“甲基橙分光光度法测下水道中氯气含量”的标准化验证研究

详细阐述了在制定行业标准《城镇排水设施气体的检测方法》（cJ／T307—2009）子项“甲基橙分光光度法测下水道中氯气含量”时,检测数据的标准化验证过程。通过统计分析基础检测数据。确定了方法检出限为0．025lrJIg／L,测定下限为0．10mg／L,测定上限为1．00nqmg／L。样品浓度为0．300mg／L时,重复性相对标准偏差1．5％,再现性相对标准偏差1．7％,相对误差0．51％±1．94％。浓度水平0．700mg／L时,重复性相对标准偏差0．70％,再现性相对标准偏差0．81％,相对误差-O．03％±0．96％,实测样品加标回收率95．2％～105％。各项技术指标满足预期目标,甲基橙分光光度法测定下水道中氯气含量可行。     

云南某砷矿区冶炼渣中Hg存在形态研究

利用BCR三步提取法提取砷冶炼渣中Hg的铁锰氧化物结合态、可交换态及碳酸盐结合态、有机物及硫化物结合态,再以高压密闭消解法分离出矿渣中的Hg元素,采用原子荧光光度法测定Hg的总含量,最后计算出残渣态Hg含量。结果表明,云南某砷矿废矿场中汞的存在形态主要是铁锰氧化物结合态、可交换态及碳酸盐结合态,这两种形态的Hg含量超过总含量的85％;有机物及硫化物结合态和残渣态的含量所占比例较小。     

Determination of thiocyanate in the vacuum carbonate desulfurization wastewater

In acidic solution, thiocyanate molecules reacted with ferric ions to produce red complexes. The concentration of thiocyanate could be determined by spectrophotometer. The effects of wavelength, volume of color reagent, acidity and color time on absorbance were investigated. The interferences of co-existing ion were discussed as well. Results showed that the relation between absorbance and the concentration of thiocyanate was in accord with Beer's law when the concentration of thiocyanate was 2–20 mg/L. The linear regression equation was Absorbance = 0.0523Concentration–0.0156, with a linear correlation coefficient of 0.9997. The average recovery rates of two kinds of vacuum carbonate desulfurization wastewater were 100.95% and 99.62%, and relative standard deviations were 0.79% and 0.14% respectively. It shows that the method was quick, high precision, accurate and easy to handle.     

精密度偏性试验在水质分析中的应用

以对总磷进行精密度实验为例,介绍了辽宁省营口水环境中心开展质量控制工作情况。每天分析1批,每次各2份,共分析6批,其中天然水样10批。结果显示：F检验无显著性变异,总标准差均小于被测浓度的5％,回收率检验合格,控制图中的数据全部落在控制限内,质控图分布合理。     

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.     

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.     

催化动力学光度法测定工业废水中的Cr（Ⅵ）

采用β-环糊精作为H₂O₂氧化茜素红褪色反应的增敏剂,建立了催化动力学光度法测定工业废水中Cr（Ⅵ）的新方法。该方法最佳反应条件为：反应体系总体积25 mL,0.1 mol/L的H₂SO₄溶液加入量2.0 mL,1.0×10^-3 mol/L茜素红溶液加入量1.5 mL,30%的H₂O₂溶液加入量4.0 mL,100 g/L的β-环糊精溶液加入量3.0 mL。在最大吸收波长554 nm处测定反应前后溶液的吸光度,Cr（Ⅵ）的质量浓度与吸光度差值（ΔA）在4.0×10^-4~5.4×10^-2 mg/L范围内符合比尔定律,线性回归方程为：ΔA=18.52ρ+ 0.018,相关系数为0.996 6,检出限为3.5×10^-4 mg/L,加标回收率为99.46%~101.3%,6次测定的相对标准偏差小于等于2.4%。该法的测定结果与GB/T 7467-1987中的二苯碳酰二肼分光光度法相近。     

Removal of fluorescence and ultraviolet absorbance of dissolved organic matter in reclaimed water by solar light

Storing reclaimed water in lakes is a widely used method of accommodating changes in the consumption of reclaimed water during wastewater reclamation and reuse. Solar light serves as an important function in degrading pollutants during storage, and its effect on dissolved organic matter(DOM) was investigated in this study. Solar light significantly decreased the UV_(254) absorbance and fluorescence(FLU) intensity of reclaimed water.However, its effect on the dissolved organic carbon(DOC) value of reclaimed water was very limited. The decrease in the UV_(254) absorbance intensity and FLU excitation–emission matrix regional integration volume(FLU volume) of reclaimed water during solar light irradiation was fit with pseudo-first order reaction kinetics. The decrease of UV_(254) absorbance was much slower than that of the FLU volume. Ultraviolet light in solar light had a key role in decreasing the UV_(254) absorbance and FLU intensity during solar light irradiation. The light fluence-based removal kinetic constants of the UV_(254) and FLU intensity were independent of light intensity. The peaks of the UV_(254) absorbance and FLU intensity with an apparent molecular weight(AMW) of 100 Da to 2000 Da decreased after solar irradiation, whereas the DOC value of the major peaks did not significantly change.     

分光光度法测定底质总磷的方法探讨

在一定条件下,用硫酸和过氧化氢进行消解,使不溶性磷酸盐和有机磷转化为正磷酸盐,待测液与钼酸盐反应生成磷钼杂多酸,加入还原剂抗坏血酸后转变成蓝色络合物,进行比色测定。实验表明,该方法回收率为93．4％～99．7％,检出限为0．009mg／L,RSD为4．0％。方法简便、可靠,能满足环境监测底质总磷分析的需要。     

不同酸对造纸黑液酸析效果的研究

采用酸析法从造纸黑液中分离木质素,同时去除部分COD和色度,从而完成对黑液的初步处理。实验研究了酸析的最佳pH值,并将硫酸、硝酸、盐酸、磷酸、甲酸和草酸作为酸析剂,分析其分别对黑液色度、COD的去除效果及对木质素提取的影响。介绍了通过快速消解分光光度法来测定COD值,和用分光光度法测定色度值,分别建立COD值和色度对吸光度的工作曲线,使测量更加方便高效快捷,其精确度和准确度都能符合分析方法要求。实验结果表明,酸析效果较好的pH取值范围为2～4,考虑用酸的经济性和处理效果,选择pH=3作为最佳酸析条件;经过对酸析过程规律和原因的分析可得,硫酸、硝酸和磷酸对黑液处理效果较为理想,其中硫酸因其经济性被选为最佳,其色度、COD去除率分别为97.9%和66.1%,木质素的析出量为8.65 g/L。