玻璃纤维滤筒处理方法的探讨

就玻璃纤维滤筒经过不同条件的处理对固定污染源中的颗粒物浓度测定产生的影响进行了探讨。得出可行的滤筒处理方法。     

烟尘监测中应注意滤筒的质量控制

在烟尘监测中,采用玻璃纤维滤筒收集烟尘,实验室进行滤筒称量时,受实验室环境湿度、冷却时间、烘干时间等因素的影响,对监测结果有显著的影响,且呈现正误差。引入标准空白滤筒的恒重控制分析称量过程,可以消除这些因素引起的误差,提高烟尘监测分析质量。     

烟尘监测时采样滤筒的质量控制

介绍了合格滤筒的筛选方法和采样滤筒在实验室分析中的质量控制,分析了影响滤筒称量恒重的原因,指出空气湿度、冷却时间和烘干时间对滤筒称量恒重都有影响.     

影响滤简分析质量的主要因素和改进方法

介绍了影响滤简称量恒重的原因，指出空气湿度、冷却时间和烘干时间等对滤简称量恒重都有影响。提出使用标准空白滤筒、在平衡室中冷却、称量滤筒、并采用专用滤简盒和刚玉滤筒采样减小系统误差。     

氨法脱硫废气中烟尘测试方法的实验研究

利用重量法测试原理,将氨法脱硫外排废气中烟尘监测滤筒用二次水经过超声波洗涤后过滤,在烘箱内于105℃烘干2 h后称量恒重,除去滤简中的硫酸铵成分,从而准确获得烟尘的含量.     

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。     

滤膜在颗粒物无机元素监测中的适用性研究

筛选国内外12个制造商的玻璃纤维、石英、特氟龙、聚丙烯、乙酸纤维、硝酸纤维和混合纤维等7类材质34种滤膜,测定滤膜中的铍、铬、锰、钴、镍、铜、锌、砷、钼、镉、锡、锑、铊和铅等14种元素含量,探讨不同材质滤膜中各元素的质量分数分布,采用大气固定源污染物排放标准中项目限值和分析方法标准中质量控制要求,对铜、锌之外的12种元素进行适用性评价。结果表明:玻璃纤维滤膜比其他材质滤膜中无机元素的质量分数高1～5个数量级,进口玻璃纤维滤膜中铬、镍、砷、镉等4种元素质量分数高于多数国产玻璃纤维滤膜,国产A、H玻璃纤维滤膜中14种元素质量分数相对较低;仅混合纤维滤膜中镉、铅的测定值浓度低于最严标准限值的10%,玻璃纤维滤膜之外的其他材质滤膜均能满足监测其余10种元素的本底需求。     

烟尘滤筒称重方法的改进

针对在烟尘测试中滤筒的称重存在天平显示不稳、恒重难的现象进行了探讨。比较了2种称量方法，提出在平衡室中冷却、称量滤筒，并采用标准滤筒来减小由于称重条件不同而产生的系统误差。结果表明，改进方法具有称量稳定、易恒重、失重少的优势。     

不同采集原理的油烟采样方法研究

通过采用玻璃纤维滤筒采集、吸收液吸收和S材料滤筒采样三种不同采集原理的油烟采样方法的试验,研究出一种油烟采样新材料--SM材料,其填充后制成的S材料滤筒的油烟采集效率大于96%的采样方法.     

高通量固定污染源废气颗粒物中总汞的测定

用玻璃纤维滤筒采集固定污染源废气颗粒物,借助硝酸和氢氟酸的作用,使滤筒和废气颗粒物在160℃下消解,再用原子荧光法测定消解液中总汞。用50%热硝酸溶液处理玻璃纤维滤筒,消除滤筒本底值不一对测定结果的干扰,并优化消解过程,使该方法在0.050μg/L~1.00μg/L范围内线性良好。当采样体积为10 L时,方法检出限为4.5×10~(-5)mg/m~3,空白加标样6次测定结果的RSD为7.2%,加标回收率为87.0%~113%。将该方法用于测定某固定污染源废气颗粒物中总汞,测定值在标准排放限值内。     

A New Method for Determination of Chlorophylls in Freshwater Algae

A new method (NMM, using acetic acid fiber filter and 90% ethanol) was established to determine chlorophyll in freshwater algae, and it was compared with US standard method (USM, using glass fiber filter and 90% acetone) and the method recommend by EPA of China (CHM, using acetic acid fiber filter and 90% acetone). The precision and repeatability of NMM is equivalent to that of USM, but NMM is safer to laboratory workers than USM and CHM because ethanol was used as solvent in NMM instead of acetone used in USM and CHM, and time and money were also greatly saved by the new method. The precision and repeatability of CHM was much less than USM and NMM, and the advice improving the method was proposed that the extraction time must be prolonged.     

硫酸雾测试方法若干问题思考

简述了我国硫酸雾测试方法的发展历史,分析和总结了《固定污染源废气硫酸雾的测定离子色谱法》(HJ 544—2016)存在的一些争议和问题,包括硫酸雾的定义、测试方法的干扰控制等。分析认为,相比《硫酸工业污染物排放标准》(GB 26132—2010),HJ 544—2016对硫酸雾的定义更加合理。实验结果表明:硫酸盐是测试方法条件下的目标物,滤筒可以显著地捕捉硫酸盐。9组样品滤筒中,被测目标物所占比例为7.9%~69.1%;滤筒和前吸收液中,被测目标物所占比例为93.7%~97.8%。HJ 544—2016新增加的两级串联碱液吸收瓶可以较完全地捕集穿透滤筒后的硫酸雾,同时也会捕集SO2。SO2会对硫酸雾测试产生正干扰,约42.9%的SO2在被吸收后转化为硫酸雾。     

On-filter determination of collected wood dust by diffuse reflectance infrared Fourier-transform spectroscopy (DRIFTS)

A new analytical technique based on DRIFTS spectroscopy has been developed for the specific and sensitive determination of size-fractionated wood dust from 37 mm glass fiber filter samples collected with the Respicon sampler. A translational diffuse reflectance apparatus was modified to accept filter samples by incorporating a special filter holder in the sample stage and a clockwork motor to drive the translational stage during infrared scanning, thus providing an average analysis across the filter face. Filter samples were pre-treated with ethyl acetate to uniformly redeposit dust onto the filter and extract potential chemical interferences. Two absorbance maxima (1251 and 1291 cm(-1)), corresponding to the cellulose content of the wood, were suitable for quantitation of wood dust. Analysis of seven species of wood at 1291 cm(-1) showed an equivalent quantitative response for all species except maple. The response at 1251 cm(-1) was more variable across species but more sensitive for the softwoods. There was a statistically significant effect of particle size on the analytical response, so that analytical standards should be matched to the samples in terms of particle size distribution. Analytical limit of detection was approximately 0.08 mg of wood dust per sample with overall precision of about 6%. Comparison of DRIFTS and gravimetric analyses of 51 pure wood dust samples ranging from about 0.2 to 2 mg yielded a slope of 1.08 and r2 equal to 0.9. Other particulate contaminants common in the industrial wood processing industry showed little or no interference with the determination of wood dust by this method.     

利用自动采样滤膜监测PM_(2.5)中铅和镉的可行性

根据PM2.5中重金属监测国标分析方法,从PM2.5采样方法、采样保存条件、滤膜材质性能等方面说明利用空气自动采样滤膜监测PM2.5中铅和镉是可行的;对手工采样(石英滤膜)和Beta射线法自动采样(自动采样滤膜)2种方法,对PM2.5实际样品中铅和镉的结果进行比较,结果显示:自动采样滤膜的空白检出和检出限均满足铅和镉的监测需求,铅和镉的回收率分别为95.2%~107%和91.8%~105%,与手工采样方法相比测得铅和镉的相对误差分别为3.6%~8.4%和1.3%~10.8%,从实践角度进一步证明了利用自动采样滤膜对PM2.5中铅和镉进行监测是可行的。     

气相色谱-质谱法分析污水中溶解态有机物

采用0.45μm玻璃纤维滤膜将污水分离为悬浮态和溶解态有机物质,以二氯甲烷为萃取剂,采用液液萃取-气质联用法对污水中溶解态有机物进行测定,同时还对萃取条件(萃取次数,萃取时间,无机盐加入量)进行优化.结果表明:萃取回收率最高的是每个pH范围各萃取2次、静置5 min,氯化钠加入15g.该方法分析时间短,准确度好(样品平均加标回收率为91.1％ ～ 103％),精密度高(相对标准偏差小于5％),易于操作.     

Speciation of arsenic using solid phase extraction cartridges

Various solid phase extraction (SPE) cartridges were investigated for speciation of arsenite [As(III)], arsenate [As(v)], monomethylarsonic acid (MMA) and dimethylarsinic acid (DMA). Cartridges containing different types of sorbent materials were tested for arsenic retention and elution characteristics. Alumina cartridges were found to completely retain all the four target arsenic species, and are suitable for removal and preconcentration purposes. For speciation analysis, different arsenic species were separated on the basis of their selective retention on and elution from specific cartridges. DMA was retained on a resin-based strong cation exchange cartridge and eluted with 1.0 M HCl. MMA and As(v) were both retained on a silica-based strong anion exchange cartridge and sequentially eluted with 60 mM acetic acid (for MMA) and 1.0 M HCl [for As(v)]. As(III) was not retained on either cartridge and remained in solution. Arsenic species in solution and those eluted from the cartridges were subsequently quantified by using flow injection with hydride generation atomic fluorescence spectrometry (FI-HGAFS) and hydride generation atomic absorption spectrometry (FI-HGAAS). A detection limit of 0.05 microg L(-1) arsenic in water sample was achieved using HGAFS. An application of the method was demonstrated at a drinking water treatment facility. As(III) and As(v) species were determined in water at various stages of treatment. The method is suitable for routine determination of trace levels of arsenic in drinking water to comply with more stringent environmental regulations.     

A diffusive sampling device for the determination of formaldehyde in air using N-methyl-4-hydrazino-7-nitrobenzofurazan (MNBDH) as reagent

A new method utilizing the diffusive sampling of formaldehyde in air has been developed. Formaldehyde is sampled with the use of a glass fiber filter impregnated with N-methyl-4-hydrazino-7-nitrobenzofurazan (MNBDH) and phosphoric acid. The formaldehyde hydrazone formed is desorbed from the filter with acetonitrile and determined by high-performance liquid chromatography (HPLC) with UV/visible detection at 474 nm. The sampling rate was determined to be 24.7 mL min-1 with a relative standard deviation of 7% for 48 experiments. The measured sampling rates were not dependent on the formaldehyde concentration (0.1-1.0 mg m-3), sampling time (15-482 min) or relative humidity (20-85%). The detection limit was 70 micrograms m-3 for a 15 min sampling period and 2 micrograms m-3 for an 8 h sampling period.     

氯苯类化合物在大气中分布特征探究

建立环境空气和有组织废气排放模拟污染源,以玻璃纤维滤膜+玻璃棉和活性炭为吸附材料采集大气中氯苯类化合物,使用气相色谱法测定各组分,考察氯苯类化合物在大气气相和颗粒物中的分布特征。结果显示,环境空气和固定污染源有组织排放废气中一氯代至四氯代苯类各组分主要分布在大气气相中,颗粒物中少有分布,说明现行环境监测方法以固体吸附剂采集测定大气中的氯苯类化合物可行。     

Indoor air sampling of organophosphate triesters using solid phase extraction (SPE) adsorbents

In this paper we demonstrate the use of SPE cartridges for sampling of organophosphate triesters in indoor air by adsorptive enrichment. The method has been optimised for the sampling and analysis of organophosphate triesters using a 25 mg aminopropyl silica SPE cartridge. The same cartridge is used for the active air sampling as well as for the subsequent extraction and clean-up of the sample. This makes the method fast and eliminates some tedious and time-consuming manual sample handling steps. Sampling and extraction efficiency was high for the investigated organophosphates, and limit of detection was in the range 0.1-0.3 ng m(-3). The method was applied to measurements of organophosphate triesters in two lecture halls and an electronics dismantling facility, and was compared with results from common filter/adsorbent sampling at each site. Analysis was made by GC with selective detection by NPD set in phosphorus mode, and by GC-MS. Thirteen organophosphate triesters (not counting isomers) were detected in the electronic dismantling facility. Chlorinated organophosphate triesters were detected in all locations with concentrations over 1 microg m(-3) in the lecture halls. This kind of adsorptive enrichment using an SPE cartridge could be adjusted to other types of analytes as well.