CN108562691A - The assay method of all iron content in troilite - Google Patents
The assay method of all iron content in troilite Download PDFInfo
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- CN108562691A CN108562691A CN201810461940.9A CN201810461940A CN108562691A CN 108562691 A CN108562691 A CN 108562691A CN 201810461940 A CN201810461940 A CN 201810461940A CN 108562691 A CN108562691 A CN 108562691A
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- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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Abstract
The invention discloses a kind of assay methods of all iron content in troilite.This approach includes the following steps：Pretreatment：Sample is crushed, sample dispersion is heated to, hermetically drying is cooling；Dissolving：First hydrochloric acid low-temperature heat is used to decompose, adds nitric acid and perchloric acid, be heated to solution and be all evaporated, white cigarette completely disappears；Be evaporated it is cooling after add hydrochloric acid and be heated to solid and all dissolve, stannous chloride solution is added dropwise to lysate in light yellow, is heated to lysate boiling and is diluted with water, obtain sample to be tested；Titration and calculating.This method is measured wherein all iron content using chloroazotic acid high chloro acid dissolution troilite, and accuracy is high, and analytical cycle is short, and testing cost is low, adapts to the demand that cost efficiency is detected high sulfide pyrite sample in laboratory.
Description
Technical field
The present invention relates to technical field of chemical detection, more particularly to a kind of assay method of all iron content in troilite.
Background technology
All iron content mostly uses greatly dichromate titration etc. and is measured in iron ore.Troilite is without the common iron ore of the image of Buddha
Stone directly uses hydrochloric acid and fluoride to decompose like that, belongs to " indissoluble " iron ore.The side of all iron content in present analysis sulphur iron ore
Method has the molten sample method of mixture of sulfuric phosphoric acid, alkali fusion and borax to melt sample method.Mixture of sulfuric phosphoric acid method is more demanding to temperature condition, if molten sample temperature
It does not reach requirement, easily generating pyrophosphoric acid consolidation object in container bottom seriously affects measurement result；Alkali fusion need to use corundum earthenware
Crucible, borax, which melts sample method, need to use platinum crucible, and testing cost is higher, and test period is long.Therefore, it is necessary to develop a kind of accurate
Property it is high, analytical cycle is short, the low assay method of testing cost, and the need of cost efficiency are detected to adapt to laboratory to high sulfide pyrite sample
It asks.
Invention content
Based on drawbacks described above, the purpose of the present invention is to provide a kind of assay method of all iron content in troilite, the party
Method use chloroazotic acid-high chloro acid dissolution's troilite after, then use titration measuring all iron content therein, quickly and easily, accuracy height,
Analytical cycle is short, can significantly improve detection efficiency, reduce analysis cost, adapts to laboratory and detects drop originally to high sulfide pyrite sample
The demand of synergy.
Above-mentioned purpose is achieved through the following technical solutions：
The assay method of all iron content, includes the following steps in a kind of troilite：
S1：Sample pretreatment crushes sample, is heated to the dispersion of sample powder, is sealed in drier, is cooled to room
Temperature；
S2：Dissolving first uses hydrochloric acid low-temperature heat to decompose on sample after pretreatment, and nitric acid is then added and perchloric acid continues to add
Heat, heating smoke are all evaporated to liquid, and white cigarette completely disappears, and reheats and dissolves and dilute constant volume, obtains sample to be tested；
S3：Titration, sample to be tested is titrated, and records the volume of consumed standard titration solution；
S4：Calculate all iron content in sample.
In step sl, the sample is content of vanadium ＜ 0.1%, and the troilite of the equal ＜ of content 0.5% of copper, titanium, chromium
Or iron concentrate.
In step sl, the sample is crushed to 100 μm of granularities below, and heating condition is 100 DEG C~110 DEG C heating 2h
~3h.
In step s 2, it specifically includes：
S21：Sample is placed in bottle after weighing pretreatment, and ammonium fluoride solution, hydrochloric acid, slightly boiling 3min~5min is added；
S22：Then nitric acid is added and perchloric acid continues to heat, heating smoke is all evaporated to liquid, and white cigarette completely disappears；
S23：After being evaporated solution cooling, adds hydrochloric acid and be heated to solid and all dissolve, stannous chloride solution is added dropwise to molten
It is in light yellow to solve liquid, is heated to lysate boiling and constant volume is diluted with water, obtain sample to be tested.
In the step s 21, pretreated sample 0.2000g is weighed with the electronic balance of a ten thousandth precision, be placed in
In the necking bottle of 400mL；The ammonium fluoride solution is about 10mL, the hydrochloric acid is 15mL~20mL.
In step S22, the nitric acid is 5mL~6mL, and the perchloric acid is 5mL~6mL.
In step S23, the hydrochloric acid is 10mL~15mL, is diluted with water to about 80mL.
Further include being rinsed with water bottle wall step in step S22.It is heated to white cigarette in addition nitric acid and perchloric acid and emits to bottle
It when high 1/2, removes, bottle wall is rinsed with water after standing 3min~5min.
In step s3, it is titrated using dichromate titration.Specifically include following steps：
5 drop 240g/L~260g/L sodium tungstate solutions will first be added dropwise in sample to be tested obtained by step S2, it is molten with titanium trichloride
Liquid is restored to tungsten blue generation, and blue disappearance is titrated to potassium bichromate standard solution,
Again plus mixture of sulfuric phosphoric acid solution, the volume ratio of mixture of sulfuric phosphoric acid solution is sulfuric acid:Phosphoric acid:Water=15:15:70, dropwise addition 3~
The diphenylamine sulfonic acid sodium salt indicator of 5 drop 2g/L, it is terminal to be titrated to solution in purple with dichromic acid standard titration solution, and record disappears
The volume of expendable weight potassium chromate standard titration solution.
Before step S 4, further include the blank test being carried out at the same time in company with sample.
In step s 4, all iron content is calculated as follows in sample：
Wherein, in formula：C-potassium bichromate standard titration solution concentration, unit mol/L；Sample matter in m-step S2
Amount, unit g；V0- titration blank test solution consumption potassium bichromate standard titration solution volume, unit mL；V-titration
Sample solution consumes potassium bichromate standard titration solution volume, unit mL；Every molal weight of 55.85-iron, unit g/
mol。
Advantageous effect：
The assay method of all iron content contains wherein full iron using chloroazotic acid-high chloro acid dissolution's troilite in troilite of the present invention
Amount is measured, easy to operate, and analyze speed is fast, and detection cycle is short, and accuracy is high.
Sample is first decomposed with hydrochloric acid low-temperature heat, adds nitric acid and perchloric acid heating by the present invention, until solution steams completely
Dry, white cigarette completely disappears, and dissolved dilution is measured after obtaining sample to be tested using dichromate titration, significantly improves detection effect
Rate reduces analysis cost, adapts to the demand that cost efficiency is detected high sulfide pyrite sample in laboratory, has good popularization and application
Foreground.
The parameter and analytical procedure that the present invention selectes are scientific and effective, and sample dissolving is complete, and testing result has good heavy
Existing property and accuracy.
Specific implementation mode
Technical scheme of the present invention is clearly and completely described below in conjunction with embodiment：
Embodiment 1
Detection (the magnetic iron ore 93-40, TFe of all iron content in sulfur-bearing standards for iron ore sample:59.84%, S:2.61%)
Detection reagent：
Sulfuric acid：A concentration of (ρ 1.84g/mL).
Phosphoric acid：A concentration of (ρ 1.69g/mL).
Nitric acid：A concentration of (ρ 1.40g/mL).
Hydrochloric acid：A concentration of (ρ 1.19g/mL).
Perchloric acid：Content is 70%~72%.
Titanium trichloride solution：Titanium trichloride:Hydrochloric acid=1:1.
Ammonium fluoride solution：It weighs 10g ammonium chlorides to be dissolved in 100mL water, shake up.
Stannous chloride solution：10g stannous chlorides 20mL hydrochloric acid is dissolved by heating, 100mL is diluted with water to.
Sodium tungstate solution 250g/L：It weighs 25g sodium tungstates and is dissolved in 95mL water (muddy then filter) and 5mL phosphoric acid (ρ is added
1.69g/mL), it shakes up.
Titanium trichloride solution：Isometric hydrochloric acid will be added in commercially available titanium trichloride, stores in brown bottle and preserve.
Diphenylamine sulfonic acid sodium solution：A concentration of 2g/L.
Sulphur phosphorus mixed acid 15:15:70：150mL sulfuric acid is slowly injected into the 1000mL beakers for filling 700mL water under stiring
In, it is cooling, 150mL phosphoric acid is added, is shaken up.
Standard titration solution：2.4515g is weighed to be cooled in 140 DEG C~150 DEG C dry 2h and in drier in advance
The potassium bichromate (standard reagent) of room temperature is dissolved in water in 250mL beakers, moves into 1000mL volumetric flasks, is diluted with water to
Scale simultaneously shakes up.
Sample detection：
S1, pretreatment：Standard sample (magnetic iron ore 93-40) is heated into 1h~2h under the conditions of 100 DEG C~110 DEG C, is sealed
In drier, it is cooled to room temperature.
S2, sample dissolving：0.2000g samples are weighed with the electronic balance precision of a ten thousandth precision, are placed in 400mL neckings
In bottle, 10mL ammonium fluoride solutions, 15mL hydrochloric acid is added, on electric hot plate after slightly boiling 3min~5min, be added about 5mL nitric acid and
5mL perchloric acid continues to be heated to occur dense white cigarette in bottle, when white cigarette is emitted to bottle height 1/2, removes, after standing 3min~5min,
It is rinsed with water bottle wall, reheats smoke until liquid is all evaporated, white cigarette disappears.15mL hydrochloric acid is added after being evaporated solution cooling,
Be heated to bottom of bottle solid all to dissolve, stannous chloride solution be added dropwise to lysate in light yellow, in slightly boiling 2min on electric hot plate~
3min is diluted with water to about 80mL, obtains sample to be tested.
S3, titration：Sodium tungstate solution 5 is added dropwise in sample to be tested obtained by step S2 to drip, tungsten is restored to titanium trichloride solution
Indigo plant generates, and is titrated to blue disappearance just with potassium bichromate solution, adds 10mL sulphur phosphorus mixed acid solutions, 5 drop diphenylamines sulphurs are added dropwise
Sour sodium indicator, it is terminal to be titrated to solution in stable purple with potassium bichromate standard titration solution, writes down and consumes weight chromium
The volume V of sour potassium standard titration solution.
S31, blank test：Blank test is done in company with sample, records the volume of consumed potassium bichromate standard titration solution
V0For 0.05mL.
S4, content calculation：The calculating of all iron content is as follows：
Wherein, in formula：
C --- potassium bichromate standard titration solution concentration is 0.0500 (mol/L)；
M --- the sample mass in step S2 is 0.2000g；
V0--- titration blank test solution consumption potassium bichromate standard titration solution volume is 0.05mL；
V --- titration sample solution consumes potassium bichromate standard titration solution volume, is 42.88mL；
55.85 --- every molal weight of iron, unit are (g/mol).
Embodiment 2
Detection (the iron ore W-7177, TFe of all iron content in sulfur-bearing standards for iron ore sample:40.61%, S:1.961%)
Detection reagent：With embodiment 1
Sample detection：
Step S1, S2, S3, S31 are the same as embodiment 1.
Step S4, content calculation：
Embodiment 3
Detection (the bloodstone 7011, TFe of all iron content in sulfur-bearing standards for iron ore sample:42.94%, S:0.891%)
Detection reagent：With embodiment 1
Sample detection：
Step S1, S2, S3, S31 are the same as embodiment 1.
Step S4, content calculation：
Embodiment 4
The detection of all iron content and its check experiment in sample containing troilite
(1) Dandong Kuan Dian high sulfide pyrites sample
Detection reagent：With embodiment 1
Sample ore detects：
S1, sample pretreatment：Sample is crushed to 100 μm of granularity, in 100 DEG C~110 DEG C dry 1h~2h, is sealed in
In drier, it is cooled to room temperature.
Step S2, S3, S31 are the same as embodiment 1.
Step S4, content calculation：
(2) check experiment
Sample ore pre-processes：With embodiment 4；
Assay method：According to potassium bichromate titrimetric method in GB/T 2463-2008, it is 57.85% to measure result.
The preci-sion and accuracy of assay method of the present invention is tested
Experimental method：3 troilite standard samples are selected, assay method of the present invention is pressed respectively and carries out all iron content
It measures, and calculates relative standard deviation, experimental result is shown in Table 1.
The preci-sion and accuracy experimental result of 1 detection method of the present invention of table
By above-mentioned experimental result it is found that the measurement result deviation of assay method of the present invention is small, accuracy is high, can meet
Analysis requires, and easy to operate, is easily mastered, is worthy of popularization.
Claims (8)
1. the assay method of all iron content in a kind of troilite, which is characterized in that include the following steps：
S1：Sample pretreatment crushes sample, is heated to the dispersion of sample powder, is sealed in drier, is cooled to room temperature；
S2：Dissolving first uses hydrochloric acid low-temperature heat to decompose on sample after pretreatment, nitric acid then is added and perchloric acid continues to heat,
Heating smoke is all evaporated to liquid, and white cigarette completely disappears, and is reheated and is dissolved and dilute, obtains sample to be tested；
S3：Titration, sample to be tested are titrated, and the volume of consumed standard titration solution is recorded；
S4：Calculate all iron content in sample.
2. the assay method of all iron content in troilite as described in claim 1, which is characterized in that in step sl, described
Sample is content of vanadium ＜ 0.1%, and the troilite or iron concentrate of the equal ＜ of content 0.5% of copper, titanium, chromium.
3. the assay method of all iron content in troilite as claimed in claim 2, which is characterized in that in step sl, described
Sample is crushed to 100 μm of granularities below, and heating condition is 100 DEG C~110 DEG C heating 1h~2h.
4. the assay method of all iron content in troilite as described in claim 1, which is characterized in that in step s 2, specifically
Including：
S21：Sample is placed in bottle after weighing pretreatment, and ammonium fluoride solution, hydrochloric acid, slightly boiling 3min~5min is added；
S22：Then nitric acid is added and perchloric acid continues to heat, heating smoke is all evaporated to liquid, and white cigarette completely disappears；
S23：After being evaporated solution cooling, adds hydrochloric acid and be heated to solid all dissolvings, stannous chloride solution is added dropwise to lysate
In light yellow, it is heated to lysate boiling and is diluted with water, obtain sample to be tested.
5. the assay method of all iron content in troilite as claimed in claim 4, which is characterized in that in the step s 21, weigh
Pretreated sample is 0.2000g, is placed in the necking bottle of 400mL；The ammonium fluoride solution being added is 10mL, the salt
Acid is 15mL~20mL；
In step S22, the nitric acid is 5mL~6mL, and the perchloric acid is 5mL~6mL；
In step S23, the hydrochloric acid is 10mL~15mL, is diluted with water to about 80mL.
6. the assay method of all iron content in troilite as claimed in claim 4, which is characterized in that in step S22, also wrap
Include and be rinsed with water bottle wall step, when nitric acid and perchloric acid is added and is heated to white cigarette and emits to bottle height 1/2, remove, stand 3min~
After 5min, it is rinsed with water bottle wall.
7. the assay method of all iron content in troilite as described in claim 1, which is characterized in that in step s3, use
Dichromate titration titrates.
8. the assay method of all iron content in troilite as claimed in claim 7, which is characterized in that before step S 4, also
It include the blank test being carried out at the same time in company with sample；In step s 4, all iron content is calculated as follows in sample：
Wherein, in formula：C-potassium bichromate standard titration solution concentration, unit mol/L；Sample mass in m-step S2,
Unit is g；V0- titration blank test solution consumption potassium bichromate standard titration solution volume, unit mL；V-titration sample
Solution consumption potassium bichromate standard titration solution volume, unit mL；The molal weight of 55.85-iron, unit g/mol.
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Cited By (5)
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| CN110426391A (en) * | 2019-07-08 | 2019-11-08 | 广州海关技术中心 | The measuring method of all iron content in a kind of iron ore |
| CN111122562A (en) * | 2020-01-21 | 2020-05-08 | 包头钢铁（集团）有限责任公司 | Method for determining TFe content in steel slag magnetic separation powder |
| CN111896418A (en) * | 2020-06-29 | 2020-11-06 | 广东韶钢松山股份有限公司 | Method for measuring sulfur content in ferrosulfur alloy |
| CN113176221A (en) * | 2021-06-08 | 2021-07-27 | 金川镍钴研究设计院有限责任公司 | Method for measuring content of nickel and copper in Lix984 organic phase |
| CN113514602A (en) * | 2021-03-25 | 2021-10-19 | 长沙矿冶研究院有限责任公司 | Method for determining ferrous iron in sulfur-containing minerals |
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| CN113176221A (en) * | 2021-06-08 | 2021-07-27 | 金川镍钴研究设计院有限责任公司 | Method for measuring content of nickel and copper in Lix984 organic phase |
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Application publication date: 20180921 |