CN103317250A - Method for measuring content of rutile in electrode covering - Google Patents

Abstract

The invention discloses a method for measuring content of rutile in electrode covering. The method comprises the following steps: 1, preparing samples: removing metal and alloy materials in the electrode covering and obtaining samples containing rutile, nonmetallic minerals and chemical materials; 2, separating rutile in the samples in an electric separation method, performing electric separation on the samples obtained in step 1, and obtaining electric separation concentrate of the rutile, wherein the yield of the electric separation concentrate is the specific value of the mass of the electric separation concentrate and total amount of the samples; 3, analyzing the content of rutile TiO2 in the electric separation concentrate; 4, confirming the content of the rutile TiO2 in the electrode covering. The method for measuring the content of the rutile in the electrode covering is easy and convenient in steps of obtaining the electric separation concentrate through the electric separation method, can easily separate the rutile and does not need to separate by adopting chemical agents, the content of the rutile separated in the electric separation method approaches a theoretical value, and determination errors are less. The content of the rutile TiO2 is determined by adopting the chemical analysis method, the method is easy, and using amount of reagent is less.

Description

The assay method of rutile content in a kind of electrode coating

Technical field

The present invention relates to the assay method of rutile content in a kind of electrode coating, specifically measure in the electrode coating rutile TiO in the rutile content and electric separation concentrate ₂Content.

Background technology

Extrusion is called coating in the coating on core wire surface.The chemical composition of coating has vital impact to the performance of welding rod, and the prescription of therefore studying electrode coating is of great significance for designing and manufacturing high-quality high performance welding rod.Electrode coating is comprised of raw materials such as each quasi-mineral, alloy and chemical products, its constituent very complex, and they interfere with each other in quantitative analysis, and this brings many difficulties for the quantitative analysis of electrode coating.This paper separates the rutile composition in the electrode coating by the method that electric separation separates, and adopts chemical analysis method to rutile TiO in the electric separation concentrate ₂Content is analyzed, simultaneously the red stone content of Gold Samples is verified, the analysis result that obtains accurately and reliably, thereby explored the method for separating rutile in the electrode coating and detected rutile TiO in the electrode coating ₂The effective ways of content.

Summary of the invention

Purpose of the present invention provides the assay method of rutile content in a kind of electrode coating, the method is at first utilized the good electric conductivity of rutile, the rutile in the electrode coating and other component separation are obtained containing the electric separation concentrate of rutile with electrical concentration, then to rutile TiO in the electric separation concentrate ₂Analyze mensuration.

In order to reach above-mentioned technique effect, the present invention takes following technical scheme:

The assay method of rutile content in a kind of electrode coating may further comprise the steps:

Step 1: the preparation of sample: remove metal and alloy material in the electrode coating, obtain to contain the sample of rutile, nonmetallic mineral and industrial chemicals;

Step 2: utilize the rutile in the electrical concentration sample separation: the sample that step 1 is obtained carries out the electric separation separation, obtains to contain the electric separation concentrate of rutile, and the productive rate of electric separation concentrate is the ratio of quality and the sample total amount of electric separation concentrate; The condition that electric separation separates: drum barrel rotating speed: 60～120r/min, voltage: 20～55kV.The conduction property of coating Minerals such as following table 1.

Table 1: various mineral conduction properties

Mineral name	Molecular formula	DIELECTRIC CONSTANTS	Conduction property
				Rutile	TiO 2	87～173	Conductor
Fluorite	CaF 2	6.7～7.0	Non-conductor
				Wollastonite	Ca(Si 3O 9)	6.17	Non-conductor
Marble	CaCO 3	6	Non-conductor

Step 3: rutile TiO in the electric separation concentrate ₂The mensuration of content: the electric separation concentrate is added thermal decomposition through sodium fluoride and watery hydrochloric acid, collect residue after filtering, will cool off after the residue ashing, add the potassium pyrosulfate melting, dissolve filtration washing with dilute sulfuric acid heating leaching to frit, collect filtrate, filtrate being used for measured rutile TiO ₂Content;

Step 4: determine rutile TiO ₂Content in electrode coating: according to rutile TiO in the productive rate of the electric separation concentrate of step 2 and the step 3 electric separation concentrate ₂Content calculates rutile TiO ₂Content in electrode coating, rutile TiO ₂Content in electrode coating is rutile TiO in the productive rate of electric separation concentrate and the electric separation concentrate ₂The product of content.

Analyze rutile TiO in the electric separation concentrate in the above-mentioned step 3 ₂The mensuration of content specifically may further comprise the steps:

Rutile TiO in A, the electric separation concentrate ₂Extraction: accurately take by weighing the electric separation concentrate, place beaker, add sodium fluoride and watery hydrochloric acid, place and heat 1.5h on the electric hot plate, take off cooling, filter with fine and close quantitative filter paper, wash beaker and residue with rare HCl, the yellow of non-iron-ion to the filter paper; Residue is put into porcelain crucible place the Muffle furnace ashing, in 700 ℃ of calcination 20-30min, take out cooling, add potassium pyrosulfate and place Muffle furnace in 650-700 ℃ of melting 30min, use the dilute sulfuric acid heating leaching, be heated to the frit dissolving, filter while hot, with the dilute sulfuric acid washing, filtrate moves in the volumetric flask, be diluted with water to scale, this solution is measures rutile TiO in the electric separation concentrate ₂Sample solution;

B, draw the titania solution calibration curve: pipette 0.00,0.50,1.00,2.00,4.00,6.00,8.00, the titanium dioxide standard liquid of 10.00mL concentration 100.0 μ g/mL, place the 50mL volumetric flask, add the ascorbic acid solution that 5mL concentration is 20g/L, shake up, placed several minutes, add the hydrochloric acid 5mL of volume fraction 50%, concentration is 10mg/L diantipyrylmethane solution 20mL, is diluted with water to scale and shakes up; On spectrophotometer, survey absorbance in wavelength 420nm place after 1 hour, draw the titania solution calibration curve;

Rutile TiO in C, the mensuration electric separation concentrate ₂Content: the solution of minute getting above-mentioned steps A adds the ascorbic acid solution that 5mL concentration is 20g/L in the 50mL volumetric flask, shake up, placed several minutes, and added the hydrochloric acid 5mL of volume fraction 50%, concentration is 10mg/L diantipyrylmethane solution 20mL, be diluted with water to scale, shake up; On spectrophotometer, survey absorbance after 1 hour in wavelength 420nm place, check in rutile TiO in the electric separation concentrate sample solution according to the calibration curve of step B ₂Quality.

In above-mentioned assay method, rutile TiO in the described electric separation concentrate ₂Content calculates according to the following equation:

$\mathrm{\ω}\left({\mathrm{TiO}}_2\right)/{10}^{-2}=\frac{(m_1-m_0)\×V\×{10}^{-4}}{m\×V_1}$

In the formula:

ω (TiO ₂)/10 ^-2---rutile TiO in the electric separation concentrate ₂Mass fraction;

m ₁---check in rutile TiO the electric separation concentrate sample solution from calibration curve ₂Quality, μ g;

m ₀---check in the quality of titanium dioxide the sample blank solution, μ g from calibration curve;

V ₁---the volume of minute power taking concentrate selection sample solution, mL;

V---the cumulative volume of electric separation concentrate sample solution, mL;

M---take by weighing the quality of electric separation concentrate sample, g.

The present invention compared with prior art has following beneficial effect:

(1) after the present invention removes the metal in the electrode coating and alloy, adopts electrical concentration to obtain having the electric separation concentrate of conduction property, be rutile in this electric separation concentrate, adopt chemical analysis method to analyze rutile TiO in the electric separation concentrate ₂Content, adopt electrical concentration to obtain the simple operating steps of electric separation concentrate, be easy to rutile is sorted out, need not to adopt chemical reagent to separate, the rutile content that electric separation separates is approaching with theoretical value, evaluated error is little; Adopt chemical analysis method to TiO in the rutile ₂Content is measured, and method is simple, and using amount of reagent is few.

(2) the present invention provides method for the mensuration of rutile content in the electrode coating, for rutile content in the electrode coating provides test basis to the electrode coating performance impact, also provides technical support for the new formulating of electrode coating simultaneously.

The specific embodiment

The invention will be further elaborated and explanation below in conjunction with embodiments of the invention.

Embodiment:

Take certain self-control electrode coating sample as example, its prescription is: iron powder 17%, chromium powder 9%, nickel powder 9%, manganese powder 2%, molybdenum-iron 7%, ferrosilicon 4%, rutile 3.7%, marble 18%, fluorite 7%, wollastonite 4.3%, ice crystal 19%.

(1) get this electrode coating of 100g, remove wherein metal and alloy raw material, remaining sample weight is 48.3g.

(2) the remaining sample 48.3g that obtains in the step 1 being carried out electric separation as raw material separates, obtain 3.57g electric separation concentrate, then the productive rate of this electric separation concentrate is 3.57%, and namely the content of rutile is 3.57% in the electrode coating, and rutile content 3.70% is substantially approaching in this result and the composition of raw materials.

(3) analyze rutile TiO in the electric separation concentrate ₂Content:

Rutile TiO in A, the electric separation concentrate ₂Extraction: accurately take by weighing 0.2000g electric separation concentrate, place the 200mL polytetrafluoroethylene beaker, adding 0.5g sodium fluoride and 50mL mass fraction are 35% hydrochloric acid, on electric hot plate, under 250～300 ℃, heat 1.5h, take off cooling, filter with fine and close quantitative filter paper, wash beaker and residue with the HCl washings of 70～85 ℃ of mass fractions 5%, the yellow of non-iron-ion to the filter paper; Residue is put into the porcelain crucible ashing, in 700 ℃ of calcination 20-30min, take out cooling, add the 5-6g potassium pyrosulfate and place Muffle furnace in 650-700 ℃ of melting 30min, with sulfuric acid heating leaching in the 200mL beaker of 50mL mass fraction 6%, be heated to the frit dissolving, filter while hot, with 70～85 ℃ of mass fraction 6% sulfuric acid scrubbings, filtrate moves in the 100mL volumetric flask, be diluted with water to scale, this solution is measures rutile TiO in the electric separation concentrate ₂Sample solution;

B, draw the titania solution calibration curve: pipette 0.00,0.50,1.00,2.00,4.00,6.00,8.00, the titanium dioxide standard liquid of 10.00mL concentration 100.0 μ g/mL, place the 50mL volumetric flask, add the ascorbic acid solution that 5mL concentration is 20g/L, shake up, placed several minutes, add the hydrochloric acid 5mL of mass fraction 50%, concentration is 10mg/L diantipyrylmethane solution 20mL, is diluted with water to scale and shakes up; On spectrophotometer, survey absorbance in wavelength 420nm place after 1 hour, draw the titania solution calibration curve;

Rutile TiO in C, the mensuration electric separation concentrate ₂Content: the solution of minute getting 5-10mL above-mentioned steps A adds the ascorbic acid solution that 5mL concentration is 20g/L in the 50mL volumetric flask, shake up, placed several minutes, and added the hydrochloric acid 5mL of mass fraction 50%, concentration is 10mg/L diantipyrylmethane solution 20mL, be diluted with water to scale, shake up; On spectrophotometer, survey absorbance after 1 hour in wavelength 420nm place, check in electric separation concentrate sample solution rutile TiO according to the calibration curve of step B ₂Quality.

Rutile TiO in D, the described electric separation concentrate ₂Content calculates according to the following equation:

$\mathrm{\ω}\left({\mathrm{TiO}}_2\right)/{10}^{-2}=\frac{(m_1-m_0)\×V\×{10}^{-4}}{m\×V_1}$

In the formula:

ω (TiO ₂)/10 ^-2---rutile TiO in the electric separation concentrate ₂Mass fraction;

m ₁---check in rutile TiO the electric separation concentrate sample solution from calibration curve ₂Quality, μ g;

m ₀---check in the quality of sample blank solution titanium dioxide from calibration curve, μ g;

V ₁---the volume of minute power taking concentrate selection sample solution, mL;

V---the cumulative volume of electric separation concentrate sample solution, mL;

M---take by weighing the quality of electric separation concentrate sample, g.

Analyze rutile TiO in the 3.57g electric separation concentrate ₂Content is 87.56%.

(4) the electric separation concentrate yield is 3.57%, rutile TiO in the electric separation concentrate ₂Content is 87.56%, then rutile TiO ₂Content in electrode coating is: 3.57% * 87.56%=3.13%.

Although invention has been described with reference to explanatory embodiment of the present invention here, above-described embodiment only is the better embodiment of the present invention, embodiments of the present invention are not restricted to the described embodiments, should be appreciated that, those skilled in the art can design a lot of other modification and embodiments, and these are revised and embodiment will drop within the disclosed principle scope and spirit of the application.

Claims (4)

1. the assay method of rutile content in the electrode coating is characterized in that may further comprise the steps:

Step 1: the preparation of sample: remove metal and alloy material in the electrode coating, obtain to contain the sample of rutile, nonmetallic mineral and industrial chemicals;

Step 2: utilize the rutile in the electrical concentration sample separation: the sample that step 1 is obtained carries out the electric separation separation, obtains to contain the electric separation concentrate of rutile, and the productive rate of electric separation concentrate is the ratio of quality and the sample total amount of electric separation concentrate;

Step 3: rutile TiO in the electric separation concentrate ₂The mensuration of content: the electric separation concentrate is added thermal decomposition through sodium fluoride and watery hydrochloric acid, collect residue after filtering, will cool off after the residue ashing, add the potassium pyrosulfate melting, dissolve filtration washing with dilute sulfuric acid heating leaching to frit, collect filtrate, filtrate being used for measured electric separation concentrate rutile TiO ₂Content;

Step 4: determine rutile TiO ₂Content in electrode coating: according to rutile TiO in the productive rate of the electric separation concentrate of step 2 and the step 3 electric separation concentrate ₂Content calculate rutile TiO ₂Content in electrode coating, rutile TiO ₂Content in electrode coating is rutile TiO in the productive rate of electric separation concentrate and the electric separation concentrate ₂The product of content.

2. the assay method of rutile content in a kind of electrode coating according to claim 1 is characterized in that the condition that the described electric separation of step 2 separates is: drum barrel rotating speed: 60～120r/min, voltage: 20～55kV.

3. the assay method of rutile content in a kind of electrode coating according to claim 1 and 2 is characterized in that rutile TiO in the described electric separation concentrate of step 3 ₂The mensuration of content specifically may further comprise the steps:

Rutile TiO in A, the electric separation concentrate ₂Extraction: accurately take by weighing the electric separation concentrate, place beaker, add sodium fluoride and watery hydrochloric acid, place and heat 1.5h on the electric hot plate, take off cooling, filter with fine and close quantitative filter paper, wash beaker and residue with rare HCl, the yellow of non-iron-ion to the filter paper; Residue is put into porcelain crucible place the Muffle furnace ashing, in 700 ℃ of calcination 20-30min, take out cooling, add potassium pyrosulfate and place Muffle furnace in 650-700 ℃ of melting 30min, use the dilute sulfuric acid heating leaching, be heated to the frit dissolving, filter while hot, with the dilute sulfuric acid washing, filtrate moves in the volumetric flask, be diluted with water to scale, this solution is measures rutile TiO in the electric separation concentrate ₂Sample solution;

B, draw the titania solution calibration curve: pipette 0.00,0.50,1.00,2.00,4.00,6.00,8.00, the titanium dioxide standard liquid of 10.00mL concentration 100.0 μ g/mL, place the 50mL volumetric flask, add the ascorbic acid solution that 5mL concentration is 20g/L, shake up, placed several minutes, add the hydrochloric acid 5mL of volume fraction 50%, concentration is 10mg/L diantipyrylmethane solution 20mL, is diluted with water to scale and shakes up; On spectrophotometer, survey absorbance in wavelength 420nm place after 1 hour, draw the titania solution calibration curve;

The content of rutile TiO2 in C, the mensuration electric separation concentrate: divide and get the solution of above-mentioned steps A in the 50mL volumetric flask, add the ascorbic acid solution that 5mL concentration is 20g/L, shake up, placed several minutes, the hydrochloric acid 5mL that adds volume fraction 50%, concentration is 10mg/L diantipyrylmethane solution 20mL, is diluted with water to scale, shakes up; On spectrophotometer, survey absorbance in wavelength 420nm place after 1 hour, check in the quality of rutile TiO2 in the electric separation concentrate sample solution according to the calibration curve of step B.

4. the assay method of rutile content in a kind of electrode coating according to claim 3 is characterized in that rutile TiO2 content calculates according to the following equation in the described electric separation concentrate:

$\mathrm{\ω}\left({\mathrm{TiO}}_2\right)/{10}^{-2}=\frac{(m_1-m_0)\×V\×{10}^{-4}}{m\×V_1}$

In the formula:

ω (TiO ₂)/10 ^-2---rutile TiO in the electric separation concentrate ₂Mass fraction;

m ₁---check in rutile TiO the electric separation concentrate sample solution from calibration curve ₂Quality, μ g;

m ₀---check in the quality of titanium dioxide the sample blank solution, μ g from calibration curve;

V ₁---the volume of minute power taking concentrate selection sample solution, mL;

V---the cumulative volume of electric separation concentrate sample solution, mL;

M---take by weighing the quality of electric separation concentrate sample, g.