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Correction method of hydrogen determination instrument

A calibration method and instrument technology, applied in the direction of weighing by removing certain components, can solve problems such as low accuracy, high price, poor accuracy of standard sample determination, etc., to achieve high accuracy and fast volatilization speed , to avoid the effect of excessive error

Active Publication Date: 2020-11-03
武汉钢铁有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Even so, some hydrogen standard samples purchased from the market still have problems such as large uncertainty, low accuracy and high price.
In addition, if the standard sample is used to calibrate the analytical instrument, the uncertainty of the standard sample will be transmitted into the test data of the sample, which will adversely affect the accuracy of the sample analysis results.
It can be seen from this that the hydrogen standard samples purchased from the market have problems such as large uncertainty, poor calibration accuracy of the standard samples, and the content range of the standard samples cannot meet the actual analysis requirements.

Method used

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  • Correction method of hydrogen determination instrument
  • Correction method of hydrogen determination instrument
  • Correction method of hydrogen determination instrument

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] 1. Heat the reference oxalic acid in an oven at 105°C to remove moisture and place it in a desiccator for use.

[0059] 2. Accurately weigh 0.4500g of reference oxalic acid, dissolve it with diethyl ether (analytical grade) and dilute it to a 100mL volumetric flask to obtain a 0.45% oxalic acid ether solution for use; divide 10mL of 0.45% oxalic acid ether solution into a 100mL volumetric flask, dilute To the scale, dubbed 0.045% ether oxalate solution;

[0060] 3. Accurately weigh 0.5000g of high-purity iron powder (Fe content >99.999%) and place it in a graphite crucible, and input the mass of high-purity iron powder into an infrared hydrogen determination instrument.

[0061] 4. Use a micropipette to accurately pipette 100 μL of the above ether oxalate solution and place it in a graphite crucible filled with pure iron. After the ether is completely volatilized, put the graphite crucible into an infrared hydrogen determination instrument for detection.

[0062] Table...

Embodiment 2

[0066] 1. Heat the reference oxalic acid in an oven at 105°C to remove moisture and place it in a desiccator for use.

[0067] 2. Accurately weigh 0.4500g of reference oxalic acid, dissolve it with diethyl ether (analytical grade) and dilute it to a 100mL volumetric flask to obtain a 0.45% oxalic acid ether solution for use; divide 5mL of 0.45% oxalic acid ether solution into a 100mL volumetric flask, dilute To the scale, make 0.0225% ether oxalate solution;

[0068] 3. Accurately weigh 0.5000g of high-purity iron powder (Fe content >99.999%) and place it in a graphite crucible, and input the mass of high-purity iron powder into an infrared hydrogen determination instrument.

[0069] 4. Use a micropipette to accurately pipette 100 μL of the above ether oxalate solution and place it in a graphite crucible filled with pure iron. After the ether is completely volatilized, put the graphite crucible into an infrared hydrogen determination instrument for detection.

[0070] Table 2...

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Abstract

The invention discloses a correction method of a hydrogen determination instrument, which comprises the following steps: dissolving anhydrous oxalic acid with the mass of M1 in a volatile solvent to obtain an oxalic acid-containing solution; presetting the mass of a to-be-detected sample to be M2, transferring the oxalic acid-containing solution into a sample container, and after the volatile solvent in the oxalic acid-containing solution is completely volatilized, obtaining the actually measured hydrogen content of the to-be-detected sample through a hydrogen determination instrument; obtaining the theoretical hydrogen content of the sample to be detected according to the M1 and the M2; and carrying out deviation correction on the hydrogen determination instrument according to the theoretical hydrogen content and the actually measured hydrogen content of the to-be-detected sample. According to the invention, oxalic acid is used as a standard substance to correct a hydrogen determination instrument, oxalic acid is slightly dissolved in a volatile solvent, the volatilization speed is high, the determination is not interfered, and a solution mode is adopted to add samples to avoid overlarge weighing error of the balance when a very small amount of samples are weighed; and the measurement standard deviation of the content of 2.0 ppm is less than 0.0993 ppm.

Description

technical field [0001] The invention relates to the field of hydrogen element detection in steel materials, in particular to a calibration method for a hydrogen determination instrument. Background technique [0002] At present, the hydrogen content in iron and steel, non-ferrous metals (aluminum, titanium, copper, etc.) is determined by inert gas fusion-thermal conduction or infrared method. The infrared method detects the content of hydrogen in steel. The principle is: the analysis sample is placed It is heated and melted in a graphite crucible in the presence of an inert gas flow, and the temperature of the pulse furnace for heating the graphite crucible can be as high as 2500 °C. The hydrogen in the sample to be measured is represented by H 2 The form is released, and the rare earth copper oxide is oxidized to H 2 After O, it is detected by an infrared detector. [0003] Calibrate the instrument with a standard sample before analyzing the sample. Due to the easy diff...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N5/04
CPCG01N5/04
Inventor 齐郁杨琳杨国义
Owner 武汉钢铁有限公司