CN102944458A - Rock mineral comprehensive analysis method - Google Patents
Rock mineral comprehensive analysis method Download PDFInfo
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- CN102944458A CN102944458A CN2012105283101A CN201210528310A CN102944458A CN 102944458 A CN102944458 A CN 102944458A CN 2012105283101 A CN2012105283101 A CN 2012105283101A CN 201210528310 A CN201210528310 A CN 201210528310A CN 102944458 A CN102944458 A CN 102944458A
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Abstract
The invention discloses a rock mineral comprehensive analysis method, and belongs to the field of rock mineral analysis. By adopting the method, loss caused by volatilization of a volatile matter for preparing glass fuse piece is quantified by introducing a volatilization coefficient (a proportion of the volatile matter) of a solvent; the glass fuse piece is quantitatively partitioned by establishing a partition factor, so that quantitative partitioning of the conventional sample can be reduced; the glass fuse piece prepared by one-time melting is suitable for various analysis measures; and then the rock mineral comprehensive analysis method is established. Compared with the prior art, the rock mineral comprehensive analysis method has the characteristics of simplicity in operation, high sample utilization rate and the like and is extremely high in popularization and application value.
Description
Technical field
The present invention relates to the rock mineral analysis field, specifically a kind of rock forming mineral comprehensive analysis method.
Background technology
In the rock mineral analysis field, along with the progress of science and technology and the growth requirement of modern geoscience, the element kind of measuring is more and more, requirement to analytical technology index (precision, accuracy and detectability etc.) is also more and more higher, therefore, corresponding analysis and testing technology is also more and more complete, nearly all analysis and testing technology has all been brought into play vital role in the rock mineral analysis field, such as X-ray fluorescence spectra analytic approach, ICP-AES analytic approach, plasma mass analytic approach, absorption flame photometry method etc.When these methods of use are carried out sample analysis, all must be quantitative take by weighing is fit to the separately required sample size of analytical approach, add again a certain amount of other chemical reagent, by special sample preparation, be prepared into the suitable separately required sample form of analytical approach, in order to implement the analytical test of various analytical approachs.
Common sample treatment generally is divided into two classes, and the one, directly use acid molten; At first use besides the fusion technology of borate-based flux, geological sample is converted into the salt that boric acid is, carry out again acidification.The former great advantage is simple, but solute effect is not good enough, and some element is difficult to enter solution (such as Nb, Zr etc.), residue often occurs.And residue appears in the latter's solute effect relatively perfection (referring to DZG20.01) hardly, so normal this method of using is processed sample at present.
In rock mineral analysis, usually adopt following method to carry out sample preparation:
(1) X-ray fluorescence spectra analytic approach: take by weighing 1 gram sample, add a certain proportion of borate-based flux, use platinum crucible, through high temperature (being generally 1050 ℃) melting, be prepared into uniform bead.
(2) ICP-AES analytic approach: take by weighing 0.3 gram sample, add a certain proportion of borate-based flux, use graphite crucible, through high temperature (being generally 1050 ℃) melting, be prepared into spherical fused glass bead, hydrochloric acid with 5% or nitric acid dissolve are prepared into liquid working fluid and measure.
(3) plasma mass analytic approach: take by weighing 0.1 gram sample, add a certain proportion of borate-based flux, use graphite crucible, through high temperature (being generally 1050 ℃) melting, be prepared into spherical fused glass bead, hydrochloric acid with 5% or nitric acid dissolve are prepared into liquid working fluid and measure.
(4) absorption flame photometry method: take by weighing 0.2 gram sample, add a certain proportion of borate-based flux, use graphite crucible, through high temperature (being generally 1050 ℃) melting, be prepared into spherical fused glass bead, hydrochloric acid with 5% or nitric acid dissolve are prepared into liquid working fluid and measure.
The disposal route of above sample (seeing DZG20.01) has been passed through long-term practical application, has higher reliability, stability and validity, generally, and the fully contentedly requirement of quality sample multielement quantitative test.But also exist certain deficiency, be mainly reflected in the repetition of the melting process of borate-based flux, this repetition can be brought following problem:
(1) because every kind of method of testing all needs to consume a certain amount of sample, thereby required sample total amount is more, when running into the analytical test object of sample size less (such as air participates, Within Monominerals etc.), just have a lot of difficulties, test assignment can't normally be finished;
(2) repetitive operation (such as borate-based sample melted) of sample preparation that every kind of method of testing is carried out can cause the waste of Efficiency Decreasing and experiment material and the energy, and this can bring the increase of cost;
(3) this repetitive operation also can increase the discharging of " three wastes ", and is unfavorable in environmental protection.
Sample and flux have certain fugitive constituent will volatilize (such as CO2, water of crystallization etc.) under high temperature fused state, and volatile quantity is different because of sample.In the X-ray fluorescence spectra analytic approach of sample use amount maximum, usually fugitive constituent is not quantized, just in the preparation process of bead, pass through the restriction (temperature, time etc.) to sampling, offset fugitive constituent to the impact of measurement result, this disposal route can satisfy the requirement of X-ray fluorescence spectra analytic approach fully.Yet if want to allow bead continue to play a role, when being applied to other analytical approach, this disposal route just can not be suitable for.Its reason is: the volatilization under high temperature fused state of sample and flux, make sample in the bead and the weight (or weight ratio) of flux that variation occur, thereby when bead is cut apart, even whole (or local) bead is carried out accurate weighing, its sample size relevant with former state of comprising of acquisition that can not be quantitative, namely concerning former state, this bead can not quantitatively be cut apart, and also just can't be analyzed analytical approach by other and use.
Summary of the invention
Technical assignment of the present invention is for above-mentioned the deficiencies in the prior art, and a kind of simple to operate, rock forming mineral comprehensive analysis method that the sample application rate is high is provided.The method quantizes by the loss that the volatility coefficient (the shared ratio of volatilization composition) of introducing flux brings the volatilization of fugitive constituent to the preparation bead; Realize quantitatively cutting apart of bead by setting up splitting factor, thereby be reduced to quantitatively the cutting apart of former state that the bead that a melting is made is applicable to various analysis means, and then sets up a kind of comprehensive analysis method of rock forming mineral.
The volatility coefficient A of flux: the volatilization composition of flux shared ratio in the flux total amount.
The volatilization factor B of sample: the volatilization composition of sample shared ratio in the sample total amount.
The splitting factor K of bead: a great deal of of former state in the unit bead.
Technical assignment of the present invention is realized in the following manner: a kind of rock forming mineral comprehensive analysis method, be characterized in by bead is quantitatively cut apart, the bead that a melting is made is cut apart and is applied to ICP-AES analysis and/or plasma mass analysis and/or absorption flame photometry
Specifically may further comprise the steps:
1) the volatility coefficient A of mensuration flux
Accurately taking by weighing weight is A
0The flux of g is in platinum crucible, at a ℃ of lower calcination melting b min, takes out and is cooled to the room temperature weighing, and deduction crucible weight obtains the weight A of the fugitive constituent that flux loses
1G, calculate volatility coefficient A by following formula:
A＝(A
0-A
1)/A
0*100％；
2) the volatilization factor B of working sample
Taking by weighing weight is m
0The sample of g and weight are m
1The flux of g, (Ministry of Land and Resources's standard method is numbered: requirement preparation DZG20.01) is suitable for the bead that X-ray fluorescence spectra is analyzed, and the weight of gained bead is m according to the rock mineral analysis method
2G, by the volatilization factor B of following formula calculation sample:
B＝(m
0-(m
2-m
1*(1-A)))/m
0*100％；
3) the splitting factor K of calculating bead
Calculated the splitting factor K of bead by following formula:
K＝(m
2-m
1*(1-A))/(m
2*(1-B))；
4) preparation bead particle
Step 2 gained bead is carried out coarse crushing, obtain granularity less than 5 millimeters bead particle;
5) utilize the bead particle to carry out analytical test
According to actual needs, taking by weighing portion or some parts of weight is m
3The bead particle of g, and with splitting factor K this weight is reduced to the weight of former state, the weight of former state represents with m:
m＝K*m
3；
Each part bead particle is used for finishing ICP-AES analysis and/or plasma mass
Analyze and/or absorption flame photometry.
Further, in the time of need to carrying out the X-ray fluorescence spectra analysis to rock forming mineral, the characteristics of above-mentioned comprehensive analysis method are: by bead is quantitatively cut apart, X-ray fluorescence spectra is analyzed used bead to be cut apart and is applied to ICP-AES analysis and/or plasma mass analysis and/or absorption flame photometry
Specifically may further comprise the steps:
1) the volatility coefficient A of mensuration flux
Accurately taking by weighing weight is A
0The flux of g is in platinum crucible, at a ℃ of lower calcination melting b min, takes out and is cooled to the room temperature weighing, and deduction crucible weight obtains the weight A of the fugitive constituent that flux loses
1G, calculate volatility coefficient A by following formula:
A＝(A
0-A
1)/A
0*100％；
2) the volatilization factor B of working sample
Taking by weighing weight is m
0The sample of g and weight are m
1The flux of g, (Ministry of Land and Resources's standard method is numbered: the requirement preparation of DZG20.01 is suitable for the bead that X-ray fluorescence spectra is analyzed, and the weight of gained bead is m according to the rock mineral analysis method
2G, by the volatilization factor B of following formula calculation sample:
B＝(m
0-(m
2-m
1*(1-A)))/m
0*100％；
3) carry out the X-ray fluorescence spectra analysis
4) the splitting factor K of calculating bead
Calculated the splitting factor K of bead by following formula:
K＝(m
2-m
1*(1-A))/(m
2*(1-B))；
5) preparation bead particle
The bead that has carried out x-ray fluorescence analysis in the step 3 is carried out coarse crushing, obtain granularity less than 5 millimeters bead particle;
6) utilize the bead particle to carry out the ICP-AES analysis and/or plasma mass divides
Analyse and/or absorption flame photometry
According to actual needs, taking by weighing portion or some parts of weight is m
3The bead particle of g, and with splitting factor K this weight is reduced to the weight of former state, the weight of former state represents with m:
m＝K*m
3；
Each part bead particle is used for finishing ICP-AES analysis and/or plasma mass
Analyze and/or absorption flame photometry.
Preferably, in the step 1, the platinum crucible of flux is housed at 1050 ℃ of lower calcination melting 15min.
Rock forming mineral comprehensive analysis method of the present invention compared with prior art has following outstanding beneficial effect:
(1) realized that multiple analysis means to the sharing of bead, is improved work efficiency, also reduced the consumption of experiment material and the energy simultaneously, thereby reduced cost, be conducive to the development of conservation-minded society;
(2) consume the analytical test that less sample can be finished multiple analysis means, be particularly conducive to the analytical test of sample size less (such as air participates, Within Monominerals etc.); Simultaneously also weakened analytical test to the sample quantitative limitation, made originally and can normally finish because of the less test assignment that can't finish of sample size;
(3) because the diluting effect of flux, make sample size obtain " amplification ", make and to realize by larger weighing than the weighing (such as plasma mass analytic approach etc.) of small sample quantities, thereby be implemented in the situation that weighing error do not reduce, come the less sample size of weighing;
(4) integrate multiple analysis means; a melting, many analysis means are shared; reduced the melting number of times; thereby effectively reduce the discharging of " three wastes "; be conducive to environmental protection; thereby be suitable for current " green living " advocated, and be particularly suitable for current " the green analytic approach " advocated in analytical test field, promote the development and progress in rock-mineral analysis field.
Embodiment
Explain below with specific embodiment rock forming mineral comprehensive analysis method of the present invention being done.
Embodiment one (volatility coefficient of flux):
In whole fusing system, sample be vary, type is different, it is single and total only having flux, the foundation of the volatility coefficient of flux is core of the present invention.Flux commonly used is generally borate-based flux, is generally: Na
2B
4O
7, Li
2B
4O
7, LiBO
2Deng and their combination.Can they obtain stable volatility coefficient and be to realize the key of quantitatively cutting apart under molten sample temperature (1050 ℃).Test as follows: accurately take by weighing 5.0000 gram flux in platinum crucible, 1050 ℃ of lower calcination meltings, choose the different melting times, take out and be cooled to room temperature weighing (comprising crucible), and deduction crucible weight, calculating volatility coefficient, the result is as shown in the table:
As can be seen from the table: Na
2B
4O
7Volatility coefficient, tend towards stability after 15 minutes in the calcination melting, the volatility coefficient of other flux tends towards stability after 10 minutes in the calcination melting, and the time of preparation melten glass sheet is generally between 10-20 minute and (sees DZG20.01).Therefore, in preparation bead time range, the volatilization of Flux Volatilization part is finished substantially, and namely through 15 minutes calcination melting, the volatility coefficient of flux commonly used tended towards stability, and can carry out quantitative Treatment to fugitive constituent in the melten glass sheet.
Embodiment two (melt temperature is on the impact of Flux Volatilization coefficient):
Along with the difference of sample, melt temperature is usually between 1000-1100 ℃.In this temperature range, volatility coefficient will directly affect the quantitative Treatment of fugitive constituent to the responsiveness of temperature, about bead can quantitatively cut apart, test as follows: accurately take by weighing 5.0000 gram flux in platinum crucible, use 950,1000,1050,1100,1150 ℃ and carry out the calcination melting, the melting time is 15 minutes, taking-up is cooled to room temperature weighing (comprising crucible), and deduction crucible weight, calculating volatility coefficient, the result is as shown in the table:
As can be seen from the above table, through 15 minutes calcination melting, volatility coefficient was stable in 1000-1100 ℃ scope, and this temperature range can satisfy the melting preparation of most of sample types.
Embodiment three mensuration of multielement (in the sample ore product)
For the present invention is further elaborated, so that advantage of the present invention is more obvious, use national standard material GBW07103, GBW07401, GBW07301 as sample, utilize comprehensive analysis method of the present invention to measure.
Common parameter is: flux and consumption: Li2B4O7; 5 grams;
Sample size: 1 gram.
Step 1) the volatility coefficient A of mensuration flux
Accurately taking by weighing weight is A
0The flux of g is in platinum crucible (A
0=5), at 1050 ℃ of lower calcination melting 15min, take out and to be cooled to the room temperature weighing, deduction crucible weight obtains the weight A of the fugitive constituent that flux loses
1G, calculate volatility coefficient A by following formula:
A＝(A
0-A
1)/A
0*100％
Step 2) the volatilization factor B of working sample
Take by weighing the flux (m that sample that weight is m0g and weight are m1g
0=1, m
1=5), according to the rock mineral analysis method (Ministry of Land and Resources's standard method is numbered: requirement DZG20.01), preparation is suitable for the bead that X-ray fluorescence spectra is analyzed, the weight of gained bead is m
2G, by the volatilization factor B of following formula calculation sample:
B＝(m
0-(m
2-m
1*(1-A)))/m
0*100％
Step 3) with X-ray fluorescence spectra assay SiO
2, Al
2O
3
Step 4) the splitting factor K of calculating bead
Calculated the splitting factor K of bead by following formula:
K＝(m
2-m
1*(1-A))/(m
2*(1-B))。
Step 5) preparation bead particle
Step 2 gained bead (having finished x-ray fluorescence analysis) is carried out coarse crushing, obtain granularity less than 5 millimeters bead particle;
Step 6) utilize the bead particle to carry out ICP-AES analysis and/or plasma
Mass spectrophotometry and/or absorption flame photometry
Taking by weighing some parts of weight is m
3The bead particle of g, and with splitting factor K this weight is reduced to the weight of former state, the weight of former state represents with m:
m＝K*m
3
Cut apart the bead particle sample that obtains by the requirement of each analytical approach among the DZG20.01, dissolve separately preparation, measure Cu, Co, Ni, Zn with the plasma emission spectrometry method respectively, with plasma mass assay La, Ce, Nb, Zr, use atomic absorption spectroscopy determination Cd etc.Measured value and standard value are compared, observe its both matching degree, the results are shown in following table:
The measurement result table of GBW07401
The measurement result table of GBW07103
The measurement result table of GBW07301
By above detection data, measured value and standard value have higher matching degree, namely has less measuring error, can satisfy the requirement of quality standard (DZ/T0130-2006) fully, this illustrates that rock forming mineral comprehensive analysis method of the present invention has higher accuracy and rationality, the contemporary requirement of rock-mineral analysis be can adapt to fully, high-efficient development and the scientific-technical progress in rock-mineral analysis field helped to promote.
Claims (3)
1. rock forming mineral comprehensive analysis method, it is characterized in that: by bead is quantitatively cut apart, the bead that a melting is made is cut apart and is applied to ICP-AES analysis and/or plasma mass analysis and/or absorption flame photometry
Specifically may further comprise the steps:
1) the volatility coefficient A of mensuration flux
Accurately taking by weighing weight is A
0The flux of g is in platinum crucible, at a ℃ of lower calcination melting b min, takes out and is cooled to the room temperature weighing, and deduction crucible weight obtains the weight A of the fugitive constituent that flux loses
1G, calculate volatility coefficient A by following formula:
A＝(A
0-A
1)/A
0*100％；
2) the volatilization factor B of working sample
Taking by weighing weight is m
0The sample of g and weight are m
1The flux of g is suitable for the bead that X-ray fluorescence spectra is analyzed according to the requirement of rock mineral analysis method preparation, and the weight of gained bead is m
2G, by the volatilization factor B of following formula calculation sample:
B＝(m
0-(m
2-m
1*(1-A)))/m
0*100％；
3) the splitting factor K of calculating bead
Calculated the splitting factor K of bead by following formula:
K＝(m
2-m
1*(1-A))/(m
2*(1-B))；
4) preparation bead particle
Step 2 gained bead is carried out coarse crushing, obtains granularity less than 5 millimeters bead particle.
5) utilize the bead particle to carry out analytical test
According to actual needs, taking by weighing portion or some parts of weight is m
3The bead particle of g, and with splitting factor K this weight is reduced to the weight of former state, the weight of former state represents with m:
m＝K*m
3；
Each part bead particle is used for finishing ICP-AES analysis and/or plasma mass analysis and/or absorption flame photometry.
2. rock forming mineral comprehensive analysis method according to claim 1, it is characterized in that, by bead is quantitatively cut apart, X-ray fluorescence spectra is analyzed used bead to be cut apart and is applied to ICP-AES analysis and/or plasma mass analysis and/or absorption flame photometry
Specifically may further comprise the steps:
1) the volatility coefficient A of mensuration flux
Accurately taking by weighing weight is A
0The flux of g is in platinum crucible, at a ℃ of lower calcination melting b min, takes out and is cooled to the room temperature weighing, and deduction crucible weight obtains the weight A of the fugitive constituent that flux loses
1G, calculate volatility coefficient A by following formula:
A＝(A
0-A
1)/A
0*100％；
2) the volatilization factor B of working sample
Taking by weighing weight is m
0The sample of g and weight are m
1The flux of g is suitable for the bead that X-ray fluorescence spectra is analyzed according to the requirement of rock mineral analysis method preparation, and the weight of gained bead is m
2G, by the volatilization factor B of following formula calculation sample:
B＝(m
0-(m
2-m
1*(1-A)))/m
0*100％；
3) carry out the X-ray fluorescence spectra analysis
4) the splitting factor K of calculating bead
Calculated the splitting factor K of bead by following formula:
K＝(m
2-m
1*(1-A))/(m
2*(1-B))；
5) preparation bead particle
The bead that has carried out x-ray fluorescence analysis in the step 3 is carried out coarse crushing, obtain granularity less than 5 millimeters bead particle;
6) utilize the bead particle to carry out the ICP-AES analysis and/or plasma mass divides
Analyse and/or absorption flame photometry
According to actual needs, taking by weighing portion or some parts of weight is m
3The bead particle of g, and with splitting factor K this weight is reduced to the weight of former state, the weight of former state represents with m:
m＝K*m
3；
Each part bead particle is used for finishing ICP-AES analysis and/or plasma mass
Analyze and/or absorption flame photometry.
3. rock forming mineral comprehensive analysis method according to claim 1 and 2 is characterized in that, in the step 1, the platinum crucible of flux is housed at 1050 ℃ of lower calcination melting 15min.
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|---|---|---|---|
| CN201210528310.1A CN102944458B (en) | 2012-12-11 | 2012-12-11 | Rock mineral comprehensive analysis method |
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|---|---|---|---|
| CN201210528310.1A CN102944458B (en) | 2012-12-11 | 2012-12-11 | Rock mineral comprehensive analysis method |
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| CN102944458B CN102944458B (en) | 2015-04-01 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103344469B (en) * | 2013-07-08 | 2015-12-23 | 洪飞 | The sample preparation flux of evaporitic rock class sample is analyzed for X-ray fluorescence spectra |
| CN105699409A (en) * | 2016-02-25 | 2016-06-22 | 山东省第四地质矿产勘查院 | Method for measuring content of barium sulfate in barite through X ray fluorescent glass sheet-melting method |
-
2012
- 2012-12-11 CN CN201210528310.1A patent/CN102944458B/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103344469B (en) * | 2013-07-08 | 2015-12-23 | 洪飞 | The sample preparation flux of evaporitic rock class sample is analyzed for X-ray fluorescence spectra |
| CN105699409A (en) * | 2016-02-25 | 2016-06-22 | 山东省第四地质矿产勘查院 | Method for measuring content of barium sulfate in barite through X ray fluorescent glass sheet-melting method |
| CN105699409B (en) * | 2016-02-25 | 2018-10-12 | 山东省第四地质矿产勘查院 | The method that x-ray fluorescence glass flux sheet method measures barium sulfate content in barite |
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