The gamma-radiolysis of HEDTA in a simulated, mixed waste

The -radiolysis of the parent compound N-(2-hydroxyethyl)ethylenediaminetriaceticacid (HEDTA) in a simulant of a Hanford mixed waste, at a -dose of7.5 . 10₆±10% R, yielded 94.4% degradation. HEDTA radiolysisyielded four degradation products: glyoxylic acid, N-( nitroso)iminodiaceticacid (NIDA) and 2 dicarboxylic acids, ethandioic (oxalic) and propandioic(malonic) acids. Glyoxylic acid had been identified in previous studies byour laboratory as N-hydroxymethyl-N-methyliminoacetic acid (HMMIA). Promptedby studies from another laboratory, the chelator fragment previously reportedby our laboratory as N-(methylamine)iminodiacetic acid (MAIDA) is re-identifiedas NIDA. A methylamine moiety previously believed to be present in MAIDA,and several other chelator fragments, as well, has been re-identified as anitroso group.     

Detailed study of HEDTA’s chemodynamics upon gamma-radiolysis in a simulated, mixed waste

Gamma-radiolysis of the parent compound N-(2-hydroxyethyl)ethylenediamine-triacetic acid (HEDTA) in a simulant of a Hanford mixed waste, at γ-doses of 0–7.5·10⁶±10% R, yielded extensive degradation. Two major degradation products, glyoxylate and N-(nitroso)iminodiacetic acid (NIDA), were identified, along with lower levels of malonate and oxalate. Comparison of HEDTA’s radiolysis with that of ethylenediaminetetraacetic acid (EDTA), nitrilotriacetic acid (NTA) and citrate, from earlier studies, reveals several fundamental similarities, along with marked differences. Comparatively speaking, HEDTA’s radiolysis is not particularly diverse, but it is very dispersive.     

Solid-phase extraction of 11-nor-delta-9-tetrahydrocannabinol-9-carboxylic acid from human urine with gas chromatographic-mass spectrometric confirmation.

A selective and sensitive technique has been developed for detecting and identifying 11-nor-delta-9-tetrahydrocannabinol-9-carboxylic acid (THC-COOH) in human urine. Using a new, "mixed-mode", bonded silica gel, solid-phase extraction column cartridge, THC-COOH was selectively isolated from urine components. Following extraction, the presence of THC-COOH was confirmed and quantitated using gas chromatography-mass spectrometry (GC-MS) or gas chromatography-flame ionization detection. A linear quantitative response curve for THC-COOH was generated over a concentration range of 10 to 300 ng/ml. Overall extraction efficiency averaged greater than 85% and the quantitative response curve exhibited a correlation coefficient of 0.999. The limit of detection and identification using GC-MS for the drug metabolite was found to be six times below the present NIDA guidelines cut-off concentration of 15 ng/ml.     

高效液相色谱-串联质谱法同时测定废水中18种酚类污染物

建立了上清液直接进样-高效液相色谱-串联质谱同时测定废水中18种酚类污染物的分析方法。取5.0 mL水样置于具塞离心管中,加氨水调节pH≥12,摇匀,加入1.0 mL二氯甲烷-正己烷(2: 1, v/v)混合溶液并振摇5 min, 4000 r/min离心5 min,用玻璃针筒抽取上清液并经0.22 μ m聚四氟乙烯滤膜过滤,用甲酸调节水样pH至中性;然后采用Thermo Hypersil ODS柱(100 mm×2.1 mm, 5.0 μ m)分离,以甲醇-0.01 mol/L甲酸铵-甲酸水溶液(pH 4.0)为流动相进行梯度洗脱,流速0.2 mL/min,柱温30℃,进样10 μ L,电喷雾负离子电离(ESI^-)模式、多反应监测(MRM)模式进行检测,外标法定量。18种酚类化合物的峰面积与其质量浓度在一定浓度范围内均呈良好的线性关系(r²≥0.9991),方法检出限为0.10~0.88 μ g/L。测定低、中、高加标浓度的样品,18种酚类化合物的相对标准偏差为2.5%~9.9%(n=6);火工药剂废水与石油化工废水样品中的平均加标回收率为68.7%~118%(n=3)。此方法操作简单,灵敏度高,干扰小,分析速度快,可适用于环境废水中18种酚类污染物的同时分析。     

Biooxidation of a synthetic waste by a microbial film grown on the liquid surface in a shallow flow reactor

A new process of biological waste treatment was developed by use of microbial films grown on the liquid surface in a shallow flow reactor. The performance of this process was tested using a synthetic waste that contained acetic acid as a model organic pollutant. About 90% of acetic acid (10,000 mg/L-1) in the synthetic waste was removed by setting alpha tau: (alpha specific liquid surface area, cm-1, and tau: hydraulic liquid detention time, h) higher than 15 cm-1/h. It was necessary to maintain alpha large enough (more than 10 cm-1 in most cases) to satisfy oxygen demand for the biooxidation. The oxygen balance and TOC determinations showed that the acetic acid removed was completely oxidized with oxygen transferred through the liquid surface. This process would contribute to energy savings, since it requires no forced aeration for oxygen supply.     

Evaluation and Optimization of Organic Acid Pretreatment of Cotton Gin Waste for Enzymatic Hydrolysis and Bioethanol Production

This paper investigates the efficiency of the organic acids on the pretreatment of an industrially generated cotton gin waste for the removal of lignin, thereby releasing cellulose and hemicellulose as fermentable sugar components. Cotton gin waste was pretreated with various organic acids namely lactic acid, oxalic acid, citric acid, and maleic acid. Among these, maleic acid was found to be the most efficient producing maximum xylose sugar (126.05?±?0.74 g/g) at the optimum pretreatment condition of 150 °C, 500 mM, and 45 min. The pretreatment efficiency was comparable to the conventional dilute sulfuric acid pretreatment. A lignin removal of 88% was achieved by treating maleic acid pretreated biomass in a mixture of sodium sulfite and sodium chlorite. The pretreated biomass was further evaluated for the release of sugar by enzymatic hydrolysis and subsequently bioethanol production from hydrolysates. The maximum 686.13 g/g saccharification yield was achieved with maleic acid pretreated biomass which was slightly higher than the sulfuric acid (675.26 g/g) pretreated waste. The fermentation of mixed hydrolysates(41.75 g/l) produced 18.74 g/l bioethanol concentration with 2.25 g/l/h ethanol productivity and 0.48 g/g ethanol yield using sequential use of Saccharomyces cerevisiae and Pichia stipitis yeast strains. The production of bioethanol was higher than the ethanol produced using co-culture in comparison to sequential culture. Thus, it has been demonstrated that the maleic acid pretreatment and fermentation using sequential use of yeast strains are efficient for bioethanol production from cotton gin waste.     

超高效亲水作用色谱-串联质谱法检测水中的苦味酸及苦氨酸

建立了一种超高效亲水作用色谱-串联质谱检测水中苦味酸及其降解产物苦氨酸的方法。采用Acquity UPLC BEH HILIC亲水作用色谱柱（100 mm×2.1 mm,1.7 μm,Waters）分离,用电喷雾电离串联质谱检测。地表水样品经过0.2 μm滤膜过滤之后即可直接进样,加标回收率达89%~107%;废水样品通过固相萃取（SPE）净化后进样分析,加标回收率达72%~101%。方法重复性的相对标准偏差为4.9%~14.7%。本方法对苦味酸和苦氨酸的检出限分别为0.1 μg/L和0.3 μg/L。此方法快速、准确,特异性强,灵敏度高,样品前处理方法简便易行,适用于地表水、废水样品的检测。     

柴油溶剂中脂肪酶催化高酸值废油脂酯化制备生物柴油

采用0＃柴油作为反应溶剂,利用固定化脂肪酶催化高酸值废油脂与甲醇酯化反应制备生物柴油。来源于Candida antarctica的固定化脂肪酶Novozym435在0＃柴油溶剂中具有极高的催化活性。以酸价高达157×10-3的废油脂为原料,废油脂质量比10%的Novozym435,甲醇与废油脂初始摩尔比2∶1,0＃柴油与废油脂质量比5∶1,摇床摇速170r/min,50℃下反应2h甲酯化率可达95.10%。0＃柴油作为反应溶剂有效地溶解了高酸值废油脂和甲醇,降低了反应体系的黏度和消除了甲醇对Novozym435的负面影响,提高了Novozym435的稳定性。同时,0＃柴油溶剂对未脱胶废油脂中残留的对脂肪酶有害的磷脂等胶类物质具有一定的稀释作用。该工艺省却了溶剂蒸馏的繁琐工序,直接得到脂肪酸甲酯和石化柴油的混合燃料。     

紫外光谱法同时测定强力霉素废水中磺基水杨酸与对甲基苯磺酸

强力霉素是以土霉素为原料经过氯代、脱水、氢化成盐、置换多步化学反应后,再经过净化、脱色、过滤、结晶、干燥而制成的一种广谱抗生素[1]。其生产原料品种多,工艺复杂,生产废水色度深、浓度高、毒性大、含盐量高[2]。磺基水杨酸与对甲基苯磺酸是强力霉素废水中两种主要污染物     

N-溴代琥珀酰亚胺-二氯荧光素化学发光体系测定废水中5-磺基水杨酸

建立了测定5-磺基水杨酸的流动注射化学发光新方法。 研究了影响化学发光强度的因素,并初步探讨了可能的发光机理。 在最佳化学发光条件下,化学发光强度与5-磺基水杨酸浓度在5.0×10-8~2.0×10-5 mol/L范围内呈良好的线性关系,检出限为1.0×10-8 mol/L,对5.0×10-6 mol/L的5-磺基水杨酸平行测定9次,其相对标准偏差为2.7%。 该法可用于强力霉素废水中5-磺基水杨酸的测定。     

KMnO4-乙二醛化学发光体系测定5-磺基水杨酸的流动注射分析

酸性介质下,KMnO4可以氧化5-磺基水杨酸产生化学发光,乙二醛对该体系有增敏作用。结合流动注射技术,建立了测定5-磺基水杨酸的流动注射化学发光方法。方法线性范围为2.0×10-8～2.0×10-5mol/L,检出限为2.0×10-9mol/L,对2.0×10-6 mol/L的5-磺基水杨酸平行测定11次,相对标准偏差为1.9%。该法可用于强力霉素废水中5-磺基水杨酸的测定。     

Valorization of Fermented Shrimp Waste with Supercritical CO2 Conditions: Extraction of Astaxanthin and Effect of Simulated Gastrointestinal Digestion on Its Antioxidant Capacity

Lactic acid fermentation increases the bioactive properties of shrimp waste. Astaxanthin is the principal carotenoid present in shrimp waste, which can be found esterified in the liquid fraction (liquor) after its lactic acid fermentation. Supercritical CO₂ technology has been proposed as a green alternative to obtain astaxanthin from fermented shrimp waste. This study aimed to optimize astaxanthin extraction by supercritical CO₂ technology from fermented liquor of shrimp waste and study bioaccessibility using simulated gastrointestinal digestion (GD) of the optimized extract. A Box–Behnken design with three variables (pressure, temperature, and flow rate) was used to optimize the supercritical CO₂ extraction. The optimized CO₂ extract was obtained at 300 bar, 60 °C, and 6 mL/min, and the estimated characteristics showed a predictive extraction yield of 11.17%, antioxidant capacity of 1.965 mmol of Trolox equivalent (TE)/g, and astaxanthin concentration of 0.6353 µg/g. The experiment with optimal conditions performed to validate the predicted values showed an extraction yield of 12.62%, an antioxidant capacity of 1.784 mmol TE/g, and an astaxanthin concentration of 0.52 µg/g. The astaxanthin concentration decreased, and the antioxidant capacity of the optimized extract increased during gastrointestinal digestion. In conclusion, our optimized supercritical CO₂ process is suitable for obtaining astaxanthin from shrimp by-products after lactic acid fermentation.     

荧光分析法测定痕量亚硝酸根

在硫酸介质中,亚硝酸根能还原吡咯红Y,使其荧光猝灭据此提出了一个测定痕量亚硝酸根的荧光分析法,方法的检出限为2.7ng/mL,线性范围为6.0-88ng/mL,可直接用于电厂废水、自来水、井水中亚硝酸根的测定。     

Urine drug testing for opioids,cocaine, and metabolites by direct injection liquid chromatography/tandem mass spectrometry

A sensitive and specific liquid chromatography/tandem mass spectrometry (LC/MS/MS) method for the simultaneous quantification of opioids, cocaine, and metabolites in urine was developed and validated. A 10-microL aliquot of urine was injected directly onto the LC/MS/MS system. The lack of sample preparation substantially reduced total analysis time. Separation was performed by reversed-phase chromatography with gradient elution for all analytes in 26 min. Atmospheric pressure chemical ionization (APCI) was a rugged and efficient ionization technique for basic drugs. Identification and quantification was based on selected reaction monitoring (SRM). Calibration, with deuterated internal standards, was performed by linear regression analysis (weighting factor 1/x). Limits of quantitation (LOQ) were established between 10-100 ng/mL and linearity was obtained up to a maximum of 10 000 ng/mL with an average correlation coefficient (R(2)) > 0.99. Analytical validation criteria for specificity, precision, accuracy, dilution integrity, matrix effect, and stability were fulfilled. The method proved to be simple and time efficient, and was applicable for illicit drug use monitoring and methadone treatment compliance in clinical research projects at the National Institute on Drug Abuse (NIDA).     

Separation and quantitation of hazardous wastes from abrasive blast media.

A sample of glass bead abrasive blasting material (ABM) waste, received from Robins Air Force Base (Georgia), was examined to determine whether the waste could be rendered nonhazardous by separating paint contaminants from the ABM. The sample was analyzed with size distribution and toxicity characteristics leaching procedure. A Microtrac analyzer was used to measure the size of fine particles (-325 Tyler mesh), and scanning electron microscopy analysis was performed to identify the nature of the contaminants in the ABM waste. Tests using froth flotation, magnetic separation, desliming, and acid washing were conducted to develop a process for removing the contaminants. A pilot plant test using the developed process rendered 82.1% or the ABM waste material nonhazardous.     

Determination of chelating agents in Hanford tank waste simulant by capillary zone electrophoresis

A capillary electrophoretic method has been developed which achieves rapid quantitative separation and determination of ethylenediaminetetraacetic acid, N-(2-hydroxyethyl)ethylenediaminetriacetic acid, diethylenetriaminepentaacetic acid, ethylenediaminediacetic acid, and nitrilotriacetic acid in Hanford tank waste simulant (TWS). Direct UV detection of Cu²⁺/chelator complexes is used to achieve enhanced sensitivity. The qualitative and quantitative reliability of the method and the quality of separations, as given by efficiency and resolution, is presented. In addition, the limits of detection and linearity of detector response with concentration are given for each chelator. The selection of Cu as the UV-absorbing species over other transition metals present in the waste is discussed.     

Development of fish gelatin-based artificial fish baits incorporating bioattractants from seafood processing waste

The study dealt with evolving an artificial fish bait by incorporating bioattractant concentrates derived from seafood processing wastes by enzymatic hydrolysis namely fish waste concentrate (FWC), squid waste concentrate (SWC), and shrimp processing concentrate (SPWC). They were characterized based on amino acid content and presence of different functional groups using FTIR. Among them, SWC was found to have the highest amino acid content of 60.85mg/100 mg followed by FWC (42.21mg/100 mg) and SPWC (24.82mg/100 mg). The developed artificial fish baits were subjected to protein leaching, solubility in seawater besides testing for acceptability by the red snapper. The study revealed that the bait incorporated with SWC at 3% level was found be the most ideal, with the protein leaching rate of 24.82 mg/g/h, solubility rate of 36.6 mg/g/h and the attractability score of 29/30. The amino acid leaching rate was 3.11 mg/h/100 mg and it was found to contain five amino acids such as glycine, proline, glutamic acid, alanine and serine. The study revealed that the hydrolyzed squid waste concentrate can be incorporated at 3% (w/w) with fish gelatin based biomatrix during gelation to prepare artificial bait.     

Degradation of chelating and complexing agents in an irradiated,simulated mixed waste

A simulant of an actual mixed waste was prepared and used to study organic degradation in nuclear wastes. Citric acid, ethylenediaminetetraacetic acid (EDTA), nitrilotriacetic acid (NTA) and N-(2-hydroxyethyl)ethylenediaminetriacetic acid (HEDTA) were added to an inorganic matrix, which contained no radionuclides. This simulated waste was then -irradiated in a⁶⁰Co-source up to 100 hours. The organics degraded exponentially at first, before tapering off; 80% had disappeared by 100 hours. Numerous degradation products (27 in all), mainly complexor and chelator fragments, ranging from small to complex species, were identified by gas chromatography/mass spectrometry. The waste's total organic content decreased with increasing radiation, indicating that radiolytic degradation is dispersive.     

P204-TBP浸渍树脂对硫酸介质中Sc3+的吸附行为研究及其应用

通过溶剂挥发法制备了含双萃取剂(TBP-P204)的浸渍树脂，利用静态法、动态法研究其在硫酸介质中对钪的吸附行为，测得静态吸附容量21．75mg／g，绘制了吸附等温线．应用于钛白废酸，用H2O2 H2SO4洗涤铁、钛，4％HCl洗脱钪，可实现钪和铁、钛的完全分离,钪的回收率96．2％。     

Acetone–Butanol–Ethanol Production from Waste Seaweed Collected from Gwangalli Beach,Busan, Korea,Based on pH-Controlled and Sequential Fermentation Using Two Strains

The optimal conditions for acetone–butanol–ethanol (ABE) production were evaluated using waste seaweed from Gwangalli Beach, Busan, Korea. The waste seaweed had a fiber and carbohydrate, content of 48.34%; these are the main resources for ABE production. The optimal conditions for obtaining monosaccharides based on hyper thermal (HT) acid hydrolysis of waste seaweed were slurry contents of 8%, sulfuric acid concentration of 138 mM, and treatment time of 10 min. Enzymatic saccharification was performed using 16 unit/mL Viscozyme L, which showed the highest affinity (K_m?=?1.81 g/L). After pretreatment, 34.0 g/L monosaccharides were obtained. ABE fermentation was performed with single and sequential fermentation of Clostridium acetobutylicum and Clostridium tyrobutyricum; this was controlled for pH. A maximum ABE concentration of 12.5 g/L with Y_ABE 0.37 was achieved using sequential fermentation with C. tyrobutyricum and C. acetobutylicum. Efficient ABE production from waste seaweed performed using pH-controlled culture broth and sequential cell culture.