2,6-二甲酰基对甲苯酚的固相合成

以活性纳米γ-MnO2为氧化剂,在无溶剂状态下用2,6-二甲羟基对甲苯酚为原料合成了2,6-二甲酰基对甲苯酚,其结构经^1H NMR,IR和元素分析确证。较适宜的反应条件为：2,6-二甲羟基对甲苯酚0．85g(5mmol),n(2,6-二甲羟基对甲苯酚)：n(活性γ-MnO2)=1：2,间歇性研磨提供充分的自扩散时间(1h～2h),总研磨时间为5h～6h,收率26％。该法与液相合成法相比,反应时间缩短到1／8,产率提高了6％。     

胶束增敏 2,3,7-三羟基-9-[3,5-二溴-4-(2,5-二羟基)苯偶氮]苯基荧光酮与锆(Ⅳ)显色反应的研究

系统研究了在混合表面活性剂 CTMAB-Tween-80 存在下,新显色剂 2,3,7-三羟基-9-[3,5-二溴-4-(2,5-二羟基)苯偶氮]苯基荧光酮(DBAPPF) 与 Zr(Ⅳ)的显色反应及其光度性质并讨论了混合表面活性剂对显色反应的增敏机理.在浓度为 0.4mol/L 的 HCl 介质中,新试剂与 Zr(Ⅳ)和表面活性剂形成胶束络合物,混合表面活性剂有较强的增敏作用,络合物最大吸收波长为 539 nm,表观摩尔吸光系数为 1.55×105 L·mol-1·cm-1.锆(Ⅳ)的质量浓度在 0～0.32 mg/L 范围内服从比尔定律.方法已用于铝合金中微量锆的测定.     

聚合物基板表面状态对异相接枝的影响研究

研究了对于羟丙基纤维素（HPC）基板进行表面修饰时,基板表面状态的调控 对基板表面化学接枝的影响。用双官能团化合物2,4-甲苯二异氰酸酯（TDI）作为 接枝桥梁,其对位的异氰酸酯基先和基板上的羟基反应,保留的邻位异氰酸酯基进 一步再与丙烯酸的羟基反应,让接枝在基板上的活性丙烯酸分子继续和丙烯酸溶液 聚合,通过这种途径在基板表面修饰聚丙烯酸。基板制备时,由于不同介质对HPC 基板表面的不同诱导作用,导致表面组成各异,大大影响了接枝反应的效果。红外 光谱和二次离子飞行时间质谱均证明了可以用2,4-甲苯-二异氰酸酯（TDI）分子 做接枝桥梁在基板表面异相接枝上羟基并进一步接枝聚丙烯酸,从而达到修饰基板 的目的。     

新试剂3,5-二溴-4-偶氮间苯二酚苯基荧光酮吸光光度法测定微量锰

2,3,7-三羟基-9-[3,5-二溴-4-(2′,4′-二羟基)苯偶氮]苯基荧光酮(DBARPF)是一种新的荧光酮类显色剂,在表面活性剂CTMAB存在下,于pH 9.0NH_3—NH_4Cl缓冲溶液介质中与Mn(Ⅱ)形成稳定的三元胶束配合物,其最大吸收波长为578nm,表观摩尔吸光系数为1.15×10~5,Mn(Ⅱ)的浓度在0～8μg/25ml范围内符合比耳定律。拟定方法用于钢铁样品中微量锰的测定,结果满意。     

2,6-二羟基甲苯的合成

2;6-二羟基甲苯的合成;二羟基甲苯;间苯二酚;二氯乙烷;烷基化;甲酰化;黄鸣龙反应     

DBM—MSA光度法测定化妆品中铅

为建立一个新的测定化妆品中铅的分光光度法,在0．24mol／L的磷酸介质中,铅与DBM—MSA{3-[（2-磺酸基苯）偶氮]-6-[2,6-二溴-4-甲基苯）偶氮]-4,5-二羟基-2,7-萘二磺酸}反应形成1：2的蓝色配合物,在波长630nm处比色测定。结果表明,铅量在0—1μg／mL范围内符合比耳定律;样品测定的相对标准偏差为1．24％～4．59％,标准加入回收率为95．0％～107．0％,化妆品中共存物质不干扰测定,方法简便,选择性好,结果满意。     

铈(Ⅳ)-3,4-二羟基苯甲酸-奎宁化学发光体系的研究与应用

实验发现,3,4-二羟基苯甲酸与铈(Ⅳ)在酸性介质中产生弱化学发光反应,奎宁存在能增强此发光,由此建立了化学发光法测定微量3,4-二羟基苯甲酸的新方法。该方法的线性范围为8.0×10-7～1.0×10-4mol/L,检出限为5.0×10-8,对8.0×10-6mol/L的3,4-二羟基苯甲酸进行11次测定的相对偏差为3.0%。该法应用于测定汉江水中加入的3,4-二羟基苯甲酸,结果令人满意。     

影响2,6-二氨基甲苯标准物质纯度的因素及研究

着重研究了以铁—盐酸为还原剂,还原2,6-二硝基甲苯制备2,6-二氨基甲苯标准物质的过程中,反应介质、温度、搅拌速度以及分离精制阶段对2,6-二氨基甲苯的产率和纯度的影响。     

固相萃取-高效液相色谱法测定鱼/虾生物体中甲苯咪唑及代谢物的残留

建立了同时测定鱼、虾生物体中甲苯咪唑及代谢物-氨基甲苯咪唑和羟基甲苯咪唑残留的分析方法。样品以水和乙酸乙酯提取,正己烷去脂、MCX固相萃取柱净化,高效液相色谱-紫外检测器测定。重点研究了样品前处理方法,并对各种不同的固相萃取柱的净化效果和准确度进行了研究。甲苯咪唑及代谢物在5～200μg/kg的添加水平下回收率为81.4%～95.3%,相对标准偏差为1.9%～8.6%,方法线性范围为10～2000ng/mL。方法检测限为甲苯咪唑:5μg/kg,羟基甲苯咪唑:5μg/kg,氨基甲苯咪唑:10μg/kg。     

5-（5-溴-2-吡啶偶氮）-2，4-二氨基甲苯催化光度法测定钯

在H2SO4介质和室温条件下,微量钯（Ⅱ）对KBrO3氧化5-（5-溴-2-吡啶偶氮）-2,4-二氨基甲苯（5-Br-PA—DAT）褪色反应具有显著的催化作用,据此建立了测定微量钯的催化光度法．方法的检测限为0．034mg／L,线性范围0．2～0．75mg／L．已用于钯碳催化剂及水样中钯含量的测定,标准加入回收率为97．2％～99．0％,结果满意．     

硫氰酸根-吡啰红G荧光光度法测定水及尿样中微量钼

本文利用吡啰红G作为荧光试剂,在强酸性条件下,用丙酮作增溶剂,硫脲作还原剂,Cu~(2+)作催化剂,使Mo(Ⅵ)还原为Mo(Ⅴ)并与SCN~-和试剂形成离于缔合物.该缔合物的荧光强度在测定条件下与钼的浓度成正比,λ_(?)=528/552nm;此法灵敏度高,选择性好,线性范围为0.0～1.4μg/25ml.直接用于自来水和尿样中钼的测定,回收率在97%～105%之间,结果满意.     

Mechanical properties of hybrid glass/sugar palm fibre reinforced unsaturated polyester composites

A research has been carried out to investigate the mechanical properties of composites made by hybridizing sugar palm fibre (Arenga pinnata) with glass fibre into an unsaturated polyester matrix. Hybrid composites of glass/sugar palm fibre were fabricated in different weight ratios of strand mat glass fibres: sugar palm fibres 4:0, 4:1, 4:2, 4:3, 4:4, and 0:4. The hybrid effects of glass and sugar palm fibre on tensile, flexural and impact properties of the composites were evaluated according to ASTM D5083, ASTM D790 and ASTM D256 respectively. Results have been established that properties of hybrid glass/sugar palm composites such as tensile strength, tensile modulus, elongation at break, toughness, flexural strength, flexural modulus and impact strength are a function of fibre content. The failure mechanism and the adhesion between fibres/matrix were studied by observing the scanning electron micrographs of impact fracture samples. In general, the incorporation of both fibres into unsaturated polyester matrix shows a regular trend of increase in the mechanical properties.     

镍—亚硝基红盐—氯化癸基吡啶体系的络合物吸附波研究及应用

在0.020mol/硼砂-0.0030％亚硝基红盐-0.0040％氯化癸基吡啶体系中,镍有一灵敏的络合物吸附波,峰电位-0.55V(υs. Ag/AgCl),线性范围0.2～1600ng/ml,可用于水样和发样的测定。镍与亚硝基红盐形成1:3的二元络合物。络合物在滴汞电极上的吸附,低浓度符合Langmuir吸附等温线,高浓度符合Frumkin吸附等温线。     

Characterisation of flavonols in broccoli (Brassica oleracea L. var. italica) by liquid chromatography-uV diode-array detection-electrospray ionisation mass spectrometry

The flavonoid composition of broccoli inflorescences has been studied by LC/UV-DAD/ESI-MSn. A large number of hydroxycinnamic acid esters of kaempferol and quercetin glucosides has been characterised. The structures of the flavonoid glycosides were analysed after alkaline hydrolysis, and were identified as 3-sophoroside/sophorotrioside-7-glucoside/sophoroside of kaempferol, quercetin and isorhamnetin (this last found in trace amount). These complex quercetin and isorhamnetin glucosides have not been previously characterised in nature. In addition, several less complex glucosides based on the same aglycones have been identified. The effect of sugar substitution and acylation on chromatographic mobility and ESI ionisation and fragmentation are discussed.     

Sugar cane bagasse lignin as stabilizer for rubbers: Part III—Styrene/butadiene rubber and natural rubber

The stabilizing effect of a natural antioxidant, sugar cane bagasse-lignin, on the photo-chemical, thermal and environmental degradation of styrene/butadiene rubber and of natural rubber has been studied. For natural rubber the stabilizer was investigated in various concentrations in the pure form and for styrene/butadiene rubber it was also studied in substitution for a hindered phenol in a commercially used formulation which includes a p-phenylenediamine. For the photo-degradation of natural rubber, stabilization becomes appreciable only above a stabilizer concentration of 5·0% whilst in thermal degradation a concentration of 1·0% is sufficient to increase the induction period by a factor of 3 in relation to pure rubber. For styrene/butadiene rubber the same effect occurs; a concentration of 2·0% increases the induction period for photo-degradation by a factor of 1·5 whilst 1·0% increases the induction period for thermodegradation by a factor of 26 in relation to the pure unstabilized rubber. Substitution of the hindered phenol by lignin in the commercial formulation increases the induction period for the thermal degradation by a factor of 6 in relation to the commercial sample. In the environmental ageing experiments the influence of the lower photo-stabilizing effect predominated over the strong thermostabilizing activity of the lignin for both rubbers.     

荧光法测定糖果中的总糖含量

合成了带有荧光基团的分子探针,光谱显示探针对糖类物质具有较强的荧光响应.通过条件优化,选取328 nm作为荧光激发波长,p H 10.0的缓冲溶液为最佳测定介质,当测试溶液中葡萄糖浓度为0.05~1 mmol/L时,显示良好的响应线性.方法对果糖中总糖含量测定的检测限为6.2μmol/L,回收率在76.4%~90.0%,RSD达到3.18%.     

Calorimetric studies of binary systems of 1,3,5-trinitrobenzene with naphthalene, anthracene and carbazole. II. Phase diagrams

The phase diagrams of the binary systems of 1,3,5-trinitrobenzene (TNB) with naphthalene, anthracene and carbazole have been determined by differential scanning calorimetry and optical microscopy over the temperature range 180 K to just above the melting point. All systems show the same features: (i) systems form nearly ideal double simple-eutectic type phase diagrams with 1 : 1 complex, (ii) each one of three known modifications of TNB may exist as a component of the complex—TNB eutectic mixtures. (iii) measured liquidus lines of complexes agree within experimental error with those calculated by the Vieland equation for a completely dissociated complex in the liquid phase, whereas the experimental liquidus lines for the parent components deviate slightly from those predicted by the Schröder—van Laar equation, indicating some degree of complexing in the liquid phase.

The solubility parameter theory has been used to clarify this discrepancy. Applying this theory to the liquidus lines of complexes, we have found that these TNB complexes are still stable upon fusion, and an approximate degree of dissociation amounted to 90% at the melting point in all three cases.

The enthalpy of complex formation, ΔH⁰, both in the liquid and solid state has been determined. The values of ΔH⁰ show that in the solid state the carbazole—TNB complex is the most stable, and the naphthalene—TNB complex is the least stable.     

Continuous ethanol production from nonsterilized carob pod extract by immobilizedSaccharomyces cerevisiae on mineral kissiris using a two-reactor system

The continuous production of ethanol from nonsterilized carob pod extract by immobilizedSaccharomyces cerevisiae on mineral kissiris using one- and two-reactor systems has been investigated. A maximum ethanol productivity of 9.6 g/L/h was obtained at an initial sugar concentration of 200 g/L and D = 0.4 h^-1 with 68% of theoretical yield and 34% of sugar utilization using the one-reactor system. AtS ₀ = 200 g/L, D = 0.05 h^-1, 83% of theoretical yield, and 64% of sugar utilization, an ethanol productivity of 2.6 g/L/h was achieved. In the tworeactor system, a maximum ethanol productivity of 11.4 g/L/h was obtained at S₀ = 200 g/L and D = 0.4 h^-1 with 68.5% of theoretical yield and 41.5% of sugar utilization. The two-reactor system was operated at a constant dilution rate of 0.3 h^-1 for 60 d without loss of the original immobilized yeast activity. In this case, the average ethanol productivity, ethanol yield (% of theoretical), and sugar utilization were 10.7 g/L/h, 71.5%, and 48%, respectively.     

Direct Spectrophotometric Determination of Trace Cadmium(II) in Food Samples with 2-Acetylmercaptophenyldiazoaminoazobenzene (AMPDAA)

A novel chromogenic reagent, 2-acetylmercaptophenyldiazoaminoazobenzene (AMPDAA), has been prepared by coupling 2-aminoacetylthiophenol to 4-aminoazobenzene through the –NH–N=N– group. In the presence of TritonX-100, AMPDAA reacts with Cd(II) in 1:1 triethanolamine medium to form a red complex with maximum absorption at 529nm. Under the optimal conditions, Beers law is obeyed over the range of 0.0 to 1.0µgmL^–1 Cd(II), and the apparent molar absorptivity is 2.4× 10⁵Lmol^–1cm^–1. Based on this, a highly sensitive and selective spectrophotometric method has been developed for direct determination of trace cadmium. The detection limit and the quantification limit were found to be 6.5 and 9.7µgL^–1, respectively. The absorbance of AMPDAA-Cd(II) complex was 0.1881± 7.5×10^–3 with a 4.9% relative standard deviation for five repeated measurements of the sample containing 2µg of cadmium in 25mL solution under the same experimental conditions. Interference of foreign ions was also investigated. Except for Ag(I) and Hg(II), most foreign ions can be tolerated in considerable amounts. Interference caused by Ag(I) and Hg(II) can be reduced by adding sodium thiosulfate. The proposed method has been applied to the determination of trace cadmium in rice, grain and flour samples with satisfactory results.     

蔗糖酯合成新方法的研究

本法以苛性钾与脂肪酸甲（乙）酯首先反应生成的部分中性皂作为乳化分散剂，使蔗糖和脂肪酸甲（乙）酯在熔融状态下直接发生酯交换反应合成蔗糖酯．适宜的反应条件为：蔗糖／硬脂酸甲酯／苛性钾／催化剂的摩尔比１：（１～２）：（０．４～０．６）：０．００３６；１３５～１４０℃、２６６６～６６６５Ｐａ负压下反应３～３．５ｈ。所得粗产物含蔗糖酯５５％，其中单酯６２％。