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首页> 外文期刊>Glass Science and Technology >Quantification of H_2O contents in silicate glasses using IR spectroscopy - a calibration based on hydrous glasses analyzed by Karl-Fischer titration
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Quantification of H_2O contents in silicate glasses using IR spectroscopy - a calibration based on hydrous glasses analyzed by Karl-Fischer titration

机译：使用红外光谱法对硅酸盐玻璃中的H_2O含量进行定量分析-基于通过卡尔·费休滴定法分析的含水玻璃的校准

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摘要

Water-related IR absorption bands were investigated in hydrous soda-lime-silica glass (SLS) and float glass (FG). Glasses containing between 0.5 and 6 wt% H_2O (corresponding to 0.7 and 8 mol/l) were synthesized in platinum capsules by re-melting glass powder to which water had been added. Synthesis were perfomed in an internally heated gas pressure vessel at temperatures of 1200 to 1250 deg C and pressures 100 to 500 MPa. The total water content (C_water) of glasses was analyzed by poyrolysis and subsequent Karl-Fischer titration. Five bands at 3550, 2850, 1730 and 1635 cm~(-1) in the IR spectrum of an SLS glass containing 4 wt% H_2O were identified as vibration modes of water-related species by comparison with a D_2O-bearing glass. With increasing C_water the absorbance band at 3550 cm~(-1) (OH steretch of weakly H-bonded hydrous species) grows in intensity relative to the band at 2850 cm~(-1) (OH stretch of strongly H-bonded hydrous species). As a consequence, the practical absorption coefficient for the band at 3550 cm~(-1) (epsilon_3550pract, defined by assigning the total water to this band) is 20% lower at 0.1 wt% water than at 4 wt% water. The dependence of epsilon_3550pract on C_water is most pronounced above 0.5 wt% but appears to be present also in water-poor glasses. In contrast, epsilon_2850pract does not noticeably depend on water content (FG: epsilon_2850pract = (40.2(+-)2.4) l centre dot mol~(-1) centre dot cm~(-1); SLS: epsilon_2850pract=(50.8 (+-) 2.0) 1 centre dot mol~(-1) centre dot cm~(-1)) and, hence, it is preferered for water determination in float glass and soda-lime-silica glass. Scholze's two-band method [1] using the peak height of bot bands at 3550 and 2850 cm~(-1) to quantify C_water in glasses is a suitable first approach also for hydrous glasses, predicting the water content within 20% relative. However, for a more precise determination the dependence of the epsilon-values on C_water has to be considered. A preliminary evaluation of the H_2O bending vibration band at 1635 cm~(-1) shows that molecular H_2O is a minor hydrous species in FG and SLS glasses with a maximum concentration of 2.0 wt% in FG glass containing 5.7 wt% total water. On the basis of the new spectroscopic results and data from literature the assignment of the so-called ABC triplet (bands 2850, 2350 and 1750 cm~(-1) cm~(-1)) is discussed.
机译：在含水钠钙硅玻璃（SLS）和浮法玻璃（FG）中研究了与水有关的IR吸收带。通过使添加了水的玻璃粉末重熔，在铂制胶囊中合成了含有0.5〜6重量％的H_2O（相当于0.7〜8 mol / l）的玻璃。在内部加热的气压容器中于1200至1250℃的温度和100至500MPa的压力下进行合成。通过热解和随后的Karl-Fischer滴定分析玻璃的总水含量（C_water）。通过与含D_2O的玻璃进行比较，确定了含有4wt％的H_2O的SLS玻璃的红外光谱中的3550、2850、1730和1635 cm〜（-1）的五个波段为水相关物质的振动模式。随着C_water的增加，相对于2850 cm〜（-1）的吸收带（强H结合的水合物种的OH拉伸），在3550 cm〜（-1）处的吸收带强度（相对于2850 cm〜（-1）的吸收带）强度增加。 ）。结果，在3550 cm〜（-1）处的谱带的实际吸收系数（ε_3550pract，通过将总水分配给该谱带定义）在0.1 wt％的水比在4 wt％的水低20％。超过0.5 wt％的epsilon_3550实践对C_water的依赖性最为明显，但似乎也存在于贫水玻璃中。相反，epsilon_2850pract并不明显依赖于水含量（FG：epsilon_2850pract =（40.2（+-）2.4）l中心点mol〜（-1）中心点cm〜（-1）; SLS：epsilon_2850pract =（50.8（+ -）2.0）1中心点mol〜（-1）中心点cm〜（-1）），因此优选用于浮法玻璃和钠钙硅玻璃中的水测定。 Scholze的两波段方法[1]使用bot波段的峰值高度在3550和2850 cm〜（-1）来量化玻璃中的C_water也是适用于含水玻璃的第一种方法，它预测相对含水量在20％以内。然而，为了更精确地确定，必须考虑ε值对C_water的依赖性。在1635 cm〜（-1）处的H_2O弯曲振动带的初步评估表明，分子H_2O在FG和SLS玻璃中是次要的水合物种，在总水含量为5.7 wt％的FG玻璃中最大浓度为2.0 wt％。根据新的光谱结果和来自文献的数据，讨论了所谓的ABC三重态（2850、2350和1750 cm〜（-1）cm〜（-1）波段）的分配。

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