【已撤稿】淡水磷监测中钼酸铵分光光度法的改进

我国现行淡水水体中磷测定方法为钼酸铵分光光度法（GB 118931989）,该方法检测下限为0.01 mg/L,但我国南亚热带地区部分水体的总磷以及多数水体的溶解态磷浓度均低于0.01 mg/L,通过对标准试样和野外水样的测定,分析该方法在监测低磷浓度水体中可能出现的问题并提出改进方法.结果表明：对于磷浓度低于0.01 mg/L的水体,国标法灵敏度低,准确性差.通过3个方面的改进可提高该方法测定的灵敏度和准确性：1）将消解水样体积由25 ml增加到50 ml,消解后不再进行二次稀释定容;2）改变显色剂的配制,显色剂由14%硫酸溶液50 ml、酒石酸锑钾溶液5 ml、4%钼酸铵溶液15 ml和0.1 mol/L的抗坏血酸溶液30 ml混合而成,现配现用;3）将测定波长设置为880 nm.改进后方法的灵敏度有较大提高,能准确、有效地检测磷浓度在0.003~0.01 mg/L的水样.     

二安替比林间溴苯基甲烷—高碘酸钾体系动力学光度法测定钌

在Ｈ３ＰＯ４介质中,Ｒｕ（Ⅲ）对ＫＩＯ４氧化二安替比林间溴苯基甲烷（ＤＡｍＢＭ）的显色反应有明显的催化作用。基于此,建立了测定痕量钌的催化分光光度分析法,并且测定了一些动力学参数。方法的检出限为２,３μｇ／Ｌ,钌的质量浓度在０￣１２μｇ／Ｌ符合比尔定律。方法已应用于矿样中痕量钌的测定,５次测定的ＲＳＤ〈５％,加标回收率在９６￣１０１％。     

在线有机相析出法流动注射液—液萃取测定矿石中铜的研究

用自制的分相器与流动注射仪联用,对有机相同液－液萃取光度法测定微量铜的流路参数和操作程序进行优化。以新铜试剂为显色剂,用含一定量乙醇的辛醇溶液作载流,采用双产流路,在４５８ｎｍ外进行检测。方法的线性范围是０．０５￣１．０５ｍｇ／Ｌ,萃了 倍数１０,检测限为２０μｇ／Ｌ,分析速度３６／ｈ,方法的精密度（ＲＳＤ）是４．０％。测定锌矿石样品中铅,结果与推荐值一致。     

2,6-二氯苯酚的催化氯化合成

报道一种在区域选择性催化剂存在下,以２氯苯酚直接氯化合成２,６二氯苯酚的方法。该法具有合成工艺简单和产率较高等特点。     

光度法测定造币镀液及其废液中的铁和镍

在酸性介质中,Ｆｅ＾３＋与磺基水杨酸络合物的吸收峰在５１０ｎｍ处,在此波长处大量Ｎｉ＾２＋的吸收最弱,而Ｎｉ＾２＋在７２０ｎｍ处出现吸收峰,此外铁的络合物的吸收亦很弱,据此建立了题示样品中铁和镍的光度分析方法。铁和镍的相互干扰可用中以消除,其它共享离子不干扰测定。测定造币镀液及其废液样品中铁和镍的相对标准偏差（ｎ＝５）分别〈２．５％和〈１．８％,加标加收率分别为９７．０％～１０２．１％和９７．４％     

Measurement of trace manganese (II) by the catalytic kinetic spectrophotometric method

A new kinetic spectrophotometric method is developed for the measurement of manganese (II) in water. The method is based on the catalytic effect of manganese (II) with the oxidation of weak acid brilliant blue dye (RAWL) by KIO₄ using the Nitrilo triacetic acid (NTA) as an activation reagent. The optimum conditions obtained are 40 mgL⁻¹ RAWL, 1×10⁻⁴molL⁻¹ KIO₄, 2×10⁻⁴ molL⁻¹ Nitrilo triacetic acid (NTA), pH = 5.8, the reaction time of 3.00 min and the temperature of 20.0 °C. Under the optimum conditions, the proposed method allows the measurement of manganese (II) in a range of 0–50.0 ng mL⁻¹ and with a detection limit of down to 0.158 ng mL⁻¹. The recovery efficiency in measuring the standard manganese (II) solution is in a range of 98.5%–102%, and the RSD is in a range of 0.76%–1.25%. The new method has been successfully applied to the measurement of manganese (II) in both fresh water and seawater samples with satisfying results. Moreover, few cations and anions interfere with the measurement of manganese (II). Compared with other kinetic catalytic methods and instrumental methods, the proposed method shows fairly good selectivity and sensitivity, low cost, cheapness, low detection limit and rapidity. It can be applied on boats easily.     

Measurement of Trace Manganese(Ⅱ) by the Catalytic Kinetic Spectrophotometric Method

A new kinetic spectrophotometric method is developed for the measurement of manganese (Ⅱ) in water. The method is based on the catalytic effect of manganese (Ⅱ) with the oxidation of weak acid brilliant blue dye (RAWL) by KIO4 using the Nitrilo triacetic acid (NTA) as an activation reagent. The optimum conditions obtained are 40mgL-1 RAWL, 1×10-4molL-1 KIO4, 2×10-4molL-1 Nitrilo triacetic acid (NTA), pH = 5.8, the reaction time of 3.00 min and the temperature of 20.0 ℃. Under the optimum con-ditions, the proposed method allows the measurement of manganese (Ⅱ) in a range of 0-50.0ngmL-1 and with a detection limit of down to 0.158 ng mL-1. The recovery efficiency in measuring the standard manganese (Ⅱ) solution is in a range of 98.5%-102%, and the RSD is in a range of 0.76%-1.25%. The new method has been successfully applied to the measurement of manganese (Ⅱ) in both fresh water and seawater samples with satisfying results. Moreover, few cations and anions interfere with the measurement of man-ganese (Ⅱ). Compared with other kinetic catalytic methods and instrumental methods, the proposed method shows fairly good selec-tivity and sensitivity, low cost, cheapness, low detection limit and rapidity. It can be applied on boats easily.     

催化光度法测定煤中钒

催化光度法测定煤中钒邵谦１葛圣松刘志强贝太伟山东矿业学院济南分院济南２５００３１利用Ｖ（Ⅴ）对溴酸盐氧化还原型罗丹明Ｂ反应的催化作用，文献［１］建立了测定痕量钒的催化荧光法。本文以此反应为指示反应，改测其激发波长下的吸光度，建立了催化光度法测定痕量钒...     

新显色剂2—（2—咪唑偶氮）—苯甲酸的合成及其与钴的显色反应研究

合成了新显色剂２（２咪唑偶氮）苯甲酸（简称ＩＡＢＡ）,分子式Ｃ１０Ｈ８Ｎ４Ｏ２,分子量２１６．２０,熔点２１３℃,各级酸离解常数ｐＫａ１为３．２,ｐＫａ２为９．８,研究了它的性质及其与钴显色反应的条件。在ｐＨ７的ＮＨ４Ａｃ介质中,试剂与钴形成紫红色络合物,λｍａｘ为５４６ｎｍ,试剂的λｍａｘ为４６２ｎｍ,Δλ为８４ｎｍ,Ｃｏ２＋与试剂络合比为１∶２,摩尔吸光系数１．６１×１０４Ｌ·ｍｏｌ－１·ｃｍ－１,Ｃｏ２＋在０～０．８ｍｇ／Ｌ遵守比尔定律。所拟方法直接测定了工业废水及ＶＢ１２中痕量钴,结果与原子吸收法相符,加标回收率为１０１．３％～１０２．２％,ＲＳＤ（ｎ＝６）在２．０％～２．７％。