自动酸化吹气预处理测定水中硫化物

采用DCS-S8型硫化物自动酸化吹气仪,以GB/T 16489—1996《水质硫化物的测定亚甲基蓝分光光度法》为依据,建立了水质硫化物自动酸化吹气预处理方法.通过对加酸量和时间间隔、加热温度、氮气流量和吹气时间等参数的优选实验,获得水质硫化物测定的最佳预处理条件,用亚甲基蓝分光光度法检测样品.实验结果表明,实际样品加标...     

快速溶剂萃取-水浴氮吹-高效液相色谱法检测土壤16种多环芳烃

建立了快速溶剂萃取-水浴氮吹-高效液相色谱法检测土壤样品中16种多环芳烃(PAHs)的方法。分别对比了快速溶剂萃取与索式抽提、旋转蒸发浓缩与水浴氮吹浓缩、硅酸镁固相萃取柱与硅胶固相萃取柱净化的预处理效果,经实验对比后,确认优化预处理条件为：快速溶剂萃取温度120℃,静态萃取时间16 min,萃取次数两次,水浴氮吹浓缩,氮吹温度40℃,浓缩液经硅酸镁固相萃取柱净化。方法检出限和测定下限分别为0.21～0.47μg/kg和0.84～1.88μg/kg。在优化条件下,加标水平为0.5 mg/kg时,目标物加标回收率为72.66%～113.90%,替代物加标回收率为69.25%,108.63%,相对标准偏差(n=7)为0.69%～11.8%,适合实际土壤样品中PAHs的检测。     

离子色谱法测定土壤中残留的草甘膦

通过对前处理和色谱条件的优化,建立一种测定土壤中草甘膦的离子色谱分析方法。土壤样品采用20 mmol/L NaOH超声提取30 min,提取液经净化后,采用AS19色谱柱,35 mmol/L KOH等度洗脱,抑制型电导检测器检测。草甘膦在0.02～2.00 mg/L范围内线型关系良好,相关系数r为0.999 0,检出限为0.086 mg/kg。在低、中、高三种加标水平下,草甘膦的平均回收率分别为81.5%、86.3%和88.3%,重复测定相对标准偏差(RSD%)分别为6.49%、5.0%和2.24%。该方法操作简单,线性良好,可以准确地测定土壤中草甘膦的含量。     

提高水中氨氮测定精准度的研究

纳氏试剂光度法是污水中氨氮测定广泛采用的方法,文章通过实验分析讨论实验室环境、水样预处理、酒石酸钾钠和显色温度、显色时间、pH值等实验条件对氨氮测定精准度的影响。实验结果表明:改善实验室环境,在20²5℃、显色15min、显色后pH值为13的条件下,用滤膜代替滤纸,向酒石酸钾钠中加入NaOH煮沸浓缩定容能显著提高氨氮测定的精准度。     

钻井及油气田废水重金属检测干扰消除探讨

钻井废水和油气田采出废水成分复杂,在使用原子吸收分光光度法测定废水中重金属时,干扰严重。为获得准确可靠的检测数据,以硝酸、盐酸、高氯酸和氢氟酸综合消解法代替传统消解法,对废水进行预处理,试验所得回收率达90%以上,准确度达99%,质控样品100%合格。结果证明:此消解方法可行,可应用于钻井及油气田废水中重金属检测。     

火电行业脱硫废水除垢技术小试实验研究

本文以新疆某火力发电厂脱硫废水为研究对象,通过实验室软化预处理小试研究,为火电行业脱硫废水零排放提供理论支持和数据支撑。研究结果表明:在该火电厂脱硫废水软化预处理过程中沉淀剂(NaOH/Na_2CO_3)最佳投加顺序为先投加NaOH沉淀Mg~(2+),后加Na_2CO_3沉淀Ca~(2+);最佳投加量为n(NaOH)/n(Mg~(2+))=6:1, n(Na_2CO_3)/n(Ca~(2+))=1:1,该脱硫废水中Ca~(2+)/Mg~(2+)的去除率可以达到99%以上,脱硫废水硬度(以CaCO_3计)低于450 mg/L,为火电脱硫废水后续处理提供水质保证。     

废水预处理混凝沉淀实验分析

针对生物医药生产废水,通过添加氢氧化钠(NaOH)、聚合氯化铝(PAC)及聚丙烯酰胺(PAM)进行了混凝沉降实验.文章根据实验结果,确定了最佳pH值的范围、加药量、搅拌时间,并根据实验结果调整了污水处理站的运行参数,达到了高效、节约成本的预处理效果.     

亚甲基蓝分光光度法测定油泥中硫化物

参考水和废水硫化物测定标准,采用亚甲基蓝法测定油田污泥中硫化物含量,硫化物回收率仅为60%左右;而在阶梯式氮气吹扫条件下,60℃为最佳反应温度,样品量在5g以下时吹扫测定,回收率可达80%¹20%。采用1120%。采用1³g石油磺酸盐、3mL异丙醇对含油超过20%的油泥进行乳化预处理,比无预处理或萃取除油预处理时硫化物测定结果更准确;在乳化预处理及0.15mol/L抗坏血酸、EDTA保护下,含油20%以上油泥中硫化物回收率可达到80%以上。而含油20%以下油泥不需乳化预处理,经吹扫测定,回收率可以达到90%以上。通过实际样品平行试验及回收率测定,四次测定相对标准偏差3.34%,回收率在92%以上。该方法平行性好,结果准确,达到油泥硫化物测定质控要求。     

对氨基二甲基苯胺光度法测定水样中硫化物的几个问题

本文介绍用对氨基二甲基苯胺光度法测定水样中硫化物时，如何降低空白值、提高硫化钠标液的稳定度以及提高酸化吹气回收率的原理和方法。     

对氨基二甲基苯胺光度法测定硫化物中几个问题的试验研究

介绍了如何降低空白值、提高硫化纳溶液的稳定度以及提高酸化吹气回收率的原理和方法。     

Heavy metals extraction from contaminated soil: recovery of the flushing solution

The optimum conditions for the recovery of copper from a contaminated soil by using the soil flushing technique are evaluated. Tests on a soil artificially contaminated with copper chloride were carried out in order to evaluate the influence of the speed of percolation and of the chelating agent concentration (aqueous solution of an ethylendiaminotetraacetic acid di-sodium salt Na2-EDTA). At pH=7.3 an efficiency up to 93.9% for copper extraction was achieved by flushing 500 ml of Na2-EDTA 0.05 M solution and 100 ml of pure water at 0.792 cm/h. At these operating conditions the formation of EDTA complexes with other competitive cations (calcium and iron) was negligible. The experimental results were in agreement with the ones obtained using a model describing the chemistry of metal extraction. This model assessed that above pH=6 the formation of calcium and iron EDTA complexes was excluded and only the chelation of copper was allowed. The recovery of 91.6% of EDTA was also achieved by evaporating and acidifying the extracted solution: after filtration, solid EDTA was obtained, through the addition of sodium hydroxide Na2-EDTA. About 99.5% of the extracted copper was finally precipitated under alkaline conditions from the liquid phase.     

Optimizing phosphorus characterization in animal manures by solution phosphorus-31 nuclear magnetic resonance spectroscopy

A procedure involving alkaline extraction and solution 31P nuclear magnetic resonance (NMR) spectroscopy was developed and optimized for the characterization of P in animal manures (broiler, swine, beef cattle). Inclusion of ethylenediaminetetraacetic acid (EDTA) in the alkaline extraction solution recovered between 82 and 97% of the total P from the three manures, which represented a significant improvement on recovery in NaOH alone. Low concentrations of paramagnetic ions in all manure extracts meant that relatively long delay times (> 5 s) were required for quantitative analysis by solution 31P NMR spectroscopy. The manures contained inorganic orthophosphate, orthophosphate monoesters, orthophosphate diesters, and inorganic polyphosphates, but results were markedly influenced by the concentration of NaOH in the extractant, which affected both spectral resolution and the apparent P composition of the extracts. For example, extraction of swine manure and broiler litter with 0.5 M NaOH + 50 mM EDTA produced remarkable spectral resolution that allowed accurate quantification of the four signals from phytic acid, the major organic P compound in these manures. In contrast, more dilute NaOH concentrations produced considerable line broadening that obscured individual signals in the orthophosphate monoester region of the spectra. Spectral resolution of cattle manure extracts was relatively unaffected by NaOH concentration. Improvements in spectral resolution of more concentrated NaOH extracts were, however, compromised by the disappearance of phospholipids and inorganic polyphosphates, notably in swine and cattle manure extracts, which indicated either degradation or a change in solubility. The optimum extraction conditions will therefore vary depending on the manure type and the objectives of the study. Phytic acid can be accurately quantified in swine manure and broiler litter by extraction with 0.5 M NaOH + 50 mM EDTA, while a more dilute NaOH concentration should be used for complete P characterization or comparison among different manure types.     

Caution needed in pretreatment of sediments for refining phosphorus-31 nuclear magnetic resonance analysis: results from a comprehensive assessment of pretreatment with ethylenediaminetetraacetic acid

Pretreatment with chemicals such as ethylenediaminetetraacetic acid (EDTA) is often used to improve the analysis of sediment P with solution P-31 nuclear magnetic resonance spectroscopy (35P-NMR), but there is a lack of a comprehensive assessment of the methodology. In this study, the effects of EDTA pretreatment on sediment P extracted using a mixture of 0.25 mol L(-1) NaOH and 50 mmol L(-1) EDTA (NaOH-EDTA) were examined with 45 different sediments. The results showed that EDTA pre-extraction decreased the amount of P extracted by NaOH-EDTA when the concentration ratio of sediment Ca to the sum of sediment Fe and Al [Ca/(Fe+Al), on a wt/vol basis] was lower than 0.4. An increase in total extracted P, coupled with substantial increases in total extracted paramagnetic ions such as Fe and Mn, was observed for another group of sediments with Ca/(Fe+Al) > 0.5, possibly due to the matrix effect. Analysis of 16 representative sediments with 31P-NMR showed that orthophosphate diesters were substantially removed by EDTA pre-extraction for sediments with Ca/ (Fe+Al) between 0.4 and 0.7, reflecting a high risk posed by this pretreatment. Phosphorus diversity and concentration of individual P compounds were markedly improved for sediments with Ca/(Fe+Al) > 0.7, suggesting that EDTA pretreatment was particularly useful for 31P-NMR analysis of calcareous sediments. The present study showed that sediment properties played an important role in determining pretreatment effects. Caution is advised when applying pretreatment methods to different sediments.     

Soil and litter phosphorus-31 nuclear magnetic resonance spectroscopy: extractants, metals, and phosphorus relaxation times

Phosphorus-31 nuclear magnetic resonance (NMR) spectroscopy is an excellent tool with which to study soil organic P, allowing quantitative, comparative analysis of P forms. However, for 31P NMR to be tative, all peaks must be completely visible, and in their correct relative proportions. There must be no line broadening, and adequate delay times must be used to avoid saturation of peaks. The objective of this study was to examine the effects of extractants on delay times and peak saturation. Two samples (a forest litter and a mineral soil sample) and three extractants (0.25 M NaOH, NaOH plus Chelex (Bio-Rad Laboratories, Hercules, CA), and NaOH plus EDTA) were used to determine the differences in the concentration of P and cations solubilized by each extractant, and to measure spin-lattice (T1) relaxation times of P peaks in each extract. For both soil and litter, NaOH-Chelex extracted the lowest concentrations of P. For the litter sample, T1 values were short for all extractants due to the high Fe concentration remaining after extraction. For the soil sample, there were noticeable differences among the extractants. The NaOH-Chelex sample had less Fe and Mn remaining in solution after extraction than the other extractants, and the longest delay times used in the study, 6.4 s, were not long enough for quantitative analysis. Delay times of 1.5 to 2 s for the NaOH and NaOH-EDTA were adequate. Line broadening was highest in the NaOH extracts, which had the highest concentration of Fe. On the basis of these results, recommendations for future analyses of soil and litter samples by solution 31P NMR spectroscopy include: careful selection of an extractant; measurement of paramagnetic ions extracted with P; use of appropriate delay times and the minimum number of scans; and measurement of T1 values whenever possible.     

土壤中半挥发性有机物前处理方法的比较研究

现阶段索氏萃取法、超声波萃取法、微波辅助萃取法和加压流体萃取法是主流的土壤样品前处理技术,每种方法有着各自的特点。以多环芳烃和有机氯农药为目标化合物,通过研究每种萃取方法的萃取效率,进行横向比较研究后发现,索氏萃取法的萃取效率较高,但是自动化程度不高;而加速溶剂萃取法和微波辅助萃取法在保证了样品萃取效率的前提下,具有节省溶剂、自动化程度高等特点,特别适合于大批量样品的前处理工作。     

土壤中有机磷农药的测定及光催化降解的研究

本文以建立加速溶剂萃取-固相萃取小柱净化-气相色谱法测定土壤中有机磷农药的方法及其光降解为主要研究目的。通过条件优化摸索出更为优越的土壤有机磷农药前处理方法,利用高灵敏度、高选择性的FPD检测器进行定性、定量分析。使用溶胶凝胶法自制纳米二氧化钛粉体,讨论土壤中乐果光催化降解的影响因素。研究结果显示硅胶小柱的净化效果好;敌敌畏由于本身的性质,回收只有30%左右。催化剂剂量、反应时间、光照强度对乐果的光催化降解均有较大的影响。     

油污土壤呼吸作用强度的测定

通过土壤呼吸作用强度可以考察油污染物被微生物降解的情况,因此进行了土壤呼吸作用强度测定方法的研究。方法原理是用ＮａＯＨ溶液吸收土壤呼吸释放出的ＣＯ２,然后再用酸滴定剩余的ＮａＯＨ,从而计算出ＣＯ２释放量。测定结果说明添加菌和营养物的油污土壤呼吸作用强、释放的ＣＯ２量大、油降解量大。     

混合酸消解变化对土壤和沉积物中痕量硒分析影响

基于各3种采集环境样本、国家标准物质的土壤和沉积物,以当前环境监测行业常用的3种消解方法,探讨20种混合酸系统条件在消解条件变化中对复杂样本硒元素测定的影响.确定了最佳土壤和沉积物消解的组合为王水系统(盐酸∶硝酸∶氢氟酸∶过氧化氢∶高氯酸=3∶1∶1∶1∶1),各消解法的处理结果部分(n=5):水浴法消解时间仅需0.5...     

A washing procedure to mobilize mixed contaminants from soil: II. Heavy metals

We conducted a laboratory study to assess the efficiency of nonionic and anionic surfactants in combination with a sparing quantity of ethylenediaminetetraacetate (EDTA) to simultaneously extract heavy metals (HMs) and polychlorinated biphenyl (PCB) compounds from a field-contaminated soil. A soil wash that mobilized both HMs and PCBs was combined with back-extraction with hexane to remove PCBs from the aqueous wash. The aqueous washing suspension was then regenerated by precipitation of the HMs induced by corrosion and hydrolysis of zero-valent Mg to provide a cleaned soil and innocuous extract. Finally, the washing suspension was recycled twice to mobilize more contaminants from the soil particulate fraction. After ultrasonic equilibration, EDTA in admixture with a nonionic surfactant did not appreciably change the efficiency of mobilization of most heavy metals (Al, Cd, Cr, Fe Mn, Ni, and Zn), but did increase the recovery of Cu and Pb. The release of EDTA from HM complexes was efficient for most metals (99%) but was influenced by the chemical characteristics of the surfactant. The EDTA recovery (62-65%) after three cycles of soil washing, hexane back-extraction, and Mg(0) treatment was similar for all reagent combinations. In toto, these studies demonstrate that after treatment with ultrasound, selected heavy metals can be coextracted efficiently from soil with a single washing suspension containing EDTA and a nonionic surfactant.     

Comparison of phosphorus forms in wet and dried animal manures by solution phosphorus-31 nuclear magnetic resonance spectroscopy and enzymatic hydrolysis

Both enzymatic hydrolysis and solution (31)P nuclear magnetic resonance (NMR) spectroscopy have been used to characterize P compounds in animal manures. In this study, we comparatively investigated P forms in 0.25 M NaOH/0.05 M EDTA extracts of dairy and poultry manures by the two methods. For the dairy manure, enzymatic hydrolysis revealed that the majority of extracted P was inorganic P (56%), with 10% phytate-like P, 9% simple monoester P, 6% polynucleotide-like P, and 18% non-hydrolyzable P. Similar results were obtained by NMR spectroscopy, which showed that inorganic P was the major P fraction (64-73%), followed by 6% phytic acid, 14 to 22% other monoesters, and 7% phosphodiesters. In the poultry manure, enzymatic hydrolysis showed that inorganic P was the largest fraction (71%), followed by 15% phytate-like P and 1% other monoesters, and 3% polynucleotide-like P. NMR spectroscopy revealed that orthophosphate was 51 to 63% of extracted P, phytic acid 24 to 33%, other phosphomonoesters 6 to 12%, and phospholipids and DNA 2% each. Drying process increased orthophosphate (8.4% of total P) in dairy manure, but decreased orthophosphate (13.3% of total P) in poultry manure, suggesting that drying treatment caused the hydrolysis of some organic P to orthophosphate in dairy manure, but less recovery of orthophosphate in poultry manure. Comparison of these data indicates that the distribution patterns of major P forms in animal manure determined by the two methods were similar. Researchers can utilize the method that best fits their specific research goals or use both methods to obtain a full spectrum of manure P characterization.