CN107121521A - The method for determining fluorine from minerals and chlorinity - Google Patents
The method for determining fluorine from minerals and chlorinity Download PDFInfo
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- CN107121521A CN107121521A CN201710375880.4A CN201710375880A CN107121521A CN 107121521 A CN107121521 A CN 107121521A CN 201710375880 A CN201710375880 A CN 201710375880A CN 107121521 A CN107121521 A CN 107121521A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/96—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation using ion-exchange
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/065—Preparation using different phases to separate parts of sample
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/96—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation using ion-exchange
- G01N2030/965—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation using ion-exchange suppressor columns
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Abstract
The step of method of fluorine from minerals and chlorinity being determined the invention discloses a kind of, including pre-treatment is carried out to mineral sample with pyrohydrolytic method, and the step of with ion-chromatographic determination content of fluoride ion therein and chloride ion content, unlike the prior art：In the step of being handled before being carried out with pyrohydrolytic method to mineral sample, cosolvent is used, described cosolvent is aluminum oxide.Compared with prior art, the present invention in pyrohydrolysis by adding cosolvent so that fluorine, chlorion are kept completely separate out from sample, cause fluorine, chlorion can be washed out and be separated well in elution 10min with reference to follow-up chromatographic condition, fluorine, the content of chlorion and peak area are in good linear relationship in measurement range, and method test limit is respectively 0.11ng/mL (F‑) and 0.24ng/mL (C1‑), recovery of standard addition is 95.0 101.0%, and RSD is respectively less than 2%.
Description
Technical field
The present invention relates to the detection method of specific component content in mineral, and in particular to one kind determines fluorine from minerals and chlorine contains
The method of amount.
Background technology
Fluorine and chlorine are the pollutants received much concern in mineral (mineral products).In smelting process, the comburant of fluorine is with gas
Or the form of aerosol causes fluorine poisoning to human body, chlorine forms the carcinogens such as dioxin in combustion.Fluorine in nature,
The elements such as chlorine are more to be existed in ionic compound form, and only a few exists in the covalent bond form of the silicate containing halogen.
The conventional pre-treating method of detection fluorine from minerals, chlorinity mainly has steam distillation, ultrasonic extraction, alkali fusion, oxygen bomb
Burning and pyrohydrolysis etc..Wherein, oxygen bomb combustion processing sample is fast and convenient, but be used for that coal etc. can burn it is organic
Material；Ultrasonic extraction is only capable of determining soluble chloride；Alkali fusion can induce one a large amount of interference elements；Steam distillation method is in detection process
Need to use sulfuric acid to be distilled, a large amount of SO can be introduced in absorbing liquid4 2-Cause to elute overlong time.Pyrohydrolysis technology is most
Just by Warf (Warf J C, Cline W D, Tevebaugh R D.Pyrohydrolysis in determination of
Fluoride and other halides [J] .Ana1.Chem.1954,26 (2)：342-346.) propose, concrete principle is water
Steam flows through the mixture of sample and catalyst, under the high temperature conditions decomposes sample and halide is converted into halogen acids is dissolved in
In vapor, the detection of halogen in coal, soil and geological sample is had been widely used at present.Pyrohydrolysis sample pretreatment
Method is a more ripe method, and it has the characteristics of high temperature pyrolysis distills with water.At present be mainly used in coal, soil and
The detection of halogen in geological sample.
Fluorine from minerals, chlorine element make fluorine, chlorion be transferred in solution after pre-treatment, generally using potentiometric titration,
Ion selective electrode method or the chromatography of ions are measured, wherein the chromatography of ions because easy to operate, result it is accurate, obtained
It is widely applied.
Existing use pyrohydrolysis pre-treatment coupled ion chromatography determination fluorine from minerals ion and chloride ion content
, there is component to be measured and extract the deficiencies such as incomplete, interference is big, elute time length or test limit is not ideal enough in method.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of method for determining fluorine from minerals and chlorinity.This method is in height
Cosolvent is added in warm water solution so that fluorine, chlorine element are kept completely separate out from sample, is caused with reference to follow-up chromatographic condition
The elution time is short, test limit is low and precision is good.
It is of the present invention to determine the method for fluorine from minerals and chlorinity, including mineral sample is carried out with pyrohydrolytic method
The step of pre-treatment, and the step of with ion-chromatographic determination content of fluoride ion therein and chloride ion content, with existing skill
Unlike art：In the step of being handled before being carried out with pyrohydrolytic method to mineral sample, cosolvent, described hydrotropy have been used
Agent is aluminum oxide.
In the method for the invention, described mineral are usually nonferrous metals ore, can be specifically sulphide ore or oxide ore.
In the method for the invention, using aluminum oxide as cosolvent, not only make fluorine, chlorion complete from mineral sample
Separate, can also effectively reduce influence of the reagent blank to determination of chloride ion result.For the consumption of cosolvent, usually ore deposit
0.5-1.5 times of more than 0.2 times of consumption, more preferably mineral sample weight of thing sample weight, more preferably mineral
0.8-1.2 times of sample weight.After cosolvent is well mixed with mineral sample, then mineral sample surface cover one layer help
Solvent, usually, is covered in the thickness usually 0.5-2mm of the cosolvent on mineral sample surface.Preferable particle size is 50-200 μm
Aluminum oxide be used as cosolvent.
In the method for the invention, the high-temperature water used in the step of carrying out pre-treatment to mineral sample with pyrohydrolytic method
The Nomenclature Composition and Structure of Complexes for solving device is same as the prior art, and absorbent used etc. is with showing when specific hydrolysis temperature, time, hydrolysis
There is technology identical.Can also be that use can realize other alternate devices of existing pyrohydrolysis apparatus function (such as in the step
Automatic fluorine-detector etc.) realize the pre-treatment to mineral sample.In this application, absorbent used during hydrolysis is preferably hydrogen-oxygen
Change sodium water solution, more preferably 8.0g/L sodium hydrate aqueous solution.
In the method for the invention, with ion-chromatographic determination content of fluoride ion therein and chloride ion content step
Various operations are same as the prior art (including chromatographic condition etc.), including drawing fluorine, the calibration curve of chlorine element and passing through
Calibration curve obtains fluorine, the big step of content two of chlorion in mineral sample.But when using following chromatographic conditions, it can obtain more
Few elution advantage such as time and lower test limit, specifically, fluorine ion and chlorion when using the chromatographic condition
Retention time is respectively 5.19min and 8.96min；Described chromatographic condition is：High power capacity IonPactm AS19 anion analysis
Post；AG19 anion guard columns；Column temperature is 30 DEG C；Leacheate is the 0-100mol/L KOH aqueous solution, and elution mode is drenched for gradient
Wash；Elution flow velocity is 1.0mL/min；Sampling volume is 25 μ L.
Compared with prior art, the present invention in pyrohydrolysis by adding cosolvent so that fluorine, chlorion are from sample
In be kept completely separate out, with reference to follow-up chromatographic condition cause elution 10min in fluorine, chlorion can be washed out and carried out very
Good separation, fluorine, the content of chlorion and peak area are in that (coefficient correlation is for good linear relationship in measurement range
0.9999), method test limit is respectively 0.11ng/mL (F-) and 0.24ng/mL (C1-), recovery of standard addition is 95.0-
101.0%, precision (RSD) is respectively less than 2%.
Embodiment
With reference to specific embodiment, the present invention is described in further detail, to more fully understand present disclosure, but
The present invention is not limited to following examples.
Embodiment 1
1.1 key instruments and condition
Dionex ICS-1100 types chromatography of ions (U.S. Thermo Fisher), is equipped with RFC-30 leacheates and occurs automatically
Device, produces the KOH aqueous solution, and gradient elution (sees below table 1)；The chromatographic work stations of Chromeleon 7.0, ECD-1 Conductivity detections
Device；AS-DV automatic samplers；AERS 500 (4mm) anion cyclic regeneration suppressor；0.22 μm of composite fibre resin micropore filter
Film (German CNW companies)；Milli-Q ultra-pure waters all-in-one (Millipore companies of the U.S.).Experimental water is Milli-Q pure water
Ultra-pure water prepared by system (resistivity is 18.25MQcm).
Chromatographic condition：High power capacity IonPactm AS19 anion analysis posts (4 × 250mm)；AG19 anion guard columns
(4m×50mm)；Post case temperature is 30 DEG C；Suppressor electric current is 112mA；Elution flow velocity is 1.0mL/min；Sampling volume is
25μL；With peak area quantification.
The automatic fluorine-detectors of 5E-FL2200 (Chinese Katyuan instrument company).
Then all glasswares use water using being preceding both needed to soak 4h respectively with 2mol/L sodium hydroxide solutions and water successively
Rinse 3-4 times, dry standby.
Table 1：KOH leacheate gradients
| Time (min) | KOH eluent concentrations (mmol/L) |
| 0 | 10 |
| 8 | 10 |
| 8.1 | 45 |
| 16 | 45 |
| 20 | 10 |
1.2 reagent material
Aluminum oxide：Analyze pure, granularity (150-200 μm)；
Sodium hydroxide solution：8.0g/L, weighs 8g top pure grade sodium hydroxides and is dissolved in 1000mL water.
Sulfuric acid solution：Measure 200mL top pure grades sulfuric acid (ρ 1.84g/mL) to be poured slowly into 100mL water, mix.
Fluorine Standard Stock solutions, 1.00mg/mL：Weigh sodium fluoride primary standard substances of the 2.2110g in 105-110 DEG C of dry 2h
Matter, is dissolved with water, is moved into 1000mL volumetric flasks, is diluted with water to scale, shakes up.
Chlorine Standard Stock solutions, 1.00mg/mL：The advance calcinations at 500-600 DEG C of 1.6485g are weighed to the chlorination of constant
Sodium primary standard substance, is dissolved with water, in the volumetric flask for moving into 1000mL, is diluted with water to scale, is shaken up.
1.3 experimental method
0.5g (being accurate to 0.0001g) predrying mineral sample is weighed, is placed in 10mL porcelain boats, 0.5g aluminum oxide is added,
It is careful well mixed, then with about 0.5g aluminum oxide beddings above.Sample is put into automatic fluorine-detector sample box, works as vapor
When generating means temperature rises to 50 DEG C, sample is pushed into combustion tube.Sample decomposes the condition as described in table 2 and carried out.In test solution
10.0mL sodium hydroxide solutions (8.0g/L) are added in receiver, the F for failing to condense in time is absorbed-、C1-.Test solution collects about 70mL
When stop receive.Test solution is transferred in 100mL volumetric flasks completely, scale is diluted to, mixed.By blank solution and sample solution
With 0.22 μm of membrane filtration, according to ion chromatography condition, F in test solution is determined-、C1-Content.
Table 2：Sample decomposition condition
2. discussion of results
2.1 sample treatment
Silica, calcium oxide and aluminum oxide are selected using copper concentrate certified reference material GSB04-2710-2011 respectively
As cosolvent, test according to the method described above, while being not added with the experiment of cosolvent.
As a result show, when being not added with cosolvent and being cosolvent from calcium oxide, certified reference material measurement result is remote
Less than nominal value；During from silica and aluminum oxide for cosolvent, sample measurement result is consistent with sample asserting value.
Blank test result shows, F in cosolvent silica-、C1-Measurement result be respectively：0.0106%th,
0.0056%；F in cosolvent aluminum oxide-、C1-Measurement result be respectively：0.0121% and 0.0015%.Due in mineral products
C1-Content is relatively low, to reduce reagent blank to C1-The influence of assay result, experiment is determined using aluminum oxide as cosolvent.
The selection of 2.2 chromatography of ions conditions
Pyrohydrolytic method handles mineral products sample, except can be by F-、C1-Separated with sample ore matrix, the sulphur in sulphide ore can also be produced
Raw substantial amounts of SO4 2-.Due to SO4 2-With F-、C1-Retention time difference is big, is ensureing F-、C1-Efficiently separate, again can be by SO4 2-Deng
The longer ion of retention time is eluted in the short time, the gradient elution of this experimental selection.Experiment is automatic using RFC-30 leacheates
Generator can on-line automatic generation 0.1-100mmol/l gradient concentration KOH solutions.Under the elution gradient condition of experimental selection,
F-、C1-Retention time be respectively：5.19min(F-) and 8.96min (C1-)。
2.3 linear equations and Monitoring lower-cut
By diluting the F that configuration concentration is respectively 0.00,0.50,1.00,2.00,5.00,10.00 μ g/mL step by step-、C1-
Series standard solution, be with chromatographic peak area fitted calibration curve according to concentration：
Fluorine y=0.5013x+0.0267 (R2=0.9999)；
Chlorine y=0.3108x-0.0077 (R2=0.9999).
With 3 times of signal-to-noise ratio computation F-The detection of ion is limited to 0.11ng/mL, C1-The detection of ion is limited to 0.24ng/mL.Phase
For detection F-、C1-Conventional ion selective electrode method, the sensitivity of this method improves about 1000 times.
The experiment of 2.4 rate of recovery, Comparability test and actual sample test
Mark-on reclaims experiment is carried out to polymetallic ore sample according to test method, certified reference material is measured, and
Contrasted with asserting value, the results are shown in Table 3.
Table 3：The rate of recovery is tested and actual sample analysis result
Claims (6)
1. the step of determining the method for fluorine from minerals and chlorinity, including pre-treatment carried out to mineral sample with pyrohydrolytic method,
And the step of with ion-chromatographic determination content of fluoride ion therein and chloride ion content, it is characterised in that：With high-temperature water
In the step of solution carries out pre-treatment to mineral sample, cosolvent is used, described cosolvent is aluminum oxide.
2. according to the method described in claim 1, it is characterised in that：Described mineral are nonferrous metals ore.
3. according to the method described in claim 1, it is characterised in that：Described mineral are sulphide ore or oxide ore.
4. the method according to any one of claim 1-3, it is characterised in that：The consumption of the cosolvent is mineral sample
More than 0.2 times of weight.
5. the method according to any one of claim 1-3, it is characterised in that：The consumption of the cosolvent is mineral sample
0.5-1.5 times of weight.
6. the method according to any one of claim 1-3, it is characterised in that：With ion-chromatographic determination fluorine therein
In the step of ion concentration and chloride ion content, when using following chromatographic conditions, the retention time point of fluorine ion and chlorion
Wei not 5.19min and 8.96min；
Chromatographic condition：High power capacity IonPactm AS19 anion analysis posts；AG19 anion guard columns；Column temperature is 30 DEG C；Elution
Liquid is the 0-100mol/L KOH aqueous solution, and elution mode is gradient elution；Elution flow velocity is 1.0mL/min；Sampling volume is
25μL。
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108663405A (en) * | 2018-06-19 | 2018-10-16 | 湖南师范大学 | A kind of Oxygen Bomb Combustion quickly measures the detection method of chlorine content in coal |
| CN108802156A (en) * | 2018-06-13 | 2018-11-13 | 沈阳工程学院 | Measure the assay method of content of iodine in coal |
| CN109060976A (en) * | 2018-07-09 | 2018-12-21 | 德山化工（浙江）有限公司 | Chlorine ion concentration measuring method in silica |
| CN110231430A (en) * | 2019-05-20 | 2019-09-13 | 中国船舶重工集团公司第七二五研究所 | A kind of ion chromatographic method for chloride content determination in titanium sponge |
| CN110726790A (en) * | 2019-11-27 | 2020-01-24 | 九江天赐高新材料有限公司 | Method for measuring chloride ions in fluorine-containing lithium salt |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108802156A (en) * | 2018-06-13 | 2018-11-13 | 沈阳工程学院 | Measure the assay method of content of iodine in coal |
| CN108663405A (en) * | 2018-06-19 | 2018-10-16 | 湖南师范大学 | A kind of Oxygen Bomb Combustion quickly measures the detection method of chlorine content in coal |
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| CN109060976B (en) * | 2018-07-09 | 2021-04-30 | 德山化工（浙江）有限公司 | Method for measuring chloride ion concentration in silicon dioxide |
| CN110231430A (en) * | 2019-05-20 | 2019-09-13 | 中国船舶重工集团公司第七二五研究所 | A kind of ion chromatographic method for chloride content determination in titanium sponge |
| CN110726790A (en) * | 2019-11-27 | 2020-01-24 | 九江天赐高新材料有限公司 | Method for measuring chloride ions in fluorine-containing lithium salt |
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Application publication date: 20170901 |