• Analytical Science and Technology
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• v.15 no.1
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• pp.87-90
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• 2002

The content of $SiHCl_3$ as a trace impurity in $SiCl_4$ was analyzed by Near IR spectrophotometer with optical fiber. The strong absorption bands of $5345{\sim}5116cm^{-1}$ and $4848{\sim}4349cm^{-1}$ were used for analysis of $SiHCl_3$, and the detection limit of impurity $SiCl_3$ was appeared to be 0.005 ％ in the spectrum. The quantitative analysis by Near IR spectrophotometry showed the analytical possibility of trace impurity in $SiCl_4$ without sample pre-treatment not only in the laboratory but also in the field.

• Analytical Science and Technology
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• v.17 no.4
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• pp.308-314
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• 2004

When the polymer was used for the guard raw materials of electronic device, the content of U, Th and their daughter nuclides were known as a factor of soft error. Because emitted alpha ray could be caused of mis-operation. And ionic impurities such as Cl, Fe, Na could shorten the device life-time. For the analysis of trace impurities in the polymer, neutron activation analysis(NAA) and ICP/AES have been studied. To improve the accuracy and sensitivity of the trace and ultratrace metallic impurities in the epoxy and phenol polymer, sample pretreatment method and optimum analytical condition of NAA were developed. Using the above method, U, Th and other 23 trace impurity elements were analyzed.

• Mass Spectrometry Letters
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• v.1 no.1
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• pp.17-20
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• 2010

As background significantly affects measurement accuracy and a detection limit in determination of the trace amounts of uranium, it is necessary to minimize the impurities in the filaments used for thermal ionization mass spectrometry (TIMS). We have varied the degassing condition such as the heating currents and duration times to reduce the backgrounds from the filaments prepared with zone-refined rhenium tape. The most efficient degassing condition of the heating current and the duration time was determined as 3.5 A and 60 min, respectively. The TIMS measurement combined with the isotope dilution mass spectrometry (IDMS) technique showed that the uranium backgrounds were determined to be in a few fg level from blank rhenium filaments. The background minimized filaments were utilized to measure the uranium isotope ratios of a U030 (NIST) standard sample. The excellent agreement of the measurement with the certified isotope ratios showed that the degassing procedure optimized in this study efficiently reduced the impurity signals of uranium from blank rhenium filaments to a negligible level.

• Analytical Science and Technology
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• v.32 no.6
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• pp.233-242
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• 2019

Substance identification is the first step of the REACH registration. It is essential in terms of Classification, Labelling and Packaging (CLP) regulation and because even trace amounts of impurities or additives can affect the classification. In this study, a scheme for the screening, quantification, and interpretation of trace amounts of hazardous inorganic substances is proposed to detect the presence of more than 0.1% hazardous inorganic substances that have been affecting the hazard classification. An exemplary list of hazardous inorganic substances was created from the substances of very high concern (SVHCs) in REACH. Among 201 SVHCs, there were 67 inorganic SVHCs containing at least one or ~2-3 heavy metals, such as As, Cd, Co, Cr, Pb, Sb, and Sn, in their molecular formula. The inorganic SVHCs are listed in excel format with a search function for these heavy metals so that the hazardous inorganic substances, including each heavy metal and the calculated ratio of its atomic weight to molecular weight of the hazardous inorganic substance containing it, can be searched. The case study was conducted to confirm the validity of the established scheme with zinc oxide (ZnO). In a substance that is made of ZnO, Pb was screened by XRF analysis and measured to be 0.04% (w/w) by ICP-OES analysis. After referring to the list, the presence of Pb was interpreted just as an impurity, but not as an impurity relevant for the classification. Future studies are needed to expand on this exemplary list of hazardous inorganic substances using proper regulatory data sources.

• Nuclear Engineering and Technology
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• v.24 no.2
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• pp.163-167
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• 1992

Nondestructive neutron activation analysis of copper in high purity Aluminum samples which can be used as a parameter of impurity is investigated and determined. Other 23 trace impurity elements in the samples are also determined. In the analysis of copper, the new irradiation method using thermal column was applied to reduce the interfering activity of 24Na produced by 27Al(n,$\alpha$)24Na reaction induced by fast neutron. As a result, the interference can be reduced to 100 times more than other activation methods. Also the influence by activity of 24Na is found in the range of 2~3 %. It has been observed that the copper contents in so-ratted“six nine”class standard aluminum samples are about 0.54 $\pm$ 0.08 ppm. By the comparison with other values re-ported, our results are reasonable and can be available as a improved routine analysis.

• Analytical Science and Technology
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• v.33 no.2
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• pp.98-107
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• 2020

Methamphetamine (MA) is currently the most abused illicit drug in Korea. MA is produced by chemical synthesis, and the final target drug that is produced contains small amounts of the precursor chemicals, intermediates, and by-products. To identify and quantify these trace compounds in MA seizures, a practical and feasible approach for conducting chromatographic fingerprinting with a suite of traditional chemometric methods and recently introduced machine learning approaches was examined. This was achieved using gas chromatography (GC) coupled with a flame ionization detector (FID) and mass spectrometry (MS). Following appropriate examination of all the peaks in 71 samples, 166 impurities were selected as the characteristic components. Unsupervised (principal component analysis (PCA), hierarchical cluster analysis (HCA), and K-means clustering) and supervised (partial least squares-discriminant analysis (PLS-DA), orthogonal partial least squares-discriminant analysis (OPLS-DA), support vector machines (SVM), and deep neural network (DNN) with Keras) chemometric techniques were employed for classifying the 71 MA seizures. The results of the PCA, HCA, K-means clustering, PLS-DA, OPLS-DA, SVM, and DNN methods for quality evaluation were in good agreement. However, the tested MA seizures possessed distinct features, such as chirality, cutting agents, and boiling points. The study indicated that the established qualitative and semi-quantitative methods will be practical and useful analytical tools for characterizing trace compounds in illicit MA seizures. Moreover, they will provide a statistical basis for identifying the synthesis route, sources of supply, trafficking routes, and connections between seizures, which will support drug law enforcement agencies in their effort to eliminate organized MA crime.

• Analytical Science and Technology
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• v.30 no.5
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• pp.240-251
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• 2017

1,1,1,2-Tetrafluoroethane (HFC-134a), which is used as refrigerant in air conditioners, has been recently regulated as a greenhouse gas and is recommended for reuse by refining. It is very important to quantitatively analyze trace impurities present in the refrigerant to evaluate the criteria for reuse. In this study, trace impurities including C, H, Cl, and F, which are difficult to quantify because there are no reference materials, were quantitatively analyzed by a gas chromatograph-atomic emission detector (GC/AED); for this analysis, this was preceded by a qualitative analysis with a GC-mass selective detector (GC/MSD). In addition, the AED response was investigated using a hydrocarbon mixed reference material, which was proportional to the number of atoms in the component. Fifteen refrigerant components were detected as trace impurities in HFC-134a by qualitative analysis of trace impurities including C, H, Cl, and F in the samples. Based on the results of the qualitative analysis, quantitative analysis of trace impurities using AED showed that the highest mole fractions were for the $CHClF_2$ component ($45438.38{\mu}mol/mol$) in one sample and for the $C_2H_2ClF_3$ component ($1311.47{\mu}mol/mol$) in another sample. From this study, it has been shown that it is possible for this analytical method to be applied to the qualitative and quantitative analysis of trace compounds in refrigerants, which are difficult to quantify because of the absence of reference materials.

• Journal of the Korean Vacuum Society
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• v.14 no.1
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• pp.17-23
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• 2005

Glow discharge mass spectrometry(GDMS) was used to determine the impurity concentrations of the deposited Cu films and the 6N Cu target. Cu films were deposited on Si (100) substrates at zero substrate bias voltage and a substrate bias voltage of -50 V using a non-mass separated ion beam deposition method. Since do GDMS has a little difficulty to apply to thin films because of the accompanying non-conducting substrate, we have used an aluminum foil to cover the edge of the Cu film in order to make an electrical contact of the Cu film deposited on the non-conducting substrate. As a result, the Cu film deposited at the substrate bias voltage of -50 V showed lower impurity contents than the Cu film deposited without the substrate bias voltage although both the Cu films were contaminated during the deposition. It was found that the concentration change of each impurity in the Cu films by applying the negative substrate bias voltage is related to the difference in their ionization potentials. The purification effect by applying the negative substrate bias voltage might result from the following reasons: 1) Penning ionization and an ionization mechanism proposed in the present study, 2) difference in the kinetic energy of accelerated Cu+ ions toward the substrate with/without the negative substrate bias voltage.

• Korean Journal of Materials Research
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• v.26 no.6
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• pp.306-310
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• 2016

To produce 4N grade high-purity silica powder from natural ore, the mineralogical characteristics of natural silica ore were investigated and their effects on the purification process were revealed. The Chinese silica mineral ore used was composed of iron and aluminum as main impurities and calcium, magnesium, potassium, sodium, and titanium as trace impurities; these trace impurities generally exist as either single oxides or complex oxides. It was confirmed that liberation and acidic washing of the impurities were highly dependent on the particle size of the ground silica ore and on its mineralogical characteristics such as the distribution and phases of existing impurities. It is suggested that appropriate size reduction of silica ore should be realized for optimized purification according to the origin of the natural silica ore. A single step purification process, the mechano-chemical washing (MCW) process, was proposed and verified in comparison with the conventional multi step washing process.

• Mass Spectrometry Letters
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• v.7 no.2
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• pp.31-40
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• 2016

The analysis of nuclear materials and environmental samples is an important issue in nuclear safeguards and nuclear forensics. An analysis technique for safeguard samples has been developed for the detection of undeclared nuclear activities and verification of declared nuclear activities, while nuclear forensics has been developed to trace the origins and intended use of illicitly trafficked nuclear or radioactive materials. In these two analytical techniques, mass spectrometry has played an important role in determining the isotope ratio of various nuclides, contents of trace elements, and production dates. These two techniques typically use similar analytical instruments, but the analytical procedure and the interpretation of analytical results differ depending on the analytical purpose. The isotopic ratio of the samples is considered the most important result in an environmental sample analysis, while age dating and impurity analysis may also be important for nuclear forensics. In this review, important aspects of these techniques are compared and the role of mass spectrometry, along with recent progress in related technologies, are discussed.