目前,牛肉及其制品中多种有机磷农药残留量测定方面的报道,国内外都较少,尤其是使用同一根填充色谱柱,一次检测九种有机磷农药残留量的方法,国内尚未报道。Brown 等人在测定动物脂肪中二嗪磷等六种有机磷农药残留量时,采用3%OV—210Chro...目前,牛肉及其制品中多种有机磷农药残留量测定方面的报道,国内外都较少,尤其是使用同一根填充色谱柱,一次检测九种有机磷农药残留量的方法,国内尚未报道。Brown 等人在测定动物脂肪中二嗪磷等六种有机磷农药残留量时,采用3%OV—210Chrom—Osorb W HP(80—100目)的色谱柱,利用扫集共蒸馏仪处理样品。但此柱对敌敌畏等农药无响应。展开更多
The cubane-type mixed Mo W cluster[Mo2W2S4 (OAc)2(dtp)3 (dtpH)]·CH2Cl2 (dtp= (EtO)2PS2, dtpH = (EtO)2PS (SH) has been prepared by reduction and addition reaction between dinuclear W2S4 (dtp)2 and Mo(CO)6 in HOAc...The cubane-type mixed Mo W cluster[Mo2W2S4 (OAc)2(dtp)3 (dtpH)]·CH2Cl2 (dtp= (EtO)2PS2, dtpH = (EtO)2PS (SH) has been prepared by reduction and addition reaction between dinuclear W2S4 (dtp)2 and Mo(CO)6 in HOAc and Ac2O solution in the presence of dtp-ligand. Crystallographic data: Mr=1632. 71,monoclinic, space group P2/n, a=13. 146 (8), b=11. 961 (5),c=17. 157 (9) β =105. 99(8)°, V=2593(8), Z=2, Dc=2. 09 /cm￣3 ,λ(MoKa) =0.71073 ,F (000)=1578, final R=0. 029, Rw = 0. 041 for 3765 unique intensity data [I≥4σ (I)]. The result of X-ray study and elemental analysis indicated that, in the crystal lattice, molybdenum and tungsten are statistically distributed in the metal positions each with 0. 5 fractional occupation.展开更多
The cluster compound [Mo4S4 (μ-O2CC6H5)2(dtp)4] (dtp = S2P (OEt)2)was obtained by the ligand substitution reaction of tetranuclear molybdenum cluster [Mo4S4(μ-dtp)2(dtp)4] in the mixed solvent of acetone, ethanol an...The cluster compound [Mo4S4 (μ-O2CC6H5)2(dtp)4] (dtp = S2P (OEt)2)was obtained by the ligand substitution reaction of tetranuclear molybdenum cluster [Mo4S4(μ-dtp)2(dtp)4] in the mixed solvent of acetone, ethanol and water in the presence of C6H5CO2Na. It is monoclinic and crystallizesin space group C2/c, Mr =1495. 09, a=12. 175 (5) , b=22. 01 (1) , c=20.875(9) ,β=99. 04(4)°; V=5570(5) ; Z=4; Dc= 1. 78g/cm3;μ(MoKα) = 14. 52 cm-1; F(000) =2984. Final R factor is 0. 066. The result reveals that the [Mo4S4] cluster core and t-(dtp)1ligands are retained and onlyμ-bridged (dtp)1- ligands are substituted by (C6H5CO2)1in the substitution reaction, thus producing the title cluster compound,the structure of which contains two species of bidentate ligand.展开更多
The extraction of cadmium and zinc with di-(2-ethylhexyl)-dithiophosphoric acid(D2EHDTPA)-toluene and D2EHDTPA-trioctyl amine(TOA)-toluene has been investigated. Infrared spectrum analysis, the nuclear magnetic resona...The extraction of cadmium and zinc with di-(2-ethylhexyl)-dithiophosphoric acid(D2EHDTPA)-toluene and D2EHDTPA-trioctyl amine(TOA)-toluene has been investigated. Infrared spectrum analysis, the nuclear magnetic resonance spectrum(NMR) analysis and conductivity measurements confirm that the probable structures of the extracted complexes are CdA2 and ZnA2. Cadmium can be extracted by D2EHDTPA very easily. Almost all the cadmium can be extracted, but stripping of cadmium from the organic phase is very difficult. When a mixture of D2EHDTPA and TOA is used, selective extraction of cadmium from zinc sulfate solution can be achieved. Cadmium can be easily stripped from the organic phase.展开更多
The molecular structure of N, N-bis ( 2-chloroethyl )-N'-isopropyl-N'-phenyl thioureido phosphoramide has been determined by X-ray diffraction method. The crystal(C_14H_23Cl_4N_4OPS) is monoclinic with space g...The molecular structure of N, N-bis ( 2-chloroethyl )-N'-isopropyl-N'-phenyl thioureido phosphoramide has been determined by X-ray diffraction method. The crystal(C_14H_23Cl_4N_4OPS) is monoclinic with space group P21/n,α=13. 398(2) , b= 10. 351(4), c= 14. 595(3) A, β= 101. 45(1)°, V=1983(2) A3 Mr=397. 31, Z=4, Dx=1. 34 g/cm3 , μ= 5. 17 cm-1, F(000) = 832 , R=0. 056 and Rω=0. 060 for 1856 reflections with I≥3σ(Ⅰ).The chemical shifts of the hydrogen atoms bonded to nitrogen atoms N (4) and N (33 are 10. 96 ppm and 7. 57 ppm respectively locating in the lower field. This abnormal situation can be explained by the formation of intramolecular and intermolecular hydrogen bonds. And the X-ray crystallographic analysis demonstrates the existence of the H-bonding six-membered ring in the structure.展开更多
The first successful attempt to prepare W_3S_4 {S_2P (OEt )_2}_4(H_2O) in organic phase is reported. Its substitution and addition reactions are investigated systematically, and the substitution sequences of the '...The first successful attempt to prepare W_3S_4 {S_2P (OEt )_2}_4(H_2O) in organic phase is reported. Its substitution and addition reactions are investigated systematically, and the substitution sequences of the 'loose' ligands are determined. The crystallographic data of the cluster compounds with [W_3S_4]￣(4+) and [W_3CuS_4]￣(5+) cores are compared and their UV-Vis spectra are firstly reported. Thus, the 'quasi-aromaticity' of the [W_3S_4]￣(4+) core of these cluster compounds is discussed.展开更多
The interface and surface properties of nano-hydroxyapatite(n-HA) and poly( 1, 4-phenylene sulfide)-poly (2,4-phenylene sulfide acid)(PPS-PPSA) copolymer composite were investigated. The results show that there are so...The interface and surface properties of nano-hydroxyapatite(n-HA) and poly( 1, 4-phenylene sulfide)-poly (2,4-phenylene sulfide acid)(PPS-PPSA) copolymer composite were investigated. The results show that there are some strong interface combinations of calcium ion (Ca2+ ), car-boxyl (-COO- ) and phosphate radicle ion (PO_4~3- ) between copolymer and n-HA in the composite. The presence of the 2,4-phenylene sulfide acid in copolymer can increase the affinity to n-HA, which causes the formation of chemical bindings between the PPS-PPSA copolymer and n-HA. XRD analysis and IR surface analysis indicate that n-HA is not encapsulated by copolymer but exposed on the surface of the composite, and has same structure and properties with the origi-nal n-HA. The presence of the interface chemical bindings between the PPS-PPSA copolymer and n-HA can increase the content of n-HA in composite but does not cause the decrease of the composite mechanical strength.展开更多
文摘目前,牛肉及其制品中多种有机磷农药残留量测定方面的报道,国内外都较少,尤其是使用同一根填充色谱柱,一次检测九种有机磷农药残留量的方法,国内尚未报道。Brown 等人在测定动物脂肪中二嗪磷等六种有机磷农药残留量时,采用3%OV—210Chrom—Osorb W HP(80—100目)的色谱柱,利用扫集共蒸馏仪处理样品。但此柱对敌敌畏等农药无响应。
文摘The cubane-type mixed Mo W cluster[Mo2W2S4 (OAc)2(dtp)3 (dtpH)]·CH2Cl2 (dtp= (EtO)2PS2, dtpH = (EtO)2PS (SH) has been prepared by reduction and addition reaction between dinuclear W2S4 (dtp)2 and Mo(CO)6 in HOAc and Ac2O solution in the presence of dtp-ligand. Crystallographic data: Mr=1632. 71,monoclinic, space group P2/n, a=13. 146 (8), b=11. 961 (5),c=17. 157 (9) β =105. 99(8)°, V=2593(8), Z=2, Dc=2. 09 /cm￣3 ,λ(MoKa) =0.71073 ,F (000)=1578, final R=0. 029, Rw = 0. 041 for 3765 unique intensity data [I≥4σ (I)]. The result of X-ray study and elemental analysis indicated that, in the crystal lattice, molybdenum and tungsten are statistically distributed in the metal positions each with 0. 5 fractional occupation.
文摘The cluster compound [Mo4S4 (μ-O2CC6H5)2(dtp)4] (dtp = S2P (OEt)2)was obtained by the ligand substitution reaction of tetranuclear molybdenum cluster [Mo4S4(μ-dtp)2(dtp)4] in the mixed solvent of acetone, ethanol and water in the presence of C6H5CO2Na. It is monoclinic and crystallizesin space group C2/c, Mr =1495. 09, a=12. 175 (5) , b=22. 01 (1) , c=20.875(9) ,β=99. 04(4)°; V=5570(5) ; Z=4; Dc= 1. 78g/cm3;μ(MoKα) = 14. 52 cm-1; F(000) =2984. Final R factor is 0. 066. The result reveals that the [Mo4S4] cluster core and t-(dtp)1ligands are retained and onlyμ-bridged (dtp)1- ligands are substituted by (C6H5CO2)1in the substitution reaction, thus producing the title cluster compound,the structure of which contains two species of bidentate ligand.
基金Supported by the National Natural Science Foundation of China(No.59474009).
文摘The extraction of cadmium and zinc with di-(2-ethylhexyl)-dithiophosphoric acid(D2EHDTPA)-toluene and D2EHDTPA-trioctyl amine(TOA)-toluene has been investigated. Infrared spectrum analysis, the nuclear magnetic resonance spectrum(NMR) analysis and conductivity measurements confirm that the probable structures of the extracted complexes are CdA2 and ZnA2. Cadmium can be extracted by D2EHDTPA very easily. Almost all the cadmium can be extracted, but stripping of cadmium from the organic phase is very difficult. When a mixture of D2EHDTPA and TOA is used, selective extraction of cadmium from zinc sulfate solution can be achieved. Cadmium can be easily stripped from the organic phase.
文摘The molecular structure of N, N-bis ( 2-chloroethyl )-N'-isopropyl-N'-phenyl thioureido phosphoramide has been determined by X-ray diffraction method. The crystal(C_14H_23Cl_4N_4OPS) is monoclinic with space group P21/n,α=13. 398(2) , b= 10. 351(4), c= 14. 595(3) A, β= 101. 45(1)°, V=1983(2) A3 Mr=397. 31, Z=4, Dx=1. 34 g/cm3 , μ= 5. 17 cm-1, F(000) = 832 , R=0. 056 and Rω=0. 060 for 1856 reflections with I≥3σ(Ⅰ).The chemical shifts of the hydrogen atoms bonded to nitrogen atoms N (4) and N (33 are 10. 96 ppm and 7. 57 ppm respectively locating in the lower field. This abnormal situation can be explained by the formation of intramolecular and intermolecular hydrogen bonds. And the X-ray crystallographic analysis demonstrates the existence of the H-bonding six-membered ring in the structure.
文摘The first successful attempt to prepare W_3S_4 {S_2P (OEt )_2}_4(H_2O) in organic phase is reported. Its substitution and addition reactions are investigated systematically, and the substitution sequences of the 'loose' ligands are determined. The crystallographic data of the cluster compounds with [W_3S_4]￣(4+) and [W_3CuS_4]￣(5+) cores are compared and their UV-Vis spectra are firstly reported. Thus, the 'quasi-aromaticity' of the [W_3S_4]￣(4+) core of these cluster compounds is discussed.
文摘The interface and surface properties of nano-hydroxyapatite(n-HA) and poly( 1, 4-phenylene sulfide)-poly (2,4-phenylene sulfide acid)(PPS-PPSA) copolymer composite were investigated. The results show that there are some strong interface combinations of calcium ion (Ca2+ ), car-boxyl (-COO- ) and phosphate radicle ion (PO_4~3- ) between copolymer and n-HA in the composite. The presence of the 2,4-phenylene sulfide acid in copolymer can increase the affinity to n-HA, which causes the formation of chemical bindings between the PPS-PPSA copolymer and n-HA. XRD analysis and IR surface analysis indicate that n-HA is not encapsulated by copolymer but exposed on the surface of the composite, and has same structure and properties with the origi-nal n-HA. The presence of the interface chemical bindings between the PPS-PPSA copolymer and n-HA can increase the content of n-HA in composite but does not cause the decrease of the composite mechanical strength.
