Multi-element Standards Research Articles

Analytical performance characteristics of Micro-structured surfaces for laser-induced breakdown spectroscopic analysis of liquids

We have previously shown the design and fabrication studies of 3-D micro-structured surfaces, to be used as a sample loading substrate for liquids analysis via dried-droplet LIBS methodology. Among the three designs, the substrate structured with 20-μm diameter cylinders, CYL-20, has shown the highest signal enhancement for the elements, Cu, Cr, and Pb, compared to 5-μm diameter cylinders, CYL-5, and 5-μm side-length triangular prisms, TAP-5, surfaces. Here, in this study, the analytical performance characteristics (LOD, accuracy, and precision) of these micro-structured Si-wafer surfaces are presented in comparison with unstructured surfaces. The dried-droplet residue of aqueous heavy metal solutions of Pb, Cr, and Cu were analyzed at their respective emission wavelengths under optimized experimental conditions. The results obtained from CYL-20 structured surfaces in comparison to 300 nm thin-film coated surfaces indicate up to 17, 11, and 7-fold increases in LIBS signal strength for Cu, Cr, and Pb, respectively. The experiments were performed using single and multi-element standards, and certified reference water samples. Sub-picogram absolute detection limits, 0.8 pg Pb, 0.5 pg Cu, and 0.45 pg Cr were obtained from the analysis of 500 nanoliters standard solutions, via dried-droplet methodology. Results with 70–75% accuracy and 95% precision were obtained from the repeated measurements. Though the results are promising, more extensive fabrication and application studies are required to find optimum structures of different sizes and shapes.

Self-characterization of irradiation facility using synthetic multi-element standard for determination of k0-factors of seven radionuclides of interest

In this study, the k0 factors of 7 short and medium-lived radionuclides (i.e. 66Cu, 52V, 38Cl, 134mCs, 128I, 140La and 56Mn) were experimentally determined at the Dalat nuclear research reactor (DNRR). The synthetic multi-element standard (SMELS) samples were irradiated at Channel 7-1 installed at the DNRR. SMELS Type III contains Au and Zr, thus also allowing the self-characterization of the irradiation facility (i.e. the direct determination of f and a with only this material). The k0 factors of 7 short and medium-lived radionuclides obtained in this work are a good agreement with the reference k0 factors. The ratio values between the experimental and reference k0 values were 66Cu of 1.004, 52V of 1.004, 38Cl of 0.961 and 0.976 (1642.7 keV and 2167.4keV, respectively), 134mCs of 0.831, 128I of 1.022, 140La of 0.936, 0.955 and 0.955 (328.8 keV, 487.0 keV and 1596.2keV, respectively), 56Mn of 0.985 and 0.973 (846.8 keV and 1810.7keV, respectively). The radionuclides range of uncertainty values were lower than 7%. The present result indicates that the k0 factors can be determined by using synthetic multi-element standards (SMELS).

Effect of sample carriers on analytical parameters in total reflection X-ray fluorescence - a tool for multi-trace elemental analysis

The Total reflection X-ray Fluorescence technique is increasingly popular for its simplicity and rapid elemental screening. This study evaluates the various analytical parameters including spectroscopic resolution, absolute sensitivity, relative element sensitivity, lowest limits of detection, accuracy and precision of the Total reflection X-ray Fluorescence spectrometer. This evaluation is conducted using quartz and acrylic sample carriers with mono and multi-element standards. Notably, the quartz sample carrier demonstrated excellent values of spectroscopic resolution, absolute sensitivity, the lowest limits of detection, a recovery rate of 90–110% and a coefficient of variation of 3–6% for the quantified elements from mono and multi-element standards. These findings underscore the robust analytical capability of the Total reflection X-ray Fluorescence technique for multi-trace elemental analysis. This research article not only provides practical and straightforward guidelines for handling Total reflection X-ray Fluorescence spectrometer but also confirms the practicality and effectiveness of the sample carriers for rapid and reliable elemental screening applications.

Semiquantitative Analysis for High-Speed Mapping Applications of Biological Samples Using LA-ICP-TOFMS.

Laser ablation (LA) in combination with inductively coupled plasma time-of-flight mass spectrometry (ICP-TOFMS) enables monitoring of elements from the entire mass range for every pixel, regardless of the isotopes of interest for a certain application. This provides nontargeted multi-element (bio-)imaging capabilities and the unique possibility to screen for elements that were initially not expected in the sample. Quantification of a large range of elements is limited as the preparation of highly multiplexed calibration standards for bioimaging applications by LA-ICP-(TOF)MS is challenging. In this study, we have developed a workflow for semiquantitative analysis by LA-ICP-TOFMS based on multi-element gelatin micro-droplet standards. The presented approach is intended for the mapping of biological samples due to the requirement of matrix-matched standards for accurate quantification in LA-ICPMS, a prerequisite that is given by the use of gelatin-based standards. A library of response factors was constructed based on 72 elements for the semiquantitative calculations. The presented method was evaluated in two stages: (i) on gelatin samples with known elemental concentrations and (ii) on real-world samples that included prime examples of bioimaging (mouse spleen and tumor tissue). The developed semiquantification approach was based on 10 elements as calibration standards and provided the determination of 136 nuclides of 63 elements, with errors below 25%, and for half of the nuclides, below 10%. A web application for quantification and semiquantification of LA-ICP(-TOF)MS data was developed, and a detailed description is presented to easily allow others to use the presented method.

Bioaccessibility, exposure and risk assessment of potentially toxic elements and essential micronutrients in ayurvedic, traditional Chinese and Ghanaian medicines.

Potentially toxic constituents in traditional medicines remain a concern due to health risks posed to consumers. Thirty-six traditional medicines (TM) consisting of 14 Indian Ayurvedic Medicines, 11 Chinese Traditional Medicines and eleven Ghanaian Traditional Medicines were evaluated using Total Reflection X-ray Fluorescence Spectrometer (T-XRF) after microwave assisted acid digestion. Physiologically Based Extraction Test (PBET) was used to obtain bioaccessible elemental concentrations. Merck XVI multi-element standard were used to evaluate the accuracy of the analytical method. The concentrations of the elements were quantified in (mg kg-1): Cr (0.01-698), Mn (0.01-1140), Fe (15-73300), Ni (1-1340), Cu (3-8160), Zn (0.01-224). The greatest bioaccessible concentrations of arsenic was 0.80mgkg-1 and 0.44mgkg-1 in the gastric and intestinal phases respectively. In order to evaluate the human health risks from ingesting these TM, the Acceptable Daily Intake (ADI) was calculated for each medicine based on element-specific bioaccessibility-adjusted concentrations and results compared with the United States Environmental Protection Agency (USEPA) Reference Dose (RfD) limits. The Acceptable Daily Intake (ADI) values for risks were within the USEPA RfD. Hazard quotients (HQ) of TM were < 1, meaning elemental concentrations do not pose non-carcinogenic risks to adult consumers. In summary the methods applied in the study gives a new insight on human health risks of potentially toxic and essential micronutrients elements in TM.

The potential of bioprinting for preparation of nanoparticle-based calibration standards for LA-ICP-ToF-MS quantitative imaging.

This paper discusses the feasibility of a novel strategy based on the combination of bioprinting nano-doping technology and laser ablation-inductively coupled plasma time-of-flight mass spectrometry analysis for the preparation and characterization of gelatin-based multi-element calibration standards suitable for quantitative imaging. To achieve this, lanthanide up-conversion nanoparticles were added to a gelatin matrix to produce the bioprinted calibration standards. The features of this bioprinting approach were compared with manual cryosectioning standard preparation, in terms of throughput, between batch repeatability and elemental signal homogeneity at 5μm spatial resolution. By using bioprinting, the between batch variability for three independent standards of the same concentration of 89Y (range 0-600mg/kg) was reduced to 5% compared to up to 27% for cryosectioning. On this basis, the relative standard deviation (RSD) obtained between three independent calibration slopes measured within 1 day also reduced from 16% (using cryosectioning) to 5% (using bioprinting), supporting the use of a single standard preparation replicate for each of the concentrations to achieve good calibration performance using bioprinting. This helped reduce the analysis time by approximately 3-fold. With cryosectioning each standard was prepared and sectioned individually, whereas using bio-printing it was possible to have up to six different standards printed simultaneously, reducing the preparation time from approximately 2 h to under 20 min (by approximately 6-fold). The bio-printed calibration standards were found stable for a period of 2 months when stored at ambient temperature and in the dark.

Production and characterization of standard particles for rL-SNMS

In this work, uranium-and plutonium-baring particles were produced by fast iron co-precipitation for the purpose of creating homogeneous multi-element standards. A set of single isolated particles showing no inhomogeneities in the element distribution were selected. These particles were used to determine the maximal achievable suppression ratios for uranium in Resonant Laser Secondary Neutral Mass Spectrometry (rL-SNMS) measurements of plutonium. It was shown for the first time directly that suppression-ratios in the order of three magnitudes are achievable with a resonant two-step excitation scheme for non-destructive measurements.

Post-measurement compressed calibration for ICP-MS-based metal quantification in mine residues bioleaching.

Bioleaching is an actual economical alternative to treat residues, which allows, depending on the chosen strategy, two possible outcomes: (1) a leachate enriched with target metals, or (2) a residue enriched in target metals through the leaching of interfering components (IC). This work aimed to study the metals released by bioprocessing the Panasqueira mine tailings, as a strategy to increase critical metals' relative concentration in residues. Biostimulation of the local microbiota was compared to a bioaugmentation approach using the autochthonous Diaphorobacter polyhydroxybutyrativorans strain B2A2W2. Inductively Coupled Plasma Mass Spectrometry (ICP-MS) was selected to study the metals released in the leachate through multi-element external standards. A new data treatment method was developed to use a preliminary sweep of intensities to quantify the non-initial target metals concentration in the leachate, based on preliminary ICP-MS intensity measurements. The results demonstrated that biostimulation was an efficient bioleaching strategy for the IC silicon, aluminium, magnesium, selenium, manganese, zinc, iron, and copper, by decreasing concentration, resulting in a relative increase in the gallium and yttrium (10x) levels in the treated residue. The strategy followed to quantify a large number of elements with ICP-MS using a reduced number of data points for calibration proved valid and speeded up the analytical process.

Quantification in bioimaging by LA-ICPMS - Evaluation of isotope dilution and standard addition enabled by micro-droplets

This study explores quantitative bioimaging as enabled by laser ablation-inductively coupled plasma time-of-flight mass spectrometry (LA-ICP-TOFMS), designing standardization methods based on robotic micro-droplet dispensing. The potential of producing controlled and highly precise pL-volume droplets was exploited to establish on-tissue isotope dilution and standard addition. Both strategies eliminate matrix effects and offer high metrological order traceable to SI units. The absolute quantity was obtained for μm-sized regions of interest in tissue samples, as defined by the extension of the deposited pL-volume droplet. While the gold standard isotope dilution (ID) was restricted to the accurate quantification of a single element, i.d. platinum in different tissue samples (mouse liver, spleen and tumor tissue), multiplexed matrix-matched calibration was obtained by on-tissue standard addition by depositing a dilution series of certified multi-element standards. Here, the working range was determined by the heterogeneity of the tissue samples and the background levels of elements intrinsically present and/or artificially introduced during sample preparation. Both methods, ID and standard addition served as reference methods for validation of external calibration using gelatin-based micro-droplet standards. Given full ablation, these external standards revealed a high dynamic range together with an excellent repeatability. Where applicable, the cross-validation revealed consistent quantitative results for the three quantification approaches. The comparable sensitivity obtained for standard addition and external standardization, respectively expressed as slope of the calibration function, provided proof that gelatin-based micro-droplets could serve as matrix-matched calibrations. Therefore, gelatin micro-droplets offer a valid tool for multiplexed matrix-mimicking standardization at high-throughput.

Recovery of critical metals from leach solution of electronic waste using magnetite electrospun carbon nanofibres composite.

Scarcity in mining and geo-political direction diverts attention toward critical metal recycling. Gallium (Ga), indium (In) and germanium (Ge) are among the critical metals that consume approximately 80% of world mining in the innovative production of electrical and electronic equipment. The fast obsolescing rate generates a large amount of electronic waste, which is now seen as a secondary reservoir for critical metals. These metal resources need to be dealt with with effective recycling capabilities. Based on solid-phase extraction, magnetic nano-hydrometallurgy is opening a new area of metallic contents recovery in conventional hydrometallurgy. In the present work, polyacrylonitrile (PAN) based electrospun nanofibres were synthesized and carbonized at 800°C in an inert environment. After surface oxidation, carbon nanofibres were decorated with magnetite particles through co-precipitation. The saturation magnetization value (Ms = 23.6emu/g) confirms high loading of magnetite particles. The selected critical metal ions are freely present in an aqueous solution at pH 1 to 3; thus, highest removal efficiency was observed at pH 2. Pseudo-second-order kinetics confirm the chemical/charge interaction between sorbent and sorbate ions. Maximum sorption capacity calculated through Langmuir isotherm was 226, 191 and 171mg/g for Ge(IV), Ga(III) and In(III) metal ions, respectively. The RL value (0 < RL < 1) indicates favourable sorption process. The sorbed target metal ions were collectively eluted using 1mol/L hydrochloric acid. The preconcentration factor was calculated at 1080 for Ge(IV) and In(III) while 1260 for Ga(III). The method was validated with 5µg/mL spiked multi-element standards and applied to multiple acid-leached electronic waste samples like PCBs, waste LCD panels and solar panels. Recoveries in the range of 96.2% for Ga(III), 95.6% for In(III) and 97.4% for Ge(IV) in the presence of diverse ions indicate the suitability of the proposed method for target metal ions even in a complex matrix.

Online microdroplet calibration for accurate nanoparticle quantification in organic matrices.

Single-particle inductively coupled plasma time-of-flight mass spectrometry (spICP-TOFMS) is a high-throughput method for the multiplexed analysis of nanoparticles (NPs). However, matrix interferences are a significant challenge that must be overcome for accurate NP sizing and number concentration determination. In online microdroplet calibration, multi-element droplet standards are mixed with nebulized aerosols from a NP-containing sample in a dual-sample introduction system before entering the ICP. Microdroplet standards are used to determine absolute sensitivities and calibrate the mass amount(s) of analyte element(s) in particle events. A plasma-uptake standard is added to NP-containing samples to account for variations in the nebulization and transport efficiency of aerosols into the plasma, which are used in the determination of particle number concentrations (PNCs). Since the microdroplets experience the same plasma conditions as analyte NPs, this creates a matrix-matched calibration. We studied the efficacy of online microdroplet calibration for the quantification of NPs in three organic matrices: ethanol, acetone, and acetonitrile. Organic solvents can cause a pronounced increase in sample uptake and cause plasma-related signal attenuation for nanoparticle measurements. Online microdroplet calibration corrects for both effects without the use of nanoparticle standards. Our results demonstrate accurate NP sizing and PNC determinations in organic matrices up to 98% (v/v), even when these matrices caused signals to be attenuated up to 35-times and nebulizer transport efficiencies to be up to four-times higher than that of a pure water matrix.

Development and testing of a multi-element ICP standard

Determination of the calibration dependence of spectrometers’ output signal on the content of the measured elements is of great importance for the metrological assurance of the high-precision inductively coupled plasma (ICP) massspectrometry and optical emission spectrometry methods. This paper presents the results of a study on establishing the certified values of reference material of composition of multi-element solution of metals intended for inductively coupled plasma methods (ICP-CRM solution Multi 1). The reference material (RM) is a solution with certified values of the mass fraction of metals: barium, cadmium, cobalt, lithium, lead, and zinc. The solution was packed in high-density polyethylene bottles with the capacity of 4, 8, 15, 30, 60 and 125 cm 3 . The certified value of the mass fraction of metals in the solution was established by the calculation and experimental procedure and confirmed by the GET 217-2018 State Primary Standard of Unit of Mass Fraction and Unit of Mass (Molar) Concentration of Inorganic Components in Aqueous Solutions Based on Gravimetric and Spectral Methods. The permissible certified values of the mass fraction of metals in the developed ICP-CRM are shown to range from 900 mg/kg to 1100 mg/kg. The authors have embarked on the study of the reference material by testing RMs for long-term stability and determination of the RMs’ expiration date. It is assumed that the expanded uncertainty of measurements of the certified value of the mass fraction of metals in the solution of the multi-element ICP-CRM solution Multi 1 will not exceed 0.5 %. The ICP-CRM solution Multi 1 can be used for ensuring the metrological traceability of measurements in inorganic analysis using ICP-MS and ICP-OES to the GET 217-2018. The developed solution will also allow one of the main advantages of these methods to be applied in routine analysis, namely the ability to quickly and simultaneously measure several elements in samples.

Quantitative Imaging of Silver Nanoparticles and Essential Elements in Thin Sections of Fibroblast Multicellular Spheroids by High Resolution Laser Ablation Inductively Coupled Plasma Time-of-Flight Mass Spectrometry.

We applied high resolution laser ablation inductively coupled plasma time-of-flight mass spectrometry (LA-ICP-TOF-MS) with cellular spatial resolution for bioimaging of nanoparticles uptaken by fibroblast multicellular spheroids (MCS). This was used to quantitatively investigate interactions of silver nanoparticles (Ag NPs) and the distributions of intrinsic minerals and biologically relevant elements within thin sections of a fibroblast MCS as a three-dimensional in vitro tissue model. We designed matrix-matched calibration standards for this purpose and printed them using a noncontact piezo-driven array spotter with a Ag NP suspension and multielement standards. The limits of detection for Ag, Mg, P, K, Mn, Fe, Co, Cu, and Zn were at the femtogram (10-15 g) level, which is sufficient to investigate intrinsic minerals in thin MCS sections (20 μm thick). After incubation for 48 h, Ag NPs were enriched in the outer rim of the MCS but not detected in the core. The localization of Ag NPs was inhomogeneous in the outer rim, and they were colocalized with a single-cell-like structure visualized by Fe distribution (pixel size of elemental images: 5 × 0.5 μm). The quantitative value for the total mass of Ag NPs in a thin section by the present method agreed with that obtained by ICP-sector field (SF)-MS with a liquid mode after acid digestion.

Quantification techniques of mass-separation and ion yield for the detection of radioactive isotopes

This research demonstrates two methods of quantifying ion yield efficiency using an inductively coupled plasma mass spectrometer. The mass spectrometer is used as a means of separation where individual decay mass-chains are isolated (i.e., implanted) onto a conductive substrate. Quantifying the ion yield of this recovery process is crucial to understanding the abundance of the separated isotope present in the unseparated starting sample. The first method measured the accumulated charge directly incident on the conductive substrate in real-time while the second method performed a full chemical analysis of the substrate after dissolution. Our previous results demonstrated and compared these quantification methods with a multi-element standard of stable isotopes. This research expands on previous results and utilizes the stable mass ion yield to quantify trace amounts of the (radioactive) isotope of interest present in the sample. The mass-separated radioactive isotopes were fission products produced from thermal neutron irradiation of a highly enriched 235U foil. Five peak-yield mass chains were targeted. The results indicate good correlation between the two methods of measuring the ion yield and imply that coupling this method with traditional radiometric counting can result in an accurate means of quantifying radioactive isotopes. The final results we report here are within 1-sigma of the published cumulative fission yields.

Distribution of rare earth elements in coal combustion fly ash, determined by SHRIMP-RG ion microprobe

During coal combustion for electric power generation, rare earth elements (REE) are strongly retained in the ash fraction leading to significant enrichment compared to the REE content of the respective feed coals. Knowing how the REE are distributed in coal ash is essential to devising effective approaches for REE extraction from this potential resource. To better understand the distribution of REE in coal ash, we used the Stanford-USGS SHRIMP-RG ion microprobe to determine grain-scale REE partitioning in a suite of 19 U.S. and international coal fly ash samples. SHRIMP-RG microanalysis used a nominal spot size of 15μm and an oxygen negative-ion primary beam. NIST multi-element glass standards SRM 611 and SRM 613 were used for REE calibration. Prior to SHRIMP-RG analysis, samples were characterized by backscattered electron imaging and wavelength-dispersive elemental mapping to delineate constituents of interest for REE microanalysis. Results confirm the occurrence of REE in aluminosilicate glasses consistent with previous results that showed a strong positive correlation between Al and REE content in a larger group of U.S. and international coal fly ash samples. Among these glasses, aluminosilicates consisting of Al and Si and lacking other major constituents tend to have REE contents similar to, or slightly lower than the bulk sample REE content, whereas Ca- and/or Fe-enriched aluminosilicate glasses are similar to, or more REE-enriched than the bulk sample. Co-occurring quartz and/or high-silica glass is almost always the most REE depleted fly ash constituent, having much lower REE contents than the aluminosilicate glasses. Fe-oxide magnetospheres have REE content with relative proportions of light (LREE) to heavy (HREE) rare earths that are more variable than in the aluminosilicate glasses. Results suggest that extraction of REE from the aluminosilicate glass fraction in coal ash will yield a significant portion of the REE present and therefore, this fraction should be targeted in ongoing efforts to recover REE from coal fly ash.

Role of the mass attenuation coefficient database in standardization of a silicon drift X‐ray detector for PIXE analysis

A simple, inexpensive procedure is described for calibrating a silicon drift detector‐based PIXE system for the analysis of geological and other “thick‐target” materials. It rests on the use of single element, chemical compound, and National Institute for Standards and Technology multielement standards. Much less effort has been focussed on the impact of mass attenuation coefficients on PIXE's analytical accuracy than on ionization cross sections and fluorescence yields. The calibrated system enables us to investigate the effects of inserting different mass attenuation coefficient datasets into the GUPIX database. For the K X‐rays of light elements, accuracy is significantly improved by replacing the formerly used XCOM self‐attenuation coefficients by the corresponding FFAST values; this effect decreases rapidly with increasing atomic number. Similar improvement was found for L X‐rays of medium‐Z, but not for high‐Z atoms.

Gelatin gels as multi-element calibration standards in LA-ICP-MS bioimaging: fabrication of homogeneous standards and microhomogeneity testing.

Highly homogeneous multi-element gelatin calibration standards were fabricated for quantitative LA-ICP-MS bioimaging. Heterogeneity issues caused by the so-called "coffee-stain" and/or "Marangoni" effects were found to be element-dependent but could be circumvented by careful selection of drying/setting conditions. A micro-homogeneity test was developed for certification of the standards.

Comparison of different excitation modes for the analysis of light elements with a TXRF vacuum chamber

The aim of this work was to compare different excitation modes for the analysis of light elements from carbon (Z = 6) upwards using a total reflection X-ray fluorescence analysis (TXRF) vacuum chamber which allows the attachment of different X-ray tubes and detectors. In the first set of experiments, two water-cooled high-power X-ray tubes with Cr (Z = 25) and Cu (Z = 29) anodes, respectively, were compared with an air-cooled low-power tube with Mo anode (Z = 42) and a thin Be window for the transmission of Mo-L lines. In the first two cases, monochromatic Kα radiation was used for excitation, while in the case of the Mo tube the multilayer acted as a cut-off reflector and part of the Mo bremsstrahlung continuum together with the Mo-L series were used for excitation. Multi-element standards containing elements ranging from Na (Z = 11) to Ti (Z = 22) were analyzed by a silicon drift detector (SDD) with a 300 nm ultrathin polymer window (UTW). Detection limits were calculated and compared for the three excitation modes. The second set of experiments was performed using an air-cooled low-power X-ray tube with Rh anode (Z = 45) in order to show that a conventional SDD with a 25 μm beryllium window can be used for the detection of elements from Na upwards. The use of compact air-cooled low-power X-ray tubes together with Peltier-cooled SDDs with UTW should lead to the development of highly sensitive tabletop vacuum TXRF spectrometers with a design optimized for the analysis of light elements. Detection limits as achieved by vacuum chambers using conventional water-cooled high-power tubes (e.g. Streli et al., 2004) are realistically achievable with the new approach.

Analysis of SMELS by k 0-based IM-NAA method using PFTS position of KAMINI reactor for quality control exercise

As a part of QA/QC of k0-based internal monostandard neutron activation analysis (IM-NAA), three types of synthetic multielement standards (SMELS) were analyzed using pneumatic fast transfer system irradiation position of KAMINI reactor, IGCAR. Radioactive assay of activation products was carried out by high resolution gamma ray spectrometry. IM-NAA was used to determine relative concentration ratios of 22 elements with respect to gold internal monostandard. Absolute concentrations were calculated using assigned concentration of Au in all the types of SMELS. Z-score values within ±1 at 95.5 % confidence level and percentage deviations within ±5 % indicated good quality of the results by IM-NAA in most of the cases. Using this methodology, an ilmenite mineral sample was analyzed and concentrations of 14 elements were determined using Sc as monostandard.

Trace element determination in high-purity aluminum clad samples by k 0-based internal monostandard instrumental neutron activation analysis

The k0-based internal monostandard instrumental neutron activation analysis (IM-INAA) method was applied for quantification of trace impurities in seven high purity aluminum samples used as fuel cladding in a research reactor. Samples along with BCS CRM 182 (Si–Al alloy) were irradiated in high flux reactor neutrons for 10–15 h. In situ detection efficiency, needed in concentration calculation ratio by IM-INAA, was obtained using gamma rays of activation products produced in the samples. Elemental concentration ratios obtained with respect to Fe (used as internal monostandard) were converted to absolute concentrations by determining concentration of Fe by relative method of NAA. Concentrations of ten trace elements (Sc, Cr, Co, Zn, Ga, La, Ce, Sm, W and Hf) including major element Fe were determined in this work. The method used is non-destructive in nature and does not need multielement standards. Results of IM-INAA were compared with those obtained by relative method of INAA and inductively coupled plasma atomic emission spectrometry (ICP-AES). Details of methodologies and results obtained by all methods are discussed and compared in the paper.