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建立了加速溶剂提取、凝胶渗透色谱法净化-超高效液相色谱/串联质谱快速测定土壤中20种磺酰脲类除草剂的方法。土壤经过冷冻干燥、粉碎过筛,用加速溶剂仪提取(ASE),经凝胶渗透色谱净化(GPC),以超高效液相色谱/串联质谱(UPLC-MS/MS)多级监测模式(MRM)外标法进行定性定量分析。结果表明:土壤中20种磺酰脲类除藻剂的检出限为2~5 ng/kg。对同一环境样品进行了3个不同添加量(1、5、10μg/L)的加标回收实验,平均回收率为65. 7%~106. 1%,相对标准偏差为2. 3%~12. 1%。该方法快速、灵敏、准确,可有效应用于土壤中20种磺酰脲类除草剂的快速监测。 相似文献
534.
基于Qu ECh ERS提取方法,用液相色谱-串联质谱法测定水中14种常见除草剂,通过优化样品前处理条件,使14种除草剂在0.005 mg/L~0.500 mg/L范围内线性良好,相关系数均0.99,方法检出限为0.005 mg/L。空白水样3个质量浓度水平的加标回收率为74.5%~109%,5次测定结果的RSD为3.9%~11.4%。将该方法用于测定长江流域3个重点城市的水体,结果为未检出。 相似文献
535.
采用电感耦合等离子光谱和质谱法对超纯水、去离子水和蒸馏水3种实验用水进行半定量和定量分析。通过对主要相关元素的分析结果比较,超纯水的水质优于其他两种,更适宜作为无机元素痕量分析的实验用水。 相似文献
536.
脂质是生物体的重要代谢分子,参与重要的细胞生物功能,已有报道表明环境中污染物会干扰生物体正常循环及代谢机制,导致脂肪代谢紊乱。基于数据非依赖型(DIA)采集质谱技术,通过优化UPLC-QTOF MS(超高效液相色谱飞行时间质谱联用)液相分离方法,开发了少量人体血液样品中脂质代谢分子的高通量分析方法,并将其应用于57个普通人群的血液样品分析,在10μL人体血液样品中检出2 598个信号,经脂代组学质谱库匹配解析鉴定出八大类1 780个脂质分子,其中分子数目占比最大的脂质为甘油磷脂类(37%),其次依次为脂肪酸类(23%)、固醇脂类(13%)、甘油脂类(10%)、鞘脂类(9.0%)、孕烯醇酮脂类(4.8%)。上述研究建立的脂质分子高通量分析方法为以脂质代谢为毒性终点的污染物毒性筛查和毒理机制研究提供方法学基础。 相似文献
537.
Min He Dan Song Hong C. Jia 《Journal of environmental science and health. Part. B》2016,51(9):594-601
To study the dissipation rates and final residual levels of chlorantraniliprole and thiamethoxam in maize straw, maize, and soil, two independent field trials were conducted during the 2014 cropping season in Beijing and Anhui Provinces of China. A 40% wettable powder (20% chlorantraniliprole?+?20% thiamethoxam) was sprayed onto maize straw and soil at an application rate of 118 g of active ingredient per hectare (g a.i.ha?1). The residual concentrations were determined by ultra-high-performance liquid chromatography–tandem mass spectrometry. The chlorantraniliprole half-lives in maize straw and soil were 9.0–10.8 and 9.5–21.7 days, respectively. The thiamethoxam half-lives in maize straw and soil were 8.4–9.8 and 4.3–11.7 days, respectively. The final residues of chlorantraniliprole and thiamethoxam in maize straw, maize, and soil were measured after the pesticides had been sprayed two and three times with an interval of 7 days using 1 and 1.5 times the recommended rate (72 g a.i. ha?1 and 108 g a.i. ha?1, respectively). Representative maize straw, maize, and soil samples were collected after the last treatment at pre-harvest intervals of 7, 14, and 28 days. The chlorantraniliprole residue was below 0.01 mg kg?1 in maize, between 0.01 and 0.31 mg kg?1 in maize straw, and between 0.03 and 1.91 mg kg?1 in soil. The thiamethoxam residue concentrations in maize, maize straw, and soil were <0.01, <0.01, and 0.01–0.03 mg kg?1, respectively. The final pesticide residues on maize were lower than the maximum residue limit (MRL) of 0.02 mg kg?1 after a 14-day pre-harvest interval. Therefore, a dosage of 72 g a.i. ha?1 was recommended, as it can be considered safe to human beings and animals. 相似文献
538.
Osman Tiryaki 《Journal of environmental science and health. Part. B》2016,51(10):722-729
This study was undertaken to validate the “quick, easy, cheap, effective, rugged and safe” (QuEChERS) method using Golden Delicious and Starking Delicious apple matrices spiked at 0.1 maximum residue limit (MRL), 1.0 MRL and 10 MRL levels of the four pesticides (chlorpyrifos, dimethoate, indoxacarb and imidacloprid). For the extraction and cleanup, original QuEChERS method was followed, then the samples were subjected to liquid chromatography-triple quadrupole mass spectrometry (LC-MS/MS) for chromatographic analyses. According to t test, matrix effect was not significant for chlorpyrifos in both sample matrices, but it was significant for dimethoate, indoxacarb and imidacloprid in both sample matrices. Thus, matrix-matched calibration (MC) was used to compensate matrix effect and quantifications were carried out by using MC. The overall recovery of the method was 90.15% with a relative standard deviation of 13.27% (n = 330). Estimated method detection limit of analytes blew the MRLs. Some other parameters of the method validation, such as recovery, precision, accuracy and linearity were found to be within the required ranges. 相似文献
539.
张理扬 《中国环境管理干部学院学报》2012,(5):57-59,91
固相微萃取是一种操作简便、分析快速、无溶剂参与的样品前处理技术。通过采用固相微萃取富集水中的松节油,气相色谱质谱法分析,整个过程只需要25 min。该方法检出限为0.02 mg/L,样品加标回收率为90.0%~130%,相对标准偏差为3.49%~14.6%,完全能够满足日常环境管理需要。 相似文献
540.
The photocatalytic degradation of crotamiton in aqueous solution using TiO2 was investigated. To investigate the effect of initial pH, the photodegradation behaviors of three types of pharmaceuticals were compared (crotamiton, clofibric acid, sulfamethoxazole). The degradation rates of crotamiton in the pH range 3-9 were nearly equal, but those of clofibric acid and sulfamethoxazole were affected by pH. At pH > 6.5, TiO2 particles, clofibric acid and sulfamethoxazole had negative charge, therefore, the repulsive force between TiO2 particles and anionic pharmaceuticals occurred and a low reaction rate at high pH was observed. The effect of UV intensity and TiO2 concentration on photodegradation efficiency was also investigated. Linear and logarithmical relationships between UV intensity, TiO2 concentration and the reaction rate constant were confirmed. Furthermore, the structures of photodegradation intermediates formed concomitantly with the disappearance of crotamiton were estimated. Seven intermediates were characterized by LC/MS/MS analyses, and it was assumed that the photocatalytic degradation of crotamiton was initiated by the attack of electrophilic hydroxyl radicals on aromatic rings and alkyl chains. 相似文献