水杨酸法检测水质氨氮的改进方法

该氨氮检测方法是对水杨酸分光光度法的改进,通过将50 g/L的水杨酸改为150 g/L的水杨酸钠,将有效氯为3. 5 g/L的次氯酸钠溶液改为5 g/L的二氯异氰尿酸钠溶液,增加了检测试剂的稳定性和贮存时间,同时将氨氮测定上限从1 mg/L提高至2. 5 mg/L,并将显色时间从60 min优化为30 min,使得此方法更为便捷。该方法的氨氮标准曲线线性关系良好,相关系数为0. 999 6,准确性和精密度高,加标回收率良好,适用于不同类型水质中氨氮的检测。     

金膜吸附-冷原子吸收光谱法测定空气中的汞

采用新型金膜吸附-冷原子吸收光谱法测定空气中的汞，在0μg/L～100μg/L范围内线性良好，相关系数为0．9991。方法检出限为1．6 ng/m3，RSD为0．5％～2．7％，测定两种不同浓度的汞标准样品，相对误差为6．1％和3．2％。与两种现行国标方法（巯基棉富集和高锰酸钾溶液吸附法）比较，该方法所需试剂种类少，操作简便、吸附效率好，加标回收率高。     

环境水质氨氮的快速检测

采用全固体混合试剂,将改进的水杨酸分光光度法应用于水质氨氮的测定.络合物的最大吸收波长为697 nm,表观摩尔吸光系数为2.00×104 L/(mol·cm),氨氮质量浓度在0.01 mg/L～1.00 mg/L之间符合比尔定律,反应产物颜色在3 h内保持稳定,常见的共存离子均不干扰测定,混合试剂保存期长,可用于环境水质氨氮的快速检测.     

胭脂红酸分光光度法测定废水中硼

用胭脂红酸分光光度法测定废水中的硼，着重进行了方法的条件和干扰试验。方法检测限为0.063mg/L，线性范围为0.21mg/L-1.25mg/L。5个实验室对5.00mg/L硼标准样品测得重复性相对标准差为3．4％，再次性相对标准差为3．6％；相对误差为－0．8％－1．4％，回收率在95．2％－104．6％之间。     

在线蒸馏-无人值守连续流动分析法测定污水中氨氮

采用在线蒸馏-无人值守连续流动分析法对污水中氨氮进行检测,方法在0.00~10.0 mg/L范围内线性良好,检出限为0.014 mg/L,实际样品测定的相对标准偏差为1.24%~4.15%,加标回收率为93.0%~108%,精密度和准确度均能满足污水中氨氮的测定要求。     

气相色谱法测定环境空气中乙醇和异丙醇

采用蒸馏水吸收空气中的乙醇和异丙醇，气相色谱法测定，该方法在3．14 mg/L ～15．8 mg/L 范围内线性良好，乙醇标准曲线的相关系数为0．9994，异丙醇标准曲线的相关系数为0．9996。测定低浓度标准溶液，得到乙醇和异丙醇的检出限分别为0．418 mg/L 和0．399 mg/L；采样体积为0．04 m3时，乙醇和异丙醇最低检出质量浓度均为0．05 mg/m3。乙醇和异丙醇标准溶液的回收率为95．4％～104％，RSD＜5％。样品稳定性试验表明，采集的乙醇和异丙醇样品保存时间越长损失率越大，一般保存7 d为宜。     

污水处理厂氮排放特征

为了更好地掌握污水处理厂运行和排放情况，在全国南方、北方分别选取3个省共11个城市122家污水处理厂，于2013年8—10月进行了专项监测。结果表明：75?4％的污水处理厂氨氮出水质量浓度小于2 mg／L，氨氮平均去除率达90?2％，但总氮的平均去除率仅为55?5％，污水处理厂排水中仍存在较多非氨氮形态的氮污染进入环境。氨氮排放达标的污水处理厂中，有约20％的总氮排放未达标。65?5％的污水处理厂出水氨氮占总氮的比例低于10％，而84?4％的污水处理厂进水中氨氮占总氮的比例高于50％。总氮是影响污水处理厂达标排放的主要污染因子。     

纳氏试剂比色法测定海水中的氨氮

进行了用纳氏试剂比色法直接测定海水中氨氮的试验。试验表明，可用酒石酸钾钠溶液—氢氧化钠溶液作为掩蔽剂排除海水中钙、镁离子对测定的干扰。着重对氢氧化钠溶液用量、显色剂用量和显色时间进行了试验，以用200g／L氢氧化钠溶液2．5mL，纳氏试剂1．5mL，显色25min为最佳测定条件，并对水样中的盐度影响作了考察。氨氮质量浓度在0．01mg／L—0．40mg/L范围内符合比耳定律，检出限为0．01mg／L；平行样相对偏差为9％，加标回收率在91％—108％之间；相对盐度为10—32的海水可以直接测定。     

原子荧光光谱法测定水中低含量锡

采用原子荧光光谱法测定水中锡，结果表明，方法检测限为0．14μg／L，在0、0μg／L～100μg／L范围内线性良好。不同浓度标准溶液测定的相对误差≤2．0％，实际样品测定的加标回收率在90．0％～109％之间，相对标准差≤6．1％，准确度和精密度均较好。     

超高效液相色谱紫外-三重四级杆质谱检测器联用测定地表水中甲萘威

采用二氯甲烷提取地表水，浓缩后经超高效液相色谱紫外-三重四级杆质谱检测器联用测定甲萘威。试验表明：紫外检测器测定甲萘威，在2．00μg/L～500μg/L范围内线性良好，相关系数为0．9992，检出限为0．500μg/L；三重四级杆质谱检测器测定甲萘威，在0．100μg/L～200μg/L范围内线性良好，相关系数为0．9990，检出限为0．009μg/L；实际水样3个浓度水平的加标回收率为92．4％～98．4％，RSD为2．5％～6．5％。该方法中双检测器联用测定地表水加标样品，使得定性定量更加准确。     

基于Berthollet反应示波极谱法测定水中微量氨

在亚硝基铁氰化钾存在下,氨在氢氧化钠介质中与苯酚、次氯酸钠反应,其产物靛酚在滴汞电极上产生－灵敏的吸附波,ＮＨ３－Ｎ在０．００３～０．２２ｍｇ／Ｌ内,导数峰电流与其呈良好的线性关系。用于环境水中ＮＨ３－Ｎ的测定,其相对标准偏差小于３％,回收率为９７％～１０５％,方法具有较好的选择性。     

PM2.5中典型水溶性离子在线观测标准曲线优化研究

为了研究在线离子色谱法测定大气PM2.5中NH4^+、NO3^-、SO4^2-的不确定性来源,探讨了标准曲线的浓度范围及浓度梯度设置对离子浓度结果的影响,并对标准曲线设定方案进行了优化。结果表明:不同浓度范围的标准曲线对于NH4+的浓度结果有较大的影响,存在1. 87%~14. 91%的偏差,对于NO3^-、SO4^2-的影响较小,相对偏差分别为2. 94%和2. 82%;非均匀布点和均匀布点标准曲线定量NH4+的结果存在4. 15%~4. 25%的偏差,对于NO3^-和SO4^2-,相对偏差分别为0. 10%和5. 99%。对于二次拟合的NH4^+,在样品浓度波动较大时,可以将样品划分为低浓度范围和高浓度范围,分别选用低浓度段标准曲线和高浓度段标准曲线,以期得到更合理的浓度结果。     

Atmospheric NO2 and NH3 deposition into a typical agro-ecosystem in Southeast China

The dry deposition of atmospheric nitrogen (including NO(2) and NH(3)) into a typical agro-ecosystem in Southeast China during 2006-2007 was estimated. Results indicated that the dry deposition velocities of NO(2) and NH(3) ranged from 0.04-0.24 cm s(-1) and 0.09-0.47 cm s(-1), respectively. The higher values appeared in the non-crop growing period. Concentrations of atmospheric NO(2) and NH(3) ranged from 24.64-104.10 μgN m(-3) and 14.40-389.6 μgN m(-3), respectively. Variation of the NH(3) mixing ratio showed a clear double-peak. NO(2) and NH(3) deposition fluxes were 74.68-80.75 kgN ha(-1), which was equivalent to 162.4 and 175.5 kg ha(-1) of urea applied in 2006-2007. The N deposition fluxes were 13.91-40.38 and 5.33-22.73 kgN ha(-1) in peanut and rice growing periods, accounting for 8.18%-40.38% and 2.13%-23.06% of N fertilizer usages, respectively. NO(2) and NH(3) deposition were significant for the red soil farmland.     

垃圾渗滤液氨态氮与挥发性脂肪酸馏出规律研究

为了提高垃圾渗滤液氨态氮（NH4^＋-N）与挥发性脂肪酸（VFA）联合滴定分析结果的准确性，试验研究了NH4^＋-N与VFA的馏出规律，并在此基础上对联合滴定方法的优化进行了探讨。结果表明：测得的NH4^＋-N质量浓度（Y1）、VFA浓度（Y2）与馏出液体积（X）分别符合函数关系式；联合滴定分析过程中，渗滤液样品NH4^＋-N质量浓度应稀释至150mg／L-200mg／L，NH4^＋-N馏出液应大于蒸馏液体积的60％；VFA分析应采用“一次蒸馏80％＋二次蒸馏”的方式，且VFA二次馏出液应大于蒸馏液体积的75％（相对误差限εr〈5％）。     

砷化氢-钼蓝光度法测定环境样品中砷

介绍了用砷化氢 -钼蓝光度法测定水质、土壤和沉积物样品中砷 ,对测定条件中的砷化氢反应时间、显色酸度、碘 -碘化钾溶液用量、钼酸铵用量和干扰物质等进行了试验。方法检测限为 7μg/L ,平均回收率在 97%～ 10 5 %之间 ,相对标准差为 2 5 % ,摩尔吸收系数为 2 4× 10 4 。     

海河下游水体中DO与NH_3-N、COD_(Mn)相关关系探讨

本文应用近年来海河下游监测数据对ＤＯ与ＮＨ３Ｎ和ＣＯＤＭｎ进行一元线性回归，得到两回归方程：ＮＨ３Ｎ＝－１２８ＤＯ＋１０５４；ＣＯＤＭｎ＝－１１３ＤＯ＋１６９２。并经相关系数和回归系数显著性检验，表明在９９９％的置信水平下ＤＯ与ＮＨ３Ｎ和ＣＯＤＭｎ线性相关均极其显著     

氯化铵-火焰原子吸收光谱法测定地表水中的总铬

应用原子吸收法测定水样中的总铬，在不同条件下对空白样品、标准样品和实际样品进行试验分析，进一步验证了方法的准确度和精密度，加标回收率在96.8%-103%之间，相对标准偏差为2.1%。试验表明，该方法准确可靠，实际操作具有可行性，适用于工业废水和受污染地表水中总铬的测定。     

Monitoring ammonia in urban, inner alpine and pre-alpine ambient air

Passive samplers were used to monitor ammonia concentrations at rural inner alpine and pre-alpine, as well as urban, sites in Austria and Bavaria. Elevated concentrations were measured both at farms (up to 36 microg NH3 m(-3)) and at urban locations (up to 28 microg NH3 m(-3)). At urban locations a linear relationship between the traffic density and the NH3 concentration was found, but there was no marked seasonal trend. The highest ammonia concentrations were measured in a traffic tunnel (up to 78 microg NH3 m(-3)). The presence of livestock breeding or small scale alpine pastures resulted in elevated concentrations at the rural sites (8.1-12 and 2.5-4.6 microg NH3 m(-3), respectively), compared to the surrounding areas (3.1 and 0.9 microg NH3 m(-3)). Agriculture related sources are usually limited either spatially or seasonally. As the emissions were moderate in our case, a rapid removal and dilution of ammonia was possible and therefore the NH3 burden was only local. Sources related to traffic are more evenly distributed both geographically and seasonally. The WHO guideline, annual average concentration of 8 microg m(-3) for the protection of vegetation, was only exceeded at farms, at the urban station with the heaviest traffic and in the Tauerntunnel.     

Ammonia Monitoring in Switzerland with Passive Samplers: Patterns, Determinants and Comparison with Modelled Concentrations

Gaseous ammonia (NH3) is an important form of N deposition to ecosystems, but it is not being routinely monitored in Switzerland. Therefore, a study was conducted to estimate annual means and seasonal patterns of NH3 concentrations for different site types in Switzerland, and to compare annual measured and modelled NH3 concentrations. NH3 concentrations were measured using the 'Zürcher' passive sampler, a Palmes type sampler with an acidic solution as absorbent. Twenty-four sampling sites were run for one year, and 17 for two years. The samplers were changed fortnightly or monthly. Spatial emission patterns were mapped by combining information on (1) the location of emission sources, (2) national statistics on NH3-emitting activities and (3) activity-specific emission factors. The spatial resolution was one hectare. The mean annual NH3 concentration in the ambient air of the 41 sites was 2.5+/-0.3 microg m(-3) (mean+/-standard error). It ranged from 0.4 to 7.5 microg m(-3). The site type and the season were the most important factors explaining the variation in the seasonal mean concentration. NH3 concentrations were highest in intensively used agricultural areas and in cities, and lowest in Alpine sites remote from emission sources. At 39 out of 41 sites, the NH3 concentrations were higher in summer (3.1+/-0.3 microg m(-3)) than in winter (2.0+/-0.3 microg m(-3)). Modelled NH3 concentrations did not systematically deviate from measured concentrations (r2 = 0.69). With the combined monitoring and modelling approach, it is now possible to obtain a reasonable and consolidated picture of the overall NH3 situation in Switzerland.     

甲醇等5种强极性有机物污染事故中的监测分析方法

建立了在突发性水污染事故中定量分析水样中甲醇、丙酮、乙腈、N,N-二甲基甲酰胺和N,N-二甲基乙酰胺等5种极性有机物的实验室和现场应急监测分析方法。采用顶空-车载气相色谱质谱法用于现场快速定性定量分析;顶空-气相色谱法用于实验室准确定量分析。通过优化顶空及气相参数,在最佳实验条件下测得顶空-气相色谱质谱法中甲醇、丙酮、乙腈、N,N-二甲基甲酰胺、N,N-二甲基乙酰胺等5种化合物的检出限分别为1.0、0.06、0.5、10.0、15.0 mg/L,平行测定7次结果的相对标准偏差分别为2.1%~3.8%,加标回收率为69.4%~104%;顶空-气相色谱法灵敏度高于气相色谱质谱法,检出限分别为0.08、0.01、0.03、1.7、1.7 mg/L,平行测定7次结果的相对标准偏差分别为2.5%~4.1%,加标回收率为78.1%~116%。