The microstructural evolution of Sn-40Pb/Cu joints has been investigated under 125 o C thermal exposure conditions using single shear lap joints. A scanning electron microscope (SEM) was used to observe the morphology of the phases and energy dispersive x-ray (EDX) was used to estimate the elemental compositions of the phases. A double layer of Cu6Sn5 and Cu3Sn were observed. The Cu6Sn5 developed with a scalloped morphology, while the Cu3Sn always grew as a somewhat undulated planar layer in phase with the Cu6Sn5. The Cu6Sn5 layer began to transform from scallop shape to planar type after aging for 375 hours due to reduction in the interfacial energy. The intermetallic layers showed a linear dependence on the square root of aging time. The growth rate constant of the intermetallic compounds are estimated as 15.2 x 10 - 14 and 0.152 x 10 -14 cm 2 /s for Cu6Sn5 and Cu3Sn intermetallic, respectively.
Being an imperative material for man either used as building materials, pottery or as components in material industry and technology, knowledge of clays elemental contents is important. In the present study ten clay samples obtained from various locations in North-West Peninsular Malaysia were used. Majority of the clays were economically manufactured to be used as building materials or pottery. The objective of study was to determine the main elemental contents of the samples, and relate the results to the types of minerals, as well as to compare them with clays from other studies. In the study X-ray Fluorescence (XRF) coupled to samples dilution method and standard calibration samples was used. The elements detected in the study were Si, Al, Fe, Ti, K and Ca. Depending on locations, the percentage concentration ranged between 24.8 – 32.4 for Si, 10.8 – 19.0 for Al, 0.09 – 2.12 for Fe, 0.08 – 1.13 for Ti, 0.45 – 3.39 for K and trace amount of Ca and P. However, Mg that normally found in typical clay was not found in the studied samples. Comparing the oxide of the major elements with other studies, it was found that the clay samples contained mixtures of kaolinite (two-layered structure) and illite (three-layered structure).
Phenolic resin-silica nanocomposites samples in pellet shape have been successfully prepared by intercalation of polymer solution through the hot pressing method. The phenolic resin is modified with organic elastomers of silica nanoparticles, which is about 20 nanometer in diameter. The change of density and porosity was studied based on the addition of silica content in the phenolic resin composites. The densities of composites increased with the addition of the silica content from 10 wt.% to 40 wt.%. On the other hand, the porosity percentage was decreased with increasing of silica contents. The mechanical properties (Young’s modulus, energy to break and time to failure) of the nanocomposites samples were identified using the Universal Testing Material Machine (UTM). The results of Young’s modulus, energy to break and time to failure of the phenolic resin composites were found to be slightly increased with silica content from 10 wt.% to 30 wt.%. The X-Ray Microtomogaphy (XRM) topographies have shown that the porosity exists on fracture structure for each nanocomposite. The nanocomposites surface structure has been analyzed using Scanning Electron Microscope (SEM). The observation shows that the fracture surface of the pure phenolic resin is relatively smooth and glassy, which is typical for a brittle material, but the phenolic resin- silica composites fracture surface is not smooth at all. The observations indicate the pure phenolic resin is brittle than phenolic resin-silica nanocomposites. Consequently, the physical properties of the phenolic resin-silica nanocomposites were improved with the addition of 10 wt.% to 30 wt.% silica contents, as compared to that of the pure phenolic resin.
In these studies, cordierite was mechanically synthesized after a sol-gel process. The effect of milling time of cordierite was investigated. Aluminium nitrate nonahydrate, magnesium nitrate hexahydrate and tetraethylorthosilicate (TEOS) were used as starting materials. Gels obtained were mechanically activated in planetary ball mill by at 300rpm grinding speed and grinding time (15min, 30min, 45min and 60min). Powders produced were characterized by X-Ray Diffraction (XRD) and Field Emission Scanning Electron Microscope (FESEM) and Energy Dispersive X-Ray (EDX). XRD analysis proved that α-cordierite was formed at lower temperature (1200°C) as compliment to without grinding, whereby it is formed at1300°C. FESEM analysis shows the size of the cordierite were in submicron scale. EDX analysis proved that magnesium, aluminium, silicon and oxygen are elements existed in cordierite.
Sodium silicate was used to synthesize silica fine particles at room temperature using non-ionic surfactant of triethanolamine (TEA), dissolution salt and precipitating agent. The experiments were conducted by different composition of precursor material, nonionic surfactant and dissolution salt concentrations through the sol-gel process. Various particle sizes in the range 100-300nm were synthesized. The particle size of silica powders were analyzed via Field Emission Scanning Electron Microscope (FESEM), Energy Dispersive X-ray Analysis (EDAX), X-Ray Fluorescence (XRF), and Fourier Transformation Infrared (FTIR). The result has demonstrated that the particle size can be controlled by changing the ratio of non-ionic surfactant and dissolution salt or the sodium silicate concentration.
Chemical composition of fine (PM2.5) aerosol samples collected for the 5 years period (2001- 2005) using Gent Stacked filter unit sampler at Klang Valley (3 o 10 ’ 30 ’’ N, 101 o 43 ’ 24 ’’ E) were analysed using Neutron Activation Analysis (NAA) and Proton Induced X-ray Emission (PIXE). Results of the study show that the major component of the fine aerosol was black carbon and sulfur with the mass concentration ranged from 4.4 - 6.7µg m -3 and 1.2 - 1.9µg m -3 , respectively. The total fine aerosol mass concentration were in the ranged of 25 - 31µg m -3 with the reconstructed mass was about 50% as relative to the gravimetric mass. Statistical method, factor analysis with varimax approach has been applied to the aerosol composition data for the fingerprint identification. The analysis produces five identified fingerprint represent soil, industry, motor vehicles/biomass burning and Pb and Zn sources. There is also an unidentified source that could be related to unknown industrial activities.
Taman Negara is a famous tourism destination for nature lover in Malaysia. The area is well kept from human activities and disturbances. Since there is no data for human exposure to natural radiation, there is a need to do this study. It will give a baseline data for surface dose and radionuclide concentrations and one can estimate the external hazards index for the visitor to this unexplored area, i.e. UiTM-Perhilitan research station, Kuala Keniam, Taman Negara, Malaysia. The surface dose rate measurements were done in-situ using portable radiation survey meter at the surface and 1 m above the surface. The top soil samples were taken using hand auger up to 15 cm depth at nine locations around research station. Samples were brought back to the UiTM laboratory in Shah Alam, dried, ground to powder form, and sieved using 250 μm sieve. Then the uranium and thorium concentrations were analyzed using Energy Dispersive X-Ray Fluorescence (EDXRF).The mean value for surface dose rates on surface were 0.164 μSv/hr while the mean value for surface dose rates on 1m above the surface were 0.161 μSv/hr. The mean concentration of thorium was 2.62μg/g while the mean concentration of uranium was 0.61μg/g.
Considerable amount of uranium and thorium are found in our local zircon and the level is much higher than the maximum value adopted by Malaysia and many importing countries. Energy Dispersive X-ray Flourescence (EDXRF) proves to be a very valuable tool in the determination of these radioactive elements as it can perform the analysis simultaneously in shorter time. Quantitative analysis of this mineral involves the use of a fundamental parameter technique developed by National Bureau of Standard, USA and Geological Survey Canada (NBS-GSC FPT). The analysis for tin slag is more challenging as there is no reference standard of similar material. Thus the standard addition method was applied to correct the error from the matrix of the sample.
Measurement of major cation such as Na+, K+, and Ca2+ in water are normally carried out using
AAS, ICP-OES or flame photometry. In this study, an attempt was made to measure these cations
using Energy Dispersive X-ray Fluorescent Spectrometry (EDXRF). Hot spring s water was taken from varies hot spring in Selangor and divided into two portions that is filtered and unfiltered. 5 mL of water samples were pipette into a special liquid cups (sample holders) which has a thin mylar film underneath. The MiniPal4 XRF instrument was used in this study. The resolution for the instrument use is 145 keV with energy resolution at 5.9 keV. The spectrum of cations were analysed by using MiniPal/MiniMate software to determine the cations concentration. For K+ and Ca2+, Al-thin filter was used and default filter was used for Na+. The concentration of Na+ obtained for filtered and unfiltered samples were ranged from 38.00 to 66.05 and 43.26 to 76.95 ppm. Meanwhile, concentrations of K+ for filtered and unfiltered samples were ranged from 2.42 to 8.07 and 6.18 to 29.28 ppm. Concentrations of Ca2+ for filtered and unfiltered samples were ranged from 2.59 to 10.94 and 3.18 to 12.99 ppm.
Texture evolution of NiO formed during oxidation of polycrystalline single oriented (100) Ni-Cr was investigated. This foil was also termed rolling assisted biaxially textured substrate (RABiTS). X-ray diffractograms of oxidized Ni-Cr RABiTS foil showed the existence of mostly (200) NiO indicating (100)-type NiO formed exclusively on (100) singly oriented Ni-Cr grains. Epitaxial relationship between the two layers is observed. However the dual-in-plane texture was recorded.
The in-plane texture was assessed by conducting phi scan and plotting series of pole figures measured at (111) NiO peak. The mechanism of the oxides formation was proposed to take into account the formation of (100)-type NiO. Cross section morphology of the oxidised foils reveals two oxidation layers; fast growing external layer consisting of the (100)-type NiO and an internal layer consisted of mostly Cr2O3 and maybe NiCr2O4. The thickness of NiO was ~ 10Pm. Cr2O3 formed as needle-like oxides embedded in a matrix of Ni foil. Inward diffusion of oxygen is believed to have caused this to happen. The external NiO layer was consisted of duplex microstructure characterised by columnar layer growing vertical on the surface of the metal and a few micron thick of equiaxed NiO. Delamination of the outer NiO layer often occurred at the columnarequiaxed interface which could be cured by CeO2 deposition on the foil prior to the oxidation process. CeO2 was deposited by conversion immersion using Ce(NO3)3.6H2O solution. (200) NiO formed on this coated sample as well.
P-type transparent conductive oxide of copper aluminum oxide (CuAlO2) thin films were prepared by using sol-gel method with nitrate solutions as starting precursor. Copper nitrate and aluminum nitrate were selected as raw materials that provide the copper and aluminum source. The CuAlO2 thin films were deposited on pre-cleaned silicon substrate by spin-coating technique. To study of phase formation of CuAlO2, as prepared sample was dried and subjected to heat treatment at various temperatures. The heat-treated samples were characterized by x-ray diffraction (XRD) and energy dispersive x-ray (EDX). From XRD analysis result found that CuAlO2 phase was formed after annealing at 1100 o C for 4 hrs. EDX result of annealed sample at 1100 o C shows composition of Cu and Al that indicate the possibility of forming CuAlO2.
Tetragonal Y2O3 stabilized Zirconia (t-Y-ZrO2) powders were doped with Nb2O5 to seek a possibility if electronics doping would enhance the electronics conductivity of the insulating oxide. In this work Y2O3 was added as a stabilizer to produce tetragonal ZrO2 whereas Nb2O5 was added for the electronic doping. Several compositions of powders were prepared by thermal decomposition method and were post annealed at different temperatures. Precursor solutions were prepared from the mixture of zirconyl nitrate, yttrium nitrate and niobium tartarate as well as TEA (triethanolamine). The mixed solution were evaporated, pyrolysed and calcined to produce nanosized powders. The phase formation of the as-made powders was investigated by x-ray diffractometer. The additions of 7% Y2O3 were found to stabilize the tetragonal phase of zirconia.
The addition of Nb2O5 did not alter the stability of the tetragonal phase but it was found that the conductivity of the material has changed. The band gap as measured by the UV-Visible Spectrometer gave a value in the range of 2.97 to 5.01 eV. XRD was also used to deduce the crystallite size (by using Scherer’s equation) and transmission electron microcopy was used to view the particle sizes and shapes. The Nb doped t-Y-ZrO2 prepared in this work was to be nanosized crystal with size ranges from 7 nm to 15 nm.
Small-angle X-ray scattering (SAXS) was used to investigate the nanostructure of the microfibrils of cell wall in Acacia Mangium wood. Parameters, such as the fibre length (L), surface area of the single fibre (S), the correspondence distance from the center of the fibre to the center of its neighbor and the shape of the fibre were determined as a function to the distance from pith towards the bark. The results indicate that the fibre length ranged from 53.44 nm to 13.72 nm from pith to bark. Surface area of the single fibre varied from 0.65 nm 2 to 4.36 nm 2 , the highest being found at the end of bark region. The mean value of the correspondence distance is 13.95 nm. Surface structure analysis from scattering graph showed a rod shape of fibre in the pith region of Acacia Mangium wood. The use of SAXS technique and scanning electron microscope (SEM) micrographs gives the most reliable dimensions values.
Tin slag was collected from a slag dump in the Penang Island and was analysed for its elemental composition using microfocus XRF with a 300ȝm x-ray spot diameter. The tin slag sample was analysed direct without any sample treatment and analysis was conduct on four different spots. The result gives different elemental composition on these different spots. Among the elements analysed are Al2O3, SiO2, SnO2, CaO, TiO2, Nd2O3, MnO, Fe2O3, TaO, W2O3, As2O3, ThO2, U3O8, ZrO2 and Nb2O5. Elemental mapping was also done to show the distribution of these elements in the sample.
There are many essential and non-essential elements including metals and radionuclides present in vegetables. Howeve r, the accumulation of the several metals and radionuclides might cause the contamination to vegetables itself. Green m ustard (Brasissca rapa var. Parachinesis L.) was selected to represent the vegetable in this study. Objectives of this stud y are to determine the concentration of metals and radionuclides in the samples and to calculate the enrichment factor ( EF) and also to estimate the uptake, base on biological accumulation coefficient (BAC), for the various parts of selecte d vegetables. Three farmlands in the Cameron Highlands were studied namely Bharat, Kg Raja and Bertam area. The g reen mustard and soil samples were collected during the harvest season. Samples were dried, ground and sieved prior t o analysis. Analyses for both samples were done by using X-rays Fluorescence Spectroscopy (XRF) to measure the conc entration of Fe, Zn, Hg, U and Th. The concentration of all elements in the soils is lower than their concentration in the control soil, except for Zn, U and Th. The concentration of all elements in Green Mustard is lower than their concentrat ion in the soil where it was grown. The EF values in the Brasissca rapa var. Parachinesis L are lower than 2 except for U and Th, indicating some degree of contamination due to anthropogenic activities or naturally origin. The BAC values show that Zn and Hg were accumulated in the green mustard, depending on where the plant grows.
One of the non-destructive methods used for the identification and verification of metals is by the energy-dispersive X-ray fluorescence (EDXRF) technique. EDXRF analysis provides several important advantages such as simultaneous determination of the elements present, enable to analyse a very wide concentration range, fast analysis with no tedious sample preparation. The paper shows how this technique is developed and applied in the identification and verification of different grades of stainless steels. Comparison of the results obtained from this analysis with certified reference standards show very small differences between them.
Layered double hydroxide (LDH) with Mg/Al molar ratio of 4/1 (MAN-4) was synthesized by co-precipitation and followed by hydrothermal method. The compound was allowed to undergo ion exchange with K2HPO4 for 48 hours to produce MgAlHPO4 (MAHP-4). The solid produced was characterized using X-ray diffraction (XRD) and Fourier Transform Infrared spectroscopy (FTIR). Adsorption of copper solution by MAHP-4 was carried out using batch experiment by mixing the copper solution and the sorbent MAHP-4. The effects of
various parameters such as contact time, pH, adsorbent dosage and initial concentration were investigated. The optimum pH for copper removal was found to be 4 and the optimum time of copper removal was found at 4 hours. The isotherm data was analysed using model isotherm Langmuir with the correlation coefficient of 0.999 was recorded. The maximum adsorption capacity, Qo (mg/g) of 142.8 mg/g was also recorded from the Langmuir isotherm. The remaining copper solution was determined by using EDXRF (Energy Dispersive XRay Fluorescence spectrometry) model MiniPal 4 (PAN analytical). The results in this study indicate that MAHP-4 has potential as an effective adsorbent for removing copper from aqueous solution.
Well water is a renewable natural resources and one of the drinking water sources. The well water may constituted of dissolved essential chemicals such as K+, Ca''+ and Na+ ; and natural radionuclides such as radioisotopes from uranium-thorium decay series. The geology and mineral composition of the soil will determined the kinds and levels of chemical contents in the groundwater resources. The water flows through the geological formation and dissolved the chemicals before reaching the aquifers. To evaluate how much chemicals and natural radioactive in the water resources, a study has been carried out. Well water samples in this study were taken from 3 districts in Kelantan, which is Bachok, Machang and Kuala Krai. Similarly, in situ water quality parameters were measured using YSI portable water quality parameter include pH, salinity, dissolve oxygen(DO), conductivity, turbidity and total dissolved solids(TDS). The concentrations of K', Ca" and Na' were determined using Energy Dispersive X-ray Fluorescence (EDXRF). Five ml of filtered sample was pipette into the sample cup and, irradiated and measured for 100 seconds counting times. The type of filter used for measuring If+ and Cat{ was Al-thin and default for Nat The ranged of concentration of Kt Ce and Na+ is 23.04-251.89, 3.12-.45.41, and 3.71-125.75 ppm, respectively.
Indialite or α-cordierite was synthesized by glass crystallization method using mainly talc and kaolin and with small amount of MgO, Al2O3, SiO2 to compensate the chemical formulation of non-stoihiometric compositions of cordierite. (3MgO.1.5Al2O3.5SiO2). B2O3, P2O5 and CaO was also added to decrease the melting and sintering temperature of cordierite. The glasses were pelletized and sintered from 850 o C up to 1050 o C. Phase compositions of both heat treated glass was quantified by X-ray powder diffraction data by the Rietveld method using TOPAS Ver 3 software. Result shows that about 60wt% of α cordierite has successfully crystallized at 850 o C. Beside secondary phases (forsterite) which come from initial raw materials, phases from grinding media were also presents in the sample. The contamination was considered high since it has reacted with existence phases to form a new phase at higher temperature. Without any contamination from grinding it was expected to obtain more than 90wt% α cordierite using the same composition.
The linear and the mass attenuation coefficients of Rhizophora spp. wood in the photon energy range of 11.22 - 28.43 keV were determined. This was done by studying the attenuation of x-ray fluorescent (XRF) photons from selenium, molybdenum, silver and tin targets. Both the Kα and Kβ peaks were utilised. The results were compared with theoretical values for average breast tissues for youngage, middle-age and old-age groups calculated by using a XCOM computer programme. The mass attenuation coefficient of Rhizophora spp. was found to be close to that of the calculated young-age breast in this photon energy range.