Mild hydrotreating over NiMo/sepiolite catalyst

Summary In order to introduce an alternative catalyst for hydrotreating (HDT) reaction a study of NiMo supported on natural sepiolite catalysts is presented. The sepiolite catalyst has been prepared in this laboratory and a NiMo/Al₂O₃ commercial catalyst is used as a reference. The textural properties of the materials and their catalytic activity in hydrotreating (HDT) and hydrodesulfuration (HDS) using a FCC feed at 400-475°C and 50 MPa total pressure, have been evaluated. The support of the commercial catalyst is alumina containing mesopores. The sepiolite support is a hydrated magnesium phylosilicate containing micropores but with an open structure that confers the possibility to use it as a catalyst. The hydrotreating conversion (wt.% HDT) is defined here as the net hydrotreating conversion into products boiling below 380°C. For the commercial catalyst the wt.% HDT was only 5% higher than for the catalyst supported on sepiolite and the product selectivity was very similar. HDS conversion was 20% lower for the sepiolite supported catalyst. Taking into account these results the sepiolite is a suitable support of HDS catalysts.     

XPS study of molybdenum sulfide catalyst exposed to CO and H2

Amorphous MoS(3) (air-dried precipitate), crystalline MoS(2) (made in the laboratory under nitrogenous atmosphere), and commercial molybdenum disulfide catalysts have been investigated by X-ray photoelectron spectroscopy (XPS). The chemical species present on the surface and the S/Mo atomic ratios of laboratory catalysts were compared to those present on a commercial molybdenum disulfide catalyst before and after treatment with CO and H(2). Pretreatment of MoS(2) with CO followed by H(2) showed that CO was adsorbed on the surface with no change in the chemical oxidation state of Mo and S. However, the results indicated that CO was not adsorbed when the sequence of gas exposures was reversed.     

Embedded flow-batch system with electrochemical detection for the determination of lead in propolis samples

A lab-made prototype consisting of a potentiostat with a flow-batch system was designed and implemented under the commercial off the shelf paradigm. The prototype is light-weight and suitable for laboratory performance. Its performance was evaluated with linear sweep voltammetry (LSV) study of ferrocyanide/ferricyanide redox couple and the obtained results were comparable to that obtained with a commercial potentiostat. The system was applied in the determination of lead in propolis samples. For this purpose, bismuth film electrode by square wave anodic stripping voltammetry (SWASV) was employed. The obtained results were validated by atomic emission spectroscopy with inductively coupled plasma and very good agreement was obtained.     

On-line FT-MIR/NIR process analysis

FT-IR spectrometers designed for laboratory operation are generally not suited for plant production areas where ambient temperatures often exceed 120° F and noise levels are extremely high. The Nicolet Pro-IR 5 process FT-IR spectrometer can operate in hostile environments over the spectral range from 10 000 to 250 wavenumbers. We have evaluated the performance of this system using a set of commercial detergent samples and a wide range of gas mixtures. The detergent samples were simultaneously analyzed for twelve components using a sophisticated partial least-squares statistical analysis software package. The concentrations ranged from 0.1 to over 50 wt.-%, with water being the major component. A comparison will be made between the NIR and MIR results using flow-through ATR (attenuated total reflectance) and transmission cells.     

商品二氧化钛的光催化性能比较

以甲醛的光催化氧化反应为指标反应 ,对商品二氧化钛的光催化性能进行了对比研究 ,发现不同的商品二氧化钛 ,其光催化活性呈现较大的差异 .利用XPS ,XRD等手段研究了各种二氧化钛的表面物种和晶体结构 .探讨了影响二氧化钛光催化性能的各种因素     

Determination of glucosamine in raw materials and dietary supplements containing glucosamine sulfate and/or glucosamine hydrochloride by high-performance liquid chromatography with FMOC-Su derivatization: collaborative study

A collaborative study was conducted for determination of glucosamine in raw materials and dietary supplements containing glucosamine sulfate and/or glucosamine hydrochloride by high-performance liquid chromatography (HPLC) with N-(9-fluorenyl-methoxycarbonyloxy) succinimide (FMOC-Su) derivatization. Thirteen blind materials, one pair of which were duplicates, were tested by 12 collaborating laboratories. The test samples consisted of various commercial products, including tablets, capsules, drink mix, and liquids as well as raw materials, blanks, and those for spike recovery analyses. The tests with blank products and products spiked with glucosamine showed good specificity of the method. The average recoveries at spike levels of 100 and 150% of the declared amount were 99.0% with a relative standard deviation (RSD) of 2.1%, and 101% with an RSD of 2.3%, respectively. The test results between laboratories on each commercial product were reproducible with RSD values of no more than 4.0%, and the results were repeatable in the same laboratory with an average RSD of 0.7%. HorRat values ranged from 0.5 to 1.7 on both tests of spike recovery and reproducibility between laboratories on commercial products. The average determination coefficient of the calibration curves from the laboratories was 0.9995 with an RSD of 0.03%. All of the 12 collaborating laboratories succeeded in the study and none of their reported test results were outliers, partly indicating the robustness of the method. It is recommended that the method be accepted by AOAC INTERNATIONAL as Official First Action.     

Proficiency testing as a tool for assessing the medical and economic impact of laboratory results: The blood coagulation case

An international commercial proficiency testing scheme was used to evaluate the impact of laboratory results on clinical decisions. The affect on atrial fibrillation was chosen as a model with 16 Israeli laboratories participating in an international study. A Markov model was constructed to evaluate the impact of any inaccurate results on the clinical outcomes. From the proficiency test study and the Markov model, 13–21% of the results were inaccurate and would have yielded erroneous medical decisions.     

Near infrared spectroscopy in the study of polymorphic transformations

The potential of near infrared (NIR) spectroscopy for the characterization of polymorphs in the active principle of a commercial formulation prior to and after the manufacturing process was assessed. Polymorphism in active principles is extremely significant to the pharmaceutical industry. Polymorphic changes during the production of commercial pharmaceutical formulations can alter some properties of the resulting end-products. Multivariate curve resolution-alternating least squares (MCR-ALS) methodology was used to obtain the “pure” NIR spectrum for the active principle without the need to pretreat samples. This methodology exposed the polymorphic transformation of Dexketoprofen Trometamol (DKP) in both laboratory and production samples obtained by wet granulation. No polymorphic transformation, however, was observed in samples obtained by direct compaction. These results were confirmed using by X-ray powder diffractometry (XRD) and differential scanning calorimetry (DSC) measurements. Pure crystalline polymorphs of DKP were available in the laboratory but amorphous form was not, nevertheless the developed methodology allows the identification of amorphous and crystal forms in spite of the lack of pure DKP.     

聚偏氟乙烯微孔膜处理含铬(Ⅲ)水溶液的研究

采用自制聚偏氟乙烯（ＰＶＤＦ）微膜和商品ＰＶＤＦ膜对含铬（Ⅱ）水溶液进行了减压膜蒸馏分离实验研究。结果表明,两种膜的膜通量相接近,商品对铬的截留率达９０％以上,了膜性能参数和实验条件对膜通量和截留率的影响。     

Phase behavior of pseudoternary brine/alkane/alcohol-secondary alkanesulfonates systems

Dodecanesulfonates (isomer mixtures) have been synthesized by the process developed in our laboratory. First, pseudoternary phase diagrams of water or (brine) decane/dodecanesulfonates-butan-1-ol systems were drawn and compared with those of a commercial sample (Hostapur 60). In the presence of NaCl, a three-phase region (Winsor III) appears for the two systems, and is larger with the home-made surfactants. This region is interesting in enhanced oil recovery because it leads to very low interfacial tensions. Then, the behavior of the Winsor III region was investigated as a function of the alcohol/surfactant mass ratio (C/T). At a constant salinity (2.5 mass% NaCl) a value of 2 for C/T gives the best compromise for a larger WIII region with both systems. For this ratio, optimal salinity values of 1.55 and 1.65 mass% for our sample and Hostapur 60, were found, respectively.     

Gel Filtration of Model Albumin-Analgin Mixture through Sephadex To Isolate Albumin

The preparative isolation of albumin from a model albumin-analgin mixture by filtration through Sephadex G-25 was studied. The conditions providing optimal protein decontamination to remove low-molecular-weight impurities were established, and recommendations on both laboratory and industrial application of this technique were made. Based on laboratory experiments, a commercial installation for production of refined vaccines was designed.     

RESEARCH AND DEVELOPMENT OF FUEL ALCOHOL SYNTHESIS FROM SYNGAS

The research and development of catalyst preparation and catalytic technology for fuel alcohol synthesis from syngas have been conducted. The laboratory research work includes the investigation on the effects of preparation method, the composition and K2O content on the catalyst performance. The influences of reaction temperature, pressure, GHSV and feed composition on higher alcohols synthesis have also been investigated. On the basis of laboratory results, the catalysts have been further tesied in micro-pilot reactor under the industrial condition to investigate the effects of commercial preparation of catalyst, the reactor scaling up and (he use of industrial coal based syngas on the fuel alcohol ( mixture of methanol and higher alcohols ) synthesis. The catalyst stability has been tested by a 1000 h continuous operation. These provide the fundamental for further commercial plant design.     

Enthalpy of solution of α-cyclodextrin in water and in formamide at 298.15 K

A new dissolution microcalorimeter that can measure enthalpies of dissolution of slightly soluble solids was developed by Ingemar Wadsö at Lund University, and the prototype as well as the commercial vessel were tested in our laboratory. Recently we did report the testing of the prototype and we are now extending the previous investigation to measurements with an organic solvent in the commercial vessel. The instrument performance was found to be as good with formamide as with water.The vessel was calibrated chemically (dissolution of KCl in water) and electrically, by means of a permanent and an insertion heater. The results obtained from the three methods are compared and discussed.The enthalpy of dissolution of α-cyclodextrin, dry and hydrated with six water molecules, was determined in water and in formamide. The results are discussed in terms of the difference between water and formamide as regarding dissolution and binding to the cyclodextrin molecule.     

Effect of vanadium over NiMo/sepiolite hydrotreating catalyst

Summary Hydrotreating (HDT) and hydrodesulfuration (HDS) using an FCC feed were carried out at 673-748 K and 50 MPa total pressure. The effect of vanadium impregnated on a NiMo catalyst supported on sepiolite for HDT and HDS reactions was studied. A commercial NiMo/Al₂O₃ catalyst was used as reference. The hydrotreating conversions (wt.% HDT) is defined here as the net hydrotreating conversion into products boiling below 653 K. The results were compared with an accelerated ageing test using the catalysts on a FCC feed, with vanadium in the form of naphthenate (2000 ppm of V) added to rapidly deactivate catalysts via metal deposition. The results indicate that vanadium affects more the catalyst supported on sepiolite that the commercial catalyst. Also, at our reaction conditions, the effect of vanadium on sepiolite catalyst is similar, to those used with vanadium impregnated on the catalyst or on the catalyst where the vanadium in naphthenate form was added to FCC feed.     

利用实验室间国际比对验证15N丰度的测定能力

参加了由FAO／IAEA组合的全氮和^15N丰度检测能力验证的实验室国际间的比对两年的比对结果表明,我们实验室对3个植株样品全氮和^15N丰度的测定值与指定值十分吻合,检测结果准确,此项计划的实施,证明了本实验室的检测能力和国际实验室间的水平。     

Use of Commercial Acrylonitrile Standard for Wastewater Analysis

Abstract

It was found that a commercially available aqueous standard solution of acrylonitrile (1 mg/ml) was below manufacturer specification in concentration when compared to an authentic standard prepared from the pure compound. Comparative analyses of the two solutions, commercial and laboratory prepared acrylonitrile, were conducted by gas chromatography using a flame ionization detector with analytical conditions similar to those recommended by the EPA for acrylonitrile analyses. The acrylonitrile content of the commercial solution was found to be approximately 30% lower than specified. Commercial venders have provided solutions of the 114 organic priority pollutants which are convenient for instrumental calibration. There needs to be concern for experimental results reported with regards to accuracy and estimated detection limit when using such standards.     

Thermal analysis: an effective characterization method of polyvinyl acetate films applied in corrosion inhibition field

Journal of Thermal Analysis and Calorimetry - To prepare a commercial product with economic and technical relevance, polyvinyl acetate (PVAc) was synthesized, under our laboratory conditions,...     

Syntheses of spherical silica and titania from alkoxides on a laboratory scale

Summary A process to synthesize silica and titania as spherical packing materials has been investigated on the laboratory scale by the sol-gel method. The silica and titania obtained were tested under normal-phase separation conditions for comparison of their retention characteristics silica witha a commercial. The silica was found to be similar in its retention behaviour to the commercial silica. The titania showed basic properties and strongly retained acidic compounds.     

A synthesis of N-alkyl and N,N-dialkyl O-ethyl thiocarbamates from diethyl dixanthogenate using different oxidants

Abstract  

A novel synthesis of N-alkyl and N,N-dialkyl O-ethyl thiocarbamates from diethyl dixanthogenate and primary and secondary amines, using three oxidizing systems, has been developed on the laboratory scale, and the method using sodium hypochlorite has been applied on a semi-industrial scale. The effect of the oxidizing agents, sodium hypochlorite, in-situ-generated peracetic acid, and the manganese(II) acetate/oxygen system on product purity and yield was studied. The results obtained by use of these three methods were compared with those obtained by reaction of sodium ethyl xanthogenacetate and amines, and of sodium ethyl xanthate with amines in the presence of sulfated nickel zeolite catalyst. The reaction mechanism of sodium hypochlorite oxidation has been established on the basis of isolation of reaction intermediates and determination of their structure by use of Fourier-transform infrared, ¹H and ¹³C NMR, and mass spectrometric methods. The suggested sodium hypochlorite and manganese(II) acetate/oxygen systems have many advantages in comparison with commercial and catalytically promoted synthetic methods, because they are new ecologically friendly syntheses.     

Nano-liquid chromatography and capillary electrochromatography hyphenated with mass spectrometry for tryptic digest protein analysis: A comparison

Nano-LC and CEC were studied for the separation of cytochrome c tryptic digest. The peptides mixture was analyzed using either a nano-LC commercial or a laboratory assembled instrumentation coupled with an IT-ESI-MS by using a nanospray interface. CEC experiments were carried out with a CE apparatus coupled with the IT-ESI-MS through a liquid junction interface. Analytes were separated utilizing C18 silica based stationary phases, of different properties and origin, silica derivatized with cyano groups and C18 monolithic material. The last column, just because the chemical composition (absence of charged/chargeable groups) was tested only using nano-LC. Best results mainly related to the highest number of peptides separated and column equilibration time were obtained by nano-LC employing the C18 stationary phase (detection of 20 peptides, coverage of 88%). Similar results were achieved using both commercial and laboratory assembled instrumentation. The use of CEC revealed a higher separation efficiency and shorter analysis time. However, the number of separated peptides were lower than those observed in nano-LC. In CEC the use of capillaries packed with cyanosilica particles offered better results; however, less satisfactory than those observed in the miniaturized LC technique. Provided the use of the same stationary phase and taking into account the driving forces, the two techniques can be considered complementary, offering different information related to the retention times of the studied peptides.