JP2010117284A - Autosampler, atomic absorption photometer, and pretreatment method - Google Patents

Abstract

【Task】
Provided is an atomic absorption photometer autosampler capable of performing pretreatment of an atomic absorption photometer by a simple method without taking time and effort.
[Solution]
The autosampler of the present invention is provided in an atomic absorption photometer, and is an autosampler that introduces a metal into an atomization portion of an atomic absorption photometer, which is a solid-phase extraction in which a metal in a liquid sample is adsorbed Agent 10 is provided at the tip. Thereby, since the metal can be adsorbed to the solid-phase extraction agent 10, the pretreatment can be performed using an autosampler, that is, by automating the metal by elution using an eluent after washing. .
[Selection] Figure 1

Description

  The present invention relates to an atomic absorption photometer, an autosampler, and a pretreatment method for taking out a metal to be introduced into the atomic absorption photometer.

  In elemental analysis methods such as atomic absorption spectrophotometry and inductively coupled plasma emission spectrometry, coexisting substances other than the target metal contained in the liquid sample may interfere with the target metal, and a correct analytical value may not be obtained. Also, depending on the analyzer used, when the concentration of the target metal is dilute, the analytical value cannot be obtained because it is below the detection limit value.

  In order to solve such problems, generally organic solvent extraction or solid phase extraction is performed, the target metal contained in the liquid sample is separated from the interfering substance, that is, pretreatment is performed, and the interfering substance is removed in advance. The analysis is performed after removing or concentrating the target metal.

JP-A-7-289925

  However, in order to perform pretreatment of a liquid sample using a solid-phase extraction agent, conditioning such as cleaning of the solid-phase extraction agent, passing of the liquid sample, washing of the solid-phase extraction agent after passing the liquid sample, The pretreatment liquid (measurement solution) is obtained through the procedure of passing the eluent and measured by the analyzer. Conventionally, these operations have been performed manually, which has been troublesome.

  The present invention is intended to solve this problem, and provides an autosampler, an atomic absorption photometer, and a pretreatment method capable of pretreating a liquid sample by a simple method without taking time and effort. To do.

  Patent Document 1 discloses a chip in which a plastic sintered product is used as a plug at a position in the middle or upper part of the inside of the chip and a carboxyl group or an amino group is introduced into the pore surface.

  In order to solve the above problems, an autosampler of the present invention is an autosampler that introduces a metal into an atomization part of an atomic absorption photometer, and a solid phase extractant that adsorbs a metal contained in a liquid sample is used as a tip part. It is characterized by having prepared for.

  Here, the liquid sample is a liquid in which the interfering substance before the pretreatment and the target metal are mixed. In addition, the conventional autosampler only introduces the measurement solution containing the target metal after completion of the pretreatment into the atomization section, whereas in the present invention, this pretreatment itself is performed by the autosampler. It can be carried out. This is because with the above configuration, a liquid sample can be sucked from the autosampler and the target metal can be adsorbed to the solid phase extractant. The target metal adsorbed on the solid phase extraction agent can be eluted with an eluent. Therefore, the pretreatment of the liquid sample, which has been conventionally performed in the manual, can be performed using the autosampler of the atomic absorption photometer.

  In Patent Document 1, the plug has the purpose of preventing DNA, peptides, proteins, etc. from reaching above the plug, whereas the solid-phase extraction agent of the present invention actively samples the sample. The target metal is adsorbed to the solid phase extractant. This point is significantly different from Patent Document 1. That is, the purpose of the plug described in Patent Document 1 and the solid-phase extraction agent of the present application are different.

  Also, an autosampler that introduces metal into the atomization part of an atomic absorption photometer, a chip that sucks and discharges a liquid sample, and a solid-phase extraction agent that adsorbs the target metal in the liquid sample to the tip of the chip The same effect can be obtained by an autosampler having

  Also, a chip that sucks and discharges a liquid sample, and an autosampler equipped with a solid phase extractant that adsorbs the target metal in the liquid sample at the tip of the chip, and a liquid sample is sucked from the chip and then discharged and discharged. The same applies to an atomic absorptiometer equipped with a control unit that controls the autosampler so that the target metal is eluted from the solid phase extractant with the eluent after the solid phase extractant is washed with the cleaning solution. There is an effect.

  Furthermore, a tip equipped with a solid phase extractant is attached to the autosampler provided in the atomic absorption photometer, and at least the liquid sample is sucked from this tip to the solid phase extractant and then discharged. The same effect can be obtained by a pretreatment method of an atomic absorption photometer in which the elution solution is sucked from the chip to at least the solid phase extraction agent and then discharged after the solution is passed.

  As described above, the autosampler of the present invention is provided with the solid-phase extraction agent that adsorbs the target metal in the liquid sample at the tip. Therefore, it is possible to provide an autosampler, an atomic absorption photometer, and a pretreatment method that can perform pretreatment of the atomic absorption photometer by a simple method without taking time and effort. Again, the merit of the present invention is that the atomic absorption photometer is used by devising the structure of the autosampler of the atomic absorption photometer as a pretreatment that has been performed manually separately from the atomic absorption photometer. In other words, the preprocessing is performed by automation, and this is the greatest effect. Furthermore, since it is automated, the risk of contamination of the pretreatment solution can be greatly reduced compared to manual work, and a reliable analytical value can be obtained.

(Configuration of atomic absorption photometer)
FIG. 2 is a schematic configuration diagram showing an atomic absorption photometer (photometer) having the electric heating furnace of the present embodiment. As shown in FIG. 1, this photometer includes a light source 2, an atomization unit (electric heating furnace) 3, a spectroscope 4, a detector 5, a control computer (control unit) 6, and an autosampler 1.

  The light emitted from the light source 2 causes a resonance absorption phenomenon between the atomization unit 3 and the atomic vapor of the target metal. Quantitative analysis can be performed using an event in which light from the light source 2 is quantitatively absorbed by the amount of the target metal. The light that has passed through the atomization unit 3 from the light source 2 is split by the spectroscope 4 to extract light having a necessary wavelength, and is detected by the photodetector 5 and converted into an electrical signal. The control computer 6 controls each member.

  The autosampler 1 introduces a measurement solution into the atomization unit 3. The present embodiment is characterized in that the autosampler 1 also performs pretreatment of the liquid sample before introducing the measurement solution into the atomization unit 3. Conventionally, there has been no idea of performing pretreatment of a liquid sample using an autosampler of an atomic absorption photometer, and pretreatment could not be performed with a conventional autosampler. Hereinafter, the reason why the liquid sample can be pretreated by the autosampler of the present embodiment will be described.

[Configuration of autosampler]
The autosampler 1 of the present embodiment includes a tip 11 as shown in FIG. 1 at the tip, and a solid-phase extraction agent 10 is disposed at the tip of the tip 11. For convenience of explanation, the upper part of the chip 11 of the autosampler 1 is omitted in FIG. As shown in the figure, the solid phase extractant 10 is preferably fixed by filters (fixing members) 12 and 13 so as not to flow out of the chip 11 or to float up.

  The solid phase extraction agent 10 preferably has a polyaminopolycarboxylic acid type chelate functional group. This is because adsorption of alkali metals and alkaline earth metals can be prevented if they have such a chelate functional group. However, this is merely an example, and the material of the solid-phase extraction agent can be variously changed according to the use, that is, depending on the metal to be adsorbed and the metal to be prevented from adsorbing. Those having a chelate functional group of this polyaminopolycarboxylic acid type are as shown in FIG.

[Operation explanation of autosampler]
Next, the procedure of preprocessing (preprocessing method) using the chip 11 of the autosampler 1 shown in FIG. 1 will be described with reference to FIGS. By using the chip 11 configured as in the present embodiment, the following series of pre-processing can be easily realized without taking time and effort.

[Chip attachment process]
First, a new chip (new chip) 11 filled with the solid phase extractant 10 as described above is attached to the autosampler 1 (S1).

[Conditioning process]
Thereafter, an organic solvent (acetone, acetonitrile, etc.) is passed through the chip 11 to swell the solid phase extractant 10 (S2). Next, for example, 3 mol / L of nitric acid is passed through the chip 11 to remove the contamination of the solid phase extractant 10 and clean the solid phase extractant 10 (S3). Further, ultrapure water is passed through to wash away 3 mol / L of nitric acid passed through (rinsing step; S4). Thereafter, for example, a 0.1 mol / L ammonium acetate solution is passed through to adjust the pH of the solid-phase extraction agent 10 to, for example, about 5.6 (S5). Here, the reason for adjusting the pH is to adsorb the target metal to the solid-phase extraction agent 10.

[Liquid sample sampling process]
Next, using the conditioned chip 11, as shown in FIG. 5, the liquid sample (here, seawater sample as an example) 21 that has entered the autosampler cup 20 is sucked and discharged. Thereby, the metal is adsorbed on the solid-phase extraction agent 10. For example, the liquid sample 21 adjusted to the pH with the highest adsorption efficiency for the target metal is sucked and then discharged (S6, 7). Here, the pH is adjusted in order to adsorb the target metal to the solid-phase extraction agent 10. The adsorption efficiency of the target metal on the solid phase extractant 10 is higher when the pH of the solid phase extractant 10 and the pH of the liquid sample 21 are closer to each other. However, the pH may be in a range that can be adsorbed, and the pH value is merely an example.

  When the target metal is adsorbed on the solid phase extractant 10, alkali metals such as sodium (Na) and potassium (K), which are interfering substances in the atomic absorption measurement, are not adsorbed on the solid phase extractant 10. And is contained in the waste liquid. Here, the reason why these alkali metals are not adsorbed by the solid phase extractant 10 is because the solid phase extractant 10 has a polyaminopolycarboxylic acid type chelate functional group. In order to change the interfering substance, the material of the solid-phase extraction agent 10 may be changed. As described above, since the liquid sample 21 passes through the solid-phase extraction agent 10 a total of two times at the time of inhalation and at the time of exhalation, the adsorption efficiency can be increased as compared with the case of one time.

[Washing process of filling resin (solid phase extractant)]
Next, as shown in FIG. 6, the tip of the chip 11 is immersed in a cleaning port 30 containing a cleaning liquid (ultra pure water) 31. Thereafter, a cleaning liquid (same cleaning liquid as the cleaning liquid 31 entering the cleaning port) is flowed into the chip 11 from the side opposite to the tip (from above). Thereby, the solid phase extractant 10 on which the target metal is adsorbed is washed with ultrapure water (cleaning liquid), and the liquid sample 21 remaining in the solid phase extractant 10 is removed (S8).

[Elution process of packed resin (solid phase extractant) adsorbing element (metal)]
After the washing process of the fixed extractant 10, as shown in FIG. 7, the chip 11 is soaked in the autosampler cup 22 containing the eluent 41, and the eluent 41 is sucked above the solid extractant 10 (S9). ). Thereby, the target metal adsorbed on the solid phase extraction agent 10 is eluted. Also in this step, since the eluent 41 passes through the solid-phase extraction agent 10 a total of two times of suction and discharge, the elution efficiency can be increased as compared with the case of one time. In this step, the target metal can be concentrated by making the volume of the eluent smaller than the volume of the liquid sample.

[Introduction process to the analysis department]
Finally, as shown in FIG. 8, the target metal (measurement solution) 24 eluted by the eluent 41 is discharged into the GA cuvette 23 of the atomization unit 3 (S10). Thereafter, a normal measurement process is performed using a photometer.

[Chip removal process]
Thereafter, the chip 11 is removed (S11), and the process returns to S1. In this way, the chip 11 can be replaced.

[Function and effect]
As described above, according to the autosampler 1 of the present embodiment, the atomic absorption spectrophotometer can be obtained simply by providing the solid-phase extraction agent 10 at the tip of the chip 11 and adding the operation control of the autosampler 1 corresponding thereto. In other words, preprocessing can be performed using automation. Therefore, it is possible to save much labor compared with the pretreatment of the conventional atomic absorption photometer. Furthermore, since it is automated, the risk of contamination of the pretreatment solution can be greatly reduced compared to manual work, and a reliable analytical value can be obtained.

  If automation (mechanization) is performed, no human is involved in the process, so that contamination of the solution can be prevented. Humans contribute to pollution sources for elemental analysis. Examples include semiconductor factories and food manufacturing factories.

  The autosampler of the present invention can be used for an atomic absorption photometer.

It is a block diagram which shows the outline of the chip | tip of the autosampler of this invention. It is a block diagram which shows the outline of the atomic absorption photometer of this invention. It is a figure which shows the chelate functional group of a polyamino polycarboxylic acid type. It is a flowchart which shows the flow of the pre-processing of this invention. It is a schematic block diagram which shows 1 process of the pre-processing of this invention. It is a schematic block diagram which shows 1 process of the pre-processing of this invention. It is a schematic block diagram which shows 1 process of the pre-processing of this invention. It is a schematic block diagram which shows 1 process of the pre-processing of this invention.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Autosampler 2 Light source 3 Atomization part 4 Spectrometer 5 Detector 6 Control computer (control part)
10 Solid phase extractant 11 Chip 12 Filter (fixing member)
13 Filter (fixing member)
21 Liquid sample 31 Cleaning liquid 41 Eluent

Claims (10)

An autosampler that introduces metal into the atomization part of an atomic absorption photometer,
An autosampler comprising a solid-phase extraction agent that adsorbs a metal in a liquid sample at the tip. An autosampler that introduces metal into the atomization part of an atomic absorption photometer,
A chip for sucking and discharging liquid samples;
An autosampler comprising: a solid phase extractant that adsorbs a metal in a liquid sample to a tip portion of a chip.   The autosampler according to claim 1, wherein the solid-phase extraction agent has a polyaminopolycarboxylic acid type chelate functional group.   The autosampler according to claim 1, further comprising a fixing member that sandwiches the solid phase extractant from both sides and fixes the solid phase extractant to the autosampler.   An atomic absorption photometer comprising the autosampler according to claim 1, a light source, an atomization unit, a spectroscope, and a detector. A chip that sucks and discharges a liquid sample, and an autosampler equipped with a solid-phase extraction agent that adsorbs metal in the liquid sample to the tip of the chip;
Control that controls the autosampler to adsorb the metal in the liquid sample to the solid-phase extractant, wash the solid-phase extractant with the washing solution after adsorption, and elute the metal from the solid-phase extractant with the eluent after washing And an atomic absorption photometer.   The atomic absorption photometer according to claim 6, wherein the control unit controls the volume of the eluent to be sucked to be smaller than the volume of the liquid sample to be sucked.   An autosampler comprising a solid phase extraction agent at a tip portion for introducing a liquid sample and an eluent. A pretreatment method for obtaining a metal to be introduced into an atomic absorption photometer,
Attach a tip with a solid phase extractant to the autosampler provided in the atomic absorption photometer,
Inhale the liquid sample from this chip at least to the solid phase extractant,
After discharging, the cleaning solution is passed through the chip,
A pretreatment method comprising sucking and discharging the eluent from the chip to at least the solid phase extraction agent after passing through.   The pretreatment method according to claim 9, wherein the volume of the eluent to be sucked is made smaller than the volume of the liquid sample to be sucked.

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