High strength fiberglass is one of the most widely used special functional fiberglass, with high strength, high temperature resistance, impact resistance, wave transmission, corrosion resistance and other excellent comprehensive properties, mainly used in aerospace, military and other high-end fields. TiO2, Cao, Na2O, Fe2O3, B2O3 and other oxides are usually used as clarifiers and fluxes in order to obtain high-strength fiberglass with excellent performance, so as to reduce the upper limit temperature of crystallization and drawing temperature and the number of bubbles. The introduction of cosolvent and the adjustment of the proportion of the main components of high-strength fiberglass can help to optimize the glass production process, but reduce the mechanical properties of the fiberglass. Therefore, in the production and inspection process of high-strength glass fiber, accurate determination of trace metal elements can provide theoretical basis for evaluating the performance of glass fiber, and provide technical support for the development and process improvement of high-strength glass fiber.
Li Yanling, the fifth and Third Research Institute of China ordnance industry group, used hydrofluoric acid, perchloric acid and hydrochloric acid to dissolve the samples in two stages, and established an ICP-OES Method for the simultaneous determination of nine metal elements in high-strength fiberglass powder. The method is simple, rapid, accurate and reliable. It is suitable for the simultaneous determination of various metal elements in high-strength fiberglass.
Main instruments and reagents
ICP-OES instrument: icap6300 type, Thermo Fisher Scientific Co., Ltd;
Electric heating plate: C – MAG HP7, IKA, Germany;
Perchloric acid, hydrofluoric acid, hydrochloric acid: superior grade, Sinopharm Group Chemical Reagent Co., Ltd;
Standard material for composition analysis of borosilicate glass: gbw03132, national building materials testing center;
Single element standard solution of aluminum, magnesium, calcium, iron, titanium, cerium, sodium and potassium: the mass concentration is 1000 μ g / ml, with the numbers of GBW (E) 080981, GBW (E) 080976, GBW (E) 08977, GBW (E) 081004, GBW (E) 08098, GBW (E) 081018, GBW (E) 080973, GBW (E) 080974, Jinan Zhongbiao Technology Co., Ltd;
Lithium single element standard solution: 1000 μ g / ml, GBW (E) 080512, Beijing Institute of chemical metallurgy, nuclear industry;
High strength fiberglass powder sample: No.53 Research Institute of China ordnance industry group;
The experimental water is high-purity water with a resistivity of not less than 18 m Ω· cm.
Instrument operating conditions
RF power: 1100 W; sample volume: 1.5 ml / min; atomized gas: argon (purity: 99.99%), flow rate: 0.7 L / min; auxiliary gas: argon (purity: 99.99%), flow rate: 0.85 L / min; stabilization time: 5 s; sample lifting time: 30 s (flushing pipeline); atomizer cleaning time: 5 s; repeated measurement times: 3 times; see Table 1 for each element analysis line.
Sample pretreatment
Weigh 0.15 g high-strength glass fiber powder into platinum crucible, add a small amount of water to wet it, then add 5 ml hydrofluoric acid and 4 ml perchloric acid in turn, heat it on electric heating plate at low temperature (about 100 ℃), after all silica is converted into SiF4 and evaporated completely, heat it to 300 ℃, continue heating until white perchloric acid smoke is exhausted, remove superfluous hydrofluoric acid, and cool it. Add 5 ml hydrochloric acid and 10 ml water, heat until the sample is completely dissolved, transfer the dissolved clear solution to a 100 ml volumetric flask, fix the volume with water to the mark line, shake well, it is the original sample solution. The blank solution was prepared by the same method. Take another 2 ml of the original sample solution and put it into a 50 ml volumetric flask, add 2.0 ml hydrochloric acid, dilute it with water and dilute it to the standard line, shake it well, that is, dilute the sample solution. The original sample solution is used for the determination of metal elements with the content no more than 1%; the diluted sample solution is used for the determination of metal elements with the content between 1% and 30%.
Test results
Hydrofluoric acid, perchloric acid and hydrochloric acid were used to dissolve the samples in two stages, and the content of each element was determined by ICP-AES under the selected analytical lines. There is a good linear relationship between the nine metal elements and the spectral intensity in their respective mass concentration range. The correlation coefficient is more than 0.999, and the detection limit is 8.0-17.4 μ g / g. The relative standard deviation was less than 1.8% (n = 6), and the recovery was 97.6% - 103.7%. The method is accurate, simple and rapid, and can be used for the simultaneous determination of polymetallic elements in high-strength glass fiber.
Excerpted from Volume 29, issue 2, chemical analysis and metrology, 2020
Reference materials | analysis and test | sample processing | measurement technology | summary
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