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A kind of preparation method of wall-mounted crucible for xrf analysis
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A technology of crucible and platinum crucible, which is applied in the field of preparation of wall-mounted crucibles for XRF analysis, can solve the problems of splashing samples, long time, low amount of boron trioxide, etc. high efficiency effect
Active Publication Date: 2020-10-13
WUHAN UNIV OF SCI & TECH +2
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Problems solved by technology
Although it is possible to increase the proportion of lithium tetraborate by adding boric acid after pre-oxidation, the water vapor released by the decomposition of boric acid under high temperature conditions is likely to cause splashing and loss of samples.
[0004] The problems of the above method are: 1. High energy consumption for making a wall-mounted crucible at high temperature; 2. The labor intensity and long time for preparing a wall-mounted crucible; The amount of diboron trioxide in the layer is low, and the glass sheet for analysis is easy to devitrify and crack; 5. The single preparation efficiency is low
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Embodiment 1
[0028] A method for preparing a wall-mounted crucible for XRF analysis. The steps of the preparation method are:
[0029] Step 1. According to the mass ratio of lithium tetraborate: boric acid: oxalic acid is 2: (4-5): 0.1, the lithium tetraborate, the boric acid and the oxalic acid are uniformly mixed to obtain the wall-hanging flux.
[0030] Step 2: Put 7.50-8.00 g of the wall-mounted flux into a platinum crucible, then move the platinum crucible and the wall-mounted flux into a high-temperature furnace, and keep warm at 700-760°C for 10-20 minutes , to prepare a wall-mounted crucible for XRF analysis.
Embodiment 2
[0032] A method for preparing a wall-mounted crucible for XRF analysis. The steps of the preparation method are:
[0033] Step 1. According to the mass ratio of lithium tetraborate: boric acid: oxalic acid is 2: (3-4): 0.1, the lithium tetraborate, the boric acid and the oxalic acid are uniformly mixed to obtain the wall-hanging flux.
[0034] Step 2: Put 7.00-7.50 g of the wall-mounted flux into a platinum crucible, then move the platinum crucible and the wall-mounted flux into a high-temperature furnace, and keep warm at 760-820°C for 10-20 minutes , to prepare a wall-mounted crucible for XRF analysis.
Embodiment 3
[0036] A method for preparing a wall-mounted crucible for XRF analysis. The steps of the preparation method are:
[0037] Step 1. According to the mass ratio of lithium tetraborate: boric acid: oxalic acid is 2: (2-3): 0.1, the lithium tetraborate, the boric acid and the oxalic acid are uniformly mixed to obtain the wall-hanging flux.
[0038] Step 2: Put 6.50-7.00 g of the wall-mounted flux into a platinum crucible, then move the platinum crucible and the wall-mounted flux into a high-temperature furnace, and keep warm at 820-880°C for 10-20 minutes , to prepare a wall-mounted crucible for XRF analysis.
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Abstract
The invention particularly relates-a production method of a wall hanging crucible for XRF analysis. The method comprises the following steps: uniformly mixing lithium tetraborate, boric acid and oxalic acid according-a mass ratio of 2:(1-5):0.1 to obtain a wall hanging flux; and adding 6.00-8.00 g of the wall hanging flux into a platinum crucible, then transferring the platinum crucible and the wall hanging flux into a high-temperature furnace, and keeping the temperature at 700-930 DEG C for 10-20 min to produce the wall hanging crucible for XRF analysis. The volume of the platinum crucible is 25-40 mL, and the material of the platinum crucible is Pt or a Pt and Au alloy, wherein a mass ratio of Pt to Au in the Pt and Au alloy is 95:5, and the purity of Pt is equal to or more than 99.99 wt%. The method has the characteristics of low energy consumption, small working intensity, high yield, high production efficiency and few crystallization cracks.
Description
technical field [0001] The invention belongs to the technical field of wall-mounted crucibles. Specifically relates to a preparation method of a wall-mounted crucible for XRF analysis. Background technique [0002] At present, when preparing glass slides for XRF analysis, "wall hanging technology" is used to protect platinum or platinum crucibles from corrosion. The so-called "wall hanging technology" is to first melt a certain amount of lithium tetraborate at a temperature higher than 1050 ° C, and rotate the crucible before the melt loses its fluidity, so that the flux adheres to the lower and bottom of the crucible, forming a pair of crucibles. The protective layer. Due to the high melting point of lithium tetraborate, lithium tetraborate will not melt when the sample containing reducing substances is pre-oxidized and melted with lithium carbonate, a flux with a lower melting point. Due to the small contact area between lithium tetraborate and the low-melting-point flu...
Claims
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Application Information
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