CN106124486A - A kind of assay method of stannum in ore deposit, Huang gang - Google Patents
A kind of assay method of stannum in ore deposit, Huang gang Download PDFInfo
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- CN106124486A CN106124486A CN201610712616.0A CN201610712616A CN106124486A CN 106124486 A CN106124486 A CN 106124486A CN 201610712616 A CN201610712616 A CN 201610712616A CN 106124486 A CN106124486 A CN 106124486A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
A kind of assay method of stannum in ore deposit, Huang gang, comprise the following steps: Huang gang sample ore product are added sodium peroxide and melt by (1), it is cooled to room temperature, it is subsequently adding 60～80 DEG C and extracts sample, be subsequently added into liquid at the bottom of 60% ferrum, dropping hydrochloric acid acidifying, it is configured to stanniferous standard solution series 0%, 0.025%, 0.050%, 0.10%, 0.20%, 0.50%, it is diluted with water to scale, shakes up, stand；Draw the standard curve of stanniferous standard solution series；(2) Huang gang sample ore product are added sodium peroxide to melt, it is cooled to room temperature, adds 60～80 DEG C and extract sample, dropping hydrochloric acid acidifying, move in volumetric flask, it is diluted with water to scale, shakes up, stand, solution is introduced ICP light source, with reagent blank as reference, it is analyzed according to ICP AES spectral analysis procedure, measures the content of stannum.The present invention has that detection limit is low, precision good, spectral interference is little, easily and fast, accurately, the advantage such as energy-conserving and environment-protective, labor productivity can be increased substantially.
Description
Technical field
A kind of assay method of stannum in ore deposit, Huang gang of the present invention, is specifically related to one and utilizes inductively coupled plasma former
In ore deposit, Huang gang, sub-emission spectrographic determination Inner Mongol, the mensuration of stannum analyzes method.
Background technology
Huang gang tin-iron mine bed is the large-scale polymetallic deposit that in In The South Segment of The Daxinganling polymetallic area is important, for
The Tin-polymetallic Deposits that China's North of Yangtze River is maximum, is also the second largest iron mine in Inner Mongolia Autonomous Region.Verify this mineral deposit ferrum, stannum
Reserves are large-scale, and in ore deposit, Huang gang, the content of stannum is higher than general iron ore.
At present, measure the classical chemical analysis method complex operation of stannum in iron ore, cycle length, by some interference factors
With the impact of condition, result is the most satisfied.Such as Li Haiming, Yang Shaobin, Hg-afs Determination iron mine
Trace tin in stone, " spectrographic laboratory " the 2nd phase of volume 22, in March, 2005, uses hydride generation-atomic fluorescence spectrometric method to survey
Determining trace tin in iron ore, the method complex operation, cycle are long, and the method is only applicable to the mensuration of trace tin in iron ore.
Dong Youming, the mensuration of trace tin in iron ore, " Heilungkiang metallurgical " the 4th phase in 1997, use with CTAB as solubilizing agent, phenylfluorone
For trace tin in the spectrphotometric method for measuring iron ore of developer and dressing product thereof, the method instrument is 721 type spectrophotometrics
Meter, is the traditional chemical analysis method of a kind of comparison, operating process length, highly professional, be difficult to grasp.Li Weishu, remaining Xiao Fang,
In iron ore, the X fluorescence spectrum of stannum measures, " metallurgical collection " the 1st phase in 1998, uses X fluorescence spectrum method to measure stannum in Ore
Content, needs a set of applicable standard sample, and the standards for iron ore sample that can have bought seldom can provide the standard value of stannum amount,
The standard sample simultaneously making a set of applicable X-fluorescence is relatively difficult.Therefore, exploitation is a kind of simple to operate, and the detection cycle is short, is subject to
It is significant that what the impact of interference factor and condition was little measures the method for stannum in ore deposit, Huang gang.
It addition, Zhao Yu, Theil indices study on determination method in cassiterite, the method uses zinc powder-Borax-boric acid dissolved samples,
Utilizing ICP-AES to measure the content of stannum, be easily caused sample and be completely dissolved, add molten sample amount of medicament greatly, cost is high.
Summary of the invention
The technical problem to be solved be to provide a kind of in ore deposit, Huang gang stannum to have detection limit low, accurate
Spend, light disturbs little, quick, accurate, practical assay method.
The present invention solves its technical problem and employed technical scheme comprise that, a kind of assay method of stannum in ore deposit, Huang gang, bag
Include following steps:
(1) drafting of standard curve: spectroscopic pure tin reagent is added sodium peroxide and melts, be cooled to room temperature, be subsequently adding
60～80 DEG C are extracted sample, are subsequently added into liquid at the bottom of 60% ferrum, and dropping hydrochloric acid acidifying makes bronzing ferric hydroxide precipitate all dissolve
Present the settled solution of yellow, be configured to stanniferous standard solution series 0%, 0.025%, 0.050%, 0.10%, 0.20%,
0.50%, it is diluted with water to scale, shakes up, stand；Then stanniferous standard solution series is utilized to prepare curve, finally with tin element
Concentration is abscissa, and emissive porwer is that vertical coordinate draws series standard curve；(2) sample determination: Huang gang sample ore product were added
Sodium oxide melts, and is cooled to room temperature, adds 60～80 DEG C and extracts sample, and dropping hydrochloric acid acidifying makes bronzing ferric hydroxide precipitate complete
The settled solution presenting yellow is dissolved in portion, moves in volumetric flask, is diluted with water to scale, shakes up, and stands, solution is introduced ICP
Light source, with reagent blank as reference, is analyzed according to ICP-AES spectral analysis procedure, measures the content of stannum.
Further, the described assay method of stannum in ore deposit, Huang gang, comprise the following steps:
(1) drafting of standard curve: add sodium peroxide 3g in the corundum crucible adding spectroscopic pure tin reagent in 700 DEG C
Muffle furnace melts 10 minutes, after being cooled to room temperature, is subsequently placed in 250mL beaker 70 DEG C of 100mL of addition and sample is extracted, in
Adding liquid at the bottom of 10mL60% ferrum in 250mL beaker, dropping hydrochloric acid acidifying makes bronzing ferric hydroxide precipitate all dissolve to present Huang
The settled solution of color, moves in 250mL volumetric flask, be then configured to stanniferous standard solution series 0%, 0.025%, 0.050%,
0.10%, 0.20%, 0.50%, it is diluted with water to scale, shakes up, stand；Then by 1000 μ g/mL stannum mark liquid through the dilutest
Releasing to 10 μ g/mL, with tin element concentration as abscissa, emissive porwer is that vertical coordinate draws series standard curve；
(2) drafting of working curve: weigh 0.1000g Huang gang sample ore product in corundum crucible, add 3g sodium peroxide in
700 DEG C of Muffle furnaces melt 10～15 minutes, after being cooled to room temperature, is placed in 250mL beaker 70 DEG C of 100mL of addition by sample
Extracting, dropping hydrochloric acid acidifying makes bronzing ferric hydroxide precipitate all dissolve the settled solution presenting yellow, moves into 250mL capacity
In Ping, it is diluted with water to scale, shakes up, stand, solution is introduced ICP light source, with reagent blank as reference, according to ICP-AES
Spectral analysis procedure is analyzed, and measures the content of stannum.
The present invention uses inductively-coupled plasma spectrometer to measure Huang gang sample ore product, substantially reduces compared to chemical method
Operating process, shortens minute, improves production efficiency；Detection limit is low, precision good, light interference is little；Measurement result is steady
Fixed, accurate, quick, practical.Simultaneously compared to classical chemical method, greatly reduce the use of medicine, saved material one-tenth
This, and use standard solution preparation standard working curve, stannum standard solution is easily bought；Production efficiency is high, can be labor-saving
Expenditure；Method is simple, and operator are prone to grasp, and can detect the Inner Mongol Huang Gangkuang that Theil indices is higher, and measurement error is marked in country
In the tolerance of quasi-regulation, alternative complex analysis method in routine analysis.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is illustrated further.
One, key instrument and reagent
ICP plasma emission spectrometer (5300DV type, PE company of the U.S. produces)
Sodium peroxide；Sn standard solution 1000 μ g/mL；Hydrochloric acid.
Two, instrument and running parameter
ICP-AES: PE company of the U.S. produces, and direct-reading plasma-speetrometer composed entirely by OPTIMA5300DV Bidirectional observation type, Gu
Detector (CCD), wave-length coverage 190～780nm, echelle grating, gem decussation nebulizer, SCOTTON fog chamber, high
Rotary spray chamber during content, winXP computer operating system, Winlab32 software, running parameter is shown in Table 1.The mensuration wavelength of stannum
For: 189.927nm.
Table 1-ICP-AES instrument operating condition parameters table
| Parameter | Higher frequency | Power | Cooling gas flow | Secondary air amount | Carrier gas flux | Solution elevating amount |
| Numerical value | 40.68MHZ | 1300W | 15L/min | 0.2L/min | 0.8L/min | 1.5mL/min |
| Parameter | Washing time | Prespark period | The time of integration | Reading time delay | Observed altitude | Observed pattern |
| Numerical value | 8s | 45s | 2～10s is automatic | 30s | 15mm | Axially or radially |
Embodiment 1
1, the drafting of standard curve
In corundum crucible, add sodium peroxide 3g in 700 DEG C of Muffle furnaces, melt 10 minutes, after being cooled to room temperature, then
It is placed in 250mL beaker 70 DEG C of 100mL of addition to be extracted by sample, in 250mL beaker, adds liquid at the bottom of 10mL 60% ferrum, dropping
Hydrochloric acid (1+1) is acidified, and moves in 250mL volumetric flask, be then configured to stanniferous standard solution series 0%, 0.025%,
0.050%, 0.10%, 0.20%, 0.50%, it is diluted with water to scale, shakes up, stand；Then by 1000 μ g/mL stannum mark liquid warps
Cross stepwise dilution to 10 μ g/mL, pipette mark liquid preparation curve by table 2；The instrument working condition finally set according to table 1 treats instrument
With concentration of element as abscissa after Wen Ding, emissive porwer is that vertical coordinate draws series of tasks curve, and its standard curve is linearly good,
The correlation coefficient of element is more than 0.999.
Table 2-utilizes stannum standard solution series to prepare standard curve
| Label | Stannum mark liquid | Theil indices % |
| Blank | 0ml | 0.00 |
| Standard curve 1 | 2.5ml(10μg/mL) | 0.025 |
| Standard curve 2 | 5ml(10μg/mL) | 0.050 |
| Standard curve 3 | 10ml(10μg/mL) | 0.10 |
| Standard curve 4 | 20ml(10μg/mL) | 0.20 |
| Standard curve 5 | 50ml(10μg/mL) | 0.50 |
2, sample determination
Weigh 0.1000g sample in corundum crucible, add sodium peroxide 3g and melt 10～15 points in 700 DEG C of Muffle furnaces
Clock, after being cooled to room temperature, is placed in 250mL beaker 70 DEG C of 100mL of addition and is extracted by sample, and dropping hydrochloric acid (1+1) acidifying moves into
In 250mL volumetric flask, it is diluted with water to scale, shakes up, stand；Solution is introduced ICP light source, with reagent blank as reference, presses
It is analyzed according to Instrumental Analysis program, measures the content of stannum.
3, result and discussion
(1) accuracy and precision
In order to verify the accuracy of embodiment 1 method, select standard sample that 1 Theil indices is higher and three produce
Huang gang sample ore product are tested, and compare with Atomic Fluorescence Spectrometry definite value and standard value with the measured value of embodiment 1, are shown in Table 3.
Table 3-accuracy
Table 4-tolerance
From table 3,4, measurement error is the least, in the range of error that national standard allows, can fully meet mensuration and want
Ask.
Same sample is carried out continuously 10 measurements, has carried out validation instrument short-term precision, as shown in table 5.
Table 5-instrument precision
As shown in Table 5, the good stability of the general line of selected analysis, illustrate that the unit in embodiment 1 method is have very well by instrument
Analysis precision.
The experiment of embodiment 1 method precision uses same sample to carry out 5 parallel molten samples, carries out on same calibration curve
Measuring, carry out the repeatability of verification method, result is as shown in table 6.
Table 6-precision
As shown in Table 6, under the operation of not homogeneous, the collimation of result is fine, illustrates to use embodiment 1 molten sample effect very
Good.
Claims (2)
1. the assay method of stannum in ore deposit, Huang gang, it is characterised in that comprise the following steps: the drafting of (1) standard curve:
Spectroscopic pure tin reagent is added sodium peroxide melt, be cooled to room temperature, be subsequently adding 60～80 DEG C and extract sample, be subsequently added into
Liquid at the bottom of 60% ferrum, dropping hydrochloric acid acidifying makes bronzing ferric hydroxide precipitate all dissolve the settled solution presenting yellow, is configured to
Stanniferous standard solution series 0%, 0.025%, 0.050%, 0.10%, 0.20%, 0.50%, is diluted with water to scale, shakes up,
Stand；Then utilizing stanniferous standard solution series to prepare curve, finally with tin element concentration as abscissa, emissive porwer is sat for vertical
Mark and draw series standard curve processed；(2) sample determination: Huang gang sample ore product are added sodium peroxide and melts, be cooled to room temperature, add 60
～80 DEG C of extraction samples, dropping hydrochloric acid acidifying makes bronzing ferric hydroxide precipitate all dissolve the settled solution presenting yellow, moves
Enter in volumetric flask, be diluted with water to scale, shake up, stand, solution is introduced ICP light source, with reagent blank as reference, according to
ICP-AES spectral analysis procedure is analyzed, and measures the content of stannum.
The assay method of stannum in ore deposit, Huang gang the most according to claim 1, it is characterised in that comprise the following steps:
(1) drafting of standard curve: add sodium peroxide 3g in the corundum crucible adding spectroscopic pure tin reagent in 700 DEG C of Muffles
Stove melts 10 minutes, after being cooled to room temperature, is subsequently placed in 250mL beaker 70 DEG C of 100mL of addition and sample is extracted, in
Adding liquid at the bottom of 10mL60% ferrum in 250mL beaker, dropping hydrochloric acid acidifying makes bronzing ferric hydroxide precipitate all dissolve to present Huang
The settled solution of color, moves in 250mL volumetric flask, be then configured to stanniferous standard solution series 0%, 0.025%, 0.050%,
0.10%, 0.20%, 0.50%, it is diluted with water to scale, shakes up, stand；Then by 1000 μ g/mL stannum mark liquid through the dilutest
Releasing to 10 μ g/mL, with tin element concentration as abscissa, emissive porwer is that vertical coordinate draws series standard curve；
(2) drafting of working curve: weigh 0.1000g Huang gang sample ore product in corundum crucible, adds 3g sodium peroxide in 700 DEG C
Muffle furnace melts 10～15 minutes, after being cooled to room temperature, is placed in 250mL beaker 70 DEG C of 100mL of addition and sample is extracted, drip
Adding hydrochloric acid acidifying makes bronzing ferric hydroxide precipitate all dissolve the settled solution presenting yellow, moves in 250mL volumetric flask, uses
Water is diluted to scale, shakes up, and stands, solution introduces ICP light source, with reagent blank as reference, according to ICP-AES spectrum analysis
Program is analyzed, and measures the content of stannum.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106706533A (en) * | 2016-12-30 | 2017-05-24 | 杭州谱育科技发展有限公司 | Sample intelligent analysis method |
| CN113358735A (en) * | 2021-06-02 | 2021-09-07 | 河北省地质实验测试中心(国土资源部保定矿产资源监督检测中心、河北省金银宝玉饰品质量监督检验站) | Method for decomposing cassiterite-containing mineral suitable for measuring tin content and application thereof |
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| CN104807808A (en) * | 2015-05-11 | 2015-07-29 | 梧州市产品质量检验所 | Method for detecting tin in ore |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104807808A (en) * | 2015-05-11 | 2015-07-29 | 梧州市产品质量检验所 | Method for detecting tin in ore |
Non-Patent Citations (2)
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| 王法春: "锡矿中锡的测定分析研究", 《中国石油和化工标准与质量》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106706533A (en) * | 2016-12-30 | 2017-05-24 | 杭州谱育科技发展有限公司 | Sample intelligent analysis method |
| CN106706533B (en) * | 2016-12-30 | 2019-11-01 | 杭州谱育科技发展有限公司 | Sample intelligent analysis method |
| CN113358735A (en) * | 2021-06-02 | 2021-09-07 | 河北省地质实验测试中心(国土资源部保定矿产资源监督检测中心、河北省金银宝玉饰品质量监督检验站) | Method for decomposing cassiterite-containing mineral suitable for measuring tin content and application thereof |
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