Use of mobile phase 18-crown-6 to improve peak resolution between mono- and divalent metal and amine cations in ion chromatography

It is difficult to quantify NH4+ by ion chromatography in the presence of high concentrations of Na+ due to peak overlap. The Dionex IonPac CS15 column, which contains phosphonate, carboxylate, and 18-crown-6 functional groups, was originally developed to overcome this problem. We have found that the addition of 18-crown-6 to the eluent promotes improved peak resolution between Na+ and NH4+ even at concentrations as high as 60,000 to 1 using this column. Its use also improves the separation of alkali and alkaline earth metal and amine cations. Mobile phase 18-crown-6 increased the retention times of CH3NH3+, NH4+, and K+, and decreased the retention time of Sr2+. The retention times of Li+, Na+, Mg2+, Ca2+, (CH3)2NH2+, and (CH3)3NH+ were not affected. This method makes possible the direct analysis of ammonia from nitrogenase, the enzyme responsible for biological nitrogen fixation. The resolution of the NH4+ peak from the Na+ and Mg2+ peaks improved from zero resolution to values of 6.19 and 5.65, respectively. This technique considerably reduces the analysis time of NH4+ in the presence of high concentrations of Mg2+ and Na+ over traditional indophenol measurements.     

Surface properties of the binary mixed systems of alkylpyridinium halides and sodium alkylsulfonates

Surface properties of the binary mixed systems of decyl- and dodecylpyridinium chloride or bromide and sodium pentyl- and heptylsulfonate have been investigated. The surface tension of solutions of equimolar mixtures of surfactants and individual surfactants was measured, and the composition of mixed monolayers and surface interaction parameter β were calculated with the regular solution theory. Our results indicate that the properties of mixed films depend on both ionic strength and the kind of added inorganic electrolyte. With the increase of inorganic electrolyte concentration, the content of more surface active ions in the adsorption films enhances and is the highest in the presence of NaI and the smallest when solutions contain NaCl. Mutual interactions in mixed adsorbed films were found to be attractive. However, the strength of interaction weakens with the increase of ionic strength and depends on the kind of inorganic ions in the order: Cl⁻>Br⁻>I⁻.     

Sodium “stuffed” Ba2−xSrxFe4O8 ferrites: new cationic conductors

Sodium insertion in the tetrahedral layer structure of the ferrites Ba_2−xSr_xFe₄O₈ was performed by solid state reaction at 1220 K in air. Superstoichiometric oxides with the actual formula (Ba_2−xSr_x)_1−y/4Na_yFe₄O₈—y0.56; 0.60Ba/Sr1.67—were characterized by X-ray and neutron powder diffraction. The hexagonal unit-cell volume shows an increasing dependence on the sodium insertion when the Ba/Sr ratio reaches the largest values. The marked expansion of the c parameter is the likely signature of the location of the inserted sodium cations within the interlayer space. One-half of the sodium cations partly sits on the Sr(Ba) sites in octahedral coordination and the other half occupies extra octahedral and tetrahedral sites. ac conductivity measurements point to a cationic conductivity whose thermally activated regime—E_a 0.7 eV—evidenced from 570 K, is unsensitive to the sodium content. The bottleneck of the 2D sodium mobility regards the crossing of the oxygen triangular faces shared by the different polyhedra within the interlayer space.     

双水相萃取法分离铍(Ⅱ)、铁(Ⅲ)与铁(Ⅱ)、铬(Ⅲ)、锰(Ⅱ)、铝(Ⅲ)

研究了在聚乙二醇2000(PEG)-硫酸钠(Na2SO4)-邻苯二酚紫(PV)体系中铍(Ⅱ)、铁(Ⅲ)、铁(Ⅱ)、铝(Ⅲ)、铬(Ⅲ)、锰(Ⅱ)的萃取行为。试验结果表明,铍(Ⅱ)在pH 3.5-7.0及铁(Ⅲ)在pH 4.0-7.0范围内可以被PEG相几乎完全萃取,而铝(Ⅲ)、铬(Ⅲ)在pH 1.0-7.0、锰(Ⅱ)在pH 1.0-4.5、铁(Ⅱ)在pH 1.0-4.5则不被萃取。从而实现了将铍(Ⅱ)(pH 3.5)、铁(Ⅲ)(pH 5.0)与铝(Ⅲ)、铬(Ⅲ)、锰(Ⅱ)、铁(Ⅱ)混合离子的定量分离。同时探讨了PEG相的萃取机理。     

甲基紫共振瑞利散射光谱法测定透明质酸钠

在pH5的乙酸盐缓冲介质中,甲基紫与透明质酸钠作用形成结合产物时将导致溶液共振瑞利散射(RRS)大大增强并产生新的RRS光谱,其最大散射峰位于341 nm处。透明质酸钠在0~2.5 mg.L-1范围内其浓度与RRS强度成正比。该法具有高灵敏度,对透明质酸钠的检出限(3σ)为20.1μg.L-1,选择性较好。此法用于测定从鸡冠组织中提取的透明质酸的粗品,测定结果的平均相对标准偏差为2.3%,加标平均回收率为98.9%。     

聚全氟乙丙膜电子束引发预辐射接枝AA和SSS制备阳离子交换膜的研究

利用电子束引发预辐射接枝技术,在聚全氟乙丙烯(FEP)薄膜上接枝丙烯酸(AA)和对苯乙烯磺酸钠(SSS),制备一种含羧酸基团和磺酸基团的阳离子交换膜,详细研究了反应温度、单体总浓度、pH值变化、辐照气氛及添加剂对接枝率的影响规律,明确了实验条件与接枝率的对应关系。FTIR测试证明了接枝产物是全氟乙丙烯和丙烯酸、对苯乙烯磺酸钠的接枝共聚物。     

二苯胺磺酸钠共振光散射法测定牛尿中白蛋白的研究

研究了以二苯胺磺酸钠为共振光散射探针测定牛尿中牛血清白蛋白的分析方法.该方法基于在pH=3.0的Britton-Robinson缓冲溶液中,牛血清白蛋白(BSA)与二苯胺磺酸钠结合后有强烈的共振光散射作用,在λ=469 nm处,共振光散射强度最大且光散射的强度与BSA的浓度成正比.方法简便、快速、灵敏度高,对BSA的检出限为0.18 mg/L,线性范围为0.20～16 mg/L,相关系数r=0.996.该法用于牛尿样品的分析测定,结果满意.     

离子色谱法测定芳香族聚酰胺纤维中硫、钠、钾、钙、镁

应用离子色谱法(IC)测定芳香族聚酰胺纤维中硫、钠、钾、镁及钙。测定阴离子时,试样置于铂坩埚中用艾斯卡试剂覆盖,置于马弗炉中,450℃灼烧1 h使有机物碳化,取出,稍冷,再加少许艾斯卡试剂,升温至850℃灼烧1．5 h,使有机物完全分解。坩埚中的熔块经冷却后用去离子水浸出,用18 mmol·L-1碳酸钠及17 mmol·L-1碳酸氢钠混合溶液定容后,用IC法的阴离子方式测定。用IC法测定阳离子时,试样置于铂坩埚中,不必加艾斯卡试剂,置于马弗炉直接灼烧至有机物完全分解。残渣用1 mol·L-1硝酸或1 mol·L-1盐酸超声波处理,用去离子水洗涤坩埚并定容至100 mL,按所测得峰面积值从标准曲线查得其含量。用此方法测定SO42-,Na+,K+,Mg2+及 Ca2+的检出限依次为0．02,0．25,0．25,0．70及0．80 mg·L-1。     

NaF薄膜的脉冲激光沉积法制备与结构研究

 采用脉冲激光沉积(PLD)方法在Si(100)衬底上制备了NaF薄膜。在激光重复频率2 Hz,能量密度3 J/cm²,本底真空度5×10^-5 Pa的条件下,研究衬底温度对薄膜沉积速率及结构的影响。台阶仪分析表明：薄膜的沉积速率随衬底温度增加呈指数函数增加,算出NaF薄膜的反应激活能为48.67 kJ/mol。原子力显微镜分析表明：薄膜致密而光滑,均方根粗糙度为0.553 nm。扫描电镜截面微观形貌分析表明：薄膜呈现柱状结构。X射线衍射分析表明：NaF薄膜为面心立方晶体结构,并具有显著的择优取向;当衬底温度约为400 ℃时,平均晶粒尺寸最大(129.6 nm),晶格微应变最小(0.225%)。     

木质素磺酸盐的分离提纯

以粗木质素磺酸钠为原料, 采用树脂法、超滤法、长链胺法和溶剂萃取法对其进行了提纯. 红外光谱、元素分析、凝胶渗透色谱等测试结果表明, 溶剂萃取法不能达到提纯目的; 树脂法、超滤法、长链胺法可除去相对分子量小于1000的杂质, 粗木质素磺酸钠经提纯后木质素磺酸钠的质量分数从59.0%提高到90%左右, 且提纯产品的重均分子量和数均分子量均增大, 分子量分布更均一. 从产品收率、提纯效果及提纯工艺等3方面分析表明, 长链胺法除糖效果最好, 提纯后糖含量下降了50%; 超滤法的收率最高, 可达31%, 且其提纯产品的重均分子量较高, 达到12000, 比粗木钠提高了1倍以上.