Method for determining dosage of fluxing agent for measuring sulfur element in sample by infrared absorption method

A determination method and technology of flux, which are applied in measuring devices, material analysis by optical means, instruments, etc., can solve the problems of high measurement cost and doubling bad effect of flux, so as to improve the accuracy and precision and reduce the measurement cost effect

Pending Publication Date: 2021-06-22
AVIC BEIJING INST OF AERONAUTICAL MATERIALS
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It solves the problems of the existing technology such as th

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  • Method for determining dosage of fluxing agent for measuring sulfur element in sample by infrared absorption method
  • Method for determining dosage of fluxing agent for measuring sulfur element in sample by infrared absorption method
  • Method for determining dosage of fluxing agent for measuring sulfur element in sample by infrared absorption method

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Embodiment 1

[0044] Experimental design scheme: multiple groups of samples of uniform quality are provided. Theoretically speaking, the sulfur content in each group of samples is the same, and different masses of co-solvents are added to each group of samples. The carbon-sulfur analyzer is used to pass through In the process of measuring sulfur by infrared absorption method, the measured value of sulfur is analyzed separately, and it can be seen that with the continuous increase of flux quality, the measured value of sulfur continues to increase.

[0045] For example, to measure the standard material nickel-based superalloy GBW 01641, the standard value of sulfur is S=0.0046%, and the fixed mass is 0.500 grams. With the continuous increase of the amount of multi-element flux, the measured values ​​of sulfur were analyzed separately by using a carbon-sulfur analyzer, as shown in Table 2.

[0046] Table 2 Flux quality-sulfur measurement value-sulfur growth rate table for nickel-based superal...

Embodiment 2

[0073] Measure single crystal superalloy DD6 and quantitatively judge the appropriate dosage of tungsten-tin-iron flux.

[0074] (1) Fixedly weigh the quality of single crystal superalloy DD6, 0.350 grams, and place it in a bottomed crucible;

[0075] (2) Take by weighing the tungsten-tin-iron flux quality as table 4, add in the single crystal superalloy DD6 of 0.350 gram;

[0076] (3) The carbon and sulfur analyzer uses the enhanced sensitivity mode to measure the sulfur measurement value, which is listed in Table 4;

[0077] (4) Taking flux quality 0.10 g as an interval, calculate the sulfur growth rate at each point, and list it in Table 4;

[0078] Table 4 Flux quality-measured value of sulfur-sulfur growth rate table for single crystal superalloy DD6

[0079]

[0080] In table 4, the maximum point of sulfur growth rate (0.90 grams) is the maximum release of sulfur in the sample, the first point after the maximum point, that is, 1.00 grams after adding 0.10 grams of f...

Embodiment 3

[0083] Quantitative judgment of silicon steel and tungsten-tin flux suitable dosage.

[0084] (1) Fixedly weigh the quality of silicon steel, 0.250 grams;

[0085] (2) Take by weighing the tungsten-tin flux quality of table 5, add in the silicon steel of 0.250 gram;

[0086] (3) Use the carbon-sulfur analyzer to record the sulfur measurement value, which is listed in Table 5;

[0087] (4) Taking flux quality 0.10 g as an interval, calculate the sulfur growth rate at each point, and list it in Table 5;

[0088] Table 5 Silicon steel flux quality-measured value of sulfur-sulfur growth rate table

[0089]

[0090]

[0091] In table 5, the maximum point of sulfur growth rate (1.20 grams) is the maximum release of sulfur in the sample, the first point after the maximum point, that is, 1.30 grams after adding 0.10 grams of flux, to ensure that the sulfur in the sample is fully released come out. At the same time, add 0.10 grams of flux, even if the increase of sulfur relea...

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Abstract

The invention belongs to an elemental analysis technology, and particularly relates to a flux dosage determination method for measuring a sulfur element in a sample by an infrared absorption method. If the usage amount of the fluxing agent is too large, the measurement result is slightly higher than the actual value, and the measurement cost is also increased. When the usage amount of the fluxing agent is too small, the measurement result is slightly lower than the actual value. The method comprises the following steps: weighing fluxing agents according to a fixed interval by setting incremental mass, respectively covering each sample with the fluxing agents, calculating to obtain a sulfur growth rate under the (n + 1) th fluxing agent measurement point corresponding to fluxing agent measurement points under each fluxing agent mass, and taking the fluxing agent mass corresponding to the maximum sulfur growth rate as a basic fluxing agent dosage; on the basis of the basic flux dosage, an incremental mass is added as a proper flux dosage. By means of the method, the appropriate flux dosage can be judged, it can be guaranteed that sulfur is completely released, the influence of blank in the flux can be reduced to the maximum extent, the measurement accuracy and precision are improved, and the measurement cost is reduced.

Description

technical field [0001] The invention belongs to elemental analysis technology, and in particular relates to a method for determining the amount of flux used for measuring sulfur in a sample by infrared absorption method. The method can quantitatively judge the flux in the process of measuring sulfur element by using high-frequency induction heating infrared absorption method Appropriate dosage. Background technique [0002] The basic principle of measuring sulfur element by high frequency induction heating infrared absorption method: [0003] Sulfur-containing samples (solids) are melted and burned in an oxygen-rich environment in a high-frequency furnace, where sulfur combines with oxygen to form sulfur dioxide [0004] S+O 2 =SO 2 [0005] Gaseous sulfur dioxide leaves the sample, is released, and enters the detection system. The entire analysis process is usually run automatically by the carbon-sulfur analyzer, and finally the sulfur measurement is output in percent ...

Claims

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Application Information

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IPC IPC(8): G01N21/3563
CPCG01N21/3563
Inventor 韦建环汪磊蒙益林张佩佩颜京
Owner AVIC BEIJING INST OF AERONAUTICAL MATERIALS
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