CN110132916B - Accurate quantitative analysis method for metal elements - Google Patents
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- CN110132916B CN110132916B CN201910395531.8A CN201910395531A CN110132916B CN 110132916 B CN110132916 B CN 110132916B CN 201910395531 A CN201910395531 A CN 201910395531A CN 110132916 B CN110132916 B CN 110132916B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6402—Atomic fluorescence; Laser induced fluorescence
- G01N21/6404—Atomic fluorescence
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/02—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by absorbing or adsorbing components of a material and determining change of weight of the adsorbent, e.g. determining moisture content
Abstract
The invention relates to the field of analytical chemistry, in particular to a method for accurately and quantitatively analyzing metal elements by using a patent technology combining a standard addition method and a difference method when the metal elements are accurately and quantitatively determined. The analysis method adopts a mode of combining a standard addition method and a difference method, designs a standard curve concentration calculation formula based on the difference method, combines software calculation, establishes a standard curve by using the standard addition method, improves the efficiency of preparing the standard curve, and effectively reduces the interference caused by a matrix effect, thereby realizing the accurate quantification of the metal elements. The method greatly reduces the calculated amount when the standard curve is prepared by using the traditional standard addition method, thereby improving the precision and the speed of the quantitative analysis of the harmful metal elements, enabling the standard addition method to replace the standard curve method (external standard method), enabling the accurate quantitative method of the metal elements to be applied to the detection of batch samples, and being used as a method for efficiently measuring the element concentration when a special device is not used for measuring by using the standard addition method.
Description
Technical Field
The invention relates to the field of analytical chemistry, in particular to a patent technology accurate quantitative analysis method combining a standard addition method and a difference method in application when harmful metal elements are accurately quantified.
Background
Metal elements are widely distributed in nature, and heavy metals represented by elements such as lead, cadmium, mercury and the like are applied to various fields of production and various aspects of life. However, since the individual environmental stress problem is highlighted or a part of the area is a harmful metal element production area, the detection and control of harmful metal elements in the environment and food are very important for ensuring the health of people. The standard curve method (external standard method) is suitable for the case that the matrix of the standard curve is approximately the same as that of the sample, and has the advantages of high analysis speed and the disadvantage that when the matrix of the sample is complicated and cannot be accurately matched with the standard curve solution collectively, the measurement result can cause the increase of the determination error. The standard addition method is suitable for detecting the existence of interfering substances in a sample, and is very effective when a standard solution similar to the sample solution is difficult to prepare, or the matrix composition of the sample is very high, and the influence on measurement is difficult to keep constant due to uncertain change or solid substances contained in the sample, and the standard addition method can effectively overcome the defects of a standard curve method (external standard method).
The known standard addition method generally adopts the modes of diluting and adding a standard solution with the same volume of a solution to be detected or pre-calculating and accurately adding a standard solution and the like. The method for diluting and labeling with equal volume comprises the following steps: preparing a series of standard solutions with different concentrations, adding the same amount of sample solution to be detected, testing the series of solutions one by one, drawing a standard curve by taking the concentration as an abscissa and the corresponding measurement signal intensity as an ordinate, and finally calculating the content of the component to be detected from the intersection point of the standard curve and the abscissa by combining corresponding software.
In 2015, the district in which the water circulation and water quality safety in Guangdong province and city are important in laboratories is good, the Mijinhuan and the Wang et al published a paper of ' standard addition method inductively coupled plasma mass spectrometry for simultaneously determining arsenic, cadmium and lead in polyaluminium chloride for domestic drinking water ' in Guangdong chemical industry ', the standard addition method comprises adding 6 parts of the same volume of the solution to be measured into the standard solution of the element to be measured with the same concentration and different volume from the second part, diluting with blank to the same volume, sequentially measuring the signal intensity of each solution under the same experimental condition, then drawing a calibration curve of the signal intensity to the addition concentration, in the whole process of the method, the standard solution is added into six containers and then the volume is respectively determined, and then the measurement is carried out on a machine, so that not only is the risk of system errors increased in the detection process, but also the method is very complicated and time-consuming, and therefore, the standard addition method is only used under the conditions of small number of samples and relatively complex matrix. At present, some instruments are provided with special devices for measurement by using a standard addition method, but the methods of measuring harmful metal elements, such as atomic absorption, atomic fluorescence or mass spectrometry, and the like by using a spectroscopic instrument are not provided with the special devices for measurement by using the standard addition method, so that the manual preparation of a standard curve is a more common method in the test.
Disclosure of Invention
Aiming at the defects of the existing standard addition method, the invention provides a method for accurately and quantitatively analyzing harmful metal elements in the patent technology, the analysis method adopts a mode of combining the standard addition method and the difference method, designs a standard curve concentration calculation formula based on the difference method, and establishes a standard curve by using the standard addition method, thereby greatly improving the efficiency of preparing the standard curve and reducing the interference caused by matrix effect, thereby realizing the accurate quantification of the harmful metal elements and enabling the standard addition method to replace the standard curve method (external standard method). The standard addition method can be applied to detection of batch samples, and is used as a method for efficiently and manually measuring the concentration of harmful metal elements when an instrument does not have a special device for measuring by using the standard addition method.
In order to achieve the purpose, the invention adopts the following technical scheme.
A precise quantitative analysis method of metal elements in patent technology is characterized in that.
Soaking a glass container for preparing a standard curve and a constant volume sample in a high-grade pure nitric acid solution (volume ratio = 1: 5) for 12 hours, washing with laboratory three-level water, and drying at fifty ℃ for later use; the nitric acid is superior pure.
Selecting a metal element standard solution to be detected (the concentration is 1000 micrograms per milliliter), transferring 10.00mL of the element standard solution into two bottles at 20 ℃, using a 5% high-grade pure nitric acid solution to fix the volume to 100 (0.0001) g to obtain a standard use solution (the concentration is =100 micrograms per gram), and then using an intermediate solution to prepare the standard use solution (the concentration of the use solution is =1000 nanograms per gram).
Weighing a plurality of parts of samples to be measured, adding nitric acid, digesting by a proper method, and taking one part of sample solution for later use.
And (3) putting a clean and dry volumetric flask on a balance, zeroing, adding the 10 sample solutions to the volumetric flask in a constant volume manner, and shaking up. And recording the mass of the solution after the constant volume, enabling the balance not to return to zero, taking 5mL as a standard blank (the first point), and recording the mass of the solution.
0011 Add a volume of 0009 standard solution to the last recorded mass of sample and shake it up. And recording the quality of the solution after the labeling.
Calculating the standard substance concentration in the solution after the first time of adding the standard substance by using a formula:
the second point of concentration was taken as the standard curve for the 5mL0012 spiked solution. The balance was not zeroed and the remaining mass of the solution was recorded.
0014 add a volume of 0009 standard use solution to the solution and record the mass after shaking.
And (3) calculating the concentration of the solution after the latest one-time standard addition by using a formula:
and preparing other standard points of other standard curves by using a 16 formula principle.
Combining an element standard adding method in an atomic absorption spectrophotometer, an atomic fluorescence spectrophotometer or inductively coupled plasma mass spectrometer software, inputting the concentration of each point of a prepared standard curve into a computer, placing the solution of the standard curve at a corresponding position, measuring the signal intensity of the corresponding standard point, drawing a standard curve by taking the concentration as an abscissa and the corresponding measured signal intensity as an ordinate, and finally calculating the content of an element to be measured from the intersection point of the standard curve and the abscissa.
The invention reduces the system error caused by the complicated process when the traditional standard addition method is used for preparation, saves time and reagent consumption, and is a high-efficiency and accurate method for manually measuring the element concentration when the used instrument does not have a special device for measuring by using the standard addition method.
Drawings
FIG. 1 is a flow chart of a standard curve configuration by a conventional standard addition method and its disadvantages.
FIG. 2 is a flow chart of a standard curve configuration using a novel standard addition method and its advantages.
FIG. 3 is a table showing the As and Pb measurements taken by way of example, using office software in combination with a formula for preparing a standard curve, and automatically calculating the content of the target at the first point of concentration in the standard curve after the solution is subjected to calibration after inputting the mass before and after the solution is subjected to calibration.
FIG. 4 is a table showing the As and Pb measurements taken by way of example, using office software in combination with a formula for preparing a standard curve, and automatically calculating the content of the standard substance at the second point of the concentration value in the standard curve after the solution is subjected to the calibration after the mass input before and after the calibration.
Fig. 5 is a standard curve measured with an inductively coupled plasma mass spectrometer using the novel standard addition method, taking total arsenic as an example.
Figure 6 is a standard curve measured with an inductively coupled plasma mass spectrometer using the novel standard addition method, using lead as an example.
Fig. 7 shows the reference numbers and result satisfaction certificates of the five metal element international capability verification laboratories participating in FAPAS.
Detailed Description
To explain technical contents, structural features, and objects of the present invention in detail, the following description is given with reference to the accompanying drawings in conjunction with the embodiments.
The invention preferably relates to an embodiment for simultaneously measuring total As and Pb elements of two harmful metals, and discloses a method for accurately and quantitatively analyzing metal elements, which comprises the following steps.
The total As and Pb As harmful metal substances existing in nature have definite limited values for the content of the total As and Pb in food in the national food safety standard GB2762-2017, and the total As and Pb can cause direct damage to human bodies when exceeding the limited values.
Preparing vessels and reagents required by the experiment: soaking a glass container for preparing a standard curve and a constant volume sample in a nitric acid solution (with the concentration of 20%) for 12 hours, washing with laboratory three-level water, and drying at fifty ℃ for later use; the nitric acid is superior pure. Experiments prove that: harmful metal elements in a glass container treated by the superior grade pure nitric acid solution are dissolved by nitric acid, and after the glass container is washed by three-grade pure water in a laboratory, the residual quantity of the harmful metal elements in the glass container is less than 1 ppb. In order to prepare a standard curve by a difference method conveniently, water in the glass container needs to be removed, but the volumetric flask serving as a common quantitative utensil in the test cannot be dried at high temperature, so the volumetric flask is dried at fifty ℃ by using an electrothermal constant-temperature drying oven.
Preparation of total As, Pb standard use solutions: selecting a mixed standard solution (the concentration is 1000 micrograms per milliliter) of total As and Pb, transferring 10.00mL of element standard solution into a volumetric flask at 20 ℃, carrying out constant volume to 99.9991g by using a 5% superior pure nitric acid solution to obtain a standard intermediate solution (the concentration is 100.0009 micrograms per gram), then putting 0.9978g of the standard intermediate solution into a 100 mL volumetric flask, carrying out constant volume to 99.8348g by using the 5% superior pure nitric acid solution to obtain a standard use solution (the concentration of the use solution is =999.46 nanograms per gram), wherein the standard use solution of the traditional standard addition method generally adopts a volume-fixing mode and is easily influenced by temperature, so that the error is reduced by adopting a mode of taking the volume at the first step and determining the mass at the rest steps.
Digesting a sample to be detected: the volume of the sample is determined by using a ware and a reagent in 0030: when the sample is digested, the sample is digested by a pressure tank digestion mode according to the characteristics of the element to be detected so as to completely digest the sample. Weighing 4 parts of 0.5g (accurate to 0.0001 g) sample to be detected, and adding 5mL of nitric acid for digestion.
Placing a clean and dry volumetric flask on a balance, taking 0032 one sample digestion solution as a solvent for preparing a standard curve after zeroing, fixing the volume into the volumetric flask, and shaking up. The mass of the solution after the volume was recorded to be 49.8571g, the balance did not return to zero. And (4) fixing the volume of the other three solutions on another balance by the method, shaking up, and measuring.
The balance was not zeroed, the mass solution recorded in 10 ml 0033 was taken as a standard curve blank solution (first point) in a 15 ml disposable centrifuge tube, and the solution was then placed back on the balance, at which time the mass of solution =40.8940g before adding the label was recorded. To the above sample put back on the balance, 0.25ml of the standard working solution 0031 was added and shaken up. The solution mass after labeling =41.1527g was recorded. The traditional standard adding method is characterized in that a solution to be measured is taken and added into different volumetric flasks in equal volume respectively, and due to constant volume errors existing among the different volumetric flasks, errors are eliminated by adopting a method of repeatedly adding standard use solution after the same solution is subjected to constant volume.
The formula is used to calculate the concentration of the standard substance =6.28 nanograms per gram in the solution after the first spiking:
referring to fig. 3, a table is formed by combining the formula in 0035 with office software, so that the concentration of the position of E8 (the second point of the standard curve) = (D8-B8) × C3/D8, then 41.1527g recorded in the solution after the labeling in 0034 is input to the position of D8, 40.8940g recorded in the solution before the labeling in 0034 is input to the position of B8, the concentration of the standard use solution of 0031 =999.46ng/g is input to the position of C3, and the concentration of the second point of the standard curve can be obtained through calculation of the office software.
The second point of the standard curve was taken as the post-labeling solution in about 5mL 0034. At this point the balance did not return to zero and the remaining mass of the solution =35.8283g was recorded.
5mL of the solution was taken out of 0037 and weighed into a 15 mL disposable centrifuge tube, and 0.25mL of the standard use solution (prepared in 0031) was added to the solution and weighed =36.0761g after shaking.
The solution concentration after the latest one-time labeling =13.10 nanograms per gram was calculated using the formula:
referring to fig. 4, a table is formed by combining the formula in 0039 with office software, so that the formula of the concentration calculation at the position of E9 (the third point of the standard curve) = [ (D9-B9) × C3+ E8 × B9]/D9, then 36.0761g recorded in 0038 is input to the position of D9, 35.8283g recorded in 0037 is input to the position of B9, and the concentration at the third point of the standard curve can be obtained through automatic calculation of the office software.
Step 0030-0040 is the manufacturing principle of the first concentration point and the second concentration point of the prepared standard curve, and the quality records of the solutions before and after each solution adding standard are as follows:
and preparing other standard points of the rest standard curves by using a 0039 formula principle. In the experimental process, the concentration position formulas of other standard points are respectively set on uniformly recording the weighing values and the record book for each time:
concentration of each of the other standard points = [ (mass after adding standard-mass before adding standard) × standard use solution concentration + mass before adding standard × concentration of substance in solution before adding standard ]/mass after adding standard
And then respectively inputting the mass of the solution after the labeling and the mass of the solution before the labeling into corresponding positions of office software, taking out about 5ml to 15 ml of the solution at each standard point each time, uniformly recording the weighing values at each time, and inputting the values into corresponding positions of the software to calculate the concentrations of other standard points. Obtaining a total As with a Pb concentration of 0; 6.28; 13.10; 20.62, respectively; 29.99; a standard curve of 42.75 nanograms per gram. Referring to fig. 5 and 6, the signal intensity corresponding to the standard point is measured, and a standard curve is drawn with the concentration as the abscissa and the measured signal intensity as the ordinate. And then sequentially measuring the concentration of the sample, and obtaining the concentration of the elements in the sample by calculation. The concentrations at each point of the standard curve were calculated as follows:
when the inductively coupled plasma mass spectrometry is used for simultaneously measuring As and Pb, the software has an external standard method and a standard addition principle for making a standard curve option, but the specific operation steps are the traditional standard addition method. The novel standard adding method is combined with the difference method on the basis of the traditional method, office software is applied to a specific calculation formula, error risks are reduced, configuration time is shortened, and a standard curve consistent with the input software mode of the traditional method is obtained.
Combining an element standard adding method in inductively coupled plasma mass spectrometer software, inputting the concentration of each point of a prepared standard curve into a computer, placing the solution at a corresponding position, measuring the signal intensity of the corresponding standard point, drawing the standard curve by taking the concentration as an abscissa and the corresponding measured signal intensity as an ordinate, and finally calculating the content of the element to be measured from the intersection point of the standard curve and the abscissa.
In the element determination, methods such as atomic absorption and atomic fluorescence are adopted, and based on the principle of a standard addition method, the novel standard addition method is also suitable for the two instruments, so that the method can be used for determining the harmful metal elements by an inductively coupled plasma mass spectrometer and can also be applied to determining the harmful metal elements by other spectral instruments.
The instruments and methods for measuring harmful metal elements are various, and not every instrument is equipped with a special device for measuring by using a standard addition method, so that in daily inspection and detection, a standard curve is prepared manually, the standard addition method is more accurate than the standard curve method, the novel standard addition method has higher efficiency than the traditional standard addition method, and when the concentration of the elements needs to be accurately quantified, the novel standard addition method is necessary to be used manually. Based on the characteristics of rapidness and high efficiency, the novel standard addition method can replace an external standard method and becomes a common element determination method.
Referring to fig. 7, when the concentration capacities of five elements in FAPAS soybean meal participated in 2018 are verified, a standard addition method is adopted for determination because the sample to be detected has obvious substrate interference when an external standard method is used, but the traditional standard addition method has its own limitations.
Claims (2)
1. A method for accurately and quantitatively analyzing harmful metal elements is characterized by comprising the following steps:
s1 preparation of vessels and reagents required for the experiment:
preparing a glass container of a standard curve and a constant volume sample, soaking the glass container in a nitric acid solution with the concentration of 20% for 12 hours, washing the glass container with laboratory three-level water, and drying the glass container at fifty ℃ for later use, wherein the nitric acid is high-grade pure;
s2, preparing a standard use solution of the element to be detected:
selecting a standard solution with the concentration of harmful metal elements to be detected as 1000 micrograms per milliliter, transferring 10.00mL of the element standard solution into a volumetric flask at 20 ℃, using 5 percent high-grade pure nitric acid solution to fix the volume to 100 (0.0001) g, preparing standard use solution with the concentration of 100 micrograms per gram, and then using intermediate solution to prepare the standard use solution with the concentration of 1000 nanograms per gram;
s3 digesting the sample to be measured, and fixing the volume of the sample by using a vessel and a reagent in S1:
weighing a plurality of parts of a proper amount of samples to be detected, adding nitric acid to digest the samples by a proper method, and taking one part of sample solution for later use;
s4, placing a clean and dry volumetric flask on a balance, fixing the volume of the sample solution in S3 into the volumetric flask after the solution returns to zero, shaking up, recording the mass of the solution after the volume is fixed, enabling the balance not to return to zero, taking 5mL of the solution as a standard blank, and recording the mass;
s5, adding a certain volume of standard use solution in S1 into the S4 constant volume sample, shaking up, and recording the quality of the solution after adding the standard;
s6, calculating the standard substance concentration in the solution after the first time of adding the standard substance by using the formula:
s7, taking the solution after the standard addition in the 5mLS5 as a first point after the standard addition of the standard curve, wherein the balance does not return to zero at the moment, and recording the residual mass of the solution;
s8 adding a certain volume of standard solution into the solution in S7, shaking up and recording the mass;
s9, calculating the concentration of the solution after the latest one-time labeling by using the formula:
s10 prepares other standard points of the standard curve by using the principle of the formula S9, and the preparation of the whole standard curve can be simply described as follows: 1 completely digesting the sample, fixing the volume → 2 taking out the constant volume sample with a certain volume, making a zero point of a standard curve → 3 putting the rest constant volume sample on a balance, weighing, measuring the mass → 4 adding a certain volume of standard solution using liquid into the solution in the previous step, weighing, measuring the mass, shaking up → 5 substituting the measured mass parameters into an S6 formula, calculating the concentration of a first point after the scaling → 6, taking the solution after the scaling in the previous step as a first point after the scaling of the standard curve, measuring the mass → 7, adding a certain volume of standard solution into the solution in the previous step for liquid addition, weighing, measuring the mass, shaking up → 8 substituting the values into an S9 formula for calculating the concentration of the solution after the scaling in the previous step, taking out a certain volume of the solution as a second point after the scaling of the standard curve → 9, operating according to the steps 6 to 8, in the process of an actual test, recording the solution quality weighed in each step, calculating the concentration of a first point after the standard addition by utilizing S6, and calculating the concentration of a second point after the standard addition of the standard curve and other subsequent standard points by utilizing the principle of S9;
s11, combining with an element standard adding method in software of an inductively coupled plasma mass spectrometer, an atomic absorption spectrometer and an atomic fluorescence spectrometer, inputting the concentration of each point of a prepared standard curve into a computer, placing the solution of the standard curve at a corresponding position, measuring the signal intensity of the corresponding standard point, drawing a standard curve by taking the concentration as an abscissa and the corresponding measured signal intensity as an ordinate, and finally calculating the content of the element to be measured from the intersection point of the standard curve and the abscissa.
2. The method for accurately and quantitatively analyzing a harmful metallic element according to claim 1, wherein:
after the step of preparing the standard curve from S4 to S10 is completed, all the mass values of the concentration of each standard point on the calculated standard curve are recorded; recording a calculation formula of each point of the standard curve into Excel office software according to formula principles of S6 and S9 on the Excel office software; inputting the required quality parameters for calculating each standard point on the standard curve into the corresponding position of the ExceL software, and directly reading the concentration of each standard point on the standard curve.
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