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 共查询到18条相似文献,搜索用时 78 毫秒
1.
采用直接进样一超高效液相色谱-三重四级杆串联质谱法,建立了对地表水中丙烯酰胺的分析方法。该方法不需要衍生化等前处理步骤。结果表明,丙烯酰胺含量在0.100~10.0μg/L范围内具有很好的线性相关性,实际水样加标回收率为80.0%-105%。该方法的检出限和测定下限分别为0.025μg/L和0.100μg/L,能够满足地表水环境质量标准中关于饮用水中丙烯酰胺最高安全浓度指南的要求,提高了引用水源丙烯酰胺的检测要求。  相似文献   

2.
毛细管气相色谱法测定水和废水中的丙烯酰胺   总被引:2,自引:0,他引:2  
本文采用毛细管色谱法建立了水和废水中丙烯酰胺的测定程序。在此,以活性炭柱吸附,浓缩样品中的丙烯酰胺,用甲醇洗脱,洗脱液用FID测定,方法回收率为831~990%,相对标准偏差为534%,检出限为0016mg/L。  相似文献   

3.
采用溴化衍生-液液萃取法处理地表水,用三重四极杆气相色谱质谱联用仪测定样品中α,β-二溴丙烯酰胺,再换算成丙烯酰胺的质量浓度,该方法在20.0μg/L~500μg/L范围内线性良好,相关系数r为0.998,方法检出限为0.08μg/L。实际水样2个质量浓度水平的平均加标回收率分别为87.5%和92.2%,7次测定结果的RSD分别为9.1%和6.1%。用该方法测定黄河兰州段的黄河水和实验室自来水,结果均未检出。  相似文献   

4.
针对带色浊度高的工业废水氨氮测定的预处理,提出了使用硫酸铝和聚丙烯酰胺(PAM)复合絮凝沉淀法。试验结果表明,方法不仅具有操作简单,试剂用量少,絮凝效果好,去色、去浊率高(达99.6%),且对pH5~10的各种带色浊度高的废水都能起到良好的效果,并能提高测定的精密度,其变异系数为1.2%~3.6%,回收率为90%~105%,确保了数据的准确和可靠。  相似文献   

5.
水中丙烯酰胺气相色谱测定方法研究   总被引:2,自引:2,他引:0  
研究建立了大口径毛细管柱气相色谱法测定水中丙烯酰胺的方法。优化了水中丙烯酰胺的衍生化条件,用乙酸乙酯和正己烷混合溶剂萃取衍生产物,萃取后直接进行色谱分离分析,水中丙烯酰胺的最低检测浓度为0.05μg/L,回收率在94.5%~113%之间;进行6次平行精密度试验,相对标准偏差低于11.5%。研究建立的气相色谱法简便、快速、准确、重现性好,定量、定性准确可靠,适合水中丙烯酰胺的分析测定。  相似文献   

6.
复合絮凝剂对工业废水氨氮测定的预处理   总被引:4,自引:1,他引:3  
针对带色浊度高的工业废水中氨氮测定的预处理,提出了使用硫酸铝和聚丙烯酰胺复合絮凝沉淀法,试验结果表明,方法不仅具有操作简单,试剂用量少,絮凝效果好,去色,去浊度高,且对pH5-pH10是各种带色浊度高的废水都能起到良好的效果,还能提高测定的精密度,其变异系数为1.5%-3.6%,回收率在95%-104%之间,确保数据的准确和可靠。  相似文献   

7.
采用柱后注射法和前处理后添加法评定高效液相色谱-串联质谱法(LC-MS-MS)的基质效应,研究了不同色谱条件对水样丙烯酰胺测定中基质效应的影响,提供了有效削减基质效应的方法,并建立了直接进样测定水中丙烯酰胺的LC-MS-MS法。研究表明,流动相溶剂强度、添加剂种类及浓度对LC-MS-MS直接进样测定水中丙烯酰胺的基质效应影响显著;通过调节流动相溶剂强度和甲酸高度使丙烯酰胺保留时间与基质效应出现的时间段错开,可避开基质效应;在10%甲醇-90%水流动相中添加0.01%~0.02%甲酸可显著降低基质效应,对水中丙烯酰胺的检出限为0.03μg/L,对自来水、地表水、地下水的加标回收率为96.7%~105%,相对标准偏差为1.7%~6.4%。建立的LC-MS-MS直接进样法简便、快速、灵敏度高、定性定量准确可靠,适合水中丙烯酰胺的超痕量分析。  相似文献   

8.
建立了地表水中痕量丙烯酰胺的柱前衍生-EI源串联四极杆气质联用测定方法。丙烯酰胺的双键经溴化衍生成2,3-二溴丙酰胺,加入硫酸钠盐析,乙酸乙酯萃取,浓缩取1μl进样,由串联四极杆气相色谱质谱联用仪测定。通过MRM(150→70.0/107.0)多反应监测实现定性和外标法定量分析。与其他方法相比,该方法具有定性准确、灵敏度高的特点。方法检出限为0.03μg/L,线性范围在0.030~40μg/L;相关系数r=0.9998;六次测定值RSD在14.3%;回收率在89%~196%之间,结果满意。  相似文献   

9.
建立了固相萃取-超高效液相色谱-串联质谱(SPE-UPLC-MS-MS)同时检测水样中6种雌激素(壬基酚、双酚A、雌酮、17α-雌二醇、17α-乙炔雌二醇、雌三醇)的方法.样品采用SPE小柱富集后,用90%乙腈-0.1%氨水混合溶液洗脱浓缩定容.在梯度洗脱条件下,6种雌激素用三重四极杆串联质谱检测.该方法显示出良好的线性关系(r >0.999)和精密度(RSD< 10%),方法检出限为1.3 ~5.2 ng/L.该方法成功应用于地表水、地下水和废水样品中6种雌激素分析,样品加标回收率为76.8%~117%.该方法准确、灵敏、无需衍生,可用于同时测定水样中的6种雌激素.  相似文献   

10.
便携式傅里叶红外分析仪测定水中挥发性有机污染物   总被引:1,自引:0,他引:1  
发明了一种利用GASMET FTIR Dx4020便携式傅里叶红外分析仪测定水中挥发性有机物的实用方法,该方法可以定性定量25个水中挥发性有机物.该方法具有简便快捷、灵敏度高等特点,以苯系物中各单组分物质为例,方法检测限为11 ~45μg/L,相对标准偏差为3.4% ~ 6.6%,加标回收率为98% ~ 109%,在浓度范围内具有良好的线性.但对苯系物混合物定量准确性还需进一步研究提高.  相似文献   

11.
This paper presents a wireless, passive, remote query CO2 sensor comprising a ribbon-like magnetoelastic thick-film coated with a mass-changing CO2 responsive polymer synthesized from acrylamide and isooctylacrylate. In response to a magnetic field impulse, the magnetostrictive magnetoelastic sensor vibrates at a characteristic resonant frequency that is inversely dependent upon the mass of the attached CO2 responsive polymer. The mechanical vibrations of the magnetostrictive sensor launch magnetic flux, which can be detected remotely using a pickup coil. By monitoring the resonant frequency of the passive sensor, the atmospheric CO2 concentration can be determined without the need for physical connections to the sensor or specific alignment requirements. The effect of humidity and the CO2 responsive copolymer composition on the measurement sensitivity are reported. Greatest sensitivity is achieved with a polymer comprising a 1:1 mole ratio of acrylamide to isooctyl acrylate. A 0.7% change in atmospheric CO2 concentration can be detected for a 20 microns thick polymer coated sensor.  相似文献   

12.
研究了一种便携式荧光测油仪在海上溢油应急监测中的适用性,并与现行仲裁标准方法进行比较分析。研究表明:该便携式荧光测油仪测定海水中油类样品仅需100 mL水样,平均每个样品所需的前处理时间约340 s,方法检出限为0.003 mg/L,测定下限为0.012 mg/L。测定用标准物质配制的不同浓度海水样品,相对标准偏差为0.08%~0.87%,测定标准样品的相对误差为0.49%~4.50%,实际样品加标回收率为90%~107%。对标准物质配制的海水样品进行检测,与现行仲裁标准方法在0.05水平下无显著性差异。在渤海中部海上监测中,连续6 d测定不同标准样品的相对标准偏差为0.26%~0.83%。研究结果表明,该便携式荧光测油仪适用于现场对油类的定量分析和水质评价。  相似文献   

13.
On-site measurement of lead in workplace air filter samples and paint chip samples by ultrasonic extraction and anodic stripping voltammetry (UE-ASV) was evaluated in the field during renovation and remodeling activities in residences having leaded paint. Aerosol and paint samples were collected using standard techniques, and the samples were analyzed on-site for lead content by portable UE-ASV. Lead in sample extracts was subsequently determined by atomic absorption (AA) spectrometry in a fixed-site laboratory. The remaining sample extracts plus undissolved material (air filters or paint particles) were then subjected to hot plate digestion in concentrated nitric acid-30% hydrogen peroxide prior to AA analysis for lead. Field UE-ASV lead data were thereby compared to UE-AA and hot plate digestion-AA results from fixed-site laboratory lead measurement. Determination of lead in air filter samples by UE-ASV (over the range of 5 microg to approximately 800 microg Pb per sample) was extremely well correlated with lead measurement by UE-AA and hot plate digestion-AA procedures. However, a significant negative bias associated with ASV measurement was observed, and this was attributed to a matrix effect. Lead measurement in paint chip samples by UE-ASV (over the range of approximately 10 to approximately 550 microg Pb g(-1)) was well correlated with lead measurement by UE-AA and hot plate digestion-AA procedures. However, correlation and precision were lower for lead measurement in paint samples as compared to aerosol samples, and a negative bias was also observed. Lead measurements by UE-AA were compared to lead determinations by hot plate digestion-AA; these data were highly correlated and demonstrated no significant bias. Thus it was concluded that the ultrasonic extraction procedure performed equivalently to hot plate digestion. It was reasoned that matrix effects due to the preparation and analysis of paint chip particles resulted in greater imprecision as well as negative bias by ASV measurement. Despite significant negative bias in this sample set, UE-ASV offers promise for on-site measurement of lead in samples of interest in occupational and environmental health.  相似文献   

14.
微波消解ICP-MS法测定宣威和富源土壤中的微量元素   总被引:5,自引:2,他引:3  
建立了微波消解-ICP-MS法测定土壤中32种微量元素的方法。采用氢氟酸-硝酸-过氧化氢体系微波消解,稀释定容后用ICP-MS对溶液进行元素的测定,在优化仪器工作参数后,以双内标铑(Rh)和铼(Re)进行校正。元素检出限为0.01~0.45ng/ml,测定国家标准物质西藏土壤成分分析标准物质GBW 08302中的元素,测定值与标准值或参考值基本一致,用该法测定云南宣威和富源两地24份土壤样品结果表明,该方法快速、简便、准确,适于土壤中多种微量元素的测定。  相似文献   

15.
In this work assays involving chlorinated water samples, which were previous spiked with humic substances or algae blue green and following the production of the THMs for 30 days is described. To implement the assays, five portions of 1,000 ml of water were stored in glass bottles. The water samples were treated with solutions containing 2, 3, 4 and 5 mg l−1 chlorine. The samples aliquots (60 ml) were transferred into the glass vials, 10 ml were removed to have a headspace and 100 μl of the 10 mg l−1 pentafluortoluene bromide solution was added to each vial. The extraction step was performed by adding 10 g of Na2SO4 followed by 5 ml of n-pentane. The vials were stopped with a TFE-faced septum and sealed with aluminum caps. The generated THMs were determined by gas chromatography with electron capture detector using reference solutions with concentration ranging from 8 to 120 μg l−1 THMs. Three assays were monitored during 30 days and chloroform was the predominant compound found in the water samples, while other species of THMs were not detected. The results showed that when the chlorine concentration was increased in water samples containing algae the concentration of THM varied randomly. Nevertheless, in water samples containing humic substances the increase of the THM concentration presented a relationship with the chlorine concentration. It was also observed that chloroform concentration increased with the elapsed time up to one and six days to water samples spiked with humic substances and algae blue green, respectively and decreased along 30 days. By other hand, assays performed using water samples containing decanted algae material showed that THM was not generated by the chlorine addition.  相似文献   

16.
本工作对多级串联吹出分离法测定氰化物的可行性作了探讨。试验确定在磷酸-EDTA体系中用氮气吹出分离氰化氢的条件。一次可以同时处理四个样品,富集浓缩效率可达20倍。标准水样试验结果的平均回收率为95%,相对标准偏差为1.6—5.3%。环境水样测定结果本方法和标准方法基本相符.  相似文献   

17.
2006年秋冬两季图们市大气气溶胶中多环芳烃分布规律   总被引:1,自引:0,他引:1  
大气气溶胶是目前大多数城市的首要污染物,其中的多环芳烃是对人体健康危害最大的环境污染物之一。通过图们市2006年9月、12月4个采样点的大气气溶胶样品分析,研究了大气气溶胶中多环芳烃的分布规律。采用超声波萃取法提取样品中的多环芳烃,然后对其进行旋蒸浓缩,氮气吹至1ml,用高效液相色谱进行定性和定量分析。实验结果表明,美国EPA优先控制的16种多环芳烃普遍存在于图们市区的大气气溶胶中。图们市不同时空大气气溶胶中多环芳烃的分布具有一定的规律性。  相似文献   

18.
The purposes of this study are: (1) to determine whether proficiency analytical test (PAT) materials from the American Industrial Hygiene Association can be used to provide quality data for portable X-ray fluorescence analysis (XRF) of lead in dust wipe surface samples; (2) to provide data to determine whether the on-site analysis of field dust wipe samples by XRF and the laboratory method of inductively coupled plasma emission analysis (ICP) are comparable; and (3) to determine if differences exist between different wipe materials. Several wipes meet the ASTM E1792 performance requirements of lead background level less than 5 microg per wipe, be only one layer thick, yield recovery rates of 80- 120% from spiked samples, remain damp throughout the sampling procedure, and do not contain aloe. The wipes used in this study were Pace Wipes, which are used for the PAT materials, and, for the field samples, Palintest Wipes, which were supplied by the instrument manufacturer, and Ghost Wipes, which are popular because they digest in hot, concentrated acid, so that chemical analysis is simplified. Twenty PAT wipe samples were obtained from four different proficiency test rounds. Surface wipe samples were taken at three different locations representing different industry types. All samples were analyzed using a portable XRF spectrometer and by ICP. Strong linear relationships were found for the analysis of wipe samples by ICP and by portable XRF. For the PAT samples, the results from the ICP and XRF analysis were not statistically equivalent, which indicates a bias in the ICP analysis. The bias was not excessive, since all ICP analyses fell within the acceptable range for the proficiency samples. The good correlation between the proficiency sample reference values and the XRF determinations is not surprising considering similar proficiency samples were used to calibrate the instrument response. Users of this portable XRF analyzer could enroll in the proficiency test program as part of their quality assurance program. For field samples, the relationship was strongest for Palintest wipes, and the values found for all three industries could be combined. However, the results from the ICP and XRF analysis were not statistically equivalent using the correction factor in the calculation algorithm as supplied with the instrument, and a new coefficient was derived. The mean relative error for the XRF analysis versus the ICP analysis was greater than 25%, such that the method falls within the realm of screening procedures. For Ghost Wipe samples, the precision was different for different industries, and the results could not be pooled. Differences between the two wipe materials may be related to the number of folds required for analysis.  相似文献   

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