A MICROMETHOD FOR THE DETERMINATION OF SULPHATE BY FLAME PHOTOMETRY

1960 ◽  
Vol 38 (7) ◽  
pp. 643-648 ◽  
Author(s):  
G. A. Robinson

A micromethod for the determination of 0.1 to 3.5 μg of sulphate is described. Acidified barium chloride solution is added to samples containing free and esterified sulphate, and the resultant mixtures are dried at 95 °C. Soluble materials are redissolved with a 90% solution of acidified ethanol, 0.1 N for hydrochloric acid, containing 250 μg lithium per milliliter. After addition of the ethanol solution, approximately eight hours are required for the establishment of equilibrium (as indicated by a radiosulphur label) between solid and dissolved barium sulphate. Barium present in solution is then determined quantitatively by flame photometry, with the ethanol–lithium medium increasing the primary emission of the barium by 15 times. The sulphate content of the sample is read from a standard curve. Estimations on microgram quantities of some organic and inorganic sulphur-containing compounds are given.

1960 ◽  
Vol 38 (1) ◽  
pp. 643-648
Author(s):  
G. A. Robinson

A micromethod for the determination of 0.1 to 3.5 μg of sulphate is described. Acidified barium chloride solution is added to samples containing free and esterified sulphate, and the resultant mixtures are dried at 95 °C. Soluble materials are redissolved with a 90% solution of acidified ethanol, 0.1 N for hydrochloric acid, containing 250 μg lithium per milliliter. After addition of the ethanol solution, approximately eight hours are required for the establishment of equilibrium (as indicated by a radiosulphur label) between solid and dissolved barium sulphate. Barium present in solution is then determined quantitatively by flame photometry, with the ethanol–lithium medium increasing the primary emission of the barium by 15 times. The sulphate content of the sample is read from a standard curve. Estimations on microgram quantities of some organic and inorganic sulphur-containing compounds are given.


1967 ◽  
Vol 13 (3) ◽  
pp. 227-232 ◽  
Author(s):  
Joseph S Annino

Abstract A method has been developed for determination of sodium concentration (activity) in urine using a glass electrode designed to be especially sensitive to sodium ion activity. The urine is diluted 2:20 with Tris buffer (pH 8.0) and sodium activity measured by dipping a sodium electrode and calomel reference electrode in the diluted specimen and obtaining a millivolt reading with a sensitive pH meter. The sodium concentration is then calculated from a predetermined standard curve. Concentrations of 0-200 mEq./L. may be read using the same dilution. Blind comparisons of sodium concentrations obtained by flame photometry and by sodium ion electrode showed excellent agreement.


1936 ◽  
Vol 9 (4) ◽  
pp. 648-660
Author(s):  
C. Herbert Lindsly

Abstract THERE is probably no single operation in analytical chemistry that has received more attention from investigators than that of precipitation of barium sulfate by means of a soluble barium salt for the determination of sulfate or of barium. The literature on this subject is voluminous and the conclusions reached by different investigators as to the proper procedure to employ in order to obtain a precipitate which will be filterable and reasonably pure are highly contradictory. The procedure which seems to be in most general use at present for the determination of sulfate is that of adding the barium chloride solution to the hot sulfate solution very slowly, stirring vigorously meanwhile, then allowing the whole to digest at an elevated temperature for several hours before filtering. The diversity of opinion as to the proper procedure arises, the author believes, from the fact that the barium sulfate precipitate is exceedingly sensitive to its environment and that a very slight change in the amount or kind of impurities present in the solutions during precipitation has a profound effect upon the crystal size and shape of the precipitated particles as well as upon their purity. Kolthoff and Vogelenzang (2) have stated that it is impossible to prescribe a general procedure for the accurate precipitation of sulfate in arbitrary mixtures. In other words, a precipitation procedure which gives satisfactory results in the determination of sulfur in copper ores, for instance, may not yield a satisfactory precipitate when applied to the determination of total sulfur in hard rubber dust, and a study of each type of determination, with due consideration for the amount and kind of impurities present, must be made in order to find the conditions necessary to obtain a precipitate which is pure and easily filterable.


1975 ◽  
Vol 58 (1) ◽  
pp. 146-149
Author(s):  
Laverne H Scroggins

Abstract A collaborative study was conducted on microchemical sulfur determination by oxygen flask combustion. Seven collaborators performed duplicate determinations on 5 samples: sulf anilamide, benzylisothiourea hydrochloride, cystine, potassium sulfate, and a mixture of potassium sulfate and phosphate. Following oxygen flask combustion, the resultant gases were absorbed in a solution containing 0.1/V NaOH and 30% H2O2. The acidified sample was shaken 30 min and evaporated to dryness on the steam bath; the sulfate was titrated with standard barium chloride solution. The indicator used in this study was tetrahydroxyquinone. Its reliability has been previously proved and adopted by AOAC for use with the Carius-type combustion. Evaluation of the statistical data and overall consideration indicate satisfactory results for all types of compounds studied, with the exception of phosphorus-contaminated samples. Both systematic and random errors for the pure compounds were low. The method has been adopted as official first action.


1919 ◽  
Author(s):  
◽  
Verner V. Kendall

Text from page 3: "In this paper, the authors, in determining the amount of occluded barium chloride in barium sulphate precipitated in the usual manner made use of the foregoing method."


Radiocarbon ◽  
1979 ◽  
Vol 21 (1) ◽  
pp. 131-137 ◽  
Author(s):  
Dušan Srdoč ◽  
Adela Sliepčevic ◽  
Bogomil Obelic ◽  
Nada Horvatinčic

The following list contains dates of samples measured since our previous list (R, 1977, v 19, p 465-475). As before, age calculations are based on the Libby half-life, 5570 ± 30 years, and reported in years before 1950. The modern standard is 0.95 of the activity of NBS oxalic acid. Solid sample pretreatment, combustion and counting technique are essentially the same as described in R, 1971, v 13, p 135-140. Groundwater samples were prepared following the procedure adopted by the IAEA (IAEA, 1977). Carbonates and hydrocarbonates from water samples were precipitated by adding saturated barium chloride solution while the alkalinity was adjusted to pH = 8 by adding carbonate-free saturated solution of sodium hydroxide. The precipitation was enhanced by adding iron salts and Praestol as coagulating medium. Carbon dioxide was evolved by acidification of the precipitate and converted to methane. Statistical processing of data has been computerized (Obelić and Planinić, 1975). Sample descriptions were prepared with collectors and submitters. The errors quoted correspond to 1σ variation of sample net counting rate and do not include the uncertainty in 14C half-life.


2016 ◽  
Vol 19 (3) ◽  
pp. 477-484 ◽  
Author(s):  
A. Kubátová ◽  
T. Fedorova ◽  
I. Skálová ◽  
L. Hyniová

Abstract The aim of the research was to evaluate two chemical tests for non-invasive pregnancy diagnosis from urine, the Cuboni reaction and the barium chloride test, in donkeys (Equus asinus) and alpacas (Vicugna pacos). The research was carried out from April 2013 to September 2014. Urine samples were collected on five private Czech farms from 18 jennies and 12 alpaca females. Urine was collected non-invasively into plastic cups fastened on a telescopic rod, at 6-9 week intervals. In total, 60 and 54 urine samples from alpacas and jennies, respectively, were collected. The Cuboni reaction was performed by the State Veterinary Institute Prague. The barium chloride test was done with 5 ml of urine mixed together with 5 ml of 1% barium chloride solution. Results of the Cuboni reaction were strongly influenced by the reproductive status of jennies; the test was 100% successful throughout the second half of pregnancy. However, no relationship was found between the real reproductive status of alpaca females and results of the Cuboni reaction. It was concluded that the barium chloride test is not suitable for pregnancy diagnosis either in donkeys, due to significant influence of season on the results, or in alpacas, because no relationship between results of the test and the reproductive status of alpaca females was found. In conclusion, the Cuboni reaction has potential to become a standard pregnancy diagnostic method in donkeys.


Sign in / Sign up

Export Citation Format

Share Document