Determination of Iron in Alcoholic Beverages

1970 ◽  
Vol 53 (1) ◽  
pp. 12-16
Author(s):  
M K Meredith ◽  
Sidney Baldwin ◽  
A A Andreasen
Keyword(s):  
Atomic Absorption ◽  
Collaborative Study ◽  
Colorimetric Method ◽  
Atomic Absorption Spectrophotometry ◽  
Alcoholic Beverages ◽  
Wet Oxidation ◽  
Special Equipment ◽  
Oxidation Method ◽  
Trained Personnel

Abstract Results are presented for a collaborative study on the determination of ppm iron in alcoholic beverages, except beer, by the following methods: atomic absorption spectrophotometry, direct colorimetry using 2,4,6-tripyridyl-s-triazine (TPTZ) for alcoholic beverages other than brandy, and wet oxidation using sodium hypochlorite and hydrogen peroxide followed by color development with TPTZ for brandy only. When available, atomic absorption is the method of choice because of its speed and accuracy. The colorimetric method eliminates ashing, is relatively rapid, and does not require special equipment or highly trained personnel; however, it does not give accurate results for brandy. The wet oxidation method is satisfactory for brandy but requires more time, proper ventilation, and trained personnel. Results by these methods are accurate for routine determinations and it is recommended that the first two methods be adopted as official first action for the alcoholic products specified. Study on the wet oxidation method for products containing chelating agents and/or “complexed iron” should be continued.

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.

Collaborative Study Using Atomic Absorption Spectrophotometry for the Determination of Copper in Alcoholic Products

1967 ◽  
Vol 50 (2) ◽  
pp. 338-339
Author(s):  
Duane H Strunk ◽  
A A Andreasen
Keyword(s):  
Atomic Absorption ◽  
Spectrophotometric Method ◽  
Collaborative Study ◽  
Atomic Absorption Spectrophotometry ◽  
Good Precision ◽  
Absorption Method ◽  
Standard Curve ◽  
Absorption Spectrophotometry ◽  
Determination Of Copper

Abstract A collaborative study was conducted on the 'atomic absorption spectrophotometric method for measuring the concentration of copper in alcoholic products. In this method, the samples are aspirated directly into the burner of the instrument, and the absorhance values are converted to ppm copper by reference to a standard curve. Data show good precision and are comparable to those obtained by the ZDBT method. It is recommended that the atomic absorption method be adopted as official, first action.

Atomic Absorption Spectrophotometric Method for Determination of Water-Soluble Copper in Water-Insoluble Copper Fungicides: CIPAC Collaborative Study. Comparison with Bathocuproine Method

1981 ◽  
Vol 64 (1) ◽  
pp. 75-78
Author(s):  
F Sánchez Rasero ◽  
◽  
P G Balayannis ◽  
H P Beyers ◽  
E Celma ◽  
...  
Keyword(s):  
Atomic Absorption ◽  
Collaborative Study ◽  
The United States ◽  
Atomic Absorption Spectrophotometry ◽  
Water Soluble ◽  
Absorption Spectrophotometry ◽  
Aas Method ◽  
Standard Deviations ◽  
The Difference

Abstract An atomic absorption spectrophotometric (AAS) method was collaboratively studied by 8 laboratories from Africa, the United States, Australia, and Europe. The samples were dispersed in deionized water. After centrifuging and filtering, the water-soluble copper in the filtrate was acidified and measured by atomic absorption spectrophotometry, in an airacetylene flame, at 324.7 nm. The results from 7 laboratories were satisfactory and no unfavorable comments were received. Repeatability standard deviations ranged from 0.005 to 0.023, and reproducibility standard deviations ranged from 0.012 to 0.062. When compared with the bathocuproine method, the difference in bias between both methods is not significant. They were both adopted as full CIPAC methods, with the bathocuproine method as the referee method. Both methods have been adopted official first action.

Atomic Absorption Spectrophotometric Method for Determination of Polydimethylsiloxane Residues in Pineapple Juice: Collaborative Study

1990 ◽  
Vol 73 (5) ◽  
pp. 721-723
Author(s):  
Robert D Parker
Keyword(s):  
Nitrous Oxide ◽  
Atomic Absorption ◽  
Spectrophotometric Method ◽  
Collaborative Study ◽  
Atomic Absorption Spectrophotometry ◽  
Pineapple Juice ◽  
Absorption Spectrophotometry ◽  
Relative Standard ◽  
Standard Deviations

Abstract An atomic absorption spectrophotometric method for determination of polydimethylsiloxane (PDMS) residues In pineapple juice was collaboratively studied by 9 laboratories. PDMS residues are extracted from pineapple Juice with 4- methyl-2-pentanone and the extracted silicone Is measured by atomic absorption spectrophotometry using a nitrous oxide/ acetylene flame. Collaborators analyzed 5 samples Including 1 blind duplicate. Reproducibility relative standard deviations (RSDR) were 13.1% at 31 ppm, 6.9% at 18 ppm, 14.8% at 7.9 ppm, and 16.1 % at 4.9 ppm PDMS. The method has been approved Interim official first action by AOAC.

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 Spectrophotometric Determination of Calcium and Magnesium and Colorimetric Determination of Phosphorus in Cheese: Collaborative Study

1991 ◽  
Vol 74 (1) ◽  
pp. 27-31 ◽  
Author(s):  
Roger M Pollman
Keyword(s):  
Atomic Absorption ◽  
Collaborative Study ◽  
Atomic Absorption Spectrophotometry ◽  
Colorimetric Determination ◽  
The Third ◽  
Number Of Factors ◽  
Relative Standard ◽  
Calcium Phosphorus ◽  
Calcium And Magnesium

Abstract The determination of calcium, phosphorus, and magnesium In cheese was collaboratively studied. The sample is dried and ashed and the residue is dissolved In an acidified aqueous solution. Calcium and magnesium are determined by atomic absorption spectrophotometry and phosphorus Is determined by colorlmetry. The study was repeated 3 times because of high within- and between-laboratory relative standard deviations (RSDr and RSDR, respectively). Poor precision In the first 2 studies was caused by a number of factors, Including use of contaminated glassware, Improperly maintained Instruments, and Impure reagents as standards. In each study, 5 varieties of cheese were distributed as 10 blind duplicate samples along with a practice sample. Thirteen laboratories participated in the third study, which was generally problem-free. The range of results and the average RSDr and RSDR found In the cheeses were: calcium, 608- 1107 mg/100 g, 1.5%, 2.6%; magnesium, 23.9-50.6 mg/ 100 g, 2.8%, 3.8%; phosphorus, 444-695 mg/100 g, 1.2%, 1.6%. The method has been adopted official first action by AOAC.

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.

Collaborative Study of the Determination of Boric Acid in Foods by Atomic Absorption Spectrophotometry

1972 ◽  
Vol 55 (4) ◽  
pp. 890-891
Author(s):  
Walter Holak
Keyword(s):  
Nitrous Oxide ◽  
Boric Acid ◽  
Atomic Absorption ◽  
Methyl Isobutyl Ketone ◽  
Collaborative Study ◽  
Atomic Absorption Spectrophotometry ◽  
Methyl Isobutyl ◽  
Isobutyl Ketone ◽  
Absorption Spectrophotometry

Caviar and dried apricots containing a known amount of added boric acid were subjected to a collaborative study. The samples were digested with sulfuric-nitric acid under reflux; the boron was then complexed with 2-ethyl-1,3-hexanediol and extracted into methyl isobutyl ketone. Boron in the organic phase was determined by atomic absorption, using a nitrous oxide-acetylene flame. The recoveries were satisfactory: 103, 95, and 93% for 300, 1000, and 1600 μg boron/g apricots and 95, 90, and 92% for the corresponding caviar samples. The method has been adopted as official first action.

Liquid Chromatographic-Atomic Absorption Spectrophotometric Method for Determination of Methyl Mercury in Seafood: Collaborative Study

1989 ◽  
Vol 72 (6) ◽  
pp. 926-930
Author(s):  
Walter Holak
Keyword(s):  
Atomic Absorption ◽  
Methyl Mercury ◽  
Collaborative Study ◽  
Sodium Thiosulfate ◽  
Mercury Vapor ◽  
Atomic Absorption Spectrophotometry ◽  
Acetate Solution ◽  
Relative Standard ◽  
Liquid Chromatographic

Abstract A previously developed method that uses a simplified sample preparation procedure and atomic absorption detection of liquid chromatographic eluates for the determination of methyl mercury in seafood has been collaboratively studied. The unique feature of the method involves the use of a specially designed interface for the generation of mercury vapor. Methyl mercury is isolated from the blended sample by chloroform elution from a diatomaceous earth-hydrochloric acid column. The organomercury compound is then extracted into a small volume of 0.01M sodium thiosulfate solution. An aliquot of this solution is injected onto a Zorbax ODS column and eluted with methanol-ammonium acetate solution (3 + 2), pH 5.7, containing 0.01% mercaptoethanol. Mercury is detected by flameless atomic absorption spectrophotometry using the interface. The samples analyzed in the study were unspiked swordfish, unspiked and spiked lobster, and unspiked and spiked tuna. The spiked samples contained methyl mercury both above and below the U.S. Food and Drug Administration guideline level of 1 fig Hg/g. Reproducibility relative standard deviations ranged from 10.5% at 1 fig Hg/g to 18.2% at about 0.1 fig Hg/g. Accuracy, measured by comparison to reference values obtained by the Associate Referee, ranged from 94.4 to 99.6%. The method has been adopted official first action.

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.

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