共查询到20条相似文献,搜索用时 62 毫秒
1.
超声波萃取-高效液相色谱法测定土壤中邻苯二甲酸酯 总被引:3,自引:0,他引:3
邻苯二甲酸酯类(PAEs)是环境激素类物质中的一类化合物。文章对土壤中6种被美国EPA列入"优先监测污染物名单"的PAEs类物质邻苯二甲酸二甲酯(DMP)、二乙酯(DEP)、二丁酯(DBP)、邻苯二甲酸二(2-乙基己基)酯(DEHP)、二辛酯(DOP)、丁基苄基酯(BBP)邻苯二甲酸酯经超声波萃取、柱层析净化后,采用高效液相色谱法测定。对影响加标回收率的实验条件如萃取溶剂比例、萃取时间和萃取溶剂的选择等进行优化。方法回收率为94.1%~108.2%,相对标准偏差(RSD,n=7)为0.70%~2.42%,方法检出限为0.003~0.009μg/g。建立的方法样品前处理简单、快速,溶剂用量少,液相色谱法分析6种PAEs类物质仅用10 min,适用于大批量土壤样品中PAEs类物质的测定。 相似文献
2.
气相色谱-质谱联用法测定土壤中邻苯二甲酸酯类增塑剂 总被引:4,自引:1,他引:4
应用加速溶剂萃取,气相色谱-质谱联用法测定土壤中6种邻苯二甲酸酯类有机污染物。对邻苯二甲酸酯类污染物的提取溶剂进行了优化选择,确定二氯甲烷作为最佳提取溶剂。对色谱柱升温程序进行了优化,以使两个出峰时间较接近的目标物邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)能够达到基线分离。方法标准曲线的线性范围为0.50~20.0mg/L,线性相关系数均大于0.9970,方法检出限为67μg/kg,加标回收率为81.9%~111.4%。方法检出限较低,精密度好,简便快速,可满足大批量样品分析对质量和进度的要求。 相似文献
3.
石油类物质是中国建设用地土壤污染风险管控的污染物之一,开展土壤中石油类物质的检测对土壤污染防治工作具有重要意义。本文采用正己烷为萃取溶剂,土壤经振荡提取后,以荧光光度法为检测手段,建立了一种绿色环保、灵敏高效的土壤石油类物质检测方法。通过对实验过程进行优化,该方法的线性相关系数r≥0.999,检出限为3mg/kg。使用10种不同类型土壤进行方法精密度和准确度验证,精密度为2.5%~9.2%,基体加标回收率为80.0%~110%。为验证方法可比性,分别使用本方法和《土壤 石油类的测定 红外分光光度法》(HJ 1051—2019)对5种不同类型土壤进行检测比对,测定结果相对偏差在5.0%~15%之间,具有较好的一致性。 相似文献
4.
建立了一套利用加速溶剂萃取仪在线净化,气相色谱氮磷检测器测定土壤中20种有机磷农药的方法。考察了加速溶剂萃取仪的萃取温度、氧化铝的类型和加入方式、溶剂萃取体系、分散剂用量等因素对土壤中有机磷农药残留测定的影响。合适的萃取温度在萃取效率和回收效率之间找到最佳平衡点,酸性氧化铝和底部加入方式保证了土壤的净化效果和有机磷的回收率,分散剂的加入使得土壤中有机磷分布更加均匀。以酸性氧化铝和石墨碳黑为净化剂,水为分散剂,土壤样品经加速溶剂萃取仪在线净化萃取,浓缩后采用气相色谱氮磷检测器检测。在萃取温度为60℃,酸性氧化铝底部加入,分散剂水为1.0 mL的条件下,20种有机磷的检出限为0.005~0.014 mg/L。本方法将萃取过程与净化过程合二为一,简化了操作步骤,提高了工作效率。 相似文献
5.
在线渗析-离子色谱法测定土壤中有效氟 总被引:1,自引:1,他引:0
土壤样品经超声波超声静置,提取上清液,经渗析进入色谱柱,采用Metrohm A Supp 4-250阴离子交换柱,以1.8 mmol/L碳酸钠-1.7 mmol/L碳酸氢钠混合溶液作为流动相,用在线渗析技术与离子色谱法联用测定土壤中的有效氟。与常规方法相比,建立的方法操作简单,避免了繁琐的样品前处理。加标回收率为90.5%~95.7%,精密度(RSD,n=6)为1.60%。该方法具有高效、快速、灵敏等特点,能够用于环境土壤样品中有效氟的检测。 相似文献
6.
7.
超声提取-气相色谱法测定覆盖区土壤中的六六六和滴滴涕 总被引:6,自引:2,他引:4
将超声波提取技术引入到覆盖区土壤样品六六六、滴滴涕组分的预处理中,建立了超声提取,磺化法净化,气相色谱测定的分析方法。对被测组分在超声波提取中的稳定性进行了试验,对超声提取时间、提取温度、提取溶剂用量以及磺化净化过程可能导致组分损失的各种相关条件逐个试验筛选,采用样品加标回收法对六六六、滴滴涕的8种组分进行了两种浓度的精密度和准确度试验,RSD值均小于10%,平均回收率92.5%-103.9%。方法对各种异构体的六六六、滴滴涕的最低检测浓度为0.30-3.89ng/g。 相似文献
8.
报告了利用填充玻璃柱,恒温气相色谱法,选用电子捕获检测器,简便、快速地分离测定土壤中八种有机氯农药残留量的实验条件及测定结果。 相似文献
9.
对土壤中14种有机氯农药的超声提取技术和磺化、固相萃取小柱两种净化方法进行系统研究。结果表明,超声提取节省提取时间,提高分析效率;磺化法和固相萃取小柱法都有净化作用,但磺化法使样品中的艾氏剂、狄氏剂和异狄氏剂全部损失;固相萃取小柱净化当丙酮-正己烷淋洗液体积比为1∶9、淋洗液收集8 mL时回收率>90%,干扰最小。方法检出限为0.63~2.59μg/kg,精密度(RSD,n=7)为1.17%~14.66%,基体加标平均回收率为82.78%~106.94%。方法用于生态地球化学调查评价批量土壤样品的实际分析,检测结果满足评价工作需要。 相似文献
10.
建立了气相色谱-质谱联用技术(GC-MS)测定罗氏海盘车中6种邻苯二甲酸酯类化合物(PAEs)的方法,采用丙酮-正己烷混合溶剂超声提取,通过中性氧化铝和弗罗里硅土填装层析柱净化样品,选用HP-5MS毛细色谱柱分离,选择离子监测模式(SIM)进行定性定量。该方法能同时分离测定罗氏海盘车中邻苯二甲酸二甲酯、邻苯二甲酸二乙酯、邻苯二甲酸二正丁酯、邻苯二甲酸丁基苄酯、邻苯二甲酸二(2-乙基己基)酯、邻苯二甲酸二正辛酯等6种邻苯二甲酸酯类化合物。在优化条件下,方法标准曲线的相关系数为0.9975~0.9996,回收率为80.30%~119.00%,精密度(RSD,n=7)为2.2%~5.7%,方法最低检出限为10.00 ng/g。运用建立的方法对罗氏海盘车样品进行分析,检测出罗氏海盘车中含有邻苯二甲酸二异丁酯、邻苯二甲酸二正丁酯、邻苯二甲酸二(2-乙基己基)酯3种污染物,3种污染物含量均低于欧盟的限量标准,同时远低于其他各类食品中的检出含量,样品中邻苯二甲酸二(2-乙基己基)酯平均含量偏高。本法具有高的选择性、灵敏度和准确度,适用于罗氏海盘车中痕量PAEs的测定,为保护海洋环境及海洋资源开发提供技术支持。 相似文献
11.
Biodegradation of phthalic acid esters in sewage sludge by composting with pig manure and rice straw
Jie Fu Fei Pan Shuang Song Li-Rong Zhang Yin Luo Wu Chen Ying Liang 《Environmental Earth Sciences》2013,68(8):2289-2299
To comparatively study the biodegradation of phthalic acid esters (PAEs) in sewage sludge by composting with pig manure or with rice straw, four composting modes were designed: Mode 1 (sewage sludge + pig manure + intermittent aeration), Mode 2 (sewage sludge + pig manure + continuous aeration), Mode 3 (sewage sludge + rice straw + intermittent aeration) and Mode 4 (sewage sludge + rice straw + continuous aeration). Physicochemical parameters of composts were measured according to standard methods and PAEs were analyzed by gas chromatography coupled with mass spectrometry (GC/MS). The biodegradation of each PAE was also discussed. The results showed that Mode 1 was the best mode to biodegrade PAEs, which might be related to the wide class of indigenous microbial communities in pig manure and high efficiency of intermittent ventilation for providing oxygen. During the biodegradation process, di(2-ethylhexyl) phthalate was the most abundant and decisive for the removal of total PAEs. It showed a first-order kinetic degradation model. In conclusion, composting with pig manure could be suggested as an effective detoxification process for the removal of PAEs from sewage sludge, providing a safe end product. 相似文献
13.
14.
15.
16.
Ultrasonic wave extraction and simultaneous analysis of polycyclic aromatic hydrocarbons (PAHs) and phthalic esters in soil 下载免费PDF全文
ZHANG Yong-tao ZHAO Guo-xing LIU Jing-shang ZHANG Li LI Xiao-ya GUI Jian-ye ZHANG Chen-ling 《地下水科学与工程》2017,5(3):249-253
A method is developed for detection of polycyclic aromatic hydrocarbons(PAHs) and Phthalic Acid Esters(PAEs) in soil samples. Ultrasonic Wave Extraction under airtight circumstances is adopted to extract the analytes in soil samples with n-hexane–acetone(V:V=1:1) as extraction solvent. This method has several advantages, including high extraction efficiency, short time, convenience and simplicity. It can be used to detect polycyclic aromatic hydrocarbons(PAHs) and Phthalic Acid Esters(PAEs) in soil. 相似文献
17.
18.
The bioavailability of metals and their potential for environmental pollution depends not simply on total concentrations but on their chemical form. Consequently, knowledge of aqueous metal speciation is essential in investigating potential metal toxicity and mobility. Dissolved (<1 kDa), colloidal (1 kDa–0.45 μm) and particulate (>0.45 μm) size fractions of sulfate, organic C (OC) and 18 metals/metalloids were investigated in the extremely acidic Vörå River system in Western Finland, which is strongly affected by acid sulfate (AS) soils. In addition, geochemical modelling was used to predict the formation of free ions and complexes in these acidic waters. The most important finding of this study is that the very large amounts of elements known to be released from AS soils (including Al, Ca, Cd, Co, Cu, Mg, Mn, Na, Ni, Si and U) occur and can prevail mainly in toxic forms throughout acidic river systems; as free ions and/or sulfate-complexes. This has serious effects on the biota and particularly dissolved Al can be expected to have acute effects on fish and other organisms. In the study area, only the relatively forested upstream area (higher pH and contents of OC) had significant amounts of a few bioavailable elements (including Al, Cu, Ni and U) due to complexation with the more abundantly occurring colloidal OC in the upstream area. It is, however, notable that some of the colloidal/particulate metals were most likely associated with metal bearing phyllosilicates eroded from clay soils. Moreover, the mobilisation of Fe and As was small and As was predicted to be associated with Fe oxides, indicating a considerable influence of Fe oxides on the mobilisation/immobilisation processes of As. Elements will ultimately be precipitated in the recipient estuary, where the acidic metal-rich river water will gradually be diluted/neutralised with brackish seawater in the Gulf of Bothnia. According to speciation modelling, such a pH rise may first cause precipitation of Al, Cu and U together with organic matters closest to the river mouth, in line with previous sediment studies from the estuary. 相似文献
19.
Ying Zi Cui Yu-Jun Duc Myriam Benahmed Nadia Bessaies-Bey Hela Chen Bo 《Acta Geotechnica》2021,16(4):1101-1111
Acta Geotechnica - Previous studies stated that, with increasing salinity, the decreased liquid limit for expansive soils was attributed to the shrinkage of diffuse double layer, while the... 相似文献
20.
《Quaternary Science Reviews》1987,6(1):43-54
Uncertainties in the measurements necessary for the calculation of amino acid age estimates and paleotemperatures can be propagated through age and temperature equations to yield estimates of precision. It is found that aIle/Ile ratios can be used to calculate numerical ages with a precision generally no better than ±40–50% if the age equation is not calibrated locally and with a precision approaching 15% if appropriate calibration samples are available locally. The effective diagenetic temperature of a sample of known age can be calculated to within about 2°C, although the local relationship between ground and air temperatures may add additional uncertainty when interpreting the effective temperature in terms of climate. The effective temperature for an interval of time bracketed by samples of known age can be known to within about 2–4°C under favorable circumstances. The change in effective temperature between an interval of time bracketed by two samples of known age and the period of time following that interval can be calculated to within 1–2°C in may instances. 相似文献