• 한국환경보건학회지
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• 제26권4호
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• pp.75-81
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• 2000

A matrix modification was studied for the determination of trace manganese in several seaweeds by electrothermal atomic absorption spectrophotometry(ETAAS). The type and quantity of modifiers were investigated to realize the efficient modification. Palladium was chosen as a single modifier. By the addition of palladium(5$\mu\textrm{g}$/$m\ell$) to 2ng/$m\ell$ manganese solution, the temperatures were raised from 1,00$0^{\circ}C$ to 1,20$0^{\circ}C$ for the charring and from 2,10$0^{\circ}C$ to 2,20$0^{\circ}C$ for the atomization as well as the sensitivity and reproducibility were improved. With such optimum conditions, the trace amount of manganese in several seaweeds(laver, tangle and brown seaweed) could be determined by a calibration curve method, and good recoveries of more than 965 were also obtained in the samples in which a given amount of manganese was spiked. The detection limit of this method was about 0.048ng/$m\ell$.

• 분석과학
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• 제8권4호
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• pp.435-442
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• 1995

A matrix modification was studied for the determination of trace bismuth in water samples by graphite furnace atomic absorption spectrophotometry. The type and quantity of modifiers as well as the use of auxiliary modifiers were investigated to realize the efficient modification. Palladium was chosen as a single modifier. By the addition of palladium($5{\mu}g/mL$) to 100 ng/mL bismuth solution, the temperatures could be raised from $500^{\circ}C$ to $1,300^{\circ}C$ for the charring and from $2,000^{\circ}C$ to $2,200^{\circ}C$ for the atomization as well as the sensitivity and reproducibility were improved. The absorbance of bismuth was maximum and not changed in the range of Pd $3-25{\mu}g/mL$. And several materials were examined as an auxiliary modifier. The mixed solution of $1{\mu}g/mL$ palladium and $200{\mu}g/mL$ nickel have raised the temperatures as with $5{\mu}g/mL$ palladium only. The maximum absorbance of bismuth was shown in the nickel concentration range of $100-300{\mu}g/mL$ in $1{\mu}g/mL$ palladium modified system. With such optimum conditions, the trace amount of bismuth in several water samples could be determined by a calibration curve method, and good recoveries were also obtained.

• Bulletin of the Korean Chemical Society
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• 제21권1호
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• pp.56-60
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• 2000

The mechanism of a matrix modification for the trace determination of volatile lead and bismuth by an electro-thermal atomic absorption spectrophotometry was studied by a X-ray diffractometry (XRD). For the investigation of structures, the ash products of the elements were produced by using a palladium as a matrix modifier with or without aluminum or nickel as an auxiliary modifier. The same charring conditions as in the analysis of samples were applied together with much concentrated solution of analytical elements and modifiers in a graphite furnace to get a large amount of the product for XRD. The XRD patterns showed PbPd3 for lead and BiPd3 for bismuth. These mean that the reaction procedures through the charring and atomization were changed from $Pb^{2+}$ ${\rightarrow}$ PbO ${\rightarrow}$$Pb^0$ to $Pb^{2+}$ ${\rightarrow}$ PbO ${\rightarrow}PbPd_3$ ${\rightarrow}$ Pb o for lead and from $Bi^{3+}$ ${\rightarrow}$ BiO ${\rightarrow}$ Bi o to $Bi^{3+}$ ${\rightarrow}$ BiO ${\rightarrow}$ $BiPd_3$ ${\rightarrow}$ $Bi^0$ for bismuth by the addition of modifiers. The volatile elements were stabilized by the formation of palladium alloys through a charring process. Charring temperatures were raised about 500 $^{\circ}C$ by the alloying and the atomization was also stabilized for the enhancement of sensitivities.

• 대한화학회지
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• 제40권2호
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• pp.109-116
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• 1996

물시료 중 존재하는 흔적량 게르마늄을 전열 원자흡수 분광광도법으로 정랑하기 위해 사용되는 매트릭스 개선제의 종류와 사용량, 이에 따를 회화 및 원자화 온도의 변화, 보조제의 사용여부 및 양에 관하여 연구하였다. 게르마늄은 회화단계에서 이산화 게르마늄이 흑연로 성분인 탄소로 인해 휘발성 일산화 게르마늄으로 환원되에 감도 및 재현성을 저하시킨다. 따라서 개선제를 사용하여 게르마늄을 열적 및 화학적으로 안정화시켜야 한다. 이를 위해 단일 개선제를 사용할 경우 파라듐이 가장 좋은 효과를 나타내었다. 이 경우 원자화온도는 변화시키지 않지만, 회화온도는 800.deg.C에서 1, 000.deg.C로 올릴수 있었고 흡광도도 증가하였다. 이런 조건에서 팔라듐의 농도가 게르마늄에 대해 몰비로 14-100인 10-70.mu.g/mL까지 흡광도가 일정하였다. 보조개선제의 사용도 검토하였는데, 1% 수산화암모늄을 가하여 회화온도를 1, 000.deg.C까지 증가시켰다. 이제까지 검토한 최적조건을 바탕으로 광천수 3가지를 분석한 결과 게르마늄이 2.46, 1.60 및 0.020.mu./mL이었다. 끝으로, 시료에 일정량의 게르마늄을 첨가하여 얻은 회수율은 모두 95%이상으로 정량적이라고 할 수 있고, 검출한계는 6.9ng/mL로 흔적량 게르마늄 분석에 유용한 것으로 판단되었다.