Collaborative Study of a Colorimetric Determination of Nitrate in Tobacco

1969 ◽  
Vol 52 (4) ◽  
pp. 756-759
Author(s):  
C James Rosene
Keyword(s):  
Sulfuric Acid ◽  
Standard Deviation ◽  
Systematic Error ◽  
Collaborative Study ◽  
Colorimetric Method ◽  
Water Soluble ◽  
Colorimetric Determination ◽  
Error Standard Deviation

Abstract A colorimetric method for determining water-soluble nitrate in tobacco was studied by 14 laboratories on eight Burley and two cigar filler tobacco samples with nitrate levels of 0.5–2.4%. In the method, ground tobacco is extracted with water and filtered, and an aliquot is then treated with 2,4-xylenol in sulfuric acid; then the resulting 6-nitro-2,4-xylenol is removed by distillation and measured spectrophotometrically at 450 µm. Results show that, althoughthe precision standard deviation among laboratories is generally acceptable, the systematic error standard deviation is unacceptably high. This study will be continued.

Collaborative Study of a Fluorometric Method for Determining Selenium in Foods

1974 ◽  
Vol 57 (2) ◽  
pp. 373-378 ◽  
Author(s):  
Milan Ihnat
Keyword(s):  
Standard Deviation ◽  
Systematic Error ◽  
Collaborative Study ◽  
Bovine Liver ◽  
Standard Reference Materials ◽  
Fluorometric Method ◽  
Naturally Occurring ◽  
Coefficients Of Variation ◽  
Error Standard Deviation

Abstract A fluorometric method for the determination of selenium in foods reported previously was studied collaboratively. Nineteen laboratories reported analytical results on 10 samples representative of vegetables, cereal, dairy products, meat, and fish, and containing naturally occurring selenium. For the 5 pairs of samples, the coefficients of variation based on precision standard deviation were 2 5 . 9% at 16 ng selenium, 15.8% at 98 ng, 8.5% at 233 ng, 6.1% at 379 ng, and 4.1 % at 427 ng. The corresponding coefficients of variation computed from overall standard deviations were 65.3, 17.5, 8.9, 8.1, and 5.6%. Systematic error was significant for 2 pairs (F-test, p = 0.01), but not for the remaining 3 (p = 0.05). The ratio of the systematic error standard deviation to the precision standard deviation varied from 0.21 to 1.64. Analyses of 2 NBS standard reference materials, orchard leaves (75 ng selenium) and bovine liver (208 ng selenium), yielded results higher by 16 and 10%, respectively. The precision and accuracy of the collaborative procedure were deemed acceptable and the method has been adopted as official first action.

Colorimetric Determination of Hydroxyproline as Measure of Collagen Content in Meat and Meat Products: NMKL Collaborative Study

1990 ◽  
Vol 73 (1) ◽  
pp. 54-57 ◽  
Author(s):  
Kurt Kolar
Keyword(s):  
Collaborative Study ◽  
Colorimetric Method ◽  
Meat Products ◽  
Acid Oxidation ◽  
Colorimetric Determination ◽  
Mean Values ◽  
Collaborative Studies ◽  
Freeze Dried ◽  
Analytical Result

Abstract A colorimetric method for the determination of hydroxyproline as a measure of collagen in meat and meat products has been collaboratively studied in 18 laboratories. The method includes hydrolysis with sulfuric acid, oxidation with chloramine- T, and formation of a reddish purple complex with 4- dimethylaminobenzaldehyde. Five frozen and 3 freeze-dried samples were tested, ranging in content from 0.11 to 0.88% and from 0.39 to 4.0% hydroxyproline, respectively. The mean values of 2 identical samples were 0.245 and 0.251 %. The average recovery from a spiked sample was 96.1 %. The hydroxyproline content of a known sample (a mixture of 2 samples in the ratio 5:2) was calculated to 1.42%, which agrees well with the analytical result, 1.40%. In comparison with other collaborative studies, based on the ISO analytical method, the repeatability and reproducibility of this method agree well with the other results. This method was accepted as an official NMKL method by all national Committees, and has been adopted official first action by AOAC as an NMKLAOAC method.

Collaborative Study Using a ZDBT Colorimetric Method for the Determination of Copper in Alcoholic Products

1967 ◽  
Vol 50 (2) ◽  
pp. 334-338
Author(s):  
Duane H Strunk ◽  
A A Andreasen
Keyword(s):  
Sulfuric Acid ◽  
Carbon Tetrachloride ◽  
Collaborative Study ◽  
Colorimetric Method ◽  
Good Precision ◽  
Determination Of Copper

Abstract Results are given on a collaborative study in which a zinc dibenzyldithiocarbamate (ZDBT) colorimetric method is used to measure copper in alcoholic products such as high wine, spirits, gin, whisky, brandy, rum, and wine. In this method, the sample is made ca 0.SN with sulfuric acid, and carbon tetrachloride containing 0.2% ZDBT is added. The colored copper-ZDBT complex is extracted in the carbon tetrachloride and measured at 438 mμ against a similar carbon tetrachloride extract of a blank. Data show good precision, and it is recommended that the ZDBT method be adopted as official, first action.

Sulfuric Acid/Hydrogen Peroxide Digestion and Colorimetric Determination of Phosphorus in Meat and Meat Products: Collaborative Study

1991 ◽  
Vol 74 (1) ◽  
pp. 22-26 ◽  
Author(s):  
David K Christians ◽  
Thomas G Aspelund ◽  
Scott V Brayton ◽  
Larry L Roberts
Keyword(s):  
Hydrogen Peroxide ◽  
Sulfuric Acid ◽  
Collaborative Study ◽  
Meat Products ◽  
Colorimetric Determination ◽  
Pork Sausage ◽  
Relative Standard ◽  
Significant Difference ◽  
Standard Deviations

Abstract Seven laboratories participated In a collaborative study of a method for determination of phosphorus in meat and meat products. Samples are digested In sulfuric acid and hydrogen peroxide; digestion Is complete In approximately 10 mln. Phosphorus Is determined by colorimetric analysis of a dilute aliquot of the sample digest. The collaborators analyzed 3 sets of blind duplicate samples from each of 6 classes of meat (U.S. Department of Agriculture classifications): smoked ham, water-added ham, canned ham, pork sausage, cooked sausage, and hamburger. The calibration curve was linear over the range of standard solutions prepared (phosphorus levels from 0.05 to 1.00%); levels in the collaborative study samples ranged from 0.10 to 0.30%. Standard deviations for repeatability (sr) and reproducibility (sR) ranged from 0.004 to 0.012 and 0.007 to 0.014, respectively. Corresponding relative standard deviations (RSDr and RSDR, respectively) ranged from 1.70 to 7.28% and 3.50 to 9.87%. Six laboratories analyzed samples by both the proposed method and AOAC method 24.016 (14th Ed.). One laboratory reported results by the proposed method only. Statistical evaluations Indicated no significant difference between the 2 methods. The method has been adopted official first action by AOAC.

Collaborative Study of Betaine in Orange Juice

1970 ◽  
Vol 53 (3) ◽  
pp. 568-571
Author(s):  
Grayson R Rogers
Keyword(s):  
Amino Acids ◽  
Standard Deviation ◽  
Ion Exchange ◽  
Systematic Error ◽  
Orange Juice ◽  
Collaborative Study ◽  
Colorimetric Method ◽  
Actual Data ◽  
Random Errors ◽  
Water Solutions

Abstract An ion exchange-colorimetric method for determining betaine in orange juice was studied by 11 collaborators on 4 orange juice samples and 2 synthetic water solutions consisting of sucrose, dextrose, and various amino acids found in orange juice. Average recoveries in the collaborative study were 96.7 and 95.9%. Results show that the precision standard deviation among laboratories is generally acceptable. The distribution of the actual data is greater than normally expected, but random errors appear to be responsible since no significant systematic error can be detected in the data. The method is recommended for adoption as official first action.

Collaborative Study of a Method for Sodium Lauryl Sulfate in Egg Whites

1968 ◽  
Vol 51 (3) ◽  
pp. 540-543
Author(s):  
John Wiskerchen
Keyword(s):  
Sulfuric Acid ◽  
Quantitative Determination ◽  
Sodium Lauryl Sulfate ◽  
Collaborative Study ◽  
Colorimetric Method ◽  
Egg White ◽  
Mean Deviation ◽  
Lauryl Sulfate ◽  
Benzethonium Chloride

Abstract A colorimetric method for the quantitative determination of sodium lauryl sulfate in liquid, frozen, and powdered egg white was studied by eight collaborators. Determinations were made on flake and powdered egg white at levels of 0.05, 0.1, and 0.2% (w/w) and on liquid egg white at levels of 0.006, 0.0125, and 0.0250% (w/w) sodium lauryl sulfate. The egg white is dissolved in water, and the protein is precipitated with ethanol and removed by filtration. An aliquot of the filtrate is evaporated to dryness, and the residue is dissolved in water and acidified with sulfuric acid. The sodium lauryl sulfate is complexed with Azure A, extracted into chloroform, and determined spectrophotometrically at 637 mμ. A blank determination is made on another aliquot of the filtrate by complexing the sodium lauryl sulfate with benzethonium chloride. This is a stable colorless complex. Average recoveries in the collaborative study were 98—102% with a mean deviation of 2.8—5.4%. It is recommended that the method be adopted as official, first action.

Colorimetric Determination of Dillapiole in Wheat

1979 ◽  
Vol 62 (1) ◽  
pp. 203-204
Author(s):  
Swadesh K Handa
Keyword(s):  
Sulfuric Acid ◽  
Colorimetric Method ◽  
Chromotropic Acid ◽  
Colorimetric Determination ◽  
Wheat Grain ◽  
Maximum Absorbance

Abstract A rapid colorimetric method has been developed for determining residues of dillapiole (3,4-methylenedioxy-5,6-dimethoxy allyl benzene) in wheat grain. Dillapiole is reacted with sulfuric acid to liberate formaldehyde which reacts with chromotropic acid to yield a pink compound with maximum absorbance at 575 nm. The method can detect 1—15 μg residue /ml.

Collaborative Study of the Thermistor Cryoscopic Method for the Determination of the Freezing Point Value of Milk

1968 ◽  
Vol 51 (4) ◽  
pp. 816-821
Author(s):  
R W Henningson
Keyword(s):  
Standard Deviation ◽  
Systematic Error ◽  
Freezing Point ◽  
Collaborative Study

Abstract Data from 19 collaborators for two sample pairs were used to estimate the precision and systematic error of the thermistor cryoscopic method for determining the freezing point value of milk. Precision was greater for the milks (0.0015°) than for the standards (0.004°). The systematic error was estimated to be 0.0033°. The standard deviation for interlaboratory individual determinations was estimated to be 0.0049°.

Colorimetric Determination of 3-Amino-l,2,4-Triazole in Grain or Meal

1982 ◽  
Vol 65 (1) ◽  
pp. 24-27
Author(s):  
Michel Galoux ◽  
Jean-C Van Damme ◽  
Albert Bernes
Keyword(s):  
Sulfuric Acid ◽  
Limit Of Detection ◽  
Colorimetric Method ◽  
Colorimetric Determination ◽  
Colored Complex ◽  
Adsorption Desorption

Abstract This colorimetric method for the determination of 3-amino-l,2,4-triazole in grain or meal is a modification of the Storherr and Burke method. The herbicide is extracted from grain with methanol, and purified by adsorption-desorption on resin. The extract is cleaned by digestion with sulfuric acid and clarified with charcoal. The colored complex formed by coupling with N-(1-naphthyl)ethylenediammonium dichloride is measured spectrophotometrically at 455 nm. The limit of detection is 0.05 ppm.

Collaborative Study of the Colorimetric Determination of Nitrate and Nitrite in Cheese

1976 ◽  
Vol 59 (2) ◽  
pp. 284-288
Author(s):  
James E Hamilton
Keyword(s):  
Azo Dye ◽  
Collaborative Study ◽  
Colorimetric Method ◽  
Sulfanilic Acid ◽  
Zinc Hydroxide ◽  
Colorimetric Determination ◽  
Standard Curve ◽  
Nitrite Nitrate ◽  
Nitrate And Nitrite

Abstract A quantitative colorimetric method for the determination of nitrate and nitrite in cheese has been subjected to collaborative study. The method includes clarification of an aqueous extract of cheese with zinc hydroxide, reduction of nitrate to nitrite via a spongy cadmium column (the nitrite originally present is unaltered), diazotization of sulfanilic acid with the nitrite, and coupling with 1-naphthylamine hydrochloride to form a pink azo dye whose absorbance is measured at 522 nm. The spectrophotometric responses are compared to a standard curve. In samples containing both nitrate and nitrite, nitrate is determined by difference. A standard deviation of 5.5 was obtained (5 of 6 collaborators) when a cheese sample spiked with 276 ppm sodium nitrate was analyzed by the method. The method has been adopted as official first action.

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