石墨炉原子吸收分光光度法测定土壤中铍的不确定度评定研究

根据石墨炉原子吸收分光光度法(GFAAS)测定土壤中铍的过程,建立相应的数学模型并对模型中各个参数进行了不确定度来源分析.依据测量不确定度的评定理论,对样品称量、定容体积、标准溶液的配制、曲线拟合、仪器测量重复性、干物质含量等影响不确定度的分量进行计算,给出了合成标准不确定度和扩展不确定度,结果表明,测定结果的不确定性主要来源于标准拟合引入的不确定度,其次为仪器重复测定引入的不确定度,该评定方法为石墨炉原子吸收分光光度法测定土壤中重金属元素的不确定度评定提供参考依据.     

亚甲基蓝分光光度法测定硫化物校准曲线斜率、截距参考值研究

通过近三年实验室采用亚甲基蓝分光光度法测定硫化物校准曲线制作的一系列原始数据的收集,并通过数理统计方法对校准曲线、-余标准偏差、斜率扩展不确定度、截距扩展不确定度开展了详细讨论,得出亚甲基蓝分光光度法测定硫化物校准曲线斜率(b)参考范围为:0.019 1±0.00044,截距(a)参考值范围:0.003 3±0.005 0.此结果对实验室分析人员判定硫化物项目校准曲线制作是否合格具有一定的参考价值.     

地表水中镍的石墨炉－原子吸收分光光度法的优化研究

本研究对地表水中镍的石墨炉原子吸收分光光度法进行了优化。通过对该方法的试样酸度、不同基体改进剂添加效果、狭缝宽度及主要升温程序等因素的探讨和摸索,确定了最佳的实验条件。在以0.2％硝酸为定容介质、狭缝宽度为0.2 nm、灰化温度1200℃保持5 s、原子化温度2300℃保持5 s的条件下测定方法检出限、精密度及加标回收率。结果表明,方法检出限为0.95μg／L,精密度为1.87％～3.01％,加标回收率介于87.4％～102.9％,优化后的方法检出限低,精密度与准确度良好,适于清洁地表水中镍的测定。     

Novel extractive colorimetric and UV spectrophotometric estimation of etizolam in bulk and tablet by forming ion association complex with methyl orange and bromocresol green

A novel, sensitive, and rapid UV spectrophotometric and colorimetric method was developed for estimation of etizolam (ETZ) in bulk and tablet. The UV spectrophotometric method (method I) is based on quantitative estimation of ETZ using 0.1N NaOH as the solvent which exhibits maximal absorption at 378 nm. Colorimetric methods (method II and III) were based on the formation of color complex in association with ions between basic nitrogen of the drug with methyl orange (MO) and bromocresol green (BCG) in acidic medium. The formed color complexes were quantitatively extracted with chloroform and measured at 509 nm for Drug–MO complex and at 442 nm for Drug–BCG complex, respectively. Beer's law was obeyed over the linear ranges 2–16 µg/ml (method I), 5–45 µg/ml (method II), and 2–20 µg/ml (method III). The correlation coefficient (r²) for ETZ was 0.999, 0.997, and 0.998 for method I, II, and III, respectively. All methods were successfully applied for the assay of the drug in tablet. The % purity was found to be 98.52 (method I), 98.72 (method II), and 99.18 (method III). These developed methods were fully validated with % relative standard deviation (RSD) for accuracy less than 2 for all methods. The % RSD of the intra-day and inter-day variations was found to be less than 2%. The limit of detection and quantitation were as follows: 0.108 µg/ml and 0.327 µg/ml (method I), 0.24 µg/ml and 0.75 µg/ml (method II), 0.1 µg/ml and 0.5 µg/ml (method III) indicating marked method sensitivity. Empirical evidence from all three methods concludes that developed methods are simple, sensitive, and reliably validated for useful routine quality control analysis of ETZ.     

Ultraviolet light-emitting diodes in water disinfection

Background, aim, and scope  The novel system of ultraviolet light-emitting diodes (UV LEDs) was studied in water disinfection. Conventional UV lamps, like mercury vapor lamp, consume much energy and are considered to be problem waste after use. UV LEDs are energy efficient and free of toxicants. This study showed the suitability of LEDs in disinfection and provided information of the effect of two emitted wavelengths and different test mediums to Escherichia coli destruction. Materials and methods  Common laboratory strain of E. coli (K12) was used and the effects of two emitted wavelengths (269 and 276 nm) were investigated with two photolytic batch reactors both including ten LEDs. The effects of test medium were examined with ultrapure water, nutrient and water, and nutrient and water with humic acids. Results  Efficiency of reactors was almost the same even though the one emitting higher wavelength had doubled optical power compared to the other. Therefore, the effect of wavelength was evident and the radiation emitted at 269 nm was more powerful. Also, the impact of background was studied and noticed to have only slight deteriorating effect. In the 5-min experiment, the bacterial reduction of three to four log colony-forming units (CFU) per cubic centimeter was achieved, in all cases. Discussion  When turbidity of the test medium was greater, part of the UV radiation was spent on the absorption and reactions with extra substances on liquid. Humic acids can also coat the bacteria reducing the sensitivity of the cells to UV light. The lower wavelength was distinctly more efficient when the optical power is considered, even though the difference of wavelengths was small. The reason presumably is the greater absorption of DNA causing more efficient bacterial breakage. Conclusions  UV LEDs were efficient in E. coli destruction, even if LEDs were considered to have rather low optical power. The effect of wavelengths was noticeable but the test medium did not have much impact. Recommendations and perspectives  This study found UV LEDs to be an optimal method for bacterial disinfection. The emitted wavelength was found to be an essential factor when using LEDs; thus, care should be taken in selecting the proper LED for maximum disinfection.     

工业总排放水中Cr~(6+)含量测量不确定度的评定

采用分光光度法对工业总排放水中Cr6+进行不确定度评定,充分考虑测量重复性、标准溶液的配制、标准曲线的制备等因素对测量的影响,测得Cr6+的合成标准不确定度为0.023mg/L。     

分光光度法测定硝酸盐氮中的干扰因素

对酚二磺酸分光光度法测定水样中硝酸盐氮的标准方法进行研究,在不同浓度的氯化物、氨氮和亚硝酸盐氮中加入不同浓度的硝酸盐氮标准溶液进行干扰试验。结果表明:在最佳的试验条件控制下,氯离子对低浓度硝酸盐氮测定产生的负干扰明显大于对高浓度硝酸盐氮产生的负干扰;随着加入的氨氮和氯化物浓度的增加,硝酸盐氮含量的测定结果低于实际值,且逐渐减小;在试验浓度范围内亚硝酸盐氮浓度对硝酸盐氮的测定几乎无影响。     

土壤中常见离子在紫外区的吸收特Ⅰ.低浓度离子溶液

将分析纯物质配制成10μg/ml浓度,应用岛津UV-1601紫外分光光度计,在波长190~335nm内扫描溶液的吸收峰,结果表明,硝酸相盐物质在201nm处有一稳定的吸收峰,吸收值与浓度成良好的线性关系,相对于硝酸盐物质而言,亚硝酸钠吸收峰红移至210nm,CaSO4、SrCl2均呈现低吸收,但其吸收峰在<200nm的远紫外区,在该浓度下,NH4Cl、HCl和KCl均呈现低吸收,并集中在远紫外区,而KH2PO4和NH4F几乎没有吸收．     

土壤中常见离子在紫外区的吸收特性──Ⅱ.高浓度离子溶液与低浓度混合

探讨不同离子浓度与不同无机溶液的混合对紫外光吸收的影响,结果表明,盐酸盐在较高浓度下吸收值迅速增大,吸收峰向红区移动,而硫酸盐在远紫区有一定程度的吸收,KH2PO4与NH4F接近无吸收。多数情况下,无机溶液对紫外光的吸收主要决定于阴离子类型,而与阳离子无关.不同类型溶液的混合基本不改变溶液的吸收特性,硝酸盐在低浓度下对紫外的吸收极为稳定,基本不受共存离子的干扰。0.01mol/LCuSO4与2mol/LKCI吸收峰与硝酸盐吸收峰重叠,但饱和CaSO4与硝酸盐吸收峰不重叠。     

流动注射分光光度法在线分析水中总铁

采用流动注射邻菲哕啉分光光度法在线分析水中总铁,考察了显色剂、消解液、酸度、反应盘管长度、载流流量、注样体积、采样时间等因素对试验的影响。方法在0.100mg／L-10.0mg／L范围内线性良好,检出限为0.04mg／L,实际水样平行测定的RSD≤3.7％,加标回收率为95.0％-96.0％。