CN104655712A - Method for measuring lithium isotope in fluid inclusion water in quartz vein of porphyry deposit - Google Patents

Method for measuring lithium isotope in fluid inclusion water in quartz vein of porphyry deposit Download PDF

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CN104655712A
CN104655712A CN201510093763.XA CN201510093763A CN104655712A CN 104655712 A CN104655712 A CN 104655712A CN 201510093763 A CN201510093763 A CN 201510093763A CN 104655712 A CN104655712 A CN 104655712A
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quartz
fluid inclusion
lithium isotope
fluid
isotope
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CN104655712B (en
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杨丹
杨志明
赵悦
侯可军
田世洪
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Institute of Mineral Resources of Chinese Academy of Geological Sciences
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Abstract

The invention discloses a method for measuring lithium isotopes in fluid inclusion water. Comprises 1) detecting lithium isotope in quartz, dissolving quartz sample after surface purification, fluid inclusion extraction and ultrasonic extraction, chemically purifying, and detecting lithium isotope; 2) according to empirical formulas: linear equation of Δ7LiQuartz-fluid-23.197 × (1000/T) +38.057, coefficient of linear correlation R2The lithium isotope in the fluid inclusion water was calculated as 0.9583. The method can conveniently and rapidly measure the lithium isotope in the fluid inclusion, and has important significance for the research of the ore deposit.

Description

The assay method of lithium isotope in fluid inclusion water in a kind of quartz vein of Porphyry-type Deposit
Technical field
The present invention relates to isotope field tests, say further, relate to the assay method of lithium isotope in fluid inclusion water in a kind of quartz vein of Porphyry-type Deposit.
Background technology
Porphyry copper is huge with it, and the even mineralising of total rock, buries shallow, and be suitable for exploitation, recovery rate in ore-dressing is high, becomes most important copper mine type in the world.In recent years, because of exposure in earth's surface, be easy to identify Porphyry-type Deposit be found more, reconnoitre the searching that need proceed to more blind deposit.Force people only can not be satisfied with descriptive one-tenth ore deposit-exploration model, start tectono-magmatic process (Richards et al., 2001 that on region-of-interest yardstick more, porphyry deposit is formed; , and the Deep Process that formed of mineralized porphyry and Geodynamic Background (Richards, 2003,2007 Richards, 2003); Hou et al., 2003,2004; Cooke et al., 2005); Meanwhile, (Ulrich et al., 2001 such as detailed evolutionary process and metallogenic material PRECIPITATION MECHANISM of BIFhosted gold deposit; Rusk et al., 2004; Redmond et al., 2004; Harris et al., 2005) emphasis studied especially.
BIFhosted gold deposit is most active geologic agent in mineralizing process, and in whole mineralizing process, it extracts, dissolve, carry, precipitate and have accumulated metallogenic material, is to link up ore source field, the medium of migration field and ore stockyard and tie (Zhai Yusheng, 1999).To develop closely-related Porphyry-type Deposit for mineralizing process and magmatic hydrotherm especially, carrying out detailed BIFhosted gold deposit research to it, contribute to reinventing magma-fluid-ore-forming evolution process, is the key of announcement origin of ore deposit.
The detailed evolutionary process of BIFhosted gold deposit and metallogenic material PRECIPITATION MECHANISM etc. are all the most important things of mineral deposit research all the time.BIFhosted gold deposit is mineral deposit, especially hydrothermal deposit main medium when being formed, and plays an important role in the activation of mineral, migration and precipitation process.It is generally acknowledged, dissimilar hydrothermal deposit, its BIFhosted gold deposit source is not quite similar; Therefore, finding out that the source of BIFhosted gold deposit is for understanding mineralization in depth, finding out that water-filling conditions tool is of great significance.Usually, when hydroxyl altered mineral (as hornblende, chlorite, mica mineral) is grown in a large number, we can by measuring this type of mineral Hydrogen-oxygen Isotope composition (White, 1974), and utilize respective isotope fractionation equation, converse the Hydrogen-oxygen Isotope composition of BIFhosted gold deposit during mineral formation, be used for the source of spike BIFhosted gold deposit and Evolution Paths (as Sheppard andGustafson, 1975; Harris et al., 2005).But when the agensis of hydroxyl altered mineral or less growth, people, usually through the Determination of Oxygen Isotopes containing oxygen gangue mineral, converse the oxygen isotope of BIFhosted gold deposit during mineral formation; By the direct mensuration of this type of mineral inner fluid inclusion hydrogen isotope, investigate thoroughly the hydrogen isotope composition of BIFhosted gold deposit.
As gangue mineral the most common in hydrothermal deposit, quartz, with its metastable feature, makes its benefit extensive concern in ore-forming source.Usually, conventional BrF is adopted 5method measures quartzy oxygen isotope composition, and hydrogen isotope then uses decrepitation method to get inclusion water, the hydrogen manufacturing of zinc method, result mass spectroscopy.The quartzy oxygen isotope composition δ finally obtained 18o quartz, the OXYGEN ISOTOPE FRACTIONATION equation 1000ln α of the quartz-water utilizing Clavton to recommend quartz-water18o quartz18o water=3.38*10 6t -2the experience Fractionation Equations that the quartz that-3.40 (200-500 DEG C) (Clavton et al., 1972) or Zhang Ligang provide-water equilibrium oxygen isotope exchanges: 1000ln α quartz-water18o quartz18o water=3.42*10 6t -2-2.86 (Zhang Ligang, 1985), are calculated to be and exchange BIFhosted gold deposit oxygen isotope when reaching balance with mineral isotope and form δ 18o water, its result is thrown at δ D-δ together with fluid inclusion hydrogen isotope 18o waterin diagram (Zheng Yongfei, 2000), to judge the source of BIFhosted gold deposit.
These ways have it to be difficult to the defect avoided above.Quartz decrepitation method gets inclusion water to obtain hydrogen isotope composition: be 1. difficult to avoid second inclusion to mix (Yang Zhiming, 2009); 2. the explosive spalling isotope fractionation that may cause, Faure (2003) obtains conclusion through experiment: same quartz specimen burst at 800 DEG C extract water than 500 DEG C at the δ D of explosion extraction aquametry h2Olow by 10 ~ 15 ‰, clearly explosive spalling can cause hydrogen isotope fractionation, can not represent into the isotopics of fluid during ore deposit, and separately have document (Sheetset al., 1996; O'Reilly et al., 1997; Gleeson et al., 1999; Barker et al., 2000) show the δ D that more than the 1000 DEG C Quartz inclusion extraction water burst obtain h2Oit is unusual low value; 3. inclusion opens the pollution that may cause; These all can make hydrogen isotope composition be affected.
For traditional stable isotope (as C, H and O), lithium isotope is a kind of unconventional stable isotope.Lithium isotope geochemistry is the research field (Zhang Hongfu etc., 2007) that international ground educational circles is emerging in recent years.The Geochemical Properties that lithium has many uniquenesses makes it in the various geologic function that spike is relevant with fluid, demonstrate special superiority
It is the mineral that mica mineral, spodumene, hornblende etc. lithium content is higher that lithium isotope measures current conventional mineral, quartz due to the low and indissoluble solution of lithium content, less use.But Just because of this, quartz has fabulous physical chemistry patience, therefore often can not with its physicochemical property of environment change, therefore, the isotopics in the quartz that same period is not secondary in fluid inclusion water can reflect the not time BIFhosted gold deposit isotopics same period
Study BIFhosted gold deposit by lithium isotope, the lithium isotope in fluid inclusion water measures can obtain direct result.But in hydrothermal deposit to become the relevant quartz vein in ore deposit mostly tiny, and comprise in quartz vein that fluid inclusion quantity is few, volume is little, the fluid inclusion water extracted is difficult to satisfiedly test needs.It is the mineral that mica mineral, spodumene, hornblende etc. lithium content is higher that lithium isotope measures current conventional mineral, and quartz is due to lithium content low and indissoluble solution, also less use.Therefore, in the urgent need to the pre-treating method setting up a quartz specimen, quartz and fluid inclusion are separated, and set up an experimental formula, by the lithium isotope (δ of quartz 7li quartz) and fluid inclusions homogenization temperature (T homogeneous) Accurate Determining, lithium isotope composition (δ can be obtained in fluid inclusion water 7li fluid).
Summary of the invention
For solving produced problem in prior art, the invention provides the assay method of lithium isotope in fluid inclusion water in a kind of quartz vein of Porphyry-type Deposit.By setting up quartz and the fractionation experimental formula of lithium isotope in fluid inclusion water, only need to measure δ in quartz 7li and fluid inclusions homogenization temperature (T), calculate the δ that can obtain in fluid by fractionation experimental formula 7li fluid.
The object of this invention is to provide the assay method of lithium isotope in a kind of fluid inclusion water.
Comprise:
1) mensuration of lithium isotope in quartz
Quartz specimen is dissolved after surface cleaning, fluid inclusion extraction, ultrasonic extraction, and chemical purification, carries out the mensuration of lithium isotope;
2) empirically formula: linear equation is △ δ 7li quartz-fluid=-23.197 × (1000/T)+38.057, linearly dependent coefficient R 2=0.9583 calculates lithium isotope in fluid inclusion water;
T is fluid inclusions homogenization temperature (K), T=t+273.15 (K), 350 DEG C≤t≤600 DEG C, preferably 353 DEG C≤t≤586 DEG C.
Wherein, preferred:
Described quartz specimen is the Pure quartz sample that purity is greater than 98%, granularity 60-80 order.
In step (1), polishing is adopted to extract fluid inclusion.
In step (1), the number of times of ultrasonic extraction is more than or equal to 5 times.
In step (1), quartz specimen first adds HNO 3, after add HF dissolve.
The consumption dissolving the HF of 1g quartz is more than or equal to 5ml.Add HNO 3can adjust according to actual conditions with the amount of HF, suitable to be fully dissolved as.In the present invention, can be preferred: 1g quartz specimen needs 0.5mLHNO 3and 5mLHF.
In the present invention, in quartz, lithium isotope measuring method can adopt the measuring method of common lithium isotope in prior art, as the surface cleaning of quartz specimen, the extraction of fluid inclusion water, the dissolving method etc. of quartz specimen can adopt conventional method of the prior art, in the present invention, can preferably carry out according to the following steps:
A. sample surfaces purification
The Pure quartz sample purity of select being greater than 99% adds appropriate chloroazotic acid and to be positioned on heating plate 120 DEG C of insulations 3 hours, inclines remaining acid also with ultrapure water cleaning, is washed till cleansing solution conductance consistent with ultrapure water conductance, ultrapure water soaked overnight.Incline soak solution, adds ultrapure water, with ultrasonic cleaner ultrasonic cleaning sample number minute, suction filtration immediately, and with milli-Q water for several times, sample is placed in porcelain dish, in 100 DEG C of oven dry.
B. sample size
Porphyry-type Deposit quartz vein sample > 0.5g, about 1g is best, and the lithium content of quartz itself can meet test needs.The lithium content that extracts in fluid inclusion liquid phase indefinite, still only have a small amount of sample can meet test needs.
C. polishing opens fluid inclusion
Load weighted sample is ground to more than 200 orders, now can think that fluid inclusion is all grated.
D. extraction time
By above-mentioned ground sample ultrapure water ultrasonic washing suction filtration sample 5 times, fluid inclusion liquid phase can be extracted comparatively completely.Quartz specimen after extraction is placed in porcelain dish, in 80 DEG C of oven dry.
E. sample dissolution
The sample of above-mentioned drying is added HNO 3carry out the molten sample of the first step with HF, about 1g sample adds 0.5mL HNO 3+ 5mL HF, first adds HNO during molten sample 3, after add HF.All the other molten sample steps and universal method (Rudnick, 2004; Tian et.al.2012) consistent.
1. 1g sample adds 0.5mL HNO 3+ 5mL HF, first adds HNO during molten sample 3, after add HF; 2. tighten bottle cap, shake 10 minutes in ultrasound wave, be placed in heater plate 24 hours (temperature is 120 DEG C); 3. evaporate to dryness solution, adds a certain amount of dense HNO 32-4 time, each all evaporates to dryness; 4. add dense HCl in the sample to which, heat under 120 DEG C of conditions, until solution dissolves completely; 5. evaporate to dryness sample, adds 1.2mL4MHCl, for subsequent use.
F. purifying
Because the lithium content of fluid inclusions in quartz and quartz itself and Main elements content are all far smaller than several international standard sample, therefore, chemical purification method (Rudnick, 2004 consistent with universal method; Tianet.al.2012), namely can meet purification requirements, after purifying, sample carries out MC-ICP-MS and tests the lithium isotope ratio that can obtain in fluid inclusions in quartz and quartz.Universal method refers to the method for prior art routine, as follows.
1. exchange column 1
Exchange column 1 is for being filled with the polypropylene exchange column of 1.2mL Zeo-karb (AG50W-X8).Leacheate is 2.8M HCl.First add 1mL 4M HCl and balance pillar, then get 1mL sample (molten sample process final sample adds 1.2mL 4M HCl, gets 1mL after centrifugal) and add exchange column 1, then add 5mL leacheate one by one.The 1mL sample added more than collecting with Teflon beaker and 5mL leacheate.Evaporate to dryness (100 ~ 120 DEG C) on electric hot plate, it is for subsequent use to add 2mL 0.15M HCl.Rare earth element can thoroughly be separated by this exchange column, can be separated roughly Main elements (mainly referring to Na, K, Ca, Fe, Mg) simultaneously.
2. exchange column 2
Exchange column 2 is for being filled with the polypropylene exchange column of 1.5mL Zeo-karb (AG50W-X8).Leacheate is 0.15M HCl.By 2mL through previous step working solution add exchange column 2, then add 21mL leacheate, collect (note: do not collect sample solution, only collect leacheate) with Teflon beaker.Electric hot plate heats evaporate to dryness (100 ~ 120 DEG C), and it is for subsequent use to add 1mL 0.15M HCl.Li with Na is separated with other Main elements by this exchange column.
3. exchange column 3
Exchange column 3 is for being filled with the quartzy exchange column of 1mL Zeo-karb (AG50W-X8).Leacheate is 0.5M HCl 30%C 2h 5oH.By 1mL through previous step working solution add exchange column 3, then add 9mL leacheate, and collect with Teflon beaker, electric hot plate heats evaporate to dryness (100 ~ 120 DEG C).In order to separating effect is better, exchange column 3 was generally wanted twice.This exchange column can be separated Li and Na.
Mass spectrometric measurement
By after purifying the sample of evaporate to dryness add 1.2mL 2%HNO 3, prepare to carry out mass spectrometric measurement.
Thermo Finnigan Neptune type MC-ICP-MS is used to test, 7li and 6li uses two contrary Faraday cups to measure simultaneously, and the former is positioned at high-quality Faraday cup (H4), and the latter is positioned at inferior quality Faraday cup (L4) (Hou Kejun, 2007; 2008; 2010).Instrument working parameter: RF power 1200W, cold gas is about 15L/min, and assisted gas is about 0.6L/min, and carrier gas is about 1.15L/min, and atomizer type is Menhard atomizer (50 μ L/min), analyzer vacuum 4 × 10 -9~ 8 × 10 -9pa (Hou Kejun, 2007; 2008; 2010).For accurate test, appliance requires preheating just can reach fully stable for 1 ~ 2 hour.
When test starts, first half vector quantization test is carried out to Na/Li, if Na/Li>20, need again to cross exchange column 3 to sample, be separated Na further.For lithium isotope, the mass fractionation produced by plasma source reaches 25%, but the testing process of bracketing method, (Millot, 2004 can be corrected to it; Hou Kejun, 2008), be specially: standard specimen → blank → sample → blank → standard specimen.Test result represents: δ 7li=[(R sP/ R sT)-1] × 1,000 ‰, wherein R sPfor sample 7li/ 6the measured value of Li ratio, R sTfor twice standard specimen adjacent with sample 7li/ 6the mean value of Li ratio measurement.Isotopic standard material used is L-SVEC or IRMM-016.Often organize collection 20 data during sample test, gather 2 ~ 4 groups of data altogether, 7li/ 6li uncertainty of measurement≤± 0.2 ‰ (2 σ).Between every twice test, with the HNO of 2% and 5% 3alternately purging system.
Obtain the result of lithium isotope in quartz.
According to the measurement result of lithium isotope in quartz, according to experimental formula of the present invention, lithium isotope in fluid inclusion can be calculated.
Experimental formula according to we obtain: △ δ 7li quartz-fluid=-23.197 × (1000/T)+38.057, this formula Applicable temperature scope is 315 ~ 596 DEG C, if be 400 DEG C and 500 DEG C to fixed temperature, the △ δ obtained 7li quartz-fluidfor+4 ‰ and+8 ‰, with the measured value of Lynton et al. (2005) (400 DEG C, △ quartz-aqueous≈+4 ~+6 ‰; 500 DEG C, △ quartz-aqueous≈+8 ~+12 ‰).Contrast with document, use this formula to obtain △ δ when 400 DEG C and 500 DEG C 7li quartz-fluidconsistent with measured value.Therefore, experimental formula of the present invention is accurately.
Embodiment
Below in conjunction with embodiment, further illustrate the present invention.
Instrument
Lithium isotope composition test analysis completes in Neptune type many receptions plasma mass spectrograph (MC-ICP-MS) of Isotope Geology key lab of Ministry of Land and Resources.This instrument configuration 9 Faraday cups and 5 ion counters.8 Faraday cups are configured in centerpiece both sides, drive carry out accurate position adjustments with motor; An electron-multiplier is housed after centerpiece, and 4 ion counters are equipped with in a minimum quality number glass outside.MC-ICP-MS is double focusing (Voice segment and quality focus on) type mass spectrometer, adopts dynamic zoom (ZOOM) patented technology, mass dispersion can be extended to 17%.Enter the stable sampling system (stable introduction system, SIS) that the said firm produces after sample atomization, this stable sampling system is the combination of cyclone and Si Kete atomizer, can provide more stable signal and shorten scavenging period [46].
Labware and main agents
Complete in the Superclean Lab that the pre-treatment of sample is operated in isotope key lab of Ministry of Land and Resources, Cleanliness is thousand grades, is hundred grades in superclean bench.
In experiment flow, vessel used are polypropylene or polytetrafluoroethylmaterial material, adopt strict cleaning process, to reduce the background of vessel: wash for the first time---the pure HNO of top grade 3(7mol/L) immersion---ultrapure water cleaning, immersion---dry for standby that the pure HCl of top grade (6mol/L) soaks---ultrapure water cleaning, immersion---.
Test ultrapure water used to be obtained by Millipure purifying, resistivity is 18.2M Ω cm.Main chemical reagent has HCl, HNO 3, HF and absolute ethyl alcohol, wherein HCl, HNO 3, HF by the pure acid of MOS level through Savillex DST-1000 sub-boiling distillation secondary system distillation gained; Ethanol is MOS level pure reagent, and concentration is 99.9%.
Laboratory sample
In the experiment that sample size size affects lithium isotope measured value, international conventional lithium standard substance IRMM – 016 is selected to be purchased from US Geological Survey.
Testing procedure:
A sample surfaces purifies
The Pure quartz sample purity of select being greater than 99% adds appropriate chloroazotic acid and to be positioned on heating plate 120 DEG C of insulations 3 hours, inclines remaining acid also with ultrapure water cleaning, is washed till cleansing solution conductance consistent with ultrapure water conductance, ultrapure water soaked overnight.Incline soak solution, adds ultrapure water, with ultrasonic cleaner ultrasonic cleaning sample number minute, suction filtration immediately, and with milli-Q water for several times, sample is placed in porcelain dish, in 100 DEG C of oven dry.
B sample size
Porphyry-type Deposit quartz vein sample > 0.5g, about 1g is best, and the lithium content of quartz itself can meet test needs.The lithium content that extracts in fluid inclusion liquid phase indefinite, still only have a small amount of sample can meet test needs.
C. polishing opens fluid inclusion
Load weighted sample is ground to more than 200 orders, now can think that fluid inclusion is all grated.
D. extraction time
By above-mentioned ground sample ultrapure water ultrasonic washing suction filtration sample 5 times, fluid inclusion liquid phase can be extracted comparatively completely.Quartz specimen after extraction is placed in porcelain dish, in 80 DEG C of oven dry.
E. sample dissolution
The sample of above-mentioned drying is added HNO 3carry out the molten sample of the first step with HF, about 1g sample adds 0.5mL HNO 3+ 5mL HF, first adds HNO during molten sample 3, after add HF.All the other molten sample steps are consistent with universal method.
F. purifying
Because the lithium content of fluid inclusions in quartz and quartz itself and Main elements content are all far smaller than several international standard sample, therefore, chemical purification method is consistent with universal method, namely can meet purification requirements, after purifying, sample carries out MC-ICP-MS and tests the lithium isotope ratio that can obtain in fluid inclusions in quartz and quartz.Universal method refers to the method for prior art routine.
According to the measurement result of lithium isotope in quartz, according to experimental formula of the present invention, lithium isotope in fluid inclusion can be calculated.
Embodiment 1 ~ 6
Test according to above step, result is as table 1.
Table 1

Claims (7)

1. the assay method of lithium isotope in fluid inclusion water in the quartz vein of Porphyry-type Deposit, is characterized in that described method comprises:
1) mensuration of lithium isotope in quartz
Quartz specimen is dissolved after surface cleaning, fluid inclusion extraction, ultrasonic extraction, and chemical purification, carries out the mensuration of lithium isotope;
2) empirically formula: linear equation is △ δ 7li quartz-fluid=-23.197 × (1000/T)+38.057, linearly dependent coefficient R 2=0.9583 calculates lithium isotope in fluid inclusion water;
T is fluid inclusions homogenization temperature K, T=t+273.15K, 350 DEG C≤t≤600 DEG C.
2. the assay method of lithium isotope in fluid inclusion water in the quartz vein of Porphyry-type Deposit as claimed in claim 1, is characterized in that:
Described quartz specimen is the Pure quartz sample that purity is greater than 98%, granularity 60-80 order.
3. the assay method of lithium isotope in fluid inclusion water in the quartz vein of Porphyry-type Deposit as claimed in claim 1, is characterized in that:
In step (1), polishing is adopted to extract fluid inclusion.
4. the assay method of lithium isotope in fluid inclusion water in the quartz vein of Porphyry-type Deposit as claimed in claim 1, is characterized in that:
In step (1), the number of times of ultrasonic extraction is more than or equal to 5 times.
5. the assay method of lithium isotope in fluid inclusion water in the quartz vein of Porphyry-type Deposit as claimed in claim 1, is characterized in that:
In step (1), quartz specimen first adds HNO 3, after add HF dissolve.
6. the assay method of lithium isotope in fluid inclusion water in the quartz vein of Porphyry-type Deposit as claimed in claim 5, is characterized in that:
The consumption dissolving the HF of 1g quartz is more than or equal to 5ml.
7. the assay method of lithium isotope in fluid inclusion water in the quartz vein of Porphyry-type Deposit as claimed in claim 2, is characterized in that:
In step (1), polishing is adopted to extract fluid inclusion;
In step (1), the number of times of ultrasonic extraction is more than or equal to 5 times;
In step (1), quartz specimen first adds HNO 3, after add HF dissolve.
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CN113358780A (en) * 2021-06-03 2021-09-07 中国地质大学(北京) Method for detecting potassium isotope in plant

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CN107422024A (en) * 2017-08-03 2017-12-01 核工业北京地质研究院 The analysis system and method for not oxygen-containing mineral inclusion water oxygen isotopics
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CN109425649A (en) * 2018-10-09 2019-03-05 中国地质科学院矿产资源研究所 Method for searching blind ore body based on element content of cow dung lithium
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