Digestion method and detection method of Tungsten-base class sample

A sample, tungsten-based technology, applied in the field of digestion and detection of tungsten-based samples, can solve the complex composition of the sample solution matrix, unsolved problems such as the preparation and element detection of tungsten carbide and metal tungsten, and the blockage of carbide particles

Inactive Publication Date: 2011-10-12
PANZHIHUA IRON AND STEEL +1
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

This type of method obviously has many disadvantages: for example, the composition of the digestion system is complex, the matrix composition of the prepared sample solution is complex and the concentration of salts is too high, and the digestion of samples with alkaline reagents such as ammonia water and sodium peroxide is very unsuitable for ICP-AES, Determination requirements for detection instrument methods such as ICP-MS; in particular, organic complexing reagents such as ammonium citrate and tartaric acid used in large quantities are mostly used in traditional chemical analysis methods and are not suitable for instrumental analysis methods, such as se

Method used

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  • Digestion method and detection method of Tungsten-base class sample
  • Digestion method and detection method of Tungsten-base class sample
  • Digestion method and detection method of Tungsten-base class sample

Examples

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Embodiment 1

[0030] Digestion of tungsten samples

[0031] Weigh 0.1000g tungsten powder sample (FWI-I, W>99.9%, produced by Zhuzhou Cemented Carbide Factory) (hereinafter referred to as No. 1 sample) into the microwave digestion inner tank, add appropriate amount of water and rinse the inner wall of the container. Adhered samples; add 4.0mL of concentrated nitric acid and 1.0mL of phosphoric acid; then put on the outer tank, cover the lid and tighten it with a torque wrench to ensure a good seal. Put the sealed outer tank into the microwave digestion furnace according to the operation steps of the instrument, connect the temperature and pressure sensors, and carry out microwave digestion and complexation reaction. In this embodiment, the microwave reaction method of ramping up the temperature is adopted, the pressure is controlled below 800 psi (1 psi=6.895 KPa), and the microwave heating program is set to raise the temperature of the material in the container to 180° C. in 4 minutes and...

Embodiment 2

[0036] The sample to be digested is 0.5000g tungsten powder sample (FWI-I, W > 99.9%, produced by Zhuzhou Cemented Carbide Factory) (hereinafter referred to as No. 2 sample), add 8.0mL concentrated nitric acid and 5.0mL concentrated phosphoric acid, microwave program The setting is: heating up to 200°C in 6 minutes and holding for 20 minutes.

[0037] Besides, the metal tungsten sample was digested according to the same method as in Example 1, and the supernatant was detected by ICP-AES.

Embodiment 3

[0039] The sample to be digested is 0.1000g tungsten carbide sample (FWC-1, WC > 99.8%, hereinafter referred to as sample No. 3), add 4.0mL concentrated nitric acid and 1.0mL concentrated phosphoric acid, and set the microwave program as follows: 5min to heat up to 190°C and Keep warm for 10 minutes. Besides, the tungsten carbide sample was digested and detected by ICP-AES according to the same method as in Example 1.

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Abstract

The invention discloses a digestion method of a Tungsten-base class sample, wherein the digestion method comprises the following steps: weighting and putting the tungsten-base class sample in a container, rinsing the wall of the container with a right amount of water; adding nitric acid and phosphoric acid, and then carrying out sample digestion and complex reaction by virtue of microwaves withinthe closed container; and after microwave processing is finished, cooling and diluting until an appropriate volume is achieved, thereby obtaining a sample solution used for detection. In addition, inductive coupling plasma atomic emission spectrum method and other detection methods are chosen to determine elements.

Description

technical field [0001] The invention relates to the field of detection and analysis of metal or alloy products such as tungsten carbide, metal tungsten, and cemented carbide, etc., with tungsten as the main matrix component. Simultaneously use the inorganic complexing agent phosphoric acid to complex tungsten, so that the tungsten matrix is ​​stably stored in the solution in the form of tungsten without tungstic acid precipitation. The method for preparing sample solutions such as tungsten carbide, metal tungsten or hard alloy, and A method for elemental detection of prepared sample solutions using analytical methods such as inductively coupled plasma atomic emission spectrometry (ICP-AES) Background technique [0002] Metal tungsten and its alloys are one of the most important functional materials in modern industry, national defense and high-tech applications. They are used in many fields such as aerospace, atomic energy, marine automobiles, electronics, petrochemicals, me...

Claims

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Application Information

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IPC IPC(8): G01N1/38G01N1/44G01N27/62
Inventor 成勇袁金红胡金荣肖军彭慧仙
Owner PANZHIHUA IRON AND STEEL
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