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1.
固相萃取-离子色谱法测定地下水中痕量高氯酸根离子   总被引:1,自引:0,他引:1  
Ye L  You H  Yao J  Su H 《色谱》2012,30(1):76-79
建立了测定地下水中痕量高氯酸根(ClO~4)的固相萃取-离子色谱(SPE-IC)分析方法。0.7 L水样经预处理降低主要干扰离子Cl~、CO2~3和SO2~4的干扰后,使用Cleanert PWAX弱阴离子交换固相萃取小柱对地下水中痕量(μg/L级)的ClO~4进行富集,用6 mL 1%NaOH溶液洗脱,富集液经0.45 μm水膜过滤后,用IonPac AS20阴离子分离柱、50 μL进样环、40 mmol/L KOH溶液淋洗、抑制电导检测分离分析。结果表明,地下水样品中ClO~4的方法检出限和测定下限分别为0.15 μg/L和0.60 μg/L,进样质量浓度在1~15 μg/L范围内有很好的线性关系,线性相关系数为0.9992,回收率为99.7%~100.5%;该方法经济有效,可用于地下水中痕量ClO~4的检测。利用该方法测定了哈尔滨周边部分地区地下水中ClO~4浓度,检测结果与离子色谱-质谱联用法的检测结果的相对误差为1.85%~9.24%。  相似文献   

2.
离子色谱法测定饮用水中无机消毒副产物   总被引:11,自引:0,他引:11  
采用直接进样离子色谱法,对饮用水中无机消毒副产物(DBP):ClOˉ2、BrO、ClOˉ3和Brˉ进行分离检测;研究了分离柱的选择、淋洗液的浓度和流速对分离的影响;在优化的条件下,4种离子的工作曲线范围为1.0~50μg/L;检出限为ClOˉ2 0.3μg/L、BrOˉ3 0.6μg/L、ClOˉ3 0.9μg/L和Brˉ0.6μg/L;4种离子的RSD(n=8)分别为3.8%、3.6%、4.0%和5.0%;本法操作简单、运行费用低、灵敏度高,应用于饮用水的分析。结果令人满意。  相似文献   

3.
本实验采用单柱离子色谱系统,在SeO_4~(2-)、SeO_3~(2-)与F~-、Cl~-、NO_3~-、SO_4~(2-)离子共存时,以1.0mmol/L邻苯二甲酸氢钾为淋洗液测定了SeO_4~(2-),以1.0mmol/LKNO_3为淋洗液测定了SeO_3~(2-)。SeO_4~(1-)和SeO_3~(2-)的最低检出浓度分别为0.3μg/mL和0.7μg/mL,线性范围分别为0.8~80μg/mL和1.4~150μg/mL,相对标准偏差分别为2.01%和1.85%。并应用本方法测定了加SeO_4~(2-)和SeO_3~(2-)的自来水样,SeO_4~(2-)和SeO_3~(2-)的回收率分别为96%和98%。  相似文献   

4.
李朦  于泓  郑秀荣 《色谱》2014,32(3):299-303
建立了同时分析碘酸根、碘离子、溴酸根和溴离子的离子色谱-紫外检测分析方法。用季铵型阴离子交换柱,以柠檬酸-乙腈为流动相,采用紫外检测器实现了4种离子的同时分离和检测。研究了检测波长和流动相种类、浓度、pH值等因素对4种离子分离和测定的影响,探讨了保留规律,优化了色谱分析条件。在检测波长为210 nm、流动相为1.0 mmol/L柠檬酸-乙腈(85∶15,v/v;pH5.0)、流速为0.9 mL/min、柱温为40℃条件下,4种离子完全分离,且系统峰不干扰测定。4种离子的检出限(S/N=3)为0.07~0.16 mg/L,连续5次进样测定的峰面积和保留时间的相对标准偏差均在1%以下。将此方法用于离子液体样品及地下水样品的分析,结果准确、可靠。  相似文献   

5.
单柱离子色谱法测定钼酸根和钨酸根离子的研究   总被引:4,自引:0,他引:4  
于泓 《分析化学》1993,21(5):541-543
本文采有单柱离子色谱系统测定了MoO_4~(2-)和WO_4~(2-)。以1.0mmol/L钼酸钠为淋洗液测定WO_4~(2-),以1.0mmol/L钨酸钠为淋洗液测定MoO_4~(2-),常见阴离子Cl~-、NO_3~-、SO_4~(2-)不干扰测定,MoO_4~(2-)和MO_4~(2-)的检出限分别为3.55μg/ml和5.03μg/ml,相对标准偏差为1.04%和1.66%,工作曲线的线性范围为3.55~1500μg/ml和5.03~1500μg/ml。应用于钼、钨、硅杂多酸中钼和钨的测定,结果满意。  相似文献   

6.
周益奇  王子健  许宜平  马梅 《色谱》2007,25(3):430-434
水中的碘酸根、亚氯酸根和溴酸根是重要的消毒副产物,主要通过大体积浓缩后直接电导检测,或通过柱前或柱后化学反应将目标物转化成容易检测的物质后检测。本方法采用大体积进样柱后衍生紫外检测的分析方法,通过条件优化获得了较高的灵敏度和信噪比。利用一套自动分析系统,可以满足饮用水中痕量碘酸根、亚氯酸根、溴酸根的同时监测。碘酸根、亚氯酸根和溴酸根的检出限分别为0.5,0.4,0.1 μg/L。对于不同的加标样品,碘酸根、亚氯酸根和溴酸根的回收率分别为70.8%~98.0%,92.4%~100%和93.2%~104.1%。该方法应用于北京市场上的瓶装饮用水分析,结果显示瓶装纯净水中的碘酸根、亚氯酸根、溴酸根浓度均低于检出限,而瓶装矿泉水中碘酸根、溴酸根的最高含量分别达到9.4 μg/L和78.4 μg/L。  相似文献   

7.
郭明  孔亮  历欣  邹汉法 《色谱》2002,20(2):137-139
 用磺化四苯基卟啉 (TPPS4 )作柱前衍生试剂 ,在微波作用下进行衍生反应 ,研究了衍生和分离Ni2 + ,Mn2 + ,Zn2 + 和Cu2 + 的最佳条件。在 75 0W的微波作用下衍生反应 3min ,在C18柱上采用乙腈 水 (体积比为 2 2 5∶77 5 )体系作流动相 ,四乙基溴化铵 (TEABr)作离子对试剂 ,在 415nm处检测 ,建立了微波衍生 离子对高效液相快速分离、光度检测Ni2 + ,Mn2 + ,Zn2 + 和Cu2 + 的新方法。络合物和反应试剂在 15min内出峰完毕。Zn2 + ,Cu2 + ,Ni2 + 和Mn2 + 的检测限分别为 0 0 5 μg/L ,0 0 1μg/L ,0 10 μg/L和 0 40 μg/L。  相似文献   

8.
用离子色谱法测定水中的二氧化氯、氯、亚氯酸根及氯酸根   总被引:15,自引:0,他引:15  
田芳  谢家理 《分析化学》2004,32(4):522-524
建立了一种测定水中的ClO2、Cl2、ClO2^-、ClO3^-离子色谱法,在含有碳酸氢钠缓冲溶液的中性条件下,用NaNO2将ClO2、Cl2还原为ClO2^-、Cl^-,通过测定ClO^-和NO3^-的变化值,间接测定ClO2和Cl2。加入硫代乙酰胺(TAA)作掩蔽剂测定ClO2^-。  相似文献   

9.
二甲基黄褪色光度法测定微量溴酸根离子的研究   总被引:6,自引:0,他引:6  
研究了二甲基黄与 Br O- 3的褪色反应 ,确定了最佳反应条件 ,建立了一种光度测定微量溴酸根离子的新方法。结果表明 :方法的表观摩尔吸光系数ε′=3.2× 1 0 4L· mol- 1· cm- 1,检出限为 4.2 9× 1 0 - 8g/m L ,线性范围为 0~ 1 2μg/1 0 m L。用于化学试剂中溴酸根离子的测定 ,结果满意  相似文献   

10.
采用离子色谱法同时测定了大气可吸入颗粒物PM10中的多种水溶性阴阳离子。样品采用超纯水超声萃取各种水溶性离子,优化的萃取溶液体积为40mL,萃取时间为15 min,萃取液用0.45μm纤维滤膜过滤,阴、阳离子分别采用响应的离子色谱柱分离,流动相分别采用3.6 mmol/L Na2CO3溶液+0.6 mmol/L NaHCO3溶液,2 mmol/L HNO3溶液,其中阳离子检测未使用抑制器,电导检测器检测。14种离子在一定浓度范围内线性关系良好,相关系数r都>0.999,F-,BrO3-,Cl-,NO2-,Br-,NO3-,PO42-,SO42-等8种阴离子的检出限分别为1.5,7.5,1.6,4.2,6.5,12.5,10.4,3.3μg/L,Li+,NH4+,Na+,K+,Mg2+,Ca2+等6种阳离子的检出限分别为4.6,12.3,8.5,19.8,12.4,17.9μg/L,平均回收率为92.3%~99.7%,标准偏差小于5%。方法适用于同时测定PM10中的多种水溶性离子。  相似文献   

11.
A simple sample preconcentration technique employing microwave-based evaporation for the determination of trace level bromate and perchlorate in drinking water with ion chromatography is presented. With a hydrophilic anion-exchange column and a sodium hydroxide eluent in linear gradient, bromate and perchlorate can be determined in one injection within 35 min. Prior to ion chromatographic analysis, the drinking water sample was treated with an OnGuard-Ag cartridge to remove the superfluous chloride and concentrated 20-fold using a PTFE beaker in a domestic microwave oven for 15 min.The recoveries of the anions ranged from 94.6% for NO2- to 105.2% for F-. The detection limits for bromate, perchlorate, iodate and chlorate were 0.1, 0.2, 0.1 and 0.2 microg/l, respectively. The developed method is applicable for the quantitation of bromate and perchlorate in drinking water samples.  相似文献   

12.
The on-line-coupling of ion chromatography (IC) and inductively coupled plasma mass spectrometry (ICP-MS) is a powerful tool for the determination of bromate in drinking waters. The use of a high-capacity and high-performance anion-exchanger combined with an NH4NO3-based elution system allows the determination of bromate in almost every water sample without any sample pretreatment. The method detection limits in the water samples investigated are 50 to 65 ng/L or 44 to 58 pg bromate, respectively. Considering sensivity as well as imprecision (5% at 500 ng/L bromate) and short analysis times (8 to 15 min per sample including sample uptake), the described IC-ICP-MS coupling is well suited for precise routine analyses of bromate in drinking waters at the sub μg/L level.  相似文献   

13.
离子色谱法测定水中的高氯酸盐   总被引:2,自引:0,他引:2  
采用离子色谱法测定了饮用水中痕量的高氯酸盐,以30mmol/LNaOH为淋洗液,1mL/min流量,1000μL进样,在25min内可完成测定高氯酸盐;利用加热浓缩的方法对水样进行前处理,浓缩10倍后进样。结果表明,该法回收率为87.9%,检测限为0.10μg/L,具有实际应用价值。  相似文献   

14.
Kosaka K  Asami M  Takei K  Akiba M 《Analytical sciences》2011,27(11):1091-1095
An analytical method for determining bromate in drinking water was developed using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The (18)O-enriched bromate was used as an internal standard. The limit of quantification (LOQ) of bromate was 0.2 μg/L. The peak of bromate was separated from those of coexisting ions (i.e., chloride, nitrate and sulfate). The relative and absolute recoveries of bromate in two drinking water samples and in a synthesized ion solution (100 mg/L chloride, 10 mg N/L nitrate, and 100 mg/L sulfate) were 99-105 and 94-105%, respectively. Bromate concentrations in 11 drinking water samples determined by LC-MS/MS were <0.2-2.3 μg/L. The results of the present study indicated that the proposed method was suitable for determining bromate concentrations in drinking water without sample pretreatment.  相似文献   

15.
Bromate is a well known by-product produced by the ozonation of drinking water; the allowed concentration for human consumption has to be regulated to low microgram l-1 range. By using a high-capacity anion-exchange column, it should be possible to determine bromate at this low concentration by direct injection of a very large volume (up to 1 ml) without any sample preconcentration and pretreatment. The feasibility of this technique for the determination of bromate in drinking water has been explored in our work. The experimental results showed that matrix effect, due to inorganic ions contained in drinking water, strongly influenced the chromatographic behaviour of the bromate peak. The increase of the total ion content led to a correlated decrease in the efficiency of the analyte peak so that effective detection limits depended on the matrix composition. In this work chromatographic parameters (efficiency, asymmetry and resolution) of bromate peak are discussed in relation to the concentration of the main inorganic anions, and the injection volume (from 250 microliters to 1 ml).  相似文献   

16.
抑制型电导检测离子色谱法测定饮用水中的痕量溴酸盐   总被引:3,自引:1,他引:3  
应波  李淑敏  岳银玲  鄂学礼 《色谱》2006,24(3):302-304
建立一种直接进样测定饮用水中痕量溴酸盐的电导检测离子色谱法。选用Metrosep A Supp 5阴离子交换分离柱,碳酸盐淋洗液。抑制型电导检测采用化学抑制器和CO2抑制器顺序双抑制系统。实验结果显示,溴酸根阴离子与常见共存阴离子完全分离,溴酸盐含量在5~100 μg/L范围内具有良好的线性(r=0.9999),精密度高(相对标准偏差(RSD)<4%),方法的检出限为0.50 μg/L,样品加标平均回收率为96.1%~107%。该方法操作简单,分离效果好,可与常见阴离子实现同时分析,灵敏度高,重现性好,可作为饮用水中溴酸盐的标准测定方法。  相似文献   

17.
Barron L  Paull B 《Talanta》2006,69(3):621-630
A new analytical procedure for the simultaneous determination of trace oxyhalides and haloacetic acids (HAs) in drinking water and aqueous soil extracts is described. The method uses micro-bore ion chromatography (IC) coupled with suppressed conductivity (SC) and electrospray ionization mass spectrometric detection (ESI-MS). The IC-SC-ESI-MS system included a secondary flow of 100% MeOH, which was added to the column eluate (post-suppressor) and resulted in a significant increase in sensitivity for all analytes. All ESI-MS parameters were optimized for HA analysis and sensitivity quantitatively compared to suppressed conductivity. Full analytical performance characteristics for the developed method are presented for monochloro-, monobromo-, dichloro-, dibromo-, trichloro-, bromochloro, chlorodifluoro-, trifluoro-, dichlorobromo- and dibromochloroacetic acid, as well as the oxyhalides iodate, bromate, chlorate and perchlorate. In the case of the HAs, an optimised 25-fold SPE preconcentration method meant all analytes could be readily detected well below the USEPA 60 μg/L regulatory limit using conductivity and/or ESI-MS. The IC-ESI-MS method was applied to the determination of oxyhalides and HAs in both soil extracts and drinking water samples. Soil samples were extracted using ultra pure water with subsequent determination of perchlorate at 1.68 μg/g of soil. A drinking water sample containing HAs was preconcentrated using LiChrolut EN solid phase extraction cartridges with subsequent sulphate and chloride removal. Total HAs were determined at 13 μg/L.  相似文献   

18.
建立一种检测饮用水中痕量溴酸盐的离子色谱方法。利用On GuardⅡAg柱过滤去除水中氯离子,直接进样,电导检测器检测。该方法避免了氯离子对溴酸盐的干扰,测定水质溴酸盐的灵敏度和准确度均有很大提高。溴酸盐的检出限为0.005 mg/L,测定结果的相对标准偏差为7.56%(n=7),加标回收率为92.0%~110.0%。该方法操作简便快速、准确度高,适合于饮用水中痕量溴酸盐的测定。  相似文献   

19.
Bromate ion in drinking water was determined by capillary zone electrophoresis (CZE) with direct photometric detection. Bromate ion in the sample solution was introduced and concentrated into the capillary by electrokinetic injection for 50s at -10 kV. Electrophoretic separation was made at an applied voltage of -25 kV and bromate ion was detected at wavelength 193 nm, at which the baseline was stabilized with less UV-absorbing acidic phosphate buffer. Bromate ion was detected within 5 min in the electropherogram. By increasing the electric conductivity in the migrating solution with 10 mM Na2SO4, a limit of detection (LOD) of 9 x 10(-10)M (0.1 microg/L BrO3-) was achieved. The proposed method was applied to the analysis of tap water and river water samples, but bromate ion was not detected. Because the practical samples contain relatively large amount of foreign ionic substances, the tap water sample was diluted to avoid the matrix ions. Bromate ion added in a tap water at the concentration of 8 x 10(-8)M was quantitatively recovered by diluting it 1/10.  相似文献   

20.
The development of a rapid method for the determination of perchlorate in rain and drinking waters is presented. In the optimised method, an on-line preconcentration technique was employed utilising a 10 mm × 4.6 mm Phenomenex Onyx monolithic guard cartridge coated with (N-dodecyl-N,N-dimethylammonio)undecanoate for selective preconcentration, with subsequent elution into a fixed volume injection loop (‘heart-cut’ of the concentrator column eluate) and separation using an IonPac AS16 (250 mm × 2 mm) anion exchange column and a potassium hydroxide concentration gradient. Off-line optimisation studies showed that the coated monolith displayed near quantitative recovery up to 50 μg/L perchlorate level from standards prepared in reagent water. On-line preconcentration of perchlorate obtained detection limits down to 56 ng/L in reagent water, between 70 and 80 ng/L in rainwater samples and 2.5 μg/L in non-pretreated drinking water. After an additional sample sulphate/carbonate removal step, low ng/L perchlorate concentrations could also be observed in drinking water. The complete on-line method exhibited reproducibility for n = 10 replicate runs of R.S.D. ≤ 3% for peak height/area and R.S.D. = 0.08% for retention time. The optimised method, of 20 min total duration, was applied to the determination of perchlorate by standard addition in 10 rainwater samples and one drinking water sample. Concentrations of perchlorate present ranged from below the detection limit for four rainwater samples, with another three samples showing perchlorate present at between 70 and 100 ng/L, and one sample showing perchlorate present at 2.8 μg/L. Levels of 1.1 μg/L in the drinking water sample were also recorded.  相似文献   

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