JPH06123742A - Automatic alloying degree measuring device for galvannealed layers - Google Patents

Abstract

(57) [Summary] [Purpose] The alloying degree of the galvannealed layer is automatically measured with high accuracy. [Structure] The turntable 1 is provided with a beaker installation place 18, and a single operation device such as a dissolved acid injector 11, a measurement sample mounting device 12, a beaker plate transfer machine 13, a solution sampling device 15 is arranged along the circumference thereof The sampled solution sample is sent to the analyzer 2 to measure the amounts of Zn and Fe. The computing unit 3 performs a series of operation commands and content rate computations. An atomic absorption method, a colorimetric method, or the like is used for the component amount measurement, and the flow injection method is appropriate. [Effect] Since the sample can be collected by chemical dissolution, it is possible to collect only the plating layer more accurately than the physical sampling method, and in combination with the measurement method, the measurement value can be obtained with high accuracy and precision while saving labor. To be

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a device for measuring the degree of alloying of a galvannealed steel sheet by chemical analysis.

[0002]

2. Description of the Related Art The degree of alloying of a galvannealed layer is an important factor that affects the workability, weldability, and paintability of plated steel sheets. Has been.

Reflected / scattered light measurement and X-ray measurement are performed because the instantaneous results are required in the online measurement, and chemical analysis methods are performed because accurate measured values are required in the offline measurement.

In the chemical analysis method, only the plating layer is dissolved with an acid added with an inhibitor that suppresses the dissolution of steel, and the amounts of Zn and Fe contained in the solution are determined by a colorimetric method, an atomic absorption method, a luminescence method, etc. The alloying degree is calculated from the content ratio. When this method is carried out by so-called manual analysis, precise measured values can be obtained, but there is a drawback that the measurement takes time and requires a lot of man-hours.

In order to make up for the drawback, analysis of equipment has been studied, and the Grim glow discharge method has hitherto been widely used.
When a voltage is applied between the analysis sample and the counter electrode in the atmosphere of an appropriate vacuum degree, glow discharge occurs and the sample is dug down from the surface layer of the sample to the deep layer. Since light emission continues through this process, the change of the contained element in the depth direction can be known by measuring the emission spectrum with time. The depth at which the Zn spectrum is no longer generated is the boundary between the plating layer and the steel substrate, and their content ratios can be obtained from the integrated value of the spectral intensities of Zn and Fe up to this boundary (for example, Nippon Steel Pipe Technical Report No. 117 P39-44).

[0006]

However, in the actual sample, the steel base may be exposed in a part of the measurement surface, but the plating layer may remain in the other part, so that the boundary is clearly defined. It was difficult to grasp and it was difficult to measure with sufficient accuracy. The present invention has been made in order to solve this problem, and aims at labor saving by automating the operation while maintaining the accuracy of the chemical analysis.

[0007]

Means for achieving this object is an automatic measuring device comprising a measuring sample adjusting device, a measuring device and a central processing unit, wherein the measuring sample adjusting device is a dissolved acid injector, Measuring sample mounter, beaker reversing machine, re-inversion take-out machine, sample desorber, solution sampler, rejector and beaker cleaning device, etc., which are sequentially arranged along the same circumference and beakers along this circumference. And a turntable for installing the measurement device, the measuring device has a Zn analyzer and an Fe analyzer connected to the solution sampler, and each part of these devices is operated by a central processing unit and a detection result is calculated. This is an automatic alloying degree measuring device for the galvannealed layer.

[0008]

[Operation] Dissolved acid injector, measurement sample mounter, beaker reversing machine, re-inversion take-out machine, sample desorption machine, along the same circumference
The solution extractor, the rejector, and the beaker washing device are arranged in this order, the beaker is installed on the turntable, and when the beaker is rotated in the above-described direction, the beaker returns to its original position via each device. Then, during this time, the alloyed plating layer is properly melted and the beaker is ready to receive the next sample.

First, install a beaker on the turntable,
Rotate the turntable. The beaker will eventually come to the dissolved acid injector as it moves along the same circumference along which the instruments are placed. Here, a dissolved acid that dissolves the alloyed plating layer is injected into the beaker. At the next position, the sample is mounted above the beaker by the measurement sample mounting device, and when the beaker is inverted by the beaker reversing machine in the following order, the sample is immersed in the dissolved acid and the alloying plating layer starts to dissolve. After a suitable time for dissolution, the beaker reaches the re-inversion take-out machine, where when it is turned over again, the sample escapes from the dissolved acid and is taken out.

In the next step, a solution in which the alloyed plating layer is dissolved (hereinafter referred to as a solution sample) is sampled by a solution sampler and sent to a measuring device. The beaker is further carried by the turntable, discards the solution remaining at the rejector, is cleaned by the cleaning device, and returns to its original position. At this point, the beaker is ready for the next sample preparation and can be used automatically and repeatedly. If a plurality of beaker installation locations are provided on the turntable, a plurality of solution samples can be collected while the turntable makes one rotation.

The measuring device has a Zn analyzer and an Fe analyzer, and the amount of the solution sample collected and sent to the measuring device is measured by these analyzers. As the analyzer, a colorimeter atomic absorption device, an emission spectroscopic analysis device, or the like can be used. In general, when measuring, Zn and Fe have different dilution ratios and reagents, so it is preferable to provide a Zn analysis circuit and an Fe analysis circuit in parallel.

The central processing unit controls the rotation speed of the turntable according to the melting time of the alloyed plating layer or tunes other equipment, and calculates the alloying degree from the analysis result. As can be easily inferred from the above description, this automatic alloying degree measuring apparatus for an alloyed zinc plating layer can be selected by appropriately selecting a reagent, and the alloying degree of another alloying plating, for example, zinc- Nickel, zinc-
It can also be used to measure alloy plating of cobalt, aluminum-chrome, etc.

[0013]

EXAMPLE Using one example of the apparatus according to the present invention, the degree of alloying of the alloyed plating layer was measured and its accuracy was investigated. The apparatus used is shown in FIG. In the figure, 1 is a turntable, 2
Is a measuring device, 3 is a central processing unit, 11 is a dissolved acid injector, 1
2 is a sample mounting device, 13 is a beaker reversing machine, 14 is a reversing retrieving machine, 15 is a solution sampler, 16 is a rejector, and 17
Is a beaker cleaning device, and 18 is a beaker installation place.

Eight beaker installation locations 18 were provided on the turntable 1 so that eight samples could be measured once. Further, various devices arranged along the turntable 1 such as the dissolved acid injector 11 and the measurement sample mounting device 12 are arranged at equal intervals, so that the beaker installation places 18 are also arranged at equal intervals, and the longest dissolution is required. The turntable was stopped in time.

The structure of the sample mounting mechanism and the beaker is shown in FIG. A ring receiver was provided along the circumference on the opening side of the beaker 31, a rubber O-ring packing 32 was applied, and a test piece 33 was used to cover. The movement of the test piece 33 was performed by the suction type robot hand 34. After mounting the test piece 33,
When the beaker 31 is inverted, the test piece 4 is dipped in the dissolved acid 35,
It comes out when re-inverted.

The details of the measuring device 2 are shown in FIG. 21 is a diluter, 22 is a reagent adder, 23 is a Zn analyzer, 24 is F
e analyzer. A colorimeter was used for the Zn analyzer 23 and the Fe analyzer, and measurement was performed by a flow injection method.
The flow tube had an inner diameter of 0.5 mm and the flow rate was 1 to 2 ml per minute. The measurement results are shown in Table 1.

[0017]

[Table 1]

In the embodiment of the present invention, a value (≤ ± 0.04%) extremely close to the analysis value obtained by manual analysis was obtained, but in the conventional discharge method, a value farther than this value (+0.
It is about 1 to 0.5%).

[0019]

As described above, according to the present invention, the chemical analysis method is used for measuring the alloying degree of the plating layer. However, from the dissolution of the sample, the solution is collected, the components are analyzed, and the alloying degree is calculated. All can be done automatically. For this reason, highly accurate measurement values can be obtained without requiring human intervention, and precise control of product quality becomes easy. The effect of the present invention that contributes to the technology for stably producing high-quality products in this way is great.

[Brief description of drawings]

FIG. 1 is a diagram showing an outline of an automatic analyzer used in an embodiment of the present invention.

FIG. 2 is a diagram showing an outline of an analyzer used in an example of the present invention.

FIG. 3 is a sub-sectional view of a beaker and a test piece used in an example of the present invention.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 turntable 2 measuring device 3 central processing unit 11 dissolved acid injector 12 measurement sample mounting device 13 beaker reversing machine 14 re-reversal taking-out machine 15 solution sampling machine 16 discarding machine 17 beaker washing machine 18 beaker installation location 21 diluter 22 reagent addition Analyzer 23 Zn analyzer 24 Fe analyzer

Claims (1)

[Claims] 1. A dissolved acid injector, a measurement sample mounting device, a beaker reversing machine, a reversing retrieving machine, a sample desorption device, a solution sampling device,
A measurement sample adjusting device, in which a rejector and a beaker washing device are sequentially arranged along the same circumference and a turntable for installing a beaker along the circumference is arranged, a Zn analyzer connected to the solution sampler, An automatic alloying degree measuring apparatus for an alloyed galvanized layer comprising a measuring apparatus having a Fe analyzer and a central processing unit.