A method for measuring the content of trace metal elements in pan-based carbon fibers
A technology of metal element content and metal element, applied in the direction of material excitation analysis, thermal excitation analysis, etc., can solve the problems of inability to completely separate metal elements from carbon fiber matrix, difficult operation of ashing, errors, etc.
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Embodiment 1
[0079] 1. Instruments and reagents
[0080] Analytical balance, division value 0.1mg; platinum crucible, purity 99.99%, about 50g; vacuum oven, vacuum degree -0.1MPa, temperature -200℃ controllable; ashing furnace, heating range 30℃~1200℃; pure water Machine, which can stably prepare ultrapure water with a resistivity of 18.2MΩ·cm; pipette gun, with a range of 0-1.0ml; graduated pipette, with a range of 1.00ml and 5.00ml; volumetric flask, with a glass capacity of 25ml Bottle, 50ml plastic volumetric bottle.
[0081] Ultrapure water, resistivity 18.2MΩ·cm (GB / T6682-92); nitric acid, 65-68wt%, analytically pure; hydrofluoric acid, 40wt%, analytically pure; hydrochloric acid, 35-38wt%, analytically pure.
[0082] 2. Standard solution
[0083] Prepare a single-element standard stock solution and dilute it in a 50ml volumetric flask:
[0084] The concentration of Na element standard solution is: 10ppm, 12ppm, 14ppm;
[0085] The concentration of K element standard solution is:...
Embodiment 2
[0103] Adopt the instrument and reagent of embodiment 1 to detect the content of sodium, iron, calcium and magnesium metal element in the PAN-based carbon fiber sample:
[0104] The conditions for the ashing treatment of each element are shown in Table 2.
[0105] Table 2
[0106] element Na Fe Ca Mg Ashing temperature (℃) 630 680 625 625 Constant temperature time (hours) 6.5 8.5 6 7.5
[0107] Volatile silicon: Add 1ml HF and 2ml HNO dropwise with a pipette 3 Mix the acid to fully dissolve the ash and infiltrate it several times along the crucible wall, then place it on the induction cooker to evaporate to dryness. Second silicon evaporation: After the first silicon evaporation is completed, the pipette gun extracts 2ml of HF to dissolve the ash again, soaks the crucible wall, and evaporates to dry again on the induction cooker. To prevent the solution from splashing out when evaporating to dryness, generally choose a heating voltage...
Embodiment 3
[0120] According to the ashing time and temperature shown in Table 5, the ashing step is carried out to the content of micro trace metal elements in the PAN-based carbon fiber sample, which is the same as in Example 1 with the steps:
[0121] table 5
[0122] element Na Fe Ca Mg Ashing temperature (℃) 650 690 638 615 Constant temperature time (hours) 6.5 9 5.8 7.2
[0123] Volatile silicon: Add 1ml HF and 2ml HNO dropwise with a pipette 3 Mix the acid to fully dissolve the ash and infiltrate it several times along the crucible wall, then place it on the induction cooker to evaporate to dryness. Second silicon evaporation: After the first silicon evaporation is completed, the pipette gun extracts 2ml of HF to dissolve the ash again, soaks the crucible wall, and evaporates to dry again on the induction cooker. To prevent the solution from splashing out when evaporating to dryness, generally choose a heating voltage of 140V, and reduce th...
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