CN105717252A - Determination method for chlorine in coal - Google Patents
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- CN105717252A CN105717252A CN201610138627.2A CN201610138627A CN105717252A CN 105717252 A CN105717252 A CN 105717252A CN 201610138627 A CN201610138627 A CN 201610138627A CN 105717252 A CN105717252 A CN 105717252A
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- G—PHYSICS
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- G01N21/79—Photometric titration
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N31/162—Determining the equivalent point by means of a discontinuity
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Abstract
The invention relates to a determination method for chlorine in coal. None of several existing determination methods for chlorine in coal is suitable for popularization in a power plant coal detection lab. The determination method is characterized in that release and absorption of chlorine in coal are completed through the heat value determination process, a series of treatment such as PH regulation, labeling and sedimentation is carried out after absorption liquid collection, standard potassium thiocyanate solution titration is carried out finally, and thus rapid and accurate determination of the chlorine content in coal is achieved. The determination method is simple, rapid and easy to popularize.
Description
Technical field
The invention belongs to coal analysis field, be specifically related to Determination Method of Chlorine in a kind of coal.
Background technology
In coal, chlorine mainly exists with inorganic matter form, exists with organic form on a small quantity.The height of chlorine content in coal reflects the content height of the elements such as middle sodium potassium that produce coal indirectly, and the latter is the key factor of Pollution of Boiler.In coal, the overwhelming majority is with HC1 or poisonous organic chloride in burning or pyrolytic process for chlorine, as two uh the forms such as English, furan discharge, and contaminated environment, it is detrimental to health, the release of chlorine also can cause the corrosion of furnace wall and pipeline.
Measure chlorine content in coal and have been subjected to include the close attention of more and more departments of environmental administration.Chlorinity has become one of important indicator of coal property evaluation, coal processing and utilization and foreign trade.In coal, the detection method of chlorinity is more, mainly there are combustion hydrolytic method, Emhorn card precipitation titration, By Oxygen Bomb Combustion potentiometric titration, ion selective electrode method etc., if publication date is on 08 06th, 2008, publication number is in the Chinese patent of CN101236174, and what disclose that the assay method of a kind of chlorine content in coal adopts is electrode method.
China's inspection and quarantining for import/export industry standard is SN/T2087-2008 high performance liquid chromatography.Existing GB is GB/T3558-2014 Emhorn card-precipitation titration and high-temperature combustion hydrolytic-potentiometric titration, high-temperature combustion hydrolytic method and high performance liquid chromatography all need to install a set of special equipment, and the factor affecting measurement result is a lot；Although Emhorn block-regulations is simple to operate, but the initial processing steps of sample is relatively complicated, and easily occurs that calcination is incomplete, affects the accuracy of measurement result.Therefore existing several method is all unsuitable for the popularization in coal testing laboratory of power plant.
Summary of the invention
It is an object of the invention to overcome above shortcomings in prior art, and the assay method of chlorine in a kind of coal simple, quick, easy to spread is provided.
This invention address that the problems referred to above be the technical scheme is that being characterized in that of the assay method of chlorine in this coal: described assay method is by heating-value determination process in coal, complete release and the absorption of chlorine in coal, after absorbing liquid collection, by regulating PH, mark-on, a series of process such as precipitation, finally by standard potassium thiocyanate solution titration, thus rapid and accurate determination chlorine content in coal.
As preferably, the assay method of the present invention includes following step:
1) accurately weigh uniform sample 1 ± 0.1g(and be accurate to 0.0001g), it is placed in combustion boat, adding 10mL mass percentage concentration in oxygen bomb is the sodium carbonate liquor of 5%, carefully tighten oxygen bomb lid, the oxygen bomb installed is inserted in calorimeter, slowly it is filled with 2.0MPa～3.0MPa oxygen, by calorimeter operation sequence, sample is lighted.
2), after combustion test terminates, oxygen bomb takes out after cooling 10min in cooling water, is at the uniform velocity discharged lentamente by pressure within no less than the time of 2min.
3) open oxygen bomb, fully clean each several part in oxygen bomb (including inside and outside bullet bucket, vent valve, combustion boat and combustion residue) with a branch of thin hot water.Whole wash pools in a beaker (fixing fabric structure of beaker is at about 80mL).
4) in washing liquid, add 1 phenolphthalein indicator, it is adjusted to red disappearance with concentrated nitric acid, after amount 5mL, the sodium chloride standard solution that 5mL concentration is 0.1mg/L and the standard silver nitrate solution that 5mL concentration is 0.025mol/L is accurately pipetted in beaker with transfer pipet, place 2-3min, add 2-5mL hexanol, cap upper surface ware, beaker is placed on magnetic stirring apparatus quickly after stirring 2-3min, adds 1mL ammonium ferric sulfate indicator.
5) with the standard potassium thiocyanate solution titration demarcated, when solution is become light orange by milky, it is terminal, writes down the volume of potassium thiocyanate solution.
6) measure every a collection of coal sample, perform twice at above blank determination (being not added with coal sample) by above step, take its arithmetic mean of instantaneous value as blank value.The computing formula of chlorine content in coal is
In formula: CladFor the content of chlorine in air-dried basis coal sample, unit is %；0.03545 is mM quality of chlorine, and unit is g/mmol；C is the thing mass concentration of potassium thiocyanate, and unit is mmol/mL；V1Potassium thiocyanate consumption during for mensuration coal sample, unit is mL；V2Potassium thiocyanate solution consumption during for measuring blank, unit is mL；M is air-dried sample quality, and unit is g.
By Oxygen Bomb Combustion and chemical titration are combined by the present invention, while surveying caloric value, complete release and the absorption of chlorine in coal, simple to operate, with low cost.
As preferably, the present invention is applicable to the mensuration of brown coal, bituminous coal and smokeless chlorine content in coal, if finding after By Oxygen Bomb Combustion that coal sample is splashed or uncombusted, should adopt an effective measure and again test, it is ensured that in coal, chlorine all discharges and is absorbed by liquid absorption.
As preferably, the preparation of standard silver nitrate solution of the present invention: accurately weigh the standard reagent silver nitrate 4.2472g being cooled to room temperature in advance after 110 DEG C of dry 1h and in exsiccator, it is dissolved in a small amount of water, then proceeds in 1000ml volumetric flask, be diluted with water to graduation mark.
As preferably, the preparation of standard potassium thiocyanate solution of the present invention and being demarcated as: weigh 2.5g potassium thiocyanate soluble in water, then proceed in 1000mL volumetric flask, be diluted with water to scale, shake up；10mL silver nitrate standard solution is accurately pipetted with transfer pipet, inject 50mL water, 3ml nitric acid and 1ml ammonium ferric sulfate indicator, it is titrated to solution with potassium thiocyanate standard solution to be become light orange from milky and be terminal, write down potassium thiocyanate solution consumption, carry out 4-8 time to demarcate, using the meansigma methods of repeatedly consumption as consumption volume (V), according to formula c=V0× k/V calculates the concentration of potassium thiocyanate solution, and in formula, c is the concentration of potassium thiocyanate solution, unit mmol/mL；V0For silver nitrate standard solution consumption, unit is mL；K is the concentration value of silver nitrate standard solution, and in 0.0250, unit is mol/L；V is the consumption of potassium thiocyanate standard solution, and unit is mL.
As preferably, the preparation of sodium chloride standard solution of the present invention: accurately weigh the top grade pure sodium chloride 0.1649g being cooled to room temperature in advance after 500-600 DEG C of calcination 1h and in exsiccator, be dissolved in a small amount of water, then proceed in 1000ml volumetric flask, it is diluted with water to scale, shakes up.
The present invention is compared with prior art, have the following advantages and effect: adopt By Oxygen Bomb Combustion and chemical titration to combine, do not need additionally to build experimental provision, while surveying caloric value, complete release and the absorption of chlorine in coal, can carry out absorbing the quantitative titration of liquid, with low cost, simple to operate, large-scale promotion application suitable in each coal testing laboratory by pipeline system.
Accompanying drawing explanation
Fig. 1 is the distribution schematic diagram of the chlorine content in coal obtained by assay method in the embodiment of the present invention 3.
Detailed description of the invention
Below in conjunction with accompanying drawing and by embodiment, the present invention is described in further detail, and following example are explanation of the invention and the invention is not limited in following example.
Embodiment 1.
Measuring sample in the present embodiment is chlorine standard substance in a kind of coal, and in coal, the operating procedure of the assay method of chlorine is as follows.
1) accurately weigh uniform sample 1 ± 0.1g(and be accurate to 0.0001g), it is placed in combustion boat, adding 10mL weight/mass percentage composition in oxygen bomb is the sodium carbonate liquor of 5%, carefully tighten oxygen bomb lid, the oxygen bomb installed is inserted in calorimeter, slowly it is filled with 2.0MPa～3.0MPa oxygen, by calorimeter operation sequence, sample is lighted.
2), after combustion test terminates, oxygen bomb takes out after cooling 10min in cooling water, is at the uniform velocity discharged lentamente by pressure within no less than the time of 2min.
3) open oxygen bomb, fully clean each several part in oxygen bomb (including inside and outside bullet bucket, vent valve, combustion boat and combustion residue) with a branch of thin hot water.Whole wash pools in a beaker (fixing fabric structure is at about 80mL).
4) in washing liquid, add 1 drip phenolphthalein indicator, it is adjusted to red disappearance with concentrated nitric acid, after amount 5mL, 5mL0.1mg/L sodium chloride standard solution and 5mL0.025mol/L standard silver nitrate solution is accurately added with transfer pipet, place 2-3min, add 2-5mL hexanol cap upper surface ware, beaker is placed on magnetic stirring apparatus quickly after stirring 2-3min, adds 1mL ammonium ferric sulfate indicator.
5) with the standard potassium thiocyanate solution titration demarcated, when solution is become light orange by milky, it is terminal, writes down the volume of potassium thiocyanate solution.
6) measure every a collection of coal sample, perform twice at above blank determination (being not added with coal sample) by above step, take its arithmetic mean of instantaneous value as blank value.Chlorine content in coal calculates according to formula
In formula: CladFor the content of chlorine in air-dried basis coal sample, unit is %；0.03545 is mM quality of chlorine, and unit is g/mmol；C is the thing mass concentration of potassium thiocyanate, and unit is mmol/mL；V1Potassium thiocyanate consumption during for mensuration coal sample, unit is mL；V2Potassium thiocyanate solution consumption during for measuring blank, unit is mL；M is air-dried sample quality, and unit is g.
Measurement result is in Table 1.
From the measurement result of table 1, mark coal measured value is in the uncertain region of standard value, and the repeatability of measurement is good.
Embodiment 2.
For the situation that domestic chlorine content in coal is generally relatively low, therefore the standard substance of another kind of low chlorine is measured again by the present embodiment, and in coal, the assay method of chlorine comprises the following steps that.
1) accurately weigh uniform sample 1 ± 0.1g(and be accurate to 0.0001g), it is placed in combustion boat, adding 10mL weight/mass percentage composition in oxygen bomb is the sodium carbonate liquor of 5%, carefully tighten oxygen bomb lid, the oxygen bomb installed is inserted in calorimeter, slowly it is filled with 2.0MPa～3.0MPa oxygen, by calorimeter operation sequence, sample is lighted.
2), after combustion test terminates, oxygen bomb takes out after cooling 10min in cooling water, is at the uniform velocity discharged lentamente by pressure within no less than the time of 2min.
3) open oxygen bomb, fully clean each several part in oxygen bomb (including inside and outside bullet bucket, vent valve, combustion boat and combustion residue) with a branch of thin hot water.Whole wash pools in a beaker (fixing fabric structure is at about 80mL).
4) in washing liquid, add 1 drip phenolphthalein indicator, it is adjusted to red disappearance with concentrated nitric acid, after amount 5mL, 5mL0.1mg/L sodium chloride standard solution and 5mL0.025mol/L standard silver nitrate solution is accurately added with transfer pipet, place 2-3min, add 2-5mL hexanol cap upper surface ware, beaker is placed on magnetic stirring apparatus quickly after stirring 2-3min, adds 1mL ammonium ferric sulfate indicator.
5) with the standard potassium thiocyanate solution titration demarcated, when solution is become light orange by milky, it is terminal, writes down the volume of potassium thiocyanate solution.
6) measure every a collection of coal sample, perform twice at above blank determination (being not added with coal sample) by above step, take its arithmetic mean of instantaneous value as blank value.Chlorine content in coal calculates according to formula
In formula: CladFor the content of chlorine in air-dried basis coal sample, unit is %；0.03545 is mM quality of chlorine, and unit is g/mmol；C is the thing mass concentration of potassium thiocyanate, and unit is mmol/mL；V1Potassium thiocyanate consumption during for mensuration coal sample, unit is mL；V2Potassium thiocyanate solution consumption during for measuring blank, unit is mL；M is air-dried sample quality, and unit is g.
Measurement result is in Table 2.
Measurement result from table 2, although measurement reproducibility is slightly deteriorated, but mark coal measured value is still in the uncertain region of standard value.It follows that present invention may be broadly applicable to the rapid and accurate determination of chlorine in coal.
Embodiment 3.
Chlorine in the coal of certain main burning coal in thermoelectricity coal-burning power plant of group domestic has been carried out batch and has measured by the present embodiment, and in coal, the assay method of chlorine comprises the following steps that.
1) accurately weigh uniform sample 1 ± 0.1g(and be accurate to 0.0001g), it is placed in combustion boat, adding 10mL weight/mass percentage composition in oxygen bomb is the sodium carbonate liquor of 5%, carefully tighten oxygen bomb lid, the oxygen bomb installed is inserted in calorimeter, slowly it is filled with 2.0MPa～3.0MPa oxygen, by calorimeter operation sequence, sample is lighted.
2), after combustion test terminates, oxygen bomb takes out after cooling 10min in cooling water, is at the uniform velocity discharged lentamente by pressure within no less than the time of 2min.
3) open oxygen bomb, fully clean each several part in oxygen bomb (including inside and outside bullet bucket, vent valve, combustion boat and combustion residue) with a branch of thin hot water.Whole wash pools in a beaker (fixing fabric structure is at about 80mL).
4) in washing liquid, add 1 drip phenolphthalein indicator, it is adjusted to red disappearance with concentrated nitric acid, after amount 5mL, 5mL0.1mg/L sodium chloride standard solution and 5mL0.025mol/L standard silver nitrate solution is accurately added with transfer pipet, place 2-3min, add 2-5mL hexanol cap upper surface ware, beaker is placed on magnetic stirring apparatus quickly after stirring 2-3min, adds 1mL ammonium ferric sulfate indicator.
5) with the standard potassium thiocyanate solution titration demarcated, when solution is become light orange by milky, it is terminal, writes down the volume of potassium thiocyanate solution.
6) measure every a collection of coal sample, perform twice at above blank determination (being not added with coal sample) by above step, take its arithmetic mean of instantaneous value as blank value.Chlorine content in coal calculates according to formula
In formula: CladFor the content of chlorine in air-dried basis coal sample, unit is %；0.03545 is mM quality of chlorine, and unit is g/mmol；C is the thing mass concentration of potassium thiocyanate, and unit is mmol/mL；V1Potassium thiocyanate consumption during for mensuration coal sample, unit is mL；V2Potassium thiocyanate solution consumption during for measuring blank, unit is mL；M is air-dried sample quality, and unit is g.
In a collection of coal, chlorine measurement result is shown in Fig. 1, therefrom selects the coal of three kinds of different chlorinities representatively, and measurement result is in Table 3.
In addition; it should be noted that; described specific embodiment can be made various amendment or supplements or adopt similar mode to substitute by those skilled in the art; without departing from the structure of the present invention or surmount the scope that present claims book is defined, protection scope of the present invention all should be belonged to.
Claims (7)
1. the assay method of chlorine in a coal, it is characterized in that: described assay method utilizes heating-value determination process in coal, complete the release of chlorine in coal, and after absorbed liquid collection, the pH value of liquid, mark-on and precipitation process is absorbed by regulating, finally by standard potassium thiocyanate solution titration, thus measuring the content of chlorine in coal fast and accurately.
2. the assay method of chlorine in coal according to claim 1, it is characterised in that: the step of described assay method is as follows:
1) uniform sample 1 ± 0.1g is accurately weighed, it is placed in the combustion boat in oxygen bomb, adding 10mL mass percentage concentration in oxygen bomb is the sodium carbonate liquor of 5%, carefully tighten oxygen bomb lid, oxygen bomb after installing is inserted in calorimeter, slowly it is filled with 2.0MPa～3.0MPa oxygen, by calorimeter operation sequence, sample is lighted；
2), after combustion test terminates, oxygen bomb takes out after cooling 10min in cooling water, is at the uniform velocity discharged lentamente by pressure within be more than or equal to the time of 2min；
3) open oxygen bomb, fully clean the various piece in oxygen bomb with a branch of thin hot water, whole wash pools in a beaker；
4) in washing liquid, add 1 phenolphthalein indicator, it is adjusted to red disappearance with concentrated nitric acid, after amount 5mL concentrated nitric acid, the sodium chloride standard solution that 5mL concentration is 0.1mg/L and the standard silver nitrate solution that 5mL concentration is 0.025mol/L is accurately pipetted in beaker with transfer pipet, place 2-3min, add 2-5mL hexanol, cap upper surface ware, beaker is placed on magnetic stirring apparatus quickly after stirring 2-3min, adds 1mL ammonium ferric sulfate indicator；
5) with the standard potassium thiocyanate solution titration demarcated, when solution is become light orange by milky, it is terminal, writes down the volume of potassium thiocyanate solution；
6) measure every a collection of coal sample, perform twice at above blank determination by above step, take its arithmetic mean of instantaneous value as blank value；The computing formula of chlorine content in coal is
In formula: CladFor the content of chlorine in air-dried basis coal sample, unit is %；0.03545 is mM quality of chlorine, and unit is g/mmol；C is the thing mass concentration of potassium thiocyanate, and unit is mmol/mL；V1Potassium thiocyanate consumption during for mensuration coal sample, unit is mL；V2Potassium thiocyanate solution consumption during for measuring blank, unit is mL；M is air-dried sample quality, and unit is g.
3. the assay method of chlorine in coal according to claim 2, it is characterised in that: described assay method is applicable to the mensuration of brown coal, bituminous coal and smokeless chlorine content in coal.
4. the assay method of chlorine in coal according to claim 2, it is characterised in that: if finding after By Oxygen Bomb Combustion that coal sample is splashed or uncombusted, should adopt an effective measure and again test, it is ensured that in coal, chlorine all discharges and is absorbed by liquid absorption.
5. the assay method of chlorine in coal according to claim 2, it is characterized in that: the preparation steps of standard silver nitrate solution is as follows: accurately weigh the standard reagent silver nitrate 4.2472g being cooled to room temperature in advance after 110 DEG C of dry 1h and in exsiccator, it is dissolved in a small amount of water, proceed to again in 1000ml volumetric flask, be diluted with water to graduation mark.
6. the assay method of chlorine in coal according to claim 2, it is characterised in that: the preparation of standard potassium thiocyanate solution and demarcating steps be: weighs 2.5g potassium thiocyanate soluble in water, then proceeds in 1000mL volumetric flask, is diluted with water to scale, shakes up；10mL silver nitrate standard solution is accurately pipetted with transfer pipet, inject 50mL water, 3ml nitric acid and 1ml ammonium ferric sulfate indicator, it is titrated to solution with potassium thiocyanate standard solution to be become light orange from milky and be terminal, write down potassium thiocyanate solution consumption, carry out 4-8 time to demarcate, using the meansigma methods of repeatedly consumption as consumption volume, according to formula c=V0× k/V calculates the concentration of potassium thiocyanate solution, and in formula, c is the concentration of potassium thiocyanate solution, unit mmol/mL；V0For silver nitrate standard solution consumption, unit is mL；K is the concentration value of silver nitrate standard solution, and in 0.0250, unit is mol/L；V is the consumption of potassium thiocyanate standard solution, and unit is mL.
7. the assay method of chlorine in coal according to claim 2, it is characterized in that: the preparation steps of sodium chloride standard solution is: accurately weigh the top grade pure sodium chloride 0.1649g being cooled to room temperature in advance after 500-600 DEG C of calcination 1h and in exsiccator, it is dissolved in a small amount of water, proceed in 1000ml volumetric flask again, it is diluted with water to scale, shakes up.
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Cited By (3)
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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 |
| CN110431414A (en) * | 2017-08-18 | 2019-11-08 | 株式会社Lg化学 | The quantitative analysis method of Cl is remained in zinc ferrite |
| CN112198266A (en) * | 2020-11-07 | 2021-01-08 | 山西省疾病预防控制中心 | Method for measuring chlorine content in coal and coal gasification products |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110431414A (en) * | 2017-08-18 | 2019-11-08 | 株式会社Lg化学 | The quantitative analysis method of Cl is remained in zinc ferrite |
| US11249060B2 (en) | 2017-08-18 | 2022-02-15 | Lg Chem, Ltd. | Method for quantitatively analyzing residual Cl in zinc ferrite |
| CN110431414B (en) * | 2017-08-18 | 2022-03-11 | 株式会社Lg化学 | Quantitative analysis method for residual Cl in zinc ferrite |
| 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 |
| CN112198266A (en) * | 2020-11-07 | 2021-01-08 | 山西省疾病预防控制中心 | Method for measuring chlorine content in coal and coal gasification products |
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