碱熔-离子色谱法同时测定玻璃中的氟和硫

玻璃样品中加入氢氧化钠,在700℃马弗炉中加热熔融,热水浸提,所得溶液通过OnGuardⅡAg/H柱后上机测定,消除加入的氯和碱的干扰,再经IonPac AG14柱和AS14柱分离,采用小体积的定量环直接进样,离子色谱法测定氟离子和硫酸根的含量。氟离子和硫酸根的线性范围分别为0.1～2μg/mL和0.5～20μg/mL,方法检出限氟为2.0 mg/kg和硫为1.0 mg/kg,测定结果的相对标准偏差(RSD)小于5.0%。实际玻璃样品用离子色谱法和化学法测定,两种分析方法的结果无显著性差异。     

离子色谱-电感耦合等离子体质谱法测定乳粉的汞形态

对于乳粉的汞形态分析,由于基质的复杂性,有机汞非常容易与样品中蛋白质上的巯基结合,形成稳定的络合物,在前处理过程中须保证各形态提取完全且各形态之间不会发生相互转化,因此样品前处理是汞形态分析的难点;同时乳粉中汞含量极低,对方法检出限提出了更高的要求。本文通过优化样品前处理过程,建立了离子色谱-电感耦合等离子体质谱测定乳粉中三种汞形态(二价汞、甲基汞、乙基汞)的方法。实验采用多种复合酶(蛋白酶、脂肪酶、淀粉酶)对乳粉基质中的蛋白、脂肪、淀粉进行解离,采用L-半胱氨酸-盐酸-甲醇的混合溶液作为提取剂进行超声提取,样品过RP固相萃取小柱去除杂质后用C18色谱柱(5μm,4.6 mm×150 mm)进行分离,流动相采用10 mmol/L乙酸铵-0.12%L-半胱氨酸-5%甲醇混合溶液进行淋洗,5 min内即可实现三种汞形态的基线分离。二价汞、甲基汞和乙基汞的加标回收率在79.9%~111.2%之间,检出限分别为0.5μg/kg、0.6μg/kg、0.9μg/kg。实际样品分析表明,汞总量很低的乳粉,汞各形态的提取率也能达到70%以上,能够满足检测要求。本方法在样品前处理过程中采用酶解的方式解离复杂基体中的汞形态,提高了提取率至80%以上;仪器分析方面采用甲醇作为增敏剂,提高了检测灵敏度,适用于乳粉样品中痕量汞形态的检测。     

太湖流域长兴县浅层地下水氮污染特征及影响因素研究

对太湖流域长兴县浅层地下水的氮污染进行了系统的调查与研究,共取地下水样43个并测定了其三氮含量.结果表明氨氮、硝酸盐和亚硝酸盐的超标率分别为13.95％、16.27％和16.27％.三氮污染最严重的地区主要为农业活动集中区,即夹浦镇、小浦镇、洪桥镇和虹星桥镇等,其中虹星桥镇硝酸盐污染最为严重,高达22mg/L.采用地质统计学方法对太湖流域长兴县43个浅层地下水样“三氮”含量进行了区域空间变异分析,结果表明长兴县地下水NO3-N和NO2-N浓度变异函数满足球状模型,而NH3-N浓度变异函数为高斯模型,硝酸盐氮、亚硝酸盐氮和氨氮浓度的空间自相关距离分别为9.98、1.51和3.82kmn.对硝酸盐污染因素进行了分析,结果表明:硝酸盐浓度与氮肥使用量呈明显正相关关系,年平均施肥量(以N计)为300kg/ha地区平均硝酸盐氮浓度达6.7mg/L,年平均施肥量(以N计)为100kg/ha地区平均硝酸盐氮浓度为2.2mg/L;地下水硝酸盐与地下水位埋深有直接关系,埋深较浅(1～3m)地区的硝酸盐浓度较高;当土地利用类型相同时,硝酸盐氮浓度与人口密度具有线性正相关关系.     

富硒土壤镉的赋存状态

采用7步提取法对某地富硒土壤样品进行镉的形态分析,发现镉质量分数较高,镉平均为0.374 mg/kg,最高为0.943 mg/kg。各形态含量差异较大,基本是残渣态离子交换态铁锰氧化物结合态腐殖酸结合态强有机结合态碳酸盐态水溶态,在7种形态中以残渣态、离子交换态、铁锰氧化物结合态3种形态占主导。     

凹凸棒石-双交联水凝胶微球钝化修复镉污染土壤研究

为研究凹凸棒石-双交联水凝胶微球(SA/PVA/ATP)对镉污染土壤钝化修复的效果,将SA/PVA/ATP添加到镉浓度为3.72 mg/kg的土壤中进行淹水培育,采用模拟酸雨、二乙烯三胺五乙酸(DTPA)和三乙醇胺(TEA)混合提取剂(DTPA提取剂)提取土壤有效态镉;采用欧共体标准局顺序提取方法(BCR)提取土壤中不同形态镉;讨论了SA/PVA/ATP添加量、土壤有效态镉和各形态镉的相关性;计算了钝化容量、修复效率和重金属风险评价指数,探究了SA/PVA/ATP对土壤镉的钝化机理。结果显示,随着SA/PVA/ATP的增加,DTPA提取剂和酸雨提取的有效态镉含量分别从1.72 mg/kg和0.024 mg/kg下降到0.66 mg/kg和0.004 4 mg/kg;土壤中的弱酸可提取态镉和可还原态镉含量分别从1.40 mg/kg和0.81 mg/kg下降到1.01 mg/kg和0.41 mg/kg,而可氧化态镉和残渣态镉含量分别从0.86 mg/kg和0.63 mg/kg增加到0.95 mg/kg和1.27 mg/kg。材料添加量与土壤中有效态镉、弱酸提取态镉和可还原态镉含量呈极显著负...     

多壁碳纳米管固相萃取快速检测水样中铅镉铜铁

传统的固相萃取填料应用于环境样品的重金属处理过程中,存在pH不稳定和不同极性萃取物共同萃取较为困难等方面的不足,因此寻找新型固相萃取填料显得尤为重要。本文采用多壁碳纳米管填充固相萃取柱,萃取水中金属元素铅、镉、铜和铁,采用石墨炉原子吸收光谱法测定铅和镉,电感耦合等离子体发射光谱法测定铜和铁。实验考察了多壁碳纳米管的性质、溶液pH值、洗脱溶液、样品流速以及基体效应对测定结果的影响。结果显示:溶液pH=9,1 mol/L硝酸为洗脱溶液,样品流速为2 mL/min时,外径8 nm未修饰的多壁碳纳米管有较好的萃取效率,对溶液中铅、镉、铜和铁的最大吸附容量分别为44.91、42.31、54.68和49.07 mg/g,四种元素的吸附容量均衡;钾、钠、钙、镁离子以及苯和甲苯等基质对四种金属元素的萃取影响不大。方法回收率为95.3%~99.5%,精密度(RSD,n=7)为1.2%~3.2%。本方法采用外径8 nm的多壁碳纳米管固相萃取,与传统萃取方法相比,富集效果好、回收率较高,而且操作简便、准确度高;与前人采用外径20~30 nm的多壁碳纳米管的性能相比,镉和铜的吸附容量更高,还可实现对铁的吸附,且铅、镉、铜和铁四种元素的吸附容量均衡,更适合用于检测水样中的金属元素。     

川东北地区水稻镉积累与生态健康风险评价

【研究目的】重金属镉主要通过“土壤-植物”系统进入食物链进而影响人体健康,开展农作物镉积累研究对保障人类健康安全具有重要意义。【研究方法】系统采集了四川省东北部南充市、巴中市、广安市等地的土壤及水稻样品,采用ICP-MS方法检测了土壤和水稻中的镉含量,并运用CART决策树和相关系数法进行了数据分析。【研究结果】结果显示,川东北地区表层土壤镉含量相对较低,为0.071~0.92 mg/kg,平均0.254 mg/kg,几乎所有（99.9%）样品镉含量都低于标准限值;水稻（糙米）镉含量差异性较大,为0.002~0.803 mg/kg,平均0.076 mg/kg,超标率达14.0%;水稻镉超标区成人每日通过稻谷摄入的镉达90.4 μg/d,已超过允许摄入量标准60 μg/d。【结论】土壤镉不超标而农作物镉超标的现象可能与土壤的低pH、低CaO、高SiO₂等特点有关,这一认识对于指导区域内粮食安全生产具有重要指导意义。创新点：土壤和水稻综合调查发现土壤镉不超标但农作物超标的现象,CART和相关系数法分析了其原因。     

抑制型离子色谱法同时测定水中锂和锶

对离子色谱法测定水中的锂、锶含量及其影响因素进行了研究。以甲烷磺酸为流动相，用IonPacCS12A阳离子色谱柱分离后，电导检测器同时测定矿泉水中锂和锶，其检出限分别为0．003mg／L和0．006mg／L。对Li^＋和Sr^2＋的离子色谱条件进行了优化，并对流动相的选择及干扰离子的影响进行了讨论。     

东海陆架泥质沉积物中固相Fe形态及其对有机质、Fe、S成岩路径的制约意义

利用化学提取法对中国东海具有不同陆源物质的内陆架(0701)和外陆架(0508)泥质沉积物柱样进行的多种形态固相铁含量及其剖面分布研究结果表明,Fe形态及其分布对有机质、Fe和S早期成岩作用具有明显的制约意义.0508和0701两站点柱状沉积物总活性Fe平均含量分别为12.14 mg/g和10.03 mg/g,其中,氧...     

利用原子荧光光谱-电感耦合等离子体质谱法研究济南市大气干湿沉降重金属含量及年沉降通量特征

大气降尘是地表土壤重金属元素的重要来源,研究大气降尘中重金属元素的地球化学特征并进行源解析对制定污染防控政策具有重要的指导作用。本文采用原子荧光光谱法、电感耦合等离子体质谱法、X射线荧光光谱法分析济南市大气干湿沉降中8种重金属(砷镉铬铜汞镍铅锌)含量特征;采用相关分析及主成分分析方法对大气干湿沉降重金属进行源解析。结果表明,大气干湿沉降物中镉铬铜汞镍铅锌平均含量分别为2.07 mg/kg、135.9 mg/kg、65.7 mg/kg、218.6μg/kg、110.7 mg/kg、380 mg/kg,显著高于土壤背景值,且富集程度高,明显受人为活动污染。镉铜汞铅主要来源于燃煤,砷铬来源于道路尘,镍来源于土壤,锌来源于交通尘;燃煤和道路尘对大气降尘的贡献率为50.13%,两者是济南市大气降尘污染的主要来源。大气干湿沉降对城区表层土壤中镉汞铬铅锌及砷的含量水平影响显著,其中锌年沉降通量最高(均值148 mg·m-2·a-1),汞年沉降通量最低(均值0.085 mg·m-2·a-1),且镉汞含量增长速率较高;大气干湿沉降对砷铬在土壤中的累积影响显著。     

高温燃烧水解-离子色谱法测定植物样品中的氟

建立了高温燃烧水解-离子色谱测定植物样品中不同含量范围氟的分析方法,色谱条件为Dionex IonPacAS18分离柱(4 mm×250 mm),Dionex IonPac AG18保护柱(4 mm×50 mm),ASRS ULTRAⅡ自动再生微膜抑制器,电导检测器。采用纯水作为吸收介质,使样品溶液与标准溶液基体一致,过滤后可直接测定。样品溶液中常见的Cl-、NO3-、SO24-、PO43-、CO23-、HCO3-等阴离子不干扰F-的测定。为消除样品热解过程中产生的乙酸干扰,对氟含量较高(xx～xxxμg/g)的样品,采用20 mmol/L的NaOH淋洗液等度淋洗,进样体积为25μL;对氟含量较低的样品(0.x～xμg/g),进样体积为100μL。方法具有较宽的线性范围和较好的稳定性,检出限为0.5 mg/kg,适用于痕量分析;应用于灌木枝叶和茶叶等4个氟含量较高(xx～xxxμg/g)的植物标准物质的测定,相对标准偏差(RSD)<6%(n=6);应用于低氟的小麦粉和大米粉样品测定,加标回收率为90%～110%,可以满足不同氟含量植物样品中氟测定的需要,具有自动化程度高、操作简单、对环境友好等特点。     

Accumulation of lead, cadmium, manganese, copper and zinc by sludge worms; Tubifex tubifex in sewage sludge

Tubifex tubifex has been shown to survive in organic polluted environments, however, not much has been done on its inorganic pollution tolerance. Samples of T. tubifex and their respective sewage sludge were taken from Soche wastewater treatment plant in Blantyre City, Malawi during July 2007 to November 2008. The total number of sludge samples taken was fifty one which was made into seventeen composite samples. A total of seventeen T. Tubifex samples were also collected. The samples were analyzed for copper, lead, manganese, zinc and cadmium using standard methods from American Public Health Association and Association of Official Analytical Chemists. The concentrations of metals in sewage sludge and T. tubifex were on dry weight basis and the metals determined were acid extractable. In general, heavy metals concentration was lower in T. tubifex than in sewage sludge. The range of heavy metals concentrations were (in sludge and (T. tubifex)): zinc 275.3–361.5 mg/kg (45.0–82.2 mg/kg), manganese 293.7–230.1 mg/kg (1.21–3.69 mg/kg), copper 86.5–120.1 mg/kg (1.6–4.7 mg/kg), lead 11.2–22.4 mg/kg (Below detection limit–0.95 ) and cadmium 1.12–2.31 mg/kg (1.08–2.18 mg/kg). The results showed significant differences between the concentrations of manganese, copper, lead and zinc in sewage sludge and T. tubifex (p < 0.05). However there was no significant difference between the concentrations of cadmium in sewage sludge and T. tubifex (p > 0.05). T. tubifex did not show the ability to accumulate heavy metals (attributed to its high defecation and metabolic rate) except for cadmium hence cannot be used as a bioindicator for heavy metal pollution in sludge.     

Synthesis of nano-γ-Al<Subscript>2</Subscript>O<Subscript>3</Subscript>/chitosan beads (AlCBs) and continuous heavy metals removal from liquid solution

In this work, synthesis of chitosan beads impregnated with nano-γ-Al₂O₃ (AlCB) was carried out. The characteristics of the synthesized adsorbent were obtained by using Brunauer Emmett and Teller technique and Scanning Electron Microscopy method. The use of AlCB in continuous removal of chromium, lead, nickel and cadmium ions from liquid solution was studied using fixed-bed column system. Bed depths and flow rate effects on breakthrough and uptake capacity of the adsorbent in column were also examined. Dynamic parameters of the adsorption were calculated by using bed depth service time (BDST) and Thomas models. In both models, the data were analyzed by error analyzing and combining the values of determined coefficient (R ²) from regression analysis. The adsorption capacities of AlCB in breakthrough were 158.33, 183.33, 63.33 and 31.67 mg/g for chromium, lead, nickel and cadmium, respectively. In addition, BDST model was found to be an acceptable kinetic model to describe the experimental data.     

Interactive effect of cadmium and zinc on chromium uptake in spinach grown in Vertisol of Central India

A pot culture experiment was conducted to study impact and interaction of multi-metals on growth, yield and metals uptake by spinach (variety All Green). Three levels of each chromium (0, 50 and 100 mg/kg), cadmium (0, 1 and 2 mg/kg) and zinc (0, 10 and 20 mg/kg) in combinations (total treatments 3 × 3 × 3 = 27) were applied in a Vertisol (5 kg). The results showed that increasing the concentration of chromium, cadmium and zinc in soil enhanced the respective metal concentrations in spinach root and shoot. When cadmium at 2 mg/kg along with chromium at 100 mg/kg soil was applied, chromium concentration and uptake were decreased in root and shoot. Meanwhile, zinc application had no significant effect on chromium uptake and concentration in spinach biomass. From the results, it was concluded that cadmium at higher dose had an antagonistic effect over chromium. On the other hand, in chromium, cadmium and zinc combinations particularly at their higher levels, a competition among each other was found. Therefore, the findings could be used as guidelines for controlling and management of heavy metals pollution in farmland.     

手持式消光光度计的研制及用于掺杂牛奶的现场快速检测

自行设计新型消光池,研制了一种廉价的手持式消光光度计,并在此基础上建立了掺杂牛奶的现场检测方法。实验结果表明,所建立的方法无需对牛奶进行复杂处理,可对常见掺杂(如搀水、米汤、奶粉、豆浆、尿素等)牛奶和含重金属离子汞的牛奶,进行现场检测。由于采用新型消光池,有效地减小了蛋白质粒子因重力沉降所带来的误差,能够成功区分同密度劣质牛奶。该方法灵敏度高,对掺水牛奶的检出限低于2%,对重金属(如汞)的检出限为0.005μg/g。单个样品测定时间不到2 min,适合于牛奶品质的现场快速检测。     

高效液相色谱-荧光检测同时测定污泥中7种氟喹诺酮类抗生素

为了监测污泥中氟喹诺酮类抗生素(FQs)的含量和水平,建立了基于固相萃取高效液相色谱荧光检测法测定污泥中7种FQs的分析方法。污泥样品选用乙腈∶磷酸盐缓冲液(1∶1,V∶V)(pH=3)提取,以亲水亲油平衡(hydrophilic-lipophilic balance, HLB)小柱净化富集,经甲醇洗脱、浓缩后用高效液相色谱荧光检测器(HPLC-FLD)检测,采用乙腈/0.1%的甲酸作为流动相并以外标法定量。FQs在0.005～1.0 mg/L浓度范围内呈现良好线性关系,R2为0.992 7～0.999 8。添加量为0.05、0.5和1.0 mg/kg时,污泥中7种氟喹诺酮类的加标回收率为78.3%～106.4%,其相对标准偏差为3.68%～12.06%(N=5)。方法的检出限为0.001～0.01 mg/kg,方法定量限为0.004 6～0.038 4 mg/kg。用该方法对北京地区3个污水处理厂活性污泥样品中7种FQs进行分析,检出浓度范围为未检出至1.09 mg/kg。     

The high contents of lead in soils of northern Kosovo

A soil-based geochemical survey was carried out in an area of about 350 km² in northern Kosovo around the Zve?an Pb-Zn smelter. The concentrations of As, Cd, Co, Cr, Cu, Ni, Pb, Sb, Tl, Th, U, Zn were determined in 452 topsoil and 82 subsoil samples. High contents of Pb, Cd, As, Sb, Zn and Cu were found in topsoil over a vast area including the Ibar and Sitnica river valleys. The highest concentrations were usually measured close to the Zve?an smelter. In some zones, the lead contents in surface soils exceeded 5000 mg/kg. Arsenic and antimony levels were usually more than 200 and 50 mg/kg, respectively, while cadmium contents were in the range 5-20 mg/kg. South of the Zve?an area, lead, antimony and cadmium pollution was strong in the densely populated urban area of Kosovska Mitrovica and along the agricultural alluvial plain of the Sitnica River. Depending on the chemical element, the pollution extended 15-22 km north and south of the Zve?an smelter. There was a progressive decrease of heavy element concentrations with increasing distance from the smelting plant. The contents of Pb, Zn, Cu, As, Cd, Sb significantly decreased with soil depth; in fact, the pollution only affected the upper 50 cm of soil. Crops were affected by soil pollution and many food-stuffs exceeded the EU standards. Suggestions for soil remediation are given.     

用离子色谱法测定金矿区水样中常规无机离子

利用DX－120离子色谱仪进行阴阳离子的精密度和准确度测定，100mg/L时相对标准偏差范围为1．00％－3．80％，回收经95．83％－105．00％；5mg／L时相对标准偏差范围为1．18％－4．57％，回收率92．40％－103．20％，完全达到实际要求。用该离子色谱仪测定甘肃阳山金矿山水样中常规无机离子，数据表明该区域水质较好，所测离子浓度都未超过饮用水标准。