[Objective] The aim was to analyze sugar components in fermented rice wine by ion chromatography. [Method] The optimal condition for chromatography system of sugar analysis was selected by measuring sugars in fermente...[Objective] The aim was to analyze sugar components in fermented rice wine by ion chromatography. [Method] The optimal condition for chromatography system of sugar analysis was selected by measuring sugars in fermented rice wine with ion chromatography and pulsed amperometric detection. [Result] The optimal measurement conditions were as follows： Leacheate （Leachate）, consisting of NaOH and CH3COONa, was eluted by gradient concentrations, with column temperature at 35 ℃ and flow rate at 0.4 ml/min. In the condition, sugars in rice wine were ana- lyzed and the results showed that the method is featured by low detection limit, good repetition and high recovery rate. [Conclusion] The research establishes and determines the approaches and optimum conditions for sugar analysis in rice wine by ion chromatography and pulsed amperometric detection, providing references for advancement of research on quality improvement of fermented rice wine.展开更多
A method was developed for determination of chlorine and bromine in plant materials by ion chromatography using temperature programing-semi molten for sample preparation. Values of detection limits of the method found...A method was developed for determination of chlorine and bromine in plant materials by ion chromatography using temperature programing-semi molten for sample preparation. Values of detection limits of the method found were 1.0×10^-5 for CI and 1.3×10^-6 for Br. The measuring range of the method found were 0.3-20.0 mg/L for CI and 4,0-120,0 μg/L for Br. The results obtained agreed quite well with those reference values.展开更多
Simple, reliable and sensitive analytical methods to determine anticariogenic agents, preservatives, and artificial sweeteners contained in commercial gargles are necessary for evaluating their effectiveness, safety, ...Simple, reliable and sensitive analytical methods to determine anticariogenic agents, preservatives, and artificial sweeteners contained in commercial gargles are necessary for evaluating their effectiveness, safety, and quality. An ion chroma-tography (IC) method has been described to analyze simultaneously eight anions including fluoride, chloride, sulfate, phosphate, monofluorophosphate, glycerophosphate (anticariogenic agents), sorbate (a preservative), and saccharin (an artificial sweetener) in gargles. In this IC system, we applied a mobile phased gradient elution with KOH, separation by IonPac AS18 columns, and suppressed conductivity detection. Optimized analytical conditions were further evaluated for accuracy. The relative standard deviations (RSDs) of the inter-day's retention time and peak area of all species were less than 0.938% and 8.731%, respectively, while RSDs of 5-day retention time and peak area were less than 1.265% and 8.934%, respectively. The correlation coefficients for targeted analytes ranged from 0.999 7 to 1.000 0. The spiked recoveries for the anions were 90%~102.5%. We concluded that the method can be applied for comprehensive evaluation of commercial gargles.展开更多
A simple, sensitive and convenient ion chromatography(IC) method was established for the simultaneous determination of twelve water-soluble inorganic anions(F -, Cl -, NO - 2, NO - 3, SO 2- 3, SO 2- ...A simple, sensitive and convenient ion chromatography(IC) method was established for the simultaneous determination of twelve water-soluble inorganic anions(F -, Cl -, NO - 2, NO - 3, SO 2- 3, SO 2- 4, PO 3- 4), and fifteen water-soluble organic ions(formate, acetate, MSA, oxalate, malonate, succinate, phthalates, etc.) in atmospheric aerosols. The linear concentrations ranged from 0.005 μg/m 3 to 500 μg/m 3(r = 0.999—0.9999). The relative standard deviation(RSD) were 0.43%—2.00% and the detection limits were from 2.7 ng/m 3 to 88 ng/m 3. The proposed method was successfully applied to the simultaneous determination of those inorganic ions and organic ions in PM 2.5 of Beijing.展开更多
A new method for the simultaneous determination of fluorine and iodine in urine by ion chromatography （IC） with electrochemical pretreatment has been developed. The pretreatment was performed in a novel electrochemi...A new method for the simultaneous determination of fluorine and iodine in urine by ion chromatography （IC） with electrochemical pretreatment has been developed. The pretreatment was performed in a novel electrochemical oxidationneutralization device （EOND）, in which iodide of the sample was oxidized to iodate and the alkaline digestion sample solution was neutralized. Under the optimized conditions, the limits of detection （LOD, S/N = 3） were 2.5 μg/L for fluoride and 20 μg/L for iodate, respectively. The recoveries were in the range of 93-102% for fluoride and 86-98% for iodate.展开更多
For preparing fluorinated quinolone antibiotic medicine locally used in stomatology, simultaneous determination of norfloxacin, ciprofloxacin, and enoxacin was carried out by multiphase ion chromatography with fluores...For preparing fluorinated quinolone antibiotic medicine locally used in stomatology, simultaneous determination of norfloxacin, ciprofloxacin, and enoxacin was carried out by multiphase ion chromatography with fluorescence detection. Quinolone antibiotics were separated by Dionex OmniPac PAX-500 column with an eluent of 15 mmol/L H2SO4 and 35% methanol （v/v） at a flow-rate of 1.0 ml/min and detected with fluorescence with excitation and emission wave lengths of 347 ran and 420 ran respectively. The detection limits （S/N=3） of norfloxacin, ciprofloxacin and enoxacin were 50, 105 and 80 ng/ml respectively. The relative standard deviations of retention time, peak area and peak height were less than 1.1% and good linear relationship resulted. The developed method was applied to pharmaceutical formulations and biological fluids.展开更多
A method for the simultaneous separation and determination of organic acids and inorganic anions in Bayer liquors was developed by gradient ion chromatography with suppressed conductivity detection. Formate, acetate, ...A method for the simultaneous separation and determination of organic acids and inorganic anions in Bayer liquors was developed by gradient ion chromatography with suppressed conductivity detection. Formate, acetate, propionate, oxalate, succinate, glutarate, fluoride, chloride and sulfate were separated and determined in 33 min. The samples were pretreated with solid-phase extraction, which has high selectivity for removing a large number of metallic ions in the Bayer liquors, and filtered with a 0.45 μm filter membrane before being injected into the ion chromatographic system. The separation of six organic acids and three inorganic anions was achieved on an IonPac AS11-HC column with KOH as the eluent, and the detection was performed by a conductivity detection mode. 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. The relative standard derivation of the peak area of analytes is less than 2.14%. Under optimum conditions the detection ranges from 0.2 to 100.0 mg/L. The average recoveries of the added standards are between 94.3% and 102.8%.展开更多
The ion chromatography combined solid phase extraction （SPE） method was developed for the analysis of low concentration haloacetic acids （HAAs）, a class of disinfection by-products formed from chlorination of hosp...The ion chromatography combined solid phase extraction （SPE） method was developed for the analysis of low concentration haloacetic acids （HAAs）, a class of disinfection by-products formed from chlorination of hospital wastewater. The monitored HAAs included monochloroacetic acid, monobromoacetic acid, dichloroacetic acid, dibromoacetic acid and trichloroacetic acid. The method employed a sodium hydroxide eluent at a flow rate of 0.8 ml/min, electrolytically generated gradients, and suppressed conductivity detection. To analyze the HAAs in real hospital wastewater samples, C18 pretreatment cartridge was utilized to reduce samples＇ turbidity. Preconcentration with SPE and matrix elimination with treatment cartridges were investigated and found to be able to obtain acceptable detection limits. Linearity, repeatability and detection limits of the above method were evaluated. The detection limits of monobromoacetic acid and dibromoacetic acid were 2.61 μg/L and 1.30 μg/L, respectively, and the other three acids are ranging from 0.48 to 0.82μg/L under 25-fold preconcentration. When the above optimization procedure was applied to three hospital wastewater samples with different treatment processes in Tianjin, it was found that the dichloroacetic acid was the major compound, and the growth ratios of the HAAs after disinfection by sodium hypochlorite were 91.28%, 63.61% and 79.50%, respectively.展开更多
An ion chromatographic method with a valve switching facility was developed to determine trace nitrate concentrations in seawater using two pumps, two different suppressors, and two columns. A carbohydrate membrane de...An ion chromatographic method with a valve switching facility was developed to determine trace nitrate concentrations in seawater using two pumps, two different suppressors, and two columns. A carbohydrate membrane desalter was used to reduce the high concentrations of sodium salts in samples. In this method, trace nitrate was eluted from the concentrator column to the analytical columns, while the matrix fl owed to waste. Neither chemical pre-treatment nor sample dilution was required. In the optimized separation conditions, the method showed good linearity( R >0.99) in the 0.05 and 50 mg/L concentration range, and satisfactory repeatability(RSD<5%, n =6). The limit of detection for nitrate was 0.02 mg/L. Results showed that the valve switching system was suitable and practical for the determination of trace nitrate in seawater.展开更多
Ion chromatography-ultra violet-hydride generation-Atomic Florescence Spectrometry was applied to detect 5 arsenic species in seafoods. The arsenic species studied include arsenobetaine(As B), arsenite(As(III)), dimet...Ion chromatography-ultra violet-hydride generation-Atomic Florescence Spectrometry was applied to detect 5 arsenic species in seafoods. The arsenic species studied include arsenobetaine(As B), arsenite(As(III)), dimethylarsinic acid(DMA), monomethylarsonic acid(MMA), and arsenate(As(V)), which were extracted from samples using 2% formic acid. Gradient elution using 33 mmol L^(-1) CH_3COONH_4 and 15 mmol L^(-1) Na_2CO_3 with 10 mL CH_3CH_2OH at pH 8.4 allowed the chromatographic separation of all the species on a Hamilton PRP-X100 anion-exchange column in less than 8 min. In this study, an ultrasound extraction method was used to extract arsenic species from seafood. The extraction efficiency was good and the recoveries from spiked samples were in the range of 72.6%–109%; the precision between sample replicates was higher than 3.6% for all determinations. The detection limits were 3.543 μg L^(-1) for As B, 0.4261 μg L^(-1) for As(III), 0.216 μg L^(-1) for DMA, 0.211 μg L^(-1) for MMA, and 0.709 μg L^(-1) for As(V), and the linear coefficients were greater than 0.999. We also developed an application of this method for the determination of arsenic species in bonito, Euphausia superba, and Enteromorpha with satisfactory results. Therefore, it was confirmed that this method was appropriate for the detection of arsenic species in seafood.展开更多
A novel method for determination of formaldehyde sulfoxylate, sulfite, thiocyanate, and thiosulfate in foodstuffs by ion chromatography separation with postcolumn derivation and UV detection has been developed. All sp...A novel method for determination of formaldehyde sulfoxylate, sulfite, thiocyanate, and thiosulfate in foodstuffs by ion chromatography separation with postcolumn derivation and UV detection has been developed. All species are separated at Dionex IonPac AG22A and AS22A with mobile phase of a mixture of 4.5 mmol/L sodium carbonate and 0.8 mmol/L sodium bicarbonate at a flow-rate of 1.0 mL/min. The postcolunm derivation solution was 0.24% iodine in 0.2% phosphate acid and the detection wavelength was set at 288 nm. The detection limits （LOD, signal-to-noise ratio of 3） of formaldehyde sulfoxylate, sulfite, thiocyanate, and thiosulfate were 0.004, 0.006, 0.006, and 0.007 mg/L, respectively. Within-day relative standard deviations （RSD, n = 10） of formaldehyde sulfoxylate, sulflte, thiocyanate, and thiosulfate were 3.24%, 3.76%, 2.68%, and 2.07%, respectively. The recoveries of the four anions were in the range of 67.2-116.5%.展开更多
In order to verify the accuracy of ion chromatography for cyanide detection,optimization conditions were studied,and comparison was made for the detection results of cyanide between titration and isonicotinic acid pyr...In order to verify the accuracy of ion chromatography for cyanide detection,optimization conditions were studied,and comparison was made for the detection results of cyanide between titration and isonicotinic acid pyrazolone spectrophotometry. The results showed that ion chromatography has good linearity and reproducibility,with the recovery rate of 95%-105% and the limit of detection of 0. 001 mg/L. This method is simple,rapid,safe,selective,and suitable for the determination of cyanide in pollution-free livestock product breeding water.展开更多
In this work, a novel hollow fiber membrane extractor was set up to extract inorganic anions from ethyl acetate using deionized water. Inorganic anions in slightly soluble organic solvents can be determined by the in-...In this work, a novel hollow fiber membrane extractor was set up to extract inorganic anions from ethyl acetate using deionized water. Inorganic anions in slightly soluble organic solvents can be determined by the in-line hollow fiber membrane extractor coupled with ion chromatography at first time. Different aspects of the extraction procedure such as magnetic stirring speed, extraction flow rate and extraction time were optimized to achieve high extraction efficiency and good separation results. Satisfactory linear range, limits of detection and good repeatability were obtained. The procedure was applied to analyze inorganic anions in two commercial ethyl acetate samples.展开更多
In the present work, a novel analytical method was proposed for the determination of toluene diisocyanate （TDI） in syntheticrubber track by ion chromatography （IC） coupled with an ultraviolet detector setting at 2...In the present work, a novel analytical method was proposed for the determination of toluene diisocyanate （TDI） in syntheticrubber track by ion chromatography （IC） coupled with an ultraviolet detector setting at 212 nm. TDI can be hydrolyzed to toluene diamine （TDA） which can be separated by cation-exchange IC easily. The optimum IC separation was performed on an IonPac CS12A column （150 mm ×4.0 mm） using 20 mmol L^-1 sodium sulfate, 10 mmol L^-1 sulfuric acid and 10% acetonitrile as eluent. It was found that a higher signal response of TDA could be obtained under alkaline condition. A suppressor was used to change the acidic eluent into alkaline one. 0.8 mol L^-1 potassium hydroxide was chosen as the optimum regeneration eluent. With the added suppressor and regenerant, signal response was magnified by about 16 times and lower limit of detection （LOD, 0.13 μg L^-1） was obtained. Within-day relative standard deviation （R.S.D.） was less than 3.6%. The recoveries of TDI spiked in synthetic-rubber track samoles were 96.4-110.6%.展开更多
Ion chromatography （IC） is a suitable analytical method for the determination of anions. As analytical methods for the halogen compounds in flue gas, those of bromine compound, fluorine compound, chlorine （Cl2） an...Ion chromatography （IC） is a suitable analytical method for the determination of anions. As analytical methods for the halogen compounds in flue gas, those of bromine compound, fluorine compound, chlorine （Cl2） and hydrogen chloride （HCI） are listed in JIS. However, IC has not been adopted in JIS except for HCI and C12. Because the carbon dioxide in flue gas is absorbed in a 0.1 M sodium hydroxide solution as an absorber, it is interfered with the measurement of F^- and Cl^- ions. This paper describes the development of the pretreatment equipment for the flue gas analysis by IC, and its applications to real flue gas analysis. The F^-, Cl^-, Br^- and SO4^2- in the absorbing solution can be clearly separated by IC using the pretreatment equipment. The halogen compounds and sulfur oxides in flue gas can be simultaneously determined by IC.展开更多
The analysis of hexavalent chromium, Cr(VI), in soil and sediment samples has been predominantly carried out in materials containing elevated levels. Reliable analysis of trace-level of Cr(VI) in sediment samples rema...The analysis of hexavalent chromium, Cr(VI), in soil and sediment samples has been predominantly carried out in materials containing elevated levels. Reliable analysis of trace-level of Cr(VI) in sediment samples remains challenging. Cr(VI) analyses with multipoint calibration and speciated isotope dilution (SID) adapted from U.S. EPA method 6800 were used to measure lower-level Cr(VI) on an ion chromatograph coupled with a tandem mass spectrometer (IC-MS/MS). Lake sediment samples were collected from various locations in Northern Ontario and Cr(VI) was extracted using both alkaline digestion and ethylene diaminetetraacetic acid (EDTA) extraction. Certified reference materials were extracted and analyzed by IC-MS/MS and UV-VIS detection. The SID-MS approach allowed for the quantification of Cr(VI) in samples with concentration levels below 0.5 μg.g-1 wet weight.展开更多
The application of non-suppressed ion chromatography for monitoring of trace elements in air particulate matter was studied in the present investigation. The results indicate that the use of microwave acid digestion m...The application of non-suppressed ion chromatography for monitoring of trace elements in air particulate matter was studied in the present investigation. The results indicate that the use of microwave acid digestion method is superior in comparison with the conventional thermal acid digestion method as it leads to higher recovery, better reproducibility, lower volatility loss, better protection against environmental contamination and much less digestion time (5 minutes vs. 24 hours). The use of eluent as extractant is shown to reduce the water dip problem in the chro-matogram. The addition of chelating agent in the eluent coupled with UV detection is shown to provide satisfactory chromatographic separation and good sensitivity for the analysis of transition metals present in the air particulate matter. Using the U.S. National Bureau of Standards Reference Material 1648 Urban Particulate Matter as standard for checking, the analytical procedure is shown to give good recovery and reproducibility for the detection of the following cations and anions in air particulate matter: Fe2 Cu, Mn, Pb, Zn, Mg, Na, HN4+, Cl-, NO3- and SO42-. Field test was also performed to check the applicability of the method and the results obtained were discussed in the present paper.展开更多
In this research, a glassy carbon electrode modified with the functionalized multi-wall carbon nanotubes(MWNT-COOHs) film was used as an amperometric sensor for the determination of S_2O^(2-)_3, SO^(2-)_3, I^- and SCN...In this research, a glassy carbon electrode modified with the functionalized multi-wall carbon nanotubes(MWNT-COOHs) film was used as an amperometric sensor for the determination of S_2O^(2-)_3, SO^(2-)_3, I^- and SCN^-. The electrochemical behavior of those oxidizable inorganic anions at this modified electrode was studied by means of cyclic voltammetry(CV). The experimental results indicate that the modified electrode exhibits a high electrocatalytic activity towards the oxidation of those anions with a relatively high sensitivity, a good stability and a long-life. Separated by ion chromatography(IC) with 1.25 mmol/L H_2SO_4 as an eluent, those oxidizable anions can be determined by the MWNT-COOHs modified electrode successfully. Under the optimal chromatographic conditions, the detection limits are 1.5×10^(-7) mol/L for S_2O^(2-)_3, 2.5×10^(-7) mol/L for SO^(2-)_3, 1.2×10^(-7) mol/L for I^- and 2.0×10^(-7) mol/L for SCN^-, respectively. The method was applied successfully to the determination of those anions in environmental water展开更多
The research aimed to develop and validate an ion chromatography method for the simultaneous analysis of Cr(Ⅲ) and Cr(Ⅵ)from pumpkin. A new analytical method based on ion chromatography techniques was developed by t...The research aimed to develop and validate an ion chromatography method for the simultaneous analysis of Cr(Ⅲ) and Cr(Ⅵ)from pumpkin. A new analytical method based on ion chromatography techniques was developed by the Cr(Ⅲ) pre-column derivatization and Cr(Ⅵ) post-column derivatization. The ion chromatography condition was optimized and the detection sensitivity was improved. Cr(Ⅲ) and Cr(Ⅵ) were determined by 365 and 530 nm,respectively. The temperature of water bath,the heating time for pre-column derivatization,and the flow rate of post-column derivative liquid were screened on the basis of single factor experiment,the effects of various factors were determined by the method of L16( 43) orthogonal experiment design. Considering the results of orthogonal experiments and the variation tendency of peak area under different factors,the optimum derivatization conditions were chose as follows: the flow rate of post-column derivative liquid is0. 5 m L/min,the temperature of water bath for pre-column derivatization is 100 ℃ and the heating time is 5 min. The conditions were optimized by means of orthogonal experiments under the p H of leacheate ranged from 6. 5 to 6. 8 and the I-concentration of 5 mmol/L. Under optimized derivatization conditions,the detection limits for Cr(Ⅲ) and Cr(Ⅵ) were 0. 17 and 0. 019 mg,respectively. And the average recoveries of Cr(Ⅲ) in pumpkin were in the range of 82%-85%. Results indicated that pumpkin does not contain Cr(Ⅵ) according to this ion chromatography method of simultaneously determination for Cr(Ⅲ) and Cr(Ⅵ).展开更多
A chromatographic analysis method for determining inorganic anions and melamine in fertilizers was established using ion chromatography(IC).The fertilizer samples were extracted by ultrasonic method with 7 g/L trichlo...A chromatographic analysis method for determining inorganic anions and melamine in fertilizers was established using ion chromatography(IC).The fertilizer samples were extracted by ultrasonic method with 7 g/L trichloroacetic acid solution and centrifuged.The supernatant is purified by a solid phase extraction column.Then,the anions in the solution were purified using SH-AP-1(250 mm×4.0 mm)as a separation column,and measured by a suppressed conductivity detector;the melamine in the solution was separated using SH-CC-4(200 mm×4.0 mm)as a separation column and detected by a UV detector.The results show that the mass concentration of anions had a linear relationship with its peak area within a certain range,the linear correlation coefficient r of the standard curve was greater than 0.999,the recovery rate of spiked samples was 93.4%-104.4%,and the relative standard deviation(RSD)of the measured value(n=6)was less than 4%.Thus,this method is widely suitable for detection of anions and cations in a variety of fertilizer samples.展开更多
基金Supported by Changsha Key Project in Hunan Province(K1005007-21)~~
文摘[Objective] The aim was to analyze sugar components in fermented rice wine by ion chromatography. [Method] The optimal condition for chromatography system of sugar analysis was selected by measuring sugars in fermented rice wine with ion chromatography and pulsed amperometric detection. [Result] The optimal measurement conditions were as follows： Leacheate （Leachate）, consisting of NaOH and CH3COONa, was eluted by gradient concentrations, with column temperature at 35 ℃ and flow rate at 0.4 ml/min. In the condition, sugars in rice wine were ana- lyzed and the results showed that the method is featured by low detection limit, good repetition and high recovery rate. [Conclusion] The research establishes and determines the approaches and optimum conditions for sugar analysis in rice wine by ion chromatography and pulsed amperometric detection, providing references for advancement of research on quality improvement of fermented rice wine.
文摘A method was developed for determination of chlorine and bromine in plant materials by ion chromatography using temperature programing-semi molten for sample preparation. Values of detection limits of the method found were 1.0×10^-5 for CI and 1.3×10^-6 for Br. The measuring range of the method found were 0.3-20.0 mg/L for CI and 4,0-120,0 μg/L for Br. The results obtained agreed quite well with those reference values.
基金Project supported by the National Natural Science Foundation of China (Nos. 20375035 and 20527005)the Natural Science Foundation of Zhejiang Province, China (Nos. Z404105 and Y405415)the Science and Technology Department of Zhejiang Province, China (No. 2007C33016)
文摘Simple, reliable and sensitive analytical methods to determine anticariogenic agents, preservatives, and artificial sweeteners contained in commercial gargles are necessary for evaluating their effectiveness, safety, and quality. An ion chroma-tography (IC) method has been described to analyze simultaneously eight anions including fluoride, chloride, sulfate, phosphate, monofluorophosphate, glycerophosphate (anticariogenic agents), sorbate (a preservative), and saccharin (an artificial sweetener) in gargles. In this IC system, we applied a mobile phased gradient elution with KOH, separation by IonPac AS18 columns, and suppressed conductivity detection. Optimized analytical conditions were further evaluated for accuracy. The relative standard deviations (RSDs) of the inter-day's retention time and peak area of all species were less than 0.938% and 8.731%, respectively, while RSDs of 5-day retention time and peak area were less than 1.265% and 8.934%, respectively. The correlation coefficients for targeted analytes ranged from 0.999 7 to 1.000 0. The spiked recoveries for the anions were 90%~102.5%. We concluded that the method can be applied for comprehensive evaluation of commercial gargles.
文摘A simple, sensitive and convenient ion chromatography(IC) method was established for the simultaneous determination of twelve water-soluble inorganic anions(F -, Cl -, NO - 2, NO - 3, SO 2- 3, SO 2- 4, PO 3- 4), and fifteen water-soluble organic ions(formate, acetate, MSA, oxalate, malonate, succinate, phthalates, etc.) in atmospheric aerosols. The linear concentrations ranged from 0.005 μg/m 3 to 500 μg/m 3(r = 0.999—0.9999). The relative standard deviation(RSD) were 0.43%—2.00% and the detection limits were from 2.7 ng/m 3 to 88 ng/m 3. The proposed method was successfully applied to the simultaneous determination of those inorganic ions and organic ions in PM 2.5 of Beijing.
文摘A new method for the simultaneous determination of fluorine and iodine in urine by ion chromatography （IC） with electrochemical pretreatment has been developed. The pretreatment was performed in a novel electrochemical oxidationneutralization device （EOND）, in which iodide of the sample was oxidized to iodate and the alkaline digestion sample solution was neutralized. Under the optimized conditions, the limits of detection （LOD, S/N = 3） were 2.5 μg/L for fluoride and 20 μg/L for iodate, respectively. The recoveries were in the range of 93-102% for fluoride and 86-98% for iodate.
基金Project supported by the National Natural Science Foundation of China (Nos.20375035 and 20527005)the Natural Science Foundation of Zhejiang Province (No.Z404105), China
文摘For preparing fluorinated quinolone antibiotic medicine locally used in stomatology, simultaneous determination of norfloxacin, ciprofloxacin, and enoxacin was carried out by multiphase ion chromatography with fluorescence detection. Quinolone antibiotics were separated by Dionex OmniPac PAX-500 column with an eluent of 15 mmol/L H2SO4 and 35% methanol （v/v） at a flow-rate of 1.0 ml/min and detected with fluorescence with excitation and emission wave lengths of 347 ran and 420 ran respectively. The detection limits （S/N=3） of norfloxacin, ciprofloxacin and enoxacin were 50, 105 and 80 ng/ml respectively. The relative standard deviations of retention time, peak area and peak height were less than 1.1% and good linear relationship resulted. The developed method was applied to pharmaceutical formulations and biological fluids.
基金Project(2005CB623702) supported by the National Key Basic Research Program of China
文摘A method for the simultaneous separation and determination of organic acids and inorganic anions in Bayer liquors was developed by gradient ion chromatography with suppressed conductivity detection. Formate, acetate, propionate, oxalate, succinate, glutarate, fluoride, chloride and sulfate were separated and determined in 33 min. The samples were pretreated with solid-phase extraction, which has high selectivity for removing a large number of metallic ions in the Bayer liquors, and filtered with a 0.45 μm filter membrane before being injected into the ion chromatographic system. The separation of six organic acids and three inorganic anions was achieved on an IonPac AS11-HC column with KOH as the eluent, and the detection was performed by a conductivity detection mode. 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. The relative standard derivation of the peak area of analytes is less than 2.14%. Under optimum conditions the detection ranges from 0.2 to 100.0 mg/L. The average recoveries of the added standards are between 94.3% and 102.8%.
基金Project supported by the Hi-Tech Research and Development Program(863) of China (No. 2003AA601130).
文摘The ion chromatography combined solid phase extraction （SPE） method was developed for the analysis of low concentration haloacetic acids （HAAs）, a class of disinfection by-products formed from chlorination of hospital wastewater. The monitored HAAs included monochloroacetic acid, monobromoacetic acid, dichloroacetic acid, dibromoacetic acid and trichloroacetic acid. The method employed a sodium hydroxide eluent at a flow rate of 0.8 ml/min, electrolytically generated gradients, and suppressed conductivity detection. To analyze the HAAs in real hospital wastewater samples, C18 pretreatment cartridge was utilized to reduce samples＇ turbidity. Preconcentration with SPE and matrix elimination with treatment cartridges were investigated and found to be able to obtain acceptable detection limits. Linearity, repeatability and detection limits of the above method were evaluated. The detection limits of monobromoacetic acid and dibromoacetic acid were 2.61 μg/L and 1.30 μg/L, respectively, and the other three acids are ranging from 0.48 to 0.82μg/L under 25-fold preconcentration. When the above optimization procedure was applied to three hospital wastewater samples with different treatment processes in Tianjin, it was found that the dichloroacetic acid was the major compound, and the growth ratios of the HAAs after disinfection by sodium hypochlorite were 91.28%, 63.61% and 79.50%, respectively.
基金Supported by the National Special Fund for Major Research Instrumentation Development(No.2012YQ090229)the Instrument Functional Exploitation and Technical Innovation Fund,Chinese Academy of Sciences(No.yg2010072)the Shandong Provincial Technology Development Plan Fund(Nos.2011SJGZ06,2012SJGZ12,2012424012)
文摘An ion chromatographic method with a valve switching facility was developed to determine trace nitrate concentrations in seawater using two pumps, two different suppressors, and two columns. A carbohydrate membrane desalter was used to reduce the high concentrations of sodium salts in samples. In this method, trace nitrate was eluted from the concentrator column to the analytical columns, while the matrix fl owed to waste. Neither chemical pre-treatment nor sample dilution was required. In the optimized separation conditions, the method showed good linearity( R >0.99) in the 0.05 and 50 mg/L concentration range, and satisfactory repeatability(RSD<5%, n =6). The limit of detection for nitrate was 0.02 mg/L. Results showed that the valve switching system was suitable and practical for the determination of trace nitrate in seawater.
基金funded by the National Major ScientificInstrument and Equipment Development Project of China (No.2012YQ090229)
文摘Ion chromatography-ultra violet-hydride generation-Atomic Florescence Spectrometry was applied to detect 5 arsenic species in seafoods. The arsenic species studied include arsenobetaine(As B), arsenite(As(III)), dimethylarsinic acid(DMA), monomethylarsonic acid(MMA), and arsenate(As(V)), which were extracted from samples using 2% formic acid. Gradient elution using 33 mmol L^(-1) CH_3COONH_4 and 15 mmol L^(-1) Na_2CO_3 with 10 mL CH_3CH_2OH at pH 8.4 allowed the chromatographic separation of all the species on a Hamilton PRP-X100 anion-exchange column in less than 8 min. In this study, an ultrasound extraction method was used to extract arsenic species from seafood. The extraction efficiency was good and the recoveries from spiked samples were in the range of 72.6%–109%; the precision between sample replicates was higher than 3.6% for all determinations. The detection limits were 3.543 μg L^(-1) for As B, 0.4261 μg L^(-1) for As(III), 0.216 μg L^(-1) for DMA, 0.211 μg L^(-1) for MMA, and 0.709 μg L^(-1) for As(V), and the linear coefficients were greater than 0.999. We also developed an application of this method for the determination of arsenic species in bonito, Euphausia superba, and Enteromorpha with satisfactory results. Therefore, it was confirmed that this method was appropriate for the detection of arsenic species in seafood.
基金supported by National Natural Science Foundation of China(No.20775070) Zhejiang Provincial Natural Science Foundation of China(No.Y507252)+1 种基金Zhejiang Qianjiang Project of Science and Technology for Competent People(No.2008R10028) Zhejiang Provincial Analysis and Testing Foundation of China(No.2007F70061)
文摘A novel method for determination of formaldehyde sulfoxylate, sulfite, thiocyanate, and thiosulfate in foodstuffs by ion chromatography separation with postcolumn derivation and UV detection has been developed. All species are separated at Dionex IonPac AG22A and AS22A with mobile phase of a mixture of 4.5 mmol/L sodium carbonate and 0.8 mmol/L sodium bicarbonate at a flow-rate of 1.0 mL/min. The postcolunm derivation solution was 0.24% iodine in 0.2% phosphate acid and the detection wavelength was set at 288 nm. The detection limits （LOD, signal-to-noise ratio of 3） of formaldehyde sulfoxylate, sulfite, thiocyanate, and thiosulfate were 0.004, 0.006, 0.006, and 0.007 mg/L, respectively. Within-day relative standard deviations （RSD, n = 10） of formaldehyde sulfoxylate, sulflte, thiocyanate, and thiosulfate were 3.24%, 3.76%, 2.68%, and 2.07%, respectively. The recoveries of the four anions were in the range of 67.2-116.5%.
文摘In order to verify the accuracy of ion chromatography for cyanide detection,optimization conditions were studied,and comparison was made for the detection results of cyanide between titration and isonicotinic acid pyrazolone spectrophotometry. The results showed that ion chromatography has good linearity and reproducibility,with the recovery rate of 95%-105% and the limit of detection of 0. 001 mg/L. This method is simple,rapid,safe,selective,and suitable for the determination of cyanide in pollution-free livestock product breeding water.
基金supported by National Natural Science Foundation of China(No.20775070)by Zhejiang Provincial Natural Science Foundation of China(No.R4080124)Zhejiang Qianjiang Project of Science and Technology for Competent People(No.2008R10028).
文摘In this work, a novel hollow fiber membrane extractor was set up to extract inorganic anions from ethyl acetate using deionized water. Inorganic anions in slightly soluble organic solvents can be determined by the in-line hollow fiber membrane extractor coupled with ion chromatography at first time. Different aspects of the extraction procedure such as magnetic stirring speed, extraction flow rate and extraction time were optimized to achieve high extraction efficiency and good separation results. Satisfactory linear range, limits of detection and good repeatability were obtained. The procedure was applied to analyze inorganic anions in two commercial ethyl acetate samples.
基金supported by the National Natural Science Foundation of China(No.20775070)Zhejiang Provincial Natural Science Foundation of China(No.Y507252).
文摘In the present work, a novel analytical method was proposed for the determination of toluene diisocyanate （TDI） in syntheticrubber track by ion chromatography （IC） coupled with an ultraviolet detector setting at 212 nm. TDI can be hydrolyzed to toluene diamine （TDA） which can be separated by cation-exchange IC easily. The optimum IC separation was performed on an IonPac CS12A column （150 mm ×4.0 mm） using 20 mmol L^-1 sodium sulfate, 10 mmol L^-1 sulfuric acid and 10% acetonitrile as eluent. It was found that a higher signal response of TDA could be obtained under alkaline condition. A suppressor was used to change the acidic eluent into alkaline one. 0.8 mol L^-1 potassium hydroxide was chosen as the optimum regeneration eluent. With the added suppressor and regenerant, signal response was magnified by about 16 times and lower limit of detection （LOD, 0.13 μg L^-1） was obtained. Within-day relative standard deviation （R.S.D.） was less than 3.6%. The recoveries of TDI spiked in synthetic-rubber track samoles were 96.4-110.6%.
文摘Ion chromatography （IC） is a suitable analytical method for the determination of anions. As analytical methods for the halogen compounds in flue gas, those of bromine compound, fluorine compound, chlorine （Cl2） and hydrogen chloride （HCI） are listed in JIS. However, IC has not been adopted in JIS except for HCI and C12. Because the carbon dioxide in flue gas is absorbed in a 0.1 M sodium hydroxide solution as an absorber, it is interfered with the measurement of F^- and Cl^- ions. This paper describes the development of the pretreatment equipment for the flue gas analysis by IC, and its applications to real flue gas analysis. The F^-, Cl^-, Br^- and SO4^2- in the absorbing solution can be clearly separated by IC using the pretreatment equipment. The halogen compounds and sulfur oxides in flue gas can be simultaneously determined by IC.
文摘The analysis of hexavalent chromium, Cr(VI), in soil and sediment samples has been predominantly carried out in materials containing elevated levels. Reliable analysis of trace-level of Cr(VI) in sediment samples remains challenging. Cr(VI) analyses with multipoint calibration and speciated isotope dilution (SID) adapted from U.S. EPA method 6800 were used to measure lower-level Cr(VI) on an ion chromatograph coupled with a tandem mass spectrometer (IC-MS/MS). Lake sediment samples were collected from various locations in Northern Ontario and Cr(VI) was extracted using both alkaline digestion and ethylene diaminetetraacetic acid (EDTA) extraction. Certified reference materials were extracted and analyzed by IC-MS/MS and UV-VIS detection. The SID-MS approach allowed for the quantification of Cr(VI) in samples with concentration levels below 0.5 μg.g-1 wet weight.
文摘The application of non-suppressed ion chromatography for monitoring of trace elements in air particulate matter was studied in the present investigation. The results indicate that the use of microwave acid digestion method is superior in comparison with the conventional thermal acid digestion method as it leads to higher recovery, better reproducibility, lower volatility loss, better protection against environmental contamination and much less digestion time (5 minutes vs. 24 hours). The use of eluent as extractant is shown to reduce the water dip problem in the chro-matogram. The addition of chelating agent in the eluent coupled with UV detection is shown to provide satisfactory chromatographic separation and good sensitivity for the analysis of transition metals present in the air particulate matter. Using the U.S. National Bureau of Standards Reference Material 1648 Urban Particulate Matter as standard for checking, the analytical procedure is shown to give good recovery and reproducibility for the detection of the following cations and anions in air particulate matter: Fe2 Cu, Mn, Pb, Zn, Mg, Na, HN4+, Cl-, NO3- and SO42-. Field test was also performed to check the applicability of the method and the results obtained were discussed in the present paper.
基金supported by the National Natural Science Foundation of China(No.2 0 175 0 0 6 ) and Nano Projects from Shanghai Sci-ence and Technology Com mittee(No.0 2 14 nm0 78and0 35 9nm0 0 2 )
文摘In this research, a glassy carbon electrode modified with the functionalized multi-wall carbon nanotubes(MWNT-COOHs) film was used as an amperometric sensor for the determination of S_2O^(2-)_3, SO^(2-)_3, I^- and SCN^-. The electrochemical behavior of those oxidizable inorganic anions at this modified electrode was studied by means of cyclic voltammetry(CV). The experimental results indicate that the modified electrode exhibits a high electrocatalytic activity towards the oxidation of those anions with a relatively high sensitivity, a good stability and a long-life. Separated by ion chromatography(IC) with 1.25 mmol/L H_2SO_4 as an eluent, those oxidizable anions can be determined by the MWNT-COOHs modified electrode successfully. Under the optimal chromatographic conditions, the detection limits are 1.5×10^(-7) mol/L for S_2O^(2-)_3, 2.5×10^(-7) mol/L for SO^(2-)_3, 1.2×10^(-7) mol/L for I^- and 2.0×10^(-7) mol/L for SCN^-, respectively. The method was applied successfully to the determination of those anions in environmental water
基金Supported by Science and Technology Innovation Ability Construction Special Item of Beijing Academy of Agriculture and Forestry Sciences(KJCX20140302,KJCX20140111)
文摘The research aimed to develop and validate an ion chromatography method for the simultaneous analysis of Cr(Ⅲ) and Cr(Ⅵ)from pumpkin. A new analytical method based on ion chromatography techniques was developed by the Cr(Ⅲ) pre-column derivatization and Cr(Ⅵ) post-column derivatization. The ion chromatography condition was optimized and the detection sensitivity was improved. Cr(Ⅲ) and Cr(Ⅵ) were determined by 365 and 530 nm,respectively. The temperature of water bath,the heating time for pre-column derivatization,and the flow rate of post-column derivative liquid were screened on the basis of single factor experiment,the effects of various factors were determined by the method of L16( 43) orthogonal experiment design. Considering the results of orthogonal experiments and the variation tendency of peak area under different factors,the optimum derivatization conditions were chose as follows: the flow rate of post-column derivative liquid is0. 5 m L/min,the temperature of water bath for pre-column derivatization is 100 ℃ and the heating time is 5 min. The conditions were optimized by means of orthogonal experiments under the p H of leacheate ranged from 6. 5 to 6. 8 and the I-concentration of 5 mmol/L. Under optimized derivatization conditions,the detection limits for Cr(Ⅲ) and Cr(Ⅵ) were 0. 17 and 0. 019 mg,respectively. And the average recoveries of Cr(Ⅲ) in pumpkin were in the range of 82%-85%. Results indicated that pumpkin does not contain Cr(Ⅵ) according to this ion chromatography method of simultaneously determination for Cr(Ⅲ) and Cr(Ⅵ).
文摘A chromatographic analysis method for determining inorganic anions and melamine in fertilizers was established using ion chromatography(IC).The fertilizer samples were extracted by ultrasonic method with 7 g/L trichloroacetic acid solution and centrifuged.The supernatant is purified by a solid phase extraction column.Then,the anions in the solution were purified using SH-AP-1(250 mm×4.0 mm)as a separation column,and measured by a suppressed conductivity detector;the melamine in the solution was separated using SH-CC-4(200 mm×4.0 mm)as a separation column and detected by a UV detector.The results show that the mass concentration of anions had a linear relationship with its peak area within a certain range,the linear correlation coefficient r of the standard curve was greater than 0.999,the recovery rate of spiked samples was 93.4%-104.4%,and the relative standard deviation(RSD)of the measured value(n=6)was less than 4%.Thus,this method is widely suitable for detection of anions and cations in a variety of fertilizer samples.
