Determination of total organic halogen (TOX) in humic acids after microwave-induced combustion

Chemically chlorinated organic matter as well as natural background humic acids contain significant amounts of organically bound halogens that must be determined for assessment of environmental pollution. In this work the use of ion chromatography (IC) and inductively coupled plasma mass spectrometry (ICP-MS) is proposed for the determination of total organic Cl, Br and I concentration in humic acids extracted from various forest soil horizons after a single digestion by microwave-induced combustion (MIC). Samples were pressed as pellets and combusted using 20 bar of oxygen and ammonium nitrate solution as igniter. Analytes were absorbed in diluted alkaline solution (50 mM (NH₄)₂CO₃) and a reflux step was applied after combustion to improve analyte recoveries (5 min, microwave power of 1400 W). The accuracy was evaluated using certified reference materials (CRM) and spiked samples. Using MIC the agreement with CRM values and spike recoveries was higher than 97% for all analytes. As an advantage over conventional procedures, using MIC it was possible to digest up to eight samples in only 25 min, obtaining a single solution suitable for all halogens determination in humic acids samples by different techniques (IC and ICP-MS). The limit of detection (3σ) for Cl, Br and I obtained by IC was 1.2, 2.5 and 4.3 μg g⁻¹ and by ICP-MS it was 1.4, 0.03 and 0.002 μg g⁻¹, respectively.     

Chelating resin immobilized sawdust packed chromatographic column: Application to separation and preconcentration of lead ion

Naturally abundant rubber sawdust has been utilized as a stationary support, which after immobilization with a chelating polyelectrolyte (xylenol orange as counterion) gets converted into a suitable column packing material for isolation and enrichment of trace level target analyte, accurately detectable by the technique of differential pulse anodic stripping voltammetry. The sorbent is robust and re-usable in column-chromatography without showing any leaching and interference complications. Its unique lead ion selectivity from multielemental complex matrices (synthetic water sample, blood serum) at optimized column conditions (pH 2.5 and flow rate 0.5?mL?min^?1) mitigates the usual problems of intermetallic and readsorption effects. Effects of flow rate, pH, equilibration time, and other variables are reported. The system has advantageous feature to be used in a single-column ion chromatography with satisfactory performance. A modest attempt has been made to determine lead fractions in human blood serum samples on the bases of selective retention of ionic and labile fractions on complexing resin.     

固相萃取气相色谱法测定水中15种硝基苯类化合物

使用Oasis HLB固相萃取柱,以正己烷/丙酮混合溶剂(体积比为3∶1)为洗脱溶剂,采用毛细管柱气相色谱电子捕获检测器同时测定水中15种硝基苯类化合物,以保留时间定性,外标标准曲线法定量。硝基苯和硝基甲苯在50.0μg/L～1 000μg/L、其他硝基苯类化合物在5.00μg/L～100μg/L范围内线性良好,检出限硝基苯和硝基甲苯为0.035μg/L～0.052μg/L,其他硝基苯类化合物为0.003 5μg/L～0.005 6μg/L,加标水样平行测定的RSD为1.4%～4.0%,平均回收率为92%～100%。     

地表水中SVOCs和氨基甲酸酯类农药同步萃取技术的探讨

采用大体积固相萃取富集地表水中SVOCs和氨基甲酸酯类农药,再以气相色谱-质谱和超高效液相色谱-串联质谱联用对目标物定性定量。通过优化固相萃取条件,使SVOCs在0.500 mg/L~10.0 mg/L之间,氨基甲酸酯类农药在1.00μg/L~100μg/L之间线性良好,方法检出限为0.002μg/L~0.009μg/L,加标回收率分别为70.5%~105%和78.5%~124%。用该方法测定某流域地表水,结果邻苯二甲酸酯类物质、多环芳烃类、酚类、硝基苯环类化合物等SVOCs,以及克百威、仲丁威等氨基甲酸酯类农药检出。     

磷钼杂多化合物脱硫体系脱硫特性与再生规律

以液相氧化脱硫工艺开发为目的,采用尾气H₂S浓度动态监测法研究了磷钼杂多化合物脱硫体系的脱硫特性;采用氧化还原电位监测法研究了该体系的再生规律结果表明,磷钼酸钠（NaHPA）体系的脱硫性能随温度升高而有所降低,随进气H₂S浓度的提高而相应降低,随吸收剂浓度的提高而显著增强．几种主要因素对磷钼酸钠脱硫体系再生过程的影响规律为吸收剂浓度提高再生时间缩短;温度升高再生时间缩短温度超过 50℃冉生时间缩短幅度趋缓;增大空气流最冉生时间缩短,空气流量超过1.650Lmmin冉生时间趋于恒定：进气 H₂S浓度提高冉生时间延长．NaHPA复配体系的再生性能较单一的NaHPA为优,偏钒酸钠对体系的再生有催化作用     

半挥发性有机物GC/MS分析方法研究

用气相色谱／质谱（ＧＣ／ＭＳ）研究分析了环境中的半挥发性有机标准物。以十氟三苯基磷作调机物,对ＧＣ／ＭＳ仪器系统进行了调整,离子丰度值符合美国环保局（Ｕ．Ｓ．ＥＰＡ）１９８６年推荐的离子丰度标准。测定了３２种目标化合物的保留时间及相对保留因子ＲＦ值,结果表明除五氯苯酚不达标外,其余化合物的ＲＦ值均符合要求,３１种目标化合物的加标回收率为２１％～９７％,相对标准偏差为３．１％～２４．１％,符合美国环保局８２７０方法质量控制检验标准。最后对建立定量校正库与ＧＣ／ＭＳ分析进行了讨论     

基于超声透射特性的密闭容器液位测量与装置设计*

针对金属密闭容器内液体液位测量问题,设计1种基于超声透射特性的非接触式液位测量装置。测量装置根据被测容器内液体介质与气体介质透射系数不同的原理,通过超声接收探头回波情况判断容器内液体位置,利用软件与硬件结合,调整超声发射探头与接收探头的放大倍数,实现对不同材料、厚度容器内液位的测量。测量装置可以将所测液位、容器倾斜程度等数据通过上位机、阿里云平台等多方位显示。研究结果表明:该测量装置可测量不同材料、厚度密闭容器内承装液体的液位,所测数据较为稳定,测量误差范围不大于3 mm。     

固相萃取富集高压液相色谱分析饮用水中的苯并(a)

本文以高压液相色谱仪作为样品分析手段,对Ｃ１８键合相吸附剂富集饮用水中苯并（ａ）芘回收效率的影响因素逐一进行系统研究。实验结果显示,在优化的样品富集和样品分析条件下,该方法具有快速、安全、高效和低耗等优点,在绝对进样量００２５～０３ｍｇ之间,线性良好,方法最低检出限为０５ｎｇ／Ｌ,同时准确度和精密度也得到很好地控制。另外,该方法在自来水及其源水的样品分析中获得了良好的结果。     

混合液回流比对多点进水新型A/O/A/A/O泥膜耦合工艺脱氮除磷的影响

针对中国南方城镇低碳氮比(低C/N)生活污水的脱氮除磷问题,开发并设计了新型多点进水A1/O2/A3/A4/O5泥膜耦合工艺及中试装置.在进水点1和进水点2的进水流量比为4:6的条件下,通过改变混合液回流比,研究了其对系统中有机物、氮、磷的去除影响及氮素的转化规律.结果表明:当平均进水低C/N比为2.09,混合液回流比...     

离子色谱法测定水中无机阴离子水样的预处理

本文介绍了用离子色谱法测定无机阴离子，对污染严重的水样通常采用预处理柱法。论述了预处理柱的制备、再生，测定了预处理柱对重金属及有机物的去除率及无机阴离子的回收率。