CN117368179A - Method for detecting total boron content in soil and sediment - Google Patents
Method for detecting total boron content in soil and sediment Download PDFInfo
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- CN117368179A CN117368179A CN202310989318.6A CN202310989318A CN117368179A CN 117368179 A CN117368179 A CN 117368179A CN 202310989318 A CN202310989318 A CN 202310989318A CN 117368179 A CN117368179 A CN 117368179A
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- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 title claims abstract description 162
- 229910052796 boron Inorganic materials 0.000 title claims abstract description 161
- 238000000034 method Methods 0.000 title claims abstract description 103
- 239000002689 soil Substances 0.000 title claims abstract description 71
- 239000013049 sediment Substances 0.000 title claims abstract description 66
- 239000000243 solution Substances 0.000 claims abstract description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000005259 measurement Methods 0.000 claims abstract description 28
- 239000007788 liquid Substances 0.000 claims abstract description 26
- 239000012086 standard solution Substances 0.000 claims abstract description 25
- 239000012085 test solution Substances 0.000 claims abstract description 23
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 claims abstract description 22
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 claims abstract description 22
- 239000003513 alkali Substances 0.000 claims abstract description 21
- 238000002844 melting Methods 0.000 claims abstract description 20
- 230000008018 melting Effects 0.000 claims abstract description 20
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 16
- 238000001914 filtration Methods 0.000 claims abstract description 13
- 238000005303 weighing Methods 0.000 claims abstract description 7
- 238000010790 dilution Methods 0.000 claims abstract description 4
- 239000012895 dilution Substances 0.000 claims abstract description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 32
- 239000004033 plastic Substances 0.000 claims description 30
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 30
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 26
- 238000004364 calculation method Methods 0.000 claims description 23
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 22
- 238000004458 analytical method Methods 0.000 claims description 15
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 15
- 238000011088 calibration curve Methods 0.000 claims description 14
- 230000004927 fusion Effects 0.000 claims description 13
- 229910052697 platinum Inorganic materials 0.000 claims description 13
- 238000012360 testing method Methods 0.000 claims description 13
- 229910052759 nickel Inorganic materials 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000002861 polymer material Substances 0.000 claims description 7
- 150000003839 salts Chemical class 0.000 claims description 7
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 6
- 239000004327 boric acid Substances 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000010813 internal standard method Methods 0.000 claims description 4
- 239000003595 mist Substances 0.000 claims description 4
- 238000010812 external standard method Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000001514 detection method Methods 0.000 description 33
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 238000000184 acid digestion Methods 0.000 description 11
- 238000001816 cooling Methods 0.000 description 9
- 238000007500 overflow downdraw method Methods 0.000 description 9
- 238000002798 spectrophotometry method Methods 0.000 description 9
- VFLDPWHFBUODDF-FCXRPNKRSA-N curcumin Chemical compound C1=C(O)C(OC)=CC(\C=C\C(=O)CC(=O)\C=C\C=2C=C(OC)C(O)=CC=2)=C1 VFLDPWHFBUODDF-FCXRPNKRSA-N 0.000 description 8
- 239000011159 matrix material Substances 0.000 description 8
- 229910000029 sodium carbonate Inorganic materials 0.000 description 7
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 239000002253 acid Substances 0.000 description 6
- 230000006872 improvement Effects 0.000 description 6
- 239000011521 glass Substances 0.000 description 5
- WTEOIRVLGSZEPR-UHFFFAOYSA-N boron trifluoride Chemical compound FB(F)F WTEOIRVLGSZEPR-UHFFFAOYSA-N 0.000 description 4
- 229940109262 curcumin Drugs 0.000 description 4
- 235000012754 curcumin Nutrition 0.000 description 4
- 239000004148 curcumin Substances 0.000 description 4
- VFLDPWHFBUODDF-UHFFFAOYSA-N diferuloylmethane Natural products C1=C(O)C(OC)=CC(C=CC(=O)CC(=O)C=CC=2C=C(OC)C(O)=CC=2)=C1 VFLDPWHFBUODDF-UHFFFAOYSA-N 0.000 description 4
- PFUVRDFDKPNGAV-UHFFFAOYSA-N sodium peroxide Chemical compound [Na+].[Na+].[O-][O-] PFUVRDFDKPNGAV-UHFFFAOYSA-N 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 230000029087 digestion Effects 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 238000002203 pretreatment Methods 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910015900 BF3 Inorganic materials 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical group [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000004993 emission spectroscopy Methods 0.000 description 2
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000011835 investigation Methods 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 238000012417 linear regression Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- MFHCZIKFNAPYFH-UHFFFAOYSA-N nitric acid perchloric acid hydrochloride hydrofluoride Chemical compound Cl.F.[N+](=O)(O)[O-].Cl(=O)(=O)(=O)O MFHCZIKFNAPYFH-UHFFFAOYSA-N 0.000 description 2
- 230000002572 peristaltic effect Effects 0.000 description 2
- -1 polypropylene Polymers 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- AKEKKCGPLHMFCI-UHFFFAOYSA-L potassium sodium hydrogen carbonate Chemical compound [Na+].[K+].OC([O-])=O.OC([O-])=O AKEKKCGPLHMFCI-UHFFFAOYSA-L 0.000 description 2
- 238000011002 quantification Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 239000013582 standard series solution Substances 0.000 description 2
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- 208000035240 Disease Resistance Diseases 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000112 cooling gas Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000374 eutectic mixture Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000000120 microwave digestion Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- OLAPPGSPBNVTRF-UHFFFAOYSA-N naphthalene-1,4,5,8-tetracarboxylic acid Chemical compound C1=CC(C(O)=O)=C2C(C(=O)O)=CC=C(C(O)=O)C2=C1C(O)=O OLAPPGSPBNVTRF-UHFFFAOYSA-N 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 238000010587 phase diagram Methods 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 229910052604 silicate mineral Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
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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
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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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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- 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
- G01N1/34—Purifying; Cleaning
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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
- G01N1/40—Concentrating samples
- G01N1/4077—Concentrating samples by other techniques involving separation of suspended solids
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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
- G01N1/44—Sample treatment involving radiation, e.g. heat
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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
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- G01N27/626—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 using heat to ionise a gas
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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
- G01N1/40—Concentrating samples
- G01N1/4077—Concentrating samples by other techniques involving separation of suspended solids
- G01N2001/4088—Concentrating samples by other techniques involving separation of suspended solids filtration
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Abstract
The invention discloses a method for detecting total boron content in soil and sediment, which comprises the following steps: preparing a boron standard solution with a first concentration value and a boron standard intermediate solution with a second concentration value; preparing a boron standard curve solution based on gradient dilution of a standard intermediate solution; setting a first melting reagent, weighing a sample to be detected, carrying out low-temperature alkali melting treatment on the sample to be detected based on the first melting reagent, and transferring the leached frit into a volumetric flask by using hot water to fix the volume to obtain a first test solution; filtering the first test solution to obtain a to-be-tested solution; measuring the boron standard curve solution and the liquid to be tested based on ICP-AES or ICP-MS to obtain measurement result data, and calculating the total boron content in the sample to be tested according to the measurement result data; the method can be used for efficiently, sensitively and accurately measuring the total boron content in the soil and the sediment, can be widely used for detecting the total boron content in various types of soil and sediment, and has low limitation.
Description
Technical Field
The invention relates to the technical field of chemical detection, in particular to a method for detecting total boron content in soil and sediment.
Background
The boron (B) element is an important trace element in soil, and particularly, the boron element has obvious effect on the growth and development process of plants, and can also enhance the disease resistance and drought resistance of crops. However, when the boron content in the soil is too high, boron poisoning of plants may also be induced. Therefore, the total boron (total boron) content of the soil is a conventional test index for the third soil screening in the whole country and is also an important index in geochemical investigation and agricultural geological investigation work.
Currently, the existing sample pretreatment method mainly comprises the following steps of: the acid digestion method and the alkali fusion method have the following problems:
for acid digestion: in the nature, boron mainly exists in the forms of borosilicate, borate and the like, and as boron elements are embedded in silicate minerals, the silicate structure of soil sediments cannot be damaged by adopting a conventional aqua regia method, so that the total boron test result is low; by adopting a hydrochloric acid-nitric acid-hydrofluoric acid-perchloric acid tetra-acid digestion method, although silicate in soil sediment can be destroyed by hydrofluoric acid, boron reacts with hydrofluoric acid to generate strong-volatility boron trifluoride to be dissipated from a system in the digestion process, and the test result is also lower; therefore, the conventional aqua regia digestion method or hydrochloric acid-nitric acid-hydrofluoric acid-perchloric acid tetrahydric acid digestion method in the acid digestion method can lead to lower determination results of the total boron content in soil and sediment; in addition, although the literature reports that about 0.5mL of phosphoric acid is added into a conventional mixed acid digestion system to play a role in fixing boron and further accurately measure total boron in soil sediments, in the method, as most of various acid reagents are contained in a glass bottle containing boron, interference is easily introduced in actual measurement, and measurement results are easily high; therefore, the acid digestion method can affect the accuracy of the determination of the total boron content in the soil and sediment;
for the alkali fusion method: compared with an acid digestion method, the alkali fusion method can introduce higher salt into a sample matrix, and although salt accumulation of an analysis instrument is easy to occur, the alkali fusion method is still a better pretreatment method for the total amount measurement of inorganic nonmetallic elements, such as boron, silicon and the like, in soil sediment, which are easy to lose in acid digestion; at present, common melting reagents for measuring the total boron mainly comprise sodium carbonate, sodium hydroxide, sodium peroxide and the like; when sodium carbonate is used as a melting reagent, since the melting point of the sodium carbonate is as high as 851 ℃, an expensive platinum crucible is required to be used for alkali melting at a high temperature above 900 ℃, so that the large-scale popularization and application of the method are limited; sodium hydroxide or sodium peroxide is used as a melting reagent, the fused block after alkali melting is in strong alkalinity although the temperature of a melting sample is low, and filtration and acid addition neutralization are required in the preparation process of the sample, so that corrosion to an analysis instrument is prevented, and the method is complicated and tedious; meanwhile, acid treatment can lead to a large amount of iron and aluminum in soil sediment to be dissolved out, so that spectral line interference is caused to the ICP-AES test of boron, and on the other hand, exogenous boron interference can be introduced when acid contained in a boron-containing glass reagent bottle is used; therefore, the existing alkali fusion method has poor accuracy, high application cost and complex operation;
in addition to the above sample pretreatment methods, the existing boron element detection methods include: azomethine spectrophotometry, curcumin spectrophotometry, inductively coupled plasma emission spectrometry (ICP-AES method) and inductively coupled plasma mass spectrometry (ICP-MS method). Among these methods, the methods of the azomethine spectrophotometry and the curcumin spectrophotometry have higher detection limit, are easily interfered by the matrix in the soil, and have inaccurate measurement results for the soil and sediment samples with low total boron content and complex matrix; in contrast, the ICP-AES method and the ICP-MS method have the characteristics of high sensitivity, accurate quantification and strong anti-interference capability, and become the main method for measuring the boron element.
In summary, the existing methods for detecting boron elements in soil and sediments have the following defects:
in the first aspect, an acid digestion method (microwave digestion method and electric plate digestion method) is adopted to measure total boron in soil and sediment samples, and due to the volatile property of boron trifluoride and the property of various acid reagents contained by a boron-containing glass bottle, boron dissipation or boron interference is caused in actual measurement, so that the measurement result is seriously lower or higher, and the measurement accuracy is influenced;
in the second aspect, the sodium carbonate alkali fusion method is adopted to measure the total boron in soil and sediment samples, and as the melting point of sodium carbonate is as high as 851 ℃, an expensive platinum crucible is required to be adopted for alkali fusion at a high temperature of more than 900 ℃, so that the large-scale popularization and application of the method are limited, the detection universality is poor, and the detection cost is too high;
in the third aspect, the sodium hydroxide or sodium peroxide alkali fusion method is adopted to measure the total boron in soil and sediment samples, the fusion temperature is low, but the fusion cake after alkali fusion is strong alkaline, filtration and acid neutralization are needed in the preparation process of the samples, so that an analysis instrument is prevented from being corroded, the method is complicated and tedious, interference factors such as iron, aluminum, boron and the like are easily introduced, and the detection efficiency, the detection convenience and the detection result accuracy are influenced;
in the fourth aspect, the total boron in the soil and sediment samples is measured by adopting an azomethine spectrophotometry or a curcumin spectrophotometry, and the measurement result is not accurate enough for the soil and sediment samples with low total boron content and complex matrix and also does not have higher detection accuracy because the spectrophotometry has higher detection limit and is easily interfered by the matrix in the soil.
Disclosure of Invention
The invention aims to solve the problems in the prior art, and provides a method for detecting the total boron content in soil and sediment, so as to solve the problems of high detection cost, complex detection operation, low detection precision and low detection efficiency in the conventional detection method.
In order to solve the technical problems, the specific technical scheme of the invention is as follows:
the invention provides a method for detecting total boron content in soil and sediment, which comprises the following steps:
preparing a standard solution;
preparing a boron standard solution with a first concentration value and a boron standard intermediate solution with a second concentration value;
preparing a boron standard curve solution based on gradient dilution of a standard intermediate solution;
sample pretreatment:
setting a first melting reagent, weighing a sample to be detected, carrying out low-temperature alkali melting treatment on the sample to be detected based on the first melting reagent, and transferring the melted block extracted by hot water into a volumetric flask for constant volume to obtain a first test solution;
filtering the first test solution to obtain a to-be-tested solution;
sample testing:
and determining the boron standard curve solution and the to-be-detected liquid based on ICP-AES or ICP-MS to obtain determination result data, and calculating the total boron content in the to-be-detected sample according to the determination result data.
As an improvement, the preparing the boron standard solution with the first concentration value and the boron standard intermediate solution with the second concentration value comprises the following steps:
preparing a boron standard solution with the first concentration value by adopting boric acid;
and preparing the boron standard intermediate solution with the second concentration value based on the boron standard solution by taking the boron-free pure water as a solvent.
As an improvement, the first melting agent includes: anhydrous sodium carbonate and anhydrous potassium carbonate; the mass sum of the anhydrous sodium carbonate and the anhydrous potassium carbonate is within a first range value, and the mass ratio of the anhydrous sodium carbonate to the anhydrous potassium carbonate is 2:3-3:2;
the low-temperature alkali fusion treatment is carried out, the fusion cake is extracted by hot water and transferred into a volumetric flask for constant volume, and a first test solution is obtained, and the method comprises the following steps:
setting a second mass range and a third mass range based on the first range value;
selecting the anhydrous sodium carbonate according to the second mass range;
selecting the anhydrous potassium carbonate according to the third mass range;
adding the sample to be detected, the anhydrous sodium carbonate and the anhydrous sodium carbonate which are selected into a specific crucible, uniformly mixing, and covering a crucible cover;
placing the crucible into a high-temperature electric furnace or a muffle furnace to heat to a first temperature range, keeping the temperature for a first time range, taking out the crucible after the furnace temperature is cooled, and adding boron-free pure water into the crucible;
heating the crucible added with pure water to boil and dissolve the frit, and transferring the obtained extracting solution into a plastic beaker; transferring the extract in the plastic beaker to a plastic volumetric flask after the extract is cooled;
repeatedly cleaning the crucible and the beaker by using boiling water, and transferring the cooled washing liquid into the volumetric flask;
and (3) adopting pure water to fix the volume of the liquid in the volumetric flask, shaking uniformly, and standing to obtain the first test solution.
As an improvement, the filtering process includes:
and filtering the first test solution through a filter made of polymer materials to obtain the test solution to be tested.
As an improved solution, the measuring the boron standard curve solution and the to-be-measured solution based on ICP-AES or ICP-MS to obtain measurement result data, and calculating the total boron content in the to-be-measured sample according to the measurement result data, including:
setting ICP-AES instrument conditions, and measuring the boron standard curve solution and the liquid to be tested by adopting an external standard method based on the ICP-AES to obtain measurement result data; setting a first calculation formula, and calculating the total boron content according to the measurement result data and the first calculation formula;
or alternatively, the first and second heat exchangers may be,
setting ICP-MS instrument conditions, and measuring the boron standard curve solution and the liquid to be tested by adopting an internal standard method based on the ICP-MS to obtain measurement result data; setting a second calculation formula, and calculating the total boron content according to the measurement result data and the second calculation formula.
As an improvement, the ICP-AES instrument conditions include:
the quantitative wavelength is: 208.957nm;
the reference wavelength is: 249.772nm, 249.677nm;
the high frequency power is: 1300W;
the sample injection speed is as follows: 1.0mL/min;
the atomizer is: a high salt mist resistant device;
the carrier gas flow rate of the atomizer is as follows: 0.7L/min;
the plasma cooling air flow is: 10L/min;
the auxiliary air flow is as follows: 0.3L/min;
the observation mode is as follows: and (5) axially observing.
As an improvement, the ICP-MS instrument conditions include:
the high frequency power is: 1500W;
the atomizer is: a high salt mist resistant device;
the atomizer flow is: 1.0L/min;
the peristaltic pump rotational speed is: 20.0r/min;
the mass numbers of the analysis elements are as follows: 11;
the internal standard is as follows: 72 Ge；
the analysis mode is as follows: and KED mode.
As an improved solution, the first calculation formula is:；
in the first calculation formula:
w is the total boron content;
ρ is the mass concentration of boron calculated from the calibration curve during the calculation;
v is the constant volume of the liquid to be tested;
m is the mass of the sample to be detected;
w H2O is the water content of the sample to be detected.
As a modification, the secondThe calculation formula is as follows:；
in the second calculation formula:
w is the total boron content;
ρ is the mass concentration of boron calculated from the calibration curve during the calculation;
v is the constant volume of the liquid to be tested;
m is the mass of the sample to be detected;
w dm is the dry matter mass of the sample to be tested.
As an improvement, the first concentration value is: 1000 μg/mL;
the second concentration value is: 5.0-20 mug/mL;
the first range value is: 2.0-2.5 g;
the second mass range is as follows: 0.8-1.2 g;
the third mass range is as follows: 0.8-1.2 g;
the specific crucible is as follows: nickel crucible, or platinum crucible;
the filter is as follows: a 0.45 μm hydrophilic needle filter of polymeric material;
the first temperature range is: 725-750 ℃;
the first time length range is: 25-30 min.
The technical scheme of the invention has the beneficial effects that:
1. the method for detecting the total boron content in the soil and the sediment can be used for efficiently, sensitively and accurately detecting the total boron (total boron) content in the soil and the sediment, can be widely applied to detection of the total boron content in various types of soil and sediment, has low limitation, and overcomes the defects of the existing detection method.
2. According to the method for detecting the total boron content in the soil and the sediment, disclosed by the invention, the soil/sediment sample is treated by adopting the alkali fusion method, so that acid digestion by using hydrofluoric acid with great toxic action on the environment and the human body can be avoided, and the environmental protection and the safety of the method are improved.
3. Compared with the operation of alkali fusion of sodium carbonate in the prior art, the method for detecting the total boron content in the soil and the sediment provided by the invention has the advantages that the required temperature condition is reduced from 950 ℃ to 725-750 ℃, the energy consumption can be effectively saved, and the sodium hydroxide or sodium peroxide with strong corrosiveness is not required, so that the detection convenience is improved, and the detection difficulty is reduced.
4. According to the method for detecting the total boron content in the soil and the sediment, disclosed by the invention, the nickel crucible with low cost can be used for replacing an expensive platinum crucible for alkali fusion, so that the detection cost is reduced on the premise of not affecting the measurement accuracy, the method is convenient to popularize and apply in a large scale, the limitation of the method is reduced, and the method universality is improved.
5. Compared with the conventional alkali fusion method, the method for detecting the total boron content in the soil and the sediment has the advantages that the problem of spectral line interference caused by the introduction of impurities such as iron and aluminum into the fusion cake by sulfuric acid or hydrochloric acid leaching and the problem of exogenous boron interference caused by the introduction of acid contained in a glass bottle are avoided, the detection accuracy is further improved, and the interference factors are optimized.
6. The method for detecting the total boron content in the soil and the sediment does not need to use filter paper for filtration, and can be directly transferred in full quantity and fixed in volume after hot water leaching.
7. The method for detecting the total boron content in the soil and the sediment can avoid the interference of boron introduced by the boron-containing glass by not using glassware and reagents contained in the glassware in the whole experimental process, so that the measuring result is more accurate.
8. The method for detecting the total boron content in the soil and the sediment adopts the ICP-AES or ICP-MS method to detect the boron, and compared with the traditional azomethine spectrophotometry and curcumin spectrophotometry, the method has the advantages of lower detection limit, higher capability of resisting complex matrix interference and greatly improved sensitivity and accuracy of detection results.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic flow chart of a method for detecting total boron content in soil and sediment according to example 1 of the present invention;
FIG. 2 is a detailed flow chart of the method for detecting total boron content in soil and sediment according to example 1 of the present invention;
FIG. 3 is a sodium carbonate-potassium carbonate phase diagram using sodium carbonate-potassium carbonate as a flux;
FIG. 4 is an ICP-AES calibration curve for boron;
fig. 5 is an ICP-MS calibration curve for boron.
Detailed Description
The preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings so that the advantages and features of the present invention can be more easily understood by those skilled in the art, thereby making clear and defining the scope of the present invention.
In the description of the present invention, it should be noted that the described embodiments of the present invention are some, but not all embodiments of the present invention; all other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The terms first, second and the like in the description and in the claims and in the above-described figures, are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used may be interchanged where appropriate such that the embodiments described herein may be capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, apparatus, article, or device that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed or inherent to such process, method, article, or device.
In describing the present invention, it should be noted that:
1. in the examples of the present invention, the following examples of the apparatus, reagents and conditions are given as an embodiment, and the embodiment may be adapted according to the environment, object or condition of the method in the example.
2. In an embodiment of the invention, the instrumentation used is as follows:
1. inductively coupled plasma emission spectroscopy (equipped with high salt resistant atomizer);
2. an oven (temperature controllable);
3. analytical balance (inductance 0.0001 g);
4. muffle furnace or box type high temperature electric furnace (highest temperature up to 1200 ℃);
5. platinum crucible or nickel crucible (capacity 30 mL);
6. plastic beaker (250 mL capacity);
7. nylon screen (capacity 0.149mm <100 mesh >);
8. plastic volumetric flasks (50 mL, 100mL, 250 mL);
9. general instrumentation (including but not limited to, graduated pipettes, volumetric flasks, measuring cylinders, pipettes, 10mL centrifuge tubes, etc.).
3. In the examples of the present invention, the reagent materials used and their standards are as follows:
1. anhydrous sodium carbonate (purity is superior purity);
2. anhydrous potassium carbonate (purity is superior purity);
3. boron unit element standard solution: (parameters are 1000mg/L,50 mL), and the good-grade pure boric acid is used for preparing or purchasing a commercially available standard product with evidence, and the good-grade pure boric acid is refrigerated and stored in a sealed manner in a dark place;
4. boron standard use solution: 10mg/L in pure water; the preparation method comprises the following steps: transferring 1.0mL of boron single element standard solution into a 100mL volumetric flask, fixing the volume to a scribing line by pure water, shaking uniformly, refrigerating and preserving;
5. a hydrophilic needle filter (pore size 0.45 μm) of polymer material;
6. argon (purity is more than or equal to 99.999%);
7. matrix matching liquid (blank test liquid); the preparation method comprises the following steps: 10g of anhydrous sodium carbonate and 10g of anhydrous potassium carbonate are weighed into a plastic beaker, added with water for dissolution, cooled and transferred into a 1000mL volumetric flask, and the volumetric flask is fixed to 1000mL by pure water and shaken uniformly.
Example 1
The embodiment provides a method for detecting total boron content in soil and sediment, as shown in fig. 1-5, comprising the following steps:
as one implementation mode of the invention, in the detection method, the sodium carbonate and potassium carbonate eutectic mixture is used as a melting reagent to reduce the melting temperature, a nickel crucible is adopted for low-temperature alkali fusion treatment of soil/sediment samples to reduce the detection cost, the fusion cake is directly fixed to a score line after being leached by hot water, and the test solution is analyzed by ICP-AES or ICP-MS after being filtered by a hydrophilic needle filter made of 0.45 mu m polymer material, so that the detection efficiency is improved and the detection difficulty is reduced; based on the method, the total boron content in the soil and sediment can be finally and rapidly and efficiently measured, and the method comprises the following specific steps:
s100, a standard solution preparation step, which comprises the following steps:
preparing a boron standard intermediate solution with the concentration of 5.0-20 mug/mL (namely a second concentration value) by using 1000 mug/mL (namely a first concentration value) boron standard solution prepared by boric acid or using a commercially available 1000 mug/mL boron standard solution and using boron-free pure water as a solvent;
gradient diluting with standard intermediate liquid, and fixing volume with matrix matching liquid to prepare boron standard curve solution;
in this embodiment, the linear range of the standard curve for ICP-AES analysis is recommended to be 0-5 μg/mL; the linear range of the standard curve for ICP-MS analysis is preferably 0-500 mug/L, and 6-8 mass concentration points are preferably prepared in total;
s200, a sample pretreatment step, which comprises the following steps:
accurately weighing 0.20-0.25 g (accurate to 0.0001 g) of soil or sediment sample in a nickel crucible or a platinum crucible by using an electronic balance;
adding 0.8-1.2 g (namely, a second mass range) of anhydrous sodium carbonate and 0.8-1.2 g (namely, a third mass range) of anhydrous potassium carbonate (total 2.0-2.5 g < namely, a first range value >), wherein the mass ratio of the anhydrous sodium carbonate to the anhydrous potassium carbonate is 2:3-3:2); after fully and uniformly mixing, covering a crucible cover, putting the crucible into a high-temperature electric furnace or a muffle furnace, heating to 725-750 ℃ (namely, a first temperature range), keeping for 25-30 min at the temperature (namely, a first time range), and taking out the crucible after the furnace temperature is cooled to below 200 ℃;
adding about 10mL of pure water into the extracted crucible, heating to boil and dissolve the frit, transferring the corresponding extracting solution into a plastic beaker, and transferring all the test solution in the plastic beaker into a 100mL plastic volumetric flask after slightly cooling;
repeatedly washing the crucible and the plastic beaker with about 10mL of boiling water for 2-3 times, slightly cooling, combining and transferring the washing liquid into a plastic volumetric flask of 100mL or 250mL, fixing the volume to a marking line by pure water, shaking uniformly, standing for 15-30 min, taking 5-10 mL of test liquid, and filtering the test liquid into a plastic centrifuge tube or a plastic sample tube of 10mL through a filter of 0.45 mu m made of polymer material to obtain the test liquid to be tested.
S300, sample testing:
according to the set ICP-AES or ICP-MS reference conditions, measuring the standard curve solution and the sample to be measured by an external standard method or an internal standard method;
after the measurement, corresponding instrument measurement values and the like are obtained, and then data such as the instrument measurement values, the sample weighing amounts and the like are substituted into corresponding formulas to calculate the total boron (total boron) content in soil, sediment and agriculture and forestry soil samples, and the results are expressed in mg/kg.
Example 2
The present example provides a method for detecting total boron content in soil and sediment, wherein, based on the technical scheme described in example 1, another implementation mode is provided for the standard solution preparation step, and the method specifically includes the following steps:
preparing a boron standard solution: 0.5719g of boric acid is weighed into a 100mL plastic beaker, then added with boron-free pure water for dissolution, and transferred into a 100mL plastic volumetric flask; after the volume is fixed to the scribing line, shaking uniformly to prepare 1000 mug/mL boron standard solution;
preparing a boron standard intermediate solution: transferring 2.0mL of the boron standard solution into a 100mL plastic volumetric flask, and fixing the volume to a scribing line; after shaking, preparing a boron standard intermediate solution with the concentration of 20 mug/mL;
preparing boron standard curve solution: the solution was diluted with a standard intermediate solution to prepare boron standard curve solutions for ICP-AES analysis at mass concentrations of 0. Mu.g/mL, 0.05. Mu.g/mL, 0.1. Mu.g/mL, 0.2. Mu.g/mL, 0.5. Mu.g/mL, 1.0. Mu.g/mL and 2.0. Mu.g/mL, respectively.
Example 3
The present example provides a method for detecting total boron content in soil and sediment, wherein, based on the technical scheme described in example 1, another implementation mode is provided for the standard solution preparation step, and the method specifically includes the following steps:
preparing a boron standard solution and a boron standard intermediate solution: taking a commercially available standard solution of boron with a standard of 1000 mug/mL, transferring 0.5mL of the standard solution of boron into a 100mL plastic volumetric flask, fixing the volume to a scribing line, and shaking uniformly to prepare a standard intermediate solution of boron with a concentration of 5.0 mug/mL;
preparing boron standard curve solution: the standard intermediate solution is used for gradient dilution to prepare boron standard curve solution for ICP-MS analysis, and the mass concentration of the boron standard curve solution is respectively 0 mug/L, 10 mug/L, 20 mug/L, 50 mug/L, 100 mug/L, 200 mug/L and 500 mug/L.
Example 4
The embodiment provides a method for detecting total boron content in soil and sediment, wherein based on the technical scheme described in the embodiment 1, another implementation mode is provided for the sample pretreatment step, and the method specifically comprises the following steps:
accurately weighing 0.24g (accurate to 0.0001 g) of sediment sample in a platinum crucible by using an electronic balance;
adding 0.9 g anhydrous sodium carbonate and 1.2g anhydrous potassium carbonate into a platinum crucible, fully and uniformly mixing, and covering a crucible cover; placing the platinum crucible into a muffle furnace, heating to 750 ℃, keeping the temperature for 30min, cooling to the furnace temperature below 200 ℃, and taking out the platinum crucible;
adding about 10mL of pure water into a platinum crucible, heating to boil and dissolve the frit, transferring the corresponding extracting solution into a plastic beaker, and transferring all the test solution in the beaker into a 100mL plastic volumetric flask after slightly cooling;
repeatedly washing the platinum crucible and the plastic beaker with about 10mL of boiling water for 2-3 times, slightly cooling, and combining and transferring the washing liquid into a 100mL polypropylene plastic volumetric flask; adopting pure water to fix the volume to the marked line, and shaking uniformly; and standing for 20min, and then taking 6mL of test solution, and filtering the test solution into a 10mL plastic sample tube through a 0.45 mu m filter made of polymer materials to obtain the test solution to be tested for ICP-AES analysis.
Example 5
The embodiment provides a method for detecting total boron content in soil and sediment, wherein based on the technical scheme described in the embodiment 1, another implementation mode is provided for the sample pretreatment step, and the method specifically comprises the following steps:
accurately weighing 0.20g (accurate to 0.0001 g) of soil and sediment samples in a nickel crucible by using an electronic balance;
adding 1.0 anhydrous sodium carbonate and 1.0g anhydrous potassium carbonate into a nickel crucible, fully and uniformly mixing, covering a crucible cover, and putting into a high-temperature electric furnace to heat to 725 ℃; keeping the temperature for 30min, cooling to the temperature below 200 ℃, and taking out the nickel crucible;
adding about 10mL of pure water into a nickel crucible, heating to boil and dissolve the frit, transferring the corresponding extracting solution into a plastic beaker, slightly cooling, and transferring all the test solution in the beaker into a 250mL plastic volumetric flask;
repeatedly washing the nickel crucible and the plastic beaker with about 10mL of boiling water for 2-3 times, slightly cooling, combining and transferring the washing liquid into a 250mL polypropylene plastic volumetric flask, fixing the volume to a marked line by using pure water, and shaking uniformly; and standing for 20min, and filtering 7mL of the test solution into a 10mL plastic centrifuge tube through a 0.45 mu m filter made of polymer material to obtain the test solution to be tested for ICP-MS analysis.
Example 6
The present embodiment provides a method for detecting total boron content in soil and sediment, wherein, based on the technical scheme described in the embodiment 1, another implementation mode is provided for the sample testing step, and the method specifically includes the following steps:
according to the set conditions of an ICP-AES instrument (the conditions are as follows, the quantitative wavelength is 208.957nm, the reference wavelength is 249.772nm and 249.677nm, the high-frequency power is 1300W, the sample injection speed is 1.0mL/min, the atomizer is a high-salt-resistant atomizer, the carrier gas flow of the atomizer is 0.7L/min, the plasma cooling gas flow is 10L/min, the auxiliary gas flow is 0.3L/min, and the observation mode is axial observation, and the standard series solutions are sequentially measured from low concentration to high concentration;
drawing a corresponding calibration curve by taking the emission intensity of boron as an ordinate and the mass concentration of the standard solution as an abscissa; wherein the linear range of the calibration curve is 0-5 mug/mL, the preferred mass concentration is 0 mug/mL, 0.05 mug/mL, 0.1 mug/mL, 0.2 mug/mL, 0.5 mug/mL, 1.0 mug/mL, 2.0 mug/mL and 5.0 mug/mL respectively, and 6-8 calibration curve concentration points are prepared altogether; when the sampling amount is 0.25g and the constant volume is 100mL, the detection limit of the method of full boron is 5mg/kg, and the measurement lower limit (calculated according to 4 times of the detection limit) is 20mg/kg; then, measuring the sediment sample to be measured, carrying out calculation in a linear regression equation to obtain the mass concentration of boron in the sediment sample, and calculating according to the following formula (namely a first calculation formula):
in (1) ratio of
w is the total boron (total boron) content of the deposit in units of: mg/kg;
ρ is the mass concentration of boron calculated from the calibration curve in units of: mg/L;
v is the constant volume of the sample, and the unit is: mL;
m is the mass of the weighed sediment sample, and the unit is: g;
w H2O the water content of the sediment sample is expressed as: percent of the total weight of the composition.
Example 7
The present embodiment provides a method for detecting total boron content in soil and sediment, wherein, based on the technical scheme described in the embodiment 1, another implementation mode is provided for the sample testing step, and the method specifically includes the following steps:
according to the set ICP-MS instrument conditions (the conditions are that the internal standard method is used for quantification, the high-frequency power is 1500W, the atomizer is a high-salt-resistant atomizer, the flow rate of the atomizer is 1.0L/min, the rotating speed of a peristaltic pump is 20.0r/min, the mass number of analysis elements is 11, and the internal standard is that: 72 ge; analysis mode: a collision reaction cell mode (KED)), sequentially measuring standard series solutions from low concentration to high concentration, and measuring signal response values of the element to be measured and the internal standard element;
the concentration of the element to be measured is taken as an abscissa, the ratio of the response signal value of the element to be measured to the response signal value of the selected internal standard element is taken as an ordinate, and a corresponding calibration curve is drawn; wherein the linear range of the calibration curve is 0-500 mug/L, and the preferable mass concentration is 0 mug/L, 10 mug/L, 20 mug/L, 50 mug/L, 100 mug/L, 200 mug/L, 300 mug/L and 500 mug/L respectively, and 6-8 calibration curve concentration points are prepared altogether; when the sampling amount is 0.20g and the constant volume is 250mL, the detection limit of the method of full boron is 2mg/kg, and the measurement lower limit (calculated according to 4 times of the detection limit) is 8mg/kg; then, the soil sample to be tested is measured, the mass concentration of boron in the sediment sample is calculated by taking the linear regression equation, and the mass concentration is calculated according to the following formula (namely a second calculation formula):
in (2) ratio of
w is the total boron (total boron) content of the soil, and the unit is: mg/kg;
ρ is the mass concentration of boron calculated from the calibration curve in units of: mg/L;
v is the constant volume of the sample, and the unit is: mL;
m is the mass of the weighed soil sample, and the unit is: g;
w dm the dry matter content of the soil sample is given in units of: percent of the total weight of the composition.
Compared with the prior art, the method for detecting the total boron content in the soil and the sediment can be used for efficiently, sensitively and accurately determining the total boron (total boron) content in the soil and the sediment, can be widely applied to detection of the total boron content in various types of soil and sediment, has low limitation, and overcomes the defects of the existing detection method.
It should be understood that, in the various embodiments herein, the sequence number of each process described above does not mean the sequence of execution, and the execution sequence of each process should be determined by its functions and internal logic, and should not constitute any limitation on the implementation process of the embodiments herein.
It should also be understood that in embodiments herein, the term "and/or" is merely one relationship that describes an associated object, meaning that three relationships may exist. For example, a and/or B may represent: a exists alone, A and B exist together, and B exists alone. In addition, the character "/" herein generally indicates that the front and rear associated objects are an "or" relationship.
Those of ordinary skill in the art will appreciate that the elements and algorithm steps described in connection with the embodiments disclosed herein may be embodied in electronic hardware, in computer software, or in a combination of the two, and that the elements and steps of the examples have been generally described in terms of function in the foregoing description to clearly illustrate the interchangeability of hardware and software. Whether such functionality is implemented as hardware or software depends upon the particular application and design constraints imposed on the solution. Skilled artisans may implement the described functionality in varying ways for each particular application, but such implementation decisions should not be interpreted as causing a departure from the scope of the present disclosure.
It will be clear to those skilled in the art that, for convenience and brevity of description, specific working procedures of the above-described systems, apparatuses and units may refer to corresponding procedures in the foregoing method embodiments, and are not repeated herein.
The foregoing description is only illustrative of the present invention and is not intended to limit the scope of the invention, and all equivalent structures or equivalent processes or direct or indirect application in other related technical fields are included in the scope of the present invention.
Claims (10)
1. A method for detecting the total boron content in soil and sediment, which is characterized by comprising the following steps:
preparing a standard solution;
preparing a boron standard solution with a first concentration value and a boron standard intermediate solution with a second concentration value;
preparing a boron standard curve solution based on gradient dilution of a standard intermediate solution;
sample pretreatment:
setting a first melting reagent, weighing a sample to be detected, carrying out low-temperature alkali melting treatment on the sample to be detected based on the first melting reagent, and transferring the melted block extracted by hot water into a volumetric flask for constant volume to obtain a first test solution;
filtering the first test solution to obtain a to-be-tested solution;
sample testing:
and determining the boron standard curve solution and the to-be-detected liquid based on ICP-AES or ICP-MS to obtain determination result data, and calculating the total boron content in the to-be-detected sample according to the determination result data.
2. The method for detecting the total boron content in soil and sediment according to claim 1, wherein the method comprises the following steps:
the preparation of the boron standard solution with the first concentration value and the boron standard intermediate solution with the second concentration value comprises the following steps:
preparing a boron standard solution with the first concentration value by adopting boric acid;
and preparing the boron standard intermediate solution with the second concentration value based on the boron standard solution by taking the boron-free pure water as a solvent.
3. The method for detecting the total boron content in soil and sediment according to claim 1, wherein the method comprises the following steps:
the first fusing agent includes: anhydrous sodium carbonate and anhydrous potassium carbonate; the mass sum of the anhydrous sodium carbonate and the anhydrous potassium carbonate is within a first range value, and the mass ratio of the anhydrous sodium carbonate to the anhydrous potassium carbonate is 2:3-3:2;
the low-temperature alkali fusion treatment is carried out, the fusion cake is extracted by hot water and transferred into a volumetric flask for constant volume, and a first test solution is obtained, and the method comprises the following steps:
setting a second mass range and a third mass range based on the first range value;
selecting the anhydrous sodium carbonate according to the second mass range;
selecting the anhydrous potassium carbonate according to the third mass range;
adding the sample to be detected, the anhydrous sodium carbonate and the anhydrous sodium carbonate which are selected into a specific crucible, uniformly mixing, and covering a crucible cover;
placing the crucible into a high-temperature electric furnace or a muffle furnace to heat to a first temperature range, keeping the temperature in the first temperature range, taking out the crucible after the furnace temperature is cooled, and adding boron-free pure water into the crucible;
heating the crucible added with pure water to boil and dissolve the frit, and transferring the obtained extracting solution into a plastic beaker; transferring the extract in the plastic beaker to a plastic volumetric flask after the extract is cooled;
repeatedly cleaning the crucible and the beaker by using boiling water, and transferring the cooled washing liquid into the volumetric flask;
and (3) adopting pure water to fix the volume of the liquid in the volumetric flask, shaking uniformly, and standing to obtain the first test solution.
4. The method for detecting the total boron content in soil and sediment according to claim 1, wherein the method comprises the following steps:
the filtering process includes:
and filtering the first test solution through a filter made of polymer materials to obtain the test solution to be tested.
5. The method for detecting the total boron content in soil and sediment according to claim 1, wherein the method comprises the following steps:
the method for measuring the boron standard curve solution and the liquid to be tested based on ICP-AES or ICP-MS to obtain measurement result data, and calculating the total boron content in the sample to be tested according to the measurement result data comprises the following steps:
setting ICP-AES instrument conditions, and measuring the boron standard curve solution and the liquid to be tested by adopting an external standard method based on the ICP-AES to obtain measurement result data; setting a first calculation formula, and calculating the total boron content according to the measurement result data and the first calculation formula;
or alternatively, the first and second heat exchangers may be,
setting ICP-MS instrument conditions, and measuring the boron standard curve solution and the liquid to be tested by adopting an internal standard method based on the ICP-MS to obtain measurement result data; setting a second calculation formula, and calculating the total boron content according to the measurement result data and the second calculation formula.
6. The method for detecting the total boron content in soil and sediment according to claim 5, wherein the method comprises the following steps:
the ICP-AES instrument conditions include:
the quantitative wavelength is: 208.957nm;
the reference wavelength is: 249.772nm, 249.677nm;
the atomizer is: a high salt mist resistant device;
the observation mode is as follows: and (5) axially observing.
7. The method for detecting the total boron content in soil and sediment according to claim 5, wherein the method comprises the following steps:
the ICP-MS instrument conditions include:
the atomizer is: a high salt mist resistant device;
the mass numbers of the analysis elements are as follows: 11;
the analysis mode is as follows: and KED mode.
8. The method for detecting the total boron content in soil and sediment according to claim 5, wherein the method comprises the following steps:
the first calculation formula is:；
in the first calculation formula:
w is the total boron content;
ρ is the mass concentration of boron calculated from the calibration curve during the calculation;
v is the constant volume of the liquid to be tested;
m is the mass of the sample to be detected;
w H2O is the water content of the sample to be detected.
9. The method for detecting the total boron content in soil and sediment according to claim 5, wherein the method comprises the following steps:
the second calculation formula is:；
in the second calculation formula:
w is the total boron content;
ρ is the mass concentration of boron calculated from the calibration curve during the calculation;
v is the constant volume of the liquid to be tested;
m is the mass of the sample to be detected;
w dm is the dry matter mass of the sample to be tested.
10. A method for detecting the total boron content of soil and sediment according to claim 2, wherein:
the first concentration value is: 1000 μg/mL;
the second concentration value is: 5.0-20 mug/mL;
the first range value is: 2.0-2.5 g;
the second mass range is as follows: 0.8-1.2 g;
the third mass range is as follows: 0.8-1.2 g;
the specific crucible is as follows: nickel crucible, or platinum crucible;
the filter is as follows: a 0.45 μm hydrophilic needle filter of polymeric material;
the first temperature range is: 725-750 ℃;
the first time range is: 25-30 min.
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