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。     

茚三酮分光光度法测定水中氨氮

根据茚三酮在一定条件下可与氨发生显色反应的原理,提出了利用茚三酮测定氨氮含量的新方法,探讨了显色剂和还原剂用量、介质环境、反应温度及反应时间等条件对反应体系的影响。在优化条件下测定了氨氮的工作曲线,在实际样品测量中,与纳氏试剂分光光度法进行了比较。氨氮检测范围0.01~5 mg/L,优于纳氏试剂法,可广泛应用于检测机构的水质检测活动。     

铍试剂Ⅱ—CPB三元络合物分光光度法测定镁

建立了一种以铍试剂Ⅱ为显色剂，在氨性介质中加入表面活性剂，并加入动物胶作为稳定剂，与镁形成三元络合物，用分光光度法测定镁的方法。对测定波长、显色时间及各种组分的用量进行了考察，选择了最佳的实验条件，并进行了回收率实验。     

铍试剂Ⅱ—CPB短元络合物分光光度法测定镁

建立了一种以铍试剂Ⅱ为显色剂，在氨性介质中加入表面活性剂，并加入动物胶作为稳定剂，与镁形成三元络合物，用分光光度法测定镁的方法。对测定波长、显色时间及各种组分的用量进行了考察，选择了最佳的实验条件，并进行了回收率实验。     

紫外分光光度法测定蔗糖含量

有关蔗糖含量的测定法有很多,如旋光法、气相色谱法、液相色谱法、分光光度法等。旋光法测量准确性较差;气相色谱法和液相色谱法测量过程较复杂;文献报道的分光光度法,是在蔗糖的溶液中加入显色剂间苯二酚或2,4,6-三硝基酚,反应生成有色物质,并测其吸光度,文献报道的分光光度法,用酶水解蔗糖,加入4-氨替吡啉苯酚显色,再测吸光度。     

室内空气中甲醛检测方法研究进展

介绍室内空气中甲醛的检测方法.室内空气中甲醛含量的传统实验室检测方法包括AHMT分光光度法、乙酰丙酮分光光度法、酚试剂分光光度法和气相色谱法,现场检测方法有简便取样仪器检测方法.AHMT分光光度法灵敏度较高、选择性较好,但显色反应时间一致性对检测结果有很大影响;乙酰丙酮分光光度法所用乙酰丙酮显色剂稳定,重复性及选择性较...     

高灵敏度显色剂在分光光度法测定铅中的应用

综述了近年来国内各类高灵敏度的显色剂,包括卟啉类、变色酸双偶氮试剂、甲基百里香酚蓝等显色剂的显色原理及其在分光光度法测定铅离子中的应用(综述文献46篇)。     

怀地黄中微量铁的测定

为探讨邻二氮菲分光光度法测定怀地黄中微量元素铁含量的可行性,根据铁离子与特定显色剂显色产生可见吸收的原理,采用混合酸V(HN03)+V(HClO4)=4+1对怀地黄样品湿法消化处理,在pH2-9的溶液中试剂与铁生成稳定的橙色络合物,并用分光光度法测定了怀地黄中微量元素铁含量.结果表明,怀地黄中铁含量为552.48-56...     

分光光度法测定工业水中的酚酞碱度

建立了分光光度法测定工业及锅炉用水中酚酞碱度的分析方法。以间硝基苯酚为显色剂,采用分光光度法,测定了吸光度与酚酞碱度之间的线性关系。对测定波长、显色剂用量、显色时间等条件进行优化选择,考察了该方法的准确度和精密度。方法检出限为0.004 5 mmol/L,测定结果的相对标准偏差为0.20%～0.70%(n=9),加标回收率为97.0%～99.0%。该方法检出限低,精密度高,受样品颜色,浑浊度等的影响小,适合工业及锅炉用水酚酞碱度的测定,尤其适用于低酚酞碱度水样。     

分光光度法测定微量银

三氮烯类试剂是一类测定ⅠB、ⅡB族金属离子的高灵敏试剂,一般用于样品中Cd^2＋、Hg^2＋、Cu^2＋、Zn^2＋等金属离子的测定,但用于银（Ⅰ）的分光光度法分析报道并不多。本法研究了显色剂1-（2,6-二氯-4-硝基苯）-3-（4-硝基苯）-三氮烯（DCNPNPT）与银（Ⅰ）的显色反应。     

流动注射-分光光度法在线全自动测定正磷酸盐

通过将GB/T6913-2008分光光度法在线化,设计研制了正磷酸盐流动注射自动在线监测仪;优化了显色剂浓度、载流液浓度、采样环长度等实验参数,建立了水中正磷酸盐流动注射全自动在线分析方法,并考察了其实际使用效果.结果表明,当待测水样中PO34浓度在0～15.0 mg/L范围内时,吸光度和浓度呈良好的线性关系,检出限为...     

水杨酸钠紫外分光光度法测定烟草中的总氮

建立水杨酸钠紫外分光光度法测定烟草中总氮含量的方法。烟草样品经硫酸铜–硫酸钾–浓硫酸消化,用水杨酸钠–二氯异氰尿酸钠显色后用紫外分光光度计检测,并对波长、显色剂用量和反应时间等实验条件进行了优化。总氮的质量浓度在5~60 mg/L范围内与其吸光度呈良好的线性关系,线性相关系数为0.998 8,方法的检出限为0.14 mg/L。样品分析结果的相对标准偏差为3.22%(n=6),样品加标回收率为99.30%~101.62%。该方法具有较高的精密度和准确度,尤其适用于样品量少时对烟草中总氮的测定。     

Determination of sulfate in natural and residual waters by turbidimetric flow-injection analysis

A turbidimetric flow-injection system was developed for the determination of sulfate in natural and residual water samples, with no previous treatment, using spectrophotometric detection. The precipitating agent, 7.0% (w/v) barium chloride solution prepared in 0.10% (w/v) polyvinyl alcohol, was added by using the merging-zones approach. A 100 mg/L sulfate solution in 0.07M nitric acid was mixed with the sample before it entered the injection loop to improve the detection limit, provide in-line pH adjustment, and prevent the interference of some anionic species. The relative standard deviations of the results were between 1.4 and 3.0% and were in agreement with results obtained by the reference method. Samples within a linear concentration range of 10-120 mg SO4(2-)/L can be analyzed at a rate of 40/h. The detection limit is 5 mg SO4(2-)/L.     

离子色谱法测定“地沟油”中钠离子和氯离子的含量及其比例关系

采用离子色谱法测定“地沟油”样品中钠离子和氯离子的含量,通过计算两者的比例关系确定样品中是否含有“地沟油”。使用去离子水提取“地沟油”样品中钠离子和氯离子。氯离子以20 nmol/L KOH溶液为淋洗液,AS19分离柱(250 mm×4 mm)分离,抑制器电流112 mA;钠离子以20 nmol/L甲基磺酸(MSA)为淋洗液,CS12分离柱(250 mm×4 mm)分离,抑制器电流59 mA;两者分离采用的其他相同色谱条件为: 柱温、检测器温度30 ℃,电导检测器检测,进样量25 μL,流量1 mL/min,峰面积定量。氯离子的检出限为0.005 mg/L,在0～5 mg/L范围内有良好的线性关系（r2=0.999988）;钠离子的检出限为0.001 mg/L,在0～5 mg/L范围内有良好的线性关系（r2=0.999926）。氯离子平均加标回收率为94.2%,相对标准偏差(RSD)为2.4%;钠离子平均加标回收率为92.5%, RSD为2.7%。经测定、计算,正常食用油中钠离子和氯离子的物质的量比约为1,而“地沟油”中钠离子与氯离子的物质的量比高于4。“地沟油”中钠离子和氯离子的含量及其比例关系可作为判断“地沟油”的重要依据。     

用铁氰化钾分光光度法测定头孢噻肟钠

建立了以铁氰化钾测定头孢噻肟钠的分光光度法。 在0.20 mol/L NaOH溶液中,头孢噻肟钠(CTX)于100 ℃水浴中降解生成的巯基化合物能将Fe(Ⅲ)(pH=3.0)还原为Fe(Ⅱ),根据Fe(Ⅱ)与K3[Fe(CN)6]反应生成可溶性普鲁士蓝(KFeⅢ[FeⅡ(CN)6])的吸光度,可以间接测定头孢噻肟钠的含量。 头孢噻肟钠在0.040~24 mg/L范围内与吸光度(A)呈线性关系,线性回归方程:A=0.05088+0.2166ρ(mg/L),相关系数R=0.9986,检出限为0.01 mg/L,相对标准偏差(RSD)为1.36%(n=11),表观摩尔吸光系数ε=2.3×105 L/(mol·cm)。 此方法可用于药物及血清中头孢噻肟钠含量的测定。     

Flow injection spectrophotometric determination of copper, iron, manganese, and zinc in animal feeds using a common manifold

A rapid and simple procedure was developed for the determination of copper, iron, manganese, and zinc in animal feeds using an identical flow injection spectrophotometric manifold but different chromogenic reagents and different detection wavelengths. Bis(cyclohexanone)oxalydihydrazone, formaldoxime, 1,10-phenanthroline, and xylenol orange were adopted as chromogenic reagents for Cu, Mn, Fe, and Zn, respectively. Detection conditions such as manifold parameters, buffer pH, reagent concentration, temperature, and acidity of sample solution were optimized. Analytical characteristics of the method and interference of metal ions commonly present in feeds were studied. By changing the reagents and detection wavelengths, which can be done quickly, the proposed low cost flow injection system can determine Cu, Fe, Mn, or Zn in the range of 0.5-10 mg/L with a sampling throughput of 120/h.     

Flow injection spectrophotometric determination of anionic surfactants using methyl orange as chromogenic reagent

A flow injection(FI) spectrophotometric method for the determination of anionic surfactants was developed on the basis of the competition for the cationic surfactant cetyl pyridine (CP+) chloride between the acidic dye methyl orange (MO) and anionic surfactants. In a pH 5.0 medium the cation of cetyl pyridine (CP+) reacts with dissociated methyl orange (MO-) to form an ion-associate complex, causing a blue shift of lambda(max) from 465 nm for MO- to 358 nm for the CP+ x MO- associate. The MO- in the ion-associate complex can be quantitatively substituted by such anionic surfactants as sodium dodecyl benzene sulfonate (DBS) or sodium lauryl sulfate (LS), leading to an increase in the absorbance measured at 465 nm. This increased absorbance value is proportional to the concentration of anionic surfactants. Various chemical and physical parameters for the FI spectrophotometric method were optimized, and interference-free levels were examined. At the optimized conditions, Beer's law was obeyed in the range 1.4 approximately 25 mg/L sodium DBS for an injected sample volume of 180 microL, and a detection limit of 0.22 mg/L for sodium DBS was achieved at a sampling rate of 90 h(-1). Eleven determinations of a 16 mg/L sodium DBS solution gave a RSD of 0.4%. The proposed method has successfully been applied to the determination of anionic surfactant concentration in waste water and in detergents.     

Determination of ammonia in beers by pervaporation flow injection analysis and spectrophotometric detection

A pervaporation flow injection (PFI) method is described for the determination of ammonia in beers. After injecting the sample into a NaOH donor solution, ammonia and other volatiles are transferred in the pervaporation unit from the donor stream to an acceptor stream containing sodium salicylate and nitroprusside, which subsequently mixes with alkaline sodium dichloroisocyanurate to allow the classical Berthelot reaction to take place. The blue-coloured complex formed is monitored spectrophotometrically at 655 nm. A linear calibration curve with a range of 0.1–40 mg l⁻¹ was obtained. The method has a detection limit of 0.05 mg l⁻¹ and is capable of a sampling frequency of 11 h⁻¹ at 4 mg l⁻¹ ammonia. It was applied successfully to the determination of ammonia in synthetic samples and unfiltered lager beers. The advantages of the present method over the ammonia ion-selective electrode method and the PFI system based on mixed indicator detection are discussed.     

离子色谱法检测食品添加剂焦碳酸二甲酯中的氯离子

建立离子色谱法检测食品添加剂焦碳酸二甲酯（DMDC）中的杂质氯离子的方法。样品用水溶解超声定容后,采用SH-AC-1阴离子交换柱（250mm×4．6mm,5μm）分离,抑制电导法检测。考察了淋洗液种类、浓度对氯离子与干扰离子分离度的影响。最佳色谱条件：以0．005mol／L的四硼酸钠水溶液为淋洗液,流速1．0mL／min。在此条件下,样品中的氯离子可以和其它干扰离子分离,而且分离度达3．0以上,峰形对称。在氯离子浓度为0．1～5．0mg／L的范围内,可获得良好的线性关系,线性相关系数大于0．999;氯离子检出限（S／N=3）达0．007mg／L,加标回收率为97．5％～98．9％。该方法可以用于食品添加剂DMDC中氯离子的测定。     

流动注射催化动力学光度法测定碘离子

Based on catalysis of I- on the decolor reaction between potassium bromate and indigo carmine in the acid medium,and combined with flow injection analysis,a new flow-injection catalytic kinetic spectrophotometric method was found for determination of iodide in sample.The experimental results show that the determination is carried out at temperature of 80℃ and the concentration of H_2SO_4,KBrO_3,and indigo carmine is 1.2 mol/L,1.8×10~(-2) mol/L and 1.0×10~(-4) mol/L respectively,the linear range for the method is 0.50～1.8 mg/L.The detection limit is 0.0022 mg/L.The relative standard deviation is 1.92%.The proposed method was applied to the determination of iodide in troche successfully.The recovery was between 99.2% and 103.6%.