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1.
建立了固相萃取-毛细管气相色谱测定地表水中硝基苯类化合物的方法,优化了试验条件。方法线性良好,10种硝基苯类化合物的检出限为0.05μg/L~0.15μg/L,实际样品测定的RSD为1.7%~5.0%,平均加标回收率为80.8%~117%。  相似文献   

2.
采用顶空固相微萃取(HS -SPME)技术萃取水中6种氯苯类化合物,全面分析对目标物萃取效率的影响因素,并确定萃取试验的最佳条件。用顶空固相微萃取联合气相色谱法(HS -SPME -GC)测定水中6种氯苯类化合物,方法在0.500 ng/L~2.00×10^5 ng/L范围内线性良好,检出限为0.05 ng/L ~2000 ng/L,空白样品加标回收率为69.8%~121%, RSD为4.8%~18.3%。用该方法测定实际水样,平行双样的相对偏差低于20%。  相似文献   

3.
对测定水中硝基苯类化合物的锌还原-盐酸萘乙二胺分光光度法进行优化,简化了操作步骤,并将参加显色反应的水样体积由4.0 mL增加至8.0 mL,比色皿厚度由10 mm增加至20 mm,方法推荐检出限由0.20 mg/L降至0.05 mg/L,实验室检出限为0.042 mg/L,改进后的方法对标准样品的测定结果符合要求。  相似文献   

4.
洪泽湖硝基苯类化合物的污染特征   总被引:2,自引:2,他引:0       下载免费PDF全文
对洪泽湖水质、底泥及水生生物样品10种硝基苯类化合物的浓度进行了测定,水样中总硝基苯类化合物的含量在0.179~5.17μg/L,北部湖区和南部湖区的总硝基苯类化合物的浓度较高,其中成河北(S7)的浓度最高。底泥中的含量在0.137~4.50μg/kg,北部湖区及出湖口附近形成一个硝基苯类化合物的污染带,其中成河东(S6)的浓度最高。水生生物体内的总硝基苯含量按鲫鱼、白鱼、泥鳅、龙虾、河蚌、螺蛳依次升高。  相似文献   

5.
在现行分析水中硝基苯类污染物标准分析方法的基础上,将参加显色反应的水样体积和比色皿厚度各增加一倍,方法检出限由0.20mg/L降低至0.05mg/L。用改进法分析很低浓度的硝基苯类水样,具有很好的现实意义。  相似文献   

6.
采用液液萃取-气相色谱法测定饮用水中10种硝基苯类化合物,通过萃取条件优化试验,选择正己烷为萃取剂,使目标物在0μg/L~38.5μg/L之间线性良好,检出限为0.002μg/L ~0.005μg/L。实际饮用水样的加标回收率为80.8%~104%,RSD<3%。用该方法测定桂林市4个水厂饮用水,结果硝基苯、间-二硝基苯、2,4-二硝基氯苯未检出,其余7种硝基苯类化合物虽有检出,但检出值均低于标准规定的限值。  相似文献   

7.
采用碱性过硫酸钾消解水样,OnGuardⅡBa柱萃取、过滤,去除消解液中大量硫酸盐,离子色谱法测定地表水中总氮含量。试验表明,方法在0ms/L~20.0mg/L之间线性良好,相关系数r为0.9994,方法检出限为0.007mg/L。该方法与国标法同时测定标准物质,测定值均在定值范围内,6次平行测定结果的RSD分别为2.3%和1.8%,地表水样的加标回收率为95.7%~105%。实际水样的测定结果与国标法比对,无明显差异。  相似文献   

8.
采用磁性分散固相萃取技术富集水中氯苯类化合物,用气相色谱法测定,并对萃取剂的用量、萃取时间、解吸溶剂、氯化钠加入量等条件进行优化。试验表明,方法在0.001 mg/L~2.50 mg/L 范围内,氯苯类化合物各组分线性良好,方法检出限在0.600μg/L~5.00μg/L范围内。地表水实际水样的加标回收率为83.1%~93.4%,RSD为4.8%~7.3%。  相似文献   

9.
石墨炉原子吸收光谱法测定农产品中痕量铍   总被引:1,自引:0,他引:1       下载免费PDF全文
采用石墨炉原子吸收光谱法测定农产品中痕量铍,比较了微波消解和电热板消解两种前处理方法,选择了基体改良剂。方法在0μg/L—4.00μg/L范围内线性良好,微波消解法和电热板消解法的检出限分别为0.002mg/kg和0.0002mg/kg,标样平行测定的RSD为2.4%—4.1%,农产品加标回收率为80.0%—95.0%。  相似文献   

10.
采用动态顶空气相色谱FID法测定水中乙醛、丙酮、甲醇、丙烯醛、丙烯腈、乙腈、吡啶等7种极性水溶性有机物,通过优化动态顶空条件,使该方法在0.157mg/L~7.92mg!L之间线性良好。方法检出限在0.008mg/L~0.048mg/L之间,空白水样的加标回收率为103%~111%,RSD为5.4%~8.7%。用该方法测定某制药企业排口污水和地表水,只有污水中甲醇、乙腈、吡啶有响应值。  相似文献   

11.
采用流动注射二乙氨基二硫代甲酸钠分光光度法测定废水中的铜,优化了试验条件,讨论了干扰离子的影响。方法在0mg/L-10.0mg/L范围内线性良好,检出限为0.07mg/L,水样测定的RSD≤0.8%,加标回收率为98.5%-101%,标准样品的测定结果符合要求。  相似文献   

12.
研究了溴代十六烷基吡啶、正丁醇、正庚烷和水自制微乳溶液介质中,4-(6-甲氧基-8-喹啉偶氮)-间苯三酚与铜的显色反应,建立了分光光度法测定微量铜的新方法。在显色液中铜的质量浓度在0.010 mg/L~0.700 mg/L范围内符合比尔定律,方法检出限为0.003 mg/L,铝合金和水样测定的RSD为0.3%~1.7%,加标回收率为96.3%~104%。  相似文献   

13.
气相色谱法测定水中呋喃丹   总被引:1,自引:0,他引:1       下载免费PDF全文
建立了二氯甲烷提取、高效毛细管柱分离、气相色谱-氮磷检测器测定水中呋喃丹的方法.优化了试验条件,以HP-5和HP-1301双柱定性,方法在0.00 mg/L~1.00 mg/L之间线性良好,检出限为2.0×10-5 mg/L,RSD≤6.5%,加标回收率为93.6%~110%.  相似文献   

14.
气相色谱/质谱法测定环境毒饵中溴敌隆   总被引:1,自引:0,他引:1       下载免费PDF全文
采用气相色谱/质谱联用法测定环境毒饵中溴敌隆,优化了试验条件。方法在0mg/L~10.0mg/L范围内线性良好,检出限为0.01mg/kg,标准溶液测定的相对标准偏差为2.2%~4.6%,样品加标回收率为92.5%-96.3%。  相似文献   

15.
The concentration of total arsenic and five different arsenic species [As(III), As(V), monomethylarsonic acid (MMA), dimethylarsenic acid (DMA), and arsenobetaine (AsB)], were measured in the muscle, liver and gastrointestinal tract (GIT) of five different fish species [lake whitefish (Coregonus clupeaformis), walleye (Stizostedion vitreum), northern pike (Esox lucius), white sucker (Catostomus commersoni) and longnose sucker (Catostomus catostomus)] from Back Bay, Great Slave Lake, near the city of Yellowknife, NT, Canada. The total concentration (dry weight) of arsenic in muscle ranged from 0.57 to 1.15 mg/kg, in the liver from 0.42 to 2.52 mg/kg and in the GIT from 1.48 to 8.92 mg/kg. Among fish species, C. commersoni had significantly higher total arsenic concentrations in the GIT than S. vitreum, E. lucius and C. clupeaformis, and higher total arsenic concentrations in the liver than C. clupeaformis. The mean concentration of As(III) and As(V) in the muscle of all fish ranged from < or =0.01 to 0.05 mg/kg and < or =0.01 to 0.02 mg/kg, respectively, and together comprised < or =7.5% of the total arsenic measured in muscle. The concentrations of MMA were below detection in the muscle of all five fish species. However, AsB and DMA were measured in all fish species and nearly all fish tissues. The concentrations of AsB ranged from 0.01 to 0.13 mg/kg and the concentrations of DMA ranged from <0.02 to 0.45 mg/kg. The majority (>50%) of organic arsenic in almost all of the tissues from fish caught in Back Bay was not directly identified. Evidence from the literature suggests that most of these other organic arsenic species were likely trimethylated arsenic compounds, however, further analytical work would need to be performed to verify this hypothesis.  相似文献   

16.
用二氯甲烷提取稻田水和水稻植株样品中的丙草胺,稻田土壤样品用二氯甲烷-甲醇混合溶剂(体积比为9∶1)提取,再用高效液相色谱仪测定。方法在0.02 mg/L~2.00 mg/L的范围内线性良好,相关系数为0.9998;稻田水、土壤,水稻植株中丙草胺的检出限分别为0.001 mg/L、0.005 mg/kg、0.01 mg/kg;对稻田水、土壤和水稻植株分别做3个浓度水平的加标回收试验,重复5次,平均回收率在75.5%~84.7%之间,测定结果的相对标准偏差为2.0%~10.5%。  相似文献   

17.
Eutrophic conditions, in both saline and freshwater systems, result from nutrient export from upstream watersheds. The objective of this study was to quantify the surface runoff losses of nitrate-nitrogen (NO?-N), total nitrogen (TN), dissolved reactive phosphorus (DRP), and total phosphorus (TP) resulting from prevailing practices on a managed golf course. Inflow and outflow discharge waters on a sub-area of Northland Country Club (NCC) located in Duluth, Minnesota were measured for both quantity and quality from April through November from 2003 to 2008. Nutrient losses were detectable throughout the year, had a seasonal trend, and routinely exceeded recommended levels to minimize eutrophication. The median outflow TN concentration (1.04 mg L?1) was significantly greater (p < 0.05) than the median inflow (0.81 mg L?1) concentration. Similarly, the median outflow TP concentration (0.03 mg L?1) was significantly greater (p < 0.05) than the median inflow concentration (0.02 mg L?1). Maximum recorded concentrations during the study period were 1.9 mg L?1 NO?-N, 3.93 mg L?1 TN, 0.34 mg L?1 DRP, and 1.11 mg L?1 TP. Mean annual export coefficients at NCC were 0.7 kg ha?1 NO?-N (1.7% of applied), 4.43 kg ha?1 TN (10.7% of applied), 0.14 kg ha?1 DRP (2.6% of applied), and 0.25 kg ha?1 TP (4.6% of applied). The findings of this study highlight the need for adopting conservation practices aimed at reducing offsite nutrient transport.  相似文献   

18.
The integrated pest management (IPM) modules of pesticide schedule on Basmati rice were validated at field experiments conducted in Northern India for consecutive 3 years (2005–2008). The pesticide residues were found below the detectable limit (<0.01–0.001 mg/kg) in soil and irrigation water samples of Kaithal region. In Dehra Dun region of Uttrakhand, the residues of carbendazim in rice grains and soil were detected below <0.01 mg/kg level. In second year experiments (2006–2007), only four non-IPM soil samples indicated the presence of chlorpyrifos and endosulfan in the range of ND <0.001 to 0.07 mg/kg, out of 45 samples analyzed. Carbendazim applied as seed treatment at Dehradun and Kaithal field trials was found below detectable limit in both IPM and non-IPM rice grains (<0.01 mg/kg) and irrigation water (0.01 μl/ml). Chlorpyrifos was detected in five water samples from Kaithal and one from Pant Nagar in the range of 0.003–0.006 μl/L, α- and β-isomer of endosulfan in the range of 0.005–0.03, and 0.005–0.02 μl/ml, respectively, in one sample from Pant Nagar and two from Kaithal, out of a total of 22 samples. In the region of Uttrakhand and Uttar Pradesh during 2007–2008, four non-IPM samples of soil indicated trace levels of endosulfan, out of 16 samples analyzed. The residues were detected below detection limit for carbendazim (<0.01 mg/kg) in soil samples of Dehradun IPM fields and for endosulfan and carbendazim (0.001–0.01 μl/L) in water samples each from IPM and non-IPM fields of Uttar Pradesh. The results of 3-year trials of IPM module indicated basmati rice as safe and economical with pesticide residue-free rice grains.  相似文献   

19.
A rapid and simple HPLC method has been developed for the quantitation of 4-chloro-2-methylphenoxyacetic acid (MCPA) in both wheat and soil samples. Samples were extracted in acidic media and cleaned up by solid-phase extraction with C(18) cartridges before HPLC-DAD detection. The limits of detection and quantification of MCPA were 0.02 ng and 0.01 mg/kg for both wheat and soil. The mean recoveries ranged from 87.1% to 98.2%, and the RSDs ranged from 0.604% to 3.44% for the three spiked levels (0.01, 0.1, 0.5 mg/kg). The proposed method was successfully applied to the analysis of MCPA residues in wheat and soil samples from an experimental field. The dissipation half-lives in soil were calculated to be 3.22 days (Beijing) and 3.10 days (Tianjin), respectively. Direct confirmation of the analytes in real samples was achieved by gas chromatography-mass spectrometry. The results indicated that at harvest time, the residues of MCPA in wheat were well below the maximum residue levels and were safe to apply in wheat.  相似文献   

20.
A simple and accurate method of determining metalaxyl and cymoxanil in pepper and soil was developed by ultra-performance liquid chromatography–photodiode array detection. The limits of detection were 0.015 mg/kg for metalaxyl and 0.003 mg/kg for cymoxanil. The limits of quantification were 0.05 mg/kg for metalaxyl in pepper and soil as well as 0.01 mg/kg for cymoxanil in pepper and soil. Recoveries of pepper and soil were investigated at three spiking levels and ranged within 77.52 to 102.05 % for metalaxyl and 87.15 to 103.21 % for cymoxanil, with relative standard deviations below 9.30 %. For field experiments, the half-lives of metalaxyl were 3.2 to 3.9 days in pepper and 4.4 to 9.5 days in soil at the three experimental locations in China. At harvest, pepper samples were found to contain metalaxyl and cymoxanil well below the maximum residue limit MRLs of the European Union (EU) following the recommended dosage and the interval of 21 days after last application.  相似文献   

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