The mechanism of the poisoning of ammonia synthesis catalysts by oxygenates O2, CO and H2O: an in situ method for active surface determination

The effect of adding an oxygenated poison (O₂, CO or H₂O) to a hydrogen/nitrogen stream producing ammonia over a triply promoted (K₂O, CaO, Al₂O₃) commercial catalyst is not unsurprisingly rapidly to poison the catalyst. However, immediately the oxygenated poison reacts with the catalyst and before total poisoning has occurred, which in these experiments took 10 min, there was an explosive release of ammonia producing concentrations in the gas phase in excess of the equilibrium value. This is thought to be due to a convulsive reorganisation of the surface of the catalyst in forming regions of an oxide overlayer, resulting in the expulsion of the standing surface nitrogen atom coverage as ammonia. However, in contradistinction to the observation of complete poisoning of the triply promoted catalyst shortly after switching the water (2.9%) into the hydrogen/nitrogen stream, when polycrystalline iron was used as the catalyst, after the initial pulse of ammonia was observed, the small quantity of water (2.9%) in the hydrogen/nitrogen stream resulted in an increased rate ( ×3) of ammonia synthesis which declined only slightly over the twenty minute duration of the experiment. The difference in behaviour between the triply promoted catalyst and the polycrystalline iron is thought to be due to the relative ease of reduction of the latter, so that submonolayer quantities of oxide can be stabilised on the surface of the polycrystalline iron. The promoting effect of this oxide overlayer is either structural or electronic; no distinction can be made from these experiments. The technique of injecting either O₂ or CO into a hydrogen/nitrogen stream which is producing ammonia over promoted catalysts in quantities insufficient to cause complete poisoning and measuring the oxygen coverage of the catalyst to a measured decrease in the ammonia synthesis rate, appears to be a ready, in situ method for the determination of the active catalyst area.     

改进的卡尔费休法滴定装置对葡萄糖酸镁水含量的测定

用带橡皮塞的导管将滴定管的上口与锥形瓶连接构成一个密闭的滴定装置，将此装置应用于卡尔费休法容量法测定水含量，在滴定过程中所有试剂与外界完全隔开，防止了空气中的水蒸气干扰，滴定终点明显。且能长时间稳定（8h以上）。该装置结构简单，操作方便。利用此方法成功测定了葡萄糖酸镁中的水含量，其平均回收率为102．0％。     

Product and process parameters determination for quality and cost

The purpose of this study is to conduct a concurrent product and process parameters determination for further cost reduction and quality enhancement. The process design-related parameters, such as process mean, process tolerance and product design-related parameters, such as product tolerance, are considered simultaneously in the proposed approach. To reflect the response from these three key controllable characteristics: process mean, process tolerance and product tolerance, the key measurement score, which is the sum of the mean cost, tolerance cost, quality loss and failure cost, is used to evaluate the present model. Two examples are provided for demonstrating the application of single and multiple quality characteristics.     

气相色谱法测定3-氯-1-丙醇

以填充柱气相色谱对 3 氯 1 丙醇进行了分析研究 ,方法变异系数 0 .5 % ,回收率99.5 0 %～ 10 0 .6 7%     

国内外活性氧化锌的进展

叙述了活性氧化锌的简史，特点、应用、生产方法的进展，活性的测定方法及标准。     

傅立叶变换红外光谱仪测定压缩空气中油的含量

介绍了傅立叶变换红外光谱仪（FTIR）测定压缩空气中油含量的方法，讨论了应用FTIR的注意问题。     

凯氏定氮法在测试氯乙烯-丙烯腈共聚树脂中丙烯腈含量的应用

介绍了凯氏定氮法在测定氯乙烯-丙烯腈共聚树脂中丙烯腈含量的应用及反应原理,对测试结果的准确性和重复性进行了研究,并与灼烧法进行了比较。实验结果表明:采用凯氏定氮法测定氯乙烯-丙烯腈共聚树脂中丙烯腈的含量是可行的,测定结果准确,重现性较好。     

黄姜皂素样品的测定

以浓H2SO4为显色剂,采用分光光度法测定黄姜中的皂素。对皂素提取条件进行了优化,在最佳条件下测定结果令人满意。     

硝酸磷肥中有效钙的提取与测定

对经特殊工艺试制的硝酸磷肥中总钙进行测定。用中性柠檬酸铵提取、草酸沉淀、高锰酸钾滴定 ,提取率达 88.3 %～ 91.7% ,测定值的标准偏差为 0 .11,回收率为 98.4%～ 10 1.9%。     

甲氧胺盐酸盐的含量测定方法

提出了以酚酞为指示剂，氢氧化钠为滴定剂测定甲氧胺盐酸盐含量的方法。测定了甲氧胺盐酸盐的离解常数Ka，考察了干扰因素对测定的影响。结果表明，干扰物质NH4Cl在样品中的含量小于5％不影响测定。该方法具有简便、快速，准确等特点,测定了数批样品结果较满意。