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1.
张宗祥  陈军 《江苏地质》2010,34(2):206-208
采用高效液相色谱法测定鱼组织中孔雀石绿的残留量.样品经高速均质后,用乙腈提取,合并提取液,用二氯甲烷再次萃取,有机相浓缩后过酸性氧化铝和PRS复合小柱洗脱,用乙腈定容.以乙腈-乙酸盐缓冲溶液为流动相,高效液相色谱分离,用荧光检测器检测,外标法定量.其检出限为0.75μg/kg,加标回收率为84.0%~90.1%,相对标准偏差RSD为2.98%~6.21%.  相似文献   

2.
研究了液液萃取-反相高效液相色谱法分离测定水中苯并[a]芘的方法。采用Eclipse XDB-C18色谱柱;流动相为甲醇:水=85∶15;荧光检测器激发波长Ex=266nm,发射波长Em=412nm的条件进行分析。方法检出限为0.001μg/L,加标回收率为94.4%~101%,相对标准偏差(RSD)(n=7)为2.6%。  相似文献   

3.
盛东  王美飞  练鸿振 《岩矿测试》2009,28(5):407-410
建立了高效液相色谱-紫外光谱法测定聚氨酯扩链剂氢醌-双(β-羟乙基)醚(HQEE)工业品中HQEE主含量和对苯二酚残留的方法。在氰基柱上,以甲醇-水-1%乙酸溶液(体积比10∶50∶40)为流动相,流速1.0 mL/min时,HQEE、对苯二酚及其他相关杂质得到良好分离,紫外光谱285 nm检测。方法简便、快捷,结果准确可靠,在工业生产中可有效地指导HQEE合成过程的质量控制。  相似文献   

4.
建立了高温燃烧水解-离子色谱测定植物样品中不同含量范围氟的分析方法,色谱条件为Dionex IonPacAS18分离柱(4 mm×250 mm),Dionex IonPac AG18保护柱(4 mm×50 mm),ASRS ULTRAⅡ自动再生微膜抑制器,电导检测器。采用纯水作为吸收介质,使样品溶液与标准溶液基体一致,过滤后可直接测定。样品溶液中常见的Cl-、NO3-、SO24-、PO43-、CO23-、HCO3-等阴离子不干扰F-的测定。为消除样品热解过程中产生的乙酸干扰,对氟含量较高(xx~xxxμg/g)的样品,采用20 mmol/L的NaOH淋洗液等度淋洗,进样体积为25μL;对氟含量较低的样品(0.x~xμg/g),进样体积为100μL。方法具有较宽的线性范围和较好的稳定性,检出限为0.5 mg/kg,适用于痕量分析;应用于灌木枝叶和茶叶等4个氟含量较高(xx~xxxμg/g)的植物标准物质的测定,相对标准偏差(RSD)<6%(n=6);应用于低氟的小麦粉和大米粉样品测定,加标回收率为90%~110%,可以满足不同氟含量植物样品中氟测定的需要,具有自动化程度高、操作简单、对环境友好等特点。  相似文献   

5.
曹攽  马军  李云木子 《岩矿测试》2010,29(5):539-542
应用荧光-紫外检测器联用的高效液相色谱法分析地下水中16种多环芳烃。对高效液相色谱条件进行优化,建立了分析方法,并用于实际水样分析。在较佳的实验条件下,加标回收率为86.3%~105%,方法精密度(RSD,n=7)为0.39%~2.55%,检出限为0.001~0.010μg/L。分析16种PAHs仅用20min,比EPA8310方法中采用的液相色谱法缩短了17min。方法灵简便、准确,灵敏度高,分析时间短,适用于大批量地下水中痕量多环芳烃的分析。  相似文献   

6.
薛佳 《福建地质》2012,31(4):358-367
采用超声提取,固相小柱净化,高效液相色谱-荧光-紫外二极管阵列检测器串联的方法测定水、土壤、植物中16种多环芳烃含量。用正交法优化了固相萃取条件,并通过选择最佳荧光激发和发射光谱波长提高了荧光检测的灵敏度。仪器检出限0.02~8.15ug/L,方法精密度1.38%~7.59%,线性范围0.2~300ug/L,相关系数>0.999 1,样品加标回收率75.1%~96.3%。  相似文献   

7.
复方化学消毒剂中苯扎氯铵的高效液相色谱测定   总被引:1,自引:0,他引:1  
建立了一种测定复方化学消毒剂中苯扎氯铵成分十二烷基二甲基苄基氯化铵、十四烷基二甲基苄基氯化铵和十六烷基二甲基苄基氯化铵的反相离子对高效液相色谱法。色谱柱为Platisil ODS(5μm,250 mm×4.6mm),流动相为甲醇-0.2 mol/L己烷磺酸钠(含1%三乙胺,V/V,用高氯酸调节至pH=6.0,体积比85∶15),紫外220 nm检测。用己烷磺酸钠作为离子对试剂,增强了苯扎氯铵成分的保留,三乙胺作为扫尾剂,通过抑制固定相表面残存的硅羟基对苯扎氯铵成分的吸附,减少了色谱峰拖尾。3种苯扎氯铵成分分离良好,标准曲线的线性范围分别为0.002~5 mg/mL、0.005~10 mg/mL和0.005~10 mg/mL,检测限分别为0.0005 mg/mL、0.001mg/mL和0.001 mg/mL。方法具有良好的准确度和精密度,在测定低浓度样品时优势明显。实际用于测定苯扎氯铵消毒液和医用消毒纸巾中3种苯扎氯铵成分的含量,回收率为99.3%~104.1%,日内和日间测定相对标准偏差(RSD)均小于2.0%。  相似文献   

8.
杨红霞  刘崴  李冰 《岩矿测试》2008,27(6):405-408
建立了碱消解-高效液相色谱-电感耦合等离子体质谱联用系统测定生物样品中甲基汞(MeHg)与乙基汞(EtHg)的分析方法。为提高灵敏度,选用微流量的PFA雾化器,在优化的检测条件下,MeHg及EtHg检出限可达到0.036μg/L和0.03μg/L;线性范围达到4个数量级,两条工作曲线线性相关系数为1。对1.78μg/L MeHg、1.65μg/L EtHg的混合标准溶液重复测定7次,色谱峰面积的相对标准偏差(RSD)分别为1.79%和1.44%。对标准物质BCR 464(金枪鱼)的分析结果表明,测定值与标准值基本吻合,但略低于标准值;甲基汞和乙基汞的加标回收率分别为85.9%和84.5%。高效液相色谱与质谱联用技术的高灵敏度和低检出限能够满足生物样品中汞形态定量分析的要求。  相似文献   

9.
熊文明  张志军 《岩矿测试》2011,30(6):768-771
玻璃样品中加入氢氧化钠,在700℃马弗炉中加热熔融,热水浸提,所得溶液通过OnGuardⅡAg/H柱后上机测定,消除加入的氯和碱的干扰,再经IonPac AG14柱和AS14柱分离,采用小体积的定量环直接进样,离子色谱法测定氟离子和硫酸根的含量。氟离子和硫酸根的线性范围分别为0.1~2μg/mL和0.5~20μg/mL,方法检出限氟为2.0 mg/kg和硫为1.0 mg/kg,测定结果的相对标准偏差(RSD)小于5.0%。实际玻璃样品用离子色谱法和化学法测定,两种分析方法的结果无显著性差异。  相似文献   

10.
研究建立了超高效液相色谱电喷雾串联质谱法(UPLC/MS/MS)测定土壤中四环素(TC)、土霉素(OTC)、金霉素(CTC)、多西环素(DC)4种四环素类抗生素(TCs)及5种降解产物的残留分析方法。采用乙腈与EDTA-Mcllvaine缓冲液混合提取土壤样品中TCs,净化采用HLB固相萃取小柱,电离方式为ESI(+),定量方法为多反应监测(MRM)模式。在0.001~0.5 mg/kg范围内, 4种四环素类抗生素及其降解产物的峰面积与质量浓度的线性关系良好( R2>0.99)。仪器检出限为1.085~15.780 μg/kg,方法的定量限为3.617~42.526 μg/kg。在3个添加水平 0.05、0.1和 0.5 mg/kg下,除脱水四环素和差向脱水四环素(其回收率<30%)外,其余四环素类抗生素及代谢产物在土壤中的添加回收率为62.1%~87.6%,相对标准偏差为2.35%~13.42%。该方法线性关系良好,灵敏度高,适用于土壤中四环素类抗生素及其降解产物的残留分析。  相似文献   

11.
Tubifex tubifex has been shown to survive in organic polluted environments, however, not much has been done on its inorganic pollution tolerance. Samples of T. tubifex and their respective sewage sludge were taken from Soche wastewater treatment plant in Blantyre City, Malawi during July 2007 to November 2008. The total number of sludge samples taken was fifty one which was made into seventeen composite samples. A total of seventeen T. Tubifex samples were also collected. The samples were analyzed for copper, lead, manganese, zinc and cadmium using standard methods from American Public Health Association and Association of Official Analytical Chemists. The concentrations of metals in sewage sludge and T. tubifex were on dry weight basis and the metals determined were acid extractable. In general, heavy metals concentration was lower in T. tubifex than in sewage sludge. The range of heavy metals concentrations were (in sludge and (T. tubifex)): zinc 275.3–361.5 mg/kg (45.0–82.2 mg/kg), manganese 293.7–230.1 mg/kg (1.21–3.69 mg/kg), copper 86.5–120.1 mg/kg (1.6–4.7 mg/kg), lead 11.2–22.4 mg/kg (Below detection limit–0.95 ) and cadmium 1.12–2.31 mg/kg (1.08–2.18 mg/kg). The results showed significant differences between the concentrations of manganese, copper, lead and zinc in sewage sludge and T. tubifex (p < 0.05). However there was no significant difference between the concentrations of cadmium in sewage sludge and T. tubifex (p > 0.05). T. tubifex did not show the ability to accumulate heavy metals (attributed to its high defecation and metabolic rate) except for cadmium hence cannot be used as a bioindicator for heavy metal pollution in sludge.  相似文献   

12.
A pot experiment was conducted to investigate the influence of elemental sulfur, gypsum and chelating agent (Ethylenediaminetetraacetic acid) on copper, zinc, nickel, cadmium, chromium and lead uptake by Brassica juncea from sewage sludge. Addition of sulphur acidified the sludge, which caused the pH decrease to 5.4 with an initial pH 6.7. The shoot and root biomass were increased with sulfur addition, while decreased with Ethylenediaminetetraacetic acid addition. Applications of Ethylenediaminetetraacetic acid and sulfur resulted in a considerable increase in copper and lead concentrations in the plant. The highest root concentration of copper obtained to be 110?mg/kg?dw at Ethylenediaminetetraacetic acid treatment. For sulfur treatment, lead concentrations in shoots indicated almost high concentrations 77?mg/kg, about twofold increases relative to roots (34?mg/kg). The Transportation Index of all studied metals were quite low (TI?<?0.5), whereas the Bioaccumulation Factor values were much higher, varied from 0.01 to 9.67. Furthermore, the plant showed better Bioaccumulation Factor for copper and lead metals in both shoot and root. The efficiency to remove copper and lead from sludge is high in this plant. As a result, elemental sulfur will be effective amendment for phytoextraction of heavy metals from sewage sludge.  相似文献   

13.
In this study, the characteristics of sewage of small community were determined for 6 months to ascertain the type of treatment required in subtropical conditions. The results demarcated sewage of this community as a medium-strength wastewater (chemical oxygen demand: 475 mg/L, biochemical oxygen demand: 240 mg/L and total suspended solids: 434 mg/L). Chemical oxygen demand to sulphate ratio of the sewage (11.6) established that it was amenable to anaerobic digestion. The temperature, strength, biodegradability and components of sewage were suitable for anaerobic digestion, and thus, upflow anaerobic sludge blanket reactor (UASB) was selected for its treatment. These reactors are often shutdown in small communities due to environmental and/or socio-economic factors. The ability of two UASB reactors, seeded with cow dung (UASBCD) and activated sludge of a dairy treatment plant (UASBASDIT) to restart after a long idle period of 12 months, was investigated along with sludge analysis by scanning electron microscope. Biomass in both reactors reactivated rapidly after shutdown period and within 30 days after substrate feeding achieved uniform removal efficiencies for chemical oxygen demand, total suspended solids, total dissolved solids, chloride and oil and grease. Chemical oxygen demand removal efficiency of both reactors became uniform and remained close to 80% after 30 days through reactivation of microbes in sludge bed due to adequate food and temperature conditions. During restart-up, at an average organic loading rate of 0.902 kg COD/m3 per day, methane yields of 0.091 and 0.084 m3/kg COD removed were achieved for UASBCD and UASBASDIT reactors, respectively.  相似文献   

14.
土壤和白菜中低分子量有机酸的气相色谱分析   总被引:4,自引:0,他引:4  
利用甲醇-硫酸混合液(体积比10∶7)对土壤和白菜中低分子量有机酸同时进行提取和甲酯化衍生,然后利用二氯甲烷液-液萃取,气相色谱法分析。土壤中7种低分子量有机酸(草酸、丙二酸、反丁烯二酸、琥珀酸、马来酸、L-苹果酸、柠檬酸)的添加回收率为81.93%~95.58%,白菜中的添加回收率为84.78%~106.99%,方法的检出限为0.72~4.14 mg/kg。方法用于测定根际、非根际土壤和白菜根系、茎叶中的低分子量有机酸,结果准确可靠。  相似文献   

15.
In Thailand, sewage sludge production from the Bangkok metropolitan area can reach up to 63,000 ton/y by 2010. The Beer-Thai Company, Thailand, produces beer and generates lots of sludge as waste. Sewage sludge and brewery sludge can be used to generate energy which could be saved on the fossil fuels conventionally used as a source of energy. The possibility was explored to mix brewery sludge with sewage sludge at different mixing ratios for anaerobic digestion so that the energy can be generated as biogas and at the same time, digested sewage sludge can be used as fertilizer for agricultural applications. A batch anaerobic reactor under mesophilic condition for a digestion period of 40 days was used in the laboratory. The acrylic reactor was cylindrical with a working weight of 12 kg. The diameter was 23.7 cm and the height was 34.5 cm. Sludge mixtures at different ratios were fed into the reactors and the optimum mixing ratio was determined. Experimental results showed that the sludge mixture at ratio of 25:75 % by weight (sewage:brewery) yielded higher biogas production. A reduction in heavy metals and pathogens was observed at this ratio after the digestion indicating its safe use as fertilizer. Nitrogen content was about 4.95 % which is well above the commercial fertilizers. At optimum mixing ratio of 25:75, the amount of the generated biogas is 1.15×106 m3/y. This large amount of biogas is equivalent to 1.44 million kWh/y of electricity, 561,000 L/y of diesel oil and 936,000 L/y of vehicle gasoline.  相似文献   

16.
Compacted sewage sludge as a barrier for tailing impoundment   总被引:1,自引:1,他引:0  
The feasibility of compacted sewage sludge serving as a barrier for tailing impoundment was evaluated by the batch test and hydraulic conductivity test with respect to heavy metal retardation and impermeability. The batch test results showed that the effective removal of heavy metals approached 97.8 and 93.4% for Zn and Cd, respectively. Formation of precipitation of oxy(hydroxide) and carbonate minerals was mainly responsible for the attenuation of heavy metals in the early period of the test. Nevertheless, the further removal of heavy metals can be attributed to the sulfate reduction. The hydraulic conductivity test indicated that almost all of the heavy metals contained in simulated acid pore water were retarded by compacted sewage sludge. The hydraulic conductivity of the compacted sewage sludge ranged from 3.0 × 10−8 to 8.0 × 10−8 cm s−1, lower than 1.0 × 10−7 cm s−1, which is required by regulations for the hydraulic barrier in landfill sites. Thus, this study suggested that compacted sewage sludge could be used as a bottom barrier for tailing impoundment.  相似文献   

17.
The adsorption and desorption behaviors of 17??-ethinylestradiol on various sludges derived from different treatment units of a sewage treatment plant were investigated using batch equilibration experiments. The results showed that adsorption process could be well described by pseudo-second-order kinetic model and fast adsorption played a main role. Adsorption ability varied as the order of aerobic sludge????anoxic sludge????primary sludge?>?sludge cake?>?anaerobic sludge. Adsorption/desorption isotherms were well fitted by the modified Freundlich model, and $ K_{f}^{\prime } $ values increased with the organic matter content. Thermodynamic analysis indicated that 17??-ethinylestradiol adsorption/desorption was exothermic and conducted spontaneously. After heat treatment for removing the organic carbon, $ K_{f}^{\prime } $ values decreased by more than 78%, but organic carbon normalized adsorption constant was 7.76?C29.51?mg/g. The 17??-ethinylestradiol adsorption capacity was found to decrease from 0.95?C1.39 to 0.44?C0.49?mg/g with sludge concentration increasing from 500 to 4,000?mg/L, being almost unchanged at pH 3?C10 and sharply decreasing with pH?>?10. The adsorption capacity was also found to fluctuate in the range of 2.0?C3.0?mg/g when Ca2+ concentration was <0.5?mol/L and increased rapidly above 0.5?mol/L. Addition of methanol and acetonitrile could improve 17??-ethinylestradiol desorption effect, which increased with the content of organic solvents, and the desorption degree of acetonitrile was higher than methanol.  相似文献   

18.
太仓郊区河流沉积物重金属污染现状及评价   总被引:4,自引:0,他引:4       下载免费PDF全文
选择太仓市郊区河流沉积物为研究对象,开展了重金属污染现状及评价研究。研究表明,相对于地壳或页岩平均值,沉积物中大部分重金属呈现不同程度的富集;地质累积指数和富集因子分析表明,位于城镇附近的采样点受到污染,且主要污染因子为Cr、Cu、Cd、Pb、Zn等。结果显示,沉积物Zn含量高达1770mg/kg,是农用污泥Zn使用容许最高值500mg/kg的3倍多,沉积物由于Zn、Cr、Cu等的严重污染不能用作施用污泥;利用重金属与Fe之间的相关特征结果显示,城镇工业、生活污水的排放是沉积物重金属污染的主要因素。  相似文献   

19.
The concentrations of some widely used pharmaceuticals, namely fluoroquinolones (ciprofloxacin C17 H18FN3O3, norfloxacin C17 H18FN3O3 and ofloxacin C18 H20FN3O4 and sulfonamides (sulfadimethoxine C12 H14N4O4s and sulfamethoxazole C10 H11N3O3S were determined in urban sewage sludge utilized for making compost. The levels of degradation of these pharmaceuticals resulting from sludge treatment were assessed. The concentrations of the studied pharmaceuticals sufficiently varied both in sewage sludge and in compost and due to this phenomenon the possible danger resulting from the presence of pharmaceuticals in sewage sludge, used for composting, can not be ignored. The concentrations of the studied pharmaceuticals were lower in compost, if compared to the relevant concentrations in sewage sludge. The highest pharmaceutical concentration in sewage sludge — 426 μg/kg — was detected in the case of ciprofloxacin. The highest concentrations present in compost were 22 μg/kg of norfloxacin and 20 μg/kg of ciprofloxacin. Results show that before using the sewage sludge for making compost or before using the compost a fertilizer for food plants, they should be carefully tested against the content of commonly used pharmaceuticals.  相似文献   

20.
连续流气提式流化床启动过程中好氧颗粒污泥的形成机制   总被引:4,自引:0,他引:4  
探讨连续流气提式好氧颗粒污泥流化床(CAFB)反应器的运行特征,对该工艺颗粒污泥形成过程、形成机理和颗粒性质进行分析。以市政污泥为接种污泥,以醋酸钠为碳源,在连续运行方式下培养好氧颗粒污泥。研究结果表明:CAFB反应器启动的第4-5天即有大量颗粒污泥形成,颗粒直径800~1 000 μm,比重1.006,生物相丰富,能够分泌大量胞外聚合物。当COD有机负荷高达8 和13 kg/(m3·d)时,对COD处理效率均维持在93%~97%,COD出水质量浓度仅为30~80 mg/L,引起启动后期丝状菌的大量繁殖,污泥流失。进一步提高污泥负荷有望控制污泥膨胀。  相似文献   

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