Bromine, detection

Bromine detected in blood and organs of humans and other animals and birds by A. Damiens... 

A numerical matrix correction technique is used to linearise fluorescent X-ray intensities from plant material in order to permit quantitation of the measurable trace elements. Percentage accuracies achieved on a standard sample were 13% for sulfur and phosphorus and better than 10% for heavier elements. The calculation employs all of the elemental X-ray intensities from the sample, relative X-ray production probabilities of the elements determined from thin film standards, elemental X-ray attenuation coefficients, and the areal density of the sample cm2. The mathematical treatment accounts for the matrix absorption effects of pure cellulose and deviations in the matrix effect caused by the measured elements. Ten elements are typically calculated simultaneously phosphorus, sulfur, chlorine, potassium, calcium, manganese, iron, copper, zinc and bromine. Detection limits obtained using a rhodium X-ray tube and an energy-dispersive X-ray fluorescence spectrometer are in the low ppm range for the elements manganese to strontium. 

Bromine test. Dissolve 0 2 g. or 0 2 ml. of the compound in 2 ml. of carbon tetrachloride, and add a 2 per cent, solution of bromine in carbon tetrachloride dropwise until the bromine colour persists for one minute. Blow across the mouth of the tube to detect any hydrogen bromide which may be evolved (compare Sections III,6 and 111,11). 

Before sample preparation, surrogate compounds must be added to the matrix. These are used to evaluate the efficiency of recovery of sample for any analytical method. Surrogate standards are often brominated, fluorinated, or isotopically labeled compounds that are not expected to be present in environmental media. If the surrogates are detected by GC/MS within the specified range, it is... 

Bromine and bromides can be detected quaUtatively by a number of methods. In higher concentrations bromine forms colored solutions in solvents such as carbon tetrachloride [56-23-5] and carbon disulfide [75-15-0]. Bromine reacts with yeUow disodium fluorescein [518-47-8] to form red disodium tetrabromofluorescein (eosin) [548-26-5] C2QH Br4Na20. As Httle as 0.3 p.g of bromide can be detected and chlorides do not interfere (56). Bromine reacts with platinum sulfate [7446-29-9] Pt(S0 2> solution to form red to brown crystals of potassium hexabromoplatinate [16920-93-7] K PtBr ( )-... 

Impurities in bromine may be deterrnined quantitatively (54). Weighing the residue after evaporation of a bromine sample yields the total nonvolatile matter. After removing the bromine, chloride ion may be deterrnined by titration with mercuric nitrate, and iodide ion by titration with thiosulfate water and organic compounds may be detected by infrared spectroscopy sulfur may be deterrnined turbidimetricaHy as barium sulfate and heavy metals may be deterrnined colorimetricaHy after conversion to sulfides. 

Detection of Bromine Vapor. Bromine vapor in air can be monitored by using an oxidant monitor instmment that sounds an alarm when a certain level is reached. An oxidant monitor operates on an amperometric principle. The bromine oxidizes potassium iodide in solution, producing an electrical output by depolarizing one sensor electrode. Detector tubes, usefiil for determining the level of respiratory protection required, contain (9-toluidine that produces a yellow-orange stain when reacted with bromine. These tubes and sample pumps are available through safety supply companies (54). The usefiil concentration range is 0.2—30 ppm. 

Hydroxyquinoline forms the complex with Cu(II) in ratio 1 1 at pH 5-7. The composition of the complex is changed on 1 2 at pH>7. 8-Hydroxy-quinoline accepts bromine therefore its excess has been removed with NaOH solution. The complex was extracted with chloroform. It was shown that double extraction was enough to extract the complex. The detection limit is 5x10 M during 10c and at current generation IxlO A. 

Detection and result The chromatogram was freed from mobile phase (heated to 110°C for 30 min) and then exposed to bromine vapor for 1 h in a chamber, after blowing off excess bromine from the layer it was immersed for 1 s in the reagent solution. On drying in air dibutyltin dilaurate hRf 25 — 30), dibutyltin dichloride (kR( 25 — 30), dioctyltin oxide (hR( 40), tributyltin oxide (hRf 80), tributyltin chloride (hRf 80) and tetrabutyltin (hRf 85-90) produced persistent blue zones on a yellow ochre background (Fig. 1). 

This activation of the ortho position is most strikingly illustrated in the reactivity of 2,5-dimethylthiophene, which competitive experiments have shown to undergo the SnCb-catalyzed Friedel-Crafts reaction more rapidly than thiophene and even 2-methylthiophene. The influence of the reagent on the isomer distribution is evident from the fact that 2-methoxythiophene is formylated and bromi-nated (with A -bromosuccinimide) only in the 5-position. Similarly, although 3-bromo-2-methylthiophene has been detected in the bromi-nation of 2-methylthiophene with bromine, only the 5-isomer (besides some side-chain bromination) is obtained in the bromination of alkylthiophenes with A -bromosuccinimide. ° However, the mechanism of the latter type of bromination is not established. No lines attributable to 2-methyl-3-thiocyanothiophene or 2-methyl-3-chIoro-thiophene could be detected in the NMR spectra of the substitution products (5-isomers) obtained upon thiocyanation with thiocyanogen or chlorination with sulfuryl chloride. 2-Methyl- and 2-ethyl-thiophene give, somewhat unexpectedly, upon alkylation with t-butyl chloride in the presence of Feds, only 5-t-butyl monosubstituted and... 

Although direct nitration was not possible, 2-amino-4-methylselena-zole can be directly brominated by treatment with bromine in carbon tetrachloride, the hydrogen bromide salt of 2-amino-4-methyl-5-bromoselenazole, mp 180°C (decomp.) is formed. However, all attempts to obtain the free base from this salt failed and led to complete decomposition. In this bromination, an equivalent quantity of bromine must be used excess also leads to complete destruction of the molecule. From the decomposition products an oily compound can be detected similar to bromoacetone. ... 

C,4H2204, melting at 182 5. The formation of this cedrene-dicarboxylic acid serves for the detection of cedrene in essential oils. It is sufficient if the fraction to be examined be oxidised by permanganate or ozone, and the acid obtained (boiling-point at 10 mm. = 200° to 220° C.) be then oxidised further, either by an alkaline solution of bromine or by nitric acid. Even very small proportions of cedrene have definitely led to the obtaining of this acid melting at 182 5° C. 

The presence of free bromine, and consequently the end-point, can be detected by its yellow colour, but it is better to use indicators such as methyl orange, methyl red, naphthalene black 12B, xylidine ponceau, and fuchsine. These indicators have their usual colour in acid solution, but are destroyed by the first excess of bromine. With all irreversible oxidation indicators the destruction of the indicator is often premature to a slight extent a little additional indicator is usually required near the end point. The quantity of bromate solution consumed by the indicator is exceedingly small, and the blank can be neglected for 0.02M solutions. Direct titrations with bromate solution in the presence of irreversible dyestuff indicators are usually made in hydrochloric acid solution, the concentration of which should be at least 1.5-2M. At the end of the titration some chlorine may appear by virtue of the reaction ... 

Bromine in pyridine largely dibrominated 2-amino- and 2-hydroxy-1,3-diazulenes (35), although some mono- and tri-bromo products were also detected (88BCJ2690). 

Attempts to brominate benzothiazoles with bromine in acetic acid at room temperature have given only perbromides, but when these were heated in ethanolic solution, products in which bromine had substituted in the benzene moiety were detected. At 100°C bromine in acetic acid gave rise to the 4,6-dibromo derivative in accord with calculated -densities (70BSF2705). Vapor-phase bromination gave the 2-bromo product (84MI27). 

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