CN117169046A - Single column purification and isotope determination method for Sr-Nd-Sm with sample quantity less than 3mg - Google Patents
Single column purification and isotope determination method for Sr-Nd-Sm with sample quantity less than 3mg Download PDFInfo
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Abstract
Embodiments of the present disclosure provide a single column purification and isotope determination method for Sr-Nd-Sm in a sample amount of less than 3mg, comprising: selecting a rock sample to be measured, weighing the rock sample, and dissolving the weighed rock sample to be measured to obtain a target dissolving solution; carrying out chemical separation and purification on the target solution by adopting a single resin column and acids with different concentrations and types, and separating out three elements of Sr, nd and Sm and matrix elements and interfering elements at one time to obtain samples to be measured of the Sr, nd and Sm elements; establishing a cup structure for measuring the isotopes of Sr, nd and Sm, and carrying out isotope thermal ionization mass spectrometry on a sample to be measured of Sr, nd and Sm according to the corresponding cup structure; and respectively processing the measured data to respectively obtain the isotope ratios of Sr, nd and Sm elements. The method can separate Sr, nd, sm elements and interfering elements at one time, saves the sample consumption, saves the cost and the time, and reduces the background of the chemical flow.
Description
Technical Field
The embodiment of the disclosure belongs to the technical field of Sr, nd and Sm isotope tracing and dating, and particularly relates to a single-column purification and isotope determination method for Sr-Nd-Sm with a sample size of less than 3 mg.
Background
87 Rb- 86 Sr、 147 Sm- 143 Nd and Nd 146 Sm- 142 Nd isotope systems are well known years and tracer tools used in the field of geochemistry and cosmic chemistry research. As a longevityThe system of the radioactive isotope is used for the purpose of preparing, 87 Rb- 86 sr and 147 Sm- 143 nd can be used in chronology research of the overall process of planetary formation and evolution. 87 Rb- 86 Sr and 147 Sm- 143 the Nd isotope system can be applied to the annual and tracing of geological processes such as rock causes, magma sources, shell-valance interactions and the like. In addition, in the case of the optical fiber, 146 sm as a extinct short-lived nuclide and decays to produce 142 Nd, half-life 103Ma (or 68Ma, half-life of which is currently still controversial). Thus, the first and second substrates are bonded together, 146 Sm- 142 the Nd system can be used as a high precision timer for geological events within the early 500Ma of solar system formation. At the same time 149 Sm can monitor the effect of cosmic radiation on the sample. Therefore, the single column Sr, nd and Sm are separated from the same sample, and the isotope composition data of the single column Sr, nd and Sm are obtained, so that the single column Sr, nd and Sm has very important significance for the research of precious samples.
Currently, two column separations and TIMS assays are employed for rock samples of 3mg to 5mg sample volumes. Concentrated HF and HNO are adopted 3 、HClO 4 Dissolving a stone sample, and then separating by two columns, wherein the first column uses rare earth special Resin (RE) to separate and purify Rare Earth Elements (REE), and the second column uses Sr special resin to separate Sr. The method adopts a two-column method to separate, increases the flow time and the flow background, and in addition, the method only separates Sr and Rare Earth Element (REE) containing Nd, namely Nd and Ce can not be separated, thus only measuring 143 Nd, not accurately measured 142 Nd also cannot be performed 146 Sm- 142 Nd system study.
In addition, nd, sm and rare earth elements were separated and TIMS measured on rock samples of 3mg to 5mg sample volumes using LN resin single column. The method can not separate Sr, nd and Sm at the same time, can not separate Ce and Nd well, and has low Nd recovery rate of only 40%.
In addition, for rock samples, concentrate HF, HCl, HBF is used 4 Dissolving the sample, automatically separating Sr, nd and Pb three elements by using DGA resin single column, and then measuring isotope group by using a multi-receiving inductance coupling plasma mass spectrometer (MC-ICPMS)And (3) forming the finished product. The method can not separate Sm, and the background of the whole process is high, and the background of Sr, nd and Pb is respectively 350pg, 2280pg and 150pg.
In summary, there has been no chemical separation method so far that can separate three elements Sr, nd, and Sm at one time for a sample single column of less than 3mg sample amount, and well separate interfering elements, nor is there a high-precision Sm isotope TIMS measurement method for a small sample amount.
Disclosure of Invention
Embodiments of the present disclosure aim to solve at least one of the technical problems existing in the prior art, and provide a single column purification and isotope determination method for Sr-Nd-Sm with a sample size of less than 3 mg.
Embodiments of the present disclosure provide a single column purification and isotope determination method for Sr-Nd-Sm in a sample amount of less than 3 milligrams, the method comprising:
selecting a rock sample to be measured, weighing the rock sample, dissolving the weighed rock sample to be measured to obtain an initial dissolving solution, evaporating the initial dissolving solution to dryness, re-dissolving the initial dissolving solution and storing the initial dissolving solution in a preset acid medium to obtain a target dissolving solution;
carrying out chemical separation and purification on the target solution by adopting a single resin column and different concentrations and different types of acids, and separating out three elements of Sr, nd and Sm and matrix elements and interference elements thereof at one time to respectively obtain samples to be measured of the Sr, nd and Sm elements;
respectively establishing cup structures for performing Sr, nd and Sm isotope measurement, and respectively performing isotope thermal ionization mass spectrometry on samples to be measured of Sr, nd and Sm elements according to the corresponding cup structures;
and respectively processing the measured Sr isotope data, nd isotope data and Sm isotope data to respectively obtain the isotope ratios of Sr, nd and Sm elements.
Optionally, the target solution is chemically separated and purified by using a single TODGA resin column and acids with different concentrations and types, three elements of Sr, nd and Sm, and matrix elements and interfering elements thereof are separated at one time, including:
adopting a TODGA resin column, and preprocessing the TODGA resin column;
slowly adding 0.1-0.3 mL of the target solution into the TODGA resin column after pretreatment;
slowly adding 0.8-1.0 mL of 3mol/L nitric acid into the TODGA resin column to separate and purify a first matrix element;
slowly adding 1.1-1.3 mL of 4mol/L nitric acid into the TODGA resin column to separate and purify Sr element;
slowly adding 0.8-1 mL of 4mol/L nitric acid into the TODGA resin column, and slowly adding 1.1-1.3 mL of 0.1mol/L nitric acid to separate and purify a second matrix element Ca;
slowly adding 3 mL-5 mL of 2.5mol/L hydrochloric acid into the TODGA resin column to separate and purify interfering elements La, ce and Pr;
slowly adding 1.1-1.3 mL of 1.2mol/L hydrochloric acid into the TODGA resin column to separate and purify Nd element;
slowly adding 2.4-2.6 mL of 1.2mol/L hydrochloric acid into the TODGA resin column to separate and purify Sm element;
slowly adding 0.4-0.6 mL of 1.2mol/L hydrochloric acid into the TODGA resin column to separate and purify heavy rare earth elements.
Optionally, the sample to be measured for obtaining Sr, nd and Sm elements respectively includes:
and (3) steaming the separated and purified solutions respectively containing the Sr, nd and Sm elements until the solutions are wet and dry, so as to obtain samples to be measured of the Sr, nd and Sm elements respectively.
Optionally, the pretreating the TODGA resin column includes:
slowly adding 2-4 mL of 0.05mol/L hydrochloric acid into the TODGA resin column, and cleaning the TODGA resin column;
slowly adding 2-4 mL of ultrapure water into the TODGA resin column to enable the TODGA resin column to be in a neutral state;
slowly adding 2-4 mL of 3mol/L nitric acid which is consistent with the preset acid medium in the target solution into the TODGA resin column, so that the TODGA resin column is in an equilibrium state.
Optionally, the respectively establishing cup structures for performing the isotope measurement of Sr, nd and Sm, and respectively performing isotope thermal ionization mass spectrometry on the sample to be measured of Sr, nd and Sm according to the corresponding cup structures, including:
according to the natural abundance of Sr, nd and Sm, a Faraday cup and amplifiers of different types are adopted for combination, and cup structures for measuring the isotopes of Sr, nd and Sm are respectively established;
and respectively carrying out isotope thermal ionization mass spectrometry on the sample to be tested of the Sr, nd and Sm elements according to the established cup structure for the isotope measurement of the Sr, nd and Sm.
Optionally, the established cup structure for Sr isotope measurement includes:
84 sr and 85 sr is respectively connected with 10 by adopting a third low cup L3 and a second low cup L2 13 An omega amplifier receives;
86 Sr、 87 sr and 88 sr is respectively connected with 10 by adopting a first low cup L1, a central cup C and a first high cup H1 12 An omega amplifier receives;
according to the established cup structure for the Sr isotope measurement, respectively performing isotope thermal ionization mass spectrometry on the sample to be measured of the Sr element to obtain the isotope ratio of the Sr element, wherein the method comprises the following steps:
carrying out spot-strip treatment on the sample to be measured of the Sr element on a W strip to finish spot application;
the evaporation belt is electrified to rise to 3500 mA-4500 mA at the speed of 50 mA/min-150 mA/min, the temperature is 1300 ℃ to 1400 ℃, 88 Sr + and when the signal intensity reaches 1.5V-3V, single W-band measurement of the Sr isotope thermal ionization mass spectrum is carried out.
Optionally, the cup structure of the established Nd isotope assay includes:
140 Ce、 145 Nd、 147 Sm、 148 nd is respectively connected with 10 by adopting a third low cup L3, a first high cup H1, a third high cup H3 and a fourth high cup H4 13 An omega amplifier receives;
142 Nd、 143 Nd、 144 Nd、 146 nd is respectively connected with 10 by adopting a second low cup L2, a first low cup L1, a central cup C and a second high cup H2 12 An omega amplifier receives;
according to the established cup structure for Nd isotope determination, respectively performing isotope thermal ionization mass spectrometry on the sample to be determined of the Nd element to obtain the isotope ratio of the Nd element, wherein the method comprises the following steps:
carrying out spot-strip treatment on the sample to be measured of the Nd element on a Re strip to finish spot application;
the ionization current is increased to 2500 mA-3500 mA at the speed of 200 mA/min-300 mA/min, and the evaporation band is increased to 1200 mA-2000 mA at the speed of 100 mA/min-150 mA/min, 142 Nd + and (3) performing Nd isotope thermal ionization mass spectrometry dual Re band measurement when the signal intensity reaches 0.1V-0.3V.
Optionally, the established cup structure for Sm isotope determination comprises:
146 Nd、 148 Sm、 150 Sm、 155 gd is respectively connected with 10 by a third low cup L3, a first low cup L1, a first high cup H1 and a fourth high cup H4 13 An omega amplifier receives;
147 Sm、 149 Sm、 152 Sm、 154 sm is respectively connected with 10 by adopting a second low cup L2, a central cup C, a second high cup H2 and a third high cup H3 12 An omega amplifier receives;
according to the established cup structure for the Sm isotope measurement, respectively performing isotope thermal ionization mass spectrometry on the sample to be measured of the Sm element to obtain the isotope ratio of the Sm element, wherein the method comprises the following steps:
carrying out spot-strip treatment on the sample to be measured of the Sm element on a Ta strip to finish spot application;
the current of the evaporation belt is increased to 3000 mA-3400 mA at the speed of 50 mA/min-150 mA/min, the temperature is 1300 ℃ to 1400 ℃, 152 Sm + when the signal intensity reaches 0.1V-0.4V, sm isotope thermal ionization mass spectrometry single Ta band measurement is carried out.
Optionally, the processing the measured Sr isotope data, nd isotope data, and Sm isotope data to obtain isotope ratios of Sr, nd, and Sm elements, respectively, includes:
processing the Sr isotope data, comprising:
rb homoisobaric subtraction was determined by 85 Rb and Rb 87 Rb/ 85 Rb= 0.3860 for calculation;
instrument quality fractionation correction uses a logarithmic law sum 88 Sr/ 86 Sr= 8.375209;
processing the Nd isotope data, including:
sm and Ce homoisobars were determined by subtraction 147 Sm、 140 Ce and 147 Sm/ 144 Sm＝4.8827、 147 Sm/ 148 sm= 1.3336 140 Ce/ 142 Ce= 7.9584 for calculation;
instrument quality fractionation correction uses a logarithmic law sum 146 Nd/ 144 Nd= 0.7219;
processing the Sm isotope data, comprising:
homoisobaric subtraction of Nd and Gd was determined by 146 Nd、 155 Gd (Gd) 148 Nd/ 146 Nd＝0.3314、 150 Nd/ 146 Nd＝0.3255、 152 Gd/ 155 Gd=0.0135 and 154 Gd/ 155 gd= 0.1473;
instrument quality fractionation correction uses a logarithmic law sum 147 Sm/ 152 Sm= 0.56081.
Optionally, selecting and weighing the rock sample to be measured, dissolving the weighed rock sample to be measured to obtain an initial solution, evaporating the initial solution to dryness, redissolving the initial solution and storing the initial solution in a preset acid medium to obtain a target solution, wherein the method comprises the following steps:
selecting a plurality of rock samples with different lithology, wherein the lithology and the concentration of Sr, nd and Sm elements of each sample are different;
weighing 1mg to 3mg of each rock powder sample and placing the rock powder samples into a 5ml to 10ml Teflon bottle;
adding 0.1 ml-0.3 ml of concentrated HF and 0.05 ml-0.15 m of concentrated HNO into the Teflon bottle respectively 3 Sealing the Teflon bottle, placing the Teflon bottle on an electric heating plate, and preserving the temperature of 120-150 ℃ for 3-5 days to obtain an initial solution;
evaporating the initial solution to dryness at 100-140 ℃, adding 0.1-0.3 ml of 5 mol/L-7 mol/L HCl again for redissolution, evaporating the redissolved solution to dryness at 100-140 ℃, and adding 0.1-0.3 ml of 3mol/L HNO 3 Preserving in a medium to obtain the target dissolving liquid.
The single-column purification and isotope determination method for Sr-Nd-Sm with the sample quantity less than 3mg realizes the one-time sample dissolution of the sample with the sample quantity less than 3mg, adopts a single resin column and different concentrations and different types of acids to chemically separate and purify the target solution, and separates three purification elements of Sr, nd and Sm and matrix elements and interference elements thereof at one time so as to ensure that more accurate isotope composition is obtained, the sample consumption is saved, the cost and time are saved, and the researcheable content of one sample is increased; simplifying the separation process, reducing the process blank and improving the recovery rate.
The Sr-Nd-Sm single column purification and isotope determination method with the sample quantity less than 3mg is characterized in that cup structures for carrying out Sr, nd and Sm isotope determination are respectively established, isotope thermal ionization mass spectrometry is respectively carried out on samples to be determined of Sr, nd and Sm elements according to the corresponding cup structures, a high-precision determination method is established for the Sr, nd and Sm isotopes of low-content samples, the best precision of the determination with the conventional method can be obtained when the sample dosage is only 1/5-1/10 of the conventional dosage, a means for in-depth research is provided for precious sample research, and the method is particularly suitable for determination of precious samples such as moon, mars, single-particle minerals and the like, and provides technical guarantee for the current moon and Mars detection plan in China.
Drawings
FIG. 1 is a schematic flow chart of a single column purification and isotope determination method for Sr-Nd-Sm with a sample size less than 3mg according to one embodiment of the present disclosure;
fig. 2 is a schematic diagram of a process for separating each element from a target solution in a single column at a time according to an embodiment of the disclosure.
Detailed Description
In order to enable those skilled in the art to better understand the technical solutions of the embodiments of the present disclosure, the embodiments of the present disclosure are described in further detail below with reference to the accompanying drawings and detailed description.
The disclosed embodiments provide a single column purification and isotope determination method S100 for Sr-Nd-Sm in a sample amount of less than 3mg, the method S100 comprising:
s110, selecting a rock sample to be measured, weighing the rock sample, dissolving the weighed rock sample to be measured to obtain an initial dissolving solution, evaporating the initial dissolving solution to dryness, re-dissolving the initial dissolving solution and storing the initial dissolving solution in a preset acid medium to obtain a target dissolving solution.
First, a plurality of rock samples of different lithology are selected, wherein each sample has a different lithology and concentration of elements Sr, nd and Sm.
Specifically, as shown in Table 1, in this example, five rock samples BIR-1a (basalt), BHVO-2 (basalt), BCR-2 (basalt) AGV-2 (andesite) and GSP-2 (granite amphibole) were selected for the experiment. As shown in table 1, the lithology and Sr, nd, and Sm element concentrations of the 5 samples were different, and were widely representative.
Secondly, weighing 1mg to 3mg of each rock powder sample and placing the rock powder samples into a 5ml to 7ml Teflon bottle. Specifically, in this example, 3mg each of the above five rock powder samples were weighed separately and placed in 7ml teflon bottles.
Again, 0.1ml to 0.3ml of concentrated HF and 0.05ml to 0.1ml of concentrated HNO are respectively added into the Teflon bottle 3 Sealing the Teflon bottle, placing the Teflon bottle on an electric heating plate, and preserving the temperature for 2-5 days at 120-150 ℃ to obtain an initial solution.
Specifically, in this example, 0.2ml of concentrated HF and 0.1ml of concentrated HNO were added to Teflon bottles, respectively 3 Sealing the Teflon bottle, placing the Teflon bottle on an electric heating plate, and preserving the temperature for 3 days at 140 ℃ to obtain an initial dissolving solution.
Then, evaporating the initial solution to dryness at 100-140 ℃, adding 0.1-0.3 ml of 5 mol/L-7 mol/L HCl again for redissolution, evaporating the redissolved solution to dryness at 100-140 ℃, adding 0.1-0.3 ml of 3mol/L HNO 3 Preserving in a medium to obtain the target dissolving liquid.
Specifically, in this example, the initial solution was evaporated to dryness at 120℃and re-dissolved by adding 0.2ml of 6mol/L HCl, and the re-dissolved solution was evaporated to dryness at 120℃and 0.2ml of 3mol/L HNO was added 3 Preserving in a medium to obtain the target dissolving liquid.
Table 1 rock sample information
S120, carrying out chemical separation and purification on the target solution by adopting a single resin column and different concentrations and different types of acids, and separating out three elements of Sr, nd and Sm and matrix elements and interference elements thereof at one time to respectively obtain samples to be measured of the Sr, nd and Sm elements.
A TODGA resin column was used and pretreated. Here, a Teflon resin column (3 cm long, 4mm inner diameter) was used, and 0.25ml of resin (TODGA, 50 μm to 100 μm) was packed to obtain a TODGA resin column.
TABLE 2 chemical separation and purification process of Sr, nd and Sm
As shown in table 2, pretreatment of the TODGA resin column included:
1) Slowly adding 2-4 mL of 0.04-0.06 mol/L hydrochloric acid into the TODGA resin column, and cleaning the TODGA resin column.
In this example, preferably, 3mL of 0.05mol/L hydrochloric acid was slowly added to the TODGA resin column, and the TODGA resin column was washed to complete the column washing.
2) Slowly adding 2-4 mL of ultrapure water into the TODGA resin column to make the TODGA resin column in a neutral state.
In this example, preferably, 3mL of ultrapure water is slowly added to the TODGA resin column to bring the TODGA resin column to a neutral state, and the column reduction is completed.
3) Slowly adding 2-4 mL 3mol/L nitric acid which is consistent with the preset acid medium in the target solution into the TODGA resin column, so that the TODGA resin column is in an equilibrium state.
In this example, it is preferable that the TODGA resin column is in an equilibrium state in accordance with the acid medium of the loaded target solution since the target solution is stored in the medium of 3mol/L nitric acid, 3mL of 3mol/L nitric acid in accordance with the preset acid medium in the target solution and the acid solution used in the first separation and purification step are slowly added to the TODGA resin column, and column equilibrium is completed.
After finishing the pretreatment of the TODGA resin column, adding target dissolution liquid into the TODGA resin column, and sequentially and respectively adding different concentrations and different types of acids to perform chemical separation and purification on the target dissolution liquid, wherein the specific chemical separation and purification are as follows:
1) Slowly adding 0.1-0.3 mL of target solution into the TODGA resin column after pretreatment. In this example, it is preferable that 0.2mL of the target solution is slowly added to the pretreated TODGA resin column (3 mL of 3mol/L nitric acid medium) to complete loading.
2) Slowly adding 0.8-1.0 mL of 3mol/L nitric acid into the TODGA resin column to separate and purify the first matrix element. In this example, preferably, 0.9mL of 3mol/L nitric acid is slowly added to the TODGA resin column to separate and purify the first matrix element, which includes the major elements and most of the trace elements, such as Na, mg, fe, and the like.
3) Slowly adding 1.1-1.3 mL of 4mol/L nitric acid into the TODGA resin column to separate and purify Sr element. In this example, preferably, 1.2mL of 4mol/L nitric acid is slowly added to the TODGA resin column to separate and purify Sr element.
4) Slowly adding 0.8-1 mL of 4mol/L nitric acid into the TODGA resin column, and slowly adding 1.1-1.3 mL of 0.1mol/L nitric acid to separate and purify the second matrix element Ca.
In this example, preferably, 0.9mL of 4mol/L nitric acid is slowly added to the TODGA resin column, followed by 1.2mL of 0.1mol/L nitric acid, to separate and purify the second base element Ca.
5) 3 mL-5 mL of 2.5mol/L hydrochloric acid is slowly added into the TODGA resin column to separate and purify the interfering elements La, ce and Pr. In this example, preferably, 4mL of 2.5mol/L hydrochloric acid was slowly added to the TODGA resin column to separate and purify the interfering elements La, ce and Pr.
6) Slowly adding 1.1-1.3 mL of 1.2mol/L hydrochloric acid into the TODGA resin column to separate and purify Nd element. In this example, preferably, 1.2mL of 1.2mol/L hydrochloric acid is slowly added to the TODGA resin column to separate and purify Nd element.
7) Slowly adding 2.4-2.6 mL of 1.2mol/L hydrochloric acid into the TODGA resin column to separate and purify Sm element. In this example, preferably, 2.5mL of 1.2mol/L hydrochloric acid was slowly added to the TODGA resin column to separate and purify Sm.
8) Slowly adding 0.4-0.6 mL 1.2mol/L hydrochloric acid into the TODGA resin column to separate and purify Heavy Rare Earth Element (HREE). In this example, preferably, 0.5mL of 1.2mol/L hydrochloric acid was slowly added to the TODGA resin column to isolate the Heavy Rare Earth Element (HREE) after Sm purification.
As shown in fig. 1, three purified elements of Sr, nd and Sm, and matrix elements and interfering elements thereof can be purified and separated at one time through the above chemical separation and purification steps; the total process background of Sr, nd and Sm obtained by the process is respectively smaller than 80pg, 7pg and 3pg; the recovery rate is more than 91 percent.
After the target solution was chemically separated and purified, 2 mL-4 mL of 0.05mol/L diluted hydrochloric acid was slowly added to the TODGA resin column to clean the TODGA resin column. In this example, preferably, 3mL of 0.05mol/L dilute hydrochloric acid is slowly added to the TODGA resin column to wash the TODGA resin column, thereby completing the column washing.
In addition, the separated and purified solutions containing the elements Sr, nd and Sm, respectively, were distilled to wet dryness to obtain samples to be measured of the elements Sr, nd and Sm, respectively.
In the embodiment, a single TODGA resin column and different concentrations and different types of acids are adopted to carry out chemical separation and purification on the target solution, three purification elements of Sr, nd and Sm and matrix elements and interference elements thereof are separated at one time, so that more accurate isotope composition is ensured to be obtained, the sample consumption is saved, the cost and time are saved, and the content of a sample which can be researched is increased; simplifying the separation process, reducing the process blank and improving the recovery rate. The method is also suitable for samples with conventional sample sizes, and only needs to replace a large resin column and increase the corresponding resin dosage.
S130, respectively establishing cup structures for performing Sr, nd and Sm isotope measurement, and respectively performing isotope thermal ionization mass spectrometry on samples to be measured of Sr, nd and Sm elements according to the corresponding cup structures.
Firstly, according to the natural abundance of Sr, nd and Sm, a Faraday cup receiver (FC) and different types of amplifiers are adopted for combination, so that the problem of great difference of the abundance between isotopes is solved, and cup structures for measuring the Sr, nd and Sm isotopes are respectively established.
And secondly, respectively carrying out isotope thermal ionization mass spectrometry on samples to be tested of Sr, nd and Sm elements according to the established cup structure for the isotope measurement of Sr, nd and Sm. The cup structure established for the three elements Sr, nd and Sm isotopes is given in table 3.
TABLE 3 Faraday cup structure for Sr, nd, and Sm isotopes
As shown in table 3, the cup structure of the Sr isotope assay is established, specifically comprising:
84 sr and 85 sr is respectively connected with 10 by adopting a third low cup L3 and a second low cup L2 13 The omega amplifier receives.
86 Sr、 87 Sr and 88 sr is respectively connected with 10 by adopting a first low cup L1, a central cup C and a first high cup H1 12 The omega amplifier receives.
According to the established cup structure for Sr isotope measurement, respectively performing isotope Thermal Ionization Mass Spectrometry (TIMS) measurement on a sample to be measured of Sr element to obtain the isotope ratio of Sr element, which comprises the following steps:
firstly, carrying out spot-strip treatment on a sample to be measured of Sr element on a W strip to finish spot application.
Specifically, the spotting sequence is as follows: 1 μl TaF 5 Evaporating the exciting agent on the W band at 0.5A; the Sr evaporated after purification is redissolved in 1. Mu.l of 1mol/L HNO 3 Then spot on W belt, 0.5A evaporate to dryness; 1 μl TaF 5 The exciting agent is sprayed on the W belt, and 0.5A is evaporated to dryness; slowly increasing the current to 3A 5s, rapidly reducing to 0, and finishing spotting.
After the sample is placed in a sample chamber of an instrument, the evaporation belt is electrified to 3500 mA-4500 mA at the speed of 100 mA/min-150 mA/min, the temperature is 1300 ℃ to 1400 ℃, 88 Sr + and when the signal intensity reaches 1.5V-3V, single W-band measurement of the Sr isotope thermal ionization mass spectrum is carried out.
Specifically, the evaporation belt is electrified to 3500 mA-4500 mA at a speed of 100mA/min, and the temperature is about 1300 ℃ to 1400 ℃; 88 Sr + the measurement was performed when the signal intensity reached 1.5V to 3V. Measurement parameters: data were collected 200 per time (20 cycles x 10 blocks); integration time (Integration time) 4s, and Idle time (Idle time) 12s.
As shown in table 3, the cup structure of Nd isotope measurement was established, specifically including:
140 Ce、 145 Nd、 147 Sm、 148 nd is respectively connected with 10 by adopting a third low cup L3, a first high cup H1, a third high cup H3 and a fourth high cup H4 13 The omega amplifier receives.
142 Nd、 143 Nd、 144 Nd、 146 Nd is respectively connected with 10 by adopting a second low cup L2, a first low cup L1, a central cup C and a second high cup H2 12 The omega amplifier receives.
According to the established cup structure for Nd isotope measurement, respectively performing isotope Thermal Ionization Mass Spectrometry (TIMS) measurement on samples to be measured of Nd elements to obtain isotope ratios of the Nd elements, wherein the method specifically comprises the following steps:
firstly, carrying out spot-strip treatment on a sample to be measured of Nd element on a Re strip to finish spot application.
Specifically, the spotting sequence is as follows: nd evaporated after purification was redissolved in 1. Mu.l of 1mol/L HNO 3 Then point onto the Re band. The current was slowly increased to 2A for 1 minute to complete spotting.
After the sample is placed in a sample chamber of an instrument, the ionization current is increased to 2500 mA-3500 mA at the speed of 200 mA/min-300 mA/min, and the evaporation band is changed to 1200 mA-2000 mA at the speed of 100 mA/min-150 mA/min, 142 Nd + and (3) performing Nd isotope thermal ionization mass spectrometry dual Re band measurement when the signal intensity reaches 0.1V-0.3V.
Specifically, the ionization zone current is raised to 3000mA at a speed of 200mA/min, and the evaporation zone is raised to 1200 mA-2000 mA at a speed of 100 mA/min; 142 Nd + the measurement is performed when the signal intensity reaches 0.1V to 0.3V. Data were collected 200 per time (20 cycles x 10 blocks); integration time (Integration time) 8s, and Idle time (Idle time) 12s.
As shown in table 3, the cup structure of the established Sm isotope assay specifically includes:
146 Nd、 148 Sm、 150 Sm、 155 gd is respectively connected with 10 by a third low cup L3, a first low cup L1, a first high cup H1 and a fourth high cup H4 13 The omega amplifier receives.
147 Sm、 149 Sm、 152 Sm、 154 Sm is respectively connected with 10 by adopting a second low cup L2, a central cup C, a second high cup H2 and a third high cup H3 12 The omega amplifier receives.
According to the established cup structure for Sm isotope measurement, respectively performing isotope Thermal Ionization Mass Spectrometry (TIMS) measurement on a sample to be measured of Sm element to obtain the isotope ratio of the Sm element, wherein the method specifically comprises the following steps:
first, a sample to be measured of the Sm element is subjected to spot-plating treatment on a Ta belt, and spot printing is completed.
Specifically, the spotting sequence is as follows: as with the Sr deposition method, a sandwich method was used. Sm evaporated to dryness after purification was redissolved in 1. Mu.l 1mol/L HNO 3 In 1. Mu.l TaF 5 Exciting agent, 1 μl sample, 1 μl TaF 5 Sequentially spotting the exciting agent onto the Ta belt, and heating the liquid drops to dry by using 0.5A current after each step of spotting; finally, the filament current was slowly increased to 1.8A, and the sample application was completed after waiting for 1 minute.
After the sample is put into a sample chamber of an instrument, the current of the evaporation belt is increased to 3000 mA-3400 mA at the speed of 100 mA/min-200 mA/min, the temperature is 1300 ℃ to 1400 ℃, 152 Sm + when the signal intensity reaches 0.1V-0.4V, sm isotope thermal ionization mass spectrometry single Ta band measurement is carried out.
In this embodiment, a Faraday cup receiver (FC) and a different type of amplifier (10 12 Omega and 10 13 Ω), respectively establishing cup structures for measuring the isotopes of Sr, nd and Sm, respectively performing isotope thermal ionization mass spectrometry on samples to be measured of Sr, nd and Sm elements according to the corresponding cup structures, and establishing a high-precision measurement method for the isotopes of Sr, nd and Sm of low-content samples, in particular establishing a high-precision Sm isotope TIMS measurement method for small sample volumes (less than 3 mg); when the sample dosage is only 1/5-1/10 of the conventional dosage, the optimal precision of the measurement with the conventional method can be obtained, a means for deep research is provided for the research of precious samples, the method is particularly suitable for the measurement of precious samples such as moon, mars and single-particle minerals, and technical support is provided for the current moon and Mars detection plan in China.
And S140, respectively processing the measured Sr isotope data, nd isotope data and Sm isotope data to respectively obtain the isotope ratios of Sr, nd and Sm elements.
And (3) performing off-line correction on the measured Sr isotope data, nd isotope data and Sm isotope data, wherein the off-line correction comprises interference subtraction and mass fractionation correction, and the specific process is as follows:
the specific process for processing the Sr isotope data comprises the following steps:
rb homoisobaric subtraction was determined by 85 Rb and Rb 87 Rb/ 85 Rb= 0.3860. Instrument quality fractionation correction uses a logarithmic law sum 88 Sr/ 86 Sr= 8.375209.
The specific process for processing Nd isotope data comprises the following steps:
sm and Ce homoisobars were determined by subtraction 147 Sm、 140 Ce and 147 Sm/ 144 Sm＝4.8827、 147 Sm/ 148 sm= 1.3336 140 Ce/ 142 Ce= 7.9584. Instrument quality fractionation correction uses a logarithmic law sum 146 Nd/ 144 Nd= 0.7219;
the specific process for processing Sm isotope data comprises the following steps:
homoisobaric subtraction of Nd and Gd was determined by 146 Nd、 155 Gd (Gd) 148 Nd/ 146 Nd＝0.3314、 150 Nd/ 146 Nd＝0.3255、 152 Gd/ 155 Gd=0.0135 and 154 Gd/ 155 gd= 0.1473. Instrument quality fractionation correction uses a logarithmic law sum 147 Sm/ 152 Sm= 0.56081.
It is to be understood that the above implementations are merely exemplary implementations employed to illustrate the principles of the disclosed embodiments, which are not limited thereto. Various modifications and improvements may be made by those skilled in the art without departing from the spirit and substance of the embodiments of the disclosure, and these modifications and improvements are also considered to be within the scope of the embodiments of the disclosure.
Claims (10)
1. A single column purification and isotope determination method for Sr-Nd-Sm in a sample amount less than 3mg, the method comprising:
selecting a rock sample to be measured, weighing the rock sample, dissolving the weighed rock sample to be measured to obtain an initial dissolving solution, evaporating the initial dissolving solution to dryness, re-dissolving the initial dissolving solution and storing the initial dissolving solution in a preset acid medium to obtain a target dissolving solution;
carrying out chemical separation and purification on the target solution by adopting a single resin column and different concentrations and different types of acids, and separating out three elements of Sr, nd and Sm and matrix elements and interference elements thereof at one time to respectively obtain samples to be measured of the Sr, nd and Sm elements;
respectively establishing cup structures for performing Sr, nd and Sm isotope measurement, and respectively performing isotope thermal ionization mass spectrometry on samples to be measured of Sr, nd and Sm elements according to the corresponding cup structures;
and respectively processing the measured Sr isotope data, nd isotope data and Sm isotope data to respectively obtain the isotope ratios of Sr, nd and Sm elements.
2. The method according to claim 1, wherein the target solution is chemically separated and purified by using a single TODGA resin column and acids of different concentrations and types, three elements Sr, nd and Sm, and their matrix elements and interfering elements are separated at one time, comprising:
adopting a TODGA resin column, and preprocessing the TODGA resin column;
slowly adding 0.1-0.3 mL of the target solution into the TODGA resin column after pretreatment;
slowly adding 0.8-1.0 mL of 3mol/L nitric acid into the TODGA resin column to separate and purify a first matrix element;
slowly adding 1.1-1.3 mL of 4mol/L nitric acid into the TODGA resin column to separate and purify Sr element;
slowly adding 0.8-1 mL of 4mol/L nitric acid into the TODGA resin column, and slowly adding 1.1-1.3 mL of 0.1mol/L nitric acid to separate and purify a second matrix element Ca;
slowly adding 3 mL-5 mL of 2.5mol/L hydrochloric acid into the TODGA resin column to separate and purify interfering elements La, ce and Pr;
slowly adding 1.1-1.3 mL of 1.2mol/L hydrochloric acid into the TODGA resin column to separate and purify Nd element;
slowly adding 2.4-2.6 mL of 1.2mol/L hydrochloric acid into the TODGA resin column to separate and purify Sm element;
slowly adding 0.4-0.6 mL of 1.2mol/L hydrochloric acid into the TODGA resin column to separate and purify heavy rare earth elements.
3. The method according to claim 2, wherein the obtaining the sample to be measured of Sr, nd and Sm elements, respectively, comprises:
and (3) steaming the separated and purified solutions respectively containing the Sr, nd and Sm elements until the solutions are wet and dry, so as to obtain samples to be measured of the Sr, nd and Sm elements respectively.
4. The method of claim 2, wherein the pre-treating the TODGA resin column comprises:
slowly adding 2-4 mL of 0.05mol/L hydrochloric acid into the TODGA resin column, and cleaning the TODGA resin column;
slowly adding 2-4 mL of ultrapure water into the TODGA resin column to enable the TODGA resin column to be in a neutral state;
slowly adding 2-4 mL of 3mol/L nitric acid which is consistent with the preset acid medium in the target solution into the TODGA resin column, so that the TODGA resin column is in an equilibrium state.
5. The method according to any one of claims 1 to 4, wherein the establishing of the respective cup structures for performing the isotope determination of Sr, nd and Sm, and the performing the isotope thermal ionization mass spectrometry of the respective samples to be determined of Sr, nd and Sm elements according to the respective cup structures, comprises:
according to the natural abundance of Sr, nd and Sm, a Faraday cup and amplifiers of different types are adopted for combination, and cup structures for measuring the isotopes of Sr, nd and Sm are respectively established;
and respectively carrying out isotope thermal ionization mass spectrometry on the sample to be tested of the Sr, nd and Sm elements according to the established cup structure for the isotope measurement of the Sr, nd and Sm.
6. The method of claim 5, wherein the established cup structure for Sr isotope measurement comprises:
84 sr and 85 sr is respectively connected with 10 by adopting a third low cup L3 and a second low cup L2 13 An omega amplifier receives;
86 Sr、 87 sr and 88 sr is respectively connected with 10 by adopting a first low cup L1, a central cup C and a first high cup H1 12 An omega amplifier receives;
according to the established cup structure for the Sr isotope measurement, respectively performing isotope thermal ionization mass spectrometry on the sample to be measured of the Sr element to obtain the isotope ratio of the Sr element, wherein the method comprises the following steps:
carrying out spot-strip treatment on the sample to be measured of the Sr element on a W strip to finish spot application;
the evaporation belt is electrified to rise to 3500 mA-4500 mA at the speed of 50 mA/min-150 mA/min, the temperature is 1300 ℃ to 1400 ℃, 88 Sr + and when the signal intensity reaches 1.5V-3V, single W-band measurement of the Sr isotope thermal ionization mass spectrum is carried out.
7. The method of claim 5, wherein the established cup structure for Nd isotope determination comprises:
140 Ce、 145 Nd、 147 Sm、 148 nd is respectively connected with 10 by adopting a third low cup L3, a first high cup H1, a third high cup H3 and a fourth high cup H4 13 An omega amplifier receives;
142 Nd、 143 Nd、 144 Nd、 146 nd is respectively connected with 10 by adopting a second low cup L2, a first low cup L1, a central cup C and a second high cup H2 12 An omega amplifier receives;
according to the established cup structure for Nd isotope determination, respectively performing isotope thermal ionization mass spectrometry on the sample to be determined of the Nd element to obtain the isotope ratio of the Nd element, wherein the method comprises the following steps:
carrying out spot-strip treatment on the sample to be measured of the Nd element on a Re strip to finish spot application;
the ionization current is increased to 2500 mA-3500 mA at the speed of 200 mA/min-300 mA/min, and the evaporation band is increased to 1200 mA-2000 mA at the speed of 100 mA/min-150 mA/min, 142 Nd + and (3) performing Nd isotope thermal ionization mass spectrometry dual Re band measurement when the signal intensity reaches 0.1V-0.3V.
8. The method of claim 5, wherein the established cup structure for the Sm isotope assay comprises:
146 Nd、 148 Sm、 150 Sm、 155 gd is respectively connected with 10 by a third low cup L3, a first low cup L1, a first high cup H1 and a fourth high cup H4 13 An omega amplifier receives;
147 Sm、 149 Sm、 152 Sm、 154 sm is respectively connected with 10 by adopting a second low cup L2, a central cup C, a second high cup H2 and a third high cup H3 12 An omega amplifier receives;
according to the established cup structure for the Sm isotope measurement, respectively performing isotope thermal ionization mass spectrometry on the sample to be measured of the Sm element to obtain the isotope ratio of the Sm element, wherein the method comprises the following steps:
carrying out spot-strip treatment on the sample to be measured of the Sm element on a Ta strip to finish spot application;
the current of the evaporation belt is increased to 3000 mA-3400 mA at the speed of 50 mA/min-150 mA/min, the temperature is 1300 ℃ to 1400 ℃, 152 Sm + when the signal intensity reaches 0.1V-0.4V, sm isotope thermal ionization mass spectrometry single Ta band measurement is carried out.
9. The method according to any one of claims 1 to 4, wherein the processing of the measured Sr isotope data, nd isotope data, and Sm isotope data, respectively, to obtain the isotope ratios of Sr, nd, and Sm elements, respectively, comprises:
processing the Sr isotope data, comprising:
rb homoisobaric subtraction was determined by 85 Rb and Rb 87 Rb/ 85 Rb= 0.3860 for calculation;
instrument quality fractionation correction uses a logarithmic law sum 88 Sr/ 86 Sr= 8.375209;
processing the Nd isotope data, including:
sm and Ce homoisobars were determined by subtraction 147 Sm、 140 Ce and 147 Sm/ 144 Sm＝4.8827、 147 Sm/ 148 sm= 1.3336 140 Ce/ 142 Ce= 7.9584 for calculation;
instrument quality fractionation correction uses a logarithmic law sum 146 Nd/ 144 Nd= 0.7219;
processing the Sm isotope data, comprising:
homoisobaric subtraction of Nd and Gd was determined by 146 Nd、 155 Gd (Gd) 148 Nd/ 146 Nd＝0.3314、 150 Nd/ 146 Nd＝0.3255、 152 Gd/ 155 Gd=0.0135 and 154 Gd/ 155 gd= 0.1473;
instrument quality fractionation correction uses a logarithmic law sum 147 Sm/ 152 Sm= 0.56081.
10. The method according to any one of claims 1 to 9, wherein the selecting and weighing the rock sample to be measured, dissolving the weighed rock sample to be measured to obtain an initial solution, evaporating the initial solution to dryness, redissolving the initial solution and storing the redissolved solution in a preset acid medium to obtain a target solution, and the method comprises the following steps:
selecting a plurality of rock samples with different lithology, wherein the lithology and the concentration of Sr, nd and Sm elements of each sample are different;
weighing 1mg to 3mg of each rock powder sample and placing the rock powder samples into a 5ml to 10ml Teflon bottle;
to the Teflon bottle, 0.1ml to 0.3ml of concentrated HF and 0.05m were added respectivelyConcentrated HNO of l-0.15 m 3 Sealing the Teflon bottle, placing the Teflon bottle on an electric heating plate, and preserving the temperature of 120-150 ℃ for 3-5 days to obtain an initial solution;
evaporating the initial solution to dryness at 100-140 ℃, adding 0.1-0.3 ml of 5 mol/L-7 mol/L HCl again for redissolution, evaporating the redissolved solution to dryness at 100-140 ℃, and adding 0.1-0.3 ml of 3mol/L HNO 3 Preserving in a medium to obtain the target dissolving liquid.
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