灰化消解-极谱法测定油料中五个重金属元素

建立了灰化消解-极谱法测定油样中镉、铅、铜、镍、钴等5种微量重金属元素的含量.油料样品通过灰化法消解后,用极谱法在乙酸-乙酸盐缓冲溶液和磺基水杨酸-磷酸-氨水体系中测定5种重金属元素的含量.5种微量重金属元素的检出限为1.3×10-4～9.8×10-4 g·L-1,加标回收率为90%～106%,相对标准偏差为0.22%～3.16%.     

矿区植物重金属元素测定的两种前处理方法比较

分别采用酸消解法和干灰化法处理16种矿区植物,并用原子吸收分光光度法测定其中的Mn、Cd、Cr和Zn的含量。结果表明:除Cd外,两种处理方法对Mn、Cr、Zn的测定结果有明显影响。测定植物组织Cd时,两种处理方法都可采用;测定Mn、Cr元素,采用酸消解法较为合适;测定Zn则宜采用干灰化法,并可适当延长木质部分(根、茎)的灰化时间。     

ICP-AES法同时测定动植物作用残体中几种主量与微量元素

本文对石英砂摄取的残体样品采取灰化干烧、加稀酸溶解的方法，空白值低，无环境污染，利用ICP－AES法测定其主量及微量元素，获得满意结果。     

灰分分析法测定羧甲基壳聚糖羧甲基取代度

本文建立了表征羧甲基壳聚糖羧甲基取代度的化学分析方法－灰分分析法，并将该方法与元素分析和电位滴定方法进行了比较。统计分析的结果表明，灰分分析方法的精度和准确度要高于电位滴定，其准确度较接近元素分析，是一种准确的分析方法。     

Ashing and microwave digestion of aerosol samples with a polypropylene fibrous filter matrix

Radionuclide monitoring is one of the key techniques required by the International Monitoring System (IMS) and On-Site Inspection (OSI) in the Comprehensive Nuclear Test Ban Treaty (CTBT). There shall be a global network of 80 radionuclide monitoring stations. Atmospheric aerosols are collected generally on filters in the stations. A polypropylene (PP) fibrous filter is often used in sampling atmospheric aerosols. There might be much information to be obtained by measuring aerosol samples after digestion rather than nondestructive analysis directly by γ-spectrometry. The present work focused on pretreatment of the filter samples, which includes the influence of different ashing or microwave digestion conditions on the recoveries of analytes. The inductively coupled plasma-atomic emission spectrometric detection results indicated that the recoveries of elements in the PP fibrous filters by ashing were influenced by ashing time, temperature and the properties of the elements. High recoveries of volatile elements and consistent recovery for other elements were obtained by using a closed microwave system to digest the filters. Higher sensitivity was also obtained when the intercomparison sample was measured by a HPGe well detector after pretreatment by the recommended ashing and microwave digestion procedures.     

ICP-AES测定黔产天麻中微量元素

用干法灰化,电感耦合等离子体-原子发射光谱法(ICP-AES)测定黔产野生和栽培天麻中人体必须微量元素的含量,实验证明,用干法灰化黔产野生和栽培天麻,样品消解完全,可以满足ICP-AES的检测要求,在选定的最佳条件下用ICP-AES检测各元素回收率在82%-99.5%之间,检出限为5-12ng·mL-1,该方法的相对标准偏差小于3.2%.为天麻中微量元素的测定提出了一个准确可行的方法,并为黔产野生及栽培天麻的开发提供可靠的依据.     

Dry-Ashing Preconcentration for Micro-Reactor-Based Neutron Activation Analysis of Food and Plant Samples

The application of preconcentration by dry-ashing to the neutron activation analysis of biological samples using a SLOWPOKE-2 low-power reactor is reported. Samples of selected food crops (banana, callaloo, carrot, mango, and yam) and bioindicator plants (lichen, moss, Tillandsia sp., and tree bark) were analysed both as plant tissue, and as ashed sample. The results are presented for 21 elements. Good agreement between both procedures (<10% relative standard error) was obtained for 13 elements: Al, Ca, Cd, Cr, Fe, K, La, Mg, Mn, Na, Sm, Ti, and V. For Dy, Rb, and Zn the agreement was 10-15%. Relatively poorer agreement (>15-30%) was obtained for As, Br, Cl, and Sb. Dry ashing produced improved analytical results for those samples that were of low ash content. However, the increased background counts observed in ashed samples can sometimes negate the concentration gain, particularly in plants with high ash contents but low levels of certain elements.     

微波灰化-氢化物发生-原子荧光光谱法测定出口小麦淀粉中痕量铅

建立了微波灰化,断续流动-氢化物发生-双道原子荧光光度计测定小麦淀粉中痕量铅的方法,解决了小麦淀粉前处理难的问题,研究了加入硝酸后对铅测定的影响,探讨了酸度、还原剂浓度、基体效应对氢化物发生的影响。铅的线性范围为1.00-200.0μg/L,方法检出限为0.57μg/L,回收率为88.50%-103.3%,精密度为2.54%-4.82%。     

A multisyringe sequential injection method for monitoring water in the energy cogeneration system of a municipal waste incinerator

Leading-edge urban solid waste ashing plants use burning heat energy to obtain electrical power. Water fed to their boilers for conversion into steam should be highly pure in order to minimize corrosion, scaling and similar phenomena, which can lead to malfunctioning and a reduced useful life but can be avoided by proper management and control of the water supply. In this work, we developed a multiparameter monitor based on multisyringe sequential injection for the sequential determination of up to eight important parameters, namely: pH, specific and acid conductivity, hydrazine, ammonium, phosphate, silicate and total iron.Acid conductivity was determined by passing the sample through a cation-exchange resin in order to retain ammonium ion and release protons. This parameter was deemed the most accurate indicator of dissolved solids in boiler water. Chemical parameters were determined spectrophotometrically: hydrazine by reaction with p-dimethylaminobenzaldehyde, ammonium by the modified Berthelot reaction, iron with o-phenanthroline, and phosphate and silica by formation of a molybdoheteropoly blue dye in the presence of ascorbic acid as reductant. Use of the optimum chemical and physical operating conditions provided 3s_blank detection limits of 0.01 mg l⁻¹ N₂H₄, 0.13 mg l⁻¹ NH₄⁺, 0.04 mg l⁻¹ Fe, 0.03 mg l⁻¹ SiO₂ and 0.05 mg l⁻¹ PO₄³⁻, and relative standard deviations not greater than 2.5%. The methods integrated in the proposed monitor were successfully applied to real samples from the water-steam cycle at the Son Reus ashing plant in Palma de Mallorca (Spain).     

Ashing of Organic Compounds with Spray-Type Plasma Reactor at Atmospheric Pressure

We examined the ashing treatment at atmospheric pressure by means of three spray-type reactors fed with O₂/He or O₂/Ar mixture gases. These differed in the size or the shape of their nozzles. Such reactors were able to ash an organic compound (OFPR-800; a photoresist) even at atmospheric pressure. The results showed that the following procedures are important for increasing the ashing rate: to make the gas speed after blowing out fast; to decrease the O₂ content while increasing the gas speed; and to use a gas mixture which has a slow decay rate of the active species, such as the oxygen radicals. Especially, when we used O₂/Ar mixture gas for the ashing treatment, the ashing rate became quite fast and was as fast as that of a general low pressure glow plasma.