Determination of 241Pu in nuclear waste slurries: a comparative study using LSC and ICP-MS.

(241)Pu was determined in slurry samples from a nuclear reactor decommissioning project at the Paul Scherrer Institute (Switzerland). To validate the results, the (241)Pu activities of five samples were determined by LSC (TriCarb and Quantulus) and ICP-MS, with each instrument at a different laboratory. In lack of certified reference materials for (241)Pu, the methods were further validated using the (241)Pu information values of two reference sediments (IAEA-300 and IAEA-384). Excellent agreement with the results was found between LSC and ICP-MS in the nuclear waste slurries and the reference sediments.

CO2 sparging for improving the filtration properties of iron ore slurries

Iron ore treatment processes are usually continuous and high tonnage and filtration equipment has to meet these requirements. In magnetite (Fe3O4) treatment process continuous rotary disc filters are often used for filtration. Carbon dioxide (CO2) treatment is a fairly novel and un-known filtration enhancing process. The interest to use CO2 is quite high because CO2 is a greenhouse gas that is abundant, readily available and capture and use of CO2 would be environmentally beneficial. The focus of this thesis was to investigate if CO2 could be used to enhance the filtration of magnetite with ceramic disc filter. Previous studies have suggested that CO2 could be used to enhance the filtration properties of different iron ores thus increasing the filtration capacity. In the literature part, the basic theory of filtration and the particle properties affecting filtration were discussed. The basic steps of a typical ore treatment process were presented. The reasons why CO2 might enhance the filtration properties of different ores were investigated. A literature survey of earlier studies of CO2 addition as a filter aid was presented and the basic chemical properties and reactions of CO2 were also discussed. The experimental part was done at the LUT Laboratory of Separation Technology using different magnetite samples from the industry. The filtration experiments indicated that CO2 had a positive influence on the filtration properties of magnetite slurry. Zeta potential of untreated and CO2 treated magnetite was measured and CO2 treated magnetite had lower zeta potential values than the untreated magnetite. The filtration capacity was increased while the cake moisture levels were only slightly increased.

Application of biogas slurries from energy crops to arable soils and their impact on carbon and nitrogen dynamics

The use of renewable primary products as co-substrate or single substrate for biogas production has increased consistently over the last few years. Maize silage is the preferential energy crop used for fermentation due to its high methane (CH4) yield per hectare. Equally, the by-product, namely biogas slurry (BS), is used with increasing frequency as organic fertilizer to return nutrients to the soil and to maintain or increase the organic matter stocks and soil fertility. Studies concerning the application of energy crop-derived BS on the carbon (C) and nitrogen (N) mineralization dynamics are scarce. Thus, this thesis focused on the following objectives: I) The determination of the effects caused by rainfall patterns on the C and N dynamics from two contrasting organic fertilizers, namely BS from maize silage and composted cattle manure (CM), by monitoring emissions of nitrous oxide (N2O), carbon dioxide (CO2) and CH4 as well as leaching losses of C and N. II) The investigation of the impact of differences in soil moisture content after the application of BS and temperature on gaseous emissions (CO2, N2O and CH4) and leaching of C and N compounds. III) A comparison of BS properties obtained from biogas plants with different substrate inputs and operating parameters and their effect on C and N dynamics after application to differently textured soils with varying application rates and water contents. For the objectives I) and II) two experiments (experiment I and II) using undisturbed soil cores of a Haplic Luvisol were carried out. Objective III) was studied on a third experiment (experiment III) with disturbed soil samples. During experiment I three rainfall patterns were implemented including constant irrigation, continuous irrigation with periodic heavy rainfall events, and partial drying with rewetting periods. Biogas slurry and CM were applied at a rate of 100 kg N ha-1. During experiment II constant irrigation and an irrigation pattern with partial drying with rewetting periods were carried out at 13.5°C and 23.5°C. The application of BS took place either directly before a rewetting period or one week after the rewetting period stopped. Experiment III included two soils of different texture which were mixed with ten BS’s originating from ten different biogas plants. Treatments included low, medium and high BS-N application rates and water contents ranging from 50% to 100% of water holding capacity (WHC). Experiment I and II showed that after the application of BS cumulative N2O emissions were 4 times (162 mg N2O-N m-2) higher compared to the application of CM caused by a higher content of mineral N (Nmin) in the form of ammonium (NH4+) in the BS. The cumulative emissions of CO2, however, were on the same level for both fertilizers indicating similar amounts of readily available C after composting and fermentation of organic material. Leaching losses occurred predominantly in the mineral form of nitrate (NO3-) and were higher in BS amended soils (9 mg NO3--N m-2) compared to CM amended soils (5 mg NO3--N m-2). The rainfall pattern in experiment I and II merely affected the temporal production of C and N emissions resulting in reduced CO2 and enhanced N2O emissions during stronger irrigation events, but showed no effect on the cumulative emissions. Overall, a significant increase of CH4 consumption under inconstant irrigation was found. The time of fertilization had no effect on the overall C and N dynamics. Increasing temperature from 13.5°C to 23.5°C enhanced the CO2 and N2O emissions by a factor of 1.7 and 3.7, respectively. Due to the increased microbial activity with increasing temperature soil respiration was enhanced. This led to decreasing oxygen (O2) contents which in turn promoted denitrification in soil due to the extension of anaerobic microsites. Leaching losses of NO3- were also significantly affected by increasing temperature whereas the consumption of CH4 was not affected. The third experiment showed that the input materials of biogas plants affected the properties of the resulting BS. In particular the contents of DM and NH4+ were determined by the amount of added plant biomass and excrement-based biomass, respectively. Correlations between BS properties and CO2 or N2O emissions were not detected. Solely the ammonia (NH3) emissions showed a positive correlation with NH4+ content in BS as well as a negative correlation with the total C (Ct) content. The BS-N application rates affected the relative CO2 emissions (% of C supplied with BS) when applied to silty soil as well as the relative N2O emissions (% of N supplied with BS) when applied to sandy soil. The impacts on the C and N dynamics induced by BS application were exceeded by the differences induced by soil texture. Presumably, due to the higher clay content in silty soils, organic matter was stabilized by organo-mineral interactions and NH4+ was adsorbed at the cation exchange sites. Different water contents induced highest CO2 emissions and therefore optimal conditions for microbial activity at 75% of WHC in both soils. Cumulative nitrification was also highest at 75% and 50% of WHC whereas the relative N2O emissions increased with water content and showed higher N2O losses in sandy soils. In summary it can be stated that the findings of the present thesis confirmed the high fertilizer value of BS’s, caused by high concentrations of NH4+ and labile organic compounds such as readily available carbon. These attributes of BS’s are to a great extent independent of the input materials of biogas plants. However, considerably gaseous and leaching losses of N may occur especially at high moisture contents. The emissions of N2O after field application corresponded with those of animal slurries.

Study of Monoethanolamine Nitrate Content Reduction in Explosive Slurries

The reduction of the fuel content of a monoethanolamine nitrate (MEAN) fueled explosive slurry was investigated. The work was performed in three phases. The first one involved the MEAN content reduction in a reference slurry from its initial value of 36 down to 24% by weight, the balance being filled with ammonium nitrate, the least expensive item in the slurry composition. This proved to be successful, leading to an overall cost reduction of 17%, while keeping the overall performance quite satisfactory. The second phase consisted in trying to bring the MEAN content down from 24 to 17%. Although this led to further cost reduction, the formulations, obtained by substituting part of the MEAN content by ammonium nitrate/fuel oil (ANFO), produced unsatisfactory results regarding ignition and densities. In the third phase, the Design of Experiments Technique was used to find formulations displaying not only lower cost, but also acceptable overall performance. This led to a raw material cost reduction ranging from 23 to 26% relative to the initial reference slurry formulation.

Determination of selenium by GFAAS in slurries of fish feces to estimate the bioavailability of this micronutrient in feed used in pisciculture

This paper presents a simple, fast and sensitive method to determine selenium in samples of feces and of fish feed by graphite furnace atomic absorption spectrometry (GFAAS) through the direct introduction of slurries of the samples into the spectrometer's graphite tube. The limits of detection (LOD) and quantification (LOQ calculated for 20 readings of the blank of the standard slurries (0.50% m/v of feces or feed devoid of selenium) were 0.31 mu g 1(-1) and 1.03 mu g 1(-1), respectively, for the standard feces slurries and 0.35 mu g 1(-1) and 1.16 mu g 1(-1), respectively, for the standard feed slurries. The proposed method was applied in studies of bioavailability of selenium in different fish feeds and the results proved consistent with that obtained from samples mineralized by acid digestion using the microwave oven. (C) 2007 Elsevier Ltd. All rights reserved.

Determination of chromium by GFAAS in slurries of fish feces to estimate the apparent digestibility of nutrients in feed used in pisciculture

This paper presents a simple, fast and sensitive method to determine chromic oxide (used as a biological marker of fish feed) in samples of fish feces by GFAAS through the direct introduction of slurries of the samples into the spectrometer's graphite tube. The standard samples of feces and of fish feed containing 0.10-1.00 mg kg(-1) of Cr2O3 were pre-frozen for I min in liquid nitrogen and then ground a cryogenic mill for 2 min, which reduced the samples' grain size to less than 60 mu m. The standard slurries were prepared by mixing 20 mg of standard samples of fish feed or feces with I mL of a solution containing 0.05% (v/v) of Triton X-100 and 0.50% (v/v) of suprapure HNO3 directly in the spectrometer's automatic sampling glass. The final concentrations of Cr2O3 present in the standard slurries were 2, 4, 8, 16 and 20 mu g L-1. After sonicating the mixture for 20s, 10 mu L of standard slurries were injected into the graphite tube, whose internal wall was lined with a metallic palladium film that acted as a permanent chemical modifier. The limits of detection (LOD) and quantification (LOQ) calculated for 20 readings of the blank of the standard slurries (2%, m/v of feces or feed devoid of minerals) were 0.81 and 2.70 mu g L-1 of Cr2O3 for the standard feces slurries, 0.84 and 2.83 mu g L-1 of Cr2O3 for the standard feed slurries. The proposed method was applied in studies of nutrient digestibility of different fish feeds and its results proved compatible with the results obtained from samples pre-mineralized by acid digestion. (c) 2005 Elsevier B.V. All rights reserved.

Effect of modifiers on thermal behaviour of Se in acid digestates and slurries of vegetables by graphite furnace atomic absorption spectrometry

The influence of sample preparation strategy of vegetables on the electrothermal behaviour of Se without and with chemical modifiers such as Pd(NO3)(2), Pd(NO3)(2) + Mg(NO3)(2), Pd(NO3)(2) + Cd(NO3)(2), pre-reduced Pd, Mg(NO3)(2), and Ni(NO3)(2) was investigated. Acid digestates and slurries of vegetables (0.1% m/v in 1% m/v HNO3 + 0.005% v/v of Triton X-100) were used to prepare reference solutions or slurries. For 10 mul of each modifier tested, pyrolysis and atomization temperatures were evaluated using pyrolysis and atomization curves, respectively. Best conditions, such as thermal stability, signal profile, repeatability and sensitivity were attained using Pd(NO3)(2) as chemical modifier. The following heating program (temperature, ramp/hold time) of the graphite tube of the Varian SpectrAA-800Z atomic absorption spectrometer was used: dry step (85 degreesC, 5/0 s; 95 degreesC, 40/0 s; 120 degreesC, 10/.5 s); pyrolysis step (1400 degreesC, 10/3s); atomization step (2200 degreesC, 1/2 s); clean step (2600 degreesC, 2/0 s). This pyrolysis temperature is 800 degreesC higher than when measuring without any modifier. For 20 muL sample volume and 10 mug Pd(NO3)(2), analytical curves in the 3.0-30 mug Se 1(-1) range were obtained. The method was applied for Se determination in acid digestates and slurries of 10 vegetable samples and one standard reference material (rice flower) and results were in agreement at 95% confidence level. Recoveries varied from 89 to 95% for spiked samples. The lifetime of the graphite tube was ca. 250 firings and the relative standard deviations (n = 12) for a typical acid digestate and slurry containing 20 mug Se 1(-1) were 3.8% and 8.3%, respectively. The limits of detection were 2.0 mug Se 1(-1) and 0.6 mug Se 1(-1) Se for digestates and slurries, respectively. (C) 2002 Elsevier B.V. Ltd. All rights reserved.

Determination of vanadium in human hair slurries by electrothermal atomic absorption spectrometry

This work describes an analytical procedure for vanadium determination in human hair slurries by electrothermal AAS using longitudinal heating (LHGA) and transversal heating (THGA) graphite furnace atomizers. The samples were powdered using cryogenic grinding and the hair slurries containing 0.2% (m/v) were prepared in three different media for determination of vanadium: 0.14 mol L-1 HNO3, 0.1% (v/v) Triton X-100 and 0.1% (v/v) water soluble tertiary amines (CFA-C, pH 8). The limits of detection (LOD), limits of quantification (LOQ), and characteristic masses obtained were 0.28, 0.95 mu g L-1 and 35 pg (LHGA) and 0.34, 1.13 mu g L-1 and 78 pg (THGA), respectively. The accuracy of the analytical results obtained by the proposed procedure in both equipments was confirmed by a paired t-test at the 95% confidence level and compared with a conventional procedure based on acid digestion. (c) 2006 Elsevier B.V. All rights reserved.

Analysis of cement slurries by inductively coupled plasma optical emission spectrometry with axial viewing

The feasibility of Portland cement analysis by introduction of slurries in an inductively coupled plasma optical emission spectrometer (ICP-OES) with axial viewing has been evaluated. After a fast manual grinding of the cement samples, owing to the pulverized state of this material, 0.1% m/v slurries were prepared in 1% v/v HCl. The calibration was performed adopting two strategies: one based on slurries prepared from different masses (50, 75, 100 and 125 mg) of a Portland cement standard reference material (NIST SRM 1881), and the other one based on aqueous reference solutions. A complete analysis of cement for major (Al, Ca, Fe, Mg and Si), minor and trace elements (Mn, P, S, Sr and Ti) was accomplished. Both strategies led to accurate results for commercial Portland cement samples, except for Si and Ti. for which the calibration with aqueous reference solutions resulted in low values. Applying a paired t-test it was shown that most results were in agreement at a 95% confidence level with a conventional fusion decomposition procedure. The ICP-OES with axial viewing and end-on gas configuration for removal of the recombination plasma zone was effective for cement slurry analysis without any undesirable particle deposition in the pre-optics interface and without severe spectral interferences. (C) 2002 Elsevier B.V. B.V. All rights reserved.

Manganese determination by GFAAS in feces and fish feed slurries

This paper presents a simple, fast and sensitive method to determine manganese in samples of feces and fish feed by graphite furnace atomic absorption spectrometry (GFAAS) by the direct introduction of slurries into the graphite tube. The limits of detection (LOD) and quantification (LOQ) calculated for 20 readings of the blank of the standard slurries (0.50 % m/v of feces or feed devoid of manganese) were 28 and 92 μg kg-1 for the standard feces slurries and 34 and 110 μg kg-1 for the standard feed slurries. The proposed method was applied in bioavailability studies of manganese in different fish feeds and their results proved compatible with those obtained for samples mineralized by acid digestion using microwave oven. ©2007 Sociedade Brasileira de Química.

The effect of slurry composition on methane potential emissions from fattening pig slurries: a review of three nutrition assays

This study reviews the effects of pig slurry composition on the biochemical methane (CH4) potential (B0), using the information collected in three nutrition assays. A total of 84 animals were used to test the effect of 13 different diets.

Development of a modified char adsorbent for the recovery of uranium from ore slurries : summary report /

"Western Laboratories ; Arthur D. Little, Inc ; San Francisco, Calif."

Drying of portland cement raw material slurries:predicting the performance of a counter-current spray drier

An extensive review of literature has been carried out concerning the drying of single drops, sprays of droplets and the prediction of spray drier performances. The experimental investigation has been divided into two broad parts mainly: (1) Single Drop Experiments, and (2) Spray Drying and Residence Time Distribution Experiments. The thermal conductivity of slurry cakes from five different sources have been experimentally determined using a modified Lee's Disc Apparatus and the data collected was correlated by the polynominal... Good agreement was observed between the experimental thermal conductivity values and the predicted ones. The fit gave a variance ... for the various samples experimented on. A mathematical model for estimating crust mass transfer coefficient at high drying temperatures was derived.