Ojima Jun
National Institute of Industrial Health, Kawasaki, Japan.
J Occup Health. 2003 Mar;45(2):94-103. doi: 10.1539/joh.45.94.
Infrared Spectrophotometry (IR) is now widely used to determine crystalline silica in industrial dust samples. Though the IR method has many advantages when dealing with respirable dust samples, some serious analytical errors are often caused by interference minerals contamination. These minerals have a characteristic absorption band corresponding in position to the analytical peak for crystalline silica. In this paper, six typical interference minerals (Kaolinite, Mullite, Muscovite, Pyrophyllite, Montmorillonite and Amorphous silica) were pre-size controlled to respirable range and their infrared spectra were measured by means of an FT-IR with the well-known potassium bromide tablet technique. The effects of these interference minerals on the Japanese OEL or the administrative control level for respirable dust which depend on the silica content were calculated and expressed in figures. The measured absorption coefficients of the interference minerals and quartz were 1.36-6.98 Abs/mg and 24.46 Abs/mg, respectively. The absorption band height ratios of each interference minerals were also measured. Then the efficiency and applicability of two spectrum correction methods for the interference minerals, absorbance ratio method and difference spectrum method were examined by using artificially mixed samples (standard interference mineral + standard quartz). By comparing the quantifying results for the mixture samples, it was revealed that the interfered spectra were almost corrected successfully when using the difference spectrum method, whereas correction by the absorbance ratio method resulted in apparent negative errors. Furthermore, the difference spectrum method was proven to be superior to the absorbance ratio method in applicability.
红外分光光度法(IR)目前广泛应用于测定工业粉尘样品中的结晶二氧化硅。尽管红外法在处理可吸入粉尘样品时有许多优点,但干扰矿物污染常常会导致一些严重的分析误差。这些矿物具有一个特征吸收带,其位置与结晶二氧化硅的分析峰相对应。本文将六种典型的干扰矿物(高岭石、莫来石、白云母、叶蜡石、蒙脱石和无定形二氧化硅)预先控制粒度至可吸入范围,并采用著名的溴化钾压片技术,通过傅里叶变换红外光谱仪测量它们的红外光谱。计算了这些干扰矿物对日本职业接触限值(OEL)或取决于二氧化硅含量的可吸入粉尘管理控制水平的影响,并以图表形式表示。干扰矿物和石英的测量吸收系数分别为1.36 - 6.98 Abs/mg和24.46 Abs/mg。还测量了每种干扰矿物的吸收带高度比。然后,通过使用人工混合样品(标准干扰矿物 + 标准石英),研究了两种干扰矿物光谱校正方法(吸光度比法和差示光谱法)的效率和适用性。通过比较混合样品的定量结果发现,使用差示光谱法时,干扰光谱几乎能成功校正,而吸光度比法校正则导致明显的负误差。此外,差示光谱法在适用性方面被证明优于吸光度比法。