在线衍生化吹扫捕集-气相色谱/质谱分析水中的五氯酚

建立了通过乙酸酐衍生化-吹扫捕集-气相色谱／质谱分析水中五氯酚的新方法，探讨了吹扫时间、样品池温度、离子强度以及衍生化试剂的加入量等条件对捕集效果的影响。结果表明：采用吹扫时间25min、样品池温度60℃、离子强度20％氯化钠以及衍生化试剂的量200μl等条件对水中的五氯酚有较好的捕集效果，用于水中五氯酚的测定，结果满意。     

Associations of trace elements in aerosol at the south Adriatic coast

We applied statistical methods to the data of a 5-year sampling period to characterize the features of trace elements in airborne particulate matter at the South Adriatic Coast. The analysis of surface soil samples was also performed. The data were processed by cluster analysis, enrichment factor determination and receptor rose statistics. It is shown that the principal element association consists of Fe, Mn and Ti originating from surface material resuspension. Hg and Se were shown to originate from more complex natural and anthropogenic processes. A strong emission source of Cd and Se was identified in the SSE direction.Selected article from the Regional Symposium on Chemistry and Environment Krusevac, Serbia, June 2003, organized by Dr. Branimir Jovancicevic.     

LC-MS/MS determination of pesticide residues in fruits and vegetables

The aim of the research is to evaluate pesticide residue contamination of fresh and frozen fruits and vegetables, agricultural raw material, purchased from Polish farmers for production of frozen fruits and vegetables, and the estimation of the multiresidue method effectiveness expressed as the proportion of pesticides detected in food samples to the total number of pesticides analyzed by multiresidue methods. A total of 144 samples (of black currants, red currants, raspberries, cherries, strawberries, blackberries, cauliflowers and broccoli) were analyzed using LC-MS/MS method for the determination of 60 pesticides. QuEChERS extraction, matrix-matched calibration and dynamic multiple reaction monitoring method were used. Residues of 15 compounds, mainly fungicides and insecticides, were detected in 46 samples. The percentage of samples with residues above the maximum residue levels (MRL) was 15%, whereas samples with residues below MRL were 17%. A total of 13 samples contained more than one pesticide residue. Pesticide residues were detected most often in samples of black currants (50%), broccoli (36.4%), raspberries (29%) and red currants (21.8%). The most frequently detected pesticides were carbendazim and acetamiprid. The proportion of pesticides detected during our study to the total number of analyzed pesticides amounted to 25%. It was compared to literature findings. For three fourth of multiresidue methods, the proportion was below 50% for methods developed for the analysis of less than 100 pesticides, and below 30% for methods developed for the analysis of more than 100 pesticides. It appears that a lot of efforts and means is lost on pesticides never or rarely detected in examined samples. The workload and cost effectiveness of the development and application of multiresidue methods along with the range of pesticides covered by the method should be carefully and thoroughly considered anytime when a new method or workflow is developed. Including non-targeted screenings in pesticide residue control seems to be an alternative worth considering.     

新型固体进样汞镉测定仪测定固体样品中的镉

使用由北京吉天仪器有限公司开发的新型固体进样汞镉测定仪(DCMA-200),对采集的土壤、大气颗粒物和固体废物样品中镉的浓度进行分析。在测试过程中,选择9种标准土(GBW07407、GBW07402、GBW07410、GBW07425、GBW07426、GBW07428、GBW07419、GBW07309和GBW07418),研究了进样量对测定的影响,并分别在1.0~10.0 mg称量范围内建立了标准曲线(R ²> 0.93)。当固体样品进样量为10.0 mg时,镉的检出限为0.004 7 mg/kg,测定下限为0.016 mg/kg。利用7种标准土(GBW07418和GBW07419除外)绘制的标准曲线,测得的5种实际土壤中镉的浓度与利用电感耦合等离子体质谱仪(ICP-MS)测得的结果较一致。但与ICP-MS测得的结果相比,利用该固体进样汞镉测定仪测得的大气颗粒物中镉的浓度明显偏高,而危险废物中镉的浓度偏低。因此,建议在检测某地区的固体样品时,尽可能选择该区域和该类固体样品的标准品来设计标准曲线,从而提高测试结果的准确性。     

荧光素酶报告基因法测定废气中二英类物质

研究二噁英类生物检测法的主要目的是简化二噁英类分析流程,并找出快速检测的结果与HRGC-HRMS(高分辨气相色谱-高分辨质谱)结果之间的换算系数,从而可以利用快速检测的结果和换算系数来推算HRGC-HRMS的结果. 介绍了CALUX(荧光素酶报告基因法)分析废气中二噁英类物质的原理,并采用该方法分析了我国27个废气样品,以期找出其测定结果与HRGC-HRMS结果之间的换算系数. 结果表明,这2种测试方法数据相关性显著,R2为0.994 8,数据间的换算系数为0.379. 试验表明,CALUX法具有很好的推广性,如果再适当增加废气样品的数量,对换算系数进行适当的优化,则所得换算系数可推广.      

火焰原子吸收法测定苹果中波尔多液的农药残留

通过原子吸收法测定苹果果皮、果肉上波尔多液的农药残留铜的含量,结果表明:喷洒了波尔多液的苹果果皮上铜含量明显大于果肉,在果皮上有一定的农药残留;而未喷洒波尔多液的苹果果皮和果肉中铜的含量的差异很小。     

混合酸消解变化对土壤和沉积物中痕量硒分析影响

基于各3种采集环境样本、国家标准物质的土壤和沉积物,以当前环境监测行业常用的3种消解方法,探讨20种混合酸系统条件在消解条件变化中对复杂样本硒元素测定的影响.确定了最佳土壤和沉积物消解的组合为王水系统(盐酸∶硝酸∶氢氟酸∶过氧化氢∶高氯酸=3∶1∶1∶1∶1),各消解法的处理结果部分(n=5):水浴法消解时间仅需0.5...     

军用浸渍活性炭中银含量测定方法——火焰原子吸收分光光度法

本研究建立了一种用空气-乙炔火焰原子吸收分光光度法测定浸渍活性炭中银含量的分析方法，对酸介质浓度、共存元素的干扰进行了探讨，在0—1．0ml沪范围内，银含量与吸光度呈线性关系，相关系数为0．9999。对09型浸渍活性炭标准物质进行测定，测定结果的相对标准偏差为0．191％（n=10），加标回收率为97．5％-101．4％。     

红外法测定石油类项目中标准曲线的简化绘制

目前GB/T164 88-1996以红外分光光度法这测定石油类的有一种方法。该法用四氯代碳作莘取剂 ,四氯化碳用量大。四氯化碳是一种有毒、挥发性较强的有机溶剂。在监测该项目时 ,绘制标准曲线所用的标准储备液的配制相当复杂且形成的系统误差比较大 ,为减少误差并准确地绘制标准曲线 ,本文采取了简化配制步骤的方法来绘制曲线 ,并达到了与JDS -10 0型红外分光测油仪使用说明书中提供的方法一致的效果。     

基于单颗粒质谱技术的石家庄冬春季气溶胶成分特征及混合状态研究

利用位于石家庄市大气梯度监测站(20 m)的单颗粒气溶胶质谱仪分析了冬、春季大气环境中气溶胶的化学组成及混合状态,并采用ART-2a分类法对气溶胶分类。结果表明,石家庄市大气中主要存在8类颗粒物,即元素碳(EC)、有机碳(OC,相对分子质量小于150)、高分子有机碳(HOC,相对分子质量大于150)、混合碳(元素-有机碳混合,ECOC)、重金属、左旋葡聚糖碎片(LEV)、矿物质和富钾颗粒。8类颗粒中绝大部分包含SO_4~-、NO_2~-和NO_3~-等二次离子组分,表明采集到的颗粒物大都经历了不同的老化,或与二次组分进行了不同程度的混合。冬季气溶胶的主要成分是OC(数浓度36.1%),谱图含有C2H+3、C_2H_3O~+、C_5H_3~+、C_6H_5~+等离子,主要来自化石燃料、生物质等燃烧产生的一次排放颗粒,以及由挥发性有机物光化学氧化而成的二次有机颗粒;春季气溶胶的主要成分是EC(数浓度43.6%)和矿物质(数浓度15.4%)。EC中含有一系列单质碳峰,来自化石燃料或木材等生物质不完全燃烧的一次排放;矿物质颗粒中含有Mg~+、Al~+、Ca~+、Fe~+及SiO_3~-,主要来自扬尘。发生灰霾时,冬季OC和ECOC颗粒占比增大,EC颗粒占比减小;春季矿物质和ECOC颗粒占比变大,OC颗粒占比变小。随着灰霾天气发生,冬、春季碳气溶胶与二次无机气溶胶颗粒的混合加剧,而NH_4~+与碳气溶胶的混合加剧最为明显。冬季气溶胶的数浓度与气象因素的相关性高于春季,而低风速、高湿度和低气压易导致灰霾出现。石家庄市春季和冬季气溶胶污染应分别从机动车尾气、扬尘及燃煤、制药企业加以管控。