Sequential flow injection determination of iodate and periodate with spectrophotometric detection

A flow injection (FI) system is described for the sequential determination of periodate and iodate based on their reaction with iodide at pH 3.5. Two sample plugs were injected into the same carrier stream sequentially. One injection is for the iodate determination and the other for the sum of iodate and periodate determination. For iodate determination, molybdate solution buffered at pH of 3.5 was used for selective masking of periodate. The influences of reagent concentrations were studied by a univariable method and the influence of FI manifolds was studied using univariable and simplex method. Periodate and iodate can be determined in the range of 0.050-5.0 and 0.050-10 microg/ml, respectively. The 3 sigma limit of detection was 0.030 and 0.050 microg/ml for periodate and iodate, respectively. The proposed method has been applied for the sequential determinations of periodate and iodate in water samples.     

Quick analytical method for the determination of iodide and iodate ions in aqueous solutions

An analytical quick-test method was developed to determine iodide and iodate ions in aqueous solutions using solid phase extraction cartridges for sample preparation. Work was focussed on finding simple, but efficient conditions for quantitative separation of iodate and iodide. Iodine amounts were then determined by standard methods. Ion-exchange absorbers in cartridge form were used. Selectivity and yield of the species separation were studied at pH value of 5-10 and various solution compositions using ¹³¹I radioactive tracer. The electrolytes used were diluted alkaline, nitrate and boric acid-borate solutions. Application to nuclear reactor cooling water analysis or environmental investigations and monitoring is proposed.     

Determination of sulphide by anion-exchange with lead iodate

A quick anion-exchange reaction, suitable for the determination of sulphide, has been found to occur on stirring a suspension of lead iodate (solubility product, K(s0) = 1.2 x 10(-13)) with sulphide solution at pH 5-8. After removal of the precipitates of lead iodate and lead sulphide (K(s0) = 3.4 x 10(-28)), the iodate released can be determined by its reaction with acidified iodide to give tri-iodide which is either titrated with thiosulphate or measured spectrophotometrically as its blue complex with starch. Chloride, bromide, iodide, fluoride, oxalate, sulphate, thiocyanate and phosphate do not interfere. Thiosulphate, sulphite, nitrite and thiols do not give an anion-exchange reaction but do interfere in the redox reaction of iodate with acidified iodide. However, this is avoided if they are first oxidized with bromine (the liberated iodate remains unaffected before iodometry.     

Speciation of iodate and iodide in seawater by non-suppressed ion chromatography with inductively coupled plasma mass spectrometry

A non-suppressed ion chromatography (IC) with inductively coupled plasma mass spectrometry (ICP-MS) has been developed for simultaneous determination of trace iodate and iodide in seawater. An anion-exchange column (G3154A/101, provided by Agilent) was used for the separation of iodate and iodide with an eluent containing 20 mM NH₄NO₃ at pH 5.6, which reduced the build-up of salts on the sampler and skimmer cones. The influences of competing ion (NO₃⁻) in the eluent on the retention time and detection sensitivity were investigated to give reasonable resolution and detection limits. Linear plots were obtained in a concentration range of 5.0–500 μg/L and the detection limit was 1.5 μg/L for iodate and 2.0 μg/L for iodide. The proposed method was used to determinate iodate and iodide in seawaters without sample pre-treatment with exception of dilution.     

Reverse flow injection spectrophotometric determination of iodate and iodide in table salt

A very simple and sensitive reverse flow injection method is described for the determination of iodate and iodide. The iodate reacts with excess iodide in acidic medium to form tri-iodide, which can be spectrophotometrically monitored at 351 nm, and the absorbance is directly related to the concentration of iodate in the sample. The determination of iodide is based on oxidizing iodide to iodate. The calibration curve is linear in the range of 0.02-3.0 μg ml⁻¹ I with r²=0.9998, and the limit of detection is 0.008 μg ml⁻¹ I. The chemical and flow injection variables were studied and optimized to make the procedure suitable for quantitating iodate and iodide in table salts. It is shown that the reverse flow injection analysis could greatly improve the sensitivity and precision for determination of iodate with a relative standard deviation of 0.9%. A complete analysis, including sampling and washing, could be performed in 35 s. The procedure was applied successfully to the determination of iodate and iodide in table salts, and the results were statistically compared with results determined by standard iodometry method.     

The oxidation of iodide to iodate for the polarographic determination of total iodine in natural waters

A simple method has been designed for the oxidation of iodide to iodate in natural waters and subsequent determination of the iodate by differential pulse polarography. Iodide is oxidized to iodate with sodium hypochlorite and the excess of oxidizing agent is destroyed with sodium sulphite. The concentration of iodide is calculated as the difference between the concentrations of iodate in a sample before and after the oxidation.     

Flow-injection amplification for the spectrophotometric determination of iodide

A flow manifold is described in which iodide (0.05–15 μg ml^?1) in a 50-μl sample is oxidized by bromine water to iodate, most of the excess of bromine is reduced by formic acid, and the iodate is reacted with more iodide to form triiodide, which is determined spectrophotometrically. Six-fold amplification is achieved. The relative standard deviation is ca. 1%).     

Selection of optimum pH for the iodate determination using differential pulse polarography

The concentration of iodate in seawater samples was determined at various pH values using differential pulse polarography (DPP). The sensitivity for the iodate determination decreased rapidly below pH 7 and above pH 9. The decrease below pH 7 may be caused by conversion of iodate to iodide, followed by the successive formation of I₂ and I₃ ^–. The decrease above pH 9 is probably due to the combination of iodate and hydroxide. Theoretical calculations have demonstrated that the optimum pH for iodate determination is above pH 7.4 for Po₂ = 0.101 Pa.     

Spectrophotometric determination of periodate, iodate and bromate mixtures based on their reaction with iodide.

A rapid, simple, precise and accurate method is proposed for the determination of ternary mixtures of periodate-iodate-bromate based on their reaction with iodide ion at different pH values. The absorbance was measured at 352 nm. Three sets of reaction conditions were developed. In the first set of conditions, only periodate reacted with iodide, but in the second set the periodate and iodate reacted with iodide and in the third set the three ions reacted with iodide during the first 3 min after initiation of the reaction. The method could be used for individual determinations of periodate, iodate and bromate in the concentration range of 0.05-8.0 microg/ml, 0.05-5.0 microg/ml and 0.2-12 microg/ml, respectively. The data were evaluated by simultaneous equations.     

Determination of iodide by derivatization to 4-iodo-N,N-dimethylaniline and gas chromatography-mass spectrometry

A real-time determination of iodide is proposed which involves the oxidation of iodide with 2-iodosobenzoate in the presence of N,N-dimethylaniline. The reaction is completed within 1 min to yield 4-iodo-N,N-dimethylaniline, which is extracted in cyclohexane and determined by GC-MS. It was also possible to determine iodine by derivatization in the absence of 2-iodosobenzoate, and iodate by its reduction with ascorbic acid to iodide and subsequent derivatization. A rectilinear calibration graph was obtained for 0.02-50 micrograms l-1 iodide with a correlation coefficient of 0.9998. The limit of detection was 8 ng l-1 iodide. The method was applied to the determination of iodate in iodized table salt and free iodide and total iodine in sea-water, and to spiked samples when the recovery was in the range 96.8-104.3% (RSD 1.9-3.6%). A sample clean-up by solid-phase extraction with a LiChrolut EN cartridge is proposed.     

Flow gradient liquid chromatography using a coated anion exchange microcolumn

Ion chromatography on a 4.0-mm-long (3.0 mm ID) ion exchange column is presented. Using a 10 mM phosphate buffer (pH 2.22) the separation of up to six UV-absorbing anions was obtained using the microcolumn, containing 5 microm RP support (Phenomenex Gemini) coated with the zwitterionic surfactant, (N-dodecyl-N,N-dimethylammonio) undecanoate. The short analytical column facilitated the application of a flow gradient programme over the flow range 0.3-5 mL/min resulting in optimum resolution of nitrite, nitrate, benzoate, iodide, thiocyanate and trichloroacetate in less than 10 min. The effect of both eluent concentration and pH on the retention of six selected anions was investigated, showing a strong pH capacity dependence. The microcolumn was found to exhibit no selectivity towards chloride and so was well suited to the analysis of saline samples. To illustrate this, the rapid analysis of a concentrated iodized table salt sample (20 g/L) was carried out. Following standard addition, a concentration of 3.55 +/- 0.05 microg iodide/g and 1.05 +/- 0.02 microg iodate/g in the solid salt sample was determined.     

Indirect amplification method for determining formaldehyde and chloralhydrate by differential pulse polarography

An indirect differential pulse polarographic method for the determination of formaldehyde and chloralhydrate is described; it is based on the oxidation of the alkaline sample solutions of formaldehyde and chloralhydrate with a chloroform solution of iodine and removal of its excess. The resulting iodide is oxidized with bromine water and measured polarographically as iodate (at pH 9.3) with sixfold amplification.     

Selection of optimum pH for the iodate determination using differential pulse polarography

The concentration of iodate in seawater samples was determined at various pH values using differential pulse polarography (DPP). The sensitivity for the iodate determination decreased rapidly below pH 7 and above pH 9. The decrease below pH 7 may be caused by conversion of iodate to iodide, followed by the successive formation of I₂ and I₃ ^–. The decrease above pH 9 is probably due to the combination of iodate and hydroxide. Theoretical calculations have demonstrated that the optimum pH for iodate determination is above pH 7.4 for Po₂ = 0.101 Pa. Received: 14 July 1998 / Revised: 2 October 1998 / Accepted: 3 October 1998     

Spectrophotometric determination of iodine species in table salt and pharmaceutical preparations

A sensitive spectrophotometric method for the determination of iodine species like iodide, iodine, iodate and periodate is described. The method involves the oxidation of iodide to ICl(2)(-) in the presence of iodate and chloride in acidic medium. The formed ICl(2)(-) bleaches the dye methyl red. The decrease in the intensity of the colour of the dye is measured at 520 nm. Beer's law is obeyed in the concentration range 0-3.5 microg of iodide in an overall volume of 10 ml. The molar absorptivity of the colour system is 1.73 x 10(5) l mol(-1) cm(-1) with a correlation coefficient of -0.9997. The relative standard deviation is 3.6% (n=10) at 2 microg of iodide. The developed method can be applied to samples containing iodine, iodate and periodate by prereduction to iodide using Zn/H(+) or NH(2)NH(2)/H(+). The effect of interfering ions on the determination is described. The proposed method has been successfully applied for the determination of iodide and iodate in salt samples and iodine in pharmaceutical preparations.     

Iodometric microdetermination of certain organic acids

A rapid and accurate method for the determination of certain organic acids is described. The acid sample solution is treated with suitable quantities of solid potassium iodate and potassium iodide followed by the titration of the liberated iodine with thiosulphate after 3-5 min. The results are accurate to within 0.3%.     

Iodometric microdetermination of hydrazines by amplification reactions

Two new, simple, rapid, and accurate iodometric amplification methods are described for the micro and submicro determination of hydrazine. The first depends on oxidation with a chloroform solution of iodine and removal of its excess, oxidation of the resulting iodide with bromine, and iodometric titration of the liberated iodate. The second method is based on oxidation with periodate at pH 8, masking of the excess of periodate with molybdate at pH 3, and iodometric titration of the iodate. The order of amplification involved in the two methods is 6- and 3-fold, respectively. Micro amounts of hydrazine sulphate and dihydrochloride were determined satisfactorily by both methods, the average recoveries being 98.6 and 99.4%.     

Titrimetric microdetermination of inorganic or organic mercury by amplification reactions

A simple titrimetric method for estimation of 0.05-7 mg of Hg(II) is presented. The acidic sample solution is treated with a measured and excessive amount of iodide, then mercuric iodide is extracted at ph 2-3.5, and the unreacted iodide is determined iodometrically after 6- or 36-fold amplification by use of bromine water for oxidation of iodide to iodate. Periodate oxidation of excess of iodide gives 24-fold amplification. The coefficient of variation does not usually exceed 1% for above 1 mg of mercury but increases to 4% at the 0.05-mg level. The 6-fold amplification method is used for microdetermination of organically bound mercury following oxygen-flask combustion. The average absolute error for 10 determinations (3 compounds) amounted to +/-0.6%; one determination takes less than one hour.     

离子色谱法测定婴幼儿营养米粉中的碘含量

采用离子色谱分离和脉冲安培检测婴幼儿营养米粉中添加的碘化钾或碘酸钾含量.考察了蛋白质去除的方法和试剂用量,优化了超声提取净化方案,研究了碘酸钾转化成碘化钾的最佳还原剂用量,进行了淋洗液浓度和检测器波形等仪器条件的选择.在优化实验条件下,碘化钾和碘酸钾的线性范围均为1～100 μg/L,相关系数分别为0.999 1和0....     

Oxidation of micro or trace amounts of bromide to bromate by peroxodisulphate before their iodometric determination by titration or spectrophotometry

The optimum conditions for the oxidation of bromide to bromate by peroxodisulphate at 120 degrees as well as for the decomposition of the excess of oxidant have been determined. The predicted advantages of this oxidizing agent, viz. minimal blanks and destruction of small amounts of interfering organic matter and reducing substances, were confirmed. The bromate was determined iodometrically either by titration with thiosulphate or by spectrophotometry in absence of oxygen at 355 nm. The titrimetric finish applied to 0.8-8 micromole of bromide gave a mean yield of 100.0%, s = 6 nmole. The spectrophotometric finish applied to 0.05-0.25 micromole of bromide gave a mean yield of 98.9%, s = 1.1 nmole. Interfering amounts of iodide present in the sample and oxidized to iodate can be corrected for by making use of the pH-dependence of the reaction of iodide with bromate and iodate.     

Indirect amplification method for determining mercury by direct-current polarography. Application to organomercury compounds

An amplification method for the determination of 0.5–70 ppm (2.5 × 10⁻⁶ to 3.5 × 10⁻⁴ M) of Hg(II) is described. Hg(II) is reacted with a slight excess of KI, and the excess iodide is oxidized by bromine water and measured polarographically as iodate with sixfold amplification. Alternatively, the iodate formed is reacted to liberate iodine which is then reduced to iodide, and again oxidized to yield six iodate ions for every iodide ion originally present;

2. Microdetermination of Mercury in Organomercurial Compounds

polarographic reduction requires 36 electrons. Oxidation of the excess iodide with periodate yields four iodate ions for every iodide ion and therefore allows 24-fold amplification.Microdetermination of mercury in organomercurials is achieved using the sixfold method following closed flask combustion: the average percentage error for 10 determinations is ±0.40 and the time required for one sample run is 45 min.