CN106198853B - The detection method of ammonium sulfate and Glycine Levels in a kind of sulfate blackening liquid - Google Patents
The detection method of ammonium sulfate and Glycine Levels in a kind of sulfate blackening liquid Download PDFInfo
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- CN106198853B CN106198853B CN201610450614.9A CN201610450614A CN106198853B CN 106198853 B CN106198853 B CN 106198853B CN 201610450614 A CN201610450614 A CN 201610450614A CN 106198853 B CN106198853 B CN 106198853B
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
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Abstract
The invention provides the detection method of ammonium sulfate and Glycine Levels in a kind of sulfate blackening liquid, using formol titration detection ammonium sulfate and the total content of glycine consumption sodium hydroxide standard liquid, spectroscopic methodology is aided in using principle of charge conservation, detect that the content of ammonium sulfate and ammonium sulfate can consume the content of sodium hydroxide standard liquid in sample, finally use and subtract the content that glycine is calculated in poor method.The present invention realizes the accurate detection that both materials of ammonium sulfate Yu glycine in sulfate blackening liquid are realized using one-time detection, and the detection method can also detect other necessary detection projects in blackening liquid, save the overall detection time of blackening liquid, detection efficiency significantly improves, data processing software can be used to calculate testing result, intermediate computations are greatly reduced, method and step is simple, detection time is short, as a result accurate stable, the requirement of high-precision rolled copper foil later stage surface treatment medium-high frequency time medicine detection can be met completely.
Description
Technical field
The present invention relates to high-precision rolled copper foil technical field of surface, more particularly, to sulphur in a kind of sulfate blackening liquid
The detection method of sour ammonium and Glycine Levels.
Background technology
Rolled copper foil is to be processed into ingot casting, then hot rolled cogging by copper is first smelting, is rolled into by roughing and finish rolling
0.1mm~0.15mm copper foil mother metal, most formed afterwards through copper foil milling train repeat-rolling, its thickness is usually 6 μm~70 μm.So
The crystallographic texture of rolled copper foil is laminated structure, and electrolytic copper foil is better than in terms of strength and toughness.In addition rolled copper foil
Consistency is higher, and surface is more smooth, and more conducively the signal after circuit board quickly transmits, in high-frequency high-speed transmission, fine-line
Printed wiring board on have a wide range of applications.
Blackening liquid is mainly used in the production of the Darkening process of rolled copper foil, i.e. Darkening process paper tinsel, and melanism copper foil is lower visitor
The product that family has the call, and blackening liquid is to be used to deposit one layer of atrament in roughening of copper foil face, improves the corrosion resistant of copper foil
Corrosion energy and peel strength.Main component has the sulfate such as copper sulphate, cobaltous sulfate and ammonium sulfate, sweet ammonia in sulfate blackening liquid
Acid.Ammonium sulfate and glycine concentration control are extremely important in whole production technology, and both can be complexed with copper cobalt ions, electroplate
Cathodic polarization effect is improved during processing, makes the metallic particles of deposition finer and closely woven, can also improve deep plating property.
At present, the detection method of ammonium sulfate and glycine mixed liquor is seldom, the detection scheme of mainly independent solution.
The detection of ammonium sulfate at present can use formaldehyde method, and specific method is to add phenolphthalein into sample few drops, with hydroxide
Sodium drops to pale red, adds neutral formalin 15mL (being changed according to the specific concentration of sample), uses sodium hydroxide standard liquid 0.1mol/L
It is terminal that sodium hydroxide standard liquid, which is titrated to colourless, but this method, simultaneously suitable for the detection of glycine, both interfere；In addition
Weight method can also be used, specific method is that barium chloride is added into sample, generates barium sulfate precipitate, solution is transferred to
In the crucible of constant weight, constant weight is heated in high temperature oven, claims the quality that must be precipitated, further calculates the content of ammonium sulfate,
Because there is a variety of sulfate in the sample, sulfuric acid root origin is more, is not suitable for ammonium sulfate and individually detects.
The detection of glycine at present can use formaldehyde method, identical with ammonium sulfate detecting step, because both of which and formaldehyde
Reaction, is interfered；Another is perchloric acid non-aqueous titration, and this is the detection method in national standard, but this method is applicable
It is inapplicable in glycine solid, glycine solution detection；The solution not had also for disadvantages described above.
At present in high-precision rolled copper foil processing industry, in sulfate blackening liquid the property of ammonium sulfate and glycine there is
Common ground, it can be reacted with alkali and formaldehyde, there is presently no the detection that good screener is used for both, and sulfate is wherein
Detection is influenceed, causes existing detection method testing result inaccuracy to be present, step is complicated, and detection time length, detection terminal is not
The defects of sensitive, detection efficiency can not meet high-precision rolled copper foil later stage surface treatment medium-high frequency time medicine detection with accuracy
It is required that.
So work out it is a set of be directed to sulfate blackening liquid in the rapid analysis method of ammonium sulfate and glycine, have step
Rapid simple, detection time is short, testing result accurate stable, disclosure satisfy that high-precision rolled copper foil later stage surface treatment high frequency time medicine
The detection scheme of testing requirements, it is the technical problem of current those skilled in the art's urgent need to resolve.
The content of the invention
It is an object of the invention to provide the detection method of ammonium sulfate and Glycine Levels in a kind of sulfate blackening liquid, the inspection
Survey method has step simple, and detection time is short, testing result accurate stable, disclosure satisfy that at surface of high-precision rolled copper foil later stage
Manage the requirement of medium-high frequency time medicine detection.
To solve above-mentioned technical problem, technical scheme provided by the invention is：
The detection method of ammonium sulfate and Glycine Levels in a kind of sulfate blackening liquid, comprises the following steps：
1) ammonium sulfate in formol titration detecting the contet of sulphate blackening liquid is used to consume the total of sodium hydroxide standard liquid with glycine
Volume VAlways；
2) the respective content C of Cu and Co metal ions and sulfate ion in detecting the contet of sulphate blackening liquidCu、CCoAnd
CSulfate radical；
Then according to the content of sulfate ion, Cu and Co metal ions, the content of ammonium ion is calculated；
Then the content C of ammonium sulfate is extrapolatedAmmonium sulfateAnd the volume V of ammonium sulfate consumption sodium hydroxide standard liquid1；
3) calculation procedure 1) in VAlwaysWith the V in step 2)1Difference, obtain glycine consumption sodium hydroxide standard liquid body
Product, thus instead release the content of glycine in sulfate blackening liquid.
Preferably, the content of copper sulphate is 1~50g/L in the sulfate blackening liquid, and the content of cobaltous sulfate is 1~50g/
L, 20~100g/L of ammonium sulfate, 20~100g/L of glycine.
Preferably, the concrete operations of the step 1) are：
Add phenolphthalein indicator first into sulfate blackening liquid to be detected, then titrated with sodium hydroxide solution, it is extremely light
Red, neutral formalin solution is then added, it is titration end-point to be then titrated to colourless with sodium hydroxide standard liquid, metering, is obtained
Ammonium sulfate and the cumulative volume V of glycine consumption sodium hydroxide standard liquid in sulfate blackening liquidAlways。
Preferably, in the step 2), using Cu and Co metal ions and sulphur in spectroscopic methodology detection sulfate blackening liquid
The respective content C of acid ionCu、CCoAnd CSulfate radical。
Preferably, the spectroscopic methodology is inductively coupled plasma atomic emission spectrometry.
Preferably, the concentration of the sodium hydroxide standard liquid is 0.1mol/L.
Compared with prior art, the invention provides the detection of ammonium sulfate and Glycine Levels in a kind of sulfate blackening liquid
Method, compared with existing detection method, the main flow of detection method provided by the invention is detected using formol titration
Ammonium sulfate and the total content of glycine consumption sodium hydroxide standard liquid, aid in spectroscopic methodology using principle of charge conservation, detect sample
The content and ammonium sulfate of middle ammonium sulfate can consume the content of sodium hydroxide standard liquid, and finally use subtracts poor method and glycine is calculated
Content.The present invention realizes realizes the accurate of both materials of ammonium sulfate and glycine in sulfate blackening liquid using one-time detection
Detection, and the detection method can also detect other necessary detection projects in blackening liquid, such as metal ion Cu and Co
Detection, the overall detection time of blackening liquid is saved, detection efficiency significantly improves, and data processing software can be used to calculate detection
As a result, such as EXCEL computation sheets, intermediate computations are greatly reduced, and method and step is simple, and detection time is short, as a result accurate
It is really stable, the requirement of high-precision rolled copper foil later stage surface treatment medium-high frequency time medicine detection can be met completely.
Embodiment
For a further understanding of the present invention, the preferred embodiment of the invention is described with reference to embodiment, still
It should be appreciated that these descriptions simply further illustrate the feature and advantage of the present invention, rather than the limit to the claims in the present invention
System.
The invention provides the detection method of ammonium sulfate and Glycine Levels in a kind of sulfate blackening liquid, including following step
Suddenly：
1) ammonium sulfate in formol titration detecting the contet of sulphate blackening liquid is used to consume the total of sodium hydroxide standard liquid with glycine
Volume VAlways；
2) the respective content C of Cu and Co metal ions and sulfate ion in detecting the contet of sulphate blackening liquidCu、CCoAnd
CSulfate radical；
Then according to the content of sulfate ion, Cu and Co metal ions, the content of ammonium ion is calculated；
Then the content C of ammonium sulfate is extrapolatedAmmonium sulfateAnd the volume V of ammonium sulfate consumption sodium hydroxide standard liquid1；
3) calculation procedure 1) in VAlwaysWith the V in step 2)1Difference, obtain glycine consumption sodium hydroxide standard liquid body
Product, thus instead release the content of glycine in sulfate blackening liquid.
In one embodiment of the invention, the content of copper sulphate is 1~50g/L in the sulfate blackening liquid, sulfuric acid
The content of cobalt is 1~50g/L, 20~100g/L of ammonium sulfate, 20~100g/L of glycine.
In one embodiment of the invention, the concrete operations of the step 1) are：
Add phenolphthalein indicator first into sulfate blackening liquid to be detected, then titrated with sodium hydroxide solution, it is extremely light
Red, neutral formalin solution is then added, it is titration end-point to be then titrated to colourless with sodium hydroxide standard liquid, metering, is obtained
Ammonium sulfate and the cumulative volume V of glycine consumption sodium hydroxide standard liquid in sulfate blackening liquidAlways。
In one embodiment of the invention, in the step 2), use in spectroscopic methodology detection sulfate blackening liquid Cu with
And the respective content C of Co metal ions and sulfate ionCu、CCoAnd CSulfate radical。
In one embodiment of the invention, the spectroscopic methodology is inductively coupled plasma atomic emission spectrometry.
In one embodiment of the invention, the concentration of the sodium hydroxide standard liquid is 0.1mol/L.
Detection method step provided by the invention is simple, and detection time is short, as a result accurate stable, the high-precision rolled copper foil later stage
It is surface-treated the requirement of medium-high frequency time medicine detection.This detection method is while ammonium sulfate and glycine is detected, by melanism
Metal ion detection comes out in liquid, and this is also the parameter of the necessary control in Darkening process paper tinsel.
The present invention can be calculated the content C of ammonium sulfate by formula 1Ammonium sulfate：
CAmmonium sulfate=(CSulfate radical/ 96-CCu/ 64-CCo/59)×132
In formula 1, CCuThe concentration of copper ion, g/L in-sample；
CCo--- the concentration of cobalt ions, g/L in sample；
CSulfate radicalThe total concentration of sulfate radical, g/L in-sample；
The molal weight of 64-copper ion, g/mol；
The molal weight of 59-cobalt ions, g/mol；
The molal weight of 96-sulfate radical, g/mol；
The molal weight of 132-ammonium sulfate, g/mol.
The present invention can be calculated the volume V of ammonium sulfate consumption sodium hydroxide standard liquid by formula 21：
V1=CAmmonium sulfate×VSample/66.07/CMark
CAmmonium sulfateThe concentration of ammonium sulfate, g/L in-sample；
VSampleThe volume of-sample, L；
The 1/2, g/mol of 66.07-ammonium sulfate molal weight；
CMarkThe concentration of-sodium hydroxide standard liquid, mol/L.
The present invention can be calculated the content C of glycine in sample by formula 3Glycine：
CGlycine=(VAlways-V1)×CMark×75.07/VSample
VAlwaysThe cumulative volume of-ammonium sulfate and glycine consumption sodium hydroxide standard liquid, L；
V1- ammonium sulfate consumes the volume of sodium hydroxide standard liquid, L；
CMarkThe concentration of-sodium hydroxide standard liquid, mol/L；
The molal weight of 75.07-glycine, g/mol；
VSampleThe volume of-sample, L.
For a further understanding of the present invention, with reference to embodiment to sulphur in a kind of sulfate blackening liquid provided by the invention
The detection method of sour ammonium and Glycine Levels is described in detail, and protection scope of the present invention is not limited by the following examples.
Embodiment 1
10ml melanism fluid samples are taken, are placed in 100ml beakers, and add phenolphthalein few drops, it is molten with 0.2mol/L sodium hydroxides
Then drop adds neutral formalin 15ml, shakes up, static 5 minutes, nothing is titrated to 0.1mol/L sodium hydroxide standard liquids to pale red
Color is terminal, obtains ammonium sulfate and the cumulative volume V of glycine consumption sodium hydroxide standard liquidAlways。
1ml melanism fluid samples are taken again, are added to constant volume in 1000ml volumetric flasks, using in ICP detecting the contet of sulphate blackening liquids
The concentration of Cu, Co metal ion and sulfate radical；Then ammonium in ammonium sulfate is calculated by the data obtained using principle of charge conservation
The concentration of radical ion, further calculate and obtain the concentration C of ammonium sulfateAmmonium sulfateAnd ammonium sulfate consumption 0.1mol/L sodium hydroxide standard liquids
Volume VAmmonium sulfate。
Pass through the difference (V of above-mentioned consumption sodium hydroxide standard liquid volumeAlways-V1That is the body of glycine consumption sodium hydroxide standard liquid
Product VGlycine), the anti-concentration C for releasing glycine in blackening liquidGlycine。
The precision of embodiment 2 is tested with the degree of accuracy
Precision refers to the degree that measurement result is consistent each other is repeated several times under the same conditions, and the size of precision is used
Relative standard deviation represents that the smaller explanation precision of deviation is higher.
Match somebody with somebody Sulphuric acid Asia blackening liquid, wherein sulfuric acid with analytical pure sulfuric acid ammonium, analysis pure glycine, metallic copper and metallic cobalt
The normal concentration of ammonium is 100g/l, and the normal concentration of glycine is 100g/l.
Using same sample parallel determination of the method provided by the invention to the sulfate blackening liquid of above-mentioned preparation 4 times, so
The relative standard deviation of measurement result is calculated afterwards, as described in Table 1.
The accuracy of the embodiment of the present invention of table 1 and degree of accuracy testing result
Because existing detection method can not complete the detection to ammonium sulfate and glycine simultaneously, defect is larger, therefore does not have
There is carry out contrast experiment, from the point of view of testing result above, this method preferably, disclosure satisfy that height in accuracy and the degree of accuracy
The requirement of smart rolled copper foil later stage surface treatment high frequency time medicine detection, has certain dissemination.
The explanation of above example is only intended to help the method and its core concept for understanding the present invention.It should be pointed out that pair
For those skilled in the art, under the premise without departing from the principles of the invention, the present invention can also be carried out
Some improvement and modification, these are improved and modification is also fallen into the protection domain of the claims in the present invention.
The foregoing description of the disclosed embodiments, professional and technical personnel in the field are enable to realize or using the present invention.
A variety of modifications for these embodiments are it will be apparent that defined herein one for those skilled in the art
As principle can realize in other embodiments without departing from the spirit or scope of the present invention.Therefore, the present invention will
It will not be intended to be limited to the embodiments shown herein, and be to fit to consistent with principles disclosed herein and features of novelty
Widest range.
Claims (6)
1. the detection method of ammonium sulfate and Glycine Levels in a kind of sulfate blackening liquid, it is characterised in that comprise the following steps：
1) ammonium sulfate and the cumulative volume of glycine consumption sodium hydroxide standard liquid in formol titration detecting the contet of sulphate blackening liquid are used
VAlways；
2) the respective content C of Cu and Co metal ions and sulfate ion in detecting the contet of sulphate blackening liquidCu、CCoAnd CSulfate radical；
Then according to the content of sulfate ion, Cu and Co metal ions, the content of ammonium ion is calculated；
Then the content C of ammonium sulfate is extrapolatedAmmonium sulfateAnd the volume V of ammonium sulfate consumption sodium hydroxide standard liquid1；
3) calculation procedure 1) in VAlwaysWith the V in step 2)1Difference, obtain glycine consumption sodium hydroxide standard liquid volume, by
This anti-content for releasing glycine in sulfate blackening liquid.
2. detection method according to claim 1, it is characterised in that the content of copper sulphate is in the sulfate blackening liquid
1~50g/L, the content of cobaltous sulfate is 1~50g/L, 20~100g/L of ammonium sulfate, 20~100g/L of glycine.
3. detection method according to claim 1 or 2, it is characterised in that the concrete operations of the step 1) are：
First into sulfate blackening liquid to be detected plus phenolphthalein indicator, then titrated with sodium hydroxide solution, to pale red,
Then neutral formalin solution is added, it is titration end-point to be then titrated to colourless with sodium hydroxide standard liquid, metering, obtains sulfate
Ammonium sulfate and the cumulative volume V of glycine consumption sodium hydroxide standard liquid in blackening liquidAlways。
4. detection method according to claim 1 or 2, it is characterised in that in the step 2), using spectroscopic methodology detection sulphur
The respective content C of Cu and Co metal ions and sulfate ion in hydrochlorate blackening liquidCu、CCoAnd CSulfate radical。
5. detection method according to claim 4, it is characterised in that the spectroscopic methodology is inductively coupled plasma atom
Emission spectrometry.
6. detection method according to claim 1 or 2, it is characterised in that the concentration of the sodium hydroxide standard liquid is
0.1mol/L。
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| CN113358812A (en) * | 2021-04-27 | 2021-09-07 | 阳煤丰喜肥业（集团）有限责任公司 | Quantitative analysis method for isocyanic acid radical in melamine tail gas |
| CN113533625A (en) * | 2021-05-27 | 2021-10-22 | 中国航发南方工业有限公司 | Method for rapidly detecting ammonium sulfate in magnesium alloy oxidation tank liquid |
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| JPH0368795A (en) * | 1989-08-07 | 1991-03-25 | K D K Kk | Production of copper foil for printed circuit |
| KR100633790B1 (en) * | 2004-06-02 | 2006-10-16 | 일진소재산업주식회사 | Manufacturing method of blackening surface treated copper foil for electromagnetic wave shield and copper foil and composite material manufactured using the same |
| CN1865366B (en) * | 2005-05-16 | 2010-12-15 | 3M创新有限公司 | Method and composition for improving adhesion of organic polymer coating to copper surface |
| JP5865619B2 (en) * | 2011-07-15 | 2016-02-17 | 日本パーカライジング株式会社 | Water-based metal surface treatment agent and metal material treated with the treatment agent |
| CN102618902B (en) * | 2012-04-24 | 2015-04-01 | 山东金宝电子股份有限公司 | Surface treatment process of copper foil for flexible copper-clad plate |
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Effective date of registration: 20230719 Address after: 6 households, including No. 3, OBT Building, Shifangyuan, Economic Development Zone, Linqing City, Liaocheng City, Shandong Province, 252000 Patentee after: Zhongse Zhengrui (Shandong) Copper Industry Co.,Ltd. Address before: 252600 north head of East 2nd Ring Road, Linqing City, Liaocheng City, Shandong Province Patentee before: CNMC ALBETTER ALBRONZE Co.,Ltd. |