离子色谱法测定岩石,土壤,水系沉积物等样品中的氯,溴,碘

本文采用碳酸钠一氧化锌烧结法分解样品,利用DIONEX2020i离子色谱仪,电导、电化学检测器,建立了一测定岩石等样品中氯、溴、碘的分析流程。实验表明,本方法选择性好,灵敏度高,检出限分别为:氯1.03×10~(-6)、溴0.012×10~(-6)、碘0.014×10~(-6)。     

气化—离子色谱法测定岩石中的氯

氯的化学性质活泼,在酸性介质中具有挥发性,由碱性物质吸收,样品在密封的气化吸收器中经处理后用离子色说测定,无污染,操作简单,精度与准确度高,该法用于多种样品的分析,获得较满意的结果。     

离子色谱法测定煤中的氯

采用离子色谱法测定原煤中的总氯,标准工作曲线的线性范围在０ ．０１ ～２４ ｍｇ／ Ｌ,相关系数为０ ．９９９ ８ ,测定ρ（ Ｃｌ－ ） ＝ １ ．２０ ｍｇ／ Ｌ 的标准溶液１０ 次,ＲＳＤ 为０ ．７７ ％ 。用艾氏卡试剂在８００ ℃±２５ ℃下分解煤样,去离子水浸提后用离子色谱法测定原煤中的总氯。测定了１８ 个煤样中的氯,加标回收率为９７ ．８ ％ ～１０４ ．４ ％ ,与银量滴定法对照,两种方法基本相符。     

超声提取-离子色谱法测定铁矿石中水溶性氟氯溴及硝酸根

铁矿石样品经超声提取、离心机分离沉淀后,分别通过IC-RP柱、IC-Na柱及0.22μm微孔过滤膜过滤,25.00 mmol/L NaOH溶液作为淋洗液,利用AS-19型阴离子分离柱和ASRS 300-4 mm连续自动再生化学抑制器分离样品中氟、氯、溴和硝酸根多种水溶性阴离子和采集数据。经过IC-RP柱可吸附样品溶液中有机质,通过IC-Na柱可将溶液中重金属离子置换成Na+,使之与淋洗液的阳离子成分一致。对水溶性阴离子的提取效率进行实验,确定提取时间为30 min。在标准溶液及待测样品溶液中加入一定量相应的淋洗液,使溶液和淋洗液的电导值相匹配来消除水负峰的影响。F-、Cl-、Br-、NO3-的方法检出限分别为2.1、3.5、2.5、2.0μg/g,工作曲线的相关系数>0.999。用铁矿石标准样品GBW 07218a验证方法的准确度与精密度,测定值与标准值基本吻合,精密度(RSD,n=10)小于5%,加标回收率为96%～104%。用于实际样品的分析,测定值与离子选择电极法结果接近。方法线性范围宽,操作简单,快速高效,适用于实验室日常检测工作。     

水蒸气蒸馏-离子色谱法测定岩石中的氟和氯

氟和氯的化学性质活泼,在酸性介质中具有挥发性,试验建立了样品经磷酸溶解用水蒸气将氟和氯带出,用离子色谱法测定Ｆ,Ｃｌ的方法,该法具有操作简单,快速,可靠等优点。     

离子色谱法测定土壤中有效氟

利用离子交换-电导检测离子色谱法对土壤中有效氟进行测定。选用30 mmol/L氢氧化钾溶液作为淋洗液,流速1.20 mL/min,准确测定有效态(可提取态)氟含量。方法加标回收率为95%~108%,精密度好,检出限低,操作简单,对环境无污染,适合于土壤污染状况的调查。     

离子色谱梯度淋洗技术检测水中阴离子

通过实验确定了使用梯度淋洗技术检测矿泉水中阴离子的方法。检出限能够达到5.4～25.5ng/mL,精密度能够达到0.33%～1.10%。     

气相色谱法测定土壤中六六六和滴滴涕

采用丙酮～石油醚提取,以浓硫酸净化,用带电子捕荻检测器的气相色谱仪测定。方法的检出限分别为α-六六六1．6ng／g,β-六六六3．2ng／g,γ-六六六1．7ng／g,δ-六六六2.0ng／g,P,P’-DDE3．1ng／g,P,P’-DDD3．2ng／g,o．P’-DDT3．4ng／g,P,p’-DDT、4．1ng／g。测得精密度RSD(n=6)≤9．0,回收率89．0％～99．9％。     

电导检测器—单柱离子色谱法同时测定饮用水中几种微量阴离子

本文研究了单柱离子色谱法测定饮用水中微量阴离子的方法 ,样品经微孔滤膜过滤即可直接进样分析。淋洗液最佳浓度为 2 5mmol/L邻苯二甲酸氢钾溶液 ;电导检测器检测灵敏度为 3 2 μS/cm2 。该方法简便快捷、灵敏 ,选择性好     

离子色谱法测定冰川末端大气PM2.5可溶性离子及其来源解析

为了研究祁连山西段冰川末端地区大气PM_2.5细粒子中可溶性无机离子组分的变化特征,于2011年采集了一批大气PM_2.5的Telfon滤膜样品,并应用离子色谱对可溶性离子进行了分析。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25 mL,萃取时间为30 min,萃取液用0.45μm纤维滤膜过滤,各种离子在一定浓度范围内线性关系良好,相关系数r>0.999。所测样品的阴阳离子中,SO₄^2-、NO₃^-、Ca²⁺、和NH₄⁺的质量浓度约占到水溶性离子总量的88%。可溶性离子浓度呈现出春夏高、秋冬低的季节变化特征,夏季可溶性离子浓度最高。     

电导检测器—单柱离子色谱法同时测定饮用水中几种微量阴离子

本文研究了单柱离子色谱法测定饮用水中微量阴离子的方法，样品经微孔滤膜过滤即可直接进样分析，淋洗液最佳浓度为2．5mmol/L邻苯二甲酸氢钾溶液；电导检测器检测灵敏度为3．2μS/cm^2，该方法简便快捷、灵敏，选择性好。     

Analysis of fluoride, chloride, nitrate and sulphate in natural waters using ion chromatography

The analysis of anion components of thirty natural water samples using an ion-chromatographic method were compared to analyses for F, Cl, NO₃ and SO₄ obtained by presently used techniques. Of these thirty samples, five were replicates. Precision estimates were also calculated from synthetic solution replicates. In addition, a comparison of results obtained through separator columns of two different lengths (250 mm and 500 mm) was completed. An inter-anion interference test indicated that, at pH 6, analysis of low concentrations of any one of the four anions studied was not affected by large concentrations of the other three anions. Reported detection limits for the ion-chromatographic technique are one to two orders of magnitude below routine methods. Replicate sample analysis indicated that a relative standard deviation below 1 percent was possible for F, Cl, NO₃ and SO₄.     

吹扫捕集-气相色谱-质谱法测定土壤中挥发酚的方法研究

文章研究了吹扫捕集-气相色谱-质谱法测定土壤中挥发酚的方法,分析了吹扫捕集各参数对挥发酚测定的影响,优化了吹扫捕集条件和气相色谱-质谱条件.通过与索氏提取技术对比,证明吹扫捕集-气相色谱-质谱法在实际样品检测中具有操作简便、分析周期短、试剂用量少、干扰小等优点,适用于测定沸点较低、溶解度较小的挥发酚,推荐选择经典的索氏提取技术测定沸点较高、溶解度较大的挥发酚.     

Analysis of bromate and bromide in drinking water by ion chromatography-inductively coupled plasma mass spectrometry

A method for the detection of bromate and bromide in drinking water by ion chromatography-inductively coupled plasma mass spectrometry (IC-ICP-MS) was developed. The optimized conditions of IC including pH and concentration of the effluent were studied. The results showed that the above two species of bromine were baseline separated within nine minutes under the optimized conditions. The detection limits (S/N=3) of bromate and bromide were 0.23 and 0.12 μg/L, respectively. The RSD (n=6) of the peak areas was 1.2%-3.5%. The method has been successfully applied to the determination of the type bromide in drinking water samples. The recoveries were 95%-109%. The method can be used for the regular analysis of bromate and bromide in real drinking water samples.     

Measurement of free heavy metal ion concentrations in soils using Donnan membrane technique

In natural systems heavy metals are present in very low concentrations (less than micro-molar) , so precise measurement of the free metal ions is difficult. Recently, a new method has been developed called the Donnan membrane technique (DMT). Several heavy metals could be measured simultaneously using this method. Furthermore, all the metals did not interfere with each other, and the balance between the measured system and the surrounding condition could not be disturbed. Improvements were made according to the internal condition. The free heavy metal ion concentrations were measured in different systems using the improved method, and satisfied results have been obtained.