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1.
研究依据测定不确定度的基本理论和ISO 21748:2017《采用重复性、再现性和正确度评估测量不确定度的导则》,提出了基于中国环境监测分析方法标准多家实验室验证中已获得的数据计算合成标准不确定度的方法,将方法标准中规定的重复性、再现性等指标与合成标准不确定度进行了衔接。分析了近年发布的6项水质监测分析方法标准中钴、铬、钼、钛等4种金属元素的相对合成标准不确定度,结果表明:被测量的浓度是影响方法标准测量不确定度的重要因素。对于火焰原子吸收分光光度法(FAAS)和石墨炉原子吸收分光光度法(GAAS),样品浓度为方法标准测定下限3倍左右时,测定结果的相对标准不确定度可保持在15%以下;对于电感耦合等离子体发射光谱法(ICP-AES),样品浓度为方法标准测定下限3~5倍时,测定结果的相对标准不确定度为12%~17%;对于电感耦合等离子体质谱法(ICP-MS),钛元素浓度为测定下限3倍左右时,相对标准不确定度在15%以下,而钴、铬、钼的浓度在测定下限40~100倍以上时,相对标准不确定度在15%以下。6项方法标准可分别用于《地表水环境质量标准》(GB 3838—2002)以及22项水污染物排放标准钴、铬、钼、钛的达标监测。  相似文献   

2.
采用超细玻璃纤维滤膜采集环境空气中钴,硝酸-过氧化氢-氢氟酸混合进行消解,采用硝酸镁和硝酸混合液作为基体改进剂,石墨炉原子吸收光谱法测定环境空气中钴。此方法对测定环境空气中钴的灵敏度、准确度都有很大的提高,方法的最低检出浓度为0.25μg/L,当采样体积为100 L,钴最低检出质量浓度为0.000 1 mg/m3。对实际样品进行分析,钴的加标回收率为91.0%~106.5%。  相似文献   

3.
ICP-MS法同时测定地表水中18种金属元素   总被引:3,自引:1,他引:2  
以115In-103Rh为双内标校正系统,采用电感耦合等离子体质谱法同时测定地表水中铜、锌、硒、砷、汞、镉、铅、铁、锰、钼、钴、铍、锑、镍、钡、钒、钛、铊等18种金属元素,优化了测量同位素、内标元素等试验条件。18种金属元素在0μg/L~100μg/L范围内线性良好,检出限为0.006μg/L~0.123μg/L,标准样品的测定值均在保证值范围内,平行测定的RSD为1.7%~4.2%,实际水样加标回收率为89.0%~100%。  相似文献   

4.
闽东某钼矿周边农田土壤钼和重金属的污染状况   总被引:7,自引:1,他引:6  
调查了闽东某钼矿周边农田土壤和稻米钼及重金属的污染状况,对土壤钼的人体健康风险进行了评价,探讨了土壤钼的安全阈值。结果表明,部分土壤遭受了铜和镉的污染,以轻度污染为主;部分稻米出现镍和镉的污染,以轻度污染为主;土壤全钼含量为3.30~325.6 mg/kg,最高值高出福建省土壤中钼的环境背景值87倍,说明该区土壤已遭受严重的钼污染。稻米钼含量为0.58~12.04 mg/kg,对人体具有很高的健康风险;根据稻米钼含量与土壤钼含量之间的关系和人体健康风险评价结果,推算出土壤中钼(全钼)的安全阈值不高于4.51 mg/kg。  相似文献   

5.
本文借5-Br-PADAP与CPB体系显色,用卡尔曼滤波-分光光度法同时测定钴镍铜锌镉五组分混合物,本方法用于合成试样、水、头发、指甲等环境样品分析,结果较好。  相似文献   

6.
在文献的基础上,利用钼磷酸在浓硫酸作用下于乙醇介质中优先氧化萜烯酸及其衍生物,而本身被还原为钼兰的性质,本文建立了测定矿山废水中松脂油的方法,方法检出限为0.006mg/5ml,回收率在88%—107%之间,相对标准偏差为5.05%。本文还对钼磷酸的溶剂选择,钼磷酸和浓硫酸的用量对吸光度的影响,以及浓盐酸的用量对萃取效率影响做了详细研究。  相似文献   

7.
我国的环境监测分析方法种类较少、更新较慢,新技术和新仪器的开发较为滞后,有些监测项目在缺乏标准和统一方法的情况下,可采用美国EPA等效分析方法。美国EPASW-846报告中收录了307个测试方法,《EPA测试方法索引》。中收录了1613个测试方法,其中数字编号方法1036个,非数字编号方法577个,  相似文献   

8.
本文研究了5-Br-PADAP-乳化剂OP分光光度法测定钴、镍、铜的适宜条件以及同时测定的卡尔曼滤波算法。建立了不经分离直接测定三组分的灵敏度与选择性均较好的方法。用于某些环境样品分析,结果良好。  相似文献   

9.
采用碱熔-钼锑抗分光光度法测定土壤中总磷时,显色溶液的酸度影响磷钼络合物的形成和稳定,p H指示剂2,4-二硝基苯酚在环境温度低时配制困难、辨色不明显。分析了显色酸度对吸光值的影响,并对2,4-二硝基苯酚的配制方法进行了改进,方法操作简单,提高了分析结果的准确性。  相似文献   

10.
用0.50 mol/L碳酸氢钠溶液浸提中性和石灰性土壤中的有效磷.碳酸氢钠可以抑制溶液中Ca2+的活度,使某些活性较大的磷酸钙盐被浸提出来,同时也可使活性磷酸铁、铝盐水解而被浸出.浸提液与钼锑抗显色剂反应生成磷钼蓝,在波长880 nm处测量吸光度.当取样量为2.50 g时,使用50 mL碳酸氢钠溶液浸提,使用1 cm比...  相似文献   

11.
The Ko factor method in neutron activation analysis adopts all the principles of comparator method and can be used for the rapid determination of elemental comcentrations during routine monitoring of environmental samples. The method necessiates the use of same in-pile conditions, such as irradiation time, irradiation position and the type of neutron spectrum, for which the factors have been generated. The K_o factors were estimated for various elements of environmental importance for three irradiation positions of Apsara Reactor at Bhabha Atomic Research Centre. Standard reference materials of soil and coal were used for all the elements except for Hg for which HgCl2 was used. The concentration of the elements determined using these factors in a flyash standard reference material revealed good agreement within 10% of the certified values. The efficacy of the method compared well with that of specific element comparator method as revealed by the elemental concentrations obtained by both the techniques.  相似文献   

12.
海洋沉积物中多种重金属的X射线荧光分析法   总被引:1,自引:0,他引:1  
建立了海洋沉积物中包括砷、铜、铅、锌、镍和总铬在内的多种重金属X射线荧光分析法,测量不需要任何消解前处理过程,可在约1h内测量1个样品中的50余种元素,用该方法分析了8个海洋沉积物标准样品,还与原子荧光光谱法或原子吸收分光光度法比对分析了2个实际样品,结果表明,该方法可信度较高,且具有快速、简便、高效等特点,是一种非破坏性分析方法。  相似文献   

13.
建立了一种电感耦合等离子体质谱测定土壤中微量稀土金属的方法.分析了土壤标准样品中的微量稀土元素,结果与标准值一致.土壤实际样品分析也得到可靠结果.该方法样品采用微波溶样,灵敏度高,是一种比较可靠的微量稀土元素分析新方法.  相似文献   

14.
The concentrations and distribution of the elements, including heavy metals such as As, Ba, Br, Co, Cr, Cs, Fe, Ga, K, Mn, Na, Rb, Sc, Sr, Th and Zn, were investigated in dated sediment cores of Nainital Lake located in the Himalayan region, in Uttar Pradesh state of India, which is considered as a remote background area. The concentrations of the elements were measured by instrumental neutron activation analysis using the k0 method. The International Atomic Energy Agency certified reference material SL-3 was used to evaluate the accuracy of the method. The normalized data for a series of elements were used to understand the source of loading. Elements like Br, Co, Cr, Fe, K, Mn and Zn show a negative correlation with increasing depth whereas elements like As, Ba, Cs, Na and Rb show a positive correlation with increasing depth. By considering the concentration for the bottom segments of the core as close to the baseline concentration, recent flux values for different elements were calculated. An increase in the flux value was observed for Br, Cr, Fe, K, Mn and Zn, which can be attributed to anthropogenic contribution in recent years.  相似文献   

15.
以长春为例研究环境空气中TSP、PM_(10)和PM_(2.5)的相关性   总被引:2,自引:0,他引:2  
选取长春市解放大路与人民大街的交叉口为研究地点,分别进行TSP、PM10和PM2.5的采样和分析.然后利用相关系敷法和t检验对测定结果进行相关性分析,得到备元素的含量在三种污染物中的相关系敖:在TSP与PM10中为0.9349;在PM2.5与PM10中为0.8797;在TSP与PM2.5中为0.7824.得到各元素含量在三种污染物中的T检验统计值,在TSP与PM10中为0.90103;在PM2.5与PM10中为0.04745;在TSP与PM2.5中为0.047986.从分析结果可以看出,各元素含量在TSP与PM10中的相关性最好,在PM2.5与PM10中次之,研究结果为相关环境管理提供科学依据.  相似文献   

16.
ICP-MS在环境分析中的质谱干扰及其消除   总被引:6,自引:1,他引:5       下载免费PDF全文
针对环境领域20个无机元素的ICP-MS分析,总结了同量异位素、氧化物和双电荷、多原子离子等质谱干扰,探讨了影响质谱干扰的因素,提出了消除或降低每个元素质谱干扰的方法:选取合适的同位素、编辑校正方程、选择合适的模式、设置合理的等离子条件等,为建立ICP-MS相关环境标准方法提供参考。  相似文献   

17.
研究以单元素标准膜为基础,结合NIST SRM 2783颗粒物滤膜标准样品,建立了波长色散-X射线荧光光谱法测定PM2.5中23种无机元素的测定方法,优化了测试条件,测量一个样品耗时约15 min,计算了各元素的方法检出限。对NIST SRM 2783滤膜标准品在一周内重复测定10次来计算方法的准确度与精密度,测定结果显示大多数元素的测量值在给出的参考值范围内,且测量标准偏差一般在10%以内。对比了石英与聚四氟乙烯材质(Teflon)滤膜的空白值,石英滤膜中Si、Fe、Na、Mg、Al、K、Ca等元素的背景值较高,Teflon滤膜的背景值较低,推荐选用Teflon滤膜作为PM2.5组分分析采样滤膜。分别用波长色散-X射线荧光光谱法及酸消解-ICP-MS法测定了样品膜中的元素组分,得到的测定结果基本一致。  相似文献   

18.
电感耦合等离子体质谱法测定地下水中痕量元素   总被引:1,自引:0,他引:1  
张建中  孙亦静 《干旱环境监测》2012,26(3):133-135,157
采用电感耦合等离子体质谱法(ICP-MS)同时测定地下水中痕量元素。结果表明,ICP-MS可同时测定地下水中的16种元素,方法检出限为0.02~0.2μg/L,元素的精密度(RSD,n=5)为1.46%~4.36%,加标回收率为96.6%~105.6%,符合环境监测无机组份测试质量控制的要求。该方法应用于直接测定元素浓度范围在ng/L~mg/L级的实际地下水样品,具有样品前处理简单、干扰少、测定快速、元素同时分析、省时省力等优点。  相似文献   

19.
The aim of this work is to determine the content of essential and toxic elements in 25 raw propolis samples, when considering pollution agents and geographical and botanical factors. The microwave-assisted digestion was the most reliable and accurate method for determination of inorganic elements in propolis samples. The results were obtained using certified reference materials in a good agreement with certified values. Inductively coupled plasma atomic emission spectroscopy was used for the determination of 23 macro- and microelements (Ag, Al, As, B, Ca, Cd, Co, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, P, Pb, S, Sb, Se, Si, Sn, and Zn). A Mercury analyzer was also utilized for the detection of the total Hg. Among the analyzed metals, Ca, K, Mg, Zn, Si, S, Fe, Al, P, and Na were found to be the most predominant. Heavy metals (As, Cd, Hg, and Pb) were determined in minimal concentration, and Pb was the highest mean contained toxic (<3.80 mg/kg), without influence on provisional tolerable weekly intake values. The method can be applied for routine analysis and quality and environmental pollution controls of toxic elements in propolis samples. The results obtained indicate no pollution of the collection areas and naturally high concentration of Al (460?±?62.2 mg/kg).  相似文献   

20.
A study of the elemental leachability and retention capability of compost   总被引:2,自引:0,他引:2  
In this work a comparison is made between the different approaches that can be taken to evaluate the mobility of elements in compost. The practical consequences of the results obtained are also discussed in terms of methods for cleaning up compost and using compost in environmental remediation. The mobility of potentially toxic elements in compost is evaluated by leaching with four selected eluents, i.e. diluted sulfuric acid, oxalate, citrate and EDTA. In contrast to the chelating agents, diluted sulfuric acid was found to generally have a low leaching capability for removal of heavy metals from compost. This implies that the risk of heavy metal leaching caused by natural rainfall is likely to be low. The results obtained in the leaching experiment were compared with previous results obtained from sequential fractionation. This comparison confirmed that both methods gave similar results for predicting the lability of elements in compost. A non-linear regression analysis of the leaching curves was also conducted. The leaching curves for elements with high lability could be fitted with a two components model. The labile components identified by the kinetic model are approximately in accordance with the fractions obtained from the first step of the sequential extraction method. The kinetic speciation method is shown to be a relatively rapid and simple procedure for compost which gives more information about element lability than simple leaching experiments. The leaching reagents used in this work were not effective enough to be used for cleaning up compost with a high metal content. Compost was however shown to have a high affinity for heavy metals, with the order of affinity of metal for the compost being very similar to that seen for humic acid. Compost may therefore prove to be a good remediation material for metal contaminated waste.  相似文献   

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