CN110672707A - Method for measuring boron, arsenic, bromine and tungsten in geochemical sample by ICP-MS - Google Patents
Method for measuring boron, arsenic, bromine and tungsten in geochemical sample by ICP-MS Download PDFInfo
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Abstract
The invention relates to the technical field of environmental engineering, in particular to a method for measuring boron, arsenic, bromine and tungsten in a geochemical sample by ICP-MS; the method comprises the following steps: (1) alkali fusion treatment: adding sodium hydroxide into a geochemical sample, uniformly mixing, adding sodium peroxide, heating to 440-460 ℃, keeping the temperature for 25-35 min, then continuously heating to 690-710 ℃, and keeping the temperature for 8-12 min; (2) extraction: adding an ethanol solution into the geochemical sample after the alkali fusion treatment, washing with water, cooling, diluting with water, standing for clarification, and taking supernatant; (3) exchange treatment: and (3) adding cation exchange resin into the supernatant obtained in the step (2), and statically adsorbing for 0.8-1.2 h to be tested. The method realizes simultaneous determination of boron, arsenic, bromine and tungsten in the geochemical sample, integrates the original four matching schemes together, optimizes the method, not only saves the actual production cost, but also obviously improves the detection efficiency and simultaneously improves the detection accuracy.
Description
Technical Field
The invention relates to the technical field of environmental engineering, in particular to a method for measuring boron, arsenic, bromine and tungsten in a geochemical sample by ICP-MS.
Background
In a multi-target matching method, the boron is measured by adopting an emission spectrometry, the electric arc direct-reading emission spectrometry has high sensitivity and low analysis component, but the analysis steps are complicated, the analysis time is long, and the analysis result is greatly influenced by the emission spectrometry process; in addition, the measurement of boron also comprises closed acid dissolution-ICP-MS method, ICP-OES method, alkali fusion-ICP-MS method and the like, but the open sample dissolution of mixed acid is easy to volatilize boron, and the temperature is not easy to control; the closed acid dissolution solves the problem of easy volatilization of boron, but the time is too long; microwave digestion is not suitable for analysis of large-batch chemical samples; the problem of high salt content needs to be solved in the alkali fusion ICP-MS measurement of samples.
Arsenic is decomposed by aqua regia, hydride generation-atomic fluorescence spectrometry, and the atomic fluorescence method belongs to single element measurement and cannot realize simultaneous measurement of multiple elements. Although the hydride generation-inductively coupled plasma emission spectrometry solves the above problems, the sensitivity and precision of the analytical elements need to be improved.
The bromine is measured by powder tabletting method and directly by X-ray fluorescence spectrometer. However, the analysis process is easily contaminated and the cost is high.
And the determination of tungsten adopts alkali fusion decomposition and the determination of inductively coupled plasma mass spectrometry after acidification.
Therefore, four elements (boron, arsenic, bromine and tungsten) in the geochemical sample need four ore melting methods, and relate to four detection means (an emission spectrometer, an atomic fluorescence spectrometer, an X-fluorescence spectrometer and an inductively coupled plasma mass spectrometer), so that the analysis cost is high, and the analysis and detection efficiency is low.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
In order to solve the technical problems, the invention provides the method for measuring the boron-arsenic-tungsten bromide in the geochemical sample by the ICP-MS, which can realize one-time measurement of the boron-arsenic-tungsten bromide in the geochemical sample, thereby saving the cost and obviously improving the detection efficiency.
Specifically, a geochemical sample is subjected to an alkali fusion treatment with an alkali and then to an exchange treatment with a cation exchange resin.
Geochemical samples of the invention include, but are not limited to, soil or water based sediments; the geochemical sample is treated by alkali fusion, a large amount of sodium salt and nickel ions are introduced into fused ores in a nickel crucible, the determination of four elements (boron-arsenic-bromine-tungsten) is influenced, and the expected requirements are difficult to achieve by direct dilution because the salt content and the nickel ion content are very high and the abundance values of the four elements (boron-arsenic-bromine-tungsten) are not high; further, the present inventors have found that the exchange treatment with a cation exchange resin is carried out to exchange H in the cation exchange resin+Exchange with a large amount of sodium ions in the solution, and simultaneously exchange a large amount of metal ions such as nickel, lead, copper and the like in the solution, reduce the matrix interference of salt and the metal ions, and realize the simultaneous determination of boron, arsenic, bromine and tungsten in the geochemical sample.
Preferably, the base is sodium hydroxide and/or sodium peroxide.
Preferably, the base is sodium hydroxide or sodium peroxide (preferably).
Preferably, the mass ratio of the alkali to the geochemical sample is 8-10: 1.
in a specific embodiment, the present invention employs a 732 type cation exchange resin for the exchange treatment.
In order to further improve the accuracy of the determination method, the determination method is optimized (all the preferable schemes are combined to obtain the optimal scheme of the invention), and the method comprises the following specific steps:
preferably, the alkali fusion treatment adopts a step-by-step heating method: the temperature is raised to 440-460 ℃ and kept for 25-35 min, and then the temperature is raised to 690-710 ℃ and kept for 8-12 min.
The alkali fusion treatment according to the present invention is preferably carried out in a muffle furnace; the distributed heating can enable the melting to be more complete, the NaOH is splashed out to cause fluorine loss due to too fast temperature rise, and the measured value can be closer to the true value due to the distributed heating.
Preferably, the method of the present invention further comprises the step of extracting: adding an ethanol solution into the geochemical sample after the alkali fusion treatment, washing with water, cooling, diluting with water, standing for clarification, and taking supernatant; the extraction step is carried out after the alkali fusion treatment.
Preferably, the mass-to-volume ratio of the geochemical sample to the ethanol solution, in g/ml, is 0.5-1.5: 1.
preferably, the mass-to-volume ratio of the cation exchange resin to the supernatant in g/ml is 1: 1.5 to 2.5.
As a preferred embodiment of the present invention, the method of the present invention comprises the steps of:
(1) alkali fusion treatment: adding sodium hydroxide into a geochemical sample, uniformly mixing, adding sodium peroxide, heating to 440-460 ℃, keeping the temperature for 25-35 min, then continuously heating to 690-710 ℃, and keeping the temperature for 8-12 min;
(2) extraction: adding an ethanol solution into the geochemical sample after the alkali fusion treatment, washing with water, cooling, diluting with water, standing for clarification, and taking supernatant;
(3) exchange treatment: and (3) adding cation exchange resin into the supernatant obtained in the step (2), and statically adsorbing for 0.8-1.2 h to be tested.
The invention has the beneficial effects that:
in the multi-target matching method, four elements of boron, arsenic, bromine and tungsten in a geochemical sample are measured, and four matching methods and four instruments are involved.
Drawings
FIG. 1 is a flow chart of example 1.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
The instrumentation and reagents involved in the examples are as follows:
iCAPQa inductively coupled plasma mass spectrometer (thermoelectric corporation, usa).
Type 732 cation exchange resin: soaking cation exchange resin in water, cleaning for several times, loading the resin into a glass column with diameter of about 1.5cm and length of about 30cm, and connecting the top end with a pear-shaped separating funnel; adding 150mL of sulfuric acid (2mol/L) into a separating funnel, flowing through an exchange column at the flow rate of 1.5mL/min, after the flow is finished, flowing through the exchange column with water at the same flow rate until the effluent is washed to be free of sulfate radicals, carrying out vacuum filtration on the regenerated resin until the regenerated resin is dried, and bottling for later use.
The sodium hydroxide, the sodium peroxide and the absolute alcohol are analytically pure, and the experimental water is distilled water.
Example 1
The embodiment provides a method for measuring boron, arsenic, bromine and tungsten in a geochemical sample by ICP-MS, which comprises the following steps (as shown in figure 1):
(1) alkali fusion treatment: weighing 0.5g of a geochemical sample, placing the geochemical sample in a nickel crucible, adding 4.0g of sodium hydroxide, uniformly mixing, adding 0.5g of sodium peroxide, placing the mixture in a muffle furnace, firstly heating to 450 ℃, firing for 30min, then continuously heating to 700 ℃, and preserving heat for 10 min;
(2) extraction: taking the nickel crucible out of the muffle furnace, slightly cooling, placing the nickel crucible in a plastic beaker filled with 50mL of boiling water, adding 0.5mL of ethanol solution into the nickel crucible, washing the nickel crucible with water after the melt completely falls off, cooling to room temperature, transferring into a 100mL plastic volumetric flask, diluting with water to a scale, shaking up, standing for clarification, and taking 10mL of supernatant;
(3) exchange treatment: and (3) adding 5g of 732 type cation exchange resin into the supernatant obtained in the step (2), and statically adsorbing for 1h to be tested.
(4) Standard solution:
the rhodium internal standard mother liquor is 1000 mug/mL and is diluted by water to the working solution concentration of 10 ng/mL.
The standard solution of boron, arsenic, bromine and tungsten is 1000 mug/mL (national iron and steel test center); for convenient use, preparing four single element standard solutions into a mixed standard solution; diluting the mixed standard solution to a scale by using a 2% sodium hydroxide solution, and preparing a working curve solution along with the supernatant of the geochemical sample; the concentrations of the elements in the mixed standard solution are shown in table 1;
TABLE 1 concentration of each element in the mixed standard solution
(5) Parameters of ICP-MS are as shown in Table 2;
TABLE 2 parameters of ICP-MS
The experimental verification process and the results of the method of the invention are shown in experimental example 1.
Experimental example 1 accuracy, precision, detection Limit of the method
(1) Method accuracy
In the experimental example, 12 national water system sediments and soil standard substances are selected as samples to be tested, and the test is carried out according to the method in the example 1, and the results are shown in a table 3;
TABLE 3 accuracy of the method
As can be seen from Table 3, the accuracy logarithmic errors △ lgC of the methods of the four elements B, As, Br and W are all less than 0.05, and the requirements of 'DZ/T0130.5-2006 geological mineral laboratory test quality specifications' (△ lgC is less than or equal to 0.1 within the three-time detection limit, △ lgC is more than the three-time detection limit is less than or equal to 0.05) in geological samples are met.
(2) Precision and detection limits of the method
According to the method of example 1, selecting national standard substances GSS-22, GSS-13 and GSD-8a to perform 12 times of measurement to determine the relative standard deviation of the method, simultaneously preparing 12 parts of blank solution, and calculating the detection limit by a three-time standard deviation (3S) calculation method; the results are shown in tables 4 and 5;
precision of the method of Table 4
TABLE 5 detection limits of the methods
In DZ/T0130.5-2006 geological mineral laboratory test quality specification, the detection limits of B, As, Br and W are 1 mug/g, 1.5 mug/g and 0.4 mug/g in sequence, the detection limit is more than 3 times and less than 1%, and the precision requirement is less than 10%; as can be seen from Table 5, the detection limits of B, As, Br and W in the method are 0.872. mu.g/g, 0.147. mu.g/g, 0.923. mu.g/g and 0.261. mu.g/g in sequence, and the precision is less than 5 percent, thereby meeting and being superior to the standard requirement.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (9)
1. The ICP-MS method for measuring boron, arsenic, bromine and tungsten in a geochemical sample is characterized in that alkali fusion treatment is carried out on the geochemical sample by alkali, and then exchange treatment is carried out by cation exchange resin.
2. The method of claim 1, wherein the base is sodium hydroxide and/or sodium peroxide.
3. The method of claim 1 or 2, wherein the base is sodium hydroxide or sodium peroxide.
4. A method according to any one of claims 1 to 3, wherein the ratio of the alkali to the geochemical sample is from 8 to 10: 1.
5. the method according to any one of claims 1 to 4, wherein the alkali fusion treatment is carried out by a stepwise temperature rise method: the temperature is raised to 440-460 ℃ and kept for 25-35 min, and then the temperature is raised to 690-710 ℃ and kept for 8-12 min.
6. The method according to any one of claims 1 to 5, further comprising the step of extracting: adding an ethanol solution into the geochemical sample after alkali fusion treatment, washing with water, cooling, diluting with water, standing for clarification, and taking supernatant.
7. The method according to claim 6, wherein the mass to volume ratio of the geochemical sample to the ethanol solution, in g/ml, is from 0.5 to 1.5: 1.
8. the method according to claim 6, wherein the mass to volume ratio of the cation exchange resin to the supernatant in g/ml is 1: 1.5 to 2.5.
9. A method according to any one of claims 1 to 8, comprising the steps of:
(1) alkali fusion treatment: adding sodium hydroxide into a geochemical sample, uniformly mixing, adding sodium peroxide, heating to 440-460 ℃, keeping the temperature for 25-35 min, then continuously heating to 690-710 ℃, and keeping the temperature for 8-12 min;
(2) extraction: adding an ethanol solution into the geochemical sample after the alkali fusion treatment, washing with water, cooling, diluting with water, standing for clarification, and taking supernatant;
(3) exchange treatment: and (3) adding cation exchange resin into the supernatant obtained in the step (2), and statically adsorbing for 0.8-1.2 h to be tested.
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Cited By (5)
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| CN111398401A (en) * | 2020-04-10 | 2020-07-10 | 浙江省地质矿产研究所 | Method for determining boron in soil by using alkali fusion-static ion exchange-inductively coupled plasma mass spectrometry |
| CN112147116A (en) * | 2020-09-17 | 2020-12-29 | 中化地质矿山总局地质研究院 | Method for measuring germanium in geochemical sample by alkali fusion-atomic fluorescence spectrometry |
| CN112147209A (en) * | 2020-09-21 | 2020-12-29 | 中化地质矿山总局地质研究院 | Method for measuring arsenic in geochemical sample by ICP-MS |
| CN112147118A (en) * | 2020-09-21 | 2020-12-29 | 中化地质矿山总局地质研究院 | Method for determining 34 elements in geochemical sample |
| CN113670897A (en) * | 2021-09-13 | 2021-11-19 | 广东韶钢松山股份有限公司 | Method for rapidly determining content of boron oxide and aluminum oxide in slag condenser for steelmaking |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111398401A (en) * | 2020-04-10 | 2020-07-10 | 浙江省地质矿产研究所 | Method for determining boron in soil by using alkali fusion-static ion exchange-inductively coupled plasma mass spectrometry |
| CN112147116A (en) * | 2020-09-17 | 2020-12-29 | 中化地质矿山总局地质研究院 | Method for measuring germanium in geochemical sample by alkali fusion-atomic fluorescence spectrometry |
| CN112147209A (en) * | 2020-09-21 | 2020-12-29 | 中化地质矿山总局地质研究院 | Method for measuring arsenic in geochemical sample by ICP-MS |
| CN112147118A (en) * | 2020-09-21 | 2020-12-29 | 中化地质矿山总局地质研究院 | Method for determining 34 elements in geochemical sample |
| CN113670897A (en) * | 2021-09-13 | 2021-11-19 | 广东韶钢松山股份有限公司 | Method for rapidly determining content of boron oxide and aluminum oxide in slag condenser for steelmaking |
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