Simultaneous Multi-element Analysis Research Articles

Nitrogen purged TXRF for the quantification of silver and palladium

Total reflection X-ray fluorescence (TXRF) analysis is a powerful technique for simultaneous multi-element analysis. Benefits include limits of detection in the microgram per litre range, limited sample preparation for liquid samples and low operating costs. However, the determination of elements such as silver and palladium suffers from interferences, e.g. if an X-ray tube with a molybdenum anode is used, which normally offers the lowest detection limits for most of the elements of the periodic table. Argon emits its X-ray fluorescence radiation in the same energy range as these metals and therefore hinders their detection and subsequent quantification. Since argon is abundant in the atmosphere with approx. 0.93% and is easily activated by X-rays in a TXRF instrument, this interference is always present under routine measurement conditions. We have developed a new method for the analysis of silver and palladium by TXRF. A commercially available TXRF system was modified for being operated under a nitrogen purged atmosphere by surrounding it with an airtight and water-cooled box, which still allows accessing the main hardware components, changing the sample discs or performing long term measurements without temperature drift effects. An easy removal of the box is possible for a rapid change between the nitrogen purged and the common mode under ambient atmosphere. After flushing the system with nitrogen, the signal of argon decreased significantly, allowing the determination of silver and palladium with limits of detection for silver and palladium of 6.6 μg L−1 and 16.6 μg L−1 respectively.

A quantitative analysis of elements in soil using laser-induced breakdown spectroscopy technique

Laser-induced breakdown spectroscopy (LIBS) was applied to the quantitative analysis of elemental composition of soil. The experiment was performed in air at atmospheric pressure and at room temperature. A Nd:YAG laser with the fundamental wavelength of 1064 nm was employed to generate the soil plasma. The emission spectra from the plasma were collected by the Cerny-Turner type of spectrometer, which was equipped with an intensified charge-coupled device (ICCD). The plasma temperature and electron density were evaluated by the Boltzmann plot method and the Saha-Boltzmann equation respectively. Then the concentrations of elements in soil were further obtained by the internal standard of iron element and some selected atomic/ionic lines. In order to prove the credibility and reliability of the present LIBS results, a comparison between the LIBS results and the nominal concentrations was performed. It was found that the LIBS results agree with the nominal concentrations. Therefore the LIBS technique promises to fast and in simultaneous multi-element quantitative analysis of soil.

LIBS for the Analysis of Metallurgical and Solar Grade Silicon

Laser-induced breakdown spectroscopy (LIBS) has been employed for the fast and reliable chemical characterization of silicon used for the photovoltaic industry. Silicon for photovoltaic panels is subject to certain constraints on its purity, and notably must contain low concentration of boron. The use of LIBS could be advantageous because it allows rapid and simultaneous multi-elemental chemical analysis of silicon without any sample preparation. LIBS was applied to boron analysis and a detection limit of 0.23 ppmw was found for optimized gas and pressure conditions.

Multi-element analysis of bread, cheese, fruit and vegetables by double-focusing sector-field inductively coupled plasma mass spectrometry

An analytical method using double-focusing sector-field ICP MS was developed for the routine simultaneous multi-element analysis for essential and toxic elements (Ag, Al, As, Cd, Co, Cr, Cu, Fe, Hg, In, Li, Ni, Mn, Mo, Pb, Si, Sb, Se, Sn, V and Zn) in different food samples (bread, cheese, fruit and vegetables). Samples were hot-plate digested with a mixture of concentrated HNO3 and H2O2. Interfering ions involving matrix constituents were detected for several elements at the resolution of 300 (typical for a quadrupole analyzer) and could be separated at the 4000 and 10 000 resolution. The method was validated by the analysis of certified reference materials: wheat flour (NIST 1567a), non-fat milk powder (NIST 1549) and brown bread (BCR-IRMM 191). The method used in our laboratory over the period of one year for the analysis of over 300 samples showed a typical interday precision of 3–5% and intraday precision of 5–10% for virtually all the elements and investigated matrices.

Low power capacitively coupled plasma microtorch for simultaneous multielemental determination by atomic emission using microspectrometers

A new, low power capacitively coupled plasma microtorch (30 W, 13.56 MHz, 0.5 L min −1 Ar) was investigated in conjunction with commercially available microspectrometers for the simultaneous multielemental analysis by atomic emission spectrometry of liquid samples without desolvation. Emission spectrum is simpler than in ICP-AES, the resonance lines are the most intense, so that a microspectrometer with FWHM of at least 1.5 nm is satisfactory for the record. The deviation from the Boltzmann distribution for Fe I has demonstrated the departure from the LTE in plasma. The non-spectral matrix effects of Li, Na, K, Ca and Mg on analytes emission are depressive and depend on matrix volatility, ionization potential of the interferent and analyte excitation energy. The detection limits (μg mL −1) are in the range 0.003 (Li) and 1.5 (Mn). The use of the standard additions method allowed the simultaneous determination of elements in environmental certified reference materials with overall recovery of 95 ± 10% and relative standard deviation of 1.7–8.2%. Compared to the traditional ICP, the microtorch has a simple construction, runs at low argon flow and can be integrated in a portable system suitable for in-situ simultaneous determination of elements.

Rapid simultaneous multi-element determination of soils and environmental samples with polarizing energy dispersive X-ray fluorescence (EDXRF) spectrometry using pressed powder pellets

A rapid simultaneous multi-element analysis method for soils and environmental samples has been established using polarizing energy dispersive X-ray fluorescence (EDXRF) spectrometry. The pressed powder pellet technique was adopted because it is simple and requires no specialized skills for sample preparation. The analytes examined were: Na2O, MgO, Al2O3, SiO2, P2O5, K2O, CaO, TiO2, MnO, Fe2O3, V, Cr, Co, Ni, Cu, Zn, Rb, Sr, Y, Zr, Nb, Sn, Sb, Cs, Ba, La, Ce, Pr, Nd, Pb and Th. Twenty-six reference samples were used for the calibrations. Compton scatter radiation was used as an internal standard to compensate for variations in the sample matrix, particle size, packing density and operating characteristics of the instrument. The correlation coefficients of the linear regression lines were >0.98, with the exception of Na2O, MgO, Al2O3, SiO2, P2O5, Co, Pr and Nd. The values obtained using the proposed EDXRF spectrometry were compared with the values obtained using other methods. Out of the 31 analytes examined, the results for 12 compounds (CaO, K2O, TiO2, MnO, Fe2O3, Ni, Zn, Rb, Sr, Cs, Ba and Ce) obtained by the proposed EDXRF spectrometry compared favorably with those determined through conventional wet chemical methods. In contrast, the results for eight compounds (Na2O, MgO, Cr, Co, Zr, Sn, Sb and Pr) obtained by the proposed EDXRF spectrometry exhibited poor agreements with those obtained using chemical methods. Among these analytes, the poor agreements of Cr, Zr and Sn were attributable to incomplete dissolution and/or volatilization losses during the chemical treatments based on an acid attack. It can be concluded, therefore, that there is a high possibility of underestimating the concentrations of these elements if wet chemical methods are used. Although the results of the other 11 analytes were not as good as those of the first group, they still appeared to be of practical use, considering the time consuming and potentially hazardous wet chemical pretreatment.

The Ben Lawers Historic Landscape Project: Simultaneous Multi-element Analysis of Former Settlement and Arable Soils by X-ray Fluorescence Spectrometry

X-ray fluorescence spectrometry (XRFS) was used in the analysis of A horizon soil samples collected from a former farming settlement and its associated area of infield (i.e. arable) located in the Central Highlands of Scotland. To date, XRFS has not been extensively used in geoarchaeological research, but in our study the simultaneous multi-element capabilities of this instrumental technique allowed the total concentrations of 25 major, minor, and trace elements to be fully quantified with acceptable levels of accuracy and precision. Included within this group of chemical elements are a number (e.g. Ba, Ca, P, Pb, Sr and Zn) that have proved to be of value to archaeological interpretation in earlier investigations undertaken in Scotland. In our preliminary work documented here, significant differences were found between the A horizon soils of former settlement and infield areas for 18 chemical elements. Subjecting the XRFS data—and three other measured variables: soil organic carbon (SOC), pH and A horizon depth—to discriminant analysis indicates that soils of former settlement and arable farming can be effectively classified according to their pH, SOC content and Ca, Cu, Mg, Rb, and Zn concentrations. The inference is that areas of former infield and settlement elsewhere at this study location in the Central Highlands may be able to be identified according to their soil chemical composition and use of discriminant function, even though the surface remains of pre-eighteenth century settlement sites are not readily evident today because they were constructed of perishable materials.

Applicability of Standardless Semiquantitative Analysis of Solids by High-Irradiance Laser Ionization Orthogonal Time-of-Fight Mass Spectrometry

A compact high-irradiance laser ionization time-of-flight mass spectrometry system has been developed for the multielemental analysis of solids. Helium was introduced into the ion source as a buffer gas to cool high kinetic energy ions and suppress the interference of multicharged ions. A special pulse train repelling mode was used to achieve explicit spectra. Two quantitative methods are described for the laser ionization mass spectrometry in this paper. The first of these is the routine calibration curve quantitation, in which various matrix-matched standards are required; the second method, which is based on the uniform correlation between the signal and elemental concentration of different samples, is more convenient and covers a typical dynamic range of 6 orders. All the investigations and results indicate satisfactory performance of the newly developed instrument and its applicability for simultaneous multielemental analysis of solid samples.

Searching the Most Appropriate Sample Pretreatment for the Elemental Analysis of Wines by Inductively Coupled Plasma-Based Techniques

Different sample preparation methods were evaluated for the simultaneous multielement analysis of wine samples by inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS). Microwave-assisted digestion in closed vessel, thermal digestion in open reactor, and direct sample dilution were considered for the determination of Li, Be, Na, Mg, Al, K, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Sr, Y, Mo, Cd, Ba, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Tl, Pb, and Bi in 12 samples of red wine from Valencia and Utiel-Requena protected designation of origin. ICP-MS allows the determination of 17 elements in most of the samples, and using ICP-OES, a maximum of 15 elements were determined. On comparing the sample pretreatment methodology, it can be concluded that the three assayed procedures provide comparable results for the concentration of Li, Na, Mg, Al, K, Ca, Mn, Fe, Zn, and Sr by ICP-OES. Furthermore, ICP-MS data found for Cu, Pb, and Ba were comparable. Digestion treatment provides comparable values using both total decomposition in open system and microwave-assisted treatment for Cu by ICP-OES and for Cr, Ni, and Zn by ICP-MS. Open vessel total digestion provides excess values for Cr, Mn, Fe, and Zn by ICP-OES and defect values for Se. However, direct measurement of diluted wine samples provided uncomparable results with the digestion treatment for Mn, Cu, Pb, Zn, Ba, and Bi by ICP-OES and for Mg, Cr, Fe, Ni, and Zn by ICP-MS. Therefore, it can be concluded that microwave-assisted digestion is the pretreatment procedure of choice for elemental analysis of wine by ICP-based techniques.

Laser-induced breakdown spectroscopy: A versatile tool for monitoring traces in materials

Laser-induced breakdown spectroscopy (LIBS) is an emerging technique for simultaneous multi-elemental analysis of solids, liquids and gases with minute or no sample preparation and thus revolutionized the area of on-line analysis technologies. The foundation for LIBS is a solid state, short-pulsed laser that is focused on a sample to generate a high-temperature plasma, and the emitted radiation from the excited atomic and ionic fragments produced within the plasma is characteristic of the elemental composition of the sample that can be detected and analyzed using a suitable optical spectrograph. In the present paper, the applicability of LIBS for different solid samples having homogeneous (silver ornament, aluminum plate) or heterogeneous composition (soil) using nanosecond laser pulses is discussed. Nanosecond pulse laser makes plasma at the sample surface even at very low pulse energies and also allows for precise ablation of the substrate material with little damage to the surrounding area. We have also studied the penetration of different heavy metals inside the soil surface.

Development of an accurate, sensitive, and robust isotope dilution laser ablation ICP-MS method for simultaneous multi-element analysis (chlorine, sulfur, and heavy metals) in coal samples

A method for the direct multi-element determination of Cl, S, Hg, Pb, Cd, U, Br, Cr, Cu, Fe, and Zn in powdered coal samples has been developed by applying inductively coupled plasma isotope dilution mass spectrometry (ICP-IDMS) with laser-assisted introduction into the plasma. A sector-field ICP-MS with a mass resolution of 4,000 and a high-ablation rate laser ablation system provided significantly better sensitivity, detection limits, and accuracy compared to a conventional laser ablation system coupled with a quadrupole ICP-MS. The sensitivity ranges from about 590 cps for (35)Cl+ to more than 6 x 10(5) cps for (238)U+ for 1 microg of trace element per gram of coal sample. Detection limits vary from 450 ng g(-1) for chlorine and 18 ng g(-1) for sulfur to 9.5 pg g(-1) for mercury and 0.3 pg g(-1) for uranium. Analyses of minor and trace elements in four certified reference materials (BCR-180 Gas Coal, BCR-331 Steam Coal, SRM 1632c Trace Elements in Coal, SRM 1635 Trace Elements in Coal) yielded good agreement of usually not more than 5% deviation from the certified values and precisions of less than 10% relative standard deviation for most elements. Higher relative standard deviations were found for particular elements such as Hg and Cd caused by inhomogeneities due to associations of these elements within micro-inclusions in coal which was demonstrated for Hg in SRM 1635, SRM 1632c, and another standard reference material (SRM 2682b, Sulfur and Mercury in Coal). The developed LA-ICP-IDMS method with its simple sample pretreatment opens the possibility for accurate, fast, and highly sensitive determinations of environmentally critical contaminants in coal as well as of trace impurities in similar sample materials like graphite powder and activated charcoal on a routine basis.

Simultaneous multi-element analysis of some edible pulses using neutron activation analysis

This paper comprises the application of instrumental neutron activation analysis (INAA) for multi-element determination in some edible pulse samples. These edible pulses are usually daily used in the Egyptian kitchen. These were: anise, cumin, coriander, caraway, black cumin, white kidney bean, lupine, lentil, chickpea, broad bean, peanut, almond, and fenugreek. The pulses have been analyzed as dehulled pulses, in the case of legume and oil pulses with simultaneous analysis of their respective skins. The determined elements were: Ce, Co, Cr, Cs, Eu, Fe, Hf, Rb, Sb, Sc, Sr, Th and Zn. The element content in the dehulled pulses and their respective skins has been compared. Some elements were major or minor elements where others were trace elements. Standard reference materials were used to assure quality control, accuracy and precision of the technique.

Improvement of Metals and Phosphorus Analysis in Water Samples by Inductively Coupled Plasma Optical Emission Spectroscopy, Radio Frequency Power, and Nebulizer Gas Flow Rate Modification

Inductively coupled plasma optical emission spectrometry (ICP‐OES) is a powerful tool for simultaneous multielement analysis. The objective of this study was to determine optimum ICP‐OES operational parameters for aluminum (Al), copper (Cu), iron (Fe), manganese (Mn), sodium (Na), phosphorus (P), and zinc (Zn) in natural water samples. Five radio‐frequency forward powers (RF powers) and four nebulizer gas flow rates were tested. Different RF power values and nebulizer gas flow rates were found to be ideal for each element. Performance was best for Al, Na, and P at 1400 W RF power, whereas the optimal nebulizer gas flow rate for Na, Fe, Zn, and Al was 1 L min−1. The differences in RF power and nebulizer gas flow rates were found to be driven by changes in 1) element emission lines for different RF powers and 2) evaporation rates, mean diameter drop sizes, solvent loading, and analyte signal intensities for different nebulizer gas flow rates and analyte concentrations. Grouping the elements with similar parameters will avoid reading delays.

A Simple Method for Precise Determination of 23 Trace Elements in Granitic Rocks by ICP-MS after Lithium Tetraborate Fusion

Abstract. An improved alkali fusion method followed by HF-HNO3-HC1O4 treatment is performed for simultaneous determination of 23 trace elements (Sr, Y, Zr, Nb, Ba, Hf, Ta, Th, U, and REE) by ICP-MS in rock reference materials: basaltic rocks (JB-2, JB-3) and granitic rocks (JG-la, JG-2, JG-3). Our improved method offers several advantages including: (1) suppression of whitish precipitates probably composed of insoluble fluorides by addition of HCIO4, (2) simple and reliable preparation procedure, (3) instrument calibration which enables straightforward simultaneous multi-elemental analysis, and (4) the very low background levels by using pure lithium tetraborate flux. We obtained the analytical results with a reproducibility of mostly <2 % (1s) for the basaltic rocks and <7 % for the granitic rocks. The higher relative standard deviation (RSD) values for granitic rocks may be attributed to sample heterogeneity of coarse-grained granitic rocks. The analytical results of the granitic rocks demonstrate that Zr and Hf abundances are consistent with the compiled values and that REE concentrations agree well with recently published data, suggesting that the Li2B4O7 fusion method applied in the present study is suitable for the analysis of the granitic rocks.

Identify the injury implements by SEM/EDX and ICP-AES

The forensic investigator is frequently confronted with the discrimination and deduction of injury implements, which is one of the most important physical testimonies in courts. The usual method used in actual cases is from points of morphology. In the forensic discrimination of injury implements, such as metal implements, the analysis and comparison of elements are expected to provide excellent results, and simultaneous multi-elemental analysis is required to analyze various kinds of elements. This study was designed to establish discrimination and deduction of metal injury implements by scanning electron microscope/energy disperse X-ray microanalyzer (SEM/EDX) and inductively coupled plasma atomic emission spectrometry (ICP-AES). Examined metal particles in five wounds made on the skin of domestic pigs, respectively, using Cu–Zn or Cr–Ni coated and carbon steel kitchen implements by EDX. For carbon steel kitchen implements, analyzed five samples from the back and blade separately in the contents and varieties of elements by ICP-AES. In the wounds by the coated implements, the special particles only containing Cu, Zn or Cr, Ni were found. In the wounds by carbon steel kitchen implements, the particles containing Fe, Cr, Si or Fe, Mn, Si were found. The differences of contents of elements between the back and blade was no significant except No. 5 for carbon steel kitchen implements, and the significant differences of elements exited in Cr, Mn, Si, Cu, Mo among the stainless kitchen knives, Mn, Si among the other kitchen implements and for the blade of No. 5 knife, relative standard deviations (R.S.D.s) were significantly different in Mn, Si, Mo, Ti, S, P, Ni. Using EDX to examine the particles in wounds can deduce the categories of metal injury implements, and we can still deduce the different implements in the same category by ICP-AES.

Laser ablation–inductively coupled plasma–dynamic reaction cell–mass spectrometry for the multi-element analysis of polymers

In this work, the potential of laser ablation–inductively coupled plasma–mass spectrometry for the fast analysis of polymers has been explored. Different real-life samples (polyethylene shopping bags, an acrylonitrile butadiene styrene material and various plastic bricks) as well as several reference materials (VDA 001 to 004, Cd in polyethylene) have been selected for the study. Two polyethylene reference materials (ERM-EC 680 and 681), for which a reference or indicative value for the most relevant metals is available, have proved their suitability as standards for calibration. Special attention has been paid to the difficulties expected for the determination of Cr at the μg g − 1 level in this kind of materials, due to the interference of ArC + ions on the most abundant isotopes of Cr. The use of ammonia as a reaction gas in a dynamic reaction cell is shown to alleviate this problem, resulting in a limit of detection of 0.15 μg g − 1 for this element, while limiting only modestly the possibilities of the technique for simultaneous multi-element analysis. In this regard, As is the analyte most seriously affected by the use of ammonia, and its determination has to be carried out in vented mode, at the expense of measuring time. In all cases studied, accurate results could be obtained for elements ranging in content from the sub-μg g − 1 level to tens of thousands of μg g − 1 . However, the use of an element of known concentration as internal standard may be needed for materials with a matrix significantly different from that of the standard (polyethylene in this work). Precision ranged between 5% and 10% RSD for elements found at the 10 μg g − 1 level or higher, while this value could deteriorate to 20% for analytes found at the sub-μg g − 1 level. Overall, the technique evaluated presents many advantages for the fast and accurate multi-element analysis of these materials, avoiding laborious digestion procedures and minimizing the risk of analyte losses due to the formation of volatile compounds.

Simultaneous multi-element analysis of total As, Se and Sb on titanium dioxide by slurry sampling—graphite furnace atomic absorption spectrometry

A simple and rapid method for simultaneous determination of As, Se and Sb was studied by graphite furnace atomic absorption spectrometry (GFAAS). Titanium dioxide adsorbing As, Se and Sb was separated from sample solution (100 ml) with a membrane filtration (0.45 μm), and then prepared to be slurry (5.0 ml) by adding ultrapure water. The behavior and influence of titanium dioxide on determination of As, Se and Sb were investigated in this experiment. The optimal conditions of a furnace for these elements were chosen as follows: pyrolysis temperature was 150 °C, and atomization temperature was 2300 °C. The optimal conditions of adsorption for As, Se and Sb on titanium dioxide were listed: pH 2.0 in sample solution; 10 min of stirring time; and 20.0 mg titanium dioxide. The difference of the chemical valence of each element had no effect on the recovery of each element at the same optimal conditions. Limits of detection (3 σ) for As, Se and Sb were found to be 0.21 μg l −1, 0.15 μg l −1 and 0.15 μg l −1, respectively, with enrichment rate of 20, when 20 μl of slurry was injected into a Zr-coating tube. The proposed method was applied to tap water and river water.

Analytical Characteristics of a Continuum-Source Tungsten Coil Atomic Absorption Spectrometer

A continuum-source tungsten coil electrothermal atomic absorption spectrometer has been assembled, evaluated, and employed in four different applications. The instrument consists of a xenon arc lamp light source, a tungsten coil atomizer, a Czerny-Turner high resolution monochromator, and a linear photodiode array detector. This instrument provides simultaneous multi-element analyses across a 4 nm spectral window with a resolution of 0.024 nm. Such a device might be useful in many different types of analyses. To demonstrate this broad appeal, four very different applications have been evaluated. First of all, the temperature of the gas phase was measured during the atomization cycle of the tungsten coil, using tin as a thermometric element. Secondly, a summation approach for two absorption lines for aluminum falling within the same spectral window (305.5-309.5 nm) was evaluated. This approach improves the sensitivity without requiring any additional preconcentration steps. The third application describes a background subtraction technique, as it is applied to the analysis of an oil emulsion sample. Finally, interference effects caused by Na on the atomization of Pb were studied. The simultaneous measurements of Pb and Na suggests that negative interference arises at least partially from competition between Pb and Na atoms for H2 in the gas phase.

Fraunhofer Effect Atomic Absorption Spectrometry

The dark lines in the solar spectrum were discovered by Wollaston and cataloged by Fraunhofer in the early days of the 19th century. Some years later, Kirchhoff explained the appearance of the dark lines: the sun was acting as a continuum light source and metals in the ground state in its atmosphere were absorbing characteristic narrow regions of the spectrum. This discovery eventually spawned atomic absorption spectrometry, which became a routine technique for chemical analysis in the mid-20th century. Laboratory-based atomic absorption spectrometers differ from the original observation of the Fraunhofer lines because they have always employed a separate light source and atomizer. This article describes a novel atomic absorption device that employs a single source, the tungsten coil, as both the generator of continuum radiation and the atomizer of the analytes. A 25-microL aliquot of sample is placed on the tungsten filament removed from a commercially available 150-W light bulb. The solution is dried and ashed by applying low currents to the coil in a three-step procedure. Full power is then applied to the coil for a brief period. During this time, the coil produces white light, which may be absorbed by any metals present in the atomization cloud produced by the sample. A high-resolution spectrometer with a charge-coupled device detector monitors the emission spectrum of the coil, which includes the dark lines from the metals. Detection limits are reported for seven elements: 5 pg of Ca (422.7 nm); 2 ng of Co (352.7 nm); 200 pg of Cr (425.4 nm); 7 pg of Sr (460.7 nm); 100 pg of Yb (398.8 nm); 500 pg of Mn (403.1 nm); and 500 pg of K (404.4 nm). Simultaneous multielement analyses are possible within a 4-nm spectral window. The relative standard deviations for the seven metals are below 8% for all metals except for Ca (10.7%), which was present in the blank at measurable levels. Analysis of a standard reference material (drinking water) resulted in a mean percent recovery of 91%. This report attempts to give an historical perspective on the development of a novel atomic spectrometer based on the Fraunhofer effect.

ＰＩＸＥ法による石英繊維フィルターに捕集された大気粉じんの多元素同時分析

石英繊維フィルターに捕集された大気粉じんのPIXE法による元素分析の確立を目的に, 小型チャンバー等を用いてPd-carbon粉末を混入させたNIST標準物質 (Urban Particulate Matter; SRM 1648) を石英繊維フィルター (Pallflex Fiber Filter, Model 2500 QAST, 47mmφ) 上に捕集し, 硝酸による簡便な化学的前処理を行い, フィルター上からのNIST標準物質の脱離状況と分析精度を検討した。フィルター試料からのNIST標準物質は, 簡便な小型容器を用いた硝酸―マイクロウェーブ法によりほぼ完全に脱離していることが確認できた。PIXE分析による元素定量値は, NIST標準物質の認証値及び参考値に対して70～110%で, 概ね一致する結果が得られた。