CN116735565A - Method for measuring barium by internal standard-ICP-OES - Google Patents

Method for measuring barium by internal standard-ICP-OES Download PDF

Info

Publication number
CN116735565A
CN116735565A CN202310600375.0A CN202310600375A CN116735565A CN 116735565 A CN116735565 A CN 116735565A CN 202310600375 A CN202310600375 A CN 202310600375A CN 116735565 A CN116735565 A CN 116735565A
Authority
CN
China
Prior art keywords
barium
sample
solution
standard
measuring
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202310600375.0A
Other languages
Chinese (zh)
Inventor
卢艳蓉
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Baotou Iron and Steel Group Co Ltd
Original Assignee
Baotou Iron and Steel Group Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Baotou Iron and Steel Group Co Ltd filed Critical Baotou Iron and Steel Group Co Ltd
Priority to CN202310600375.0A priority Critical patent/CN116735565A/en
Publication of CN116735565A publication Critical patent/CN116735565A/en
Pending legal-status Critical Current

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/66Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence
    • G01N21/68Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence using high frequency electric fields
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/66Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence

Landscapes

  • Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)

Abstract

The invention discloses a method for measuring barium by internal standard-ICP-OES, which combines the modern analysis technology, sodium hydroxide, sodium peroxide fusion sample and dilute hydrochloric acid are leached and acidified, and then the ratio of the ionic strength of barium ions to the ionic strength of the internal standard element is used as the measurement strength, thereby improving the measurement accuracy and precision. The invention has the advantages of high sensitivity, high measuring speed, simple and convenient operation, small interference relative to other methods and good selectivity; the measurement stability is improved by adopting a vertical observation method.

Description

Method for measuring barium by internal standard-ICP-OES
Technical Field
The invention relates to the technical field of ferrous metallurgy analysis, in particular to a method for measuring barium by internal standard-ICP-OES.
Background
Currently, barium in silicon-barium alloy, silicon-aluminum-barium, silicon-calcium-barium and barite is measured by adopting the weight of sulfate. The related literature reports that X-ray spectrometry is used for detecting silicon, aluminum, calcium and barium in silicon-aluminum-calcium-barium alloy, and the method adopts a sample and a mixed flux (anhydrous sodium carbonate: boric acid: potassium nitrate=3:2:1) to be placed in a muffle furnace at 950 ℃ together with graphite powder, and then fused into a molten ball; then placing the molten ball and lithium tetraborate together in a platinum crucible, melting into glass fuse pieces in a high-temperature electric melting furnace, and measuring by using an X-ray fluorescence spectrometry; the method for measuring barium and strontium in the barite by using the inductively coupled plasma emission spectrometry has low accuracy and precision because the content of the barium in the barite is very high (more than 25 percent); the method adopts nitric acid and hydrofluoric acid to dissolve the sample, and adopts a barium sulfate weight method to measure after filtering and residue treatment, and the method has complex operation and long process.
Disclosure of Invention
The invention aims to provide a method for measuring the light-emitting diode of the invention, which has the advantages of high sensitivity, high measuring speed, simple and convenient operation, small interference compared with other methods and good selectivity; by adopting a vertical observation method, the measurement stability is improved, and the internal standard ICP-OES for providing accurate data for the control process of smelting components can be used for measuring barium in silicon-barium, silicon-aluminum-barium and silicon-calcium-barium.
In order to solve the technical problems, the invention adopts the following technical scheme:
the invention relates to a method for measuring barium by internal standard-ICP-OES, which comprises the following steps:
step 1: weighing sodium hydroxide, melting the sodium hydroxide in a cleaned and dried corundum crucible, cooling to room temperature,
weighing a sample in the corundum crucible, adding sodium peroxide and the sample, uniformly stirring, and covering sodium peroxide in a muffle furnace to melt until the sample is completely decomposed; taking out, cooling to room temperature, and taking a blank sample;
step 2: placing the cooled corundum crucible in a beaker, adding 65-75 ℃ warm water and hydrochloric acid to leach the clinker, transferring the sample and blank sample solution into a volumetric flask, and diluting with high-purity water to a scale;
step 3: adding hydrochloric acid into a 250mL volumetric flask, accurately adding yttrium standard solution, diluting to scale with high-purity water, shaking, and waiting for loading;
step 4: preparation of standard calibration Curve solution
Barium single element standard solution: the concentration is 1000 mug/mL, and is derived from the national standard substance center;
yttrium single element standard solution: the concentration is 1000 mug/mL, and is derived from the national standard substance center;
6 parts of hydrochloric acid is taken in a volumetric flask, barium unitary element standard solution is added, and the solutions are prepared to contain Ba0, 0.50, 1.00, 5.00, 7.50 and 10.00 percent respectively, then 5.00mL of yttrium standard solution with the concentration of 50ug/mL is accurately added, and the solution is diluted to scale by high-purity water and is uniformly shaken. The solution is used for preparing a standard curve;
step 5: selecting spectral lines
Determining Ba standard solution, adjusting spectral line position, and determining Ba455.403 nm as analysis line and Y371.03nm as analysis line;
step 6: drawing a calibration curve: introducing a standard calibration curve solution into an inductively coupled plasma emission spectrometer, measuring the signal intensity of Ba and Y ions, and drawing a calibration curve by taking the mass percent as an abscissa and the signal intensity ratio of the Ba and Y ions as an ordinate;
step 7: introducing a sample solution of a sample and a blank sample solution into an inductively coupled plasma emission spectrometer, measuring the signal intensity of Ba and Y ions, and solving the content of Ba in the sample solution according to a standard solution calibration curve with known mass percent;
the content of barium element in the sample is calculated according to the following formula:
W%=W i -W 0
wherein: w is the mass percentage of elements in the sample;
W 0 -the mass percentage of the element in the blank solution to be measured;
W i -the mass percentage of the element in the sample to be measured.
Further, the measuring instrument is Optima 5300DV (PE company of America); the observation mode is vertical observation.
Furthermore, the detection range of the method is 0.10 at% to 35.0at% of Ba.
Compared with the prior art, the invention has the beneficial technical effects that:
1. according to the invention, only 2g of sodium hydroxide, 2g of sodium peroxide and 15mL of hydrochloric acid are used, so that less chemical reagent is used, and materials are saved; the invention has simple operation, completes the measurement within 3 hours, and shortens the operation flow and the measurement time.
2. The signal intensity of the barium is reduced by adopting a vertical observation mode, so that the measurement range is enlarged, the measurement stability is improved, and the measurement result has high sensitivity and more accurate result.
3. The internal standard method is to eliminate the error caused by instrument drift to a certain extent by measuring the relative value of the barium element and the yttrium internal standard, so that the accuracy and precision of the measurement result are high; the output signal of the barium element can be controlled within the optimal detection range (1X 104-3X 106) of the ICP-OES spectrometer, so that the measurement stability is improved, and the sensitivity of the measurement result is high.
The internal standard ICP-OES is used for measuring the barium content of the deoxidizer such as silicon barium, silicon aluminum barium, silicon calcium barium and the like, wherein the barium content is 0.10at percent to 35.0at percent. The invention has good application effect through multiple tests on silicon barium, silicon aluminum barium and silicon calcium barium samples. The invention has the characteristics of wide linear range, high sensitivity, simple operation, high analysis speed and accurate and reliable analysis result, and provides reliable data for detection of barium in silicon-barium, silicon-aluminum-barium and silicon-calcium-barium.
Detailed Description
The invention will be further illustrated with reference to specific examples.
In the examples of the present invention, the reagents used are preferably:
sodium hydroxide; sodium peroxide;
hydrochloric acid: high-grade purity;
barium single element standard solution: the concentration is 1000 mug/mL, and is derived from the national standard substance center; yttrium single element standard solution: the concentration is 1000 mug/mL, and is derived from the national standard substance center; 250mL volumetric flask; corundum crucible; argon: argon purity is more than or equal to 99.9%; compressed air.
Preferably, the model of the inductively coupled plasma emission spectrometer is PE company Optima 5300DV; the observation mode is vertical observation.
A method for measuring barium by internal standard-ICP-OES, comprising:
1. sample analysis
2g of sodium hydroxide is weighed, melted in a cleaned and dried corundum crucible, and cooled to room temperature.
Weighing 0.1000g of sample into the corundum crucible, adding 1g of sodium peroxide and stirring the sample uniformly, and then covering 1g of sodium peroxide and melting the mixture in a muffle furnace at 750 ℃ for 15min until the sample is completely decomposed. Taking out, cooling to room temperature, placing in a 300mL beaker, adding 70 ℃ warm water 80mL, (1+1) hydrochloric acid 20mL to leach the frit, transferring the solution into a 250mL volumetric flask, and diluting the solution to a scale with high-purity water. And (3) separating 50mL to 250mL of the test solution, adding 10mL of (1+1) hydrochloric acid into a volumetric flask, accurately adding 5.00mL of 50ug/mL yttrium standard solution, diluting to a scale with high-purity water, shaking uniformly, and waiting for loading. Along with blank sample
Preparation of standard calibration Curve solution
Weighing 6 parts of (1+1) hydrochloric acid 10mL in a 250mL volumetric flask, adding a barium unitary element standard solution, preparing solutions containing Ba0, 0.50, 1.00, 5.00, 7.50 and 10.00% respectively, accurately adding 5.00mL of yttrium standard solution of 50ug/mL, diluting to scale with high-purity water, and shaking uniformly. The solution was used to make a standard curve.
Selecting spectral lines:
ba455.403 nm as analysis line and Y371.03nm as analysis line.
The content of barium element in the sample is calculated according to the following formula:
W%=W i -W 0
wherein: w is the mass percentage of elements in the sample;
W 0 -the mass percentage of the element in the blank solution to be measured;
W i -the mass percentage of the element in the sample to be measured;
the detection range of the method is 0.10 at% to 35.0at% of Ba.
Example 1
Working curves were prepared according to the above method, the curve correlation coefficient r of barium was 0.99991, and the measurement was performed by preparing 11 parts of blank solution 3 times according to the detection limit formula C defined by International Union of Pure and Applied Chemistry (IUPAC) L =3S b /k(S b For standard deviation of the blank, k is the corresponding calibration curve slope) the method detection limit Ba is calculated to be 0.011%.
Example 2
The internal standard method-ICP-OES method was used to measure standard substances such as silicon aluminum calcium barium (YSB 14612-2007), (YSB 14613-2007), (YSB 14610-2007), silicon aluminum barium (YSB 14608-2001), silicon calcium barium (YSB 14605) and silicon barium alloy (GBW (E) 010393). The results are shown in Table 1.
TABLE 1 Standard sample measurement results
Example 3
Weigh sample 3 of Si-Ca-Ba # 、4 # The barium was measured by the method and the acid-soluble barium sulfate weight method, respectively, and the results are shown in Table 2.
TABLE 2 measurement results of silicon calcium barium samples
Example 4
Labeling and recycling experiments:
and weighing a standard sample, performing a standard adding recovery experiment, and comparing the measurement result with the identification value. Table 3.
TABLE 3 labeled recovery test
Example 5
The precision of the method is as follows:
under the selected experimental method, weighing silicon calcium barium samples No. 5 and No. 6, preparing 11 sample solutions in parallel, and performing precision investigation. The Standard Deviation (SD) and the Relative Standard Deviation (RSD) of the measurement results of the respective components were calculated, and Table 4.
TABLE 4 results of precision experiments
Therefore, through the verification of the embodiment example, the method for the barium in the silicon-barium alloy, the silicon-aluminum-barium and the silicon-calcium-barium, disclosed by the invention, adopts a vertical observation mode to reduce the signal intensity of the barium, so that the measurement range is enlarged, the measurement stability is improved by an internal standard method, and the measurement result has high sensitivity and more accurate result.
The internal standard-ICP-OES is used for measuring the barium content of the silicon-barium alloy, the silicon-aluminum-barium and the silicon-calcium-barium, wherein the barium content is 0.10at percent to 35.0at percent. The invention has good application effect through multiple tests on silicon-barium alloy, silicon-aluminum-barium and silicon-calcium-barium samples. The invention has the characteristics of wide linear range, high sensitivity, simple operation, high analysis speed and accurate and reliable analysis result, and provides reliable data for the detection of barium in silicon-barium alloy, silicon-aluminum-barium and silicon-calcium-barium.
The above embodiments are only illustrative of the preferred embodiments of the present invention and are not intended to limit the scope of the present invention, and various modifications and improvements made by those skilled in the art to the technical solutions of the present invention should fall within the protection scope defined by the claims of the present invention without departing from the design spirit of the present invention.

Claims (3)

1. A method for measuring barium by internal standard-ICP-OES, comprising the steps of:
step 1: weighing sodium hydroxide, melting the sodium hydroxide in a cleaned and dried corundum crucible, cooling to room temperature,
weighing a sample in the corundum crucible, adding sodium peroxide and the sample, uniformly stirring, and covering sodium peroxide in a muffle furnace to melt until the sample is completely decomposed; taking out, cooling to room temperature, and taking a blank sample;
step 2: placing the cooled corundum crucible in a beaker, adding 65-75 ℃ warm water and hydrochloric acid to leach the clinker, transferring the sample and blank sample solution into a volumetric flask, and diluting with high-purity water to a scale;
step 3: adding hydrochloric acid into a 250mL volumetric flask, accurately adding yttrium standard solution, diluting to scale with high-purity water, shaking, and waiting for loading;
step 4: preparation of standard calibration Curve solution
Barium single element standard solution: the concentration is 1000 mug/mL, and is derived from the national standard substance center;
yttrium single element standard solution: the concentration is 1000 mug/mL, and is derived from the national standard substance center;
6 parts of hydrochloric acid is taken in a volumetric flask, barium unitary element standard solution is added, and the solutions are prepared to contain Ba0, 0.50, 1.00, 5.00, 7.50 and 10.00 percent respectively, then 5.00mL of yttrium standard solution with the concentration of 50ug/mL is accurately added, and the solution is diluted to scale by high-purity water and is uniformly shaken. The solution is used for preparing a standard curve;
step 5: selecting spectral lines
Determining Ba standard solution, adjusting spectral line position, and determining Ba455.403 nm as analysis line and Y371.03nm as analysis line;
step 6: drawing a calibration curve: introducing a standard calibration curve solution into an inductively coupled plasma emission spectrometer, measuring the signal intensity of Ba and Y ions, and drawing a calibration curve by taking the mass percent as an abscissa and the signal intensity ratio of the Ba and Y ions as an ordinate;
step 7: introducing a sample solution of a sample and a blank sample solution into an inductively coupled plasma emission spectrometer, measuring the signal intensity of Ba and Y ions, and solving the content of Ba in the sample solution according to a standard solution calibration curve with known mass percent;
the content of barium element in the sample is calculated according to the following formula:
W%=W i -W 0
wherein: w is the mass percentage of elements in the sample;
W 0 -the mass percentage of the element in the blank solution to be measured;
W i -the mass percentage of the element in the sample to be measured.
2. The method for measuring barium by internal standard-ICP-OES according to claim 1, wherein the measuring instrument is Optima 5300DV; the observation mode is vertical observation.
3. The method for measuring barium by internal standard-ICP-OES as claimed in claim 1, wherein the detection range of the method is 0.10 at% to 35.0at%.
CN202310600375.0A 2023-05-25 2023-05-25 Method for measuring barium by internal standard-ICP-OES Pending CN116735565A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202310600375.0A CN116735565A (en) 2023-05-25 2023-05-25 Method for measuring barium by internal standard-ICP-OES

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202310600375.0A CN116735565A (en) 2023-05-25 2023-05-25 Method for measuring barium by internal standard-ICP-OES

Publications (1)

Publication Number Publication Date
CN116735565A true CN116735565A (en) 2023-09-12

Family

ID=87907170

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202310600375.0A Pending CN116735565A (en) 2023-05-25 2023-05-25 Method for measuring barium by internal standard-ICP-OES

Country Status (1)

Country Link
CN (1) CN116735565A (en)

Similar Documents

Publication Publication Date Title
CN102253030B (en) Method for determining impurity content in high-titanium slag
CN107976481B (en) Method for detecting scandium content in traditional Chinese medicinal materials
CN103604823A (en) Method for measuring contents of potassium, sodium, lead and zinc in iron ore
CN113295676A (en) Method for measuring calcium, aluminum and barium in deoxidizer
CN113049654A (en) Method for analyzing content of fluorine ions in dolomite, limestone and lime
CN112014379A (en) Method for measuring calcium oxide in limestone and dolomite
CN111122549A (en) Method for measuring magnesium oxide, potassium oxide, manganese oxide, titanium oxide and silicon dioxide in limestone and dolomite
CN116735565A (en) Method for measuring barium by internal standard-ICP-OES
CN107389716A (en) The method of impurity in x-ray fluorescence spectrometry Copper Ores
CN114739982A (en) Method for detecting element content in glass
CN113295760A (en) Method for simultaneously measuring low contents of lanthanum, cerium, praseodymium, neodymium, samarium and barium in furnace slag and mold powder
CN108414505A (en) A kind of method of copper, lead, Zn-ef ficiency content in measurement silver alloy
CN111239172A (en) Method for determining phosphorus content in coal
JPS6362695B2 (en)
CN110261535A (en) Indium content measuring method in a kind of high-purity indium oxide
CN112763439A (en) Method for determining boron element in refining slag of gear steel
CN110715913A (en) Method for measuring selenium in geochemical sample by atomic fluorescence spectrometry
CN112129744A (en) Chemical phase analysis method for lithium in ore
CN114609121A (en) Method for measuring ferric oxide and aluminum oxide in limestone and dolomite
LU504019B1 (en) Method for determining contents of major elements, trace elements and rare earth elements in cobalt-rich crusts and polymetallic nodules
CN113030286B (en) Determination of hexamethyldisilazane content in tris (trimethylsilyl) phosphate
CN110108593B (en) Method for detecting titanium content in carbon material
CN114354580A (en) Method for measuring contents of potassium, sodium, lead, zinc and copper elements in iron ore, furnace slag, blast furnace dust and iron-containing tail mud
CN117849028A (en) Method for measuring calcium fluoride and silicon dioxide in fluorite
CN117517294A (en) Method for synchronously analyzing multiple elements in metallurgical sintering material and pellet and application thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination