brown volumetric flask, diluting the silver nitrate with water to a scale, and shaking up;
chloride standard solution: 3.97g of chloramine T (C) was weighed out7H7ClNNaO2S·3H2O), placing the mixture into a 100mL volumetric flask, dissolving the mixture in water, diluting to a scale, shaking up, taking out 1mL of the mixture by a pipette, transferring the mixture into another 100mL volumetric flask, adding water to dilute to the scale, and shaking up for later use;
standard turbidimetric solution: 2mL, 4mL, 6mL, 8mL, 10mL, 12mL, 14mL, 16mL, 18mL, and 20mL of the chloride standard solution were taken out of a 25mL colorimetric tube, 1mL of a (1+1) nitric acid solution and 1mL of a silver nitrate solution were added, diluted with water to the scale, and shaken up.
(2) Weighing 0.5g + -0.01 g sample, placing in a conical flask (2 in FIG. 1), adding 20ml phosphoric acid, and heating;
(3) when the sample begins to dissolve, connecting a conical flask and a round-bottom flask (1 in figure 1) containing water which is boiled in advance, introducing water vapor into the conical flask, and stopping heating before white smoke emerges;
(5) continuously introducing water vapor into the conical flask to allow hydrogen chloride to completely escape, introducing into a collecting bottle (4 in figure 1) via a condensing tube (3 in figure 1), transferring the distillate into a 100mL volumetric flask, and adding water to dilute to scale;
(6) transferring 10mL of test solution by using a pipette, placing the test solution in a 25mL colorimetric tube, adding 1mL (1+1) of nitric acid solution and 1mL of silver nitrate solution, diluting the test solution to a scale with water, shaking up, and placing for 2 min;
(7) comparing the sample colorimetric tube with the standard turbidimetric solution, wherein the turbidity is not deeper than the standard turbidimetric solution.
TABLE 2 results of measuring chloride ion content in industrial iron oxide by visual turbidimetry
Claims (3)
1. A method for measuring the content of chloride ions in industrial iron oxide by an automatic potentiometric titration method is characterized by comprising the following steps: the method comprises the following steps:
(1) and (3) drying: drying an industrial iron oxide sample to constant weight, and cooling;
(2) grinding: grinding the dried industrial iron oxide obtained in the step (1), and sieving;
(3) dissolving and filtering: weighing the grinded and sieved industrial iron oxide obtained in the step (2) into a beaker, adding a nitric acid solution for dissolving, filtering, and transferring the obtained filtrate into a reaction cup of an automatic potentiometric titrator to obtain a sample to be detected;
(4) calibration: except that the sample to be tested is not added in the blank test, the use amount and the processing conditions of other components are consistent with those of the sample solution to be tested, and the volume V0 of the silver nitrate standard solution consumed in the blank test at the potential jump point is recorded;
(5) titration: titrating the sample to be tested obtained in the step (3) to a terminal point by using a silver nitrate standard solution under magnetic stirring, and recording the volume V of the silver nitrate standard solution consumed in the process of potential jump point;
(6) and (3) calculating: calculating the chloride ion content according to the formula:
in the formula, omega is the content of chloride ions and the unit weight percent;
c is the concentration of the silver nitrate standard solution in the step (5), and the unit mol/L;
m is the molar mass of chlorine in the industrial iron oxide and is 35.5 g/mol;
v is the volume of the silver nitrate standard solution consumed by titrating the sample to be detected to the end point, and the unit is mL;
v0 is the volume of silver nitrate standard solution consumed by titrating a blank sample to the end point, in mL;
m is the mass of the sample to be measured, unit g.
2. The method for measuring the chloride ion content of industrial iron oxide by the automated potentiometric titration according to claim 1, wherein: the drying temperature is 105-110 ℃.
3. The method for measuring the chloride ion content in industrial iron oxide by the automated potentiometric titration according to claim 1 or 2, wherein: the sieving is a standard sieve with the sieving mesh number not more than 120 meshes.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113341063A (en) * | 2021-05-25 | 2021-09-03 | 贵州省产品质量检验检测院 | Method for measuring chelating capacity of agricultural ammonium polyphosphate |
Citations (4)
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|---|---|---|---|---|
| EP0523446A1 (en) * | 1991-07-17 | 1993-01-20 | Gebr. Knauf Westdeutsche Gipswerke KG | Method and apparatus for continuously monitoring the content of chlorides in flue gas gypsum |
| CN1727886A (en) * | 2004-07-29 | 2006-02-01 | 宝山钢铁股份有限公司 | Method for measuring total content of chlorine in iron ore and brown iron oxide |
| CN105092776A (en) * | 2015-08-13 | 2015-11-25 | 超威电源有限公司 | Method for measuring chlorine content in industrial barium sulfate through full-automatic potenitiometric titration |
| CN106404995A (en) * | 2016-08-31 | 2017-02-15 | 大连博融新材料股份有限公司 | Method for measuring content of chlorine in mixed acid electrolyte through potentiometric titration |
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- 2019-10-11 CN CN201910961718.XA patent/CN110850025A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0523446A1 (en) * | 1991-07-17 | 1993-01-20 | Gebr. Knauf Westdeutsche Gipswerke KG | Method and apparatus for continuously monitoring the content of chlorides in flue gas gypsum |
| CN1727886A (en) * | 2004-07-29 | 2006-02-01 | 宝山钢铁股份有限公司 | Method for measuring total content of chlorine in iron ore and brown iron oxide |
| CN105092776A (en) * | 2015-08-13 | 2015-11-25 | 超威电源有限公司 | Method for measuring chlorine content in industrial barium sulfate through full-automatic potenitiometric titration |
| CN106404995A (en) * | 2016-08-31 | 2017-02-15 | 大连博融新材料股份有限公司 | Method for measuring content of chlorine in mixed acid electrolyte through potentiometric titration |
Non-Patent Citations (1)
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| 廖霞: "《大学化学基础实验(I)》", 31 August 2008, 贵州大学出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113341063A (en) * | 2021-05-25 | 2021-09-03 | 贵州省产品质量检验检测院 | Method for measuring chelating capacity of agricultural ammonium polyphosphate |
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Application publication date: 20200228 |