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失去活性的钯催化剂是以三氧化二铝为主体(97％以上),含有部分碳、二氧化硅以及少量铁、镁等常见元素的混合物,其中含有一定量的钯。催化剂中钯的测定常用化学分析。用光谱法测定此种催化剂中钯含量的报道不多,为此,建立光谱测定方法还是有必要的。一、标样的制备以Al_2O_3为基体,加入一定量的钯标液。在红外灯下烤干,捣细,在石英管内通氢气600℃还原1小时,磨均,配制一高含量标样。然后以Al_2O_3依次稀释配制含钯量0.003％至0.2％的一套标准试样。标样与碳粉以1:1混合。往碳粉中加入Co_2O_3,钴在碳粉中的含量为0.1％,以钴作内标元素。
Inactive palladium catalysts are based on aluminum oxide (97% or more) containing a mixture of carbon, silicon dioxide and small amounts of common elements such as iron and magnesium which contain a certain amount of palladium. Determination of palladium in the catalyst commonly used chemical analysis. There are few reports on the determination of palladium in this catalyst by spectrometry. Therefore, it is still necessary to establish a spectrometric method. First, the standard preparation Al 2 O 3 as the matrix, adding a certain amount of palladium standard solution. Roasted in the infrared light, pound fine, hydrogen in the quartz tube through 600 ℃ reduction 1 hour, grinding average, preparation of a high content of standard samples. Then a series of standard samples containing 0.003% to 0.2% palladium were prepared by sequential dilution with Al 2 O 3. The standard sample and toner are mixed 1: 1. To the toner by adding Co_2O_3, cobalt content in the toner is 0.1%, with cobalt as the internal standard element.