CN112557164B - Sr isotope pretreatment method for mixed rock - Google Patents
Sr isotope pretreatment method for mixed rock Download PDFInfo
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- CN112557164B CN112557164B CN202011371530.9A CN202011371530A CN112557164B CN 112557164 B CN112557164 B CN 112557164B CN 202011371530 A CN202011371530 A CN 202011371530A CN 112557164 B CN112557164 B CN 112557164B
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Abstract
The invention discloses a Sr isotope pretreatment method for a mixed rock, which comprises the following steps: s1, weighing 50mg of a mixed rock sample and putting the mixed rock sample into a digestion tank; s2, adding 3ml of concentrated nitric acid with the concentration of 1.5 mol/L; s3, taking out the digestion tank, cooling to room temperature, sucking supernatant and centrifuging; s4, adding 4ml of 1mol/L sodium hydroxide; s5, adding 3ml of 0.5mol/L sodium hydroxide; s6, adding 3ml of 0.5mol/L sodium hydroxide; s7, adding 3ml of 1.5mol/L sodium hydroxide; s8, cooling to room temperature, adding 3ml of hydrochloric acid with the concentration of 1mol/L, taking supernate and centrifuging; s9, taking the supernatant, putting the supernatant into a digestion tank, and adding 1ml of hydrochloric acid with the concentration of 0.5 mol/L. The invention effectively avoids the harm generated in the treatment process and improves the safety factor in the pretreatment process; and the test of two components of carbonate and silicate in the mixed rock is realized.
Description
Technical Field
The invention relates to a Sr isotope pretreatment method for a mixed rock.
Background
Mixed rock accumulation: the mixed rock refers to a rock formed by mixing two sediments including land-source detritus and sea-phase carbonate (excluding cement), and consists of components (detritus, clay and biochemical components) with various causes. Generally, rocks with compositions greater than 25% carbonate and greater than 10% land-source detritus are referred to as mixed rock.
Strontium (Sr): strontium (Sr) is an alkaline earth metal with yellow luster in silver white color, is the element with the least abundance in alkaline earth metals (except beryllium), and exists in a compound state in nature. The strontium element on earth is mainly (80%) from the weathering of carbonate and sulfate.
Isotope (Isotope): the different species of the same element with the same number of protons and different numbers of neutrons are isotopes of each other (Isotope).
Strontium Isotope (Strontium Isotope): namely to 84 Sr、 86 Sr、 87 Sr、 88 Strontium in the form of four isotopes of Sr. Strontium in nature 84 Sr， 86 Sr， 87 Sr， 88 Sr exists in four isotope forms, and has relative abundanceRespectively 0.56%,9.86%,7.02%,82.56%, wherein 87 Sr is composed of 87 Rb decay to produce, evolution over time 87 Sr increases unidirectionally. When studying the composition of strontium isotopes 86 Sr as a basis for comparison, determining 86 Sr/ 88 The Sr ratio. In geology according to 87 Rb/ 86 Determination of age of geologic body based on decay relationship between Sr and based on initial formation of geologic body by extrapolation of isochrones or determination of strontium-containing minerals 87 Sr/ 86 Sr marks its source of matter.
87 Sr/ 86 Sr ratios are widely used in geochemical tracing and petrological research, especially in carbonate rocks. To obtain accuracy 87 Sr/ 86 Sr, the traditional method needs to digest a rock sample by two acid liquids of nitric acid and hydrochloric acid under a certain concentration gradient, and then adopts a resin ion exchange (cation exchange column AG 50W-X8/12) mode to achieve enrichment of Sr isotopes.
The strontium isotope composition of the carbonate rock sample is an important means for researching the deposition environment and diagenesis of the carbonate rock. It is believed that the isotopic composition of strontium (I) ((II)) 87 Sr/ 86 Sr ratio) is not altered by the concomitant isotopic fractionation in physical, chemical and biological processes, but is largely controlled by the strontium source. The strontium source comprises three types of land source, sea source and mantle source. Wherein, the land source mainly comprises silicate minerals such as feldspar and the like, fresh air and the like, the sea source mainly comprises sources such as synchronous (near-synchronous) seawater, synchronous or non-synchronous marine carbonate debris and the like, and the mantle source (deep part of the earth) mainly comprises sources such as magma invasion and other hydrothermal fluids and the like. The strontium isotope composition of the carbonate mineral of the reservoir with different geological background causes can be understood as the result of mixing the three strontium sources together, but it should be noted that in practical cases, the rock can be a single source or a mixture of multiple sources, if the whole rock is directly ground according to the current test scheme to test, the components of different sources can interfere with each other, and the mixed result is not beneficial for researchers to divide the source types of the rock structure according to the strontium isotope ratio of different carbonate mineral structures, and then the research personnel can further classify the source types of the rock structure according to the strontium isotope ratio of different carbonate mineral structuresAnd by utilizing the difference between the strontium isotope ratios, researching the material sources and the forming relative time of the carbonate minerals, inferring the change trend of the strontium isotope composition of the pore fluid in the diagenetic process, and evaluating the influence of the land source, the sea source and the mantle source materials on the diagenetic process.
The mixed rock is a rock containing multiple sources simultaneously. The research work of the mixed rock is quite difficult due to the multi-source texture components, and the large difference between the components (the land source texture is mainly siliceous components, and other sources such as sea sources are mainly calcium components) causes the large difference between the mixed test result of the whole rock sample and the single test result of each component, so that the invention of the strontium isotope test scheme for separating each component of the mixed rock and realizing the independent test of each component has important significance.
At present, the strontium isotope test is mainly based on rock, mineral rubidium strontium isotope geological age and strontium isotope ratio determination (DZ/T0184.4-1997), and the specific steps are shown in figure 1 and mainly comprise the following steps:
firstly, accurately weighing 0.1g of sample by using an electronic balance and putting the sample into a polytetrafluoroethylene digestion tank; the polytetrafluoroethylene digestion tank is soaked by a nitric acid solution before use and digested at 120 ℃.
And secondly, adding 2ml of concentrated nitric acid and 1ml of concentrated hydrofluoric acid into the polytetrafluoroethylene digestion tank, slightly shaking the digestion tank, covering the tank, putting the tank into a steel sleeve, screwing down the tank, and putting the tank into a high-temperature closed oven.
And thirdly, adjusting the temperature of the oven to 100 ℃, keeping the temperature of the oven for one hour when the temperature of the oven reaches 100 ℃, then adjusting the temperature of the oven to 180 ℃, and performing high-temperature closed digestion for more than 36 hours to ensure that the sample is completely digested.
And fourthly, taking out the digestion tank from the oven, cooling the outer steel sleeve to room temperature, taking out the digestion tank, then placing the digestion tank on a hot plate, taking down the digestion tank cover, adjusting the temperature of the hot plate to 120 ℃, evaporating the nitric acid and the hydrofluoric acid in the digestion tank to dryness, then adding 2ml of concentrated nitric acid, evaporating to dryness again, adding 1ml of concentrated nitric acid again, and finally evaporating to dryness.
And fifthly, after evaporation to dryness, adding 2ml of concentrated nitric acid and 5ml of ultrapure water, covering, filling into a cylinder sleeve, and redissolving.
Sixthly, the redissolution temperature must be kept at 140 ℃ for more than 4 hours, then the mixture is cooled and evaporated to dryness, and then the mixture is dissolved by hydrochloric acid solution with certain concentration, so that the collection is completed.
The prior art mainly has the following defects:
(1) The prior pretreatment technical scheme is suitable for high-purity limestone and dolomite, has low digestion efficiency on the rock sample of the mixed accumulated rock and is difficult to completely digest.
(2) The existing treatment scheme ignores the isotopic enrichment difference of each component Sr, directly mixes the whole rock sample and then carries out digestion, and cannot realize effective separation of each component, so that the components interfere with each other, and researchers are not facilitated to develop the research work of the mixed rock environment and the diagenesis process.
(3) Concentrated hydrofluoric acid (>40%) and continental clastic component (SiO) in the rock 2 ) Reacting to produce gaseous silicon tetrafluoride (SiF) 4 ) Easily decomposed in air to form silicic acid (H) 2 SiO 3 ) And Hydrogen Fluoride (HF), which is extremely toxic and has significant potential safety hazards.
(4) Gaseous silicon tetrafluoride (SiF) 4 ) Reacting with excessive hydrofluoric acid (HF) in a polytetrafluoroethylene digestion tank to generate fluosilicic acid (H) 2 SiF 6 ) Dissolving in a solution, etching the resin (AG 50) for subsequent cation exchange [5] The denaturation of the resin is disabled, and the enrichment of Sr isotope cannot be carried out.
(5) The existing scheme does not specify the specific concentrations of concentrated nitric acid, concentrated hydrofluoric acid and hydrochloric acid.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide an effective improvement on the basis of the traditional carbonate rock Sr isotope geochemical test analysis pretreatment scheme; the harm generated in the treatment process is effectively avoided, and the safety factor in the pretreatment process is improved; and the Sr isotope pretreatment method aiming at the mixed rock for testing two components of carbonate and silicate in the mixed rock is realized.
The purpose of the invention is realized by the following technical scheme: a Sr isotope pretreatment method for a mixed rock comprises the following steps: s1, weighing 50mg of a mixed rock sample by adopting an electronic balance, and putting the mixed rock sample into a polytetrafluoroethylene digestion tank;
s2, adding 3ml of concentrated nitric acid with the concentration of 1.5mol/L into the polytetrafluoroethylene digestion tank, shaking the digestion tank to fully mix the accretion rock sample with the concentrated nitric acid, then covering an upper cover of the polytetrafluoroethylene digestion tank, and placing the polytetrafluoroethylene digestion tank on a heating plate at 110 ℃ for continuous heat preservation for 24 hours;
s3, taking out the polytetrafluoroethylene digestion tank, cooling to room temperature, sucking the supernatant by using a liquid transfer gun, transferring to a centrifuge tube, and centrifuging at 3000r/m to finish the collection of carbonate rock components;
s4, adding 4ml of 1mol/L sodium hydroxide solution into the digestion tank after the supernatant is completely sucked, and then keeping the temperature of the digestion tank at 60 ℃ for 24 hours;
s5, adding 3ml of sodium hydroxide solution with the concentration of 0.5mol/L into the digestion tank, then preserving the temperature of the digestion tank at 60 ℃ for 24 hours, and evaporating to dryness after preserving the temperature;
s6, continuously adding 3ml of sodium hydroxide solution with the concentration of 0.5mol/L into the digestion tank, then preserving the temperature of the digestion tank at 60 ℃ for 24 hours, and evaporating to dryness after heat preservation;
s7, continuously adding 3ml of 1.5mol/L sodium hydroxide solution into the digestion tank, then preserving the temperature of the digestion tank at 120 ℃ for 48 hours, and evaporating to dryness after preserving the temperature;
s8, taking out the digestion tank, cooling to room temperature, adding 3ml of hydrochloric acid solution with the concentration of 1mol/L, sucking supernate by using a liquid transfer gun after the solution is fully reflected, transferring the supernate to a centrifugal tube, and selecting 1000r/m for centrifugation;
s9, placing the centrifuged supernatant in a polytetrafluoroethylene digestion tank, adding 1ml of hydrochloric acid solution with the concentration of 0.5mol/L, covering an upper cover of the digestion tank, then preserving the temperature of the digestion tank at 90 ℃ for 2 hours, and cooling to room temperature to complete the collection of silicate components.
Further, in the step S1, the polytetrafluoroethylene digestion tank is soaked in a nitric acid solution with the concentration of 5% -15% before use.
The beneficial effects of the invention are: the invention overcomes the defect that an effective and safe pretreatment scheme is lacked in the conventional pretreatment research of the Sr isotope of the mixed rock, and provides possibility for a thermal ionization multi-receiving mass spectrum test scheme of the Sr isotope of the mixed rock. The method is effectively improved on the basis of the traditional carbonate rock Sr isotope geochemical test analysis pretreatment scheme; the harm generated in the treatment process is effectively avoided, and the safety factor in the pretreatment process is improved; and the test of two components of carbonate and silicate in the mixed rock is realized, and the measurement accuracy can be improved.
Drawings
FIG. 1 is a flow chart of rock, mineral rubidium strontium isotope geological age and strontium isotope ratio determination standard test in the prior art;
FIG. 2 is a flow chart of the Sr isotope pretreatment method for the mixed rock according to the present invention;
FIG. 3 is a graph showing the intensity variation of Sr signal at different sample weights;
FIG. 4 is a graph showing the intensity variation of Sr signal at different temperatures;
FIG. 5 is a graph showing the change of the remaining silicate in sodium hydroxide solutions of different concentrations;
figure 6 is a graph of sodium silicate viscosity versus temperature.
Detailed Description
The technical scheme of the invention is further explained by combining the attached drawings.
As shown in fig. 2, the Sr isotope pretreatment method for the mixed rock of the present invention includes the following steps:
s1, weighing 50mg of a mixed rock sample by using an electronic balance, and putting the mixed rock sample into a polytetrafluoroethylene digestion tank; FIG. 3 is a graph showing the intensity variation of Sr signal at different sample weights;
s2, adding 3ml of concentrated nitric acid with the concentration of 1.5mol/L into a polytetrafluoroethylene digestion tank, shaking the digestion tank to fully mix the mixed rock sample and the concentrated nitric acid, then covering an upper cover of the polytetrafluoroethylene digestion tank, and placing the polytetrafluoroethylene digestion tank on a heating plate at 110 ℃ for continuous heat preservation for 24 hours;
s3, taking out the polytetrafluoroethylene digestion tank, cooling to room temperature, sucking the supernatant by using a liquid transfer gun, transferring to a centrifuge tube, selecting 3000r/m for centrifugation, digesting carbonate and clay components in an acid environment, and completing the collection of carbonate rock components through the steps S1-S3.
Silicate minerals generally do not react with acid (only react with hydrofluoric acid), but hydrofluoric acid is extremely toxic, and silicon tetrafluoride is easily lost as a substance which is easily converted into a gaseous state, so the method for treating the silicate component by adding sodium hydroxide specifically comprises the following steps:
s4, adding 4ml of 1mol/L sodium hydroxide solution into the digestion tank after the supernatant is completely sucked, and then keeping the temperature of the digestion tank at 60 ℃ for 24 hours;
s5, adding 3ml of sodium hydroxide solution with the concentration of 0.5mol/L into the digestion tank, then preserving the temperature of the digestion tank at 60 ℃ for 24 hours, and evaporating to dryness after preserving the temperature;
s6, continuously adding 3ml of sodium hydroxide solution with the concentration of 0.5mol/L into the digestion tank, then preserving the temperature of the digestion tank at 60 ℃ for 24 hours, and evaporating to dryness after preserving the temperature;
the silicate component is a series of silicon-oxygen tetrahedra combined with other cations, and the structure determines the chemical properties of the silicate to be very similar to those of silicon dioxide. The silicate can react with a certain amount of strong base at normal temperature, and only the generated sodium silicate is easily viscous to influence the collection of subsequent supernatant fluid, and the viscosity of the generated sodium silicate needs to be controlled by controlling reaction conditions. Therefore, in the method, the reaction progress is controlled by adding sodium hydroxide into the digestion tank by multiple times of small metering and controlling the reaction temperature, fig. 3 is a change curve of Sr signal intensity under different sample weights, fig. 4 is a change curve of Sr signal intensity under different temperatures, fig. 5 is a change curve of residual silicate in sodium hydroxide solutions with different concentrations, fig. 6 is a change curve of sodium silicate viscosity along with temperature, and by combining fig. 4, fig. 5 and fig. 6, the method adopts 0.5-1 mol/L sodium hydroxide solution, keeps the temperature at 60 ℃, and can achieve a better reaction effect. The effect of controlling the viscosity of the sodium silicate produced is achieved.
S7, continuously adding 3ml of 1.5mol/L sodium hydroxide solution into the digestion tank, then preserving the temperature of the digestion tank at 120 ℃ for 48 hours, and evaporating to dryness after preserving the temperature; adding excessive sodium hydroxide, and increasing the heat preservation temperature and time to ensure that the silicate and the sodium hydroxide fully react;
s8, taking out the digestion tank, cooling to room temperature, adding 3ml of hydrochloric acid solution with the concentration of 1mol/L, sucking supernate by using a liquid transfer gun after the solution is fully reflected, transferring the supernate to a centrifugal tube, and selecting 1000r/m for centrifugation;
s9, placing the centrifuged supernatant into a polytetrafluoroethylene digestion tank, adding 1ml of hydrochloric acid solution with the concentration of 0.5mol/L, covering an upper cover of the digestion tank, then keeping the temperature of the digestion tank at 90 ℃ for 2 hours, and cooling to room temperature to finish the collection of silicate components.
Further, in the step S1, the polytetrafluoroethylene digestion tank is soaked in a nitric acid solution with the concentration of 5% -15% before use, and other substances existing in the digestion tank are eliminated to influence an experimental result.
It will be appreciated by those of ordinary skill in the art that the embodiments described herein are intended to assist the reader in understanding the principles of the invention and are to be construed as being without limitation to such specifically recited embodiments and examples. Those skilled in the art can make various other specific changes and combinations based on the teachings of the present invention without departing from the spirit of the invention, and these changes and combinations are within the scope of the invention.
Claims (2)
1. The Sr isotope pretreatment method for the mixed rock is characterized by comprising the following steps of:
s1, weighing 50mg of a mixed rock sample by adopting an electronic balance, and putting the mixed rock sample into a polytetrafluoroethylene digestion tank;
s2, adding 3ml of concentrated nitric acid with the concentration of 1.5mol/L into a polytetrafluoroethylene digestion tank, shaking the digestion tank to fully mix the mixed rock sample and the concentrated nitric acid, then covering an upper cover of the polytetrafluoroethylene digestion tank, and placing the polytetrafluoroethylene digestion tank on a heating plate at 110 ℃ for continuous heat preservation for 24 hours;
s3, taking out the polytetrafluoroethylene digestion tank, cooling to room temperature, sucking supernatant liquid by using a liquid transfer gun, transferring the supernatant liquid to a centrifuge tube, and centrifuging at 3000r/m to collect carbonate rock components;
s4, adding 4ml of 1mol/L sodium hydroxide solution into the digestion tank after the supernatant is completely sucked, and then keeping the temperature of the digestion tank at 60 ℃ for 24 hours;
s5, adding 3ml of sodium hydroxide solution with the concentration of 0.5mol/L into the digestion tank, then preserving the temperature of the digestion tank at 60 ℃ for 24 hours, and evaporating to dryness after preserving the temperature;
s6, continuously adding 3ml of sodium hydroxide solution with the concentration of 0.5mol/L into the digestion tank, then preserving the temperature of the digestion tank at 60 ℃ for 24 hours, and evaporating to dryness after preserving the temperature;
s7, continuously adding 3ml of 1.5mol/L sodium hydroxide solution into the digestion tank, then preserving the temperature of the digestion tank at 120 ℃ for 48 hours, and evaporating to dryness after preserving the temperature;
s8, taking out the digestion tank, cooling to room temperature, adding 3ml of hydrochloric acid solution with the concentration of 1mol/L, sucking supernate by using a liquid transfer gun after the solution is fully reflected, transferring the supernate to a centrifugal tube, and selecting 1000r/m for centrifugation;
s9, placing the centrifuged supernatant into a polytetrafluoroethylene digestion tank, adding 1ml of hydrochloric acid solution with the concentration of 0.5mol/L, covering an upper cover of the digestion tank, then keeping the temperature of the digestion tank at 90 ℃ for 2 hours, and cooling to room temperature to finish the collection of silicate components.
2. The Sr isotope pretreatment method for the mixed rock as recited in claim 1, wherein in the step S1, the polytetrafluoroethylene digestion tank is soaked in a nitric acid solution with a concentration of 5% -15% before use.
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