An NMR study of methanol diffusion in polymer electrolyte fuel cell membranes

Methanol diffusion in two polymer electrolyte membranes, Nafion 117 and BPSH 40 (a 40% disulfonated wholly aromatic polyarylene ether sulfone), was measured using a modified pulsed field gradient NMR method. This method allowed for the diffusion coefficient of methanol within the membrane to be determined while immersed in a methanol solution of known concentration. A second set of gradient pulses suppressed the signal from the solvent in solution, thus allowing the methanol within the membrane to be monitored unambiguously. Over a methanol concentration range of 0.5–8 M, methanol diffusion coefficients in Nafion 117 were found to increase from 2.9 × 10⁻⁶ to 4.0 × 10⁻⁶ cm² s⁻¹. For BPSH 40, the diffusion coefficient dropped significantly over the same concentration range, from 7.7 × 10⁻⁶ to 2.5 × 10⁻⁶cm² s⁻¹. The difference in diffusion behavior is largely related to the amount of solvent sorbed by the membranes. Increasing the methanol concentration results in an increase in solvent uptake for Nafion 117, while BPSH 40 actually excludes the solvent at higher concentrations. In contrast, diffusion of methanol measured via permeability measurements (assuming a partition coefficient of 1) was lower (1.3 × 10⁻⁶ and 6.4 × 10⁻⁷ cm² s⁻¹ for Nafion 117 and BPSH 40 respectively) and showed no concentration dependence. The differences observed between the two techniques are related to the length scale over which diffusion is monitored and the partition coefficient, or solubility, of methanol in the membranes as a function of concentration. For the permeability measurements, this length is equal to the thickness of the membrane (178 and 132 μm for Nafion 117 and BPSH 40 respectively) whereas the NMR method observes diffusion over a length of approximately 4–8 μm. Regardless of the measurement technique, BPSH 40 is a greater barrier to methanol permeability at high methanol concentrations.     

Fluorometric detection with a packed flow cell in micro high-performance liquid chromatography

Summary A packed flow cell was used for fluorometric detection in micro high-performance liquid chromatography. The flow cell consisted of fused-silica tubing packed with the same material as the separation column. A focusing effect of the stationary phase on the signal intensity was observed, leading to an improvement of the mass detection limit, as achieved by on-column detection.     

Electroorganic synthesis of benzathine

Benzathine is prepared in good yields from cyanobenzene by a combination of electrochemical hydrogenation and Kolbe electrolysis using nickel and platinum electrodes in the presence of methanolic sodium methoxide in an undivided cell.     

TiO2／Ti／TiO2半导体隔片光电化学电池的性能

研究了半导体隔片光电化学电池(SC-SEP)中光池溶液的pH、暗池溶液的氧化还原电对以及两池中的暗电极对电池的开路电压、光生电压、短路光电流和光伏安特性的影响。对它们的影响机制进行了初步分析。通过合理选择电池体系,SC-SEP的性能可比单隔室的光电化学电池(PEC)优越。     

ICP-MS法快速测定丙烯腈/乙腈中的铁、铜

采用带八级杆碰撞/反应池(ORS)的电感耦合等离子体质谱法(ICP-MS),直接测定丙烯腈或乙腈产品中的Fe、Cu,标准加入法定量.结果表明,方法的线性范围宽,线性相关系数均大于0.999.2种元素的相对标准偏差均低于5%,加标回收率在90%~110%.该方法简便、快速、准确.     

STUDIES ON PREPARATION OF INACTIVATED VACCINES FROM CELL CULTURES OF MINK ENTERITIS VIRUS (MEV) AND THEIR IMMUNITY

In this paper, superhigh reproductive rate strains of MEV with titre more than HA8192* or TCID50 log9.7 10 have been achieved both by cultivation in cell lines with different susceptibility to MEV and by isolating and identifying in field by the author. The systematic tests proved that S18 and L12 strains of MEV are the best strains for vaccine preparation. In this study, the best means for the tissue cultivation of MEV and the most advanced technological process for the production and detection of serum-free cell-cultured MEV fluids with super-high HA titre in batches in large quantities have been established for the first time. Optimum conditions for MEV inactivation were determined, and safe and effective inactivated vaccines with mineral oil or A1(OH)3 gel adjuvant were successfully prepared with serum-free cell-cultured MEV fluids. Both vaccines with different adjuvants can be manufactured in batches in large quantities and have been widely used all over China since 1986. The change laws of the imm     

The effect of capillary column diameter on the performance of thermal conductivity detectors

The concentration sensitivity of a thermal conductivity detector (TCD) depends, among other factors, on the amount of sample mixture in the detector's sensing cell. Since the cell volume has to be appropriately matched with column diameter, it makes the concentration sensitivity of a TCD dependent on column diameter and, therefore, on the speed of gas chromatography. Through reduction of column diameter, higher speed tends to lead to a reduction in the concentration sensitivity of the cell. The factor which the most directly affects the concentration sensitivity of a TCD cell is the heat power conducted through the cell. The higher the power, the greater the sensitivity. The limit of detection of a TCD depends on the concentration-sensitivity of its cell and on the level of statistical errors in the measurement. The errors increase with increasing analysis speed. As the column diameter is reduced, the errors cause additional worsening (on top of the decrease in concentration sensitivity) of the detection limit, dynamic range, and other performance characteristics of the TCD.     

A SAPO-11 Silicoaluminophosphate Molecular Sieve with Stable Crystal Structure

A SAPO-11 silicoaluminophosphate molecular sieve with stable crystal structure was synthesized for the first time. After removing template by calcination, its crystal space group still retains Icm2 which the as-synthesized has. The catalyst deriving from the present SAPO-I 1 materials shows higher isomerization selectivity and higher paraffin hydroisomerization yield than those reported elsewhere.     

应用单细胞微凝胶电泳技术研究氯化镉对人血淋巴细胞DNA的损伤效应

详细介绍了单细胞微凝胶电泳（ＳＣＧ）技术的原理和操作过程，并应用该技术研究了氯化镉（ＣｄＣｌ２）对人血淋巴细胞ＤＮＡ的损伤效应，结果表明，ＣｄＣｌ２能引起细胞ＤＮＡ迁移长度增加，且呈显著的剂量效应关系，对未处理对照细胞的ＤＮＡ迁移的原因及ＳＣＧ实验操作过程中应注意的事项也进行了讨论。     

Speciation of mercury in salmon egg cell cytoplasm in relation with metallomics research

Speciation of mercury in salmon egg cell cytoplasm was investigated by surfactant-mediated high-performance liquid chromatography/inductively coupled plasma mass spectrometry (HPLC/ICP-MS), where an ODS (octadecylsilica) column coated with a bile acid derivative, CHAPS (3-[(3-cholamidopropyl)-dimethylammonio]-1-propane sulfonate), was used for species separation. Prior to the speciation analysis, total Hg in the cell cytoplasm was determined by ICP-MS at m/z 202 in a flow injection mode. For the precise measurement, salmon egg cell cytoplasm was diluted five-fold with 0.1 M Tris (Tris(hydroxymethyl)aminomethane)-HNO₃ buffer solution, and the standard addition method was employed. Thus, the total concentration of Hg in cell cytoplasm was estimated to be 12.4 ng g⁻¹ on the wet weight basis. Next, the cell cytoplasm diluted five-fold with 0.1 M Tris-HNO₃ buffer solution was analyzed by surfactant-mediated HPLC with the dual detection system of a UV absorption detector and an ICP-MS instrument. Two peaks corresponding to some proteins and small molecules were mainly observed in those chromatograms. When salmon egg cell cytoplasm was diluted five-fold with 0.01 M Tris buffer solution or pure water, some precipitates appeared probably because of precipitation of hydrophobic proteins in cytoplasm. After the precipitates were eliminated with a membrane filter, the filtrate was subjected to the analysis by surfactant-mediated HPLC/UV/ICP-MS. As a result, the peaks for small molecular species of Hg were clearly observed at the retention time near 4.0 min (corresponding to low-molecular weight zone) in the chromatograms with UV absorption detection as well as with Hg- and S-specific ICP-MS detections. The small molecule bound with Hg was identified as cysteine through the cysteine-spiked experiment. In addition, the protein fraction on the chromatogram obtained by using the CHAPS-coated ODS column was further analyzed by SEC (size exclusion chromatography). Consequently, several protein peaks with molecular weight of 300, 50 and 12 kDa were observed in all the detections of UV absorption, Hg and Se, although two peaks among them were coincident in the case of S. These results indicate that Hg in salmon egg cell cytoplasm binds with proteins containing selenocysteine and/or cysteine residues in proteins.