CN111398400B - Method for determining Se and Te by alkali fusion inductively coupled plasma mass spectrometry - Google Patents

Method for determining Se and Te by alkali fusion inductively coupled plasma mass spectrometry Download PDF

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CN111398400B
CN111398400B CN202010244580.4A CN202010244580A CN111398400B CN 111398400 B CN111398400 B CN 111398400B CN 202010244580 A CN202010244580 A CN 202010244580A CN 111398400 B CN111398400 B CN 111398400B
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阳国运
何雨珊
潘倩妮
覃盛
张文捷
刘梓楠
黄献珠
齐永辉
黄庆柒
唐裴颖
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Guangxi Geology & Mineral Test Research Center
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Abstract

The invention discloses a method for determining Se and Te by an alkali fusion inductively coupled plasma mass spectrometry, which comprises the steps of weighing a soil sample to be determined, melting and decomposing the soil sample by sodium peroxide, adding tartaric acid into solution to enable tungsten, molybdenum, tin and the like to form complex anions, adding 732 type cation exchange resin, adsorbing most of sodium, iron, aluminum, zinc and the like in the solution onto the resin, and obtaining a solution to be determined; measuring the mass spectrum counting of selenium and tellurium on an inductively coupled plasma mass spectrometer in a KED mode, simultaneously measuring a working curve, substituting the obtained emission intensity meter value into the working curve, and calculating the content of selenium and tellurium in the liquid to be measured. According to the method, the hydrogen is used as the reaction gas of the collision pool, the interference of polyatomic ions such as double argon, argon and chlorine is eliminated, the signal-to-back ratio is improved by 5-10 times, the selenium detection limit is 0.005 microgram/g, the tellurium detection limit is 0.002 microgram/g, and the problems that the current polyatomic ions such as double argon or chlorine argon and zinc oxide have the interference on selenium and tellurium, the signal-to-back ratio is low, and the detection limit cannot meet the detection requirement are solved.

Description

Method for determining Se and Te by alkali fusion inductively coupled plasma mass spectrometry
Technical Field
The invention relates to the technical field of soil trace element determination, in particular to a method for determining Se and Te by an alkali fusion 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, selenium and tellurium in soil and water system sediments are generally detected by dissolving ores with (acid, hydrofluoric acid and perchloric acid) or (nitric acid and perchloric acid), heating until concentrated perchloric acid is emitted, taking off the ores, cooling, reducing hexavalent selenium and tellurium by 1+1 hydrochloric acid, adding ferric salt, and then respectively detecting selenium and tellurium by an atomic fluorescence method. Because the inductively coupled plasma mass spectrometry has the characteristics of simultaneous determination of single elements, high sensitivity and high detection speed, in recent years, workers try to determine tellurium in soil and water system sediments by using the inductively coupled plasma mass spectrometry, but excessive treatment is not carried out on the interference of tellurium, and the accuracy of results is difficult to ensure by complex samples. For selenium, the detection limit is difficult to meet the detection requirement due to the interference of polyatomic ions such as double argon, chlorine argon, zinc oxide and the like.
For example, the Chinese patent discloses a method for simultaneously measuring iodine, boron, tin and germanium elements in soil, which comprises the steps of raw material pretreatment, determination liquid preparation, working curve drawing and determination of the content of each element in the soil. The raw material pretreatment is to use sodium peroxide for pretreatment, a citric acid solution and cationic resin are added into a pretreated sample to prepare a determination solution, and the obtained determination solution is determined by adopting an inductively coupled plasma mass spectrometry. The method can simultaneously measure a plurality of elements of iodine, boron, tin and germanium in the soil, has high working efficiency and simple operation, utilizes the inductively coupled plasma mass spectrometry to measure, and has the advantages of higher sensitivity, lower detection limit, stronger anti-interference capability, higher accuracy and the like compared with the atomic fluorescence spectrometry. The detection limits of the elements are respectively 0.005 mu g/g of selenium and 0.002 mu g/g of tellurium after determination, which is superior to the detection limit of the atomic fluorescence spectrometry. For example, zhang Jie discloses a method for determining tungsten, molybdenum, tin, germanium, selenium and tellurium in lead-zinc ore by using resin exchange separation-inductively coupled plasma mass spectrometry, wherein the detection limits of selenium and tellurium in the method are 0.05 mu g/g and 0.03 mu g/g respectively. Because the selenium and tellurium content in the soil is low, the interference of polyatomic ions such as double argon or chlorine argon and zinc oxide on the selenium and tellurium cannot be eliminated by the conventional method, the detection limit is high, and a small amount of selenium and tellurium elements in the soil cannot be accurately determined.
Disclosure of Invention
The invention aims to provide a method for determining Se and Te by an alkali fusion inductively coupled plasma mass spectrometry. The method can completely dissolve selenium and tellurium by adopting alkali fusion, not only removes a large amount of salt through resin adsorption, but also eliminates the interference of zinc, and then eliminates the interference of double-argon polyatomic ions through a KED mode (taking hydrogen as reaction gas and having the flow of 6.2 mL/min), thereby further leading the double-argon polyatomic ions to be capable of dissolving selenium and tellurium completely 78 The signal-to-back ratio of Se is improved by 5 to 10 times, and most metal ions are removed by resin adsorption, 126 the interference on Te is obviously reduced, and the actual detection limit is obviously reduced, so that the selenium and tellurium in the soil and the water system sediments can be simultaneously measured, and the result is accurate and the efficiency is high.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a method for determining Se and Te by alkali fusion inductively coupled plasma mass spectrometry comprises the following steps:
(1) Weighing 0.4000g of soil sample to be detected in a corundum crucible, and adding 2.0g of Na 2 O 2 After being stirred uniformly, the corundum crucible is placed on a fire-resistant plate which is heated to 450-550 ℃, baked for about 5 minutes until sodium peroxide is in a scorch shape, and then moved into the corundum crucible which is heated to 450-Heating to 750 ℃ in a muffle furnace at 500 ℃, preserving heat, melting for 6-10min, taking out the crucible, cooling, putting the crucible into a beaker, adding 80-100mL of hot water, adding 5mL of internal standard solution, stirring uniformly by using a plastic rod, and taking out the crucible to obtain a sample to be detected;
(2) Stirring and dividing 4mL of sample to be measured into a polytetrafluoroethylene crucible, adding 2.5mL of tartaric acid solution, shaking uniformly, adding 2-3g of cationic resin, shaking uniformly, placing on an oscillator, oscillating for 15-20min, adding 8mL of water, shaking uniformly, and then placing on the oscillator, oscillating for 15-20min to obtain a measurement solution;
(3) Setting working parameters on an inductively coupled plasma mass spectrometer, pumping a measured liquid into an atomizer, introducing ammonia water and an ethanol solution into a tee joint by taking argon as a carrier gas, introducing an atomized gas into plasma flame to excite ionization, introducing hydrogen into the plasma flame in a KED mode, wherein the flow is 6.2mL/min, measuring mass spectrum counting of selenium and tellurium, measuring a working curve, substituting the obtained emission intensity meter value into the working curve, and calculating the content of selenium and tellurium in the liquid to be measured.
Further, the operating parameters of the inductively coupled plasma mass spectrometer are as follows: the power is 1500W, the plasma gas flow is 14L/min, the auxiliary gas flow is 0.8L/min, the atomizer flow rate is 1.1L/min, the sample injection flushing time is 16s, the scanning mode is peak jump, the residence time is 0.15s, the single element integration time is 6s, the total time of the single element is zero,
Figure BDA0002433653140000031
A sampling cone with the diameter of 1.1mm,
Figure BDA0002433653140000032
0.7mm of cut, and the detected isotope is 78 Se、 126 Te、 185 Re。
Further, the reaction gas of the collision cell is hydrogen, and the flow rate is 6.2mL/min.
Further, the concentration of the tartaric acid solution was 0.8%.
Furthermore, the concentration of the ammonia water is 0.8%, the concentration of the ethanol is 5%, and the ammonia water is pumped in by a peristaltic pump in a three-way mode.
Further, the internal standard solution is Re internal standard solution with the concentration of 0.5 mu g/mL.
Further, the drawing method of the working curve comprises the following steps: 2.0g Na was added to a series of Teflon beakers 2 O 2 Adding about 50mL of water, adding 5.00mL of internal standard solution, adding a series of selenium and tellurium standard solutions, adding water to about 90mL, stirring uniformly to obtain a sample to be detected, pretreating the sample according to the step (2), measuring mass spectrum counting of selenium and tellurium according to the step (3) on an inductively coupled plasma mass spectrometer, and drawing a working curve according to the mass spectrum counting.
Further, the cation exchange resin is 732 type cation exchange resin.
Compared with the prior art, the invention has the advantages and beneficial effects that:
1. the method can completely dissolve selenium and tellurium by adopting alkali fusion, not only removes a large amount of salt through resin adsorption, but also eliminates the interference of zinc, and then eliminates the interference of double-argon polyatomic ions through a KED mode (taking hydrogen as reaction gas and having the flow of 6.2 mL/min), thereby further leading the double-argon polyatomic ions to be capable of dissolving selenium and tellurium completely 78 The signal-to-back ratio of Se is improved by 5 to 10 times, and most metal ions are removed by resin adsorption, 126 the interference on Te is obviously reduced, wherein the detection limit of selenium is 0.005 mu g/g, the detection limit of tellurium is 0.002 mu g/g, and the detection limit is obviously reduced, so that the selenium and tellurium in soil and water system sediments can be simultaneously measured, and the result is accurate and the efficiency is high. The problems that the interference of multi-atom ions such as double argon or chlorine argon and zinc oxide on selenium and tellurium, the signal-to-back ratio is low and the detection limit cannot meet the detection requirement at present are solved.
2. The method adds ammonia water and ethanol in the determination process, has sensitization effect, can double the sensitivity, and meets the determination requirement of low-content selenium and tellurium in the current soil.
3. The method has the advantages of higher sensitivity, lower detection limit, higher anti-interference capability, higher accuracy and the like, and can be used for simultaneously measuring the selenium and tellurium with low content in soil.
Drawings
FIG. 1 is a standard working curve diagram of elemental selenium;
FIG. 2 is a standard operating curve of tellurium.
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 experimental methods used are conventional methods unless otherwise specified, and the materials, reagents and the like used in the following examples are commercially available, and only reagents and ultrapure water which are confirmed to be superior pure are used in the analysis.
Example 1
A method for determining Se and Te by alkali fusion inductively coupled plasma mass spectrometry comprises the following steps:
(1) Weighing 0.4000g of soil sample to be measured in a corundum crucible, and adding 2.0g of Na 2 O 2 After uniformly stirring, placing the corundum crucible on a fire-resistant plate heated to 500 ℃, baking for about 5 minutes until sodium peroxide is in a scorched state, transferring the corundum crucible into a muffle furnace heated to 500 ℃, heating to 750 ℃, preserving heat and melting for 8min, taking out the crucible, cooling, placing the crucible into a beaker, adding 80mL of hot water, adding 0.5 mu g/mL of 5.00mLRe internal standard solution, uniformly stirring by using a plastic rod, and taking out the crucible to obtain a sample to be detected;
(2) Stirring and taking 4mL of a sample to be detected while stirring into a 30mL polytetrafluoroethylene crucible, adding 2.5mL of tartaric acid solution (the concentration is 0.8%), shaking uniformly, adding 3g of 732 type cation exchange resin, shaking uniformly, placing on an oscillator for oscillation for 20min, adding 8mL of water, shaking uniformly, and then placing on the oscillator for oscillation for 15min to obtain a determination solution;
(3) On an inductively coupled plasma mass spectrometer, setting working parameters as follows: the power is 1500W, the plasma gas flow is 14L/min, the auxiliary gas flow is 0.8L/min, the atomizer flow rate is 1.1L/min, the sample injection pump flow rate is 30rpm, the sample injection flushing time is 16s, the scanning mode is peak jump, the residence time is 0.15s, the single element integration time is 6s, the total time of the single element is zero,
Figure BDA0002433653140000041
A sampling cone with the diameter of 1.1mm,
Figure BDA0002433653140000042
0.7mm of cut, and the detected isotope is 78 Se、 126 Te、 185 Re. The method comprises the steps of pumping a measured liquid into an atomizer, using argon as carrier gas, introducing 0.8% ammonia water and 5% ethanol solution into a tee joint, introducing atomized gas into plasma flame to excite ionization, measuring mass spectrum counting of selenium and tellurium in a KED mode (reaction gas is hydrogen gas, and the flow is 6.2 mL/min), measuring a working curve, substituting the obtained emission intensity meter value into the working curve, and calculating the content of selenium and tellurium in the measured liquid.
Drawing a working curve: 2.0g Na was added to a series of Teflon beakers 2 O 2 Adding about 50mL of water, adding 5.00mL of internal standard solution, adding a series of selenium and tellurium standard solutions, adding water to about 90mL, stirring to obtain a sample to be detected, pretreating the sample according to the step (2), measuring mass spectrum counting of selenium and tellurium according to the step (3) on an inductively coupled plasma mass spectrometer as shown in tables 1 and 2, and drawing a working curve according to the mass spectrum counting as shown in FIGS. 1 and 2.
Table 1: configuration of selenium element working curve
Concentration (ug/L) Emission intensity count value
0.00 13
0.10 74
0.50 336
1.00 649
5.00 3276
10.0 6487
20.0 13092
Table 2: configuration of tellurium element working curve
Concentration (ug/L) Emission intensity count value
0.00 2
0.05 97
0.25 456
0.50 951
2.50 4525
5.00 8927
10.0 17662
In order to verify the accuracy of the method, a plurality of standard samples with known selenium and tellurium contents are taken, a determination solution is prepared by the same method as the steps (1) and (2), then inductively coupled plasma mass spectrometry is added, mass spectrometry counting of selenium and tellurium is measured in a KED mode (reaction gas is hydrogen, and the flow is 6.2 mL/min), the determination results are substituted into the standard curves of all elements, then the contents of selenium and tellurium are respectively calculated, and the determination results are shown in the following table 3.
Table 3: standard value and measured value of selenium and tellurium national standard substance
Figure BDA0002433653140000061
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 4.
Table 4: limit of selenium and tellurium detection
Figure BDA0002433653140000062
Figure BDA0002433653140000071
From the results, the detection limit of selenium and tellurium in the invention is 0.005 mug/g and 0.002 mug/g, and the sensitivity 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 is not intended to limit the practice of the invention to those descriptions. 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 (1)

1. A method for measuring Se and Te by alkali fusion inductively coupled plasma mass spectrometry is characterized by comprising the following steps:
(1) Weighing 0.4000g of soil sample to be detected in a corundum crucible, and adding 2.0g of Na 2 O 2 After uniformly stirring, placing the corundum crucible on a fire-resistant plate heated to 450-550 ℃, baking for about 5 minutes until sodium peroxide is in a scorched state, transferring the corundum crucible into a muffle furnace heated to 450-500 ℃, heating to 750 ℃, preserving heat, melting for 6-10min, taking out the crucible, cooling, placing the crucible into a polytetrafluoroethylene beaker, adding 80-100mL of hot water, adding 5.00mL internal standard solution, uniformly stirring by using a plastic rod, and taking out the crucible to obtain a sample to be measured;
(2) Stirring and dividing 4mL of sample to be measured into a polytetrafluoroethylene crucible, adding 2.5mL of tartaric acid solution, shaking uniformly, adding 2-3g of cation exchange resin, shaking uniformly, placing on an oscillator, oscillating for 15-20min, adding 8mL of water, shaking uniformly, and then placing on the oscillator, oscillating for 15-20min to obtain a measurement solution;
(3) Setting working parameters on an inductively coupled plasma mass spectrometer, pumping a measured liquid into an atomizer, introducing ammonia water and an ethanol solution into a tee joint by taking argon as a carrier gas, introducing an atomizing gas into plasma flame to excite ionization, and measuring mass spectrum counting of selenium and tellurium by using a KED mode, wherein hydrogen is introduced into the KED mode as a reaction gas, and the flow rate is 6.2 mL/min; meanwhile, measuring a working curve, substituting the obtained numerical value of the emission intensity meter into the working curve, and calculating the contents of selenium and tellurium in the liquid to be measured;
the working parameters of the inductively coupled plasma mass spectrometer are as follows: the power is 1500W, the plasma gas flow is 14L/min, the auxiliary gas flow is 0.8L/min, the atomizer flow rate is 1.1L/min, the sample introduction and washing time is 16s, the scanning mode is peak jump, the residence time is 0.15s, the single element integration time is 6s, the brada sampling cone is 1.1mm, 0.7mm is cut off from the brada, and the detection isotopes are 78Se, 126Te and 185Re;
the concentration of the tartaric acid solution is 0.8%;
the concentration of the ammonia water is 0.8%, the concentration of the ethanol solution is 5%, and the ammonia water and the ethanol solution are pumped in by a peristaltic pump in a three-way mode;
the internal standard solution is Re internal standard solution with the concentration of 0.5 mug/mL;
the drawing method of the working curve comprises the following steps: 2.0g Na was added to a series of Teflon beakers 2 O 2 About 50mL water was added,
adding 5.00mL internal standard solution, adding a series of selenium and tellurium standard solutions, adding water to about 90mL, and stirring to obtain the solution to be measured
Pretreating the sample according to the step (2), measuring the mass spectrum counting of selenium and tellurium on an inductively coupled plasma mass spectrometer according to the step (3), and drawing a working curve according to the mass spectrum counting;
the cation exchange resin is 732 type cation exchange resin.
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