CN111398399A - Method for determining silver by inductively coupled plasma mass spectrometry - Google Patents
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- 229910052709 silver Inorganic materials 0.000 title claims abstract description 50
- 239000004332 silver Substances 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 title claims abstract description 15
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000002689 soil Substances 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 239000000243 solution Substances 0.000 claims abstract description 13
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001819 mass spectrum Methods 0.000 claims abstract description 10
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 10
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000012490 blank solution Substances 0.000 claims abstract description 9
- 238000009616 inductively coupled plasma Methods 0.000 claims abstract description 9
- 239000012086 standard solution Substances 0.000 claims abstract description 9
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 7
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 6
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000005303 weighing Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000007789 gas Substances 0.000 claims description 8
- 239000013049 sediment Substances 0.000 claims description 8
- 239000001307 helium Substances 0.000 claims description 7
- 229910052734 helium Inorganic materials 0.000 claims description 7
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000012159 carrier gas Substances 0.000 claims description 3
- 239000000112 cooling gas Substances 0.000 claims description 3
- 238000005485 electric heating Methods 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 3
- 230000010354 integration Effects 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 238000005070 sampling Methods 0.000 claims description 3
- 150000003378 silver Chemical class 0.000 claims description 3
- 238000009736 wetting Methods 0.000 claims description 3
- 238000009532 heart rate measurement Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 239000000779 smoke Substances 0.000 abstract description 3
- 238000001514 detection method Methods 0.000 description 20
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 11
- 239000010955 niobium Substances 0.000 description 11
- 229910052758 niobium Inorganic materials 0.000 description 10
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 10
- 229910052726 zirconium Inorganic materials 0.000 description 10
- 238000005259 measurement Methods 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000004993 emission spectroscopy Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000012937 correction Methods 0.000 description 2
- 238000000673 graphite furnace atomic absorption spectrometry Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000012495 reaction gas Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 239000011573 trace mineral Substances 0.000 description 2
- 235000013619 trace mineral Nutrition 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910000484 niobium oxide Inorganic materials 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 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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Abstract
The invention discloses a method for determining silver by an inductively coupled plasma mass spectrometry, which comprises the steps of weighing a soil sample to be determined, adding perchloric acid, nitric acid and hydrofluoric acid, heating to 200 ℃, when white smoke is exhausted, cooling to 160 ℃, adding aqua regia and an internal standard solution, slightly heating until the solution is clear, taking down and cooling, taking out a clear solution of 0.5m L, adding dilute nitric acid of 5m L into a polytetrafluoroethylene crucible, shaking uniformly to obtain a liquid to be determined, measuring mass spectrum counting of silver in a KED mode on an inductively coupled plasma mass spectrometer, determining a working curve, preparing a sample blank solution, substituting an emission intensity counting value into the working curve, and calculating the silver content according to a formula.
Description
Technical Field
The invention relates to the technical field of trace element determination, in particular to a method for determining silver by an inductively coupled plasma mass spectrometry.
Background
Soil is the most fundamental and important natural resource for human survival development, and surface soil has been commonly contaminated to varying degrees as human production activities have gone through considerable periods of time, especially with the rapid development of modern industries. Therefore, the method is an important basic work for measuring the contents of the constant and secondary elements and the trace elements in the soil, and has important significance for monitoring the ecological environment, researching regional resources, regulating and controlling agricultural economy and planning sustainable development of national economy.
At present, silver in domestic soil and water system sediments is mainly measured by an emission spectrometry or a graphite furnace atomic absorption spectrometry, the emission spectrometry adopts an electric arc to excite a powder sample, the introduced reagent blank is low, the detection of a low-content sample is very favorable, but the linear range is narrow, and in addition, the detection effect is not ideal enough for organic matter, sulfide and carbonate samples due to easy splashing. While graphite furnace atomic absorption spectrometry can also obtain ideal detection effect, due to single measurement, the detection efficiency is low, and the requirement of batch detection is difficult to meet. The inductively coupled plasma mass spectrometry has the characteristics of simultaneous determination of single elements, high sensitivity and high detection speed, and has more work in recent yearsAttempts have been made to determine silver in soil and water based deposits using inductively coupled plasma mass spectrometry,107ag receiver91Zr16Interference of O and109ag receiver93Nb16The interference of O is difficult to realize the direct determination of silver on a mass spectrometer, at present, the interference is eliminated by a chemical method for precipitating zirconium and niobium or a method for adsorbing zirconium and niobium by resin, and then the determination is carried out, the flow is long, the procedure is complicated, a reagent blank is easy to introduce, and the determination effect is not ideal.
The method can also be used for simultaneously measuring various elements such as copper, lead, zinc, nickel and cadmium in the soil, has high working efficiency and simple operation, and has the advantages of higher sensitivity, lower detection limit, stronger anti-interference capability, higher accuracy and the like compared with an emission spectrometry by utilizing the inductively coupled plasma mass spectrometry for measurement. The detection limit of the silver is 0.002 mug/g respectively after measurement, which is lower than the detection limit of an emission spectrometry. Due to the fact that the content of silver in a geochemical sample is low, the existing method is interfered by zirconium and niobium oxide ions to silver, actual detection limit is high, and signal-to-back ratio is low, so that trace silver elements in soil and water system sediments cannot be directly and accurately determined.
Disclosure of Invention
The method can eliminate the interference of oxide ions of zirconium and niobium by a collision reaction mode of introducing helium in a KED mode, obviously reduces the detection limit, increases the signal-to-back ratio, and has the key point that when the flow of inert gas is increased to 7.2m L/min, although the signal response value is reduced by 5-10 times, the interference of the oxides of zirconium and niobium can be reduced by about 20 times, the actual detection capability is essentially improved, so that the method can directly measure the silver in soil and water system sediments without adopting interference coefficient correction and chemical separation of zirconium and niobium.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a method for determining silver by inductively coupled plasma mass spectrometry comprises the following steps:
(1) weighing 0.2000g of soil or water system sediment sample to be detected in a polytetrafluoroethylene crucible, wetting the sample with a small amount of water, adding 1m L perchloric acid, 2-3m L nitric acid and 2-3m L hydrofluoric acid, heating to 200 ℃ until white smoke is exhausted, adding 5-6m L1 +1 aqua regia (1+1) when the temperature is reduced to about 160 ℃ and the solution is hot, adding 10.00m L internal standard solution, continuously heating on an electric heating plate for 5-10min until the solution is clear, taking down and cooling, placing the solution on an oscillator to shake uniformly, transferring 0.5m L clear liquid into the polytetrafluoroethylene crucible, adding 5m L dilute nitric acid, and shaking uniformly to obtain liquid to be detected;
(2) setting working parameters on an inductively coupled plasma mass spectrometer, pumping a measured liquid into an atomizer, introducing an atomizing gas into plasma flame by using argon as a carrier gas to excite ionization, measuring the mass spectrum count of silver in a KED mode, wherein the KED mode gas is helium, the flow rate is 7.2m L/min, measuring a working curve, preparing a sample blank solution, substituting the obtained emission intensity meter value into the working curve, calculating the content of silver in the liquid to be measured, and calculating the content of silver according to the following formula;
in the formula: m is1-from the working curve the silver content, ng, in the liquid to be measured;
m0-finding the silver content, ng, in the blank solution from the working curve;
ms-sample mass, g.
Preferably, the internal standard solution is 200ng/m L Rh and 200ng/m L Re.
Preferably, the inductively coupled plasma mass spectrometer sets working parameters of 1400W of power, 14L/min of cooling gas, 0.8L/min of auxiliary gas flow, 1.1L/min of atomizer flow rate, 15s of sample injection and flushing time, peak jump in a scanning mode, 0.15s of residence time, 6s of single element integration time, pulse measurement mode,
A sampling cone with the diameter of 1.1mm,
Intercepting 0.7mm, Rh mass number 103 and Re mass 185, and detecting109Ag。
Preferably, the sample has a particle size of less than 0.097mm and is dried at 105 ℃ for 2 h.
Preferably, the method for drawing the working curve comprises the following steps: and (3) dividing a series of silver standard solutions, preparing a solution to be detected according to the step (1), detecting the mass spectrum counting of the silver on an inductively coupled plasma mass spectrometer according to the step (2), and drawing a working curve according to the mass spectrum counting.
Compared with the prior art, the invention has the advantages and beneficial effects that:
1. the method can eliminate the interference of oxide ions of zirconium and niobium by a collision reaction mode of introducing helium in a KED mode, the detection limit is obviously reduced, the signal-to-back ratio is increased, the key is to increase the flow of helium to 7.2m L/min (the flow of helium is lower and generally does not exceed 5m L/min in order to ensure sufficient signal intensity when the KED mode is automatically tuned, and the yield of the oxide is still higher at the moment), although the signal response of an instrument is reduced by 5-10 times at the flow, the signal-to-back ratio is not greatly improved, but the interference of the oxide ions of zirconium and niobium can be reduced by about 20 times, the actual detection capability is essentially improved, so that the interference of the oxide ions of zirconium and niobium to silver in soil and water system sediments can be directly detected without correcting an interference coefficient and chemically separating the zirconium and the niobium.
2. The method has the advantages of higher sensitivity, lower detection limit, stronger anti-interference capability, higher accuracy and the like, can directly measure the silver in soil and water system sediments without interference coefficient correction and chemical separation of zirconium and niobium, and has simple operation and high working efficiency.
Drawings
FIG. 1 is a standard operating curve of elemental silver.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments. It should be emphasized that the following description is merely exemplary in nature and is not intended to limit the scope of the invention or its application.
The materials, reagents and the like used in the following examples are commercially available unless otherwise specified, and only reagents and ultrapure water identified as superior grade are used in the analysis, and hydrochloric acid (ρ ═ 1.19g/m L), nitric acid (ρ ═ 1.40g/m L), hydrofluoric acid (ρ ═ 1.13g/m L), perchloric acid (ρ ═ 1.67g/m L), aqua regia (1+1) are prepared by mixing 750m L hydrochloric acid with 250m L nitric acid, adding 1000m L water, shaking and formulating.
Example 1
A method for determining silver by inductively coupled plasma mass spectrometry comprises the following steps:
(1) weighing 0.2000g of soil sample to be detected (the grain size of the sample is less than 0.097mm, and the sample is dried at 105 ℃ for 2 hours) in a 30ml polytetrafluoroethylene crucible, wetting the soil sample with a small amount of water, adding 1m L perchloric acid, 3m L nitric acid and 3m L hydrofluoric acid, heating to 200 ℃ until white smoke is exhausted, cooling to 160 ℃ while the temperature is still hot, adding 6m L1 +1 aqua regia, adding 10.00m L internal standard solution (200ng/m L +200ng/m L Re), continuously heating on an electric heating plate for 5-10min until the solution is clear, taking down and cooling, placing the solution on an oscillator for shaking uniformly, transferring clear solution 0.5m L into the polytetrafluoroethylene crucible, adding dilute nitric acid (the concentration is 1%) and 5m L, and shaking uniformly to obtain liquid to be detected;
(2) on an inductively coupled plasma mass spectrometer, working parameters are set as 1400W of power, 14L/min of cooling gas, 0.8L/min of auxiliary gas flow, 1.1L/min of atomizer flow rate, 15s of sample injection and flushing time, peak jump in a scanning mode, 0.15s of residence time, 6s of single element integration time, pulse in a measuring mode, pulse in a pulse mode and pulse in a pulse mode,
A sampling cone with the diameter of 1.1mm,
Intercepting 0.7mm, Rh mass number 103, Re mass number 185 and silver mass number 109, pumping the measured liquid into an atomizer, introducing the atomized gas into a plasma flame to excite ionization by using argon as a carrier gas, and carrying out a KED (KED) modeHelium is used as reaction gas, the flow rate is 7.2m L/min), the mass spectrum counting of the silver is measured, the measurement of a working curve is carried out, a sample blank solution is prepared, the obtained value of the emission intensity meter is substituted into the working curve, the content of the silver in the liquid to be measured is calculated, and then the content of the silver is calculated according to the following formula.
In the formula: m is1-from the working curve the silver content, ng, in the liquid to be measured;
m0-finding the silver content, ng, in the blank solution from the working curve;
mS-sample mass, g.
The drawing method of the working curve comprises the following steps: and (3) dividing a series of silver standard solutions, preparing a solution to be detected according to the step (1), measuring the mass spectrum counting of the silver on an inductively coupled plasma mass spectrometer according to the step (2), and drawing a working curve according to the mass spectrum counting, wherein the result is shown in table 1 and is shown in attached figure 1.
Table 1: working curve of silver element
| Concentration (ug/L) | Emission intensity count value |
| 0.00 | 43 |
| 0.20 | 4237 |
| 0.50 | 10369 |
| 1.00 | 21076 |
| 5.00 | 101391 |
| 10.0 | 195077 |
| 20.0 | 389642 |
The method is used for verifying the accuracy, 25 geochemical primary standard substances (water system sediments and soil) are selected, a corresponding solution to be detected is prepared according to the step (1), a sample blank solution is prepared at the same time, then inductively coupled plasma mass spectrometry is added, the mass spectrometry count of silver is measured in a KED mode (helium is used as reaction gas, the flow is 7.2m L/min), the measurement result is substituted into the standard curve of each element, then the content of the silver is calculated respectively, and the measurement result is shown in the following table 2.
TABLE 2 Standard values and measured values of national silver standards
Note: when the content detection limit is more than 3 times, the element accuracy meets the requirement that the absolute value of delta log C is less than or equal to 0.05.
The detection limit of each element in the blank solution was measured by a 3-fold signal-to-noise ratio method, and the results are shown in table 3.
TABLE 3 detection limits of silver element
From the results, the detection limit of the silver element measured by the method reaches 0.002 mu g/g, which is obviously higher than that of the existing detection method.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. It will be apparent to those skilled in the art that various substitutions and modifications can be made to the described embodiments without departing from the spirit of the invention, and such substitutions and modifications are to be considered as within the scope of the invention.
Claims (5)
1. A method for determining silver by inductively coupled plasma mass spectrometry is characterized by comprising the following steps:
(1) weighing 0.2000g of soil or water system sediment sample to be detected in a polytetrafluoroethylene crucible, wetting with a small amount of water, adding 1m L perchloric acid, 2-3m L nitric acid and 2-3m L hydrofluoric acid, adding 5-6m L1 +1 aqua regia when the temperature is reduced to about 160 ℃, adding 10.00m L internal standard solution, continuously heating on an electric heating plate for 5-10min until the solution is clear, taking down and cooling, placing on an oscillator to shake uniformly, transferring 0.5m L clear liquid into the polytetrafluoroethylene crucible, adding 5m L dilute nitric acid, and shaking uniformly to obtain liquid to be detected;
(2) setting working parameters on an inductively coupled plasma mass spectrometer, pumping a measured liquid into an atomizer, introducing an atomizing gas into plasma flame by using argon as a carrier gas to excite ionization, measuring the mass spectrum counting of silver in a KED mode, introducing helium as a collision gas in the KED mode, measuring a working curve, preparing a sample blank solution, substituting the obtained emission intensity counting value into the working curve, and calculating the content of silver according to the following formula;
in the formula: m is1-from the working curve the silver content, ng, in the liquid to be measured;
m0by finding the blank solution from the working curveSilver content, ng;
mS-sample mass, g.
2. The method for measuring silver by inductively coupled plasma mass spectrometry as claimed in claim 1, wherein the internal standard solution is 200ng/m L Rh and 200ng/m L Re.
3. The method for measuring silver by the inductively coupled plasma mass spectrometry as claimed in claim 1, wherein the inductively coupled plasma mass spectrometer is set to have the operating parameters of 1400W of power, 14L/min of cooling gas, 0.8L/min of auxiliary gas flow, 1.1L/min of atomizer flow rate, 15s of sample flushing time, peak jump in a scanning mode, 0.15s of residence time, 6s of single element integration time, pulse measurement mode,
A sampling cone with the diameter of 1.1mm,
Intercepting 0.7mm, Rh mass number 103 and Re mass 185, and detecting109Ag。
4. The method for determining silver by inductively coupled plasma mass spectrometry as claimed in claim 1, wherein: the sample has a particle size of less than 0.097mm and is dried at 105 ℃ for 2 hours.
5. The method for determining silver by inductively coupled plasma mass spectrometry as claimed in claim 1, wherein: the drawing method of the working curve comprises the following steps: and (3) dividing a series of silver standard solutions, preparing a solution to be detected according to the step (1), detecting the mass spectrum counting of the silver on an inductively coupled plasma mass spectrometer according to the step (2), and drawing a working curve according to the mass spectrum counting.
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| CN114608931A (en) * | 2022-03-11 | 2022-06-10 | 江苏省南通环境监测中心 | Pretreatment method for determining silver in soil and sediment by inductively coupled plasma mass spectrometry |
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