CN113514365B - Method for measuring silicon-calcium content in silicon-calcium wire - Google Patents
Method for measuring silicon-calcium content in silicon-calcium wire Download PDFInfo
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- CN113514365B CN113514365B CN202110701518.8A CN202110701518A CN113514365B CN 113514365 B CN113514365 B CN 113514365B CN 202110701518 A CN202110701518 A CN 202110701518A CN 113514365 B CN113514365 B CN 113514365B
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- OSMSIOKMMFKNIL-UHFFFAOYSA-N calcium;silicon Chemical compound [Ca]=[Si] OSMSIOKMMFKNIL-UHFFFAOYSA-N 0.000 title claims abstract description 73
- 238000000034 method Methods 0.000 title claims abstract description 43
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000011575 calcium Substances 0.000 claims abstract description 50
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 48
- 239000000126 substance Substances 0.000 claims abstract description 29
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000010703 silicon Substances 0.000 claims abstract description 21
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 21
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000005303 weighing Methods 0.000 claims abstract description 13
- 229910052742 iron Inorganic materials 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 18
- 229910008455 Si—Ca Inorganic materials 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000002253 acid Substances 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 description 12
- 239000002184 metal Substances 0.000 description 12
- 238000011084 recovery Methods 0.000 description 9
- 229910000882 Ca alloy Inorganic materials 0.000 description 8
- 229910000831 Steel Inorganic materials 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- 229910000676 Si alloy Inorganic materials 0.000 description 4
- 239000002198 insoluble material Substances 0.000 description 4
- 238000001514 detection method Methods 0.000 description 3
- 238000004448 titration Methods 0.000 description 3
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- WNQQFQRHFNVNSP-UHFFFAOYSA-N [Ca].[Fe] Chemical compound [Ca].[Fe] WNQQFQRHFNVNSP-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000003926 complexometric titration Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- RGKMZNDDOBAZGW-UHFFFAOYSA-N aluminum calcium Chemical compound [Al].[Ca] RGKMZNDDOBAZGW-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 239000000378 calcium silicate Substances 0.000 description 1
- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000003009 desulfurizing effect Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The application discloses a method for measuring the content of silicon and calcium in a silicon and calcium line, which comprises the following steps: step 1: cutting a silicon-calcium wire sample; step 2: adding a dilute acetic acid solution into the silicon-calcium wire sample, dissolving until no bubbles are generated, taking out the iron sheet on the surface of the silicon-calcium wire, cleaning and drying; step 3: filtering the solution in the step 2, putting the filtered first insoluble substance and filter paper into a baking oven at 120 ℃ for drying for 1h, and weighing the first insoluble substance after cooling and marking the first insoluble substance as M3; step 4: adding the first insoluble substance into the dilute hydrochloric acid solution in the step 3 to dissolve the first insoluble substance without generating bubbles, putting the filtered second insoluble substance and filter paper into a baking oven at 120 ℃ to be dried for 1h, and weighing the second insoluble substance after cooling and marking the second insoluble substance as M4; step 5: and calculating the silicon-calcium content in the silicon-calcium line according to a weight method. The determination method solves the problem that the silicon and calcium contents of the silicon-calcium wire are difficult to accurately determine due to difficult stripping by the selectivity of different substances to the dissolved acid, and is simple and rapid, and high in accuracy.
Description
Technical Field
The application relates to the technical field of metallurgical chemistry detection and analysis, in particular to a method for measuring the content of silicon and calcium in a silicon and calcium line.
Background
The silicon-calcium wire is a cored wire made by coating silicon-calcium alloy. The Si-Ca wire is usually added as an additive to molten steel, wherein Si element not only has a strong deoxidizing ability but also has a good deoxidizing function. The metal calcium can be used for deoxidizing and desulfurizing molten steel, changing the form of impurities, promoting the floating of the impurities, purifying the molten steel and improving the castability of the molten steel.
In the prior art, the silicon content in the silicon-calcium line is usually measured by adopting an industry standard YB/T5312-2016 < < measurement of silicon content of silicon-calcium alloy > by a perchloric acid dehydration weight method, but the detection efficiency is influenced by considering that the operation steps are too complex. The method of EDTA complexometric titration is usually adopted for measuring the calcium in the silicon-calcium line, but the sample is not easy to be taken out from the iron sheet, the titration interference is serious, the end point is not easy to be observed, and the effect is not ideal.
Patent CN103822850B discloses a method for determining the content of metal calcium in a calcium cored wire, under normal temperature and pressure, using NH 4 Cl solution as a sample dissolving reagent and high purity metal magnesium or metal calcium as a standard, using a gas capacity method and related devices to determine the volume of hydrogen generated by a metal magnesium or metal calcium standard sample and a sample to be tested under the same experimental conditions, and calculating the content of metal calcium in the calcium iron cored wire by a comparison method according to a gas state equation. The method is not only suitable for measuring the metal calcium in the calcium-iron cored wires with different calcium contents, but also suitable for measuring the metal calcium in the calcium-series cored wires such as the aluminum-calcium cored wires, the silicon-calcium wires and the like with different calcium contents. However, the technical scheme described in patent CN103822850B has the problems of difficult sampling, easy oxidation of calcium and complicated operation, and the scheme does not solve the problem that the silicon-calcium wire is difficult to sample and peel.
Patent CN108663476a discloses a method for detecting the content of calcium in a seamless calcium line, which is to completely separate metal calcium from a steel pipe shell by reacting the metal calcium with water, determine the mass percent of calcium in the seamless calcium line and the mass percent of calcium in the calcium core of the seamless calcium line by using a gravimetric method and a complexometric titration method, further calculate the mass percent of calcium in the seamless calcium line, solve the problem that no quality acceptance method exists in the seamless calcium line of a new purchase factory, and establish a method for rapidly detecting the content of calcium in the seamless calcium line and the content of calcium in the calcium core. However, in the scheme described in patent CN108663476a, water reacts with calcium to form calcium hydroxide which is coated on the surface of metal calcium, so that the reaction is slow, and the determination of calcium adopts EDTA complexation titration method, so that titration interference is serious, endpoint is not easy to observe, and effect is not ideal.
Disclosure of Invention
The invention aims to provide a method for measuring the silicon-calcium content in a silicon-calcium line, which aims to overcome the defects in the prior art.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a method for measuring the content of silicon and calcium in a silicon and calcium wire comprises the following steps:
Step 1: cutting a silicon-calcium line sample, and weighing the sample and marking the mass as M1;
Step 2: adding a dilute acetic acid solution into a silicon-calcium wire sample, dissolving until no bubbles are generated, taking out iron sheets on the surface of the silicon-calcium wire, cleaning and drying, and then weighing the mass of the iron sheets to be M2;
Step 3: filtering the solution in the step 2, putting the filtered first insoluble substance and filter paper into a baking oven at 120 ℃ for drying for 1h, and weighing the first insoluble substance after cooling and marking the first insoluble substance as M3;
Step 4: adding the first insoluble substance into the dilute hydrochloric acid solution in the step 3 to dissolve the first insoluble substance without generating bubbles, putting the filtered second insoluble substance and filter paper into a baking oven at 120 ℃ to be dried for 1h, and weighing the second insoluble substance after cooling and marking the second insoluble substance as M4;
step 5: the Si-Ca content in the Si-Ca line is calculated according to the following formula:
WCa(％)＝[(M1-M2)-M3]/(M1-M2)*100
WSi(％)＝M4/(M1-M2)*100
Wherein: w Ca (%) is the calcium content in the Si-Ca wire, and W Si (%) is the silicon content in the Si-Ca wire.
Preferably, in the step2, the volume ratio of the dilute acetic acid solution is 1:9.
Preferably, in the step 4, the volume ratio of the diluted hydrochloric acid solution is 1:4.
Preferably, the filter paper is quantitative slow filter paper.
Preferably, in the step 3, the filtered first insoluble matter and the filter paper are washed with deionized water.
Preferably, in the step 4, the filtered second insoluble material and the filter paper are washed with deionized water.
Preferably, in the step 1, when the sample of the silicon-calcium wire is cut, 3 sections of the silicon-calcium wire are uniformly separated at intervals, more than 25cm is removed from the head end and the tail end, each section is 2cm long, and a section of the silicon-calcium wire with the mass of 2.50g is weighed as the sample.
Compared with the prior art, the method for measuring the silicon-calcium content in the silicon-calcium wire well solves the problem that the silicon and calcium contents of the silicon-calcium wire are difficult to accurately measure due to difficult stripping of the silicon-calcium wire by the selectivity of different substances to dissolved acid, is simple and quick, has high accuracy, and is beneficial to popularization and application.
Detailed Description
The following describes the technical solutions in the embodiments of the present invention in detail in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
A method for measuring the content of silicon and calcium in a silicon and calcium wire comprises the following steps:
Step 1: cutting a sample, cutting a silicon-calcium wire, dividing the silicon-calcium wire into 3 sections (more than 25cm is removed from the head end and the tail end of the silicon-calcium wire) per meter of the sample, weighing a section of silicon-calcium wire (the mass is 2.50 g) and placing the section of silicon-calcium wire into a 250ml beaker; the representative measurement sample is ensured.
Step 2: adding 30ml of dilute acetic acid solution into a beaker, dissolving until no bubbles are generated, loosening a silicon-calcium wire, taking out an iron sheet coated with the silicon-calcium alloy, cleaning, drying and weighing;
Step 3: filtering the solution in the beaker by using slow quantitative filter paper, washing the filter paper and the first insoluble matters by using deionized water for 3-5 times, transferring the first insoluble matters and the filter paper into a baking oven at 120 ℃ to bake for 1h, and weighing the insoluble matters after cooling;
Step 4: and adding 20ml of diluted hydrochloric acid solution into the cooled first insoluble substance to dissolve until no bubbles are generated, filtering the solution by using filter paper at a slow speed, washing the filter paper and the second insoluble substance with deionized water for 3-5 times, and transferring the second insoluble substance and the filter paper into a baking oven at 120 ℃ to bake for 1h. After cooling, the insoluble material is weighed,
Step 5: the contents of calcium and silicon are obtained by weight conversion.
WCa(％)＝[(M1-M2)-M3]/(M1-M2)*100
WSi(％)＝M4/(M1-M2)*100
Wherein M1 is the sum of the mass of the silicon-calcium alloy and the coated silicon-calcium alloy iron sheet, and the unit is gram (g); m2, the mass of the coated calcium-silicon alloy iron sheet is in grams (g); m3-the mass of insoluble material after insolubilization of the dilute acetic acid solution in grams (g). M4-the mass of insoluble material after insolubilization of the dilute hydrochloric acid solution, in grams (g).
Examples
3 Samples are arbitrarily selected to perform the repeatability and recovery rate test of the method by the method for measuring the silicon-calcium content in the silicon-calcium line, and the detection results are shown in the following table:
table 1 shows the results of the precision test of calcium silicate (n=8)
(II) recovery test
Calcium recovery test:
Since the calcium-silicon alloy is generally used as a raw material of the calcium-silicon wire, a certain amount of calcium-silicon alloy standard sample (GSB 03-2197-2008) is added into the sample for the calcium recovery test, and the calcium recovery test is performed on the calcium-silicon wire with different addition amounts according to the test condition A, and the test results are shown in Table 2 compared with the sample without the calcium-silicon alloy standard sample.
Table 2 shows the calcium recovery test
Recovery test of silicon:
The silicon-calcium alloy is usually used as a raw material of the silicon-calcium wire, so that a certain amount of silicon-calcium alloy standard sample (GSB 03-2197-2008) is added into the sample in the silicon recovery test, the silicon in the silicon-calcium wire with different addition amounts is recovered according to the test condition A, and the test result is shown in Table 3 compared with the sample without the silicon-calcium alloy standard sample.
Table 3 shows the silicon recovery test
From the above, as can be seen from tables 1 to 3, the method for measuring the silicon-calcium content in the silicon-calcium line provided by the application has the advantages of high accuracy in analyzing the silicon-calcium content in the silicon-calcium line, good repeatability and convenience for popularization and application.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises an element.
The foregoing is merely exemplary of the application and it will be appreciated by those skilled in the art that variations and modifications may be made without departing from the principles of the application, and it is intended that the application also be limited to the specific embodiments shown.
Claims (7)
1. A method for measuring the content of silicon and calcium in a silicon and calcium line is characterized by comprising the following steps of: comprising the following steps:
Step 1: cutting a silicon-calcium line sample, and weighing the sample and marking the mass as M1;
Step 2: adding a dilute acetic acid solution into a silicon-calcium wire sample, dissolving until no bubbles are generated, taking out iron sheets on the surface of the silicon-calcium wire, cleaning and drying, and then weighing the mass of the iron sheets to be M2;
Step 3: filtering the solution in the step 2, putting the filtered first insoluble substance and filter paper into a baking oven at 120 ℃ for drying for 1h, and weighing the first insoluble substance after cooling and marking the first insoluble substance as M3;
Step 4: adding the first insoluble substance into the dilute hydrochloric acid solution in the step 3 to dissolve the first insoluble substance without generating bubbles, putting the filtered second insoluble substance and filter paper into a baking oven at 120 ℃ to be dried for 1h, and weighing the second insoluble substance after cooling and marking the second insoluble substance as M4;
step 5: the Si-Ca content in the Si-Ca line is calculated according to the following formula:
WCa(％)＝[(M1-M2)-M3]/(M1-M2)*100
WSi(％)＝M4/(M1-M2)*100
Wherein: w Ca (%) is the calcium content in the Si-Ca wire, and W Si (%) is the silicon content in the Si-Ca wire.
2. The method for measuring the silicon-calcium content in the silicon-calcium wire according to claim 1, wherein the method comprises the following steps: in the step 2, the volume ratio of the dilute acetic acid solution is 1:9.
3. The method for measuring the silicon-calcium content in the silicon-calcium wire according to claim 1, wherein the method comprises the following steps: in the step 4, the volume ratio of the dilute hydrochloric acid solution is 1:4.
4. The method for measuring the silicon-calcium content in the silicon-calcium wire according to claim 1, wherein the method comprises the following steps: the filter paper is quantitative slow filter paper.
5. The method for measuring the silicon-calcium content in the silicon-calcium wire according to claim 1, wherein the method comprises the following steps: in the step 3, the filtered first insoluble matter and the filter paper are washed by deionized water.
6. The method for measuring the silicon-calcium content in the silicon-calcium wire according to claim 1, wherein the method comprises the following steps: in the step 4, the filtered second insoluble matter and the filter paper are washed by deionized water.
7. The method for measuring the silicon-calcium content in the silicon-calcium wire according to claim 1, wherein the method comprises the following steps: in the step 1, when the silicon-calcium wire sample is sheared, 3 sections are evenly separated from each meter of silicon-calcium wire at intervals, more than 25cm is removed from the head end and the tail end, each section is 2cm long, and a section of silicon-calcium wire with the mass of 2.50g is weighed as the sample.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102213704A (en) * | 2011-03-30 | 2011-10-12 | 太原重工股份有限公司 | Method for measuring contents of silicon-calcium elements in silicon-calcium alloy |
| CN103822850A (en) * | 2014-02-26 | 2014-05-28 | 华中科技大学 | Method for determination of content of calcium metal in calcium-series cored wires |
| CN108663476A (en) * | 2017-03-30 | 2018-10-16 | 上海梅山钢铁股份有限公司 | The detection method of calcium content in a kind of seamless calcium line |
| KR20210044986A (en) * | 2019-10-16 | 2021-04-26 | 주식회사 엘지화학 | Analysis method for metal contents in the anode material |
| CN112858570A (en) * | 2021-01-13 | 2021-05-28 | 广东韶钢松山股份有限公司 | Method for detecting calcium content in solid calcium wire |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101701914A (en) * | 2009-10-29 | 2010-05-05 | 江西稀有金属钨业控股集团有限公司 | Analysis detection method for calcium element in ore |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102213704A (en) * | 2011-03-30 | 2011-10-12 | 太原重工股份有限公司 | Method for measuring contents of silicon-calcium elements in silicon-calcium alloy |
| CN103822850A (en) * | 2014-02-26 | 2014-05-28 | 华中科技大学 | Method for determination of content of calcium metal in calcium-series cored wires |
| CN108663476A (en) * | 2017-03-30 | 2018-10-16 | 上海梅山钢铁股份有限公司 | The detection method of calcium content in a kind of seamless calcium line |
| KR20210044986A (en) * | 2019-10-16 | 2021-04-26 | 주식회사 엘지화학 | Analysis method for metal contents in the anode material |
| CN112858570A (en) * | 2021-01-13 | 2021-05-28 | 广东韶钢松山股份有限公司 | Method for detecting calcium content in solid calcium wire |
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