CN102183574A - Method for determining chloride ions in chrome ore - Google Patents
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Abstract
The invention discloses a method for determining chloride ions in a chrome ore, which belongs to the technical field of determining the content of chloride ions in the chrome ore. In the method, a chrome ore sample is dissolved by a sulfur-phosphor mixed acid, so that a solution to be determined is prevented from generating Cr6+; loss of the chloride ions is prevented by dissolving the chrome ore sample with a capped closed container; influence of coexistence elements on the determination result of the chrome ore solution to be determined is reduced by adding a total ionic strength adjustment buffer (TISAB), and the content of the chloride ions can be accurately determined by an ion selective electrode method.
Description
Technical field
The present invention relates to a kind of method of measuring chloride ion content in the chrome ore, belong to the technical field of measuring trace chlorine content in the chrome ore.
Background technology
Chrome ore is important large resource mineral products, at metallurgical industry, chemical industry and refractory industry purposes is widely arranged.Because chrome ore belongs to short resource in China, the import chrome ore becomes the main source that satisfies the smelting demand.Annual consumption figure 80% left and right sides dependence on import, therefore China becomes one of main body entrance big country of global chrome ore.
Chlorine is the harmful element that produces in the metallic ore smelting process, not only can corrosion pipeline equipment, influence product quality, but and contaminated environment, environmentally safe and people ' s health threatens.Along with a large amount of imports of chrome ore, its potential hazard is also increasing, and therefore must carry out quality control to the import chrome ore.There is not methods of chlorine ions in the chrome ore at present.
Analyze reason and mainly contain 2 points:
1, sample pre-treatments difficulty: the chrome ore chemical composition is (Mg, Fe) Cr2O4, the composition more complicated, its chemical general formula: (Mg2+, Fe2+) (Cr3+, AI 3+, Fe3+) 2O4 or (Mg2+, Fe2+) O(Cr, Al, Fe3+) 2O3, its Cr2O3 content is 30 %～57 %, is the magnesium aluminate spinel mineral of indissoluble.
Magnesia-alumina spinel structure at normal temperatures and pressures down, is difficult to dissolving.Sour sample dissolution under the condition of high temperature, chlorion and hydrogen ion easily generate hydrogen chloride gas and volatilize, and cause the chlorion loss; Alkali fusion sample under the condition of high temperature, a large amount of alkali fusion agent meetings of adding are with Cr
3+Be oxidized to Cr
6+, disturb determination of chloride ion, the mensuration blank value is increased, be unfavorable for trace chlorine mensuration.
2, silver nitrate potentiometric titration and turbidimetry can not be used for measuring the chrome ore trace chlorine: chromate ion and silver ion generate the siliver chromate precipitation, disturb the judgement of silver nitrate potentiometric determination chlorion titration end-point; Chrome ore solution itself has color, can not measure chlorion with silver nitrate turbidimetry method.
In view of above-mentioned analysis, the method difficult point of measuring chloride ion content in the chrome ore is how to extract trace chlorine in the chrome ore, how to eliminate hexavalent chromium in the solution to be measured, how to reduce the influence of coexistence elements to the chlorine measurement result.
Summary of the invention
The object of the present invention is to provide a kind of method that can accurately measure trace chlorine content in the chrome ore.
For achieving the above object, mainly may further comprise the steps:
A kind of method of measuring chlorion in the chrome ore, it may further comprise the steps:
(1) produces the analytic sample of chrome ore: adopt muller to produce certain detailed catalogue chrome ore analytic sample;
(2) take by weighing quantity of sample: accurately take by weighing a certain amount of chrome ore analytic sample, be put in the micro-wave digestion jar;
(3) add a certain amount of acid: after using low amounts of water moistening, add a certain amount of sulphur-phosphorus nitration mixture, shake up, covered and enclosed is put into the micro-wave digestion stove;
(4) micro-wave digestion program setting:, determine micro-wave digestion power, digestion time and digestion condition according to sample weighting amount and micro-wave digestion jar number;
(5) chrome ore solution to be measured is prepared: treat that micro-wave digestion stops, after the cooling of micro-wave digestion jar, take out, add total ionic strength adjustment buffer degree correctives (TISAB), regulate chrome ore pH value of solution value to be measured, treat that test solution is cooled to room temperature after, constant volume is in the volumetric flask of certain volume, do filtration with fine and close filter paper, discard initial filtrate, preservation filtrate is to be determined;
(6) chrome ore matrix solution preparation: choose a certain amount of chrome ore analytic sample, add sulphur-phosphorus nitration mixture, heating for dissolving number minute on electric hot plate makes the chlorion of dissolving generate the hydrogen chloride gas volatilization, preparation chrome ore matrix solution;
(7) drafting of preparation of chlorion standard solution and typical curve: the chlorion standard solution of preparation variable concentrations, the content of the chrome ore matrix solution in the chlorion standard solution, sulphur-phosphorus nitration mixture, total ionic strength adjustment buffer degree correctives (TISAB) is identical with content in the chrome ore solution to be measured, regulate chlorion standard solution pH, constant volume is drawn the chlorion typical curve in the volumetric flask of certain volume;
(8) measure chloride ion content: measure with ion selective electrode method,, calculate the content of chlorion in the chrome ore solution to be measured by the chlorion typical curve.
When measuring according to described step (8), the chlorion standard solution and the chrome ore solution to be measured of variable concentrations are injected dry beaker respectively, add magnetic stir bar, beaker is put on the magnetic stirring apparatus, with the constant speed agitating solution, press chlorine ion concentration order sequentially determining chlorion standard solution and chrome ore solution to be measured from low to high, and read stable potential value by the same fixing response time;
With the potential value is ordinate, and the negative logarithm of chlorine ion concentration is a horizontal ordinate, and the drawing standard curve by the typical curve linear equation, calculates chloride ion content in the chrome ore solution to be measured by following formula:
In the formula:
W---the massfraction of chrome ore solution chlorion to be measured, %;
C---the concentration of chlorion from the chrome ore solution to be measured that typical curve checks in, μ g/mL;
V---the volume of chrome ore solution to be measured, mL;
The quality of m---chrome ore to be measured, g.
The detailed catalogue of described chrome ore analytic sample requires≤75 um.
Described chrome ore solution to be measured, chlorion standard solution pH value of solution are to adopt sodium hydroxide solution to regulate, and the pH value of solution value is adjusted to 2～5.
Described total ionic strength adjustment buffer degree correctives (TISAB) adopts sodium citrate-potassium nitrate.
The ratio of sulfuric acid, phosphorus nitration mixture is 1:1 in described sulphur-phosphorus nitration mixture.
The chrome ore analytic sample that described step (2) takes by weighing is 0.5g～1.0g.
Sulphur-phosphorus nitration mixture that described step (3) adds is 10 mL～15 mL.
Beneficial effect of the present invention:, can guarantee not produce in the solution to be measured Cr with sulphur-phosphorus nitration mixture dissolve chromium sample ore product
6+Adopt covered and enclosed container dissolve chromium sample ore product to guarantee not loss of chlorion, the adding of total ionic strength adjustment buffer degree correctives (TISAB) has reduced the influence of coexistence elements to chrome ore measured in solution result to be measured, adopts ion selective electrode method can accurately measure chloride ion content.
Embodiment
A kind of method of measuring chlorion in the chrome ore, it may further comprise the steps:
(1) produce the analytic sample of chrome ore: adopt muller to produce certain detailed catalogue chrome ore analytic sample, the detailed catalogue of analytic sample requires≤75 um;
(2) take by weighing quantity of sample: accurately take by weighing the chrome ore analytic sample of 0.5g～1.0g, be put in the micro-wave digestion jar;
(3) add a certain amount of acid: after using low amounts of water moistening, add sulphur-phosphorus nitration mixture of 10 mL～15 mL, shake up, covered and enclosed is put into the micro-wave digestion stove;
(4) micro-wave digestion program setting:, determine micro-wave digestion power, digestion time and digestion condition according to sample weighting amount and micro-wave digestion jar number;
(5) chrome ore solution to be measured is prepared: treat that micro-wave digestion stops, after the cooling of micro-wave digestion jar, take out, add total ionic strength adjustment buffer degree correctives (TISAB), transfer the pH value of chrome ore solution to be measured to transfer to 2～5, treat that test solution is cooled to room temperature after, constant volume is in the volumetric flask of certain volume, do filtration with fine and close filter paper, discard initial filtrate, preservation filtrate is to be determined;
(6) chrome ore matrix solution preparation: choose a certain amount of chrome ore analytic sample, add sulphur-phosphorus nitration mixture, heating for dissolving number minute on electric hot plate makes the chlorion of dissolving generate the hydrogen chloride gas volatilization, preparation chrome ore matrix solution;
(7) drafting of preparation of chlorion standard solution and typical curve: the chlorion standard solution of preparation variable concentrations, the content of the chrome ore matrix solution in the chlorion standard solution, sulphur-phosphorus nitration mixture, total ionic strength adjustment buffer degree correctives (TISAB) is identical with content in the chrome ore solution to be measured, transferring the pH value of chlorion standard solution is 2～5, constant volume is drawn the chlorion typical curve in the volumetric flask of certain volume;
(8) measure chloride ion content: measure with ion selective electrode method,, calculate the content of chlorion in the chrome ore solution to be measured by the chlorion typical curve.
During measurement, the standard solution and the solution to be measured of variable concentrations are injected dry beaker respectively, add magnetic stir bar, beaker is put on the magnetic stirring apparatus, with the constant speed agitating solution, press chlorine ion concentration order sequentially determining chlorion standard solution and chrome ore solution to be measured from low to high, all test solutions should read stable potential value by the same fixing response time; Response time is 3 min to 5 min.
With the potential value is ordinate, and the negative logarithm of chlorine ion concentration is a horizontal ordinate, and the drawing standard curve by the typical curve linear equation, calculates chloride ion content in the chrome ore solution to be measured by following formula.
In the formula:
W---the massfraction of chrome ore solution chlorion to be measured, %;
C---the concentration of chlorion from the chrome ore solution to be measured that typical curve checks in, μ g/mL;
V---the volume of chrome ore solution to be measured, mL;
The quality of m---chrome ore to be measured, g.
The selection of a pair of sample detailed catalogue of embodiment
The chrome ore chemical composition is (Mg, Fe) Cr2O4, composition more complicated, magnesium aluminate spinel mineral for indissoluble, chrome ore sample to be measured is ground to certain detailed catalogue, during the detailed catalogue of chrome ore analytic sample≤75 um, can guarantees the dissolving to greatest extent in acid of chrome ore sample.
The selection analysis of embodiment two sampler-dissolving methods
1. the comparative analysis of solvent
1), peroxidating sodium fusion sample: sodium peroxide is a kind of strong oxidizing property basic solvent, and chromite is had very strong capacity of decomposition, in the process that sample decomposes, following reaction may take place and makes chlorine volatilization loss.1. sodium peroxide can be oxidized to chlorine and volatilization loss with chloride; 2. chromium is oxidized to sexavalence quantitatively in the chromite, and hexavalent chromate has oxidisability, can make chlorine volatilization loss with chloride generation redox reaction, as CrO
2Cl
2Boiling point 115.8, chromium meeting and chlorion generate volatile chlorochromic anhydride and remove.Therefore, sodium peroxide is difficult for measuring muriatic flux as sample dissolution.
2), NaOH flux: NaOH is non-oxidizable basic solvent, also can fine decomposition silicate mineral.Behind NaOH decomposition sample, it is orange-yellow that its filtrate shows.Trivalent chromium is an amphotere, in acid medium, is difficult to be oxidized to sexavalent chrome.But in alkaline medium, be easy to be generated chromate by some oxygenant institute's oxidations.Owing to adopt high temperature furnace fusion fusion solid sample, be equivalent under the higher situation of concentration, trivalent chromium is unavoidably produced the small additions of chromium hydrochlorate by oxygen institute oxidation in the air.Chromate disturbs the measurement result of chlorion, therefore, makes measurement result on the low side.
3), zinc paste-sodium carbonate flux: with zinc paste-sodium carbonate flux roasting chromite, it is light yellow that filtrate shows, and have the chromate ion of sexavalent chrome form to generate, and insolubles is more.It is higher to measure the solution blank simultaneously, therefore, is unsuitable for measuring chlorion.
Measurement result shows, uses the alkali dissolution sample, and the chlorion recovery is very low, and measurement result is very not parallel.
4), sour sample dissolution: by chromite chemical general formula and structure as can be known, chromium has oxytropism and affinity for iron, and is stronger with oxytropism, and chromium generally is trivalent under the endogenic action condition, so the extensive distribution of chromium is arranged in magnesium, iron and silicon hydrochlorate mineral and accessory mineral.Under the strong oxidizing condition of epigenetic zone, trivalent chromium is oxidized to the chromate ion of sexavalent chrome form, and the chromate negative ion that makes inactive chromium ion become Yi Rong moves.The electrode potential of chromium from the trivalent to the sexavalence is higher in acid solution, therefore is difficult for oxidized.
The qualitative judgement of chromate ion
Be two kinds of methods of highly acid with diphenylcarbazide examination color method and regulator solution pH value and qualitatively judge whether there is chromate ion in the solution to be measured.
1), divide and to get the above-mentioned solution to be measured that comes from different basic solvents in 3 small beakers, regulator solution pH value is 2, tries look with diphenylcarbazide, 3 beaker solution all have red the generation, judging thus has the chromate generation in the solution.If redness is darker, prove that the chromate ion that generates is more; If redness is more shallow, prove that the chromate ion that generates is less.
2), divide and to get the above-mentioned solution to be measured that comes from different basic solvents in 3 small beakers, be 2 o'clock with nitric acid regulator solution pH value, solution reddens, and illustrates in the filtrate to contain a large amount of Cr
6+
This is because trivalent chromic ion easily is oxidized to chromate CrO under alkali condition
4 2-, after acidifying, making pH=2～3, chromate becomes dichromate ion: 2CrO
4 2-+ H+==Cr
2O
7 2-+ H
2O that is to say, sexavalent chrome under acid condition mainly with dichromate ion (Cr
2O
7)
2-Form exist, pH is more little, dichromate ion concentration is big more, when pH ≈ 1.2, sexavalent chrome exists with the form of dichromate ion basically.Therefore we can see that peony generates.
3), with sulfuric acid, phosphoric acid and sulphur-phosphorus nitration mixture sample dissolution, solution is bottle green, uses the diphenylcarbazide qualitative identification, the solution nondiscolouring proves not contain chromate ion in the solution; The regulator solution pH value is 9, observes solution colour and changes, and does not have yellow the generation, further proves not contain Cr in the liquid to be measured
6+Solution placement to be measured after 24 hours, is differentiated once more whether trivalent chromic ion is converted into sexavalent chrome in the solution, and experimental result shows, do not detect hexavalent chromium in the solution, therefore, can avoid the generation of hexavalent chromium, also just from the sample pre-treatments link, eliminate Cr with sour molten method
6+Influence to determination of chloride ion.
Sampler-dissolving method and choice of Solvent
From the structure analysis of chrome ore itself, chlorine is mainly from the residue of watering (river/river or seawater) and depositing dust in institute's water and the cargo handling process in the ore dressing process in the chrome ore.These chlorides can dissolve in acid fully, and therefore, the present invention adopts sour sample dissolution to measure sour molten chloride content.
In acid medium, chlorion and acid reaction might generate hydrogen chloride and volatilization loss, therefore, adopt the molten sample system dissolves of closed microwave sample, under airtight molten batten spare, the volatile chloride of generation is difficult for loss, and the micro-wave digestion special advantages can increase the degree of sample dissolution, therefore, micro-wave digestion sample determination chlorion is splendid selection.
Adopting sulfuric acid or sulphur-phosphorus nitration mixture is the mixed solution dissolve chromium sample ore product of sulfuric acid, phosphoric acid, calculates the stripping quantity of coexistence elements in insolubles weight and the filtrate, the results are shown in Table 1, table 2.
By determination data as can be known, the stripping quantity of coexistence elements in different acid do not have significant difference in the chrome ore, and acid non-soluble substance weight does not obviously change yet, but good slightly in sulphur-phosphorus nitration mixture, the stripping quantity of coexistence elements is more relatively.This is because phosphoric acid has very strong mineral capacity of decomposition in the time of 100 ℃～300 ℃, if add sulfuric acid again, decomposition temperature can reach 360 ℃～380 ℃, more helping sample decomposes, can prevent simultaneously the appearance of pyrosulfate, improve the condition of using the phosphoric acid dissolved samples separately greatly, make molten sample operation be easy to grasp.In addition, phosphoric acid can complex solution in the part interfering ion, as ferric ion etc., and reduce ferric ion to measuring the interference of chlorion.Sulphur-phosphorus nitration mixture is the mixed solution of sulfuric acid, phosphoric acid, and the ratio of sulfuric acid, phosphorus nitration mixture is 1:1 in preferred sulphur-phosphorus nitration mixture.
The selection of embodiment three total ionic strength adjustment buffer degree correctivess (TISAB)
1. the selection of total ionic strength adjustment buffer degree correctives (TISAB) kind
Ion-selective electrode is an activity of measuring effects of ion according to Nernst equation, and the activity of ion equals the product of activity coefficient and concentration.The activity of certain ion depends mainly on the ionic strength of solution in the solution.Obviously, certain in temperature, ionic strength one timing, the activity coefficient of ion is certain.Total ionic strength adjustment buffer degree correctives (TISAB, Total Ionic Strength Adjustment Buffer) is a kind ofly to be used to keep solution to have the buffer solution of higher ionic strength.Because potential value in potentiometry is often linear with the logarithm of the activity of analyzed ion, therefore, total ionic strength adjustment buffer degree correctives has great important for the accuracy of analyzing.
In general, total ionic strength adjustment buffer degree correctives also usually can have some other function by way of parenthesis except the effect with stabilizing ion intensity, to improve the accuracy of analyzing better.Therefore, have one or more following compositions:
1) high concentration indifferent electrolyte, this is to keep the stable key of total ionic strength adjustment buffer degree.
2) the soda acid buffering is right, and the acidity that has form and solution of most analyte is related.In order to guarantee that analyte all exists with the form that can be detected, the pH value that needs to guarantee solution is in certain scope.In solution, add buffer solution and can accomplish this point well.
3) screening agent because analyzed system is complicated often, wherein may contain various interfering material Interference Detection, shelters chaff interference so often need to add suitable screening agent in the solution.
Common (TISAB) mainly contains citrate, tartrate, oxalates, ascorbic acid, EDTA, potassium nitrate, sodium nitrate etc., and this standard was done comparison test to citrate, tartrate, EDTA, potassium nitrate, sodium nitrate etc. respectively, saw Table 3, table 4.
Because contain impurity elements such as chromium, silicon, iron, aluminium, magnesium in the chrome ore sample, expect by the adding of EDTA, make some impurity elements and EDTA complexing and eliminate interference, but test findings shows that behind the adding EDTA, solution is placed a moment promptly can occur precipitation, therefore, can not select EDTA to make screening agent.Other several TISAB all can, take all factors into consideration, sodium citrate-potassium nitrate is better as the ionic-strength adjustment buffer screening agent of holding concurrently.
The selection of total ionic strength adjustment buffer degree correctives (TISAB) consumption
Simulate chrome ore dissolving condition of sample to be measured, in 5 50 mL small beakers, add 20 respectively
Ug/mLChlorine, concentration are 0.5% chrome ore matrix solution 5 mL, and sulphur-phosphorus nitration mixture concentration 10 % adds the TISAB of variable concentrations simultaneously, and transferring the pH value of solution value with sodium hydroxide solution is 2-4, treat that solution is cooled to room temperature fully after, be dissolved in surely in the 50 mL volumetric flasks, to be determined.
Solution is poured into respectively in the small beaker of 150 mL dryings, put into electromagnetism and stir Pan, beaker is put on the magnetic stirrer, insert chloride ion-selective electrode, respectively at 3 min, 4 min, 5min reading potential value sees Table 5.
Experimental result shows that do not add sodium citrate-potassium nitrate solution, the potential value fluctuation ratio is bigger, differs about 1mV/min, is not easy to stablize, and is not easy to control the pH value of solution.Add 5 mL～25 mL sodium citrate-potassium nitrate solutions, potential value changes more stable, consider that sample dissolves with acid, acidity is higher in the solution, and it is moderate that the amount of sodium citrate-potassium nitrate solution adds, and uses sodium hydroxide solution less during adjust pH, take all factors into consideration, use 20 mL sodium citrate-potassium nitrate solutions, both can guarantee has stronger electrolyte and complexing agent in the liquid to be measured, has guaranteed that again the concentration of citrate can not be greater than 0.5 mol/L.
The anti-interference test of total ionic strength adjustment buffer degree correctives (TISAB)
In order further to verify the consumption antagonism effects of jamming of TISAB, we have done comparative experiments.In one group of 50 mL beaker, add di-iron trioxide and a certain amount of TISAB of variable concentrations, under the identical situation of chlorine ion concentration, the variation of record potential value sees Table 6.
As known from Table 6,10 mL total ionic strength adjustment buffer degree correctivess can suppress the interference of the di-iron trioxide of 0.16 %, and are when di-iron trioxide concentration is higher than 0.4 %, can the sensation amount not enough, when increasing sodium citrate solution and be 20 mL, 0.8% di-iron trioxide matrix is interference measurement not also.
Embodiment four chrome ore matrix solution coexistence elements disturb and proofread and correct
From the chemical composition of chrome ore as can be known, mainly contain elements such as chromium, iron, aluminium, magnesium, silicon in the chrome ore, table 7 is the content of element oxide in the common chrome ore in laboratory.
Content range by each element and oxide in the concentration gradient deducibility chrome ore of each element oxide in 20 chrome ore samples is: Cr
2O
3Generally between 30 %～57 %, Fe is generally at 8 %～29 %, Al
2O
36 %～16.8 %, MgO 7.6 %～26.19 %, SiO
20.71 %～15.1 %.
Select 1 chrome ore sample to do comparative experiments, make solvent with sulphur-phosphorus nitration mixture, the stripping quantity of each element oxide and dissolution rate see Table 8 in the chrome ore
As can be known from the above table, except that magnesium oxide, other element leaching rate is less in sulphur-phosphorus nitration mixture.Therefore, the present invention carries out the interference test of coexistence elements by the actual dissolution rate of chrome ore.
Test findings shows: coexistence elements are very little to element influence to be measured, can ignore.
Embodiment five interpretations checking
1. the same breadboard precision and the recovery
Choose 2 chrome ore samples, 10 of each sample dissolution are dissolved mensuration by preceding method, and measurement result sees Table 9, calculate relative standard deviation.Divide and get 2 parts of testing sample 10 mL in small beaker, adding concentration respectively is 100
uChlorine standard solution 2.5 mL and 5.0 mL of g/mL add sodium citrate-potassium nitrate solution, and transferring pH value of solution is 2～5, are dissolved in surely in the 50 mL volumetric flasks, and measuring the recovery is between 90 %～110 %.
2. the precision confirmatory experiment of different experiments chamber
By 8 tame laboratories 2 samples are carried out demonstration test.Each sample provides 3 panel datas.By the check of consistance and outlier, there is not qi from value and outlier.The precision statistics is calculated and is seen Table 10.
Claims (8)
1. method of measuring chlorion in the chrome ore, it may further comprise the steps:
(1) produces the analytic sample of chrome ore: adopt muller to produce certain detailed catalogue chrome ore analytic sample;
(2) take by weighing quantity of sample: accurately take by weighing a certain amount of chrome ore analytic sample, be put in the micro-wave digestion jar;
(3) add a certain amount of acid: after using low amounts of water moistening, add a certain amount of sulphur-phosphorus nitration mixture, shake up, covered and enclosed is put into the micro-wave digestion stove;
(4) micro-wave digestion program setting:, determine micro-wave digestion power, digestion time and digestion condition according to sample weighting amount and micro-wave digestion jar number;
(5) chrome ore solution to be measured is prepared: treat that micro-wave digestion stops, after the cooling of micro-wave digestion jar, take out, add total ionic strength adjustment buffer degree correctives, the pH value of regulating chrome ore solution to be measured, treat that test solution is cooled to room temperature after, constant volume is in the volumetric flask of certain volume, do filtration with fine and close filter paper, discard initial filtrate, preservation filtrate is to be determined;
(6) chrome ore matrix solution preparation: choose a certain amount of chrome ore analytic sample, add sulphur-phosphorus nitration mixture, heating for dissolving number minute on electric hot plate makes the chlorion of dissolving generate the hydrogen chloride gas volatilization, preparation chrome ore matrix solution;
(7) drafting of preparation of chlorion standard solution and typical curve: the chlorion standard solution of preparation variable concentrations, the content of the chrome ore matrix solution in the chlorion standard solution, sulphur-phosphorus nitration mixture, total ionic strength adjustment buffer degree correctives is identical with content in the chrome ore solution to be measured, regulate the pH of chlorion standard solution, constant volume is drawn the chlorion typical curve in the volumetric flask of certain volume;
(8) measure chloride ion content: measure with ion selective electrode method,, calculate the content of chlorion in the chrome ore solution to be measured by the chlorion typical curve.
2. according to the method for chlorion in the described mensuration chrome ore of claim 1, it is characterized in that: when measuring according to described step (8), the chlorion standard solution and the chrome ore solution to be measured of variable concentrations are injected dry beaker respectively, add magnetic stir bar, beaker is put on the magnetic stirring apparatus, with the constant speed agitating solution, press chlorine ion concentration order sequentially determining chlorion standard solution and chrome ore solution to be measured from low to high, and read stable potential value by the same fixing response time;
With the potential value is ordinate, and the negative logarithm of chlorine ion concentration is a horizontal ordinate, and the drawing standard curve by the typical curve linear equation, calculates chloride ion content in the chrome ore solution to be measured by following formula:
In the formula:
W---the massfraction of chrome ore solution chlorion to be measured, %;
C---the concentration of chlorion from the chrome ore solution to be measured that typical curve checks in, μ g/mL;
V---the volume of chrome ore solution to be measured, mL;
The quality of m---chrome ore to be measured, g.
3. according to the method for chlorion in the described mensuration chrome ore of claim 1, it is characterized in that: the detailed catalogue of described chrome ore analytic sample requires≤75 um.
4. according to the method for chlorion in the described mensuration chrome ore of claim 1, it is characterized in that: described chrome ore solution to be measured, chlorion standard solution pH value of solution are to adopt sodium hydroxide solution to regulate, and the pH value of solution value is adjusted to 2～5.
5. according to the method for chlorion in the described mensuration chrome ore of claim 1, it is characterized in that: described total ionic strength adjustment buffer degree correctives adopts sodium citrate-potassium nitrate.
6. according to the method for chlorion in the described mensuration chrome ore of claim 1, it is characterized in that: the ratio of sulfuric acid, phosphoric acid is 1:1 in described sulphur-phosphorus nitration mixture.
7. according to the method for chlorion in the described mensuration chrome ore of claim 1, it is characterized in that: the chrome ore analytic sample that described step (2) takes by weighing is 0.5g～1.0g.
8. according to the method for chlorion in the described mensuration chrome ore of claim 1, it is characterized in that: sulphur-phosphorus nitration mixture that described step (3) adds is 10 mL～15 mL.
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| CN110398471A (en) * | 2019-08-31 | 2019-11-01 | 深圳市中金岭南有色金属股份有限公司 | Chloride ion conductor method in zinc concentrate |
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| CN110006736A (en) * | 2019-03-07 | 2019-07-12 | 江阴兴澄特种钢铁有限公司 | The method that ICP-AES quickly measures Main elements aluminum oxide, silica and chromic oxide content in high alumina refractories containing chromium |
| CN110398471A (en) * | 2019-08-31 | 2019-11-01 | 深圳市中金岭南有色金属股份有限公司 | Chloride ion conductor method in zinc concentrate |
| CN110398471B (en) * | 2019-08-31 | 2022-03-11 | 深圳市中金岭南有色金属股份有限公司 | Method for determining chloride ions in zinc concentrate |
| CN110632271A (en) * | 2019-10-17 | 2019-12-31 | 绍兴市三合检测技术有限公司 | Method for detecting heavy metal in soil |
| CN111735907A (en) * | 2020-08-04 | 2020-10-02 | 湖南航天磁电有限责任公司 | Method for measuring chloride ion content in industrial lanthanum oxide by potentiometric titration |
| CN113155931A (en) * | 2021-04-09 | 2021-07-23 | 国家烟草质量监督检验中心 | Method for detecting chloride ions in tobacco and tobacco planting soil |
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