JP2888086B2 - Kit for measuring concentration of activator in drainer and method of measurement - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a measuring kit and a measuring method for easily measuring the concentration of an activator in a draining agent containing methylene chloride as a main component.

[0002]

2. Description of the Related Art
As a typical draining agent, there is known one having methylene chloride as a main component, to which an activator is added to obtain a high draining effect. As the activator, carboxylic acids and amines are generally used, and a surfactant is provided by forming a carboxylic acid amine salt in a draining agent. In this case, an excess of amines is added. This improves the draining performance.

When water is taken into the draining agent when the draining agent containing methylene chloride as a main component is used, the solubility of water in the draining agent (methylene chloride) is low.
Separate into two layers, a methylene chloride layer and an aqueous layer. This aqueous layer is separated by a water separator and removed outside the system, but the carboxylic acid amine salt and excess amines in the draining agent are slightly dissolved in water, and a part of them is transferred to the aqueous layer, It will be discharged out of the system. Therefore, when the draining agent is used for a long period of time, the concentration of the activator in the draining agent decreases, and the draining function is deteriorated.

[0004] Separately, the concentration of the activator in the drainer may increase due to volatilization of methylene chloride.
If the concentration of the activator is thus high, the activator tends to remain on the drained material, which is not preferable. For this reason, it is essential to control the activator concentration of the draining agent to an appropriate value.

Conventionally, the activator concentration of a drainer is typically controlled by measuring the excess amine concentration. That is, the decrease in the excess amine concentration is due to a decrease in the concentration of the activator caused by the transfer of the activator into the water taken into the drainage agent, and the decrease in the concentration results in a decrease in the drainage performance. In this case, it is necessary to add an activator to increase the activator concentration. On the other hand, the increase in the excess amine concentration is caused by the increase in the concentration of the activator due to the volatilization of methylene chloride, and this increase in the concentration poses a risk of the activator remaining in the drainage. In this case, methylene chloride is added. It is necessary to dilute the activator in the drainer, thereby reducing the activator concentration.

A typical method of measuring the excess amine concentration is a method by neutralization titration. That is, a coloring agent and a compatibilizing agent are added to a draining agent containing methylene chloride as a main component, hydrochloric acid is dropped, and a point at which the coloring indicator changes color is set as an end point. The concentration of the activator is determined by collating with a calibration curve showing the relationship between the amount and the concentration of the activator.

Here, the compatibilizer is added for the purpose of preventing two-layer separation by hydrochloric acid titration and poor color formation, which occur due to the hydrophobic nature of methylene chloride, which is the main component of the draining agent.

[0008] On the other hand, bromophenol blue is typically used as a color-forming indicator, but it is necessary to be skilled to determine the end point due to the change from blue to yellow, and individual differences are likely to occur. In addition, when the amount of the color-forming indicator is small, the coloration is reduced and the change in color is reduced, so that it is difficult to determine the end point. Further, after the completion of the hydrochloric acid titration, in order to determine the concentration of the activator from the amount of hydrochloric acid dropped, it is necessary to perform operations such as checking with a calibration curve. When a concentration abnormality occurs, it is difficult to take an immediate response.

The present invention has been made in view of the above circumstances,
It is an object of the present invention to provide a measurement kit that can easily measure the concentration of an activator in a draining agent containing methylene chloride as a main component, and a measurement method using the same.

[0010]

SUMMARY OF THE INVENTION The present invention provides a measuring kit for measuring the concentration of an activator in a draining agent containing methylene chloride as a main component. An acidic substance for adjusting the pH to a predetermined pH range, a color-forming indicator that changes color in the pH range, and an analytical solution containing a compatibilizer that makes the acidic substance and the color-forming indicator compatible with the drainage agent, Provided is a kit for measuring the concentration of an activator in a draining agent, comprising a color sample showing a color when the above-mentioned solution for analysis is added to the draining agent having a known concentration of an activator to form a color.

[0011] The present invention also provides a draining agent test sample containing methylene chloride as a main component whose activator concentration is to be measured, and adding the above-described analysis solution to the test sample to form a color. The present invention provides a method for measuring the concentration of an activator in a drainage agent, which comprises determining the concentration of the activator in the test sample by comparing the indicated color with the color sample.

According to the method for measuring the concentration of an activator in a draining agent using the measurement kit of the present invention, a color is formed only by adding a certain amount of the above-mentioned draining agent to a certain amount of the solution for analysis and shaking the hand. The activator concentration in the draining agent can be determined simply by colorimetrically comparing with the color sample, so that the activator concentration can be measured by a simple operation, and there is little individual difference in the measurement results. Since the measurement can be performed, it is possible to instantaneously cope with an abnormality in the activator concentration.

Hereinafter, the present invention will be described in more detail. The kit for measuring the concentration of an activator in a draining agent according to the present invention is different from an analytical solution comprising an acidic substance, a color-forming indicator and a compatibilizing agent at different pHs. This is a kit for measuring the activator concentration of a draining agent containing methylene chloride as a main component.

The activator in the draining agent, that is, the activator to be measured in the present invention, is a carboxylic acid and an amine and a carboxylic acid amine reacted with them, and specifically, n-caproic acid. , N-octylamine and the like, and according to the present invention, the concentration of these activators in methylene chloride can be determined simply and quickly.

Here, the acidic substance contained in the analysis solution is added to adjust the pH region corresponding to the color indicator. That is, the pH determined by water extraction of a draining agent containing methylene chloride as a main component is about 8, and the pH determined by water extraction of the draining agent whose activator concentration has decreased and the draining performance has deteriorated is about 7.3. Therefore, when the draining agent is used without adding an acidic substance, the fluctuation in pH is small, and the difference in coloring cannot be determined. For this reason, by adding an acidic substance to the solution for analysis, the fluctuation range of the pH is increased, and the pH is adjusted to a pH range corresponding to the discoloration range of the color-forming indicator.

Specific examples of the acidic substance include hydrochloric acid, sulfuric acid, and organic acids. Of these, hydrochloric acid is particularly preferable because it is inexpensive. The concentration of the acidic substance in the analysis solution varies depending on the concentration of the coloring indicator used and the compatibilizer added to the draining agent. For example, methylene chloride is used as a main component, and carboxylic acids and amines are used as an activator. When a typical drainer is measured using a color indicator whose discoloration range is 3 to 5 in the pH range, 0.02 to 0.
It is preferably set to 03 mol / l. If the pH is out of this range, the pH range is shifted to either side, and the difference in color development may be difficult to understand.

As the above-mentioned coloring indicator, those having a large change in indicator color at pH 3 to 5 are preferable. Discoloration area is p
If a color indicator less than H3 is used, excessive hydrochloric acid is required for pH adjustment, which is economically disadvantageous. Further, when a color-forming indicator having a discoloration range exceeding pH 5 is used, the fluctuation range of pH with respect to the concentration of the activator becomes small, and colorimetry may be difficult. Specific examples of the color-forming indicator include bromophenol blue (BPB), bromthymol green, and the like.

The concentration of the color indicator in the analysis solution may be arbitrary as long as the degree of color development can be understood. For example, BP
When using B, BPB for 30 ml of the solution for analysis
It is preferable to add 3 to 4 drops of a 0.1 g / 100 ml aqueous solution.

The compatibilizing agent is not particularly limited as long as it can mix the hydrophobic draining agent and the analysis solution, but the general formula R—OH (where R is the number of carbon atoms) Alcohols represented by 1 to 3) are preferred, and ethanol is particularly preferred from the viewpoint of safety.

The concentration of the compatibilizer in the analysis solution may be any amount as long as the draining agent and the analysis solution can be completely mixed. It is preferred to add. For example, when ethanol is used, it is preferable that ethanol be 20 ml or more for 10 ml of a draining agent.

The color sample shows the color when a certain amount of a draining agent containing methylene chloride as a main component at various concentrations of an activator is added to a certain amount of the solution for analysis. In this case, in the draining agent, it is necessary for the activator to be within a certain control range in order to obtain good drainage performance. In some cases, it is preferable to include three types in the case of being at the control lower limit, and it is generally effective to create three to six types. It should be noted that the color sample can be usually placed in a colorless and transparent container such as a test tube or a sample bottle in an amount of about 20 to 50 ml, and compared with the color of the test sample in the same container. Alternatively, a color sample that is color-printed on paper or the like in the same color as the color sample sample thus formed can be used, and the form of the color sample is not particularly limited.

In order to measure the concentration of the activator in the drainer containing methylene chloride as a main component using the kit for measuring the concentration of the activator of the present invention, a certain amount of a test sample of the drainer and a certain amount of the analysis solution are used. The test sample is colored by mixing, and the indicated color is compared with the color sample to determine the concentration range of the activator in the test sample from the concentration of the activator added to the color sample. In this case, the mixing of the draining agent and the analysis solution in the measurement of the active concentration is the same amount as when the color sample was prepared,
The same mixing ratio or the same mixing ratio is recommended for accurate measurement. In addition, the mixing at the time of measuring the active concentration is not particularly limited as long as the draining agent and the solution for analysis are uniformly mixed and the color development becomes clear, and a hand gesture is sufficient.

The mixing ratio of the analysis solution and the draining agent is not particularly limited, but it is preferable that the ratio of the analysis solution (ml) / the draining agent (ml) is 0.8 to 3. When this ratio is less than 0.8, a large amount of draining agent used for analysis is required,
If it exceeds 3, both are not economical because a large amount of analysis solution is required.

[0024]

The present invention will be described below in more detail with reference to Examples, but the present invention is not limited to the following Examples. [Example 1] First, an analysis solution was prepared with the following composition. 1/10 N hydrochloric acid 7.5 ml Ethanol 20 ml 0.1 g / 100 mg BPB aqueous solution 5 drops Next, Table 1 using an activator containing methylene chloride as a main component and prepared by mixing n-octylamine and n-caproic acid was used. A draining agent sample having the composition shown was prepared, and 10 ml of the draining agent and 25 ml of the solution for analysis were mixed by hand shaking. The coloration state is also shown in Table 1.

[0025]

[Table 1]

As described above, methylene chloride is the main component,
A draining agent using n-octylamine and n-caproic acid as activators was prepared, and a draining agent having a good draining state was sampled. 25 ml of the same solution for analysis and 10 ml of a draining agent were added and stirred by hand. No. 2
And No. 3 and the activator concentration of this drainer could be determined to be 1.5-1.7% by weight.

Example 2 Example 1 was repeated except that a sample of a draining agent having a poor drainage state used for draining was used as a sample.
It measured by the same operation as above. No. 1 and No. 2, and the activator concentration of this drainer is 1.2 to
It could be determined to be 1.5% by weight.

[0028]

According to the present invention, the concentration of the activator of the draining agent containing methylene chloride as a main component can be determined and measured quickly and easily without any individual differences.

──────────────────────────────────────────────────続 き Continuing from the front page (72) Inventor Takaaki Shimizu 28-1 Nishifukushima, Kazagi-son, Nakakubijo-gun, Niigata Shin-Etsu Chemical Industry Co., Ltd. Synthetic Technology Laboratory (58) Field surveyed (Int. Cl. ⁶ , DB G01N 31/22 123 G01N 31/00 G01N 33/00

Claims (2)

(57) [Claims] 1. A measuring kit for measuring the concentration of an activator in a draining agent containing methylene chloride as a main component, comprising: an acidic substance for adjusting the draining agent to a predetermined pH range;
An analytical solution containing a color-forming indicator that changes color in the pH range, a compatibilizer that makes these acidic substances and the color-forming indicator compatible with the draining agent, and the analytical solution containing the known draining agent having various known activator concentrations. A kit for measuring the concentration of an active agent in a draining agent, comprising a color sample showing a color when a solution is added to form a color. 2. A sample of a draining agent containing methylene chloride as a main component to be measured for the concentration of an activator is collected, and the solution for analysis according to claim 1 is added thereto to color the sample. A method for measuring the concentration of an activator in a drainer, comprising determining the concentration of the activator in the test sample by comparing the indicated color at that time with the color sample.