控温消解-氢化物发生-原子荧光光谱法测定水中硒形态
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摘要
取10.00 mL水样,于60～70℃加热蒸发至近干,加入硝酸-高氯酸(1+1)混合酸2.0mL,继续加热至白烟冒尽,加入盐酸2.0 mL,摇匀,加热保持微沸3～5 min,冷却后转移至10mL比色管中,用去离子水定容,使用氢化物发生-原子荧光光谱仪测定总硒的含量。另取10.00mL水样,加入盐酸2.0mL,于60～70℃加热至溶液体积小于5mL,转移至10mL比色管中,用去离子水定容,使用氢化物发生-原子荧光光谱仪测定无机硒(即四价硒和六价硒的总和)的含量。另取水样5.00mL于10mL比色管中,加入盐酸2.0mL,用去离子水定容,使用氢化物发生-原子荧光光谱仪测定四价硒的含量。用总硒含量减去无机硒含量即为有机硒含量,无机硒含量减去四价硒含量即为六价硒含量。在最佳仪器工作条件下,硒的质量浓度在1.00～20.0μg·L~(-1)内与其对应的荧光强度呈线性关系,硒的检出限(3s)和测定下限(10s)分别为0.11,0.36μg·L~(-1)。采用本方法测定某地区水中的总硒、无机硒和四价硒,加标回收率在95.7%～104%之间,相对标准偏差(n=6)在1.9%～3.2%之间。采用本方法测定了不同地区水中的总硒、无机硒和四价硒,利用差减法计算得有机硒和六价硒的含量。
10.00 mL of water sample were taken and heated to evaporate to near dry at 60-70℃,2.0 mL of mixed acid of nitric acid and perchloric acid(1+1)were added,and the mixture was heated until white smoke was exhausted.After 2.0 mL of hydrochloric acid was added,the mixture was shaked well and heated to keep slight boiling for 3-5 minutes.After cooling,the solution was transferred to a colorimetric tube and made up to 10.00 mL with deionized water.The total selenium content was determined by hydride generation-atomic fluorescence spectrometry.Another 10.00 mL of water sample were taken,and 2.0 mL of hydrochloric acid were added.After the mixture was heated at 60-70℃ until the solution volume were less than 5 mL,the solution was transferred to a colorimetric tube and made up to 10.00 mL with deionized water.The content of inorganic selenium(the sum of tetravalent selenium and hexavalent selenium) was determined by hydride generation-atomic fluorescence spectrometry.Another 5.00 mL of water sample was taken into a 10 mL colorimetric tube,2.0 mL of hydrochloric acid was added,and the volume was made up to 10.00 mL with deionized water to determine the content of tetravalent selenium by hydride generation-atomic fluorescence spectrometry.The total selenium content minus the inorganic selenium content was the organic selenium content,and the inorganic selenium content minus the tetravalent selenium content was the hexavalent selenium content.Under the optimal working conditions of the instrument,the mass concentration of selenium was linearly related to the corresponding fluorescence intensity in the range of 1.00-20.0μg·L~(-1).The detection limit(3 s)and the lower limit of determination(10 s)of selenium were 0.11,0.36μg·L~(-1),respectively.The method was applied to determination of total selenium,inorganic selenium and tetravalent selenium in water of an area,giving recovery obtained by standard addition method between95.7% and 104%,and RSDs(n=6)in the range of 1.9%-3.2%.The total selenium,inorganic selenium and tetravalent selenium in water from different regions were determined by this method,and the contents of organic selenium and hexavalent selenium were obtained by calculating with subtraction method.
10.00 mL of water sample were taken and heated to evaporate to near dry at 60-70℃,2.0 mL of mixed acid of nitric acid and perchloric acid(1+1)were added,and the mixture was heated until white smoke was exhausted.After 2.0 mL of hydrochloric acid was added,the mixture was shaked well and heated to keep slight boiling for 3-5 minutes.After cooling,the solution was transferred to a colorimetric tube and made up to 10.00 mL with deionized water.The total selenium content was determined by hydride generation-atomic fluorescence spectrometry.Another 10.00 mL of water sample were taken,and 2.0 mL of hydrochloric acid were added.After the mixture was heated at 60-70℃ until the solution volume were less than 5 mL,the solution was transferred to a colorimetric tube and made up to 10.00 mL with deionized water.The content of inorganic selenium(the sum of tetravalent selenium and hexavalent selenium) was determined by hydride generation-atomic fluorescence spectrometry.Another 5.00 mL of water sample was taken into a 10 mL colorimetric tube,2.0 mL of hydrochloric acid was added,and the volume was made up to 10.00 mL with deionized water to determine the content of tetravalent selenium by hydride generation-atomic fluorescence spectrometry.The total selenium content minus the inorganic selenium content was the organic selenium content,and the inorganic selenium content minus the tetravalent selenium content was the hexavalent selenium content.Under the optimal working conditions of the instrument,the mass concentration of selenium was linearly related to the corresponding fluorescence intensity in the range of 1.00-20.0μg·L~(-1).The detection limit(3 s)and the lower limit of determination(10 s)of selenium were 0.11,0.36μg·L~(-1),respectively.The method was applied to determination of total selenium,inorganic selenium and tetravalent selenium in water of an area,giving recovery obtained by standard addition method between95.7% and 104%,and RSDs(n=6)in the range of 1.9%-3.2%.The total selenium,inorganic selenium and tetravalent selenium in water from different regions were determined by this method,and the contents of organic selenium and hexavalent selenium were obtained by calculating with subtraction method.
引文
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[13]蒋天成,刘守廷,梁利诚,等.微波消解ICP-MS法测定广西北部湾海鸭蛋中硒和锗的含量[J].化学分析计量,2012,21(4):27-30.
[14]邓爱华,庞晋山,彭晓俊,等.高效液相色谱-氢化物发生原子荧光法同时测定塑料制品中的3种有机锡[J].分析测试学报,2014,33(8):928-933.
[15]张硕,弓振斌.高灵敏度原子荧光光谱系统应用于砷、硒形态分析的研究[J].分析测试学报,2014,33(9):979-985.
[16]姜能座,陈剑侠.国内农产品中总有机硒的几种常用测定方法[J].福建分析测试,2017,26(5):17-22.
[17]张美琴,季华曼,杨洪生,等.氢化物发生-原子荧光光谱法测定水产品中有机硒和无机硒[J].中国水产科学,2012,19(5):900-905.
[18]王梅,张红香,邹志辉,等.原子荧光光谱法测定富硒螺旋藻片中不同形态、价态的硒[J].食品科学,2011,32(6):179-182.
[2] XIE L T,WU X,CHEN H X,et al.A low level of dietary selenium has both beneficial and toxic effects and is protective against Cd-toxicity in the least killifish Heterandria formosa[J].Chemosphere,2016,161:358-364.
[3] BARACHE U B,SHAIKH A B,LOKHANDE T N,et al.Acid switched efficient,cost effective,selective separation and determination of selenium(Ⅳ)[J].Journal of Environmental Chemical Engineering,2017,5(5):4828-4840.
[4] DO NASCIMENTO P C,JOST C L,DE CARVALHO L M,et al.Voltammetric determination of Se(Ⅳ)and Se(Ⅵ)in saline samples:Studies with seawater,hydrothermal and hemodialysis fluids[J].Analytica Chimica Acta,2009,648(2):162-166.
[5] HU B W,CHEN G H,JIN C G,et al.Macroscopic and spectroscopic studies of the enhanced scavenging of Cr(Ⅵ)and Se(Ⅵ)from water by titanate nanotube anchored nanoscale zero-valent iron[J].Journal of Hazardous Materials,2017,336:214-221.
[6] SHARMA V K,MCDONALD T J,SOHN M,et al.Assessment of toxicity of selenium and cadmium selenium quantum dots:A review[J].Chemosphere,2017,188:403-413.
[7] GB/T 14848.4.2-2017地下水环境质量标准[S].
[8] GB 5749.4.1.9-2006生活饮用水卫生标准[S].
[9]史云东,贾琳,王元忠,等.FI-HG-AAS测定中草药灯盏花中的微量硒[J].江苏农业科学,2011,39(3):443-444.
[10] PEREIRA J B,DANTAS K G F.Evaluation of inorganic elements in cat′s claw teas using ICP-OES and GF-AAS[J].Food Chemistry,2016,196:331-337.
[11] FLEMING D E B,NADER M N,FORAN K A,et al.Assessing arsenic and selenium in a single nail clipping using portable X-ray fluorescence[J].Applied Radiation and Isotopes,2017,120:1-6.
[12]赵尔敏,方勇,王明洋,等.ICP-MS直接进样对大米酶解液中痕量硒的测定[J].食品科学,2017,38(10):168-172.
[13]蒋天成,刘守廷,梁利诚,等.微波消解ICP-MS法测定广西北部湾海鸭蛋中硒和锗的含量[J].化学分析计量,2012,21(4):27-30.
[14]邓爱华,庞晋山,彭晓俊,等.高效液相色谱-氢化物发生原子荧光法同时测定塑料制品中的3种有机锡[J].分析测试学报,2014,33(8):928-933.
[15]张硕,弓振斌.高灵敏度原子荧光光谱系统应用于砷、硒形态分析的研究[J].分析测试学报,2014,33(9):979-985.
[16]姜能座,陈剑侠.国内农产品中总有机硒的几种常用测定方法[J].福建分析测试,2017,26(5):17-22.
[17]张美琴,季华曼,杨洪生,等.氢化物发生-原子荧光光谱法测定水产品中有机硒和无机硒[J].中国水产科学,2012,19(5):900-905.
[18]王梅,张红香,邹志辉,等.原子荧光光谱法测定富硒螺旋藻片中不同形态、价态的硒[J].食品科学,2011,32(6):179-182.
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