CN101587093A - Method for measuring content of chloridion in wet flat liquid - Google Patents
Method for measuring content of chloridion in wet flat liquid Download PDFInfo
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- CN101587093A CN101587093A CNA2008100380062A CN200810038006A CN101587093A CN 101587093 A CN101587093 A CN 101587093A CN A2008100380062 A CNA2008100380062 A CN A2008100380062A CN 200810038006 A CN200810038006 A CN 200810038006A CN 101587093 A CN101587093 A CN 101587093A
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- wet
- chloridion
- leveling liquid
- ion content
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Abstract
The invention relates to a method for measuring the content of chloridion, in particular to a method for measuring the content of chloridion in wet flat liquid. The establishment of the method for measuring the content of chloridion in the wet flat liquid mainly adopts a calcination method to carbonize organic amine matters which restrict the chloridion, to form soluble inorganic matters, enables the chloridion to be dissociated, so that the content of the chloridion can be measured by a potentiometric titration method. The invention can accurately measure the content of chloridion in the wet flat liquid, provides an effective means for incoming quality control of the flat liquid, and avoids unqualified product being stored.
Description
Technical field
The present invention relates to chlorine ion content determination method, relate in particular to the chlorine ion content determination method in the alkaline solution.
Background technology
At present, various informative to methods of chlorine ions both at home and abroad, for example utilize K
4CrO
4The silver nitrate standard solution titration is used in the agent of giving instruction, and forms red siliver chromate precipitation in the time of near equivalent point, and solution is red by xanthochromia simultaneously, thereby judges the indicator method of titration end-point; Utilize chromatography of ions to carry out the advanced chromatography of ions of microanalysis; The potentiometric titration that also has the environmental protection and economy of using always the most now.These methods cut both ways, and the indicator method color change is not clearly, thereby with the naked eye judge and may cause very big personal error, and this method can not be applicable to the mensuration of muddy or coloured sample.The chromatography of ions then need through stepwise dilution, and cost is higher, is difficult to promote the wider application for the sample of conventional concentration.Potentiometric titration acquires a certain degree of difficulty for trace analysis.But the sort of method is all direct at inorganics, and does not also have relevant document announcement as organism other country concerning the noisy sample of determination of chloride ion that this class of wet-leveling liquid contains.
Wet-leveling liquid is mainly continued to use the compound method of water-base metal clean-out system, emulsion and rust preventive cutting fluid, based on water-soluble and oil-soluble rust preventive, is made up of surfactant, rust preventive, defoamer, lubricant and softening water etc. in addition.Because in preparation, prescription purity is not enough, and process chlorions such as packing, transportation sneak into, and makes to contain chlorion in the smooth liquid.Wet-leveling liquid is alkalescence under the normality, and pH need the solution of preparation is transferred to acidity when surveying chlorion, but the organic amine in the wet-leveling liquid can be tied up acid, forms (NH between 9～10
2)
nThe material of RHCl can not dissociate chlorion in water, thereby influences the normal measurement of chlorion, and organic solvent generally commonly used also can't be broken this kind phenomenon, and we adopt and add the target mode and experimentize, result verification this conclusion.Inquire into company such as Dutch Kui Ke chemistry for this reason,, also confirmed to make of general chlorine ion content determination method through their identical experiment.
Summary of the invention
The present invention is intended to solve the above-mentioned defective of prior art, and chlorine ion content determination method in a kind of alkaline wet-leveling liquid is provided.The present invention can accurately measure chloride ion content in the wet-leveling liquid, for smooth liquid receiving inspection provides effective means, avoids the substandard product warehouse-in.
The present invention is achieved in that
Chlorine ion content determination method in a kind of wet-leveling liquid, it comprises:
Step 1, crucible accurately take by weighing sample;
Step 2 is placed on crucible on the electric furnace and burns, and treats to be placed on when sample becomes black solid on the naked light electric furnace, makes the inflammable substance burning clean, goes to temperature then and shifts out behind the 30min in the muffle furnace more than 800 ℃, puts into beaker after the cooling;
Step 3, adding distil water was not to having crucible, with taking out after the ultrasonic Treatment in beaker;
Step 4 is cleaned crucible with distilled water, finally uses HNO
3Solution transfers to the pH of solution between 2.5～4.5;
Step 5 is placed on the sample bottle of handling well on the puddle support of potentiometric titrimeter, with the AgNO for preparing
3Standard solution titration finally records the content of chlorion in the wet-leveling liquid to terminal.
Chlorine ion content determination method in the described wet-leveling liquid, described step 1 weighing is accurate to 0.01g.
Chlorine ion content determination method in the described wet-leveling liquid, described step 4 ultrasonic treatment time is 20-30 minute.
Chlorine ion content determination method in the described wet-leveling liquid, potentiometric titration electricity consumption very Ag electrode and Ag in the described step 5
2The S electrode.
The organic amine material carbonization of the feasible constraint of calcining method chlorion has mainly been adopted in the present invention's foundation of wet-leveling liquid chlorine ion content determination method this time, form the inorganics of solubility, cause chlorion to dissociate out, thereby utilize potentiometric titration accurately to record chlorine ion concentration.The present invention avoids the substandard product warehouse-in for smooth liquid receiving inspection provides effective means.
Embodiment
The present invention has mainly adopted the organic amine material carbonization of the feasible constraint of calcining method chlorion, forms the inorganics of solubility, causes chlorion to dissociate out, thereby utilizes potentiometric titration to record.Analytic process is at first accurately taking by weighing sample Mg with crucible, be accurate to 0.01g (what of sample weighting amounts what of chloride ion-containing determine per sample), crucible is placed on the electric furnace burns, treat to be placed on when sample becomes black solid on the naked light electric furnace, make the inflammable substance burning clean as far as possible, go to temperature then in the muffle furnace more than 800 ℃, shift out after approximately burning 30min, put into beaker after the cooling, adding distil water is to not having crucible, take out the back about super 25min in ultrasound wave, cleans crucible with distilled water, finally uses HNO
3Solution transfers to the pH of solution between 2.5～4.5.The sample of handling well is placed on the puddle support of potentiometric titrimeter, with the AgNO for preparing
3Standard solution titration finally records the content of chlorion in the wet-leveling liquid to terminal.
Gordian technique is the pre-treatment of wet-leveling liquid, because the quality of pre-treatment directly has influence on chlorine ion content determination result's accuracy; Another key is the selection of chlorine ion electrode, and Ag electrode and Ag are arranged at present
2The S electrode for the situation that measurement result is had relatively high expectations, is selected Ag
2The S electrode is comparatively suitable.
SP-3 wet-leveling liquid in certain cold rolling mill valuable cargo and PTJ-2 wet-leveling liquid have been carried out the experimental study of up to a hundred times chloride ion content.Verified the availability of new method with great deal of experiment data, brought very big economic benefit to department.
Two kinds of smooth liquid are from different manufacturers, though slightly different on prescription, all exist organic amine substance to disturb Determination of chlorine ion content.Can remove the organic amine material that disturbs chloride ion content to measure in the wet-leveling liquid according to the pre-treating method that we adopt, obtain limpid wet-leveling liquid solution.We have also adopted and have added the target mode and carry out identical experiment, experimental result such as following table 1:
Contrast test data before and after two kinds of wet-leveling liquids of table 1 are handled
| Test specimen | Sample weighting amount (g) | The calcination processing test findings (10 -6g) | Test findings (10 after the calcination processing -6g) | The benchmark NaCl recovery (%) |
| Benchmark NaCl | 0.003 | 1085.12 | 1074.41 | 99.02 |
| The SP-3 wet-leveling liquid | 30 | 0 | 168.60 | / |
| SP-3+ benchmark NaCl | 30+0.003 | 0 | 1194.41 | 95.51 |
| The PTJ-2 wet-leveling liquid | 30 | 0 | 660.30 | / |
| PTJ-2+ benchmark NaCl | 30+0.003 | 0 | 1697.69 | 96.59 |
Chloride ion content to two kinds of wet-leveling liquids in the form has carried out handling the front and back contrast, analysis by test figure, as can be seen, if do not adopt the pre-treating method of calcining just can't record chloride ion content in the wet-leveling liquid, the interfering material effect that exists in the wet-leveling liquid is very big, even at adding benchmark sodium chloride material shielding action is arranged still later on.The calcining pre-treating method that we adopt just can solve can't the chlorine detection ion concentration with direct dissolution method practical problems, data can see that the experimental data that two kinds of wet-leveling liquids record can obtain the higher relatively benchmark NaCl recovery after processing from show.
Claims (4)
1. chlorine ion content determination method in the wet-leveling liquid is characterized in that it comprises:
Step 1, crucible accurately take by weighing sample;
Step 2 is placed on crucible on the electric furnace and burns, and treats to be placed on when sample becomes black solid on the naked light electric furnace, makes the inflammable substance burning clean, goes to temperature then and shifts out behind the 30min in the muffle furnace more than 800 ℃, puts into beaker after the cooling;
Step 3, adding distil water was not to having crucible, with taking out after the ultrasonic Treatment in beaker;
Step 4 is cleaned crucible with distilled water, finally uses HNO
3Solution transfers to the pH of solution between 2.5～4.5;
Step 5 is placed on the sample of handling well on the puddle support of potentiometric titrimeter, with the AgNO for preparing
3Standard solution titration finally records the content of chlorion in the wet-leveling liquid to terminal.
2. chlorine ion content determination method in the wet-leveling liquid according to claim 1 is characterized in that, described step 1 weighing is accurate to 0.01g.
3. chlorine ion content determination method in the wet-leveling liquid according to claim 1 is characterized in that, described step 4 ultrasonic treatment time is 20-30 minute.
4. chlorine ion content determination method in the wet-leveling liquid according to claim 1 is characterized in that, potentiometric titration electricity consumption very Ag electrode and Ag in the described step 5
2The S electrode.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100380062A CN101587093A (en) | 2008-05-23 | 2008-05-23 | Method for measuring content of chloridion in wet flat liquid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100380062A CN101587093A (en) | 2008-05-23 | 2008-05-23 | Method for measuring content of chloridion in wet flat liquid |
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| CN101587093A true CN101587093A (en) | 2009-11-25 |
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| CNA2008100380062A Pending CN101587093A (en) | 2008-05-23 | 2008-05-23 | Method for measuring content of chloridion in wet flat liquid |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101980010A (en) * | 2010-05-25 | 2011-02-23 | 江西中烟工业有限责任公司 | Method for measuring chlorine and sulphur in tobaccos and tobacco products |
| CN102253101A (en) * | 2011-05-06 | 2011-11-23 | 山东鸿瑞石油化工有限公司 | Method for detecting chloride ions in polyisobutylene |
| CN102539511A (en) * | 2012-01-31 | 2012-07-04 | 金发科技股份有限公司 | Method for detecting content of bromine in fire retardant through automatic potentiometric titration |
| CN102620977A (en) * | 2012-01-31 | 2012-08-01 | 金发科技股份有限公司 | Decomposition method for bromine in bromine-based flame retardant agent |
| CN102879452A (en) * | 2012-09-21 | 2013-01-16 | 贵州红林机械有限公司 | Method for determining content of micro chlorine ions in surface treatment solution |
| CN103063726A (en) * | 2013-01-10 | 2013-04-24 | 广州天赐高新材料股份有限公司 | Detection method for chlorine ion content in lithium-ion battery electrolyte |
| CN105675831A (en) * | 2015-11-08 | 2016-06-15 | 张开航 | Apparatus and method for measuring chlorine ion and total organic carbon in water |
| CN106645136A (en) * | 2016-08-29 | 2017-05-10 | 海安华达石油仪器有限公司 | Chlorine salt content meter |
| CN108107142A (en) * | 2017-12-21 | 2018-06-01 | 上海微谱化工技术服务有限公司 | A kind of analysis method of Wax removal water |
| CN110108836A (en) * | 2019-05-30 | 2019-08-09 | 岭东核电有限公司 | The measuring method and its application of chlorine ion concentration in nuclear power plant's liquid waste treatment system |
| CN113533626A (en) * | 2021-06-25 | 2021-10-22 | 江苏省沙钢钢铁研究院有限公司 | Method for measuring chloride ion content in cold-rolled chromium-containing sludge |
| CN113687016A (en) * | 2021-09-09 | 2021-11-23 | 南通联亚药业有限公司 | Method for detecting chloride ion content in cyclobenzaprine hydrochloride |
| CN113820445A (en) * | 2020-06-18 | 2021-12-21 | 宝山钢铁股份有限公司 | Method for detecting concentration of cold rolling circulating leveling liquid |
| CN113820446A (en) * | 2020-06-18 | 2021-12-21 | 宝山钢铁股份有限公司 | Method for detecting concentration of leveling liquid |
-
2008
- 2008-05-23 CN CNA2008100380062A patent/CN101587093A/en active Pending
Cited By (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101980010A (en) * | 2010-05-25 | 2011-02-23 | 江西中烟工业有限责任公司 | Method for measuring chlorine and sulphur in tobaccos and tobacco products |
| CN102253101A (en) * | 2011-05-06 | 2011-11-23 | 山东鸿瑞石油化工有限公司 | Method for detecting chloride ions in polyisobutylene |
| CN102253101B (en) * | 2011-05-06 | 2013-03-27 | 山东鸿瑞石油化工有限公司 | Method for detecting chloride ions in polyisobutylene |
| CN102539511A (en) * | 2012-01-31 | 2012-07-04 | 金发科技股份有限公司 | Method for detecting content of bromine in fire retardant through automatic potentiometric titration |
| CN102620977A (en) * | 2012-01-31 | 2012-08-01 | 金发科技股份有限公司 | Decomposition method for bromine in bromine-based flame retardant agent |
| CN102539511B (en) * | 2012-01-31 | 2013-09-04 | 金发科技股份有限公司 | Method for detecting content of bromine in fire retardant through automatic potentiometric titration |
| CN102879452A (en) * | 2012-09-21 | 2013-01-16 | 贵州红林机械有限公司 | Method for determining content of micro chlorine ions in surface treatment solution |
| CN103063726A (en) * | 2013-01-10 | 2013-04-24 | 广州天赐高新材料股份有限公司 | Detection method for chlorine ion content in lithium-ion battery electrolyte |
| CN103063726B (en) * | 2013-01-10 | 2015-01-07 | 广州天赐高新材料股份有限公司 | Detection method for chlorine ion content in lithium-ion battery electrolyte |
| CN105675831A (en) * | 2015-11-08 | 2016-06-15 | 张开航 | Apparatus and method for measuring chlorine ion and total organic carbon in water |
| CN106645136A (en) * | 2016-08-29 | 2017-05-10 | 海安华达石油仪器有限公司 | Chlorine salt content meter |
| CN108107142A (en) * | 2017-12-21 | 2018-06-01 | 上海微谱化工技术服务有限公司 | A kind of analysis method of Wax removal water |
| CN108107142B (en) * | 2017-12-21 | 2020-05-22 | 上海微谱化工技术服务有限公司 | Analysis method of surfactant in wax removal water |
| CN110108836A (en) * | 2019-05-30 | 2019-08-09 | 岭东核电有限公司 | The measuring method and its application of chlorine ion concentration in nuclear power plant's liquid waste treatment system |
| CN113820445A (en) * | 2020-06-18 | 2021-12-21 | 宝山钢铁股份有限公司 | Method for detecting concentration of cold rolling circulating leveling liquid |
| CN113820446A (en) * | 2020-06-18 | 2021-12-21 | 宝山钢铁股份有限公司 | Method for detecting concentration of leveling liquid |
| CN113820446B (en) * | 2020-06-18 | 2023-11-14 | 宝山钢铁股份有限公司 | Method for detecting concentration of leveling liquid |
| CN113820445B (en) * | 2020-06-18 | 2023-11-14 | 宝山钢铁股份有限公司 | Method for detecting concentration of cold rolling circulation leveling liquid |
| CN113533626A (en) * | 2021-06-25 | 2021-10-22 | 江苏省沙钢钢铁研究院有限公司 | Method for measuring chloride ion content in cold-rolled chromium-containing sludge |
| CN113687016A (en) * | 2021-09-09 | 2021-11-23 | 南通联亚药业有限公司 | Method for detecting chloride ion content in cyclobenzaprine hydrochloride |
| CN113687016B (en) * | 2021-09-09 | 2023-09-12 | 南通联亚药业股份有限公司 | Method for detecting chloride ion content in cyclobenzaprine hydrochloride |
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Application publication date: 20091125 |