饮用水中的亚氯酸盐、氯酸盐和溴酸盐的离子色谱测定法

目的 建立同时测定饮用水中亚氯酸盐、氯酸盐和溴酸盐的离子色谱法.方法 选择IonPacAS23色谱柱,淋洗液为4.5mmol/L Na_2CO_3-0.8 mmol/L NaHCO_3,流速为1.0 ml/min,进样量为250 μl,电导检测池温度为30℃,色谱柱温度为35 ℃,流动相瓶加压为40 kPa,抑制器抑制模式为自动再生模式,抑制器电流为25 mA.结果 在0～1 000.0 mg/L范围内,亚氯酸盐的线性方程为:y=0.009 6+1.600 0x,r=0.999 3,检出限为5μg/L;溴酸盐的线性方程为:y=0.003 2+3.184 7x,r=0.999 9,检出限为5μg/L;氯酸盐的线性方程为:y=0.001 8+1.788 9x,r=0.999 9,检出限为5μg/L.加标回收试验结果显示,该方法的平均回收率为89.0%～108.0%,RSD为0.21%～2.70%.结论 该法操作简单、快速、准确,灵敏度高、干扰少,适用于饮用水中亚氯酸盐、氯酸盐和溴酸盐的同时测定.

Abstract：

Objective To develop an ion chromatography (IC) for simultaneous determination of chlorite, chlorate and bromate in drinking water. Methods The IC separation was carried out with the IonPAC AS23 column by using 4.5 mmol/L Na_2CO_3-0.8 mmol/L NaHCO_3 at the flow rate of 1.0 ml/min. The injection volume was 250 μl.the temperature of conductivity detector cell and column were 30 ℃ and 35 ℃, respectively. The pressure upon the bottle of mobile phase was 40 kPa. The current of auto-regenerating suppressor was 25 mA. Results The results showed that in the range of 0 to 1 000 mg/L, the calibration equation for chlorite was y=0.009 6+1.600 0 x (r=0.999 3),for bromate was y=0.003 2+3.184 7 x (r=0.999 9),for chlorate was y= 0.001 8+1.788 9 x(r=0.999 9).The detection limit of chlorite,chlorate and bromate were all 5 μg/ L,the recovery rates were 89.0% -108.0% and the relative standard deviations (RSD) were 0.21%-2.70%. Conclusion The method is simple,fast,accurate, sensitive, little interference and is applicable to the simultaneous determination of chlorite, chlorate and bromate in drinking water.     

离子色谱法同时测定饮用水中氯酸盐、亚氯酸盐和溴化物的研究

目的:建立饮用水中氯酸盐、亚氯酸盐和溴化物的离子色谱检测方法。方法:水样经过IonPac AS23型阴离子柱(4×250 mm)、IonPac AG23 4×50 mm保护住,采用ASRS300阴离子抑制器,利用4.5 mmol/L Na2CO3-0.8 mmol/L NaHCO3淋洗液,流速为1.00 ml/min和DS6型电导检测器进行检测。结果:本方法线性良好r,≥0.9996,精密度高(RSD<2%),样品加标回收率为88.0%～104.0%,最低检出量为0.0015 mg/L～0.0018 mg/L。结论:该方法操作简单、快速、准确、灵敏度高,适用于实际水样的测定。     

换柱测定生活饮用水中亚氯酸盐和氯酸盐的离子色谱法研究

目的建立能够同时测定生活饮用水中亚氯酸盐和氯酸盐的离子色谱法。方法在原来离子色谱仪的基础上把METROSEP A SUPP4色谱柱更换成METROSEP A SUPP7色谱柱,将水样经过0.45μm微孔滤膜过滤后,使水样中待测阴离子随淋洗液进入离子柱系统,以保留时间定性,以峰面积定量,定量方法为外标法。淋洗液为3.6 mmol/L的Na2CO3,流速为0.70 ml/min,进样量为20μl,柱温为45℃。结果在0 mg/L^0.5 mg/L内,亚氯酸盐的线性方程为Q=2.81233A+0.0171715,相关系数r=0.9995,检出限为0.001 mg/L;氯酸盐的线性方程为Q=2.87165A+0.396459,相关系数r=0.9999,检出限为0.001 mg/L。线性关系良好(r≥0.9995),精密度高(RSD<5%),检出限低(ClO2-和ClO3-均为0.001 mg/L),加标回收率ClO2-为96.5%~102.3%,ClO3-为97.0%~107.0%。结论该方法在不改变主要仪器的基础上,通过更换色谱柱。具有操作简单、分离效果好、准确、灵敏度高,适用于生活饮用水中亚氯酸盐和氯酸盐的检测。     

二氧化氯消毒饮用水中亚氯酸盐污染的初步研究

[目的]了解二氧化氯消毒饮用水产生的亚氯酸盐（ClO2^-)污染现状,并探讨其成因和对策。[方法]选择2个自来水厂,其中水厂以受轻度有机物污染的地面水为水源,乙水厂以未受有机物污染的地下水为水源,两个水厂均使用二氧化氯发生器,主要原料甲厂为亚氯酸盐,乙厂为氯酸盐。采用电流滴定仪法测定这2个水厂出厂水中ClO2^-浓度。[结果]出厂水ClO2^-浓度：甲厂0．530－0．760mg/L,为标准值的2．6－3．8倍,超标率100％;乙厂0．100－0．733mg/L,其中超标浓度值范围0．257－0．733mg/L,为标准值的1．3－3．7倍,超标率83．3％。[结论]甲、乙自来水厂出厂水中由二氧化氯消毒产生的消毒副产物亚氯酸盐污染较严重。     

饮用水中亚氯酸盐、溴酸盐和氯酸盐的离子色谱测定法

目的建立能同时测定饮用水中亚氯酸盐、溴酸盐和氯酸盐的方法。方法采用离子色谱法,选用IonPacAS9分离柱,10.0mmol/LNa2CO3为淋洗液,水样经沉淀脱色后,过滤进样分析。结果方法的相关性好(r0.9992),线性范围广,检出限低(0.0028～0.0087mg/L),RSD2.82%,样品加标回收率为92.6%～102.6%。结论该法干扰小,灵敏度高,结果准确、操作简便,适合饮用水中亚氯酸盐、溴酸盐和氯酸盐的同时检测分析。     

Algal toxicity of the alternative disinfectants performic acid (PFA), peracetic acid (PAA), chlorine dioxide (ClO2) and their by-products hydrogen peroxide (H2O2) and chlorite (ClO2−)

Environmental effect evaluation of disinfection of combined sewer overflow events with alternative chemical disinfectants requires that the environmental toxicity of the disinfectants and the main by-products of their use are known. Many disinfectants degrade quickly in water which should be included in the evaluation of both their toxicity as determined in standardized tests and their possible negative effect in the water environment. Here we evaluated according to the standardized ISO 8692 test the toxicity towards the green microalgae, Pseudokirchneriella subcapitata, of three disinfectants: performic acid (PFA), peracetic acid (PAA) and chlorine dioxide (ClO₂) as well as two by-products of their use: hydrogen peroxide (H₂O₂) and chlorite. All of the five chemicals investigated showed clear toxicity to the algae with well-defined dose response curves. The EC₅₀ values ranged from 0.16 to 2.9 mg/L based on nominal concentrations leading to the labeling of the chemicals as either toxic or very toxic. The five investigated chemicals decreased in toxicity in the order chlorine dioxide, performic acid, peracetic acid, chlorite and hydrogen peroxide. The stability of the chemicals increased in the same order as the toxicity decrease. This indicates that even though ClO₂ has the highest environmental hazard potential, it may still be suitable as an alternative disinfectant due to its rapid degradation in water.     

氢氧根淋洗离子色谱法测定水中亚氯酸盐和氯酸盐

目的建立氢氧根淋洗系统离子色谱法测定水中亚氯酸盐、氯酸盐,应用该方法检测消毒副产物含量。方法选用AS19和AG19阴离子交换柱,ICS1100赛默飞离子色谱仪,要求仪器具备有电导检测器,使用外标法定量。选用100μl量环,RFC30自动淋洗装置,优化淋洗程序。结果在0500μg/L浓度范围内,亚氯酸盐和氯酸盐线性关系良好,r=0.999 0,测定亚氯酸盐的加标回收率为96.2%106.3%,RSD为1.9%6.9%,检出限为0.06μg/L。氯酸盐加标回收率为91.4%106.8%,RSD为1.7%5.4%,检出限为0.11μg/L。结论该方法用于克服碳酸盐淋洗系统背景电导高等缺点,使基线更加平稳、快速、准确、灵敏度高,检出限大幅降低。     

离子色谱法测定饮用水中3种加氯消毒副产物

目的 建立离子色谱法测定饮用水中CIO2^-、BrO3^-、CIO3^-等加氯消毒副产物。方法 采用AS9-HC阴离子分离柱，9mmoL／L碳酸钠淋洗液，流速为1．2ml／min，进样量20μ可在15min内分离3种加氯消毒副产物。结果 3种物质浓度在O～1OO0μg／L范围内时，其色谱峰面积与浓度呈良好的线性关系，相关系数在0．999以上。检出限分别为CIO2^2．1μg／L、BrO3^-8．5μg／L、CIO3^-4．1μg／L。高、中、低3个浓度水平的加标回收率在96．8％～104．3％之间；日内变异为2．6％～7．5％，日间变异为3．8％～9．2％。结论 离子色谱法符合定量分析的要求，可推广应用于实际水样的测定。     

离子色谱法测定饮用水消毒副产物亚氯酸盐、氯酸盐和溴酸盐

目的建立饮用水中消毒副产物（DBP）亚氯酸盐、溴酸盐、氯酸盐的离子色谱检测方法。方法用IonPac23（4×250mm）型阴离子分析柱和（4×50mm）型阴离子保护柱。DS6抑制型电导检测器,抑制器采用ASRS3004mm型,淋洗液浓度：4.5mmol/L Na2CO3~0.8 mmol/L NaHCO3,流速：1.0ml/min。结果本方法线性关系良好（r≥0.999）,精密度高,5.0μg/L添加水平相对标准偏差（RSD）〈10%。在10.0μg/L、50.0μg/L、150.0μg/L三种浓度添加水平下,平均回收率在96.9%~99.1%之间。亚氯酸盐、溴酸盐、氯酸盐最低检测浓度分别为3.1μg/L、3.0μg/L、3.7μg/L。结论该方法操作简单,灵敏度高,适用于饮用水中亚氯酸盐、溴酸盐、氯酸盐的检测。     

饮用水中氯酸盐、亚氯酸盐和溴酸盐的离子色谱测定法

目的 建立水中亚氯酸盐、氯酸盐及溴酸盐的离子色谱最佳检测方法.方法 水样经0.22μm的水性滤膜过滤,然后经过IonpacAS19-HC型分离柱(4 mm ×250 mm)、IonpacAG19-HC型保护柱、ASRS300(4-mm)阴离子抑制器、KOH自动淋洗液、电导检测器检测,保留时间定性,峰面积定量.结果 该方法线性良好(ClO2-:r =0.9994;BrO3-:r=0.9992;ClO3-:r =0.9998),精密度高(RSD ＜5％),样品加标平均回收率为88.5％ ～ 101.2％.结论 该方法具有操作简单、快速、准确、灵敏度高、干扰少的优点,具有较好的实用性.