Combined method for measuring content of impurity elements and matrix element niobium in niobium-iron alloy

An impurity element and ferroniobium alloy technology, applied in material excitation analysis, thermal excitation analysis, etc., can solve the problems of long inspection process, complicated operation, secondary pollution, etc., and achieve good accuracy and reliability, convenient operation and low cost Effect

Active Publication Date: 2014-07-16
PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, in the prior art, niobium and tantalum are mainly determined by paper chromatography gravimetric method, silicon by gravimetric method, phosphorus by molybdenum blue photometric method, titanium by chromotropic acid photometric method, tungsten by thiocyanate photometric method, EDTA Volumetric determination of aluminum, etc., that is, the determination of the above-mentioned 12 impurity elements and matrix elements one by one with 12 different chemical analysis methods, the operation is complicated, the inspection process is long, the consumption of chemical reagents and human resources is large, the inspection cost is high, and harmful chemical The use of reagents affects the health of operators and causes secondary pollution to the environment
In particular, the chemical analysis method is inefficient, and consumes a lot of personnel and time. Each of the 12 elements needs to be measured one by one using 12 analysis methods. It usually takes 3-5 hours to measure each impurity element, and it takes about 48 hours to measure niobium. use of hazardous chemicals

Method used

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  • Combined method for measuring content of impurity elements and matrix element niobium in niobium-iron alloy
  • Combined method for measuring content of impurity elements and matrix element niobium in niobium-iron alloy
  • Combined method for measuring content of impurity elements and matrix element niobium in niobium-iron alloy

Examples

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example 1

[0044] In the example of the present invention, the ICP-OES is an iCAP6300 Inductively Coupled Plasma Atomic Emission Spectrometer from Thermo Fisher Corporation of the United States.

[0045] 1. Digestion and preparation of ferroniobium test samples and standard samples

[0046] Weigh 0.1g of ferroniobium sample or standard sample into a polytetrafluoroethylene beaker, rinse the cup wall and disperse the sample without adding water, directly add 2mL hydrofluoric acid drop by drop to rinse the cup wall and ensure that the sample is completely soaked in hydrofluoric acid, at room temperature React under ambient conditions until the solution has no bubbles, add 3mL of concentrated nitric acid, immediately add 2mL of hydrogen peroxide when a large amount of nitrogen oxide brown smoke such as nitrogen dioxide is produced in the reaction, continue to react at room temperature until the sample is completely digested, dilute with water to volume In a 100mL plastic volumetric flask, m...

example 2

[0054] Except for the following differences, all the others adopt the same method as Example 1 to measure the ferroniobium sample of Example 2: 0.3g of ferroniobium sample is weighed, 3mL of hydrofluoric acid consumption, 8mL of concentrated nitric acid consumption, 3mL of hydrogen peroxide consumption . The working parameters of the ICP spectrometer are RF power 1700W, peristaltic pump speed 80r / min, and atomizing gas pressure 0.40MPa. When measuring niobium for the second time, dilute the sample solution to be tested and 8 mixed standard solutions at a ratio of 20 times, that is, take 5.0mL of the sample solution to be tested and the mixed standard solution in a 100mL plastic volumetric flask and dilute with water to determine Allow. The carbon content in sample 2 is about 3.5%.

example 3

[0056] Except for the following differences, all the others adopt the same method as Example 1 to measure the ferroniobium sample of Example 3: the ferroniobium sample is weighed 0.15g, the amount of hydrofluoric acid is 2.5mL, the amount of concentrated nitric acid is 6mL, and the amount of hydrogen peroxide is 2.5mL. The working parameters of the ICP spectrometer are RF power 1600W, peristaltic pump speed 75r / min, atomizing gas pressure 0.38MPa. For the second determination of niobium, divide 8.0mL of the sample solution to be tested and the mixed standard solution into a 100mL plastic volumetric flask and dilute with water to volume. The carbon content in sample 3 is 0.07%.

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Abstract

The invention provides a combined method for measuring the content of impurity elements and a matrix element niobium in a niobium-iron alloy. The method comprises the following steps: digesting a sample at room temperature by concentrated hydrofluoric acid, concentrated nitric acid and concentrated hydrogen peroxide, thereby forming a to-be-measured solution; and respectively preparing series standard solutions comprising impurity elements and a niobium element, detecting the standard solutions by inductively coupled plasma atomic emission spectrometry, drawing an impurity element calibration curve and a niobium element calibration curve, measuring the to-be-measured solution by the inductively coupled plasma atomic emission spectrometry, and combining the measurement result with the calibration curves to obtain the content of the impurity elements and the niobium element in the niobium-iron alloy sample. The method has the advantages that the content of the impurity elements such as silicon, tantalum, tungsten, titanium, aluminum, copper, phosphorus, manganese, lead, tin and vanadium and the content of the matrix element niobium in the niobium-iron alloy can be simultaneously measured; the method is high in accuracy and reliability and has the characteristics of convenience in operation, rapidness, environment friendliness, low cost and the like.

Description

technical field [0001] The invention belongs to the field of detection and analysis of ferroniobium alloys, in particular, it relates to a joint determination of impurity elements (including silicon, tantalum, tungsten, titanium, aluminum, copper, phosphorus, manganese, lead, tin, vanadium, etc.) and matrix in ferroniobium alloys. Method for elemental niobium content. Background technique [0002] Generally speaking, ferroniobium is a precious alloy material with a wide range of applications. Ferroniobium is an important alloy additive in the iron and steel industry. Adding niobium is beneficial to improve the plasticity and corrosion resistance of stainless steel and heat-resistant steel. Adding niobium to structural steel can improve welding performance and increase strength, plasticity and prevent welds. Corrosion, adding niobium to high-temperature steel, tool steel and high-temperature alloys can improve the high-temperature strength, creep resistance and toughness of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/71G01N21/73
Inventor 成勇
Owner PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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