新方法在挥发酚测定中的探讨

新型显色剂2-对氨基苯基-2'-羟基二乙胺与水中挥发酚在碱性条件下,经铁氰化钾作用发生反应,反应产物用乙酸丁酯萃取后在可见紫外分光光度计600 nm波长下比色定量。该方法测定挥发酚在0.001 mg/L~0.100 mg/L范围内线性良好,方法检出限为0.000 8 mg/L,加标回收率为100%。用该方法与4-氨基安替吡啉三氯甲烷萃取分光光度法同时测定实际水样,结果无显著差异。     

水中挥发酚测定中的几个问题

1试剂提纯 :将 1 0 0 ml2 % 4 - AAP溶液置于50 0 ml分液漏斗中 ,加 5ml三氯甲烷盖塞后剧烈摇荡 2 min,静置分层 ,上清液留作显色液。 2缓冲溶液的 p H值控制 :缓冲溶液 p H值随配制时间而变化 ,放置两周后应适当增加缓冲溶液用量或重新配制 ,使其达到水溶液 p H值在 9.6～ 1 1 .5范围内 ,否则会使水样吸光度偏高。 3萃取时间控制 :在测定低浓度挥发酚时 ,加入氯仿后适当把振摇时间增加至 3min,其结果更接近保证值。 4铁氰化钾反应时间控制 :同一批水样数量最好不超过 1 0个。每个水样间隔 3～ 4min加铁氰化钾 ,使每个样品保证在加入铁氰…     

萃取法测定水中挥发酚后氯仿的回收和应用

利用氯仿低沸点的性质,用分馏回收的方法处理废氯仿并再用于酚的分析,同时以标准样品进行保证检验,得到较满意的结果。 一、废氯仿的前处理:测定挥发酚后留下的废氯仿液中含有少量的氧化剂铁氰化钾以及微量的显色剂4-氨基安替比林。此时加入一定量的还原剂亚硫酸钠消除废液中的氧化性物质。每400ml废氯仿可加20％亚硫酸钠水液1ml,充分摇匀,稍放置片刻,即可分馏提取。     

地表水总铅的原子荧光法测定条件的优化研究

对地表水中总铅的原子荧光法测定条件进行了优化。考察了仪器负高压和灯电流、载气和屏蔽气流量、原子化器高度、介质及酸度、硼氢化钾浓度、铁氰化钾浓度等测定条件对结果的影响。优化确定条件为:负高压240V、灯电流80mA、原子化器高度10mm、载气流量300mL/min、屏蔽气流量800 mL/min、介质盐酸、酸度1.0%、硼氢化钾浓度1.0%、铁氰化钾浓度1.0%。在最佳测定条件下,标准曲线在0～50μg/L内线性良好,检出限为0.07μg/L,精密度为1.52%～2.79%,加标回收率为93.0%～101%。     

苯酚一次氯酸钠光度法测定水中微量苯胺

在亚硝基铁氰化钾存在下,苯胺在磷酸盐介质（pH＝11．4）中与次氯酸钠、苯酚反应形成靛酚。苯胺在0．06－6．40mg/L内服从比耳定律,用于环境水中微量苯胺的测定,结果与标准方法吻合。     

以过硫酸钾为氧化剂测定水中挥发酚

以过硫酸钾代替铁氰化钾作氧化剂 ,在pH 1 0± 0 2溶液中 ,用 4-氨基安替比林萃取法比色测定低浓度挥发酚 ,于 460nm处有最大吸收峰 ,在 0 μg/2 50mL～ 1 5μg/2 50mL范围内符合比尔定律。 4次校准曲线相关系数为 0 9999～ 0 9994。相对标准偏差为 0 2 % ,回收率为 91 %～ 97%。显色反应的选择性、稳定性、重现性和准确性均较好。氧化剂较稳定 ,易保存、无毒性。     

苯酚-次氯酸钠光度法测定水中微量苯胺

在亚硝基铁氰化钾存在下 ,苯胺在磷酸盐介质 ( p H=1 1 .4 )中与次氯酸钠、苯酚反应形成靛酚。苯胺在 0 .0 6～6 .4 0 mg/ L内服从比耳定律 ,用于环境水中微量苯胺的测定 ,结果与标准方法吻合。     

测定酚产生高空白的原因探讨

利用4－氨基安替比林萃取法测定不样中的挥发酚，其空白值很高且极不稳定，共萃取现象严重。文中利用氯仿作萃取剂，以控制4－氨基安替比林和铁氰化钾的使用量，降低共萃取现象带来的高空白值，提高萃取效率。     

流动注射法测定水和废水中挥发酚

采用流动注射法在线测定水和废水中挥发酚,优化了仪器测试条件,试验了铁氰化钾缓冲液的稳定性.该方法在0 μg/L～200 μg/L线性关系良好,检出限为0.7 μg/L,精密度和准确度均能满足要求,而且分析速度快,试剂消耗量少,适用于大批量饮用水、地表水、生活和工业排放废水中挥发酚的测定.     

不蒸馏直接比色判断挥发酚考核样的稀释倍数

按考核样说明进行稀释后取５０ｍｌ移入５００ｍｌ分液漏斗中,加缓冲液２０ｍｌ,使ｐＨ＝１０±０２,加４氨基安替比林溶液１５０ｍｌ、铁氰化钾１５ｍｌ,充分混匀呈浅绿色放置１０ｍｉｎ,加１０００ｍｌ三氯甲烷,剧烈振摇２ｍｉｎ,待有机相与水相充分...     

超声辅助离子液体-分散液液微萃取-高效液相色谱法测定水中苯胺类化合物

本研究建立了超声辅助离子液体-分散液液微萃取-高效液相色谱测定环境水样中苯胺(AN)、对氟苯胺(4-FA)、对硝基苯胺(4-NA)、对氯苯胺(4-CA)四种苯胺化合物的方法。以最常用的烷基咪唑六氟磷酸盐类离子液体为萃取剂,通过超声加速萃取剂的分散程度,提高了萃取效率。该方法的检测限达到0.1~73 ng/ml,对黄河水和自来水中的加标回收率均在90.5%~113%之间,回收效果良好。与传统的液液萃取相比,该萃取方法具有绿色、快速、富集效果好、有机溶剂消耗小的优点,可以满足环境水体中苯胺类化合物的测定。     

Hydrochemistry of Wet Atmospheric Precipitation Over an Urban Area in Northern Indo-Gangetic Plains

Rain water samples were collected to study the chemical composition of wet atmospheric precipitation (first event) over the Lucknow city in the northern Indo-gangetic alluvial plains. The samples were collected in the month of July, 2005 from different sites. The wet precipitation samples were analyzed for pH, EC, major ions (, Cl⁻, , , , F⁻, Na⁺, K⁺, Ca²⁺, Mg²⁺, ) and heavy metals (As, Cd, Al, Co, Cr, Cu, Fe, Mn, Mo, Ni, Hg, Pb, Se, Sn, Ti, V, Zn). The pH values of wet precipitation samples ranged between 6.5 and 8.7. The analysis of linear regression applied to the set of studied variables and computation of neutralization factors showed that neutralization occurred in precipitation samples and Ca²⁺ had the maximum neutralization capacity. It was found that Cl⁻, , Ca²⁺, Mg²⁺, Na⁺ and K⁺ in the precipitation samples originated mainly from crustal/anthropogenic sources in the region. On an average Fe, and Al accounted for >72% of the total concentration of trace metals in the wet precipitation samples followed by Zn (>10%). Enrichment factors calculated for heavy metals over reference background level in seawater and Earth’s crust showed relatively higher enrichment of Zn. The principal component analysis (PCA) identified the possible sources of ionic species and heavy metals in the wet precipitation samples.     

Triethoxysilyl-substituted aminoethanethiol ligands for zinc and cadmium complexes and aminoethanethiol-modified silica gel. Evaluation of the corresponding supported molecular trap for metallic pollutant uptake (Cd2+, Hg2+ and Pb2+)

The reaction of 2-[3-(triethoxysilyl)propylamino]ethanethiol (LH, a) and 1-methyl-2-[3-(triethoxysilyl)propylamino]ethanethiol (LH, b) with ZnX2 and CdX2 (X = Cl, Br, I, NO3) in tetrahydrofuran (THF) or CH2Cl2 gives several complexes depending on the experimental conditions. Elemental analyses, IR, Raman, 13C[1H], 1H NMR and mass spectroscopies indicated the formation of mononuclear and dinuclear complexes. In the absence of NEt3 as proton quencher, the protonated ligands react in their zwitterionic form giving dinuclear [M(LH)X2]2 [M = Zn (1), Cd (2); LH = a, b; X = Cl, Br, I] or mononuclear M(NO3)2(LH)2 [M = Zn (5), Cd (6); LH = a] complexes. In both cases, coordination occurs through the S atoms, the ligands acting as terminal and bridging species. With NEt3, the deprotonated ligands are chelated through their N and S atoms and bridging occurs through the S atoms in [MLX]2 [M = Zn (3), Cd (4); LH = a; X = Cl, Br] complexes. The LH ligand is chemically grafted onto silica, the procedure optimized and the resulting material characterized by 13C and 29Si cross-polarization, magic-angle spinning (CP-MAS) NMR and DRIFT. This material is evaluated as a supported molecular trap for binding heavy metals (Cd2+, Hg2+, Pb2+) in aqueous solution. In both batch and column processes, it appears that Hg2+ and Pb2+ are trapped more than Cd2+, but in all cases values lower than those allowed were obtained.     

基于Berthollet反应示波极谱法测定水中微量氨

在亚硝基铁氰化钾存在下,氨在氢氧化钠介质中与苯酚、次氯酸钠反应,其产物靛酚在滴汞电极上产生－灵敏的吸附波,ＮＨ３－Ｎ在０．００３～０．２２ｍｇ／Ｌ内,导数峰电流与其呈良好的线性关系。用于环境水中ＮＨ３－Ｎ的测定,其相对标准偏差小于３％,回收率为９７％～１０５％,方法具有较好的选择性。     

Chemical speciation in mining affected waters: the case study of Asarel-Medet mine

The inorganic chemical species in Maresh and Luda Yana rivers affected by the Cu– Mo Asarel-Medet mine, Bulgaria were determined during a low-flow and a high-flow period. The mining activities, the weathering and the oxidation processes strongly influenced the physicochemical processes in the whole water system. The main pollution source was a small lake receiving the acid effluents of the mining activities. High levels of SO₄ ^2???, Cu, Mg, Al, Mn and Fe were determined at the mining polluted and affected stations. Cu^2?+? and CuCO₃ ⁰ species (1:1) were present in the reference waters and Cu^2?+? and CuSO₄ ⁰ species (1:1) in the polluted and affected waters; Cu^2?+? species was dominating downstream. Me^2?+? followed by $\rm{MeSO}_{4}^{\kern3pt{0}}$ (Me = Mn, Zn, Cd and Pb), $\rm{PbCO}_{3}^{\kern3pt{0}}$ and $\rm{PbHCO}_{3}^{\kern3pt{+}}$ species as well as $\rm{Fe(OH)}_{2}^{\kern3pt{+}}$ , $\rm{Al(OH)}_{4}^{\kern3pt{-}}$ , $\rm{Al(OH)}_{2}^{\kern3pt{+}}$ , $\rm{Al(OH)}_{3}^{\kern3pt{0}}$ were prevailing in the system. $\rm{MeSO}_{4}^{\kern3pt{+}}$ and $\rm{Me(SO}_{4})_{2}^{\kern3pt{-}}$ (Me = Fe, Al), $\rm{Me(SO}_{4})_{2}^{\kern3pt{2-}}$ (Me = Zn, Cd and Pb), $\rm{Me(SO}_{4})_{3}^{\kern3pt{4-}}$ (Me = Zn, Cd) and $\rm{Cd(SO}_{4})_{4}^{\kern3pt{6-}}$ species polluted and affected waters. The major elements K and Na were mainly Me^?+? species, whereas Ca and Mg were Me^2?+? and $\rm{MeSO}_{4}^{\kern3pt{0}}$ species in different ratios. The concentration of concentration of $\rm{NO}_{2}^{\kern3pt{-}}$ , $\rm{NO}_{3}^{\kern3pt{-}}$ and $\rm{NH}_{4}^{\kern3pt{+}}$ species as well as complex phosphorous species such as H₂ $\rm{PO}_{4}^{\kern3pt{-}}$ , $\rm{FeHPO}_{4}^{\kern3pt{+}}$ , $\rm{HPO}_{4}^{\kern4pt{2-}}$ , $\rm{CaPO}_{4}^{\kern3pt{-}}$ , $\rm{CaHPO}_{4}^{\kern3pt{0}}$ and $\rm{MgHPO}_{4}^{\kern3pt{0}}$ were also calculated. The trace element concentrations decreased downstream due to dilution, sorption processes and precipitation, but the percentage of free metal species, which are more toxic, increased. An exception was iron and aluminum of which the dominant hydroxy colloidal and sulphate species were easily incorporated into the suspended phase.     

Atmospheric concentrations of nitric acid, sulfur dioxide, particulate nitrate and particulate sulfate, and estimation of their dry deposition on the urban- and mountain-facing sides of Mt. Gokurakuji, Western Japan

Atmospheric concentrations of nitric acid (HNO₃), sulfur dioxide (SO₂), particulate nitrate and particulate sulfate on the urban- and mountain-facing sides of Mt. Gokurakuji were measured from November 2002 to October 2003, in order to evaluate the effects of anthropogenic activity on air quality and dry deposited nitrate and sulfate on the surfaces of pine foliage. The results showed that HNO₃, SO₂ and concentrations were significantly higher (P < 0.05) on the urban-facing side (1.54, 2.48 and 0.65 μg m⁻³, respectively) than the mountain-facing side (0.67, 1.19 and 0.37 μg m⁻³, respectively), while concentrations did not differ significantly between the two sides (urban-facing: 2.80 μg m⁻³; mountain−facing: 2.05 μg m⁻³). Indirect estimates of dry deposition rates of nitrate and sulfate to the surfaces of pine foliage based on the measured concentrations approximately agreed with the measured values determined by the foliar rinsing technique in a previous study. It was found that HNO₃ was the major source (approximately 80%) of dry deposited nitrate on pine foliage, while the contribution from was about equal to that from SO₂. In conclusion, HNO₃ and SO₂ appear to be dominant species reflecting higher dry deposition rates of nitrate and sulfate on the urban-facing side compared to the mountain-facing side of Mt. Gokurakuji.     

荧光分光光度法测定废水中的微量硫化物

建立了一种基于荧光素汞在碱性条件下与S^2-作用生成荧光性的物质，从而使荧光素汞的荧光强度下降，根据荧光强度的下降值来测定水样中S^2-含量的方法，测定范围为0.007-0.8mg/L，线性相关系数r为0.9987。大部分共存物质不干扰测定，加入甲醛溶液可消除CN^-的干扰，加入酒石酸可消除Fe^3 的干扰，测定结果令人满意。     

Aluminium in UK rivers: a need for integrated research related to kinetic factors, colloidal transport, carbon and habitat

Dissolved aluminium concentrations ([Al]) in the <0.45 μm filtered fraction are described for 54 UK river sites covering rural, acidic/acid sensitive, agricultural and urban typologies, and wide pH range (4 to 11). High [Al] occurred under acidic conditions and for acid runoff neutralised by bicarbonate rich groundwater. Thermodynamic analysis indicates Al hydroxide/hydroxy-silicate oversaturation at circumneutral pH across the rivers, but undersaturation at lower/higher pH. The oversaturation reflects in part the presence of Al bearing colloids as indicated by (1) [Al] being correlated with components associated with both lithogenic (Fe, Ti and lanthanides) colloids and organic carbon, (2) baseflow studies using cross-flow ultrafiltration and (3) comparison of our data with Acid Waters Monitoring Network (AWMN) information on labile and non-labile Al. Tree harvesting and emission reductions of SO(x) in acidic and acid sensitive catchments in mid-Wales led to acidification reversal, lower [Al] and changing [H(+)] - [Al] relationships. The [Al] decline was confined to acidic conditions while [Al] increased during the later part of the monitoring period with a peak around 2002 for moorland and forested systems. Colloidal production across the flow range was indicated late in the record by comparison of our data with information collected by the AWMN for a site in mid-Wales. This production seems interlinked with organic carbon and with dissolved CO(2) changes. In order for further understanding of Al hydrogeochemistry in river systems there is a need to integrate research that moves from equilibrium to kinetic and colloidal consideration including the critical issues of organic and inorganic controls within the context of bioavailability and aquatic stress. The colloidal Al may well be of low environmental concern to fish and other factors such as habitat may well be critical.     

Polycyclic aromatic hydrocarbons study and toxic equivalency factor (TEFs) in Tehran, IRAN

Polycyclic aromatic hydrocarbons (PAHs) are toxic pollutants released by various urban combustion sources. Benzo[a]pyrene (BaP) is a representative member of the class of PAHs. Health risk assessment associated with inhalatory PAHs uptake is often estimated on the basis of the BaP concentrations in air. Atmospheric particulate PAHs concentrations were measured at five locations in Tehran, Iran. Sixteen PAHs were extracted from the airborne particles and analyzed by HPLC. Total PAHs concentrations (16 compounds) at five station Arjanteen, Enghelab, Azadi, Bahman, Haft Houz were respectively, 70.2, 96.5, 130, 79.1, 44.1 ng/m(3). The information obtain from the present study indicated that mean of human carcinogens are: benzo[a]antheracene (0.17-4.76 ng/m(3)), chrysene (1.74-3.62 ng/m(3)), benzo[b]fluoranthene (0-5.25 ng/m(3)), benzo[k]fluoranthene (0.32-1.72 ng/m(3)), benzo[a]pyrene (1.41-3.82 ng/m(3)), dibenzo[a,h]anthracene (0.33-2.13 ng/m(3)), and indeno[1,2,3-cd]pyrene (0.25-11.08 ng/m(3)). The development and the establishment of a toxicity equivalency factor (TEF) are used in the assessment of mixtures containing PAHs. The contribution of the carcinogenic potency of BaP alone is in the range of 49.6-76.3% of the total carcinogenic activity. The annual number of lung cancer cases (persons per million) among Tehran residents (population = 10 millions) attributable to these carcinogenic PAHs compounds in 2005 was estimated at 58 persons per million. In Tehran urban areas vehicular emission are the primary contributor to PAHs concentrations, with additional local contributors like industrials emissions.     

Fertigation effect of distillery effluent on agronomical practices of Trigonella foenum-graecum L. (Fenugreek)

The fertigation effect of distillery effluents concentrations such as 5%, 10%, 25%, 50%, 75% and 100% were studied on Trigonella foenu-graecu (Pusa early bunching) along with control (bore well water). On irrigation of soil with different effluents up to 90 days of harvesting, it was observed that there was a significant effect on moisture content (P < 0.001), EC, pH, Cl⁻, total organic carbon (TOC), HCO₃^-_{3}^{-}, CO₃^-2_{3}^{-2}, Na⁺, K⁺, Ca^2 +, Mg^2 +, Fe^2 +, TKN, NO₃^2-_{3}^{2-}, PO₄^3-_{4}^{3-}, and SO₄^2-_{4}^{2-} (P < 0.0001) and insignificant effect on WHC and bulk density (P > 0.05).There was no significant change in the soil texture of the soil. Among various concentrations of effluent irrigation, the irrigation with 100% effluent concentration decreased pH (16.66%) and increased moisture content (30.82%), EC(84.13%), Cl⁻ (292.37%), TOC (4311.61%), HCO₃^-_{3}^{-} (27.76%), CO₃^-2_{3}^{-2} (32.63%), Na⁺ (273%), K⁺ (31.59%), Ca^2 + (729.76%), Mg^2 + (740.47%), TKN (1723.32%), NO₃^2-_{3}^{2-} (98.02%), PO₄^3-_{4}^{3-} (337.79%), and SO₄^2-_{4}^{2-} (77.78%), Fe^2 + (359.91%), Zn (980.48%), Cu (451.51%), Cd (3033.33%), Pb (2350.00%), and Cr (2375.00%) in the soil. The agronomical parameters such as shoot length, root length, number of leaves, flowers, pods, dry weight, chlorophyll content, LAI, crop yield, and HI of T. foenum-graecum were recorded to be in increasing order at low concentration of the effluent, i.e., from 5% to 50% and in decreasing order at higher effluent concentration, i.e., from 75% to 100% as compared to control. The enrichment factor of various heavy metals was ordered for soil Cd>Cr> Pb>Zn>Cu>Fe and for T. foenum-graecum plants Pb>Cr>Cd>Cu>Zn>Fe after irrigation with distillery effluent.