利用除尘灰制备活性炭的工艺研究

以除尘灰为原料,用物理活化法制备活性炭．研究了活化温度、活化时间、活化剂流量对活性炭性能的影响．实验结果表明,活化温度和活化时间对活性炭的BET比表面积和吸附性能有很大影响;该方法可制得1nm以下微孔和10nm以下中孔均比较发达的活性炭．     

Relation between silico-aluminous fly ash and its coal of origin

Fly ashes are typical complex solids which incorporate at the same time intrinsic properties derived from the layers （various mineralogical and dimensional spectra） and major transformations generated during prior processing. To use fly ashes in various applications, it is necessary to characterise them completely. The first research to date carried out on silico-aluminous fly ashes in order to characterise them physically, morphologically, chemically and mineralogically, resulted in the recognition that they are relatively simple materials. In the present study, a silico-aluminous fly ash coming from the power station of Albi （France） was selected. Heat treatment at 450 and 1200℃ together with coal simulated the treatment undergone by coal in the power station in order to mimic real coal residue. In conclusion, the diversity of the particles contained in fly ash could only be exolained by the relation existing between the fly ash and its coal of origin.     

Horizontal attenuated total reflection applied to simultaneous determination of ash and protein contents in commercial wheat flour

Partial least-squares (PLS) regression was used to generate various models for the determination of both the protein and the ash contents of wheat flours by using spectroscopic data in the mid-infrared region obtained with a horizontal attenuated total reflectance (HATR) accessory. One hundred samples of wheat flour were used as purchased in the market: 55 for constructing the calibration model and 45 as external samples. The protein content varied between 8.85 and 13.23% and the ash content, between 0.330 and 1.287%, as determined by reference methods. Raw spectra and those corrected by multiplicative signal correction (MSC), first and second derivative spectra, were used as data for building the models. Different pre-treatments, such as mean centered and/or variance scaled (VS) methods, were tested and compared. Very good models were built as judged by the correlation coefficients (R²), root mean square error of calibration (RMSEC), root mean square error of validation (RMSEV) and root mean square error of prediction (RMSEP) that were obtained. Best results were achieved with MSC treated spectra.     

An ultrasound-assisted digestion method for the determination of toxic element concentrations in ash samples by inductively coupled plasma optical emission spectrometry

A method of ultrasound-assisted digestion followed by inductively coupled plasma optical emission spectrometry (ICP-OES) used for the determination of toxic element concentrations (arsenic, barium, cobalt, copper, lead, nickel, strontium, vanadium and zinc) in ash samples was developed. All the measurements were performed in robust plasma conditions which were tested by measuring the Mg(II) 280.270 nm/Mg(I) 285.213 nm line intensity ratios. The highest line intensity ratios were observed when a nebulizer gas flow of 0.6 L min⁻¹, auxiliary gas flow of 0.2 L min⁻¹ and plasma power of 1400 W were used for radially viewed plasma. The analysis of SRM 1633b showed that the ultrasound-assisted method developed is highly comparable with the microwave digestion method standardized by the United States Environmental Protection Agency (EPA-3052). The ultrasound-assisted digestion with a digestion solution of aqua regia and hydrofluoric acid (HF) resulted in recovery rates of over 81%. One exception is arsenic which resulted in recoveries of about 60% only; however, it could be digested with good recovery (>90%) using a digestion solution of 5 mL of water and 5 mL of aqua regia. The major advantage of the ultrasound-assisted digestion over microwave digestion is the high treatment rate (30 samples simultaneously with a sonication time of 18 min).     

Comparative Efficiencies of Trace Metal Extraction from Municipal Incinerator Ashes

Abstract

Five laboratory solvent extraction methods for the determination of leachable trace metals from municipal incinerator fly and bottom ashes are evaluated. The trace elements of interest were cadmium, chromium, copper, manganese and lead. Five different extractants, 0.1NHCl, 1.0 N ammonium acetate, methyl isobutyl ketone (MIBK), chloroform and hexane were used on each ash to determine comparative extraction efficiencies.

Extraction efficiencies of the five solvents were determined based on total metal concentration, and were found to rank in the following order: 0.1NHCl<1.0N ammonium acetate < MIBK < chloroform < hexane. No one solvent was optimal for obtaining environmentally available values for all five metals. The inorganic solvents, 0.1NHCl and 1.0N ammonium acetate, exhibited higher removal of trace metals from ash particles relative to the organic solvents. Manganese concentrations were removed more efficiently by 0.1NHCl, whereas 1.0 N ammonium acetate was more efficient for removing copper concentrations. Cadmium, Cr, and Pb could effectively be extracted by either of the two inorganic solvents. Concentrations of trace metals extracted from refuse ash appeared to be a function of the elemental boiling point and the species that exist on combustion. However, the classification of elements for refuse ash in this study strayed somewhat from the traditional geochemical classification scheme into which coal ash is placed.     

以除尘灰分离碳粉制备活性炭的新方法研究

利用除尘灰分离碳粉作原料,采用添加适量化学药品KOH的方法制备颗粒活性炭。研究了随着KOH加入量的变化,活性炭性能和对苯的吸附量的变化规律,以及KOH的加入量对活性炭的微晶结构和表面形貌产生的影响。并探讨了添加剂在活性炭制备的炭化和活化阶段的产生的影响。实验结果表明在KOH加入量为1.5%时,碘吸附值、比表面积和对苯的吸附量达到最高值,KOH过量反而对吸附性能有负面影响。     

Experience with wheat flour reference material

The Chemical Section of the National Office of Measures, Hungary (OMH) [1] embarked on the preparation of a wheat sample series as a Certified Reference Material [2] (CRM) in 1992. The practical implementation of the wheat sample series has shown that test- ing laboratories are in great need of easy-to-use flour reference samples to objectively and independently qualify wheat. To fill this need, we have developed a three-term flour reference sample series. The certification process was car-ried out according to ISO recommendations. Investigations of the long-term stability [3] and the application of wheat and flour CRMs are continuing. Wheat is one of the most widely grown crops in Hun- gary and it is one of the major determinative factors in the economy. Its uniform and objective qualification is of outstanding importance. There are well-equipped laborato-ries with sufficient experience to assess wheat flour quality, howev- er, proficiency testing has shown that certified samples need to be used to achieve exact and uniform measuring results. Received: 12 November 1999 Accepted: 16 August 2000     

The determination of trace element concentrations in fly ash samples using ultrasound-assisted digestion followed with inductively coupled plasma optical emission spectrometry

A method of ultrasound-assisted digestion followed by inductively coupled plasma optical emission spectrometry (ICP-OES) used for the determination of trace element (chromium, copper, lead, nickel, vanadium and zinc) concentrations in fly ash samples was developed. All the measurements were performed in robust plasma conditions. Ultrasound-assisted digestion procedures using digestion solutions of aqua regia and hydrofluoric acid (HF) resulted in recovery rates of over 80% for all the analyte elements. Ultrasound-assisted two-step digestion with digestion solutions of 6 mL of HNO₃ (Step 1) and 3 mL of HNO₃ + 3 mL of HF (Step 2) resulted in recovery rates of over 92% for all the analyte elements with one exception, chromium, which had a recovery of about 85%. The analysis of SRM 1633b showed that the two-step ultrasound-assisted digestion method developed resulted in chromium, copper, nickel and zinc concentrations higher than the microwave digestion method standardized by the United States Environmental Protection Agency (USEPA method 3052). This is the very first time when a digestion method using ultrasound resulted in higher efficiency than microwave (USEPA method 3052) for chromium and nickel in very hard to dissolve samples. The major advantages of the ultrasound-assisted digestion over microwave digestion is the high treatment rate (about 30 samples simultaneously with a sonication time of 18 min) and the possibility to use new sample vessels without a significant increase in costs.     

激光能量对飞灰颗粒流中未燃碳LIBS检测影响研究

飞灰含碳量是评价锅炉燃烧效率的重要指标之一,对其进行在线测量有助于实时进行燃烧优化调整,从而提高整个机组的经济性和安全性。利用螺杆式给粉机搭建飞灰颗粒流含碳量测量台架,将脉冲激光直接作用于飞灰颗粒流,形成等离子体,利用激光诱导击穿光谱技术测量飞灰颗粒流中的含碳量信息。重点研究了激光能量对飞灰颗粒流中未燃碳有效激发和测量的影响规律。研究结果显示,在40～130 mJ能量的脉冲激光作用下,碳谱线强度随着激光能量的增大线性增强,而其信噪比则先增加后趋于稳定,无效光谱的剔除率则呈下降趋势。本实验条件下,激光能量在90～100 mJ之间,可得到较强的等离子体发射信号和较优的光谱数据利用率。因而激光能量与颗粒流的激发状态、碳元素特征谱线强度等密切相关。合理的激光能量有利于保证飞灰颗粒流的有效稳定激发,并获得具有良好信噪比的等离子体光谱信号。