Atomic Absorption Spectrophotometric Determination of 4-Hydroxy-3-Nitrobenzenearsonic Acid (Roxarsone) in Premixes

1975 ◽  
Vol 58 (5) ◽  
pp. 945-948 ◽  
Author(s):  
Larry J Frahm ◽  
Marven E Albrecht ◽  
J Patrick Mcdonnell
Keyword(s):  
Atomic Absorption ◽  
Ammonium Carbonate ◽  
Atomic Absorption Spectrophotometry ◽  
Electrodeless Discharge ◽  
Absorption Spectrophotometry ◽  
Coefficients Of Variation ◽  
Instrument Response ◽  
Variation Range ◽  
Standard Solution

Abstract Roxarsone (4-hydroxy-3-nitrobenzenearsonic acid) is extracted from the premix with aqueous 1% ammonium carbonate. The extract is filtered, diluted, and analyzed by atomic absorption spectrophotometry, using an air-acetylene flame and an arsenic electrodeless discharge lamp. The instrument response of the sample is compared to that of a standard solution of arsenic trioxide. Recoveries range from 99.7 to 100.4% and coefficients of variation range from 0.35 to 0.63%.

Collaborative Study of a Method for the Atomic Absorption Spectrophotometric and Polarographic Determination of Cadmium in Food

1973 ◽  
Vol 56 (4) ◽  
pp. 876-881
Author(s):  
Raymond J Gajan ◽  
John H Gould ◽  
James O Watts ◽  
John A Fiorino
Keyword(s):  
Phase I ◽  
Atomic Absorption ◽  
Orange Juice ◽  
Collaborative Study ◽  
Atomic Absorption Spectrophotometry ◽  
Absorption Method ◽  
Acid Digestion ◽  
Absorption Spectrophotometry ◽  
Coefficients Of Variation

Abstract The method studied involves acid digestion, dithizone extraction, and determination by atomic absorption spectrophotometry and polarography. This study consisted of 2 phases, with 10 laboratories participating in Phase I and 15 laboratories in Phase II. The 12 commodities studied (lettuce, potatoes, orange juice, shredded wheat, milk, sugar, eggs, fish, frankfurters, rice, beans, and oysters) were spiked at 0.05, 0.1, 0.2, 0.4, 0.5, 1.0, 1.5, and 2.0 ppm cadmium. Only 3 collaborators submitted polarographic results. There were no statistically demonstrable differences for the atomic absorption method between spiking levels, commodities, or laboratories. Coefficients of variation were acceptable. The atomic absorption spectrophotometric method for determining cadmium has been adopted as official first action.

Atomic Absorption Determination of Lead in Apples

1974 ◽  
Vol 57 (4) ◽  
pp. 970-972
Author(s):  
John R Markus
Keyword(s):  
Atomic Absorption ◽  
Atomic Absorption Spectrophotometry ◽  
Absorption Spectrophotometry ◽  
Atomic Absorption Determination ◽  
Methods Of Analysis ◽  
Coefficients Of Variation ◽  
Absorption Determination ◽  
Official Methods Of Analysis

Abstract Two studies have been conducted on the analysis of apples for lead by atomic absorption spectrophotometry using the official first action method, 25.B01–25.B05. Sixteen laboratories participated in each study. Recoveries ranged from 92.6 to 110% (101.6% average) in the first study. A second study, in which procedural modifications were made, showed recoveries ranging from 91.2 to 109.7%, with an average of 100.0%. Coefficients of variation for the first and second studies were 5.19 and 4.94%, respectively. On the basis of the second study, procedural modifications have been incorporated into the 12th Edition of Official Methods of Analysis.

Determination of Lead in Fish by Atomic Absorption Spectrophotometry and by Polarography. II. Collaborative Study

1972 ◽  
Vol 55 (4) ◽  
pp. 733-736
Author(s):  
Raymond J Gajan ◽  
Damon Larry
Keyword(s):  
Atomic Absorption ◽  
Collaborative Study ◽  
Atomic Absorption Spectrophotometry ◽  
Polarographic Method ◽  
Absorption Spectrophotometry ◽  
Paired Samples ◽  
Coefficients Of Variation ◽  
Different Types ◽  
Average Lead

Abstract Nineteen laboratories, using 6 different models of atomic absorption spectrophotometers and 4 different types of polarographs, participated in this collaborative study. The average lead recoveries from 6 paired samples at 1–2, 5–6, and 10–11 ppm levels were 97.7% by polarography and 100.7% by atomic absorption. The average standard deviations were 0.32 and 0.41 ppm, respectively, and the average coefficients of variation were 7.9 and 13.1%, respectively. With collaborators reporting on both methods, the results of the overall method average were 4.3 ppm for polarography and 4.4 ppm for atomic absorption. Since there were no significant differences (p > 0.05) found between the method averages, except at one of the unspiked levels, the 2 methods can be used to confirm each other at levels of 1-11 ppm. The polarographic method has been adopted as official first action for the determination of lead in fish.

A Simplified Determination of Urinary Cadmium, Lead, and Thallium, with Use of Carbon Rod Atomization and Atomic Absorption Spectrophotometry

1973 ◽  
Vol 19 (9) ◽  
pp. 954-958 ◽  
Author(s):  
Norman P Kubasik ◽  
Michael T Volosin
Keyword(s):  
Atomic Absorption ◽  
Matrix Effects ◽  
Atomic Absorption Spectrophotometry ◽  
Small Sample ◽  
Absorption Spectrophotometry ◽  
Coefficients Of Variation ◽  
Standard Additions ◽  
Cadmium Lead ◽  
Carbon Rod Atomizer

Abstract Lead, cadmium, and thallium are determined in a single 3-ml urine sample. The three metals, simultaneously chelated with sodium diethyldithiocarbamate, are extracted (at pH 3-7) into methyl isobutyl ketone (isopropylacetone), and the carbon rod atomizer, in conjunction with atomic absorption spectrophotometry, is used to analyze the extracts. Small sample requirements (1.6 µl) permit the extraction to be carried out in small-volume disposable glassware, with use of disposable pipets. Within-run coefficients of variation were all less than 5%; recovery ranged from 96-106%. Several normal urinary constituents, added in excess, negligibly affected recoveries. Ethylenediaminetetraacetate in the urine inhibited recovery of lead; this was reversed by adding excess calcium to the urine before extraction. The method of standard additions was used to compensate for differences between standards and unknowns caused by matrix effects.

Determination of Lead in Evaporated Milk by Atomic Absorption Spectrophotometry and Anodic Stripping Voltammetry: Collaborative Study

1973 ◽  
Vol 56 (5) ◽  
pp. 1246-1251
Author(s):  
John A Fiorino ◽  
Robert A Moffitt ◽  
Albert L Woodson ◽  
Raymond J Gajan ◽  
Glen E Huskey ◽  
...  
Keyword(s):  
Atomic Absorption ◽  
Anodic Stripping Voltammetry ◽  
Collaborative Study ◽  
Stripping Voltammetry ◽  
Atomic Absorption Spectrophotometry ◽  
Absorption Spectrophotometry ◽  
Coefficients Of Variation ◽  
Anodic Stripping ◽  
Ppm Level

Abstract A method for the determination of lead in evaporated milk was successfully collaborated by 11 laboratories. Five laboratories used both atomic absorption spectrophotometry (AAS) and anodic stripping voltammetry (ASV) for the determination, 5 used only the atomic absorption method, and 1 used only the polarographic method. Each collaborator received 12 samples, 2 at each of the 5 different levels (0.06–0.95 ppm) and 2 practice samples with a known lead content. Both AAS and ASV were equally suitable for the determination of lead in the concentration range studied. The pooled variation between duplicate determinations was 0.0010 and 0.0016 for the AAS and ASV methods, respectively. For the AAS determinations the coefficients of variation (random error components) decreased from 43% at the lowest Pb level to 4% at the highest level. Although the ASV results did not show the same regularity of decreasing coefficients of variation with increasing Pb level, the coefficients of variation were acceptable: 28% at the 0.06 ppm level and 6% at the 0.22 ppm level. The AAS method has been adopted as official first action and the ASV method as interim official first action.

Atomic Absorption Spectrophotometric Determination of Lead, Cadmium, Zinc, and Copper in Clams and Oysters: Collaborative Study

1977 ◽  
Vol 60 (6) ◽  
pp. 1400-1407
Author(s):  
Stephen G Capar
Keyword(s):  
Atomic Absorption ◽  
Butyl Acetate ◽  
Collaborative Study ◽  
Atomic Absorption Spectrophotometry ◽  
Flame Atomic Absorption Spectrophotometry ◽  
Absorption Spectrophotometry ◽  
Flame Atomic Absorption ◽  
Coefficients Of Variation ◽  
Aspiration Technique

Abstract In the method studied, clams and oysters are dry ashed at 475°C, the ash is dissolved in dilute HNO3, and Pb, Cd, Zn, and Cu are determined by flame atomic absorption spectrophotometry (AAS). Sample solutions containing levels of Pb and Cd too low for direct AAS are extracted as the 1-pyrrolidinecarbodithioate complex into n-butyl acetate before AAS. The method was subjected to a collaborative study to determine the precision and accuracy of the analysis. Concentration ranges in the samples studied were approximately 0.06–2 ppm Pb, 0.03–2 ppm Cd, 40–600 ppm Zn, and 5–50 ppm Cu. Within these ranges, Cd levels <0.5 ppm and Pb at all levels required extraction prior to AAS. The average coefficients of variation for Pb, Cd, Zn, and Cu were, respectively, 66.0, 93.2, 8.5, and 20.5% for the lowest levels and 13.5, 3.8, 6.7, and 6.8% for the highest levels. Recoveries were computed by using the sum of the average collaborative results for the totally unfortified samples plus the fortification levels as the expected concentration. The average recoveries of Pb, Cd, Zn, and Cu were, respectively, 94.0, 99.7, 99.3, and 100.2 % for the lowest fortification level and 94.8, 95.6, 96.5, and 97.5% for the highest level. High levels of Cu and/or Zn caused incomplete extraction of Pb and Cd, with Cd being affected more severely than Pb. Data obtained also suggest that background corrections may be needed for determining Zn and Cd with the direct aspiration technique. No recommendation is made for official action.

Improved assay for bismuth in biological samples by atomic absorption spectrophotometry with hydride generation.

1988 ◽  
Vol 34 (2) ◽  
pp. 382-384 ◽  
Author(s):  
P R Froomes ◽  
A T Wan ◽  
P M Harrison ◽  
A J McLean
Keyword(s):  
Atomic Absorption ◽  
Biological Fluids ◽  
Hydride Generation ◽  
Atomic Absorption Spectrophotometry ◽  
Reference Intervals ◽  
Clinical Samples ◽  
Acid Digestion ◽  
Electrodeless Discharge ◽  
Absorption Spectrophotometry

Abstract This simple, rapid, sensitive, reliable, and economical assay for bismuth in plasma, erythrocytes, and urine is based on atomic absorption spectrophotometry with hydride generation. Acid digestion eliminates the problem of foaming, which hitherto has complicated such assay of bismuth in plasma and erythrocytes. The detection limit of the assay has been improved to 0.1 micrograms/L, as compared with a previously documented limit of 2.5 micrograms/L. Average recovery exceeded 95% in all biological fluids. Economy of use derives from elimination of need for electrodeless discharge lamps and atomic absorption grade borohydride. Determination of basal concentrations of bismuth in clinical samples of body fluids gave reference intervals of 0.1-3.5 micrograms/L for plasma, 0.3-4.6 micrograms/L for urine.

Determination of Minor Nutrients in Fertilizers by Atomic Absorption Spectrophotometry: Second Collaborative Study

1965 ◽  
Vol 48 (6) ◽  
pp. 1100-1103
Author(s):  
C H Mcbride
Keyword(s):  
Atomic Absorption ◽  
Collaborative Study ◽  
Atomic Absorption Spectrophotometry ◽  
Absorption Method ◽  
Atomic Absorption Method ◽  
Absorption Spectrophotometry ◽  
Minor Nutrients

Abstract The atomic absorption method studied last year was re-examined and extended to include calcium and sodium. The procedures were submitted to 16 collaborators for determination of Ca, Cu, Fe, Mg, Mn, Na, and Zn. Results for Ca and Na were discouraging; further study is recommended.

Comparison of Methods for Determining Biuret in Urea

1979 ◽  
Vol 62 (1) ◽  
pp. 153-159
Author(s):  
Luis F Corominas ◽  
Victor M Boy ◽  
Manuel Guijosa
Keyword(s):  
Atomic Absorption ◽  
Spectrophotometric Determination ◽  
Atomic Absorption Spectrophotometry ◽  
International Organization ◽  
Comparison Of Methods ◽  
Definite Advantage ◽  
Absorption Spectrophotometry ◽  
Alternative Procedures ◽  
Aoac Method

Abstract The official first action AOAC method for the spectrophotometric determination of biuret in urea, 2.072—2.074, was compared with official first action AOAC method 2.C01-2.C03 (atomic absorption spectrophotometry), 2 simplified versions of 2.072-2.074, and modified versions of 2 alternative procedures of the International Organization for Standardization. Three synthetic urea samples (0.3, 1.4, and 3.0% biuret) and 1 commercial urea sample (1.0% biuret) were analyzed. The methods proved to be equivalent and none showed a definite advantage over 2.072-2.074. The purification of biuret and the interference by ammonia are also discussed.

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