JPH0643151A - Method for analyzing glycol acid sodium in carboxymethylcellulose - Google Patents

Abstract

PURPOSE:To analyze glycol acid sodium rapidly by dissolving carboxymethylcellulose with sodium perchlorate and by adding the liquid solution to gel permeation chromatograph(GPC) with sodium perchlorate as a mobile phase. CONSTITUTION:After carobxymetylcellulose is dissolved by sodium perchlorate, the liquid solution is analyzed for GPC with sodium perchlor ate as a mobile phase. The ratio of carobxymethylcellulose which is dissolved in perchloric acid is approximately 0.2. An ultraviolet ray light absorption detector is preferable as a means for detecting the GPC. Namely, the mobile phase is allowed to flow from a mobile phase storage tank 1 by a pump 2 for creating a steady state. Then, a specimen is poured from a manual injector 3, the poured specimen is sent to a column 4 inside a column oven 5 and sodium glycolate in carboxymetylcellulose is analyzed by an ultraviolet light absorption detector 6. Processing is performed by a data processing device 7 and a quantitative calculation is performed.

Description

Detailed Description of the Invention

[0001]

FIELD OF THE INVENTION The present invention relates to a method for analyzing sodium glycolate in carboxymethyl cellulose.
More specifically, it relates to a method for analyzing sodium glycolate in carboxymethyl cellulose, which is suitable for quality control, performance evaluation and the like of carboxymethyl cellulose using a gel permeation chromatograph (hereinafter referred to as GPC).

[0002]

2. Description of the Related Art Carboxymethyl cellulose is a kind of cellulose ether and is obtained by allowing a sodium salt of monochloroacetic acid to act on cellulose in the presence of an alkali. Soda salts having an etherification degree of 50 or more and about 100 are dissolved in water at room temperature, and heavy metal salts are precipitated. This cellulose ether is a water-soluble polymer compound such as C.I. M. It is called C and is manufactured industrially.

Therefore, quality control, performance evaluation, etc. are required for use in such materials, and it is desired to analyze sodium glycolate in carboxymethyl cellulose. Therefore, conventionally, after dissolving carboxymethylcellulose in water, pretreatment was performed and analysis was performed by liquid chromatography.

[0004]

However, in the conventional method, there is a drawback that the pretreatment takes a long time because the pretreatment is very complicated. Therefore, carboxymethylcellulose cannot be quickly evaluated, which is a difficulty in industrialization.

Therefore, an object of the present invention is to solve the above problems by analyzing sodium glycolate in carboxymethyl cellulose by a novel analysis method.

[0006]

Means for Solving the Problems The inventors of the present invention have made extensive studies to solve the above problems, and as a result, have found that when sodium glycolate in carboxymethyl cellulose is analyzed in GPC mode, the conventional problems can be solved at once. The present invention has been completed.

That is, the present invention is characterized in that carboxymethylcellulose is dissolved in sodium perchlorate and then the solution is subjected to gel permeation chromatography using sodium perchlorate as a mobile phase for analysis. It is a thing.

[0008] Here, the concentration of sodium perchlorate may be any as long as it dissolves carboxymethylcellulose, but is preferably about 100 to 400 mM. This is because the solubility of carboxymethyl cellulose is low below this range, and the solubility does not change above this range. Sodium perchlorate itself may be a commercially available product or may be purified before use.

To dissolve carboxymethylcellulose in sodium perchlorate, for example, carboxymethylcellulose may be placed in a beaker and an appropriate amount of sodium perchlorate may be added thereto, but the method is not limited. The amount of sodium perchlorate required for dissolution obviously depends on the sample amount, but the proportion of carboxymethyl cellulose dissolved is about 0.2% by weight.
When sodium perchlorate is added to carboxymethyl cellulose, sodium glycolate in carboxymethyl cellulose is dissolved and subjected to GPC. GP
A known sample introduction device can be used for attaching to C, whereby a predetermined amount of solution can be injected into GPC.

The solution injected into GPC is applied to a separation column with sodium glycolate as a mobile phase. Here, it is preferable for the operation of the apparatus that the mobile phase of GPC and the solution for dissolution are the same.

As the separation column used in GPC, a column packed with a general-purpose polymer gel can be used. For example, a packed column of vinyl alcohol copolymer gel can be mentioned as a suitable example.

As the GPC detection means, for example, an ultraviolet absorption detector is preferably used.

[0013]

According to the present invention, it is possible to analyze sodium glycolate in carboxymethyl cellulose simply by dissolving the carboxymethyl cellulose and then immediately applying it to GPC.

[0014]

DESCRIPTION OF THE PREFERRED EMBODIMENTS An apparatus configuration for carrying out the method of the present invention will be described with reference to the drawings. FIG. 1 shows an example of an apparatus for carrying out the method of the present invention, 1 is a mobile phase storage tank, 2 is a liquid feed pump, 3 is a manual injector, 4 is a column, 5 is a column oven, and 6 is an ultraviolet absorption detector. , 7 are data processing devices.

In the analysis, the mobile phase is preliminarily flowed from the mobile phase storage tank 1 by the pump 2 to make a steady state.
Next, the sample is injected from the manual injector 3.
The injected sample is sent to the column 4 in the column oven 5 by the mobile phase and detected by the ultraviolet absorption detector 6.
This data is processed by the data processing device 7, and quantitative calculation is performed.

Using the above apparatus, analysis was carried out under the following analysis conditions. (1) Pretreatment of sample 10 mg of carboxymethyl cellulose was dissolved in 5 ml of sodium perchlorate, and a membrane filter (pore size:
0.45 μm). Next, add 200 μl of the filtrate to G
Attached to PC.

(2) Analytical conditions Column: Asahipak GS-710H, 310H
(Manufactured by Shimadzu Corporation) Two connected (each 7.6 mm ID × 250 mm) Mobile phase: 200 mM sodium perchlorate Flow rate: 1.0 ml / min Temperature: 40 ° C. Detector: SPD-6A ( Ultraviolet absorption detector (manufactured by Shimadzu Corporation) Sensitivity: 0.16 AUFS Wavelength: 220 nm (3) Analysis results The results of analysis under the above analysis conditions are shown in FIG. As can be seen by comparing this FIG. 3 with the chromatogram of sodium glycolate (FIG. 2), the peak is the peak of sodium glycolate. From this figure, according to the present invention, sodium glycolate in carboxymethyl cellulose is analyzed with high sensitivity. I know that I can do it. 2 and 3, the vertical axis represents signal intensity and the horizontal axis represents holding time.

[0018]

INDUSTRIAL APPLICABILITY According to the present invention, sodium glycolate in carboxymethyl cellulose can be efficiently analyzed,
It has the advantage that it can be performed accurately and that the analysis can be completed in a short time because no pretreatment is required. further,
It has a special effect that quality control and performance evaluation of nitrile rubber can be easily performed by quantifying sodium glycolate in carboxymethyl cellulose.

[Brief description of drawings]

FIG. 1 shows an apparatus for implementing the arrangement of the present invention.

Figure 2: Chromatogram of sodium glycolate

FIG. 3 is a diagram showing the results of analysis by the method of the present invention.

[Explanation of symbols]

 1: Mobile phase storage tank 4: Analytical column 6: Detector

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[Procedure amendment]

[Submission date] August 24, 1993

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[Document name to be corrected] Drawing

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[Procedure Amendment 2]

[Document name to be corrected] Drawing

[Name of item to be corrected] Figure 3

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[Figure 3]

Claims (1)

[Claims] 1. Dissolving carboxymethylcellulose with sodium perchlorate, and subjecting the solution to gel permeation chromatography using sodium perchlorate as a mobile phase for analysis. Analytical method for sodium glycolate.