水质总氮测定影响因素分析

总氮是水质监测特别是湖库水质的重要指标之一,应用碱性过硫酸钾消解紫外分光光度法测定总氮时,空白校正吸光度不易控制,主要考虑药剂与消解时间,要选择合乎标准要求的过硫酸钾,必要时加以重结晶提纯,且碱性过硫酸钾溶液宜现用现配。消解时间不足,难以完全消解所有的过硫酸钾,应保证在达到规定的温度与压力后,消解时间保持在40min以上。     

地面水总氮测定中样品消解时间的改进

针对过硫酸钾氧化－紫外分光光度法测定水样总氮方法中消解时间需保持３０ｍｉｎ的问题，进行了缩短时间为试验，确认消解时间由３０ｍｉｎ缩短至１０ｍｉｎ，总氮测定结果令人满意。     

总氮测试中碱性过硫酸钾溶液的稳定性

采用GB 11894-1989<过硫酸钾氧化-紫外分光光度法>测定地表水中总氮时,方法规定碱性过硫酸钾溶液最长可贮存1周,为了节约时间和试剂,现对配制的碱性过硫酸钾溶液作稳定性试验,以了解碱性过硫酸钾溶液在常温下的最长保存时间.     

烘箱加热—碱性过硫酸钾消解—离子色谱法分析水中总氮

总氮是地表水监测的指标,目前采用的方法是碱性过硫酸钾消解—紫外分光光度法。该法操作繁琐,空白值较高及选择性较差。笔者在参考有关文献的基础上,研究了烘箱加热—碱性过硫酸钾消解—离子色谱法测定水中总氮,结果表明,该法操作简便,选择性好,测定精密度和准确度满足要求,表明该方法测定结果可靠,具有一定的应用价值。     

紫外法测定水中总氮校准曲线制备的简化

《水和废水监测分析方法 (第 3版 )》中测定总氮 ,通常在碱性介质条件下 ,用过硫酸钾对水样进行消解处理。在制备校准曲线时 ,标准系列亦需经过消解处理。今对标准系列作消解、不消解两种方法对比 ,用紫外分光光度法 (分别于波长 2 2 0ｎｍ与 2 75ｎｍ处测定吸光值 ,按式Ａ =Ａ2 2 0 - 2Ａ2 75计算硝酸盐氮的吸光值 ,从而算出总氮的含量 )测定。1　空白值测定用 6份无氨水各加碱性过硫酸钾溶液 5ｍＬ ,按操作方法进行消解处理 ,测定结果见表 1。表 1　空白测定值 (Ａ0 =Ａ0 2 2 0 - 2Ａ0 2 75)Ａ ｘ ｓ空白值 0 0 2 6 2 0 0 0 0 75本方法…     

测定水样中总氮的方法探讨

针对过硫酸钾氧化-紫外分光光度法测定水样中总氮消解时间和水样中含悬浮物较多情况,通过多次试验。确认消解时间应在40min以上,并离心去除悬浮物,测定总氮效果良好。     

地表水中总氮测定方法的改进

测定地表水中总氮通常选用的是碱性过硫酸钾消解紫外分光光度法(HJ636-2012),但是在监测分析过程中发现,由于过硫酸钾溶解度较低,每配制200mL该试剂在不停地手工搅拌下需要1~4h左右对过硫酸钾进行溶解,非常难配制,而过硫酸钠易溶于水,用过硫酸钠配制碱性消解液比较容易,所以,通过实验用两种消解剂对总氮样品进行消解测定,比较两种试剂对校准曲线、实测样品、精密度与准确度的影响,提出了用过硫酸钠配制消解剂对地表水中总氮样品进行消解测定的实验方法。     

水样总氮测定空白值偏高的探讨

根据《水质总氮的测定碱性过硫酸钾消解紫外分光光度法》（GB11894—89）测定地表水中的总氮时,空白试验的吸光值常偏高。经对加热消解时间、试验用水水质、试剂添加顺序、储存时间等因素进行了试验,并对操作步骤影响吸光度空白值作了探讨。     

水中总氮测定方法存在问题的研究及改进

碱性过硫酸钾消解紫外分光光度法测定水中总氮采用的消解器皿是玻璃比色管,易造成空白偏高、结果偏低等问题。采用双圆柱状的消解杯对水样进行消解。结果表明,消解杯消解水中总氮,线性相关系数均大于0.999,检出限为0.05 mg/L,相对标准偏差小于5%,相对误差为0.88%~1.00%;改进后的消解器皿具有较好的精密度和准确度,能够更加准确测定水中总氮的含量。     

碱性过硫酸钾消解测定城市污泥中总氮

城市污水处理厂污泥经风干粉碎后，用碱性过硫酸钾溶液在高压器皿中于124℃消解，取上清液以紫外分光光度法测定总氮。对11个污泥样品测定，相对标准差≤1．5％精密度较好。并用L-谷氨酸标准物加入11个溶液样品中作回收试验，回收率在94％～107％之间，准确度亦较好。     

Atmospheric aerosol concentration level and chemical characteristics of water-soluble ionic species in wintertime in Beijing,China

Total suspended particulate (TSP) samples were collected during wintertime from November 24, 1998 to February 12, 1999 in Beijing. Ionic species including Cl-, NO3(-), SO4(2-), Na+, NH4(+), K+, Mg2+ and Ca2+ were determined by Ion Chromatography (IC). The sum average concentration of all the determined ions accounted for 18.9% of the TSP concentration, and SO4(2-) appeared the dominant ion with an average concentration of 30.84 microg m(-3); the sum mass concentration of SO4(2-), NO3(-), Ca2+ and NH4(+) accounted for about 83.2% of all the eight ions measured. The study indicated that the chemical form of sulfate and ammonium varies with TSP concentration levels. During heavy pollution periods, the average TSP concentration was 0.66 mg m(-3), and the NH4(+)/SO4(2-) molar ratio was low (0.58). It indicated that sulfate may present as CaSO4 and (NH4)2SO4 x CaSO4 x 2H2O. When TSP concentration (average 0.186 mg m(-3)) was relatively low, the NH4(+)/SO4(2-) molar ratio was 1.94, close to the theoretical ratio of 2 of (NH4)2SO4. Under this condition (NH4)2SO4 is expected to exist as the major form of sulfate. When the TSP concentration level was medium (average 0.35 mg m(-3)), the NH4+/SO4(2-) molar ratio appeared an average value (1.27), (NH4)2SO4, (NH4)2SO4 x CaSO4 x 2H2O and CaSO4 are expected to be present in those aerosol particles. Meteorological conditions including wind speed and wind direction were related to the TSP concentration level.     

石家庄市大气颗粒物中水溶性无机离子污染特征研究

用超声萃取－离子色谱法分析了石家庄市大气颗粒物中8种水溶性无机离子。结果表明,NO3－、SO2－4、NH4＋及 Ca2＋为主要组分;各个离子的质量浓度均有季节及空间变化差异;不同粒径颗粒物中 SO2－4和 NO3－相关性均很好,NH4＋与 SO2－4、NO3－在细颗粒物中具有良好的相关性,Ca2＋在粗粒子中与 NO3－和 SO2－4的相关性也较好。SO2－4／NO3－质量比季节变化表明,春、夏季固定源与流动源对大气颗粒物贡献相当,秋季流动源贡献较大,冬季固定源贡献较大。PM2．5中SO2与SO2－4、NO2与 NO3－转化率表明,SO2－4、NO3－主要是由二次转化而来。     

乌鲁木齐市可吸入颗粒物水溶性离子特征及来源解析

采暖期时在乌鲁木齐市采集了环境空气中的可吸入颗粒物,对可吸入颗粒物质量浓度及8种水溶性离子的特征和来源进行了分析。结果表明,细粒子和粗粒子的月平均质量浓度分别是53.5～233.3μg/m3和38.9～60.9μg/m3;细粒子和粗粒子中水溶性离子主要由SO24-、NH4+和NO3-组成;粗粒子中NH4+与NO3-和SO24-的相关性分别是0.70和0.66,细粒子中NH4+与NO3-和SO24-的相关性分别是0.89和0.93,铵盐是乌鲁木齐可吸入颗粒物主要存在形式;煤烟尘是乌鲁木齐市采暖期可吸入颗粒物的主要来源。     

水中汞监测存在的问题与解决办法

利用中日合作 (JICA)项目资金 ,对测定地表水中汞存在的主要问题 ,如水样的保存和处理 ,水样的消解 ,测汞的冷原子吸收法和原子荧光法等进行了研究。通过对 33个环境监测站的样品考核 ,发现测定结果与标准值相比 ,偏高的数据达 75 %以上。提出了用 1%H2 SO4 和 0 1%K2 Cr2 O7保存水样最好 ;高锰酸钾 -过硫酸钾消解法适用于消解含有机物、悬浮物和组成复杂的废水样 ,高锰酸钾 -硫酸消解法适用于消解被有机物轻度污染的废水 ,溴酸钾 -溴化钾消解法适用于消解地表水和含较少有机物的生活污水及工业废水。研究表明 :尤以硫酸 -高锰酸钾 -过硫酸钾消解体系消解地表水和废水效果良好。对冷原子吸收法和原子荧光法中影响汞测定的因素 ,如空白值高、干扰物的消除、载气种类和流量、反应瓶体积和气液比以及反应时间等提出了详尽的解决方法     

大气痕量有机硫化物的光电离色谱法测定及硫酸铵在湿浸土壤中释放有机硫化物的研究

采用国产光电离色谱仪(GC-PID)对有机硫化物:乙基硫醇,二甲基硫,二甲基二硫进行了分离分析,其最小检知量在亚微克/升级,并对北京郊区的某些天然源环境样品进行了有机硫化物浓度的测定,实验数据证实,在鸡场,猪场,水稻田与塑料蔬菜大棚等环境大气中含有机硫化物。研究了硫酸铵作为氮肥加入到水浸土壤中后,由于缺氧而生成有机硫化物的现象,观察了其对有机硫化物的释放规律及硫酸铵与葡萄糖分别作为硫源与碳源对有机硫化物生成的影响,实验结果认为:硫酸铵在五种不同类型的水浸土壤中(环境温度25℃),均可解离释放出有机硫化物,随其在土壤中加入量的增多,释放气中的有机硫浓度增加,二甲基硫的释放量最大。     

高氯低COD值水样的无汞快速测定法

以硝酸银和硫酸铬钾代替硫酸汞来消除 COD 测定中的氯离子干扰,同时将重铬酸钾溶液的浓度降低为0.100 mol／L,并用硫磷混酸代替硫酸,该方法经过对标准样品和实际样品的测定,表现出对于测定氯离子含量低于25000 mg／L的高氯低 COD 值水样具有较好的准确度和精密度,同时可以实现银盐的回收再利用。     

土壤和底泥中砷、铬、锰测定的前处理技术

试验了土壤和底泥中砷的前处理技术,其目的是能对土壤、底泥中砷、铬、锰在一次前处理中制备成试液,比色法分析。试验表明,用Ｈ２ＳＯ４－Ｈ３ＰＯ４－Ｈ２Ｏ２进行前处理是可行的。方法简单、挥发酸雾少,用标准参考物质检验证明,分解完全,数据准确,有粒较好一致性。     

Investigation of arsenic speciation on drinking water treatment media utilizing automated sequential continuous flow extraction with IC-ICP-MS detection

Three treatment media, used for the removal of arsenic from drinking water, were sequentially extracted using 10 mM MgCl2(pH 8), 10 mM NaH2PO4(pH 7) followed by 10 mM (NH4)2C2O4(pH 3). The media were extracted using an on-line automated continuous extraction system which allowed the arsenic in each of the extraction fluids to be speciated on-line using IC-ICP-MS. The 10 mM MgCl2 preferentially extracted As(III) from each of the media. The percentage of the arsenic extracted by the MgCl2, relative to a HNO3/H2O2 digestion of the media, ranged from 0.1-2.3% for the three solids. The next sequential extraction fluid, 10 mM NaH2PO4, extracted some of the residual As(III) remaining on each of the media but the predominant species extracted was As(V). The 10 mM NaH2PO4 extracted 15.3 to 42.8% of the total arsenic relative to a total digested concentration for each of the media. The As(III) and As(V) stability studies conducted in these two extraction fluids indicated that conversion between As(III) and As(V) was not significant for the short extraction fluid sample contact time associated with the on-line continuous flow extraction cell. Finally, the 10 mM (NH4)2C2O4 extraction fluid was utilized in an off-line analysis mode because the Fe and As concentrations extracted from the media were not compatible with direct ICP-MS detection. The (NH4)2C2O4 extracted 2.9-29% As(III) for all three media and caused an oxidation of As(III) to As(V) during the extraction period for one of the three media. The sum of the arsenic from each of the three extraction fluids represented 92%, 44% and 53% of the available total arsenic for the three media, respectively. The speciation results for each media were obtained by adding all the speciation results from all three extraction fluids together and the resulting distribution of As(III)/As(V) compared well with the speciation results obtained via XANES.     

Altered Soil-soil Water Interactions Inferred from Stream Water Chemistry at an Artificially Acidified Watershed at Bear Brook Watershed, Maine USA

The Bear Brook Watershed in Maine, USA is the site of a paired watershed study. West Bear (WB) catchment is being artificially acidified with 1,800 eq ha-1 y-1 of (NH4)2SO4. East Bear (EB) serves as the control. After six years of artificial acidification, volume-weighted concentrations in WB, normalized to EB, increased approximately as follows, in eq L-1 : H+, 15; Al (umoles), 50; Al (eq L-1), 100; Ca. 50; Mg. 20; Na, 10; K, 2; SO4, 120; NH4, 2; NO3, 80; HCO3 has decreased 10 eq L-1. Based on changing chemistry, several inferences can be made about soil-soil water interactions.1. Various combinations of cation pairs in stream waters from both catchments are significantly correlated on an annual basis. The strongest linear correlations (r2 typically greater than 0.5), with positive slopes, occur for Mg versus Ca. These relationships suggest soil-soil water equilibria of the type:Ca+2 + Mg-X = Mg+2 + Ca-X; KCa-Mg = ([Mg+2]/[Ca+2])/([Mg-X]/[Ca-X]) or, with assumptions:K'Ca-Mg = [Mg+2]/[Ca+2]The value of K'Ca-Mg remains relatively constant through time in both watersheds, except in WB in and after the fourth year of the manipulation of WB. Thereafter there is preferential depletion (Mg>Ca>na>K), primarily along shallow flow paths - thus altering the solid activity ratios of the exchange surfaces. In EB, base cation concentrations decline with increasing discharge (increasing H+), due to dilution and interaction with soils with lower base saturation. In WB the acidification reverses this relationship, perhaps partly because of displacement of cations by NH4 from the amendments. With progressive depletion of Ca and Mg in the quick-flow paths, concentrations start to decline at higher discharge, in spite of lower pH.2. Sulfate concentrations increased in WB to as high as 230 eq L-1 at high flow. The percentage of added SO4 leached to the stream increased to approximately 65% by the end of 1995. Thus, soils along base-flow paths adsorbed about 35% of the added SO4 in 1995.3. Aluminum concentrations in WB have increased from a pre-manipulation maximum of 10 mole/L at high flow to 60 mole/L. The relationship between Al and H+ is:Al = 0.13(H+)2 + 4.35which could result from either desorption or dissolution of Al to a 2+ specie. This relationship has been relatively constant through the manipulation. The Al/Ca molar ratio increased from pre-manipulation values of 0.1 to 0.3 to 0.8, at higher flow.4. The minimum pH in WB, achieved at highest flow, has decreased from about 5.3 to <4.7, an increase of about 15 eq H+ L-1. The increase in H+ has been approximately 2 eq L-1 yr-1. Neutralization of acidity has been initially accommodated by mobilization of Ca>Mg>Al>Na>K>H; by 1995 the neutralization involves the release of Al>Ca>Mg>NaH>K. Thus, the soils are inferred to (1) have reduced base saturation, (2) preferential proportional loss of mg over Ca, (3) increased SO4 saturation, and (4) higher exchangeable acidity.     

Study on Size Distribution of Total Aerosol and Water-Soluble Ions During an Asian Dust Storm Event at Jeju Island, Korea

Soil dust particles transported from loess regions of the Asian continent, called Asian dust, highly influences the air quality of north-eastern Asia and the northern Pacific Ocean. In order to investigate the effects of these dust storms on the chemical composition of atmospheric aerosol particles with different size, measurements of size distributions of total aerosol and major ion species were carried out on Jeju Island, Korea during April 2001. Juju Island was chosen for the study because the levels of emissions of anthropogenic air pollutants are very low. A 5-stage cascade impactor was used to sample size-fractionated aerosol particles. Samples were analyzed for major water-soluble ions using Dionex DX-120 ion chromatograph. The average mass concentration of total aerosol was found to be 24.4 and 108.3 microg m(-3) for non-Asian dust and Asian dust periods, respectively. The total aerosol size distribution, measured during the non-Asian dust period, was bimodal, whereas the coarse particles dominated the size distribution of total aerosol during the Asian dust period. It was found that SO4(2-), NH4+ and K+ were mainly distributed in fine particles, while Cl-, NO3-, Na+, Mg2+ and Ca2+ were in coarse particles. Although SO4(2-) was mainly distributed in fine particles, during the Asian dust period, the concentrations in coarse particles were significantly increased. This indicates heterogeneous oxidation of SO2 on wet surfaces of basic soil dust particles. The NH4+ was found to exist as (NH4)2SO4 in fine particles, with a molar ratio of NH4+ to SO4(2-) of 2.37 and 1.52 for non-Asian dust and Asian dust periods, respectively. Taking into account the proximity of the sampling site to the sea, and the observed chloride depletion, coarse mode nitrate, during the non-Asian dust period, is assumed to originate from the reaction of nitric acid with sodium chloride on the surfaces of sea-salt particles although the chloride depletion was not shown to be large enough to prove this assumption. During the Asian dust period, however, chloride depletion was much smaller, indicating coarse nitrate particles were mainly produced by the reaction of nitric acid with surfaces of basic soil particles. Most chloride and sodium components were shown to originate from sea-salt particles. Asian dust aerosols, arriving at Jeju Island, contained considerable amounts of sea-salt particles as they passed over the Yellow Sea. Ca2+ was shown to be the most abundant species in Asian dust particles.