• Analytical Science and Technology
• /
• v.14 no.4
• /
• pp.317-323
• /
• 2001

Dissolution procedures of Monsanto catalyst which has been used to produce acrylronitrile by ammoxidation of propylene have been studied. Optimum dissolution condition of the catalyst supported on silica was obtained by microwave digestion system with mixed of HCl, HF and $H_2O_2$. When a safety device was activated by increased pressure in microwave vessel, Bi, Fe, Mo, Sb and U were not volatilized even though silica was volatilized as $SiF_4$. Quantification results by this method were $SiO_2$ $50.5{\pm}0.4%$, $Sb_2O_3$ $29.6{\pm}0.6%$, $UO_2$ $10.2{\pm}0.1%$, $Fe_2O_3$ $6.1{\pm}0.1%$, $MoO_3$ $0.73{\pm}0.01%$ and $Bi_2O_3$ $0.49{\pm}0.01%$ by ICP-AES and the relative error was within ${\pm}10%$ except bismuth.

• Analytical Science and Technology
• /
• v.10 no.4
• /
• pp.240-245
• /
• 1997

An accurate analysis method for the determination of lead in whole blood by ICP/MS was developed. Whole blood samples were decomposed in microwave digestion system without any contamination and loss of lead. The 96 samples were analyzed by ICP/MS using mass$^{208}$ isotope of lead. Lead concentrations of human whole blood were ranged of $2.50{\sim}22.8{\mu}g/dL$. The accuracy of this analysis method was verified by analyzing of NIST SRM 955a series(lead in blood).

• Mass Spectrometry Letters
• /
• v.11 no.4
• /
• pp.108-112
• /
• 2020

A certified reference material (CRM) for the analysis of nutrient elements in an edible mushroom (Ganoderma lyceum) powder has been developed (KRISS CRM 108-10-011). The mass fractions of calcium (Ca), iron (Fe), and zinc (Zn) were measured by isotope dilution inductively coupled plasma mass spectrometry (ID ICP/MS). To dissolve the fungi cell wall of mushroom consisted of chitin fibers, sample preparation method by single reaction chamber type microwave-assisted acid digestion with acid mixtures was optimized. The mean measurement results obtained from 12 sample bottles were used to assign as the certified values for the CRM and the between-bottle homogeneities were evaluated from the relative standard deviations. The certified values were metrologically traceable to the definition of the kilogram in the International System of Units (SI). This CRM is expected to be used for validation of analytical methods or quality control of measurement results in analytical laboratories when they determine the mass fractions of elements in mushroom or other similar samples.

• Analytical Science and Technology
• /
• v.9 no.2
• /
• pp.145-160
• /
• 1996

Inorganic analytical laboratory of Korea Research Institute of Standards and Science participated in an interlaboratory comparison program operated by Quebec Toxicology Centre of Canada in 1994 and again in 1995. The objective of this program is to enable participating laboratories to assess reproducibility and accuracy of their analytical results for trace toxic elements in human biological fluids. This laboratory determined Cd and Pb concentrations in 3 levels of human blood samples by isotope dilution inductively coupled plasma mass spectrometry. 0.5mL of blood sample is added to the digestion bomb together with 2mL of nitric acid and enriched spike isotopes and then decomposed in the microwave digestion system. The decomposed sample is diluted to 10mL and nebulized into ICP-MS. The Cd and Pb values reported by all participating laboratories are presented and compared. The values reported by this laboratory are within the acceptable range of target values.

• Analytical Science and Technology
• /
• v.12 no.4
• /
• pp.273-278
• /
• 1999

Simultaneous determination of mercury and arsenic has been studied by reductive vapor generation-ICP-AES. Samples were digested with a microwave digestion system and extracted with acids. Reductive vapor generation was carried out with 6N HCI and 2% $NaBH_4$. Detection limit of Hg and As are found to be 0.06 ppb and 0.08 ppb, respectively. Measured values of Hg and As in inorganic samples agree well with reference value of SRMs, but the recovery of As from organic samples is obtained approximately 80% of the reference values.

• Environmental Analysis Health and Toxicology
• /
• v.18 no.2
• /
• pp.101-109
• /
• 2003

Humans are exposed to toxic element arsenic (As) from air, food and water The current study was performed to investigate the levels of arsenic in the internal organs (liver, kidney cortex, lung, cerebrum. abdominal muscle and abdominal skin) and to find out correlation with age and interrelationship between tissues in Korean human bodies who had lived in Seoul or Gyeonggi Province and Honam district. The tissues from 43 Korean cadavers were digested with microwave digestion system and arsenic was determined by inductively coupled plasma mass spectrometer (ICP-MS). The mean recovery percentages of arsenic In liver were about 80％ and artenic concentrations in human tissues were almost uniform. The mean level of arsenic in internal tissues were at follow ; liver 44.556${\pm}$25.199 ppb, kidney cortex 42.652${\pm}$22.082 pub, lung 31.020 ${\pm}$ 17.504 ppb. cerebrum 35.703 ${\pm}$22.191 ppb, muscle 43.413${\pm}$26.619 ppb and skin 42.106${\pm}$25.8,11 ppb. No significant difference was found in the levels of arsenic between sexes. Meanwhile significant differences between districts where they had lived were found in all tissues tested. The levels of arsenic in the tissues of cadavers who had lived in Seoul Gyeonggi Province were higher than those of Honam district. In addition a positive correlation between As concentration and age was observed only in the cerebrum (p < 0.05). A significantly high correlations between tissues were observed in all tissues tested. This result also shows that the distribution of arsenic is uniform in internal tissues.

• Mass Spectrometry Letters
• /
• v.3 no.2
• /
• pp.58-61
• /
• 2012

A method based on flow injection-isotope dilution-cold vapor-inductively coupled plasma mass spectrometry (FI-IDCV-ICP/MS) has been applied to determine trace level of mercury in fly ash. $^{200}Hg$ isotopic spike was added to 0.25 g of BCR176R fly ash and then decomposed by microwave digestion procedure with acid mixture A (8 mL $HNO_3$ + 2 mL HCl + 2 mL HF) and acid mixture B (8 mL $HNO_3$ + 2 mL $HClO_4$ + 2 mL HF) for applying IDMS. Mercury cold vapor was generated by using reductant solution of 0.2% (w/w) $NaBH_4$ and 0.05% (w/w) NaOH. The measurements of n($^{200}Hg$)/n($^{202}Hg$) isotope ratio was made using a quadrupole ICP/MS system. The accuracy in this method was verified by the analysis of certified reference material (CRM) of fly ash (BCR 176R). The indicative value of Hg in BCR 176R fly ash was $1.60{\pm}0.23$ mg/kg (k = 2). The determined values of Hg in BCR 176R fly ash by the method of FI-CV-ID-ICP/MS described in this paper were $1.60{\pm}0.24$ mg/kg (k = 3.18) and the analysis results were in well agreement with the indicative value within the range of uncertainty.

• Environmental Analysis Health and Toxicology
• /
• v.19 no.4
• /
• pp.383-388
• /
• 2004

In order to elucidate the relationships between cadmium, copper, mercury, zinc levels and metallothionein in the liver and kidney cortex of Korean, the levels of Cd, Zn, Hg, Cu and metallothionein (MT) were determined in the kidney cortex and liver of 50 subjects deceased in the period of January-November, 2001 in the area of Seoul and Gyeonggi Province of Korea. The mean age of the population studied was 36.3+/-12.3 years. The tissues were digested with microwave digestion system and the elements were determined by inductively coupled plasma atomic emission spectrometry. MT was determined by the Cd-hemoglobin affinity assay. The determined levels (mean+/-SD) were: 33.9+/-18.9 micrograms Cd/g wet weight; 47.5+/-12.6 micrograms Zn/g wet weight; 2.5+/-0.57 microgram Cu/g wet weight; 0.26+/-0.31 micrograms Hg/g wet weight, 4.0+/-3.1 mg MT/g wet weight in renal cortex and 2.5+/-1.9 micrograms Cd/g wet weight; 46.9+/-15.0 micrograms Zn/g wet weight; 6.2+/-2.5 micrograms Cu/g wet weight; 0.10+/-0.15 micrograms Hg/g wet weight, 0.92+/-0.57 mg MT/g wet weight in the liver. Positive relationships between Cd and MT, sum of four divalent metal and MT in the kidney cortex were observed. No other correlation was found between Cu and MT, Hg and MT, Zn and MT in either organs.

• Resources Recycling
• /
• v.32 no.6
• /
• pp.3-9
• /
• 2023

Separation of LED packages from PCBs and analysis of the adhesive components was conducted to enhance the recycling potential of LED modules. LED package was separated from PCBs using heat treatment under optimal conditions: temperature of above 250 ℃ and time of 20 minutes. The separation equipment can be established using a hot air injector with controlling the rotational speed of the internal screw. The separation efficiency of each type of substrate (aluminum and glass fiber) was investigated with the thickness range of the adhesive materials (0.25-0.30 and 0.30-0.35 mm). Under the optimal conditions, the efficiency can reach to 97.5% for both types of substrates with adhesive materials of thickness 0.25~0.30mm. Characterization of the residual adhesive substances from the separated LED package and PCB using microwave digestion and ICP analysis showed that the residue contained of 95% of Sn, less than 5% of Cu and Ag.

• Journal of Soil and Groundwater Environment
• /
• v.11 no.1
• /
• pp.54-64
• /
• 2006

Chromated copper arsenate (CCA), a wood preservative, has been widely used to protect wood products from attacks by bacteria, fungi and insects. However, the use of CCA is currently forbidden or limited to some applications in many countries because the toxic elements (Cr, Cu, and As) of CCA are released into the environments during outdoor uses, which may cause adverse health effects on humans and ecological systems. This study was conducted to investigate the distributions of chromium, copper and arsenic in soils adjacent to two CCA-treated wood structures. In a 7 month old pond entry structure, ten surface soil samples (0-2.5 cm) were collected at lateral distances of 0, 0.5, and 1 m from the stairway, and nine surface soil samples were collected beneath the deck. Nine top soil samples were taken from a 2 year old sound barrier structure at lateral distances of 0, 1, and 2 m. Background surface soil samples were also collected from each structure. Samples were analyzed for some physicochemical properties such as pH, electrical conductivity, organic matter content, and soil texture. Following the extraction of the elements with a microwave digestion system, samples were analyzed for Cr, Cu, and As. The concentrations of the three elements in soils adjacent to the structures were significantly elevated compared to the background levels, indicating that the elements have been leached out of the structures. Released e1ements showed lateral concentration gradients within 1 m. The elevations of the three elements in soils underneath the deck did not seem different (background-corrected concentrations: Cr, 5.01 mg/kg; Cu, 5.50 mg/kg; As, 4.91 mg/kg), while the elements in soils near the sound barrier were elevated in the order of As>Cu>Cr with measured concentrations of 49.7, 44.7 and 52.5 mg/kg, respectively. Background As, Cu, and Cr concentrations near the sound barrier were 9.88, 30.8, and 46.5 mg/kg, respectively. These results showed that CCA constituents are released into the environment and it is suggested that risk assessment need to be conducted to investigate harmful effects of the released elements on humans and ecological systems.