CN108956494A - A kind of method of sulfate radical content in quick measurement bauxite - Google Patents

A kind of method of sulfate radical content in quick measurement bauxite Download PDF

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CN108956494A
CN108956494A CN201810686618.6A CN201810686618A CN108956494A CN 108956494 A CN108956494 A CN 108956494A CN 201810686618 A CN201810686618 A CN 201810686618A CN 108956494 A CN108956494 A CN 108956494A
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bauxite
absorbance
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sulfate radical
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胡璇
张树朝
石磊
匡玉云
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Aluminum Corp of China Ltd
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    • G01—MEASURING; TESTING
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Abstract

The invention discloses a kind of methods of sulfate radical content in measurement bauxite, comprising steps of (1) obtains test solution: taking high-sulfur bauxite sample to be measured, solution is made through hydrochloric acid decomposition, and handle solution；(2) it draws calibration curve: preparing the sulfate radical calibration solution of various concentration, hydrochloric acid solution is added into the calibration solution, barium chromate suspension is added, it is in lemon yellow that ammonium hydroxide to liquid, which is then added dropwise, the absorbance A of the absorbance A of measurement calibration solution and blank calibration solution at 420nm wavelength0；According to the concentration value and corresponding absorbance A-A of sulfate radical in calibration solution0Draw calibration curve；(3) in bauxite sulfate radical content: measure the absorbance A ' of the test solution and the blank solution absorbance A in company with test solution0', according to absorbance A-A0' calculates the content of sulfate radical in the test solution in conjunction with the calibration curve, and then obtains the content of sulfate radical in bauxite.

Description

A kind of method of sulfate radical content in quick measurement bauxite
Technical field
A kind of method of sulfate radical content in measurement bauxite, it is raw to be related to a kind of analysis of sulfate radical, especially aluminium oxide Produce the detection method with sulfate radical content in bauxite.
Background technique
Sulphur can bring some problems during bauxite into alumina, such as cause digesting efficiency of alumina decline, corruption Pipeline, suppression solution desiliconization are lost, serious person also will cause red mud separating, washing difficulty, or even influence product quality.High-sulfur aluminium Have 50% or more the grade of ore higher in native mine, this kind of ore with high alumina, in low silicon, high-sulfur, low-high iron, middle high aluminium silicon ratio For main feature.It is tight for improving the grade of ore and alleviation ore resource if solving the desulphurization problem of high-sulfur bauxite The situation opened has great significance.
In the sulfur removal technology of bauxite, the content of sulfate radical is one of them important indicator.Sulfate radical content in bauxite Analysis, existing analysis method has: atomic absorption method, EDTA volumetric method and gravimetric method etc..Often use gravimetric detemination in laboratory The content of sulfate radical in bauxite need to complete a sulphur by cumbersome tediously long steps such as precipitates overnight, separating, washing, calcinations The measurement of sour barium gravimetric method needs two day time.EDTA volumetric method also needs experience precipitates overnight, and atomic absorption method needs to use Expensive instrument is difficult to meet daily the needs of accurately quickly detecting.
Barium Chromate Spectrophotometer speed is fast, and accuracy is high, is generally used for the analysis of sulfate radical content in water quality.Due to bauxite The particularity of ingredient, wherein the aluminium contained, iron, titanium and calcium matrix, it is easy to be formed and be co-precipitated with sulfate radical, and iron exists There is strong visible absorbance at 420nm, if do not shielded, the measurement of sulfate radical certainly will be interfered.Only eliminate it is dry Under the premise of disturbing ion influence, in conjunction with the content of sulfate radical in Barium Chromate Spectrophotometer analysis bauxite, it can be only achieved quick and precisely Purpose.
Summary of the invention
The purpose of the present invention is to deficiencies existing for above-mentioned prior art, change to water quality Barium Chromate Spectrophotometer Into, provide it is a kind of accurate, quickly in measurement bauxite sulfate radical content method, the calibration solution of this method is not necessarily to matrix Match, whole experiment process only needs just achievable less than two hours.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of method of sulfate radical content in measurement bauxite, which is characterized in that steps are as follows:
(1) it obtains test solution: taking high-sulfur bauxite sample to be measured, solution is made through hydrochloric acid decomposition, is added a certain amount of Ammonia precipitation process separates aluminium, iron and titanium, and ammonium carbonate precipitation and separation calcium is added, and dilutes constant volume with distilled water, mixes, with quantitatively filtering at a slow speed Paper filtering, collects filtrate, divides and 10-25mL filtrate is taken to use distilled water dilution as test solution, and blank test is done in companion；
(2) it draws calibration curve: preparing the sulfate radical calibration solution of various concentration, hydrochloric acid is added into the calibration solution Solution, heating are boiled, and barium chromate suspension is added, and heating is boiled, and it is in lemon yellow that ammonium hydroxide to liquid, which is then added dropwise, are used after cooling Distilled water is settled to, mixing identical as test solution volume, with the filtering of quantitative filter paper at a slow speed, filtrate is collected, at 420nm wavelength The blank that the absorbance A and sulfate concentration of measurement calibration solution are 0 calibrates the absorbance A of solution0；According to sulphur in calibration solution The concentration value of acid group and corresponding absorbance A-A0Draw calibration curve；
(3) in bauxite sulfate radical content: with hydrochloric acid solution adjust test solution pH value, by the side in step (2) Formula measures the absorbance A ' of the test solution and the blank solution absorbance A in company with test solution0', according to absorbance A '-A0', knot The calibration curve is closed, the content of sulfate radical in the test solution is calculated, and then obtains the content of sulfate radical in bauxite.
Further, test solution is obtained in the step (1), specially weighs 2.0 ± 0.0002g sample in 300mL In beaker, add 20-40mL6mol/L hydrochloric acid solution, heat resolve；Add boiling water to volume about 150mL, boils 1min, 4-6 is added dropwise 0.5% bromothymol blue indicator is dripped, under stiring, it is blue that solution is neutralized to 7mol/L ammonium hydroxide；After slightly cold, it is added 10-20mL10% sal volatile, solution and precipitating are fully transferred in 250mL volumetric flask, are diluted to scale, are mixed；With slow Fast quantitative filter paper filtering, collects filtrate in dry combustion method cup, divides and take proper volume in 150mL conical flask, add distilled water to 50mL. The dosage of its ammonium hydroxide and ammonium carbonate is determined according to the amount of matrix element in bauxite.Divide the 10-25mL filtrate distilled water taken It is diluted to volume about 50mL, content should be not less than 5mg/L.
Further, a series of step (2) specifically: to conical flasks equipped with various concentration sulfate radical calibration solution In plus 1-3mL2.5mol/L hydrochloric acid solution, heating boil 5min, then plus 2-4mL barium chromate suspension, heating boil 5min；It takes 7mol/L ammonium hydroxide is added dropwise to liquid in lemon yellow in inferior pyramidal bottle；After cooling, move into 50mL volumetric flask, it is fixed with distilled water Hold, mixes.It is filtered with quantitative filter paper at a slow speed, collects filtrate, the absorbance of measurement calibration solution at 420nm wavelength.
Further, in the step (3): adjusting the pH value of test solution to 1-2 with 2.5mol/L hydrochloric acid solution.
The method of sulfate radical content in a kind of measurement bauxite of the invention is decomposed high-sulfur bauxite using hydrochloric acid, is added A certain amount of ammonia precipitation process separates aluminium, iron, titanium, and uses ammonium carbonate precipitation and separation calcium, and calibration solution utilizes chromium without Matrix Match Sour barium-spectrophotometry measurement sulfate radical content, method is accurate, quick, precision is good, meets the needs of fast quantification.
Detailed description of the invention
Fig. 1 is the fitting result of calibration curve.
Specific embodiment
A kind of method of sulfate radical content in measurement bauxite is decomposed high-sulfur bauxite using hydrochloric acid, is added a certain amount of Ammonia precipitation process separates aluminium, iron and titanium, and uses ammonium carbonate precipitation and separation calcium, and calibration solution utilizes barium chromate-point without Matrix Match The content of light photometry measurement sulfate radical.
Key step includes:
1) dissolution of sample
2.0 ± 0.0002g sample is weighed in 300mL beaker, adds 20mL6mol/L hydrochloric acid solution, the glass in heating Stick stirring, then it is diluted to volume about 150mL with distilled water, 1min is boiled, 0.5% bromothymol blue indicator of 4-6 drop is added dropwise, Under stiring, to be neutralized to solution with 7mol/L ammonium hydroxide blue；After slightly cold, it is added 20mL10% sal volatile, solution and heavy Shallow lake is fully transferred in 250mL volumetric flask, is diluted to scale, is mixed；It is filtered with quantitative filter paper at a slow speed, collects filtrate in dry combustion method cup In, divide and take proper volume in 150mL conical flask, adds distilled water to 50mL.
2) preparation of blank
Blank test is done in company with sample.
3) preparation of solution is calibrated
Take 7 150mL conical flasks, be separately added into 0mL, 0.25mL, 0.50mL, 1.00mL, 3.00mL, 5.00mL and 7.00mL sulfate radical standard solution, respectively plus distilled water is to 50mL.
4) barium chromate-spectrophotometry colour developing
To step 1), step 2) solution in respectively plus 1-3mL2.5mol/L hydrochloric acid solution, 5min or so is boiled in heating, then Add 2-4mL barium chromate suspension, 5min or so is boiled in heating.Conical flask is removed, 7mol/L ammonium hydroxide is added dropwise to liquid to each bottle Body is in lemon yellow.After cooling, moves into 50mL volumetric flask, add distilled water to be diluted to scale, shake up.With quantitative filter paper mistake at a slow speed Filtrate is collected in filter, and absorbance is measured at 420nm wavelength.
5) in bauxite sulfate radical content calculating
The absorbance A of measurement calibration solution and the absorbance A of calibration blank solution0, according to sulfate radical in calibration solution Concentration value and corresponding absorbance A-A0Draw calibration curve；Measure the absorbance A ' of test solution and molten in company with the blank of test solution Liquid absorbance A0', according to absorbance A '-A0' and calibration curve, calculate the content of sulfate radical in test solution, and then obtain alumina The content of sulfate radical in mine.
The invention has the advantages that using hydrochloric acid decomposing bauxite, be added a certain amount of ammonium hydroxide and ammonium carbonate precipitation and separation aluminium, The matrixes such as iron, titanium, calcium and interference element, calibration solution are not necessarily to Matrix Match, measure sulfate radical using barium chromate-spectrophotometry Content, method is accurate, quickly, precision it is good, meet the needs of fast quantification.
Below with reference to embodiment, invention is further described in detail, but the embodiment that do not invent is without being limited thereto.
Embodiment 1: the mass fraction of sulfate radical is 0.5% in the surveyed bauxite of the present embodiment, and detailed process is as follows:
1) dissolution of sample
2.0 ± 0.0002g sample is weighed in 300mL beaker, adds 20mL6mol/L hydrochloric acid solution, the glass in heating Stick stirring, then it is diluted to volume about 150mL with distilled water, boil 1min；0.5% bromothymol blue indicator of 4-6 drop is added dropwise, Under stiring, to be neutralized to solution with 7mol/L ammonium hydroxide blue.After slightly cold, it is added 10mL10% sal volatile, solution and heavy Shallow lake is fully transferred in 250mL volumetric flask, is diluted to scale, is mixed.It is filtered with quantitative filter paper at a slow speed, collects filtrate in dry combustion method cup In, divide and take 25mL in 150mL conical flask, adds distilled water to 50mL.
2) preparation of blank
Blank test is done in company with sample.
3) preparation of solution is calibrated
5 150mL conical flasks are taken, the 1mg/mL sulfuric acid of 0mL, 0.25mL, 0.50mL, 1.00mL, 3.00mL are separately added into Root standard solution, respectively plus distilled water is to 50mL.
4) barium chromate-spectrophotometry colour developing
To step 1), step 2) solution in respectively plus 1mL2.5mol/L hydrochloric acid solution, 5min or so is boiled in heating, then plus 5min or so is boiled in 2.5mL barium chromate suspension, heating.Conical flask is removed, 7mol/L ammonium hydroxide is added dropwise to liquid to each bottle In lemon yellow.It after cooling, moves into 50mL volumetric flask, is diluted to scale with distilled water, mix.It is filtered with quantitative filter paper at a slow speed, Filtrate is collected, absorbance is measured at 420nm wavelength.
5) in bauxite sulfate radical content calculating
The absorbance A of measurement calibration solution and the absorbance A of calibration blank solution0, according to sulfate radical in calibration solution Concentration value and corresponding absorbance A-A0Draw calibration curve；The pH value of test solution is adjusted to 1- with 2.5mol/L hydrochloric acid solution 2, measure the absorbance A ' of test solution and the blank solution absorbance A in company with test solution0', according to absorbance A '-A0' and calibration are bent Line, calculates the content of sulfate radical in test solution, and then obtains the content of sulfate radical in bauxite.
The linear equation for the calibration curve that above step measures such as Fig. 1.
Embodiment 2: the mass fraction of sulfate radical is 2.5% in the surveyed high-sulfur bauxite of the present embodiment, and detailed process is as follows:
1) dissolution of sample
2.0 ± 0.0002g sample is weighed in 300mL beaker, adds 40mL6mol/L hydrochloric acid solution, the glass in heating Stick stirring, then it is diluted to volume about 150mL with distilled water, it boils, 0.5% bromothymol blue indicator of 4-6 drop is added dropwise, is stirring It mixes down, it is blue to be neutralized to solution with 7mol/L ammonium hydroxide.After slightly cold, 20mL10% sal volatile is added, solution and precipitating are complete Portion is transferred in 250mL volumetric flask, is diluted to scale, is mixed.It is filtered with quantitative filter paper at a slow speed, collects filtrate in dry combustion method cup, Dividing takes 10mL in 150mL conical flask, adds distilled water to 50mL.
2) preparation of blank
Blank test is done in company with sample.
3) preparation of solution is calibrated
5 150mL conical flasks are taken, the 1mg/mL sulfuric acid of 0mL, 0.50mL, 1.00mL, 3.00mL and 5.00mL are separately added into Root standard solution, respectively plus distilled water is to 50mL.
4) barium chromate-spectrophotometry colour developing
To step 1), step 2) solution in respectively plus 3mL2.5mol/L hydrochloric acid solution, 5min or so is boiled in heating, then plus 5min or so is boiled in 3mL barium chromate suspension, heating.Conical flask is removed, 7mol/L ammonium hydroxide to liquid, which is added dropwise, to each bottle is in Lemon yellow.It after cooling, moves into 50mL volumetric flask, is diluted to scale with distilled water, mix.It is filtered, is received with quantitative filter paper at a slow speed Collect filtrate, absorbance is measured at 420nm wavelength.
5) in bauxite sulfate radical content calculating
The absorbance A of measurement calibration solution and the absorbance A of calibration blank solution0, according to sulfate radical in calibration solution Concentration value and corresponding absorbance A-A0Draw calibration curve；The pH value of test solution is adjusted to 1- with 2.5mol/L hydrochloric acid solution 2, measure the absorbance A ' of test solution and the blank solution absorbance A in company with test solution0', according to absorbance A '-A0' and calibration are bent Line, calculates the content of sulfate radical in test solution, and then obtains the content of sulfate radical in bauxite.
Accuracy experiment
Accuracy experiment is carried out to the sulfate radical in bauxite 1# and 2# sample respectively using embodiment 1 and embodiment 2, i.e., Recovery testu, the results are shown in Table 1, and the rate of recovery of sulfate radical illustrates the measurement of the method for the present invention between 95-105% As a result accurate and reliable.
1 accuracy experimental result of table
Sample Additional amount/g Measured amount/g Yield/g The rate of recovery/%
1# 0.0074 0.022 0.0070 95
2# 0.024 0.073 0.025 105
Precision Experiment
Essence is carried out to the sulfate radical in bauxite 1# and 2# sample respectively using embodiment 1 and method as described in example 2 Density experiment, experiment are measured in parallel 6 times (n=6), the data measured are made Mathematical Statistics Analysis, the results are shown in Table 2, relatively Standard deviation (< 5%) within the scope of 1.57-3.00% illustrates that the measurement result precision of the method for the present invention is good.
2 precision experiment result of table (n=6)
Comparative experiments
Using embodiment 1 and method as described in example 2 respectively to the sulfate radical content in bauxite 1# and 2# sample into Row measurement, meanwhile, the sulfate radical content in 1# and 2# is measured using gravimetric method, the results are shown in Table 3, two methods Absolute error illustrates that the measurement result of the method for the present invention is consistent with gravimetric method result less than 0.1%.
3 contrast and experiment of table
Measuring method 1#/% 2#/%
Spectrophotometry 0.74 2.39
Gravimetric method 0.78 2.48
Absolute error 0.04 0.09

Claims (5)

1.一种测定铝土矿中硫酸根含量的方法，其特征在于，步骤如下：1. a method for measuring sulfate radical content in bauxite, is characterized in that, step is as follows: （1）获取待测试液：取待测高硫铝土矿试样，经盐酸分解制成溶液，加入一定量的氨水沉淀分离铝、铁和钛，加入碳酸铵沉淀分离钙，用蒸馏水稀释定容，混匀，用慢速定量滤纸过滤，收集滤液，分取10-25mL滤液用蒸馏水稀释作为待测试液，并随同做空白试验；(1) Obtain the solution to be tested: take the high-sulfur bauxite sample to be tested, decompose it with hydrochloric acid to make a solution, add a certain amount of ammonia water to precipitate and separate aluminum, iron and titanium, add ammonium carbonate to precipitate and separate calcium, and dilute the solution with distilled water. Contain, mix well, filter with slow quantitative filter paper, collect the filtrate, take 10-25mL of the filtrate and dilute it with distilled water as the test solution, and do a blank test along with it; （2）绘制校准曲线：配制不同浓度的硫酸根校准溶液，向所述校准溶液中加入盐酸溶液，加热煮沸，再加入铬酸钡悬浊液，加热煮沸，然后滴加氨水至液体呈柠檬黄，冷却后用蒸馏水定容至与待测试液体积相同，混匀，用慢速定量滤纸过滤，收集滤液，于420 nm波长处测量校准溶液的吸光度A和空白校准溶液的吸光度A0；根据校准溶液中硫酸根的浓度值和对应的吸光度A- A0绘制校准曲线；(2) Draw a calibration curve: Prepare different concentrations of sulfate root calibration solutions, add hydrochloric acid solution to the calibration solution, heat to boil, then add barium chromate suspension, heat to boil, then add ammonia water dropwise until the liquid turns lemon yellow , after cooling, dilute to the same volume as the liquid to be tested with distilled water, mix well, filter with slow quantitative filter paper, collect the filtrate, measure the absorbance A of the calibration solution and the absorbance A of the blank calibration solution at a wavelength of 420 nm; according to the calibration The concentration value of sulfate radical in the solution and corresponding absorbance A- A 0 draw calibration curve; （3）铝土矿中硫酸根的含量：用盐酸溶液调节待测试液的pH值，按步骤（2）中的方式测定所述待测试液的吸光度A＇和随同试液的空白溶液吸光度 A0＇，根据吸光度A - A0＇，结合所述校准曲线，计算所述待测试液中硫酸根的含量，进而得到铝土矿中硫酸根的含量。(3) Sulfate content in bauxite: adjust the pH value of the solution to be tested with hydrochloric acid solution, and measure the absorbance A' of the solution to be tested and the absorbance A of the blank solution accompanying the test solution according to the method in step (2). 0 ', according to the absorbance A - A 0 ', combined with the calibration curve, calculate the content of sulfate in the liquid to be tested, and then obtain the content of sulfate in bauxite. 2.如权利要求1所述的一种测定铝土矿中硫酸根含量的方法，其特征在于，所述步骤（1）中获取待测试液，具体为称取2.0±0.0002 g试样于300 mL烧杯中，加20-40 mL6 mol/L盐酸溶液，边加热边用玻璃棒搅拌，再用蒸馏水稀释至体积为150mL，煮沸1 min；滴加4-6滴0.5 %溴麝香草酚蓝指示剂，在搅拌下，以7 mol/L氨水中和至溶液呈蓝色；稍冷后，加入10-20 mL10 %碳酸铵溶液，溶液及沉淀全部转移至250 mL容量瓶中，稀释至刻度，混匀；用慢速定量滤纸过滤，收集滤液于干烧杯中，分取10-25mL滤液于150 mL锥形瓶内，加蒸馏水至50mL。2. A method for determining sulfate content in bauxite as claimed in claim 1, characterized in that, in said step (1), the solution to be tested is obtained, specifically weighing 2.0 ± 0.0002 g sample in 300 Add 20-40 mL6 mol/L hydrochloric acid solution to a mL beaker, stir with a glass rod while heating, then dilute with distilled water to a volume of 150mL, boil for 1 min; add 4-6 drops of 0.5% bromothymol blue for indication Under stirring, neutralize with 7 mol/L ammonia water until the solution turns blue; after cooling slightly, add 10-20 mL of 10% ammonium carbonate solution, transfer all the solution and precipitate to a 250 mL volumetric flask, dilute to the mark, Mix well; filter with slow quantitative filter paper, collect the filtrate in a dry beaker, divide 10-25mL of the filtrate into a 150 mL Erlenmeyer flask, add distilled water to 50mL. 3.如权利要求1所述的一种测定铝土矿中硫酸根含量的方法，其特征在于，所述步骤（1）中：分取的10-25mL滤液用蒸馏水稀释至体积约50mL，其含量应不低于5mg/L。3. a kind of method for measuring sulfate radical content in bauxite as claimed in claim 1, is characterized in that, in described step (1): the 10-25mL filtrate that divides is diluted to volume about 50mL with distilled water, its The content should not be less than 5mg/L. 4.根据权利要求1所述的一种测定铝土矿中硫酸根含量的方法，其特征在于，所述步骤（2）具体为：向一系列装有不同浓度硫酸根校准溶液的锥形瓶中加1-3 mL2.5 mol/L盐酸溶液，加热煮沸5 min，再加2-4 mL铬酸钡悬浊液，加热煮沸5 min；取下锥形瓶，逐滴加入7mol/L氨水至液体呈柠檬黄；冷却后，移入50 mL容量瓶中，用蒸馏水定容，混匀，用慢速定量滤纸过滤，收集滤液，于420 nm波长处测量校准溶液的吸光度。4. a kind of method for measuring sulfate radical content in bauxite according to claim 1 is characterized in that, described step (2) is specially: to a series of Erlenmeyer flasks that different concentration sulfate radical calibration solutions are housed Add 1-3 mL of 2.5 mol/L hydrochloric acid solution, heat and boil for 5 min, add 2-4 mL of barium chromate suspension, heat and boil for 5 min; remove the Erlenmeyer flask, add 7 mol/L ammonia water drop by drop Until the liquid turns lemon yellow; after cooling, transfer it to a 50 mL volumetric flask, make up to volume with distilled water, mix well, filter through slow quantitative filter paper, collect the filtrate, and measure the absorbance of the calibration solution at a wavelength of 420 nm. 5.根据权利要求1所述的一种测定铝土矿中硫酸根含量的方法，其特征在于，所述步骤（3）中：用2.5 mol/L盐酸溶液调节待测试液的pH值至1-2。5. A method for determining sulfate content in bauxite according to claim 1, characterized in that, in said step (3): adjust the pH value of the liquid to be tested to 1 with 2.5 mol/L hydrochloric acid solution -2.
CN201810686618.6A 2018-06-28 2018-06-28 A kind of method of sulfate radical content in quick measurement bauxite Pending CN108956494A (en)

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