稀土铈（Ⅳ）离子和钼酸钠在盐酸溶液中对冷轧钢的缓蚀协同效应

用失重法和电化学法研究了盐酸介质中，稀土铈(Ⅳ)离子和钼酸钠对冷轧钢的缓蚀协同效应．研究结果表明，钼酸钠和稀土Ce^4 对冷轧钢都有一定的缓蚀作用，但最大缓蚀率不超过42％．通过吸附模型的讨论发现，在Langmuir吸附模型的基础上进行校正后的模型能更合理地解释实验结果，并求出了三个吸附参数(△H^-，ΔG^-，△S^-)．通过对比实验，发现稀土铈(Ⅳ)离子和钼酸钠对冷轧钢产生了明显的缓蚀协同效应，最大缓蚀率可达90％左右。     

稀土Ce~(4+)和香兰素在H_3PO_4介质中对钢的缓蚀协同效应

采用失重法、电化学法和紫外-可见吸收光谱研究了3.0mol/LH3PO4介质中,稀土Ce4+和香兰素(4-羟基-3-甲氧基-苯甲醛)对冷轧钢的缓蚀协同效应。结果表明,香兰素对冷轧钢有中等程度的缓蚀作用,缓蚀率随其浓度的增加而增大,最大缓蚀率为66%,在钢表面的吸附符合Freundlich吸附模型;稀土Ce4+对冷轧钢的缓蚀作用较差,最大缓蚀率仅为20%左右。稀土Ce4+和香兰素复配后对冷轧钢产生了明显的缓蚀协同效应,最大缓蚀率可达90%。稀土Ce4+和香兰素在H3PO4介质中复配后形成了新的配合物,为混合抑制型缓蚀剂。     

阴/阳离子型表面活性剂对A3碳钢缓蚀的协同效应

采用电化学方法、静态失重法和观察法研究了阳离子双子表面活性剂(12-2-12)和阴离子表面活性剂十二烷基苯磺酸钠(SDBS)及其复合体系在1M HCl溶液中对A3碳钢的缓蚀性能。研究结果表明:二者具有很好的离子协同效应,在较低浓度下即具有很好的缓蚀效果,属于阴极/阳极混合型抑制剂,当二者复合摩尔比为1:0.8时,协同效应最佳,缓蚀率达到99.9%。通过实验所得数据对其缓蚀机理进行推导,结果表明其缓蚀机理符合Langmuir吸附模型。     

CO_2体系中咪唑啉季铵盐与十二烷基磺酸钠之间的缓蚀协同效应

采用失重法、电化学阻抗谱(EIS)、极化曲线、X射线光电子能谱仪(XPS)及扫描电子显微镜(SEM)研究了CO2饱和的3.5%NaCl腐蚀介质中,咪唑啉季铵盐(IAS)与十二烷基磺酸钠(SDSH)对Q235钢的缓蚀协同效应.结果表明,IAS与低浓度SDSH在腐蚀介质中具有较好的缓蚀协同效应,且当二者以1:1(50 mg·L-1:50 mg·L-1)的浓度比例复配时,协同效应最明显,缓蚀率为88.5%;而IAS与高浓度SDSH间会产生拮抗效应.本文通过建立合理的吸附模型,阐述了协同效应及拮抗效应的机理.SDSH与IAS在Q235钢表面的吸附过程均为放热的自发过程,前者符合Frumkin吸附模型,后者符合Temkin吸附模型.单独使用较高浓度的SDSH对Q235钢也有较好的缓蚀作用,缓蚀率接近90%.     

十二烷基二甲基苄基氯化铵与KI对钢在柠檬酸中的缓蚀协同效应

采用静态失重法、动电位极化曲线、电化学阻抗谱(EIS)、扫描电子显微镜(SEM)首次研究了阳离子表面活性剂十二烷基二甲基苄基氯化铵(1227)对冷轧钢在1.0 mol/L柠檬酸(H₃C₆H₅O₇)溶液中的缓蚀性能,并研究其与碘化钾(KI)复配后缓蚀协同效应和作用机制。结果表明：单独1227或KI均能一定程度抑制冷轧钢在柠檬酸中的腐蚀,100 mg/L 1227与200 mg/L KI复配后最大缓蚀率高达95.3%。缓蚀协同效应系数(s)高于1,表明两者复配后存在协同效应。1227、KI及1227/KI的吸附行为均符合Langmuir吸附等温方程式。1227与KI协同后的吸附平衡常数进一步增大,标准吸附Gibbs自由能(ΔG^?)降低;极化曲线表明1227、KI、1227/KI同时对阴阳两极反应产生抑制作用,为“几何覆盖”模型的混合抑制型缓蚀剂。Nyquist图呈两个时间常数的高频区弥散容抗弧和低频区的小感抗弧,1227与KI复配后的电荷转移电阻进一步增大,缓蚀性能进一步增强;SE...     

苯骈三氮唑与碘化钾对冷轧钢在三氯乙酸中的缓蚀协同效应

采用失重法、电化学阻抗谱(EIS)、动电位极化曲线和扫描电子显微镜(SEM)研究了苯骈三氮唑(BTA)与碘化钾(KI)对冷轧钢在0.10 mol·L^-1三氯乙酸(Cl₃CCOOH)中缓蚀协同效应。结果表明：BTA与KI复配后较BTA、KI对冷轧钢在0.10 mol·L^-1 Cl₃CCOOH中缓蚀效果明显提升,最大缓蚀率达87.5%,且缓蚀协同效应参数大于1,BTA与KI存在缓蚀协同效应。BTA与KI复配前后在钢表面的吸附规律符合Langmuir吸附等温式,BTA/KI复配后具有更大的吸附平衡常数和更负的吸附Gibbs自由能改变值;Nyquist图谱主要包含高频区的容抗弧和低频区的感抗弧,且BTA与KI复配后电荷转移电阻进一步增大。BTA、KI、BTA/KI均为以阴极抑制为主的混合型缓蚀剂,且BTA/KI复配后腐蚀电流密度较复配前显著下降,证实了BTA与KI存在缓蚀协同作用;SEM微观形貌分析得出,BTA与KI复配后能显著减缓三氯乙酸对钢表面的腐蚀程度。     

螯合吸附材料ASA-PGMA/SiO2对稀土离子的吸附性能研究

采用静态吸附法研究了ASA-PGMA/SiO2对稀土离子的螯合吸附性能、吸附动力学和热力学。实验结果表明,其对稀土离子的吸附能力分别为:La3+:38.6 mg.g-1,Pr3+:39.6 mg.g-1,Nd3+:41.8 mg.g-1,Sm3+:42.8 mg.g-1,Tb3+:46.2 mg.g-1。吸附等温模型符合Lang-muir型单分子层吸附。介质pH值对材料的吸附能力有很大影响,pH值为6时吸附量最大。以盐酸为洗脱剂,当酸度为0.1 mol.L-1时,洗脱率为99.8%。连续吸附-脱附实验表明,ASA-PGMA/SiO2重复使用10次后,吸附能力变化很小。     

新型吸附剂偏磷酸铈对铀酰的吸附性能研究

研究新型吸附剂偏磷酸铈对铀酰离子的吸附行为。分别考察了溶液的pH值、温度、接触时间和铀酰离子初始浓度对偏磷酸铈吸附铀酰离子的影响;通过动力学、热力学以及吸附等温线初步研究了吸附机理;最后探究了共存离子和富里酸对吸附的影响。当溶液的pH值为5、温度为30℃、接触时间为60min、铀酰初始浓度为10~(-3)mol/L时为最佳吸附条件,最大吸附量可达到261.78mg/g;动力学研究表明,偏磷酸铈对铀酰离子吸附行为符合准二级动力学方程;Langmuir吸附等温线模型可以更准确的描述铀酰离子在偏磷酸铈上的吸附过程,说明此吸附过程为单分子层吸附;热力学研究表明,偏磷酸铈对铀酰离子的吸附属于吸热反应,反应自发进行,高温促进吸附行为。     

两种席夫碱缓蚀剂对碳钢材料的缓蚀性能探究

采用了电化学方法研究了2种席夫碱缓蚀剂水杨醛基邻苯甲酸亚胺(SB-I)和N,N’-二水杨醛基-1,2-邻苯二亚胺(SB-II)在1 mol/L盐酸溶液中对20#碳钢的缓蚀性能。通过极化曲线和交流阻抗谱研究该席夫碱对碳钢的缓蚀效果表明:席夫碱对碳钢材料具有良好的缓蚀作用,其最大缓蚀率可达到83%。研究了席夫碱在碳钢表面的吸附模式,结果表明,席夫碱在碳钢表面上的吸附吉布斯自由能在-30 kJ/mol之间,表现为混合型缓蚀剂,即通过化学吸附和物理吸附之间的一种混合吸附在碳钢工作电极的表面,通过抑制、阻止延缓金属的电化学过程而起到缓蚀的作用。另外,实验还发现,SB-I比SB-II具有更好的缓蚀性能,该实验结果与理论计算结果相符合。     

2-氨基嘧啶在盐酸介质中对钢的缓蚀性能

用失重法、动电位极化曲线和电化学阻抗谱（EIS）研究了2-氨基嘧啶(2-AP)在1.0~5.0 mol/L HCl溶液中（20~50 ℃）对冷轧钢的缓蚀作用。 结果表明,2-AP对冷轧钢在1.0 mol/L HCl中具有良好的缓蚀作用,且在钢表面的吸附符合校正的Langmuir吸附模型;缓蚀率随缓蚀剂浓度的增加而增大,但随温度的升高和HCl浓度的增加而降低。 2-AP为混合抑制型缓蚀剂;EIS谱呈半圆容抗弧,电荷转移电阻随缓蚀剂浓度的增加而增大。     

Osmotic and activity coefficients of aqueous bile salt solutions at 25, 37, and 45°C

Osmotic coefficients measured by vapor pressure osmometry are reported for aqueous bile salt solutions at 25, 37, and 45°C. Solute activities decrease rapidly with increasing concentration due to premicellar association and micelle formation. In all cases, activities of the dihydroxy bile salts are lower than those of the trihydroxy bile salts. Osmotic coefficients and activity coefficients increase with increasing temperature. It is suggested that hydrophobic forces contribute substantially to the stability of primary bile salt aggregates and micelles.     

胆酸盐在酸性介质中自聚集作用的共振瑞利散射光谱及其分析应用研究

研究了牛磺胆酸钠、甘牛胆酸钠、胆酸钠和脱氧胆酸钠等四种胆酸盐在酸性介质中的聚集作用对共振瑞利散射光谱的影响及其分析应用. 结果表明: 在一定浓度的HCl, H₂SO₄或HNO₃溶液中, 四种胆酸盐均能自聚集形成粒径增大的聚集体. 该聚集体能导致溶液RRS显著增强, 并产生了新的RRS光谱. 不同胆酸盐在同种介质中的反应产物具有相似的光谱特征, 最大RRS波长分别位于349 (HNO₃介质), 359 (H₂SO₄介质)和369 nm (HCl介质). 在一定范围内, 胆酸盐的浓度与散射强度(ΔI_RRS)成正比. 对于不同的体系其检出限在12.0～21.8 ng/mL之间. 方法灵敏度高, 选择性较好, 而且十分简便快速. 可用于市售蛇胆川贝液和血清样品中胆酸盐的测定.     

Facile Stabilization of the Sodium Metal Anode with Additives: Unexpected Key Role of Sodium Polysulfide and Adverse Effect of Sodium Nitrate

Sodium metal is an attractive anode for next‐generation energy storage systems owing to its high specific capacity, low cost, and high abundance. Nevertheless, uncontrolled Na dendrite growth caused by the formation of unstable solid electrolyte interphase (SEI) leads to poor cycling performance and severe safety concerns. Sodium polysulfide (Na₂S₆) alone is revealed to serve as a positive additive or pre‐passivation agent in ether electrolyte to improve the long‐term stability and reversibility of the Na anode, while Na₂S₆‐NaNO₃ as co‐additive has an adverse effect, contrary to the prior findings in the lithium anode system. A superior cycling behavior of Na anode is first demonstrated at a current density up to 10 mA cm^?2 and a capacity up to 5 mAh cm^?2 over 100 cycles. As a proof of concept, a high‐capacity Na‐S battery was prepared by pre‐passivating the Na anode with Na₂S₆. This study gives insights into understanding the differences between Li and Na systems.     

30%亚硫酸氢钠溶液样品中Cl~-和SO_4~(2-)的同时测定

建立了采用离子色谱测定 30%亚硫酸氢钠溶液样品中的氯化钠和硫酸钠含量的新方法。采用IonPacAS14分析柱,选择三乙醇胺为亚硫酸氢钠的稳定剂,以丙酮为有机改进剂,淋洗液组成为 1 5mol/LNa2CO3 3 5mol/LNaHCO3 10% (体积分数) (CH3 )2CO,流速为 1 0mL/min,抑制电导检测。实验结果表明,氯离子、硫酸根离子分别在 0.05~1.5mg/L,0.20~15mg/L时,其峰面积与质量浓度呈线性关系,相关系数均大于 0.999,检出限分别为0 01mg/L和 0 03mg/L。该法用于实际样品分析,操作便捷,结果可靠。     

Mechanism of glass ampoule breakage prevention during the freeze-drying process of sodium thiopental lyophilization products on addition of sodium chloride

Glass ampoule breakage during the freeze-drying process was prevented by the addition of sodium chloride to the formulation of lyophilization products of sodium thiopental. In order to clarify the ampoule breakage prevention mechanism, the physicochemical behavior of the freeze-drying process was monitored by simultaneous XRD-DSC measurements and thermal mechanical analysis (TMA). During the freezing process of formulated solution, the smaller heat of fusion of crystallized ice with the addition of sodium chloride was observed in comparison to that without sodium chloride. Although a greater amorphous portion remained, a higher crystal habit of hexagonal ice was reproducibly observed in the XRD patterns with the addition of sodium chloride during the freezing process. In the measurement of TMA, the scattering of the thermal expansion rate of formulated solution was significantly reduced by the addition of sodium chloride. These observations indicated that the addition of sodium chloride minimized the scattering of the thermal expansion rate and might be a cause for the inhibition of glass ampoule breakage during the freeze-drying process.     

Studies on the Effects of Salt and Surfactant in Wet Phase Separation of Polysulfone

This study investigates the effect of additives in the nonsolvent water in terms of cloud point during the phase inversion of Polysulfone (PS) in dimethyl formamide (DMF). The exponential pattern is observed with PS concentration (0.2 to 0.6% (w/w)). It needs a low amount of water to get the cloud point at low temperature. The cloud point varied with the nature of water matrix and depended on the amount of salt, as well as the PS amount. The presence of salts (sodium chloride and sodium sulfate) lowers the cloud point of the solution. The network distribution of the particles at the cloud point is disturbed in the presence of salt. The requirement is more for Sodium lauryl sulfate (SLS) added water to reach the cloud point in the low range of PS solution up to 0.3% PS (w/w). The morphological and distribution pattern of PS particles are very different compared to PS particles produced from pure water. XRD study of PS particles produced from the mixed water system reflects relatively more amorphous character with respect to PS particles from pure water. The presence of both surfactant and salts in water systems also influences the cloud point in synergistic manner.     

Crystal Structure of a New Form of Sodium Octoborate β-Na2B8O13

Single crystals of a new form of sodium octoborate, β-Na₂B₈O₁₃, were obtained fortuitously from a complex Na₂O-B₂O₃-P₂O₅ mixture, and studied. The compound is monoclinic, space group P2₁/c; the unit cell parameters are a=11.731(4) Å, b=7.880(3) Å, c=10.410(4) Å, β=99.883(3)°; Z=4. The crystal structure was solved from 1653 reflections until R₁=0.0444; it consists of two infinite, independent, and interleaved boron-oxygen networks containing a complex borate anion (B₈O₁₃)²⁻ formed by six BO₃ triangles (Δ) and two BO₄ tetrahedra (T), which can be viewed as a B₅O₁₀ group linked to a B₃O₇ group; this leads to a Fundamental Building Block (FBB) with the shorthand notation: 8: ∞³ [(5:4Δ+T)+(3:2Δ+T)]. This FBB is identical to that described in other octoborates such as α-Na₂B₈O₁₃ and Ag₂B₈O₁₃. However, some subtle differences exist in the interlinking of the octoborate anions found in these three compounds, which explains their different structure and unit cell parameters.     

自动电位滴定法测定工业碳酸钠中氯化钠含量

采用自动电位滴定法,用硝酸银标准溶液作为滴定剂,测定工业碳酸钠中氯化钠含量。方法检出限为0.13mg/L,不同含量氯化钠样品加标回收率为99.7%~100.3%,相对标准偏差(n=5)为0.17%~2.0%,方法简单、快速,精密度和准确度高,适合大批量快速分析样品。     

毛细管电泳法测定注射用头孢哌酮钠他唑巴坦钠中目标成分

建立了毛细管区带电泳法同时测定注射用头孢哌酮钠他唑巴坦钠中目标成分含量的方法。采用石英毛细管(75 cm×75 μm i.d.,有效长度63 cm),以40 mmol/L硼砂溶液为背景电解质(BGE),以氢氯噻嗪为内标,分离电压12.0 kV,检测波长220 nm,重力进样10 s(高度10 cm)。实验结果表明,头孢哌酮钠与他唑巴坦钠分别在0.25～3.96 g/L和0.062～0.99 g/L范围内呈良好的线性关系,相关系数(r)分别为0.9995和0.9996。精密度和重复性均良好,相对峰面积的相对标准偏差(RSD)均小于3%,制剂在208 min内稳定,回收试验结果符合方法学要求。该方法简单、准确、耗费少、污染小,可用于注射用粉针剂头孢哌酮钠他唑巴坦钠中头孢哌酮钠和他唑巴坦钠的定量分析。     

复合硝基酚钠盐的胶束电动力学毛细管色谱分析

本文在自行研制的高效毛细管电泳仪上建立了复合硝基酚钠盐的胶束电动力学毛细管色谱分析方法。用５０ｍｍｏｌ／Ｌ十二烷基硫酸钠、ｐＨ＝９．０的硼酸盐缓冲溶液，在２０ｋＶ电压下分离了５－硝基愈创木酚钠、对硝基酚钠、邻硝基酚钠，此法用于Ａｔｏｎｉｋ型植物生长调节剂的定量分析，相对偏差小于２％，回收率在１０１％￣１０５％之间。