流动注射化学发光法测定茶叶和蔬菜中亚硝酸根

利用亚硝酸根对鲁米诺-溴酸钾体系的化学发光具有显著增强作用,结合流动注射技术,建立了一种简单、快速测定亚硝酸根方法。方法的线性范围为4.0×10-3~4.0 mg.L-1;检出限为2.0×10-3mg.L-1(3σ);分别对0.01 mg.L-1和0.40 mg.L-1的亚硝酸根进行了平行测定(n=11),其相对标准偏差分别为1.3%与1.5%。应用于茶叶、蔬菜中的亚硝酸根的测定,回收率为92.3%~108.0%。     

痕量亚硝酸根的光度测定——基于亚硝酸根对溴酸钾氧化甲酚红的催化作用

研究了在稀硫酸介质中,亚硝酸根催化溴酸钾氧化甲酚红褪色反应的适宜条件和影响因素,建立了测定痕量亚硝酸根的方法.方法的线性范围为8.0～140 μg·L-1,检出限为0.98 μg·L-1,方法用于水样中亚硝酸根的测定,RSD为1.9%～3.1%.     

动力学催化光度法测定痕量亚硝酸根

基于硫酸介质中亚硝酸根催化溴酸钾氧化间甲酚紫的褪色反应,建立了测定痕量亚硝酸根的新方法,并探讨了动力学条件,测定了反应的表观速率常数(k′=1.03×10-4s-1)和表观活化能(E′a=10.25kJ.mol-1)。方法的测定范围为8.0~150μg.L-1,检出限为0.9μg.L-1。方法已用于水样中亚硝酸根的测定。     

吖啶橙催化荧光光度法测定痕量亚硝酸根

在盐酸介质中,亚硝酸根催化溴酸钾氧化吖啶橙,使得吖啶橙在激发波长为492 nm,发射波长为538 nm处的荧光强度明显下降,从而建立了催化荧光光度法测定痕量亚硝酸根的方法,线性范围为2.0×10-6~60×10-6g.L-1,检出限为1.62×10-6g.L-1。相对标准偏差小于5%,回收率在96%~105%之间。方法用于水中痕量亚硝酸根的测定。     

荧光分光光度法测定痕量亚硝酸根——基于对劳氏紫的荧光猝灭作用

在盐酸介质中亚硝酸根能与劳氏紫发生重氮化偶联反应,基于劳氏紫的荧光强度随亚硝酸根的加入量增加而明显降低的现象,建立了荧光猝灭一荧光分光光度法测定痕量亚硝酸根的方法,线性范围为0.04～0.40 mg·L-1,用于泡菜样品中痕量亚硝酸根的测定,测得回收率在96%～104%之间.     

甲基橙褪色光度法快速测定食品中亚硝酸根含量

基于在室温下HOAc介质中亚硝酸能使甲基橙褪色的原理,建立了测定亚硝酸根的快速褪色光度方法。通过正交试验优化了方法的测定条件,在最佳条件下,方法的表观摩尔吸光系数分别为4ε16=1.1×104L.mol-1.cm-1,5ε06=5.2×104L.mol-1.cm-1;线性范围及回归方程分别为5.0~600.0 mg.L-1、ΔA416=0.000 344 6c+0.002 23、r=0.999 6(416 nm);1.0~300.0 mg.L-1、ΔA506=0.000 147c+0.021 02、r=0.985 3(506 nm);检出限为5.0 mg.L-1(416 nm)1、.0 mg.L-1(506 nm)。用于食物中亚硝酸根的测定,RSD为0.2%~4.2%,加标回收率在98%~103%。经t检验,其测定结果与国标GB/T 5009.33-1996方法的测定结果一致。     

反相流动注射催化光度法测定亚硝酸根

采用反相流动注射技术与催化光度法相结合 ,研究了亚硝酸根在盐酸介质中催化溴酸钾氧化维多利亚蓝的灵敏褪色反应 ,用自制的微机化流动注射分析仪能准确控制时间 ,优化了试验条件 ,建立了测定痕量亚硝酸根的反相流动注射催化光度新方法。分析速度 36次·h- 1,克服了催化反应时间难以控制引起的方法精密度 ,准确度不高的弱点。亚硝酸根在 0 .0 0～ 2 .0 0mg·L- 1范围内 ,回归方程斜率为 0 .2 6 2。方法直接测定水中的亚硝酸根获得满意结果     

微波消解试样-催化动力学光度法测定腌菜中亚硝酸根

腌菜试样用稀磷酸及过氧化氢置于PTFE罐中,在微波炉先后在400 W及500 W消解2 min及4 min,所得试样溶液于100 mL容量瓶中定容供光度测定.在稀磷酸介质中偶氮胂Ⅰ溶液与溴酸钾溶液的氧化褪色反应因亚硝酸根的存在而催化加速.有及没有亚硝酸根存在的两份相同试液的吸光度A及A0之差△A与亚硝酸根质量浓度在50 μg·L-1以内呈线性关系,其检出限为0.82 μg·L-1用此方法分析3件腌菜试样,测定结果的相对标准偏差(n=6)均小于2%.以此样品为基体,加入亚硝酸根标准溶液进行回收试验,测得的回收率在98.0%～102.0%之间.     

催化溴酸钾氧化1-(2-吡啶偶氮)-2-萘酚动力学光度法测定痕量亚硝酸根

研究了在磷酸介质中,亚硝酸根对溴酸钾氧化1-(2-吡啶偶氮)-2-萘酚(PAN)的催化作用的反应条件,建立了测定亚硝酸根的动力学光度法。试验结果线性范围为0.2~8.0μg/25 mL,检出限为5.7μg.L-1,用于样品中亚硝酸根的测定,测定结果的RSD小于2.5%,回收率在101%~104%之间。     

催化溴酸钾氧化萘酚绿B褪色紫外光度法测定亚硝酸根

亚硝酸根广泛存在于环境、水体、食品中,它可与胺类及酰胺类化合物反应生成致癌物质亚硝胺,因此,痕量亚硝酸根的测定方法研究一直受到重视。目前国内外主要利用偶氮染料的分光光度法。催化动力学光度法[1]测定亚硝酸根等也有报道[2~6],而紫外催化光度法测定亚硝酸根的报道不多。在稀磷酸介质中,溴酸钾氧化萘酚绿B,亚硝酸根对此氧化还原反应具有灵敏催化作用。据此建立了测定硝酸根的催化紫外光度方法。方法灵敏度为1.58×10-6g·L-1,线性范围为0.1~2.0μg/25 mL。1试验部分1.1主要仪器与试剂UV-265型紫外光度计亚硝酸根标准溶液:1.0 g·L…     

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%.     

催化荧光光度法测定血红蛋白

基于血红蛋白(Hb)对过氧化氢氧化靛蓝胭脂红体系的催化作用,建立了模拟酶催化荧光光度法测定血红蛋白的新方法并对催化氧化反应的机理进行了初步探讨。实验发现体系的荧光强度与血红蛋白浓度在6.20×10-11~7.75×10-8mol/L范围内线性关系良好,方法的检出限为1.67×10-11mol/L。方法用于人血中血红蛋白含量的测定,回收率为98.8%~103.2%。     

表面活性剂增敏催化光度法测定痕量亚硝酸根

基于稀磷酸介质中,溴化十六烷基吡啶对亚硝酸根催化溴酸钾氧化吡罗红B褪色反应的增敏作用,建立了测定亚硝酸根的表面活性剂增敏催化动力学光度法。加入溴化十六烷基吡啶,灵敏度增大2.2倍。测量亚硝酸根的线性范围为0.005-0.15 mg/L,检出限为0.004/L。用于水及蔬菜中痕量亚硝酸根的测定,结果满意。     

亚硝酸根在纳米金修饰玻碳电极上的电催化氧化行为及其测定

采用直接电化学沉积法制备出纳米金修饰玻碳电极,研究了其对亚硝酸根的电催化氧化作用。结果表明,亚硝酸根在该修饰电极上于0.8 V处出现了一个良好的氧化峰。在最优实验条件下,亚硝酸根的峰电流与其浓度在2×10-6～2×10-3mol/L范围内呈一定的线性关系,检出限为6.0×10-7(S/N=3),提出了用循环伏安法测定亚硝酸根的方法。纳米金修饰电极用于东莞自来水水样中亚硝酸根的测定,回收率在98.1%～101.4%之间。对比本方法,用分光光度法对东莞自来水样中亚硝酸根进行了测定,结果满意。     

流动注射催化光度法测定痕量亚硝酸根

采用流动注射技术与催化光度法相结合,研究了亚硝酸根催化溴酸钾氧化维多利亚绿G的高灵敏度褪色反应,用自制的微机化流动注射分析仪能准确控制时间,优化了实验条件,建立了测定痕量亚硝酸根的流动注射催化光度方法。分析速度每小时80次,克服了催化反应时间难以控制引起的方法精密度,准确不谪的弱点。亚硝酸根在0.0-0.3mg/L范围内,回归方程斜率为0.708;亚硝酸根在0.3-2.0mg/L范围内,回归方程斜率为0.339,方法用于直接测定水中的亚硝酸根获得满意结果。     

A fluorescence quenching method for the determination of nitrite with Rhodamine 110

A simple and sensitive fluorescence quenching method for the determination of trace nitrite has been developed. The method is based on the reaction of Rhodamine 110 with nitrite in acidic medium to form a new compound, which has much lower fluorescence. The optimum experimental conditions were studied. The linear range was obtained at a nitrite concentration of 1.0 x 10(-8)-3.0 x 10(-7)mol l(-1) with a detection limit of 7.0 x 10(-10) mol l(-1) (S/N=3). The proposed method has been successfully applied to the determination of nitrite in tap water and lake water without extraction.     

A simple simultaneous flow injection method based on phosphomolybdenum chemistry for nitrate and nitrite determinations in water and fish samples

A direct spectrophotometric flow injection method for the simultaneous determination of nitrite and nitrate has been developed. The method is based on the oxidation of a phosphomolybdenum blue complex by the addition of nitrite and the decrease in absorbance of the blue complex is monitored at 820 nm. The injected sample is split into two segments. One of the streams was directly reacted with the above reagent and detected as nitrite. The other stream was passed through a copperised cadmium reductor column where reduction of nitrate to nitrite occurs, and the sample was then mixed with the reagent and passed through the cell of the spectrophotometer to be detected as nitrite plus nitrate. The conditions for the flow injection manifold parameters were optimised by experimental design and the concentration of nitrite and nitrate was determined in the linear range from 0.05 to 1.15 mug ml(-1) nitrite and 0.06 to 1.6 mug ml(-1) nitrate with a detection limit of 0.01 mug ml(-1) for nitrite and 0.025 mug ml(-1) for nitrate. The method is suitable for the simultaneous determination of nitrite and nitrate in fish and water samples with a sampling rate of 25+/-2 sample per hour.     

多壁碳纳米管负载铁氰化铜-铁修饰电极的制备及对亚硝酸根的测定

采用循环伏安法制备了多壁碳纳米管负载铁氰化铜-铁修饰复合陶瓷碳电极(CuFeHCF/MWCNT/CCE),研究了该修饰电极的电化学性质及对NO-2的电催化活性。 结果表明,该修饰电极对NO-2的电氧化具有强的催化活性,安培法检测NO-2的线性范围为2.0×10-7~1.4×10-3 mol/L,灵敏度为104.1 μA/(mmol·L-1),检出限（3sb）为5.0×10-8 mol/L。 利用该方法测定了土壤中NO-2的含量,结果令人满意。     

A kinetic method for the determination of nitrite by its catalytic effect on the oxidation of chlorpromazine with nitric acid.

A catalytic spectrophotometric method for the determination of trace amounts of nitrite is proposed. In acidic solution, chlorpromazine (CP) is oxidized by nitric acid to form a red compound, which is further oxidized to a colorless compound. The reaction is accelerated by trace amounts of nitrite and can be followed by measuring the absorbance at 525 nm: nitrite ion is regenerated and multiplied by nitric acid. The absorbance of the reaction increased with an increase in the reaction time, reached a maximum and decreased rapidly. Since the time required for the absorbance to reach the maximum decreased with increasing nitrite concentration, this value was used as the measured parameter for the nitrite determination. Under the optimum experimental conditions (2.3 M nitric acid, 1.2 x 10(-5) M CP, 40 degrees C), nitrite can be determined in the range 0-100 microg l(-1). The relative standard deviations (n = 6) are 4.7 and 1.8% for 40 and 100 microg l(-1) nitrite, respectively. The detection limit of this method (3sigma) is 1.2 microg l(-1). This method was successfully applied to a determination of nitrite in natural water samples.     

Flow-injection analysis-spectrophotometric determination of nitrite and nitrate in water samples by reaction with proflavin

A flow-injection manifold is proposed for determination of nitrite based on the reaction with 3,6-diamino acridine (proflavin sulfate) in hydrochloride acid medium. The assembly is adapted for nitrate determination by including a reductive column filled with copperized cadmium. The influence of foreign substances is also studied. The method gives a linear calibration graph over the range 0.06-4 mg 1(-1) nitrite, with an RSD <0.5%. The method was applied to nitrite and nitrate determinations in either waste water or coastal marine water samples.