CN105181777B - A kind of method of sulfamic acid content in electroplate liquid using Capillary Electrophoresis - Google Patents
A kind of method of sulfamic acid content in electroplate liquid using Capillary Electrophoresis Download PDFInfo
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- CN105181777B CN105181777B CN201510540726.9A CN201510540726A CN105181777B CN 105181777 B CN105181777 B CN 105181777B CN 201510540726 A CN201510540726 A CN 201510540726A CN 105181777 B CN105181777 B CN 105181777B
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Abstract
The present invention relates to detection and analysis technical field, the method for specifically disclosing sulfamic acid content in a kind of electroplate liquid using Capillary Electrophoresis, this method includes：1) preparation of sulfamic acid standard liquid：Sulfamic acid standard liquid is prepared, and establishes standard curve；2) preparation of buffer solution：Cushioning liquid is prepared using to Potassium Hydrogen Phthalate and hexadecyltrimethylammonium chloride；3) sample determines：Bath sample is diluted at normal temperatures, so that electroplate liquid measured value, in the standard curve range of linearity, the sample after dilution is measured in HPCE, the content of sulfamic acid in the plating solution sample of measure is read on standard curve.The present invention realizes the measure of plating solution complexing agent content, and strong foundation is provided for plating solution adjustment；Other auxiliary complex-formers and the more interference of trace mineral supplement measure can be overcome, there is the characteristics of accurate, quick, easy.
Description
Technical field
The present invention relates to detection and analysis technical field, and in particular to one kind utilizes ammonia in Capillary Electrophoresis electroplate liquid
The method of base sulfonic acid content.
Background technology
In electroplating industry, additive monitoring to plating solution control, product quality, cost savings and environmental protection to close weight
Will.And because complicated component, plating solution sample propose series of challenges to ion chromatography method.See both at home and abroad and used capillary
Electrophoresis tests the electroplate liquid (phosphites of the formic acid of 1. sulfate 2. (salt) 3. malic acid (salt) 4. hypophosphites 5.EDTA 6.
7. the lactic acid of 8. bronze medal of acetate, 9. nickel 10.) and environment in zwitterion the methods of, existing document report utilizes gas phase or liquid
The method of phase chromatographic determination solution additive, but for the method using the sulfamic acid in Capillary Electrophoresis electroplate liquid
Have not been reported.
Capillary Electrophoresis is for driving force, using capillary as split tunnel with high voltage electric field (30kV).It is filled with its pipe
Buffer solution or gel, a kind of liquid phase separation skill of separation is realized according to mobility between each component in sample and the difference of distribution
Art.In electrophoresis process, electrode solution is inserted at capillary both ends, and this electrode solution is generally consistent with the buffer solution in pipe.Positive and negative electrode
It is connected to high voltage device, sample disc moves during sample introduction, the sample introduction end of capillary and the electrode at this end is properly inserted sample cell
In, after giving certain electric field or pressure, sample is inhaled into capillary, is then again moved to capillary and is started electrophoresis in electrode solution
(as shown in Figure 1).In Capillary Electrophoresis, in order to maintain charge balance, the cation in solution is adsorbed to quartz surfaces and formed
Electric double layer, after voltage is applied at capillary both ends, this layer of cation tends to negative pole movement, and drives the solution in capillary
Negative pole (electric osmose) is shifted to stream forms.High pressure is used because the surface-to-volume ratio of capillary is big, during plus electrophoresis, electricity
Ooze has two major features in Capillary Electrophoresis：Liquid along capillary wall Uniform Flow, its forward position be flat；Carry different electricity
The molecule of lotus moves in one direction, and neutral molecule also can together move with electric osmose and realize separation.
The content of the invention
For overcome the deficiencies in the prior art, it is an object of the invention to provide one kind to utilize Capillary Electrophoresis electricity
The method of sulfamic acid content in plating solution, the measure of plating solution complexing agent content is realized, strong foundation is provided for plating solution adjustment；Can
Overcome other auxiliary complex-formers and the more interference of trace mineral supplement measure, there is the characteristics of accurate, quick, easy.
To achieve the above object, scheme of the present invention is as follows：
The method of sulfamic acid content, this method include in a kind of electroplate liquid using Capillary Electrophoresis：
1) preparation of sulfamic acid standard liquid：Sulfamic acid standard liquid is prepared, and establishes standard curve；
2) preparation of buffer solution：Buffer solution is prepared using to Potassium Hydrogen Phthalate and hexadecyltrimethylammonium chloride；
3) sample determines：Bath sample is diluted at normal temperatures, so that the measured value of electroplate liquid is in standard curve
In the range of linearity, the sample after dilution is measured in HPCE, and the plating solution sample of measure is read on standard curve
The content of middle sulfamic acid.
In the above method, step 2) is specially：Weigh to Potassium Hydrogen Phthalate and hexadecyltrimethylammonium chloride in
In same beaker, and deionized water dissolving is added, obtain buffer solution；With the pH to 5.5-6.5 of sodium hydroxide regulation buffer solution；Its
In, it is 12-16mmol/L to Potassium Hydrogen Phthalate concentration, hexadecyltrimethylammonium chloride concentration is 0.15-0.2mmol/
L。
In the above method, the parameter that sample determines in step 3) is respectively：Capillary column internal diameter is 50 μm, length 60cm；
Detection wavelength is 254nm, and input mode uses 50 millibars of hydrodynamic injection, sample injection time 10 seconds, 25 DEG C of column temperature, separation voltage-
20kV。
Further, capillary column effective length of the present invention is 52cm.
In the above method, step 1) is specially：Sulfamic acid 0.5g accurately is weighed in small beaker, is added deionized water, is treated
Solid all after dissolving, moves into 100ml volumetric flasks, is settled to scale with deionized water, shakes up；
Above-mentioned solution 4ml, 8ml, 12ml are accurately pipetted respectively into 100ml volumetric flasks, scale is settled to deionized water,
Shake up, obtain sulfamic acid standard liquid that concentration is respectively 200ppm, 400ppm, 600ppm and establish standard curve.
Compared with prior art, the beneficial effects of the present invention are：
1. the concrete content of sulfamic acid, realizes plating solution in method application capillary electrophoresis detection plating solution of the present invention
The measure of complexing agent content, strong foundation is provided for plating solution adjustment；Overcome other auxiliary complex-formers and more micro add
The interference for adding agent to determine, there is the characteristics of accurate, quick, easy；
2. method of the present invention is further research of the plating alloy material in production etc. with field, change is reached
Learn the deposit purpose of basic detection technique.
Brief description of the drawings
Fig. 1 is the collection of illustrative plates of the sulfamic acid detected by the method for the present invention；
The canonical plotting that Fig. 2 is established for the present invention.
Embodiment
The method of sulfamic acid content, this method include in the electroplate liquid of the present invention using Capillary Electrophoresis：
1) preparation of sulfamic acid standard liquid：Sulfamic acid standard liquid is prepared, and establishes standard curve；
2) preparation of buffer solution：Buffer solution is prepared using to Potassium Hydrogen Phthalate and hexadecyltrimethylammonium chloride；
3) sample determines：Plating solution sample is diluted at normal temperatures, so that its measured value is in the standard curve range of linearity
Interior, the sample after dilution is measured in HPCE, and amino sulphur in the plating solution sample of measure is read on standard curve
The content of acid；The collection of illustrative plates of the sulfamic acid detected by the method for the present invention is as shown in Figure 1.
In capillary electrophoresis, the constant of EOF is to ensure that blending ingredients efficiently separate and obtained the premise of reappearance,
And can EOF be stablized and influenceed by the pH value and concentration of buffer solution, influence of the pH value to electroendosmotic mobility is more complicated, mesh
Preceding also no clear and definite rule；In the present invention in the range of the pH5.5-6.5 by controlling buffer solution, EOF is set to be in flat
Surely, the accuracy and repeatability of detection are advantageous to.The component and concentration of other buffer solution can also directly affect the size of EOF
And stability.Therefore, in the above method, step 2) is specially：Accurately weigh to Potassium Hydrogen Phthalate and cetyl front three
For ammonium chloride (CTAC) in beaker, adding deionized water makes its dissolving, and pH to 5.5-6.5 is adjusted with sodium hydroxide；Wherein, it is right
Potassium Hydrogen Phthalate concentration is 12-16mmol/L, and hexadecyltrimethylammonium chloride concentration is 0.15-0.2mmol/L.At this
In invention, back-ground electolyte is used as in buffer solution to Potassium Hydrogen Phthalate, and hexadecyltrimethylammonium chloride is as electricity
Seepage flow modifying agent.
In the above method, the parameter that sample determines in step 3) is respectively：Capillary column internal diameter is 50 μm, length 60cm；
Detection wavelength is 254nm, and input mode uses 50 millibars of hydrodynamic injection, sample injection time 10 seconds, 25 DEG C of column temperature, separation voltage-
20kV.In capillary electrophoresis, column temperature, separation voltage are also to influence an important factor for detection is repeated, in grinding for the present invention
Study carefully middle discovery, when the parameter of measure is in above-mentioned setting value, can effectively reduce influence of the Joule heat to result reappearance, and can be with
Improve separating effect.
Further, capillary effective length of the present invention is 52cm.
In the above method, step 1) is specially：Sulfamic acid 0.5g accurately is weighed in small beaker, is added deionized water, is treated
Solid all after dissolving, moves into 100ml volumetric flasks, is settled to scale with deionized water, shakes up；
Above-mentioned solution 2ml, 4ml, 6ml, 8ml, 10ml are accurately pipetted respectively into 100ml volumetric flasks, is determined with deionized water
Hold to scale, shake up, obtain the sulfamic acid that concentration is respectively 100mg/L, 200mg/L, 300mg/L400mg/L, 500mg/L
Standard liquid simultaneously establishes standard curve, standard curve such as Fig. 2 of foundation.
It is specific embodiment of the present invention below, involved reagent can be by being commercially available in the following embodiments；
Wherein, used HPCE is the HPCEs of Agilent 7100 of Agilent company production；All implementations
Fig. 2 standard curve is used in example.
Embodiment 1
Using the method for sulfamic acid content in Capillary Electrophoresis electroplate liquid, this method includes：
1) according to plating solution formula, electroplate liquid is voluntarily prepared, wherein sulfamic acid is 21g/L；
2) preparation of buffer solution：Buffer solution is prepared using to Potassium Hydrogen Phthalate and hexadecyltrimethylammonium chloride；
The pH=5.5 of buffer solution, wherein being 12mmol/L to Potassium Hydrogen Phthalate concentration, hexadecyltrimethylammonium chloride concentration is
0.15mmol/L；
3) sample determines：It will be measured after 100 times of the plating bath dilution of step 1) with HPCE, it is bent in standard
The content of sulfamic acid in the plating solution sample of measure is read on line；Measurement result is shown in Table 1.
Embodiment 2
Using the method for sulfamic acid content in Capillary Electrophoresis electroplate liquid, this method includes：
1) according to plating solution formula, electroplate liquid is voluntarily prepared, wherein sulfamic acid is 21g/L；
2) preparation of buffer solution：Buffer solution is prepared using to Potassium Hydrogen Phthalate and hexadecyltrimethylammonium chloride；
The pH=5.8 of buffer solution, wherein being 13mmol/L to Potassium Hydrogen Phthalate concentration, hexadecyltrimethylammonium chloride concentration is
0.18mmol/L；
3) sample determines：It will be measured after 100 times of the plating bath dilution of step 1) with HPCE, it is bent in standard
The content of sulfamic acid in the plating solution sample of measure is read on line；Measurement result is shown in Table 1.
Embodiment 3
Using the method for sulfamic acid content in Capillary Electrophoresis electroplate liquid, this method includes：
1) according to plating solution formula, electroplate liquid is voluntarily prepared, wherein sulfamic acid is 21g/L；
2) preparation of buffer solution：Buffer solution is prepared using to Potassium Hydrogen Phthalate and hexadecyltrimethylammonium chloride；
The pH=6 of buffer solution, wherein being 14mmol/L to Potassium Hydrogen Phthalate concentration, hexadecyltrimethylammonium chloride concentration is
0.16mmol/L；
3) sample determines：The electroplate liquid of step 1) is measured with HPCE, reads and surveys on standard curve
The content of sulfamic acid in fixed plating solution sample；Measurement result is shown in Table 1.
Embodiment 4
Using the method for sulfamic acid content in Capillary Electrophoresis electroplate liquid, this method includes：
1) according to plating solution formula, electroplate liquid is voluntarily prepared, wherein sulfamic acid is 21g/L；
2) preparation of buffer solution：Buffer solution is prepared using to Potassium Hydrogen Phthalate and hexadecyltrimethylammonium chloride；
The pH=6 of buffer solution, wherein being 15mmol/L to Potassium Hydrogen Phthalate concentration, hexadecyltrimethylammonium chloride concentration is
0.18mmol/L；
3) sample determines：It will be measured after 100 times of the plating bath dilution of step 1) with HPCE, it is bent in standard
The content of sulfamic acid in the plating solution sample of measure is read on line；Measurement result is shown in Table 1.
Embodiment 5
Using the method for sulfamic acid content in Capillary Electrophoresis electroplate liquid, this method includes：
1) according to plating solution formula, electroplate liquid is voluntarily prepared, wherein sulfamic acid is 21g/L；
2) preparation of buffer solution：Buffer solution is prepared using to Potassium Hydrogen Phthalate and hexadecyltrimethylammonium chloride；
The pH=6.5 of buffer solution, wherein being 16mmol/L to Potassium Hydrogen Phthalate concentration, hexadecyltrimethylammonium chloride concentration is
0.2mmol/L；
3) sample determines：It will be measured after 100 times of the plating bath dilution of step 1) with HPCE, it is bent in standard
The content of sulfamic acid in the plating solution sample of measure is read on line；Measurement result is shown in Table 1.
Table 1：Concentration known plating solution result is tested using the method for the present invention
The result of table 1 demonstrates the accuracy of the method test plating solution complexing agent of the present invention, and other compositions in plating solution
Material does not have an impact to the measure of sulfamic acid.And found after a large amount of METHOD FOR CONTINUOUS DETERMINATIONs, sulfamic acid peak type is stable, week
Enclose that interfering material is few, the relative standard deviation of sulfamic acid measure be 4.4% (＜ 5%), it is seen that method of the invention is with very
High Stability and veracity.
Above-mentioned embodiment is only the preferred embodiment of the present invention, it is impossible to the scope of protection of the invention is limited with this,
The change and replacement for any unsubstantiality that those skilled in the art is done on the basis of the present invention belong to institute of the present invention
Claimed scope.
Claims (1)
1. a kind of method of sulfamic acid content in electroplate liquid using Capillary Electrophoresis, it is characterised in that this method bag
Include：
1) preparation of sulfamic acid standard liquid：Sulfamic acid 0.5g accurately is weighed in small beaker, is added deionized water, is treated solid
All after dissolving, move into 100ml volumetric flasks, be settled to scale with deionized water, shake up, obtain sulfamic acid solution；Accurately
Above-mentioned sulfamic acid solution 2ml, 4ml, 6ml, 8ml, 10ml are pipetted respectively into 100ml volumetric flasks, is settled to deionized water
Scale, shake up, obtain the sulfamic acid standard that concentration is respectively 100mg/L, 200mg/L, 300mg/L, 400mg/L, 500mg/L
Solution simultaneously establishes standard curve；
2) preparation of buffer solution：Take to Potassium Hydrogen Phthalate and hexadecyltrimethylammonium chloride in same beaker, and add
Enter deionized water dissolving, obtain buffer solution, the pH to 5.5-6.5 of buffer solution is adjusted with sodium hydroxide；Wherein, to hydrogen phthalate
Potassium concn is 12-16mmol/L, and hexadecyltrimethylammonium chloride concentration is 0.15-0.2mmol/L；
3) sample determines：Bath sample is diluted at normal temperatures, so that electroplate liquid measured value is in the linear model of standard curve
In enclosing, the sample after dilution is measured in HPCE, and amino in the plating solution sample of measure is read on standard curve
The content of sulfonic acid, the parameter of sample measure are respectively：Capillary column internal diameter is 50 μm, length 60cm；Detection wavelength is 254nm,
Input mode uses 50 millibars of hydrodynamic injection, sample injection time 10 seconds, 25 DEG C of column temperature, separation voltage -20kV.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1703541A (en) * | 2002-11-06 | 2005-11-30 | 米凯尔·帕夫洛夫 | Measurement of the concentration of a reducing agent in an electroless plating bath |
| CN104020168A (en) * | 2014-06-06 | 2014-09-03 | 黄棚兰 | Method for detecting main components of electroplating effluent |
-
2015
- 2015-08-28 CN CN201510540726.9A patent/CN105181777B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1703541A (en) * | 2002-11-06 | 2005-11-30 | 米凯尔·帕夫洛夫 | Measurement of the concentration of a reducing agent in an electroless plating bath |
| CN104020168A (en) * | 2014-06-06 | 2014-09-03 | 黄棚兰 | Method for detecting main components of electroplating effluent |
Non-Patent Citations (2)
| Title |
|---|
| Analytical Technique for Plating Bath - Principle of Capillary Electrophoresis and it`s Application;Katsushi SASA;《Journal of The Surface Finishing Society of Japan》;20130223;第63卷(第8期);第482页右栏至第484页右栏 * |
| Determination of the inorganic degradation products sulfate and sulfamate in the antiepileptic drug topiramate by capillary electrophoresis;A. Klockow-Beck et.al;《Journal of Chromatography B: Biomedical Sciences and Applications》;19981211;第720卷(第1-2期);全文 * |
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