Iodate detection

In the iodate detection system (ASTM D1552), the sample is burned in a stream of oxygen at a sufficiently high temperature to convert about 97% by weight of the sulfur to sulfur dioxide. The combustion products are passed into an absorber containing an acidic solution of potassium iodide and starch indicator. A faint blue color is developed in the absorber solution by the addition of standard potassium iodate solution. As combustion proceeds, bleaching the blue color, more iodate is added. The sulfur content of the sample is calculated from the amount of standard iodate consumed during the combustion. 

Perchlorate and iodate detection in water has improved significantly in recent years, due to improvements in analytical methodology. 

Salimi A, MamKhezri H, Hallaj R, Zandi S. Modification of glassy carbon electrode with multi-walled carbon nanotubes and iron(lll)-porphyrin film application to chlorate, bromate and iodate detection. Electrochim Acta 2007 52 6097-105. 

The pH must be kept at 7.0—7.2 for this method to be quantitative and to give a stable end poiut. This condition is easily met by addition of soHd sodium bicarbonate to neutralize the HI formed. With starch as iudicator and an appropriate standardized iodine solution, this method is appHcable to both concentrated and dilute (to ca 50 ppm) hydraziue solutious. The iodiue solutiou is best standardized usiug mouohydraziuium sulfate or sodium thiosulfate. Using an iodide-selective electrode, low levels down to the ppb range are detectable (see Electro analytical techniques) (141,142). Potassium iodate (143,144), bromate (145), and permanganate (146) have also been employed as oxidants. 

The potentiometric micro detection of all aminophenol isomers can be done by titration in two-phase chloroform-water medium (100), or by reaction with iodates or periodates, and the back-titration of excess unreacted compound using a silver amalgam and SCE electrode combination (101). Microamounts of 2-aminophenol can be detected by potentiometric titration with cupric ions using a copper-ion-selective electrode the 3- and... 

In addition to the stable I2O5 and moderately stable I4O9 and I2O4, several short-lived radicals have been detected and characterized during y-radiolysis and flash photolysis of iodates in aqueous alkali ... 

Discussion. Iodine (or tri-iodide ion Ij" = I2 +1-) is readily generated with 100 per cent efficiency by the oxidation of iodide ion at a platinum anode, and can be used for the coulometric titration of antimony (III). The optimum pH is between 7.5 and 8.5, and a complexing agent (e.g. tartrate ion) must be present to prevent hydrolysis and precipitation of the antimony. In solutions more alkaline than pH of about 8.5, disproportionation of iodine to iodide and iodate(I) (hypoiodite) occurs. The reversible character of the iodine-iodide complex renders equivalence point detection easy by both potentiometric and amperometric techniques for macro titrations, the usual visual detection of the end point with starch is possible. 

The amount of reddish-purple acid-chloranilate ion liberated is proportional to the chloride ion concentration. Methyl cellosolve (2-methoxyethanol) is added to lower the solubility of mercury(II) chloranilate and to suppress the dissociation of the mercury(II) chloride nitric acid is added (concentration 0.05M) to give the maximum absorption. Measurements are made at 530nm in the visible or 305 nm in the ultraviolet region. Bromide, iodide, iodate, thiocyanate, fluoride, and phosphate interfere, but sulphate, acetate, oxalate, and citrate have little effect at the 25 mg L 1 level. The limit of detection is 0.2 mg L 1 of chloride ion the upper limit is about 120 mg L . Most cations, but not ammonium ion, interfere and must be removed. 

Cyanide and thiocyanate anions in aqueous solution can be determined as cyanogen bromide after reaction with bromine [686]. The thiocyanate anion can be quantitatively determined in the presence of cyanide by adding an excess of formaldehyde solution to the sample, which converts the cyanide ion to the unreactive cyanohydrin. The detection limits for the cyanide and thiocyanate anions were less than 0.01 ppm with an electron-capture detector. Iodine in acid solution reacts with acetone to form monoiodoacetone, which can be detected at high sensitivity with an electron-capture detector [687]. The reaction is specific for iodine, iodide being determined after oxidation with iodate. The nitrate anion can be determined in aqueous solution after conversion to nitrobenzene by reaction with benzene in the presence of sulfuric acid [688,689]. The detection limit for the nitrate anion was less than 0.1 ppm. The nitrite anion can be determined after oxidation to nitrate with potassium permanganate. Nitrite can be determined directly by alkylation with an alkaline solution of pentafluorobenzyl bromide [690]. The yield of derivative was about 80t.with a detection limit of 0.46 ng in 0.1 ml of aqueous sample. Pentafluorobenzyl p-toluenesulfonate has been used to derivatize carboxylate and phenolate anions and to simultaneously derivatize bromide, iodide, cyanide, thiocyanate, nitrite, nitrate and sulfide in a two-phase system using tetrapentylammonium cWoride as a phase transfer catalyst [691]. Detection limits wer Hi the ppm range. 

USP XIX directs that hydralazine be determined in the raw material, tablets, and injections by potassium iodate titration in strongly acid solution, using chloroform to detect the presence of iodine (19). 

Shi and Adams recently created a rapid IC/ICF-MS method for simultaneously measuring iodoacetic acids, bromoacetic acids, iodate, and bromate in drinking water, groundwater, surface water, and swimming pool water [165]. Method detection limits were sub-pg/L for iodinated DBFs, and low-pg/L for brominated DBFs. 

Chlorine gas may be identified readdy by its distinctive color and odor. Its odor is perceptible at 3 ppm concentration in air. Chlorine may be measured in water at low ppm by various titrimetry or colorimetric techniques (APHA, AWWA and WEF. 1999. Standard Methods for the Examination of Water and Wastewater, 20th ed. Washington DC American Pubhc Health Association). In iodometric titrations aqueous samples are acidified with acetic acid followed by addition of potassium iodide. Dissolved chlorine liberates iodine which is titrated with a standard solution of sodium thiosulfate using starch indicator. At the endpoint of titration, the blue color of the starch solution disappears. Alternatively, a standardized solution of a reducing agent, such as thiosulfate or phenylarsine oxide, is added in excess to chlorinated water and the unreacted reductant is then back titrated against a standard solution of iodine or potassium iodate. In amperometric titration, which has a lower detection limit, the free chlorine is titrated against phenyl arsine oxide at a pH between 6.5 and 7.5. 

Torimura etal. [194] developed an analytical approach capable of determining subnanomolar amounts of carbohydrates based on the indirect detection of iodate, 103 , at a glassy carbon electrode. The method was applied as a postcolumn detection system for HPLC separation. 

This technique is easy to use and its most important merit is that it can readily indicate absence of iodate in case adulterants that give false positive iodometric test are used in its place. The method also enables trace quantities of iodide to be detected even in the presence of large excess of chloride ion. Interferences from impurities normally present in salt were insignificant. 

Kumar S. D., Maiti B. Mathur P. K. Determination of iodate and sulfate in iodized common salt by ion chromatography with conductivity detection. Talanta 2001 53(4) 701-705. 

Rebary B., Paul P. Ghosh P. K. Determination of iodide and iodate in edible salt by ion chromatography with integrated amperometric detection. Food Chemistry 2010 123(2) 529-534. 

Detection and determination.—The periodates behave towards reducing agents like the iodates. They are usually but slightly soluble in water and readily soluble in dil. nitric acid. When soln. of sodium periodate are added to barium, strontium, calcium, lead, and silver salts, precipitates of dimesoperiodates are obtained, and the mother liquor has an acid reaction—the silver salt is pale yellow, the others white—silver iodate is also white. The silver precipitate becomes dark red when boiled in water the fresh precipitate is very soluble in ammonia, the dark red... 

Detection limit. A sensitive chromatographic method was developed to measure sub-part-per-billion levels of the disinfectant by-products iodate (I03), chlorite (C I02 ), and bromate (BrOf) in drinking water. As the oxyhalides emerge from the column, they react with Br to make Brj, which is measured by its strong absorption at 267 nm. For example, each mole of bromate makes 3 mol of Br by the reaction BrOj" + 8Br + 6H+ —> 3Brj + 3H20. 

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