石油亚砜树脂分离稀土的性能研究

应用石油亚砜萃取树脂与ＮＨ＿４ＣＮＳ体系，测定了稀土元素的分配比（Ｋｄ）、分离因素（β）和分离度Ｒｓ），讨论了ＮＨ＿４ＣＮＳ的浓度、稀土进样量和温度等对稀土分离的影响。应用于混合稀土的分离和测定，分析了６０．３２％的氧化钇，相对标准偏差为±１．４７％。     

氧化淀粉变性基团的分析方法

介绍了淀粉工业中氧化淀粉变性基团羧基和羰基的测定方法     

ICP-AES法测定叶面肥中硼、铜、铁、锰、钼和锌

研究电感耦合等离子发射光谱仪(ICP AES)测定微量元素叶面肥中硼、铜、铁、锰、钼和锌等6种元素的方法。此法准确可靠、简便快捷,提高了测定叶面肥中微量元素的效率。方法回收率在98.1%~101.6%,相对标准偏差小于1.9%,方法的检出限为0.0005~0.008 m g/L。     

Détermination de constantes cinétiques du craquage catalytique par la modélisation du test de microactivité (MAT)

The microactivity test (MAT) for cracking catalyst test works with an approximately plug flow isothermal reactor. The yields at the outlet of such a reactor is numerically computed in the case of lumped kinetic with large molecular expansion and rapid catalyst deactivation expressed versus poison concentration. The poison (coke in cracking reaction) is considered as a product formed by several reaction routes. The results are applied to catalytic cracking kinetic with a four lump model (feedstock, gasoline, gas, coke). The comparison between experimental and computed yields, permits the adjustment of kinetic constants with a set of experimental results obtained from a laboratory scale reactor derived from the MAT. The simulation of concentration profile in the reactor permits a better understanding of the reaction courses.     

气相色谱-质谱联用法测定金属皂中的多环芳烃

建立了金属皂中16种美国环保局(EPA)优先监控的多环芳烃的气相色谱-质谱(GC/MS)联用测定方法,样品先用二甲基亚砜萃取,再用环己烷进行反萃取,经硅胶柱净化后,用GC/MS分离测定。优化了16种多环芳烃(PAHs)的分离测定条件,结果16种PAHs的平均回收率为75.32%￣98.72%,精密度实验相对标准偏差(RSD)为2.19%￣6.93%,检测限(S/N=5)为0.002￣0.010mg/kg。该方法灵敏度高、准确性好,完全可以满足金属皂中多环芳烃的检测要求。     

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.     

多壁碳纳米管修饰电极测定水样中痕量镉

通过多壁碳纳米管修饰玻碳电极,建立了水样中痕量镉的线性扫描阳极溶出伏安分析法。优化了支持电解质及pH、修饰剂用量、富集电位及时间等测定条件,在pH 4.0的NaAc-HAc缓冲液中,-1.10 V富集5 min后,溶出峰电流与Cd2 浓度在2.0×10-8~5.0×10-5mol/L的范围内呈良好的线性关系,检测限为8.0×10-9mol/L。该法用于实际水样中痕量镉的测定,平均回收率在98.7%~105.0%之间,结果满意。     

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.     

负载硫化镉的碳纳米管载镉量分析

经高温灰化法预处理后用配位滴定分析法测定负载硫化镉的碳纳米管(CdS/CNTS)的载镉量,测试数据可靠准确,表明制备负载硫化镉碳纳米管催化剂时所加入的镉并不全部吸附在碳纳米管上,载镉效率随着碳纳米管载镉量的增加而降低。