Determination of Trace Nitrite Amounts in Soil by Developed Cloud Point Extraction-Spectrophotometry Method

H. Al-Lami, A. A. Abdulwahid, Yossra A. Marich, Hasanain Abdulkareem
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Abstract

A new and simple method for the selective and sensitive determination of trace amounts of nitrite in soil samples is developed by a combination of cloud point extraction (CPE) and spectrophotometry technique. The procedure is based on the Griess reaction on 3,3`-dimethyl benzidine with nitrite in the presence of 1-naphthol in acidic media to form a yellow diazo dye, which shows absorption at lambda max 455nm. The formation of colored diazo dye is followed by extraction into the Triton X-114rich phase. Cloud point extraction method parameters such as surfactant amount, temperature, and incubation time are evaluated and optimized. The results obtained showed a very good linear range of 10-1250 μgL, with good regression coefficients (R) ≥ 0.9997 and a preconcentration factor of 12.5. The limit of detection (LOD) describes as 3SDblank/m, and the quantification limit (LOQ) describes as 10SDblank/m, where m is the slope of the calibration curve and they are equal to 7.50 and 22.71 μgL respectively. The recommended method can apply to determine the ultra-trace amount of nitrite in soil samples.
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发展浊点萃取-分光光度法测定土壤中痕量亚硝酸盐
建立了一种简便、灵敏、选择性测定土壤样品中痕量亚硝酸盐的云点萃取与分光光度法相结合的新方法。在酸性介质中,在1-萘酚的存在下,3,3 ' -二甲基联苯胺与亚硝酸盐发生Griess反应,生成黄色重氮染料,该染料在λ max为455nm处有吸收。彩色重氮染料的形成随后被萃取到Triton x -114富相。对表面活性剂用量、温度、培养时间等浊点提取工艺参数进行了评价和优化。结果表明:在10 ~ 1250 μgL范围内线性良好,回归系数(R)≥0.9997,预富集系数为12.5。检出限(LOD)为3SDblank/m,定量限(LOQ)为10SDblank/m,其中m为校准曲线斜率,分别为7.50和22.71 μgL。该方法可用于土壤样品中亚硝酸盐的超痕量测定。
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