色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2009年
6期
825-828
,共4页
尹丽倩%袁东星%郭娟%刘锡尧
尹麗倩%袁東星%郭娟%劉錫堯
윤려천%원동성%곽연%류석요
离子色谱法%亚硫酸根离子%烟气脱硫%海水
離子色譜法%亞硫痠根離子%煙氣脫硫%海水
리자색보법%아류산근리자%연기탈류%해수
ion chromatography (IC)%sulfite%flue gas desulfurization%seawater
建立了燃煤电厂烟气脱硫海水中亚硫酸根(SO~(2-)_3)的离子色谱-脉冲安培检测方法.色谱柱为IonPac AS14A阴离子交换柱,流动相为14 mmol/L NaOH-12 mmol/L Na_2CO_3溶液(pH 11.7),流速1.2 mL/min,脉冲安培法检测.因SO~(2-)_3 易被氧化,故在采样时加入甲醛作为保护剂,使之稳定存在.在测定海水样品前,用NaOH溶液(pH 12.0)沉淀海水中的Mg~(2+),以避免其在pH较高的流动相中生成沉淀堵塞色谱柱.采用该方法检测SO~(2-)_3 的线性范围为0~100 mg/L,平均回收率为116.8%,检出限为0.05 mg/L;对7.5,25.0和75.0 mg/L 的海水基底加标溶液分别进行9次平行测定,其相对标准偏差(RSD)分别为2.1%,3.1%和4.0% .该方法具有快速、灵敏、选择性好等特点,用于烟气脱硫的海水中SO~(2-)_3 的检测,可得到令人满意的结果.
建立瞭燃煤電廠煙氣脫硫海水中亞硫痠根(SO~(2-)_3)的離子色譜-脈遲安培檢測方法.色譜柱為IonPac AS14A陰離子交換柱,流動相為14 mmol/L NaOH-12 mmol/L Na_2CO_3溶液(pH 11.7),流速1.2 mL/min,脈遲安培法檢測.因SO~(2-)_3 易被氧化,故在採樣時加入甲醛作為保護劑,使之穩定存在.在測定海水樣品前,用NaOH溶液(pH 12.0)沉澱海水中的Mg~(2+),以避免其在pH較高的流動相中生成沉澱堵塞色譜柱.採用該方法檢測SO~(2-)_3 的線性範圍為0~100 mg/L,平均迴收率為116.8%,檢齣限為0.05 mg/L;對7.5,25.0和75.0 mg/L 的海水基底加標溶液分彆進行9次平行測定,其相對標準偏差(RSD)分彆為2.1%,3.1%和4.0% .該方法具有快速、靈敏、選擇性好等特點,用于煙氣脫硫的海水中SO~(2-)_3 的檢測,可得到令人滿意的結果.
건립료연매전엄연기탈류해수중아류산근(SO~(2-)_3)적리자색보-맥충안배검측방법.색보주위IonPac AS14A음리자교환주,류동상위14 mmol/L NaOH-12 mmol/L Na_2CO_3용액(pH 11.7),류속1.2 mL/min,맥충안배법검측.인SO~(2-)_3 역피양화,고재채양시가입갑철작위보호제,사지은정존재.재측정해수양품전,용NaOH용액(pH 12.0)침정해수중적Mg~(2+),이피면기재pH교고적류동상중생성침정도새색보주.채용해방법검측SO~(2-)_3 적선성범위위0~100 mg/L,평균회수솔위116.8%,검출한위0.05 mg/L;대7.5,25.0화75.0 mg/L 적해수기저가표용액분별진행9차평행측정,기상대표준편차(RSD)분별위2.1%,3.1%화4.0% .해방법구유쾌속、령민、선택성호등특점,용우연기탈류적해수중SO~(2-)_3 적검측,가득도령인만의적결과.
The technology for flue gas desulfurization (FGD) with seawater is widely adopted by coal-fired power plants in coastal areas. SO_2 in the flue gas is absorbed by alkaline seawater and transfered in aqueous phase as sulfite (SO~(2-)_3) , and most SO~(2-)_3 is transformed to sulfate (SO~(2-)_4) after an aeration process. The remaining SO~(2-)_3 in the seawater discharged to sea area may be harmful to marine organism because of its biological toxicity, thus it is necessary to determine the concentration of SO~(2-)_3 in the seawater for desulfurization. In this study, the method of determination of SO~(2-)_3 in the seawater by ion chromatography was investigated. The separation was achieved on an IonPac ASH A column with 14 mmol/L NaOH-12 mmol/L Na_2CO_3 solution as the mobile phase at a flow rate of 1.2 mL/min, and the detection was performed by a pulsed amperometric detector. Formaldehyde was added as a protective agent when sampling because the SO~(2-)_3 is easy to be oxidized. To avoid the formation of Mg(OH)_2 in the mobile phase with high pH value which might block the column, the Mg~(2+) in seawater was precipitated by NaOH solution (pH 12. 0) before sample determination. The method showed good linearity within the range of 0-100 mg/L with an average recovery of 116. 8%. The meth-od detection limit ( MDL) reached as low as 0. 05 mg/L. The relative standard deviations (RSD) for seawater matrix samples spiked at levels of 7. 5, 25. 0 and 75.0 mg/L were 2. 1%, 3. 1% and 4.0% (n =9) , respectively. The method has been applied for the determination of SO~(2-)_3 in flue gas desulfurization seawater with the advantages of being fast, sensitive and selective.