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1.
为测定污染土壤中的6种低残留喹诺酮类抗生素(氧氟沙星、培氟沙星、恩诺沙星、环丙沙星、诺氟沙星、恶喹酸),全面优化了一种联合加速溶剂萃取(ASE)、固相萃取(SPE)和高效液相色谱/三重四级杆质谱(HPLC/MSMS) 3种检测技术的分析方法。样品采用甲醇和0.1 mol/L EDTA-McIlvaine缓冲液(1∶1)进行加速溶剂萃取,经Bond Elut Plexa型HLB固相萃取小柱富集纯化,土壤中6种喹诺酮类抗生素的基质效应因子控制在0.84~1.04。在0.2~100.0μg/L(以恶喹酸计)质量浓度范围内,目标化合物的线性关系良好(r0.999),6种目标化合物的检出限为0.09~0.75μg/kg,加标回收率为60.9%~89.9%。该方法自动化程度和准确度较高,可极大程度地降低基质效应,提高测定方法的灵敏度,适用于土壤中喹诺酮类抗生素残留的检测。 相似文献
2.
采用液液萃取处理水样,用气相色谱-串联质谱法测定样品中五氯酚及其钠盐,通过优化测定条件,使方法在1.00μg/L~500μg/L范围内线性良好。检出限和定量限分别为1.00μg/L和5.00μg/L,空白水样五氯酚钠3个质量浓度水平的加标回收率为89.8%~98.4%,5次平行试验测定结果的RSD为5.5%~10.7%。 相似文献
3.
Inna E. Popova Matthew J. Morra Sanjai J. Parikh 《Journal of environmental science and health. Part. B》2019,54(1):35-40
Veterinary antibiotics used in agriculture can be introduced into the environment through land application of animal manure, accumulating in soils and groundwaters and posing a significant risk to human health and animal well-being. As the analysis of tetracyclines in soil is challenging due to their strong interaction with soil minerals and organic carbon, the objective of this study was to develop a reliable and reproducible method for quantitative analysis of chlortetracycline and oxytetracycline, and their respective metabolites in soils. A method based on pressurized liquid extraction (PLE) with in-cell clean-up was developed for the extraction of chlortetracycline and oxytetracycline and four likely metabolites from a set of four soils. Optimized conditions included a cell size of 22?mL, soil loading of 5?g, pH of 8.0, methanol:water ratio of 3:1, 50?°C, and two cycles. Soil extracts were analysed by high-performance liquid chromatography (HPLC) coupled with ion trap mass spectrometry (MS). Recoveries of seven tetracyclines from soil ranged from 41% to 110%. The limits of detection for tetracyclines were 0.08–0.3 µg g?1 soil, and intra- and inter-day variation ranged from 0.12–0.34%. The proposed PLE method is suitable for quantification of tetracyclines in agricultural soils at typical concentrations expected in contaminated environments. 相似文献
4.
采用高效液相色谱-串联质谱(HPLC-MS/MS)检测,建立了地表水中13种药物及个人护理品的测定方法。水样用盐酸与氢氧化钠溶液调p H值至7.0左右,过固相萃取小柱进行富集,用14 m L甲醇洗脱。以C18柱为分离柱,0.01%甲酸的甲醇-0.01%甲酸水溶液为流动相,目标物在10 min内分离,在0.50~250μg/L范围内,13种化合物峰面积与内标物质峰面积之比与质量浓度的线性关系良好(0.99),检出限在0.05~0.5 ng/L范围内。基质加标实验结果表明,13种化合物在水中的回收率分别在56.2%~123.2%之间(加标水平5 ng/m L)和58.0%~107.8%(加标水平50 ng/m L),相对标准偏差在1.60%~19.9%(n=6)之间。应用该方法测定了从2条纳污河流采集的10份水样,结果表明,除美托诺尔和普洛萘尔未被检出外,其余11药物的检出频率在30%~100%之间。在13种目标物质中,咖啡因的检测浓度最高达287.5ng/L,舒必利次之,为277.5 ng/L。本方法快速、准确,适用于地表水中PPCPs类的快速测定。 相似文献
5.
高效液相色谱-二极管阵列检测器测定邻苯二甲酸酯色谱条件优化 总被引:1,自引:1,他引:0
采用高效液相色谱-二极管阵列检测器对6种PAEs类物质进行测定,并对梯度洗脱条件、流速、检测波长等影响化合物色谱响应的关键参数进行优化。综合考虑样品测试效率、分析精度、实际样品中存在杂质干扰等因素,确定以乙腈-水为流动相进行梯度洗脱,洗脱0~11 min流动相乙腈-水梯度比例为50∶50,11 min后流动相调整为100%乙腈,各化合物均能完全分离;色谱分析流速为0.8 m L/min;PAEs的最佳吸收波长为225 nm。在优化的色谱条件下,6种PAEs的线性良好,相关系数均大于0.999 8,仪器检出限为0.08~0.12 mg/L,保留时间、峰面积的相对标准偏差分别为0.02%~0.60%、0.13%~0.86%。方法灵敏度较高,适合土壤等邻苯二甲酸酯含量较高基质样品的快速分析。 相似文献
6.
为了精确有效地提取声波法检测气井环空液位的回波周期,在分析环空中测试波的传播特征及基音周期检测的基础上,提出1种基于检测信号短时自相关函数(ACF)及平均幅度差函数(AMDF)的液面回波周期提取方法;利用自主搭建的室内模拟实验系统开展了不同初始环空压力下环空液位检测实验;对检测信号进行中心削波处理并计算ACF/AMDF,提取出液面回波周期并与理论计算值对比分析;同时分析了现场环空液位检测信号,提取其回波周期。研究结果表明:提出的新方法能有效地用于提取环空液面回波周期;室内实验中,该方法最大误差绝对值为1.54%;该方法能够有效抑制液面回波信号中的随机噪声及接箍反射波等,处理后的信号曲线在回波周期处峰值更加突出、集中,而在其他位置更加平滑,提高了对液面回波周期特征的辨识能力。 相似文献
7.
The vaporisation of a liquid nitrogen pool spilled on concrete ground was investigated in small scale field experiments. The pool vaporisation rate and the heat transfer from the concrete ground were measured using a balance and a set of embedded heat flux sensors and thermocouples. The ability to predict the concrete's thermal properties based on these measurements was investigated. This work showed that a simple, one-dimensional theoretical model, assuming heat conduction through a semi-infinite ground with ideal contact between the cryogenic liquid and the ground, commonly used to describe the heat transfer from a ground to the LNG, can be used to match the observed vaporisation rate. Though estimated parameters, thermal conductivity and thermal diffusivity, do not necessary represent real values. Although the observed vaporization rate follows a linear trend, and thus can be well represented by the model, the overall model prediction seems to be overestimated. The temperature profile inside the concrete is slightly over-predicted at the beginning and under-predicted at later stage of the spill. This might be an effect of the dependence of the concrete's thermal properties on the temperature or may indicate an incorrect modelling and a varying temperature of the ground surface. 相似文献
8.
建立了固相萃取-超高效液相-串联质谱法同时测定水环境中26种类固醇激素的分析方法。明确了取样体积为500 m L,Cleanert PEP为富集柱,乙酸乙酯为洗脱剂,甲醇为溶剂进行提取操作。选择了正离子模式,以0. 1%甲酸/甲醇-水为流动相,负离子模式以0. 1%氨水/乙腈-水为流动相,试样经AcquityTMUPLC BEH C18色谱柱分离后,选用质谱检测模式进行定性、定量分析。通过方法验证,26种类固醇激素的方法检出限为0. 3~1. 5 ng/L,测定下限为1. 2~6. 0 ng/L,代表性样品测定结果的相对标准偏差为2. 6%~13. 7%(n=6),加标回收率为71. 2%~121%。该方法操作便捷,灵敏度高,精密度和准确度良好,可适用于水环境中多种痕量、超痕量类固醇激素的定性定量分析。 相似文献
9.
Many release problems involve two-phase releases of hazardous materials of superheated liquids with high energy into the atmosphere. Such accidents are accompanied by violent phase transition and form catastrophic flashing jets. In this work, experimental and theoretical analyses were conducted to investigate dynamic characteristics of flashing jet morphology and their dependence on pressure-decay dynamics under different storage pressures, superheats, and nozzle diameters. Flashing jet morphology and angle throughout two-phase releases were captured by a high-speed camera, and the corresponding source pressure in the superheated liquid tank was measured simultaneously. Results show that three typical phases, expansion, stabilization, and decay, are characterized throughout two-phase release based on the evolution of flashing jet morphology. The jet initially expands gradually due to the enhancement of phase transition intensity, and then keeps stable when the intensity reaches its maximum, and terminally decays rapidly due to the depletion of superheated liquid. Phase transition intensity at the nozzle exit is mainly controlled by the pressure-decay dynamics. Bubbles nucleation inception sites gradually move upstream of the nozzle during the pressure decay process increasing the phase transition intensity. The increase of storage pressure, superheat and nozzle diameter promotes the mechanical and thermodynamic effects on the jet breakup. The significant increase of mechanical and thermodynamic effects effectively accelerates droplets evaporation and further affects flashing jet morphology. 相似文献
10.