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Method for determining content of niobium oxide in steel

A determination method, niobium oxide technology, applied in the field of analytical chemistry, can solve problems such as complicated operation and easy pollution

Active Publication Date: 2015-04-29
INNER MONGOLIA BAOTOU STEEL UNION
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Niobium oxide analysis is included in the determination method of the total amount of oxide inclusions in steel. This method is currently the main method for determining niobium oxide in steel; the electrolysis time of this method is more than 48 hours, and the carbide is processed, and the precipitate obtained is total oxide inclusions. Quantity, high temperature melting, ICP-AES determination of its silicon, calcium, aluminum, niobium and other components, the analysis time is 5 to 7 days, the operation is complicated and easy to pollute

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  • Method for determining content of niobium oxide in steel

Examples

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Embodiment 1

[0071] A rare earth steel sample containing 0.016% niobium was made into a column with a diameter of 8.5mm and a length of 80mm, and a groove with a depth of 2mm was dug at a distance of 4mm from the top. Observation showed that the steel sample had no holes or cracks.

[0072] Soak the steel sample in a measuring cup filled with 25mL water and 25mL hydrochloric acid of ρ1.19g / mL for 10min, take it out, wash it, rinse it with ethanol, and dry it in the air; weigh the steel sample accurately in m 1 is 89.4826g, put the glass beaker filled with the prepared 250mL electrolyte into the electrolytic cell, and the electrolyte is an aqueous solution containing 7% potassium chloride by mass percentage and 1% citric acid by mass . Use the weighed steel sample as the anode, and the stainless steel cylinder as the cathode, turn on the silicon rectifier, set the electrolysis current to 0.6A, and conduct electrolysis at room temperature. After 70 minutes of electrolysis, remove the steel s...

Embodiment 2

[0076] A niobium steel sample with a total niobium content of 0.030% was made into a column with a diameter of 8.mm and a length of 85 mm, and a groove with a depth of 2 mm was dug at a distance of 3 mm from the top. Observation showed that the steel sample had no holes or cracks.

[0077] Soak the steel sample in a measuring cup filled with 20mL of water and 20mL of ρ1.19g / mL hydrochloric acid for 15 minutes, take it out, wash it, rinse it with ethanol, and dry it in the air; accurately weigh the weight of the steel sample in m 1 It is 98.3462g, and the glass beaker that fills the prepared 200mL electrolytic solution is put into the electrolytic cell, and the potassium chloride that the mass percentage composition is 8% and the citric acid aqueous solution that the mass percentage composition is 1.5% in this electrolytic solution . Use the weighed steel sample as the anode, and the stainless steel cylinder as the cathode, turn on the silicon rectifier, set the electrolysis cu...

Embodiment 3

[0081] A heavy steel sample with a total niobium content of 0.012% was made into a column with a diameter of 8.mm and a length of 81 mm, and a groove with a depth of 2 mm was dug at a distance of 4 mm from the top. Observation showed that the steel sample had no holes or cracks.

[0082] Soak the steel sample in a measuring cup filled with 30mL water and 30mL hydrochloric acid of ρ1.19g / mL for 20min, take it out, wash it, rinse it with ethanol, and dry it in the air; weigh the steel sample accurately in m 1 It is 93.3815g, and the glass beaker that fills the prepared 250mL electrolytic solution is put into the electrolytic cell, and this electrolytic solution is the citric acid aqueous solution that the mass percentage content is 7% potassium chloride and the mass percentage content is 1%. Use the weighed steel sample as the anode, and the stainless steel cylinder as the cathode, turn on the silicon rectifier, set the electrolysis current to 0.6A, and perform electrolysis at ro...

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Abstract

The invention discloses a method for determining the content of niobium oxide in steel. The method comprises the following steps: soaking a steel sample with water and hydrochloric acid and then cleaning, rinsing with ethanol, drying and weighing to obtain the mass of the sample before electrolysis; taking the steel sample as an anode, taking stainless steel as a cathode, and taking a mixed solution of potassium chloride and citric acid as electrolyte for electrolysis; washing off electrolytic residues on the steel sample, rinsing with ethanol, drying, and weighing to obtain the mass of the steel sample after electrolysis; adding hydrochloric acid, nitric acid and perchloric acid to the electrolytic residues, heating and dissolving to obtain a first test solution; adding hydrochloric acid and tartaric acid to the first test solution, boiling and filtering to obtain a precipitate; adding nitric acid to the precipitate, and adding perchloric acid to obtain a second test solution; adding nitric acid and hydrofluoric acid for dissolution to obtain a third test solution; fixing the volume of the third test solution at 25 mL or 50 mL; taking cesium as an internal standard element, determining the mass of niobium oxide in the third test solution and the mass of niobium oxide in a blank solution by ICP-MS; obtaining the content of niobium oxide in steel according to a formula.

Description

technical field [0001] The invention relates to the technical field of analytical chemistry, in particular to a method for determining the content of niobium oxide in steel. Background technique [0002] As an alloying element in steel, niobium can refine the grains of steel and reduce the overheating sensitivity and temper brittleness of steel. Niobium can improve the welding performance of steel, increase the strength and corrosion resistance of heat-resistant steel, etc. Niobium is similar to vanadium, titanium, zirconium, etc., and has the function of having a good influence on the properties of steel. [0003] Niobium mainly exists in the form of solid solution niobium, carbonitride and niobium oxide in steel, and different forms of niobium have different effects. Niobium has the functions of preventing grain growth, inhibiting recrystallization of deformed austenite and producing significant precipitation effect, so it has been widely used in steel. Niobium is a ver...

Claims

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Application Information

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IPC IPC(8): G01N27/62G01N1/28G01N27/626
Inventor 石琳丁美英白玉臻李锋
Owner INNER MONGOLIA BAOTOU STEEL UNION
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