论文部分内容阅读
锗锰铜中含锗量,有的高达7不左右。这样高的含量,又有大量铜、锰、少量镍、铁等元素共存,其测定在国内未见有报导。苯菊酮法是目前测定微量锗应用最广泛的方法,其灵敏度高,但选择性不好,它能与许多金属离子呈显色反应。我们采用四氯化碳萃取,使锗与大量杂质分离,是较为特效的方法。目前在高含量锗的测定中,存在着萃取率不够高等问题。资料介绍,在萃取过程中,不允许硝酸存在,否则影响结果。我们试以在硝酸存在下,使萃取液中含锗量从微克级增大至毫克级,并对萃取酸度,次数与萃取率的关系作了试验。结果表明:当盐酸酸度《SN时,锗不进入有机相;当酸度李gN时,萃取率达99.50~100终。当萃取液中含有1000~7000拼9 Ge与ssmg Cu,12mg Mn,2.smg Ni,o.smgFe等离子共存时,经二次萃取,可完全回收。同时,对不同悬浮剂存在下的显色酸度,反应速度及稳定性作了比较试验。实验表明,以聚乙烯醇为优。在0.5一INHCI下,25分钟可显色完全,其色泽稳定性能保持18小时基本不变。测得克分子吸光系数为4.19xl少。在测定波长的选择上,我们选取中等灵敏的52Onm波长,而不采用高灵敏的500nm波峰波长,其特点是试剂空白大为降低,量程扩大一倍,即锗的比耳定律浓度扩大一倍,使Ge含量在80傀/looml以内符合比耳定律,减少了稀释手续,适宜于高含量的测定。
Ge germanium manganese content of germanium, some up to 7 or so. Such a high content, there are a large number of copper, manganese, a small amount of nickel, iron and other elements coexist, the determination of no reports in the country. The method of biochin is the most widely used method for the determination of trace germanium. Its sensitivity is high, but its selectivity is not good. It can develop color reaction with many metal ions. We use carbon tetrachloride extraction, the separation of germanium and a large number of impurities, is a more effective method. Currently in the determination of high content of germanium, there is the problem of insufficient extraction rate. Information, in the extraction process, does not allow the presence of nitric acid, or affect the results. In the presence of nitric acid, we try to increase the content of germanium in the extract from microgram to milligram, and the relationship between the extraction acidity, the number of times and the extraction rate has been tested. The results show that germanium does not enter the organic phase when the acidity of hydrochloric acid is “SN”, and when the acidity is Li gN, the extraction rate reaches 99.50-100. When the extract contains 1000 ~ 7000 spell 9 Ge and ssmg Cu, 12mg Mn, 2.smg Ni, o.smgFe plasma coexist, after secondary extraction, can be completely recovered. At the same time, comparative experiments were carried out on the chromogenic acidity, reaction speed and stability in the presence of different suspending agents. Experiments show that polyvinyl alcohol is better. In a 0.5 INHCI, 25 minutes to develop color completely, its color stability can be maintained for 18 hours basically unchanged. Measured molecular extinction coefficient of 4.19xl less. In the determination of the wavelength of choice, we choose the medium sensitive 52Onm wavelength, rather than using the 500nm peak wavelength sensitive, which is characterized by a greatly reduced blank reagent, quantum scale doubled, that is, the law of germanium Beer double the concentration, The Ge content of 80 pup / looml in line with the Beer’s law, reducing the dilution procedures, suitable for high content determination.