高效液相色谱-电感耦合等离子体质谱法同时测定化妆品中5种含溴防腐剂

建立了同时测定化妆品中苯扎溴铵、2-溴-2-硝基-1,3-丙二醇、5-溴-5-硝基-1,3-二■烷、甲基二溴戊二腈、溴氯芬5种含溴防腐剂的高效液相色谱-电感耦合等离子体质谱法(HPLC-ICP-MS)。样品经含0.1%甲酸的甲醇溶液超声提取后,采用Agilent Eclipse-C_(18)(150 mm×4.6 mm,5μm)色谱柱分离,以0.1%甲酸-甲醇为流动相进行梯度洗脱,ICP-MS测定组分中的~(79)Br,以保留时间定性,外标法定量。5种含溴防腐剂均在0.5～100 mg/L范围内线性关系良好(r0.999),检出限为1.5～3.0μg/g,不同基质化妆品中的回收率为91.2%～108%,相对标准偏差(n=6)为1.3%～4.2%。该方法快速、准确、灵敏、专属性强,适用于化妆品中5种含溴防腐剂的定性定量分析。     

Metallaphotoredox⁃Catalyzed O⁃Arylation of Serine北大核心CSCD

A metallaphotoredox catalyzed hydroxyl aromatization of serine is developed to achieve rapid synthesis of aryl ethers of various serine derivatives. Under the catalytic system of ethylene glycol dimethyl ether nickel bromide （NiBr2 （dme））/4,4'-dimethoxy-2,2'-bipyridine/zinc powder and synergistic iridium photoredox catalysis, nickel is catalyzed and inserted into the C—Br bond, and then followed by transmetalation with the hydroxyl group of serine. The resulting Ni（Ⅱ）species are oxidized by the excited Ir（Ⅲ）species to a Ni（Ⅲ）intermediate. This intermediate is unstable and reductive elimination takes place rapidly to give the target product O-arylated serine in the yields from 65% to 39%. Through a metallaphotoredox catalysis strategy,the reaction features mild,efficient,clean and broad scope of substrate, providing a new way for the synthesis of various serine derivatives with medicinal value. © 2022, Science Press (China). All rights reserved.     

偶氮苯高分子的光致可逆固液转变

偶氮苯化合物是一种极具吸引力以及较为常用的光响应材料,本文主要介绍偶氮苯的光响应性质以及一些偶氮苯高分子的合成方法,解析光化学反应导致偶氮苯高分子固液转变的机理,并介绍其在粘结性材料、光致动器、光致热导开关器件及非热纳米压印中的应用。     

Anomalous behavior and phase transformation of α-GaOOH nanocrystals under static compression

The structural compression mechanism and compressibility of gallium oxyhydroxide, α-GaOOH, are investigated by in situ synchrotron radiation x-ray diffraction at pressures up to 31.0 GPa by using the diamond anvil cell technique. Theα-GaOOH sustains its orthorhombic structure when the pressure is lower than 23.8 GPa. The compression is anisotropic under hydrostatic conditions, with the a-axis being most compressible. The compression proceeds mainly by shrinkage of the void channels formed by the coordination GaO_3(OH)_3 octahedra of the crystal structure. Anomaly is found in the compression behavior to occur at 14.6GPa, which is concomitant with the equatorial distortion of the GaO_3(OH)_3 octahedra. A kink occurs at 14.6 GPa in the plot of finite strain f versus normalized stress F, indicating the change in the bulk compression behavior. The fittings of a second order Birch–Murnaghan equation of state to the P–V data in different pressure ranges result in the bulk moduli B_0= 199(1) GPa for P 14.6 GPa and B_0= 167(2) GPa for P 14.6 GPa. As the pressure is increased to about 25.8 GPa, a first-order phase transformation takes place, which is evidenced by the abrupt decrease in the unit cell volume and b and c lattice parameters.     

分布式系统中进程迁移算法研究

进程迁移是改善分布式系统的负载平衡和稳定性的一种有效手段，本文总结了主要的４ 类进程迁移算法，比较了它们的优点和缺点．并将该算法与“中庸算法”相结合，为“中庸算法”的实现打下了理论基础．     

中庸算法——一种基于环型结构的并行调度算法

给出了分布式系统中的一种基于环结构的并行调度算法，以下称为中庸算法，并从理论上证明了该算法能够达到较好的负载平衡、最大限度的减少任务的迁移和通信、最大程度的计算本地化 并举例进行了说明     

气相色谱法测定苹果和土壤中的高效氯氟氰菊酯

建立了改进的QuEChERS-气相色谱检测苹果和土壤中高效氯氟氰菊酯残留的分析方法,考察和评价了苹果和土壤两种基质对高效氯氟氰菊酯的基质效应。苹果和土壤样品均用乙腈提取,经石墨化碳黑（GCB）净化后直接进样分析。结果表明：在优化后的QuEChERS条件下,高效氯氟氰菊酯在0.05~10 mg/L范围内线性关系良好,相关系数（R²）大于0.999,检出限为0.12~0.15 μg/kg,定量限为0.38~0.50 μg/kg。用基质标准曲线定量时,高效氯氟氰菊酯在土壤和苹果中的回收率分别为88.29%~97.65%和80.70%~98.69%。苹果和土壤样品对高效氯氟氰菊酯都表现出基质增强效应。该方法的回收率均能达到残留分析要求,用基质配制标准溶液能够有效、方便地校正气相色谱-电子捕获检测器测定高效氯氟氰菊酯残留时的基质效应,且能应用于苹果和土壤实际样品的检测。     

电感耦合等离子体发射光谱(ICP-OES)法测定水泥熟料中铬的干扰研究

电感耦合等离子体发射光谱法（ICP-OES）测定重金属时常面临干扰问题。为提高ICP-OES测定水泥熟料中铬的准确度,研究选取了Cr205.560、Cr267.716和Cr283.563三条谱线,根据水泥熟料中主量元素（铁、铝、钙和镁）含量,设计不同浓度单元素干扰试验,结果表明：铁对Cr283.563谱线测定有较大的正干扰,钙对三条谱线均有较大的负干扰,两者导致的相对误差（RE）均在±10%以上,其他一般为负干扰,RE在±10%以内。进一步线性回归分析发现,除铝外,其他干扰元素的干扰大小与浓度呈强线性相关性。通过多元素复合干扰试验发现干扰导致的RE约为-18%~11%,同单元素干扰加和结果比较,两者相差约为8%~10%。实际样品检测结果表明实际干扰同多元素复合干扰试验基本相同,Cr283.563谱线测定结果误差可能更小,三条谱线的实际样品加标回收率大致相当,约为80%,经回收率修正,Cr205.560和Cr267.716谱线结果满意,而Cr283.563谱线误差较大。以多元素复合干扰试验溶液作为基体,采用基体匹配法测定可基本消除干扰影响。以钙溶液作为基体的简化基体匹配法同样有效,但仅可选用Cr205.560和Cr267.716谱线。本研究从实际干扰问题出发,通过系统分析问题,找到干扰的原因,并据此提出消除干扰方法,提高了测定铬的准确度,也为检测人员解决相关干扰问题提供借鉴。     

铁磁Pr1-xSrxMnO3外延薄膜的输运性质与负磁电阻行为

利用脉冲激光淀积法生长了外延Pr_1-xSr_xMnO₃薄膜(其中x=0.1,0.2,0.3,和0.4).测量了薄膜样品在零场中与外加磁场下电阻率随温度的变化.对X≥0.2的样品在磁场下观察到负磁电阻效应.在logρ-l/T的坐标中,零磁场下的数据在很宽的温区显现很好的线性关系,具有热激活载流于输运特征.由实验数据线性拟合得到在样品成分0.1≤ X≤0.3范围的热激活能约为0.1eV.从对掺杂锰氧化物的电子结构分析出发,对这一材料的绝缘-金属相变,输运性质和负磁电阻行为进行了讨论.     

Temperature-dependent structure and magnetization of YCrO3 compound

We have grown a YCrO$_3$ single crystal by the floating-zone method and studied its temperature-dependent crystalline structure and magnetization by x-ray powder diffraction and PPMS DynaCool measurements. All diffraction patterns were well indexed by an orthorhombic structure with space group of $Pbnm$ (No. 62). From 36 K to 300 K, no structural phase transition occurs in the pulverized YCrO$_3$ single crystal. The antiferromagnetic phase transition temperature was determined as $T_\textrm{N} = 141.58(5)$ K by the magnetization versus temperature measurements. We found weak ferromagnetic behavior in the magnetic hysteresis loops below $T_\textrm{N}$. Especially, we demonstrated that the antiferromagnetism and weak ferromagnetism appear simultaneously upon cooling. The lattice parameters ($a$, $b$, $c$, and $V$) deviate downward from the Grüneisen law, displaying an anisotropic magnetostriction effect. We extracted temperature variation of the local distortion parameter $\varDelta$. Compared to the $\varDelta$ value of Cr ions, Y, O1, and O2 ions show one order of magnitude larger $\varDelta$ values indicative of much stronger local lattice distortions. Moreover, the calculated bond valence states of Y and O2 ions have obvious subduction charges.