bluuebunny/crossref_metadata_2025_split huggingface dataset:
Determination of Several Chlorinated Pesticides by the AOAC Multiresidue Method with Additional Quantitation of Perthane after Dehydrochlorination: Collaborative Study
Authors: Krause Richard T 
Published: February 2020

Abstract
The AOAC multiresidue method for chlorinated pesticides, 29.001–29.017, was studied collaboratively by 7 laboratories. Perthane, heptachlor epoxide, mirex, and dieldrin were determined in apple and cauliflower samples fortified at 2 levels, and Perthane was determined in butterfat samples fortified at 2 levels. Perthane was quantitatively measured before and after a simplified dehydrochlorination procedure. Average recoveries and coefficients of variations for pesticides in the apple samples for both levels were: Perthane 100±10%, heptachlor epoxide 102±14%, mirex 96±9%, dieldrin 101±14%, and Perthane (after dehydrochlorination and recalculation to the parent compound) 100±9%. Average recoveries and coefficients of variation for pesticides in the cauliflower samples for both levels were: Perthane 105±9%, heptachlor epoxide 103± 15%, mirex 103±7%, dieldrin 98±11%, and Perthane (after dehydrochlorination and recalculation) 100±10%. The average recovery for both levels of Perthane (after dehydrochlorination and recalculation) in the butterfat samples was 91±10%. For a spinach sample with field-incurred residues the collaborators found an average of 4.47 ppm Perthane before dehydrochlorination and 5.09 ppm Perthane as the olefin after dehydrochlorination. In most instances, the identities of all the residues were confirmed by TLC. The dehydrochlorination technique has been adopted as official first action.
Control of Authenticity of Fruit Juices by Isotopic Analysis
Authors: Bricout Jacques 
Published: February 2020

Abstract
In order to differentiate a natural fruit juice from a dilute concentrate, we have investigated the isotopic composition of their water. We have chosen the stable isotopes deuterium and 18O. The water of orange juices is strongly enriched in heavy isotopes, as compared to rain water. This enrichment is much lower for French apple juices and seems to be due to evapotranspiration. The relationship between deuterium and 18O observed for meteoric water is modified in the fruits. If a fruit juice is concentrated and then rediluted with natural water, the isotopic composition of its water would be very similar to the original deuterium and 18O content of the dilution water. Isotopic analysis allows a very confident distinction between natural fruit juices and reconstituted juices.
Use of Heat to Saponify Xanthophyll Esters and Speed Analysis for Carotenoids in Feed Materials: Collaborative Study
Authors: Quackenbush Forrest W 
Published: February 2020

Abstract
Twelve collaborators analyzed 4 pairs of samples to compare a 20 min hot (56°C) saponification technique with the overnight extraction technique at room temperature in the official first action method for analysis of carotenoids in feed materials, 39.018–39.023, with a view to (a) make the method applicable to products which contain xanthophyll esters and (b) speed up the analysis. In general, the collaborators were in good agreement, with saponification of esters essentially complete after the 20 min heating of samples that contained marigold meal. While the sum of extracted pigments from corn gluten and alfalfa meal tended to be slightly higher with the longer (overnight) contact with the solvent than with the hot extraction, the differences were not statistically significant. Significant differences between hot and cold treatments were absent also in alfalfa pigment fractions, but hot saponification significantly lowered monohydroxy pigments and increased dihydroxy pigments in extracts from corn gluten. The results showed good precision with either extraction technique. The method, modified to include hot saponification as an alternative step, is now applicable to all dried feed materials, including those which contain xanthophyll esters (e.g., marigold meal); the modification has been incorporated into the official first action method, 39.018–39.023.
Negative Finding of 2,3,7,8-Tetrachlorodibenzo-p-dioxin in Cooked Fat Containing Actual and Fortified Residues of Ronnel and/or 2,4,5-Trichlorophenol
Authors: Watts Randall R , Storherr Robert W 
Published: February 2020

Abstract
Beef fat containing residues of ronnel and its metabolite 2,4,5-trichlorophenol at 46.0 and 2.8 ppm, respectively, was examined before and after cooking for presence of 2,3,7,8-tetra-chlorodibenzo-p-dioxin. Fat samples fortified at 2000 ppm with 2,4,5-trichlorophenol or its sodium salt were cooked at 500°F for periods of 6 to 22 hr. No tetra-dioxin was found in any of the samples, using a method with a sensitivity limit of 0.05 ppm.
Rapid Detection of Aflatoxin Contamination in Agricultural Products
Authors: Pons Walter A , Cucullu Alva F , Franz Anthony O , Lee Louise S , Goldblatt Leo A 
Published: February 2020

Abstract
A rapid and simple method, originally designed for detecting aflatoxin contamination in cottonseed products within 15 min, was modified for application to a variety of agricultural products. The modified method involves rapid blender extraction of the sample with aqueous acetonitrile, treatment of an aliquot of the filtrate with lead acetate solution to remove interfering pigments, and rapid partition of aflatoxins in the treated extract into benzene to effect an 8-fold concentration of the aflatoxins. A portion of the benzene extract is adsorbed by capillary attraction onto the bottom of a small column (4 mm × 20 cm) filled with zones of acidic alumina and silica gel and the column is allowed to develop 5 min in chloroform-acetonitrile-2-propanol (93 + 5+2). Aflatoxin contamination is characterized by a sharp blue fluorescent band about 1 cm above the alumina zone when the developed column is viewed under longwave UV light. The total analysis time is about 20 min. The method was successfully applied to the oilseeds cottonseed, soybean, peanut, flax seed, and sunflower seed; to the grains corn, wheat, oats, barley, sorghum, rye, and rice; and to the tree nuts pistachios, almonds, walnuts, brazil nuts, pecans, and filberts. As little as 10 μg aflatoxin/kg can be detected, and approximate contamination levels can be placed in one of 5 categories, based on the observed intensity of the fluorescent aflatoxin band.
Microbiological Assay of Spectinomycin in Feed: Collaborative Study
Authors: Neff A William , Barbiers Arthur R , Miller Curtis C , Stahl Gerald L 
Published: February 2020

Abstract
A microbiological assay for the determination of spectinomycin in swine feeds has been developed and tested collaboratively in 9 laboratories. The design of the study involved 4 feed types and 4 levels of fortification (18, 20, 50, 55 g/ton) which represented the limits of permitted antibiotic usage. Statistical evaluation of the recovery data indicated that no real difference existed between feed types. Recoveries tended to be lower from lower content feeds than from the higher content feeds. The greatest source of variability came from the laboratory-to-laboratory component, followed by the random effects due to sampling, mixing, and assay techniques. The overall recovery was 96.4±13.4%.
Collaborative Study of a Method for the Atomic Absorption Spectrophotometric and Polarographic Determination of Cadmium in Food
Authors: Gajan Raymond J , Gould John H , Watts James O , Fiorino John A 
Published: February 2020

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.
Extraction and Cleanup for Determination of Polychlorinated Biphenyls in Paper and Paperboard
Authors: Young Susan J V , Alder Charles Finsterw , Burke Jerry A 
Published: February 2020

Abstract
A procedure is described for the determination of polychlorinated biphenyls (PCBs) in paper and paperboard. PCBs are extracted from the paper sample by reflux with alcoholic KOH. Column chromatography on Florisil is used for cleanup, if needed. Compounds are determined by GLC with electron capture detection, using conditions previously devised for organochlorine pesticides. An exhaustive extraction utilizing sulfuric acid was developed in order to obtain comparative data on extraction effectiveness. Recoveries of Aroclors 1242 and 1254 from fortified paper samples averaged 95.5 and 96.8% with the alcoholic KOH reflux and sulfuric acid digestion extractions, respectively. Aroclor 1242 determined after alcoholic KOH extraction of paperboard was 96% of the amount found after sulfuric acid digestion of comparable samples. Aroclor 1242 had been incorporated into the paperboard during manufacture.
Infrared Studies of Chlorinated Dibenzo-p-dioxins and Structurally Related Compounds
Authors: Chen Jo-Yun T 
Published: February 2020

Abstract
Reference infrared spectra of 24 chlorinated dibenzo-p-dioxins (DPD) and structurally related compounds are presented. These reference spectra are recorded using micro quantities of synthesized compounds in order to obtain spectra like those expected from chlorinated DPD residue isolates. The observed characteristic frequencies are tabulated in correlation tables. Their significance is interpreted in terms of the substituents and electronic effects. The positions of various absorption bands depend on the total number and positions of the chlorine substituents. The positions of the absorption bands indicate relative bond strengths.
Exhaustive Chlorination as a Technique in the Analysis of Aromatic Hydrocarbons
Authors: Hutzinger Otto , Jamieson W David J , Safe Stephen S , Zitko Vladimir Z 
Published: February 2020

Abstract
Perchlorination reactions of aromatic compounds have been further investigated. The preparation and properties of decachlorodiphenyl ether and the isomeric o-, m-, and p-tetradecaehloroterphenyls are described. Anthracene, as an example of a polycyclic aromatic hydrocarbon, gave octachloroanthraquinone when treated with the antimony pentachloride iodine reagent, but quantitative conversion to decachloroanthracene could not be obtained with reagent BMC (sulfuryl chloride-aluminum chloride-sulfur monochloide). A new reagent, trichlorosulfur tetra-chloroaluminate (SCl3+ AlCl4–), was shown to convert Aroclor 1254 to decadilorobiphenyl. As an application of the perchlorination technique it was shown that polychlorodibenzofurans (dibenzofuran) are not present at 0.5 μg/g in samples of Halowax 1014 and technical naphthalene, respectively. Well defined derivatives could not be obtained when phthalate esters or “hexabromobiphenyl” (fireMaster BP-6) were treated with the BMC or SbCl5–I2 reagents.
Determination of Aflatoxins in Mixed Feeds
Authors: Romer Thomas R 
Published: February 2020

Abstract
A complete extraction, purification, and cleanup method is described for the determination of aflatoxin in dairy, hog, horse, trout, and broiler finisher feeds. Thin layer chromatography is used for both confirmation and quantitative measurement of the aflatoxins. Average recovery for liquid spikes (3–100 ppb) was 92%. Average recovery found for feeds spiked (25 ppb) with cottonseed meal naturally contaminated with aflatoxin B1 was 80%. Sensitivities down to 2–4 ppb are possible with all the feeds tested. The method is also applicable to alfalfa, corn gluten meal, and fish meal, with a sensitivity of 2–4 ppb.
Determination of Maleic Hydrazide Residues in Tobacco and Vegetables
Authors: Ihnat Milan , Westerby Robert J , Hoffman Israel 
Published: February 2020

Abstract
The distillation-spectrophotometric method of Hoffman for determining maleic hydrazide has been modified to include a double distillation and was applied to the determination of 1–30 ppm maleic hydrazide residues in tobacco and vegetables. Recoveries of 1–23 μg added maleic hydrazide were independent of weight of maleic hydrazide, but did depend on sample and sample weight. The following recoveries were obtained from 0.5 g sample: pipe tobacco, 84%; commercially dehydrated potato, 83%; cigar tobacco, 81%; dried potato, 76%; fluecured tobacco, 73%; dried carrot, 71%. In the absence of sample, the recovery was 82%. When appropriate standard curves were used, maleic hydrazide levels determined in tobacco samples were essentially independent of sample weight in the range 0.1–3 g. The mean relative standard deviation for a variety of field-treated and fortified tobacco samples containing 1–28 ppm maleic hydrazide was 3%. The precision and sensitivity of this procedure seem to be substantial improvements over official method 29.111–29.117. It is recommended that the present method be subjected to a collaborative study.
Herbicide Analysis : Relationship Between Molecular Structure and Retention Index
Authors: Larose Richard H , Chau Alfred S Y 
Published: February 2020

Abstract
Retention indices are used to predict the retention time of the esters of chlorophenoxy acids. The total retention index is divided into 3 additive components: the alcohol contribution, the acid contribution, and the interaction contribution. This paper discusses 5 acids which are commonly used as herbicides, 8 alcohols, and 3 GLC columns.
Identification of cis- and trans-Cinnamoylcocaine in Illicit Cocaine Seizures
Authors: Moore James M 
Published: February 2020

Abstract
During the in-depth analysis of illicit cocaine samples small amounts of other coca alkaloids and cocaine degradation products have been detected. One of these alkaloids, cinnamoylcocaine, has been found in more than half of the samples examined, usually in concentrations of 1% or less of the amount of cocaine present. The presence of cinnamoylcocaine, as its cis and trans isomers, was established by column partition chromatographic isolation of the isomers, followed by ultraviolet, infrared, nuclear magnetic resonance, and mass spectrometric identification.
X-Ray Analysis of Forensic Samples, Using a Scanning Electron Microscope
Authors: Vasan Yel S , Stewart William D , Wagner J Bruce 
Published: February 2020

Abstract
A scanning electron microscope equipped with a wavelength dispersive spectrometer and an energy dispersive analyzer was used to examine paint chips and glasses. Line profiles of the elements in the paint show the non-uniform distribution of the pigments and extenders and, in order to obtain reproducible intensity ratios, a large area of the sample must be scanned. Layer analysis of the paint chip is possible with the energy dispersive analyzer and the resulting elemental profiles can be used to identify the chips. The difference in sodium concentration among the glasses studied provides a means of identifying the glass, but care must be taken to avoid migration of the sodium ions in the glass during electron beam bombardment.
Systematic Approach to the Detection of Explosive Residues. II. Trace Vapor Analysis
Authors: Washington Willard D , Midkiff Charles R 
Published: February 2020

Abstract
A Vapor Trace Analyzer (VTA) was found to be a valuable tool for scanning bomb debris for traces of certain types of explosives. The application of the VTA in screening bomb debris and locating secreted explosives and uses in other types of physical evidence is discussed. Thin layer chromatography is used to identify physically removed suspected explosive particles and samples from solvent extractions of blast material.
Gas Chromatographic Determination of Methyl Mercury in Fish, Sediment, and Water
Authors: Longbottom James E , Dressman Ronald C , Lichtenberg James J 
Published: February 2020

Abstract
Methyl mercury is extracted as the bromide salt from fish and sediment and as the chloride salt from water samples. All extracts are treated with a common cleanup procedure that results in the conversion of methyl mercury to the iodide salt for electron capture gas chromatographic analysis. Recoveries ranged from an average of 88.5% for water samples to averages of 95.5 and 96.3% for perch and sediments. Methods for controlling contaminants and interferences are discussed for all phases of the method. Particular problems encountered were column poisoning and detector poisoning. When the method was applied to sediment samples collected from a polluted river, a correlation could be established between total mercury and methyl mercury when the concentration of total mercury was in the 0–10 μg/g region. For samples of very high inorganic mercury, the correlation failed.
Observations on the Gas Chromatography of Kelthane (Dicofol)
Authors: Ives N Fred 
Published: February 2020

Abstract
Problems associated with the GLC of Kelthane (dicofol) are discussed. The contribution of inlet glass wool to the decomposition of dicofol to p,p′-dichlorobenzophenone is investigated and steps to minimize the problem are suggested. An impurity of the technical material, which eluted immediately after dicofol, was isolated and tentatively identified as 1,1-bis(p-chlorophenyl)-1,2,2,2-tetrachloroethane.
Spectrophotometric Determination of Gallotannins in Beer
Authors: Inskip Ervin B , King Perry , Ziegler Howard W 
Published: February 2020

Abstract
A method for the determination of traces of gallotannins in beer, in the presence of other natural tannins, has been developed. The procedure is based on the formation of a deep blue iron-tannin complex which is evaluated spectrophotometrically at 530 nm. Dimethyl sulfoxide is used to solubilize a haze that usually forms. Reproducibility of the method is quite good.
Comparison of Chicks and Rats as Test Animals for Studying Bioavailability of Iron, with Special Reference to Use of Reduced Iron in Enriched Bread
Authors: Pla Gwendolyn W , Harrison Bertha N , Fritz James C 
Published: February 2020

Abstract
Study was continued on the animal hemoglobin repletion test for measuring bioavailability of iron. With most iron sources, similar results were obtained with chicks and with rats. An important exception was noted with reduced iron. Seventeen samples were tested for solubility in dilute HCl and for bioavailability when fed to chicks and rats. The chicks utilized all samples reasonably well, but the rats were not able to efficiently utilize samples with particle sizes greater than 325 mesh. The mean relative biological value (vs. FeSO4 = 100) for the 17 samples was 50.5 ±8.3 when tested with chicks and 32.3±17.7 when tested with rats. Some, but not all, of the differences could be explained on the basis of particle size distribution. Similar relative biological values were obtained when the sample of reduced iron was added directly to the test diet or when it was used to enrich flour which was subsequently baked into bread and the bread was then added to the test diet. Plasma iron responses in human volunteers following test doses of the reduced iron samples were more closely related to the rat data, and this suggested that rats were the preferred species to measure bioavailability for man. The rat data also measured bioavailability of iron for guinea pigs.
Gas-Solid Chromatographic Determination of Propionates in Bakery Products
Authors: Jones Fitzhugh B 
Published: February 2020

Abstract
The bakery product sample is steam distilled, 10 ml distillate is evaporated, and the residue is dissolved in 1 ml dilute HCl. The propionate level is measured by gas-solid chromatography, using a Porapak Q column with a flame ionization detector and butyric acid as the internal standard. Recoveries of 5–30 mg propionic acid added to saltine crackers ranged from 97 to 102%. The method was checked by independent analyses and recoveries of 101 and 102% propionate were obtained.
Determination of FD&C Red No. 3 (Erythrosine) in Rat Blood Serum
Authors: Singh Manjeet , Graichen Charles 
Published: February 2020

Abstract
The extraction procedure used to isolate trace amounts of FD&C Red No. 3 (erythrosine) in rat blood serum is described. The blood sera from rats on diets containing FD&C Red No. 3 contained iodofluoresceins in such quantities that protein-bound iodine tests had no meaning. The lower iodinated subsidiary colors in FD&C Red No. 3 are absorbed and retained in the blood of rats to a greater degree than is tetraiodofluorescein, the main component of this color.
Polarographic Determination of Menadione Sodium Bisulfite in Pharmaceutical Preparations
Authors: Mayo Ana María , Nudelman Osmar 
Published: February 2020

Abstract
Menadione sodium bisulfite is reduced at pH 4 and determined by polarography, using a dropping mercury electrode. The method is simple and rapid and does not require special sample treatment. Average recoveries (%) and standard deviations for menadione sodium bisulfite added to synthetic mixtures at levels of 0.50, 1.00, and 5.0 mg were 99.88 ±2.12, 101.99±2.08, and 100.27±2.53, respectively.
Comparison of Methods for the Assay of Ethanol in Pharmaceutical Preparations, Cosmetics, and Alcoholic Beverages
Authors: Karawya Mohamed S , Hilal Sayed H , Elsohly Mahmoud A 
Published: February 2020

Abstract
Different methods, dichromate (iodometric and colorimetric), vanadate (spectrophotometric), critical miscibility temperature, and gas chromatography, were investigated for the determination of ethanol in various products. The results were compared with those from the official specific gravity method (USP and Egyptian Pharmacopoeia). The advantages and disadvantages, as well as the precision, are given for each method.
Differentiation of Randhuni (Apium graveolens) and Ajowan (Carum copticum) by Thin Layer Chromatographic Separation of Their Essential Oils
Authors: Sengupta Pratima , Sen Asit R , Bose Anjali , Mathew T V 
Published: February 2020

Abstract
The volatile oils of randhuni and ajowan seeds are extracted and spotted on silica gel G thin layer plates. The plates are developed in either benzene-petroleum ether (1+1) or chloroform-pyridine-benzene (65+5+30). Spraying with anisaldehyde-sulfuric acid reagent shows a single red spot for ajowan and 4 spots (violet, greenish yellow, violet, and blue) for randhuni. This procedure can also differentiate admixtures of the 2 and seeds of other Umbelliferae.
Mercury-Free Raney Catalyst Method for Total Nitrogen in Fertilizers
Authors: Johnson Frank J , Woodis Terry C , Cummings James M 
Published: February 2020

Abstract
The original Raney catalyst powder method for total nitrogen was shown not to be applicable to nitric phosphates containing non-sulfate sulfur. Interference by the non-sulfate sulfur was eliminated by the addition of morin, a mordant dye, before the reduction. The method was modified further by omitting HgO, a possible pollutant, from the digestion and by shortening the digestion time. The modified method is highly rugged for a considerable range of fertilizer materials.