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1.

Extraction is an important procedure for samples that contain soil because other compounds in soil may affect analysis of estrogens. This study was conducted to evaluate three different extraction methods for 17β-estradiol in soil. Sand, bentonite, and organic-rich silt loam were spiked with 1 mg kg? 1 of 17β-estradiol as a model compound of estrogens. 17β-estradiol and its metabolites, estrone and estriol, were extracted using (i) a modified Bligh and Dyer extraction, (ii) a pressurized fluid extraction, and (iii) a diethyl ether extraction, and measured by liquid chromatography tandem mass spectrometry. There were significant differences in the extraction efficiency for 17β-estradiol among the extraction methods and the soils: the efficiencies ranged from 10% to 97%. Overall, the diethyl ether extraction method had the largest efficiency of 17β-estradiol with 45% and 57% for bentonite and silt loam, respectively. Transformation of 17β-estradiol to estrone and estriol in the different extraction methods was less than 3.6% during the extraction procedures. This study underlined the importance of sample preparation for estrogen analysis in soil samples.  相似文献   
2.
The properties of electro-activated (EA) aqueous solutions as well as the dynamics of their changes were considered in the current study using aqueous solutions of NaCl and NaHCO3. The concentrations of the salt solutions were 0.5, 0.25, 0.125 and 0.05 M. The tests were performed at the DC current densities of 25, 37.5, and 50 Å/m2. The electro-activation reactor consisted of three individual cells assembled together and separated by anion-exchange (AEM) and cation-exchange (CEM) membranes. During the experiments, four configurations of the membrane placements and solutions concentrations were studied. The obtained results showed the dynamics of the electro-activation process that allows obtaining electro-activated solutions with targeted properties such as pH and oxydo-reduction potential (ORP). It was possible to obtain electro-activated solutions at the anodic side (acid anolyte) with pH of 3.0, 3.5, and 4.0 and ORP of +1100 ± 15 mV when NaCl solution was used as electrolyte. Furthermore, several types of electro-activated solutions with high redox potential (ORP = +921 ± 12 mV) and neutral pH (6.48 ± 0.05) were obtained on the anode side when sodium carbonate was used. At the same time, two types of solutions, one with acid pH (2.14 ± 0.14) and the other one with alkaline pH (10.46 ± 0.03) with ORP = +689 ± 10 and 110 ± 21 mV, respectively, were obtained in the central compartment which considered as electro-activated solutions obtained by means of noncontact electro-activation.  相似文献   
3.
Accurate quantification of dissolved organic nitrogen (DON) has been a challenge due to the cumulative analytical errors in the conventional method via subtracting dissolved inorganic nitrogen species (DIN) from total dissolved nitrogen (TDN). Size exclusion chromatography coupled with an organic nitrogen detector (SEC-OND) has been developed as a direct method for quantification and characterization of DON. However, the applications of SEC-OND method still subject to poor separations between DON and DIN species and unsatisfied N recoveries of macromolecules. In this study, we packed a series of SEC columns with different lengths and resin materials for separation of different N species and designed an independent vacuum ultraviolet (VUV) oxidation device for complete oxidation converting N species to nitrate. To guarantee sufficient N recoveries, the operation conditions were optimized as oxidation time ≥ 30 min, injection mass (sample concentration × injection volume) < 1000 µL × mg-N/L for macromolecular proteins, and neutral pH mobile eluent. The dissolved O2 concentration in SEC mobile phase determined the upper limit of VUV oxidation at a specific oxidation time. Compared to conventional HW50S column (20 × 250 mm), HW40S column (20 × 350 mm) with mobile phase comprising of 1.5 g/L Na2HPO4·2H2O + 2.5 g/L KH2PO4 (pH = 6.85) could achieve a better separation of DON, nitrite, nitrate, and ammonia. When applied to river water, lake water, wastewater effluent, groundwater, and landfill leachate, the SEC-OND method could quantify DON as well as DIN species accurately and conveniently even the DIN/TDN ratio reached 0.98.  相似文献   
4.
氯甲基甲醚(CMME)和二氯甲基醚(BCME)属于确认人类致癌物,因此,建立精准、绿色的CMME和BCME检测分析方法十分必要。基于2,4,6-三氯苯酚+乙醇钠+乙醇衍生化体系,利用气相色谱法(电子捕获检测器)测定了固定污染源废气中的CMME和BCME,并且系统地优化了采样条件、衍生化条件,确定了衍生化产物的结构及衍生比率。结果表明:工作曲线相关系数均大于0.990;当采样量为10 L时,检出限均为0.003 mg/m3;当实际样品加标量分别为0.010、0.100、1.00 mg/m3时,测定结果的相对标准偏差分别为15%~16%、8.9%~13%、10%~11%,加标回收率分别为89.2%~90.8%、75.3%~78.6%、76.5%~77.2%。  相似文献   
5.
建立了罐采样-气相色谱法测定环境空气中非甲烷总烃的分析方法。用罐采集环境空气样品至微负压状态,经除烃空气加压后,用气相色谱仪进行分析。并对氮气空白、除烃空气、样品保存期限、不同压力进样、不同正压压力进样、不同湿度、不同种类物质对总烃的贡献等进行了研究,在最佳实验条件下,非甲烷总烃的方法检出限为0.04μmol/mol,标准曲线相关系数均大于0.999 5,低、中、高浓度水平测定结果相对标准偏差均小于2.0%,低、中、高浓度的质控样品相对误差均小于2.0%。利用该方法对环境空气样品进行了检测分析,该法完全满足国家标准质控的要求,适用于环境空气和污染源无组织废气中非甲烷总烃的准确测定。  相似文献   
6.
固定污染源氨气的手工监测,干扰因素较多,其中采样环节尤为关键。实验通过催化氧化-化学发光法考察不同采样管线材质对氨气的吸附效果,离子色谱法考察化学吸收法采集氨气的吸收瓶类型、采样流量、吸收液种类、吸收液浓度及体积等采样条件对氨气吸收效率的影响。实验表明,316 L不锈钢与聚四氟乙烯对氨气的吸附较小,氨气的采样流量不宜超过1.0 L/min,棕色气泡式吸收瓶更适用于氨气样品的采集,磷酸溶液作吸收液对氨气的吸收效率较好,对于低浓度的氨气样品,应采用低流量长时间采集。  相似文献   
7.
采用固相萃取-高效液相色谱-串联质谱法(SPE-HPLC-MS/MS)建立了地表水中25种抗生素类药物和8种非抗生素类药物的分析方法。通过重点优化质谱参数、色谱条件、样品pH、洗脱溶剂组成及用量等确定了最佳分析条件。水样经过滤、固相萃取柱富集净化后,选择Shim-pack XR-ODS为色谱柱,以乙腈和0.2%甲酸-2 mmol/L乙酸铵-水溶液为流动相进行梯度洗脱,采用电喷雾电离源,在多反应监测模式下(MRM)分析测定,内标法定量。33种药物的仪器定量限为0.012~4.68 ng/L,方法检出限为0.011~7.60 ng/L,地表水加标回收率为53.7%~122%,相对标准偏差为1.22%~32.1%(n=6)。方法成功应用于北京市凉水河12个地表水样分析,共检出32种药物,检出质量浓度为未检出~239 ng/L。利托那韦(RTV)作为新型冠状病毒诊疗方案中推荐的药物在凉水河检出率为100%。  相似文献   
8.
梯度淋洗离子色谱法测定饮用水中6种阴离子   总被引:1,自引:0,他引:1  
采用离子色谱法同时测定饮用水中F-、Cl-、Br-、NO3-、SO24-、PO34-等6种阴离子,水样经0.22μm滤膜过滤,自动淋洗发生器产生20 mmol/L~40 mmol/L KOH淋洗液梯度洗脱,在流量0.25 mL/min条件下采用IonPac AG19保护柱和IonPac AS19分离柱分离和定量。方法线性良好,6种阴离子的检出限为0.005 mg/L~0.057 mg/L,标准溶液平行测定6次,测定值的RSD在0.5%~2.2%之间,水样加标回收率在83%~106%之间。  相似文献   
9.
文章建立了使用气相色谱仪分析气田产出水中甲醇含量的方法。通过实验在设定不同分流比的情况下,能有效监测出气田产出水中不同浓度的甲醇含量,此方法灵敏度高,最低检出限为0.02%,测定气田产出水中甲醇加标回收率达到93%~94%。  相似文献   
10.
温州近海海域海水及滩涂沉积物中PFOS和PFOA污染特征分析   总被引:2,自引:1,他引:1  
为了解温州近海海域全氟辛烷磺酸(PFOS)和全氟辛酸(PFOA)的污染状况和特征,采用固相萃取/高效液相串联质谱检测法分析了采自乐清湾、瓯江口、西湾、飞云江口及洞头半屏岛的近海海水和滩涂沉积物中PFOS和PFOA污染水平。结果显示,温州近海海水普遍存在PFOS和PFOA污染,其中,PFOS的浓度范围为<1.0~31.36 ng/L,中位浓度为2.29 ng/L;PFOA的浓度范围为<1.0~23.66 ng/L,中位浓度为5.29 ng/L。滩涂沉积物样品中PFOS和PFOA的浓度范围(干重)分别为(<1.0~11.91)×10-9(中位浓度为3.60×10-9)和(1.84~34.01)×10-9(中位浓度为6.83×10-9)。温州近海海水中PFOS和PFOA的污染水平明显高于香港沿岸、中国南海海水、韩国沿岸海水和近海珠江三角洲,与大连湾的海水相当,海岸滩涂沉积物中的PFOS和PFOA浓度远高于珠江和黄浦江沉积物中的浓度。  相似文献   
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