浊度在氨氮测定中的干扰及其消除

对饮用水、地下水、天然水和高度净化过的废水出口的清洁水样 ,采用纳氏试剂光度法测定氨氮时 ,无论是采取直接比色法还是絮凝沉淀预处理水样中 ,存在的浊度往往会对纳氏试剂比色的测定结果产生影响。为此 ,建议做补偿校正 :在5 0 ml比色管中 ,水样定容后加 1 .0 ml酒石酸钾钠溶液 ,混匀。加 1 .5 ml1 5 %氢氧化钾溶液 ,测量吸光度 (此为校正吸光度 )。然后从水样经纳氏试剂比色测得吸光度中减去校正吸光度。浊度在氨氮测定中的干扰及其消除@俞是聃$三明市环境监测站!福建三明365000…     

原子吸收分光光度计用于冷原子吸收法测汞的试验研究

实验部分 一、原理及方法:汞蒸气对波长253.7nm的光有选择性吸收,在一定温度范围内,吸光度与汞蒸气浓度成正比。 水样经消化后,将各种形态的汞全部转化为二价汞离子,过量的氧化剂用盐酸羟胺还原,然后用氯化亚锡将汞离子还原为单质汞。在室温下,由载气将单质汞蒸气导入吸收管,在波长253.7nm处测定其吸光度,根据吸光度与浓度关系进行定量。用已知不同浓度的Hg离子标     

用分光光度法测定工业废水色度的探讨

一、实验方法 1.试剂 铂钴色度标准、铬钴色度标准:按常规方法配制。 2.分光光度法 (1)按常规方法,配制0—200度的标准系列,并用分光光度计以420 nm波长、5cm比色皿测定吸光度,绘制标准曲线。 (2)澄清水样可直接测定,由标准曲线查得色度。若水样色度过高,应用蒸馏水稀释。     

总氮测定中的一点体会

在总氮测定中消解时间不够或高压锅压力不足 ,均会造成过硫酸钾分解不完全 ,从而导致空白吸光度偏高 ,标准曲线线性和结果重现性差。 ( 1 )样品消解 1 0、2 0、30、40 min,2 2 0 nm处的空白吸光度分别为 0 .378、0 .0 35、0 .0 1 5、0 .0 1 4,故样品至少需消解 30 min。 ( 2 )用家用高压锅消解样品 ,稍有漏气 ,消解 30 min,2 2 0 nm处的空白吸光度在0 .2 30～ 0 .874之间 ,空白吸光度高 (有时高于祥品吸光度 )且波动性大。不漏气情况下的空白吸光度在 0 .0 1 5左右 ,波动性小。因此消解时要注意观察高压锅是否漏气总氮测定中的一点体会@赵多…     

荧光素分光光度法测定水中痕量二氧化氯

在pH10.5NH4Cl-NH3缓冲溶液中,荧光素在490nm处有一最大吸收峰。当加入二氧化氯后,其吸收峰降低,在490nm波长处的吸光度降低值与二氧化氯浓度在0.10～4.0μgml范围成良好线性关系,检出限(3σ)为0.04μgmlClO2。据此建立了一个灵敏简便、快速准确,选择性测定痕量二氧化氯含量的分光光度法,用于水样分析,结果满意。     

磷钼蓝比色法合适工作波长及线性范围的探讨

采用抗坏血酸-钼锑抗混合液作为磷钼蓝比色法测定磷含量的显色剂,形成稳定的显色液后,应用756CRT型紫外可见分光光度计进行600~850nm范围内的波长扫描。结果表明,吸收峰在722.2nm附近,同时,对720nm波长下的吸光度值与不同磷浓度吸收峰下的吸光度值进行比较,两者无显著差异。并且考虑到对于普通型的分光光度计很难做到722.2nm这样精确的调节。所以,可把720nm作为合适的工作波长,且磷浓度在0~1.0mg/kg内呈线性范围。     

紫外分光光度法快速测定水和废水中苯胺

水样用中速滤纸过滤后 ,吸取滤液适量 (含苯胺 1 .0～ 1 2 5 μg)于 2 5 ml具塞比色管中 ,加入 2 mlp H=7的缓冲溶液 ,用蒸馏水稀释至刻度混匀 ,放置 1 0分钟后 ,以蒸馏水做参比 ,在波长 2 30 nm处用 1 cm的石英比色皿 ,测定吸光度值。n=6时 ,变异系数 0 .34%～ 3.5 %。检出限     

1-(2,6-二氯-4-硝基苯)-3-(4-硝基苯)-三氮烯光度法测定矿山废水中的锌

研究了用1-(2,6-二氯-4-硝基苯)-3-(4-硝基苯)-三氮烯(DCNPNPT)分光光度法快速直接测定锌的方法。在表面活性剂TritonX-15的存在下,pH=9.5～10.5的Na2B4O7-NaOH介质中,DCNPNPT与锌( )可生成1∶3的橙黄色络合物。最大吸收波长为445nm,同时在535nm配合物有一最大负吸收,建立以535nm为参比波长,445nm为测定波长的双峰双波长法进行测定,表观摩尔吸光系数可达1.12×105L/(mol·cm)。用拟定的方法测定矿山废水中的锌,与原子吸收法测定的结果十分吻合,结果令人满意。     

如何提高分光光度分析的准确度

分光光度测定中，从采样、预处理、溶液配制与稀释、回归方程制作、数据计算等各个环节，都要考虑有效数字的位数是否满足要求，其对分析结果准确度有举足轻重的影响；最大吸收波长的扫描、溶液稀释方式、仪器空白值的扣除等操作环节对分析结果也会产生重要影响。     

影响总氮准确定量的光谱检测因素

对现行的双波长紫外分光光度法在测定水体总氮中由光学检测本身所产生的影响因素进行了探讨,提出了一种基于三波长的光谱检测总氮量的方法。结果表明,由于仪器信号波动或光散射引起的光谱检测基线上移所造成的误差可以用在NO3-没有吸收的340 nm处的吸光度加以判断,从而用三波长的方法扣除由于光谱基线上移对220 nm和275 nm处吸光度检测的干扰。对2个水样进行同样的光谱检测,以不同的计算公式所得的数据比较可以看出,三波长法明显优于双波长法。三波长法检测重现性相对偏差小于0.2%,其总氮含量的结果要比双波长法高7%～16%。这也解决了人们对总氮含量测定结果总是偏低的困惑。     

分光光度法测定水和废水中硫化物实验条件的优化选择

在碱性介质中,水和废水中硫化物S2-可与碘反应,产物与CN-反应生成硫氰酸根,再与Fe3+反应,形成红色的硫氰酸铁,此生成物处于波长460nm处,可以通过对此红色液体进行分光光度法测定,根据吸光值大小确定水和废水中硫化物含量。     

闭管消解-萘乙二胺分光光度法测定水中总氮

通过实验研究了一种采用闭管消解-萘乙二胺分光光度法测定水样中总氮的新方法,分析了不同测试条件对测定结果的影响。结果表明:方法最佳消解时间为25min,宜选用535nm为实验波长,在10～25℃下显色5～20min完成测定。与标准方法比较,该方法具有灵敏度高、测定时间短的优点,可用于环境监测中水和废水的总氮分析。     

煤化工厂烟气中苯并(a)芘现状监测分析

通过试验建立了煤化工厂烟气中苯并(a)芘的液相色谱监测分析方法.通过条件优化,用配有荧光检测器的高效液相色谱仪分析烟气样品中苯并(a)芘的含量,该方法以乙腈、水梯度比例混合作为流动相;流速为1.0 ml/min;激发波长为255nm、发射波长为420nm;保留时间为27.38 min,测定检出限为2×10-3μg/m3...     

气相分子吸收光谱法测定印染废水中氨氮的影响因素

采用气相分子吸收法光谱测定印染废水中的氨氮,并对相关影响因素进行探讨。结果证实,硫化物和尿素会对氨氮的测定产生负干扰,硫化物干扰可用乙酸锌-乙酸钠固定液沉淀法去除,尿素干扰可以用稀释法去除,但仅适用于氨氮质量浓度0.10 mg/L且稀释后尿素质量浓度≤100 mg/L的水样;苯胺、浊度和色度对测定无干扰,可直接检测。     

The development of a chemical 'fingerprint' to characterise dissolved organic matter in natural waters

A suite of twelve assays has been used to 'fingerprint' dissolved organic matter (DOM). The assays were applied directly to filtered natural water samples. Temperature, pH and conductivity accounted for the environmental conditions on-site. Bulk carbon characteristics were assayed by measuring UV absorbance at 200 and 240 nm, colour in grade Hazen, DOC (dissolved organic carbon), fluorescence (excitation 370 nm, emission 450 nm) and the complexation of phenol itself. Measuring hydroxybenzenes ('monophenolics'), polyhydroxybenzenes ('polyphenolics') and total phenolics with the Gibbs, Prussian Blue and Folin-Ciocalteau assays, respectively, determined the phenolics pool. The methodology was tested on six freshwater sites in North Wales chosen to provide differences in vegetation, land-use and water chemistry and sampled once during each season. A novel approach for the presentation of the data has been developed that combines all range normalised assay results for each site and each season within one polar plot, hence the term 'fingerprint'. The data was also analysed using principal component factor analysis. Assays characterised as determining the chemical properties of DOM contributed to Factor 1 and explained 59% of the variation in the data. Assays apparently determined by the water matrix, contributed to Factor 2 and explained 20% of the variation within the data. The factor scores obtained for each site showed more variation for assays relating to the chemical properties of DOM than to the surrounding water matrix. The methodology was found to detect chemical changes within DOM for each site throughout the year and different responses for different sites.     

高压液相色谱法测定地表水和饮用水中的阿特拉津

通过条件实验,建立了水体中阿特拉津的高效液相色谱检测法,以ODS C18柱为色谱柱,甲醇:水=60:40为流动相,检测波长225nm,柱温40℃,用二氯甲烷萃取,外标法定量,线性范围为0.02～10.0mg/L,相关系数达0.9999,采样体积为500 ml时,方法检出限为0.012μg/L,精密度在2.5%～11.4...     

Facile and Sensitive Spectrophotometric Determination of Synthetic Pyrithroids in Their Formulations, Water and Grain Samples

A novel reagent was introduced for the facile and sensitive spectrophotometric determination of syntheitic pyrethroids in their formulations (fenvalerate, cypermethrin and decamethrin), water and grain samples. These methods were based on the hydrolysis of synthetic pyrethroids under the alkaline conditions to form respective aldehyde groups. These groups were condensation with 3-methyl-2-benzothiazolinone hydrochloride (MBTH) to yield color derivatives having λ_max at 520 nm for fenvalerate, 516 nm for cypermethrin and 512 nm for decamethrin. The proposed method could be successfully applied for the determination of synthetic pyrethroids in their formulations, water and grain samples.     

利用曲线补偿变时溶出示差技术测定Cu、Pb、Zn、Cd初步探讨

本文利用曲线补偿，变时溶出示差技术提高了测定Ｃｕ、Ｐｂ、Ｚｎ、Ｃｄ的灵敏度、精密度和准确度，进一步改变了谱图的分辨率，避免了Ｏ２波的干扰     

Translocation of Sb and Ti in an undisturbed floodplain soil after application of Sb2O3 and TiO2 nanoparticles to the surface

The pore water transport of antimony and titanium, applied as nanoparticles (NPs), was studied by spiking stable suspensions of two different nanomaterials on the surface of an undisturbed floodplain soil. For preparation of stable dispersions, two different strategies were followed. (i) Comparable to those used in industrial applications: titanium dioxide nanoparticles, with an average diameter of 99 nm, were prepared by high-energy ball milling in water, whereas for (ii) antimony trioxide (Sb(2)O(3); average diameter 121 nm) a dispersing agent (sodium salt of poly[(naphthaleneformaldehyde)sulfonate] (pNFS) in water) was used. The upper 17 cm of a floodplain soil (river Rhine, Germany) was sampled using the minimally invasive sediment or fauna incubation experiment (SOFIE? two compartment cell; 3 l volume each), which preserved the pore system of the soil. The cells were equipped with 450 and 100 nm filter probes at different depths providing a non-invasive sampling of the pore water. The pore water was sampled at different times (T = 0, 24, 48, 96 and 196 h) and analysed by inductively coupled plasma quadrupole mass spectrometry (ICP-QMS). Sb and Ti were transported via the pore water of the floodplain soil to a depth of 14 cm, corresponding to the maximum cell depth. The highest Sb concentration in the pore water was detected after 24 h at a depth of 5.5-8 cm. Although the spiked concentration was higher for Ti than for Sb, the total Ti concentration in the pore water of the spiked cell was lower. This indicates a stronger agglomeration of TiO(2) NPs or a more intensive interaction of Ti with the solid matrix and a faster transport of Sb towards deeper soil layers. The results show that metal(loid)s from metal oxide NPs are transported in the soil pore water and, hence, have the potential to act as the source of contamination of deeper soil layers after soil surface contamination.     

Determination of three alkylphenol isomers in various water samples using a new HPLC method based on a duet stationary phase

The level of three alkylphenols (APs) 4-nonylphenol, 4-octylphenol and 4-tert-octylphenol was monitored in various water samples using a new developed and validated HPLC method. The HPLC method employed a column with a mixed-mode stationary phase (C18/SCX) using a mobile phase of water to methanol?=?15:85 (v/v) delivered at a flow rate of 1 mL/min at room temperature. Both diode array, DAD and fluorescence, FLD detectors were employed. The method is linear when APs concentration ranged from 0.025 to 0.5 μg/mL with a DAD detection at 279 nm and between 0.0008 and 0.1 μg/mL when the detection was made by FLD (excitation at 220 nm, emission at 315 nm). The limit of detection and limit of quantitation for alkylphenols were found to be 5 and 15 ng/mL, respectively (detection by DAD). The method was employed with good results for the determination of APs in the presence of polycyclic aromatic hydrocarbons in various water samples.