Structural disorder, octahedral coordination and two-dimensional ferromagnetism in anhydrous alums

The crystal structures of the triangular lattice, layered anhydrous alums KCr(SO₄)₂, RbCr(SO₄)₂ and KAl(SO₄)₂ are characterized by X-ray and neutron powder diffraction (NPD) at temperatures between 1.4 and 773 K. The compounds all crystallize in the space group , with octahedral coordination of the trivalent cations. In all cases, small amounts of disorder in the stacking of the triangular layers of corner sharing MO₆ octahedra and SO₄ tetrahedra is seen, with the MO₆−SO₄ network rotated in opposite directions between layers. The electron diffraction study of KCr(SO₄)₂ supports this model, which on an average can be taken to imply trigonal prismatic coordination for the M³⁺ ions; as was previously reported for the prototype anhydrous alum, KAl(SO₄)₂. The temperature-dependent magnetic susceptibilities for ACr(SO₄)₂ (A=K, Rb, Cs) indicate the presence of predominantly ferromagnetic interactions. Low-temperature powder neutron diffraction reveals that the magnetic ordering is ferromagnetic in-plane, with antiferromagnetic ordering between planes below 3 K.     

共沉淀分离富集-ICP-AES测定饲料级硫酸铜中微量As和Pb

在氨性介质中 ,以硫酸铁铵作共沉淀剂 ,预富集硫酸铜中的微量砷、铅 ,ICP- AES测定砷、铅的含量。方法检出限可满足日常分析的需要。加标回收率 As95 .0 %— 98.8% ;Pb96 .9%— 97.5 % ;相对标准偏差As4 .4 % ;Pb5 .8%。     

The Preliminary Studies of Electrochemical Behavior of Paracetamol and Its Metabolites on Glassy Carbon Electrode by Voltammetric Methods

The new, rapid and sensitive method for the determination of paracetamol (PAR) and its glucuronide (PG) and sulfate (PS) metabolites is proposed. The electrochemical properties of the compounds were examined by cyclic voltammetry (CV) on glassy carbon electrode (GCE). All measurements were carried out in Britton–Robinson buffers (BR) with different pH values over the pH range 1.81–7.24. The preliminary research indicated that PAR could be determined simultaneously with one of its metabolites. The linearity of calibration curves was obtained for concentrations between 1.65×10^?5 and 1.65×10^?4 M for PAR, 1.53×10^?5 and 1.53×10^?4 M for PG and 2.17×10^?5 and 1.52×10^?4 M for PS.     

Structural and conductivity studies of CsKSO4Te(OH)6 and Rb1.25K0.75SO4Te(OH)6 materials

The crystal structures of the title compounds were solved using the single-crystal X-ray diffraction technique. At room temperature CsKSO₄Te(OH)₆ was found to crystallize in the monoclinic system with Pn space group and lattice parameters: ; ; ; β=106.53(2)°; ; Z=4 and . The structural refinement has led to a reliability factor of R₁=0.0284 (wR₂=0.064) for 7577 independent reflections. Rb_1.25K_0.75SO₄Te(OH)₆ material possesses a monoclinic structure with space group P2₁/a and cell parameters: ; ; ; β=106.860(10)°; ; Z=4 and . The residuals are R₁=0.0297 and wR₂=0.0776 for 3336 independent reflections. The main interest of these structures is the presence of two different and independent anionic groups (TeO₆⁶⁻ and SO₄²⁻) in the same crystal.Complex impedance measurements (Z^*=Z^′—iZ^″) have been undertaken in the frequency and temperature ranges 20-10⁶ Hz and 400-600 K, respectively. The dielectric relaxation is studied in the complex modulus formalism M^*.     

Hydrothermal synthesis of a luminescent Europium(III) sulfate with three-dimensional chiral framework structure

The crystal structure and luminescent property of hydrothermally grown crystals of [NaEu(H₂O)(SO₄)₂] (1) are reported. The crystal structure is composed of three kinds of right-handed helical chains, {EuOSO₄}, {NaOSO₄} and {EuONa}, which are connected together to form a three-dimensional framework structure via corner-shared polyhedra. The sharp peaks in the emission spectrum of 1 are assigned and analyzed. Crystal data: Trigonal, P3₁21, with , and z=3.     

硫酸根拉曼频移用于深海热液温度探测的方法探讨

作为一种典型的深海极端环境,热液区域不仅分布着各种硫化物矿产,而且孕育着特殊的生态群落,对热液流体理化性质的研究有助于深入了解热液的运动机制。激光拉曼光谱技术除了定性分析方面的优势外,已经被逐步用于定量分析,并且在原位探测中发挥了重要作用。该研究模拟了深海热液喷口流体的高温高压环境,探讨了水分子和硫酸根离子的拉曼光谱在热液流体温度探测中的应用价值。通过对水峰ν₁（H₂O）、硫酸根ν₁(SO2-₄)的拉曼频移与温度、离子浓度的关系进行研究,结果表明水峰ν₁（H₂O）和硫酸根ν₁(SO2-₄)的拉曼频移随温度表现出明显的变化,水峰ν₁（H₂O）的拉曼频移受流体硫酸根浓度的影响明显,因此不适用于硫酸根离子浓度变化明显的热液流体温度的测量。相比之下,ν₁(SO2-₄)的拉曼频移对流体硫酸根浓度和流体压力不敏感,为温度的反演提供了很好的依据。建立了ν₁(SO2-₄)的拉曼频移与温度的线性方程：Rν₁(SO2-₄)=-0.03T+980.69,其中,R2=0.998 6,可用于对深海热液喷口流体温度的原位探测等实际应用。     

卡拉胶纤维的阻燃性能

以钡盐为凝固浴, 经湿法纺丝技术获得卡拉胶纤维(CAF). 通过极限氧指数(LOI)、 锥型量热(Cone)、 扫描电子显微镜(SEM)、 元素分析(EDS)、 X射线衍射(XRD)、 热重红外(TG-FTIR)同步差示扫描量热(DSC)法、 热裂解(Py)和气相色谱-质谱法(GC-MS)对CAF进行表征. 结果表明, CAF极限氧指数高达50以上, 锥型量热过程中, CAF一直保持红热状态, 没有产生火苗, 其热释放速率及总释放热等参数均较低, 与海藻酸钙纤维(ALF)和琼胶纤维(AGF)相比, CAF具有较好的阻燃性. 可能机理为卡拉胶分子的硫酸酯基和渗入纤维内部的钡离子发生络合作用, 并促进交联成炭和改变纤维裂解过程. 裂解过程中产生的磺酰自由基与燃烧产生的氢氧自由基迅速结合, 终止燃烧反应. 同时, CAF在燃烧过程中产生大量残炭, 并形成致密的钡盐结构层和中空的纤维结构, 成为CAF阻燃的另一重要因素.     

水溶液中硫酸根离子的拉曼光谱定量分析

拉曼光谱因其具有无损、非接触以及原位的技术优势被广泛应用于科学研究领域。但是,当前拉曼光谱主要应用于定性研究,即根据拉曼波数偏移进行物质分子的鉴别,相比之下,拉曼光谱定量分析则明显不足。因此,有必要进一步开展拉曼光谱定量方面的研究。根据拉曼光谱原理分析可知,拉曼光谱定量研究应当根据相对强度比进行,也就是在定量化过程中需要选择一个参考系,可以分为内标法和外标法。拉曼光谱定量可以根据被测分子与该参考系的拉曼强度比值进行,通过这个方法可以消除测试条件的影响。对水溶液而言,可将液态水的OH伸缩振动作为内标,进行拉曼光谱定量分析。本文研究了Na₂SO₄-H₂O,K₂SO₄-H₂O以及NaCl-Na₂SO₄-H₂O体系的拉曼光谱特征。通过将水分子的OH伸缩振动（2 750~3 900 cm-1附近）拟合为两个高斯谱峰,并以I_SO2-4/I_W为参数来确定溶液中的硫酸根离子浓度,其中I_SO2-4为硫酸根离子的特征峰强度,I_W为水的两个高斯谱峰强度之和。实验结果表明,水溶液中SO2-₄浓度与拉曼强度比I_SO2-4/I_W之间有较好的线性关系,其中,R2=0.997 73,符合定量要求。据此,本文应用拉曼光谱定量分析,建立了一种相对快速、准确测量水溶液中SO2-₄浓度的方法。     

容量法测定硫酸镁注射液含量的不确定度评定

讨论了容量法测定硫酸镁注射液含量中的各种不确定度影响因素。通过对测定过程中各种影响因素进行分析评估,计算出各分量的不确定度,得出合成不确定度和扩展不确定度(k=2)。建立的不确定度计算方法适用于容量法测定硫酸镁注射液含量的不确定度评价。     

黑碳颗粒物表面SO2的非均相臭氧氧化

采用漫反射红外傅里叶变换光谱(DRIFTS)结合离子色谱(IC)、 X射线光电子能谱(XPS)研究了常温常压下SO2与O3在黑碳颗粒物(以Printex U为代表, 简称UBC)表面的非均相反应. 研究发现, 在O3和水气存在的情况下, 体系的反应产物主要是SO42-, 反应在一定时间内持续进行. UBC可提供反应活性位点, 促进SO2在其表面的臭氧氧化. O3是关键的氧化剂, 能显著提高SO2非均相氧化生成SO42-的速率. 水气的存在有利于表面活性位点再生, 使反应持续发生. 当SO2和O3的浓度为1014~1015 molecule/cm3、 相对湿度为40%时, SO2在UBC(1: 400, 以NaCl为稀释剂稀释400倍)表面非均相反应生成SO42-的稳态摄取系数(γBET)为1~6×10-6, SO42-的生成速率为1014~1015 ion·s-1·g-1.