氢氧化镁共沉淀富集分离ICP-MS测定海水中的稀土元素
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摘要
本文通过条件优化、标准验证等建立了一种直接在海水中加入NH_3·H_2O溶液使稀土元素与氢氧化镁形成共沉淀富集分离,电感耦合等离子体质谱仪测定海水中14种稀土元素的方法。海水样品通过共沉淀、离心操作后,主要基体物质得到了分离,目标稀土元素实现了富集。氢氧化镁共沉淀富集的条件是1∶1 NH_3·H_2O溶液最佳加入量为0. 35 mL,沉淀清洗次数为1次,静置时间为5 min。方法对稀土元素的加标回收率为88. 7%～107. 1%,稀土元素的方法空白为0. 008×10~(-12)～0. 441×10~(-12),方法定量下限为0. 054×10~(-12)～0. 423×10~(-12),RSD为2. 8%～8. 6%。所建立的方法与海水标准物质NASS-6的测定结果一致,方法具有准确度与精密度高、操作简便快速等优点,可用于大批量海水样品中稀土元素的定量精确测定。
Herein,through optimization of measurement conditions and standard verification,a method for the analyzing14 rare earth elements in sea water with inductively coupled plasma mass spectrometry( ICP-MS) was developed,by adding NH_3·H_2O directly into the seawater to form Mg(OH)_2 co-precipitation. After the co-precipitation and centrifugation operation,the main matrix materials were separated,and the enrichment of the target rare earth elements was achieved. The optimum conditions for the co-precipitation of magnesium hydroxide were as follows: 0. 35 mL of 1∶ 1 NH_3·H_2O solution added in seawater as precipitation matrix,cleaning the precipitation one time for matrix separation and 5 min of the deposition time. The recoveries of the method were in the range of 88. 7% ～ 107. 1%; the method blanks of14 kinds of rare earth elements covered 0. 008 × 10~(-12)～ 0. 441 × 10~(-12),the method quantitative limits were of 0. 054 ×10~(-12)～ 0. 423 × 10~(-12) and the relative standard deviations( RSDs) 2. 8% ～ 8. 6%. The result of NASS-6 analysis by applying this method was in good agreement with the literature report. The method is of high accuracy,good precision and simple operation,which well meets the requirement for determination of rare earth elements in seawater in large quantities.
Herein,through optimization of measurement conditions and standard verification,a method for the analyzing14 rare earth elements in sea water with inductively coupled plasma mass spectrometry( ICP-MS) was developed,by adding NH_3·H_2O directly into the seawater to form Mg(OH)_2 co-precipitation. After the co-precipitation and centrifugation operation,the main matrix materials were separated,and the enrichment of the target rare earth elements was achieved. The optimum conditions for the co-precipitation of magnesium hydroxide were as follows: 0. 35 mL of 1∶ 1 NH_3·H_2O solution added in seawater as precipitation matrix,cleaning the precipitation one time for matrix separation and 5 min of the deposition time. The recoveries of the method were in the range of 88. 7% ～ 107. 1%; the method blanks of14 kinds of rare earth elements covered 0. 008 × 10~(-12)～ 0. 441 × 10~(-12),the method quantitative limits were of 0. 054 ×10~(-12)～ 0. 423 × 10~(-12) and the relative standard deviations( RSDs) 2. 8% ～ 8. 6%. The result of NASS-6 analysis by applying this method was in good agreement with the literature report. The method is of high accuracy,good precision and simple operation,which well meets the requirement for determination of rare earth elements in seawater in large quantities.
引文
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[3]ZHU Y B,INAGAKI K,HARAGUCHI H,et al. On-line elution ofiron hydroxide coprecipitate carrier for determination of REEs innatural water by mix-gas ICP-MS[J]. Journal of Analytical A-tomic Spectrometry,2010,25(3):364-369.
[4]KARADAS C,KARA D. Determination of rare earth elements bysolid phase extraction using chemically modified Amberlite XAD-4 resin and inductively coupled plasma-optical emission spec-trometry[J]. Water,Air,&Soil Pollution,2014,225:2192.
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[6]KARADAS C,KARA D,FISHER A. Determination of rare earthelements in seawater by inductively coupled plasma mass spec-trometry with off-line column preconcentration using 2,6-di-acetylpyridine functionalized Amber lite XAD-4[J]. AnalyticaChimica Acta,2011,689(2):184-189.
[7]ZHU Y B,ITOH A,UMEMURA T,et al. Determination of REEsin natural water by ICP-MS with the aid of an automatic columnchanging system[J]. Journal of Analytical Atomic Spectrometry,2010,25(8):1253-1258.
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[9]戴特,格雷.电感耦合等离子体质谱分析的应用[M].北京:原子能出版社,1998:23-24.
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[11]SHABANI M B,AKAGI T,SHIMIZU H,et al. Determination oftrace lanthanides and yttrium in seawater by inductively coupledplasma mass spectrometry afterpreconcentration with solvent ex-traction and back-extraction[J]. Analytical Chemistry Society,1990,62(24):2709-2714.
[12]施意华,熊传信,黄俭惠,等.共沉淀富集分离ICP-MS法测定地球化学勘探样品中的超痕量金属金、铂、钯[J].黄金,2009,30(2):43-45.
[13]刘伟,宋金明,袁华茂,等. Mg(OH)2共沉淀和直接稀释联用ICP-MS法准确测定海水中的多种常量-微量元素[J].分析测试学报,2017,36(4):471-477.
[14]梁志冉,涂勇,田爱军,等.离子交换树脂及其在废水处理中的应用[J].污染防治技术,2006,19(3):34-36.
[15]刘刚,钟少军,瞿成利,等.应用离子色谱离线鳌合ICP-MS测定海水中多重痕量元素[J].高等学校化学学报,2007,28(1):53-55.
[16]高洪涛,屈文俊,杜安道,等.低空白镍锍试金预富集中子活化分析测定地球化学标准物质中的铂族元素[J].分析化学,1999,27(5):566-569.
[17]DAS D,DUTTA M,CERVERA M L,et al. Recent advances inon-line solid-phase pre-concentration for inductively-coupledplasma techniques for determination of mineralelements[J].Tr AC Trends in Analytical Chemistry,2012,33:35-45.
[18]林建海.共沉淀分离富集-火焰原子吸收光谱法测定痕量金属元素的研究[C].呼和浩特:内蒙古大学,2013.
[19]GB17378. 4-2007,海洋监测规范4部分:海水分析[S].
[20] ROUSSEAU T C C,SONKE J E,CHMELEFF J,et al. Rareearth element analysis in natural waters by multiple isotope dilu-tion-sectorfield ICP-MS[J]. Journal of Analytical Atomic Spec-trometry,2013,28(4):573-584.
[2]宋金明,段丽琴.渤黄东海微/痕量元素的环境生物地球化学[M].北京:科学出版社,2017:1-465.
[3]ZHU Y B,INAGAKI K,HARAGUCHI H,et al. On-line elution ofiron hydroxide coprecipitate carrier for determination of REEs innatural water by mix-gas ICP-MS[J]. Journal of Analytical A-tomic Spectrometry,2010,25(3):364-369.
[4]KARADAS C,KARA D. Determination of rare earth elements bysolid phase extraction using chemically modified Amberlite XAD-4 resin and inductively coupled plasma-optical emission spec-trometry[J]. Water,Air,&Soil Pollution,2014,225:2192.
[5] WAQAR F,JAN S,MOHAMMAD B,et al. Preconcentration ofrare earth elements in seawater with chelating resin having fluori-natedβ-diketone immobilized on styrene divinyl benzene fortheir determination by ICP-OES[J]. Journal of the ChineseChemical Society,2009,56(2):335-340.
[6]KARADAS C,KARA D,FISHER A. Determination of rare earthelements in seawater by inductively coupled plasma mass spec-trometry with off-line column preconcentration using 2,6-di-acetylpyridine functionalized Amber lite XAD-4[J]. AnalyticaChimica Acta,2011,689(2):184-189.
[7]ZHU Y B,ITOH A,UMEMURA T,et al. Determination of REEsin natural water by ICP-MS with the aid of an automatic columnchanging system[J]. Journal of Analytical Atomic Spectrometry,2010,25(8):1253-1258.
[8]RODUSHKIN I,RUTH T,KLOCKARE D. Non-spectral interfer-ences caused by a saline water matrix in quadrupole and highresolution inductively coupled plasma mass spectrometry[J].Journal of Analytical Atomic Spectrometry,1998,13(3):159-166.
[9]戴特,格雷.电感耦合等离子体质谱分析的应用[M].北京:原子能出版社,1998:23-24.
[10]ZHANG J,NOZAKI Y. Rare earth elements and yttrium in sea-water:ICP-MS determinations in the East Caroline,Coral Sea,and South Fiji basins of the western South Pacific Ocean[J].Geochimica et Cosmochimica Acta,1996,60(23):4631-4644.
[11]SHABANI M B,AKAGI T,SHIMIZU H,et al. Determination oftrace lanthanides and yttrium in seawater by inductively coupledplasma mass spectrometry afterpreconcentration with solvent ex-traction and back-extraction[J]. Analytical Chemistry Society,1990,62(24):2709-2714.
[12]施意华,熊传信,黄俭惠,等.共沉淀富集分离ICP-MS法测定地球化学勘探样品中的超痕量金属金、铂、钯[J].黄金,2009,30(2):43-45.
[13]刘伟,宋金明,袁华茂,等. Mg(OH)2共沉淀和直接稀释联用ICP-MS法准确测定海水中的多种常量-微量元素[J].分析测试学报,2017,36(4):471-477.
[14]梁志冉,涂勇,田爱军,等.离子交换树脂及其在废水处理中的应用[J].污染防治技术,2006,19(3):34-36.
[15]刘刚,钟少军,瞿成利,等.应用离子色谱离线鳌合ICP-MS测定海水中多重痕量元素[J].高等学校化学学报,2007,28(1):53-55.
[16]高洪涛,屈文俊,杜安道,等.低空白镍锍试金预富集中子活化分析测定地球化学标准物质中的铂族元素[J].分析化学,1999,27(5):566-569.
[17]DAS D,DUTTA M,CERVERA M L,et al. Recent advances inon-line solid-phase pre-concentration for inductively-coupledplasma techniques for determination of mineralelements[J].Tr AC Trends in Analytical Chemistry,2012,33:35-45.
[18]林建海.共沉淀分离富集-火焰原子吸收光谱法测定痕量金属元素的研究[C].呼和浩特:内蒙古大学,2013.
[19]GB17378. 4-2007,海洋监测规范4部分:海水分析[S].
[20] ROUSSEAU T C C,SONKE J E,CHMELEFF J,et al. Rareearth element analysis in natural waters by multiple isotope dilu-tion-sectorfield ICP-MS[J]. Journal of Analytical Atomic Spec-trometry,2013,28(4):573-584.
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