硝酸银沉淀—颗粒物返还法去除COD样品的氯化物

将样品中的颗粒物分离出来，向样品加入适量硝酸根，除去生成的氯化银沉淀，再将预先分离的颗粒物合并到水样中，混匀后测定，经过这样处理，既去除了水样中的Ｃｌ，以保留了水样中原来的组份，保证了ＣＯＤ测定结果的准确性。     

沉降时间对地表水铁锰测定的影响

地表水中铁锰总量的高低是评价水质优劣的重要指标。地表水中铁锰总量与总悬浮颗粒物浓度成正比。地表水中铁锰主要来源于悬浮颗粒物的吸附,溶解态铁锰很少。水样中铁锰含量随自然沉降时间的延长而逐渐降低。而当水样自然体系中加入硝酸后情况有所不同。因此,样品采集后自然沉降时间是影响测定结果的一个主要原因之一。     

AMA254汞分析仪测定颗粒物中痕量总汞的研究

采用AMA254汞分析仪测定大气颗粒物和煤中的痕量总汞,建立了直接测定颗粒物中痕量总汞的分析方法.测定结果表明,在汞绝对含量为0～35ng范围内线性良好,测定大气颗粒物和煤中的痕量总汞的检出限分别为0.06ng/m3和0.02ng/g,标准样品测定的RSD≤0.78%,加标回收率为92%～108%.该方法具有无需消解直接进样测定、极其简便、省时等特点,适合多种固体样品中痕量汞的测定.     

环境中萘和甲基萘的气相色谱测定

针对发生的甲基萘油车泄漏事故进行了水样和空气样品中萘和甲基萘的测定，水样中直接进样，对空气样品则以甲醇为吸收液吸收，富集，氢火焰毛细管色谱法测定。     

多波长K系数方程法同时测定水样中的Cu~(2+)、Co~(2+)、Cd~(2+)

多波长Ｋ系数方程法同时测定水样中Ｃｕ２＋、Ｃｏ２＋、Ｃｄ２＋,即选定三个测定波长,分别将三组分在两个波长处的吸光度转换为另一波长处的吸光度,即可列出一个多元一次方程组,进而解出此波长处各组分的吸光度,求得各组分的含量。对水样中的Ｃｕ２＋、Ｃｏ２＋、Ｃｄ２＋三组分同时测定,结果令人满意。     

完全氧化法测定高氯废水的COD_(Cr)

从热力学的角度出发,导出了在ＣＯＤ测定过程中Ｃｌ－ 的完全氧化条件。通过不同浓度的含氯邻苯二甲酸氢钾标准溶液和含氯乙醇标准水样的测定表明, 在所提出的完全氧化条件下,由所测得的表观ＣＯＤ减去Ｃｌ－ 的理论ＣＯＤ便得到水样的真实ＣＯＤ,测定结果与实际吻合较好。最后,对测定过程中的有关问题进行了讨论。     

水中微量五氯酚的气相色谱法测定

提出ＧＣ－ＦＣＤ分析方法测定水中微量五氯酚残留量。水样经萃取分离、衍生后，采用石油醚提取醋酸五氯酚酯，然后进入色谱柱，柱内填充２％ＯＶ－１７＋２％ＱＦ－１／ＣｈｒｏｍｏｓｏｒｂＷ－ＨＰ（８０～１００目），柱温２００℃，Ｎ＿２流量８０ｍＬ／ｍｉｎ，五氯酚酯３ｍｉｎ内出峰，最低检测浓度为０．１μｇ／Ｌ，各种样品回收率均在９０％以上，样品测试结果满意，可用于多种水体中微量ＰＣＰ残留量的测定。     

废气颗粒物中常见金属元素测定方式的优化

建立微波消解ICP-MS(电感耦合等离子体质谱法)测定废气颗粒物中常见的金属元素。将国产玻璃纤维滤筒与进口石英滤筒对比,最终选用国产玻璃纤维滤筒。样品采集后,选用HNO_3+HF+H_2O_2的消解体系,并在选定的消解参数条件下,得出这10种金属元素在0-50μg/L范围内线性良好,实际样品平行测定精密度RSD为1.8%～4.8%。此法可用于第三方检测公司批量测定废气颗粒物中的金属元素。     

测定地面水中Cr~(6+)的回收率问题的探讨

测定地面水中Ｃｒ６＋的回收率问题的探讨马文英张占银（河北邢台市环境保护局，邢台０５４０００）色度很深的水样，用锌盐沉淀分离法进行预处理脱色后还应消除氧化性物质方可进行Ｃ６＋ｒ测定，这是绝对不可忽视的一个关键。消除氧化性物质的处理步骤：水样置于１５０ｍ...     

地面水中氨氮样品稳定性试验

对三氮进行保存时间稳定性试验,结果发现,除硝酸盐氮、亚硝酸盐氮不宜保存外,１０００ｍｌ地面水氨氮水样滴加５ｍｌ硫酸酸化至ｐＨ＜２可抑制水样中氨氮的水解、氧化还原反应。水样于２０°Ｃ～２８°Ｃ温度下保存半个月,氨氮测定结果基本无影响,同一水样在不同时间所测数据经方差分析,Ｆ计＜Ｆ０．０５,无显著性差异。表明,本法保存氨氮水样,半个月后仍相当稳定,便于调整分析人员工作量。地面水中氨氮样品稳定性试验@周秀华$平湖市环境监测站!浙江平湖314200     

Multivariate cluster analysis as a versatile tool for the quality assessment of short chain chloroparaffin quantification in environmental samples

The compositions of commercially available solutions of short chain chlorinated paraffins (SCCP) and technical mixtures were determined by high resolution gas chromatography (HRGC) electron capture negative ionisation (ECNI) combined with low resolution mass spectrometry (LRMS). Differences and similarities in the relative distribution of congeners and homologues were investigated by cluster analysis. Samples could be separated into two groups/clusters with similar molecular mass, chlorination degree and congener pattern. With the exception of one sample, the use of CH4-ECNI-MS led to an overestimation of the chlorine content. Moreover, the influence of different SCCP mixtures on the quantification was studied. The results showed that small differences in the chlorine content could sometimes cause substantial systematic errors of up to 119% despite similar homologue and congener patterns. Errors of quantification corresponded to the deviations between response factors of sample and standard. As a consequence SCCPs should be quantified with a standard matching the overall response factor of the sample.     

快速测试管法现场测定水中总余氯

余氯在水中极不稳定 ,需现场测定。通过研制一种测试管 ,从而能快速、简便地测水中的总余氯。常规法测定时间需要 3～ 5小时 ,而该测试管法仅需 1 0分钟。分析成本也大为降低     

测定游离氯和总氯样品保存方法研究

建立了游离氯和总氯样品保存方法。用氢氧化钠溶液作为固定剂,现场固定含有游离氯和总氯的水样,使水样pH>12。结果表明,样品经4℃低温避光保存,5 d内测定,测量结果没有显著变化,方法检出限(以Cl2计)为0.004mg/L,加标回收率为96.7%～104%。     

固相微萃取-气相色谱在水中有机污染物测定中的应用

固相微萃取技术是一种新型的无溶剂的样品前处理方法,集取样、萃取、富集、进样于一体,具有无溶剂、可直接进样、操作简便快捷、灵敏的特点。简述了固相微萃取技术原理,综述了SPME与GC联用在水中有机污染物测定中的应用。具体介绍了该技术在苯系物、酚类化合物、多环芳烃、有机氯化物及其它有机污染物分析中的应用,并提出了该技术的发展趋势及应用展望。     

Uranium oxide and other airborne particles deposited on cypress leaves close to a nuclear facility

Enhanced activity of actinides and some decay products has been reported for the leaves of cypress trees (Chamaecyparis nootkatensis) at the edge of the Malvési uranium-processing facility, southwestern France. The enhanced activity is due to the release of actinides via the smokestacks and from artificial ponds inside the facility. This study was conducted to characterize airborne particulate matter deposited on the leaf surfaces and to investigate whether or not radioactive particles may be identified. Air-dried leaf samples were examined by scanning electron microscopy, in combination with energy-dispersive X-ray spectrometry. The samples were scanned systematically in both secondary and backscattered electron modes. Particles ranging in size from <200 nm to ~40 μm were found on most portions of the adaxial leaf surface, but they are especially abundant at the boundary between facial and lateral leaves. The majority of the analyzed particles could be attributed to five principal classes: carbonates, silicates, sulfates, oxides/hydroxides, and halides. In addition, other types of particles were found, including Fe alloys; scheelite-group phases; phosphates; sulfides; and fly ash spheres. Similar particles were also observed on the surface of a wheat sample used for comparison. Of special interest are U-rich particles, which were observed on the cypress leaves only and which were identified as U oxides, except for one particle, which was a U-oxide-fluoride. These U-rich particles were released into the atmosphere by the nuclear facility prior to their deposition on the leaf surfaces. As most of the U-rich particles are <2.5 μm across, they are respirable. Once inhaled, particles containing alpha-emitting isotopes represent a potentially long-term source of ionizing radiation inside the lungs and thus, pose a threat to the health of people living nearby.     

高氯离子废水化学需氧量分析方法的研究

提出一种测定高氯离子废水 COD的新方法。其消解条件与现行国标法基本相同 ,消解过程产生的氯气用Na OH吸收并测定出氯离子的 COD校正值。由表观 COD值减去氯离子的 COD校正值 ,即为水样的真实 COD值。标样的相对误差在 -1.5 %～ 5 %之间 ,RSD%≤ 5 .5 %。高氯废水的 RSD%≤ 8.0 %。     

关于DPD光度法测游离氯操作步骤的几点分析

对N,N-二乙基-1,4-苯二胺(DPD)分光光度法测游离氯的3个较权威的版本的操作步骤在显色效果、显色物稳定性、标准曲线和实测样品结果方面进行了对比,对<水质游离氯和总氯的测定N,N-二乙基-1,4-苯二胺分光光度法>(GB 11898-1989)操作步骤提出了一点改进建议.     

Analysis for Chemical Characterization of Atmospheric Aerosols Application of X-ray Microprobe System and Double Thin Film Method

The X-ray microprobe system was applied to ultra trace characterization of single Kosa aerosols and non-Kosa aerosols simultaneously collected at Yasaka, Japan and TaeAnn, Korea. We demonstrated remarkable mass increase of heavy metals as well as soil components in individual particles during the Kosa event compared with the non-Kosa period at Yasaka. Backward trajectory analysis suggested that the Kosa samples were in the mixing state of mineral components and anthropogenic heavy elements. Double thin film method was applied to investigate the seasonal change of the mixing states of single sea-salt aerosols associated with chlorine loss due to the heterogeneous reactions between sea-salt particles and acidic gases. It was revealed that the percentages of both chloride-nitrate mixed particles and sulfate-nitrate ones were larger in wintertime than those in summertime and fraction of chloride-nitrate mixed particles increased with an increase of particle size. Comparison between the size-segregated bulk analysis and the single particle analysis demonstrated that remarkable chloride depletion occurred in coarse particles sampled on May in the former analysis, while chloride depletion in coarse particles was not marked in the latter analysis. The discrepancy attributes to the difference of the sampling time between both analyses because significant change of air mass route occurred during the bulk sampling after completion of the single particle sampling.     

Determination of an acceptable assimilable organic carbon (AOC) level for biological stability in water distribution systems with minimized chlorine residual

There is considerable interest in minimizing the chlorine residual in Japan because of increasing complaints about a chlorinous odor in drinking water. However, minimizing the chlorine residual causes the microbiological water quality to deteriorate, and stricter control of biodegradable organics in finished water is thus needed to maintain biological stability during water distribution. In this investigation, an acceptable level of assimilable organic carbon (AOC) for biologically stable water with minimized chlorine residual was determined based on the relationship between AOC, the chlorine residual, and bacterial regrowth. In order to prepare water samples containing lower AOC, the fractions of AOC and biodegradable organic matter (BOM) in tap water samples were reduced by converting into biomass after thermal hydrolysis of BOM at alkaline conditions. The batch-mode incubations at different conditions of AOC and chlorine residual were carried out at 20°C, and the presence or absence of bacterial regrowth was determined. The determined curve for biologically stable water indicated that the acceptable AOC was 10.9 μg C/L at a minimized chlorine residual (0.05 mg Cl₂/L). This result indicated that AOC removal during current water treatment processes in Japan should be significantly enhanced prior to minimization of the chlorine residual in water distribution.     

Ascorbic acid reduction of residual active chlorine in potable water prior to halocarboxylate determination

In studies on the formation of disinfection byproducts (DBPs), it is necessary to scavenge residual active (oxidizing) chlorine in order to fix the chlorination byproducts (such as haloethanoates) at a point in time. Such research projects often have distinct needs from requirements for regulatory compliance monitoring. Thus, methods designed for compliance monitoring are not always directly applicable, but must be adapted. This research describes an adaptation of EPA Method 552 in which ascorbic acid treatment is shown to be a satisfactory means for reducing residual oxidizing chlorine, i.e., HOCl, ClO-, and Cl2, prior to determining concentrations of halocarboxylates. Ascorbic acid rapidly reduces oxidizing chlorine compounds, and it has the advantage of producing inorganic halides and dehydroascorbic acid as opposed to halogenated organic molecules as byproducts. In deionized water and a sample of chlorinated tap water, systematic biases relative to strict adherence to Method 552 were precise and could be corrected for using similarly treated standards and analyte-fortified (spiked) samples. This was demonstrated for the quantitation of chloroethanoate, bromoethanoate, 2,2-dichloropropanoate (dalapon), trichloroethanoate, bromochloroethanoate, and bromodichlorocthanoate when extracted, as the acids, into tert-butyl methyl ether (MTBE) and esterified with diazomethane prior to gas chromatography with electron capture detection (GC-ECD). Recoveries for chloroethanoate, bromoethanoate, dalapon, dichloroethanoate, trichloroethanoate, bromochloroethanoate, bromodichloroethanoate, dibromoethanoate, and 2-bromopropanoate at concentrations near the lower limit of detection were acceptable. Ascorbic acid reduction appears to be the best option presently available when there is a need to quench residual oxidants fast in a DBP formation study without generating other halospecies but must be implemented cautiously to ensure no untoward interactions in the matrix.