Rapid analysis of inorganic and organic anions in kraft pulping liquors by capillary zone electrophoresis
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Abstract:
New methods have been developed for determining and/or speciating several important inorganic sulphur species, including: thiosulphate, sulphate, sulphite, sulphide and polysulphide in kraft pulping liquors and effluents by capillary zone electrophoresis. In addition, several other key anions, including: hydroxide, carbonate, oxalate, formate and chloride can be quantified in the same process liquors. Two approaches were developed for determining the anions. In one method, anions were baseline resolved and quantified using sodium chromate, tetradecyltrimethylammonium hydroxide-based electrolytes with indirect UV-detection. In the second scheme, polysulphide was speciated, and sulphur species such as sulphide, thiosulphate and sulphite, as well as hydroxide were separated and determined using a sodium sulphate, tetradecyltrimethylammonium hydroxide-based electrolyte with direct UV-detection. A third approach, involving the use a 2- (N-Cyclohexylamino) ethanesulfonic acid, hexamethonium hydroxide electrolyte with conductivity detection was also briefly examined and found to be unsuitable for the analysis of sulphide-bearing samples.Keywords:
Chromate conversion coating
Sodium hydroxide
Isotachophoresis
Metal hydroxide
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Tributyl phosphate
Uranyl nitrate
Nitric acid
Uranyl
Terbium
Hydrogen phosphate
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Thiocyanate
Phosphoric acid
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Lanthanum
Qualitative analysis
Inorganic ions
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Polarography
Hydrochloric acid
Chromate conversion coating
Barium
Barium sulfate
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Nanochemistry
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In the determination of boron, the mercury cathods was used to remove various interfering cations from borate solutions. It was found that the remaining interferences, including aluminum and uranium, could be removed by a simple sodium hydroxide precipitation. The borate was then titrated alkalimetrically in the resulting filtrate after pH adjustment and addition of mannitol. (W.C.G.)
Mercury
Sodium hydroxide
Boric acid
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The method described for the determination of sulphate in the presence of barium can also be extended to the determination of sulphur in organic compounds and hydrocarbon oils containing barium. After oxygen-flask combustion of the sample, ammoniacal EDTA can be added directly to the solution and the total sulphate then determined nephelometrically after precipitation with 4-chloro-4′-aminobiphenyl. Alternatively, free sulphate can be determined separately by direct precipitation as chloroaminobiphenyl sulphate after filtering off precipitated barium sulphate; the latter can then be dissolved in ammoniacal EDTA solution and the sulphate also determined as chloroaminobiphenyl sulphate.
Barium sulphate
Barium
Barium chloride
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Ethylenediaminetetraacetic acid
Barium chloride
Barium
Gravimetric analysis
Barium sulphate
Oxidizing agent
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A method for the simultaneous separation and determination of organic acids and inorganic anions in Bayer sodium aluminate liquors was developed by gradient ion chromatography with suppressed conductivity detection.The organic acids(formic acid,acetic acid,propionic acid,oxalic acid,succinic acid,glutaric acid) and inorganic anions(fluorion,chlorion,sulfate readical) were separated and determined within 33 min.The sample was pretreated with solid phase extraction,which could effectively removed a large number of metallic ions from the sodium aluminate solution.The separation of six organic acids and three inorganic anions is achieved on an IonPac AS11-HC column with KOH as the eluent,no interference is found in the presence of fluorate,chlorate and sulphate when organic acids are determined.The calibration graphs of peak area for all the analytes are linear over a wide range(r=0.994 7-0.998 9).The relative standard deviations of the peak area of analytes are less than or equal to 3.2%.The detection limits for analytes are no more than 0.036 μg/mL and the recoveries of the added standards are between 94%-103%.
Oxalic Acid
Ion chromatography
Succinic acid
Organic acid
Sodium aluminate
Aluminate
Glutaric acid
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Ion chromatography
Chlorate
Organic anion
Solid phase extraction
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