CN116953060A - Method for measuring lithium in marine sediment - Google Patents
Method for measuring lithium in marine sediment Download PDFInfo
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- 239000013049 sediment Substances 0.000 title claims abstract description 38
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000001514 detection method Methods 0.000 claims abstract description 22
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 14
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 10
- 229910052732 germanium Inorganic materials 0.000 claims abstract description 9
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052751 metal Inorganic materials 0.000 claims abstract description 8
- 239000002184 metal Substances 0.000 claims abstract description 8
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 claims abstract description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 48
- 239000012488 sample solution Substances 0.000 claims description 19
- 239000007789 gas Substances 0.000 claims description 15
- 238000009616 inductively coupled plasma Methods 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 230000002378 acidificating effect Effects 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
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- 238000007873 sieving Methods 0.000 claims description 7
- 239000012224 working solution Substances 0.000 claims description 7
- 229910000990 Ni alloy Inorganic materials 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 239000012086 standard solution Substances 0.000 claims description 5
- 239000006228 supernatant Substances 0.000 claims description 5
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 5
- 239000012498 ultrapure water Substances 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 238000007865 diluting Methods 0.000 claims description 3
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- 238000002360 preparation method Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims 1
- 239000002253 acid Substances 0.000 abstract description 4
- 238000004451 qualitative analysis Methods 0.000 abstract 1
- 238000004445 quantitative analysis Methods 0.000 abstract 1
- 230000035945 sensitivity Effects 0.000 abstract 1
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- 238000005119 centrifugation Methods 0.000 description 10
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- 230000029087 digestion Effects 0.000 description 3
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- 230000004044 response Effects 0.000 description 3
- DPORRQCIAXYPGF-UHFFFAOYSA-N F.Cl.O[N+]([O-])=O Chemical compound F.Cl.O[N+]([O-])=O DPORRQCIAXYPGF-UHFFFAOYSA-N 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
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- 238000011387 Li's method Methods 0.000 description 1
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- HFCVPDYCRZVZDF-UHFFFAOYSA-N [Li+].[Co+2].[Ni+2].[O-][Mn]([O-])(=O)=O Chemical compound [Li+].[Co+2].[Ni+2].[O-][Mn]([O-])(=O)=O HFCVPDYCRZVZDF-UHFFFAOYSA-N 0.000 description 1
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- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical compound [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 208000002173 dizziness Diseases 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- GPGMRSSBVJNWRA-UHFFFAOYSA-N hydrochloride hydrofluoride Chemical compound F.Cl GPGMRSSBVJNWRA-UHFFFAOYSA-N 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- JZBDKSGOOLLKIO-UHFFFAOYSA-N nitric acid sulfuric acid hydrofluoride Chemical compound S(O)(O)(=O)=O.F.[N+](=O)(O)[O-] JZBDKSGOOLLKIO-UHFFFAOYSA-N 0.000 description 1
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- 208000027765 speech disease Diseases 0.000 description 1
- DGCPSAFMAXHHDM-UHFFFAOYSA-N sulfuric acid;hydrofluoride Chemical compound F.OS(O)(=O)=O DGCPSAFMAXHHDM-UHFFFAOYSA-N 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000002137 ultrasound extraction Methods 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
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- 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
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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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Abstract
The invention discloses a method for measuring lithium in marine sediments, and belongs to the technical field of metal detection. The invention adopts acid extracting solution prepared from concentrated nitric acid, concentrated hydrochloric acid and hydrofluoric acid to carry out high-efficiency pretreatment on marine sediment, and then uses germanium as an internal standard element and combines an inductively coupled plasma mass spectrometry to realize accurate and rapid qualitative and quantitative analysis on lithium elements in the sediment. The method has the advantages of simple operation, high sensitivity, high precision, good specificity and the like, and is a scientific method for measuring lithium in marine sediments.
Description
Technical Field
The invention belongs to the technical field of metal detection, and particularly relates to a method for measuring lithium in marine sediments.
Background
Lithium is the lightest and least dense element of the periodic table, and is not freely present in nature because lithium is the most active metal of known elements (including radioactive elements) and reacts very well with air and water due to the most negative electrode potential. However, the lithium element has certain toxicity, and the main target organ of the toxicity of the lithium element is the central nervous system of an organism. Research shows that when 10 mg/L of lithium element is contained in human blood, the human blood is subjected to slight poisoning by the lithium element, dizziness and speech disorder can occur when the content of the lithium element is 15 mg/L, and death risk exists when the dosage of the lithium element is 20 mg/L. In recent years, with the development of new energy enterprises in coastal areas, the content of lithium discharged into marine sediments is increased, and the threat to marine ecological safety is caused. In the detection of the lithium content in the marine sediment in the prior art, the digestion mode is mainly adopted to extract the lithium element in the sediment, the equipment requirement is high, the operation requirement on experimental staff is also high, and the operation safety is low. Therefore, the establishment of a simple and accurate method for measuring the lithium in the marine sediment has important practical significance.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a simple and accurate method for measuring lithium in marine sediments.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a method for determining lithium in a marine deposit comprising the steps of:
1) Preparation of sample solution: removing sundries such as branches, leaves and stones from the collected marine sediment, drying, grinding and sieving, accurately weighing 1.0 g, placing into a 50 mL centrifuge tube, adding 30 mL acidic extracting solution, and shaking; after ultrasonic treatment at 100 ℃ for 60 minutes, cooling to room temperature, centrifuging, taking supernatant 5 mL, diluting with ultrapure water, fixing the volume to a 50 mL measuring flask, and shaking uniformly to obtain a sample solution;
2) And (3) preparing a standard working curve: preparing lithium element standard working solutions with the concentrations of 5, 15, 25, 50, 75 and 100 ng/mL by adopting a lithium standard solution, measuring on an inductively coupled plasma mass spectrometer, and drawing a standard working curve of the lithium element by taking the concentration of the lithium element as an abscissa and the signal intensity of the lithium element as an ordinate;
3) Determination of sample solution: and measuring the lithium element signal intensity of the sample solution by using an inductively coupled plasma mass spectrometer, and calculating according to the standard working curve of the obtained lithium element to obtain the lithium element content in the sample solution.
Further, the acidic extracting solution in the step 1) is formed by mixing concentrated nitric acid, concentrated hydrochloric acid and hydrofluoric acid according to a volume ratio of 15:10:5.
Further, the ultrasonic treatment in the step 1) is performed in a fume hood, and the power of the ultrasonic machine is greater than or equal to 100W.
Further, the rotational speed of the centrifugation in step 1) was 2000 r/min for 10 min.
Further, in the step 2), a standard working solution of lithium element is prepared by using a 2vol% nitric acid solution.
Further, germanium is adopted as an internal standard element in inductively coupled plasma mass spectrum detection, and is added on line by a peristaltic pump.
Further, the inductively coupled plasma mass spectrometry detection conditions are: plasma gas: argon gas with the purity of 99.999 percent; instrument power: 1550 W is a metal; detection type: a KED; type of atomizer: a gas vortex flow pattern; cone type: nickel alloy cone; cooling air flow rate: 14 L/min; atomizing air flow rate: 1.06 L/min; auxiliary air flow: 0.8 L/min; collider flow rate: 5.7 mL/min; peristaltic pump speed: 40 An rpm; pump lift time: 60 s.
Compared with the prior art, the invention has the advantages that:
1. compared with the existing method, the novel method for extracting the lithium element in the sediment does not need a digestion tank or a digestion instrument, has good extraction effect, high standard adding recovery rate of test results and small relative standard deviation;
2. the invention adopts high-temperature ultrasonic extraction directly in the plastic centrifuge tube with the cover of the 50 mL screw, and then centrifugal separation, thereby avoiding the solution loss caused by repeated transfer of solution, avoiding the problems of splashing of liquid drops and low extraction efficiency during heating, and greatly improving the efficiency of measuring batch samples;
3. the method adopts an ultrasonic-heating method, so that the particle size of sediment sample particles becomes smaller and more dispersed, the contact area of the sample particles and the acid extracting solution is increased, and the leaching efficiency of lithium elements from the sediment particles is ensured;
4. the purpose of the use of internal standard elements is to correct random errors generated during the measurement of the instrument. The method introduces germanium element as an internal standard, has the signal response intensity closest to that of the lithium element, and can well correct the testing process, thereby improving the stability and precision of the measurement, widening the measurement range, and being simple, convenient, quick and accurate.
Drawings
Fig. 1 is a standard working graph of lithium element obtained in the example.
Detailed Description
A method for determining lithium in a marine deposit comprising the steps of:
1) Removing foreign matters such as branches, leaves and stones from the collected marine sediment sample, drying the marine sediment sample by using an oven, grinding and sieving the marine sediment sample, accurately weighing 1.0 g, placing the marine sediment sample into a plastic centrifuge tube with a cover of 50 mL screw, adding 30 mL acid extract (formed by mixing concentrated nitric acid, concentrated hydrochloric acid and hydrofluoric acid according to a volume ratio of 15:10:5), and shaking the marine sediment sample uniformly;
2) Covering a cover on the centrifuge tube, but not completely screwing, inserting the centrifuge tube frame, adding hot water at 100 ℃, starting an ultrasonic machine to carry out ultrasonic treatment for 60 minutes, and simultaneously starting a heating function of the ultrasonic machine, wherein the heating temperature is 100 ℃; the power of the ultrasonic machine is more than or equal to 100W;
3) After the ultrasonic treatment is finished, taking out the centrifuge tube from the ultrasonic machine, cooling to room temperature, screwing the tube cover of the centrifuge tube, and placing the centrifuge tube cover on a centrifuge for centrifugation, wherein the rotation speed of the centrifugation is 2000 r/min, and the time is 10 min;
4) Taking out the centrifuge tube after centrifugation, taking supernatant 5 mL, diluting with ultrapure water, fixing the volume to a 50 mL measuring flask, and shaking uniformly to obtain a sample solution;
5) And (3) preparing a standard working curve: preparing lithium element standard working solutions with the concentrations of 5, 15, 25, 50, 75 and 100 ng/mL by adopting a lithium standard solution, measuring on an inductively coupled plasma mass spectrometer, and drawing a standard working curve of the lithium element by taking the concentration of the lithium element as an abscissa and the signal intensity of the lithium element as an ordinate;
6) Sample measurement: and measuring the lithium element signal intensity of the sample solution by using an inductively coupled plasma mass spectrometer, and then carrying the obtained signal intensity into a standard working curve to calculate so as to obtain the lithium element content in the sample solution.
Germanium is adopted as an internal standard element in inductively coupled plasma mass spectrum detection, and is added on line by a peristaltic pump.
The inductively coupled plasma mass spectrum detection conditions are as follows: plasma gas: argon gas with the purity of 99.999 percent; instrument power: 1550 W is a metal; detection type: a KED; type of atomizer: a gas vortex flow pattern; cone type: nickel alloy cone; cooling air flow rate: 14 L/min; atomizing air flow rate: 1.06 L/min; auxiliary air flow: 0.8 L/min; collider flow rate: 5.7 mL/min; peristaltic pump speed: 40 An rpm; pump lift time: 60 s.
The influence of the composition of the acid extracting solution on the extracting effect of the lithium element is examined by the experiment. The common acidic extracting solution systems are concentrated nitric acid-concentrated hydrochloric acid-hydrofluoric acid, concentrated nitric acid-concentrated sulfuric acid-hydrofluoric acid and concentrated nitric acid-perchloric acid-hydrofluoric acid. However, due to extremely strong oxidizing property and corrosiveness of perchloric acid, high-temperature extraction of the corrosion-prone centrifuge tube and great hidden danger to the safety of operators, the influence of a nitric acid-hydrochloric acid-hydrofluoric acid system and a nitric acid-sulfuric acid-hydrofluoric acid system on the extraction effect of lithium elements is examined only by a deposit sample adding standard mode (the adding standard concentration of the lithium elements in the deposit sample is 25 ng/g), and the test results are shown in table 1.
TABLE 1 influence of the composition of the acidic extract on the extraction effect of lithium elements
The result shows that the efficiency of extracting the lithium element by using the nitric acid-hydrochloric acid-hydrofluoric acid system is higher, and the accuracy of the method is higher.
The effect of the amount of the acidic extracting solution on the extracting effect of lithium element (the standard adding concentration of the lithium element in the sediment sample is 25 ng/g) is also examined in the test, and the test results are shown in Table 2.
TABLE 2 influence of the volume of acidic extract on the extraction effect of lithium element
The results showed that the deposit samples were the highest in the labeled recovery, 96.1% on average, and 1.0% on the relative standard deviation, when the amounts of nitric acid, hydrochloric acid, and hydrofluoric acid added were 15 mL, 10 mL, and 5 mL, respectively, at which time the method was the highest in accuracy and good in precision.
In order to make the contents of the present invention more easily understood, the technical scheme of the present invention will be further described with reference to the specific embodiments, but the present invention is not limited thereto.
Example 1
A method for determining lithium in a marine deposit comprising the steps of:
1) Removing foreign matters (branches, blades, stones and the like) from the collected marine sediment sample, drying in a laboratory by using an oven, grinding and sieving, accurately weighing the sediment sample after sieving by 1.0 g, placing the sediment sample into a plastic centrifuge tube with a cover of a 50 mL screw, adding an acidic extracting solution consisting of 15 mL concentrated nitric acid, 10 mL concentrated hydrochloric acid and 5 mL hydrofluoric acid, and shaking uniformly.
2) And (3) covering the centrifuge tube with a cover, but not completely screwing, inserting the centrifuge tube frame, adding hot water at 100 ℃, starting an ultrasonic machine for ultrasonic treatment for 60 minutes, starting a heating function of the ultrasonic machine, wherein the heating temperature is 100 ℃, and the power of the ultrasonic machine is greater than or equal to 100W.
3) And after the ultrasonic treatment is finished, taking the centrifuge tube out of the ultrasonic machine, cooling to room temperature, screwing the tube cover of the centrifuge tube, and placing the centrifuge tube cover on a centrifuge for centrifugation, wherein the centrifugation speed is 2000 r/min, and the time is 10 min.
4) After centrifugation, the centrifuge tube was removed, and the supernatant 5 mL was diluted with ultrapure water and was fixed to a volume of 50 mL in a measuring flask, and shaken well to obtain a sample solution.
5) Standard working curve formulation
The standard working solution of lithium element with the concentration of 5, 15, 25, 50, 75 and 100 ng/mL is prepared by using 2vol% nitric acid solution as diluent and lithium standard solution, then the prepared standard working solution is measured on an inductively coupled plasma mass spectrometer, and the standard working curve of the lithium element is drawn by using the concentration of the lithium element as an abscissa and the signal intensity of the lithium element as an ordinate, and the result is shown in figure 1.
6) Sample measurement
And measuring the lithium element signal intensity of the sample solution by using an inductively coupled plasma mass spectrometer, and then carrying the obtained signal intensity into a standard working curve to calculate so as to obtain the lithium element content in the sample solution.
The sample measurement process uses an internal standard germanium on-line to monitor and correct short-term drift and long-term drift of signals and correct and compensate matrix effects, and the internal standard germanium is added on-line by a peristaltic pump.
The detection conditions of the inductively coupled plasma mass spectrometer are as follows: plasma gas: argon gas with the purity of 99.999 percent; instrument power: 1550 W is a metal; detection type: KED (collision mode); type of atomizer: a gas vortex flow pattern; cone type: nickel alloy cone; cooling air flow rate: 14 L/min; atomizing air flow rate: 1.06 L/min; auxiliary air flow: 0.8 L/min; collider flow rate: 5.7 mL/min; peristaltic pump speed: 40 An rpm; pump lift time: 60 s.
7) Detection limit of instrument
The detection limit of the instrument is defined as the standard solution concentration corresponding to the ICP-MS response signal to noise ratio (S/N) of 3. The instrument detection limit of the Li element is 0.17 ng/mL according to the instrument response condition.
8) Accuracy and precision
The results of the standard recovery experiment of lithium element in the sediment are shown in Table 3.
Table 3 results of Li method accuracy experiments in deposits (n=7)
The results in Table 3 show that the recovery rate of lithium with different standard adding levels is between 85.92 and 103.01 percent, and the relative standard deviation of 3 parallel samples is between 0.32 and 1.77 percent, so that the method is proved to have high accuracy and good precision.
Example 2
The new energy enterprises in the coastal area of Sanshawan in Ningde city are more, the waste water of the new energy enterprises contains battery materials such as nickel cobalt lithium manganate, lithium manganate and the like, and lithium elements discharged into the ocean are Li +1 If the lithium-containing wastewater is discharged for a long time or the lithium element content in the ocean is increased due to sudden leakage, the ecological environment of the ocean is threatened. The method of example 1 is used for detecting the content of lithium element in marine sediments at 7 sampling sites of Sanshawan in Ningde city, and is used as a method support for evaluating the environmental pollution of the lithium in the Sanshawan. The specific operation is as follows:
1) Sample collection: and selecting the Sanshawan area of Ningde city as a research area, wherein the sampling time is 8 months, and 7 sampling stations are set from the top of the gulf to the gulf. Collecting surface layer bottom mud by a mud collector, taking 10 g by a plastic spoon, placing into a polyethylene bag, sealing and sealing, and finally obtaining 7 samples. Each sample bag is labeled, including sampling points and sampling times. And (5) placing the sample in an ice bath box for light-shielding preservation, collecting the sample, transporting the sample back to a laboratory, and placing the sample at the temperature of minus 20 ℃ for preservation.
2) Removing foreign matters (branches, blades, stones and the like) from the collected marine sediment sample, drying in a laboratory by using an oven, grinding and sieving, accurately weighing the sediment sample after sieving by 1.0 g, placing the sediment sample into a plastic centrifuge tube with a cover of a 50 mL screw, adding an acidic extracting solution consisting of 15 mL concentrated nitric acid, 10 mL concentrated hydrochloric acid and 5 mL hydrofluoric acid, and shaking uniformly.
3) And (3) covering the centrifuge tube with a cover, but not completely screwing, inserting the centrifuge tube frame, adding hot water at 100 ℃, starting an ultrasonic machine for ultrasonic treatment for 60 minutes, starting a heating function of the ultrasonic machine, wherein the heating temperature is 100 ℃, and the power of the ultrasonic machine is greater than or equal to 100W.
4) And after the ultrasonic treatment is finished, taking the centrifuge tube out of the ultrasonic machine, cooling to room temperature, screwing the tube cover of the centrifuge tube, and placing the centrifuge tube cover on a centrifuge for centrifugation, wherein the centrifugation speed is 2000 r/min, and the time is 10 min.
5) After centrifugation, the centrifuge tube was removed, and the supernatant 5 mL was diluted with ultrapure water and was fixed to a volume of 50 mL in a measuring flask, and shaken well to obtain a sample solution.
6) Sample measurement
And measuring the lithium element signal intensity of the sample solution by using an inductively coupled plasma mass spectrometer, and carrying the obtained signal intensity into the standard working curve obtained in the example 1 for calculation to obtain the lithium element content in the sample solution.
The sample measurement process uses an internal standard germanium on-line to monitor and correct short-term drift and long-term drift of signals and correct and compensate matrix effects, and the internal standard germanium is added on-line by a peristaltic pump.
The detection conditions of the inductively coupled plasma mass spectrometer are as follows: plasma gas: argon gas with the purity of 99.999 percent; instrument power: 1550 W is a metal; detection type: KED (collision mode); type of atomizer: a gas vortex flow pattern; cone type: nickel alloy cone; cooling air flow rate: 14 L/min; atomizing air flow rate: 1.06 L/min; auxiliary air flow: 0.8 L/min; collider flow rate: 5.7 mL/min; peristaltic pump speed: 40 An rpm; pump lift time: 60 s.
7) Blank test
The measurement results were quality-controlled by blank test and parallel samples (2 replicates were collected for each station). The deposit sample was not added and the Li in the deposit was measured to verify that no Li component was present in the reagents and materials used in the detection process. The test result shows that no Li element is detected in the blank sample, and the reagent and the material used in the detection process are proved to have no Li component.
8) Detection result
As can be seen from table 4, the concentration range of Li in the surface deposit of the sanshawan is 43.8-60.2 μg/g, and the average value is 52.4 μg/g. The Li content of each station has no obvious change rule, and the Li content of a station 1 sediment close to a new energy enterprise is relatively low, so that the Li in the Sanshawan sediment is inferred to be not polluted by land sources. The detection result can be used as a background reference value for measuring whether the Sanshawan Li is polluted or not, and data support is provided for emergent events such as Li leakage and the like.
TABLE 4 Li element content in Sanshawan deposit
The foregoing description is only of the preferred embodiments of the invention, and all changes and modifications that come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (6)
1. A method for determining lithium in a marine deposit comprising the steps of:
1) Preparation of sample solution: removing impurities in the collected marine sediment, drying, grinding and sieving, accurately weighing 1.0 g, placing into a 50 mL centrifuge tube, adding 30 mL acidic extract, and shaking; after ultrasonic treatment at 100 ℃ for 60 minutes, cooling to room temperature, centrifuging, taking supernatant 5 mL, diluting with ultrapure water, fixing the volume to a 50 mL measuring flask, and shaking uniformly to obtain a sample solution;
2) And (3) preparing a standard working curve: preparing lithium element standard working solutions with the concentrations of 5, 15, 25, 50, 75 and 100 ng/mL by adopting a lithium standard solution, measuring on an inductively coupled plasma mass spectrometer, and drawing a standard working curve of the lithium element by taking the concentration of the lithium element as an abscissa and the signal intensity of the lithium element as an ordinate;
3) Determination of sample solution: and measuring the lithium element signal intensity of the sample solution by using an inductively coupled plasma mass spectrometer, and obtaining the lithium element content in the sample solution according to the standard working curve of the obtained lithium element.
2. The method for determining lithium in marine sediments according to claim 1, wherein the acidic extracting solution in the step 1) is formed by mixing concentrated nitric acid, concentrated hydrochloric acid and hydrofluoric acid according to a volume ratio of 15:10:5.
3. The method for determining the lithium in marine sediments according to claim 1, wherein the centrifugal speed in the step 1) is 2000 r/min and the time is 10 min.
4. The method for determining lithium in marine sediments according to claim 1, wherein the standard working solution of lithium element is prepared by adopting 2vol% nitric acid solution in the step 2).
5. The method for determining the lithium in the marine sediment according to claim 1, wherein germanium is used as an internal standard element in inductively coupled plasma mass spectrometry.
6. The method for determining lithium in marine sediments according to claim 1, wherein the inductively coupled plasma mass spectrometry detection conditions are: plasma gas: argon gas with the purity of 99.999 percent; instrument power: 1550 W is a metal; detection type: a KED; type of atomizer: a gas vortex flow pattern; cone type: nickel alloy cone; cooling air flow rate: 14 L/min; atomizing air flow rate: 1.06 L/min; auxiliary air flow: 0.8 L/min; collider flow rate: 5.7 mL/min; peristaltic pump speed: 40 An rpm; pump lift time: 60 s.
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