CN1351257A - Method for measuring content of Cl element and its burner - Google Patents
Method for measuring content of Cl element and its burner Download PDFInfo
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- CN1351257A CN1351257A CN 01129969 CN01129969A CN1351257A CN 1351257 A CN1351257 A CN 1351257A CN 01129969 CN01129969 CN 01129969 CN 01129969 A CN01129969 A CN 01129969A CN 1351257 A CN1351257 A CN 1351257A
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- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000000460 chlorine Substances 0.000 claims abstract description 31
- 238000010438 heat treatment Methods 0.000 claims abstract description 25
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 21
- 238000009841 combustion method Methods 0.000 claims abstract description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 15
- 239000000523 sample Substances 0.000 claims description 15
- 238000010521 absorption reaction Methods 0.000 claims description 13
- 241000370738 Chlorion Species 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 12
- 238000004061 bleaching Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 8
- 150000002500 ions Chemical class 0.000 claims description 7
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims description 5
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 4
- 238000009413 insulation Methods 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 239000004332 silver Substances 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 3
- 239000012670 alkaline solution Substances 0.000 claims description 2
- 239000012528 membrane Substances 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 9
- 238000002485 combustion reaction Methods 0.000 abstract description 4
- 239000003513 alkali Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 239000002351 wastewater Substances 0.000 description 9
- 239000003708 ampul Substances 0.000 description 7
- 238000003556 assay Methods 0.000 description 7
- 239000010453 quartz Substances 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 238000005660 chlorination reaction Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000035807 sensation Effects 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 239000007844 bleaching agent Substances 0.000 description 2
- -1 chloro phenol compound Chemical class 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- KVGZZAHHUNAVKZ-UHFFFAOYSA-N 1,4-Dioxin Chemical compound O1C=COC=C1 KVGZZAHHUNAVKZ-UHFFFAOYSA-N 0.000 description 1
- 241000251468 Actinopterygii Species 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 238000004616 Pyrometry Methods 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 208000031320 Teratogenesis Diseases 0.000 description 1
- YPWFISCTZQNZAU-UHFFFAOYSA-N Thiane Chemical compound C1CCSCC1 YPWFISCTZQNZAU-UHFFFAOYSA-N 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 230000033558 biomineral tissue development Effects 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 238000010411 cooking Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 150000002240 furans Chemical class 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 230000001089 mineralizing effect Effects 0.000 description 1
- 231100000350 mutagenesis Toxicity 0.000 description 1
- 231100000299 mutagenicity Toxicity 0.000 description 1
- 230000007886 mutagenicity Effects 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
A method for measuring the content of Cl element features that a high-temp combustion method is used to convert organic chlorine to inorganic one and after it is absorbed by alkali solution, its content is measured by electric level method. Its combustion equipment is composed of thermal reaction tube, heating tubes parallelly arranged to surround the thermal reaction tube and insulating layer wrapping said tubes. Its advantages include simple operation, high correctness, short measuring time and low cost.
Description
The present invention relates to a kind of assay method and burner thereof of chlorine element.
Recent two decades comes, and the paper industry of China has obtained very big development, but the harm of cooking waste liquor to environment is only noted in the environmental protection aspect, and that be concerned about is BOD
5, COD, TSS and colourity, and the sight of west paper industry developed country environmental protection has changed into from these traditional parameters and has paid attention to bleaching effluent to impact and harm that environment caused.Though many chlorine-free bleaching methods are constantly being developed and are being promoted, but traditional method of chlorine bleach cheaply is still in a large amount of uses, because of lignin degradation product and the chlorine-containing bleaching reaction that contains in the chlorine bleach waste water (acid waste water, alkaline waste water), its organic chloride of phenols chemical combination that produces, mainly be chloro phenol compound, its pollution character can be summarized as the following aspects: (1): COD in the bleaching effluent, BOD loading are bigger.Main it consumes a large amount of oxygen in water because contain a large amount of dissolved organic matters in the bleaching effluent, reduces the dissolved oxygen DO in the water, harm fish and other hydrobiological existence; (2): colourity is higher, especially back segment waste water; (3): strong toxicity, contain toxic very strong material in the bleaching effluent, mainly be the chlorination organism, they are all toxic to hydrobiont; (4): teratogenesis, mutagenicity, studies show that multiple biological induced-mutation material, particularly chlorinated diphenyl hydrazone furans are arranged in the bleaching effluent, can change biological heredity.The organic kind of chlorination is a lot, complicated component, it contains phenol, aldehyde, ketone, acid, ester, dioxin, furans and other intermediate etc. of chlorination, and every kind of compound proportion is different because of the difference of manufacturing condition, different along with the difference of raw material, there is not relative proportionate relationship.This just can not be with the number that other compound exists of how much understanding of calibrating compound.
In order to adapt to the needs that environmental protection and production control detect, the analytical approach of content of Cl element is arisen at the historic moment in the various mensuration water, and what wherein applicability was bigger has: the mensuration of total organochlorine (Total Organic Chlorine), be called for short TOCl; The mensuration of absorption organochlorine (Adsorbable Organic Chlorine) is called for short AOCl; And method of organic solvent extraction (Solvent-ExtratableChlorined Organic Matter), be called for short EOCl.The key of these three kinds of analytical approachs all is organic chlorides of collecting as much as possible in the water sample, and then at high temperature (more than 1000 ℃) make organochlorine change inorganic chlorine into oxidation operation, determines organochlorine with the content of measuring inorganic chlorine.The mensuration of TOCl makes molecular-weight gradation by ultrafiltration, again by XAD resin enrichment organochlorine, by the Schoniger burning, makes mineralization of organic material again, generates CO
2, H
2O, HCl use liquor argenti nitratis ophthalmicus titration inorganic chlorine ion wherein at last, carry out chemical analysis.AOCl is enriched with organic compounds by charcoal absorption, and separates removal inorganic chlorine ion with the sodium nitrate washing, and also through mineralizing, organic chloride generates CO in Oxygen Flow
2, H
2O, HCl use the content of microcoulombmeter titration measuring chlorion again.EOCl technology organic solvent (as thiacyclohexane, isopropyl alcohol and heptane) interrupted extraction, the solvent of getting 10-20ul after the extraction burns, and the chlorion after the burning is measured with microcoulometry.Though these assay method accuracy are high, the analysis cost costliness, for the conventional analysis of waste water time-consuming too, step is also complicated, and the papermaking enterprise and the R﹠D institution that can't be fit to China at present use.
And all assay methods all need organochlorine is changed into inorganic chlorine by burning, are measured again, and temperature of combustion will reach 1000 ℃ at least could be with the organochlorine burning fully.Existing burner is to make reaction tube heating or built-in high temperature silk or high temperature rod make the reaction tube heating around the high temperature silk outside utilizing.It is slow that this burner adds heat conduction, and if high temperature silk or high temperature rod fracture takes place changes also cumbersome.
The assay method that the purpose of this invention is to provide a kind of content of Cl element, it not only has higher accuracy, and simple and easy to do.
Another object of the present invention provides a kind of burner in this assay method, and it is fast that this device not only has heat conduction, the characteristics that the thermal efficiency is high, and also the replacing of high temperature silk is also simple.
The method of mensuration content of Cl element provided by the invention is to take high-temperature combustion method that the organochlorine in the determinand is transformed into inorganic chlorine earlier, absorb with alkaline solution, absorption liquid takes potential method to measure the wherein content of chlorine element again, its potential electrode is made up of chloride ion-selective electrode and contrast electrode, described potential electrode is inserted in the described absorption liquid, measure the electrode potential V between the described potential electrode, according to formula V=E
0+ (2.303RT/F) logK
Sp(Agcl)-(2.303RT/F) log[cl
-]-E
Ref, calculate the concentration [cl of chlorion in the absorption liquid
-], can converse the content of chlorine element in the determinand;
E wherein
0Be the standard electrode potential of silver electrode,
K
Sp(Agcl) be the ion-product constant of silver chloride,
E
RefBe the contrast electrode electromotive force,
R is a gas law constant,
T is a Kelvin temperature,
F is a Faraday constant.
Contrast electrode commonly used is saturated calomel electrode (SCE), as the mereurous sulfate contrast electrode, and the preferably two salt bridge saturated calomel electrodes of the present invention, outer salt bridge is KNO
3Solution.
It generally is with AgCl-Ag that chlorion is selected electrode
2S is the chloride ion-selective electrode of sensitive membrane, in order to measure Cl in the solution
-A kind of electrochemical sensor of ion.It and contrast electrode insert in the solution to be measured measurement battery then composed as follows: AgCl-Ag
2S (film) ‖ sample solution ‖ contrast electrode.Silver chloride is the ionic conductivity material, and wherein removable particle is a silver, so the electromotive force E of chlorion selection electrode battery, is determined by silver ion activity.Can get thus: E=E
0+ (2.303RT/F) logK
Sp(Agcl)-(2.303RT/F) log[cl
-].
Carrying out potential measurement instrument commonly used has two kinds, and a kind of is pot, and another kind is pH meter (voltage table).The same with the pH glass electrode, most of ion-selective electrodes have high resistance, generally use electrometer or pH meter to carry out direct potential and measure.
Method provided by the invention is particularly useful for organochlorine ion and inorganic chlorine ion determination in the bleaching effluent.
Burner provided by the invention comprises thermal response pipe, heating tube, heat-insulation layer, is connected with heatable high temperature resistance silk in the middle of the heating tube, and at least 3 of heating tubes, parallel ring are around the thermal response pipe, and heat-insulation layer wraps up heating tube and thermal response pipe together.
Wherein heating tube is preferably the 5-8 root.
For A.T.C, this heating arrangement is equipped with temperature controller, is inserted with temp probe 5 in the gap of heating tube 6 and thermal response pipe 2, and the power supply of described high temperature resistance silk links to each other with temperature controller 11 with temp probe 5, to realize the automatic adjusting of temperature.
The present invention utilizes organochlorine ion and the inorganic chlorine ion in firing method and the potential method mensuration bleaching effluent, to improve accuracy, simplifies the operation course.
The present invention is further detailed explanation below in conjunction with the drawings and specific embodiments.
Fig. 1 is the cut-open views of apparatus of the present invention along the A-A direction;
Fig. 2 is the cut-open view of burner of the present invention along the B-B direction.
The present invention is made up of four parts, and first is a sampling device, and second portion is a burner, and third part is a gathering-device, and the 4th part is a determinator.Burner is shown in Figure of description: by a length is 110cm, diameter is that the 20cm quartz ampoule is 30cm as thermal response pipe 2 and six roots of sensation length, diameter be the centre of 20cm be connected with heatable high temperature resistance silk quartz ampoule as heating tube 6, form a combustion and pyrolysis device (resistance of the high temperature silk in each heating tube is 500W).In the heatable quartz ampoule of the six roots of sensation, two at an end that connects positive source is one group and is connected in parallel, receive respectively on three phase lines of three-phase alternating current through exchanging the electric shock device, connect one of power cathode and terminate to together, after exchanging the electric shock device, receive on the zero line of three-phase alternating current.The six roots of sensation heating tube 6 of heating is surrounded thermal response pipe 2, but puts into the temp probe 5 of pyrometry again at the pipe intermediate gaps place of heating.Again these electrodes and temp probe 5 are received the correspondence position that exchanges electric shock device and temperature controller 11 respectively.Temperature just can be regulated automatically like this.Temperature of the present invention will reach more than 1000 ℃ at least.Heat-preservation cotton 4 is twined in the outside of heated quarty tube.
The burner that uses in the assay method of content of Cl element in traditional water is to make reaction tube heating or built-in high temperature silk or high temperature rod make the heating of thermal response pipe around the high temperature silk outside utilizing.It is slow that burner in the past adds heat conduction, and if high temperature silk or high temperature rod fracture takes place changes also cumbersome.The present invention proposes present burner in order to overcome these weak points.Device of the present invention utilizes the radiation conduction heat of quartz ampoule, and the traditional burner of heat transfer ratio is faster, and it is also fairly simple to change the high temperature silk.
Sampling device is with a diameter resistant to elevated temperatures quartz ampoule 3 littler than long tube, and quantitative filter paper is placed in the inside, is used to adsorb the bleaching effluent solution that will measure, enters thermal response pipe 2 by gathering hole 1.Gathering-device is made up of exsiccator 8 and absorption cell 9 two parts, through thermal response pipe 2 high-temp combustions, after organochlorine in the water is transformed into inorganic chlorine, enter exsiccator 8 and absorption cell 9 successively through bend pipe 7, the solution that exsiccator is 8 li is the concentrated sulphuric acid, and the solution that absorption cell is 9 li is that concentration is the sodium hydroxide solution of 0.01mol/L.The liquid of absorption cell 9 is measured wherein content of Cl element with potential method, and determinator is made up of accurate pH meter of PHS-3C type and measuring ion electrode, and potential electrode is made of together PCl--1 type chloride ion-selective electrode and contrast electrode.
The method of chlorine element is simple to operate in the mensuration water provided by the invention, the accuracy height, minute is short and expense is low, be applicable to the daily detection in domestic paper mill and the measuring of R﹠D institution, its burner utilizes the direct radiation heating of quartz ampoule to make the temperature in the thermal response pipe reach necessary requirement, contrasts traditional indirect type heat conduction, conduct heat and want fast, and the high temperature silk is placed on the central authorities of heating tube, changes the high temperature silk easily, operates fairly simple.
Embodiment:
(1): clean sample hose and thermal response long tube with deionized water wash, dry moisture content then.Oxygen supply tracheae and burning quartz ampoule order are according to the rules coupled together, and check whether each interface leaks gas.
(2): connect oxygen valve, aerating oxygen, the adjusting oxygen gas flow rate is 200ml/min, connects with the mains, and the temperature of temperature controller is transferred to 1000 ℃.Install required sample in temperature-rise period in sample hose, it is stand-by in the sample hose to pack into quantitative filter paper absorption 2ml waste liquid.
(3): the temperature on the thermometer is behind predetermined temperature, connect drying device and gathering-device, slowly sample hose is pushed into the preheating section of quartzy long tube then, temperature is roughly 200 ℃～300 ℃, guarantee that the moisture on the quantitative filter paper in the sample hose distributes gradually (to prevent at the beginning sample hose to be put into bringing-up section, moisture content gas is suddenly sent out, and sets off an explosion).After the water evaporates, sample hose is put into the fire end (temperature is 1000 ℃) of long tube, carries out thermal response.
(4): reaction is carried out always, till the moisture content in the question response long tube eliminates fully.And make reaction tube temperature cooling back with the solution washing reaction tube in the receiving flask, and make the inorganic chlorine ion that remains in the pipe enter solution, collect these solution.
(5):, calculate the concentration of chlorion with the solution that pH meter and ion selecting electrode determining are collected.Measure the concentration of the chlorion of waste water before burning again.Both subtract each other is exactly the concentration of organochlorine.The Data Processing in Experiment method is as follows:
The electromotive force of chloride electrode: E
Cl=E
0+ (2.303RT/F) logK
Sp(Agcl)-(2.303RT/F) log[cl
-]
Survey
Contrast electrode electromotive force: E
Ref
Electrode potential: V=E
Cl-E
Ref=E
0+ (2.303RT/F) logK
Sp(Agcl)-(2.303RT/F) log[cl
-]-E
Ref
E
0----------------------------the standard electrode potential of----silver electrode
K
Sp(Agcl)--------------------ion-product constant of-----silver chloride
[cl
-]
Useless=[cl
-]
Survey* extension rate-[cl
-]
Go
[cl
-]
Useless------------------------the content of the chlorine element of-----waste water
[cl
-]
Survey------------------------the content of the chlorine element of-----obtain by test figure
[cl
-]
Go------------------------------content of chlorine element in the deionized water
Before the power taking oxidation reaction, each 2ml of waste water of 3 hours, 6 hours, 9 hours, 12 hours operates according to above experimental technique behind the electro-oxidation reaction respectively.Be respectively 1.11 * 10 by formula calculating content of the chlorion of waste water before burning
-2Mol/l, 2.85 * 10
-3Mol/l, 1.39 * 10
-3Mol/l, 8.19 * 10
-4Mol/l, 4.40 * 10
-4Mol/l.After the burning different electrochemical reactions after the time content of chlorion be respectively 1.853 * 10
-2Mol/l, 6.36 * 10
-3Mol/l, 3.76 * 10
-3Mol/l, 2.27 * 10
-3Mol/l, 1.12 * 10
-3Mol/l.Chloride ion content after the burning deducts the content that the content of chlorion before the burning obtains organochlorine and is respectively 7.40 * 10
-3Mol/l, 3.51 * 10
-3Mol/l, 2.37 * 10
-3Mol/l, 1.45 * 10
-3Mol/l, 0.68 * 10
-3Mol/l.
Claims (8)
1, a kind of method of measuring content of Cl element, take high-temperature combustion method that the organochlorine in the determinand is transformed into inorganic chlorine earlier, absorb with alkaline solution, it is characterized in that absorption liquid takes potential method to measure the wherein content of chlorine element again, its potential electrode is made up of chloride ion-selective electrode and contrast electrode, described potential electrode is inserted in the described absorption liquid, measured the electrode potential V between the described potential electrode, according to formula V=E
0+ (2.303RT/F) logK
Sp(Agcl)-(2.303RT/F) log[cl
-]-E
Ref, calculate the concentration [cl of chlorion in the absorption liquid
-], can converse the content of chlorine element in the determinand; Wherein: E
0Be the standard electrode potential of silver electrode,
K
Sp(Agcl) be the ion-product constant of silver chloride,
E
RefBe the contrast electrode electromotive force,
R is a gas law constant,
T is a Kelvin temperature,
F is a Faraday constant.
2,, it is characterized in that described contrast electrode is a saturated calomel electrode according to the method described in the claim 1.
3, this is characterized in that according to the method described in the claim 2 described saturated calomel electrode is two salt bridge saturated calomel electrodes, and outer salt bridge is KNO
3Solution.
4,, it is characterized in that it is with AgCl-Ag that described chlorion is selected electrode according to the method described in the claim 1
2S is the chloride ion-selective electrode of sensitive membrane.
5,, it is characterized in that organochlorine ion in the bleaching effluent and inorganic chlorine ion determination according to the method described in the claim 1.
6, a kind of burner that is used for the described method of claim 1 to 5, comprise thermal response pipe (2), heating tube (6), heat-insulation layer (4), it is characterized in that being connected with heatable high temperature resistance silk in the middle of the heating tube (6), (6) at least 3 of heating tubes, parallel ring is around thermal response pipe (2), and heat-insulation layer (4) wraps up heating tube (6) and thermal response pipe (2) together.
7,, it is characterized in that described heating tube (6) is the 5-8 root according to the device described in the claim 6.
8, according to the device described in claim 6 or 7, it is characterized in that being inserted with temp probe (5) in the gap of heating tube (6) and thermal response pipe (2), the power supply of described high temperature resistance silk links to each other with temperature controller (11) with temp probe (5), to realize the automatic adjusting of temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01129969 CN1351257A (en) | 2001-11-27 | 2001-11-27 | Method for measuring content of Cl element and its burner |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01129969 CN1351257A (en) | 2001-11-27 | 2001-11-27 | Method for measuring content of Cl element and its burner |
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| Publication Number | Publication Date |
|---|---|
| CN1351257A true CN1351257A (en) | 2002-05-29 |
Family
ID=4669604
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|---|---|---|---|
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| CN100360928C (en) * | 2005-03-24 | 2008-01-09 | 厦门大学 | Composite scanning chlorion sensitive micro-probe and preparing process thereof |
| CN100373153C (en) * | 2005-08-10 | 2008-03-05 | 福建南平太阳电缆股份有限公司 | Method for measuring general quantity of released gas during cable material combustion |
| CN101799407A (en) * | 2010-03-26 | 2010-08-11 | 苏州市贝特利高分子材料有限公司 | Method for measuring content of halogen |
| CN101334365B (en) * | 2007-06-29 | 2010-11-17 | 上海宝钢工业检测公司 | Determination method for chloride ion content of temper rolling liquor for steel plate rolling |
| CN102262142A (en) * | 2010-05-31 | 2011-11-30 | 宜特科技(昆山)电子有限公司 | Determination method for chlorine and bromine in plastic material |
| CN103389327A (en) * | 2012-05-07 | 2013-11-13 | 中国石油化工股份有限公司 | Method for testing organochlorine content of oil extraction auxiliary agent |
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-
2001
- 2001-11-27 CN CN 01129969 patent/CN1351257A/en active Pending
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| CN100360928C (en) * | 2005-03-24 | 2008-01-09 | 厦门大学 | Composite scanning chlorion sensitive micro-probe and preparing process thereof |
| CN100373153C (en) * | 2005-08-10 | 2008-03-05 | 福建南平太阳电缆股份有限公司 | Method for measuring general quantity of released gas during cable material combustion |
| CN101334365B (en) * | 2007-06-29 | 2010-11-17 | 上海宝钢工业检测公司 | Determination method for chloride ion content of temper rolling liquor for steel plate rolling |
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| CN102262142A (en) * | 2010-05-31 | 2011-11-30 | 宜特科技(昆山)电子有限公司 | Determination method for chlorine and bromine in plastic material |
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| CN104569092A (en) * | 2015-01-22 | 2015-04-29 | 首钢总公司 | Method and device used for detecting chlorine content of blast-furnace gas |
| CN104569092B (en) * | 2015-01-22 | 2018-03-06 | 首钢总公司 | A kind of method and its device for being used to detect blast furnace gas chlorinty |
| CN104991034A (en) * | 2015-06-26 | 2015-10-21 | 浙江凯恩特种材料股份有限公司 | Combustion test method for trace chlorine elements of electrical paper and paper boards and paper pulp for production of electrical paper |
| CN107991428A (en) * | 2017-11-27 | 2018-05-04 | 攀钢集团攀枝花钢铁研究院有限公司 | The assay method of chlorinity in chlorine-containing gas |
| CN108333130A (en) * | 2018-02-13 | 2018-07-27 | 华测检测认证集团股份有限公司 | A kind of first screen system for COD automatic tests |
| CN110632134A (en) * | 2018-06-22 | 2019-12-31 | 宝山钢铁股份有限公司 | Method for rapidly detecting content of chloride ions on surface of hot-rolled pickled steel plate |
| CN110632134B (en) * | 2018-06-22 | 2022-06-28 | 宝山钢铁股份有限公司 | Method for rapidly detecting content of chloride ions on surface of hot-rolled pickled steel plate |
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