1,5-二叠氮基-3-硝基-3-氮杂戊烷溶解度参数的估算与测定

采用基团贡献法估算了1,5-二叠氮基-3-硝基-3-氮杂戊烷(DIANP)的溶解度参数。用浊度滴定法测定了其溶解度参数。研究了DIANP在不同溶剂中的溶解性。结果表明,基团贡献法的估算值与浊度滴定法的测定值相吻合。测得DIANP的溶解度参数为22.29 (J/mL) 1/2。DIANP在不同溶剂中的溶解性符合“溶解度参数相近相溶”原则。     

烟火药剂中硫磺含量测定方法的研究

确定了烟火药剂中硫磺含量的测定方法,将烟火药剂洗去有机粘合剂后,用稀盐酸充分溶解、过滤,用浓硝酸将硫磺氧化成硫酸,加入过量的钡离子,然后用EDTA容量法测定过量的钡离子,进而得到硫磺含量.试验表明,本文提出的方法回收率在98.22%～99.79%.     

卡尔-费休滴定法测定奥柳氮锌中的水分

以甲醇-氨溶液为溶剂,采用卡尔-费休滴定法快速测定新药奥柳氮锌中的水分,水分平均含量为10．89%,RSD=0．30%。该法适用于类似有机金属药物和精细石油化工产品中水分的测定。     

非银汞试剂密闭消解-电位滴定检测废水中COD

建立了非银汞复合试剂+硫磷混酸+重铬酸钾+大体积密封瓶消解样品,进行电位滴定批量测定COD的方法。自制了消解/滴定一体瓶与相应的消解器,非银汞复合试剂加量0.5 g(由硫酸锰/硫酸铜/硫酸铝钾/硫酸铬钾(质量比)=3∶2∶1∶1),0.1 mol/L K₂Cr₂O₇加量10 mL,体积比为3∶1的硫磷混酸15 mL,水样加量10 mL,(160±5)℃温度下密封消解20 min,消解液直接由黄金电极电位滴定。实验结果表明:50 mg/L水平的实际样品COD,RSD≤4.78%,与HJ 828—2017的结果相对误差≤5.80%,应用于石化废水和其他水质分析,效果满意。     

BOTA型氰化物浓度在线分析仪的升级及工业应用

氰化物浓度是氰化浸金工艺的重要参数,通过氰化物浓度在线检测控制可以有效减少氰化物消耗。介绍了BOTA型氰化物浓度在线分析仪的技术升级,由光度滴定替代电位滴定,提高了仪器测量性能及可靠性。升级后的BOTA-Ⅱ型氰化物浓度在线分析仪在排山楼金矿进行了工业应用,在氰化钠和某低氰药剂的浸出流程中均能实现氰化物浓度的在线测量,测量精度及可靠性满足要求,为企业带来了显著的经济效益。     

Solubilisation of calcium and magnesium from the marine red algae Lithothamnion calcareum

Marine minerals are a potential source of calcium and magnesium for nutritional supplementation. This study analysed the solubilisation of calcium and magnesium from the skeletal remains of Lithothamnion calcareum. Scanning electron microscopy analysis demonstrated a nonporous microstructure. Spectrophotometric determination showed that the calcium and magnesium contents were 30.01 and 6.22% (w/w), respectively. Solubilisation of calcium and magnesium was highly pH dependent. The temperature‐dependent solubilisation of calcium fitted the shrinking core model. The apparent activation energy for calcium solubilisation was 28.6 kJ mol^?1. Inclusion of caseinophosphopeptides (CPPs), casein‐derived mineral binding peptides, during the solubilisation of calcium and magnesium appeared to decrease the extent of calcium solubilisation at pH 6.0 and 8.0. The results herein have implications for the choice of optimal pH conditions for the sustained release of calcium and magnesium from marine mineral sources.     

Detailed Insight into the Interaction of Bicyclic Somatostatin Analogue with Cu(II) Ions

Somatostatin analogues are useful pharmaceuticals in peptide receptor radionuclide therapy. In previous studies, we analyzed a new bicyclic somatostatin analogue (BCS) in connection with Cu(II) ions. Two characteristic sites were present in the peptide chain: the receptor- and the metal-binding site. We have already shown that this ligand can form very stable imidazole complexes with the metal ion. In this work, our aim was to characterize the intramolecular interaction that occurs in the peptide molecule. Therefore, we analyzed the coordination abilities of two cyclic ligands, i.e., P1 only with the metal binding site and P2 with both sites, but without the disulfide bond. Furthermore, we used magnetic circular dichroism (MCD) spectroscopy to better understand the coordination process. We applied this method to analyze spectra of P1, P2, and BCS, which we have described previously. Additionally, we analyzed the MCD spectra of P3 ligand, which has only the receptor binding site in its structure. We have unequivocally shown that the presence of the Phe-Trp-Lys-Thr motif and the disulfide bond significantly increases the metal binding efficiency.     

A Critical Role for the Presence of Lignocellulosic Material in the Determination of Wood Buffering Capacity

The currently used determinations of wood buffering capacity, which are based on pH-metric titrations of aqueous wood extracts, neglect the effect of lignocellulosic material and the role of its insoluble constituents. This study examined the influence of the presence of wood in a system subjected to titration. A comparison of the results obtained from pine chip extracts and chip suspensions showed that the presence of wood and the wood-to-water ratio were critical factors that affected the measurement of the wood buffering capacity. The evidence showed that the resulting determination may vary by up to six times (0.28–1.99 ml/g), depending upon the conditions of the titration. In addition, it was found that the presence of wood had a neutralizing effect over the course of prolonged pH observations.     

重铬酸盐法测定水质化学需氧量

在水样中加入已知量的重铬酸钾溶液,并在强酸介质下,经沸腾回流后,以试亚铁灵为指示剂,用硫酸亚铁铵滴定水样中未被还原的重铬酸钾,由消耗的硫酸亚铁铵的量换算成消耗氧的质量浓度。     

Fe_2O_3含量对MnZn铁氧体中Fe~(2+)量、磁性能及导电机制的影响

通过测量MnZn铁氧体的磁性能及Fe2+、Mn3+含量,考察了MnZn铁氧体中的Fe2+含量与配方中Fe2O3、MnO含量的关系及其对MnZn铁氧体磁性能的影响,并探究了MnZn铁氧体的导电机制。结果表明:随着(Fe2O3)a(MnO)b(ZnO)c主组成配方中a值递增(52.55≤a≤53.35)、b值递减(38.33≥b≥37.52),呈现出Fe2+、Mn3+含量均增加的趋势。随着Fe2+含量增加,Pcv谷底温度向低温方向移动,Pcv(min)先减后增,Pcv(20/70/100℃)均先减后增,均在Fe2+含量=1.55%附近达到最小值;起始磁导率μi(20/70/100℃)均先增后减。根据Pcv-Fe2+含量和μi-Fe2+含量两个关系图在Fe2O3=53.15mol%附近出现极值点这一现象,初步推测铁氧体Znα2+Mnβ-x2+Mnx3+Fey2+Feχ-y3+O4+σ(0.1794≥α≥0.1786,0.754≥β≥0.734,0.0031≤x≤0.0040,0.051≤y≤0.070)的导电机制为:y0.064时小极化子间的束缚能主导,y0.064时电子跃迁主导。