ASE-气相色谱法测定油田区土壤中多种石油烃

采用气相色谱法测定油田区土壤中C_(10)～C_(40)的石油烃,通过优化加速溶剂萃取的条件,使方法在62 mg/L～3 100 mg/L范围内线性良好,方法检出限为4.8 mg/kg。用该方法测定石油区短期、中期、长期油井污染土壤样品,5次测定结果的RSD为1.3%～5.2%,加标回收率为84.8%～98.5%,有证标准样品测定结果在可信区间内。     

皂素和柠檬酸复合淋洗土壤中的钍

采用振荡淋洗和土柱动态淋洗实验研究了皂素和柠檬酸复合对土壤中钍的淋洗性能。实验结果表明:将质量浓度为20 g/L的皂素与浓度为20 mmol/L的柠檬酸以体积比1∶10配制复合淋洗液对污染土壤中钍的去除效果最佳,淋洗3.0 h,钍去除率为84.98%;准一级动力学方程能更好地描述复合淋洗液对钍的淋洗动力学特征;动态淋洗实验中当复合淋洗液用量为1 600 mL时,钍的累积去除量为73.66 mg/kg;淋洗后土壤中钍的酸可提取态、氧化结合态和有机结合态含量分别减少了79.63%、38.13%和20.34%,残渣态含量变化不大;淋洗后土壤中钍的稳定性增加。     

煤与瓦斯共采在错层位巷道布置中的机理研究及应用构想

为了完善现有煤与瓦斯共采技术，创新煤与瓦斯共采方法，对错层位巷道布置下的煤与瓦斯共采系统展开研究，利用相似模拟试验，分析错层位巷道布置覆岩运动情况，预测其开采围岩裂隙发育和瓦斯运移形式，提出了创新煤与瓦斯共采技术构想。研究结果表明:采空区覆岩三带高度随接续工作面的增加而增大，相邻采空区垮落矸石压实区呈现“O-L-O”形变化，多个相邻采空区覆岩出现大“O”形圈裂隙带；相邻采空区内瓦斯可实现相互运移，大“O”形圈裂隙带内赋存大量瓦斯气体；研究提出了地面钻井抽采瓦斯、走向高位瓦斯抽采巷和外错尾巷穿层钻孔3种煤与瓦斯共采技术，比传统巷道布置情况下的煤与瓦斯共采技术在安全、经济等方面更具优势。     

Optimal Absorbent Evaluation for the CO2 Separating Process by Absorption Loading,Desorption Efficiency,Cost, and Environmental Tolerance

The CO₂ absorption capacities of potassium glycinate, potassium sarcosinate (choline, proline), mono-ethanolamine (MEA), and tri-ethanolamine were evaluated to find the optimal absorbent for separating CO₂ from gaseous products by a CO₂ purification process. The absorption loading, desorption efficiency, cost, and environmental tolerance were assessed to select the optimal absorbent. MEA was found to be the optimum absorbent for separating the CO₂ and H₂ mixture in gaseous product. The maximum absorption loading rate was 0.77 mol CO₂ per mol MEA at temperature of 20°C and absorbent concentration of 2.5 mol/L, whereas desorption efficiency was 90% by heating for 3 h at 130°C. MEA was found to be an optimal absorbent for the purification process of CO₂ during gaseous production.     

Feasibility of honeycomb monolith supported sugar catalyst to produce biodiesel from palm fatty acid distillate (PFAD)

Carbon coated monolith was prepared by sucrose solution 65 wt.% via dip-coating method. Sulfonation of incomplete carbonized carbon coated monolith was carried out in order to synthesize solid acid catalyst. The textural structure characteristics of the solid acid catalyst demonstrated a low surface area and pore volume. Palm fatty acid distillate (PFAD), a by-product of palm oil refineries, was utilized as oil source in biodiesel production. The esterification reaction subjected to different reaction conditions was performed by using the sulfonated carbon coated monolith as heterogeneous catalyst. The sulfonation process had been performed by using vapour of concentrated H₂SO₄ that was much easier and efficient than liquid phase sulfonation. Total acidity value of carbon coated monolith was measured for unsulfonated sample (0.5 mmol/g) and sulfonated sample (4.2 mmol/g). The effect of methanol/oil ratio, catalyst amount and reaction time were examined. The maximum methyl ester content was 89% at the optimum condition, i.e. methanol/oil molar ratio (15:1), catalyst amount (2.5 wt.% with respect to PFAD), reaction time (240 min) and temperature 80 °C. The sugar catalyst supported on the honeycomb monolith showed comparable reactivity compared with the sugar catalyst powder. However, the catalyst reusability studies showed decrease in FFA% conversion from 95.3% to 68.8% after four cycles as well as the total acidity of catalyst dropped from the value 4.2 to 3.1 mmol/g during these cycles. This might be likely due to the leaching out of SO₃H group from the sulfonated carbon coated monolith surface. The leaching of active species reached a plateau state after fourth cycle.     

加速溶剂同时萃取和净化-气相色谱-三重四极杆串联质谱测定土壤和沉积物中8种多溴联苯醚

建立了土壤和沉积物中8种多溴联苯醚(PBDEs,BDE-28、BDE-47、BDE-99、BDE-100、BDE-153、BDE-154、BDE-183和BDE-209)加速溶剂同时萃取和净化-气相色谱-三重四极杆串联质谱(ASE-GC-MS-MS)的分析方法。通过优化加速溶剂萃取与弗罗里硅土在线净化和串联质谱多反应监测模式的条件,较好地去除基质干扰,并提高了三重四极杆串联质谱定性的准确性及定量的灵敏性。该方法采用改进的色谱柱能同时分析包括高溴代联苯醚BDE-209在内的8种PBDEs,其浓度范围为1～100 ng/mL(BDE-209为10～1 000 ng/mL),线性良好,线性回归系数均大于0.997。方法检出限为0.004～0.1 ng/g,方法回收率为75%～110%,方法精密度为2.4%～15.6%。适于批量处理土壤和沉积物中含有多组分痕量PBDEs的样品。     

Pre-concentration and separation of heavy metal ions by chemically modified waste paper gel

Iminodiacetic acid was immobilized on waste paper by chemical modification in order to develop a new type of adsorption gel for heavy metal ions. Adsorption behavior of the gel was investigated for a number of metal ions, specifically Cu(II), Pb(II), Fe(III), Ni(II), Cd(II), and Co(II) at acidic pH. From batch adsorption tests, the order of selectivity was found to be as follows: Cu(II)  Fe(III) > Pb(II) > Ni(II)  Co(II) > Cd(II). Column tests were carried out for pairs of metal ions to understand the separation and pre-concentration behavior of the gel. It was found that mutual separation of Ni(II) from Co(II) and that of Pb(II) from Cd(II) can be achieved at pH 3. Similarly, selective separation of Cu(II) from Cu(II)–Fe(III) and Cu(II)–Pb(II) mixtures at pH 1.5 and 2, respectively, was observed by using this new adsorption gel. In all cases, almost complete recovery of the adsorbed metal was confirmed by elution tests with HCl.     

山梨酸废水在ABR中的基质降解行为

稳态条件下,采用厌氧折流板反应器(anaerobic baffled reactor,ABR)处理山梨酸废水并进行基质降解动力学研究.实验表明,在污泥负荷为0.54～1.63 kg COD/(kg VSS·d)的范围内,COD去除率随着负荷的增加从85%降到55%.各隔室出水COD沿程递减,前3个隔室承担了去除COD的重要作用,但随着污泥负荷的增加,后部承担的COD去除率比例增大.基于各串联隔室完全混合的假定,推导ABR中山梨酸废水的基质降解动力学方程,并通过实验确定相关动力学参数及相应的动力学方程.实测值与预测值基本吻合.     

我国消防标准体系分析

为明确我国消防标准体系发展的方向和重点,分别从消防标准的数量、标龄、类型、属性和采标情况等5个方面对我国消防标准体系进行分析,并与国际标准化组织、欧盟标准化委员会和美国的消防标准体系进行了比较。研究结果表明:我国消防标准体系整体适用性在不断增强;需制定周期性标准复审计划;消防基础试验类和管理类标准应成为下一步消防标准制修订的重点;消防强制性标准所占比例有待进一步下调;需建立国际标准动态跟踪机制,同时应注重将我国先进的消防标准转化为国际标准。