JPH0579975A - Standard sample for atomic absorption analysis and manufacture thereof - Google Patents

Abstract

PURPOSE:To perform a correct analysis by providing a standard sample for direct quantitative analysis by the graphite furnace atomic absorption method, and uniformly distributing the preset quantity of a metal sample in a hardening resin. CONSTITUTION:A standard material of Cu is dissolved in xylene, and a fixed quantity of it is added to the liquid portion of two-constituent normal- temperature hardening methyl metal acrylate. The remaining resin powder is added, stirred, and hardened. It is crushed with a crusher and the like after hardening, it can be easily machined, and a standard sample can be manufactured in a short time.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a standard sample for atomic absorption spectrometry used in general chemical analysis and a method for producing the same.

[0002]

2. Description of the Related Art As one of elemental analyzes, there is an atomic absorption method. The measurement principle of this atomic absorption method is to make a sample into an atomic state at a high temperature, irradiate this atom with an electromagnetic wave (light) of a specific wavelength, excite the atom to transition to an electronic state with high internal energy, and then When it returns to, it emits fluorescence of a specific wavelength, and elemental analysis is performed by measuring this.

As a standard sample used for direct measurement by the graphite furnace atomic absorption method of the prior art, a metal element (pure substance) is used by weighing several ng to several 100 ng (nanogram), or a slightly larger weight. It was used after being weighed, diluted and dispersed with a diluent. Further, there have been few attempts to directly determine a powder sample by the atomic absorption method, and as a solid standard substance, it is mainly performed to adsorb a metal to be measured on an ion exchange resin or to use it in the form of a metal-oxine salt. It was

[0004]

However, in the above-mentioned prior art, if a powder of a pure substance is used as a standard sample, several ng to several 100 ng must be accurately weighed, and this weighing is extremely difficult. there were. Further, using a diluent or adsorbing it on an ion-exchange resin has a problem that it is not suitable as a standard sample because uniform dispersion may be difficult. Further, these standard sample preparation methods have problems that the procedure is complicated and that adsorption, drying, and the like take time.

It is an object of the present invention to provide a standard sample which can accurately measure the concentration of the sample and can be easily manufactured, and a manufacturing method thereof.

[0006]

In order to achieve the above object, the standard sample for atomic absorption analysis of the present invention is characterized in that a predetermined amount of a metal sample is uniformly dispersed in a curable resin.

In the method for producing a standard sample for atomic absorption analysis of the present invention, first, a certain amount of a metal component to be a standard sample is sampled, dissolved or uniformly dispersed in an organic solvent, and then the curable resin is prepared. It is characterized in that it is dissolved or uniformly dispersed in a liquid of a monomer or an oligomer, then a curable resin is added and mixed to the mixed liquid of the monomer or oligomer and then cured, and then the obtained polymer is ground or sliced.

[0008]

According to the structure of the present invention, a predetermined amount of the metal sample is uniformly dispersed in the curable resin so that the concentration of the sample can be accurately measured. That is, since it is a mixture of liquids to which a metal component dispersed or dissolved in a liquid of a monomer or an oligomer of a curable resin is added, it can be easily and uniformly dispersed in a resin component. A cross-linking agent or a curing agent is added to this, the mixture is stirred and cured, and since it is a standard sample using a synthetic resin as a matrix, it is easy to prepare,
And it is easy to handle. Also, since it is a solid sample,
It can be easily processed into powder or pellets by crushing or slicing after molding, and a standard substance having a uniform weight can be prepared. By using such a standard sample, the trace elements in other synthetic resins or plastics of the same matrix can be measured more accurately.

[0009]

EXAMPLE A standard sample for atomic absorption analysis of the present invention is one in which a standard sample is uniformly dispersed in a curable resin, and can be prepared through the steps shown in FIG. First, a solution of a standard substance is prepared (step 1). At this time, the solvent is preferably xylene, and any solvent may be used as long as it does not affect the curable resin. Then, the solution of the standard substance is added to a solution portion of a monomer such as methyl methacrylate or an oligomer, for example (step 2). The remaining one component (polymer) of the two-component resin is added (step 3) and stirred. Then, it is cured according to the conditions of the resin used (step 4). When carrying out the curing reaction, a curing agent and / or a crosslinking agent which are usually used are added. This polymerization method is a method called a wet molding method among molding methods for methacrylic resins such as polymethylmethacrylate.
The method of the present invention can efficiently prepare a standard sample by adopting this wet molding method.

Next, the sample concentration (step 5) is determined from the weight of the cured resin and the standard sample weight, and this is crushed with a crusher (while cooling with dry ice) or a microtome (micro slicing device). Slices (eg 10-3
0 μm) (step 6).

A detailed description will be given below. Example 1 A method for preparing a Cu (copper) standard material is as follows.

Copper (II) -acetylacetonate (hereinafter C
u (II) -AA) has a Cu concentration of 100 ppm (W /
V) is weighed and dissolved in xylene. It is preferable that the sample Cu (II) -AA is weighed in the order of mg or more from the viewpoint of easy weight measurement.

A certain amount of the sample dissolved in xylene is added to the liquid portion (monomer or oligomer) of the binary cold-curing methyl methacrylate. Furthermore, a powder (polymer) of a two-component system room temperature curing methyl methacrylate resin is added and stirred. It is left to cure at room temperature for 5 minutes.
The curing reaction varies depending on the type of curing agent, but may be room temperature curing, or may be heated to about warm water or heated to a temperature higher than that. The curing time can be arbitrary. The xylene solvent used first was scattered during the curing reaction and did not remain in the polymer.

After curing, if the total weight is measured, the concentration of Cu contained in the sample can be calculated from the amount of added Cu. After hardening, it can be crushed with a crusher (while cooling with dry ice or the like) or sliced with a microtome or the like to make powder or small pieces easily. It is preferable that the powder or the small pieces is a small piece having a thickness of, for example, about 10 to 30 μm or a powder having a particle diameter of, for example, about 1 to 30 μm.

In addition to copper, Cd (II) -CHBA
(4-cyclohexyl cadmium sulfate), Zn-CHB
A (A, S) (4-cyclohexyl butyric acid) or the like can be used. In addition, it is also possible to use a liquid extracted from an aqueous solution into an organic solvent. Organic solvents other than xylene,
Any resin that does not inhibit the curing of the resin can be used.

When crushed, it can be made into a solid standard substance having a uniform weight by shaping it into a fine pellet having a regular shape. That is, unlike a liquid, a powder sample can easily ingest a minute amount.

[0017]

EFFECT OF THE INVENTION The standard sample for atomic absorption spectrometry and the method for producing the same of the present invention can be easily and uniformly dispersed in a resin component, and can be easily pulverized or sliced after curing and molding into powder or pellet form. It can be molded, and a solid standard sample can be obtained easily and in a short time. Further, by using such a standard sample, the trace elements in other synthetic resins or plastics of the same matrix can be measured more accurately.

[Brief description of drawings]

FIG. 1 is a process diagram of preparing a standard sample of the present invention.

Claims (2)

[Claims] 1. A standard sample used when directly quantifying a solid sample by a graphite furnace atomic absorption method, wherein a predetermined amount of a metal sample is uniformly dispersed and present in a curable resin and molded into a powder or pellet form. A standard sample for atomic absorption spectrometry, which is characterized in that 2. A method for producing a standard sample used when directly quantifying a solid sample by a graphite furnace atomic absorption method, which comprises first collecting a fixed amount of a metal component to be the standard sample and dissolving or uniformly dissolving it in an organic solvent. Disperse, then dissolve or uniformly disperse this in a liquid of a curable resin monomer or oligomer, and then add and mix a curable resin to the mixed liquid of the monomer or oligomer, and then cure, and then
A method for producing a standard sample for atomic absorption spectrometry, which comprises crushing or slicing the obtained polymer.