道路交通中苯并(a)芘的高效液相色谱快速测定

用超细玻璃纤维滤膜采集杭州市某道路上机动车排放的苯并（ａ）芘,经超声萃取,高速离心后直接进ＨＰＬＣ分析。在选定的色谱条件下,苯并（ａ）芘与其他多环芳烃完全分离,绝对进样量在０．８～０．０２ ｎｇ时线性良好,相关系数为０．９９９７９,最小检出量０．８ ｐｇ,加标回收率８７．５％～９３．８％。     

Evaluation of high volume particle sampling and sample handling protocols for ambient urban air mutagenicity determinations.

An investigation of high volume particle sampling and sample handling procedures was undertaken to evaluate variations of protocols being used by the U.S. Environmental Protection Agency. These protocols are used in urban ambient air studies which collect ambient and source samples for subsequent mutagenicity analysis of the organic extracts of the aerosol fraction. Specific protocol issues investigated include: (a) duration of sampling period, (b) type of filter media used to collect air particles, (c) necessity for cryogenic field site storage and dry ice shipping of filter samples, and (d) sample handling at the receiving laboratory. Six PM10 Hi-Vol samplers were collocated at an urban site in downtown Durham, North Carolina and operated simultaneously to evaluate 12 h versus 24 h collection periods and filter media choices of glass fiber, Teflon impregnated glass fiber (TIGF), and quartz fiber. Filters from the samplers plus field blanks were collected during each of 25 sampling periods. TIGF filters from two samplers were immediately placed on dry ice in the field and transported directly to cryogenic storage. TIGF, quartz, and glass fiber filters from three samplers were transported at ambient and maintained at room temperature for three to six days prior to cryogenic storage. One TIGF sample, which was collected on a previously tared filter, was subjected to controlled environment equilibration (40 percent relative humidity, 22 degrees C) for 8 to 24 h and weighed prior to cryogenic storage. All filters were subsequently stored at -70 degrees C to -80 degrees C prior to a one-time extraction and Salmonella (Ames) mutagenicity bioassay of the entire sample set.(ABSTRACT TRUNCATED AT 250 WORDS)     

Measuring Inorganic and Alkyl Lead Emissions from Stationary Sources

Described are the results from studies done to provide test methods for state and local air pollution control agencies to measure accurately the lead emissions from stationary source stacks as required in the National Ambient Air Quality Standard for Lead. Separate test methods were developed for measuring inorganic lead and alkyl lead compounds. Inorganic lead is collected in a standard particulate sampling train, digested with 50% (V/V) nitric acid and 3% hydrogen peroxide and analyzed by atomic absorption spectrometry. Alkyl lead compounds are collected in iodine monochloride and analyzed by atomic absorption spectrometry without prior solvent extraction. Standard solutions of inorganic lead in dilute nitric acid are used to calibrate the spectrophotometer in both methods. The inorganic lead test method was evaluated using baghouse dust samples from a primary copper and a primary lead smelter and stack samples from a lead recovery furnace, a primary battery manufacturing plant, a gray iron foundry and a secondary lead smelter. The alkyl lead method was evaluated using alkyl lead motor mix fluids and samples from an alkyl lead manufacturing plant vent stack.     

Development and validation of a method for determination of trace levels of alkylphenols and bisphenol A in atmospheric samples

A method has been developed and validated in order to assess the occurrence of the alkylphenols tert-octylphenol and the isomers of technical nonylphenol as well as bisphenol A in gasphase and aerosol samples of a remote area. Gasphase samples were adsorbed to XAD2 resin, aerosol samples were taken on glass fiber filters. After ultrasonic extraction, clean-up by column chromatography and silylation of the analytes, ten nonylphenol peaks were quantified separately using a GC-MSD-SIM method. The absolute limits of detection and determination are in the range of a few pg per compound, which is a prerequisite for the quantification of the analytes in relatively unpolluted air. The precision of the whole analytical method is in the range of 1-17% and the recoveries range from 57% to 80%. Problems were encountered during method development due to the tendency of the analytes to sorb to glass surfaces. Silanisation of glassware was crucial to achieve acceptable recoveries. The widespread use of the analytes in plastic resins resulted in sample contamination. For this reason a careful choice of sampling material was necessary. Measured concentrations in gasphase samples (lower nanogram per m3 range) and aerosol samples (upper picogram per m3 range) are one to three orders of magnitude below already published concentrations.     

Survey of polynuclear aromatic compounds in oil refining areas

Air samples in and around refinery areas were collected over a 3-year period. The results of the analysis for polynuclear aromatic compounds listed as priority pollutants by the United States Environmental Protection Agency are presented. The particulate matters in the air were collected on glass fiber filters using high volume samplers. These samples were later Soxhlet extracted with cyclohexane, and then extracted with DMSO/pentane for isolation of the polynuclear aromatic compounds. These extracts were then analyzed using gas chromatography-mass spectrometry for specified polynuclear aromatic compounds. It was found that much higher concentrations of these aromatic compounds were found in one refinery compared to another one. In general, the number of these priority pollutants detected and their concentrations were higher in sites inside the refineries relative to a site outside the refineries.     

Planning A State-Wide Air Pollution Advisory Service

An investigation of high volume particle sampling and sample handling procedures was undertaken to evaluate variations of protocols being used by the U.S. Environmental Protection Agency. These protocols are used in urban ambient air studies which collect ambient and source samples for subsequent mutagenicity analysis of the organic extracts of the aerosol fraction. Specific protocol issues investigated include: (a) duration of sampling period, (b) type of filter media used to collect air particles, (c) necessity for cryogenic field site storage and dry ice shipping of filter samples, and (d) sample handling at the receiving laboratory. Six PM₁₀ Hi-Vol samplers were collocated at an urban site in downtown Durham, North Carolina and operated simultaneously to evaluate 12 h versus 24 h collection periods and filter media choices of glass fiber, Teflon® impregnated glass fiber (TIGF), and quartz fiber. Filters from the samplers plus field blanks were collected during each of 25 sampling periods. TIGF filters from two samplers were immediately placed on dry ice in the field and transported directly to cryogenic storage. TIGF, quartz, and glass fiber filters from three samplers were transported at ambient and maintained at room temperature for three to six days prior to cryogenic storage. One TIGF sample, which was collected on a previously tared filter, was subjected to controlled environment equilibration (40 percent relative humidity, 22°C) for 8 to 24 h and weighed prior to cryogenic storage. All filters were subsequently stored at ?70°C to ?80°C prior to a one-time extraction and Salmonella (Ames) mutagenicity bioassay of the entire sample set. Results indicate that the sample handling variations and collection period variables had no significant effect on recovery of organics or mutagens. However, a filter type difference was observed. The sonication extraction of organics and mutagens was significantly greater for TIGF filters than for glass fiber or quartz. Results from a second phase of study indicated differences in extracted organics and mutagens for these filter types.     

Evaluation of alternative filter media for particulate matter emission testing of residential wood heating devices

The performance of Teflon-coated glass fiber filter media (Pallflex Emfab TX40) is evaluated for particulate matter (PM) sampling of residential wood heating devices in a dilution tunnel. Thirty samples of varying duration and PM loading and concentration were collected from an U.S. Environmental Protection Agency (EPA) Method 28 dilution tunnel using dual Method 5G sample trains with untreated glass fiber and Emfab filters. Filters were weighed soon after the end of sampling and again the next day after equilibration at 35% relative humidity (RH). PM concentrations from both types of filters agreed very well with 1-day equilibration, demonstrating that Emfab filters are appropriate for use in measuring PM from residential wood burning appliances in a dilution tunnel and have performance equal to or better than the glass fiber filter media. Agreement between filter media without equilibration was erratic, with PM from glass fiber filter samples varying from slightly less than the Emfab samples to as much as 2.8 times higher. Some of the glass fiber filters lost substantial mass with equilibration, with the highest percent loss at lower filter mass loadings. Mass loss for Emfab samples was a small percentage of the mass and very consistent across the range of mass loadings. Taken together, these results may indicate water uptake on the glass fiber media that is readily removed with 1-day equilibration at moderate RH conditions.

Implications: EPA regulations now allow the use of either glass fiber or Teflon filter media for wood appliance PM emission testing. Teflon filter media minimizes the potential for acid-gas PM artifacts on glass fiber filters; this is important as EPA moves toward the use of locally sourced cordwood for testing that may have higher sulfur content. This work demonstrates that the use of Teflon-coated glass fiber filters can give similar PM measurement results to glass fiber filters after 1 day of equilibration. With no equilibration, measured PM from glass fiber filters was usually higher than from Teflon-coated glass fiber filters.     

Quantitative method for the determination of femtogram amounts of polychlorinated dibenzo-p-dioxins and dibenzofurans in outdoor air

A method for the quantitative determination of polychlorinated dibenzo-p-dioxins (PCDD) and dibenzofurans (PCDF) in ambient air is described in detail. High-volume sampling of 1000 m³ air using a glass fiber filter and polyurethane foam as collection media allows to detect femtogram/m³ amounts, when negative ion chemical ionization mass spectrometry is used as detection method.     

制备条件对不同玻璃材料负载TiO_2活性影响研究

以光催化降解苯酚为探针反应,通过正交实验,系统研究了胶液配比、涂覆次数和焙烧温度等条件对以溶胶-凝胶法分别在普通钠钙玻璃和磨砂玻璃上制备TiO2光催化性能的影响,并利用环境扫描电镜（ESEM）对TiO2催化膜形貌进行了分析。研究表明,在普通钠钙玻璃片上负载TiO2催化膜的影响因素主次顺序为：硝酸体积〉涂覆次数〉焙烧温度〉V乙醇∶V酞酸丁酯,在选定实验条件下的最优条件为：涂覆次数为4次;焙烧温度=450℃;V乙醇∶V酞酸丁酯∶V硝酸（1∶4）：V水=400∶40∶1∶4。在磨砂玻璃片上负载TiO2催化膜的的影响因素主次顺序为：涂覆次数〉硝酸体积〉焙烧温度〉V乙醇：V酞酸丁酯,在选定实验条件下的最优条件为：涂覆次数为4次;焙烧温度=500℃;V乙醇∶V酞酸丁酯∶V硝酸（1∶4）∶V水=400∶40∶2∶4。通过扫描电镜可以观察到在普通钠钙玻璃片和磨砂玻璃片表面均附着一层白色的TiO2薄膜,颗粒粒径在100 nm左右。磨砂玻璃比普通钠钙玻璃负载更多的催化剂,磨砂玻璃基TiO2活性更高。磨砂玻璃是一种非常有前景的TiO2催化剂载体材料。     

A High Volume Stack Sampler

This paper deals with the development design, and trial application of a sampling train to gather a relatively large amount of particulate sample in a short period of time. With air pollution sources installing control equipment to reduce emissions to the required low levels, it becomes necessary to use a sampling device which can collect a representative sample in a reasonable period of time. Some of the sampling trains currently being specified are expensive, awkward, and nearly impossible to use under field conditions. The high-volume train overcomes ail of these shortcomings and has some additional advantages. It uses the same glass fiber filter that is specified for ambient air particulate sampling so the emission test results are directly comparable to ambient air sampling data. The laboratories currently weighing and analyzing the glass filters need no additional equipment for the emission sampling analysis. The sample collected by the high-volume probe may be analyzed microscopically for size and characteristics of the particles. This is very important if control equipment is to be specified for the process or source. The high-volume sampler was evaluated on field tests of wood fired boilers, incinerators, wigwam burners, asphalt batching plants, seed cleaning plants, and wood fiber filtration systems. The results of several typical tests using the sampler on these sources are included in the paper.     

High Volume Sampling: Errors Incurred during Passive Sample Exposure Periods

The current Federal EPA reference method for the determination of total suspended particulate matter (TSP) in the atmosphere is the high volume method (hi-vol).¹ The hi-vol sampler is normally operated for a 24 hr period by drawing air through an 8 X 10 in. glass fiber filter at an air sampling flow rate of between 40-60 cfm. TSP samples are presently collected in this manner every 6th day (61 samples/year). Results are used to determine compliance with existing National Primary Ambient Air Quality Standards for TSP (i.e., 260 µg/m³, maximum 24 hr average, not to be exceeded more than once a year; 75 µg/m³, annual geometric mean). However, when the sampling frequency is diminished to only 61 out of a possible 365 measurements each year, the degree of certainty associated with meeting these air quality standards is also decreased.^2,3 This partial sampling schedule also introduces other sampling errors. One such error caused by the exposure of the collection filter both prior and subsequent to the desired sampling day is the subject of the following discussion.     

Flexibility of X-Ray Emission Spectrography as Adapted to Microanalysis of Air Pollutants

Methods previously published by this laboratory for analyzing thin dust coatings of airborne particulates have been further evaluated, as applied to vast air pollution surveys. It was demonstrated that choice of glass fiber filters adapted to high-volume samplers restricts the analysis to a limited number of elements, such as lead. More flexibility and versatility are attained through the use of organic membrane filters mounted in small plastic monitors which permit multi-elemental analysis at least as accurately as with other popular but time-consuming techniques. These qualities of speed and accuracy allow shorter intervals of sampling which are normally required for better statistical assessment of broad air pollution surveys. Sensitivity of the technique reaches a value close to 0.05 μg/m³, while time of analysis required is about five minutes per element after receipt of the sample.     

Effects of acid-washing filter treatment on quantification of aerosol organic compounds

The tests of standard mixtures and four sets of atmospheric particulate samples showed that an acid-wash (AW) pretreatment of fluorocarbon-coated glass fiber filters prior to aerosol sampling enhanced the quantifiable organic compounds for more than 29% (or 66 ng m⁻³); in particular, 47–273 ng m⁻³ (21–366%) more water-soluble organic compounds (WSOCs) were measured. When the acid-pretreated filters were employed, up to nine more organic species were measured in the individual daily samples. Because the acid pretreatment reduced the metal contaminants in the glass fiber filters, using the AW filters for aerosol sampling allows higher extraction recoveries of organic compounds. Since the fingerprinting compounds were more accurately determined when the aerosol samples were collected on the AW filters, better assessment of emission sources and toxicity of air pollutants can be obtained.     

Seasonal variation of heavy metals in ambient air and precipitation at a single site in Washington, DC

Atmospheric samples of precipitation and ambient air were collected at a single site in Washington, DC, for 7 months (for ambient air samples) and 1 year (for wet deposition samples) and analyzed for arsenic, cadmium, chromium and lead. The ranges of heavy metal concentrations for 6-day wet deposition samples collected over the 1-year period were 0.20-1.3 microg/l, 0.060-5.1 microg/l, 0.062-4.6 microg/l and 0.11-3.2 microg/l for arsenic, cadmium, chromium and lead, respectively, with a precision better than 5% for more than 95% of the measurements. The ranges of heavy metal concentrations for the 6-day ambient air samples were 0.800-15.7 ng/m(3), 1.50-30.0 ng/m(3), 16.8-112 ng/m(3), and 2.90-137 ng/m(3) for arsenic, cadmium, chromium and lead, respectively, with a precision better than 10%. The spread in the heavy metal concentration over the observation period suggests a high seasonal variability for heavy metal content in both ambient air and wet deposition samples.     

The recovery of selenious acid aerosols on glass fiber filters

Previous workers have shown that selenium is only partially trapped on a filter during air sampling. In some cases, these losses have been attributed to volatilization of selenium dioxide. Our results demonstrate that selenium dioxide, in the presence of moist air, is completely recovered (apparently as selenious acid aerosols) and that the previous shortfalls must be due to other selenium species as yet unidentified. Selenious acid aerosols in our study were formed by volatilizing selenium dioxide (approximately 3 mg) into a stream of moist ambient air (relative humidity, greater than 50%), and trapped on glass fiber filters using a high-volume air sampler. Selenium(IV) was ultrasonically extracted from the filter with water and analyzed by atomic absorption spectrometry. Selenious acid aerosols were trapped on the filters with high efficiency (105 +/- 5 percent) using a 50 minute sampling period. With an extended sampling period (24 hours) the recovery was 103 +/- 6 percent.     

Covariations in the concentrations of organic compounds associated with springtime atmospheric aerosols

Organic compounds that can be thermally desorbed from airborne particles change cohesively with time, providing information about sources, photochemical transformations and transport of aerosols. In the spring of 1985, 138 airborne particulate samples were collected at an urban site in Boulder, Colorado. Samples were collected by drawing approximately 300 ℓ of air, for 58 min, through a small glass tube containing a quartz fiber filter. Particles were subsequently analyzed by direct thermal desorption of volatile organic compounds into a gas Chromatographic column followed by separation and detection of compounds with flame ionization or mass spectrometry. Factor analysis on the concentrations of 42 organic compounds in 138 1-h samples with time and meteorology revealed characteristic chromatograms for photochemical activity, biological sources and motor vehicle sources. Organic compounds desorbed from particles include terpenoids from biogenic sources, alkanes from vehicular and biological sources and aldehydes, ketones, carboxylic acids, lactones and furans from photochemical transformations and other sources. Concentrations of oxygenated species increased on sunny days relative to cloudy days or nights. Terpenoid concentrations increased when the wind direction was from a forested region west of the sampling site. Odd carbon number n-alkanes increased as temperature increased with the progression of springtime.     

The Recovery of Selenious Acid Aerosols on Glass Fiber Filters

Previous workers have shown that selenium is only partially trapped on a filter during air sampling. In some cases, these losses have been attributed to volatilization of selenium dioxide. Our results demonstrate that selenium dioxide, In the presence of moist air, is completely recovered (apparently as selenious acid aerosols) and that the previous shortfalls must be due to other selenium species as yet unidentified. Selenious acid aerosols In our study were formed by volatilizing selenium dioxide (≈3 mg) Into a stream of moist ambient air (relative humidity, >50%), and trapped on glass fiber filters using a high-volume air sampler. Selenium(IV) was ultrasonlcally extracted from the filter with water and analyzed by atomic absorption spectrometry. Selenious acid aerosols were trapped on the filters with high efficiency (105 ± 5 percent) using a 50 minute sampling period. With an extended sampling period (24 hours) the recovery was 103 ± 6 percent.     

自洁式三级串联的水样在线过滤系统的研制和应用

基于玻璃纤维对小颗粒物的截留和微孔过滤,以及超声波辅助清洗等方法原理,设计和制作了带反冲洗自洁功能的三级串联在线过滤系统,将滤网（初级）、超声波作用下装填有玻璃纤维的过滤器（二级）、微孔滤管（三级）串联,对较高浊度的环境水样进行在线过滤。评估了模拟水样和实际水样中浊度的去除效果,证明该系统对水样中颗粒物有很好的去除并大幅降低水样浊度。在优化的条件下,原始浊度范围在4～100NTU的水样经过滤后,浊度均能降至1NTU以下。以标准方法测定的典型水质指标（活性磷、铵氮、亚硝酸盐氮和硝酸盐氮）的浓度为基准,计算水样经所设计的过滤系统处理后,这4种营养盐的回收率一般在85％-130％之间,说明本系统的使用基本不影响目标物的测定。     

机械活化对CRT锥玻璃浸出动力学的影响

通过研究CRT锥玻璃经机械活化后在硝酸溶液体系中浸出反应动力学规律,考察了机械球磨转速、浸出温度以及硝酸初始浓度对锥玻璃中铅的浸出效果影响。研究结果表明,锥玻璃经机械活化预处理后,反应活性显著增强,锥玻璃中铅浸出率大幅度提高。浸出反应的表观活化能和反应级数由109.4 kJ/mol和0.79降至54.3 kJ/mol和0.51。