CN102253101B - Method for detecting chloride ions in polyisobutylene - Google Patents
Method for detecting chloride ions in polyisobutylene Download PDFInfo
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- CN102253101B CN102253101B CN 201110116339 CN201110116339A CN102253101B CN 102253101 B CN102253101 B CN 102253101B CN 201110116339 CN201110116339 CN 201110116339 CN 201110116339 A CN201110116339 A CN 201110116339A CN 102253101 B CN102253101 B CN 102253101B
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- 229920002367 Polyisobutene Polymers 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 title claims abstract description 21
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000001301 oxygen Substances 0.000 claims abstract description 41
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 41
- 239000007788 liquid Substances 0.000 claims abstract description 31
- 238000010521 absorption reaction Methods 0.000 claims abstract description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000460 chlorine Substances 0.000 claims abstract description 13
- 239000002245 particle Substances 0.000 claims abstract description 12
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 9
- 238000003918 potentiometric titration Methods 0.000 claims abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 7
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 62
- 238000004448 titration Methods 0.000 claims description 51
- 239000000243 solution Substances 0.000 claims description 36
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 239000011780 sodium chloride Substances 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 7
- 238000010304 firing Methods 0.000 claims description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 150000002500 ions Chemical class 0.000 claims description 5
- 238000012360 testing method Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 239000011435 rock Substances 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 230000001186 cumulative effect Effects 0.000 claims description 3
- 238000002474 experimental method Methods 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 3
- 238000003760 magnetic stirring Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000004570 mortar (masonry) Substances 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 2
- 239000012088 reference solution Substances 0.000 claims description 2
- 230000010076 replication Effects 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 14
- 229920000642 polymer Polymers 0.000 abstract description 6
- 238000002485 combustion reaction Methods 0.000 abstract description 4
- 229920000098 polyolefin Polymers 0.000 abstract description 4
- 238000010791 quenching Methods 0.000 abstract description 4
- 230000000171 quenching effect Effects 0.000 abstract description 4
- 238000000227 grinding Methods 0.000 abstract description 3
- 239000007787 solid Substances 0.000 abstract description 3
- 229910052736 halogen Inorganic materials 0.000 abstract description 2
- 150000002367 halogens Chemical class 0.000 abstract description 2
- 238000001556 precipitation Methods 0.000 abstract 1
- 241000370738 Chlorion Species 0.000 description 21
- 239000000126 substance Substances 0.000 description 4
- 239000012086 standard solution Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 150000002605 large molecules Chemical class 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229920000620 organic polymer Polymers 0.000 description 2
- 101710134784 Agnoprotein Proteins 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012490 blank solution Substances 0.000 description 1
- 235000012206 bottled water Nutrition 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- -1 halide ions Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 238000006213 oxygenation reaction Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
Abstract
The invention discloses a method for detecting chloride ions in polyisobutylene and belongs to a detection method of a halogen element, especially to a detection method of a chlorine element in a high-molecular polymer. The method for detecting chloride ions in polyisobutylene mainly comprises the following steps of: (1) polyisobutylene pretreatment: letting a polyisobutylene sample embrittle at low temperature in liquid nitrogen and grinding the sample into particles with the particle size being 100-200 microns; (2) letting the sample combust in an oxygen combustion bottle containing an absorption solution by charging oxygen, and letting chloride ions be fully absorbed by the absorption solution; (3) detecting the content of chloride ions in the absorption solution by the potentiometric titration method; (4) calculating the content of chloride ions in polyisobutylene. By adopting the liquid-nitrogen quenching method, polyisobutylene becomes a brittle solid and is processed into particles with small size to guarantee the complete combustion of polyisobutylene and the effective precipitation of chloride ions, so as to make it possible to precisely detect the content of chloride ions in the polyisobutylene polymer. The technical scheme provided by the invention is also suitable for the detection of chloride ions in other polyolefin polymers.
Description
Technical field
The invention belongs to the detection method of chlorine element in the detection method of halogen element, particularly polyolefin.
Background technology
The chlorine element is present in many polymeric materials.For the detection of chlorion, but mostly concentrate on the detection of chlorion in the aqueous solution.Detect such as chlorion in the boiler water; Chlorion detects in the alkaline aqueous solution; Chlorion detects in the lime slurry; Chlorion detects in the potable water, and chlorion detection etc. in the sewage.Method mainly contains conductimetric method, potentiometric titration, conventional chemical titrimetry, ion photometer measuring method and the chromatography of ions.In above-mentioned all multi-methods, testing sample is the solution that the chlorine element exists with ionic condition.For the polyisobutylene polymkeric substance of jelly, can not directly adopt said method, need first the chloride ions in polyisobutylene separation and Extraction out.Traditional methods such as dissolution extraction are not suitable for polyisobutylene, because chlorion absorption, be coated in the large molecule of organic polymer, can't water directly dissolve or extract.
The detection of chlorion also has patent report in the organism, detects chlorion detection etc. in the smooth liquid such as chlorion in the organic amine.Among the patent documentation CN101587093, provide to relate to chlorine ion content determination method, related in particular to the chlorine ion content determination method in the alkaline solution.The foundation of this invention wet-leveling liquid chlorine ion content determination method has mainly been adopted the method for calcining so that fetter the organic amine material carbonization of chlorion, forms the inorganics of solubility, causes chlorion free out, thereby utilizes potentiometric titration to record.
Summary of the invention
The purpose of this invention is to provide a kind of polyisobutylene chlorion detection method.
Technical scheme of the present invention is: (1) polyisobutylene pre-service: get 3.0～8.0g polyisobutylene sample, and low temperature brittleness in liquid nitrogen, temperature adopts mortar sample to be ground into the particle of particle diameter 100～200 μ m at-120～-170 ℃;
(2) burning: take by weighing the polyisobutylene sample that 0.02～2.00g grinds, put into the platinum basket firing chamber of oxygen Molotov cocktail, add in advance 5.0～50.0mL absorption liquid in the oxygen Molotov cocktail, screw oxygen Molotov cocktail screw-cap, connect oxygen bottle, the logical oxygen 2.0min of flow velocity with 1.0～5.0L/min, after being full of oxygen in the oxygen Molotov cocktail, disconnect rapidly logical oxygen system, the oxygen Molotov cocktail that fills sample is put into burner, close the burner door, press switch, light source can continuous firing 5～20 seconds, ignite and burn complete sample.
(3) collect absorption liquid: take out the oxygen Molotov cocktail, repeatedly rock, make the ion on the oxygen Molotov cocktail inwall be dissolved in absorption liquid fully, leave standstill a period of time, slowly turn on vice, absorption liquid is transferred in the beaker, water cleaning down oxygen Molotov cocktail, cleansing solution is incorporated in the beaker, makes cumulative volume at 20mL.
(4) titration: install titration apparatus, the silver nitrate standard titration solution is added in the buret, put magneton in filling the beaker of absorption liquid, beaker is placed on the magnetic stirring apparatus,
A. electrode is inserted in the detected solution, namely can read electrode potential E (mV) value,
B. regulate " terminal point current potential " knob, make to show that the terminal point current potential is setting value, after the terminal point current potential was selected, " terminal point current potential " knob can not move again,
C. terminal point current potential and pre-control point potential setting good after, open stirrer source, reconcile rotating speed and make and stir from accelerating at a slow speed to suitable rotating speed,
D. press " titration begins " button, instrument namely begins titration, and dropping liquid drips fast, and near terminal point the time, titration is slowed down, and when reaching home, the titration lamp is no longer glittering, and the terminal point lamp is bright, and titration finishes,
E. in the titration process, record liquid volume reading V (mL) and corresponding E value in the buret.During near terminal point, every adding 0.1mL liquor argenti nitratis ophthalmicus is write down its corresponding E value,
Do parallel experiment and blank test with the same terms.
The quality percentage composition W of chlorine
ClCalculating
The quality percentage composition W of chlorine
ClCalculate by (1):
In the formula: V
1-be titrated to the volume of the required silver nitrate standard titration solution of terminal point, mL;
V
0The volume of the blank required silver nitrate standard titration solution of-titration, mL;
C-silver nitrate (AgNO
3) concentration of standard titration solution, mol/L;
The quality of m-sample, mg,
Described absorption liquid is water or alkali lye.
Described silver nitrate standard titration solution: C
(AgNO3)=0.02mol/L.
Its preparation method is: the standard solution preparation
Sulfuric acid, ρ=1.84g/mL.
0.02mol/L sodium chloride reference solution: take by weighing 1.17g benchmark sodium chloride, soluble in water, be diluted with water to 1000mL.
The silver nitrate standard titration solution
(1) preparation of silver nitrate standard titration solution: a certain amount of silver nitrate is dissolved in the 1.0L water, shakes up, solution is stored in the brown bottle.
(2) demarcation of silver nitrate standard titration solution: accurately measure the 5.0mL sodium chloride solution in beaker, be diluted with water to 25.0mL, add 2 sulfuric acid, put into magneton, on stirrer, carry out automatic potentiometric titration, draw millivolt reading to the curve of silver nitrate standard titration solution volume, the volume of Δ E/ Δ V-V curve peak titrant that consumes during corresponding to titration end-point, replication is once;
(3) calculate
The concentration C of silver nitrate standard titration solution, calculate by formula (2):
In the formula: the concentration of C-silver nitrate (AgNO3) standard titration solution, mol/L;
The quality of m-sodium chloride, g;
The V-titration end-point consumes silver nitrate standard titration solution volume, mL.
The silver nitrate standard titration solution rushes rare 10 times, is used for potentiometric titration.
The ultimate principle of the technical program is: sample is the oxygenation burning in containing the oxygen Molotov cocktail of absorption liquid, and carbon and hydrogen in the polymkeric substance are oxidized, and Chloride residue rocks the oxygen Molotov cocktail, and leaves standstill a period of time at the bottle inwall, and residual chlorion is fully absorbed.With the chlorinity in the potentiometric determination absorption liquid, thereby calculate the content of chloride ions in polyisobutylene.
The granule size that experiment showed, the polyisobutylene sample is most important for the accuracy of detection architecture.Same sample when grinding particle size is 1.0mm, is compared for≤200 μ m test results with grinding particle size, and error is about 14～15%.Granularity is large, and the content of chlorion is on the low side in the testing result, the interpret sample incomplete combustion, and chlorion is not released fully, does not adopt liquid nitrogen quenching embrittlement method, and sample can't be ground into≤molecule of 200 μ m.
The invention has the beneficial effects as follows: 1. polyisobutylene belongs to high molecular polymer, and molecular weight is from several thousand to up to a million.With the increase of molecular weight product, outward appearance becomes from thick liquid and is elastic solid (Hookean body).Polyisobutylene often contains trace impurity, such as chlorine element etc.Because the chlorine element adsorbs and is covered by in the large molecule of organic polymer, be difficult to separate, therefore can't adopt the conventional method direct-detection.The present invention adopts liquid nitrogen quenching embrittlement method, make polyisobutylene become brittle solid, and be treated to very little granularity, can guarantee the polyisobutylene burning fully, chlorion is effectively separated out, so that the chlorion detection becomes possibility in the polyisobutylene polymkeric substance, this technical scheme detects same applicable to chlorion in other polyolefin polymers.
2. adopted special oxygen Molotov cocktail, make sample perfect combustion in containing the oxygen Molotov cocktail of absorption liquid, carbon in the organism and hydrogen are oxidized to be removed, chlorion remains in bottle interior absorption liquid fully, can adopt easily the chlorinity in the potentiometric determination absorption liquid, thereby calculate the content of chloride ions in polyisobutylene
3. the technical program adopts the potentiometric determination chloride ion content, and degree of accuracy high (it is following to be accurate to 5ppm) is the convenience that detects content of halide ions in the polyolefins high polymer, reliable method.
Embodiment
Embodiment 1
Get 5.0g polyisobutylene sample (HRD-350), sample temperature is at-120～-170 ℃ behind the liquid nitrogen quenching, in mortar, grind rapidly to granularity for≤200 μ m, sample is divided into five parts, accurately take by weighing example weight and make error≤0.1mg, sample is put into platinum basket firing chamber, put into the oxygen Molotov cocktail of prior adding 10.0mL water, screw oxygen Molotov cocktail screw-cap, connect oxygen bottle, the logical oxygen 2min of flow velocity with 3.0L/min after being full of oxygen in the oxygen Molotov cocktail (oxygen pressure of generation should be lower than the safe air pressure of manufacturer's regulation), disconnects rapidly logical oxygen system.The oxygen Molotov cocktail that fills sample is put into burner, closes the burner door, press " START " switch, light source can continuous firing 10 seconds, ignite sample and burning fully.
Open sample gate, take out the oxygen Molotov cocktail.Repeatedly rock the oxygen Molotov cocktail, so that the ion on the bottle inwall is fully soluble in water.Leave standstill a period of time, slowly turn on vice, absorption liquid is transferred in the beaker, water cleaning down sample interior, cleansing solution is incorporated in the beaker, makes cumulative volume about 20.0mL.
Install titration apparatus, the silver nitrate standard titration solution is added in the buret, put magneton in filling the beaker of absorption liquid, beaker is placed on the magnetic stirring apparatus.Turn on the power switch, power light is bright, after preheating in 15 minutes, and the beginning titration, the record titration end-point consumes silver nitrate standard solution (M=0.001mol/L) volume reading V (mL).
According to above-mentioned steps, under the condition that does not add the polyisobutylene sample, measure blank solution and consume silver nitrate standard solution (M=0.001mol/L) volume V
0(mL), measurement result sees Table one.
Table one, HRD-350 sample determination of chloride ion result (sample particle diameter≤200 μ m)
Embodiment 2
Get 5.0g polyisobutylene sample (HRD-550), operation steps is with embodiment 1, and the pretreatment sample particle diameter is less than 200 μ m, and measurement result sees Table two.
Table two, HRD-550 sample determination of chloride ion result, sample particle diameter≤200 μ m.
Claims (3)
1. method for detecting chloride ions in polyisobutylene is characterized in that:
(1) polyisobutylene pre-service: get 3.0～8.0g polyisobutylene sample, low temperature brittleness in liquid nitrogen, temperature adopts mortar sample to be ground into the particle of particle diameter 100～200 μ m at-120～-170 ℃;
(2) burning: take by weighing the polyisobutylene sample that 0.02～2.00g grinds, put into the platinum basket firing chamber of oxygen Molotov cocktail, add in advance 5.0～50.0mL absorption liquid in the oxygen Molotov cocktail, screw oxygen Molotov cocktail screw-cap, connect oxygen bottle, the logical oxygen 2.0min of flow velocity with 1.0～5.0L/min, after being full of oxygen in the oxygen Molotov cocktail, disconnect rapidly logical oxygen system, the oxygen Molotov cocktail that fills sample is put into burner, close the burner door, press switch, light source can continuous firing 5～20 seconds, ignite and burn complete sample;
(3) collect absorption liquid: take out the oxygen Molotov cocktail, repeatedly rock, make the ion on the oxygen Molotov cocktail inwall be dissolved in absorption liquid fully, leave standstill a period of time, slowly turn on vice, absorption liquid is transferred in the beaker, water cleaning down oxygen Molotov cocktail, cleansing solution is incorporated in the beaker, makes cumulative volume at 20mL;
(4) potentiometric titration: install titration apparatus, the silver nitrate standard titration solution is added in the buret, put magneton in filling the beaker of absorption liquid, beaker is placed on the magnetic stirring apparatus;
A. electrode is inserted in the detected solution, namely can read electrode potential E value, the unit of E is mV,
B. regulate " terminal point current potential " knob, make to show that the terminal point current potential is setting value, after the terminal point current potential was selected, " terminal point current potential " knob can not move again,
C. terminal point current potential and pre-control point potential setting good after, open stirrer source, reconcile rotating speed and make and stir from accelerating at a slow speed to suitable rotating speed,
D. press " titration begins " button, instrument namely begins titration, and dropping liquid drips fast, and near terminal point the time, titration is slowed down, and when reaching home, the titration lamp is no longer glittering, and the terminal point lamp is bright, and titration finishes,
E. in the titration process, record liquid volume reading V and corresponding E value in the buret, the unit of V is mL, and during near terminal point, every adding 0.1mL liquor argenti nitratis ophthalmicus is write down its corresponding E value,
Do parallel experiment and blank test with the same terms,
The quality percentage composition WC1 of chlorine calculates by formula (1):
In the formula (1): V
1-be titrated to the volume of the required silver nitrate standard titration solution of terminal point, mL;
V
0The volume of the blank required silver nitrate standard titration solution of-titration, mL;
The concentration of c-silver nitrate standard titration solution, mol/L;
The quality of m-sample, mg.
2. by method for detecting chloride ions in polyisobutylene claimed in claim 1, it is characterized in that: described absorption liquid is water or alkali lye.
3. by method for detecting chloride ions in polyisobutylene claimed in claim 1, it is characterized in that: the concentration c=0.02mol/L of described silver nitrate standard titration solution, its preparation method is:
The sulfuric acid of preparation ρ=1.84g/mL,
Preparation 0.02mol/L sodium chloride reference solution: take by weighing 1.17g benchmark sodium chloride, soluble in water, be diluted with water to 1000mL,
Preparation silver nitrate standard titration solution: a certain amount of silver nitrate is dissolved in the 1.0L water, shakes up, solution is stored in the brown bottle;
Demarcate the silver nitrate standard titration solution: accurately measure the 5.0mL sodium chloride solution in beaker, be diluted with water to 25.0mL, add 2 sulfuric acid, put into magneton, on stirrer, carry out automatic potentiometric titration, draw a millivolt reading E
2To silver nitrate standard titration solution volume V
2Curve, Δ E
2/ Δ V
2-V
2The volume of curve peak titrant that consumes during corresponding to titration end-point, replication is once;
Calculate the concentration C of silver nitrate standard titration solution by formula (2):
In the formula (2): the concentration of C-silver nitrate standard titration solution, mol/L;
m
2The quality of-sodium chloride, g;
V
2-titration end-point consumes silver nitrate standard titration solution volume, mL;
The silver nitrate standard titration solution rushes rare 10 times, is used for the potentiometric titration of step (4).
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| CN102565230B (en) * | 2012-01-09 | 2013-12-11 | 山东大学 | Detection method of free chlorine ions in polyisobutylene |
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| CN105954343A (en) * | 2016-04-26 | 2016-09-21 | 重庆鹏凯精细化工有限公司 | Device for rapid determination of content of sodium chloride in hydroxyethyl/hydroxypropyl methyl cellulose |
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