CN103063671A - Rapid online analysis method for main component in acidic galvanization electroplate liquid - Google Patents
Rapid online analysis method for main component in acidic galvanization electroplate liquid Download PDFInfo
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- CN103063671A CN103063671A CN2011103187694A CN201110318769A CN103063671A CN 103063671 A CN103063671 A CN 103063671A CN 2011103187694 A CN2011103187694 A CN 2011103187694A CN 201110318769 A CN201110318769 A CN 201110318769A CN 103063671 A CN103063671 A CN 103063671A
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Abstract
A rapid online analysis method for main components in an acidic galvanization electroplate liquid. The test tools comprise a zoom table for consumption volume of silver nitrate solution corresponding to contents of boric acid, zinc chloride and potassium chloride in the acidic galvanization electroplate liquid and for potassium chloride content corresponding to volume difference, and a test kit. The test kit contains a conical flask, two plastic syringes, three plastic bottles and 9 plastic centrifuge tubes; the three plastic bottles are respectively provided with a silver nitrate solution, an EDTA solution and a sodium hydroxide solution; and the 9 plastic centrifuges are respectively provided with an EDTA solution, a silver nitrate solution, a sodium hydroxide solution, ascorbic acid and chrome black T, an ammonia buffer solution with a pH value of 10, a triethanolamine solution, 3 drops of methyl red and an EDTA solution, a few drops of phenolphthalein and glycerol, and a K2CrO4 solution. Determination of contents of boric acid, zinc chloride and potassium chloride in the electroplate liquid is realized by adding reagents, titrating, reading and searching the table. The method provided by the invention is simple and convenient, has high practical value, simple and safe operation.
Description
Technical field
The present invention relates to a kind of test chemical analytical approach, specifically the fast on-line analyzing technique of three kinds of compositions in the acid zinc plating electroplate liquid.
Background technology
The chemical analysis test technology is mainly used in the mensuration of various component contents in the electroplate liquid in Electroplate Factory.The expense that traditional measuring technology needs is larger, set up a laboratory, needs to buy various device, comprises glassware and analytical instrument, also has the needed medicine of analytical test and special analytical test personnel through training.Now the Electroplate Factory of our country mainly take individual's individual workship as main, majority is the rural migrant worker, the workman is fixing, mobility of people is large, educational level is lower, does not understand chemical analysis knowledge.And these little factories lack of capital, and can't set up the laboratory of a standard.And the composition of electroplate liquid master salt will be grasped aborning at any time, in order to add at any time, to guarantee the quality of electroplated product, the method of testing complex operation in past, test duration is long, thus be necessary to develop a kind of measuring technology of new electroplate liquid major component, to satisfy the demand in this field.
Summary of the invention
Purpose of the present invention, it is low to provide a kind of cost, easy and simple to handle, carries easily major component fast on-line analyzing method in the acid zinc plating electroplate liquid.
The technical scheme that adopts is:
Major component fast on-line analyzing method in a kind of acid zinc plating electroplate liquid, test used instrument and comprise that zinc chloride in acid zinc plating electroplate liquid mesoboric acid content zoom table, the electroplate liquid contains in scale, the electroplate liquid that zinc chloride content is corresponding to consume KCE content zoom table and test kits in the corresponding electroplate liquid of liquor argenti nitratis ophthalmicus volume zoom table, volume differences that concentration is 0.4mol/L, comprises following processing step:
Be equipped with in the described test kits: a conical flask, two disposable plastic injectors, the plastic centrifuge tube with buckle closure of three little plastic bottles with cover and 9 different sizes;
Three above-mentioned little plastic bottles with cover, one of them outside covers with lighttight black thin film, in the bottle liquor argenti nitratis ophthalmicus that concentration is 0.4mol/L is housed, in other two bottles EDTA solution and the concentration that concentration is 0.05mol/L being housed respectively is the sodium hydroxide solution of 0.1mol/L;
The plastic centrifuge tube with buckle closure of 9 above-mentioned different sizes, the first centrifuge tube is equipped with the EDTA solution 100mL that concentration is 0.1mol/L, the second centrifuge tube is equipped with the liquor argenti nitratis ophthalmicus 100mL that concentration is 0.4mol/L, the 3rd centrifuge tube is equipped with the sodium hydroxide solution 100mL that concentration is 0.3mol/L, the 4th centrifuge tube is equipped with ascorbic acid 0.2g and 0.1g eriochrome black T, the 5th centrifuge tube is equipped with the ammonia buffer 10ml of PH=10, the 6th centrifuge tube is equipped with triethanolamine solution 5ml, the 7th centrifuge tube is equipped with 3 of methyl reds and concentration is the EDTA solution 10mL of 0.05mol/L, the 8th centrifuge tube is equipped with phenolphthalein number droplet and glycerine 10ml, and the 9th centrifuge tube is equipped with K
2CrO
4Solution 3ml;
The mensuration of acid zinc plating electroplate liquid mesoboric acid content:
(1), reagent adding operation:
Get the syringe that volume is 1mL, accurately draw 1mL acid zinc plating electroplate liquid to be measured, inject conical flask, the 50mL water of productive use that reinjects, getting 3 of methyl reds and concentration is in the EDTA solution 10mL adding conical flask of 0.05mol/L again, shakes up;
(2), titration operation:
Get the syringe that volume is 10mL, the sodium hydroxide solution that accurate absorption concentration is 0.3mol/L is to scale, left hand is held syringe, and the right hand is held conical flask and rocked, and carefully drips at a slow speed, until solution becomes the yellow terminal point that is, stopping to drip, get phenolphthalein solution number droplet and glycerine 10ml again and add in the conical flask, is the sodium hydroxide solution titration of 0.3mol/L with concentration, pink by yellow to solution is titration end-point, stops to drip;
(3), reading is tabled look-up:
After stopping to drip, observe and drip reagent residue milliliter number in the syringe, deducting residue milliliter number with the milliliter number 10mL that begins to draw is consumption liquid product, looks into known acid zinc plating electroplate liquid mesoboric acid content zoom table, check analysis namely gets zinc chloride content in the acid zinc plating electroplate liquid;
The mensuration of zinc chloride content in the acid zinc plating electroplate liquid:
(1), reagent adding operation:
Get the syringe that volume is 1mL, accurately draw 1mL acid zinc plating electroplate liquid to be measured, inject conical flask, the 50mL water of productive use reinjects, the buffer solution 10ml and the triethanolamine solution 5ml that get ascorbic acid 0.2g, eriochrome black T 0.1g, PH=10 add in the conical flask again, shake up;
(2), titration operation:
Get the syringe that volume is 10mL, accurately draw concentration and be the EDTA solution of 0.1mol/L to scale, left hand is held syringe, and the right hand is held conical flask and rocked, carefully drip at a slow speed, and be terminal point until solution becomes suddenly mazarine by aubergine, stop to drip;
(3), reading is tabled look-up:
After stopping to drip, observe and drip reagent residue milliliter number in the syringe, deducting a residue milliliter number with a milliliter number 10mL who begins to draw is consumption liquid product, with zinc chloride content zoom table check analysis in the known acid zinc plating electroplate liquid, namely gets zinc chloride content in the acid zinc plating electroplate liquid;
The mensuration of KCE content in the acid zinc plating electroplate liquid:
(1), reagent adding operation:
Get the syringe that volume is 1mL, accurately draw 1mL acid zinc plating electroplate liquid to be measured, inject conical flask, the 50mL water of productive use that reinjects is got K again
2CrO
4Solution 3ml adds in the conical flask, shakes up, and is stand-by;
(2), titration operation:
Get the syringe that volume is 10mL, accurately draw concentration and be the liquor argenti nitratis ophthalmicus of 0.4mol/L to scale, left hand is held syringe, and the right hand is held conical flask and rocked, carefully drip at a slow speed, and be terminal point until solution white precipitate occurs by yellow to Chinese red is arranged, stop to drip;
(3), reading is tabled look-up:
After stopping to drip, observe and drip reagent residue milliliter number in the syringe, deducting residue milliliter number with the milliliter number 10mL that begins to draw is consumption liquid product, deducting by the corresponding consumption of zinc chloride content in known electroplate liquid concentration is the liquor argenti nitratis ophthalmicus volume zoom table of 0.4mol/L again, the consumption concentration of the zinc chloride that checks in is that the volume of the liquor argenti nitratis ophthalmicus of 0.4mol/L is counted zoom table, the consumption liquid product of gained, with KCE content zoom table check analysis in the corresponding electroplate liquid of known volume differences, namely get zinc chloride content in the acid zinc plating electroplate liquid;
Above triethanolamine solution is that the volume ratio of triethanolamine and water is 1: 1 triethanolamine aqueous solution.
Above number percent is mass percent.
Above-mentioned test kits is a Hard paper box, plastic casing or foam material box, and volume is 20cm * 12cm * 8cm.
Above-mentioned conical flask volume is 150mL.
Two above-mentioned disposable plastic injector volumes are respectively 1mL and 10mL.
Three above-mentioned little plastic bottle volumes with cover are 100mL.
The plastic centrifuge tube with buckle closure of 9 above-mentioned different sizes, volume is respectively 3mL, 5mL or 10mL.
Zoom table corresponding to consumption liquid product:
Acid zinc plating electroplate liquid mesoboric acid content zoom table
Zinc chloride content zoom table in the acid zinc plating electroplate liquid
The corresponding consumption of zinc chloride content concentration is the liquor argenti nitratis ophthalmicus volume zoom table of 0.4mol/L in the electroplate liquid
KCE content zoom table in the corresponding electroplate liquid of volume differences
The invention has the advantages that:
1, this method of testing safety and environmental protection can be measured the content of three kinds of major components quickly and easily.
2, the present invention has higher practical value, and applicable crowd's scope is wide, easy to operate, and technique is simple, and it is convenient to carry, and analyzing has certain characteristics such as operability.Adopt the present invention to carry out on-line determination to major component in the acid zinc plating electroplate liquid at any time, in order to grasp the content of major component in the electroplate liquid, guarantee to electroplate normally carrying out of producing.
3, raw materials used being easy to of the present invention bought, and be with low cost, is fit to produce in enormous quantities, can decrease acid zinc plating electroplate liquid in the testing cost of major component, be conducive to promote the commercialization process of test job.
Claims (6)
1. major component fast on-line analyzing method in the acid zinc plating electroplate liquid, test used instrument and comprise that zinc chloride in acid zinc plating electroplate liquid mesoboric acid content zoom table, the electroplate liquid contains in scale, the electroplate liquid that zinc chloride content is corresponding to consume KCE content zoom table and test kits in the corresponding electroplate liquid of liquor argenti nitratis ophthalmicus volume zoom table, volume differences that concentration is 0.4mol/L, it is characterized in that, comprise following processing step:
Be equipped with in the described test kits: a conical flask, two disposable plastic injectors, the plastic centrifuge tube with buckle closure of three little plastic bottles with cover and 9 different sizes;
Three above-mentioned little plastic bottles with cover, one of them outside covers with lighttight black thin film, in the bottle liquor argenti nitratis ophthalmicus that concentration is 0.4mol/L is housed, in other two bottles EDTA solution and the concentration that concentration is 0.05mol/L being housed respectively is the sodium hydroxide solution of 0.1mol/L;
The plastic centrifuge tube with buckle closure of 9 above-mentioned different sizes, the first centrifuge tube is equipped with the EDTA solution 100mL that concentration is 0.1mol/L, the second centrifuge tube is equipped with the liquor argenti nitratis ophthalmicus 100mL that concentration is 0.4mol/L, the 3rd centrifuge tube is equipped with the sodium hydroxide solution 100mL that concentration is 0.3mol/L, the 4th centrifuge tube is equipped with ascorbic acid 0.2g and 0.1g eriochrome black T, the 5th centrifuge tube is equipped with the ammonia buffer 10ml of PH=10, the 6th centrifuge tube is equipped with triethanolamine solution 5ml, the 7th centrifuge tube is equipped with 3 of methyl reds and concentration is the EDTA solution 10mL of 0.05mol/L, the 8th centrifuge tube is equipped with phenolphthalein number droplet and glycerine 10ml, and the 9th centrifuge tube is equipped with K
2CrO
4Solution 3ml;
The mensuration of acid zinc plating electroplate liquid mesoboric acid content:
(1), reagent adding operation:
Get the syringe that volume is 1mL, accurately draw 1mL acid zinc plating electroplate liquid to be measured, inject conical flask, the 50mL water of productive use that reinjects, getting 3 of methyl reds and concentration is in the EDTA solution 10mL adding conical flask of 0.05mol/L again, shakes up;
(2), titration operation:
Get the syringe that volume is 10mL, the sodium hydroxide solution that accurate absorption concentration is 0.3mol/L is to scale, left hand is held syringe, and the right hand is held conical flask and rocked, and carefully drips at a slow speed, until solution becomes the yellow terminal point that is, stopping to drip, get phenolphthalein solution number droplet and glycerine 10ml again and add in the conical flask, is the sodium hydroxide solution titration of 0.3mol/L with concentration, pink by yellow to solution is titration end-point, stops to drip;
(3), reading is tabled look-up:
After stopping to drip, observe and drip reagent residue milliliter number in the syringe, deducting residue milliliter number with the milliliter number 10mL that begins to draw is consumption liquid product, and the acid zinc plating electroplate liquid mesoboric acid content zoom table check analysis with known namely gets zinc chloride content in the acid zinc plating electroplate liquid;
The mensuration of zinc chloride content in the acid zinc plating electroplate liquid:
(1), reagent adding operation:
Get the syringe that volume is 1mL, accurately draw 1mL acid zinc plating electroplate liquid to be measured, inject conical flask, the 50mL water of productive use reinjects, the buffer solution 10ml and the triethanolamine solution 5ml that get ascorbic acid 0.2g, eriochrome black T 0.1g, PH=10 add in the conical flask again, shake up;
(2), titration operation:
Get the syringe that volume is 10mL, accurately draw concentration and be the EDTA solution of 0.1mol/L to scale, left hand is held syringe, and the right hand is held conical flask and rocked, carefully drip at a slow speed, and be terminal point until solution becomes suddenly mazarine by aubergine, stop to drip;
(3), reading is tabled look-up:
After stopping to drip, observe and drip reagent residue milliliter number in the syringe, deducting a residue milliliter number with a milliliter number 10mL who begins to draw is consumption liquid product, with zinc chloride content zoom table check analysis in the known acid zinc plating electroplate liquid, namely gets zinc chloride content in the acid zinc plating electroplate liquid;
The mensuration of KCE content in the acid zinc plating electroplate liquid:
(1), reagent adding operation:
Get the syringe that volume is 1mL, accurately draw 1mL acid zinc plating electroplate liquid to be measured, inject conical flask, the 50mL water of productive use that reinjects is got K again
2CrO
4Solution 3ml adds in the conical flask, shakes up, and is stand-by;
(2), titration operation:
Get the syringe that volume is 10mL, accurately draw concentration and be the liquor argenti nitratis ophthalmicus of 0.4mol/L to scale, left hand is held syringe, and the right hand is held conical flask and rocked, carefully drip at a slow speed, and be terminal point until solution white precipitate occurs by yellow to Chinese red is arranged, stop to drip;
(3), reading is tabled look-up:
After stopping to drip, observe and drip reagent residue milliliter number in the syringe, deducting residue milliliter number with the milliliter number 10mL that begins to draw is consumption liquid product, deducting by the corresponding consumption of zinc chloride content in known electroplate liquid concentration is the liquor argenti nitratis ophthalmicus volume zoom table of 0.4mol/L again, the consumption concentration of the zinc chloride that checks in is that the volume of the liquor argenti nitratis ophthalmicus of 0.4mol/L is counted zoom table, the consumption liquid product of gained, with KCE content zoom table check analysis in the corresponding electroplate liquid of known volume differences, namely get zinc chloride content in the acid zinc plating electroplate liquid;
Above triethanolamine solution is that the volume ratio of triethanolamine and water is 1: 1 triethanolamine aqueous solution.
Above number percent is mass percent.
2. major component fast on-line analyzing method in a kind of acid zinc plating electroplate liquid according to claim 1, it is characterized in that: described test kits is a Hard paper box, plastic casing or foam material box, and volume is 20cm * 12cm * 8cm.
3. major component fast on-line analyzing method in a kind of acid zinc plating electroplate liquid according to claim 1, it is characterized in that: described conical flask volume is 150mL.
4. major component fast on-line analyzing method in a kind of acid zinc plating electroplate liquid according to claim 1, it is characterized in that: described two disposable plastic injector volumes are respectively 1mL and 10mL.
5. major component fast on-line analyzing method in a kind of acid zinc plating electroplate liquid according to claim 1, it is characterized in that: described three little plastic bottle volumes with cover are 100mL.
6. major component fast on-line analyzing method in a kind of acid zinc plating electroplate liquid according to claim 1, it is characterized in that: the plastic centrifuge tube with buckle closure of described 9 different sizes, volume is respectively 3mL, 5mL or 10mL.
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Cited By (3)
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| CN103852466A (en) * | 2014-02-21 | 2014-06-11 | 安费诺(天津)电子有限公司 | Method for measuring chloride ion in acidity plating solution |
| CN104655622A (en) * | 2015-02-11 | 2015-05-27 | 沈阳理工大学 | Quick online analysis kit |
| CN106872550A (en) * | 2015-12-11 | 2017-06-20 | 上海梅山钢铁股份有限公司 | The detection method of free acid content in a kind of tin methane sulfonate system electroplate liquid |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103852466A (en) * | 2014-02-21 | 2014-06-11 | 安费诺(天津)电子有限公司 | Method for measuring chloride ion in acidity plating solution |
| CN104655622A (en) * | 2015-02-11 | 2015-05-27 | 沈阳理工大学 | Quick online analysis kit |
| CN104655622B (en) * | 2015-02-11 | 2017-09-29 | 沈阳理工大学 | Fast on-line analyzing kit |
| CN106872550A (en) * | 2015-12-11 | 2017-06-20 | 上海梅山钢铁股份有限公司 | The detection method of free acid content in a kind of tin methane sulfonate system electroplate liquid |
| CN106872550B (en) * | 2015-12-11 | 2019-06-18 | 上海梅山钢铁股份有限公司 | The detection method of free acid content in a kind of tin methane sulfonate system electroplate liquid |
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Application publication date: 20130424 |