AG50W-x8树脂分离去除钡的多原子离子对电感耦合等离子体质谱法测定稀土元素的质谱干扰

采用AG50W－x8阳离子交换树脂,以HNO3作为梯度淋洗剂,可有效地分离Ba和稀土元素,实验表明：以2mol/L HNO3淋洗时,99．5％的Ba被分离去除;以5mol/L HNO3淋洗时,稀土的回收率在96－110％之间。标准参考物质的分析结果显示测定值与标准值十分接近,表明AG50W－x8阳离子交换树脂分离可有效地去除Ba元素的多原子离子（BaO^ ,BaOH^ )对ICP－MS法测定稀土元素测定的质谱干扰,该方法准确,可靠。同时,为准确测定Eu提供了一条新的途径。     

2-乙基己基膦酸单(2-乙基己基)酯树脂色层分离电感耦合等离子体原子发射光谱法测定钢中微量稀土元素

本文采用2-乙基己基膦酸单(2-乙基己基)酯(P-507)树脂,使微量稀土元素与钢中的基体元素,铁、钛、钒和钼分离,以 3.0 mol/L盐酸溶液洗脱P-507色层柱上的稀土元素,采用电感耦合等离子体原子光谱法(ICP-AES)同时测定了钢中La、Ce、Pr、Nd、Sm、Y和 Gd 7种微量稀土元素.试样的标准加入回收率99.3％～108％;相对标准偏差小于5％.     

Cyanex 923从硫酸体系中萃取钪及其与P507和环烷酸的比较

稀土元素钪(Sc)在相关原料中含量低,伴生杂质元素多,回收困难。针对这一问题,本文系统对比了直链三烷基氧化膦(Cyanex 923)、2-乙基己基磷酸单-2-乙基己基酯(P507)、环烷酸在硫酸体系中对Sc的萃取、分离和反萃。Cyanex 923在高酸度下能完全萃取Sc,而环烷酸和P507则在低酸度下有较高萃取率。Cyanex 923分离Sc与锆(Zr)、钛(Ti)的最佳水相酸度为1 mol/L,分离系数分别为5. 6和10. 6。P507在水相H~+浓度为2 mol/L时对Sc/Zr、Sc/Ti有最大分离系数,分别是21和59. 7。虽然P507有更好的分离效果,但难以反萃。3种萃取剂中仅有Cyanex 923能被有效反萃,在反酸H+浓度为0. 4 mol/L时有最大反萃率。因此,Cyanex 923更适合从含Sc二次资源浸出液中分离回收Sc。     

离子色谱非梯度洗脱法同时测定7种稀土元素的研究

研究了离子色谱非梯度洗脱法同时测定7种稀土元素的方法，用草酸一元淋洗液，采用非梯度洗脱方式，以PAR为显色荆，在520nm处对7种稀土元素同时进行检测。考察了淋洗液的组成、浓度、pH及流量等因素对被测组分分离和测定的影响，选择了显色剂的浓度、流量和检测波长，并进行了干扰实验，在选定的最佳分离测定条件下，测定了7种稀土元素的线性回归方程、检出限0．04～0．20mg／L，回收率在94．3％～101．5％之间。本方法已用于稀土氧化物的高温氯化产物中稀土元素的测定。     

共聚型2-乙基己基膦酸单2-乙基己基酯萃淋树脂孔结构与分离效能的关系

应用性能优良的２－乙基己基膦酸单２－乙基已基酯ＨＥＨ（ＥＨＰ）萃取剂，首次制备了一系列不同孔结构的萃淋树脂，针对难以分离的镧系元素中最难分离的镨、钕，研究了孔结构等与分离效能之关系，探寻出最适宜的孔结构。其比表面积Ｓ为 ２０９ ｍ２／ｇ，平均孔径为 ７．７ｎｍ，孔体积Ｖｇ ０．４０１ｍＬ／ｇ；ＨＥＨ（ＥＨＰ）最适宜量为４６．５％，从而达到最佳分离。     

离子色谱荧光检测法测定废水中痕量2-氨基联苯和4-氨基联苯

采用离子色谱荧光检测法测定废水中的2－氨基联苯（2－ADP）和4－氨基联苯（4－ADP），流动相为1．0mL/min的0．06mol/L NaCl,0.08mol/L HCl,40%(V/V)ACN，分离柱为Dinoex OmniPac PCX-500，该法具有良好的重现性和线性关系，2－ADP和4－ADP的回收率分别为98．5％－101．4％和102．2％－104．0％，检测限分别为0．006mg/L和0．10mg/L。     

二(2-乙基己基)膦酸从盐酸介质中萃取钪(Ⅲ)、钇(Ⅲ)、镧系离子(Ⅲ)和铁(Ⅲ)

本文研究了二(2-乙基己基)膦酸(H[DEHP])的正辛烷溶液从盐酸介质中萃取钪(Ⅲ)、钇(Ⅲ)、镧系离子(Ⅲ)和铁(Ⅲ)的平衡规律。结果表明,H[DEHP]对上述离子的萃取次序是Sc³⁺>Fe³⁺>Lu³⁺>Yb³⁺>Er³⁺>Y³⁺>Ho³⁺。讨论了Sc(Ⅲ)与Fe(Ⅲ)、Y(Ⅲ)、Ln(Ⅲ)(镧系离子)以及Fe(Ⅲ)与重镧系离子(Ⅲ)分离的可能性,并与HEH[EHP]萃取上述离子的性能进行了比较。借助IR、NMR和斜率法,饱和法研究了低酸度下H[DEHP]萃取Sc(Ⅲ)、Y(Ⅲ)和Ln(Ⅲ)的平衡反应,计算了浓度平衡常数和萃取反应的热力学函数。     

固相萃取-反相高效液相色谱法测定水中的邻苯二甲酸酯

建立了固相萃取-反相高效液相色谱法检测水中3种邻苯二甲酸酯类物质邻苯二甲酸二甲酯、邻苯二甲酸二(2-乙基己基)酯、邻苯二甲酸二正辛酯的方法. 考察了固相萃取柱、洗脱溶剂、洗脱体积、上样速度以及洗脱速度对萃取效率的影响. 通过综合分析, 选定SupelcleanLC-18 SPE Tube固相萃取柱, 甲醇为洗脱剂, 洗脱体积2 mL, 上样速度为4 mL/min, 洗脱速度为1 mL/min. 在此萃取条件下, 萃取回收率在83.4%～121.2%之间. 邻苯二甲酸二甲酯、邻苯二甲酸二(2-乙基己基)酯、邻苯二甲酸二正辛酯质量浓度在2～100 mg/L之间均为线性. 经萃取后, 方法的最低检出限分别为邻苯二甲酸二甲酯0.06 μg/L, 邻苯二甲酸二(2-乙基己基)酯0.16 μg/L, 邻苯二甲酸二正辛酯0.08 μg/L. 方法的精密度在10%～15%之间. 应用该方法测定自来水中酞酸酯类化合物的含量, 加标回收率为83.6%～110.2%.     

等离子体质谱多内标法测定金属铒中多种痕量元素

本方法采用ICP—MS法同时测定高纯金属铒中14个稀土元素和15种非稀土元素杂质，确定了合适的样品稀释浓度，采用Sc、In、Cs、Tl4个内标，杂质元素的检出限在0．04～16μg／g之间，样品的加标回收率在86％～105％之间，能够满足4N金属铒产品的检测需求。     

液相色谱质谱联用检测血液和尿液中的 琥珀胆碱及对标样的稳定性评价

采用OasisR WCX固相萃取柱,用50％甲醇溶液洗脱杂质,并用1 mL甲酸-乙腈-水(1:8:1)溶液进行淋洗目标物.采用LC/MS/ESI检测其母离子为145.1,并选择115.5作为其定量离子.在尿液和血液中进行了回收率实验,测得其定量检测限分别为0.92ng/mL,1.89ng/mL( 10倍S/N),方法的...     

萃取剂HDEHP在不同稀释剂中的聚合性质

HDEHP在惰性稀释剂中由于分子间氢键作用易形成二聚体[1 ] ,其二聚常数已有报道[2 ] ,但很不一致。由于萃取动力学、液—液界面性质都与萃取剂在有机相中的存在状态密切相关 ,本文研究了不同稀释剂中 HDEHP的聚合性质 ,并实现了二聚常数与稀释剂物理常数间的定量关联。实　验　部　分一 .试剂和仪器HDEHP,工业品 ,经提纯纯度大于 99% ;氯仿、苯、甲苯、环己烷、四氯化碳、甲基异丁基酮 ,均为分析纯 ;正辛烷 ,化学纯。TOA p H计 ,日本岛津 ;KS恒温振荡器 ,山东大学化学院金工室改装 ;FTS 16 5红外光谱仪 ,美国 Bio- Rad公司。二 .…     

二（2-乙基己基）二硫代磷酸溶剂萃取铊的热动力学

在Tl₂SO₄＋Na₂SO₄＋二（2-乙基己基）二硫代磷酸＋n-C₈H₁₈＋水体系中， 测定了0.1－2.0 mol•kg^－1离子强度范围内Tl^＋ 的平衡摩尔浓度。水相中电解质Na₂SO₄ 控制溶液离子强度， 有机相中萃取剂取278.15 K至303.15 K范围内的恒定摩尔浓度。通过外推法和多项式近似得到了不同温度下的标准萃取常数K⁰，计算了萃取过程的热动力学量。     

A novel sodium bis(2-ethylhexyl) sulfosuccinate-PAGE system suitable for the separation of small peptides

A novel sodium bis(2-ethylhexyl) sulfosuccinate-PAGE (AOT-PAGE) system which delivers high resolution and sensitivity for small peptides with molecular masses of 0.8-17 kDa is described. Small peptides migrate more slowly and are less prone to leakage than in conventional SDS-PAGE, thus allowing for the in-gel detection with CBB R 250 of 0.5 mug of peptide. The system is also compatible with electroblotting, activity staining in renatured gels, and the peptide analysis by MALDI-MS. AOT-PAGE is simpler, more rapid, and cheaper than the generally adopted Tricine-SDS-PAGE method.     

对苯二甲酸单异辛酯的合成

以对苯二甲酸、氯化亚砜、异辛醇为原料，经过酰化、酯化两步合成了对苯二甲酸单异辛酯，收率40．4％,纯度99．0％。     

Synthesis,characterization, and evaluation of polymeric oil sorbent for remediation of hydrocarbons spillage

The preparation and evaluation of polymeric oil sorbent based on styrene acrylate ester and ethylhexyl acrylate (EHA) are the main target of this work. In this respect, poly styrene-co-p-chloromethyl styrene (PSCMS) was synthesized through radical copolymerization of p-CMS with styrene in the presence of benzoyl peroxide initiator. Then, the PSCMS was reacted with acrylic acid to produce macromonomer containing polymerizable C?C poly {styrene-co-[4-(methyl acrylate) styrene]} (PSSMA) that subsequently copolymerized with EHA in the presence of a cross-linker to obtain the cross-linked copolymers PSSMA/EHA (organogel). The prepared compounds were characterized by using FTIR, ¹H NMR, and gel permeation chromatography. The thermal properties of the cross-linked oil absorbents were investigated using thermogravimetric analysis, and the morphology was characterized by scanning electron microscope (SEM). The oil absorbency of oil gel was determined through oil absorption tests; the highest oil absorbencies of oil gel were found to be 82.6, 74.4, 46.7, and 38.1 g/g in N,N-dimethyl formamide, CHCl₃, toluene, and diesel, respectively.     

改性高吸油性树脂的合成

将造成环境“白色污染”的发泡聚苯乙烯添加到由丙烯酸2-乙基已酯为单体的聚合体系中,从而合成新型的高吸油性树脂。考察了发泡聚苯乙烯的添加量、交联剂和引发剂等因素对树酯吸油性能的影响,所得树脂可吸苯22g/g,吸煤油13.5/g。     

Structure and aggregation behavior of cobalt-di(2-ethylhexy1)-phosphoric acid complexes in solvent extraction systems

Ｔｈｅｓｏｌｖｅｎｔｅｘｔｒａｃｔｉｏｎｏｆｃｏｂａｌｔｗｉｔｈｏｒｇａｎｏｐｈｏｓｐｈｏｒｕｓａｃｉｄｉｃｅｘｔｒａｃｔａｎｔｓｉｓｃｈａｒａｃｔｅｒｉｚｅｄｂｙｉｔｓｈｉｇｈｅｒｅｘｔｒａｃｔｉｏｎｓｅｌｅｃｔｉｖｉｔｙｔｈａｎｎｉｃｋｅｌｆｒｏｍａｑｕｅｏｕｓｓｏｌｕｔｉｏｎｓ[1].Ｔｈｅｅｘｔｒａｃｔａｂｉｌｉｔｙａｎｄｓｅｌｅｃｔｉｖｉｔｙｏｆｍｅｔａｌｉｏｎｓａｒｅｃｌｏｓｅｌｙｒｅｌａｔｅｄｔｏｔｈｅｃｏｏｒｄｉｎａｔｉｏｎｓｔｒｕｃｔｕｒｅｏｆｍｅｔａｌｓｗｉｔｈｅｘｔｒａｃｔａｎ…     

Polymerization of neat 2‐ethylhexyl acrylate induced by a pulsed electron beam

The bulk polymerization of 2‐ethylhexyl acrylate (2‐EHA), induced by a pulsed electron beam, was investigated with pulse radiolysis, gravimetry, and Fourier transform infrared spectroscopy. The roles of the dose rate, pulse frequency, and added acrylic acid (AA) in the polymerization of 2‐EHA were examined at ambient temperature. In the range of 12.6–71.2 Gy/pulse, the polymerization of 2‐EHA was dose‐rate‐dependent: at the same total dose, a lower dose rate yielded a higher conversion. Also, a lower pulse rate gave a higher conversion at the same total dose. The addition of up to 10 wt % AA showed no increase in the conversion of 2‐EHA at a low conversion (8 kGy), but at a higher conversion (16 kGy), a 20 wt % increase in the conversion of 2‐EHA was observed. The estimated values (1.6 ± 0.3) × 10^?3 (dm³ s)^3/2 mol^?1 s^?1/2 for k_p(G/2k_t)^1/2 and 2.6 ± 0.8 dm³ s J^?1 for 2k_tG (where k_p is the rate constant of propagation, k_t is the rate constant of bimolecular termination, and G is the yield of free radicals) were obtained at relatively low conversions. The reaction rate constant of the addition of 2‐EHA^· free radicals to the monomer was measured by pulse radiolysis and found to be 2.8 × 10² mol^?1 dm³ s^?1. © 2002 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 41: 196–203, 2003     

Comparison of solidification of floating drop and homogenous liquid–liquid microextractions for the extraction of two plasticizers from the water kept in PET‐bottles

Two approaches based on solidification of floating drop microextraction (SFDME) and homogenous liquid–liquid microextraction (HLLE) were compared for the extraction and preconcentration of di‐(2‐ethylhexyl) phthalate (DEHP) and di‐(2‐ethylhexyl) adipate (DEHA) from the mineral water samples. In SFDME, a floated drop of the mixture of acetophenone/1‐undecanol (1:8) was exposed on the surface of the aqueous solution and extraction was permitted to occur. In HLLE, a homogenous ternary solvent system was used by water/methanol/chloroform and the phase separation phenomenon occurred by salt addition. Under the optimal conditions, the LODs for the two target plasticizers (DEHA and DEHP), obtained by SFDME–GC‐FID and HLLE–GC‐FID, were ranged from 0.03 to 0.01 μg/L and 0.02 to 0.01 μg/L, respectively. HLLE provided higher preconcentration factors (472.5‐ and 551.2‐fold) within the shorter extraction time as well as better RSDs (4.5–6.9%). While, in SFDME, high preconcentration factors in the range of 162–198 and good RSDs in the range of 5.2–9.6% were obtained. Both methods were applied for the analysis of two plasticizers in different water samples and two target plasticizers were found in the bottled mineral water after the expiring time and the boiling water was exposed to a polyethylene vial.     

异辛基膦酸单异辛酯稀土配合物的快原子轰击质谱(FABMS)

酸性磷酸酯金属配合物组成和结构的测定有利于阐明萃取机理,是萃取化学中令人感兴趣的课题。标题配合物由于热稳定性差、挥发性小而且分子量大(结构筒式I,简称LnL_3),常规的质谱分析(EIMS、CIMS)难以进行。本文应用FABMS成功地对此配合物作了测定,并用亚稳跃迁技术对其裂解规律进行了探讨。