Optimum Conditions for Hydride Generation of Selenium and Its Determination by Atomic Absorption Spectrophotometry

1983 ◽  
Vol 66 (1) ◽  
pp. 130-134
Author(s):  
Robert R Brooks ◽  
Janine A Willis ◽  
John R Liddle

Abstract Instrumental parameters and other variables were studied to establish the optimum indicators for determination of selenium by atomic absorption spectrophotometry using the hydride generation procedure with cold-trapping. Optimum conditions were established by consideration of the following variables: volume of reaction solution, acid concentration in the reaction mixture, lapse of time after last addition of borohydride, method of addition of borohydride, carrier gas flow rates, position of source beam in the flame cell, oxidation state of selenium, and effect of drying the cold trap between successive determinations. This latter procedure greatly improved the reproducibility of the technique (from ±28% to ±2%. The limit of detection was about 2 ng selenium.

1980 ◽  
Vol 63 (6) ◽  
pp. 1175-1180
Author(s):  
John R Liddle ◽  
Robert R Brooks ◽  
Roger D Reeves

Abstract The atomic absorption signals obtained from the reduction of arsenic(V) by sodium borohydride solution are strongly dependent on a number of parameters which are examined in this paper. If the arsine produced by sodium borohydride reduction is condensed in a cold trap and then released suddenly, the atomic absorption peak is larger and more reproducible. The procedure is more satisfactory if the borohydride solution is added to the reaction mixture in small aliquots. Peak height depends on the total volume of the reaction mixture and on the carrier gas flow rate. Peak height is also a function of the time elapsed after addition of the final aliquot of borohydride, and increases as the interval between successive aliquots is increased. Optimum conditions established were: initial volume of reaction mixture, 30 mL; 12 mL 3% NaBH4 solution added in 2 mL aliquots at 30 s intervals; carrier gas flow 1.25 L/ min; 60 s time lapse from last addition of borohydride until removal of the cold trap. Under these conditions, linear absorbance-concentration curves were obtained for 0.05–3.0 μg arsenic, with a relative standard deviation of 4.2% at the 2 %g level.


1973 ◽  
Vol 56 (6) ◽  
pp. 1306-1312
Author(s):  
Frank E Hoggins ◽  
Robert R Brooks

Abstract Studies have been made on the instrumental parameters affecting the performance of the solution-reduction and the thermal-volatilization techniques of flameless atomic absorption for mercury. Optimum conditions established for the solution-reduction technique were: gas flow 5 L/min, stirring time 100 sec, and stirring rate at least 1250 rpm. Optimum conditions for the thermal-volatilization technique were: flow rate 1.5 L/min, heating time 20 sec. The 2 techniques are compared.


1987 ◽  
Vol 33 (11) ◽  
pp. 2004-2007 ◽  
Author(s):  
S Nomoto ◽  
S Shoji

Abstract We sought to establish optimum conditions for measuring calcium in erythrocytes by atomic absorption spectrophotometry. The conditions we selected are as follows. Wash one volume of fresh heparin-treated packed cells once with 30 volumes of isotonic buffered saline (pH 7.4) at a temperature somewhat exceeding 25 degrees C. Dilute the washed packed cells 10-fold with 12 mmol/L hydrochloric acid, and analyze the supernate for calcium. Measure the hematocrit of the washed packed cells, then analyze an aliquot of them for calcium, using a computer-readout type of flame or a non-flame atomic absorption spectrophotometer equipped with a pyrocoated graphite tube. The temperature program is 1000 degrees C for ashing [corrected] and 1800 degrees C for the atomizing cycle. Intraday and day-to-day reproducibility of the assay was 6.55% and 8.19%, respectively, at the mean concentration of calcium in the erythrocytes of healthy adults, which is 4.30 mumol/L.


2014 ◽  
Vol 556-562 ◽  
pp. 64-66
Author(s):  
Chun Yan Zhang ◽  
Chuan Tao Wang ◽  
Shu Hao Wang ◽  
Ling Yun Du

ZnS semiconductor nanocrystals (NCs) were prepared by ways from primary materials of ZnCl2 and Na2S in water solution. Using the synthesized ZnS NCs, a polyclonal antibody-based ZnS-labelled immunosorbent assay for the determination of estriol (E3) was developed with atomic absorption spectrophotometry (AAS) as a detector. An immunoaffinity column was applied to testify conjugation between antibody and ZnS NCs. The linear range for determination of estriol is 40.0~600.0 ng.mL-1, and the limit of detection (LOD) is 10.0 ng.mL-1. Some serum samples have been analyzed with satisfactory results which are in good agreement with those obtained using ELISA. This work suggests the potential application of NCs as biological probes and AAS as detector in nonisotopic immunoassay.


1999 ◽  
Vol 82 (2) ◽  
pp. 364-367 ◽  
Author(s):  
Ujang Tinggi

Abstract Wet digestion using a mixture of nitric, sulfuric, and perchloric acids and an aluminum block digester effectively and rapidly decomposed meat samples for selenium determination by hydride generation atomic absorption spectrophotometry. Digestion did not require constant attention by an operator. Selenium recoveries (range, 94-105%) from National Institute ofStandards and Technology standard reference materials and spiked samples were used to validate method accuracy. Coefficients of variation (CVs) of repeatability of in-house reference materials used forprecision study were 6.4 and 5.6%, respectively, for seafood mix and mutton liver. Selenium levels in meat products from Brisbane markets varied widely: 0.042-0.142,0.081- 0.42, and 0.050-0.198 μg/g (wet weight) respectively, for beef, chicken, and pork. Overall, selenium levels in manufactured meat ranged from0.041 to 0.189 fig/g. The levels of selenium foundinthis study were generally lower than those reported in Finland but comparable with those reported in some parts of the United States


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