Cathodic Stripping Determination of Water in Organic Solvents

A cathodic stripping voltammetry (CSV) method has been developed to determine water content in organic solvents based on electrooxidation of a gold electrode in the presence of water to form gold oxides upon anodic polarizations. Following cathodic potential scan, a sharp reductive stripping peak of gold oxides is generated and the magnitude of the peak current is related to the water content in the organic solvents. The method has been applied for determination of water in four commonly used water miscible organic solvents, acetonitrile, tetrahydrofuran, acetone and glacial acetic acid, with limits of detection of 60, 10, 40 and 10 ppm, respectively.     

卡尔-费休滴定法测定有机锌盐药物中水分

采用卡尔-费休滴定法测定有机锌盐药物中水分时,改用甲醇-氨溶液(质量比180比1)作溶剂溶解试样。改进的溶剂利于有机锌盐药物的溶解及结晶水的释放。试验结果表明:有机锌盐药物中水分的测定值比药典法测定值高,相对标准偏差(n=5)在0.13%～0.36%之间。     

EDTA滴定法测定钢渣中游离氧化镁

以碘-乙醇溶液为催化剂,选择乙二醇作溶剂浸取钢渣中游离氧化镁,采用EDTA滴定法测定其中游离氧化镁的含量。试验中考察了碘-乙醇的最佳用量和K-B混合指示剂的最合适配比。结果表明:催化剂碘-乙醇溶液的添加量达碘与氧化镁的质量比为7.5比1,指示剂中酸性铬蓝K和萘酚绿B的比值为1比1.4时,滴定终点变色明显,滴定结果准确。在钢渣中加入纯氧化镁测定的平均回收率为96.5%,相对标准偏差(n=5)为1.3%。     

自动电位滴定法测定脱硫系统中氯化物

应用自动电位滴定法,在总离子强度缓冲溶液存在的情况下,在pH 5的微酸性水溶液中,用0.05mol·L~(-1)硝酸银标准溶液作为滴定剂,测定了脱硫系统样品中氯化物含量。试样用水浸取溶出氯化物,共存亚硫酸盐的干扰采用在近中性条件下加入过氧化氢煮沸至无小气泡产生予以消除,对试样的预处理方法以及各项影响测定的参数等做了试验并予以优化。方法用于测定脱硫废水、脱硫浆液和脱硫石膏样品中氯化物,加标回收率在95.7%～102.0%之间,相对标准偏差(n=5)在1.2%～5.9%之间。     

恒电位自动滴定法分析脂肪酶水解活性影响因素

利用恒电位自动滴定法分析了脂肪酶(Candida rugosa lipase,CRL)催化橄榄油水解活性的影响因素,确定了适宜的酶活性测定条件,对比了传统表面活性剂和咪唑类离子液体对酶活性的影响.37 ℃时,与酶蛋白浓度呈线性关系的酶活性测定范围为1～14 μmol/min;酶蛋白浓度范围为0.01～0.07 g/L;...     

以尿素为氮源制备氮改性二氧化钛及其改性机理

以钛酸丁酯为前驱体,以尿素为氮源,采用改进溶胶-凝胶法制备了不同N含量的改性TiO2光催化剂(N-TiO2).以重铬酸钾为目标污染物,以甲酸为空穴捕获剂,评价了可见光下该催化剂的催化还原活性.结果表明,N-TiO2催化剂活性明显高于未改性催化剂,当催化剂中N/Ti摩尔比为10%、焙烧温度为400℃时,其光催化还原活性最...     

K_3PO_4-催化的β-硝基苯乙烯衍生物与乙酰胺、NBS的区域专一性氨溴加成反应研究

在无水磷酸钾催化下,以乙酰胺（CH3CONH2）和N-溴代丁二酰亚胺（NBS）为氮源和卤素源,丙酮作溶剂,建立了β-硝基苯乙烯双键上的区域专一性氨溴加成反应新体系.该法在室温下,无需惰性气体保护可高收率的获得邻位氨卤加成产物,最高收率可达79%.实验证明,当β-硝基苯乙烯中苯环4-位具有强供电子基团时（如CH3O）,该...     

Synthesis and Structure Investigation of a Novel 3-Dimensional Potassium Supermolecular Compound Based on 2,4-Dinitro Resorcinol

A novel 3‐dimensional potassium supermolecular compound [K(HDNR)(H₂DNR)(H₂O)]_n (H₂DNR?2,4‐dinitro resorcinol) was synthesized and characterized by elemental analysis and FT‐IR spectroscopy. The crystal structure investigated by X‐ray single crystal diffraction shows that [K(HDNR)(H₂DNR)(H₂O)]_n crystallizes with a monoclinic unit cell in the space group P2(1)/c with unit cell dimensions of a=17.648(5) Å, b=12.527(3) Å, c=7.735(2) Å, β=94.33(2)°, V=1705.00(73) ų, Z=4. The structure was refined to the final R=0.0670 and wR=0.0722 for 2022 observed reflections with I>2σ(I). In the compound, potassium cation is assembled into one‐dimensional chains along c‐axis through oxygen atoms from water molecules, and the chains were connected by the bridged HDNR^? anions to form a two‐dimensional net structure. The two‐dimensional nets constructed a three‐dimensional supramolecular architecture via intermolecular hydrogen bonds and N–O···π interaction. Density functional theory (DFT) B3LYP was employed to optimize the structure and calculate energies for three tautomers of HDNR^? univalent anion. Three stable tautomers were located. It was found that the structure (I) with O(1) losing hydrogen atom is more stable than the structure (II) also with O(1) losing hydrogen atom and the structure (III) with O(4) losing hydrogen atom.     

Comparative phytotoxicity of methylated and inorganic arsenic- and antimony species to Lemna minor, Wolffia arrhiza and Selenastrum capricornutum

The alkylation of metalloids through the transfer of methyl groups is an important factor in the biogeochemical cycling of elements like arsenic and antimony. In the environment, many different organic and inorganic forms of these elements can therefore be found in soils, sediments or organisms. Studies that compare the ecotoxicity of these different chemical species however are rare. Therefore, this study aimed to generate toxicity data on two scarcely studied organic compounds of arsenic and antimony, as well as to compare their toxicity to the inorganic species, which are studied so far to a higher extent, in order to improve the environmental effect assessment of these elements. To this purpose, bioassays were performed in which three different aquatic organisms (the floating water plants Lemna minor and Wolffia arrhiza and the green alga Selenastrum capricornutum) were exposed to a concentration series of 3 different arsenic species (sodium arsenite — As(III), sodium arsenate — As(V), and monomethylarsonous diiodide — MMAs(III)) and three different antimony species (antimony potassium tartrate hydrate — Sb(III), potassium hexahydroxoantimonate — Sb(V), trimethylantimony(V) bromide — TMSb(V). The observed effect concentrations demonstrated that the inorganic (III)- and (V)-valent species of arsenic were clearly more toxic than the corresponding antimony species. The highest overall toxicity has been shown by MMAs(III) followed by the inorganic As(III). The highest toxicity of the three tested antimony species has been observed for TMSb(V). The observed differences in effect levels stress the importance once more that speciation must not be ignored in toxicity studies.     

One-pot preparation of hydroxylated potassium organotrifluoroborates and subsequent Jones oxidation to potassium organocarbonyltrifluoroborates

Alcohol-containing potassium organotrifluoroborates as starting reagents were prepared from their corresponding dibromobenzenes through a sequential one-pot reaction. The oxidation reactions of these substrates, which were carried out using 3.0 equiv of 8 N Jones reagent in acetone at 0 °C, provided a high yield of the desired carbonyl-functionalized compounds. In addition, the cross-coupling reactions of these organocarbonyltrifluoroborates were successfully performed in the presence of 3 mol % of Pd(PPh₃)₄ catalyst at 100 °C.