Two procedures were compared for extraction and clean-up of 20organophosphorus and 19 pyrethroid pesticides in sediment to identify the more effective procedurefor groups of pesticides or individual compounds. In Proc...Two procedures were compared for extraction and clean-up of 20organophosphorus and 19 pyrethroid pesticides in sediment to identify the more effective procedurefor groups of pesticides or individual compounds. In Procedure I, methanol/water and n-hexane wereused for extraction, and 1:10 (v/v) dichloromethane in n-hexane and acetone were used as eluents foreluting the analyte through the cartridge, with one evaporating steps on a rotary evaporator andtwo eluting steps on the cartridge. n-hexane/acetone (2:1, v/v) was used for extraction and elutionin Procedure II with one evaporating step on a rotary evaporator and one eluting step on thecartridge. All extractions were performed under an ultrasonic bath and gas chromatography and massspectrometry were utilized for measurements. Procedure II was developed as a rapid, timesaving, lesscostly and safer substitute for Procedure I which was an old method. Procedure II was moreeffective for almost all the organophosphorus pesticides tested and 11of the 19 pyrethroidpesticides, while Procedure I was more appropriate for analysis of 5 pyrethroid pesticides. However,recoveries of most pyrethroid pesticides were fairly low. Thus, further studies should focus onadjustment and formulation of solvents for more efficient extraction and clean-up of pyrethroidpesticides from sediment samples.展开更多
The Diels-Alder reaction of bis(diphenylphosphine oxide)butadiyne (BDPPOB) with spiro[2.4]hepta-4,6-diene affords the title compound, 2-(diphenylphosphine oxide)-3-(diphen- ylphosphine oxide ethynyl)spiro[bicyclo[2.2....The Diels-Alder reaction of bis(diphenylphosphine oxide)butadiyne (BDPPOB) with spiro[2.4]hepta-4,6-diene affords the title compound, 2-(diphenylphosphine oxide)-3-(diphen- ylphosphine oxide ethynyl)spiro[bicyclo[2.2.1] hepta-2,5-diene-7,1-cyclopropane] (DDSHC, C35H28O2P2, Mr = 542). Its crystal structure belongs to monoclinic system, space group P21/n with a =12.708(3), b = 14.666(4), c = 15.048(4) ? = 93.903(5) ? V = 2798.1(13) ?, Z = 4, Dc = 1.288g/cm3, F(000)=1136, (MoK? = 0.187mm-1, final R = 0.0626 and wR= 0.1422 for 4685 independent reflections with I > 2(I). Structural analyses reveal that the title compound is nonplanar and the dihedral angles between two phenyl rings around each phosphorus atom are 71.7(2) and 70.7(3)? respectively.展开更多
The authors spent the search for new methods of synthesis possible of organometallic compounds of phosphorus, arsenic, antimony, bismuth. For modifications classical reactions the N （nitrogen） atoms have been replac...The authors spent the search for new methods of synthesis possible of organometallic compounds of phosphorus, arsenic, antimony, bismuth. For modifications classical reactions the N （nitrogen） atoms have been replaced on atoms of P （phosphorus）, As （arsenic）, Sb （antimony） and Bi （bismuth）. The authors have proposed a new mechanism for the possible reactions.展开更多
We report in situ doping of brushite on zinc manganese oxide（ZMO）, fabricated by calcining a Mn（II） oxalate‐impregnated metal‐organic framework. The doping process was conducted in com‐bination with the photoca...We report in situ doping of brushite on zinc manganese oxide（ZMO）, fabricated by calcining a Mn（II） oxalate‐impregnated metal‐organic framework. The doping process was conducted in com‐bination with the photocatalytic water oxidation reaction which was catalyzed by ZMO in neutral phosphate‐buffered aqueous solution containing [Ru（bpy）3]^2＋‐Na2S2O8 and calcium（II） triflate salt, exhibiting greatly enhanced water oxidation performance with optimized turnover frequency of 0.18 mmol（O2） mol（Mn）^（–1） s^（–1）. Different analytical techniques indicated that photodeposited calci‐um‐phosphate（CaP） acted as a co‐catalyst to promote the O2 evolution activity of ZMO. This system involved the use of manganese oxide and calcium ion, and the operation was conducted under am‐bient temperature and neutral conditions, thus, it efficiently mimicked the oxygen‐evolving complex in photosystem II.展开更多
基金Project supported by the Outstanding Youth Fund of National Natural Science Foundation of China, the National Key Basic Research Support Foundation (NKBRSF) of China (No. 2002CB410805) and the Federal Ministry of Education and Research, Germany.
文摘Two procedures were compared for extraction and clean-up of 20organophosphorus and 19 pyrethroid pesticides in sediment to identify the more effective procedurefor groups of pesticides or individual compounds. In Procedure I, methanol/water and n-hexane wereused for extraction, and 1:10 (v/v) dichloromethane in n-hexane and acetone were used as eluents foreluting the analyte through the cartridge, with one evaporating steps on a rotary evaporator andtwo eluting steps on the cartridge. n-hexane/acetone (2:1, v/v) was used for extraction and elutionin Procedure II with one evaporating step on a rotary evaporator and one eluting step on thecartridge. All extractions were performed under an ultrasonic bath and gas chromatography and massspectrometry were utilized for measurements. Procedure II was developed as a rapid, timesaving, lesscostly and safer substitute for Procedure I which was an old method. Procedure II was moreeffective for almost all the organophosphorus pesticides tested and 11of the 19 pyrethroidpesticides, while Procedure I was more appropriate for analysis of 5 pyrethroid pesticides. However,recoveries of most pyrethroid pesticides were fairly low. Thus, further studies should focus onadjustment and formulation of solvents for more efficient extraction and clean-up of pyrethroidpesticides from sediment samples.
基金This work was supported by the NNSFC (No. 29832030 and 20072018)
文摘The Diels-Alder reaction of bis(diphenylphosphine oxide)butadiyne (BDPPOB) with spiro[2.4]hepta-4,6-diene affords the title compound, 2-(diphenylphosphine oxide)-3-(diphen- ylphosphine oxide ethynyl)spiro[bicyclo[2.2.1] hepta-2,5-diene-7,1-cyclopropane] (DDSHC, C35H28O2P2, Mr = 542). Its crystal structure belongs to monoclinic system, space group P21/n with a =12.708(3), b = 14.666(4), c = 15.048(4) ? = 93.903(5) ? V = 2798.1(13) ?, Z = 4, Dc = 1.288g/cm3, F(000)=1136, (MoK? = 0.187mm-1, final R = 0.0626 and wR= 0.1422 for 4685 independent reflections with I > 2(I). Structural analyses reveal that the title compound is nonplanar and the dihedral angles between two phenyl rings around each phosphorus atom are 71.7(2) and 70.7(3)? respectively.
文摘The authors spent the search for new methods of synthesis possible of organometallic compounds of phosphorus, arsenic, antimony, bismuth. For modifications classical reactions the N （nitrogen） atoms have been replaced on atoms of P （phosphorus）, As （arsenic）, Sb （antimony） and Bi （bismuth）. The authors have proposed a new mechanism for the possible reactions.
文摘We report in situ doping of brushite on zinc manganese oxide（ZMO）, fabricated by calcining a Mn（II） oxalate‐impregnated metal‐organic framework. The doping process was conducted in com‐bination with the photocatalytic water oxidation reaction which was catalyzed by ZMO in neutral phosphate‐buffered aqueous solution containing [Ru（bpy）3]^2＋‐Na2S2O8 and calcium（II） triflate salt, exhibiting greatly enhanced water oxidation performance with optimized turnover frequency of 0.18 mmol（O2） mol（Mn）^（–1） s^（–1）. Different analytical techniques indicated that photodeposited calci‐um‐phosphate（CaP） acted as a co‐catalyst to promote the O2 evolution activity of ZMO. This system involved the use of manganese oxide and calcium ion, and the operation was conducted under am‐bient temperature and neutral conditions, thus, it efficiently mimicked the oxygen‐evolving complex in photosystem II.
