连续流动注射分光光度法测定杏仁中氰化物和挥发酚的含量北大核心CSCD

提出了连续流动注射分光光度法同时测定杏仁中氰化物和挥发酚含量的方法。2.00 g杏仁样品经25 mL 0.05 mol·L^(-1)硫酸溶液涡旋1 min,浸泡10 min,水解释放样品中氰苷后,用2 g·L^(-1)氢氧化钠溶液固定待测物,并定容至50 mL。取上清液,经0.45μm滤膜过滤,滤液在优化的试验条件下采用连续流动注射分光光度法测定其中氰化物和挥发酚的含量。结果表明,氰化物和挥发酚的质量浓度在0.002~0.200 mg·L^(-1)内与对应的峰高呈线性关系,检出限分别为0.005 mg·kg^(-1)和0.0175 mg·kg^(-1)。取3份样品,每个样品重复测定6次,测定值的相对标准偏差(n=6)均小于2.0%。按照标准加入法对实际样品进行回收试验,回收率为97.6%~105%。方法用于分析10份杏仁样品,氰化物的检出量为10.6~56.4 mg·kg^(-1),平均值为32.3 mg·kg^(-1),挥发酚的检出量为14.7~54.8 mg·kg^(-1),平均值为31.9 mg·kg^(-1)。方法利用硫酸溶液水解样品中氰苷后用碱溶液固定,解决了碱溶液直接提取结果偏低的问题。     

全自动流动注射分析仪FIA6000在游离氰化物测定中的干扰因素及消除方法研究

本文主要论述了全自动流动注射分析仪FIA6000在测定水中游离氰化物的过程中遇到的干扰因素及其消除方法.     

天然水中亚硝酸氮和氨氮的合并带法流动注射分析

氨氮的测定,较广泛应用的是次氯酸钠作氧化剂重氮-偶氮光度法。由于次氯酸钠不稳定且氧化率较低,有人提出用次溴酸钠作氧化剂。近几年,发表了多篇流动注射分析(FIA)方法,但由于受灵敏度或仪器条件所限,难于普及使用。合并带法(MergingZones)具有试剂用量少等特点。Gine等采用合并带技术重氮-偶氮光度法FIA连续测定亚硝酸氮和硝酸氮。本文用次溴酸钠作氧化剂结合合并带技术,连续测定天然水中痕量亚     

水中氰化物的测定及保存研究

采用模块化流动注射分光光度法对环境水中的氰化物进行了测定,并与国家标准方法进行对照,所测结果经统计学处理,两种方法无显著性差异,精密度、准确度等各项分析指标符合分析标准。同时对不同水体中氰化物保存条件进行了研究,结果表明水样采集后应立即测试,不能立即测试的,加碱保存在4℃不应超过24 h。     

Cu(Ⅱ)-CAS-CTMAB三元配合物间接测定氰化物的流动注射分析方法研究

污水中氰化物的测定是环境分析与监测的重要项目之一,流动注射分析以其绝对的优势越来越受到人们的重视,本文利用铜(Ⅱ)、铬天青S(CAS)、溴化十六烷基三甲基铵(CTMAB)三元配合物间接测定氰化物,将FlA引入到三元配合物分光光度法中可大大简化操作条件,提高测试速度、精度和准确度。     

全自动流动注射-分光光度法测定土壤中氨氮

传统的氯化钾溶液提取分光光度法测定土壤中氨氮时,需要加入硝普钠-苯酚显色剂混匀后一定时间再加入二氯异氰尿酸钠显色剂,这个过程中人为接触苯酚等有机试剂的时间较长,对人体和环境有一定的危害;且传统的比色法显色时间至少需要5 h,显色时间较长,分析效率较低。应用全自动流动注射-分光光度法测定土壤中氨氮,考察了提取试剂的厂家、浓度等两个因素对实验的影响。采用氯化钾(1.00 mol/L)提取液配制标准曲线,在0～10.00 mg/L线性关系良好,方法检出限为0.031 mg/kg,样品相对偏差均小于5%,实际样品回收率为89.0%～114%。与传统的氯化钾溶液提取分光光度法相比,全自动流动注射-分光光度法具有自动进样、分析速率快,试剂耗量低,检测范围宽、保护环境等优点,适用于一般农用地、场地调查样品中氨氮的检测。     

基于吹气分离富集的异烟酸-巴比妥酸分光光度法测定水中痕量氰化物

鉴于氰化物转化成氯化氰是HJ 484-2009中异烟酸-巴比妥酸分光光度法测定氰化物的独立中间环节,利用氯化氰沸点低(14℃)、稳定性好的特性,提出了基于吹气分离富集的异烟酸-巴比妥酸分光光度法测定水中痕量氰化物含量的方法。以空气为载气,以异烟酸质量浓度为17.20 g·L^-1、巴比妥酸质量浓度为8.40 g·L^-1的溶液为吸收液(pH 5.85),利用特定的分离富集装置,完成空气净化、氰化物转化成氯化氰、氯化氰分离、氯化氰吸收及转化成聚甲炔染料等一系列过程,采用分光光度计测定吸收液在600 nm处的吸光度。结果表明：当样品、吸收液的体积分别为60.0,5.00 mL,空气流量为0.10 L·min^-1,采用3级吸收,以总吸光度作为响应值时,氰化物转化系数为94.2%,富集倍数为11.3倍,检出限(3s/k)为0.1μg·L^-1,测定线性范围为0.4～28.3μg·L^-1;方法用于井水及河水中痕量氰化物的测定,氰化物质量浓度为1.2～8.9μg·L^-1,回...     

流动注射安培法测定水中总氰化物

氰化物是一种广泛存在于自然界的剧毒物质,工业用途十分广泛,如湿法冶炼金、银等,主要污染源为电镀、炼焦、选矿、有机、化工、化肥等工业污水[1-2]。目前国内测定总氰化物的方法主要有硝酸银滴定法、分光光度法、电极法、色谱法等[3]。传统的化学法检测氰化物需蒸馏预处理,而且显色时还需水浴恒温,操作繁琐、费时、费力。流动注射安培法具有分析速度快、操作简单、样品和试剂消耗少等优点,已应用于环境、农业等领域中氰化物的检测。     

连续流动-分光光度法测定地表水中挥发酚和总氰化物

为了解北京市门头沟区永定河受污染情况,采用连续流动-分光光度法(以下简称为连续流动分析法)测定该河上、下游河水中挥发酚和总氰化物的含量。实验结果表明:永定河水未受挥发酚和总氰化物的污染,两者均在《地表水环境质量标准》中规定的Ⅴ类地表水水质限值范围之内。利用连续流动-分光光度法测定的标准曲线线性关系良好,线性相关系数均为0.999 7;重现性好,精密度分别为0.75%和0.65%;检出限低,分别为0.16μg/L和0.28μg/L;准确度高,均在真值范围内;加标回收率在92.6%～105%。与手动法相比,光度法分析速度快、试剂消耗量少、可批量检测,并减少了化学试剂对操作人员的伤害,适用于地表水中挥发酚和总氰化物的测定。     

流动注射光度法测定水中氰化物

基于氯化氰与1,3 二甲基巴比妥酸和吡啶 4碳酸在缓冲条件下反应,产生红色络合物的原理,提出了用流动注射光度法(CFA)测定自来水中氰化物。该方法线性范围为0～40.0μg·L-1,精密度和准确度高,检出限为0.002mg·L-1,适用于自来水中微量氰化物的检测。分析频率为30个样品·h-1,特别适合大批样品的测定。     

Direct determination of free cyanide in drinking water by ion chromatography with pulsed amperometric detection

Cyanide is a regulated contaminant in drinking water in the United States. This paper describes an ion chromatography method with pulsed amperometric detection (PAD) that directly determines free cyanide in drinking water. Samples are treated with sodium hydroxide to stabilize cyanide and with a cation-exchange cartridge to remove transition metals. Cyanide is separated by anion-exchange chromatography and detected by PAD with a waveform optimized for cyanide and used with a disposable silver working electrode. The recovery of cyanide spiked into five water samples was >80%. With an MDL of 1.0 microg/L, this method determines cyanide concentrations well below the reporting limits for free cyanide in drinking water.     

水中微量氰化物的测定方法：———异烟酸—巴比妥酸主次波长光度法

根据异烟酸－吡唑啉酮和吡啶－巴比妥酸光度法测定水中氰化物的基本原理，将二者重新组合成异烟酸－巴比妥酸体系，采用主次波长光度法测定。该法具有室温显色，显色所需时间较短，有色溶液稳定，对环境污染小，灵敏度高等优点，其最低检测限为０００１ｍｇ／Ｌ。特别适合于饮用水、生活污水、工业废水中微量氰化物的测定。通过对实际样品分析，与原方法进行比较，结果令人满意。     

Semi-quantitative "spot-test" of cyanide.

A selective, sensitive, rapid and simple-handling analytical method for the determination of cyanide at low detection limits in surface and underground water, soil and industrial waste samples was developed. The method is based on a reaction, proposed by Guilbault and Kramer, where free cyanide reacts with p-nitrobenzaldehyde to form an intermediate cyanohydrin, which reacts with o-dinitrobenzene to give a highly colored purple compound. The original procedure was modified for application in a small device containing a gas-permeable membrane. The cyanide is converted in the volatile hydrogen cyanide, which permeates through a PTFE membrane, reaching colorimetric reagents. In order to obtain semi-quantitative results, printed color scales were built. The method allows rapid, accurate, selective, low-cost and simple-handling determinations of free cyanide, even in complex samples. About 150 real samples were analyzed. Less than 10 ng of free cyanide per ml (10 microg l(-1)) can be easily detected. For more concentrated solutions, the results had been compared to those obtained using differential pulse polarography. The standard addition method was used for more diluted solutions.     

Kinetic spectrophotometric determination of nanogram amounts of cyanide

A sensitive kinetic method for determination of nanogram amounts of cyanide is reported. It is based on the measurement of the induction period imposed by cyanide on the copper(II)-catalysed oxidation of 3-hydroxybenzaldehyde azine (3-OHBAA) by potassium peroxydisulphate. Kinetic data are recorded spectrophotometrically at 465 nm, the maximum absorption wavelength of the oxidation product of 3-OHBAA. From the kinetic study and other experimental tests it may be concluded that the cyanide ion undergoes copper(II)-catalysed oxidation during the induction period. The calibration plot is linear in the range 150-600 ng/ml cyanide and the detection limit is 50 ng/ml. The precision of the method, expressed as the relative standard deviation, is 3.2% for 350 ng/ml cyanide. Good recoveries are obtained in applying the method to analysis for cyanide in water samples.     

A highly sensitive and selective fluorescent probe for cyanide based on the dissolution of gold nanoparticles and its application in real samples

We report a simple fluorescence method for detection of cyanide sensitively and selectively based on the dissolution of polymer-coated gold nanoparticles by cyanide. The lowest concentration for quantification of cyanide ions was 3.0×10(-7) M, and other common anions nearly have no influence. Furthermore, several real water samples spiked with cyanide, including local groundwater, tap water, boiled water, and lake water, were analyzed, and the experimental results demonstrated that our sensing system worked well in the above water samples, with a good linear correlation.     

High performance liquid chromatography determination of cyanide in urine by pre-column fluorescence derivatization

A method for the determination of cyanide in human urine has been developed. The method is based on the reaction of cyanide with 2,3-naphthalenedialdehyde and taurine to give a fluorescent product for reversed-phase HPLC separation and fluorometric detection. After centrifugation followed by dilution of urine samples, the specimens could be analysed directly by this method. The recovery of cyanide added to urine at concentration levels of 50-1000 pmol/mL was 85-96%. The detection limit of cyanide was 30 pmol/mL in urine. The method was successfully applied to the analysis of urine from smokers and nonsmokers. The mean concentrations of cyanide were found to be 215 pmol/mL for the former and 84 pmol/mL for the latter.     

Voltametrische Titration von Cyanid mit Quecksilber(II)-chlorid und ihre Anwendung zur Cyanidbestimmung in Wasser und Abwasser

Zusammenfassung Es wird ein Verfahren zur Titration von Cyanid mit Quecksilber(II)-chlorid beschrieben. Die Endpunktsbestimmung erfolgt voltametrisch unter Verwendung einer rotierenden Palladiumindicator- und einer Kalomelbezugselektrode. Die Methode ist im Bereich zwischen 40 ppb und 200 ppm anwendbar und wird vorzugsweise zur Cyanidbestimmung in Kamingasen, Wasser und Abwasser eingesetzt.

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Voltametric titration of cyanide with mercuric chloride and application to the determination of cyanide in water and waste water

A method is described for the volumetric determination of cyanide with mercuric chloride solution. The end-point detection is carried out voltametrically using a polarized rotating palladium electrode and a calomel reference electrode. The method covers a concentration range of between 40 ppb and 200 ppm cyanide and is in particular suitable for cyanide determinations in stack gases, water and waste water.

     

数码比色法测定环境及生物样品中的氰化物浓度

在传统氰化物检测方法的基础上,提出了一种新的方法—数码比色法。在一定条件下,苦味酸与氰化物生成黄色化合物,用数码相机对显色溶液拍照,通过数码比色,进行灰度处理,照片的三原色值与氰化物的浓度成线性关系,可以直接分析出其氰化物的浓度。对唾液样品测定,其回收率为98.18%,对照品测定的相对标准偏差RSD为1.5%。研究结果表明,数码比色法具有准确度和精密度都比较理想,方便快速、环境友好等特点。     

检测水中氢氰酸的新型便携式RGB色度传感器

基于氢氰酸在碱性条件下与水合茚三酮反应,溶液呈紫红色的检测原理,建立了一种快速、灵敏检测水中氢氰酸的分析方法。对显色剂种类、水合茚三酮浓度、pH值、反应温度、反应时间等因素进行优化。采用源于归一化RGB系统的RGB色度法进行检测,可克服基于RGB模型的由于光强变化导致三刺激值变化的不足。在最优条件下,色度值与氢氰酸的质量浓度在0.04～3.96 mg/L范围内呈良好线性,对R值的理论检出限为0.038 mg/L,实际检出限为0.04 mg/L。用于人工水样中氢氰酸的测定,回收率为98.3%～111%。该方法具有较高的选择性、灵敏度和较好的重复性,在检测环境中其他有毒有害物质方面同样具有应用潜力。     

Determination of cyanide by a flow injection analysis-atomic absorption spectrometric method

A new flow injection analysis (FIA) procedure is proposed for the indirect atomic absorption spectrometric determination of cyanide. The FIA manifold is based on the insertion of the sample into a distilled water carrier, then the sample flows through a solid-phase reactor filled with silver iodide entrapped in polymeric resin beads. The calibration graph is linear over the range 0.2-6.0 mg l-1 of cyanide (correlation coefficient 0.9974), the detection limit is 0.1 mg l-1, the sample throughput is 193 h-1 and the RSD is 0.8%. The method is simple, quick and more selective than other published FIA procedures. The reproducibility obtained by using different solid-phase reactors and solutions is in the range 2.2-3.1% (RSD). The method was applied to the determination of cyanide in commercial samples such as pharmaceutical formulations and industrial electrolytic baths.