127 results about "Atomic fluorescence spectrometry" patented technology

The invention discloses an electro-thermal vaporization atomic fluorescence spectrometry method and a spectrometer used for determining cadmium. An atomizer of the electro-thermal vaporization atomic fluorescence spectrometer comprises an atomizing apparatus and a collecting trap. The collecting trap is composed of a tungsten filament or a molybdenum filament, a support, a housing and a power source. A sealed space is formed by the housing and the support. The tungsten filament or the molybdenum filament is arranged on the support. The tungsten filament or the molybdenum filament is positioned in the sealed space formed by the housing and the support. An inlet and an outlet are arranged on the housing. The electro-thermal vaporization atomic fluorescence spectrometry method used for determining cadmium comprises steps that: a sample requiring testing is dried in air, and is cinerated, such that ash is obtained; under an argon atmosphere, the ash is heated to 1600 to 2000 DEG C, and the obtained vapor contacts the tungsten filament or the molybdenum filament; under an atmosphere of hydrogen and argon, the temperature of the tungsten filament or the molybdenum filament is increased to 1600 to 2000 DEG C, cadmium atoms are released, and the content of the cadmium atoms are analyzed by using a fluorescence spectrometry method. With the electro-thermal vaporization atomic fluorescence spectrometry method and the spectrometer used for determining cadmium provided by the invention, matrix interference can be effectively eliminated, and accurate measuring of cadmium can be realized.

The invention discloses a method for determination of the form of selenium in a selenium-rich plant material. The method provided by the invention is characterized by comprising the following steps of 1, a selenium-rich plant material pretreatment process comprising carrying out extraction of a crushed selenium-rich plant material sample by an extraction buffer Tris-HCl, after the extraction, adding cellulase into the extract, carrying out wall breaking of cells of the selenium-rich plant material sample, orderly adding effective amounts of protease K and protease XIV into the extract, and carrying out hydrolysis extraction to obtain a solution of a sample needing to be detected, and 2, carrying out determination processes respectively on a solution of selenium having a standard form and the solution of the sample needing to be detected by the combination of the hydride generation-atomic fluorescence spectroscopy technology and the high performance liquid chromatography. The method provided by the invention is simple, can be realized easily, adopts nontoxic reagents and does not produce pollution.

The invention provides a method of an atomic fluorescence spectrometry shape analysis by on-line pre-reducing trivalent arsonium and quinquivalent arsonium, the method comprises the following steps: (a) mixing a first arsenical sample and a first reducing agent under the temperature of 65-75 DEG C and performing a reduction of quinquivalent arsonium; (b) mixing a second arsenical sample and a second reducing agent, and determining the concentration of trivalent arsonium by the generated hydride after mixing; (c) mixing a solution obtained by reducing quinquivalent arsonium in the step (a) with the second reducing agent, and determining the concentration of total arsonium by the generated hydride after mixing. The invention also discloses an apparatus for using the method. According to theon-line pre-reduction of quinquivalent arsonium, the method of the invention is capable of effectively solving the interference problem between the valences, avoiding manual pre-treating processes inthe off-line reduction and realizing an automatic and rapid analysis of arsenic shape.

The invention relates to a detecting method for selenium speciation analysis in selenium-rich rice and particularly relates to a detecting method for organic selenium, protein selenium, polysaccharide selenium or RNA selenium in selenium-rich rice. The measuring method comprises the following steps of: (1) preparing a sample, namely sealing and storing selenium-rich rice flour to be detected for future use, wherein organic selenium is extracted through a dialysis method, and protein selenium, polysaccharide selenium and RNA selenium are respectively extracted; (2) measuring the selenium content through hydride atomic fluorescence spectrometry under measuring conditions that the negative high pressure is 340V, the lamp current is 100mA, the atomization temperature is 800 DEG C, the furnace height is 8mm, the flow rate of carrier gas is 500mL / min, the flow rate of shielding gas is 1000mL / min, the delay time is 1 second, the reading time is 10 seconds, the liquid adding time is 8 seconds, and the sample feeding volume is 2mL; and (3) data processing. The detecting method disclosed by the invention has the advantages of high sensitivity and accuracy and simplicity in operation.

The invention discloses an analysis method for determining arsenic in iron ore by using a hydride generation-atomic fluorescence spectroscopy. The method comprises the following steps of: preparing a sample solution of an iron ore sample, and preparing an arsenic standard solution; introducing the sample solution into an atomic fluorescence spectrophotometer, and determining the fluorescence intensity of the arsenic in the sample solution; and determining the content of the arsenic according to the fluorescence intensity which is determined on the basis of the arsenic standard solution with given concentration. By using the technical scheme disclosed by the invention, the content of the arsenic in the iron ore can be quickly and accurately determined.

The invention discloses a method for determining the arsenic, antimony and bismuth content of pure chromium by using atomic fluorescence spectrometry. The method comprises the following steps of: weighing a specimen; preparing a sample solution; preparing a calibration solution; drawing a working curve; measuring the concentrations of arsenic, antimony and bismuth in the sample solution; and calculating measurement results to obtain the arsenic, antimony and bismuth content. The method for determining the arsenic, antimony and bismuth content of the pure chromium is a hydride generation atomic fluorescence method, is high in analysis sensitivity, convenient to operate, short in analysis cycle and high in efficiency, has broad application prospect, and can be used for measuring the impurities arsenic, antimony and bismuth in the pure chromium which is a widely used raw material. Brazing performance can be greatly influenced by low-melting point impurity elements such as the arsenic, the antimony and the bismuth, and the like, and once the content of the elements exceeds a standard, the mechanical performance of materials can be greatly degraded, so that an accurate and reliable method is required by the measurement of the content of the elements. The requirements of scientific researches and production on control over the quality of raw materials are met, the rejection rate of the product is lowered, and development and production cost is saved.

The invention provides a liquid adsorbent and a method for controlling arsenic pollution of lake water, which relates to large-scale treatment of arsenic-polluted water. The adsorbent is reserve liquid formed by compounding iron salts FeCl3 or Fe2(SO4)3 or adding an appropriate amount of aluminum salts AlCl3 or Al2(SO4)3 with tap water or deionized water, and the mass concentration of the adsorbent is 100 to 600 g / L. The adsorbent in use is diluted by 10 to 30 times and then sprayed on the arsenic-polluted water. The adsorbent has the advantages of safety, low price, high arsenic removal efficiency and easy operation. A Yangzonghai arsenic-polluted water sample treated with the invention is detected through graphite furnace atomic absorption spectrometry and atomic fluorescence spectrometry, and detection results show that the arsenic removal rate of the invention can be greater than 92.7 percent, and the invention can reduce arsenic concentration from 0.110-0.130 mg / L to 0.003-0.008 mg / L which is lower than 0.050 mg / L specified by the national drinking water health standard (GB5749-2006) and 0.010 mg / L specified by the WHO drinking water quality standard.

The invention discloses a method for determining a selenium form in a selenium-rich egg, which is characterized by comprising the following steps: 1) pretreating the selenium-rich egg, using an extraction buffer Tris-HCl for extracting a sample of the selenium-rich egg, adding lipase for extracting if the selected selenium-rich sample is a yolk sample, then successively adding protease K and protease XIV with an effective amount for hydrolysis extraction to obtain a sample solution to be measured; directly and successively adding protease K and protease XIV with an effective amount hydrolysis extraction to obtain the sample solution to be measured if the selected selenium-rich egg sample is a egg white sample; 2) using combination of hydride generation-atomic fluorescence spectroscopy and high performance liquid chromatography for respectively determining a solution with a standard selenium form and the sample solution to be measured. The method of the invention is simple and easy to operate, the repeatability is good, and the used reagent has the advantages of no toxicity and no pollution.

The invention discloses a method for determining the form of selenium in selenium-enriched edible fungi. The method is characterized by comprising the following steps of: (1) pretreating selenium-enriched edible fungi: using deionized water as an extracting solution to extract a crushed selenium-enriched edible fungus sample, then adding effective amounts of protease K and protease XIV for hydrolysis so as to extract a sample solution to be detected; (2) conducting hydride generation: combining atomic fluorescence spectrometry with high performance liquid chromatography to determine a standard selenium form solution and the sample solution to be detected respectively. The method of the invention has the advantages of simplicity and easy operation, good repeatability, and employment of non-toxic and pollution-free reagents.

The invention discloses a method for indirectly measuring the content of uranium in soil through atomic fluorescence spectroscopy. The method is characterized in that the content of uranium is indirectly measured by measuring the content of arsenic; a complex is generated by utilizing uranium and certain arsenic-containing compounds which comprise but are not limited to arsenazo, and is separated from an original compound through a mode such as extraction, and the enriched complex subjected to separation is measured; and a standard working curve is made under the same condition and is compared so as to obtain the content of uranium by calculation. The method has the advantages that the method for indirectly measuring the content of uranium in soil through the atomic fluorescence spectroscopy is suitable for matrixes such as soil, water, coal and minerals. The method is simple and feasible, and compared with a conventional national standard method, the method according to the invention has the advantages that the used instrument is more common and is more applicable to analysis and research in a small lab.

The invention belongs to the technical field of feed quality detection, and particularly to a method for determining the selenium form in a selenium-rich feed, more particularly to a method for determining the selenium form in a selenium-rich feed by combining an ultrasonic probe-assisted enzymolysis technology and high-performance liquid chromatography-hydride generation atomic fluorescence spectrometry (HPLC-HG-AFS). According to the present invention, with the method, the content of the extracted selenium can be accurately determined, and the contents of the five forms of the selenium substances commonly contained in the selenium-rich feed can be effectively separated, such that the selenium form in the selenium-rich feed can be accurately analyzed, and the selenium-rich feed product can be rapidly and safely selected and used.

The co-using interface of the method of atom fluorescence spectrum and generation of the hybride in capillary electrophoresis relates to an apparatus thereof. This interface provides the key solutios that the capillary electrophoresis needs stable electric circuit, and that the method of atom fluorescence spectrum needs to convert analysed agent into hydride. The interface includes cross passage 1, T passage with small inner diameter 5, T passage with large inner diameter 7 and gas-liquid separator 6, cross passage 1 connected in turn to T passage with small inner diameter 5, T passage with large inner diameter 7 and gas-liquid separator 6. The interface has ingenious and novel design, having such features as small dead volume, short connecting piping and simple and practical operation.

The invention discloses a method for determining arsenic and cadmium in donkey-hide gelatin by means of hydride generation-atomic fluorescence spectrometry. The method comprises: 1) preparing appropriate reductant and current-carrying solutions; 2) setting instrument and measuring parameters; 3) preparing standard blanks of standard substance series of solutions; 4) determining the standard blanks till stabilization of the instrument; 5) measuring the fluorescence intensity of the standard substance series of solutions, and drawing standard curves with concentrations of the standard substance solution series as the independent variables, and fluorescence intensity of the standard substance solution series as the dependent variables; 6) determining the fluorescence intensity of sample blanks; 7) determining the sample fluorescence intensity; 8) calculating the sample concentration according to the sample fluorescence intensity and standard curve equations; as well as conducting sample digestion before step 6 and step 7. The method of the invention has the advantages of high sensitivity, low detection limit, less basic interference, rapidity, simplicity and convenience.

A method is disclosed for determining the concentration of trivalent chromium Cr(III) in a sample. The addition of perchloric acid has been found to increase the atomic chromium spectrometric signal due to Cr(III), while leaving the signal due to hexavalent chromium Cr(VI) unchanged. This enables determination of the Cr(III) concentration without pre-concentration or pre-separation from chromium of other valences. The Cr(III) concentration may be measured using atomic absorption spectrometry, atomic emission spectrometry or atomic fluorescence spectrometry.

The invention discloses a method for determining the selenium and tellurium content of pure chromium by using atomic fluorescence spectrometry. The method comprises the following analysis steps of: weighing a specimen; preparing a sample solution; preparing a calibration solution; drawing a working curve; measuring the concentrations of selenium and tellurium in the sample solution; and calculating measurement results to obtain the selenium and tellurium content. The method for determining the selenium and tellurium content of the pure chromium is a hydride generation atomic fluorescence method, is high in analysis sensitivity, convenient to operate, short in analysis cycle and high in efficiency, has broad application prospect, and can be used for measuring the impurities selenium and tellurium in the pure chromium which is a widely used raw material. Brazing performance can be greatly influenced by low-melting point impurity elements such as the selenium and the tellurium, and the like, and once the content of the elements exceeds a standard, the mechanical performance of materials can be greatly degraded, so that an accurate and reliable method is required by the measurement of the content of the elements. The requirements of scientific researches and production on control over the quality of raw materials are met, the rejection rate of the product is lowered, and development and production cost is saved.

The present invention discloses an atomic fluorescence spectrometry for detecting Cr (VI), and an atomic fluorescence spectrometer thereof. The atomic fluorescence spectrometer comprises an evaporator, an excitation light source, an atomizer, a photoelectric detector and a computer. The evaporator comprises a sealed housing, a heating boat and power supply. The heating boat is arranged inside thesealed housing. The sealed housing is provided with a gas inlet and a gas exhaust port. The heating boat is connected with the power supply. The gas exhaust port of the evaporator is connected with the atomizer by a duct. The atomic fluorescence spectrometry comprises the following steps: heating a sample requiring detection in mixed gas comprising hydrogen and argon to a temperature of 1000-1400DEG C until the sample requiring detection is dried and ashed; heating the ashed residue to the temperature of 2000-2600 DEG C, carrying out secondary atomization for the resulting vapour; adopting atomic fluorescence to detect the Cr (VI) content. The atomic fluorescence spectrometry for detecting the Cr (VI), and the atomic fluorescence spectrometer of the present invention have high sensitivity, simple spectral line and low interference.

The invention relates to a detection method for determining the migration quantity of harmful elements in a food contact material, especially to a detection method for determining the migration quantity of lead, cadmium, arsenic and antimony in a food contact material by the sequential injection-hydride generation-atomic fluorescence spectroscopy (HG-AFS) method. The method provided by the invention comprises the following steps of: 1, migration test; 2, food simulacrum test solution treatment; 3, blank test; 4, sequential injection-hydride generation-atomic fluorescence spectroscopy determination. By the adoption of L-cysteine as a pre-reducing agent or by the adoption of a direct dilution method to eliminate severe inhibition and interference of 4% acetate base to the determination of lead and cadmium by an atomic fluorescence method, the migration quantity of arsenic, antimony, lead and cadmium in a food contact material can be efficiently, simply and rapidly determined. The migration quantity of four harmful elements can be detected only by a simple pre-treatment. The detection limits of lead cadmium, cadmium, arsenic and antimony are respectively 0.010, 0.010, 0.010 and 0.010mg / L.

The invention relates to a method for measuring chemical gas phase genesis atomic fluorescence spectrum of chromic and corresponding apparatus. The method comprises chemical gas phase genesis process of chromic; atomize process of genesis gas phase object and fluorescence detecting process of chromic molecule. The apparatus comprises a gas-liquid separating device having a color scatter atom fluorescence spectrometer, wherein the gas-liquid separating device comprising a gas-liquid separating device and a reactor which one end being connected with reducer and current-carrying / sample pipe, the other end being connected with the gas-liquid separating device which having its one end connected with a atomize device that connected with gas mixer, and have the other end connected with exhaust pipe. The invention has the advantages of being stable and reliable.

The invention provides an extraction method for mercury compounds in sediments. The extraction method comprises the following steps: adding a complexing agent into the sediments, and carrying out complexing reaction, thereby obtaining complex; and centrifuging, taking out supernatant liquor, adding ion liquid, oscillating, centrifuging, and taking sedimentary facies at the bottom, i.e., extracts containing rich mercury compounds. The extraction method utilizes the ion liquid to extract the mercury compounds in the sediments, so that the extraction effect is good, the enrichment multiple is high, and the extraction method is simple, fast and environmental-friendly. The invention also provides a detection method for the mercury compounds in the sediments. According to the detection method, pretreatment is carried out on the sediments according to the extraction method provided by the invention, and then the obtained extracts are detected by combined use of high-performance liquid chromatography and cold atomic fluorescence spectrometry. The detection method has the advantages of fastness, accuracy, stability, sensitivity and the like and is applicable to daily environmental monitoring.

The invention discloses a method for measuring trace elements such as arsenic and selenium in industrial electro-deposit copper according to the atomic fluorescence spectrometry. The method comprises the following steps: A, preparing a solution of an industrial electro-deposit copper fine sample; B, preparing a standard arsenic solution and a standard selenium solution; C, preparing a working curve solution with the standard arsenic solution and the standard selenium solution; D, measuring the atomic fluorescence strengths of arsenic and selenium in the working curve solution with an atomic fluorescence photometer, and drawing working curves by taking the mass concentrations of arsenic and selenium as X axes, and taking the fluorescence strengths of arsenic and selenium are Y axes; E, measuring the atomic fluorescence strengths of arsenic and selenium in the sample solution with the atomic fluorescence photometer, and finding out corresponding mass concentrations of arsenic and selenium on corresponding working curves with the atomic fluorescence strengths. As a nitric acid, hydrochloric acid, potassium iodide and thiocarbamide-ascorbic acid treating sample is adopted, not only can the impact of interfering ions such as Cu, Fe, Ag, Bi and Se and the combination of the interfering ions be effectively screened, but also the impact of the copper base body on arsenic and selenium measure can be eliminated.

The invention discloses a preparation method of a nano gold colorimetric sensor and application thereof in colorimetric detection of divalent mercury ions (Hg2+), and is intended to solve the problem that existing ICP (inductively coupled plasma), AAS (atomic absorption spectrometry) and AFS (atomic fluorescence spectrometry) methods and other mercury ion detection methods generally have the defects such as strict sample storage conditions, high analysis process cost, long analytical time and high operational professionality. The stable and water-soluble nano gold colorimetric sensor modified via sodium lysinate is prepared by using gold salt and gold nano particles as sources, using sodium lysinate as a reducing agent and ligand and reacting under gold salt solution boiling. The nano gold colorimetric sensor has the advantages of good portability, high sensitivity, high selectivity, good stability and the like, allows Hg2+ to be detected fast, has the advantages of high detection speed, high sensitivity and the like, and has a promising application prospect and high marketing value.

A method for rapidly detecting trace tin in the hull steel by adopting the atomic fluorescence spectrometry relates to the technology field of the special steel detection. Tartaric acid, thiourea and ascorbic acid are adopted as a masking agent so as to successfully eliminate the interference of the elements. The analysis time of one sample requires about 5 hours. The method is suitable for measuring the tin content with a mass fraction of 0.0001%-0.10%, a mark-on recovery rate of 98%-108% and detectability of 0.76ng / ml. The method has the advantages of lower interference, wide analytical range, high stability, high speed, etc., when detecting trace tin in the hull steel.

The invention discloses a method for measuring the content of selenium in molybdenum and a molybdenum product. The method comprises the following steps: sampling, preparing a sample solution and a sample blank solution, preparing a working curve solution, drawing a working curve, measuring the content of the selenium in the sample solution, and calculating. According to the method for measuring the content of the selenium in the molybdenum and the molybdenum product, provided by the invention, the problem that an existing hydride generation-atomic fluorescence spectrometry can not be applied to the measurement of the content of the selenium in the molybdenum and the molybdenum product because the selenium hydride of the molybdenum is difficult to form is solved. The method provided by the invention is simple and convenient to operate, high in efficiency and high in sensitivity; and the detection limit is 0.13ng / mL, the recovery rate is 90.23 percent-105.1 percent, and the measurement range of the content of the selenium is 0.0001-0.0050 percent.

The invention relates to a method for detecting inorganic mercury and organic mercury in an environmental water sample, belonging to the field of environmental sample detection methods. The invention provides a method for accurately detecting inorganic mercury and organic mercury, which aims at solving the problem that a traditional monitoring method has difficulty in accurately detecting or distinguishing the content of inorganic mercury and organic mercury. The method is characterized in that total mercury and inorganic mercury are respectively determined by adopting a flow injection online hydride generation-atomic fluorescence spectrometry in the presence or absence of a brominating agent which serves as a digesting agent for organic mercury, and the content of organic mercury is solved by adopting a subtraction method. The detection method is simple and rapid to operate, high in sensitivity and less in interference; proved in a labeling recycling experiment, the recycling rate can reach 95 percent to 105 percent.

The invention discloses a method for measuring trace elements such as arsenic and antimony in industrial lead bullion according to the atomic fluorescence spectrometry. The method comprises the following steps: A, preparing a solution of an industrial lead bullion fine sample; B, preparing a standard arsenic solution and a standard antimony solution; C, preparing a working curve solution with the standard arsenic solution and the standard antimony solution; D, measuring the atomic fluorescence strengths of arsenic and antimony in the working curve solution with an atomic fluorescence photometer, and drawing working curves by taking the mass concentrations of arsenic and antimony as X axes, and taking the fluorescence strengths of arsenic and antimony are Y axes; E, measuring the atomic fluorescence strengths of arsenic and antimony in the sample solution with the atomic fluorescence photometer, and finding out corresponding mass concentrations of arsenic and antimony on corresponding working curves with the atomic fluorescence strengths. As a nitric acid, hydrochloric acid and thiocarbamide-ascorbic acid treating sample is adopted, not only can the impact of interfering ions such as Cu, Fe, Ag, Bi and Se and the combination of the interfering ions be effectively screened, but also the impact of the lead base body on arsenic and antimony measure can be eliminated.

The invention belongs to the field of water environment monitoring methods, in particular to a method for measuring arsenic and mercury in water by hydride generation-atomic fluorescence spectrometry. The method comprises the following steps of: a) preparing a mixed sample solution which contains the arsenic and the mercury; b) generating arsine vapor and mercury vapor by using the mixed sample solution and a potassium borohydride solution; and c) introducing the arsine vapor and the mercury vapor into an atomizer by using a carrier gas, exciting the arsine vapor and the mercury vapor by using a special hollow cathode light source to generate atomic fluorescence, detecting the intensity of the atomic fluorescence, and calculating the content of the corresponding components in the sample solution by utilizing the direct proportion relationship of the fluorescence intensity with the content of the arsenic and the mercury in the solution. By using the method, the content of the arsenic and the mercury in environmental water can be measured at the same time; the method is operated simply and quickly; and labor, time and reagents are saved.

The invention discloses a method for rapid determination of the selenium content in tetrastigmatis hemsleyani, wherein a microwave digestion-hydride generation-atomic fluorescence spectrometry method is adopted for determination of the selenium content. With microwave digestion, the digestion efficiency is high and fast, moreover, acid removing is not required after digestion, operation steps are simplified, pollution is reduced, the accuracy rate is increased, disadvantages of easy pollution of wet digestion and long digestion time are avoided, acid removing is not required, concentrated hydrochloric acid is directly added for reduction of selenium, and the digestion procedures are simplified; the detection cycle is greatly shortened, and the original detection cycle of 8-10 hours is shortened to 2-3 hours; and the detection is rapid and accurate, and the operation is simple.

The invention belongs to the field of water environment monitoring methods, in particular to a pretreatment method for a sewage sample during the measurement of arsenic and mercury in water by fluorescent spectrometry. The pretreatment method is characterized by comprising the following steps of: transferring 10 ml sewage sample in a 25 ml colorimetric tube; respectively adding 2.5 ml of 50 g.L<-1> thiourea solution and 2.5 ml of 5 to 10 percent hydrochloric acid solution, diluting to the scale and shaking uniformly. The fluorescent spectrometry is hydride generation atomic fluorescence spectrometry; and the solution used for measuring the arsenic and the mercury in the water by the fluorescent spectrometry is a potassium borohydride solution. By the pretreatment method, the sewage sample is pretreated, so that the measurement results of the content of the arsenic and the mercury are accurate and available.

The invention provides a method of determining the content of an arsenic element in a coal-containing sample. The method comprises the following steps: S1, preparing a solution to be detected for the coal-containing sample, wherein the solution to be detected contains the arsenic element; S2, determining the arsenic element in the solution to be detected by using hydride generation-atomic fluorescence spectrometry to obtain a detection value of arsenic atomic fluorescence intensity; S3, comparing the detection value with a calibration curve of the arsenic element to obtain the content of the arsenic element in the solution to be detected so as to further obtain the content of the arsenic element in the coal-containing sample, wherein in the hydride generation-atomic fluorescence spectrometry, working parameters of an atomic fluorescence spectrometer are as follows: the lamp current is 60 to 65mA; the negative high voltage is 280 to 290V; the height of an atomizer is 7.0 to 7.1mm; the temperature of the atomizer is 200 to 220 DEG C, and the carrier gas flow is 800 to 815mL.min<-1>. Test parameters and the addition amount of a reagent are adjusted, thereby improving the accuracy and the precision of the method.