催化动力学光度法测定痕量苯酚

研究了在硫酸介质中苯酚对Ｉ＾－１催化Ｃｅ＾４＋－Ａｓ（Ⅲ）反应的抑制作用及其动力学条件。建立了用催化动力这光度法测定痕量苯酚的新方法，结果表明，在０．００１ｍｏｌ／ＬＣｅ（ＳＯ４）２，０．００１２５ｍｏｌ／Ｌ，Ａｓ２Ｏ３，０．０１ｍｇ／Ｌ，ＫＩ，０．０１２５ｍｏｌ／Ｌ，Ｈ２ＳＯ４和０．１３％（ｗ／ｖ）ＮａＣｌ溶液中测定苯酚，其表面摩尔吸光系数为２．１×１０＾５Ｌ．ｍｏｌ＾－１．ｃｍ＾－１，线性范围     

丁基罗丹明B—钼酸盐光度法连续测定铈和钪

在聚乙烯醇（ＰＶＡ）存在下，丁基罗丹明Ｂ（ＢＲＢ）分别与铈钼、钪钼杂多酸络阴离子形成离子缔合物，其最大吸收均位于５７０ｎｍ，表面摩尔吸光度分别为εＣｅ＝３．９６×１０＾６Ｌ．ｍｏｌ＾－１．ｃｍ＾－１，εＳｃ＝４．７１×１０＾５Ｌ．ｍｏｌ＾－１．ｃｍ＾－１，服从比耳定律范围分别为０－２４μｇ／Ｌ Ｃｅ和０－６０μｇ／ＬＳｃ，测定极限为Ｃｅ１．０μｇ／Ｌ（ｎ＝１２）和Ｓｃ１．９μｇ／Ｌ（ｎ＝１０），对     

哌仑西平的单扫描示波极谱法测定

本报道一种测定哌仑西平的单扫描示波极谱法，在０．１ｍｏｌ／ＬＮＨ４Ｃｌ－ＮＨ３．Ｈ２Ｏ（ｐＨ８．０±０．１）缓冲液中，哌仑西平有一极谱还原波，其峰电位为－１．５１Ｖ（ｖｓ．ＳＣＥ），其一阶导数峰高与哌仑西闰浓度在６．６×１０＾－７－４．６×１０＾－６ｍｏｌ／Ｌ（ｒ＝０．９９８１）和６．６×１０＾－６－１．６×１０＾－５ｍｏｌ／Ｌ（ｒ＝０．９９９１）范围内有线性关系，检测限为３．４×１０－７ｍｏｌ     

α-P2W17O10-61杂多阴离子薄膜修饰电极的制备

研究了杂多酸阴离子α－Ｐ２Ｗ１７Ｏ＾１０－６１修饰电极的制备及其化学性质,α－Ｐ２Ｗ１７Ｏ＾１０－６１修饰电极对ＢｒＯ＾－３具有催化作用。催化电流△Ｉｐ与「ＢｒＯ＾－３」在７．０＊１０＾－６－１．０＊１０＾－４ｍｏｌ／Ｌ范围内呈良好线性关系。用此电极测定了天然水中ＢｒＯ＾－３的含量,结果令人满意。     

流动注射化学发光抑制法测定抗坏血酸

基于抗坏血酸对Ｌｕｍｉｎｏｌ－ＫＩＯ４－Ｈ２Ｏ２体系化学发光反应的抑制作用,建立了化学发光抑制快速测定抗坏血酸的新方法。该方法线性范围为１．０＊１０＾－７－１．０＊１０＾－５ｍｏｌ／Ｌ,检出限为６．０＊１０＾－８ｍｏｌ／Ｌ,对８．０＊１０＾－７ｍｏｌ／Ｌ抗坏血酸１１次平行测定的相对标准偏差为１．０％。用于维生素Ｃ片剂及注射液中抗坏血酸含量的测定,结果令人满意。     

硫化物的快速分光光度法测定

提出了测定微量硫化物的快速亚甲蓝分光光度法，实验结果表明，在硫酸溶液中，Ｋ２Ｃｒ２Ｏ７＋对二甲氨基苯胺＋Ｓ＾－２迅速显色反应形成亚甲蓝，表现摩尔吸收系数为４．０６×１０＾４Ｌ．ｍｏｌ＾－１．ｃｍ＾－１；最大吸收波长为６６４ｎｍ；线性范围为０～０．８ｍｇ／Ｌ，实验了采用全差示光度法直接测定水中硫化物的条件，用于某江水中２１．６μｇ／Ｌ硫化物测定时，相对标准偏差为３．２％（ｎ＝６）；试样的标准加入回收     

流动注射化学发光同时测定废水中的三价铬和六价铬

首次将镀铜锌粒作成优良的还原柱，在线还原Ｃｒ（Ⅵ）成Ｃｒ（Ⅲ），以鲁米诺－Ｈ２Ｏ２（ＫＢｒ）体系流动注射化学发光同时测定废水中两种价态的铬。分析速率为６０试样／ｈ；线性范围为１．０×１０＾－５－１．０×１０＾－９ｍｏｌ／Ｌ；测Ｃｒ（Ⅲ）及Ｃｒ（Ⅵ）的相对标准偏差（ｎ＝６）分别为０．３７％－４．０％及１．２％－４．４％；测定Ｃｒ（Ⅲ）的检出限２．３×１０＾－１１ｍｏｌ／Ｌ。测定结果与标准方法无显差     

用钼酸盐和罗丹明B连续光度法测定铈和钪

聚乙烯醇存在下，铈或钪钼杂多酸与罗丹明Ｂ（ＲＢ）形成离子缔合物，最大吸收均位于５７０ｎｍ，摩尔吸光系数分别为１．１６×１０＾６和５．６２×１０＾５Ｌ．ｍｏｌ＾－１．ｃｍ＾－１，ｃｍ＾－１，０－１．２μｇ／２５ｍＬＣｅ和０－２．０μｇ／ｍＬＳｃ服从比耳定律，检测限１．５ｎｇ／ｍＬＣｅ（ｎ＝１０）和１．１ｎｇ／ｍＬＳｃ（ｎ＝９）。缔合物的摩尔比为Ｃｅ：ｍＯ：ＲＢ＝１：６：３和 Ｓｃ：Ｍｏ：ＲＢ＝１：１     

铬（VI）与5—溴水杨基荧光酮的显色反应及应用

本文研究了Ｃｒ（Ⅵ）与５－溴水杨基荧光酮（５－Ｂｒ－ＳＡＦ）的显色反应。在ｐＨ６．０ＫＨ２ＰＯ４－ＮａＯＨ缓冲溶液中，Ｃｒ（Ⅵ）与５－Ｂｒ－ＳＡＦ、ＣＴＭＡＢ形式稳定的三元络合物，其最大吸收波长为５７２ｎｍ，表观摩尔吸光系数为１．４２×１０＾５Ｌ·ｍｏｌ＾－１·ｃｍ＾－１。Ｃｒ（Ⅵ）浓度在０￣２．５μｇ／１０ｍＬ间服从比耳定律。用此法测定了环境水样中微量Ｃｒ（Ⅵ），获得满意结果。     

用分光光度法连续测定血清中微量铜、锌的研究

研究了在ＴｒｉｔｏｎＸ－１００存在下,在ＰＨ８．０的乙醇介质中,用５－Ｂｒ－ＰＡＤＡＰ作为显色剂,应用分光光度法连续测定血清中的铜,锌。本法具有较高的灵敏度,Ｃｕ＾２＋－５－Ｂｒ－ＰＡＤＡＰ的ε为８．５０＊１０＾４Ｌ．ｍｏｌ＾－１．ｃｍ＾－１,Ｚｎ＾２＋－５－Ｂｒ－ＰＡＤＡＰ的ε为９．６５＊１０＾４Ｌ．ｍｏｌ＾－１．ｃｍ＾－１。铜线性范围为０－０．４５ｍｇ．Ｌ＾－１,锌线性范围为０－０．４０ｍｇ．     

KBrO3-KBr紫外分光光度法测定痕量苯酚

研究了在盐酸介质中以 KBrO3-KBr 紫外分光光度法测定痕量苯酚的条件,在浓度为 0.6mol/L HCl,3×10-5mol/L KBrO3,5×10-4mol/L KBr,6×10-4mol/L KI 溶液中测定苯酚时,线性范围为 0.10～2.5mg/L,表观摩尔吸光系数为 1.89×104L·mol-1·cm-1,Sandell 指数为 4.98μg/cm2.本法已用于测定废水中苯酚.     

导数-同步荧光法同时测定苯甲酸和水杨酸

本文建立了一种同时测定苯甲酸、水杨酸的新方法.苯甲酸、水杨酸的检测限分别为 0.026 μg/mL,0.083 μg/mL;相对标准偏差分别为 1.8％和 3.1％.将该方法用于商品杀菌防腐剂中苯甲酸及水杨酸的同时测定,结果满意.     

抑制褪色光度法测定油炸面制食品中痕量铝

建立抑制褪色光度法快速测定食品中痕量铝的方法。在硫酸介质中,一定量的铝离子对溴酸钾氧化罗丹明B褪色有抑制作用,据此建立了抑制褪色光度法快速测定食品中痕量铝的新体系,最大吸收波长为550 nm。在1 mol/L硫酸介质中,铝含量在0.07~0.4μg/mL范围内与吸光度具有良好的线性关系,相关系数r=0.9995,检出限为0.02μg/mL。用该方法测定油炸面制食品中痕量铝,测定结果的相对标准偏差为1.3%~3.1%(n=11),加标回收率为99.3%~103.5%。该方法测定结果准确可靠,可用于食品中痕量铝的测定。     

流动注射化学发光法测定痕量NO_2~-的研究与应用

Based on the principle of the reaction of NO2-with I-and formation of I2 in HCl solution,and the chemiluminescence(CL) reaction between luminol and I2 in an alkaline medium.A fairly sensitive,simple and rapid flow-injection analysis-chemiluminescence method for the determina-tion of trace nitrite with the luminal-I——NO2-coupling luminescence system has been developed.Experiment conditions of flow-injection analysis are optimized.When satisfying the condition that Luminol as 4.0×10-4 mol/L,0.7 % KI,0.04 mol/...     

靛蓝胭脂红-溴酸钾体系催化光度法测定微量碘

研究了在室温及0．4mol/L H2SO4介质中碘离子对KBrO3氧化靛蓝胭脂红褪色反应的催化作用,建立了一种测定微量碘的新方法。碘离子浓度在0．20－2．0μg/mL范围内与△A呈线性关系,检测限为0．14μg/mL。多数常见离子无干扰。可用于海带中微量碘的测定。     

Interaction of nickel with 4-(2'-benzothiazolylazo) salicylic acid (BTAS) and simultaneous first-derivative spectrophotometric determination of nickel(II) and iron(III)

The solution properties of nickel complex with 4-(2'-benzo-thiazolylazo) salicylic acid (BTAS) have been studied by zero-order absorption spectrophotometry in 40% (v/v) ethanol at 20 degrees C and an ionic strength of 0.1 mol dm(-3) (KNO(3)). The equilibria that exist in solution were established and the basic characteristics of complexes formed were determined. A new direct spectrophotometric method for the determination of trace amounts of the nickel is proposed based on the formation of the Ni (BTAS) complex at pH 7.0. The absorption maximum, molar absorbtivity, and Sandell's sensitivity of 1:1 (M:L) complex are 525 nm, 0.6 x 10(4) l mol(-1) cm(-1) and 2.824 x 10(-9) microg cm(-2), respectively. The use of first-derivative spectrophotometry eliminates the interference of iron and enables the simultaneous determination of nickel and iron using BTAS. Quantitative determination of Ni(II) and Fe(III) is possible in the range (0.59-7.08) and (2.1-8.4) microg ml(-1), respectively with a relative standard deviation of 0.5%. The proposed method has been successfully applied to the simultaneous spectrophotometric determination of nickel and iron in steel alloys and aluminum alloys.     

Selective leaching of elements associated with Mn - Fe oxides in forest soil, and comparison of two sequential extraction methods

For selective dissolution of Mn oxides as components of soil (easily reducible oxides) 0.05 mol L(-1) and 0.1 mol L(-1) NH2OH.HCl acidified to pH 2 and for dissolution of Fe oxides (crystalline form of the oxides) 0.25 mol L(-1) NH2OH.HCl in 25% acetic acid, 0.2 mol L(-1) oxalate buffer and 0.1 mol L(-1) ascorbic acid in oxalate buffer were tested. Dissolved elements were determined by ICP-MS and ICP-OES. The studies indicate that the use of 0.05 mol L(-1) NH2OH.HCl in nitric acid solution (pH 2) and 0.1 mol L(-1) ascorbic acid in 0.2 mol L(-1) oxalate buffer led to selective leaching of trace metals bound by Mn and Fe oxide phases in soil. Comparison of different extraction schemes indicates that the trace elements investigated are mainly bound to minerals consisting of crystalline Fe oxides and insoluble minerals (under the extraction conditions used). The studies also indicate that Mn oxides and organic matter retain a major mobile fraction of the elements investigated in the soil.     

Organic,inorganic and total mercury determination in fish by chemical vapor generation with collection on a gold gauze and electrothermal atomic absorption spectrometry

A method for organic, inorganic and total mercury determination in fish tissue has been developed using chemical vapor generation and collection of mercury vapor on a gold gauze inside a graphite tube and further atomization by electrothermal atomic absorption spectrometry. After drying and cryogenic grinding, potassium bromide and hydrochloric acid solution (1 mol L^− 1 KBr in 6 mol L^− 1 HCl) was added to the samples. After centrifugation, total mercury was determined in the supernatant. Organomercury compounds were selectively extracted from KBr solution using chloroform and the resultant solution was back extracted with 1% m/v L-cysteine. This solution was used for organic Hg determination. Inorganic Hg remaining in KBr solution was directly determined by chemical vapor generation electrothermal atomic absorption spectrometry. Mercury vapor generation from extracts was performed using 1 mol L^− 1 HCl and 2.5% m/v NaBH₄ solutions and a batch chemical vapor generation system. Mercury vapor was collected on the gold gauze heated resistively at 80 °C and the atomization temperature was set at 650 °C. The selectivity of extraction was evaluated using liquid chromatography coupled to chemical vapor generation and determination by inductively coupled plasma mass spectrometry. The proposed method was applied for mercury analysis in shark, croaker and tuna fish tissues. Certified reference materials were used to check accuracy and the agreement was better than 95%. The characteristic mass was 60 pg and method limits of detection were 5, 1 and 1 ng g^− 1 for organic, inorganic and total mercury, respectively. With the proposed method it was possible to analyze up to 2, 2 and 6 samples per hour for organic, inorganic and total Hg determination, respectively.     

液相微萃取-离子色谱法测定污水中痕量芳香胺

基于中空纤维液相微萃取技术,建立了河流污水中两种芳香胺类物质（邻甲苯胺和对氯苯胺）的离子色谱分析方法。采用中空纤维液相微萃取和离子色谱联用技术,对中空纤维萃取条件进行优化。优化的萃取条件：萃取溶剂为正辛醇,供体相中NaOH的浓度为0.01mol/L, NaCl的浓度为500g/L,接受相中HCl的浓度为0.1 mol/L,搅拌速度为430r/min,萃取时间为30min,在优化条件下,邻甲苯胺的富集倍数为88倍,对氯苯胺的富集倍数为124倍。供体相中邻甲苯胺和对氯苯胺的浓度在0.005–0.1mg/L范围内成良好线性,相关系数为0.9998-0.9999 ,检出限为0.2-0.5μg /L,相对标准偏差为0.85-3.38 %。结论：这种方法操作简单,环境友好,提高了离子色谱检测芳香胺类物质的灵敏度。     

微色谱柱分离-光度法测定高稀土铁矿石中的微量钍

采用HD-8微色谱柱对高稀土铁矿石样品(白云鄂博矿)中的钍进行分离富集,探讨了影响其分离富集的条件。实验表明,在4 mol/L HCl介质中钍可被树脂完全吸附,用3 mL 40 g/L草酸铵溶液可以从吸附柱上完全解吸钍,并结合偶氮胂Ⅲ分光光度法进行测定。所建立的方法适合于含铁、稀土量高的矿石样品中微量钍的分离与测定。