强碱阴离子交换树脂及碱性洗脱剂的离子排阻/阴离子交换色谱法同时测定NH4+ ，NO2-和NO3-（英文）

Ion-exclusion/anion-exchange chromatography(IEC/AEC) on a combination of a strongly basic anion-exchange resin in the OH——form with basic eluent has been developed.The separation mechanism is based on the ion-exclusion/penetration effect for cations and the anion-exchange effect for anions to anion-exchange resin phase.This system is useful for simultaneous separation and determination of ammonium ion(NH+4),nitrite ion(NO-2),and nitrate ion(NO-3) in water samples.The resolution of analyte ions can be manipulated by changing the concentration of base in eluent on a polystyrene-divinylbenzene based strongly basic anion-exchange resin column.In this study,several separation columns,which consisted of different particle sizes,different functional groups and different anion-exchange capacities,were compared.As the results,the separation column with the smaller anion-exchange capacity(TSKgel Super IC-Anion) showed well-resolved separation of cations and anions.In the optimization of the basic eluent,lithium hydroxide(LiOH) was used as the eluent and the optimal concentration was concluded to be 2 mmol/L,considering the resolution of analyte ions and the whole retention times.In the optimal conditions,the relative standard deviations of the peak areas and the retention times of NH+4,NO-2,and NO-3 ranged 1.28%-3.57% and 0.54%-1.55%,respectively.The limits of detection at signal-to-noise of 3 were 4.10 μmol/L for NH+4,1.87 μmol/L for NO-2 and 2.83 μmol/L for NO-3.     

一种甲醇直接气相羰基化新催化剂

本世纪７０年代Ｍｏｎｓａｎｔｏ公司成功开发了甲醇液相羰化ＲｈＩ催化体系，使甲醇羰化生产醋酸成为重要的工业过程．然而，由于此工艺产物与催化剂分离复杂、铑资源紧缺以及体系中还必须加大量的碘甲烷（或氢碘酸）作促进剂，设备腐蚀严重．８０年代以来，甲醇气相羰...     

碲铋渣中铋的测定

讨论了在pH=9.4～10.0的氨性溶液中,利用Fe3+与Te4+、Bi3+生成三元共沉淀物,分离其它杂质,然后用KOH溶解Te,从而达到Te,Bi分离的目的。在pH=1.5～1.7的溶液中,利用抗坏血酸掩蔽铁,以硫脲-PAR作为指示剂,用EDTA标准溶液滴定Bi。当n=6时,相对标准偏差为0.4%,回收率为98.53%～102.2%,方法准确、可靠。     

Ultraviolet Spectroscopic Detection of Nitrate and Nitrite in Seawater Simultaneously Based on Partial Least Squares

A direct, reagent-free, ultraviolet spectroscopic method for the simultaneous determination of nitrate (NO₃⁻), nitrite (NO₂⁻), and salinity in seawater is presented. The method is based on measuring the absorption spectra of the raw seawater range of 200–300 nm, combined with partial least squares (PLS) regression for resolving the spectral overlapping of NO₃⁻, NO₂⁻, and sea salt (or salinity). The interference from chromophoric dissolved organic matter (CDOM) UV absorbance was reduced according to its exponential relationship between 275 and 295 nm. The results of the cross-validation of calibration and the prediction sets were used to select the number of factors (4 for NO₃⁻, NO₂⁻, and salinity) and to optimize the wavelength range (215–240 nm) with a 1 nm wavelength interval. The linear relationship between the predicted and the actual values of NO₃⁻, NO₂⁻, salinity, and the recovery of spiked water samples suggest that the proposed PLS model can be a valuable alternative method to the wet chemical methods. Due to its simplicity and fast response, the proposed PLS model can be used as an algorithm for building nitrate and nitrite sensors. The comparison study of PLS and a classic least squares (CLS) model shows both PLS and CLS can give satisfactory results for predicting NO₃⁻ and salinity. However, for NO₂⁻ in some samples, PLS is superior to CLS, which may be due to the interference from unknown substances not included in the CLS algorithm. The proposed method was applied to the analysis of NO₃⁻, NO₂⁻, and salinity in the Changjiang (Yangtze River) estuary water samples and the results are comparable with that determined by the colorimetric Griess assay.     

Synthesis and Characterization of Chitosan‐graft‐Poly(3‐(trimethoxysilyl)propyl methacrylate) Initiated by Ceric (IV) Ion

The grafting of 3‐(trimethoxysilyl)propyl methacrylate (TMSPM) onto chitosan by ceric ion initiation was studied under homogeneous conditions in 2% acetic acid solution. The grafted polymer was characterized by FT‐IR, ¹H‐NMR, TGA and XRD and swelling studies. TGA results showed that the incorporation of TMSPM to the chitosan chains decreased the thermal stability of the grafted chitosan. Due to the grafting of TMSPM, the crystallinity of chitosan derivatives was found to be destroyed. The solubility of the grafted chitosan in water was improved. The effects of reaction conditions such as initiator concentration, monomer concentration, reaction temperature and reaction time were studied by determining the grafting parameters such as grafting and grafting efficiency. Under optimum conditions, the grafting parameters were achieved as 1440 and 97%, respectively.     

Room-Temperature Bismuth-Catalyzed Bis-arylation of Carbonyl Compounds with Aryl Ethers and Phenols

Using Bi2（SO4）3 as the catalyst and TMSCl as the additive, a wide variety of aldehydes, ketones, and acetals were smoothly condensed with aryl ethers at room temperature to provide the corresponding diarylmethanes and triarylmethanes selectively in good to excellent yields.     

Development of a manual method for the determination of mineral oil in foods and paperboard

So far the majority of the measurements of mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH) were obtained from on-line high performance liquid chromatography–gas chromatography–flame ionization detection (on-line HPLC–GC–FID). Since this technique is not available in many laboratories, an alternative method with more easily available tools has been developed. Preseparation on a small conventional liquid chromatographic column was optimized to achieve robust separation between the MOSH and the MOAH, but also to keep out the wax esters from the MOAH fraction. This was achieved by mixing a small portion of silica gel with silver nitrate into highly activated silica gel and by adding toluene into the eluent for the MOAH. Toluene was also added to the MOSH fraction to facilitate reconcentration and to serve as a keeper preventing loss of volatiles during solvent evaporation. A 50 μl volume was injected on-column into GC–FID to achieve a detection limit for MOSH and MOAH below 1 mg/kg in most foods.     

pH值对Bi2MoO6晶体形貌和可见光催化性能的影响

以(NH₄)₆Mo₇O₂₄·4H₂O和Bi(NO₃)₃·5H₂O为原料,采用普通水热法制备Bi₂MoO₆光催化剂,研究pH值对制备该光催化剂的影响.对所制备的系列样品,采用X-射线衍射仪(XRD)、扫描电子显微镜(SEM)、比表面积分析仪、X射线光电子能谱仪(XPS)和紫外-可见漫反射(UV-Vis DRS)进行表征.结果表明:pH值对Bi₂MoO₆晶体的物相组成、形貌和光催化性能均有显著影响.pH值为1~7时,所制备的样品为纯相Bi₂MoO₆,pH值为9或11时,出现第二相Bi_3.64Mo_0.36O_6.55;随着pH值的升高,形貌依次为纳米棒、纳米片和无规则纳米颗粒.在可见光(λ≥420 nm)照射下,通过光催化降解罗丹明B(Rhodamine B,RhB),探讨了制备Bi₂MoO₆的pH值对其可见光催化活性的影响.当pH=7时,制备的样品光催化效果最好,光照50 min后对初始浓度为5 mg·L^-1的罗丹明B溶液的降解率为85%.