KR950002923B1 - Untitative analysis method of the addition of amine group among zn-ni plating liquid using ultraviolet extinction photometry method - Google Patents

Untitative analysis method of the addition of amine group among zn-ni plating liquid using ultraviolet extinction photometry method Download PDF

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KR950002923B1
KR950002923B1 KR1019910018621A KR910018621A KR950002923B1 KR 950002923 B1 KR950002923 B1 KR 950002923B1 KR 1019910018621 A KR1019910018621 A KR 1019910018621A KR 910018621 A KR910018621 A KR 910018621A KR 950002923 B1 KR950002923 B1 KR 950002923B1
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solution
sample solution
amine
absorbance
additive
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KR930008448A (en
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곽해일
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포항종합제철주식회사
정명식
재단법인산업과학기술연구소
백덕현
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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

Abstract

The method comprises the a steps of; analyzing the amount of Ni in test solution taken from Zn-Ni plating solution that includes amine organic chemical comound; making a test solution by adding NiCl2 solution in the amount same as that of Ni in the test solution; prescribing gauging curve solution by adding amine organic chemical compound after taking the test solution; graphing gauging curve for the value of absorbed intensity of light according to the doping amount of additive after measuring the value of absorbed intensity of light in the gauging curve solution in 222 nm wavelength by ultraviolet absorbed intensity of light method; and calculating the concentration of amine additive in test solutions from the gauging curve after measuring the intensity of light of the test solution in 222 nm wavelength by the ultraviolet absorbed intensity of light method.

Description

자외선 흡광광도법을 이용한 Zn-Ni 도금액중 아민(Amine)계 첨가제의 정량분석방법Quantitative Analysis of Amine Additives in Zn-Ni Plating Solutions Using Ultraviolet Absorption Spectrophotometry

제1도는 본 발명에 따른 공시료용액에 대한 흡광도 측정결과를 나타낸 그래프1 is a graph showing the absorbance measurement results for the blank sample solution according to the present invention

제2도는 본 발명에 따라 작성된 검량곡선을 나타낸 그래프2 is a graph showing an calibration curve made in accordance with the present invention.

본 발명은 Zn-Ni 도금액중에 미량으로 첨가되어 있는 아민계 유기화합물의 농도를 정확하게 측정할 수있도록 자외선 흡광광동법을 이용하여 Zn-Ni 도금액중 아민계 첨가제의 양을 정량분석하는 방법에 관한 것이다.The present invention relates to a method for quantitatively analyzing the amount of an amine additive in a Zn-Ni plating solution by using an ultraviolet absorption photoelectron method to accurately measure the concentration of an amine organic compound added in a small amount in the Zn-Ni plating solution. .

일반적으로, 전기도금강판 제조공정에서는 제품의 백색도, 광택도, 도금밀착성 등을 향상시키기 위하여 여러가지 유기화합물을 미량으로 첨가하고 있다.In general, in the manufacturing process of the electroplated steel sheet, various organic compounds are added in a small amount in order to improve the whiteness, glossiness, plating adhesion, and the like of the product.

이러한 첨가제중 아민계 유기화합물 첨가제는 도금용액중에 미량으로 존재하지만 최종 도금제품에 미치는 영향이 매우 큰것으로 알려져 있어 엄격한 품질관리를 위해서는 이들 첨가제에 대한 정확한 정량분석방법이 요구되고 있으나, 현재 뚜렷한 첨가제의 농도분석방법이 정립되어 있지 않은 실정이다.Among these additives, amine-based organic compound additives are present in trace amounts in the plating solution, but the effects on the final plating products are known to be very large. Therefore, strict quality control requires accurate quantitative analysis of these additives. Concentration analysis method is not established.

최근 저정법을 이용한 정량분석방법이 개발되어 일부 사용되고 있는데, 이러한 적정법을 이용한 정량분석 방법은 다음과 같다.Recently, quantitative analysis methods using storage methods have been developed and used in part.

먼저, 아민계 첨가제가 첨가된 시료용액을 일정량 취하여 도금액의 주성분으로 된 ZnCl2, NiCl2, KCl함량을 원자흡광분석법을 이용하여 분석하고 시료의 pH를 정확히 측정하고 시료용액 15ml를 취하여 300ml-원추형 비이커(conical Beaker)에 넣고 에틸알콜(Methyl alcohol(99%이상)) 100ml가 한다(이때 침전이 많이 생기면 여과후 여액을 사용). 지시약 0.2%-브롬페놀 블루(Bromphenol Blue) 1ml를 가한 후 0.1N-HCl로 적정(V1) 산출한다.First, take a certain amount of the sample solution to which the amine additive is added, and analyze ZnCl 2 , NiCl 2 , and KCl content as the main components of the plating solution by using atomic absorption spectrometry, accurately measure the pH of the sample, and take 15 ml of the sample solution into a 300 ml-conical Put in a beaker (conical beaker) and 100 ml of ethyl alcohol (more than 99%) (if a lot of precipitation occurs, use the filtrate after filtration). After adding 1 ml of the indicator 0.2% -bromphenol blue (Bromphenol Blue) and titration (V 1 ) with 0.1N-HCl.

또한, 공시료(Blank test)용액에 소비된 0.1N-HCl량(ml)를 산출하기 위해, 시료용액에서 원자흡광법으로 분석한 ZnCl2, NiCl2, KCl을 함량에 맞게 증류수에 용해시킨 후 pH를 시료용액과 같게 조절한다(HCl 을 사용).In addition, in order to calculate the amount of 0.1 N-HCl consumed in the blank test solution (ml), ZnCl 2 , NiCl 2 and KCl analyzed by atomic absorption method in the sample solution were dissolved in distilled water according to the content. Adjust the pH to match the sample solution (using HCl).

이 용액 15ml를 취하여 300ml-원추형 비이커(conical Beaker)에 넣고 메틸알콜(Methyl alcohol(99%이상)) 100ml 가한후 지시약 0.2%-브롬페놀 블루 1ml를 가한후, 0.1N-HCl로 적정(V2)한다.Ml of this solution was placed in a 15ml 300ml- conical beaker (Beaker conical) methyl alcohol (Methyl alcohol (99% or higher)) 100ml was added and then the indicator 0.2% bromophenol blue was added to 1ml, titrated with 0.1N-HCl (V 2 )do.

상기 V1, V2로 부터 다음식에 대입시켜 아민계 첨가제의 농도(A)를 구한다.Substituting the following formula from V 1 , V 2 to obtain the concentration (A) of the amine additive.

그러나, 상기 적정법을 사용하여 아민계 첨가제의 농도를 구할 경우 분석과정의 조작이 복잡하고 농도분석용 시료용액과 공시료용액의 pH가 일정하지 않으면 분석이 불가능하며 적정시 공존하는 타 원소들의 방해 영향으로 종말점을 찾기가 매우 힘들어 정확성 및 정밀도가 떨어지는 문제점들이 있다.However, when the concentration of the amine additive is obtained using the titration method, the analysis process is complicated and the analysis is impossible unless the pH of the sample solution and the sample solution for concentration analysis is constant. As it is very difficult to find the end point, there are problems that the accuracy and precision fall.

이에, 본 발명의 목적은 Zn-Ni 도금액중에 미량 함유되어 있는 아민계 화합물의 농도를 자외선 흡광광도법을 이용하여 신속하고 정확하게 측정할 수 있는 새로운 분석방법을 제공하고자 하는데 있다.Accordingly, an object of the present invention is to provide a new analysis method that can quickly and accurately measure the concentration of the amine compound contained in a small amount in the Zn-Ni plating solution by using the ultraviolet absorbance spectroscopy.

상기 목적달성을 위해, 본 발명은 Zn-Ni 전기도금액중의 아민계 유기화합물을 정량분석함에 있어서, 아민계 유기화합물을 포함하고 있는 Zn-Ni도금액으로부터 시료용액을 일정량 취하여 원자 흡광분석법으로 시료용액중의 Ni함량을 분석산출하는 단계; 상기 시료용액중의 Ni함량과 동일하게 NiCl2용액을 첨가하여 공시료 용액을 조제하는 단계; 상기 공시료용액을 분취한 후 아민계 유기화합물 첨가제를 첨가하여 검량곡선용액을 조제하는 단계; 자외선 흡광도계를 이용하여 222nm 파장에서 상기 검량곡선용액의 흡광도값을 측정하여 첨가제의 투입량에 따른 흡광도값을 나타내는 검량곡선을 작성하는 단계; 자외선 흡광광도계를 이용하여 222nm파장에서 상기 시료용액의 흡광도를 측정한 다음 이 시료용액의 흡광도 값으로 부터 상기 검량곡선을 이용하여 시료용액중의 아민계 첨가제의 농도를 구하는 단계를 포함하여 구성되는 자의선 흡광광도법을 이용한 Zn-Ni 도금액중 아민게 첨가제의 정량분석방법에 관한 것이다.In order to achieve the above object, the present invention, in the quantitative analysis of the amine-based organic compound in the Zn-Ni electroplating solution, by taking a certain amount of the sample solution from the Zn-Ni plating solution containing the amine-based organic compound sample by atomic absorption spectrometry Analyzing the Ni content in the solution; Preparing a blank sample solution by adding NiCl 2 solution in the same manner as the Ni content in the sample solution; Preparing a calibration curve solution by separating the blank sample solution and adding an amine organic compound additive; Measuring an absorbance value of the calibration curve solution at a wavelength of 222 nm using an ultraviolet absorber to prepare an calibration curve indicating an absorbance value according to the amount of the additive added; Measuring the absorbance of the sample solution at a wavelength of 222 nm using an ultraviolet absorbance spectrometer, and then determining the concentration of the amine additive in the sample solution using the calibration curve from the absorbance value of the sample solution. The present invention relates to a quantitative analysis method of an amine crab additive in a Zn-Ni plating solution using a line absorbance method.

이하, 본 발명의 자외선 흡광광도법을 이용한 Zn-Ni 도금액중 아민계 유기화학물의 정량분석방법을 일예를 들어 상세히 실명한다.Hereinafter, a method for quantitative analysis of an amine-based organic chemical in a Zn-Ni plating solution using the ultraviolet absorbance method of the present invention will be described in detail.

먼저, 시료용액을 일정량 취하여 원자흡광분석법으로 도금액중에 함유되어 있는 원소들중 중금속 원소의 함량을 분석한 후, 아민계 유기화학물의 정량분석시에 가장 큰 영향을 미치는 Ni의 함량만을 분석 산출한 후, NiCl2용액을 시료용액중의 Ni함량과 같도록 첨가하여 공시료용액을 조제하고, 이 용액을 준비된 여러개의 메스프라스크에 일정량씩 각각 분쉬한 후 0.1%-아민계 유기화합물 첨가제의 양을 변화시키면서 첨가하고 증류수로 표선을 채워 검량곡선용액을 조제한다.First, a certain amount of the sample solution is taken, and the content of heavy metal elements among the elements contained in the plating solution is analyzed by atomic absorption spectrometry.Then, only the content of Ni which has the greatest influence in the quantitative analysis of amine organic chemicals is calculated and calculated. Prepare a blank sample by adding NiCl 2 solution equal to the Ni content in the sample solution, and then mix the solution with a number of prepared mesopras by a predetermined amount, and then add 0.1% amine-based organic compound additive. The solution is added with change and filled with distilled water to prepare a calibration curve solution.

공시료용액 및 검량곡선용액의 조제가 완료되면 자외선 흡광광도계를 이용하여 222nm의 파장에서 흡광도값을 각각 구하여 검량곡선을 작성한 다음, 시료용액의 흡광도를 측정하여 검량곡선으로부터 아민계 유기화합물 첨가게의 양을 산출하는 방법이다.After the preparation of the blank sample and the calibration curve solution, the absorbance values were obtained by using an ultraviolet absorbance spectrophotometer at a wavelength of 222 nm, and then the calibration curve was prepared.The absorbance of the sample solution was measured to measure the absorbance of the amine-based organic compound-added crab. It is a way to calculate the quantity.

이하, 실시예를 통하여 본 발명을 더욱 상세히 설명한다.Hereinafter, the present invention will be described in more detail with reference to Examples.

실시예Example

먼저, Zn-Ni 도금액으로 부터 시료용액을 일정량 취한 후 원자흡광분석법을 이용하여 시료용액중에 함유된 금속원소의 양을 분석한 결과 Zn은 90g/L, Ni은 12g/L, K는 280g/L이었다.First, after taking a certain amount of the sample solution from the Zn-Ni plating solution and analyzing the amount of metal elements contained in the sample solution using atomic absorption spectrometry, Zn is 90g / L, Ni 12g / L, K 280g / L It was.

한편, 상기 Zn-Ni도금액의 조성은 ZnCl2+NiCl2+KCl의 혼합용액으로 되어있으며, 여기에 아민계 첨가제를 일정량 첨가하여 사용하게 되는데, 아민계 첨가제의 정확한 정량분석을 위해서는 시료용액과 성분함량이 동일하게 공시료 용액을 조제하여야 하나, 상기 3가지 성분을 모두 혼합하여 조제하면 과포화상태가 되어 조제하기가 힘들고 시간의 지연으로 공정에 영향을 끼쳐 분석에 많은 지장을 초래하게 된다.On the other hand, the composition of the Zn-Ni plating solution is a mixed solution of ZnCl 2 + NiCl 2 + KCl, and is used by adding a certain amount of the amine additive, the sample solution and components for accurate quantitative analysis of the amine additive The same sample content should be prepared, but mixing and mixing all three components will result in a supersaturated state, making it difficult to prepare and affecting the process due to the delay of time.

따라서, 어떤 방법으로 공시료 용액을 조제하면 좋은지를 알아보기 위하여, 도금용액중에 다량 함유되어 있는 이들 금속원소들중 Ni과 Zn의 함량을 맞춰준 공시료용액, Ni과 K함량을 맞춰준 공시료용액, Ni과 K와 Zn항량을 맞춰준 공시료 용액, Ni함량만을 맞춰준 공시료용액들을 각각 조제한 후 자외선흡광광도계를 이용하여 흡광도를 측정한 결과 제1도에서와 같이 222nm에서 흡광도가 모두 같은 값을 나타내었다.Therefore, in order to find out how to prepare a blank sample solution, a blank sample solution in which the Ni and Zn contents of these metal elements contained in a large amount in the plating solution, and a blank sample in which the Ni and K contents are matched After preparing a solution, a blank sample solution with Ni and K and Zn contents, and a blank sample solution with Ni content only, the absorbance was measured using an ultraviolet absorbance spectrometer. As a result, the absorbance was the same at 222 nm as shown in FIG. The value is shown.

따라서, 제1도에 의하면 시료용액중에 함유된 금속원소들중 분석에 가장 큰 영향을 끼치는 NiCl2용액의 농도만을 맞춰주면 Zn-Ni도금액중의 아민계 첨가제의 정확한 분석이 가능함을 알 수 있다. 즉, KCl, ZnCl2의 함량은 맞춰주지 않아도 이들 원소들은 222nm에서 빛을 흡수하지 않기 때문에 분석에 영향을 미치지 않게 되며 따라서 NiCl2함량만을 정확히 맞춰주면 정확한 정량분석이 가능하게 된다.Therefore, according to FIG. 1, it can be seen that accurate analysis of the amine additive in the Zn-Ni plating solution is possible only by adjusting the concentration of the NiCl 2 solution which has the greatest effect on the analysis among the metal elements contained in the sample solution. That is, even if the contents of KCl and ZnCl 2 are not matched, these elements do not absorb light at 222 nm, and thus do not affect the analysis. Therefore, if only the NiCl 2 content is correctly adjusted, accurate quantitative analysis is possible.

이에따라, 본 발명에 의한 아민계 첨가제를 정량분석하기 위하여 NiCl2시약을 사용 시료용액중에 함유된 금속원소들중 분석에 가장 큰 영향을 끼치는 Ni의 함량만을 동일하게 하여 공시료용액을 조제한 후 준비된 5개의 250ml 메스플라스크에 각각 1ml씩 가한 다음 0.1%-아민계 첨가제를 0.5ml, 1ml, 2ml, 3ml, 4ml를 넣고 증류수로 표선을 채워 검량곡선용액을 조제하고, 자외선 흡광광도계를 이용하여 222nm에서 상기검량곡선용액의 흡광도를 측정하여 그 결과를 하기표 1에 나타내고, 이표로부터 첨가제투입에 따른 흡광도값을 나타내는 검량곡선을 작성한 결과를 제2도에 나타내었다.Accordingly, in order to quantitatively analyze the amine additive according to the present invention, the NiCl 2 reagent was used to prepare the blank sample solution after preparing the blank sample solution using the same Ni content which has the greatest effect on the analysis among the metal elements contained in the sample solution. 1 ml of each 250 ml volumetric flask was added, and 0.5 ml, 1 ml, 2 ml, 3 ml, and 4 ml of 0.1% amine-based additives were added to prepare a calibration curve solution with distilled water. The absorbance of the calibration curve solution was measured, and the results are shown in Table 1 below. The calibration curve showing the absorbance values according to the addition of additives was shown in FIG.

[표 1]TABLE 1

또한, 시료용액중 아민계 유기화합물의 양을 정량분석하기 위해, 검량곡선의 작성이완료된 후, 준비된 3개의 1L 메스플라스크에 아민계 유기화합물을 1ml, 2ml, 3ml씩 각각 가한후 아민계 유기화합물이 첨가되지 않은 Zn-Ni 전기도금액으로 표선을 채워 시료용액을 조제하고 자외선 흡광도계를 이용하여 222nm에서 흡광도를 측정한 결과, 각각 0.221, 0.435, 0.643의 흡광도값을 나타내었는데, 이렇게하여 구해진 흡광도 값으로 부터 제2도의 검량곡선을 이용하여 시료용액중의 아민계 첨가제의 농도를 구하고, 그 결과를 종래의 적정법을 사용하여 측정한 분석치와 함께 하기표 2에 나타내었다.In addition, in order to quantitatively analyze the amount of the amine-based organic compound in the sample solution, after the preparation of the calibration curve, the amine-based organic compound was added to each of the prepared 1L volumetric flasks by 1 ml, 2 ml, and 3 ml. The sample solution was prepared by filling the mark with this non-added Zn-Ni electroplating solution, and the absorbance was measured at 222 nm using an ultraviolet absorbance meter. As a result, the absorbance values were 0.221, 0.435, and 0.643, respectively. From the values, the concentration of the amine additive in the sample solution was determined using the calibration curve of FIG. 2, and the results are shown in Table 2 together with the analytical values measured using a conventional titration method.

[표 2]TABLE 2

상기 표 2에 나타난 바와같이, 자외선 흡광광도법을 이용한 본 발명의 분석치는 종래의 적정법을 이용한 분석치보다 정밀도와 정확성이 우수하게 나타났다.As shown in Table 2, the analysis value of the present invention using the ultraviolet absorbance spectroscopy showed better precision and accuracy than the analysis value using the conventional titration method.

따라서, 본 발명은 자외선 흡광광도법을 이용한 분석방법의 공시료 용액을 간단하고 신속하게 조제할 수있을 뿐만아니라 정확하고 정밀도가 높은 분석결과를 신속하게 얻을 수 있음을 알 수 있다.Therefore, it can be seen that the present invention can not only prepare a blank sample solution of the analytical method using ultraviolet absorbance spectroscopy in a simple and quick manner, but also obtain an accurate and accurate analysis result quickly.

상술한 바와 같이, 본 발명에 의하면, Zn-Ni 전기도금액중의 아민계 첨가제 농도분석을 분석조작의 복잡성과 분석값의 부정확성을 해결하여 신속하게 분석할 수 있는 정량분석방법이 제공되므로써, 전기도금용액중의 첨가제를 적절한 범위내에서 농도관리를 할 수 있게 되고, 따라서 전기도금제품의 백색도와 광택도, 도금밀착성등의 품질을 향상시킬 수 있는 효과가 있다.As described above, the present invention provides a quantitative analysis method capable of quickly analyzing the amine-based additive concentration analysis in Zn-Ni electroplating solution by solving the complexity of the analysis operation and the inaccuracy of the analysis value. It is possible to control the concentration of the additives in the plating solution within an appropriate range, thereby improving the quality of the whiteness, glossiness, plating adhesion and the like of the electroplating products.

Claims (1)

자외선 흡광도법을 이용하여 Zn-Ni 도금액중 아민계 유기화합물을 정량분석함에 있어서, 아민계 유기화합물을 포함하고 있는 Zn-Ni 도금액으로부터 시료용액을 일정량 취하여 원자흡광 분석법으로 시료용액중의 Ni함량을 분석산출하는 단계; 상기 시료용액중의 Ni함량과 동일하게 NiCl2용액을 첨가하여 공시료용액을 조제하는 단계; 상기 공시료용액을 분취한 후 아민계 유기화합물 첨가제를 첨가하여 검량곡선용액을 조제하는 단계; 자외선 흡광도계를 이용하여 222nm 파장에서 상기 검량곡선 용액의 흡광도 값을 측정하여 첨가제의 투입량에 따른 흡광도값을 나타내는 검량곡선을 작성하는 단계; 자외선 흡광광도계를 이용하여 222nm 파장에서 상기 시료용액의 흡광도를 측정한 다음 이 시료용액의 흡광도값으로부터 상기 검량곡선을 이용하여 시료용액중의 아민계 첨가제의 농도를 구하는 단계를 포함하여 구성되는 것을 특징으로 하는 자외선흡광광도법을 이용한 Zn-Ni 도금액중 아민계 첨가제의 정량분석방법.In the quantitative analysis of the amine organic compound in the Zn-Ni plating solution by using the ultraviolet absorbance method, a predetermined amount of the sample solution is taken from the Zn-Ni plating solution containing the amine organic compound, and the Ni content in the sample solution is determined by atomic absorption spectrometry. Analyzing and calculating; Preparing a blank sample solution by adding NiCl 2 solution in the same manner as the Ni content in the sample solution; Preparing a calibration curve solution by separating the blank sample solution and adding an amine organic compound additive; Measuring an absorbance value of the calibration curve solution at a wavelength of 222 nm using an ultraviolet absorber to prepare an calibration curve indicating an absorbance value according to the amount of the additive added; Measuring the absorbance of the sample solution at a wavelength of 222 nm using an ultraviolet absorbance spectrometer, and then determining the concentration of the amine additive in the sample solution using the calibration curve from the absorbance value of the sample solution. A quantitative analysis method of an amine additive in a Zn-Ni plating solution using an ultraviolet absorbance method.
KR1019910018621A 1991-10-22 1991-10-22 Untitative analysis method of the addition of amine group among zn-ni plating liquid using ultraviolet extinction photometry method KR950002923B1 (en)

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KR101325430B1 (en) * 2007-07-12 2013-11-04 주식회사 포스코 The method for quantitative anaylsis of uss-p and polyethylene glycol
CN105486651A (en) * 2016-01-21 2016-04-13 湖北金洋冶金股份有限公司 Chemical analysis method of lanthanum in lead-base alloy

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KR100474418B1 (en) * 2000-09-19 2005-03-08 주식회사 포스코 Quantitative Method of the organic additives in chloride bath

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101325430B1 (en) * 2007-07-12 2013-11-04 주식회사 포스코 The method for quantitative anaylsis of uss-p and polyethylene glycol
CN105486651A (en) * 2016-01-21 2016-04-13 湖北金洋冶金股份有限公司 Chemical analysis method of lanthanum in lead-base alloy

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