首页> 外国专利> METHOD OF MEASURING MASS CONCENTRATIONS OF NIOBIUM AND TANTALUM IN AIR OF WORKING ZONE BY MASS SPECTROMETRY WITH INDUCTIVELY COUPLED PLASMA

METHOD OF MEASURING MASS CONCENTRATIONS OF NIOBIUM AND TANTALUM IN AIR OF WORKING ZONE BY MASS SPECTROMETRY WITH INDUCTIVELY COUPLED PLASMA

机译:电感耦合等离子体质谱法测定工作区空气中铌和钽的质量浓度。

摘要

FIELD: chemistry.;SUBSTANCE: invention relates to analytical chemistry. Method of measuring mass concentrations of niobium and tantalum in air of a working zone by mass spectrometry with inductively coupled plasma, according to which sampling air of the working area is performed by drawing the analysed air through an analytical aerosol filter, at rate of 2–20 l/min for 30 minutes, recording air temperature and atmospheric pressure at sampling moment, filter is placed in quartz barrel and installed in muffle furnace, held for 1.5–2 hours at temperature of 400–450 °C, 1.0 g of potassium pyrosulphate is added, held at the same temperature until transition into a liquid state, then held for 10 minutes at temperature 800–850 °C, the sample is allowed to cool, 10 ml of 10 % aqueous tartaric acid solution and heating to produce a sand bath until dissolved, the sample is transferred to a volumetric flask and adjusted to the sample volume of deionized water to 100 cm3; 4.95 cm3 of the prepared sample is introduced into a test tube of an automatic sampler of a mass spectrometer, 0.05 cm3 of an internal standard is added with mass concentration of a terbium comparison element of 1000 mcg/dm3 and then, by inductively coupled plasma mass spectrometry, concentration of niobium and tantalum is determined using a calibration curve and taking into account the amount of air withdrawn for analysis to normal conditions.;EFFECT: invention provides the possibility of determining both niobium and tantalum in the working area at a level of from 0_00002 mg/m3 or higher.;1 cl, 10 tbl, 2 dwg
机译:技术领域本发明涉及分析化学。通过电感耦合等离子体质谱法测量工作区空气中铌和钽的质量浓度的方法,根据该方法,工作区的采样空气是通过将分析后的空气通过分析型气溶胶过滤器抽吸而以2 –以20 l / min的速度运行30分钟,记录采样时刻的空气温度和大气压,将过滤器放置在石英桶中,然后安装在马弗炉中,在400-450°C的温度下保持1.5–2小时,焦磷酸钾1.0 g加入,保持在相同温度下直至转变成液态,然后在800-850°C下保持10分钟,然后将样品冷却,10 ml的10%酒石酸水溶液冷却并加热以产生沙子浴直至溶解,将样品转移至容量瓶中,并调节至去离子水样品体积至100 cm 3 ;将4.95 cm 3 制备的样品引入质谱仪自动进样器的试管中,加入0.05 cm 3 内标,质量浓度为comparison比较元素1000 mcg / dm 3 ,然后通过电感耦合等离子体质谱法,使用校准曲线并考虑为分析至正常水平而抽取的空气量,确定铌和钽的浓度效果:本发明提供了以0_00002 mg / m 3 或更高的水平测定工作区域中铌和钽的可能性。1cl,10 tbl,2 dwg

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