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
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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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