CN112730726A - Method for measuring content of metal loaded in catalyst - Google Patents
Method for measuring content of metal loaded in catalyst Download PDFInfo
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- CN112730726A CN112730726A CN202011591539.0A CN202011591539A CN112730726A CN 112730726 A CN112730726 A CN 112730726A CN 202011591539 A CN202011591539 A CN 202011591539A CN 112730726 A CN112730726 A CN 112730726A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 144
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 133
- 239000002184 metal Substances 0.000 title claims abstract description 123
- 238000000034 method Methods 0.000 title claims abstract description 59
- 238000010438 heat treatment Methods 0.000 claims abstract description 31
- 238000011282 treatment Methods 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000001035 drying Methods 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims abstract description 21
- 239000011148 porous material Substances 0.000 claims abstract description 20
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002253 acid Substances 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 238000003795 desorption Methods 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 8
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 8
- 238000001514 detection method Methods 0.000 claims abstract description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 44
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 24
- 229910017604 nitric acid Inorganic materials 0.000 claims description 24
- 238000007781 pre-processing Methods 0.000 claims description 9
- 239000011261 inert gas Substances 0.000 claims description 3
- 238000004255 ion exchange chromatography Methods 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 2
- 239000010949 copper Substances 0.000 description 30
- 238000005303 weighing Methods 0.000 description 28
- 238000012360 testing method Methods 0.000 description 27
- 230000004580 weight loss Effects 0.000 description 23
- 230000000052 comparative effect Effects 0.000 description 18
- 239000000203 mixture Substances 0.000 description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 16
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 16
- 229910052802 copper Inorganic materials 0.000 description 16
- 230000000694 effects Effects 0.000 description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 238000000605 extraction Methods 0.000 description 12
- SAGKTTMILSKORU-UHFFFAOYSA-N [Cr+3].[Ag+] Chemical compound [Cr+3].[Ag+] SAGKTTMILSKORU-UHFFFAOYSA-N 0.000 description 10
- DSMZRNNAYQIMOM-UHFFFAOYSA-N iron molybdenum Chemical compound [Fe].[Fe].[Mo] DSMZRNNAYQIMOM-UHFFFAOYSA-N 0.000 description 10
- -1 meanwhile Substances 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 9
- 150000002739 metals Chemical class 0.000 description 9
- 239000000126 substance Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 239000006259 organic additive Substances 0.000 description 8
- 229910052755 nonmetal Inorganic materials 0.000 description 7
- 239000003610 charcoal Substances 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 6
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 5
- 238000007599 discharging Methods 0.000 description 5
- 229910052749 magnesium Inorganic materials 0.000 description 5
- 239000011777 magnesium Substances 0.000 description 5
- 229910000861 Mg alloy Inorganic materials 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000005470 impregnation Methods 0.000 description 4
- 238000010998 test method Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 229910017052 cobalt Inorganic materials 0.000 description 3
- 239000010941 cobalt Substances 0.000 description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 3
- 239000013256 coordination polymer Substances 0.000 description 3
- 239000003546 flue gas Substances 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 239000011591 potassium Substances 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 238000010828 elution Methods 0.000 description 2
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- HRYZWHHZPQKTII-UHFFFAOYSA-N chloroethane Chemical compound CCCl HRYZWHHZPQKTII-UHFFFAOYSA-N 0.000 description 1
- QPJDMGCKMHUXFD-UHFFFAOYSA-N cyanogen chloride Chemical compound ClC#N QPJDMGCKMHUXFD-UHFFFAOYSA-N 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 229960003750 ethyl chloride Drugs 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/96—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation using ion-exchange
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/8868—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample elemental analysis, e.g. isotope dilution analysis
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (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)
- Catalysts (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for measuring the content of metal loaded in a catalyst, which comprises the following steps: pretreatment: drying the catalyst in a vacuum environment for 0-1.5 h; and (3) reaming treatment: placing the dried catalyst in a tubular furnace or a heating furnace, firstly adjusting to an oxygen-free atmosphere, then heating to 700-; desorption treatment and detection calculation: adding mixed acid into the catalyst after pore expansion treatment, heating, stirring and dissolving, filtering to obtain an extract liquid, measuring the metal content in the extract liquid, and converting the metal content loaded in the catalyst. The invention provides a method for measuring the content of metal loaded in a catalyst, which can accurately measure the content of the metal loaded in the catalyst by carrying out pore-expanding treatment on the catalyst by using water vapor or carbon dioxide, wherein the deviation between the measured value of each metal element in the catalyst and a theoretical value is less than 10 percent.
Description
Technical Field
The invention relates to the technical field of catalysts, in particular to a method for measuring the content of a metal loaded in a catalyst.
Background
The catalyst special for civil air defense takes columnar activated carbon with the grain diameter of 0.9mm as a basic template (namely a catalyst carrier), and different types of metal element oxides (usually copper, chromium, silver, molybdenum, zinc and other metal elements, but other different types of elements can also be contained) with different contents are loaded in the activated carbon by an impregnation process, so that the catalyst not only has excellent physical adsorption capacity, but also has a certain chemical catalysis effect. Besides the capability of adsorbing common poisonous and harmful gases such as benzene vapor, ethyl chloride and the like, the adsorbent also has the capability of adsorbing extremely toxic gases such as cyanogen chloride, hydrocyanic acid and the like. The impregnation process is that the metal active substance is firstly absorbed in the pores of the activated carbon in the form of solution, and then the solvent is volatilized by high-temperature calcination, so that the metal oxide is remained to be continuously attached in the pores of the activated carbon to play the role of chemical catalysis.
The metal substance loaded in the catalyst directly determines the application performance of the catalyst, so that the metal element loaded in the catalyst is accurately measured, and the method has great significance for pre-judging the application performance of the catalyst. The procedure for testing the metal content in the catalyst is as follows: burning the catalyst in a muffle furnace at high temperature; burning the residue in acid or alkali solution to extract the metal element in the residue into the solution; and (3) quantitatively titrating the content of metal substances in the extract liquor aiming at different metals, and then calculating the content of the metals in the catalyst through content conversion.
The existing method for measuring the metal content in the catalyst still has the following problems:
the metal element in the burning residue has two sources, firstly, the metal element is loaded on the catalyst substrate by impregnation in the preparation process of the catalyst, and the metal element exists in micropores of the catalyst and is the root cause of the catalytic performance of the catalyst; another source is the metal elements contained in the catalyst matrix itself, which are deeply buried in the catalyst matrix and do not play a catalytic role. It is statistically estimated that even a good catalyst substrate will have nearly 8% ash (i.e., the burned residues) resulting in an extract extracted as the burned residues and not truly representative of the amount of supported metal of the catalyst.
In addition, the high-temperature ignition of the catalyst is a violent oxidation reaction, along with the generation of a large amount of flue gas, a part of metal load can be scattered and lost along with the flue gas, meanwhile, metals with low evaporation temperature such as potassium, magnesium, barium and the like can be loaded when the metals are loaded, metal steam can be formed by the metal elements under the high-temperature ignition at the temperature of about 900 ℃, so that the loss of the metal elements is more, and the metal content in the ignition parameter can not represent the load metal amount of the real catalyst under the two conditions. Although there is also a method of extracting the metal in the catalyst directly with a solvent to obtain a metal extract, direct extraction cannot effectively extract the metal-impregnated material from the metal carrier in its entirety.
At present, no mature method exists, the metal loaded in the catalyst can be effectively extracted by the extraction liquid, and even if the metal can be nearly completely extracted by multiple multistage extraction, no means for representing the content of all the metals in the extraction liquid by a systematic effective method exists.
Therefore, a determination method capable of accurately measuring the content of the supported metal in the catalyst is a problem to be solved by those skilled in the art.
Disclosure of Invention
In view of the above, the present invention provides a method for measuring the content of a metal supported in a catalyst, in which a pore-expanding treatment is performed on the catalyst by using water vapor or carbon dioxide to expand the pore diameter of micropores in a catalyst carrier, so as to facilitate elution of the metal element supported in the micropores in a subsequent step. Because the steps of pretreatment and hole expanding treatment are carried out, all the metal elements loaded in the catalyst can be extracted by simply mixing and extracting the extract liquor in the extraction process.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for determining the content of a metal supported in a catalyst, comprising the steps of:
s1, preprocessing: drying the catalyst for 0-1.5h in a vacuum environment;
s2, hole expanding treatment: placing the dried catalyst in a tubular furnace or a heating furnace, firstly adjusting to an oxygen-free atmosphere, then heating to 700-;
s3, desorption processing and detection calculation: adding mixed acid into the catalyst after pore expansion treatment, heating, stirring and dissolving, filtering to obtain an extract liquid, measuring the metal content in the extract liquid, and converting the metal content loaded in the catalyst.
Preferably, in step S1, the drying is performed under the conditions of a vacuum degree of-0.05 MPa to-0.09 MPa and a temperature of 60-150 ℃.
The technical effect of adopting the technical scheme is as follows: the volatile organic additives, water and other non-metallic components added in the preparation process of the catalyst can be fully removed, and the accuracy of the detection result is improved.
Preferably, in step S2, the tube furnace or the heating furnace is adjusted to an oxygen-free atmosphere by charging inert gas.
Preferably, in step S2, heating is performed to 700-900 ℃ at a rate of 2-20 ℃/min.
Preferably, in step S2, the flow rate of the introduced water vapor or carbon dioxide is 5-20mL/min, and the time is 5-20 min.
The technical effect of adopting the technical scheme is as follows: the aperture of the catalyst carrier is divided into micropores, mesopores and macropores, wherein the radius of the micropores is less than 2nm, the radius of the mesopores is 2-50 nm, and the radius of the macropores is more than 50 nm. The metal element supported in the catalyst is mostly present in the mesopores of the catalyst, but a small amount of the metal element is present in the micropores of the catalyst carrier, and the metal element is hardly eluted from the micropores because the particle diameter of the metal active material is close to the pore diameter, so that a pore-enlarging treatment of the catalyst is required. The pore-enlarging treatment is performed on the catalyst by using water vapor or carbon dioxide to enlarge the pore diameter of the micropores in the catalyst carrier so as to facilitate the elution of the metal elements loaded in the micropores in the subsequent step.
The rule of the reaming process is as follows: at the same gas concentration and temperature, water vapor is more effective in reaming pores than carbon dioxide because water vapor is more reactive with C. Meanwhile, the higher the concentration of the introduced gas is, the faster the reaction rate is, the easier the hole expansion is realized, and the effect of adjusting the concentration of the gas is the same as the effect of increasing the temperature of the hole expansion.
Preferably, in step S3, the mixed acid is hydrofluoric acid and nitric acid, the concentration of the hydrofluoric acid is 40-50%, and the concentration of the nitric acid is 65-68%.
Preferably, the volume usage ratio of the hydrofluoric acid to the nitric acid is (3-10): (5-20).
The technical effect of adopting the technical scheme is as follows: HNO3+ HF mixed acid, the solution having strong acidity and strong oxidizing property (NO)3 -) And strong coordination ability to elements of high valency (F)-) Besides being able to dissolve conventional metal elements, are particularly suitable for dissolving transition elements (benefiting from F)-Coordination of ions) to extract the supported metal elements efficiently.
Preferably, in step S3, the usage ratio of the catalyst after pore expansion treatment to the mixed acid is (0.1-0.5) g: (8-30) mL.
Preferably, in step S3, the dissolution temperature is lower than 150 ℃ for 5-30 min.
The technical effect of adopting the technical scheme is as follows: preventing the temperature from being too high so as to avoid splashing.
Preferably, in step S3, the stirring rate is 0-50 r/min.
Preferably, in step S3, the metal content in the extract is determined by ICP ion chromatography.
According to the technical scheme, compared with the prior art, the method for measuring the content of the metal loaded in the catalyst disclosed by the invention has the following beneficial effects:
(1) the invention discloses a method for measuring the content of metal loaded in a catalyst, which is characterized in that steam or carbon dioxide is utilized to perform pore-expanding treatment on the catalyst, so that the pore diameter of micropores in a catalyst carrier is enlarged, and the metal element loaded in the micropores can be conveniently eluted in the subsequent steps. Because the steps of pretreatment and hole expanding treatment are carried out, all the metal elements loaded in the catalyst can be extracted by simply mixing and extracting the extract liquor in the extraction process.
(2) According to the method for measuring the content of the metal loaded in the catalyst, the deviation of the test result of the content of each metal element and a theoretical value can be within 10%, and the minimum average deviation can be-0.1%.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment of the invention provides a method for measuring the content of a metal loaded in a catalyst, which comprises the following steps:
s1, preprocessing: drying the catalyst in a vacuum environment for 0-1.5 h;
s2, hole expanding treatment: placing the dried catalyst in a tubular furnace or a heating furnace, firstly adjusting to an oxygen-free atmosphere, then heating to 700-;
s3, desorption processing and detection calculation: adding the catalyst after pore expansion treatment into mixed acid, heating, stirring and dissolving, filtering to obtain an extract liquid, measuring the metal content in the extract liquid, and converting the metal content loaded in the catalyst.
In order to further optimize the technical scheme, in step S1, drying is carried out under the conditions that the vacuum degree is-0.05 MPa to-0.09 MPa and the temperature is 60-150 ℃.
In order to further optimize the above technical solution, in step S2, the tube furnace or the heating furnace is adjusted to an oxygen-free atmosphere by filling inert gas.
In order to further optimize the above technical solution, in step S2, heating to 700-900 deg.C at a rate of 2-20 deg.C/min
In order to further optimize the technical scheme, in the step S2, the flow of the introduced water vapor or carbon dioxide is 5-20mL/min, and the time is 5-20 min.
In order to further optimize the technical scheme, in step S3, the mixed acid is hydrofluoric acid and nitric acid, the concentration of the hydrofluoric acid is 40-50%, and the concentration of the nitric acid is 65-68%.
In order to further optimize the technical scheme, the volume usage ratio of hydrofluoric acid to nitric acid is (3-10): (5-20).
In order to further optimize the above technical solution, in step S3, the usage ratio of the catalyst after pore expansion treatment to the mixed acid is (0.1-0.5) g: (8-30) mL.
In order to further optimize the above technical scheme, in step S3, the dissolving temperature is lower than 150 ℃ and the time is 5-30 min.
The technical effect of adopting the technical scheme is as follows: preventing the temperature from being too high so as to avoid splashing.
In order to further optimize the above technical solution, in step S3, the stirring speed is 0-50 r/min.
In order to further optimize the above technical solution, in step S3, the metal content in the extract was determined by ICP ion chromatography.
The catalyst tested in the examples of the present invention is a catalyst sample prepared by using activated carbon with a particle size of 0.9mm as a carrier, wherein the activated carbon carrier itself contains calcium and magnesium components, and the metals loaded on the activated carbon carrier by an impregnation process are as follows: copper, chromium, silver, iron, molybdenum, potassium;
the contents of the metal species in the catalysts were tested in the test manners of examples 1 to 3 and comparative examples 1 to 2, and the kinds and contents of the metals in the catalysts were as follows:
example 1
This example provides a method for determining the content of a metal supported on a catalyst, including the steps of:
s1, preprocessing:
weighing 5.00g of catalyst sample, recording the weight as m0, placing the catalyst sample in a vacuum oven, drying for 1h under the conditions of-0.06 MPa vacuum degree and 70 ℃, taking out the sample after drying, weighing the mass of the residual sample, recording the mass as m1 to 4.90g, and obtaining m1 as desorbed organic additives, moisture and other non-metal components; this procedure is reported as weight loss a 1% ═ 2%.
S2, hole expanding treatment:
placing the pretreated catalyst sample in a tubular furnace, introducing nitrogen, discharging air in the furnace, heating to 800 ℃ at the temperature of 10 ℃/min, introducing water vapor for 15min, wherein the flow rate of the water vapor is 10mL/min, obtaining a sample, weighing the sample, and weighing the sample, wherein the weight of the sample is m2, and the weight of m2 is 3.8 g; under the condition of high temperature of water vapor, the catalyst can react with (C + H) while expanding pores2O＝CO+H2High temperature), charcoal was consumed and weight loss Δ m2 ═ 1.10 g; this step is reported as weight loss a 2% ═ 22.45%.
S3, desorption treatment:
weighing 0.25 +/-0.001 g of the pore-expanded catalyst, placing the catalyst in a crucible, adding 3ml of hydrofluoric acid and 5ml of nitric acid, wherein the concentration of the hydrofluoric acid is 50% and the concentration of the nitric acid is 65%, stirring and heating the mixture to the solution temperature of 50 ℃, the stirring speed is 30r/min, dissolving the mixture for 30min, and then filtering the mixture through a funnel to obtain an extract.
And (3) CP testing:
1ml of the extract was taken and the metal content in the extract was measured by ICP. It is shown that in the catalyst, the supported metal content is:
| metal content | Copper (Cu) | Chromium (III) | Silver (Ag) | Iron | Molybdenum (Mo) | Potassium salt |
| The content wt% | 7.97％ | 1.27％ | 0.03％ | 2.03％ | 1.05％ | 1.01％ |
And (3) conversion of content:
after the pretreatment in the first step, the weight loss of the materials is as follows: when a1 is 2.00% and a2 is 22.45%, the metal content in the catalyst is:
| metal content | Copper (Cu) | Chromium (III) | Silver (Ag) | Iron | Molybdenum (Mo) | Potassium salt |
| Reduced content wt% | 6.06％ | 1.10％ | 0.03％ | 2.03％ | 1.01％ | 0.99％ |
Example 2
This example provides a method for determining the content of a metal supported on a catalyst, including the steps of:
s1, preprocessing:
weighing 5.00g of catalyst sample, recording the weight as m0, placing the catalyst sample in a vacuum oven, drying for 1h under the conditions of-0.06 MPa vacuum degree and 70 ℃, taking out the sample after drying, weighing the mass of the residual sample, recording the mass as m1 to 4.90g, and obtaining m1 as desorbed organic additives, moisture and other non-metal components; this procedure is reported as weight loss a 1% ═ 2%.
S2, hole expanding treatment:
placing the pretreated catalyst sample in a tubular furnace, introducing nitrogen, discharging air in the furnace, heating to 900 ℃ at the temperature of 10 ℃/min, introducing water vapor for 15min, wherein the flow rate of the water vapor is 10mL/min, obtaining a sample, weighing the sample, and the weight of the sample is m2, and the weight of m2 is 3.2 g; under the condition of high temperature of water vapor, the catalyst can react with (C + H) while expanding pores2O＝CO+H2High temperature), charcoal was consumed, Δ m2 ═ 1.70 g; this step is reported as weight loss a 2% ═ 34.69%.
S3, desorption treatment:
weighing 0.25 +/-0.001 g of the pore-expanded catalyst, placing the catalyst in a crucible, adding 3ml of hydrofluoric acid and 5ml of nitric acid, wherein the concentration of the hydrofluoric acid is 50% and the concentration of the nitric acid is 65%, stirring and heating the mixture to the solution temperature of 50 ℃, the stirring speed is 30r/min, dissolving the mixture for 30min, and then filtering the mixture through a funnel to obtain an extract.
ICP test:
1ml of the extract was taken and the metal content in the extract was measured by ICP. It is shown that in the catalyst, the supported metal content is:
| metal content | Copper (Cu) | Chromium (III) | Silver (Ag) | Iron | Molybdenum (Mo) | Potassium salt | Calcium carbonate | Magnesium alloy |
| The content wt% | 9.48％ | 1.74％ | 0.05％ | 3.06％ | 1.55％ | 1.56％ | 0.10％ | 0.03％ |
And (3) conversion of content:
after the pretreatment in the first step, the weight loss of the materials is as follows: when m0-m1 is 0.10g, i.e., a loss of 2%, the metal content in the catalyst is:
| metal content | Copper (Cu) | Chromium (III) | Silver (Ag) | Iron | Molybdenum (Mo) | Potassium salt | Calcium carbonate | Magnesium alloy |
| Reduced content wt% | 5.92％ | 1.13％ | 0.03％ | 1.86％ | 0.99％ | 1.01％ | 0.06％ | 0.02％ |
Example 3
This example provides a method for determining the content of a metal supported on a catalyst, including the steps of:
s1, preprocessing:
weighing 5.00g of catalyst sample, recording the weight as m0, placing the catalyst sample in a vacuum oven, drying for 1h under the conditions of-0.06 MPa vacuum degree and 70 ℃, taking out the sample after drying, weighing the mass of the residual sample, recording the mass as m1 to 4.90g, and obtaining m1 as desorbed organic additives, moisture and other non-metal components; this procedure is reported as weight loss a 1% ═ 2%.
S2, hole expanding treatment:
placing the pretreated catalyst sample in a tubular furnace, introducing nitrogen, discharging air in the furnace, heating to 700 ℃ at the temperature of 10 ℃/min, introducing water vapor for 5min, wherein the flow rate of the water vapor is 10mL/min, obtaining a sample, weighing the sample, and weighing the sample, wherein the weight of the sample is m2, and the weight of m2 is 4.6 g; under the condition of high temperature of water vapor, the catalyst can react with (C + H) while expanding pores2O＝CO+H2High temperature), charcoal was consumed, Δ m2 ═ 0.3 g; this step is reported as weight loss a 2% ═ 6.12%.
S3, desorption treatment:
weighing 0.25 +/-0.001 g of the pore-expanded catalyst, placing the catalyst in a crucible, adding 3ml of hydrofluoric acid and 5ml of nitric acid, wherein the concentration of the hydrofluoric acid is 50% and the concentration of the nitric acid is 65%, stirring and heating the mixture to the solution temperature of 50 ℃, the stirring speed is 30r/min, dissolving the mixture for 30min, and then filtering the mixture through a funnel to obtain an extract.
ICP testing;
1ml of the extract was taken and the metal content in the extract was measured by ICP. It is shown that in the catalyst, the supported metal content is:
| metal content | Copper (Cu) | Chromium (III) | Silver (Ag) | Iron | Molybdenum (Mo) | Potassium salt |
| The content wt% | 6.39％ | 1.12％ | 0.03％ | 2.07％ | 1.03％ | 1.03％ |
And (3) conversion of content:
after the pretreatment in the first step, the weight loss of the materials is as follows: when m0-m1 is 0.10g, i.e., a loss of 2%, the metal content in the catalyst is:
| metal content | Copper (Cu) | Chromium (III) | Silver (Ag) | Iron | Molybdenum (Mo) | Potassium salt |
| Reduced content wt% | 5.88％ | 1.03％ | 0.03％ | 1.90％ | 0.95％ | 0.95％ |
Comparative example 1
This comparative example provides a method for determining the content of a metal supported in a catalyst, comprising the steps of:
s1, preprocessing:
weighing 5.00g of catalyst sample, recording the weight as m0, placing the catalyst sample in a vacuum oven, drying for 1h under the conditions of-0.06 MPa vacuum degree and 70 ℃, taking out the sample after drying, weighing the mass of the residual sample, recording the mass as m1 to 4.90g, and obtaining m1 as desorbed organic additives, moisture and other non-metal components; this procedure is reported as weight loss a 1% ═ 2%.
S2, hole expanding treatment:
placing the pretreated catalyst sample in a tubular furnace, introducing nitrogen, discharging air in the furnace, heating to 500 ℃ at the temperature of 10 ℃/min, introducing water vapor for 15min, wherein the flow rate of the water vapor is 10mL/min, samples were obtained and weighed to a weight of m2, m2 ═ 4.88 g; under the condition of high temperature of water vapor, the catalyst can react with (C + H) while expanding pores2O＝CO+H2High temperature), charcoal was consumed, Δ m2 ═ 0.02 g; this step was recorded as a weight loss a 2% ═ 0.4%.
S3, desorption treatment:
weighing 0.25 +/-0.001 g of the pore-expanded catalyst, placing the catalyst in a crucible, adding 3ml of hydrofluoric acid and 5ml of nitric acid, wherein the concentration of the hydrofluoric acid is 50% and the concentration of the nitric acid is 65%, stirring and heating the mixture to the solution temperature of 50 ℃, the stirring speed is 30r/min, dissolving the mixture for 30min, and then filtering the mixture through a funnel to obtain an extract.
ICP testing;
1ml of the extract was taken and the metal content in the extract was measured by ICP. It is shown that in the catalyst, the supported metal content is:
| metal content | Copper (Cu) | Chromium (III) | Silver (Ag) | Iron | Molybdenum (Mo) | Potassium salt |
| The content wt% | 5.53％ | 0.90％ | 0.02％ | 1.66％ | 0.82％ | 0.82％ |
And (3) conversion of content:
after the pretreatment in the first step, the weight loss of the materials is as follows: when m0-m1 is 0.10g, i.e., a loss of 2%, the metal content in the catalyst is:
| metal content | Copper (Cu) | Chromium (III) | Silver (Ag) | Iron | Molybdenum (Mo) | Potassium salt |
| Reduced content wt% | 5.40％ | 0.88％ | 0.02％ | 1.62％ | 0.80％ | 0.80％ |
Therefore, the temperature during the hole expanding process is reduced, and even if the time is long enough, the hole expanding effect is not good, so that the whole content test is low and the deviation amount is large during the catalyst metal content test.
Comparative example 2:
the present comparative example provides a method for testing the content of metals supported in a catalyst by ash burning, comprising the steps of:
1. pretreatment:
weighing 5.00g of catalyst sample, recording the weight as m0, placing the catalyst sample in a vacuum oven, drying for 1h under the conditions of-0.06 MPa vacuum degree and 70 ℃, taking out the sample after drying, weighing the mass of the residual sample, recording the mass as m1 to 4.90g, and obtaining m1 as desorbed organic additives, moisture and other non-metal components; this procedure is reported as weight loss a 1% ═ 2%.
2. Ash burning and dissolving:
4.90g of the catalyst sample is placed in a muffle furnace at 950 ℃ to be fully burnt to obtain burning ash, 0.25 +/-0.001 g of burning residue is weighed and placed in a crucible, 3ml of hydrofluoric acid and 5ml of nitric acid are added, stirring and heating are carried out until the solution temperature is 50 ℃, and the stirring speed is 30 r/min.
3. ICP testing;
1ml of the extract was taken and the metal content in the extract was measured by ICP. It is shown that in the catalyst, the supported metal content is:
| metal content | Copper (Cu) | Chromium (III) | Silver (Ag) | Iron | Molybdenum (Mo) | Potassium salt | Calcium carbonate | Magnesium alloy |
| The content wt% | 5.57％ | 0.96％ | 0.03％ | 1.66％ | 0.87％ | 0.76％ | 5.39％ | 2.39％ |
And (3) conversion of content:
after the pretreatment in the first step, the weight loss of the materials is as follows: when m0-m1 is 0.10g, i.e., a loss of 2%, the metal content in the catalyst is:
| metal content | Copper (Cu) | Chromium (III) | Silver (Ag) | Iron | Molybdenum (Mo) | Potassium salt | Calcium carbonate | Magnesium alloy |
| Reduced content wt% | 5.46％ | 0.94％ | 0.03％ | 1.62％ | 0.85％ | 0.74％ | 5.28％ | 2.34％ |
To further illustrate the technical effects of the present invention, the test results obtained in examples 1-3 and comparative examples 1-2 were analyzed, and the statistical table of the deviation between the test results and the theoretical values of the different test methods is shown in fig. 1.
TABLE 1 statistical table of deviation of test results from theoretical values of test methods of examples 1-3 and comparative examples 1-2
As can be seen from the data in Table 1, the average deviation of the test results in example 1 is relatively small, and the method belongs to a relatively proper pretreatment and test process; in example 2, the temperature and time during the pore-expanding process are increased, the pore-expanding effect is increased, and the loaded metal substances can be extracted more comprehensively, but similarly, the calcium and magnesium in the original activated carbon matrix are slightly dissolved out, but the detection amount is very small, which is less than 0.1%, and can be ignored. In embodiment 3, the temperature and time during the pore-expanding process are reduced, the pore-expanding effect is weakened, the difficulty in extracting the loaded metal substance is increased, the overall test of the metal content of the catalyst is low, but the average deviation is still within 10%, and meanwhile, the calcium and magnesium elements are not detected.
In comparative example 1, the temperature at the time of the hole expanding process was lowered, and even if the time was long enough, effective hole expansion could not be achieved. The pore-expanding is ineffective, so that the loaded metal substances cannot be effectively extracted, and the overall content test is low and the average deviation is 18.17% when the metal content of the catalyst is tested; in comparative example 2, the process of directly burning and measuring the ash content of the metal residue is adopted, although the problem that the metal substances in the pore channels are difficult to completely extract is avoided, the excessive metal substances lost along with the flue gas in the burning process also cause lower test results, and particularly, the metal components of potassium and magnesium which can form metal steam in the burning process are also caused.
The content of metal species in the catalyst was tested in the test manner of example 4 and comparative example 3, and the metal species and content in the catalyst were as follows:
example 4
This comparative example provides a method for determining the content of a metal supported in a catalyst, comprising the steps of:
s1, preprocessing:
weighing 5.00g of catalyst sample, recording the weight as m0, placing the catalyst sample in a vacuum oven, drying for 1h under the conditions of-0.06 MPa vacuum degree and 70 ℃, taking out the sample after drying, weighing the mass of the residual sample, recording the mass as m1 to 4.90g, and obtaining m1 as desorbed organic additives, moisture and other non-metal components; this procedure is reported as weight loss a 1% ═ 2%.
S2, hole expanding treatment:
will be pretreatedPutting the catalyst sample in a tubular furnace, introducing nitrogen, exhausting air in the furnace, heating to 800 ℃ at the temperature of 10 ℃/min, introducing water vapor for 15min, wherein the flow rate of the water vapor is 10mL/min, obtaining a sample, and weighing the sample, wherein the weight of the sample is m2, and the weight of m2 is 3.8 g; under the condition of high temperature of water vapor, the catalyst can react with (C + H) while expanding pores2O＝CO+H2High temperature), charcoal was consumed and weight loss Δ m2 ═ 1.10 g; this step is reported as weight loss a 2% ═ 22.45%.
S3, desorption treatment:
weighing 0.25 +/-0.001 g of the pore-expanded catalyst, placing the catalyst in a crucible, adding 3ml of hydrofluoric acid and 5ml of nitric acid, wherein the concentration of the hydrofluoric acid is 50% and the concentration of the nitric acid is 65%, stirring and heating the mixture to the solution temperature of 50 ℃, the stirring speed is 30r/min, dissolving the mixture for 30min, and then filtering the mixture through a funnel to obtain an extract.
And (3) CP testing:
1ml of the extract was taken and the metal content in the extract was measured by ICP. It is shown that in the catalyst, the supported metal content is:
| metal content | Copper (Cu) | Chromium (III) | Cobalt | Iron | Nickel (II) |
| The content wt% | 8.13％ | 1.46％ | 0.61％ | 2.55％ | 1.21％ |
And (3) conversion of content:
after the pretreatment in the first step, the weight loss of the materials is as follows: when a1 is 2.00% and a2 is 22.45%, the metal content in the catalyst is:
| metal content | Copper (Cu) | Chromium (III) | Cobalt | Iron | Nickel (II) |
| Reduced content wt% | 6.18％ | 1.11％ | 0.47％ | 1.94％ | 0.92％ |
Comparative example 3
This comparative example provides a method for determining the content of a metal supported in a catalyst, comprising the steps of:
s1, preprocessing:
weighing 5.00g of catalyst sample, recording the weight as m0, placing the catalyst sample in a vacuum oven, drying for 1h under the conditions of-0.06 MPa vacuum degree and 70 ℃, taking out the sample after drying, weighing the mass of the residual sample, recording the mass as m1 to 4.90g, and obtaining m1 as desorbed organic additives, moisture and other non-metal components; this procedure is reported as weight loss a 1% ═ 2%.
S2, hole expanding treatment:
placing the pretreated catalyst sample in a tubular furnace, introducing nitrogen, discharging air in the furnace, heating to 800 ℃ at the temperature of 10 ℃/min, introducing water vapor for 15min, wherein the flow rate of the water vapor is 10mL/min, obtaining a sample, weighing the sample, and weighing the sample, wherein the weight of the sample is m2, and the weight of m2 is 3.8 g; under the condition of high temperature of water vapor, the catalyst can react with (C + H) while expanding pores2O＝CO+H2High temperature), charcoal was consumed and weight loss Δ m2 ═ 1.10 g; this step is reported as weight loss a 2% ═ 22.45%.
S3, desorption treatment:
weighing 0.25 +/-0.001 g of the pore-expanded catalyst, placing the catalyst in a crucible, adding 8ml of nitric acid, stirring and heating the mixture until the concentration of hydrofluoric acid is 50% and the concentration of nitric acid is 65%, the solution is stirred and heated to the temperature of 50 ℃, the stirring speed is 30r/min, dissolving the mixture for 30min, and filtering the solution through a funnel to obtain extract liquor.
And (3) CP testing:
1ml of the extract was taken and the metal content in the extract was measured by ICP. It is shown that in the catalyst, the supported metal content is:
| metal content | Copper (Cu) | Chromium (III) | Cobalt | Iron | Nickel (II) |
| The content wt% | 7.98％ | 1.46％ | 0.39％ | 2.58％ | 0.66％ |
And (3) conversion of content:
after the pretreatment in the first step, the weight loss of the materials is as follows: when a1 is 2.00% and a2 is 22.45%, the metal content in the catalyst is:
| metal content | Copper (Cu) | Chromium (III) | Cobalt | Iron | Nickel (II) |
| Reduced content wt% | 6.07％ | 1.11％ | 0.30％ | 1.96％ | 0.50％ |
By comparing example 4 and comparative example 3, for both cobalt and nickel and their group metals, the solubility of cobalt and nickel metals in the extraction solution is limited even if a suitable process is selected, with only the addition of nitric acid. And hydrofluoric acid is added into the extraction liquid, so that the coordination capacity of the extraction liquid and metal is improved, more thorough extraction can be realized on the premise of ensuring the same total acid addition amount, and the test result is more accurate.
To further illustrate the technical effects of the present invention, the test results obtained in example 4 and comparative example 3 were analyzed, and the statistical table 2 shows the deviation between the test results of different test methods and theoretical values
Table 2 statistical table of deviation of test results from theoretical values of test methods of example 4 and comparative example 3
The deviation of the process test of example 4 compared to comparative example 3 is as follows: in comparative example 3, the major deviations are from cobalt and nickel. By adjusting the proportion of the extraction acid solution and the balance between the coordination performance and the oxidation performance of the acid solution and the metal, more thorough extraction is realized, which has great significance for the measurement of some special metal elements.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A method for measuring the content of a metal supported on a catalyst, comprising the steps of:
s1, preprocessing: drying the catalyst in a vacuum environment for 0-1.5 h;
s2, hole expanding treatment: placing the dried catalyst in a tubular furnace or a heating furnace, firstly adjusting to an oxygen-free atmosphere, then heating to 700-;
s3, desorption processing and detection calculation: adding mixed acid into the catalyst after pore expansion treatment, heating, stirring and dissolving, filtering to obtain an extract liquid, measuring the metal content in the extract liquid, and converting the metal content loaded in the catalyst.
2. The method of claim 1, wherein the drying is performed at a vacuum degree of-0.05 MPa to-0.09 MPa and a temperature of 60 ℃ to 150 ℃ in step S1.
3. The method of claim 1, wherein in step S2, the tube furnace or the heating furnace is adjusted to an oxygen-free atmosphere by filling inert gas.
4. The method as claimed in claim 1, wherein the heating is performed at a rate of 2-20 ℃/min to 700-900 ℃ in step S2.
5. The method for determining the content of the supported metal in the catalyst according to claim 1, wherein in the step S2, the flow rate of the introduced water vapor or carbon dioxide is 5 to 20mL/min, and the time is 5 to 20 min.
6. The method according to claim 1, wherein in step S3, the mixed acid is hydrofluoric acid and nitric acid, the concentration of the hydrofluoric acid is 40-50%, and the concentration of the nitric acid is 65-68%;
the volume usage ratio of the hydrofluoric acid to the nitric acid is (3-10): (5-20).
7. The method for determining the content of the metal supported on the catalyst according to claim 1, wherein in step S3, the ratio of the amount of the pore-enlarging treated catalyst to the amount of the mixed acid is (0.1 to 0.5) g: (8-30) mL.
8. The method according to claim 1, wherein the dissolving step S3 is carried out at a temperature lower than 150 ℃ for 5-30 min.
9. The method according to claim 1, wherein the stirring is performed at a rate of 0 to 50r/min in step S3.
10. The method according to claim 1, wherein in step S3, ICP ion chromatography is used to determine the metal content in the extract.
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