F. Vanhaecke, Marieke Verstraete, L. Moens, R. Dams
Electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICPMS) was used for the determination of the Pd content in a solid aliphatic polyketone. The presence of Pd in this material has to be attributed to the use of a Pd-containing homogeneous catalyst for its production. By application of a multi-step heating programme, the organic matrix could be selectively and completely removed prior to the vaporization of the analyte element. The accuracy attainable when using (i) external calibration and (ii) single standard addition using an aqueous standard solution was evaluated by comparison of the results obtained with a reference value obtained by means of neutron activation analysis (NAA). On the basis of its similar furnace behaviour, Ir was shown to be perfectly suited to be used as an internal standard. Also the argon dimer signal (Ar2+) shows some potential to be used as an internal standard. When using Ir or Ar2+ as an internal standard and single standard addition for calibration, the ETV-ICPMS result (∼5 µg g–1) agreed within 10% with the NAA result on each occasion (deviation between average ETV-ICPMS result and reference value ∼2%). The absolute limit of detection (3s-criterion) was observed to be ∼1 pg, corresponding to a relative value of ∼1 ng g–1, taking 1 mg as a typical sample mass. However, when using Ir as an internal standard, it was established that the detection limit deteriorated to ∼20 pg, due to the presence of a measurable amount of Pd in the Ir standard solution.
{"title":"Determination of the palladium content in a solid plastic material by electrothermal vaporization ICP-mass spectrometry (ETV-ICPMS)","authors":"F. Vanhaecke, Marieke Verstraete, L. Moens, R. Dams","doi":"10.1039/A809318K","DOIUrl":"https://doi.org/10.1039/A809318K","url":null,"abstract":"Electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICPMS) was used for the determination of the Pd content in a solid aliphatic polyketone. The presence of Pd in this material has to be attributed to the use of a Pd-containing homogeneous catalyst for its production. By application of a multi-step heating programme, the organic matrix could be selectively and completely removed prior to the vaporization of the analyte element. The accuracy attainable when using (i) external calibration and (ii) single standard addition using an aqueous standard solution was evaluated by comparison of the results obtained with a reference value obtained by means of neutron activation analysis (NAA). On the basis of its similar furnace behaviour, Ir was shown to be perfectly suited to be used as an internal standard. Also the argon dimer signal (Ar2+) shows some potential to be used as an internal standard. When using Ir or Ar2+ as an internal standard and single standard addition for calibration, the ETV-ICPMS result (∼5 µg g–1) agreed within 10% with the NAA result on each occasion (deviation between average ETV-ICPMS result and reference value ∼2%). The absolute limit of detection (3s-criterion) was observed to be ∼1 pg, corresponding to a relative value of ∼1 ng g–1, taking 1 mg as a typical sample mass. However, when using Ir as an internal standard, it was established that the detection limit deteriorated to ∼20 pg, due to the presence of a measurable amount of Pd in the Ir standard solution.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"39 1","pages":"89-92"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"84294838","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}
{"title":"Influence of functional and cross-linking monomers and the amount of template on the performance of molecularly imprinted polymers in binding assays","authors":"E. Yilmaz, K. Mosbach, K. Haupt","doi":"10.1039/A901339C","DOIUrl":"https://doi.org/10.1039/A901339C","url":null,"abstract":"","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"60 1","pages":"167-170"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"84638272","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}
{"title":"Recent developments in the analysis of light isotopes by continuous flow isotope ratio mass spectrometry","authors":"A. J. Midwood","doi":"10.1039/A904908H","DOIUrl":"https://doi.org/10.1039/A904908H","url":null,"abstract":"","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"34 1","pages":"291-294"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"73256504","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 piezoresonators of a quartz-crystal microbalance were surface-coated with electropolymerised polypyrrole films. After potentiostatic reduction at –0.9 V, the reduced PPy-coated resonators were allowed to react with solutions containing different concentrations of CrVI. Mass changes of the polymer film, originated by ionic transfer during the oxidation reaction of PPy by hexavalent chromium, produced frequency shifts proportional to the concentration of CrVI. Also, frequency shifts were obtained by reaction of some antioxidants at oxidised PPy-coated resonators. The observed responses depend on several experimental parameters.
{"title":"A polypyrrole-coated, piezoelectric sensor for CrVI. Preliminary results","authors":"E. Desimoni, I. Bassani","doi":"10.1039/A809667H","DOIUrl":"https://doi.org/10.1039/A809667H","url":null,"abstract":"The piezoresonators of a quartz-crystal microbalance were surface-coated with electropolymerised polypyrrole films. After potentiostatic reduction at –0.9 V, the reduced PPy-coated resonators were allowed to react with solutions containing different concentrations of CrVI. Mass changes of the polymer film, originated by ionic transfer during the oxidation reaction of PPy by hexavalent chromium, produced frequency shifts proportional to the concentration of CrVI. Also, frequency shifts were obtained by reaction of some antioxidants at oxidised PPy-coated resonators. The observed responses depend on several experimental parameters.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"69 1","pages":"45-46"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"73645797","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}
Near-infrared (NIR) reflectance spectroscopy has been used to monitor the chemical inter-conversion of resin-bound functional groups. Measurements required no sample preparation and were made directly through the bottom of the glass reaction vessel. The time–concentration profile of the esterification of a resin-bound alcohol by acetic anhydride in a toluene medium is demonstrated.
{"title":"Non-destructive real-time reaction monitoring in solid phase synthesis by near-infrared reflectance spectroscopy—esterification of a resin-bound alcohol","authors":"Jonathan Hammond, A. Moffat, R. D. Jee, B. Kellam","doi":"10.1039/A900747D","DOIUrl":"https://doi.org/10.1039/A900747D","url":null,"abstract":"Near-infrared (NIR) reflectance spectroscopy has been used to monitor the chemical inter-conversion of resin-bound functional groups. Measurements required no sample preparation and were made directly through the bottom of the glass reaction vessel. The time–concentration profile of the esterification of a resin-bound alcohol by acetic anhydride in a toluene medium is demonstrated.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"180 1","pages":"127-129"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"75137808","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. Skudar, O. Brüggemann, A. Wittelsberger, O. Ramström
Molecularly imprinted polymers (MIPs) to penicillin V or oxacillin were prepared, and their recognition properties were investigated, both in organic and aqueous phases. The resulting MIPs proved to be efficient in distinguishing between different penicillins (penicillin V, penicillin G and oxacillin), but could also be prepared to recognise the penicillins as a group. The results indicate that MIPs can be used to prepare either selective or general recognition matrices for penicillins, which can be of potential use in separation and detection applications.
{"title":"Selective recognition and separation of β-lactam antibiotics using molecularly imprinted polymers","authors":"K. Skudar, O. Brüggemann, A. Wittelsberger, O. Ramström","doi":"10.1039/A905151A","DOIUrl":"https://doi.org/10.1039/A905151A","url":null,"abstract":"Molecularly imprinted polymers (MIPs) to penicillin V or oxacillin were prepared, and their recognition properties were investigated, both in organic and aqueous phases. The resulting MIPs proved to be efficient in distinguishing between different penicillins (penicillin V, penicillin G and oxacillin), but could also be prepared to recognise the penicillins as a group. The results indicate that MIPs can be used to prepare either selective or general recognition matrices for penicillins, which can be of potential use in separation and detection applications.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"23 1","pages":"327-331"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"81504379","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. Baggiani, G. Giraudi, C. Giovannoli, A. Vanni, F. Trotta
Polymers able to bind the pesticide bentazone were prepared by utilising the technique of the non-covalent molecular imprinting polymerisation and using different molar ratios of methacrylic acid and 4-vinylpyridine as interacting monomers. Polymers obtained were packed in HPLC columns and the imprinting effect was studied using chloroform and acetonitrile as mobile phase. The polymer obtained from equimolar amounts of methacrylic acid and 4-vinylpyridine was found to recognise bentazone better than other polymers, both in chloroform and acetonitrile. The bentazone capacity for this stationary phase was studied considering aqueous buffers with different pH values and ionic strengths. A preliminary procedure of solid phase extraction was tested on aqueous samples containing a fixed amount of bentazone. Good recoveries (91–96%) and concentration factors of 3.2–15.2 were found.
{"title":"A molecularly imprinted polymer for the pesticide bentazone","authors":"C. Baggiani, G. Giraudi, C. Giovannoli, A. Vanni, F. Trotta","doi":"10.1039/A902968K","DOIUrl":"https://doi.org/10.1039/A902968K","url":null,"abstract":"Polymers able to bind the pesticide bentazone were prepared by utilising the technique of the non-covalent molecular imprinting polymerisation and using different molar ratios of methacrylic acid and 4-vinylpyridine as interacting monomers. Polymers obtained were packed in HPLC columns and the imprinting effect was studied using chloroform and acetonitrile as mobile phase. The polymer obtained from equimolar amounts of methacrylic acid and 4-vinylpyridine was found to recognise bentazone better than other polymers, both in chloroform and acetonitrile. The bentazone capacity for this stationary phase was studied considering aqueous buffers with different pH values and ionic strengths. A preliminary procedure of solid phase extraction was tested on aqueous samples containing a fixed amount of bentazone. Good recoveries (91–96%) and concentration factors of 3.2–15.2 were found.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"29 1","pages":"263-266"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"85232743","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 sorption and elution of In(III) on a porous PTFE filter tube impregnated with bis(2-ethylhexyl) hydrogen phosphate (HDEHP) was studied. A 1 µg portion of In(III) in 1000 ml of sample solution was quantitatively complexed with HDEHP adsorbed onto a porous PTFE filter tube by passing the solution through the micropores of the filter tube. Preconcentrated In(III) was then quantitatively recovered provided that the elution, which consisted of cyclical filtering of 0.1 ml of 4 mol l–1 hydrochloric acid through the filter tube for 1 min, was repeated 3 times. The total volume of the eluent was only 0.3 ml in this case; therefore, over 3300-fold of enrichment was attained within 90 min of total preconcentration time. This method was applicable to the preconcentration of In(III) in highly saline samples. A 2.5 µg portion of In(III) could be quantitatively extracted from 500 ml of synthetic seawater and be recovered into 0.5 ml of 4 mol l–1 hydrochloric acid, with subsequent determination by flame AAS. The average recovery and the RSD of the results were 100% and of 1.4%, respectively (n = 5).
研究了浸渍磷酸氢二(2-乙基己基)(HDEHP)的多孔PTFE滤管对In(III)的吸附和洗脱。将1µg In(III)加入1000ml的样品溶液中，通过过滤管的微孔，将溶液与吸附在多孔PTFE过滤管上的HDEHP定量络合。预先浓缩的In(III)定量回收，条件是通过滤管循环过滤0.1 ml 4 mol l-1盐酸1分钟，重复3次。本实验中洗脱液的总体积仅为0.3 ml;因此，在90分钟的总富集时间内，富集量达到3300倍以上。该方法适用于高盐样品中In(III)的预富集。从500 ml合成海水中定量提取2.5µg部分In(III)，回收到0.5 ml 4 mol l-1盐酸中，火焰原子吸收法测定。结果的平均回收率为100%，RSD为1.4% (n = 5)。
{"title":"Novel sorbent extraction technique using a chelating agent impregnated porous PTFE filter tube : Preconcentration of In(III) with a bis(2-ethylhexyl) hydrogen phosphate (HDEHP) loaded porous PTFE filter tube","authors":"M. Murakami, T. Takada","doi":"10.1039/A902146I","DOIUrl":"https://doi.org/10.1039/A902146I","url":null,"abstract":"The sorption and elution of In(III) on a porous PTFE filter tube impregnated with bis(2-ethylhexyl) hydrogen phosphate (HDEHP) was studied. A 1 µg portion of In(III) in 1000 ml of sample solution was quantitatively complexed with HDEHP adsorbed onto a porous PTFE filter tube by passing the solution through the micropores of the filter tube. Preconcentrated In(III) was then quantitatively recovered provided that the elution, which consisted of cyclical filtering of 0.1 ml of 4 mol l–1 hydrochloric acid through the filter tube for 1 min, was repeated 3 times. The total volume of the eluent was only 0.3 ml in this case; therefore, over 3300-fold of enrichment was attained within 90 min of total preconcentration time. This method was applicable to the preconcentration of In(III) in highly saline samples. A 2.5 µg portion of In(III) could be quantitatively extracted from 500 ml of synthetic seawater and be recovered into 0.5 ml of 4 mol l–1 hydrochloric acid, with subsequent determination by flame AAS. The average recovery and the RSD of the results were 100% and of 1.4%, respectively (n = 5).","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"44 1","pages":"185-188"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"90663705","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. Karyakin, L. V. Lukachova, E. E. Karyakina, A. Orlov, G. P. Karpachova
Processible polyaniline (PCPAn) modified electrodes are characterized by an advanced potentiometric pH response in comparison to those based on regular polyaniline. Glassy carbon electrodes modified with PCPAn by dip-coating exhibited a fully reversible potentiometric response of approximately 90 mV pH–1 over the range pH 3–9. Such significantly higher potentiometric responses of PCPAn modified electrodes compared to existing devices is explained on the basis of the thermodynamics of polyaniline redox reactions. The potentiometric biosensor for glucose based on processible polyaniline has been developed using a non-aqueous enzymology approach for enzyme immobilization. In the model solution, which mimics blood serum, the biosensor was useful for glucose detection over the concentration range 0.1–30 mM and the maximum response value reached was ≈80 mV. The advanced potentiometric response of PCPAn modified electrodes provides their application for sensor and biosensor development.
{"title":"The improved potentiometric pH response of electrodes modified with processible polyaniline. Application to glucose biosensor","authors":"A. Karyakin, L. V. Lukachova, E. E. Karyakina, A. Orlov, G. P. Karpachova","doi":"10.1039/A900597H","DOIUrl":"https://doi.org/10.1039/A900597H","url":null,"abstract":"Processible polyaniline (PCPAn) modified electrodes are characterized by an advanced potentiometric pH response in comparison to those based on regular polyaniline. Glassy carbon electrodes modified with PCPAn by dip-coating exhibited a fully reversible potentiometric response of approximately 90 mV pH–1 over the range pH 3–9. Such significantly higher potentiometric responses of PCPAn modified electrodes compared to existing devices is explained on the basis of the thermodynamics of polyaniline redox reactions. The potentiometric biosensor for glucose based on processible polyaniline has been developed using a non-aqueous enzymology approach for enzyme immobilization. In the model solution, which mimics blood serum, the biosensor was useful for glucose detection over the concentration range 0.1–30 mM and the maximum response value reached was ≈80 mV. The advanced potentiometric response of PCPAn modified electrodes provides their application for sensor and biosensor development.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"66 1","pages":"153-156"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"89326532","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}
X-Ray photoelectron spectroscopy (XPS) is used to investigate surface species on atmospheric particulates as part of an investigation into the sources and health effects of such particulates. Oxygen and carbon species dominate the surface with trace quantities of Na+, NO3–, Cl– and SO42–. Multiple species for carbon and oxygen were evident, with major species identified as oxidised carbon, graphitic/aliphatic carbon and ruthenium oxide or a carbide. The potential of imaging XPS to show localised variation of surface species across atmospheric particulates is demonstrated.
{"title":"Investigation of imaging X-ray photoelectron spectroscopy for surface analysis of atmospheric particulates","authors":"B. Hutton, David E. Williams","doi":"10.1039/A809067J","DOIUrl":"https://doi.org/10.1039/A809067J","url":null,"abstract":"X-Ray photoelectron spectroscopy (XPS) is used to investigate surface species on atmospheric particulates as part of an investigation into the sources and health effects of such particulates. Oxygen and carbon species dominate the surface with trace quantities of Na+, NO3–, Cl– and SO42–. Multiple species for carbon and oxygen were evident, with major species identified as oxidised carbon, graphitic/aliphatic carbon and ruthenium oxide or a carbide. The potential of imaging XPS to show localised variation of surface species across atmospheric particulates is demonstrated.","PeriodicalId":7814,"journal":{"name":"Analytical Communications","volume":"42 1","pages":"17-18"},"PeriodicalIF":0.0,"publicationDate":"1999-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"79541847","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}
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