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1.
A new kinetic spectrophotometric method has been developed for the determination of iron (Ⅲ). The method is based on the catalytic effect of iron (Ⅲ) on the oxidation of weak acid brilliant blue dye (RAWL) by KIO4 in acid medium. The advantages of the proposed method are that it is sensitive, accurate, rapid, inexpensive, can be operated under room temperature and has a large determination concentration range compared to other techniques. The obtained optimum conditions are: pH 3.15, RAWL (200 mgL-1) 5.00mL, Potassium periodate solution (0.01 molL-1) 0.30mL, phenanthroline (0.02molL-1) 1.00mL, reaction temperature 25℃ and reaction time 7 miu. With this method iron could quantitively be determined in the range 0.00-0.02 mgL-1, the detection limit being 4.10×10-10mL-1. The relative standard deviations (RSD) in five replicate determinations for 3 μgL-1 and 5μgL-1 iron (Ⅲ) are 3.1% and 1.9%, respectively. The method has been applied to the determination of iron (Ⅲ) in tap water samples and seawater samples (from the South China Sea), the recovery rates being 98.0% and 100.5%, respectively.  相似文献   

2.
A new kinetic spectrophotometric method has been developed for the determination of iron (Ⅲ). The method is based on the catalytic effect of iron (Ⅲ) on the oxidation of weak acid brilliant blue dye (RAWL) by KIO4 in acid medium. The advantages of the proposed method are that it is sensitive, accurate, rapid, inexpensive, can be operated under room temperature and has a large determination concentration range compared to other techniques. The obtained optimum conditions are pH 3.15, RAWL (200 mgL-1) 5.00mL, Potassium periodate solution (0.01 molL-1) 0.30mL, phenanthroline (0.02molL-1) 1.00mL, reaction temperature 25℃ and reaction time 7 miu. With this method iron could quantitively be determined in the range 0.00-0.02 mgL-1, the detection limit being 4.10×10-10mL-1. The relative standard deviations (RSD) in five replicate determinations for 3 μgL-1 and 5μgL-1 iron (Ⅲ) are 3.1% and 1.9%, respectively. The method has been applied to the determination of iron (Ⅲ) in tap water samples and seawater samples (from the South China Sea), the recovery rates being 98.0% and 100.5%, respectively.  相似文献   

3.
A new kinetic spectrophotometric method has been developed for the determination of trace Ni (II) in natural water.The method is based on the catalytic effect of Ni (II) on the oxidation of weak acid brilliant blue dye (RAWL) by KIO4 in acid medium.The concentration of nickel (II) can be determined spectrophotometrically by measuring the decrease of absorbance of RAWL at λ= 626 nm using the fix-time method.The influencing factors are investigated by the orthogonal experimental design.The obtained optimum analytical conditions are:pH=2.00,c RAWL=5.00×10-5 mol L-1,cKIO 4= 2.00×10-5 mol L-1,the reaction time t=10 min and the temperature T=25℃..Under the optimum conditions,the developed method allows the measurement of Ni (II) in a range of 0-40.0 ng mL-1.The standard deviation of eleven independent measurements of blank reaction is S=3.08×10-3 and the limit of detection is 2.20 ng mL-1.The relative standard deviations (RSDs) in six replicate determinations of 5 ng mL-1 and 8 ng mL-1 Ni (II) are 2.87% and 1.11%,respectively.Moreover,the experiments show few cations and anions can interfere with the measurement of Ni (II).The recovery efficiencies of this method are in a range of 97.0%-102.5% in freshwater samples.But there is a decreasing effect,which is about 0.2 times the added Ni (II) in seawater medium.After reasonable calibration this processing method is used for the determination of Ni (II) in seawater samples successfully.The results show this developed method has high accuracy and precision,high sensitivity,large range of linearity and high speed.The method can,therefore,be employed at room temperature.  相似文献   

4.
A new kinetic spectrophotometric method has been developed for the determination of vanadium (Ⅴ).The method is based on the catalytic effect of vanadium (Ⅴ) on the oxidation of weak acid brilliant blue dye (RAWL) by KBrO3 using the citric acid as activation reagent.The obtained optimum conditions are:c (RAWL)=1×10-4 molL-1, c (KBrO3)=3×10-2 molL-1, c (citric acid)= 9×10-3 molL-1, pH=2.50, the reaction time being 7.0 min and the temperature being 25.0℃.Under the optimum conditions, the pro-posed method allows the determination of vanadium (Ⅴ) in the range of 0?70.0 ng mL-1 and the detection limit is down to 0.407 ng mL-1.For standard vanadium (Ⅴ) solution determination, the recovery efficiency is in the range of 98.5%?102% and the RSD ranges from 0.76%?1.25%.Moreover, it is demonstrated that most cations and anions do not interfere with the determination of vanadium (Ⅴ) under the analytical condition.The new method was successfully applied in the determination of vanadium (Ⅴ) in fresh water and seawater samples with satisfactory results.Vanadium (Ⅴ) in the seawater samples from Qingdao offshore was determined using the method and the distribution of vanadium (Ⅴ) was mapped.Compared with other instrumental analytical methods, the proposed method shows good selectivity, sensitivity, simplicity, lower cost and rapidity.It can be employed on shipboard easily.  相似文献   

5.
A highly sensitive and selective catalytic kinetic spectrophotometric method for the determination of Cu(Ⅱ) is proposed. It is based on the catalytic effect of Cu(Ⅱ) on the oxidation of glutathione(GSH) by potassium hexacyanoferrate(Ⅲ) in acidic medium at 25.0℃. The reaction is monitored spectrophotometrically by measuring the decrease in absorbance of oxidant at 420 nm using the fix-time method. Under the optimum conditions, the proposed method allows the determination of Cu(Ⅱ) in a range of 0-35.0 ng m L~(-1) with good precision and accuracy and the limit of detection is down to 0.04 ng m L~(-1). The relative standard deviation(RSD) is 1.02%. The reaction orders with respect to each reagent are found to be 1, 1/2, and 1/2 for potassium hexacyanoferrate(Ⅲ), glutathione and Cu(Ⅱ) respectively. On the basis of these values, the rate equation is obtained and the possible mechanism is established. Moreover, few anions and cations can interfere with the determination of Cu(Ⅱ). The new proposed method can be successfully used to the determination of Cu(Ⅱ) in fresh water samples and seawater samples. It is found that the proposed method has fairly good selectivity, high sensitivity, good repeatability, simplicity and rapidity.  相似文献   

6.
A new kinetic-spectrophotometric method is proposed for the determination of copper ( Ⅱ ). The method is based on the catalytic effect of copper ( Ⅱ ) on the oxidation of weak acid brilliant blue dye (RAWL) by hydrogen peroxide. The copper ( Ⅱ ) can be determined spectrophotometrically by measuring the decrease of absorbance of RAWL at λ = 626 nm using the fix-time method. The optimum reaction conditions are as follows: pH 7.20, buffer solution NaOH-KH2PO4, RAWL (200 mgL-1) 5.00 mL, H2O2 (30%) 0.50 mL, reaction temperature 80 ?? and reaction time 20 min. The linear range of this method is between 0 μg L^-1 and 12 μg L^-1 and the limit of detection is 0.011 μg L-1, the relative standard deviation (RSD) in five replicate determinations for 2 and 8 μg L-1 copper ( Ⅱ ) are 3.2% and 2.3%, respectively. Twenty ions do not interfere in the determination of copper ( Ⅱ ). The method has been applied satisfactorily to the determination of copper ( Ⅱ ) in freshwater samples (tap water and Yellow River water from Lijin, Shandong, China) and seawater samples (from the South China Sea), the recovery rates are 98.0%, 102.5% and 96.0%, respectively.  相似文献   

7.
A new analytical method using Back-Propagation (BP) artificial neural network and kinetic spectrophotometry for simultaneous determination of iron and magnesium in tap water, the Yellow River water and seawater is established. By conditional experiments, the optimum analytical conditions and parameters are obtained. Levenberg-Marquart (L-M) algorithm is used for calculation in BP neural network. The topological structure of three-layer BP ANN network architecture is chosen as 15-16-2 (nodes). The initial value of gradient coefficient μ is fixed at 0.001 and the increase factor and reduction factor of μ take the default values of the system. The data are processed by computers with our own programs written in MATLAB 7.0. The relative standard deviation of the calculated results for iron and manganese is 2.30% and 2.67% respectively. The results of standard addition method show that for the tap water, the recoveries of iron and manganese are in the ranges of 98.0%-104.3% and 96.5%-104.5%, and the RSD is in the range of 0.23%-0.98%; for the Yellow River water (Lijin district of Shandong Province), the recoveries of iron and manganese are in the ranges of 96.0%-101.0% and 98.7%-104.2%, and the RSD is in the range of 0.13%-2.52%; for the seawater in Qingdao offshore, the recoveries of iron and manganese are in the ranges of 95.3%-104.8% and 95.3%-104.7%, and the RSD is in the range of 0.14%-2.66%. It is found that 21 common cations and anions do not interfere with the determination of iron and manganese under the optimum experimental conditions. This method exhibits good reproducibility and high accuracy in the determination of iron and manganese and can be used for the simultaneous determination of iron and manganese in tap water and natural water. By using the established ANN- catalytic spectrophotometric method, the iron and manganese concentrations of the surface seawater at 11 sites in Qingdao offshore are determined and the level distribution maps of iron and manganese are drawn.  相似文献   

8.
SYNTHESIS AND PROPERTIES OF SULFHYDRYL CHITOSAN   总被引:1,自引:0,他引:1  
A new adsorbent for heavy metal ions, sulfhydryl chitosan (S-chitosan), was produced by treatment of chitosan with sulhydryl acetic acid in the presence of sulfuric acid as a catalyst. Its structure was confrrmed by elemental analysis and FI‘-IR spectra analysis. The adsorption properties of sulthydryl chitosan for Cu(Ⅱ ), Cd(Ⅱ ), Pb(Ⅱ), Cr(Ⅲ) and Ni(Ⅱ) were investigated, and the effect of pH value on adsorption, adsorption kinetics, and selective adsorption was examined. It was shown that S-chitosan has good adsorption for Pb(Ⅱ), Cu(Ⅱ) and Cd(Ⅱ) like chitosan, is also insoluble in acid solution; has good adsorption kinetic properties for heavy metal ions; and can be used in acid solution. The adsorption capacities of S-chitosan can be affected by media acidity. The adsorbed Cu(Ⅱ) Cd(Ⅱ) and Pb(Ⅱ) could be eluted by diluted chlorhydric acid.  相似文献   

9.
Ultrasound-assisted solvent extraction was confirmed as a novel,effective method for separating lipid from mackerel pro-tein,resulting in a degreasing rate (DR) of 95% and a nitrogen recovery (NR) of 88.6%.To obtain protein hydrolysates with high ni-trogen recovery and low bitter taste,enzymatic hydrolysis was performed using eight commercially available proteases.It turned out that the optimum enzyme was the ‘Mixed enzymes for animal proteolysis’.An enzyme dosage of 4%,a temperature of 50℃,and a hydrolysis time of 300 min were found to be the optimum conditions to obtain high NR (84.28%) and degree of hydrolysis (DH,16.18%) by orthogonal experiments.Glutamic acid was the most abundant amino acid of MDP (defatted mackerel protein) and MDPH (defatted mackerel protein hydrolysates).Compared with the FAO/WHO reference protein,the essential amino acid chemical scores (CS) were greater than 1.0 (1.0 1.7) in MDPH,which is reflective of high nutritional value.This,coupled with the light color and slight fishy odor,indicates that MDPH would potentially have a wide range of applications such as nutritional additives,functional ingredients,and so on.  相似文献   

10.
The East China Sea(ECS) has a high suspended-sediment concentration because of the influence of the Changjiang River,indicated by high turbidity in the water.Considering the islands off the coast and the complex topography,and the strong influence of tides and wind,the coast off the ECS is a typical region with strong oceanic mixing processes.The changes in the dynamic processes near the bottom play an important role in the control of water turbidity.The turbulent kinetic energy dissipation rate(ε) is a parameter that shows the strength of ocean mixing.This is estimated based on a structure method using current velocity that is measured by a high-frequency Acoustic Doppler Current Profiler(ADCP) from a seafloor observatory in the ECS.The results indicate strong ocean mixing processes with a mean e value of 5.7×10~(-5) W/kg and distinct tidal variations in the dissipation rate.Conversely,the variation of the water turbidity leads to changes in the water dynamical structure near the bottom.Comparing the dissipation rate with the turbidity near the bottom boundary layer,we find that the high turbidity mimics strong ocean mixing.  相似文献   

11.
Okadaic acid(OA)is a typical marine toxin with strong toxicity causing diarrheic shellfish poisoning(DSP).Aptamers show great advantages in toxin detection and attract increasing attentions in the field of food analysis.In this study,a label-free col-orimetric aptasensor was constructed for visual and rapid detection of OA in shellfish.To exploit the binding capability of the anti-OA aptamer,the inherent molecular recognition mechanism of aptamer and OA was studied,based on molecular docking,fluorescent assay,and biolayer interferometry.Consistent results showed that the stem-loop near the 3’terminal of the aptamer exhibit dominate binding capacity.Based on the revealed recognition information,the aptamer was thus rationally utilized and combined with AuNPs and cationic polymer polydiallyl dimethyl ammonium chloride(PDDA)for the development of the label-free colorimetric aptasensor,in which the 3’terminal was thoroughly exposed to OA.The aptasensor provided robust performance with a linear detection range of 100-1200 nmol L-1,a limit of detection of 41.30 nmol L-1,recovery rates of 91.6%-106.2%,as well as a high selectivity towards OA in shellfish samples.The whole detection process can be completed within 1 h.To our best knowledge,this is the first time that the anti-OA aptamer was thoroughly studied,and a label-free colorimetric aptasensor was rationally designed in this way.This study not only provides a rapid detection method for highly sensitive and specific detection of OA,but also serves as a reference for the design of efficient aptasensors in the future.  相似文献   

12.
A new analytical method using Back-Propagation(BP) artificial neural networks and spectrophotometry for simultaneous determination of calcium and magnesium in tap water,the Yellow River water and seawater is established.By condition experiment,the optimum analytical conditions for calcium,magnesium and Arsenazo(Ⅲ) color reactions are obtained.Levenberg-Marquart(L-M) algorithm is used for calculation in BP neural network.The topological structure of three-layer BP ANN network architecture is chosen as 11-10-2(nodes).The initial value of gradient coefficient μ is fixed at 0.001 and the increase factor and reduction factor of μ take the default values of the system.The data are processed by computers with our own programs written in MATLAB 7.0.The relative standard deviations of the calculated results for calcium and magnesium are 2.31% and 2.14%,respectively.The results of standard addition method show that the recoveries of calcium and magnesium are 103.6% and 100.8% in the tap water,103.2% and 96.6% in the Yellow River water(Lijin district of Shandong Province),and 98.8%-103.3% and 98.43%-103.4% in seawater from Jiaozhou Bay of Qingdao.It is found that 14 common cations and anions do not interfere with the determination of calcium and magnesium under the optimum experimental conditions.The comparative experiments do not show any obvious difference between the results obtained by this new method and those obtained by the classical complexometric titration method in seawater medium.This method exhibits good reproducibility and high accuracy in the determination of calcium and magnesium and can be used for the simultaneous determination of Ca2+ and Mg2+ in tap water and natural water.  相似文献   

13.
A method for the analysis of selenium in marine aquatic products by HG-AFS has been investigated. The method is based on the reduction of inorganic selenium to volatile SeH2 which is bubbled out by carrier gas of pure argon, and then swept to Ar-H2 flame quarts atomizer to measure its fluorescence intensity. The hydride generation, transportation, atomization and some instrumental parameters were studied by a kind of orthogonal design. The optimum conditions selected are as follows: reactive acidity, 20% HC1; the amount of NaBH4, 4.9mL; gas flow of argon, 600mLmin^-1; atomizing temperature, 200 ℃ ; negative high voltage, - 300V; light current, 100 mA; integral time, 7s. The detection limit of the presented method is 0.072μgL^-1 for selenium. The calibration curve shows a satisfactory line inthe concentration range from 0.000 to 1.000μgL^-1 Se. The recovery is 95.8%-102.2%.  相似文献   

14.
A novel method for on-site determination of trace iron was developed using membrane preconcentration and spectrophotometric detection. Fe(Ⅱ)-ferrozine complex was reacted with cetyltrimethylammonium bromide (CTAB) to form a Fe(Ⅱ)-ferrozine-CTAB paired compound, which was collected on a membrane by filtration under vacuum. The membrane was immersed in 2 mL of ethanol-nitric acid and the absorbance of the solution measured for quantitative analysis. Various factors affecting the iron collection and determination were investigated. With different sample preconcentration volumes, the range of determination was broadened to 0.5-120 g/L. The detection limit of this method reached 0.19 g/L and the recoveries were between 97.2 and 109% when the concentration enrichment was about 45. The relative standard deviation (n = 7) was 1.9% for samples containing 10 g/L Fe. Twelve seawater samples were analyzed on-site using the proposed method, and two were also analyzed in inductively coupled plasma mass spectrometry. No significant difference was shown between the two methods by the Student’s t-test. The method has also been used on-site for iron enrichment experiments with phytoplankton and concluded to be simple, accurate and inexpensive.  相似文献   

15.
Reversible protein phosphorylation, catalyzed by protein kinases and phosphatases, is an important and versatile mechanism by which eukaryotic cells regulate almost all the signaling processes. Protein phosphatase 1 (PP1) is the first and well-characterized member of the protein serine/threonine phosphatase family. In the present study, a full-length cDNA encoding the beta isoform of the catalytic subunit of protein phosphatase 1(PP1cb), was for the first time isolated and sequenced from the skin tissue of flatfish turbot Scophthalmus maximus, designated SmPP1cb, by the rapid amplification of cDNA ends (RACE) technique. The cDNA sequence of SmPP1cb we obtained contains a 984 bp open reading frame (ORF), flanked by a complete 39 bp 5' untranslated region and 462 bp 3' untranslated region. The ORF encodes a putative 327 amino acid protein, and the N-terminal section of this protein is highly acidic, Met-Ala-Glu-Gly-Glu-Leu-Asp-Val-Asp, a common feature for PP1 catalytic subunit but absent in protein phosphatase 2B (PP2B). And its calculated molecular mass is 37 193 Da and pI 5.8. Sequence analysis indicated that, SmPP1cb is extremely conserved in both amino acid and nucleotide acid levels compared with the PP1cb of other vertebrates and invertebrates, and its Kozak motif contained in the 5'UTR around ATG start codon is GXXAXXGXXATGG, which is different from mammalian in two positions A-6 and G-3, indicating the possibility of different initiation of translation in turbot, and also the 3'UTR of SmPP1cb is highly diverse in the sequence similarity and length compared with other animals, especially zebrafish. The cloning and sequencing of SmPP1cb gene lays a good foundation for the future work on the biological functions of PP1 in the flatfish turbot.  相似文献   

16.
Radiocarbon(14C) measurement of dissolved organic carbon(DOC) is a very powerful tool to study the sources, transformation and cycling of carbon in the ocean. The technique, however, remains great challenges for complete and successful oxidation of sufficient DOC with low blanks for high precision carbon isotopic ratio analysis, largely due to the overwhelming proportion of salts and low DOC concentrations in the ocean. In this paper, we report an effective UV-Oxidation method for oxidizing DOC in natural waters for radiocarbon analysis by accelerator mass spectrometry(AMS). The UV-oxidation system and method show 95%± 4% oxidation efficiency and high reproducibility for DOC in both river and seawater samples. The blanks associated with the method was also low(about 3 μg C) that is critical for 14 C analysis. As a great advantage of the method, multiple water samples can be oxidized at the same time so it reduces the sample processing time substantially compared with other UV-oxidation method currently being used in other laboratories. We have used the system and method for 14 C studies of DOC in rivers, estuaries, and oceanic environments and have received promise results.  相似文献   

17.
Shapai Roller Compacted Concrete(RCC) Arch Dam is the highest RCC arch dam of the 20th century in the world with a maximum height of 132m,and it is the only concrete arch dam near the epicentre of Wenchuan earthquake on May 12th,2008.The seismic damage to the dam and the resistance of the dam has drawn great attention.This paper analyzed the response and resistance of the dam to the seismic wave using numerical simulations with comparison to the monitored data.The field investigation after the earthquake and analysis of insitu data record showed that there was only little variation in the opening size at the dam and foundation interface,transverse joints and inducing joints before and after the earthquake.The overall stability of the dam abutment resistance body was quite good except a little relaxation was observed.The results of the dynamic finite element method(FEM) showed that the sizes of the openings obtained from the numerical modeling are comparable with the monitored values,and the change of the opening size is in millimeter range.This study revealed that Shapai arch dam exhibited high seismic resistance and overload capacity in the Wenchuan earthquake event.The comparison of the monitored and simulated results showed that the numerical method applied in this paper well simulated the seismic response of the dam.The method could be useful in the future application on the safety evaluation of RCC dams.  相似文献   

18.
Myosin subfragment-1 was prepared from the myofibrils of bighead carp (Aristichthys nobilis). The myosin subfrag- ment-1 was proved to have the activity of tripolyphosphatase (TPPase) responding to the hydrolysis of sodium tripolyphosphate (STPP). The optimum temperature and pH for the TPPase of myosin subfragment-1 were 30℃ and pH 5.0, and at pH 8.0 the TPPase also showed a high activity. Mg2 was necessary to TPPase. The TPPase activity of myosin subfragment-1 was activated by Mg2 under low concentrations, but was inhibited when the concentration was over 17 mmolL-1. The TPPase activity was also affected by KCl. The optimum concentration of KCl for TPPase was 0.3 molL-1 under the condition of 17 mmolL-1 Mg2 . The TPPase activity was significantly inhibited by EDTA-Na2. Reagents such as KBr, KI and KIO3 could inhibit the TPPase effectively. K2Cr2O7 as well as KMnO7 and KNO3 exhibited weak inhibiting effects. The TPPase converted STPP to pyrophosphate (PP) and orthophosphate (Pi) stoichiometrically with a KM of 3.2 mmolL-1.  相似文献   

19.
Among pharmaceuticals and personal care products released into the aquatic environment, antibiotics are of particular concern, because of their ubiquity and health effects. Although scientists have recently paid more attention to the threat of antibiotics to coastal ecosystems, researchers have often focused on relatively few antibiotics, because of the absence of suitable analytical methods. We have therefore developed a method for the rapid detection of 36 antibiotic residues in coastal waters, including tetracyclines (TCs), sulfanilamides (SAs), and quinolones (QLs). The method consists of solid-phase extraction (SPE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis, using electrospray ionization (ESI) in positive mode. The SPE was performed with Oasis HLB and Oasis MCX cartridges. Chromatographic separation on a C18 column was achieved using a binary eluent containing methanol and water with 0.1% formic acid. Typical recoveries of the analytes ranged from 67.4% to 109.3% at a fortification level of 100 ng/L. The precision of the method, calculated as relative standard deviation (RSD), was below 14.6% for all the compounds. The limits of detection (LODs) varied from 0.45 pg to 7.97 pg. The method was applied to determine the target analytes in coastal waters of the Yellow Sea in Liaoning, China. Among the tested antibiotics, 31 were found in coastal waters, with their concentrations between the LOD and 212.5 ng/L. These data indicate that this method is valid for analysis of antibiotics in coastal waters. The study first reports such a large number of antibiotics along the Yellow Sea coast of Liaoning, and should facilitate future comprehensive evaluation of antibiotics in coastal ecosystems.  相似文献   

20.
Based on the principle of conservative matter removal in estuary,a new method is proposed for estimating the ratio of sediment resuspension in estuaries with fine suspended sediments in the turbidity maximum zone(TMZ) of the Changjiang(Yangtze) estuary during 2005.Results show that there was a range of 18.7%±27.9% to 73.9%±22.5% per annum of total suspended particulate matter(SPM),with an average of 49.2%.Nearly half of the particulate matter in the TMZ originates from sediment resuspension.This indicates that sediment resuspension is one of the major mechanisms involved in formation of the TMZ.Compared with traditional method for calculating these ratios in the estuary,this new method evaluates the dynamic variation of SPM content carried by river runoff from the river mouth to the ocean.The new method produced more reliable results than the traditional one and could produce a better estimation of resuspension flux for particulate matter in estuaries.  相似文献   

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