Stefke Barbara, Windeisen Elisabeth, Schwanninger Manfred, Hinterstoisser Barbara
Competence Centre for Wood Composites and Wood Chemistry (Wood K plus), St. Peter Strasse 25, A-4021 Linz, Austria.
Anal Chem. 2008 Feb 15;80(4):1272-9. doi: 10.1021/ac7020823. Epub 2008 Jan 16.
The weight percentage gain (WPG) and the acetyl group content of wood due to acetylation with acetic anhydride have been analyzed by means of Fourier transform infrared spectroscopy (FTIR) and near-infrared spectroscopy (NIR). Band height ratios (BHR) (1240/1030 (1230/1030) and 1745/1030 (1740/1030)) of the bands at 1745 (1740), 1240 (1230), and 1030 cm-1 were calculated from FTIR-KBr and FTIR-ATR (attenuated total reflection) spectra. The good linear correlation with a coefficient of determination of about 0.94 over a range from 0 to 27% WPG existing between BHRs and WPG and acetyl group content, respectively, requires only a few samples to calibrate FTIR. Partial least-squares regression models based on second derivatives of the NIR spectra in the wavenumber range from 6080 to 5760 cm-1 resulted in a R2 value of 0.99, number of PLS components (rank) between 3 and 5, root-mean-square error of cross-validation between 0.6 and 0.79%, and a residual prediction deviation up to 10. Although a wide range of input parameters (i.e., various wood species and different procedures of acetylation) was used, highly satisfactory results were obtained. Both FTIR and NIR spectroscopic means fulfill the need for determining the WPG and the acetyl content of acetylated wood. By reason of its additional potential for on-line process control, the NIR method may even outperform the FTIR method.
通过傅里叶变换红外光谱(FTIR)和近红外光谱(NIR)分析了用乙酸酐乙酰化处理后木材的重量百分比增益(WPG)和乙酰基含量。从FTIR-KBr和FTIR-衰减全反射(ATR)光谱计算了1745(1740)、1240(1230)和1030 cm-1处谱带的谱带高度比(BHR)(1240/1030(1230/1030)和1745/1030(1740/1030))。BHR与WPG以及乙酰基含量之间在0至27%WPG范围内存在良好的线性相关性,决定系数约为0.94,这仅需要少量样品来校准FTIR。基于6080至5760 cm-1波数范围内NIR光谱二阶导数的偏最小二乘回归模型,得到的R2值为0.99,PLS分量数(秩)在3至5之间,交叉验证的均方根误差在0.6至0.79%之间,残差预测偏差高达10。尽管使用了广泛的输入参数(即各种木材种类和不同的乙酰化程序),但仍获得了非常令人满意的结果。FTIR和NIR光谱方法都满足测定乙酰化木材WPG和乙酰含量的需求。由于NIR方法在在线过程控制方面的额外潜力,它甚至可能优于FTIR方法。