自制模拟样及留样复测的质控技术探讨

介绍了环境监测标准滤膜、标准滤筒、模拟降尘的制备方法、使用方法、实际效果。阐述了滤膜中铅、土壤样品、底泥（沉积物）、污水厂处理污泥等留样的来源、必要性及作用。探讨了滤膜中铅留样复测质控的评判依据。     

碱溶氟离子电极法测定大气中总氟

本文叙述了“滤膜——碱溶——氟离子电极法”测定大气中总氟的分析方法.通过对比试验和加标回收试验,阐明了该法能完全溶解滤膜上的总氟物质,优于滤膜——酸溶——氟离子电极法.且方法可靠,简便易行.     

无平衡室条件下测定TSP的滤膜恒重方法

测定ＴＳＰ的滤膜需在恒温、恒湿的平衡室中平衡、称量,否则会影响测定的精密度和准确度。经多年实践,摸索出用生化培养箱代替平衡室,用于滤膜恒重,效果较好,且方法简便易行,现介绍如下,供参考。将符合标准的滤膜打上编号,分开放置于恒温20℃的生化培养箱上部(下部仍可用于样品ＢＯＤ5培养),平衡24ｈ,用镊子取出随即放入分析天平称量,在30ｓ内称量完毕,贮于滤膜盒中备用,结果见表1。由表1可见,用此法平衡滤膜24ｈ足可使滤膜达到恒重,生化培养箱还可同时进行ＢＯＤ5样品培养。考虑到在不同季节,天平室的温度和湿度会不在测定ＴＳＰ的要求…     

滤膜过滤 微波干燥法快速测定水中悬浮物

采用滤膜过滤微波干燥技术,建立了水中悬浮物的快速测定方法。以0.45μm硝酸乙酸纤维素(CN-CA)滤膜为过滤介质,采用变功率连续加热模式,空白湿滤膜在10 min内恒重(900 W/5 min+500 W/5 min),附有悬浮物的湿滤膜在13 min内恒重(900 W/8 min+500 W/5 min)。选择不同质量浓度的高岭土标准样品和不同类别的实际样品进行方法性能测试,结果表明,该方法检出限为5 mg/L,相对标准偏差(RSD)为2.7%~7.1%,相对误差为2.0%~5.0%,采用该方法与采用标准方法《水质悬浮物的测定重量法》(GB 11901—89)测定实际样品的结果吻合。该方法显著缩短了水中悬浮物测定的分析时间,精密度和准确度能够满足分析要求,可用于地表水及一般工业排放废水中悬浮物质量浓度的快速测定。     

浸渍滤膜采样——氟离子选择电极测定废气中氟化物

废气中氟化物的测定,通常采用碱液吸收——氟离子选择电极测定的方法.该方法分析部分具有快速、灵敏、适用范围宽、方法简便、准确、选择性好等优点.但现场采样部分较繁琐,不适用于根据GBJ4—3排放标准设计的排放浓度(1～10)毫克/米~3范围内氟化物的测定.本文采用《空气和废气监测分析方法》(以下简称《方法》)介绍的碳酸氢钠甘油浸渍滤膜——氟离子选择电极测定空气中氟化物的方法,对废气中氟化物含量进行测定,得到了满意的结果.     

关于硫酸盐化速率质控方法

关于硫酸盐化速率质控方法杨永祥（石河子市环境监测站８３２０００）介绍了一种硫酸盐化速率测定的质控试样制备方法，具有简便可行的目的。１质量控制方法１．１质控样品的制备将超细玻璃纤维滤膜切成直径为７ｃｍ的圆片，在上面滴加ｌｍｌ３０％的碳酸钾溶液，烘干．烘...     

波长色散-X射线荧光光谱法测定PM2.5中23种元素

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PM_2.5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PM_2.5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。     

密闭微波消解 ICP- AES 法测定大气颗粒物中金属元素

采用过氯乙烯滤膜采集、密闭微波消解、电感耦合等离子发射光谱法测定大气颗粒物中铅、镍、铬、铜、铁、锌、锰、钡、镉,优化了试验条件.方法线性良好,各元素的检出限在0.001 mg/L～0.01 mg/L之间,滤膜样品测定的RSD为0.6%～2.9%,加标回收率为96.0%～105%.     

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。     

石墨炉原子吸收法测定大气TSP、降尘、降水中的铍

本法不需专门采样,取大气例行监测TSP的滤膜、降尘、降水即可测定铍。将采有TSP的过氯乙烯滤膜干灰化消化:降尘在高压密封缺罐中消化:降水酸化到含1％H_2SO_4的测试液,在石墨管中以氨水作基体改进剂,氘灯扣除背景,峰高定量。本法绝对检出量为3.0×10~(-13)g,用于测定大气、废气中的铍,不用玻璃纤维滤膜和滤筒,试液中基体浓度低,在氨水的化学作用和氘弧灯光谱学扣背景的作用下,干扰可完全消除。采集大气10m~3,制备10ml测试液,检出浓度为8×10~(-9)mg/m~3。称取降尘残渣0.100g,检出量为2μg/g:降水的检出浓度为0.008μg/l。     

Implementing infrared determination of quartz particulates on novel filters for a prototype dust monitor

Research by the National Institute for Occupational Safety and Health (NIOSH) has pursued quartz analysis for the specialized filter assemblies of a new worker-wearable personal dust monitor (PDM). The PDM is a real-time instrument utilizing a tapered element oscillating microbalance (TEOM). Standard fiberglass TEOM filters cannot accommodate the desired P-7 infrared analytical method used by the Mine Safety and Health Administration (MSHA). Novel filter materials were tested with the objective of demonstrating this type of analysis. Low temperature ashing and spectrometric examination were employed, revealing that nylon fiber candidate filters left minimal residual ash and produced no significant spectral interference. Avoiding titanium dioxide in all filter materials proved to be a key requirement. Fine quartz particulates were collected on prototype filters in a Marple chamber, either open-faced or through PDMs during test runs. The filters were then subjected to MSHA P-7 analysis and the spectrometrically based analytical results for quartz mass were compared to reference measurements. Also, PDM instrumental mass readings were compared to filter gravimetric measurements. Results suggest that the P-7 method is adaptable to variations in filter materials and that quartz dust analysis by the P-7 method when utilizing the new ashable PDM filters can have accuracy and precision within 10% and 4%, respectively. This is within the declared 13% accuracy and 7-10% precision of the P-7 method itself. Instrument mass readings had modest positive bias but met NIOSH accuracy criteria. Continued work with specialized PDM filters is merited, as they are a new type of TEOM sample amenable to ashing analysis of particulates.     

固定源硫酸雾国内外采样方法优劣分析

固定污染源硫酸雾的国标采样方法为滤筒法,但对其采样效率研究较少。在调研国内外标准方法及相关文献的基础上,通过大量实样测定,对国标采样法进行改进：在内装滤筒的烟尘采样管后串联一个冲击式吸收瓶,此改进方法弥补了国标漏测气态硫酸雾的缺陷,采样效率达到99％以上,国标法仅为改进法的47％～68％。将国标改进法与USEPA采样法进行比对,结果表明,由于中国环境本底颗粒物浓度较高,硫酸雾易吸附于颗粒物上,致使USEPA采样效率仅为国标改进法的2?4％～12％。     

A chemosorptive cylindrical denuder designed for personal exposure measurements of isocyanates-evaluation on generated aerosols of 4,4'-methylenediphenyl diisocyanate

A denuder/filter system constructed for solvent-free personal exposure measurements was evaluated for separation of vapour and particulate 4,4'-methylenediphenyl diisocyanate (4,4'-MDI) generated from heated PUR-foam. The two different phases were collected in the denuder and on the filter, respectively, by chemosorption on a polydimethylsiloxane (SE-30)-dibutylamine (DBA) stationary phase. Both repeatability and the total mass concentration of 4,4'-MDI were similar to that obtained from the reference method, in this case an impinger/filter system. The penetration of particles through the denuder at 300 ml min(-1) was nearly 100% in the particle size range 25 to 700 nm, which fits well with the Gormley-Kennedy equation. Denuder/filter sampling of the 4,4'-MDI aerosol at 500 ml min(-1) yielded a phase distribution that was in accordance with the results from the reference method. The method limit of detection was 6 ng m(-3) and 4 ng m(-3) for the denuder and filter, respectively, when using an air sampling flow rate of 300 ml min(-1) and a sampling period of 15 min. This is well below the Swedish occupational exposure limit (OEL) of 50 and 100 microg m(-3) for an 8-hour working day and a 5-min period, respectively.     

Comparative rice seed toxicity tests using filter paper,growth pouch-tm,and seed tray methods

Paper substrate, especially circular filter paper placed inside a Petri dish, has long been used for the plant seed toxicity test (PSTT). Although this method is simple and inexpensive, recent evidence indicates that it gives results that are significantly different from those obtained using a method that does not involve paper, especially when testing metal cations. The study compared PSTT using three methods: filter paper, Growth Pouch-TM, and seed tray. The Growth Pouch-TM is a commercially available device. The seed tray is a newly designed plastic receptacle placed inside a Petri dish. The results of the Growth Pouch-TM method showed no toxic effects on rice for Ag up to 40 mg L^–1 and Cd up to 20 mg L^–1. Using the seed tray method, IC₅₀ (50% inhibitory effect concentration) values were 0.55 and 1.4 mg L^–1 for Ag and Cd, respectively. Although results of filter paper and seed tray methods were nearly identical for NaF, Cr(VI), and phenol, the toxicities of cations Ag and Cd were reduced by using the filter paper method; IC₅₀ values were 22 and 18 mg L^–1, respectively. The results clearly indicate that paper substrate is not advisable for PSTT.     

Development of a field method for measuring manganese in welding fume

Workers who perform routine welding tasks are potentially exposed to fume that may contain manganese. Manganese may cause respiratory problems and is implicated in causing the occurrence of Parkinson-like symptoms. In this study, a field colorimetric method for extracting and measuring manganese in welding fume was developed. The method uses ultrasonic extraction with an acidic hydrogen peroxide solution to extract welding fume collected on polyvinyl chloride filters. Commercially available pre-packaged reagents are used to produce a colored solution, created by a reaction of manganese(ii) with 1-(2-pyridylazo)-2-naphthol. Absorbance measurements are then made using a portable spectrophotometer. The method detection limit and limit of quantification (LOQ) were 5.2 microg filter(-1) and 17 microg filter(-1), respectively, with a dynamic range up to 400 microg filter(-1). When the results are above the LOQ for the colorimetric method, the manganese masses are equivalent to those measured by the International Organization for Standardization Method 15202-2, which employs a strong acid digestion and analysis using inductively coupled plasma-optical emission spectrometry.     

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。     

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.     

Phosphine sampling and analysis using silver nitrate impregnated filters

In the field of industrial hygiene, besides the necessity of monitoring phosphine with direct reading apparatus to prevent accidents, there is a need for a method of sampling and analysing phosphine to control workers' exposure. The use of filters impregnated with silver nitrate to collect arsine, phosphine and stibine in workplace air has been described in the literature. Having previously chosen this type of filter to collect arsine, we studied its characteristics for phosphine capture. A filter impregnated with sodium carbonate was used both as a prefilter to collect the particles and to trap arsenic trioxide. After dissolving the silver compounds in nitric acid, ICP emission spectrometry was used to carry out the analysis. This article describes the comparative sampling we performed in a microelectronic laboratory and in a fumigation chamber (130 samples) to determine the concentration of AgNO3 impregnation solution to be used, the detection limit of the method and the retention capacity of the impregnated filters. Interference with other gases reacting with silver nitrate was studied and the storage time for sampled filters and analysis solutions was checked. The detection limit of the adopted method is better than 1 microg per filter, and the retention capacity exceeds 300 microg per filter. The problem of how to sample phosphine when H2S, NH3, or HCl is present has been solved, but the problem of sampling phosphine in atmospheres where acetylene evolves remains. Sampled filters and filter solutions are stable for more than three months at ambient temperature.