• Title/Summary/Keyword: graphite furnace atomic absorption spectrometry

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A Comparative Analysis of Whole Blood Cadmium by Atomic Absorption Spectrophotometry with a Graphite Furnace (흑연로 원자흡수분광법에 의한 혈액중 카드뮴 정량분석)

  • Park, Jong An;Oh, Hye Jeong;Lee, Jong Hwa
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.6 no.2
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    • pp.301-312
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    • 1996
  • This study was performed to search a optimal analyzing method of cadmium in whole-blood. Cadmium was determined by graphite furnace atomic absorption spectrometry(GFAAS). We investigated the effect of ashing temperature on the absorbance of cadmium in a simple dilution(ten-fold) method with triton X-100 and matrix modifier methods treated with $NH_4H_2PO_4$(1 and 3%) and $Pd(NO_3)_2$(0.00l and 0.005%) as matrix modifier. We also compared the reported reference values of standard blood with values resulted from optimal analyzing conditions of this study. In case of a simple dilution method, when ashing temperature was set at $450^{\circ}C$, the absorbance of sample and background were $0.334{\pm}0.012$ and $1.382{\pm}0.245$, respectively. Background level was higher than the value(0.8) that can be corrected by $D_2$ background correction method. As ashing temperature was rised to $500^{\circ}C$, the absorbance of sample and background were $0.178{\pm}0.008$ and $0.711{\pm}0.223$ respectively. The higher ashing temperature($450^{\circ}C-650^{\circ}C$) was, the lower the absorbance of sample was. In case of a matrix modifier method with $NH_4H_2PO_4$(1 and 3%), when ashing temperature was rised from $500^{\circ}C$ to $650^{\circ}C$, the absorbance of sample slightly changed. The absorbances of sample at $600^{\circ}C$ were $0.230{\pm}0.017$ and $0.137{\pm}0.012$, respectively. These values were larger than that of simple dilution method. But the absorbance of background was higher than the level that can be corrected by $D_2$ method. In case of a matrix modifier method with $Pd(NO_3)_2$(0.001 and 0.005%), the absorbance of sample and background were higher than those of other methods and were stable and reproducible. When ashing temperature was over $550^{\circ}C$, the absorbance of sample was significantly decreased. In case of 0.005% $Pd(NO_3)_2$ carbon residue remained in graphite tube affected the absorbance of sample and background. From these results, We propose that in case of a simple dilution(ten-fold) method with triton X-100 ashing temperature must be maintained below $400^{\circ}C$. In order to diminish the absorbance of background, the alternative method is attenuation of injection volume or multiplication of dilution ratio. We recommend $Pd(NO_3)_2$ than $NH_4H_2PO_4$ as a matrix modifier. In case of a matrix modifier method with $Pd(NO_3)_2$ ashing temperature might be maintained below $550^{\circ}C$.

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Changes of Lead Content during Warm Storage of Canned Coffee Drinks (캔 커피의 온장 시 납 함량의 변화)

  • Lee, Kyung-Ju;Lee, Mi-Gyung
    • Korean Journal of Food Science and Technology
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    • v.39 no.2
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    • pp.228-230
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    • 2007
  • In this study, we investigated the change in lead content of canned coffee drinks while kept for 16 weeks in an incubator adjusted to $65^{\circ}C$. Our research aim was to ensure the safety of canned coffee purchased from vending machine and stores. The lead analysis were conducted by graphite furnace atomic absorption spectrometry after wet digestion using concentrated nitric acid. The results showed that the lead contents of all examined samples were very low at a level of not detected to 0.033 mg/L, and below 2 mg/kg, the Korean regulatory limit for the commodity. Also, no increase in lead content was observed over the elapsed time. Therefore, it appears that lead is not a hazard and need not be a concern in drinking canned coffee.

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.

Emission Characteristics of Elemental Constituents in Fine Particulate Matter Using a Semi-continuous Measurement System (준 실시간 측정시스템을 이용한 미세입자 원소성분 배출특성 조사)

  • Park, Seung-Shik;Ondov, John M.
    • Journal of Korean Society for Atmospheric Environment
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    • v.26 no.2
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    • pp.190-201
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    • 2010
  • Fine particulate matter < $1.8{\mu}m$ was collected as a slurry using the Semicontinuous Elements in Aerosol Sampler with time resolution of 30-min between May 23 and 27, 2002 at the Sydney Supersite, Florida, USA. Concentrations of 11 elements, i.e., Al, As, Cd, Cr, Cu, Fe, Mn, Ni, Pb, Se, and Zn, in the collected slurry samples were determined off-line by simultaneous multi-element graphite furnace atomic absorption spectrometry. Temporal profiles of $SO_2$ and elemental concentrations combined with meteorological parameters such as wind direction and wind speed indicate that some transient events in their concentrations are highly correlated with the periods when the plume from an animal feed supplement processing facility influenced the Sydney sampling site. The peaking concentrations of the elemental species during the transient events varied clearly as the plume intensity varied, but the relative concentrations for As, Cr, Pb, and Zn with respect to Cd showed almost consistent values. During the transient events, metal concentrations increased by factors of >10~100 due to the influence of consistent plumes from an individual stationary source. Also the multi-variate air dispersion receptor model, which was previously developed by Park et al. (2005), was applied to ambient $SO_2$ and 8 elements (Al, As, Cd, Cr, Cu, Fe, Pb, and Zn) measurements between 20:00 May 23 and 09:30 May 24 when winds blew from between 70 and $85^{\circ}$, in which animal feed processing plant is situated, to determine emission and ambient source contributions rates of $SO_2$ and elements from one animal feed processing plant. Agreement between observed and predicted $SO_2$ concentrations was excellent (R of 0.99; and their ratio, $1.09{\pm}0.35$) when one emission source was used in the model. Average ratios of observed and predicted concentrations for As, Cd, Cr, Pb, and Zn varied from $0.83{\pm}0.26$ for Pb to $1.12{\pm}0.53$ for Cd.

Direct Determination Method of Antimony in High Purity Copper Metal by Graphite Furnace Atomic Absorption Spectrometry (흑연로 원자 흡수흡광법에 의한 고순도 구리 합금중의 안티몬의 직접 분석 방법)

  • Yoo, K.S;Kyung, J.D;Kwon, J.G;Lee, J.J
    • Journal of the Korean Chemical Society
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    • v.39 no.4
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    • pp.252-256
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    • 1995
  • A study was carried out for the development of direct determination of antimony in high purity copper metal without preseparation. The large excess of copper seemed to be performed as the matrix modifier to enhance the absorbance of antimony in copper metal. Sensitivity enhancement of Sb was obtained at the condition of the ashing temperature of $600^{\circ}C(20s){\sim}700^{\circ}C(10s)$ rather than $1000^{\circ}C(20s){\sim}1100^{\circ}C(10s)$, and the atomization temperature of $2200^{\circ}C.$ The operating pressure of argon gas was readjusted to the optimum condition at 2.0 kg/$cm^2.$ The linearity of the Sb calibration graph could be obtained in the range of 20 ppb up to 200 ppb Sb in existence of 5,000 ppm Cu with the coefficient of variation of about 5%.

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Effect of Airborne Lead Concentration Characterized by Size on Blood Lead and Their Relationships (납 흡수에 영향을 미치는 요인 분석: 납 크기 특성과 혈액중 납과의 관계)

  • Park, Dong-Uk;Ha, Kwon-Chul
    • Journal of Environmental Health Sciences
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    • v.31 no.4 s.85
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    • pp.316-321
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    • 2005
  • 4개 업종(축전지제조업, 광명단 제조업, 2차 제련업, 라디에타 제조업)에서 근무하는 총 100명의 근로자를 대상으로 8단계다단충돌기(eight stages personal cascade imparter)에 의한 입자 크기 별 납농도를 측정하였다 크기 별 납 농도는 총납(PbA), 흡입성납(IPM-PbA), 흉곽성납(TPM-PbA), 호흡성납(RPM-PbA), $1{\mu}m$ 미만의 납$(Pb_{1\mu})$ 그리고 $1{\mu}m$ 이상의 소화성납$(Pb_{ing})$이었다. 동일한 근로자(100명)를 대상으로 혈액에서 납농도를 측정하였다. 혈액 중 납은 원자흡광광도계(atomic absorption spectrometry)의 Zeeman effect graphite furnace를 이용하여 분석하였다. 총 납의 노출농도는 노출기준$(50\;ug/m^3)$을 크게 초과하였다. 평균 호흡성 납 노출농도$(115.7\;ug/m^3)$ 총 납의 노출기준을 훨씬 초과하였다. $1{\mu}m$미만의 납$(Pb_{1\mu})$ 노출농도의 범위는 0.7에서 $(492.2\;ug/m^3)$이나 되었다. 근로자의 $46\%$가 혈액 중 납 농도 40 ug/dL을 초과하였다. 60 ug/dL을 초과한 경우도 $13\%$나 되었다. 입자 크기가 큰 납인 총납, 흡입성 납 그리고 호흡성 납 농도는 혈액 중 납 농도와 유의한 상관을 보였다(p<0.0001). 그러나 가장 높은 상관은 $1{\mu}m$미만의 납$(Pb_{1\mu})$ 혈액 중 납과의 관계였다. T-test에서 $50ug/m^3$이상의 호흡성 납을 나타낸 근로자 그룹과 $50ug/m^3$ 이하의 근로자 그룹간에의 혈액 중 납 농도는 유의한 차이가 있는 것으로 나타났다(p=0.000). 이러한 연구결과는 입자크기 구분이 없는 현재의 총납에 의한 노출기준과 측정방법은 미세 납 먼지에 노출되는 근로자의 납흡수를 보호하는데 한계점이 있다는 것을 의미한다. 향후 납 입자크기는 물론 근로자의 개인적인 위생과 작업내용 등을 변수로 납 흡수에 영향을 미치는 종합적인 요인을 찾아내는 연구를 진행할 필요가 있다.

Development and Validation of Reference Material for Proficiency Testing of Blood Heavy Metals in Environmental Biomonitoring (환경 바이오모니터링에서의 혈중 중금속 분석 숙련도 시험을 위한 표준물질 제조 및 적용성 평가)

  • Im, Hosub;Yang, Minho;Oh, Selim;Kim, Soyoung;Jung, Hojun;Cho, Yong Min;Lee, Jung Sub;Kim, Hyun Jeong;Lee, Chae Kwan;Moon, Chan-Seok;Lee, Jong-Wha
    • Journal of Environmental Health Sciences
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    • v.42 no.6
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    • pp.450-464
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    • 2016
  • Objectives: This study developed and validated reference materials (RMs) to analyze metal compounds in blood. Methods: We referred to KoNEHS (Korea National Environmental Health Survey) to estimate concentrations of blood metals (cadmium, Cd; lead, Pb; mercury, Hg) and applied analytical methods (inductively coupled plasma - mass spectroscopy, ICP-MS, for Cd and Pb; graphite furnace - atomic absorption spectrometry, GF-AAS, for Cd and Pb; and direct mercury analyzer, DMA, for Hg). Homogeneity and stability tests were carried out. In addition, certified values and uncertainties of RMs were calculated through internal and external experiments. All RMs were developed and assessed in various forms according to element, analytical method, and two types of concentration levels high concentration for occupational exposure and low concentration for environmental exposure. Results: All samples showed acceptable homogeneity, except for low concentration of Cd in the GF-AAS method. Short- and long-term stabilities were satisfied by ANOVA testing. In the inter-laboratory comparison, robust medians were lower than the certified values of all RMs (robust median/reference value; $1.301/1.327{\mu}g/L$ for Cd, ICP-MS, low concentration; $3.152/3.388{\mu}g/L$ for Cd, ICP-MS, high concentration; $1.219/1.301{\mu}g/L$ for Cd, GF-AAS, low concentration; $3.074/3.321{\mu}g/L$ for Cd, GF-AAS, high concentration; $14.473/14.516{\mu}g/L$ for Pb, ICP-MS, low concentration; $50.069/50.114{\mu}g/L$ for Pb, ICP-MS, high concentration; $12.881/14.147{\mu}g/L$ for Pb, GF-AAS, low concentration; $47.015/47.591{\mu}g/L$ for Pb, GF-AAS, high concentration; $4.059/4.218{\mu}g/L$ for Hg, DMA, low concentration; $11.474/11.181{\mu}g/L$ for Hg, DMA, high concentration). Conclusion: This study demonstrates procedures for developing and validating RMs for biomonitoring in the field of the environmental health.

Determination of Heavy Metal Concentration in Herbal Medicines by GF-AAS and Automated Mercury Analyzer

  • Kim, Sang-A;Kim, Young-Jun
    • Journal of Food Hygiene and Safety
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    • v.36 no.4
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    • pp.281-288
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    • 2021
  • This study was conducted to analyze and compare the concentrations of heavy metals in 430 different products of 20 types of herbal medicines available in the domestic market in Korea by Graphite Furnace-Atomic Absorption Spectrometry (GF-AAS) and automated mercury analyzer. The accuracy for lead (Pb), arsenic (As), cadmium (Cd), and mercury (Hg) was in the range 92.67-102.56%, and the precision was 0.21-6.00 relative standard deviation (RSD%), which was in compliance with the Codex acceptable range. Furthermore, the Food Analysis Performance Assessment Scheme (FAPAS) quality control (QC) material showed a recovery range of 96.7-102.0% and 0.33-4.93 RSD%. The average contents (㎍/kg) of Pb, As, Cd, and Hg in herbal medicines were 254.9 (not detected (N.D.)-2,515.2), 171.0 (N.D.-2,465.2), 99.2 (N.D.-797.1), and 6.0 (N.D.-83.6), respectively. Based on the quantitative analysis results, the heavy metal contents of 20 types of herbal medicines distributed in Korea are within the acceptable range according to the standards issued by the Ministry of Food and Drug Safety (MFDS). By using the manufacturer of herbal products as the standard for QC, the Pb, As, Cd, and Hg contents were investigated in the packaging process just before distribution to determine the actual conditions of residual heavy metals in herbal medicines. Thus, these result may contribute to monitoring the QC of herbal medicines distributed in Korea and could provide basic data for supplying safe herbal medicines to the public.

Exposed level of workers in the factory next to a lead recycling factory (연 재생공장 인접 근로자들의 연 폭로정도에 관한 조사)

  • Kim, Jin-Ha;Lee, Duk-Hee;Lee, Yong-Hwan
    • Journal of Preventive Medicine and Public Health
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    • v.29 no.3 s.54
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    • pp.693-700
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    • 1996
  • The purpose of this study was to determine whether workers at a factory next to a lead recycling factory in Pusan, were affected by lead contamination. The mean air lead concentration of lead recycling factory was $0.21mg/m^3(TWA=0.05mg/m^3)$. Thirty-nine male workers of Factory A, Cr. plating factory next to the lead recycling factory were exposed group and a comparison group, 62 male workers of Factory B were selected from another Cr. plating factory about 8.5km away from lead recycling factory. Air lead concentration of each workplace was checked for 4 times from August f to August 20 in 1995 by low volume air sampler. Each subject was interviewed about age, life-style, smoking, work history, and residence etc, and venous blood was drawn for lead measurement by graphite furnace atomic absorption spectrometry. We have observed that air lead concentration and blood lead concentration of Factory A was higher than Factory $B(2.6{\pm}1.6\;Vs.\;1.2{\pm}0.2{\mu}g/m^3,\;14.9{\pm}1.6\;Vs.\;12.2{\pm}1.6{\mu}g/dl)$. We believe that other environmental lead sources such as transportation and residence did not affect air lead and blood lead concentration differences of both factory. We concluded that high air lead and blood lead concentration of Factory A were caused by lead contamination generated by the neighboring lead recycling factory.

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Study on the screening method for determination of heavy metals in cellular phone for the restrictions on the use of certain hazardous substances (RoHS) (유해물질 규제법(RoHS)에 따른 휴대폰 내의 중금속 함유량 측정을 위한 스크리닝법 연구)

  • Kim, Y.H.;Lee, J.S.;Lim, H.B.
    • Analytical Science and Technology
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    • v.23 no.1
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    • pp.1-14
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    • 2010
  • It is of importance that all countries in worldwide, including EU and China, have adopted the Restrictions on the use of certain Hazardous Substances (RoHS) for all electronics. IEC62321 document, which was published by the International Electronics Committee (IEC) can have conflicts with the standards in the market. On the contrary Publicly Accessible Specification (PAS) for sampling published by IEC TC111 can be adopted for complementary application. In this work, we tried to find a route to disassemble and disjoint cellular phone sample, based on PAS and compare the screening methods available in the market. For this work, the cellular phone produced in 2001, before the regulation was born, was chosen for better detection. Although X-ray Fluorescence (XRF) showed excellent performance for screening, fast and easy handling, it can give information on the surface, not the bulk, and have some limitations due to significant matrix interference and lack of variety of standards for quantification. It means that screening with XRF sometimes requires supplementary tool. There are several techniques available in the market of analytical instruments. Laser ablation (LA) ICP-MS, energy dispersive (ED) XRF and scanning electron microscope (SEM)-energy dispersive X-ray (EDX) were demonstrated for screening a cellular phone. For quantitative determination, graphite furnace atomic absorption spectrometry (GF-AAS) was employed. Experimental results for Pb in a battery showed large difference in analytical results in between XRF and GF-AAS, i.e., 0.92% and 5.67%, respectively. In addition, the standard deviation of XRF was extremely large in the range of 23-168%, compared with that in the range of 1.9-92.3% for LA-ICP-MS. In conclusion, GF-AAS was required for quantitative analysis although EDX was used for screening. In this work, it was proved that LA-ICP-MS can be used as a screening method for fast analysis to determine hazardous elements in electrical products.