• Title/Summary/Keyword: GF-AAs

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Studies on Solvent Extraction and Flotation Technique Using Metal-Dithizone Complexes(II). Determination of Trace Elements in Water Samples by Solvent Sublation

  • 김영상;최윤석;최희선
    • Bulletin of the Korean Chemical Society
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    • v.19 no.10
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    • pp.1036-1042
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    • 1998
  • The preconcentration and determination of trace elements in water samples were studied by a solvent sublation utilizing dithizonate complexation. After metal dithizonates were formed, trace amounts of cadmium, cobalt, copper and lead were floated and extracted into small volume of a water-immiscible organic solvent on the surface of sample solution and determined in the solvent directly by GF-AAS. Several experimental conditions as formation condition of metal-dithizonate complexes, pH of solution, amount of dithizone, stirring time, the type and amount of surfactants, N2 bubbling rate and so on were optimized for the complete formation and effective flotation of the complexes. And also four kinds of light solvents were compared each other to extract the floated complexes, effectively. After the pH was adjusted to 4.0 with 5 M HNO3, 8.0 mL of 0.05% acetone solution of dithizone was added to 1.00 L water sample. The dithizonate complexes were flotated and extracted into the upper methyl isobutylketone (MIBK) layer by the addition of 2.0 mL 0.2% ethanolic sodium lauryl sulfate solution and with the aid of small nitrogen gas bubbles. And this solvent sublation method was applied to the analysis of real water samples and good results of more than 85% recoveries were obtained in spiked samples.

Relationship between Heavy Metal Concentrations in the Soil with the Blood and Urine of Residents around Abandoned Metal Mines (폐금속 광산지역 토양 중 중금속 농도와 주민의 혈액 및 요중 중금속 농도와의 관련성)

  • Jang, Bong-Ki;Park, Sang-Il;Kim, Nam-Soo;Jung, Kyung-Sick;Lee, Byung-Kook;Lee, Jong-Wha
    • Journal of Environmental Health Sciences
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    • v.37 no.5
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    • pp.348-357
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    • 2011
  • Objectives: This study was conducted in order to examine the relationship between heavy metal concentrations in the soil and the level of heavy metals in the blood or urine of 216 local residents living near abandoned metal mines. Methods: Residents around abandoned metal mines were interviewed about their dietary habits, including seafood consumption, medical history, cigarette smoking, and drug history. Metal concentrations in the soil were determined by atomic absorption spectrophotometer (AA-7000, Shimadzu, Japan). Lead (Pb) and cadmium (Cd) contents in the blood or urine were analyzed by GF-AAS (AA-6800, Shimadzu). Mercury (Hg) contents in the blood were determined by means of a mercury analyzer (SP-3DS, NIC). Arsenic (As) content in the soil and urine were measured by a HG-AAS (hydride vapor generation-atomic absorption spectrophotometer). Results: The heavy metal concentrations in the soil showed a log normal distribution and the geometric means of the four villages were 8.61 mg/kg for Pb, 0.19 mg/kg for Cd, 1.81 mg/kg for As and 0.035 mg/kg for Hg. The heavy metal levels of the 216 local residents showed a regular distribution for Pb, Cd, Hg in the blood and As in the urine. The arithmetic means were 3.37 ${\mu}g$/dl for Pb, 3.07 ${\mu}g$/l for Cd and 2.32 ${\mu}g$/l for Hg, 10.41 ${\mu}g$/l for As, respectively. Conclusions: As a result of multi-variate analysis for the affecting factors on the bodily heavy metal concentrations, gender and concentration in the soil (each, p<0.01) for blood lead levels; gender and smoking status (each, p<0.01) for blood cadmium levels; gender (p<0.01) for urine arsenic levels; gender, age and concentration in the soil (p<0.01) for blood mercury levels were shown to be the affecting factors.

Development and Validation of the Simultaneous Analytical Method of Urinary Metals and Metalloids for the National Biomonitoring Programs (국가 바이오모니터링 프로그램을 위한 소변 중 금속류 동시분석법 개발 및 검증)

  • Cho, Yong Min;Yang, Minho;Im, Hosub;Cha, Sangwon;Lee, Jaeick;Kim, Ki Hun;Han, Sang Beom
    • Journal of Environmental Health Sciences
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    • v.45 no.6
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    • pp.594-604
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    • 2019
  • Objectives: This study developed and validated an analysis method of urinary metals and metalloids that can be applied inductively with coupled plasma mass spectrometry (ICP-MS). Methods: 0.3 mL of urine was used to analyze 25 metal and metalloid compounds using ICP-MS. The validation of the analytical method included linearity, accuracy, precision, and the calculation of detection limits. In addition, a comparison test was performed with the graphite furnace atomic absorption spectrometry (GF-AAS) method, which is the current standard method, with urine samples of 66 healthy subjects. Results: The linearities (R2) of calibration curves of all 25 compounds were ≥ 0.999. Of the 25 compounds, the intra-day and inter-day accuracy% of 17 and 20 met ≤15%, respectively. In addition, fifteen compounds showed ≤15% recovery% for certificated reference materials. Intraclass correlation coefficients of the comparison between the current methods and new methods in this study were 0.952 (p-value<0.001) and 0.911 (p-value<0.001) for urinary cadmium and mercury, respectively. Conclusion: This study proposes an efficient simultaneous methodology that can analyze multi elements in smaller sample amounts. More reproduction experiments are needed in the future.

A Study on the Lifestyle of Korean Medical Students : Drinking Patterns and Eating Attitudes (한의대생의 생활양식 연구 - 음주양태와 섭식태도를 중심으로)

  • Go, Ho-Yeon;Lee, Jae-Hyok
    • Journal of Society of Preventive Korean Medicine
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    • v.22 no.3
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    • pp.21-29
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    • 2018
  • Objectives : The purpose of this study was to examine the lifestyle of korean medicine students based on their drinking patterns and eating attitudes. Methods : The survey was conducted on 101 korean medicine students to investigate their psychological characteristics. They were asked to complete Self-Administered Alcoholism Screening Test, Eating Attitude Test, and Minnesota Multiphasic Personality Inventory-2. Results : A total of 101 Korean medical students participated in the study. Non-drinker 19, drinker were 82. Unlikely to, possible and potential alcoholism 79(78.2%), 17(16.8%) and 5(5%) respectively. The mean and standard deviation of SAAST in the subjects were $3.88{\pm}3.33$ and the EAT score was $8.09{\pm}8.693$. There was a significant difference in the MMPI-2 items between non-drinker and drinker. The SAAST had an effect on the EAT score(${\beta}=0.319$). Conclusions : As a result of MMPI-2 test, in the potential alcoholism group, scale D, Mf, Si, INTR, TPA, SOD, Mt and GF were shown higher, and AAS and GM were shown lower than the normal group. In the bad eating attitude group, scale Hy, RC4, DISC and AA were shown higher than the good eating attitude group.

The Monitoring of Heavy Metals in Human Bloods of Middle School Students (중학생의 혈액 중 중금속 모니터링)

  • Park Hee Ra;Kim Meehye;Kwun Ki-Sung;Kim Soon Ki;Heo Su-Jeong;Kim Kwang_Jin;Yum Tae-Kyung;Choi Kwang Sik;Kim Soo Yeon
    • Journal of Food Hygiene and Safety
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    • v.20 no.2
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    • pp.83-88
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    • 2005
  • This study was conducted to estimate the contents of heavy metals including lead, cadmium, zinc, copper as well as iron status(serum iron, total iron binding capacity, feritin etc)in blood samples of middle school students(n=300). The contents of heavy metals were determined using the GF-AAS (Graphite furnace Atomic Absorption Spectrophotometer). The microwave digestion method and dilution method were compared. The dilution method showed the better recovery and detection limit than microwave digestion method. The values of toxic metals in whloe blood of boys & girls were 3.46 & 3.05 for Pb,0.063 & 0.065 for Cd respectively (ug/dL). Also the values of trace metals in serum of boys & girls were 105.9 & 92.6 for Zn, 98.3 & 99.0 for Cu respectively (ug/dL). The prevalence of iron deficiency was $7.5\%$ in 146 boys and $14.3\%$ in 156 girls. The mean values of lead in girls were higher in iron deficiency, iron deficiency anemia and anemia groups than normal group. The mean values of lead and zinc were higher in boys compared to those in girls(P<0.05), the mean values of cadmium and copper in boys were similar to those in girls. Our results of toxic metals such as Pb & Cd showed lower to CDC's(Centers for Disease Control) blood lead levels of concern for children, 10 ug/dL.

Microwave Digestion and Solid-Phase Extraction for Determination of Aluminum in Human Urine by Graphite Furnace Atomic Absorption Spectrometer (흑연로 원자흡수 분광법에 의한 사람 오줌 중 알루미늄의 정량을 위한 마이크로파 삭힘과 고체상 추출)

  • Kim, Young-Sang;Choi, Yoon-Seok
    • Analytical Science and Technology
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    • v.16 no.2
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    • pp.102-109
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    • 2003
  • Microwave digestion and solid-state extraction were studied for determination of trace aluminum{Al(III)} in human urine samples. A mixed acid of nitric acid and hydrogen peroxide was added to urine samples, organic materials were destructed in a home microwave oven and dried in a drying oven. The dried residues were dissolved in a sulfuric acid solution. The solution was eluted through a XAD-4 resin column adsorbed with 8-hydroxyquinoline(Oxine, HQ). Al(III)-8-hydroxyquinolinate complex was formed in the column and eluted with 0.5 M nitric acid solution. The Al(III) eluted was determined by graphite atomic absorption spectrophotometry. Various experimental conditions of followings were investigated for the optimization : the type of acid to dissolve the residues, the amount of HQ adsorbed on the resin, the pH of sample solutions, the type and concentration of acid to elute the complex from column and so on. The contents of Al(III) in real samples were determinated by a calibration curve method. The recovery in standard spiked samples was 94~101% and the detection limit of this procedure was 0.05 ng/mL.

Development and Verification of a Simultaneous Analytical Method for Whole Blood Metals and Metalloids for Biomonitoring Programs (바이오모니터링 프로그램을 위한 혈중 금속류 동시분석법 개발 및 확인 평가)

  • Cha, Sangwon;Oh, Eunha;Oh, Selim;Han, Sang Beom;Im, Hosub
    • Journal of Environmental Health Sciences
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    • v.47 no.1
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    • pp.64-77
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    • 2021
  • Objective: Biological monitoring of trace elements in human blood samples has become an important indicator of the health environment. The purpose of this study was to detect and evaluate multiple metal items in blood samples based on ICP-MS, to perform comparative evaluation with the existing analysis method, and to develop and verify a new method. Methods: 100 μL of whole blood from 80 healthy subjects was used to analyze ten metals (Sb, tAs, Cd, Pb, Mn, Hg, Mo, Ni, Se, Tl) using ICP-MS. Verification of the analysis method included calculation of linearity, accuracy, precision and detection limits. In addition, a comparative test with the conventional graphite furnace atomic absorption spectroscopy (GF-AAS) method was performed. In the case of Pb, Cd, and Hg in whole blood, cross-analysis between Pb, Cd, and Hg analysis methods was performed to confirm the difference between the existing method and the new method (ICP-MS). Results: The coefficient of determination (R2) was 0.999 or higher in seven items and 0.995 or higher in three items. The Pb result showed that Pearson's correlation coefficient was very high at 0.983, and the intraclass correlation coefficient was 0.966. The Cd result showed that Pearson's correlation coefficient was 0.917 between the existing method and the new analysis concentration value. Its intraclass correlation coefficient was 0.960, and there was no significant difference between the two groups. Hg had a low correlation at 0.687, and the intraclass correlation coefficient was 0.761, which was lower than that of Pb and Cd. The intra-day and inter-day accuracy of Pd and Cd were satisfactory, but Hg did not meet the criteria for both accuracy and precision when compared with the conventional analysis method. Conclusion: This study can be meaningful in that it proposes a more efficient and feasible analysis method by verifying a blood heavy metal concentration experiment using multiple simultaneous analyses. All samples were processed and analyzed using the new ICP-MS. It was confirmed that the agreement between the two methods was very high, with the agreement between the current and new methods being 0.769 to 0.998. This study proposes an efficient simultaneous methodology capable of analyzing multiple elements with small samples. In the future, studies of various applications and the reliability of ICP-MS analysis methods are required, and research on the verification of accurate, precise, and continuous analysis methods is required.

Establishments of Lead Standards through Monitoring Heavy Metals in Calcium, Chitosan, and Propolis Health Foods (칼슘, 키토산, 프로폴리스 건강보조식품중 중금속 모니터링을 통한 납기준 제정)

  • Kim, Mee-Hye;Chung, So-Young;Sho, You-Sub;Kim, Myung-Chul;Kim, Chang-Min
    • Korean Journal of Food Science and Technology
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    • v.33 no.5
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    • pp.525-528
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    • 2001
  • This study was conducted to estimate the contents of heavy metals in some health foods available on Korean markets. The samples were digested with microwave system, then analyzed using GF-AAS for the contents of lead (Pb), cadmium (Cd) and arsenic (As). The contents of mercury (Hg) were determined using a mercury analyzer. The average values of Hg, Pb, Cd and As in calcium (Ca) health foods were 0.007, 1.08, 0.02 and 0.48 mg/kg respectively. Those values in chitosan health foods were 0.001, 0.36, 0.01 and 0.03 mg/kg respectively. Those values in propolis health foods were 0.013, 4.96, 0.01 and 0.13 mg/kg, respectively. The health foods that contained cow bone powders had the highest lead contents. Based on the variation in lead contents of those products, it could be possible that they might be contaminated through raw materials and/or manufacuring process. Some propolis products were also very high in lead contents. There could be risks for some population, especially the aged who overtake those health foods, to have heavy intake of lead. Therefore, we established the lead standards of 3.0, 2.0 and 5.0mg/kg less than for Ca, chitosan and propolis health foods respectively, based on the Codex method.

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Effect of Cadmium-contaminated Brown Rice Diet on Accumulation of Heavy Metal in Rats (카드뮴 오염 현미 섭취에 의한 랫드의 체내 중금속 축적)

  • Kim, Jae-Young;Im, Hyo-Bin;Kim, Seong-Jo;Baek, Seung-Hwa
    • Journal of Food Hygiene and Safety
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    • v.27 no.2
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    • pp.133-140
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    • 2012
  • Movement and accumulation of cadmium in male Sprague-Dawley rats, fed with brown rice from nearby Janghang smeltery area were investigated. The rat fed with five different cadmium level diets made with Cd-polluted during 12 weeks. The brown rice-polluted with 0.87 ppm Cd (PBR) was sampled from products in the Janghang smeltery area. Diets of brown rice group were brown rice (BR, 0.002 ppm Cd), each 50% of BR and PBR (BR+PBR 50%, 0.44 ppm Cd) and PBR (PBR 100%, 0.87 ppm Cd). To compare with BR+PBR 50%, the another group diet composed the feed (FE, 0.002 Cd ppm) and each 50% of FE and PBR (FE+PBR 50%, 0.44 ppm Cd). Accumulation of Cd, Zn and Cu in blood, liver and kidney rats was measured by GF-AAS. The weight gain in BR groups and FE groups were different 0.22-0.26 and 1.08-1.26 g/day, respectively. Daily intake cadmium was 10.77 and 22.36 ${\mu}g/rat$ in BR+PBR 50% and PBR 100%, and 8.83 ${\mu}g/rat$ in FE+PBR 50%. Cadmium contents in diets were higher, and total intake of the heavy metals was more increased on the whole. Weights of liver and kidney in FE+PBR 50% group was 2.64 and 2.27 folds higher than those in BR+PBR 50% group. Cadmium contents in blood were increased with intake of BR diet, but Zn and Cu were decreased with them. In the diet groups with the same Cd concentration, Cd content of FE+PBR 50% was higher 1.27 times than that of BR+PBR 50%. In the diet group of BR, BR+PBR 50%, and PBR 100%, the increase of Cd concentration was significantly different to the increase of Cd content in the livers. In the same condition of Cd concentration, Cd contents were higher in the BR+PBR 50% group. In the diet groups of BR, BR+PBR 50%, and PBR 100%, the increase of Cd content in the kidneys led to the increase of Zn and Cu contents. In the same condition of Cd concentration, the diet group with the addition of BR was shown to be 3.11 times higher than with the addition of FE. In view of the results so far achieved, It was closely related with Cd, Zn, and Cu content.