用荧光光谱鉴别白酒

在对乙醇、甲醇等醇类溶液荧光光谱特性进行研究的基础上, 应用美国Roper-Scientific公司SP-2558多功能光谱测量系统, 对50多种品牌白酒及其年份酒在紫外光激励下的荧光光谱进行了检测。结果表明, 白酒在紫外光激励下能产生较强的荧光, 各品牌白酒及其年份酒的荧光光谱各有明确的特征。实验测得其三维荧光光谱, 由此构建了白酒荧光光谱指纹图库。分析各荧光光谱的特征, 以谱峰个数、峰值波长、最佳激励波长等特征值创建了各品牌年份白酒荧光光谱特征数据库。利用SQL 数据库软件和VB语言研制成一个能对白酒进行自动比对、识别的白酒荧光光谱智能鉴别系统,实现了白酒的智能化鉴别。研究结果发挥荧光光谱分析灵敏度高、准确度高和样品用量少、不需前期处理等优点, 为白酒检测、鉴别提供了一种有效的新方法, 能应用于白酒企业生产管理及白酒消费市场监督, 并为已引起广泛关注的酒类食品安全监管提供帮助。     

原煤和黑液水煤浆燃烧特性的热分析对比研究

在热天平上进行黑液水煤浆和原煤的燃烧、热解实验,得到不同升温速率下的燃烧、热解特性曲线和碳转化率特征曲线。试验结果表明,黑液水煤浆中的钠及其化合物在燃烧过程中催化作用明显,并且黑液中有机物成分对燃烧起到一定促进作用。在20 ℃/min升温速率下黑液水煤浆和原煤的燃烧活化能分别为12.98 kJ/mol和106.59 kJ/mol,反映出黑液水煤浆比原煤有更好的着火特性。     

Development of a fully buffered molybdate electrolyte for capillary electrophoresis with indirect detection and its use for analysis of anions in Bayer liquor

A new counterion-buffered molybdate electrolyte was developed and optimized for simultaneous quantitative determination of up to eight anions (chloride, sulphate, oxalate, fluoride, formate, malonate, succinate, and acetate) in Bayer liquor by capillary electrophoresis with indirect detection at 214 nm. The separation parameters were optimized in respect to separation of the critical analyte group fluoride-formate-malonate, with the optimal electrolyte prepared from molybdic trioxide containing 5.0 mmol/L MoO3, 1.3 mmol/L cetyltrimethylammonium bromide (CTAB), and buffered with diethanolamine (DEA) to pH 9.2 (ca. 20 mM DEA). Total length of separation capillary was 80 cm, resulting in run time of under 4 min. The method is suitable for a wide concentration range of the analytes (1-50 mg/L) with linear calibration plots (R2 = 0.9983-0.9999). Relative standard deviations were 0.05%-0.07% for migration times and 0.67%-2.04% for peak areas. The detection limits were in the range of 0.17-0.51 mg/L or 2-10 micromol/L (hydrostatic injection of 30 s of 1000 x diluted sample). Due to its good buffering capacity, the electrolyte exhibited an excellent ruggedness and good tolerance to the alkaline samples. Consequently, Bayer liquor samples could be diluted as little as 100 x which allows more sensitive determination of minor components over previous methods. The method was successfully applied to analysis of Bayer liquor samples with recoveries in the range of 95-105%.     

DECOMPOSITION OF BLACK LIQUOR BY ULTRASOUND PROCESS

Ultrasound (US)-induced cavitation is an effective way in oxidizing organic contaminants in wastewater either as the independent operation unit or in combination with other oxidation methods. In this paper, black liquor and filtrate after acidifying and settling were sonicated The effect of working parameters on ultrasonic degradation of black liquor, such as different combinationmethods, frequency, power supply, initial concentration, pH, duration time, ionic strength and catalyst were studied The results were as follows: (1) At the conditions of 4OkHz, IOOW, 4h, pH at 6 and temperature 30±2℃,, utilizing US/US-H2O2/US-Fenton, weak-orange filtrate turned to colloid with the increase of time and little sediment produced after settling. Especially filtrate came to be milk white collides and upper water approached to nearly achromatic by US-Fenton. Compared with the US, US-H2O2/US-Fenton COD (Chemical oxidation demand) removal ratio can increase 15%,30% respectively. Because of more hydroxyl radicals produced in tire reaction process; (2) At the condition of lOOW and 4h, the degradation efficiency of black liquor was better at 40kHz over at 20kHz. Moreover black liquor can be biodegraded easily Those based on that the big molecule of contaminants in aqueous solution can be changed into the little molecule with ultrasound (3) At the condition of 40kl-l: and 4h, the COD removal ratio of black liquor was more higher at 60W than at 80W, while the removal ratio of COD at 60W was nearly close to the ratio at 100W,“ (4) The initial concentration of black liquor influenced the effect of sonochemical degradation; (5) The variation of pH had no effect on degradation; (6) The longer the duration time, tire greater the removal ratio of COD. But this ratio increased slowly after 4h; (7) Adding 0.2g/L NaCI to change the ionic strength of the black liquor, the COD removal ratio can increase 10%; (8) The degradation rates increased by the coexistent catalysts of TiO2, Co^+2 and Ag^+.     

福建无烟粉煤纸浆黑液富氧流化床催化气化研究

在实验室小型流化床反应器中研究了福建龙岩无烟粉煤纸浆黑液富氧催化气化的特性，考察了纸浆黑液催化剂添加量不同时氧体积分数变化对碳转化率、产气率、煤气组成与热值的影响。结果表明，纸浆黑液催化和富氧气体燃烧的双重作用明显地提高了煤的碳转化率和煤气有效组成；纸浆黑液中钠碱对煤焦气化的催化与对煤灰分中SiO2和Al2O3等氧化物的熔制反应同时发生并存在着竞争；纸浆黑液中钠碱对高温碳与气化剂之间多种反应表现出不同程度的促进。龙岩无烟粉煤在纸浆黑液富氧催化气化时适宜操作条件是氧的体积分数40％和蒸汽/富氧比为1.4kg/m3～2.0kg/m3。碳转化率94％、煤产气率为3.62m3/kg、煤气热值为7.33mJ/m3。     

工业废液碱对福建无烟煤水蒸气催化气化的实验室研究

在Φ28mm的反应管中，采用工业废液碱用于福建无烟煤固定床水蒸气气化实验。结果表明，该废液碱对福建无烟煤气化有很强的催化活性。在添加3％－12％废液碱的情况下，碳转化率均比无催化剂时增加2.55倍－3．93倍，明显大于添加以Na2CO3为催化剂的碳转化率。同时该废液碱对煤气组成，产气量和煤气热值均有明显提高。在催化气化的同时加入适量的脱碱剂可极大地降低灰渣中的含碱量。     

气相色谱直接进样法分析环己烷氧化废液中的有机酸

环己烷氧化废液经酸化、抽滤等预处理后 ,采用气相色谱直接进样法分离了样品中的 1 0种有机酸 ,并测定了其含量。测定废液中各有机酸的回收率在 95 %～ 1 0 5 %之间。气相色谱固定相为 5 %新戊二醇己二酸酯 +0 .2 %磷酸/1 0 1酸洗白色担体。     

Determination of sodium oxalate in Bayer liquor using flow-analysis incorporating an anion exchange column and tris(2,2′-bipyridyl)ruthenium(II) chemiluminescence detection

Semi-automated flow injection instrumentation, incorporating a small anion exchange column coupled with tris(2,2′-bipyridyl)ruthenium(II) (Ru(bipy)₃²⁺) chemiluminescence detection, was configured and utilised to develop rapid methodology for the determination of sodium oxalate in Bayer liquors. The elimination of both negative and positive interferences from aluminium(III) and, as yet, unknown concomitant organic species, respectively are discussed. The robustness of the methodology was considerably enhanced by using the temporally stable form of the chemiluminescence reagent, tris(2,2′-bipyridyl)ruthenium(III) perchlorate in dry acetonitrile. Real Bayer process samples were analysed and the results obtained compared well with those performed using standard methods within industrial laboratories.     

分光光度法测定白酒中的糠醛

分光光度法测定白酒中的糠醛许汉英＊赵晓君（吉林进出口商品检验局长春１３００６２）（吉林大学化学系长春）关键词糠醛，白酒鉴别，紫外光度法１９９６－０８－０７收稿，１９９７－０１－０５修回白酒中的糠醛主要来源于酿酒所用的各种原辅料，如粮食、稻皮、麦夫皮、...     

Physical Properties of Highly Active Liquor Containing Molybdate Solids

The reprocessing of irradiated nuclear fuel at Sellafield produces a nitric acid based Highly Active Liquor (HAL) waste. The liquor, containing fission products and process additives, is concentrated in an evaporator in order to reduce the volume and is then stored in Highly Active Storage Tanks (HASTs) prior to vitrification. Caesium phosphomolybdate (CPM) is precipitated during the evaporation process and can convert to zirconium molybdate (ZM) during storage.During Post Operational Clean Out (POCO) of the HASTs, it is expected that their highly active content will be reduced by repeated cycles of washing using nitric acid and other reagents. Initial washings are likely to have a chemical composition comparable to concentrated HAL, becoming more dilute during the wash-out process. It is expected that the wash-out process will also recover significant quantities of molybdate solids (ZM, CPM or a mixture) from the HASTs.In order to determine the processing challenges from such washings during POCO, the physical properties of varying concentrations of non-active HAL simulants containing molybdate solids have recently been measured by the UK's National Nuclear Laboratory. The following measurements are presented and discussed:

• •Particle size distribution
• •Density
• •Settling behaviour of solids
• •Voidage of settled sediment beds
• •Viscosity
• •Yield stress
• •Influence of ZM morphology on physical properties