甲醛肟分光光度法测定三氧化钼及金属钼中微量锰

微量锰的比色测定方法,常用高锰酸盐比色法。此法虽较特效和准确,但在分析三氧化钼及金属钼中的微量锰时,需经沉淀分离,操作繁琐,且灵敏度达不到要求。用甲醛肟比色测定锰,前人已进行很多工作,我们在前人工作的基础上,拟定了用甲醛肟分光光度法测定三氧化钼及金属钼中微量锰的方法,具有灵敏、准确和操作简便等特点,适用于含锰量为1×10~(-4)％—4×10~(-3)％的样品分析。 (一)主要试剂 1.铜试剂:4％(新鲜配制,过滤后使用)。 2.甲醛肟溶液:1M,取盐酸羟胺7克溶于水中,加入38％甲醛20毫升,     

分光光度法快速测定毒鼠强的研究

本文将毒鼠强在酸性条件下分解,分解产生的甲醛用水蒸汽蒸馏使之与干扰物质分离,再根据Hantzsch反应原理,用乙酰丙酮-乙酸铵溶液作显色剂分光光度法测定甲醛,从而间接测定毒鼠强的含量。本法的线性范围为5~40 mg/kg。本法干扰少,操作简便、快速,可用于中毒样品的测定。     

高效液相色谱直接测定甲醛衍生物反应条件的研究

研究了直接用于液相色谱测定甲醛与2,4-二硝基苯肼的反应条件,使反应在弱酸性和50％的乙腈条件下进行,反应产物甲醛衍生物不需要有机溶剂萃取,可直接用于液相色谱分析,避免了萃取过程的损失。该反应条件与传统的在强酸性条件下的反应进行比较。本实验所研究的反应条件用于液相色谱测定甲醛具有操作方便、准确和应用范围广等特点。在样品中添加5．14,10．28和51．4mg/kg,回收率分别为108％、93．1％和86．2％相对标准偏差(n=10)分别为1．13％、1．34％和1．29％。     

不同吸收剂影响大气中二氧化硫测定的探讨

对盐酸玫瑰苯胺光度法测定大气中二氧化硫时所用的3种吸收剂（四氯汞钾、甲醛及三羟乙基胺）的吸收效果及方法的准确性、灵敏度等条件作了比较试验。结果表明,与另两种吸收剂相比,采用甲醛作吸收剂,吸收效果最好,测定的灵敏度,精密度和准确度也都占优,其检出限在三者中最低。用甲醛替代四氯汞钾,除了上述优点外尚可避免使用较大量的汞盐,有利于环境保护。     

室内用水性涂料及水性胶粘剂中甲醛含量测定的研究

阐述了GB18582和GB18583中对于应用乙酰丙酮分光光度法测定游离甲醛的分析方法之间的差异,主要包括乙酰丙酮试剂要求、标准曲线绘制、测定波长和样品前处理等.在详细分析区别的基础上,对标准方法进行改进,提出适合水性涂料和水性胶粘剂中游离甲醛的测定方法,该方法操作简单,具有较高的精密度和准确度.     

动力学荧光光谱法测定痕量甲醛

本文利用甲醛对溴酸钾氧化灿烂甲酚蓝的反应具有催化作用,使其荧光淬灭,在一定条件下甲醛浓度与催化体系和非催化体系的荧光强度差值成正比,建立了测定甲醛的催化动力学荧光法.并且测定湖水中甲醛回收率,结果满意.说明该方法可用于实际水样中甲醛的测定.     

动力学光度法测定甲醛

在室温及酸性条件下,甲醛对溴酸钾氧化乙基橙的反应具有显著的促进作用,量反应具有一定的诱导期。通过测量诱导建立了测定甲醛的动力学分析新方法,测定甲醛的线性范围为０．１０～１．５ｍｇ／Ｌ,检测限为０．０５ｍｇ／Ｌ。利用此法测定了废水中的甲醛,结果满意。     

单滴微萃取气相色谱质谱联用测定水发食品中的甲醛

近年来,一些不法商贩和生产厂家为追求产品的感官性状和延长保鲜时间,在食品中添加国家严令禁止使用的化工原料~([1]),甲醛即是其中一种.甲醛有极强的细胞毒性,影响人体代谢机能,具有致癌性,已被世界卫生组织确定为"三致"毒物,是食品安全研究的热点之一~([2]).目前,甲醛的检测方法主要有分光光度法、色谱法、电化学法、化学滴定法等.气相色谱法操作简便,测定线性范围宽,分离度好,干扰小.但是,由于甲醛分子太小,直接进行GC分析时,出峰太快,因此食品中甲醛的测定一般先将甲醛衍生再用GC/MS进行测定.     

一种选择性快速测定饮料中游离甲醛的示波极谱法

在pH 5.0的0.025mol·L-1HOAc-NaOAc介质中,甲醛与硫酸肼的反应产物于电位－1.04V(vs.SCE)处产生一个灵敏的还原波,其峰高(ip)与甲醛浓度在0.1～0.8mg·L-1范围内呈良好的线性关系。在此条件下,共存的数十种无机离子及有机物无影响,也不受试样中颜色及浑浊等影响,对甲醛有极高的特效性。用标准加入法直接测定炊料中微量的游离甲醛含量,分析频率为60样·h-1．其操作简便、快速、准确,是目前测定甲醛最为简便的分析方法。     

氨基酸-乙酰丙酮分光光度法测定水样中甲醛

试验了用氨基酸代替氨水或乙酸铵作为胺源的条件下,乙酰丙酮与甲醛反应生成有色化合物的适宜条件并提出了氨基酸-乙酰丙酮分光光度法测定水中甲醛的方法。优化的试验条件如下:①0.12mol·L-1甘氨酸衍生剂用量为2mL;②反应温度为50℃;③反应时间为15min;④反应体系的pH为4.7。甲醛的质量浓度在0.2~1.0mg·L-1范围内与吸光度呈线性关系,检出限为5μg·L-1。加标回收率均不小于98.0%,测定值的相对标准偏差(n=6)均不大于4%。方法应用于地表水样中甲醛的测定,测定值与国标法测定结果相符。     

Spectrophotofluorimetric determination of formaldehyde and acrolein with j-acid : Comparison with other methods

Highly sensitive spectrophotofluorimetric methods for the determination and estimation of formaldehyde and acrolein have been described. Formaldehyde and acrolein can be estimated in amounts as low as 0.0005 μg formaldehyde and 0.01 μg acrolein, Quinaldinium salts have been shown to have high sensitivity for the spectrophotometric determination of formaldehyde. The procedure in which these salts are used has a high potentiality for further improvement. Twelve different methods for the determination of formaldehyde have been compared.     

Preconcentration of trace amounts of formaldehyde from water, biological and food samples using an efficient nanosized solid phase, and its determination by a novel kinetic method

This work presents a sensitive method for the determination of formaldehyde. It is based on the use of modified alumina nanoparticles for its preconcentration, this followed by a new and simple catalytic kinetic method for its determination. Alumina nanoparticles were chemically modified by immobilization of 2,4-dinitrophenylhydrazine via sodium dodecyl sulfate as a surfactant. The formaldehyde retained on the modified adsorbent was then desorbed and determined via its catalytic effect on the oxidation of thionine by bromate ion. Factors affecting the preconcentration and determination of formaldehyde have been investigated. Formaldehyde can be detected in the range from 0.05 to 38.75 μg L^?1, and no serious interferences have been observed. The method has been successfully applied to the quantitation of formaldehyde in water, food, and certain biological samples.

二甲酚橙-溴酸钾体系催化动力学光度法测定微量甲醛

在硫酸介质中,溴酸钾在甲醛的催化作用下能氧化二甲酚橙褪色,其褪色程度与甲醛含量成正比,从而建立了光度法测定微量甲醛的新方法。方法的最大吸收波长为435 nm,在50℃水浴中反应10 min,甲醛含量在0～20μg/mL内呈线性关系。方法应用于废水中微量甲醛的测定,相对标准偏差为4.34%,回收率在91.0%～102.8%之间。     

Spectrophotometric determination of formaldehyde in air

A spectrophotometric method for the determination of formaldehyde in air is described, based on the colour reaction of formaldehyde, p-aminoazobenzene and sulphur dioxide in hydrochloric acid medium. Beer's law is obeyed at 505 nm in the range 2-12 mug of formaldehyde per 25ml of final solution (0.08-0.48 ppm). Optimum conditions for colour development, and possible interferences, have been studied.     

Formaldehyde-sensitive conductometric sensors based on commercial and recombinant formaldehyde dehydrogenase

Novel formaldehyde-sensitive conductometric biosensors have been developed that are based on commercial bacterial formaldehyde dehydrogenase (FDH) from Pseudomonas putida and recombinant formaldehyde dehydrogenase (rFDH) from the yeast Hansenula polymorpha as the bio-recognition elements. The bio-recognition membranes have mono-layer architecture and consist of enzyme cross-linked with albumin and of the cofactors NAD (for FDH-based sensor) or NAD and glutathione (for rFDH-based sensor). This architecture of the biosensor allows the determination of formaldehyde without adding NAD and glutathione to the analyzed sample at every analysis and conducting measurements on the same transducer without cofactors regeneration since the bio-membrane contains it at high concentration (100 mM for NAD and 20 mM for glutathione). The response is linear in the range from 10 to 200 mM of formaldehyde concentration depending on the enzyme used. The dependence of the biosensor output signals on pH and buffer concentration as well as operational/storage stability and selectivity/specificity of the developed conductometric biosensors have been investigated. The relative standard deviation of the intra-sensor response did not exceed 4% and 10% for rFDH- and FDH-based sensors, respectively. The relative standard deviation of the inter-sensor response constituted 20% for both dehydrogenases used. The biosensors have been validated for formaldehyde detection in some real samples of pharmaceutical (Formidron), disinfectant (Descoton forte) and an industrial product (Formalin). A good correlation does exist between the concentration values measured by the conductometric biosensor developed in this work, an enzymatic method, amperometric biosensors developed earlier, and standard analytical methods of formaldehyde determination.     

Kinetic determination of formaldehyde and hexamethylenetetramine with a cyanide-selective electrode

An automatic potentiometric reaction-rate method is described for the determination of formaldehyde and hexamethylenetetramine. The formaldehyde reacts with cyanide, and the reaction rate is followed with a cyanide-selective electrode. The time required for the reaction to consume a fixed amount of cyanide, and therefore for the potential to increase by a preselected amount (8.0 mV), is measured automatically and related directly to the formaldehyde concentration. The average error for the determination of 60–300 μg of formaldehyde in a sample volume of 1.00 ml was about 1.3%. Amounts of hexamethyl-enetetramine in the range 50–250 μg in a sample volume of 0–050 ml were determined after acid hydrolysis to formaldehyde with an average error of about 1.6%. Measurement times were in the range 18–80 s for both determinations. The method has been applied to the determination of hexamethylenetetramine in pharmaceutical preparations.     

The protonated 4,4'-diaminotriphenylmethyl cation as a reagent and cyclohexanone as an absorbant for sulphur dioxide determination

Protonated 4,4'-diaminotriphenylmethyl cation, DATM, has been investigated as a colorimetric reagent for the determination of sulphur dioxide. The bisulphite addition compound with formaldehyde alkylates a primary arylamine group in the protonated reagent to re-establish resonance, and hence produces a colour that is proportional in intensity to the concentration of either bisulphite or formaldehyde (the other being in excess). The large bathochromic spectral shift results in a negligible blank correction. Cyclohexanone in aqueous solution has been found to stabilize bisulphite solutions for up to 6 hr. The stabilization by cyclohexanone has been compared with stabilization by tetrachloromercurate(II). The Beer-Lambert law is obeyed with good precision for both sulphite and formaldehyde determination.     

甲醛电化学传感器多孔气体扩散电极不同催化层结构与响应性能研究

多孔气体扩散电极的制备是制备甲醛电化学传感器的关键所在, 其中催化层的结构直接影响到传感器的响应性能. 通过柠檬酸三钠还原法合成了纳米金-活性炭、纳米金-碳纳米管催化剂, 制备了甲醛电化学传感器多孔气体扩散电极, 并对电极进行SEM(扫描电子显微镜)物理表征. 在甲醛气体浓度为0.24和0.63 mg/m³时, 电极C具有较好的响应, 在0.1到0.84 mg/m³浓度范围内, 线性方程为y＝10.515x＋4.4049 (R²＝0.9917), 响应时间约80 s. 分析了不同催化剂的气体扩散电极结构与甲醛响应性的关系, 为研制开发性能优良的甲醛电化学传感器奠定了基础.     

Curing kinetics of amine and sodium hydroxide catalyzed phenol-formaldehyde resins

The effect of both formaldehyde content and catalyst type used in the synthesis of several resole type phenolic resins has been studied by using differential scanning calorimetry. In this study Kissinger-Akahira-Sunose (KAS), Ozawa-Flynn-Wall (OFW) and Friedman model-free kinetics are applied in order to correlate the dynamic cure behaviour with the mentioned synthesis variables. Strong upward dependency of activation energy on conversion has been detected in all cases up to a maximum value. Lower the formaldehyde content fewer changes in activation energy have been detected, revealing a more homogeneous polymerization. As formaldehyde content increases, stronger variations of energy values have been observed and the maximum value is shifted to lower conversions. By comparing triethylamine and sodium hydroxide catalysts similar behaviour has been observed, with higher energy values and shifting of the maximum in the latter. Friedman approach has been resulted in more convenient and accurate for the energy values determination and KAS method seems useful for the dynamic cure prediction of that type of thermoset.     

Specific features of the determination of carbonyl compounds in atmospheric air

It has been shown that the error of the determination of formaldehyde in atmospheric air depends both on the method of measurement of the analytical signal and on the conditions of air sampling. In most cases, the use of HPLC leads to underestimated results, while the application of spectrophotometry leads to overestimated results. A method has been developed for the selective determination of formaldehyde in atmospheric air using HPLC with a fluorescence detector, which can be used as a reference method.