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关于粉煤灰修复土壤重金属污染的研究


环境工程 吉红洁 S20120436 Study of Remediation of Soil Contamined with Heavy Metals by Coal Fly Ash
关于粉煤灰修复土壤重金属污染的研究
ABSTRACT 摘要 The labile fraction of heavy metals in soils is the most important for toxicity for plants. Thus it is crucial to reduce this fraction in contamined soils to decrease the negative effect of heavy metals. In an experiment, the effects of two additives on the labile fractions of Cu, Mn and Zn were investigated in a soil contamined during long-term application. The additive used was the coal fly ash. The treated soil was further enriched with heavy metals and allowed to age at room temperature for 30 days. After this period, they were extracted plant-available (EDTA; HNO3; CH3COOH) metal species. The addition of fly ash strongly reduced the plant-available of Mn for plants but to a lesser extent this applies to the plant-available of Cu and Zn for plants. By addition of 1% of fly ash as well as 2% of fly ash, the labile fraction of Cu, Mn and Zn were lowered by 6.3, 145.0 and 29.7 mg× kg–1, respectively. Moreover essential correlation between total Cu and Zn contents was stated in the soil with plant-available content of metals, with reference to both metals. Value of coefficients of correlation is attesting to it between the total and plant-available Cu and Zn contents which are respectively equal: R(Cu) = 0.845, R(Mn) = 0.864 and R(Zn) = 0.872 for p = 99.5%. The results suggested that leading into the soil of the additional amount of fly ash can be an effective way of chemical remediation with reference to soils contaminated by Cu or Mn or Zn. Because he causes immobilization of examined heavy metals in the soil and in the process in the arrangement a—soil is limiting the availability of these metals plant and more distant bonds of the food chain.
土壤中重金属的不稳定部分对植物来说是最重要的毒性。 因此在降低土壤重金属的负面影响方面,减少 污染土壤中的这部分是至关重要的。在同一个实验中,两种添加剂在铜、锰和锌的不稳定部分的影响应在土 壤污染中长期应用。使用的添加剂是粉煤灰。经过处理的土壤是进一步富含重金属并且室温下成熟30天。 经过该阶段,它们被提取植物可用(乙二胺四乙酸;硝酸;乙酸)金属物种。 粉煤灰的添加强烈降低了锰和锌的 植物可用性,但在较小程度上这也适用于铜和锌的植物可用性。通过添加1%的粉煤灰以及2%的粉煤灰,铜、 锰和锌的不稳定部分分别被降低了6.3,145.0和29.7毫克/公斤。而且土壤中铜和锌总含量的基本相关性被 规定,包括两种金属的植物可用性。相关性系数值证明它在植物可用铜和锌总含量平的:R(铜)=0.845, R(Mn)= 0.864和R(锌)= 0.872,p = 99.5%。结果表明,土壤中主要的额外数量的粉煤灰是一种化学修复 的有效途径,参照土壤污染的锰、铜或锌。因为他引起土壤重金属检测的固定化——限制了这些金属厂的可 用性和更远食物链的联合。

Keywords: Soil Remediation; Heavy Metals; Coal Fly Ash; FAAS
关键词:土壤修复;重金属;粉煤灰;火焰原子吸收光谱法

1. Introduction 引言 The main of the environmental problems in industrialized countries is the environmental impact, especially with heavy metals. Increased the concentration of heavy metals constitute a serious health threat of people and animals. Contamination with heavy metals can affect the whole environment, but the longest-lasting effects occur in the soils, on account of the

absorption of many metals on mineral and organic colloids. Metals, unlike other pollutants, remain in the atomic form, although their speciation can change in the time together with changes in the soil conditions [1].
在工业化国家主要的环境问题是环境影响,尤其是重金属。 重金属浓度的增加对构人类和动物的健康成 严重威胁。重金属污染会影响整个环境,但持续影响时间最长的是发生在土壤中,由于许多金属的吸收是矿 物和有机胶体。金属,与其它污染物不同,尽管他们的物种形成可以随着时间和土壤条件的改变而改变,但 它一直以原子形式存在[1]。

The long-lasting nature of contamination is dependent in the kind of the soil and its physicochemical properties. Removing heavy metals from the soil is a very difficult problem, because they are specific permanent pollution, which can in many causes data pack a few hundred or of even thousands of years [2]. It results from it the self purification processes are occurring in the soils very slowly [3]. Therefore, the contaminated soils should be recultivation, which in light of the applicable laws in Poland to lead to a reduction in the total content of pollutants in the soil to a state defined by standards of the quality of the soils and land [4].
污染物的自然持久性由土壤及其物理化学性质决定。 土壤中重金属的去除是个非常困难的问题,因为它 们是特定永久性污染,它可以在由许多原因造成,持续几百,甚至几千年[2]。它的产生与它自我净化过程 在土壤中非常缓慢[3]。 因此,被污染的土壤应当复植,该举措根据波兰适用法律减少土壤中污染物总量从而 达到土壤和土地定义标准质量[4]。

On the review of work of available methods remediation that the next technical methods remediation that the next technical methods (ex-situ extraction [5,6], and in-situ [7,8], electrochemical methods [9-12], the use of zeolites [13-15]), also offer promising prospects phytoremediation methods, especially phytoextraction, involving the removal of pollutants from the soil, together with about-ground biomass of crops [16]. It seems that the treatment is sufficiently effective immobilization of heavy metals in the soil, effectively limiting their negative impact on the environment [17]. The immobilization is one of the chemical methods remediation of soils contaminated with heavy metals, consisting of heavy metals in an inaccessible form for plants, so their presence in the food chain is much lower, thus reducing the negative health and environmental effects.
回顾工作中修复方法的可用性, 接下来的技术补救方法 (非原位提取[5,6],原位提取[7,8],电化学方 法(9 - 12),使用沸石[13 - 15]),还提供了广阔的前景,特别是植物修复方法,包括土壤污染物去除和有关 农作物物地面生物量[16]。该方法能充分有效固定土壤中重金属,有效地限制了他们对环境的负面影响 [17]。固化是一种修复重金属污染土壤的生物化学方法,包括植物不能吸收的重金属状态,这样他们在食物 链中的存在就低很多,从而减少对健康和环境的负面影响。

The availability of heavy metals to plants determined primarily by the pH of the soil, its granulometric composition and soil organic matter content [18]. It is well known that, the increased mobility of heavy metals is linked primarily to an excessive acidifications if soils. As a result, a significant acidification of soils, which increasing by anthropopressure, leading to accumulation in soils of excessive amounts of certain metal ions. This applies in particular metal ions such as Cu, Mn, Zn, which are necessary for the proper functioning of living organisms, but their excess a shortage, a threat to these organisms. The determination of availability of heavy metals for plants is the soil sorption capacity determined quality and quantity of soil colloids forming absorbent complex. The sorption properties of soils are closely related to their buffer capacity and resistance to chemical pollution.
植物对重金属的可用性首先取决于土壤的pH值、颗粒组成及土壤有机质含量[18]。众所周知,重金属流

动性的增加主要与土壤过度酸化有关。结果是,典型的土壤酸化,是由于人为压力增加,导致土壤中积累 的过量的某些金属离子。这同样适用于特定的金属离子,例如:铜、锰、锌,这些是生物体正常运作的必需, 无论过量或者缺乏,都会对生物造成威胁。植物对重金属可用性取决于土壤胶体质量和数量所决定的土壤 吸附能力,其中土壤胶体形成了复杂的吸附剂。

Based on the available literature, it appears that an effective way of contributing to the reduction of metal content in the available to plants forms is to improve the sorption of soils by providing a high content of organic matter while keeping of the high pH of soil. Above mentioned effect can be achieved through the use of various additives to the soil in the immobilization of heavy metals contained in the soil. These types of additives include for example lime [19,20], zeolites (both natural and artificially occurring in environment)[21,22], aluminosilicates and silicates [23,24]. An important supplementary source of organic matter in soil can also be brown coal and organic-mineral fertilizers from brown coal [25-27], phosphates and apatites [20,28,29] and iron and manganese oxide bearing materia[20,30]. Each of these additives has a different effect on bio-availability of the metals, micronutrient availability, soil solution pH and soil microstructure [20,21].Taking into account the content of organic matter and pH on the attention deserves also fly ash from coal combustion. Fly ash is the waste material of the composition of the dust. The positive impact of ash on the soil is due primarily by its chemical composition (low content of heavy metals, lack of radioactive element) [31]. The application of fly ashes from coal burning to the immobilization of heavy metals in relation to different types of soil and industrial wastes has been descibed in works [32-36].
基于现有文献,植物能够有效降低土壤重金属的方法是通过提高土壤有机物含量和PH值从而提高土壤 吸附能力。上述效应可以通过使用各种添加剂对土壤中重金属进行固化得到实现。这些类型的添加剂包括 例如石灰(19、20],沸石(包括环境中自然和人为的类型)(21、22),铝硅酸盐和硅酸盐(23、24)。土壤中有 机质的一个重要的补充源也可以是褐煤、褐煤中的有机和无机肥料(25 - 27],磷酸盐、磷灰石[20、28、29) 和铁锰氧化物材质 (20、30)。每种添加剂对重金属的植物有效性有着不同的影响,微量元素的可用性,土 壤溶液的pH值和土壤微结构(20、21)。考虑到值得关注的有机物质和pH值的关注值得也是煤燃烧产生飞灰。 粉煤灰是灰尘合成物的浪费材料。 土壤中灰分的积极影响主要源于其中的化学成分 (重金属含量低,放射性 元素少)[31]。煤燃烧产生的飞灰对不同类型土壤和工业废弃物中重金属固化的应用已在文章中进行描述 [32 36]。

On the light of the cited literature data it is reasonable to provide studied on the immobilization of selected heavy metals (Cu, Mn and Zn) using fly ash from coal combustion, whose purpose was to development of an effective, easily accessible and cheaper method of chemical remediation of comtamined soil of Cu, Mn and Zn. The scope done within of this study include: 1) determination of the total contents of Cu, Mn and Zn in examined soil; 2) implementation of the soil tests based on single extractions for detemination of the plant available contents of Cu, Mn and Zn; 3) study of effect of fly ash from caoal burning on the availability of Cu, Mn and Zn to plants; 4) examination of the possibility of using of fly ash as a chemical substance to support the chemical remediation of soils.
在引用文献数据时,可以有效提供粉煤灰对固定重金属(铜、锰和锌)的固化研究,旨在开发有效、简 单和经济的使用粉煤灰从煤燃烧,其目的是开发有效的、容易和便宜的铜、锰和锌重金属污染土壤的化学修 复方法。本研究范围包括:1)确定铜、锰和锌的总含量;2)基于单一植物提取实现土壤测试,决定铜、锰和 锌的植物可用性;3)研究粉煤灰对铜、锰和锌的植物有效性的影响;4)检测用粉煤灰作为一种化学物质来进 行土壤化学修复的可能性。

2. Experimental

实验

2.1. Apparatus

仪器设备

The flame atomic absorption spectrometer Perkin-Elmer 3100 Model (Shelton Instruments, CT USA) was used for Cu, Mn and Zn determination in the solutions. Measurements were performed at wavelength 324.8 nm (Cu), 279.5 nm (Mn) and 213.9 nm (Zn) using a yellow fuel-rich air-acetylene flame (acet ylene flow velocity 2.0 dm 3·min–1; air flow velocity 8.0 dm3·min–1) and burner height of 3 mm. The analytical lines were selected using a slit width 0.7 mm (Cu and Zn) and 0.2 mm (Mn) [37].Hollow cathode lamp at 10 mA (Cu and Zn), 20 mA (Mn) was used. The centrifuge tube-test Model WE 1 (Precision Engineering, Poland)—was used for the centrifugation of the soil extracts at the speed of rotary at appropriate 3000 rpm. The universal laboratory shaker Vibramax 100 Model (Heidolph Instruments, Germany) and a hot plate HP88720-26 Model (Barnstead/Thermolyne, USA) were used for the extraction. The pH of the extraction solutions was determined with a pH meter CPI-551 Model (Elmetron, Poland) supplied with a glass combination electrode.

火焰原子吸收光谱仪,Perkin-Elmer公司3100型号(谢尔顿仪器,CT USA) ,用于铜、 3 锰和锌的测定。使用黄色的富燃空气 - 乙炔火焰(乙酰二甲苯流速为2.0 dm ·min–1,空气 流速为8.0 dm3·min–1 )进行波长为324.8纳米(铜) ,279.5纳米(百万) ,213.9纳米(锌) 的测量,其燃烧器高度为3毫米。分析线选择使用的是狭缝宽度0.7毫米(铜和锌)和0.2毫 米(Mn)[37]。空心阴极灯分别使用10 mA(铜和锌)和20毫安(Mn)的。 离心管实验模 型WE1(精密工程,波兰)用于土壤在每分钟3000转的速度下进行离心分离。提取使用通 用实验室摇床Vibramax100型号(德国Heidolph仪器公司)和电热板HP88720-26型号 (Barnstead/ Thermolyne, 美国) 萃取液的pH值用玻璃复合电极的pH计CPI-551模型 。 (波 兰Elmetron)测定。
2.2. Reagents and Solutions 试剂和溶液制备 All chemicals and reagents were of analytical grade or higher purity and were obtained from POCH, Gliwice, Poland. The solutions were prepared by dissolving the appropriate compounds in double-distilled water from the Water Purification System (Rel-5 Model, MERAPOLNA, Poland). The reagents were prepared and stored in clean polyethylene bottles. Glassware and plasticware (PE) used throughout the experimental work were previously soaked in 10% nitric acid bath overnight and washed thoroughly in double distilled water.

所有的化学品和试剂从波兰格利维采博兹获得, 均为分析等级或更高纯度。 溶液是通过 在自来水净化系统(波兰,MERAPOLNA REL-5的型号)双蒸水溶解适量的化合物制得。 试剂在干净的聚乙烯瓶中制备和贮存。 在整个实验工作中使用的玻璃器皿和塑料制品(PE) 均在10%的硝酸浴中浸泡过夜,并用双蒸水充分洗涤。
Standard solutions were prepared from standard solutions for atomic absorption (Sigma-Aldrich Chemie GmbH, Switzerland)—Cu concentration 1.000 ?g·cm –3 in 1% of HNO3, Mn concentration 1.000 ?g·cm–3 in 1% of HNO3 and Zn concentration 1.000 ?g·cm–3 in 1% of HNO3。 Working standard solutions containing Cu, Mn and Zn were prepared by serial dilution of the appropriately of standard solution for atomic absorption.

标准溶液由原子吸收标准溶液(Sigma-Aldrich公司的化学公司,瑞士)——在1%的硝 酸中铜浓度为1.000?g·cm–3, 锰浓度为1.000?g·cm–3和锌浓度?g·cm–3制得, 工作标准溶液含 有铜、锰和锌,通过适当连续稀释原子吸收溶液获得。 2.3. Sample Collection and Preparation 样本收集和准备 Coal fly ash samples used for the experiments were collected from the electric filter from Rzeszów S. A powerplant (Rzeszów, Poland). The 0.5 kg sample was prepared

from overall air-dried 10kg sample by a ―quarterning‖ method—according to BN-81/0623-01 procedure [38]. After that, the air-dried ash was sieved, initially through a laboratory sieve of 1 mm diameter, and then milled in an agate mortar to fine powder ( φ ≤ 100 μ m)—according to PN-77/G-04528/00 [39]. 实验使用的粉煤灰样品均采自热舒夫 S. A 发电厂(波兰热舒夫) 。每 0.5 公斤样品是根 据 BN-81/0623-01 程序通过“quarterning”方法将 10 公斤样品风干获得 [38]。在这之后, 空气干燥灰过筛,首先通过实验室直径为 1 毫米的筛子,然后在玛瑙研钵中研磨为细粉状 (φ≤100μm)——根据 PN-77/G-04528/00[39]。 The surface soil samples (depth: 0 - 15 cm) were collected from the area of the permanent grassland from the field of 0.2 ha (the area of the University of Technology, Rzeszów, Poland) according to PN-R-04031 procedure [40]. The sample preparation was performed according to Namie?nik et al. [41]. The laboratory sample of the weight of about 0.5 kg was prepared by the ―quarter‖ method from the general sample that weighted about 10.0 kg, after getting it previously into the air-dried state in the laboratory conditions. The air-dried soil was sieved through a laboratory sieve with apertures of 1 mm and it was milled in an agate mortar to fine powder (?< 100 μ m). 表层土壤样品 (深度: - 15 厘米) 0 根据 PN-R-04031 的过程从 0.2 公顷的永久草地 (波 兰热舒夫,科技大学)区域采集[40]。样品制备根据 Namie?nik 等[41]。每 0.5 公斤实验 样品是通过“quartern”方法是通过约 10.0 公斤普通样本在实验条件下风干后获得。将空气 风干的土壤通过实验室 1 毫米的孔筛过筛,并在玛瑙研钵研磨细粉(?<100μm) 。 2.4. Procedures 步骤 2.4.1. Total Metal Determination 总金属量测定 Fly ash samples were digested in open PTFE? vessels. 1.00 g of ash was digested with and mixture of 8 cm3 65% HNO3, 4 cm3 40% HF, 2 cm3 37% HCl and 10 cm3 H2O. After evaporating of liquids in a hot plane (T = 96? C), the solution was replenished with water to 50 cm3, and Cu, Mn and Zn was determined by the Flame Atomic Absorption Spectrometer (FAAS). The analysis of the total content of manganese in soil samples with concentrated HF and HClO4 acids was described in the work [42]. In the some way the analysis of the total content of Cu and Zn was performed in the examined soil. All samples were prepared in triplicates. 粉煤灰样品开口的聚四氯乙烯容器中进行吸收。每 1.00 克粉煤灰与 8 cm3 的 65% HNO3,4 cm340%HF,2 毫升 37%的盐酸和 10 cm3 H2O 混合进行稀释。溶液在电热板 (T=96?C)蒸发后,向标准溶液中补充 50 cm3 水,铜、锰和锌含量通过火焰原子吸收光 谱仪(FAAS)进行测定。土壤样品中关于锰和浓氢氟酸与高氯酸总含量的分析在本文中已 有描述 [42]。在一些方法中,Cu 和 Zn 总含量的分析在检测土壤中进行。所有样品制备均 为一式三份。 2.4.2. Determination of Plant Available Content of Metal 植物可利用的金属含量的测定 The determination of plant available content of cooper, manganese and zinc made the experience on which to test samples of soil were added specified volume of one of the following solutions: 0.05 mol· –3 EDTA, 2.5% HOAc and 1 mol· –3 HNO3. The dm dm analytical procedure was identical in relation to all extraction solutions; weighed at 5.000 (± 0.001) g of tested soil samples, they were quantitatively transferred to bottles of PE and were added to 10 cm3 of one of the above solution, then were shaken on a laboratory shaker for about 2h. After this time the samples were filtered and/or centrifuged and

completed of redistilled water in volumetric flask to volume 50 cm 3. In the obtained solutions were determined the content of Cu, Mn and Zn by FAAS method. In parallel with tested samples were prepared reagent blank (without soil) by entering the same quantities of reagents and by following the same steps as in the preparation of samples tested. 土壤样品中铜、 锰和锌的植物可利用性含量测试土分别加入以下规定量, 解决方案如下: –3 –3 0.05 mol· dm EDTA,2.5%乙酸和 1 mol· dm 硝酸。就所有萃取液分析方法是相同的,称 重 5.000(± 0.001)克土壤样品测试,将他们定量地转移到 PE 瓶,并加入到 10 cm3 的上 述溶液,然后在实验室摇床震荡约 2h。此后过滤和/或离心分离,加入重蒸水至 50cm3。将 所得到的溶液用火焰原子吸收光谱法进行测定其中的 Cu,Mn 和 Zn 的含量。平行测试样品 制备试剂空白(不含土) ,测试样品按照相同的步骤操作。 2.4.3. Study of Effect of Fly Ash from Caoal Burning on the Availability of Cu, Mn and Zn to Plants 粉煤灰对 Cu, Mn 和 Zn 的植物可利用性影响的研究 In order to determine the effect of fly ash on the availability of cooper, manganese and zinc for the plant performed an experiment in which to tested soil was added fly ash in an amount of 10% or 20% of the sample (which represents an increase of organic carbon in the tested soil respectively 1% or 2%). In parallel with tested samples were prepared reagent blank (without fly ash) by entering the same quantities of reagents and performing the same steps as in the preparation of samples tested. The prepared samples were left to dry (to the air-dry state) for about a week. After this time the samples were transferred quantitatively with 10 cm3 of 0.05 mol· –3 EDTA into a bottles of PE, and shaken on a dm laboratory shaker for 2 h. After this time the samples were filtered and/or centrifuged and completed to the mark of redistilled water in volumetric flask with a capacity of 50 cm3. In the obtained solutions were determined the content of Cu, Mn and Zn by FAAS method. 为了确定粉煤灰对铜、锰和锌的植物可利用性的影响,因此进行了一个实验,测试土壤 中加入 10%或 20%的粉煤灰样品(即土壤中有机碳增加 1%或 2%) 。平行试验在空白制备 溶液(无粉煤灰)加入相同量的试剂,并进行相同步骤的操作。样品需要一个星期左右(达 到风干状态) 。此后将样品定量转移到 PE 瓶,并与 10 cm3 的 0.05 mol· –3 EDTA 混合, dm 在实验室摇动器上振摇 2 小时。然后将样品过滤和/或离心分离,加入重蒸水至 50cm3。将 所获得的溶液利用火焰原子吸收光谱法进行 Cu,Mn 和 Zn 含量测定。 2.4.4. Examination of the Possibility of Reducing the Availability of Metals to Plants under the Influence of Fly Ash 粉煤灰影响下植物可利用性降低金属含量的可能性 In order to identify opportunities to reduce the availability of cooper, manganese and zinc for plants under the influence of fly ash made the experiment, which comprised following steps: 为了测定粉煤灰影响下植物可利用性对降低铜、锰和锌含量的可能性,做了如下实验, 包括如下步骤: STAGE I—Preparation of working solutions of Cu, Mn and Zn 铜,锰和锌的实验溶液 制备 The following solutions were prepared: CuCl2 (10, 25, 50, 100, 300 mg· –1); MnCl2 kg –1 (300, 500, 1000, 1500, 3000 mg· ) and ZnCl2 (50, 100, 150, 300, 1500 mg· –1).The kg kg concentration of metals in this solutions are within in the limits of the content of soils polluted by industry and represent the highest doses similar to the permissible levels of these metals I soils. 制备溶液如下:氯化铜(10,25,50,100,300 mg· –1) kg ;氯化锰(300,500,1000,

1500,3000 mg· –1)和氯化锌(50,100,150,300,1500 mg· –1) kg kg 。溶液中的金属 浓度受到工业污染土壤成分的限制,并代表类似 I 类土壤中这些金属的最高剂量。 STAGE II—Analytical procedure 分析过程 The experiment was performed for three series of test samples, which contained the test soil brought into the dry air state in the laboratory conditions with the addition of fly ash (ash content 20% by mass of the sample): 试验样品包括测试土壤和另外加入的粉煤灰, 并在实验条件下风干 (样品中灰分质量含 量 20%) ,分为三个系列: Serie 1—Convicted of solutions, which contained Cu at the concentrations respect ively: 10, 25, 50, 100, 300 mg· –1; kg Serie 2—Convicted of solutions, which contained Mn in concentration as following: 300, 500, 1000, 1500, 3000 mg· –1; kg Serie 3—Convicted of solutions containing Zn at the concentrations respectively: 50, 100, 150, 300, 1500 mg· –1. kg 系列 1——溶液中铜浓度分别为:10, 25, 50, 100, 300 mg· –1; kg 系列 2——溶液中锰浓度分别为:300, 500, 1000, 1500, 3000 mg· –1; kg 系列 3——溶液中锌浓度分别为:50, 100, 150, 300, 1500 mg· –1. kg Series of tested samples were convicted for a period of four months with the solutions containing these metals in the mentioned above concentrations. After this time the tested samples were stabilized for about two weeks, moistening every two days with distilled water. Then left them to dry at room temperature in the laboratory conditions. After drying and homogenization the samples were griding in mortar (porcelain and agate), and then the samples were weighed after three representative samples, each of 5.000 ( ±0.001) g within each series prepared. For each samples were added to 10 cm 3 of EDTA at a concentrations 0.05 mol· –3 into the bottles of PE, and were shaken on the laboratory dm shaker for 2 h. Then the samples were filtered and/or centrifuged, and completed to the mark in a volumetric flask with a capacity of 50 cm 3. In the obtained solutions were performed to determine the content of Cu, Mn and Zn by FAAS method. In parallel with the series of tested samples were prepared a control samples (without ash), introducing the same quantities of reagents and performing the same steps as in the preparation of tested samples. 测试样品系列配置成上述标准溶液需为期四个月,然后测试样品需要稳定大约两个星 期,每两天用蒸馏水润湿。然后将它们在实验室条件下室温干燥。在干燥和均质化后,样品 在研钵中进行破碎(瓷器和玛瑙) ,然后称重为 3 个有代表性的样品,每个系列制备 5.000 (?0.001)克。在 PE 瓶中每个样品中加入 10 cm3 的浓度为 0.05 mol· –3EDTA,然后在 dm 实验室振荡器上振摇 2 小时。接着对样品进行过滤和/或离心分离,并完成在容量瓶中至 50 cm3 的容量刻度。用火焰原子吸收光谱法在所获得的溶液中进行铜、锰和锌含量的测定。平 行地进行一系列测试制备控制样品(无灰) ,加入相同量的试剂,并进行相同步骤的操作。 The research was taken at the same time for six samples with simultaneously three-times repeated metal detection in each sample. Results presented are the mean of three replicates, passed the test for normality and were statistically analyzed by AN OVA test (p = 0.05). The statistical estimation of the results of analysis of metal content in soil, fly ash and soil with fly ash addition were carried out on the basis of a Student’s t-test (p = 95%). Statistical analysis were made using the STATISTICA 7.1.programme.

该研究是采取在同一时间对 6 个样品同时重复 3 次的金属检测。呈现的结果是三次的 平均值,通过正常测试,并进行统计学分析(P = 0.05)OVA 测试。土壤中重金属、粉煤灰 和加入粉煤灰的土壤的分析结果统计学评估,是基于一个 Student 的 t-test (p = 95%)实现 的。统计分析使用的是 STATISTICA7.1.程序。 3. Results and Discussion 结果与讨论 3.1. Fly Ash Composition 粉煤灰成分 The results of the quantitative chemical analysis of the fly ash samples used are shown in Table 1. The results obtained (Table 1) suggest that in the studied ash the following oxides occur: SiO2—42.9%; Al2O3—20.8%; Fe2O3—6.3%; CaO—4.3%; MgO—3.5% (in calculation to the initial state). The content determined of major components (mentioned above), contained in the ash shows that the investigated fly ash can qualify as silicate ash, in which the content of major components averages respectively: SiO2(40% - 58%), Al2O3 (15% - 25%), Fe2O3(5% - 15%), CaO (2% - 10%), MgO (1% - 5%) [43]. The content of other elements did not exceed 6% to the initial mass of ash. 粉煤灰样品定量化学分析的结果如表 1。所得结果(表 1)表明,在所研究的粉煤灰中 有如下氧化物:SiO2—42.9%; Al2O3—20.8%; Fe2O3—6.3%; CaO—4.3%; MgO—3.5% (初 始状态的计算) 。粉煤灰主要成分(上面提到)含量表明,所研究的飞灰可以作为硅酸盐灰 后者的主要成分平均含量分别为:SiO2(40% - 58%), Al2O3 (15% - 25%), Fe2O3(5% - 15%), CaO (2% - 10%), MgO (1% - 5%) [43]。其他元素的含量不超过初始灰质量的 6%。

3.2. Soil Composition

土壤成分

The main physical and chemical properties of the soil are shown in Table 2. Some general comments can be made about these characteristics of the soil samples. Based on the results obtained, it may be stated that the examined soil (on account of value measured with the pH in KCl solution) could be included into neutral soils, of which the pH in KCl solution ranges from 6.6 - 7.2. The pH value is a determining factor on the mobility of trace metals in soil. In neutral soils, taking heavy metals by plants is in general smaller in comparison to strongly sour soils. The carbonate levels in the examined soil are low. The results obtained confirm the fact that in layers of surface soils the low carbonate levels account for the slightly alkaline or neutral character of the soil. The content of available forms of phosphorus, potassium and magnesium in the examined soil amounts respectively: 15.1 mg P2O 5/100 g; 13.3 mg K2O/100 g and 7.3 mg Mg/100 g of dry mass of soil. 土壤的主要物理和化学性质见于表 2。关于土壤样品的这些特征,可以做一些一般的评 价。基于所得结果,可以说,测试土壤(由于测量值与 KCl 溶液的 pH 值)可以被包括到中 性土壤,其中 KCl 溶液中的 pH 值的范围是 6.6 - 7.2。pH 值是土壤中微量金属元素移动的 一个决定性因素。与强酸性土壤相比,在中性土壤中植物对重金属的吸收性一般较小。检测 土壤中的碳酸盐含量都很低。 所得结果证实了一个事实, 即在表层土壤层的碳酸盐含量低是

由于的弱碱性或中性特点。检测土壤中可利用形式的磷,钾和镁的含量分别为:每 100g 风 干土壤中 15.1 mg P2O 5; 13.3 mg K2O 和 7.3 mg Mg。 The investigated soil showed the granulometric compositions containing 62.5% clay fraction and 20.7% silt fraction. The fraction of sand is the smallest and it amounts to 16.8%. 土壤调查表明:粒度组成,包括 62.5%的粘土和 20.7%粉粒。砂所占的百分数是最小 的,大约有 16.8%。
3.3. Total Content of Metal 金属总含量

Cooper is usually the strongly binding to surface level of soil and she does not migrate into the soil profile. However, due to the relatively high rate of bioaccumulation and high degree of anthropogenic its launch it is a risk of contamination if the local biological environment [18]. The content of Cu in the tested soil was equal to 39.9 mg· –1dry mass of soil (Table 3). In the soils of the world the content of cooper falls kg between 1 to 140 mg· –1; in Poland, the average of its content in soil is 6.5 mg· –1. kg kg –1 However often assumed permissible limit of Cu in soils is 100 mg· [18]. The obtained kg results show that the mean content of Cu in the tested soil slightly deviates from the average for the Cu concentration in Polish soils, which may be related to the emission of dust particulate matter contains metals from industrial plants operating in the area where samples were collected. 铜通常是土壤表面的强烈约束力,它不会迁移到土壤剖面。然而,由于高生物蓄积性和 高程度人为排放率,对于当地生态环境来说这是一个风险的污染 [18]。检测土壤中 Cu 的含 量是 39.9 mg· –1,相当于土壤的风干质量(表 3) kg 。世界土壤中铜的含量介于 1 至 140 –1 mg· ;在波兰,在土壤中其含量的平均值是 6.5 mg· –1。但是通常假定在土壤中 Cu 的 kg kg –1 允许极限值为 100 mg· kg [18]。所得结果表明,检测土壤中 Cu 含量稍微偏离于波兰土壤 中 Cu 的平均浓度,这可能与样品采集地区工业工厂操作过程中粉尘颗粒物排放问题有关。 Zinc is one of the mobility of metals in the soil , its accumulation in the surface levels of mineral and organic soil depends on the amount of organic matter, which creates a very stable bond with the metal. The higher plants usually take this element in proportion to its concentration in the soil, hence the bioavailability of Zn and the related risk of going into the food chain is significant because of the high solubility of compounds in which the element occurs. The concentration of Zn in the soil stood the test of 126.7 - 275.8 mg· –1 kg –1 dry mass of soil, with an average of 205.9 mg· kg dry mass of soil (Table 3). The content of Zn in soils on the world falls in the range of 150 to 400 mg· –1; in Poland, the average kg –1 content in soil of this element is 40 mg· kg [18]. The received, significantly increased the content of Zn in the studied soil may be due to the fast that zinc introduced into the soil as a result of agricultural or horticultural production is subject to the accumulation of surface soil levels. 锌是土壤中一种迁移性的金属, 其在矿物和有机土壤的积累依赖于有机物质的量, 有机 物与金属建立了非常稳定的键。 高等植物吸收的元素量通常与其在土壤中的浓度成正比, 由 于 Zn 的化合物溶解度高,因此 Zn 的生物利用度,以及其进入食物链相关的风险是值得注 意的。土壤中锌的极限浓度是:干土中 126.7 - 275.8 mg· –1,平均浓度为 205.9 mg· –1 kg kg –1 (见表 3) 。世界土壤中 Zn 含量的范围是 150?400 mg· ;在波兰,该元素在土壤中的平 kg –1 均含量为 mg· kg [18]。 在所研究的土壤中 Zn 的含量显着增加, 可能是由于 Zn 作为生产农 用或园艺用的引入,从而导致土壤表层含量增加。

The contamination of the soils manganese is associated with his form, rather than the quantity [44]. The content of Mn in soils of the world and Polish, depending on the type and nature of the soil, and it is located in the range from100 to 1300 mg· –1[18]. In the kg –1 analyzed soil the content of Mn fitted in range 283.8 - 413.1 mg· kg dry mass of soil, with –1 an average of 347.9 mg· dry mass of soil (Table 3). kg 土壤中锰的污由于形式,而不是数量[44]。世界和波兰土壤中的锰,取决于土壤的类型 和性质,它在土壤中的含量从 100 至 1300 mg· –1 [18]。在所分析的土壤中 Mn 的含量范 kg –1 围是:干土中 283.8 - 413.1 mg· ,平均含量是 347.9 mg· –1(表 3) kg kg 。

Among the studied heavy metals in the tested soil, it were found that showed the greatest variation in zinc content, and then manganese and cooper. 在所研究土壤中的重金属,据监测发现,锌的含量的变化最大,其次锰和铜。 3.4. Plant Available Content of Metal 金属的植物可利用性 To the extraction of available forms of metal in soil used the weak extraction solutions; for example solutions of salt or weak acids, which are extracted from the soil the elements in small quantities, often only found in the soil solution. It is that is a good choice for assessing the forms available for plants to use intermediate solutions, which are extracted in addition to the forms present in the soil solution, including those that are potentially available to plants when soil conditions change. For this type of substances included in mineral acids (HCl, HNO3), solutions of neutral salt or weak organic acids (NH 4OAc, CaCl2, HOAc) and chelate compounds (EDTA, DTPA). 土壤中重金属的植物可利用形式的提取采用的是低浓度提取溶液,例如盐溶液或弱酸, 它们是从土壤中提取出来的微量元素,通常只能在土壤溶液中发现。 它是使用中间溶液评 估植物可利用形式的较好选择, 该中间溶液是提取的除了土壤溶液中存在的形式, 包括那些 当土壤条件发生变化潜在具有植物可用性的形式。对于这种类型的物质包括无机酸(盐酸, 硝酸) 、中性盐或弱有机酸(醋酸铵,氯化钙,醋酸)和螯合物(EDTA,DTPA) 。 The effects of extraction conditions on the result of determination of plant are available for Cu, Mn and Zn in the soil. The soil was subjected to extraction using three extraction solutions (0.05 mol· –3 EDTA, 1 mol· –3 HNO3, 2.5% HOAc); the results dm dm shown in Table 4. On the basis of obtained results were the effectiveness of the extraction specified, taking as a criterion the maximum amount of the metal extracted. It was found that the greatest amount of copper was extracted using 0.05 mol· –3 EDTA. By contrast, dm –3 the zinc most efficient extraction solvent was a 1 mol· dm HNO3. The content of Zn –3 available to plants obtained by using 0.05 mol· dm EDTA was similar to values obtained using 1 mol· –3 HNO3. For this reason in the course in further research to extraction of dm the content of Zn and Cu available to plants was 0.05 mol· –3 EDTA solution used. The dm same is the case with regard to the Mn content in the forms available to plants. The content of studied metals in the forms available to plants in telation to their total content

depending on the type of extraction solutions used were showed on the Figures 1 - 3 . It should be emphasized high extraction efficiency of all tested metals, both highly active substances (HNO3) as well as solutions of chelating salts (EDTA) and using a relatively low extraction solution that a weak acid (HOAc). The effectiveness of the extraction solutions used decreases in the following series: for Cu EDTA > HNO3 > CH3COOH for Zn HNO3 > EDTA > CH3COOH for Mn HNO3 > EDTA > CH3COOH 提取条件对测定结果的影响是植物对土壤中铜、 锰和锌可利用性。 使用三种萃取液 (0.05 –3 –3 –3 mol· dm EDTA,1 mol· dm 硝酸,mol· dm 乙酸)对土壤进行提取,结果见表 4。在所得 结果的基础上,指定提取的有效性,作为金属提取最大限度的标准。结果表明,使用 0.05 mol· –3 的 EDTA 对铜的萃取量组大,与此相反,锌的最有效的萃取溶剂是 1 mol· –3 硝 dm dm –3 –3 酸。使用 1 mol· dm 硝酸得到的值与使用 0.05 mol· dm EDTA 得到的值相似。基于这个 原因,在进一步研究 Zn 和 Cu 含量的过程中使用的是 0.05 mol· –3 的 EDTA 溶液。相同 dm 情况下研究植物可利用形式下 Mn 的含量。 所研究金属在植物可利用形式下的含量与它们的 总含量有关,取决于提取荣与辱的类型,如图 1-3 所示。应该强调的是所测近视高的提取效 率,无论是高活性的物质(HNO3)以及螯合盐(乙二胺四乙酸) ,还是使用相对较低的提 取液是一种弱酸(醋酸) 。使用提取溶液的有效性如下所示: Cu EDTA > HNO3 > CH3COOH Zn HNO3 > EDTA > CH3COOH Mn HNO3 > EDTA > CH3COOH

In conclusion, among the test solutions the most important role is played by extraction of EDTA, the undoubted advantage is that it is a good test for heavy metals extraction solvent, without destroying the mechanical structure in the soil and has relatively little effect on its biological activity. Moreover, based on available literature it is known that he has a very good correlation between the metal content in plants and extractable fraction [45-47]. The indicated concentration of Cu, Mn and Zn within the scope of normal levels of these elements in plants and not exceed the phytotoxicity range for plants according to Kabata-Pendias [18] (Table 4). The interpretation of the obtained results in studied on plant available forms of cooper, manganese and zinc is difficult because the content of these forms, only inform us about the possibility of download these elements by plants at the time of the analysis. Just change the total content of these metals in the soil that the bioavailability of this has completely changed. In addition, the content of the analyzed elements in the forms available to plants is highly dependent on the physicochemical properties of tested soil, mainly from its pH, granulometric composition and on the abundance of soil in humus. 总之,测试溶液中,起最重要的作用的是 EDTA 萃取,其毫无疑问的优势是:在不破 坏土壤机械结构和不影响其生物活性的条件下, 它是一个很好的重金属的萃取溶剂测试。 此 外,根据现有的文献,众所周知,植物中金属含量与萃取物之间有很好的相关性[45?47]。 Cu,Mn 和 Zn 的指示浓度,其在正常范围之内,而且不超过 Kabata-Pendias 指定的植物 毒性范围[18](表 4) 。对于 Cu,Mn 和 Zn 的植物可利用形式的研究结果的相关解释是困难 的,因为这些形式的含量,在分析的时候只告知了我们植物减少这些元素的可能性。只要改 变土壤中这些金属的总含量,那么它们的生物利用性也将完全改变。此外,所分析的元素在 植物可利用形式下的含量也是高度依赖于测试土壤的物理化学性质,主要是 pH 值、粒度成 分和土壤腐殖质的丰度。 Taking into account the results of statistical analysis, found a significant correlation between the total content of Cu, Mn and Zn in soil and the plant available content of this metals. Testify to the value of the correlation coefficients between total and available to plants content of Cu, Mn and Zn, which were respectively equal to: R(Cu) = 0,845, R(Mn) = 0.864 i R(Zn) = 0,872 dla p = 0.05.There was not significant relationship between the content of Cu, Mn and Zn in the forms available to plants and the pH values or physico-chemical parameters of the tested soil. This should be attributed to too small sample subjected to statistical analysis within which the distribution of property different from the normal distribution. 考虑到统计分析的结果,发现土壤中 Cu、Mn 和 Zn 的总含量与植物可利用含量有很大 的相关性。Cu、Mn 和 Zn 的总含量与植物可利用含量见的相关系数值分别等于:R(铜) =0845,R(锰)=0.864 I, R(锌)=0872, DLA p=0.05. Cu、Mn 和 Zn 在植物可利用 形势下的含量与被测土壤的 pH 值,或土壤的物理化学参数偶很大的关联。这应归功于太多 小样本进行的统计分析,在该分析中特性分布不同正态分布。 3.5. Study of the Impact of Fly Ash on the Availability of Metals to Plants 粉煤 灰对金属植物可利用性影响的研究 The important source of organic matter in soil may be fly ashes from coal combustion. Their influence on the content of Cu, Mn, and Zn in the available to plants forms are shown in Table 5. As can be seen from the data presented in Table 5, independently whether the tested soil was added 1% or 2% ash in calculation of organic carbon (Corg) were obtained

identical results with regard to the contents of individual metals in the available to plants forms. This can be explained by the fact that the obtained results are adequate for the time at which the analysis was performed. From the results in this table shows that, the addition to tested soil the fly ash was significantly Zn and Cu immobilized and thereby reduced the availability of tested metals from plants. Namely, without the addition of ash the content of Cu in the forms available to plants is around 24.1% in relation to the total content, while in soil with ash about 15.8%. For manganese, they are respectively 47.7% and 1.9%; while for zinc are equal to respectively 22.1% and 14.4%. With regard to the tested metals was found, that ash is an effective factor in limiting the availability of various metals to plants in the following degrees: Cu (8.3%), Mn (39.8%) and Zn (7.7%). The immobilization of tested metals decreases in the following series: Mn > Cu > Zn. 土壤中有机质的重要来源可能是煤燃烧产生的飞灰。 它们对植物可利用形式的铜、 锰和 锌的含量的影响见于表 5。从表 5 中所给出的数据可以看出,无论被测试的土壤中加入 1% 或 2%的灰分,在计算有机碳(Corg)时都得到相同的结果。这可以用以下事实进行解释, 即分析时间是足够的。 从此表中的结果表明, 额外添加的粉煤灰在锌和铜的固化方面有重要 意义,从而降低了金属的植物可利用性。即,不添加灰分中的 Cu 的植物可利用形式的含量 约 24.1%,而添加灰分约 15.8%。 锰分别是 47.7%和 1.9%,而锌分别为 22.1%和 14.4%。 关于测试金属发现, 即灰是一种限制植物可用性的有效因素, 其限制结果如下: (8.3%) 铜 , 锰(39.8%)和锌(7.7%) 。测试金属固化如下:锰>铜>锌。 In conclusion, the components of fly ash show a great affinity for the formation of insoluble connections tested heavy metals. The presence of these connections will the immobilization of heavy metals in soil and consequently reduce the availability of these metals to plants, and reduce their content in the system soil-plant and downstream tropic chain. The observed fact, that the use of the certain doe of fly ash can be effectively investigated immobilization of heavy metals have a direct practical importance. This means that, the fly ash used in experiment can be taken into account, as a supplement for the remediation of soils contamined with Cu, Mn or Zn. 总之, 粉煤灰的成分对形成不溶性测试金属有很大的亲和力。 这些连接的存在将土壤中 的重金属固定化, 因此减少这些金属的植物可利用性, 并减少土壤—植物系统和下游趋向失 误链中的金属含量。 所观察到的事实, 即研究粉煤灰固化重金属的实验设计有重要的实际意 义。这意味着,实验中可以考虑使用的粉煤灰作为修复铜、锰或锌的土壤污染修复的补充。 3.6. Investigation of the Possibilities of Reduced the Availability of Metals to Plants under the Influence of Fly Ash 粉煤灰影响下降低植物可用性的可能性调查 The results of a study on the possibility of limiting the availability of Cu, Mn and Zn to plants under the influence of fly ash are given in Table 6. Based on the obtained results found, that the available to plants content of Cu respectively averaged 17.9%, Mn—38.8% and Zn 17.2% in relation to the total content in the soil without the addition of fly ash. In turn, after addition of ash to soil, the content of examined metals in the forms available to plants are respectively: Cu—12%, Mn—1.7% i Zn—16% (Table 6). This indicates for a reduction of the content of metal available to plants in the range of concentrations, respectively for Cu (10 - 300 mg·kg–1), for Mn (300 - 3000 mg·kg–1) and Zn (50 - 500 mg·kg–1), after the addition of fly ash in an amount of 2% in terms of organic carbon (Corg). The reduction of concentrations of tested metals in the forms available to plants when added to soil fly ash was due to an increase in soil pH and the introduction in the

environmental soil of additional ions (Ca2+, Mg2+, K+, Na+). The concentration of these ions determines the sorption capacity of soil, which determines the degree of retention the heavy metals by the soil. The addition of fly ash reduces the availability of Mn to the greatest extent (37.1%), to a lesser extent Cu (5.9%) and lowest Zn (1.2%). Obviously coal fly ash was less effective for immobilization of Zn compared Cu and Mn. This is due to greater affinity for Mn and Cu complexes in the soil and create lasting relationships with them. In turn, Zn does not show a large affinity for the complex compounds and the tendency to form lasting relationships with them. 粉煤灰影响下降低铜、锰和锌的植物可利用性的可能性的研究结果如表6所示。基于所 得结果发现土壤中没有添加粉煤灰,相对于总金属含量,铜的植物可利用性含量平均为 17.9%,锰为38.8%,锌是17.2%。反过来,土壤中加入粉煤灰后,测试金属的植物可利用含 量分别为: Cu—12%, Mn—1.7% i Zn—16% (表6)。这表明减少金属植物可利用性浓度范围 分别是:铜(10 - 300 mg·kg–1),为锰(300 - 3000 mg·kg–1)和锌(50 - 500 mg·kg–1),另外,在 添加粉煤灰后,增加了2%有机碳(Corg)。土壤中添加粉煤灰可以降低测试金属的植物可利用 形式下的浓度是由于增加土壤pH值和引入土壤环境中额外的离子(Ca2 +,Mg2 +,K +、Na +)。 这些离子的浓度决定了土壤的吸附能力, 从而决定了土壤保持重金属的程度。 粉煤灰的加入 降低了可用性锰最大范围(37.1%),较小范围的铜(5.9%)和最低锌(1.2%)。显然粉煤灰可以 有效减少对锌的固化,与锰、铜相比。这是由于在土壤中创建持久对锰铜配合物的更大亲。 反过来,锌没有显示出很大的亲和力。 In the interpretation of results must take into account that the behavior of heavy metals after their introduction into the soil is determined by two groups opposing processes. The first includes processes that reduce the mobility of a given element and its accumulation in the superficial layers of the soil. These are primarily ions sorption by mineral and organic absorbent complex of soil, precipitation of insoluble compounds from the soil solution and the biogenic accumulation. The second group consists of processes that increase the mobility of elements, and thus desorption, solubility and mineralization of organic compounds. Solubility and desorption of Cu, Mn, Zn increased with a decrease in pH, hence the intensity of the start of these metals in acidic soils is several times higher than in soils with pH neutral or slightly acid. The degree of mobility of metal is also studied closely with the type of soil, as well, as their geochemical properties. 对结果的解释必须考虑到重金属引入到土壤中后的行为是由两组对立的过程组成。 第一 类包括降低对给定元素及其在浅层土壤积累和迁移的过程。 这些主要是土壤中矿物和有机体 复杂的离子吸附。 第二组包括增加元素流动性的, 例如解吸, 有机化合物的溶解和矿化。 铜、 锰和锌在水中的溶解和解吸随pH值的增加而减少,因此在酸性土壤中这些金属的开始强度 比在pH中性或微酸土壤的高出几倍。金属流动性与土壤的类型以及它们的地球化学性质也 做了仔细研究。 4. Conclusion 结论 The issue related to the remediation of contaminated soils is difficult and requires a systematic research aimed at developing the most effective, cheapest and most readily available methods.The proposed method using the coal fly ash to the immobilization of heavy metals is technically easy to implement. It can be an effective means of chemical remediation for soils contamined with Cu (concentration range 10 - 300 mg·kg–1), Mn (300 - 3000 mg·kg–1) or Zn (50 - 500 mg·kg–1). The most important advantage of this method is the fact, that can be applied to large areas due to non-toxic properties of fly ash. In

addition, is an effective way to use fly ashes from coal, which the quantity from year to year systematicaly increases. Nevertheless, one must ask whether the effect if immobilization of tested heavy metals will be sustainable in a environment? 关于污染土壤修复的问题是很难的,并且需要系统的研究,旨在发展最有效、最便宜、 最具有可行性的方法。 建议采用粉煤灰固化重金属, 该方法在技术上容易实现。 对于 Cu (浓 –1 –1 –1 度范围 10 - 300 mg·kg ) ,锰(300 - 3000 mg·kg )或 Zn(50 - 500 mg·kg )的污染, 它是一种有效的化学修复方法。此方法最重要的优点是,由于粉煤灰无毒性,可以应用于大 面积。此外,该方法是使用粉煤灰的有效方法,因为粉煤灰是逐年增加的。然而,有人要问 测试重金属固化的效果,如果将在环境中可持续?


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