The characterization of novel neutral hydrophobic hypercrosslinked polystyrene MN-200 was performed. This resin was shown to exhibit anion-exchange properties in the pH range from 2.6 to 4.3 that can be attributed to the presence of protonated carbonyl groups in the framework of the polymer as no other heteroatoms are present, except for oxygen, responsible for the occurrence of positive charge at the surface. The role of high hydrophobicity of MN-200 in retention of anions is discussed. The anion-exchange selectivity of this sorbent to inorganic anions with diluted perchloric acid solutions as eluent was found to be different from that observed for the common anion-exchangers. The main features of MN-200 are weak retention of sulfate and comparatively strong retention of nitrite that can be useful in practical ion chromatography (IC).
{"title":"Anion-exchange ability of neutral hydrophobic hypercrosslinked polystyrene","authors":"N. Penner, P. Nesterenko","doi":"10.1039/A902449B","DOIUrl":"https://doi.org/10.1039/A902449B","url":null,"abstract":"The characterization of novel neutral hydrophobic hypercrosslinked polystyrene MN-200 was performed. This resin was shown to exhibit anion-exchange properties in the pH range from 2.6 to 4.3 that can be attributed to the presence of protonated carbonyl groups in the framework of the polymer as no other heteroatoms are present, except for oxygen, responsible for the occurrence of positive charge at the surface. The role of high hydrophobicity of MN-200 in retention of anions is discussed. The anion-exchange selectivity of this sorbent to inorganic anions with diluted perchloric acid solutions as eluent was found to be different from that observed for the common anion-exchangers. The main features of MN-200 are weak retention of sulfate and comparatively strong retention of nitrite that can be useful in practical ion chromatography (IC).","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"145 1","pages":"199-201"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"87045048","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
The extraction of alkali metal ions from aqueous solution (K+, Na+ : 1.7 × 10–4 mol dm–3) with supercritical CO2 (scCO2) and crown ethers [18-crown-6 (18C6), 15-crown-5 (15C5)] as ligand was investigated at 40 °C and 8.0–18.0 MPa. The recovery for potassium ion was 1–2% with 18C6 and was independent of pressure. Remarkably, the recovery increased to 40–60% in the presence of the additive pentadecafluoro-n-octanoic acid (PFOA), which is probably because PFOA has CO2-philic fluoroalkyl chains, and easily generates counter ions for the metal–ligand complex. In the case of sodium, the recovery was found to be low even with PFOA, which may be related to the cavity size of 18C6. The 15-crown-5 ligand, having the smaller cavity size increased sodium recovery up to 20–40%. These results show that alkali metals can be extracted with scCO2 and crown ether ligands and further that the recovery of the metals can be greatly increased by adding a substance that can supply a CO2-philic counter ion.
{"title":"Supercritical fluid extraction of alkali metal ions using crown ethers with perfluorocarboxylic acid from aqueous solution","authors":"S. Mochizuki, N. Wada, R. Smith, H. Inomata","doi":"10.1039/A808654K","DOIUrl":"https://doi.org/10.1039/A808654K","url":null,"abstract":"The extraction of alkali metal ions from aqueous solution (K+, Na+ : 1.7 × 10–4 mol dm–3) with supercritical CO2 (scCO2) and crown ethers [18-crown-6 (18C6), 15-crown-5 (15C5)] as ligand was investigated at 40 °C and 8.0–18.0 MPa. The recovery for potassium ion was 1–2% with 18C6 and was independent of pressure. Remarkably, the recovery increased to 40–60% in the presence of the additive pentadecafluoro-n-octanoic acid (PFOA), which is probably because PFOA has CO2-philic fluoroalkyl chains, and easily generates counter ions for the metal–ligand complex. In the case of sodium, the recovery was found to be low even with PFOA, which may be related to the cavity size of 18C6. The 15-crown-5 ligand, having the smaller cavity size increased sodium recovery up to 20–40%. These results show that alkali metals can be extracted with scCO2 and crown ether ligands and further that the recovery of the metals can be greatly increased by adding a substance that can supply a CO2-philic counter ion.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"154 1","pages":"51-52"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"86270592","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
K. Kimura, Kenta Tatsumi, M. Yokoyama, M. Ouchi, M. Mocerino
Calix[4]arene derivatives have been applied as neutral carriers for thallium(I)-selective electrodes, taking advantage of their π-coordination. Calix[4]arene derivatives without any t-butyl group at the upper rim, such as calix[4]arene tetra(propyl ether) and tetra(allyl ether), provided the thallium(I)-selective electrodes with high sensitivity and ion selectivity. t-Butylcalix[4]arene derivatives employed here did not afford very good results as for the thallium(I) neutral carrier. 1H-NMR spectroscopy indicated that thallium(I) complexation by the calixarene neutral carriers is made primarily by π-coordination of their skeletal aromatic rings. The ion-selective electrode based on calix[4]arene tetra(propyl ether) was successfully applied to thallium(I) assays in human urine.
{"title":"Remarkable thallium(I) selectivity for ion sensors based on π-coordination of calix[4]arene neutral carriers","authors":"K. Kimura, Kenta Tatsumi, M. Yokoyama, M. Ouchi, M. Mocerino","doi":"10.1039/A902803J","DOIUrl":"https://doi.org/10.1039/A902803J","url":null,"abstract":"Calix[4]arene derivatives have been applied as neutral carriers for thallium(I)-selective electrodes, taking advantage of their π-coordination. Calix[4]arene derivatives without any t-butyl group at the upper rim, such as calix[4]arene tetra(propyl ether) and tetra(allyl ether), provided the thallium(I)-selective electrodes with high sensitivity and ion selectivity. t-Butylcalix[4]arene derivatives employed here did not afford very good results as for the thallium(I) neutral carrier. 1H-NMR spectroscopy indicated that thallium(I) complexation by the calixarene neutral carriers is made primarily by π-coordination of their skeletal aromatic rings. The ion-selective electrode based on calix[4]arene tetra(propyl ether) was successfully applied to thallium(I) assays in human urine.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"5 1","pages":"229-230"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"78755917","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
A new method was developed for understanding the distribution of chemical species such as mobile-sodium, total-sodium, mobile-chloride, and total-chloride ions in seashell structures. The microwave digestion method was applied for the dissolution of different chemical species of these elements. Several kinds of solutions were used to separate the various species of sodium and chloride ions. Using this method, the distribution of sodium and chloride ions in seashell structures was revealed to differ markedly. Total-sodium ion concentration seemed to be constant in the different layers. Conversely, total-chloride ion concentration was one order of magnitude less than that of total-sodium ion. Mobile-chloride ion concentration also shows that chloride ion is more mobile than sodium ion.The method is effective in measuring the distribution of the elements of seashell structure whilst preventing their contamination from the surroundings and from the reagents used in the procedure. The detection limits were 5 ng g–1 for sodium, and 20 ng g–1 for chloride ion, respectively.
建立了一种新的方法来了解贝壳结构中流动钠离子、总钠离子、流动氯离子和总氯离子等化学物质的分布。采用微波消解法对这些元素的不同化学种类进行了溶出。用不同的溶液分离不同种类的钠离子和氯离子。利用这种方法，发现了钠离子和氯离子在贝壳结构中的分布有明显的差异。总钠离子浓度在不同的层中似乎是恒定的。相反，总氯离子浓度比总钠离子浓度低一个数量级。移动氯离子浓度也表明氯离子比钠离子更具移动性。该方法可以有效地测量贝壳结构元素的分布，同时防止它们受到周围环境和过程中使用的试剂的污染。钠和氯离子的检出限分别为5 ng g-1和20 ng g-1。
{"title":"The use of microwave digestion method for the determination of chemical forms of sodium and chloride ions in seashell structures","authors":"M. Takenaka, M. Ikeda, S. Terada","doi":"10.1039/A809486A","DOIUrl":"https://doi.org/10.1039/A809486A","url":null,"abstract":"A new method was developed for understanding the distribution of chemical species such as mobile-sodium, total-sodium, mobile-chloride, and total-chloride ions in seashell structures. The microwave digestion method was applied for the dissolution of different chemical species of these elements. Several kinds of solutions were used to separate the various species of sodium and chloride ions. Using this method, the distribution of sodium and chloride ions in seashell structures was revealed to differ markedly. Total-sodium ion concentration seemed to be constant in the different layers. Conversely, total-chloride ion concentration was one order of magnitude less than that of total-sodium ion. Mobile-chloride ion concentration also shows that chloride ion is more mobile than sodium ion.The method is effective in measuring the distribution of the elements of seashell structure whilst preventing their contamination from the surroundings and from the reagents used in the procedure. The detection limits were 5 ng g–1 for sodium, and 20 ng g–1 for chloride ion, respectively.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"2 1","pages":"109-111"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"78829182","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Whereas FTIR spectroscopic detection is routinely used in gas chromatography (B. Erikson, Anal. Chem., 1998, 70, 801A), its use for liquid chromatography (LC) and flow injection analysis (FIA) is a rather exotic exception. The most prominent reason is the strong IR absorption of most of the common solvents, especially water. Hence FTIR spectroscopy is normally not even considered a valuable detection method. This practice neglects that FTIR spectroscopy offers some unique features which now, using modern instrumentation, can be exploited in an advantageous manner. It is the aim of this Highlight article to demonstrate the wide range of possible applications in LC and FIA. To regard FTIR spectroscopy as too exotic for routine use may be a luxury paid for with the neglect of a simple analytical approach. The term flow analysis (FA) will be used to provide a common cover for both LC and FIA because both rely on the injection of a sample into a flowing stream, passage through a modulator and recording of transient peaks. Although the processes taking place in the modulator are different, being chemical reactions in FIA and separations in LC, the same interfaces can be used for a FTIR spectrometer as a detector. The interfaces used can be divided into two categories, flow through cells where the liquid is probed directly, and solvent removal interfaces where the analyte is separated from the carrier liquid prior to detection. It is necessary to emphasize the complementary nature of these techniques (D. E. Pivonka and K. M. Kirkland, Appl. Spectrosc., 1997, 51, 866) and this Highlight will stress their particular strengths and weaknesses. Special focus is laid on aqueous phase systems because of their high importance in biological systems. As water is certainly the most challenging solvent for IR detection, equal or even better performance of the presented approaches can be expected for other solvents. Additionally three developments will be discussed in detail with respect to their prospects for FA-FTIR instruments: the increasing availability of sophisticated chemometric methods, the miniaturization of analytical instruments and applicaton to combinatorial chemistry.
而FTIR光谱检测通常用于气相色谱(B. Erikson, Anal。化学。， 1998,70,801a)，但它在液相色谱(LC)和流动注射分析(FIA)中的应用是一个相当奇特的例外。最突出的原因是对大多数常见溶剂，尤其是水有较强的红外吸收性。因此，FTIR光谱通常甚至不被认为是一种有价值的检测方法。这种做法忽略了FTIR光谱提供了一些独特的特征，现在使用现代仪器，可以以有利的方式加以利用。这篇重点文章的目的是演示LC和FIA中广泛的可能应用。认为FTIR光谱学过于新奇而不适合常规使用可能是一种奢侈，因为它忽视了一种简单的分析方法。术语流动分析(FA)将用于为LC和FIA提供一个共同的掩护，因为两者都依赖于将样品注入流动的流中，通过调制器并记录瞬态峰值。虽然在调制器中发生的过程是不同的，是FIA中的化学反应和LC中的分离，但相同的界面可以用于FTIR光谱仪作为检测器。所使用的界面可分为两类，一种是直接探测液体的流过细胞，另一种是在检测之前将分析物从载体液体中分离出来的溶剂去除界面。有必要强调这些技术的互补性(D. E. Pivonka和K. M. Kirkland, apple)。Spectrosc。， 1997,51,866)，本重点将强调其特定的长处和弱点。由于水相系统在生物系统中具有很高的重要性，因此特别关注水相系统。由于水无疑是红外检测中最具挑战性的溶剂，对于其他溶剂，可以期望所提出的方法具有相同甚至更好的性能。此外，将详细讨论FA-FTIR仪器的三个发展前景:复杂化学计量方法的日益普及，分析仪器的小型化和组合化学的应用。
{"title":"FTIR spectroscopy as detection principle in aqueous flow analysis","authors":"R. Schindler, B. Lendl","doi":"10.1039/A901196J","DOIUrl":"https://doi.org/10.1039/A901196J","url":null,"abstract":"Whereas FTIR spectroscopic detection is routinely used in gas chromatography (B. Erikson, Anal. Chem., 1998, 70, 801A), its use for liquid chromatography (LC) and flow injection analysis (FIA) is a rather exotic exception. The most prominent reason is the strong IR absorption of most of the common solvents, especially water. Hence FTIR spectroscopy is normally not even considered a valuable detection method. This practice neglects that FTIR spectroscopy offers some unique features which now, using modern instrumentation, can be exploited in an advantageous manner. It is the aim of this Highlight article to demonstrate the wide range of possible applications in LC and FIA. To regard FTIR spectroscopy as too exotic for routine use may be a luxury paid for with the neglect of a simple analytical approach. The term flow analysis (FA) will be used to provide a common cover for both LC and FIA because both rely on the injection of a sample into a flowing stream, passage through a modulator and recording of transient peaks. Although the processes taking place in the modulator are different, being chemical reactions in FIA and separations in LC, the same interfaces can be used for a FTIR spectrometer as a detector. The interfaces used can be divided into two categories, flow through cells where the liquid is probed directly, and solvent removal interfaces where the analyte is separated from the carrier liquid prior to detection. It is necessary to emphasize the complementary nature of these techniques (D. E. Pivonka and K. M. Kirkland, Appl. Spectrosc., 1997, 51, 866) and this Highlight will stress their particular strengths and weaknesses. Special focus is laid on aqueous phase systems because of their high importance in biological systems. As water is certainly the most challenging solvent for IR detection, equal or even better performance of the presented approaches can be expected for other solvents. Additionally three developments will be discussed in detail with respect to their prospects for FA-FTIR instruments: the increasing availability of sophisticated chemometric methods, the miniaturization of analytical instruments and applicaton to combinatorial chemistry.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"276 1","pages":"123-126"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"73296771","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Steam or superheated water can be used to efficiently elute moderately polar and non-polar compounds from polymeric sorbents at temperatures up to 220 °C without degradation of the analyte. Acetophenone and m-cresol, as model compounds, have been concentrated from dilute aqueous solutions, using solid phase extraction (SPE) traps packed with polystyrene–divinylbenzene (PS–DVB) or poly(divinylbenzene-co-N-vinylpyrrolidone). The technique offers low cost, ease of use and an environmentally friendly eluent.
蒸汽或过热水可用于在高达220°C的温度下有效地从聚合物吸附剂中洗脱中等极性和非极性化合物，而不会降解分析物。苯乙酮和间甲酚，作为模型化合物，从稀水溶液中，使用固相萃取(SPE)陷阱填充聚苯二乙烯基苯(PS-DVB)或聚二乙烯基苯-co- n -乙烯基吡咯烷酮。该技术成本低，使用方便，是一种环保的洗脱液。
{"title":"Solid phase extraction and thermal desorption of acetophenone and m-cresol using superheated water or steam as the sole eluent","authors":"Joanne R. Bone, Roger M. Smith","doi":"10.1039/A907707C","DOIUrl":"https://doi.org/10.1039/A907707C","url":null,"abstract":"Steam or superheated water can be used to efficiently elute moderately polar and non-polar compounds from polymeric sorbents at temperatures up to 220 °C without degradation of the analyte. Acetophenone and m-cresol, as model compounds, have been concentrated from dilute aqueous solutions, using solid phase extraction (SPE) traps packed with polystyrene–divinylbenzene (PS–DVB) or poly(divinylbenzene-co-N-vinylpyrrolidone). The technique offers low cost, ease of use and an environmentally friendly eluent.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"51 1","pages":"375-377"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"76569787","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
F. Tateo, M. Bononi, E. D. Dominicis, V. Fumagalli
The enantiomeric ratios of camphor have been determined in authentic essential oils, using heptakis(6-O-t-butylsilyl-2,3-di-O-ethyl)-β-cyclodextrin as the chiral stationary phase. An enantiomeric excess of (1S)-(–) within 72–75% is characteristic of coriander oil (Coriandrum sativum L.). Contrary, an enantiomeric excess of (1R)-(+) characterizes the essential oils of sage (>90% for Salvia sclarea L. and 50–70% for Salvia officinalis L.) and of basil (>94% for Ocimum basilicum L.).
以七烷基(6- o -t-丁基硅基-2,3-二- o -乙基)-β-环糊精为手性固定相，测定了樟脑在精油中的对映体比例。香菜油(Coriandrum sativum L.)的对映体(1S)-(-)含量在72-75%之间过量。相反，鼠尾草(鼠尾草)和罗勒(basilicum L.)精油中(1R)-(+)的对映体过量(>)为90%，鼠尾草为50% - 70%)和罗勒(basimum basilicum L.)为94%。
{"title":"Update on enantiomeric composition of (1R)-(+)- and (1S)-(–)-camphor in essential oils by enantioselective gas chromatography","authors":"F. Tateo, M. Bononi, E. D. Dominicis, V. Fumagalli","doi":"10.1039/A901388A","DOIUrl":"https://doi.org/10.1039/A901388A","url":null,"abstract":"The enantiomeric ratios of camphor have been determined in authentic essential oils, using heptakis(6-O-t-butylsilyl-2,3-di-O-ethyl)-β-cyclodextrin as the chiral stationary phase. An enantiomeric excess of (1S)-(–) within 72–75% is characteristic of coriander oil (Coriandrum sativum L.). Contrary, an enantiomeric excess of (1R)-(+) characterizes the essential oils of sage (>90% for Salvia sclarea L. and 50–70% for Salvia officinalis L.) and of basil (>94% for Ocimum basilicum L.).","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"234 2 1","pages":"149-151"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77016750","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
A number of trace-level inorganic anions in sea-water have been separated efficiently by capillary zone electrophoresis using direct UV detection. The carrier electrolyte contained 100 mM KCl at pH 4.0, which offered the possibility of preventing interference from high matrix salinity and avoided the use of an additional flow modifier. As a result, no impact of the chloride ion on the migration of high-mobility anions was observed and short migration times (within 8 min) were obtained by operating at a relatively low applied voltage (–10 kV). Modifications to the carrier electrolyte composition by incorporating 18-crown-6 or tetrabutylammonium chloride were found essential for furnishing the appropriate resolution. The role of ion-association and ion-inclusion interactions, taking place in the electrophoretic system and resulting in variations of the separation selectivity, are discussed. The problem of improving the detection sensitivity for quantification of inorganic anions in sea-water is also briefly addressed.
采用毛细管区带电泳直接紫外检测法对海水中多种微量无机阴离子进行了高效分离。载体电解质在pH 4.0下含有100 mM KCl，这提供了防止高基质盐度干扰的可能性，并且避免了使用额外的流动调节剂。因此，氯离子对高迁移率阴离子的迁移没有影响，并且在相对较低的施加电压(-10 kV)下操作，可以获得较短的迁移时间(在8分钟内)。通过加入18-冠-6或四丁基氯化铵对载体电解质组成进行修饰，可以获得适当的分辨率。离子结合和离子包涵相互作用的作用，发生在电泳系统和导致分离选择性的变化，进行了讨论。本文还简要讨论了提高海水中无机阴离子定量检测灵敏度的问题。
{"title":"Separation of inorganic anions for analysis of sea-water by capillary zone electrophoresis","authors":"A. Timerbaev, T. Takayanagi, S. Motomizu","doi":"10.1039/A900323A","DOIUrl":"https://doi.org/10.1039/A900323A","url":null,"abstract":"A number of trace-level inorganic anions in sea-water have been separated efficiently by capillary zone electrophoresis using direct UV detection. The carrier electrolyte contained 100 mM KCl at pH 4.0, which offered the possibility of preventing interference from high matrix salinity and avoided the use of an additional flow modifier. As a result, no impact of the chloride ion on the migration of high-mobility anions was observed and short migration times (within 8 min) were obtained by operating at a relatively low applied voltage (–10 kV). Modifications to the carrier electrolyte composition by incorporating 18-crown-6 or tetrabutylammonium chloride were found essential for furnishing the appropriate resolution. The role of ion-association and ion-inclusion interactions, taking place in the electrophoretic system and resulting in variations of the separation selectivity, are discussed. The problem of improving the detection sensitivity for quantification of inorganic anions in sea-water is also briefly addressed.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"31 1","pages":"139-141"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"81211843","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
A major experimental consideration, and often a difficulty when interfacing capillary electrophoresis (CE) with plasma mass spectrometry via a pneumatic nebulizer, is the suction effect caused by the natural aspiration of the nebulizer. This has a marked affect on the CE experiment, since it may lead to peak overlap and, ultimately, a completely degraded separation. Placing a sol–gel frit in the sample introduction end of the capillary in a CE system, interfaced with a pneumatic nebulizer at the outlet end of the capillary, minimizes the suction effect. A two-tube oscillating capillary nebulizer (OCN) was used in this study because of its very low liquid flow capacity and potential for interfacing to ICP-MS. To test the fritted capillary for possible application to CE-ICP-MS, standard ultraviolet (UV) absorbance detection was used for the CE separation of metallothionein and ferritin with a grounded nebulizer interface at one end of the capillary. With the capillary frit and OCN interface, reasonably true electropherograms were obtained when compared to the CE separation performed in the traditional mode without a frit and with a buffer reservoir in place at the outlet. Also, during this study it was found that a make-up buffer was necessary to maintain electrical contact to the outlet of the fritted electrophoretic capillary when using the OCN.
{"title":"The use of sol–gel frits to minimize suction effects in capillary electrophoresis–nebulizer interfaces for plasma spectrometry†","authors":"C. B’hymer, R. Sutton, K. Sutton, J. Caruso","doi":"10.1039/A905088D","DOIUrl":"https://doi.org/10.1039/A905088D","url":null,"abstract":"A major experimental consideration, and often a difficulty when interfacing capillary electrophoresis (CE) with plasma mass spectrometry via a pneumatic nebulizer, is the suction effect caused by the natural aspiration of the nebulizer. This has a marked affect on the CE experiment, since it may lead to peak overlap and, ultimately, a completely degraded separation. Placing a sol–gel frit in the sample introduction end of the capillary in a CE system, interfaced with a pneumatic nebulizer at the outlet end of the capillary, minimizes the suction effect. A two-tube oscillating capillary nebulizer (OCN) was used in this study because of its very low liquid flow capacity and potential for interfacing to ICP-MS. To test the fritted capillary for possible application to CE-ICP-MS, standard ultraviolet (UV) absorbance detection was used for the CE separation of metallothionein and ferritin with a grounded nebulizer interface at one end of the capillary. With the capillary frit and OCN interface, reasonably true electropherograms were obtained when compared to the CE separation performed in the traditional mode without a frit and with a buffer reservoir in place at the outlet. Also, during this study it was found that a make-up buffer was necessary to maintain electrical contact to the outlet of the fritted electrophoretic capillary when using the OCN.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"09 1","pages":"349-353"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"80036553","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
C. Winstead, F. Mazzotti, J. Mierzwa, G. P. Miller
We report the first experimental results using electrothermal atomization-cavity ringdown spectroscopy for trace elemental analysis. Lead aqueous standard solutions were analyzed using graphite furnace-cavity ringdown spectroscopy and a preliminary detection limit of approximately 1 pg was obtained for peak height absorption measurements. No chemical matrix modifiers were used. These preliminary results together with an estimate of theoretical detection limits suggest that the coupling of ETA and CRDS has the potential to become a valuable new technique in analytical atomic spectrometry.
{"title":"Preliminary results for electrothermal atomization-cavity ringdown spectroscopy (ETA-CRDS)","authors":"C. Winstead, F. Mazzotti, J. Mierzwa, G. P. Miller","doi":"10.1039/A903563J","DOIUrl":"https://doi.org/10.1039/A903563J","url":null,"abstract":"We report the first experimental results using electrothermal atomization-cavity ringdown spectroscopy for trace elemental analysis. Lead aqueous standard solutions were analyzed using graphite furnace-cavity ringdown spectroscopy and a preliminary detection limit of approximately 1 pg was obtained for peak height absorption measurements. No chemical matrix modifiers were used. These preliminary results together with an estimate of theoretical detection limits suggest that the coupling of ETA and CRDS has the potential to become a valuable new technique in analytical atomic spectrometry.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"96 1","pages":"277-279"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"80075602","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
京公网安备 11010802042870号
京ICP备2023020795号-1
扫码关注我们
求助内容：
应助结果提醒方式：