固定解离-气相色谱法测定水中三乙胺、二乙胺、乙胺及氨

建立了同时测定水中三乙胺、二乙胺、乙胺和氨4种物质的固定解离-气相色谱法。水样用H_2SO_4酸化,对三乙胺、二乙胺、乙胺及氨固定成盐,酸化后旋转蒸发掉水分,冰水浴下以甲醇为溶剂加入固体NaOH解离,以无水Na_2SO_4干燥,0.45μm滤膜过滤后进气相色谱测定。该方法峰面积和浓度的线性相关系数达到0.9992以上,检出限为0.03～0.10 mg/L、定量限为0.10～0.28 mg/L,在10,50和100 mg/L3个水平下添加回收率为89.9%～104.8%、相对标准偏差为0.70%～2.1%。该方法适用于乙胺类物质的生产废水及降解废水中三乙胺、二乙胺、乙胺和氨的同时检测。     

盐酸乙胺丁醇-Cu(Ⅱ)配合物的紫外光谱特征及含量测定

建立了一种间接测定盐酸乙胺丁醇含量的紫外-可见分光光度法。在pH 5.0介质中,盐酸乙胺丁醇与Cu~(2+)能以1:1的配比形成络合物,且在256 nm波长处有最大吸收,稳定常数为3.4×10~7。结果表明:在55.60～333.6μg/mL范围内,盐酸乙胺丁醇的浓度c与络合物的吸光度A之间呈现良好的线性关系,A=0.0005c+0.3003,r=0.9996,检出限为6.6μg/mL。将该方法应用于实际样品制剂的含量测定,得到加标回收率为95.2%～103.5%,RSDs为1.6%～2.8%。该方法可用于盐酸乙胺丁醇的含量测定。     

阀切换-离子色谱法测定分析纯硫酸钠中痕量氯离子

建立了阀切换-离子色谱法测定分析纯硫酸钠固体中痕量氯离子含量的方法。ICS-2100离子色谱系统,配置十通阀,用IonPac AS18色谱柱将硫酸钠固体样品中的氯离子和硫酸根离子预分离后,以IonPac TAC-ULP1为富集柱,将氯离子富集后在相同的IonPac AS18色谱柱上进行定量分析。同时以淋洗液发生器产生的不同浓度的KOH作为淋洗液,以抑制型电导检测器测定氯离子的含量。结果表明,阀切换-离子色谱法测定分析纯硫酸钠固体中的痕量氯离子,检出限为10 μg/L,线性相关系数(r2)大于0.999,实际样品的加标回收率为98.0%～103.0%,具有分离度和灵敏度高,选择性好,操作简单等特点。该方法能够准确测定硫酸钠固体中痕量氯离子的含量,适用于高纯化学试剂中痕量氯离子的分离测定。     

离子色谱法同时测定蛋白胨中氯离子、硫酸根离子、碘离子

建立离子色谱法测定蛋白胨中氯离子、硫酸根离子、碘离子3种阴离子的含量。采用氢氧化钾淋洗液发生器产生的KOH溶液为流动相,进行梯度淋洗,流量为1.0 mL/min。氯离子、硫酸根离子的质量浓度分别在0.5～200μg/mL范围内与色谱峰面积呈良好的线性关系,碘离子的质量浓度在0.75～50μg/mL范围内与色谱峰面积呈良好的线性,线性相关系数均不小于0.999,检出限分别为0.003,0.01,0.22μg/mL。样品加标回收率为92.94%～96.59%,测定结果的相对标准偏差为2.42%～5.70%(n=9)。该方法灵敏、高效,可用于蛋白胨中氯离子、硫酸根离子、碘离子的快速准确测定。     

火焰原子吸收光谱法及比浊法测定聚氯乙烯中氯

以无水碳酸钠为灰化固定剂,于瓷坩埚中加热将试样灰化,于高温炉中在700℃燃烧2 h,用水溶出残渣,分取部分试液用火焰原子吸收光谱法(FAAS)或浊度法测定其中氯离子.加入过量银以沉淀样品溶液中的氯离子,用FAAS法测定银以间接测定氯,或通过测定氯化银悬浮体的表观吸光度而测定氯,建立了FAAS法及比浊法测定聚氯乙烯中氯含量的方法.线性范围:FAAS法为0～140μmol·L-1,比浊法为0.4～4.8 mg·L-1.测定结果的相对标准偏差≤1.9%,加标回收率95.0%～102.5%.两种方法测定结果的相对误差小于士1.1%.     

反向流动注射化学发光法测定盐酸乙胺丁醇

基于盐酸乙胺丁醇与高碘酸钾～鲁米诺反应产生很强的化学发光,结合反向流动注射技术,建立了流动注射化学发光法测定盐酸乙胺丁醇的新方法。在优化的实验条件下,该法的线性范围为4.0×10-8～2×10-5g/mL,检出限为8×10-9g/mL,对6.0×10-7g/mL盐酸乙胺丁醇进行11次平行测定,方法的相对标准偏差为1.9%。该法可用于片剂中盐酸乙胺丁醇的测定。     

固相萃取与超高效液相色谱-质谱联用测定生物样品中芬太尼类物质

建立了固相萃取与液相色谱-质谱(LC-MS)联用分析血清和尿液中10种芬太尼类物质的方法。样品经C18固相萃取(SPE)柱富集分离后,甲醇洗脱,洗脱液采用LC-MS测定。结果表明,尿样基质中,10种芬太尼物质质量浓度在1～100μg/L范围内线性关系良好,相关系数(R²)大于0.99,检出限(LODs)和定量限(LOQs)范围分别为0.18～0.32μg/L和0.61～1.00μg/L。血清基质中,10种芬太尼含量在2～100μg/L范围内呈现良好的线性关系,其R²大于0.99,LODs为0.15～0.33μg/L,LOQs为0.50～1.00μg/L。尿样中芬太尼类物质萃取回收率为84.2%～107.7%,血清中萃取回收率为84.7%～99.7%。该方法适用于生物流体中芬太尼类物质的同步测定。     

水蒸气蒸馏-离子色谱法测定硫化精矿中氟和氯

采用水蒸气蒸馏法分离硫化精矿样品中氟离子和氯离子,离子色谱法测定了氟离子和氯离子的含量。经AG19保护柱及AS19分离柱分离,以25.00mmol·L-1氢氧化钠溶液为淋洗液,采用连续自动再生化学抑制器检测。F-和Cl-的质量浓度均在10.00mg·L-1以内与峰面积呈线性关系,检出限(3s)分别为0.006,0.003mg·L-1。方法用于分析硫化铜精矿、锌精矿和铅精矿,氟离子和氯离子的加标回收率在94.1%～97.2%,96.4%～101%之间,相对标准偏差(n=11)分别在1.5%～2.3%,1.1%～1.9%之间。     

火焰原子吸收法间接测定二氧化硅中的氯

在酸性环境中,氯离子与银离子生成沉淀,经氨水溶解后,以火焰原子吸收法测定银,从而间接测定氯离子的含量。本方法测定氯的线性范围为1.0~30μg/mL,检出限为0.059μg/mL,回收率为95%~105%。将此法应用于二氧化硅中氯离子的测定,结果满意。     

水蒸气蒸馏-离子色谱法测定稀土氧化物中微量和痕量氟和氯

为准确测定高纯稀土氧化物中氟离子和氯离子的含量,建立了水蒸气蒸馏对样品进行前处理,离子色谱法同时测定氟离子和氯离子的分析方法。方法通过硫酸预蒸馏降低空白值。稀土氧化物经硫酸分解,其中的氟和氯随水蒸气逸出与样品分离,经水吸收,用阴离子分离柱分离,以氢氧化钾溶液梯度淋洗,抑制型电导检测器检测。通过保留时间对氟和氯进行定性分析,以标准曲线法对氟和氯进行定量分析,氟和氯的线性相关性为0.9998和0.9997,测定下限均为0.0006%。通过选择样品前处理方式、硫酸用量、样品量、蒸馏时间、吸收液等,确定实验的最佳条件。通过加标回收实验和方法比对实验评估验证方法的准确性,实验表明氟和氯的加标回收率分别在88.20%～99.68%和95.50%～103.46%之间,与现有标准方法GB/T 12690-2003测定结果相比较相对偏差小于5%。通过精密度实验验证方法的稳定性,方法的相对标准偏差氟和氯（n = 11）分别为1.66%～4.12%和1.74%～7.58%。结果表明所建立的分析方法检出限低、精密度良好、准确度高。本方法适用于对高纯稀土氧化物中微量和痕量氟离子和氯离子的快速测定,为高纯稀土氧化物中杂质氟和氯的质量与评价提供技术支撑。     

Gas chromatographic--mass spectrometric determination of phenylacetic acid in human blood

Phenyl acetic acid, a metabolite of 2-phenyl ethylamine, acts as a neuromodulator in the nigrostriatal dopaminergic pathway stimulating the release of dopamine. The evaluation of phenyl acetic acid concentration in the biological fluid reflects phenyl ethylamine levels thus allowing the assessment of the modulatory role of this endogenous substance. Changes in biological fluids levels of 2-phenylethylamine and/or in its metabolite have been reported in affective disorders, such as depression and schizophrenia. Recently, the occurrence of the "attention deficit hyperactivity syndrome" has been frequently reported in childhood population and involvement of dopaminergic dysfunction in this disease has been suspected. A fast, reliable and reproducible method for the determination of phenyl acetic acid in human blood, is therefore needed in order to have a screening tool for monitoring both healthy childhood population and suspected "attention deficit hyperactivity syndrome" patients. The gas chromatographic-mass spectrometric method here described makes use of a deuterated internal standard in order to overcome problems related to the lack of reproducibility often encountered when a derivatization step is performed.     

Kinetics of reduction of palladium(II) complexes with ethylamine on a dropping-mercury electrode

The reduction kinetics of palladium(II) complexes containing ethylamine is studied on a dropping-mercury electrode in solutions of pH 8–13.5 with different ethylamine concentrations in the presence of sodium perchlorate. An irreversible character of the reduction and a diffusion nature of limiting currents are established. Parameters of electrochemical kinetics and diffusion coefficient for the complexes are determined. At pH 11 and 12, the half-wave potential is independent of the ethylamine concentration in the concentration range 0.01 to 0.1 M. Tetraethylamine complexes of palladium(II) predominate in solution and presumably take part in the slow electrochemical step. Raising ethylamine concentration to 2 M makes E _1/2 more negative, due to specific ethylamine adsorption. Limiting currents of two waves, which occur at pH 8 and overall ethylamine concentration 0.01–0.02 M, are used to calculate two constants. One is the step stability constant for complex Pd(eta) ₄ ²⁺ . The other is the equilibrium constant for deprotonation of a ligand in Pd(eta) ₄ ²⁺ , which occurs at pH 13.1–13.5 and ethylamine concentrations 1 and 2 M.     

不纯流动相对离子法分析无机阴离子的影响(英文)

 采用离子模拟研究了流动相不纯对样品中无机阴离子测定造成的干扰。结果表明 ,在流动相中加入Cl-,使得其他 6种阴离子响应值增加。这主要是由于Cl-加入的同时也带来了相应的阳离子 ,在通过抑制器时可带来等量的H+ ,H+ 伴随着各个阴离子样品一起通过检测器 ,使总的样品离子响应值增加。在 6种阴离子中 ,F-和NO-2 对AS14柱的亲和力和Cl-相近 ,其响应值随Cl-加入量的变化趋势相似 ;Br-,NO-3 ,PO3 -4及SO2 -4因其对柱的亲和力大于Cl-,它们的响应值随Cl-加入量的变化趋势也相同。     

微量-乙胺示波极谱测定

本文研究了碱性介质中一乙胺和对硝基苯胺重氮盐所形成偶氮化合物的极谱行为,并建立了微量一乙胺极谱测定方法。该法灵敏度高,对一乙胺的选择性好,可用于水、空气中微量一乙胺的直接测定,结果满意。     

Determination of aliphatic amines in water by liquid chromatography using solid-phase extraction cartridges for preconcentration and derivatization.

Bond Elut C18 solid-phase extraction cartridges were used for preconcentration and pre-column derivatization with 3,5-dinitrobenzoyl chloride (DNB) of aliphatic amines in water. Conditions for analyte preconcentration and derivatization (including the volume of sample, concentration of reagent, time of reaction and pH) were investigated, using ethylamine, isopropylamine and dimethylamine as model compounds. On the basis of these studies, a rapid and sensitive method for the determination of aliphatic amines in water is presented. The analytes are retained and purified on the cartridges and then derivatized and desorbed by drawing in succession the DNB solution and acetonitrile. The collected extracts are subsequently chromatographed in a Hypersil ODS C18 column using acetonitrile-water for elution. The DNB derivatives are monitored at 230 nm. The method provides satisfactory reproducibility and linearity within the 0.050-1.0 mg l(-1) concentration interval, the limits of detection being 2-5 microg l(-1). Analyte recoveries were in the 70-102% range, whereas the conversion yields compared with those observed for the solution derivatization were in the 79-107% range. The total analysis time (sample treatment plus chromatography) was about 15 min. The method was applied to the determination of ethylamine, isopropylamine and dimethylamine in tap and river waters.     

高活性多羟基结构态亚铁FHC(Cl~-)去除Se(Ⅳ)的性能与机制

通过慢速滴定法合成了高活性的多羟基结构亚铁FHC(Cl~-),对FHC(Cl~-)去除Se(Ⅳ)的动力学进行了研究,并对体系中的投加量、pH值、溶解氧和氯化钠浓度进行了响应面分析.研究结果表明,FHC(Cl~-)去除Se(Ⅳ)的表观速率常数k_(obs)=0.60 min~(-1),约为纳米零价铁的4倍和零价铁的16倍.由Box-Benhnken设计拟合得出响应值对编码自变量的二次多项回归方程为Y(c/c_0)=0.14-0.20A+0.017B-0.27C-0.019D-0.047AB-0.095AC+0.13AD-0.010BC-0.082BD+0.33A~2+0.023B~2+0.097C~2+0.065D~2,最优条件为:FHC(Cl~-)投加量98 mg/L,溶液的pH=7.5,氯化钠浓度1 mmol/L,体系为封闭.产物XPS分析结果表明,Se(Ⅳ)最终被FHC(Cl~-)还原为Se(0)或Se(-Ⅱ).     

Effect of Cl~-ion on Anodic Iron Dissolution in H_2S-Containing Sulfuric Acid Solutions

ResearchershavestudiedtheeffectofCI-onthestructureandpropertiesofthecorrosionproductsinchloridesolutionscontainingH,S"'.IthasbeenfoundthattherearenocorrosioneffectsonironsurfaceswhicharesubmergedinconcentratedacidicchloridesolutionswithlowHZSlevel.Inthepast,theinteractionbetweentheCI-ionandFehasnotbeenstudiedcompletelyandintensively.TheanodicreactionofironinacidicsolutionscontainingHZSwastheironoxidationcatalyzedbyHS-3.WhenCI-ispresentinHZS-containingacidicsolutions,theeffectofCI-onir…     

Modulation of Electrochemical Oscillations by Specific Adsorption of Cl^— during the Electrooxidation of Methanol on Pt Electrode

Potential oscillation during the electrocatalytic oxidation of methanol can be modulated by the specific adsorption of Cl^- on the platinum electrode, which suppresses the electrocatalytic oxidation of methanol, and makes the cross cycle in the cyclic voltammogram become smaller and finally disappear with the increase of Cl^- concentration. The method is also applicable to the electrocatalytic oxidation of other small organic molecules.     

二烯丙基乙胺的合成

以乙胺、烯丙基氯和碱为原料合成了二烯丙基乙胺,其结构经1H NMR,FT-IR和元素分析表征。考察了反应物摩尔比、反应温度、反应时间和相转移催化剂用量对收率的影响,采用正交实验设计法对工艺条件进行了优化。较佳的反应条件为:乙胺370 mmol,n(乙胺)∶n(烯丙基氯)∶n(NaOH)=1.0∶2.1∶2.1,PEG-6005 mol%,第一段于42℃反应6 h;第二段于60℃反应7 h,收率71.58%。回用分液所得水相和减压蒸馏所得低沸点馏分,能回收存在于水相和低沸点馏分中的中间产物和产物,收率由71.58%提高到83.66%。     

碱化底液消除水负峰离子色谱法测定水中F~–,Cl~–等7种阴离子

在研究消除水负峰的基础上,建立离子色谱法测定水中F–,Cl–,NO2–,H2PO4–,Br–,NO3–,SO42–7种阴离子的方法。经实验确定淋洗液为4.5 mmol/L NaHCO3–4.0 mmol/L Na2CO3,淋洗液流量为1.0 mL/min,柱箱温度为35℃。在底液中加入与淋洗液同浓度的Na2CO3–NaHCO3可有效消除水负峰。该方法对7种阴离子的检出限为0.004~0.034 mg/L,测定结果的相对标准偏差为0.69%~3.57%(n=6),加标回收率为95%~105%。该法能有效消除水负峰及其对F–测定的影响,操作简便、测定结果准确可靠,适用于水中F–、Cl–等7种阴离子的测定。