海水重金屬監(jiān)測分析方法比較研究
發(fā)布時間：2019-02-12 12:54
【摘要】：海水中重金屬元素的監(jiān)測一直備受關(guān)注。國家標(biāo)準(zhǔn)對于每種重金屬元素的分析均給出了2-4種不同的分析方法。實(shí)際中,由于不同的實(shí)驗(yàn)室對于同一種元素的測定選擇的分析方法不同,分析結(jié)果可能有所差別。這一現(xiàn)象降低了近岸海域海水調(diào)查數(shù)據(jù)的可比性,容易導(dǎo)致一些痕量元素海洋化學(xué)行為的研究困難,限制了污染水平評價的可靠性。本研究根據(jù)實(shí)際情況,以國家近岸海域環(huán)境監(jiān)測網(wǎng)網(wǎng)絡(luò)成員單位為調(diào)查對象,對海水重金屬監(jiān)測分析方法的實(shí)際應(yīng)用情況進(jìn)行了研究,主要包括兩部分內(nèi)容。首先調(diào)查了海水重金屬監(jiān)測分析方法的實(shí)際應(yīng)用情況,然后通過對海水中總鉻、銅、鉛、鎘、鋅、汞元素不同分析方法進(jìn)行比對實(shí)驗(yàn),優(yōu)選并推薦了適合實(shí)際應(yīng)用的分析方法。 1.向近海網(wǎng)成員單位以調(diào)函形式發(fā)放了調(diào)查問卷。回收信息進(jìn)行了整理、總結(jié),得出了目前國內(nèi)監(jiān)測站海水重金屬各分析方法的實(shí)際工作使用比例。同時,確定了下一步研究工作內(nèi)容,對總鉻、銅、鉛、鎘、鋅、汞6種重金屬元素進(jìn)行方法比對實(shí)驗(yàn)。 2.比較了測定海水總鉻的GF-AAS法和DPC法,旨在考察兩方法的實(shí)驗(yàn)室實(shí)際應(yīng)用情況。GF-AAS法和DPC法測定海水總鉻的檢出限分別為0.17μg/L、0.11μig/L,加標(biāo)回收率分別為102.3%～103.5%、98.2%～101.6%,實(shí)驗(yàn)室內(nèi)相對標(biāo)準(zhǔn)偏差分別為4.52%-5.42%、4.90%-5.31%。 3.比較了測定海水中銅、鉛、鎘的GF-AAS法和ASV法,旨在考察兩方法的實(shí)驗(yàn)室實(shí)際應(yīng)用情況。GF-AAS法和ASV法測定海水中銅的檢出限分別為0.10μgL、2.33μg/L,加標(biāo)回收率分別為101.5%～107.7%、87.2%～147.8%,實(shí)驗(yàn)室內(nèi)相對標(biāo)準(zhǔn)偏差分別為4.56%～-6.59%、11.60%～19.41%。GF-AAS法和ASV法測定海水中鉛的檢出限分別為0.15μg/L,0.38μg/L,加標(biāo)回收率分別為100.7%-101.0%、97.8%-143.2%,實(shí)驗(yàn)室內(nèi)相對標(biāo)準(zhǔn)偏差分別為3.71%-8.56%、16.69%～18.72%。GF-AAS法和ASV法測定海水中鎘的檢出限分別為0.15μg/L,0.02μg/L,加標(biāo)回收率分別為98.0%-98.8%、99.8%-107.1%,實(shí)驗(yàn)室內(nèi)相對標(biāo)準(zhǔn)偏差分別為4.11%-5.02%、8.22%-8.71%。 4.比較了測定海水中鋅的FAAS法和ASV法,旨在考察兩方法的實(shí)驗(yàn)室實(shí)際應(yīng)用情況。FAAS法和ASV法測定海水中鋅的檢出限分別為1.73μg/L,1.06μg/L,加標(biāo)回收率分別為101.1%-103.7%、138.7%-145.9%,實(shí)驗(yàn)室內(nèi)相對標(biāo)準(zhǔn)偏差分別為2.93%-3.12%、16.76%～17.11%。 5.比較了測定海水中汞的CAAS法和AFS法,旨在考察兩方法的實(shí)驗(yàn)室實(shí)際應(yīng)用情況。CAAS法和AFS法測定海水中汞的檢出限分別為0.010μg/L、0.008μg/L,加標(biāo)回收率分別為97.1%～97.2%、97.0%～99.2%,實(shí)驗(yàn)室內(nèi)相對標(biāo)準(zhǔn)偏差分別為0.67%～0.99%、0.86%～1.92%。 6.依據(jù)實(shí)驗(yàn)數(shù)據(jù),考慮檢出限、方法準(zhǔn)確度和精密度、前處理過程、方法繁復(fù)性等,推薦使用GF-AAS法測定海水中總鉻、銅、鉛、鎘,使用FAAS法測定海水中鋅,使用AFS法測定海水中汞。
[Abstract]:The monitoring of heavy metal elements in seawater has been paid more and more attention. The national standard gives 2-4 different analytical methods for each heavy metal element. In practice, the analytical results may differ due to the different analytical methods for the same element in different laboratories. This phenomenon reduces the comparability of the sea water survey data in the coastal waters and easily leads to the difficulty of studying the marine chemical behavior of some trace elements and limits the reliability of the assessment of the pollution level. According to the actual situation, this paper studies the application of the method of monitoring and analyzing heavy metals in sea water by taking the member units of the national environmental monitoring network in the coastal sea area as the objects of investigation, which mainly includes two parts. This paper first investigates the practical application of heavy metal monitoring and analysis methods in seawater, and then, by comparing the analytical methods of total chromium, copper, lead, cadmium, zinc and mercury in seawater, the analytical methods suitable for practical application are selected and recommended. 1. A questionnaire was distributed to the offshore network member units in the form of dispatch letters. The recovery information is sorted out and summarized, and the actual working proportion of each analysis method of sea water heavy metals in domestic monitoring station is obtained. At the same time, the contents of the next research work were determined, and the comparison experiments of total chromium, copper, lead, cadmium, zinc and mercury were carried out. 2. The GF-AAS method and DPC method for the determination of total chromium in seawater are compared. The purpose of this paper is to investigate the practical application of the two methods in laboratory. The detection limits of total chromium in seawater by GF-AAS method and DPC method are 0.17 渭 g / L ~ (-1) ~ 0.11 渭 ig/L, respectively. The relative standard deviation in the laboratory was 4.52-5.42 and 4.90-5.31, respectively. The recoveries were 102.3and 103.5and 98.2and 101.6.The relative standard deviations in the laboratory were 4.52-5.42 and 4.90-5.31, respectively. 3. The GF-AAS method and ASV method for the determination of copper, lead and cadmium in seawater were compared. The detection limits of GF-AAS and ASV methods were 0.10 渭 gL,2.33 渭 g / L and 0.10 渭 gL,2.33 渭 g / L, respectively. The recoveries were 101.5 and 107.7, respectively, and the relative standard deviations in the laboratory were 4.56- 6.59, respectively. The detection limits of lead in seawater by 11.60%~19.41%.GF-AAS and ASV were 0.38 渭 g / L and 0.38 渭 g / L, respectively. The recoveries of standard addition were 100.7- 101.0 and 97.8- 143.2, respectively. The relative standard deviations in the laboratory were 3.71 and 8.56 and 16.699.The detection limits of cadmium in seawater by GF-AAS and ASV were 0.15 渭 g / L and 0.02 渭 g / L, respectively. The recoveries were 98.0-98.8 and 99.8- 107.1, and the relative standard deviations in the laboratory were 4.11-5.02 and 8.22-8.71, respectively. 4. The FAAS method and ASV method for the determination of zinc in seawater were compared in order to investigate the laboratory application of the two methods. The detection limits of FAAS method and ASV method for the determination of zinc in seawater were 1.73 渭 g / L ~ (-1) 渭 g / L ~ (-1) ~ (-1) 渭 g 路L ~ (-1), respectively. The recoveries were 101.1% -103.7% and 138.7% -145.9%, respectively. The relative standard deviations in the laboratory were 2.93-3.12 and 16.767.11, respectively. 5. The CAAS method and AFS method for the determination of mercury in seawater were compared to investigate the laboratory application of the two methods. The detection limits of CAAS method and AFS method for the determination of mercury in seawater were 0.010 渭 g / L ~ 0.008 渭 g 路L ~ (-1) 路L ~ (-1), respectively. The relative standard deviation in the laboratory was 0.670.990.86 and 1.92, respectively. 6. According to the experimental data, considering the detection limit, accuracy and precision of the method, the pretreatment process and the complexity of the method, the GF-AAS method is recommended for the determination of total chromium, copper, lead and cadmium in seawater, and the FAAS method for the determination of zinc in seawater is recommended. AFS method was used to determine mercury in seawater.
【學(xué)位授予單位】：大連理工大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2015
【分類號】：X834
本文編號：2420460
[Abstract]:The monitoring of heavy metal elements in seawater has been paid more and more attention. The national standard gives 2-4 different analytical methods for each heavy metal element. In practice, the analytical results may differ due to the different analytical methods for the same element in different laboratories. This phenomenon reduces the comparability of the sea water survey data in the coastal waters and easily leads to the difficulty of studying the marine chemical behavior of some trace elements and limits the reliability of the assessment of the pollution level. According to the actual situation, this paper studies the application of the method of monitoring and analyzing heavy metals in sea water by taking the member units of the national environmental monitoring network in the coastal sea area as the objects of investigation, which mainly includes two parts. This paper first investigates the practical application of heavy metal monitoring and analysis methods in seawater, and then, by comparing the analytical methods of total chromium, copper, lead, cadmium, zinc and mercury in seawater, the analytical methods suitable for practical application are selected and recommended. 1. A questionnaire was distributed to the offshore network member units in the form of dispatch letters. The recovery information is sorted out and summarized, and the actual working proportion of each analysis method of sea water heavy metals in domestic monitoring station is obtained. At the same time, the contents of the next research work were determined, and the comparison experiments of total chromium, copper, lead, cadmium, zinc and mercury were carried out. 2. The GF-AAS method and DPC method for the determination of total chromium in seawater are compared. The purpose of this paper is to investigate the practical application of the two methods in laboratory. The detection limits of total chromium in seawater by GF-AAS method and DPC method are 0.17 渭 g / L ~ (-1) ~ 0.11 渭 ig/L, respectively. The relative standard deviation in the laboratory was 4.52-5.42 and 4.90-5.31, respectively. The recoveries were 102.3and 103.5and 98.2and 101.6.The relative standard deviations in the laboratory were 4.52-5.42 and 4.90-5.31, respectively. 3. The GF-AAS method and ASV method for the determination of copper, lead and cadmium in seawater were compared. The detection limits of GF-AAS and ASV methods were 0.10 渭 gL,2.33 渭 g / L and 0.10 渭 gL,2.33 渭 g / L, respectively. The recoveries were 101.5 and 107.7, respectively, and the relative standard deviations in the laboratory were 4.56- 6.59, respectively. The detection limits of lead in seawater by 11.60%~19.41%.GF-AAS and ASV were 0.38 渭 g / L and 0.38 渭 g / L, respectively. The recoveries of standard addition were 100.7- 101.0 and 97.8- 143.2, respectively. The relative standard deviations in the laboratory were 3.71 and 8.56 and 16.699.The detection limits of cadmium in seawater by GF-AAS and ASV were 0.15 渭 g / L and 0.02 渭 g / L, respectively. The recoveries were 98.0-98.8 and 99.8- 107.1, and the relative standard deviations in the laboratory were 4.11-5.02 and 8.22-8.71, respectively. 4. The FAAS method and ASV method for the determination of zinc in seawater were compared in order to investigate the laboratory application of the two methods. The detection limits of FAAS method and ASV method for the determination of zinc in seawater were 1.73 渭 g / L ~ (-1) 渭 g / L ~ (-1) ~ (-1) 渭 g 路L ~ (-1), respectively. The recoveries were 101.1% -103.7% and 138.7% -145.9%, respectively. The relative standard deviations in the laboratory were 2.93-3.12 and 16.767.11, respectively. 5. The CAAS method and AFS method for the determination of mercury in seawater were compared to investigate the laboratory application of the two methods. The detection limits of CAAS method and AFS method for the determination of mercury in seawater were 0.010 渭 g / L ~ 0.008 渭 g 路L ~ (-1) 路L ~ (-1), respectively. The relative standard deviation in the laboratory was 0.670.990.86 and 1.92, respectively. 6. According to the experimental data, considering the detection limit, accuracy and precision of the method, the pretreatment process and the complexity of the method, the GF-AAS method is recommended for the determination of total chromium, copper, lead and cadmium in seawater, and the FAAS method for the determination of zinc in seawater is recommended. AFS method was used to determine mercury in seawater.
【學(xué)位授予單位】：大連理工大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2015
【分類號】：X834
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