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发展了用咪唑离子液体作为流动相添加剂的亲水作用色谱-间接紫外检测四丁基磷和四丁基铵的分析方法。研究了咪唑离子液体、吡啶离子液体作为流动相添加剂对四丁基磷和四丁基铵分析的影响,考察了咪唑离子液体的浓度、有机溶剂含量、检测波长等因素的影响,并讨论了离子液体的作用。采用亲水作用色谱柱,以乙腈-1.0 mmol/L 1-乙基-3-甲基咪唑四氟硼酸盐(体积比60∶40)为流动相,在色谱柱温度30℃,流速1.0 mL/min,紫外检测波长210 nm条件下,四丁基磷和四丁基铵离子在15 min内得到完全分离。检出限为1.0~1.2 mg/L,线性和重现性良好。将此方法应用于松花江水样品和克音河水样品的分析,加标回收率为95.9%~107%。该方法简单,易于应用。 相似文献
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《化学研究与应用》2015,(9)
建立了以咪唑离子液体为流动相的液相色谱-间接紫外检测分析N-甲基,丙基吗啉阳离子的方法。用反相硅胶整体柱,以咪唑离子液体-离子对试剂水溶液/有机溶剂为流动相测定吗啉阳离子。咪唑离子液体为背景紫外吸收试剂。研究了咪唑离子液体、检测波长、离子对试剂、有机溶剂、柱温、流速对测定吗啉阳离子的影响,探讨了保留规律。以0.5 mmol·L-11-乙基-3-甲基咪唑四氟硼酸盐-0.1 mmol·L-1庚烷磺酸钠水溶液/甲醇(85∶15,v/v)为流动相,检测波长210 nm,柱温30℃,流速1.0 m L·min-1,N-甲基,丙基吗啉阳离子的保留时间为2.397 min,检出限(S/N=3)为0.02 mg·L-1,峰面积的相对标准偏差(n=5)为1.1%,保留时间的相对标准偏差(n=5)为0.03%。将此方法用于分析实验室合成的N-甲基,丙基吗啉离子液体,加标回收率为100.5%。本方法简便、快捷,可满足N-甲基,丙基吗啉离子液体阳离子的定量分析要求。 相似文献
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以咪唑离子液体作为流动相添加剂,建立了哌啶离子液体阳离子的整体柱离子对色谱-间接紫外检测分析方法。系统研究了流动相、流速等因素对哌啶阳离子分离测定的影响情况。流动相中的咪唑离子液体不仅起到了背景紫外吸收剂的作用,还改善了阳离子的分离效果。用0.5mmol/L 1-乙基-3-甲基咪唑四氟硼酸盐-0.1mmol/L庚烷磺酸盐水溶液(pH=4.5)/甲醇(90/10,V/V)作为流动相,流速3.0mL/min,检测波长210nm,N-甲基-N-乙基、N-甲基-N-丙基和N-甲基-N-丁基哌啶阳离子在3.0min之内实现基线分离。3种哌啶阳离子的检出限分别为0.13、0.34和0.42mg/L。该方法测定实验室合成的哌啶离子液体样品的加标回收率范围为94%~98%。 相似文献
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建立了快速分析无紫外光吸收的哌啶离子液体阳离子的离子对色谱-间接紫外检测法。采用反相C18色谱柱,以背景紫外吸收试剂-离子对试剂水溶液/有机溶剂为流动相分离哌啶离子液体阳离子。研究了背景紫外吸收试剂、检测波长、离子对试剂、有机溶剂、柱温、流速对分离测定哌啶阳离子的影响。最佳色谱条件为:以0.5 mmol/L对氨基苯酚盐酸盐-0.1 mmol/L庚烷磺酸钠水溶液/甲醇(80:20,v/v)为流动相,检测波长210 nm,柱温30 ℃,流速1.0 mL/min。在此条件下,3种哌啶阳离子可在4 min之内基线分离。所测阳离子的检出限(S/N=3)为0.137~0.545 mg/L,峰面积和保留时间的相对标准偏差(n=5)分别不高于0.72%和0.37%。将此方法用于分析实验室合成的哌啶类离子液体,加标回收率为97.0%~98.4%。本方法简便、快速,重现性、线性关系等均能满足哌啶类离子液体阳离子的定量分析要求。 相似文献
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建立了快速分析无紫外光吸收的吡咯烷离子液体阳离子的离子对色谱-间接紫外检测法。采用反相硅胶整体柱,以(背景紫外吸收试剂-离子对试剂)水溶液-有机溶剂为流动相,分别讨论了背景紫外吸收试剂、检测波长、离子对试剂、有机溶剂、柱温及流速对分离测定吡咯烷阳离子的影响。最佳色谱条件为:以80%(V/V)(0.5 mmol/L对氨基苯酚盐酸盐-0.1 mmol/L庚烷磺酸钠)水溶液-20%(V/V)甲醇为流动相,检测波长230 nm,柱温30℃,流速2.0 mL/min。在此条件下,N-甲基,乙基吡咯烷阳离子、N-甲基,丙基吡咯烷阳离子和N-甲基,丁基吡咯烷阳离子在1.6 min之内基线分离,检出限(S/N=3)分别为0.02,0.03和0.07 mg/L,相对标准偏差(n=5)小于0.4%。将此方法用于分析实验室合成的离子液体样品,加标回收率在97.4%~98.0%之间。本方法快速、简单、准确、可靠,具有良好的实用性。 相似文献
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离子液体作高效液相色谱流动相添加剂分离测定芳香胺 总被引:3,自引:0,他引:3
建立了以离子液体作反相高效液相色谱流动相添加剂分离测定邻苯二胺、苯胺和对甲苯胺3种芳香胺的方法。实验以C18反相色谱柱为分离柱,采用紫外检测方法,考察了检测波长、甲醇含量、咪唑离子液体烷基链长度、离子液体溶液浓度等条件对分离和测定的影响,并与其它分离测定芳香胺的方法进行了比较。优化的色谱条件为:以甲醇/1-丁基-3-甲基咪唑四氟硼酸盐水溶液(3.0mmol/L,乙酸调节pH 3.5)=30/70(V/V)为流动相;检测波长254 nm;流速1.0mL/min;柱温30℃。在此条件下,3种芳香胺达到基线分离,在6.5 min之内分离完全;在1~40 mg/L范围内,线性回归方程的相关系数达到0.99以上;检出限为0.07~0.41 mg/L。将本方法应用于废水的测定,加标回收率在92.3%~96.7%之间,相对标准偏差小于3.5%。 相似文献
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离子液体作高效液相色谱流动相添加剂分离测定芳香族羧酸 总被引:1,自引:0,他引:1
以离子液体作反相高效液相色谱流动相添加剂,建立了分离测定对氨基苯甲酸、邻苯二甲酸、对羟基苯甲酸、水杨酸、苯甲酸、邻甲苯甲酸6种芳香族羧酸的方法。以C18反相色谱柱为分离柱,采用紫外检测方法,以离子液体作高效液相色谱流动相添加剂,考察了检测波长、甲醇含量、离子液体溶液的pH值、离子液体烷基链长度以及离子液体溶液浓度等分离及测定条件。优化得到的色谱条件为:以甲醇和1.0mmol/L 1-丁基-3-甲基咪唑四氟硼酸盐水溶液(pH 3.0)(体积比40∶60)为流动相;检测波长240 nm;流速1.0 mL/min;柱温30℃。在优化条件下对6种芳香族羧酸进行梯度洗脱,约在16.5 min内分离完全;在5~120 mg/L范围内,线性系数均在0.999以上;检出限为0.026~0.082 mg/L。方法的平均加标回收率为98.3%~103.8%,相对标准偏差不高于0.63%。将该方法应用于药品复方紫荆皮水杨酸溶液和足君清酊剂中芳香族羧酸的测定,结果满意。 相似文献
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研究了不同背景紫外吸收试剂对无紫外光吸收的烷基磺酸盐检测的影响。采用反相C18色谱柱的高效液相色谱-间接紫外检测法,以背景紫外吸收试剂-有机溶剂为流动相分离烷基磺酸盐。研究不同背景紫外吸收试剂对分离检测烷基磺酸盐的影响规律和分离机理。结果表明,不同类型的背景紫外吸收试剂测定烷基磺酸盐的色谱峰类型不同。阳离子型背景紫外吸收试剂测定烷基磺酸盐时,样品峰均为正峰;阴离子型和两性离子型背景紫外吸收试剂时,样品峰均为倒峰。比较不同的背景紫外吸收试剂,发现采用阳离子型紫外吸收试剂测定烷基磺酸盐的色谱峰更好,其中以咪唑离子液体最佳,检测响应值最高。 相似文献
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Philip Rosen 《International journal of quantum chemistry》1975,9(3):473-478
A theory of UV carcinogenesis is described in which damage to DNA in the form of pyrimidine dimers occurs in a critical operator region of the genome that controls the synthesis of divisional proteins. There is a chance that a mutation will occur in the region of the operator either during replication or during postreplication repair, so that unchecked growth will be passed on to daughter cells. Comparison with the experiments of Hart and Setlow (1973) indicates that agreement is semiquantitative. 相似文献
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Volker Dose 《Progress in Surface Science》1983,13(3):225-283
Recent experimental progress has introduced Bremsstrahlung spectroscopy especially in the isochromat mode as a new surface analytical tool. Bremsstrahlung production may be regarded as radiative capture by solids and is therefore the inverse process to the well known photoemission. In contrast to photoemission which probes occupied electronic states at solid surfaces, Bremsstrahlung spectroscopy opens up the possibility to investigate unoccupied electronic states including the important region between Fermi- and vacuum energy. Measurements on polycrystalline materials will be discussed on the basis of an isotropic three step model for Bremsstrahlung emission. More recent experiments on single crystals with electrons of well defined energy and initial momentum have demostrated that -resolved spectroscopy provides energy versus momentum dispersion relations for unoccupied bands. Application of spin polarized electron beams has advanced -resolved Bremsstrahlung spectroscopy to a state of maturity comparable to spin polarized angle resolved photoemission. This paper attempts to review the development and summarize the present state of ultraviolet Bremsstrahlung isochromat spectroscopy. 相似文献
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Hiroaki Imai Koichi Awazu Masarux Yasumori Hideo Onuki Hiroshi Hirashima 《Journal of Sol-Gel Science and Technology》1997,8(1-3):365-369
Structural changes in SiO2 and TiO2 gel films were investigated using ultraviolet (UV) and vacuum ultraviolet (VUV) irradiations. A significant compaction with dehydration of SiO2 gel films was induced by irradiation of photons in the range of 9–18 eV. The refractive index and the shrinkage of the irradiated SiO2 gel films were comparable to those obtained by sintering at 1000°C. Densification of TiO2 gel films was also observed with irradiation of 5–14 eV photons. However, effects of the irradiation on TiO2 gel were smaller that those on SiO2 gel. The structural changes in the gel films are attributed to electronic excitations which are induced by irradiation with photons having higher energies than the bandgap of the oxides. The photo-induced effects are presumed to depend on the optical properties and structure of the gels. 相似文献
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Conclusions The ionization constants of the 5-hydroxy groups in tectochrysin and chrysin have been determined spectrophotometrically, being 2.09×10–12 and 8.91×10–10, respectively. The 7-hydroxy group of chrysin has an ionization constant of 3.8 × 10–8.Khimiya Prirodnykh Soedinenii, Vol. 6, No. 1, pp. 24–27, 1970 相似文献
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Chemistry of Natural Compounds - The ionization constants of the 5-hydroxy groups in tectochrysin and chrysin have been determined spectrophotometrically, being 2.09×10?12 and... 相似文献
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Vacuum Ultraviolet Irradiation of Polymers 总被引:2,自引:0,他引:2
The interest in incoherent sources for wavelength-selective photochemistry has increased lately, but little is still known about the behavior of polymers when exposed to far UV and vacuum UV (VUV) radiation. The same dearth of information exists regarding UV (VUV) radiation emitted by low-pressure plasmas during polymer treatment. In order to study VUV-UV effects on several polymers (polyethylene - PE, polystyrene - PS, hexatriacontane - HTC, and poly(methyl methacrylate) - PMMA), we have used the well-characterized emissions from hydrogen (broad-band emission) and hydrogen/argon mixture (near-monochromatic radiation) plasmas as light sources. During irradiation, samples were kept under vacuum or in a flow of pure oxygen at low pressure; in both cases the radiation fluxes at the sample position have been precisely determined by careful spectroscopic calibration experiments. We have employed a quartz crystal microbalance (QCM) to measure in-situ any possible mass change of the various polymers. Following irradiation, samples were analysed by ellipsometry (for thickness and refractive index), X-ray photoelectron spectroscopy (XPS, to evaluate the near-surface composition and content of various functional groups), and atomic force microscopy (AFM, for surface topography and roughness measurements). 相似文献
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GdVO4:Eu^3+的真空紫外激发光谱研究 总被引:4,自引:1,他引:3
报道GdVO4:Eu^3 的光致发光光谱和真空紫外-紫外激发光谱。GdVO4:Eu^3 是高效率的真空紫外-紫外激发荧光材料。GdVO4:Eu^3 在60-350nm真空紫外-紫外波段的激发可能主要来源于基质的吸收,有明显的Eu^3 及Gd^3 的4f^n-15d吸收,在GdVO4:Eu^3 中,存在如下能量传递过程:VO4^3-→Eu^3 ,Gd^3 →Eu^3 ,Gd^3 →VO4^3-→Eu^3 ;通过后两个过程,Gd^3 -Eu^3 可实现量子剪裁。 相似文献