摘要
针对水中硫化物、氰化物、总磷、总氮标准方法检出限较高,存在检出即超标的风险,且需分开检测的问题,通过调整过硫酸钾和氢氧化钠的配比,并考察过硫酸钾纯度以及加热消解方式对总磷总氮检测结果的影响,确定最优的消解条件,将水中的磷和氮氧化为磷酸盐和硝酸盐。移取消解后试液与原水按1∶1混合,从而实现硫化物、氰化物、总磷、总氮的离子色谱同时测定。结果表明,在实验测定的浓度范围内,硫化物、氰化物、总磷和总氮的相对标准偏差分别为1.4%~8.1%;硫化物、氰化物、总磷和总氮的检出限分别为0.0003、0.0001、0.01、0.03 mg/L;对实际水样中加标回收率分别为95.4%~108%;与实验室现有检测方法相比,检测时间大幅压缩,提高了检测效率;应用于水中硫化物、氰化物、总磷和总氮的检测,并与参考方法具有良好的一致性。经过扩展,方法可用于白酒中硫化物和氰化物以及窖泥中总磷、总氮的检测。
In view of the high detection limits of the standard methods of sulfide, cyanide, total phosphorus and total nitrogen in water, there is a risk of exceeding the limit when detected.In addition, it needs to be detected separately for different ions.A method was proposed for the oxidation of phosphorus, nitrogen in water to phosphate, nitrate ions.Specifically, the ratio of potassium persulfate and sodium hydroxide was adjusted, the influence of potassium persulfate purity and heating digestion mode on the detection results of total phosphorus and total nitrogen were investigated.Thus the optimal digestion conditions were determined.Mixed the digested test solution with raw water at a ratio of 1∶1,so as to achieve the simultaneous determination of sulfide, cyanide, total phosphorus and total nitrogen by ion chromatography.The results showed that the relative standard deviations of sulfide, cyanide, total phosphorus and total nitrogen were 1.4%~8.1% respectively in the concentration range determined in the experiment.The detection limits of sulfide, cyanide, total phosphorus and total nitrogen were 0.000 3,0.000 1,0.01 and 0.03 mg/L respectively.The recoveries of standard additions for sulfide, cyanide, total phosphorus and total nitrogen in actual samples were 95.4%—108% respectively.Compared with the existing detection methods in the laboratory, the detection time was greatly reduced and the detection efficiency was improved.The present approach was successfully applied for the determination of sulfide, cyanide, total phosphorus and total nitrogen in water and was found to have good agreement with reference methods.After expansion, the method can be used to detect sulfide and cyanide in liquor, as well as total phosphorus and total nitrogen in pit mud.
作者
刘冰
刘金蓉
王莹
张淑玲
袁先群
党永红
崔志芳
左思琦
吴建霞
LIU Bing;LIU Jinrong;WANG Ying;ZHANG Shuling;YUAN Xianqun;DANG Yonghong;CUI Zhifang;ZUO Siqi;WU Jianxia(Kweichow Moutai Co.,Ltd.,Renhuai,Guizhou 564501,China)
出处
《中国无机分析化学》
CAS
北大核心
2023年第4期349-355,共7页
Chinese Journal of Inorganic Analytical Chemistry
关键词
离子色谱
双系统
硫化物
氰化物
总磷
总氮
ion chromatography
double-channel
sulfide
cyanide
total phosphorus
total nitrogen
