Atomic Absorption Spectrophotometric Determination of Mercury in Mercury≃Containing Drugs: Collaborative Study

1983 ◽  
Vol 66 (5) ◽  
pp. 1203-1206
Author(s):  
Walter Holak ◽  
◽  
R Baltz ◽  
L Elliott ◽  
E McGary ◽  
...  
Keyword(s):  
Atomic Absorption ◽  
Spectrophotometric Determination ◽  
Collaborative Study ◽  
Ophthalmic Solution ◽  
Mean Value ◽  
Antiseptic Solution ◽  
Aas Method ◽  
Low Levels

Abstract An atomic absorption spectrophotometric (AAS) method applicable to a wide variety of mercurycontaining drugs has been developed and subjected to a collaborative study. Samples were digested with a water-HCl-HN03 (4 + 3 + 1) mixture, and the mercury was determined in solution by AAS. High levels of mercury were measured with a conventional air-acetylene flame, whereas low levels were measured by the flameless technique. Each of 7 collaborators received duplicate synthetic samples of a tincture, an ophthalmic solution, and an antiseptic solution, and duplicate commercial samples of an ointment and an injectable. The overall mean value found by collaborators for mercury in these samples was 100.13%. The corresponding overall repeatability SD (CV, %) and reproducibility SD (CV, %) values were 2.18 (2.18) and 3.38 (3.38), respectively. The proposed AAS method has been adopted 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 Determination of Chelated Iron in Iron Chelate Concentrates: Collaborative Study

1983 ◽  
Vol 66 (4) ◽  
pp. 952-955
Author(s):  
James R Silkey ◽  
◽  
S G Angell ◽  
K Bartunek ◽  
L W Clark ◽  
...  
Keyword(s):  
Atomic Absorption ◽  
Collaborative Study ◽  
Ferric Hydroxide ◽  
Disodium Edta ◽  
Iron Chelate ◽  
Iron Citrate ◽  
Coefficients Of Variation ◽  
Chelated Iron ◽  
Aas Method

Abstract An atomic absorption Spectrophotometric (AAS) method for determining chelated iron in iron chelate concentrates was collaboratively studied by 13 laboratories. Nonchelated iron was selectively precipitated as ferric hydroxide from an aqueous solution of the sample by adjusting to pH 8.5 with sodium hydroxide. A filtered portion of the sample solution was diluted with 0.5N HC1, and the iron was determined by AAS using standards containing disodium EDTA. Six pairs of iron chelate materials (12 samples) were analyzed and the average coefficients of variation were iron EDTA 3.52%, iron HEDTA 4.16%, iron DTPA 3.55%, iron EDDHA 3.52%, iron citrate 2.86%, and iron DPS 8.47%. The method has been adopted official first action.

Graphite Furnace Atomic Absorption Spectrophotometric Determination of 4-Hydroxy-3-Nitrobenzene Arsonic Acid in Finished Animal Feed: Collaborative Study

1986 ◽  
Vol 69 (5) ◽  
pp. 838-843
Author(s):  
Glenn M George ◽  
Larry J Fra ◽  
◽  
C F Aten ◽  
J Bestianich ◽  
...  
Keyword(s):  
Atomic Absorption ◽  
Animal Feed ◽  
Graphite Furnace ◽  
Collaborative Study ◽  
Method Performance ◽  
Relative Standard ◽  
Graphite Furnace Atomic Absorption ◽  
Aas Method ◽  
Arsonic Acid

Abstract Eight laboratories participated in a collaborative study of an atomic absorption spectrophotometric (AAS) method for determination of 4- hydroxy-3-nitrobenzene arsonic acid (roxarsone), which is administered in animal feed at levels of 25-50 ppm as a growth stimulant. The drug is extracted from feed by using aqueous 1% ammonium carbonate solution. Undissolved feed particles are allowed to settle, and then a diluted aliquot of the feed extract is analyzed for total arsenic by AAS using a graphite furnace for sample atomization. Collaborators performed single analyses on 18 samples which were randomly numbered blind duplicate pairs of a complete poultry ration fortified with roxarsone at concentrations from 22.5 to 55.0 ppm. Statistical evaluation of the collaborative data showed satisfactory method performance. Overall mean recovery of roxarsone was 100.4% and the overall relative standard deviation was 6.2%. The method has been adopted official first action.

Determination of Biuret in Urea and Mixed Fertilizers by Cupric Ion Selective Electrode

1986 ◽  
Vol 69 (1) ◽  
pp. 119-122
Author(s):  
Luis F Corominas ◽  
Roberto A Navarro ◽  
Pedro Rojas ◽  
José L Cruz
Keyword(s):  
Atomic Absorption ◽  
Copper Complex ◽  
Confidence Level ◽  
Collaborative Study ◽  
Ion Selective Electrode ◽  
Selective Electrode ◽  
Cupric Ion ◽  
Excess Copper ◽  
Aas Method

Abstract A method for determining biuret in urea and mixed fertilizers by using a cupric ion selective electrode (CISE) has been developed to take advantage of the simplicity of the apparatus. The method is based on the same principle as the atomic absorption spectrophotometric (AAS) method, 2.091-2.093: formation of a biuret-copper complex, elimination of excess copper, and determination of complexed copper. However, some changes were needed to eliminate starch and alcohol interferences. The method was tested for ruggedness and then compared with the AAS method for 4 fertilizer samples. Averages and variances were equivalent at the 99% confidence level according to t- and F-tests. A collaborative study is recommended to compare behavior of both methods in different laboratories.

Spectrophotometric Determination of Raceophenidol in Feed at Very Low Levels

1968 ◽  
Vol 51 (4) ◽  
pp. 752-755
Author(s):  
Edward L Pratt ◽  
Morris E Auerbach
Keyword(s):  
Spectrophotometric Determination ◽  
Growth Promotion ◽  
Ultraviolet Spectrum ◽  
Average Value ◽  
Collaborative Studies ◽  
Low Levels ◽  
Concentration Levels

Abstract Raceophenidol in feed at concentration levels intended for growth promotion of poultry can be estimated by a curvature inversion measurement related to the ultraviolet spectrum of derived p-methylsulfonylbenzaldehyde. The drug can be accurately measured at the 0.0005% level. Collaborative studies on the method showed an average value of 94 ± 10% of claim. The method is recommended for adoption as official, first action.

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 of the Spectrophotometric Determination of Procainamide Hydrochloride

1976 ◽  
Vol 59 (4) ◽  
pp. 807-810
Author(s):  
Jeffrey C Hamm
Keyword(s):  
Sodium Hydroxide ◽  
Acid Medium ◽  
Spectrophotometric Determination ◽  
Spectrophotometric Method ◽  
Collaborative Study ◽  
Dosage Forms ◽  
Standard Deviations

Abstract The USP analysis for procainamide HCl is titrimetric and relatively nonspecific, capsule and tablet dyes may interfere, and the method is not applicable to coated tablets. In the spectrophotofluorometric method the sample deteriorates when exposed to a xenon source. In the ultraviolet spectrophotometric method reported here, the sample is dispersed in acid medium, possible interferences are extracted in chloroform, base is added, procainamide is extracted in chloroform, the residue is dissolved in sodium hydroxide, and the compound is measured by absorption at 272 nm and comparison with a standard. Recoveries of standards added to capsule, tablet, and injection composites ranged from 99.3 to 102%. Twelve collaborators reported duplicate assay results for all 3 dosage forms with per cent standard deviations for 5 samples ranging from 1.01 to 1.27%. The method has been adopted as official first action.

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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