副玫瑰苯胺无汞比色法测定室内空气中的甲醛

本文在甲醛法测定空气中二氧化硫的基础上,建立了一种测定空气中甲醛的新方法。本法用亚硫酸盐缓冲溶液配制标准溶液和样品吸收液,使甲醛生成稳定的羟甲磺酸,再用氢氧化钠分解羟甲磺酸释放出甲醛,以副玫瑰苯胺和亚硫酸钠为显色剂进行定量分析。当采集空气30 L时,检出限为0.01 mg/m3,可测浓度范围0.03~0.60mg/m3。本法适用于环境及室内空气中甲醛的测定。     

非色散原子荧光光度法测定大米中微量砷

本法是一种测定大米中微量砷的新方法。试样经硝酸-硫酸-高氯酸分解后,在盐酸介质中,用硼氢化钾将试样中各种价态的砷还原为砷化氢,用硫脲-抗坏血酸消除铜、镍、铁等元素的干扰,然后在国产的原子荧光光度计上测定砷的含量。本法能简便、快速地测定采样中10ppb到100ppm的砷,回收率在94～105%之间。     

TBP萃淋树酯反相色层分离ICP—AEP法测定岩石中的微量金

本文介绍采用TBP萃淋树酯萃取分离结合仪器分析测定岩石中微量金的方法。方法包括三部分:样品分解、分离富集、及用ICPQ—100光量计测定。本法样品称量一般为10—20g,用王水分解,经过抽滤,将滤液体积控制在150ml左右,使酸度保持为5—10%。通过萃淋树酯交换柱分离富集,并除去可能产生干扰谱线的元素。测出金的下限为0.10克/吨,经与金的管理样结果对照,本法的准确度与检出限能满足地质勘探样品金测定的要求。     

铬天青S光度法测定锌铝合金中铝

本文用盐酸及过氧化氢分解试样,在 pH5.5～5.8乙酸-乙酸钠缓冲溶液中,使铝与铬天青 S 形成紫红色络合物,进行光度测定。Fe~(3+)的干扰以抗坏血酸还原,基体锌的干扰可在标准中加入试样等量的锌加以克服,其它杂质元素不干扰测定。本法具有快速、准确的优点。主要试剂:乙酸-乙酸钠缓冲液:每升溶液中含300克无水乙酸钠和50毫升冰乙酸;锌溶液:称取     

钨砂中亚铁的快速测定

因钨砂中含有高价锰对亚铁的测定有严重干扰,至令尚未有一个比较可靠的分析方法。为此,本法在带严密保护装置的条件下,用少量氟化铵、碳酸氢钠和盐酸分解试样进行了试验。结果表明,将含亚铁9.10%的铁矿标样制成氧化锰含量为10—14%的钨砂模拟样进行分析,锰无干扰;用含氧化锰14%的钨精     

锌合金中钛的测定——变色酸比色法

试样以盐酸-硝酸的混合酸分解,在 pH2.5～3的乙酸介质中,变色酸与四价钛离子生成红褐色络合物,以此进行比色测定。用抗坏血酸消除三价铁的干扰,锌合金中的共存元素 Zn、Cu、Mg、Al 及 Mn 等均不干扰测定。本法适用于含钛0.10～1.20%的锌合金试样分析,也可用于铝合金中钛的测定。方法简易快速、准确。试剂变色酸:称取1.2克变色酸和1.2克亚硫酸钠溶于少量水中,以水稀释至100毫升,若浑浊,     

含铌钽钢中硼的比色测定

用次甲基蓝比色测定某些含铌钽钢中微量硼时,常常遇到如下困难:铌钽的严重干扰;王水分解试样时氯化硼的挥发损失;某些硼化物如碳化硼、氮化硼以及铌钽的金属间硼化物等不易被王水和硫酸所分解等。为了解决这些问题,本文研究了用焦硫酸钾熔融试样,以水解方式分离铌钽,方法简单,效果较好,避免了卤化硼的挥发损失,并解决了难溶硼化物的溶样问题。本法适用于含铌钽的镍基、铁基和部分钴基合金中微量硼的测定。     

甲醛-三氯乙酸沉淀-凯氏定氮法测定牛奶中真蛋白质

提出了一种有效去除三聚氰胺等非蛋白氮干扰的凯氏定氮法测定牛奶中真蛋白质的含量的方法。在5mL样品中加入甲醛3 mL,漩涡混匀1 min,于70℃水浴加热10 min后,加入150g·L-1三氯乙酸溶液5mL沉淀蛋白质,抽滤分离后,应用自动凯氏定氮仪测定沉淀中的蛋白质含量。经配对t检验分析,本法与国家标准方法测定牛血清白蛋白标准溶液中蛋白质含量、与考马斯亮蓝G-250法测定牛奶中真蛋白质含量以及干扰试验中各干扰物添加组与对照组中蛋白质含量的测定结果均无显著性差异。被分离的滤液中干扰物的回收率在98.4%~100%之间。     

催化动力学荧光分析法测定啤酒中的痕量甲醛

在稀硫酸溶液中,甲醛催化溴酸钾氧化吖啶红的反应并使其发生荧光猝灭。据此,建立了新的测定痕量甲醛的催化荧光动力学分析法。方法检出限为0.002 mg/L,线性范围为0.004~0.16 mg/L。本法简便、快速,用于啤酒中痕量甲醛的测定,分析结果满意。     

甲醛掩蔽铵离子电极法测定天然水和生物样品中钾

天然水和生物样品中的钾,用4,4′-二叔丁基二苯并30-王冠-10为活性物质的 PVC 膜钾电极测定时,除 Rb~+,Cs~+外,NH_4~+的干扰是主要的。本法用甲醛掩蔽 NH~+_4,省去除铵步骤,使测钾灵敏度和准确性均有所提高     

水发食品中甲醛现场测定的样品快速前处理新方法研究

提出了一种用于现场测定水发食品中甲醛含量的样品快速前处理新方法,采用乙酸锌和亚铁氰化钾沉淀样品中的蛋白质和脂肪,在弱酸性介质和沸水浴条件下提取了样品中的甲醛,并与乙酰丙酮立即发生显色反应.研究了不同样品前处理方法对甲醛提取和测定的影响,探讨了水发食品中的甲醛本底值及其是否被人为添加甲醛的判断标准.此方法的特点是样品前处理与显色反应同时进行,在10min内即可完成对水发食品中甲醛含量的定量测定.     

Level of endogenous formaldehyde in maple syrup as determined by spectrofluorimetry

The level of endogenous formaldehyde in maple syrup was established from a large number (n = 300) of authentic maple syrup samples collected during 2000 and 2001 in the province of Quebec, Canada. The average level of formaldehyde from these authentic samples was measured at 0.18 mg/kg in 2000 and 0.28 mg/kg in 2001, which is lower than previously published. These average values can be attributed to the improved spectrofluorimetric method used for the determination. However, the formaldehyde values obtained demonstrate a relatively large distribution with maximums observed at 1.04 and 1.54 mg/kg. These values are still under the maximum tolerance level of 2.0 mg/kg paraformaldehyde pesticide residue. Extensive heat treatment of maple syrup samples greatly enhanced the formaldehyde concentration of the samples, suggesting that extensive heat degradation of the sap constituents during evaporation could be responsible for the highest formaldehyde values in maple syrup.     

基于银纳米粒子的生成测定痕量甲醛

在碱性溶液中甲醛能还原Ag~+得到黄色银纳米粒子,使体系的共振光散射(RLS)强度增强,从而建立起测量环境中痕量甲醛的RLS新方法. 结果表明,新建方法测定甲醛的浓度线性范围为1.0×10~(-6)～2.0×10~(-5) mol/L,检出限为1.0×10~(-7) mol/L,样品加标测定的回收率为96.26%～103.32%. 并且不同浓度的甲醛还原Ag~+得到黄色银纳米粒子的颜色明显不同,基于此建立了一种可视化半定量测定痕量甲醛的新方法,此方法简便快速、灵敏度高. 用于环境水样、室内空气中甲醛的测定,结果满意.     

Differential-pulse voltammetric determination of trace formaldehyde using magnetic microspheres and magnetic electrode

A new type of magnetic polymer microsphere containing acylhydrazine groups on the surface was synthesized. They can be reacted with formaldehyde to produce an electroactive adduct. Reduction of these derivatives following aggregation on a magnetic electrode is possible and is effective in the indirect determination of formaldehyde. The experimental conditions and electrode structure are discussed. Under the optimum conditions, it was found that the peak potential (Ep) of formaldehyde is -1.01 V (vs. Ag/AgCl). Formaldehyde in the range 1-1000 micrograms l-1 can be determined. The detection limit for formaldehyde is 0.3 microgram l-1 and the relative standard deviation for the determination of 100 micrograms l-1 formaldehyde was 2.26%. The method was applied to the determination of formaldehyde in environmental samples with satisfactory results.     

Preconcentration with membrane cell and adsorptive polarographic determination of formaldehyde in air

The present paper describes a procedure that formaldehyde in air was preconcentrated in a membrane cell and its content was determined by adsorptive polarography. First the formaldehyde in air samples was preconcentrated in a membrane cell using water, then the formaldehyde reacted with 2,4-dinitrophenyl hydrazine to form 2,4-dinitrophenyl hydrazone, which can be adsorbed at the mercury electrode and yields a sensitive adsorptive polarographic wave. Over the range 6.0x10(-10)-5.0x10(-6) M, the peak currents are linearly proportional to the concentration of formaldehyde, the detection limit is 2.0x10(-10) M.     

Sensitive reaction rate method for the determination of low levels of formaldehyde with photometric detection

A simple and rapid method is proposed for the determination of ultra trace amounts of formaldehyde. It is based on the catalytic effect of formaldehyde on the oxidation of Brilliant cresyl blue by bromate. The reaction is monitored photometrically by measuring the decrease in absorbance of the dye. Formaldehyde in the range of 0.005–2.300 μg/mL can be determined with a limit of detection of 0.003 μg/mL. The relative standard deviation for ten replicate measurements of 1.5 μg/mL formaldehyde is 0.1%. The method was used for the determination of formaldehyde in real samples with satisfactory results.     

不同介质中甲醛在Aucore@Ptshell/Pt电极上氧化的原位SERS研究

应用化学还原法合成了Au_core@Pt_shell纳米粒子, 并用扫描电子显微镜(SEM)和能量色散光谱(EDS)对其进行了表征; 采用电化学原位表面增强拉曼散射(SERS)光谱技术研究了不同介质中甲醛在Au_core@Pt_shell/Pt电极上的电催化氧化行为, 获得了不同介质中甲醛在Au_core@Pt_shell/Pt电极上电催化氧化行为的原位SERS谱. 研究结果表明, 不论在酸性、中性还是碱性介质中, 甲醛均能在Au_core@Pt_shell/Pt电极上自发氧化解离出强吸附中间体CO, 只是在碱性介质中桥式吸附CO的比例明显增大, 且桥式吸附比线形吸附CO更易被氧化, 使CO在碱性介质中基本氧化完毕的电位比在中性及酸性介质中提前了约950 mV. 分子水平的研究结果表明, CO和甲醛在碱性介质中比在中性和酸性介质中更易被氧化.     

Catalytic-kinetic determination of trace amount of formaldehyde by the spectrophotometric method with a bromate-Janus green system

A new simple and rapid catalytic kinetic method for the determination of trace amount of formaldehyde is described. The method is based on the catalytic effect of formaldehyde on the oxidation of Janus green by bromate in the present of sulfuric acid. The reaction monitored spectrophotometrically by measuring the decrease in absorbance of the reaction mixture at 618 nm. The fixed-time method was used for the first 150 s. For initiation of the reaction, under the optimum conditions, in the concentration range of 0.003-2.5 microg ml(-1) formaldehyde can be determined with a limit of detection 0.0015 microg ml(-1). The relative standard deviation of five replicate measurements is 2.3% for 1.0 microg ml(-1) of formaldehyde. The method was used for the determination of formaldehyde in real samples with satisfactory results.     

Determination of naturally occurring formaldehyde levels in sap and wood tissue of maple trees using gas chromatgraphy/mass spectrometry

The occurrence of formaldehyde in sap and wood tissue of treated and untreated maple sugar trees was investigated using GC/MS. Samples were collected at different periods of the 2009 season and at different locations in Quebec, Canada. The natural concentration of formaldehyde found in untreated samples varied according to periods and locations and ranged from below the LOQ to 1.82 mg/kg for sap samples and from 2.39 to 8.92 mg/kg of fresh tissue for wood samples. Late season samples tended to have higher concentrations of formaldehyde. Samples of sap and wood tissue from tapholes treated with solutions of formaldehyde showed increased concentrations of formaldehyde for many days after treatment and were clearly distinct from untreated samples. These results will be useful to elaborate new inspection procedures for sugarbushes to control the illegal use of formaldehyde.     

Sensitive fluorimetric determination of formaldehyde by the co-quenching effect of formaldehyde and sulfite on the fluorescence of tetra-substituted amino aluminium phthalocyanine

A novel and sensitive fluorimetric method was developed for the determination of formaldehyde based on the co-quenching effect of formaldehyde and sulfite on the fluorescence of tetra-substituted amino aluminium phthalocyanine. Formaldehyde in the concentration range 0.040-1.19 micrograms ml-1 can be determined with a limit of detection of 7.5 ng ml-1. The relative standard deviation for nine replicate measurements of 80.0 ng ml-1 formaldehyde is 1.8%. The method was applied to the analysis of real samples with satisfactory results.