CN111122473A - Method for rapidly analyzing content of silicon in medium-low carbon ferrochrome - Google Patents
Method for rapidly analyzing content of silicon in medium-low carbon ferrochrome Download PDFInfo
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- CN111122473A CN111122473A CN201911416316.8A CN201911416316A CN111122473A CN 111122473 A CN111122473 A CN 111122473A CN 201911416316 A CN201911416316 A CN 201911416316A CN 111122473 A CN111122473 A CN 111122473A
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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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
Abstract
The invention discloses a method for rapidly analyzing the silicon content in medium-low carbon ferrochrome, which comprises the steps of weighing 0.1g of prepared medium-low carbon ferrochrome sample and a standard sample, respectively preparing detection solutions, and respectively placing the samples in 100ml steel measuring bottles; adding 10ml of hydrochloric acid solution into a steel measuring flask, adding 5ml of hydrogen peroxide solution, and heating until the sample is completely dissolved; the wall of the bottle is flushed by water and boiled to be large bubbles; cooling the steel measuring flask to room temperature, diluting to 100ml of scale mark, and shaking up; taking 10ml of mother liquor in a steel measuring flask, placing the mother liquor in a 150ml dry conical flask, and adding 25ml of water; adding 5ml of ammonium molybdate solution into 2 conical flasks; placing the mixture in an environment with the temperature of more than 15 ℃ for 20 minutes, adding 10ml of oxalic acid solution, immediately adding 5ml of ammonium ferrous sulfate solution, and shaking up; and (3) taking water as a reference solution, measuring the absorbance in a cuvette with the wavelength of 650-660 nm and the length of 1-2 cm, and simultaneously carrying a sample conversion result. The invention improves the analysis efficiency; the reagent dosage is greatly reduced, and the cost and the waste liquid treatment capacity are reduced; the accuracy of the analysis is improved.
Description
Technical Field
The invention belongs to the field of ferrous metallurgy, and particularly relates to a method for rapidly analyzing the content of silicon in medium-low carbon ferrochrome.
Background
According to the national standard, the determination of the silicon content in the medium-low carbon ferrochrome has three determination methods at present:
① precipitation of potassium silicofluorite determines silicon (GB/T5687.2).
The method has the following defects: the polytetrafluoroethylene beaker is used for dissolution, and as the beaker cannot be heated too much, the sample is large, the sample is dissolved too slowly, and the phenomenon that the sample cannot be dissolved completely often occurs, so that the time is delayed and the result error is caused.
② perchloric acid dehydration gravimetric method (GB/T5687-2007).
The method has the following defects: the method is complicated, the whole operation process consumes a long time, and the requirement of rapid production cannot be met.
③ ferrous molybdenum blue photometry
The method has the following defects: the sample is slow to dissolve or even can not be completely dissolved, the time consumption is too long, and the production requirement can not be met.
All three methods have certain defects and cannot meet the requirements of field production.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a method for rapidly analyzing the silicon content in medium-low carbon ferrochrome.
The technical scheme is as follows: the invention discloses a method for rapidly analyzing the silicon content in medium-low carbon ferrochrome, which comprises the following steps:
(1) weighing prepared medium-low carbon ferrochrome samples and similar standard samples, and respectively placing 0.1g of the samples and the similar standard samples into 2 steel measuring bottles of 100 ml;
(2) adding 10ml of hydrochloric acid solution into each steel measuring flask, and then adding 5ml of hydrogen peroxide solution;
(3) heating until the sample is completely dissolved;
(4) the wall of the bottle is flushed by water and boiled to be large bubbles;
(5) cooling 2 steel measuring flasks to room temperature, diluting the steel measuring flasks to 100ml of scale marks, and shaking up;
(6) dividing 10ml of mother liquor in 2 steel measuring flasks into 2 150ml of dry conical flasks, and adding 25ml of water;
(7) respectively adding 5ml of ammonium molybdate solution into 2 conical flasks;
(8) placing the mixture in an environment with the temperature of more than 15 ℃ for 20 minutes, adding 10ml of oxalic acid solution, immediately adding 5ml of ammonium ferrous sulfate solution, and shaking up;
(9) and (3) taking water as a reference solution, measuring the absorbance in a cuvette with the wavelength of 650-660 nm and the length of 1-2 cm, and simultaneously carrying a sample conversion result.
Wherein, the hydrochloric acid solution is prepared by uniformly mixing 37 percent hydrochloric acid and water phase with the same volume.
Wherein the concentration of the hydrogen peroxide solution is 30%.
Wherein, the ammonium molybdate solution is prepared by dissolving 5g of ammonium molybdate in water to 100 ml.
Wherein, the oxalic acid solution is prepared by dissolving 4g of oxalic acid in water to 100 ml.
Wherein, the ferrous ammonium sulfate solution is prepared by dissolving 6g ferrous ammonium sulfate in water, adding 2ml sulfuric acid, and diluting 100ml with water.
Wherein, using the instrument: 723N spectrophotometer. Similar standard samples: the content of the component to be detected in the sample is close to that of the standard sample, and the composition of the sample to be detected is similar to that of the standard sample. The conversion mode in the step (9) is as follows: determining the content of the component to be detected by using a standard sample conversion algorithm, namely simultaneously determining a standard sample and a sample to be detected according to the same condition, and obtaining the content of the component to be detected in the sample according to the ratio of absorbance; for example, if the absorbance 0.553 of the standard sample with a content of 1.02% is measured by a 723N spectrophotometer and the absorbance of the sample to be tested is 0.76, the result of the sample is 1.02% ÷ 0.553 × 0.76= 1.40%.
Has the advantages that: compared with the prior art, the invention has the following advantages:
(1) the analysis efficiency is improved, the analysis time of the traditional potassium silicofluoride precipitation method is longer than 5 hours, the analysis time of the perchloric acid dehydration gravimetric method is longer than 20 hours, the analysis time of the ferrous molybdenum blue photometry is longer than 2 hours, and the analysis time of the method is controlled within 1 hour;
(2) the method greatly reduces the reagent dosage and the cost and the waste liquid treatment capacity, the traditional potassium silicofluoride precipitation method needs to use 7 reagents, the waste liquid amount is about 160ml, the perchloric acid dehydration weight method needs to use 9 reagents, the waste liquid amount is about 280ml, the ferrous molybdenum blue photometry needs to use 7 reagents, the waste liquid amount is about 220ml, only 5 reagents need to be used, the waste liquid amount is about 60ml, and the production cost is reduced by about 70%;
(3) the analysis accuracy in the aspect is improved, compared with the traditional ferrous molybdenum blue photometry, the average value of the method is closer to the standard value, and the detection deviation value of the method for detecting the silicon content in the low-carbon ferrochrome (GBW 014250), the medium-carbon ferrochrome (ZGJT-2010-2) and the medium-carbon ferrochrome (YSBC28626-2011) is within 0.1.
Detailed Description
Example 1:
① drilling the cross section of the raw material sample according to GB/T4010-2015 standard, sieving with a 15-mesh sample sieve, ② weighing 0.1g of sample, weighing similar standard samples with similar contents, operating together, respectively placing into 100ml steel measuring flasks, ③ respectively adding 10ml of hydrochloric acid, then adding 5ml of hydrogen peroxide, heating at low temperature until the reaction is finished, ④ purging the flask wall with a small amount of water, boiling to large bubbles, taking down and cooling to room temperature, diluting to 100ml of scale line, shaking uniformly, ⑤ min taking 10ml of mother liquor into a 100ml conical flask, adding 25ml of distilled water, adding 5ml of 5% ammonium molybdate solution, standing for 15-20 min, adding 10ml of 4% oxalic acid solution, shaking to clear, immediately adding 5ml of 6% ammonium ferrous sulfate solution, shaking to obtain the product, ⑥ using distilled water as a reference, measuring absorbance in a cuvette with a wavelength of 660nm, converting by using the standard sample to obtain an analysis result, evaluating the accuracy of the analysis result, ⑦ finally performing waste liquid treatment, and finishing the analysis.
And (3) analysis results:
Claims (6)
1. a method for rapidly analyzing the silicon content in medium-low carbon ferrochrome is characterized by comprising the following steps:
(1) weighing prepared medium-low carbon ferrochrome samples and similar standard samples, and respectively placing 0.1g of the samples and the similar standard samples into 2 steel measuring bottles of 100 ml;
(2) adding 10ml of hydrochloric acid solution into each steel measuring flask, and then adding 5ml of hydrogen peroxide solution;
(3) heating until the sample is completely dissolved;
(4) the wall of the bottle is flushed by water and boiled to be large bubbles;
(5) cooling 2 steel measuring flasks to room temperature, diluting the steel measuring flasks to 100ml of scale marks, and shaking up;
(6) dividing 10ml of mother liquor in 2 steel measuring flasks into 2 150ml of dry conical flasks, and adding 25ml of water;
(7) respectively adding 5ml of ammonium molybdate solution into 2 conical flasks;
(8) placing the mixture in an environment with the temperature of more than 15 ℃ for 20 minutes, adding 10ml of oxalic acid solution, immediately adding 5ml of ammonium ferrous sulfate solution, and shaking up;
(9) and (3) taking water as a reference solution, measuring the absorbance in a cuvette with the wavelength of 650-660 nm and the length of 1-2 cm, and simultaneously carrying a sample conversion result.
2. The method for rapidly analyzing the silicon content in the medium and low carbon ferrochrome according to claim 1, wherein the hydrochloric acid solution is prepared by uniformly mixing 37% hydrochloric acid and an aqueous phase with the same volume.
3. The method for rapidly analyzing the content of silicon in medium-low-carbon ferrochrome according to claim 1, wherein the concentration of the hydrogen peroxide solution is 30%.
4. The method for rapidly analyzing the silicon content in the medium-low carbon ferrochromium according to claim 1, wherein the ammonium molybdate solution is prepared by dissolving 5g of ammonium molybdate in water to 100 ml.
5. The method for rapidly analyzing the silicon content in the medium-low carbon ferrochrome according to claim 1, wherein the oxalic acid solution is prepared by dissolving 4g of oxalic acid in water to 100 ml.
6. The method for rapidly analyzing the silicon content in the medium and low carbon ferrochromium according to claim 1, wherein the ammonium ferrous sulfate solution is prepared by dissolving 6g of ammonium ferrous sulfate in water, adding 2ml of sulfuric acid, and diluting 100ml of sulfuric acid with water.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911416316.8A CN111122473A (en) | 2019-12-31 | 2019-12-31 | Method for rapidly analyzing content of silicon in medium-low carbon ferrochrome |
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| CN201911416316.8A CN111122473A (en) | 2019-12-31 | 2019-12-31 | Method for rapidly analyzing content of silicon in medium-low carbon ferrochrome |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1904590A (en) * | 2006-08-04 | 2007-01-31 | 四川东风电机厂有限公司 | Technology of assaying silicon content in cast iron pigiron and ductile cast iron using photometry |
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- 2019-12-31 CN CN201911416316.8A patent/CN111122473A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1904590A (en) * | 2006-08-04 | 2007-01-31 | 四川东风电机厂有限公司 | Technology of assaying silicon content in cast iron pigiron and ductile cast iron using photometry |
Non-Patent Citations (2)
| Title |
|---|
| 包大杰等: "一种高碳、高铬、高钨镍基合金中硅的测定", 《柴油机设计与制造》 * |
| 范常生: "《临床生化检验复习参考》" * |
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Application publication date: 20200508 |