Elemental determination of airborne particulate matter by XRF

Multielement determination of airbone particulates collected on PTFE-membrane filters by XRF, and possibility of using this technique in Receptor Model analysis were investigated. In order to keep the background interference as low as possible, special emphasis was therefore laid on the setup of optimized analytical procedures for XRF measurement. An intercomparison between INAA and XRF methods was performed by analyzing the same filter samples.     

INAA at the top of the world: Elemental characterization and analysis of airborne particulate matter collected in the Himalayas at 5,100 m high

A magnetic filter — continuous electrodeionization (CEDI) hybrid separation system was investigated for the purification of the primary coolant in a nuclear power plant. A magnetic filter system with a 3000 Gauss magnetic field and a CEDI system with a cell consisting of 3 compartments were used for the removal of magnetite and nickel ions, respectively. The hybrid separation system achieved removal rates of 98% for magnetite and 99% for the nickel ions demonstrating its feasibility for the purification of primary coolant.The authors gratefully acknowledge the Basic Atomic Energy Research Institute (BAERI) program at the Korea Institute of Science and Technology Evaluation and Planning (KISTEP) for the financial support to carry out this work.     

Characterization of airborne particulate matter collected at Jakarta roadside of an arterial road

A total of 44 pairs of airborne particulate matter samples were collected in the intersection of Simprug, Pondok Indah, South Jakarta. Sampling of airborne particulate matter was conducted in July 2008–July 2009 using a Gent stacked filter unit sampler in two size fractions of <2.5 µm (fine) and 2.5–10 µm (coarse). Mass concentrations, black carbon as well as elemental concentrations were investigated as a pre-study in step to the evaluation of air quality in these roadside areas. Black carbon was determined by reflectance and elemental analysis was performed using proton induced X-ray emission, PIXE. The data set of fine particulate matters obtained from the characterization was then analyzed using receptor modeling EPA PMF3 for source apportionment. Source apportionment identified 5 factors, i.e. soil (9.2 %), construction mixed with road dust (20.9 %), motor vehicles (31.5 %), biomass burning mixed with seasalt (30.9 %), and industry (7.5 %). Motor vehicles is the dominant sources that contributes to the fine particulate matter in Jakarta.     

Multi-element analysis by inductively coupled plasma optical emission spectrometry of airborne particulate matter collected with a low-pressure cascade impactor

A method was developed for the elemental analysis of size segregated particles ranging from 0.03 to 10 microns. Sampling and analysis problems are discussed in this paper. Particles were collected with a Dekati low-pressure cascade impactor. PTFE filters coated with oleic acid were used as substrate. Particles were microwave digested in closed vessels. The optimum digestion mixture was composed of HNO3 (1 mL), HF (50 microL) and H2O (1 mL). The optimal power setting and digestion time were studied in order to achieve an efficient digestion. A ca. 35 min microwave digestion cycle at a 650 W maximum power allowed complete digestion of the samples. Special emphasis was placed on the pressure in the closed vessels to avoid sample losses. Solution samples were analysed by inductively coupled plasma optical emission spectrometry using an ultrasonic nebuliser for 18 elements (Al, Ba, Ca, Cd, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, Pb, S, Sr, Ti, V, Zn). This procedure was tested with NIST Standard Reference Material 1648 Urban Particulate. Recoveries for certified elements ranged from 95 to 105% except for Al (90%). The influence of cascade impactor materials was investigated with 44 field samples. Strong artefacts due to contamination were shown for analysis at environmental concentrations of Al, Cr, Mn and Ni.     

Microanalytical concept for multicomponent analysis of airborne particulate matter

Summary A microanalytical concept is presented that permits the determination of four ionic species (NH ₄ ⁺ , Cl^–, NO ₃ ^– , SO ₄ ^2– and 16 elements (Al, As, Cd, Ca, Cu, Fe, K, Mg, Mn, Na, Ni, Pb, Se, Si, V, Zn) in minute samples of filter collected atmospheric particulate matter. The multistage procedure is based on consecutive aqueous extraction and acid digestion of the entire sample. Ion analysis of the extract is made by flow injection analysis (FIA) and single column ion chromatography (SCIC) with total consumption of only 50 l sample volume. Flame and furnace atomic absorption spectroscopy (AAS) is employed for element analysis after acid decomposition in a closed microwave digestion system. Using flow injection sample introduction for flame-AAS a liquid volume of 2 ml is sufficient for determination of 10 elements. Determination of the remaining 6 elements by graphite furnace AAS requires 1 ml. The quality assurance programme is briefly described. It includes the analysis of standard reference materials, intercomparison with other laboratories and the use of alternative methods for accuracy control.     

Energy dispersive X-ray fluorescence analysis of airborne particulate matter

Positron annihilation lifetime technique was applied to study the electric field dependence of size, intensity and size distribution of free volumes in various liquid crystals negative nematic MBBA(N-(4-methoxybenzylidene)-4-n-butylaniline), positive nematic 5CB (4-cyano-4-n-pentylbiphenyl) and cholesteric mixture of MBBA and cholesteryl oleate. Positron annihilation decay curves were obtained in the direct and alternate electric field range from 0 to 120 V/mm, and annihilation curves were resolved into four lifetime components. The relation between the free volume parameters and the variation of molecular alignment is discussed for nematic and cholesteric liquid crystals.     

Emission spectrographic determination of trace elements in airborne particulate matter collected on glass fiber filter.

An emission spectrographic method is described to determine the concentrations of beryllium, cadmium, chromium, copper, iron, lead, manganese, nickel, tin, and vanadium, in airborne particulate matter collected on a glass fiber filter. Sample disks punched out from the glass fiber filter are packed in a shallow cratered electrode; an internal standard solution containing indium and cobalt is added and the disks are decomposed with sulfuric acid-hydrofluoric acid. A calcium fluoride-graphite mixture is added as a spectroscopic buffer before d.c. are excitation. The precision of the method is better than ± 18%.     

Elemental characterization of TSP and two size fractions of airborne particulate matter from Tehran by INAA and AAS

Airborne particulate matter has been collected by a high volume and a Gent-type stacked filter unit (SFU) low volume sampler during the 2000-2001 period. The high volume sampler used S&S cellulosic and the SFU two Nuclepore polycarbonate filters to collect fine and coarse size fractions. The elemental analysis of the collected TSP, fine and coarse particles has been performed using instrumental neutron activation analysis and atomic absorption spectrometry. Twenty-two trace elements on Nuclepore and twenty-four elements on S&S filters have been measured. The collected data have been compared with the previous data of Tehran air and with other cities in the world. This revised version was published online in July 2006 with corrections to the Cover Date.     

Neutron activation analysis of platinum metals in airborne particulate matter

A method is described for the determination of Au, Pt, Pd, Ag and Ir in two atmospheric aerosol samples, namely in Ghent and in the Milanese intercomparison sample. After neutron irradiation the samples are fused with Na₂O₂. Gold is extracted with ethylacetate, Pt precipitated as (NH₄)₂PtCl₆ Pd as dimethylglyoximate, Ag as chloride and Ir separated by anion-exchange adsorption and batch extraction. Ge(Li) gamma-spectrometry is applied for all determinations. The concentrations in ng·g⁻¹ in the samples are respectively: Au: 49 and 3000; Pt: below 100 for both samples; Pd: 7 and 28; Ag: 6000 and 14 000; Ir: 2.5 and 1.3.     

Determination of mercury in airborne particulate matter collected on glass fiber filters using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sampling

A study has been undertaken to assess the capability of high-resolution continuum source graphite furnace atomic absorption spectrometry for the determination of mercury in airborne particulate matter (APM) collected on glass fiber filters using direct solid sampling. The main Hg absorption line at 253.652 nm was used for all determinations. The certified reference material NIST SRM 1648 (Urban Particulate Matter) was used to check the accuracy of the method, and good agreement was obtained between published and determined values. The characteristic mass was 22 pg Hg. The limit of detection (3σ), based on ten atomizations of an unexposed filter, was 40 ng g^− 1, corresponding to 0.12 ng m^− 3 in the air for a typical air volume of 1440 m³ collected within 24 h. The limit of quantification was 150 ng g⁻¹, equivalent to 0.41 ng m⁻³ in the air. The repeatability of measurements was better than 17% RSD (n = 5). Mercury concentrations found in filter samples loaded with APM collected in Buenos Aires, Argentina, were between < 40 ng g⁻¹ and 381 ± 24 ng g⁻¹. These values correspond to a mercury concentration in the air between < 0.12 ng m⁻³ and 1.47 ± 0.09 ng m⁻³. The proposed procedure was found to be simple, fast and reliable, and suitable as a screening procedure for the determination of mercury in APM samples.     

Multi-element analysis of airborne particulate matter by various spectrometric methods after microwave digestion

A microwave digestion procedure in combination of the measurement of various spectrometric methods including atomic absorption spectrometry, inductively coupled plasma atomic emission spectrometry and inductively coupled plasma mass spectrometry was developed for the multi-element analysis of airborne particulate matter collected on PTFE filters by a dichotomous sampler. In order to achieve more sensitive and rapid multi-element analyses, special PTFE-lined digestion vessels were used. It was found that complete digestion of airborne particulates with an acid mixture of HNO₃-HClO₄-HF (3:7:1, v/v) can be achieved in the microwave-irradiated closed vessel system and direct spectroscopic measurement of the digested sample after appropriate dilution. A recovery study was conducted using a multi-element standard and NIST Standard Reference Material 1648 Urban Particulate. Sixteen major, minor, and trace elements in airborne particulate matter were determined.     

Determination of chemical elements in airborne particulate matter collected at Lembang, Indonesia by particle induced X-ray emission

Monitoring the air quality in ambient air is an important step for assessing the air pollution level in one region and its impact to the human health. In this study, the determination of chemical elements concentrations in airborne particulate matter collected in suburban area of Lembang, Indonesia was carried out. Samples were collected using a Gent stacked filter unit sampler in two size fractions of <2.5 μm (fine) and 2.5–10 μm (coarse). Sampling was conducted twice a week for 24 h from January 2008 to June 2009 and 123 pairs of samples were collected. Black carbon was determined by reflectance and chemical elements analysis were performed using particle induced X-ray emission (PIXE). PIXE as one of ion beam analysis techniques is suitable for analyzing particulate matter for its multielemental analysis with good limits of detection. Results showed that none of daily concentrations of PM_2.5 and PM₁₀ exceeded the 24 h Indonesian NAAQS for PM_2.5 and PM₁₀. Chemical elements such as Mg, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Hg and Pb were determined and the correlation between these elements was reported in order to understand the anthropogenic sources of particulate matter.     

Elemental analysis of airborne fine particles collected at the roadside of an arterial road

Airborne particulate matter was collected at the intersection of Industrial Road in Kawasaki-city, Kanagawa, Japan using a 12-stage low-pressure impactor. High concentrations of airborne particulate matter have been observed in this area. The collected samples were analyzed for 34 elements by instrumental neutron activation analysis (INAA), and data on the elemental concentrations were obtained. High concentrations of fine particles of As, Br, Sb, V, and Zn were observed. It was further observed that these fine particles were originated predominantly from the wear of tires and brakes, and not from automobile exhaust emissions.     

Elemental concentrations and source identification of air particulate matter at a Nigerian site: A preliminary study

Air particulate matter collected between July and October 1990 at a site located close to an industrial estate in Lagos, Nigeria were analyzed for 18 elements by Wavelength Dispersive X-ray Fluorescence Spectroscopy (XRF) and Atomic Absorption Spectroscopy (AAS). Varimax rotated factor analysis was used for source identification of the coarse and fine fractions. For the coarse fraction, the major sources are: Re-entrained soil, Sea-salt, Industry, Regional sulphate and fresh automobile exhaust. For the fine fraction, the sources identified are Re-entrained soil, Vehicle exhaust, Sea-salt, and Industrial processes. Two other sources which are likely to be due to specific industrues come out in the fine fraction but they have not been clearly identified.     

Spatial inhomogeneity of anions in ambient particulate matter collected on air filters: determination using a drift-corrected ion chromatography technique

The spatial inhomogeneity of anions in ambient particulate matter collected on filters has been investigated using two different sub-sampling techniques and with analysis by a drift-corrected ion chromatography technique. The results highlight the inhomogeneity in anion mass along the radius of the sampled filter, in agreement with analogous studies on metals in PM, and also, more surprisingly, significant random differences between sub-samples based on filter sectors. Implications for the sub-sampling of filters for the purposes of performing multiple analyses are discussed.     

A study of uniformity of elements deposition on glass fiber filters after collection of airborne particulate matter (PM-10), using a high-volume sampler

A study was conducted to evaluate the homogeneity of the distribution of metals and metalloids deposited on glass fiber filters collected using a high-volume sampler equipped with a PM-10 sampling head. The airborne particulate matter (APM)-loaded glass fiber filters (with an active surface of about 500 cm²) were weighed and then each filter was cut in five small discs of 6.5 cm of diameter. Each disk was mineralized by acid-assisted microwave (MW) digestion using a mixture of nitric, perchloric and hydrofluoric acids. Analysis was performed by axial view inductively coupled plasma optical emission spectrometry (ICP OES) and the elements considered were: Al, As, Cd, Cr, Cu, Fe, Mn, Ni, Pb, Sb, Ti and V. The validation of the procedure was performed by the analysis of the standard reference material NIST 1648, urban particulate matter. As a way of comparing the possible variability in trace elements distribution in a particular filter, the mean concentration for each element over the five positions (discs) was calculated and each element concentration was normalized to this mean value. Scatter plots of the normalized concentrations were examined for all elements and all sub-samples. We considered that an element was homogeneously distributed if its normalized concentrations in the 45 sub-samples were within ±15% of the mean value ranging between 0.85 and 1.15. The study demonstrated that the 12 elements tested showed different distribution pattern. Aluminium, Cu and V showed the most homogeneous pattern while Cd and Ni exhibited the largest departures from the mean value in 13 out of the 45 discs analyzed. No preferential deposition was noticed in any sub-sample.     

Elemental analysis of size-fractionated particulate matter sampled in Göteborg,Sweden

The aim of the study was to investigate the mass distribution of trace elements in aerosol samples collected in the urban area of Göteborg, Sweden, with special focus on the impact of different air masses and anthropogenic activities. Three measurement campaigns were conducted during December 2006 and January 2007. A PIXE cascade impactor was used to collect particulate matter in 9 size fractions ranging from 16 to 0.06 µm aerodynamic diameter. Polished quartz carriers were chosen as collection substrates for the subsequent direct analysis by TXRF. To investigate the sources of the analyzed air masses, backward trajectories were calculated. Our results showed that diurnal sampling was sufficient to investigate the mass distribution for Br, Ca, Cl, Cu, Fe, K, Sr and Zn, whereas a 5-day sampling period resulted in additional information on mass distribution for Cr and S. Unimodal mass distributions were found in the study area for the elements Ca, Cl, Fe and Zn, whereas the distributions for Br, Cu, Cr, K, Ni and S were bimodal, indicating high temperature processes as source of the submicron particle components. The measurement period including the New Year firework activities showed both an extensive increase in concentrations as well as a shift to the submicron range for K and Sr, elements that are typically found in fireworks. Further research is required to validate the quantification of trace elements directly collected on sample carriers.     

Intercomparison of IAEA airborne particulate matter reference material

Fifty air filters with fine and coarse fractions were prepared from NIST 2710 contaminated soil. Eighteen pairs were made and sent to laboratories of the Coordinated Research Program (CRP) on Applied Research on Air Pollution Using Nuclear-Related Analytical Techniques for elemental determination. The results of this intercomparison are discussed in this paper.     

Application of receptor models to airborne particulate matter

The human activities in their various aspects cause a change in the natural air quality. This change results more marked in very populated and in high industrialized areas. Some pollutants emitted are typical of a particular activity. Each source of pollution is identified by its profile in the composition of the emissions in the environment. Multivariate receptor models can be used in order to apportion pollutants to the different sources assessing the contribution of each source to the total pollution.This paper deals with the application of Absolute Principal Component Scores (APCS) receptor model to data obtained from the automatic network of air quality monitoring in the city of Bari (South Italy). The parameters monitored by automatic networks, as bihourly values, are PM₁₀, NO_x, CO, Benzene, Toluene, Xilene. The data shown in this paper concerning 1 month almost of sampling in different monitoring stations of Bari Municipality during the period of time from January 2005 to April 2006. Moreover preliminary results obtained applying the APCS model to daily PM_2.5 samples collected during SITECOS PRIN project are shown. The results concerning data collected in corso Cavour (Bari) during the month of October 2005.The results obtained by APCS receptor model seem to suggest a poor contribution of the “vehicular traffic source” and a relevant contribution of the “secondary particulate source” to particulate matter concentrations.