CN114324736A - Method for measuring content of elemental iron in reduced ilmenite powder - Google Patents
Method for measuring content of elemental iron in reduced ilmenite powder Download PDFInfo
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- CN114324736A CN114324736A CN202111314798.3A CN202111314798A CN114324736A CN 114324736 A CN114324736 A CN 114324736A CN 202111314798 A CN202111314798 A CN 202111314798A CN 114324736 A CN114324736 A CN 114324736A
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Abstract
The invention relates to a method for replacing elemental iron by a copper sulfate solution, which comprises the steps of reducing excessive copper sulfate by a pure aluminum sheet under an acidic condition, titrating by taking sodium diphenylamine sulfonate as an indicator and a potassium dichromate standard solution, and calculating the content of the elemental iron according to the volume of the consumed potassium dichromate standard solution. No iron ions to be measured are introduced; the method is accurate, simple and quick to operate and easy to master; the method is an accurate and quantitative analysis method, is suitable for measuring the content of the simple substance iron in the reduced ilmenite powder, and increases the selectivity of the method for measuring the simple substance iron in the reduced ilmenite powder.
Description
Technical Field
The invention belongs to the technical field of chemical component analysis methods, and particularly relates to a method for measuring the content of elemental iron in reduced ilmenite powder.
Background
Reduced ilmenite powder is one of the raw materials for manufacturing welding rods, and its main component indexes are titanium dioxide, ferrous oxide, elementary iron and small amount of impurities of carbon, sulfur, phosphorus, etc. (YB/T5141-1993), wherein the content of ferrous oxide can not exceed the specified value. The content of the ferrous oxide is determined by firstly determining the total iron content and then determining the content of the simple substance iron, and the difference between the total iron content and the simple substance iron content is the content of the ferrous oxide. The content of ferrous oxide is determined by the result of measuring the elementary substance iron, which not only influences the grade of reduced ilmenite powder, but also is the basis of the formula of the coating of the welding rod.
At present, the method for measuring the elementary substance iron in the reduced ilmenite powder is the method in GB8454-1987 (the method for measuring the ferrous content in the reduced ilmenite powder for welding rods). The method comprises the steps of leaching a sample by using a ferric trichloride solution, titrating by using a potassium dichromate standard solution, and then calculating the content of elemental iron.
When the method in GB8454-1987 (determination of ferrous content in reduced ilmenite powder for welding rods) is adopted for determination, a ferric trichloride solution is required to leach a sample, a potassium dichromate standard solution is used for titration, and then the content of the simple substance iron is calculated. Since the method adds iron ions to be measured, the operation and measurement conditions are strict and the analysis is not easy to grasp. A method for measuring elementary iron in reduced ilmenite powder. In particular to a chemical reagent for replacing elementary iron; this reagent contains no iron ions that affect the assay; titration can be performed with a potassium dichromate standard solution; the content of the simple substance iron can be calculated according to the volume of the consumed potassium dichromate standard solution
Disclosure of Invention
The invention aims to provide a method for measuring the content of elemental iron in reduced ilmenite powder. Realizes the replacement of the simple substance iron without iron ions influencing the determination; the titration can be carried out by using a potassium dichromate standard solution; the content of the elementary iron can be calculated according to the volume of the consumed potassium dichromate standard solution.
The technical scheme of the invention is that the method for measuring the content of the simple substance iron in the reduced ilmenite powder comprises the following specific steps:
first step, preparation of a sample to be measured: crushing a sample to be measured, sieving the crushed sample with a 150-mesh sieve, and weighing a certain amount of sample;
step two, preparing a potassium dichromate standard solution: drying the potassium dichromate reference reagent in an oven at 120 ℃ in advance until the weight is constant, weighing 2.4516g of the potassium dichromate reference reagent, dissolving in 100mL of water, putting the potassium dichromate reference reagent into a 1000mL volumetric flask, diluting with water to a scale, and shaking up;
step three, processing the sample to be measured: weighing 0.5g of sample in a 300mL triangular flask, adding 20mL of copper sulfate solution, heating until the reaction is complete, filtering, adding 20mL of sulfuric acid solution and 1g of pure aluminum foil into the filtrate, and adding the solution until large bubbles emerge; taking down, cooling to room temperature, adding 3 drops of sodium diphenylaminesulfonate indicator, and titrating with a potassium dichromate standard solution (0.0500moL/L) until the solution turns purple;
fourthly, calculating an analysis result:
the calculation formula is as follows,
in the formula:
55.85- - -molar mass of iron in g/moL;
w (Fe) -the content of the elementary iron in the sample, and the unit is g/L;
m < - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -weighing the weight of the sample in unit of the weight in g;
v- - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -volume of the titration solution in unit of L;
The potassium dichromate reference reagent is characterized in that the purity of copper sulfate is analytically pure, and the purity of pure aluminum foil is more than 99%.
The weight error of the sample is 0.0001g, the concentration of the copper sulfate solution is 2.5 percent, the sulfuric acid solution is a dilute sulfuric acid solution, namely 1 part of sulfuric acid and 4 parts of water, the purity of the pure aluminum foil is more than 99 percent, and the concentration of the sodium diphenylamine sulfonate indicator is 0.5 percent.
The method has the beneficial effects that the method for replacing the elemental iron by the copper sulfate solution is adopted, the excessive copper sulfate is reduced by a pure aluminum sheet under the acidic condition, sodium diphenylamine sulfonate is used as an indicator to be titrated with the potassium dichromate standard solution, and the content of the elemental iron is calculated according to the volume of the consumed potassium dichromate standard solution. No iron ions to be measured are introduced; the method is accurate, simple and quick to operate and easy to master; the method is an accurate and quantitative analysis method, is suitable for measuring the content of the simple substance iron in the reduced ilmenite powder, and increases the selectivity of the method for measuring the simple substance iron in the reduced ilmenite powder.
Detailed Description
The technical solution of the present invention is described in further detail below.
The method for measuring the content of the simple substance iron in the reduced ilmenite powder comprises the following steps: the content of elemental iron in reduced ilmenite was determined, for example, under the designation FTH 9.20.
First step, preparation of a sample to be measured: crushing the sample to be measured, sieving the crushed sample with a 150-mesh sieve, weighing a certain amount of the sample, heating and leaching the sample by using an excessive copper sulfate solution, and replacing monogenic iron.
Step two, preparing a potassium dichromate standard solution: the potassium dichromate reference reagent is dried in an oven at 120 ℃ in advance to constant weight, 2.4516g of the potassium dichromate reference reagent is weighed and dissolved in 100mL of water, the solution is moved into a 1000mL volumetric flask, diluted to scale by water and shaken up, and the solution is 0.0500 moL/L. The potassium dichromate reference reagent is copper sulfate (analytically pure); pure aluminum foil (purity > 99%).
Step three, processing the sample to be measured: a sample of 0.5g (exactly 0.0001g) was weighed into a 300mL Erlenmeyer flask, 20mL of a copper sulfate solution (2.5%) was added, the reaction was heated to completion, and filtered. To the filtrate was added 20mL of sulfuric acid solution (dilute sulfuric acid solution, 1 part sulfuric acid +4 parts water) and 1g of pure aluminum foil (purity > 99%) and added to the solution bubbling. Taking down, cooling to room temperature, adding 3 drops of sodium diphenylaminesulfonate indicator (0.5%), and titrating with a potassium dichromate standard solution (0.0500moL/L) until the solution turns to purple, namely the end point.
4. Calculation of analysis results:
the calculation formula is as follows,
in the formula:
55.85- - -molar mass of iron (g/moL);
w (Fe) -the content of elementary iron in the sample is g/L;
m < - > -weighing the mass (g) of the sample;
v- - - -volume of titration solution (L);
The invention adopts copper sulfate to replace simple substance iron, uses pure aluminum sheets to reduce excessive copper sulfate, and uses potassium dichromate titration method to measure.
Claims (3)
1. A method for measuring the content of simple substance iron in reduced ilmenite powder is characterized in that; the determination method comprises the following specific steps:
first step, preparation of a sample to be measured: crushing a sample to be measured, sieving the crushed sample with a 150-mesh sieve, and weighing a certain amount of sample;
step two, preparing a potassium dichromate standard solution: drying the potassium dichromate reference reagent in an oven at 120 ℃ in advance until the weight is constant, weighing 2.4516g of the potassium dichromate reference reagent, dissolving in 100mL of water, putting the potassium dichromate reference reagent into a 1000mL volumetric flask, diluting with water to a scale, and shaking up;
step three, processing the sample to be measured: weighing 0.5g of sample in a 300mL triangular flask, adding 20mL of copper sulfate solution, heating until the reaction is complete, filtering, adding 20mL of sulfuric acid solution and 1g of pure aluminum foil into the filtrate, and adding the solution until large bubbles emerge; taking down, cooling to room temperature, adding 3 drops of sodium diphenylamine sulfonate indicator, and titrating with a potassium dichromate standard solution (0.0500moL/L) until the solution turns purple;
fourthly, calculating an analysis result:
the calculation formula is as follows,
in the formula:
55.85- - -molar mass of iron in g/moL;
w (Fe) -the content of the elementary iron in the sample, and the unit is g/L;
m < - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -weighing the weight of the sample in unit of the weight in g;
v- - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -volume of the titration solution in unit of L;
2. The method for measuring the content of elemental iron in reduced ilmenite powder as claimed in claim 1, wherein the method comprises the following steps: the potassium dichromate reference reagent is characterized in that the purity of copper sulfate is analytically pure, and the purity of pure aluminum foil is more than 99%.
3. The method for measuring the content of elemental iron in reduced ilmenite powder as claimed in claim 1, wherein the method comprises the following steps: the weight error of the sample is 0.0001g, the concentration of the copper sulfate solution is 2.5 percent, the sulfuric acid solution is a dilute sulfuric acid solution, namely 1 part of sulfuric acid and 4 parts of water, the purity of the pure aluminum foil is more than 99 percent, and the concentration of the sodium diphenylamine sulfonate indicator is 0.5 percent.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103323449A (en) * | 2013-04-24 | 2013-09-25 | 北京神雾环境能源科技集团股份有限公司 | Determination method for metal iron and ferrous iron in direct reduction vanadium-titanium ore |
| CN109541131A (en) * | 2019-01-07 | 2019-03-29 | 长春黄金研究院有限公司 | The analysis method of copper and iron METHOD FOR CONTINUOUS DETERMINATION in a kind of ore |
| CN109580871A (en) * | 2018-11-26 | 2019-04-05 | 九江萍钢钢铁有限公司 | A kind of method of potassium bichromate standard solution calibration |
| CN111896530A (en) * | 2020-07-20 | 2020-11-06 | 九江萍钢钢铁有限公司 | Analysis method for measuring total iron content in blast furnace cloth bag dedusting ash |
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- 2021-11-08 CN CN202111314798.3A patent/CN114324736A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103323449A (en) * | 2013-04-24 | 2013-09-25 | 北京神雾环境能源科技集团股份有限公司 | Determination method for metal iron and ferrous iron in direct reduction vanadium-titanium ore |
| CN109580871A (en) * | 2018-11-26 | 2019-04-05 | 九江萍钢钢铁有限公司 | A kind of method of potassium bichromate standard solution calibration |
| CN109541131A (en) * | 2019-01-07 | 2019-03-29 | 长春黄金研究院有限公司 | The analysis method of copper and iron METHOD FOR CONTINUOUS DETERMINATION in a kind of ore |
| CN111896530A (en) * | 2020-07-20 | 2020-11-06 | 九江萍钢钢铁有限公司 | Analysis method for measuring total iron content in blast furnace cloth bag dedusting ash |
Non-Patent Citations (1)
| Title |
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| 王俊秀;薛明浩;侯俊坤;马清文;: "三氯化钛还原―重铬酸钾滴定法测定铁酸钙中Fe_2O_3", 山东冶金, no. 06 * |
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