2-(2,4-咪唑偶氮)-5-二甲氨基苯甲酸分光光度法测定钴

研究了新显色剂2-(2,4-咪唑偶氮)-5-二甲氨基苯甲酸(IZDBA)的合成及与钴的显色反应条件。2-氨基咪唑硫酸盐采用亚硝酸盐重氮化后,与间-二甲氨基苯甲酸偶联形成IZD- BA。在pH 8.0的NH_3.H_2O—NH_4Cl缓冲溶液中,IZDBA与Co~(2 )形成组成比为2:1的稳定紫色络合物,其最大吸收波长为610 nm,表观摩尔吸光系数为4.15×10~4L·mol~(-1)·cm~(-1),Co~(2 )质量浓度在0～0.8 mg/L范围内遵守比尔定律。方法具有较好的选择性和灵敏度,可以不经分离直接测定合成工业废水中微量钴,RSD(n=6)为2.2%,加标平均回收率为104.5%。     

6-氯-苯并噻唑偶氮苯甲酸光度法测定粉煤灰中痕量铜Ⅱ

研究了6-氯-苯并噻唑偶氮苯甲酸(6-Cl-BTAEB)与铜Ⅱ的显色反应,建立了分光光度法测定痕量铜Ⅱ的新方法。在pH4.0的HAc-NaAc缓冲溶液中,乳化剂OP存在下,6-Cl-BTAEB与Cu(反应生成2∶1稳定络合物,其最大吸收波长为650 nm,表观摩尔吸光系数为7.35×104L.mol-1.cm-1。铜含量在0～400μg/L内符合比尔定律,方法用于测定粉煤灰中痕量铜Ⅱ,结果与原子吸收光谱法相符,6次测定值RSD<4%。     

1-(2-苯并噻唑偶氮)-2-羟基-3-萘甲酸与铜(Ⅱ)的显色反应研究及应用

合成了新试剂1-(2-苯并噻唑偶氮)-2-羟基-3-萘甲酸(BTAHN),并研究了该试剂与铜(Ⅱ)的显色反应.在pH 6.0～8.5范围内,BTAHN与铜(Ⅱ)形成21的蓝色络合物,该络合物的最大吸收波长λmax在590 nm处,25 mL溶液中,铜的质量在0～25μg服从比尔定律,表观摩尔吸光系数ε590为2.94×10 4.所拟方法用于铝合金、合金钢、茶叶和面粉样品中微量铜的测定,结果满意.     

2-(5-羧基-1,3,4-三氮唑偶氮)-5-二乙氨基苯胺光度法测定铜Ⅱ

研究了新显色剂 2 - (5-羧基 - 1 ,3,4-三氮唑偶氮 ) - 5-二乙氨基苯胺 (CTZAN)与Cu 的显色反应条件。结果表明 ,Cu 在 pH3 0的HAc -NaAc缓冲溶液中与CTZAN形成稳定的组成比为 1∶2的紫色络合物 ,λmax=565nm ,试剂的λmax=435nm ,对比度Δλ =1 30nm ,表观摩尔吸光系数ε =3 0 3× 1 0 4 ,Cu(Ⅱ )浓度在 0～ 0 8mg/L范围内服从比尔定律 ,所拟方法用于测定镁合金和铝合金标样中微量铜 ,加标回收率为 1 0 1 4%～ 1 0 4 0 % ,RSD(n =6) =1 4%～ 3 9% ,结果满意。     

2-(2-噻唑偶氮)-5-磺丙氨基苯酚与铜的显色反应研究及应用

研究了2-(2-噻唑偶氮)-5-磺丙氨基苯酚(TASPAP)与铜离子的显色反应。试剂与铜离子在pH 5.6的Clark-Lubs缓冲溶液中形成2∶1的稳定紫红色络合物,该络合物的最大吸收波长λmax在552 nm处,铜质量浓度在0~2.00 mg/L范围内服从比尔定律,其表观摩尔吸光系数ε552为4.58×104L.mol-1.cm-1。纯铝或铝合金经过盐酸溶解、双氧水氧化和氨水沉淀分离出铜离子,采用氟化钠掩蔽高铁离子,测得铜的含量与1-(2-苯并噻唑偶氮)-2-羟基-3-萘甲酸法所得结果一致,相对标准偏差在2.3%~2.6%;水样中微量铜的测定,加标回收率为98.0%~101.6%。     

2-氯-4-溴苯基重氮氨基偶氮苯光度法测定铜

研究了在Triton X-100存在下,铜(Ⅱ)与显色剂2-氯-4-溴苯基重氮氨基偶氮苯的显色反应。在pH10.5的Na2B4O7-NaOH缓冲溶液中,铜(Ⅱ)与试剂形成1:2的红色络合物,络合物的最大吸收峰位于520nm波长处,表观摩尔吸光系数为ε=1.01×105L.mol-1.cm-1,铜(Ⅱ)含量在0～400μg/L范围内符合比尔定律。采用巯基葡聚糖凝胶(SDG)分离水中共存离子富集铜,提高了方法的选择性。本法用于水样分析,回收率为100%～102%,相对标准偏差为2.0%～2.4%。     

2-(2-噻唑偶氮)-5-磺丙氨基苯酚与镍(Ⅱ)显色反应的研究及其应用

研究了2-(2-噻唑偶氮)-5-磺丙氨基苯酚(TASPAP)与镍(Ⅱ)的显色反应,发现该试剂与镍(Ⅱ)在pH6.46的Clark-Lubs缓冲溶液中形成2∶1的稳定紫红色络合物。该络合物的最大吸收波长λmax在550 nm处,在10 mL溶液中镍质量在0~14μg服从比尔定律,测定的表观摩尔吸光系数ε550为6.346×104L.mol-1.cm-1。所拟方法用于合金钢样品和水样中微量镍的测定,加标回收率在98%~101%之间。     

1-(2-吡啶偶氮)-2-萘酚分光光度法测定硫酸阳极氧化液中铜

研究了铜与1-(2-吡啶偶氮)-2-萘酚(PAN)的显色反应,建立了测定硫酸阳极氧化液中铜的新方法。以TritonX-100为增溶增敏剂,明胶作稳定保护剂,在酸性条件下Cu-PAN络合物稳定保持在水相中,直接进行光度分析。该络合物在558nm处有最大吸收峰,其表观摩尔吸光系数ε=2.25×104L.mol-1.cm-1。方法检出限为0.028μg/mL,线性范围为0～3.2μg/mL,用于测定硫酸阳极氧化液中的铜,加标回收率为98.2%～105.6%,相对标准偏差≤0.34%。     

3-甲氧基-甲亚胺H分光光度法测定微量铜(Ⅱ)

研究了Cu(Ⅱ)与3-甲氧基-甲亚胺H的显色反应,建立了分光光度法测定微量铜的新方法。试验结果表明,在pH 5.9的HAc-NaAc缓冲溶液中,3-甲氧基-甲亚胺H与Cu(Ⅱ)及溴代十六烷基吡啶(CPB)微乳液形成1∶1∶1的淡黄色络合物。络合物的最大吸收峰位于450 nm波长处,表观摩尔吸光系数为ε=1.0×105L.mol-1.cm-1。10 mL溶液中,Cu(Ⅱ)含量在0.04~12μg范围内符合比尔定律,检出限为0.001 2μg/mL。方法可用于铝合金和水样中微量Cu(Ⅱ)的测定,回收率在97.     

2-(5-碘-2-吡啶偶氮)-5-二甲氨基苯胺与钯显色反应的研究及其应用

探讨了2-(5-碘-2-吡啶偶氮)-5-二甲氨基苯胺(5-I-PADMA)与钯(Ⅱ)的显色反应。实验表明,在0.6 mol/L高氯酸介质中,5-I-PADMA与钯(Ⅱ) 反应形成摩尔比为1∶1的蓝色稳定络合物,该络合物最大吸收峰位于613 nm处。钯(Ⅱ)含量在0~0.6 μg/mL范围内符合比尔定律,线性回归方程为△A=0.828 4 ρ(μg/mL)- 0.001 6,相关系数r=0.999 9,表观摩尔吸光系数为8.82 × 10⁴ L·mol^-1·cm^-1。方法应用于钯分子筛和矿样中钯的测定,结果与原子吸收光谱法一致,相对标准偏差(n=6)为1.2%～1.4%。     

Synthesis and biological investigations of 1-(tetrahydropyran-2'-yl)- and 1-(tetrahydrofuran-2'-yl)benzimidazoles and 1/2-(tetrahydropyran-2'-yl)- and 1/2-(tetrahydrofuran-2'-yl)benzotriazoles

Sets of benzimidazole and benzotriazole derivatives bearing on position 1 or 2 a tetrahydrofuranyl or tetrahydropyranyl moieties were prepared through the addition of the suitable benzazoles on 2,3-dihydrofuran and 3,4-dihydro-2H-pyran. The reactions were carried on either without solvent or in carbon tetrachloride solution. In the last case some peculiar chlorinated side products were isolated and characterized. Twenty compounds were screened for in vitro antitumoral and anti-HIV-1 activities and found poorly active or completely inactive. On the other hand several compounds exhibited good tracheal relaxant activity in vitro; compound 8, 11, 16, 24 and 26 resulted more active than theophylline in this test, while compound 11 was comparable to amrinone till the concentration of 3 micrograms/ml. Finally, compound 5 resulted endowed with a strong diuretic and saluretic activity at the dose of 3 mg/Kg, thus representing a new lead for discovering new diuretic agents.     

CeO2对不锈钢基SiO2-BaO-Al2O3-Cr2O3陶瓷涂层性能的影响

采用高温熔烧法于1Cr18Ni9Ti不锈钢基材表面制备掺CeO2的SiO2-BaO-Al2O3-Cr2O3陶瓷涂层,研究了不同含量CeO2对涂层的抗氧化性、抗热震性和硬度的影响。研究结果表明,含CeO2的不锈钢基SiO2-BaO-Al2O3-Cr2O3陶瓷涂层能有效阻止不锈钢基体的氧化增重,提高涂层的抗热震性能及硬度。本实验条件下,CeO2含量2.8%时,涂层具有最好的抗氧化性能和抗热震性能。     

Texture and residual strain in two SiC/Ti-6-2-4-2 titanium composites

Residual strain and texture variations were measured in two titanium matrix composites reinforced with silicon carbide fibers (Ti/SiC) of similar composition but fabricated by different processing routes. Each composite comprised a Ti-6242 α/β matrix alloy containing vol 35 pct continuous SiC fibers. In one, the matrix was produced by a plasma sprayed (PS) route, and in the other by a wiredrawn (WD) process. The PS and WD composites were reinforced with SCS-6 (SiC) and Trimarc (SiC) fibers, respectively. The texture in the titanium matrices differed significantly. The titanium matrix for the PS material exhibited random texture pre and post fabrication of the composite. For the WD material, the starting texture of the monolithic titanium matrix was ≈17 times random, but after consolidation into composite form, it was ≈6 times random. No significant differences were noted in the fiber-induced matrix residual strains between the composites prepared by the two procedures. However, the Trimarc (WD) fibers recorded higher (≈1.3 times) compressive strains than the SCS-6 (PS) fibers. Stresses and stress balance results are reported. Plane-specific elastic moduli, measured in load tests on the unreinforced matrices, showed little difference. This article is based on a presentation made in the Symposium “Mechanisms and Mechanics of Composites Fracture” held October 11–15, 1998, at the TMS Fall Meeting in Rosemont, Illinois, under the auspices of the TMS-SMD/ASM-MSCTS Composite Materials Committee.     

Texture and residual strain in two SiC/Ti-6-2-4-2 titanium composites

Residual strain and texture variations were measured in two titanium matrix composites reinforced with silicon carbide fibers (Ti/SiC) of similar composition but fabricated by different processing routes. Each composite comprised a Ti-6242 α/β matrix alloy containing vol 35 pct continuous SiC fibers. In one, the matrix was produced by a plasma sprayed (PS) route, and in the other by a wiredrawn (WD) process. The PS and WD composites were reinforced with SCS-6 (SiC) and Trimarc (SiC) fibers, respectively. The texture in the titanium matrices differed significantly. The titanium matrix for the PS material exhibited random texture pre and post fabrication of the composite. For the WD material, the starting texture of the monolithic titanium matrix was ≈17 times random, but after consolidation into composite form, it was ≈6 times random. No significant differences were noted in the fiber-induced matrix residual strains between the composites prepared by the two procedures. However, the Trimarc (WD) fibers recorded higher (≈1.3 times) compressive strains than the SCS-6 (PS) fibers. Stresses and stress balance results are reported. Plane-specific elastic moduli, measured in load tests on the unreinforced matrices, showed little difference. This article is based on a presentation made in the Symposium “Mechanisms and Mechanics of Composites Fracture” held October 11–15, 1998, at the TMS Fall Meeting in Rosemont, Illinois, under the auspices of the TMS-SMD/ASM-MSCTS Composite Materials Committee.     

Biochemical basis for a cholesterol-lowering activity of 2-[2"-(1",3"-dioxolane)]-2-methyl-4-(2'-oxo-1'-pyrrolidinyl)-6- nitro-2H-1-benzopyran (SKP-450), a novel antihypertensive agent

Administration (p.o.) of SKP-450, 2-[2"-(1",3"-dioxolane)]-2-methyl-4-(2'-oxo-1'-pyrrolidinyl)-6-nitro-2H- 1-benzopyran, a novel antihypertensive agent, to hypercholesterolemic Syrian hamsters led to a significant reduction in plasma lipids in a dose-dependent manner, i.e., a 10.8% to 29% reduction in low-density lipoprotein cholesterol at doses of 0.3 to 10 mg/kg of SKP-450. SKP-450 was found to specifically inhibit the hepatic microsomal lanosterol 14alpha-methyl demethylase (14alpha-DM) in a competitive manner (Ki:2.65 microM). Furthermore, a dose-dependent decrease in the 14alpha-DM activity by SKP-450 parallelled the cholesterol synthetic rate in vitro in both the rat hepatic S10 fractions (supernatants at 10,000 g; IC50:20 microM) and Chinese hamster ovary cells (IC50:23 microM). However, this phenomenon was not seen in AR45 cells, which are deficient in 14alpha-DM, suggesting that 14alpha-DM is the major target for the inhibitory action of SKP-450 in regard to cholesterol biosynthesis.     

The free energies of mixing of melts in the systems 2FeO-SiO2-2MnO-SiO2 and 2.33FeO-TiO2-2.33MnOTiO2

The free energies of mixing in melts in the system 2FeO · SiO₂-2MnO · SiO₂ at 1450°C and the system 2.33FeO · TiO₂-2.33MnO · TiO₂ at 1475°C have been obtained from measurement of the equilibrium Mn + FeO = Fe + MnO established between the melts and ironmanganese foils. Both systems exhibit ideal silicate mixing. The phase diagram for the system 2FeO-SiO₂-2MnO ·SiO₂ is calculated.     

Synthesis and biological investigations of 2-(tetrahydropyran-2'-yl) and 2-(tetrahydrofuran-2'-yl)benzimidazoles

A set of benzimidazole derivatives bearing on position 2 a tetrahydropyranyl or tetrahydrofuranyl residue was prepared and tested for antitumoral, anti HIV-1 and other pharmacological activities. While the anti-HIV activity was completely lacking, moderate antitumoral activity was found in a few compounds; particularly the 5,6-dichloro-2-(tetrahydropyran-2-yl)-benzimidazole (8) was able to inhibit the growth of 19 cell lines of humane tumors at near micromolar concentration. On the other hand compounds 4, 6-8 and 10 exhibited significant tracheal relaxant activity in vitro at concentration 3-10 micrograms/ml, thus resulting superior to theophylline and comparable to amrinone.     

新显色剂2-(2-咪唑偶氮)-5-二乙氨基酚光度法测定铁(Ⅲ)

研究了新显色剂2-（2-咪唑偶氮）-5-二乙氨基酚（简称IZAPN）与Fe     

Electrical properties of phases in the ZrO2 - Y2O3 - La2O3 system

An investigation was made of the electrical properties of phases with the cubic fluorite, pyrochlor, and C-Y₂O₃ structures, and the tetragonal ZrO₂ structure (T-ZrO₂) in the ternary system ZrO₂ - Y₂O₃ - La₂O₃. For comparison, the electrical conductivity of a number of specimens with the fluorite structure in the binary system ZrO₂ - Y₂O₃ and with the pyrochlor structure in the ternary system HfO₂ - Y₂O₃ - La₂O₃ was also studied. The specimens were prepared from nanocrystalline powders synthesized by the hydrolysis of zirconium salts in an acid medium at high temperatures. Conductivity was measured over the range 300–950°C in air. It was shown that phases with the fluorite and T-ZrO₂ structures in the investigated systems possess the highest electrical conductivities. Translated from Poroshkovaya Metallurgiya, Nos. 3/4(412), pp. 40–46, March–April, 2000.     

2-(6-甲基-2-苯并噻唑偶氮)-5-间二乙胺基酚分光光度法测定锌

报道 2 - (6 -甲基 - 2 -苯并噻唑偶氮 ) - 5 -间二乙胺基酚 (MBTAE)分光光度法测定微量锌。络合物的表观摩尔吸光系数为 1 0 4× 1 0 5 。络合比Zn :MBTAE =1 :2 ,Zn2 浓度在 0～ 2 0 μg/ 2 5mL范围内服从比尔定律 ,方法用于矿样中微量锌的测定 ,结果令人满意