JPH0650958A - Small amount of metal analyzer - Google Patents

Abstract

PURPOSE:To stir a specimen, hydrochloric acid, and hydrogeneration boron sodium efficiently when converting a metal contained in the specimen to hydroxide gas. CONSTITUTION:An outer pipe 1 where both edges are sealed and a carrier gas supply port 1a is provided and an inner pipe 2 where impregnation ports 2b and 2d of a specimen and a reagent are provided at the other edge and which penetrates through the outer pipe 1 are laid out coaxially and at the same time a gas transmission region 2a is formed at one part of the inner pipe 2. A hydrogeneration gas detection means 4 is connected to a delivery port 2e of the inner pipe 2 via a gas/liquid separation means 3. A specimen which is impregnated along with hydrochloric acid and hydrogeneration boron sodium from the specimen impregnation ports 2b-2d generates a hydrogeneration gas efficiently by receiving bubbling due to a carrier gas which intrigued from the gas transmission material 2a in a process for traveling the inner pipe 2. The gas is separated by the gas/liquid separation means 3 and flows to the hydrogeneration gas detection means 4, thus measuring the concentration.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a technique for converting a metal into a hydride gas for analysis.

[0002]

2. Description of the Related Art The analysis of trace amounts of metals such as arsenic, selenium, antimony, bismuth, tellurium, tin, mercury and germanium contained in a sample is carried out by mixing sodium hydride and hydrochloric acid into a hydride gas. It is carried out by converting and separating the hydride dissolved in hydrochloric acid as a gas, and introducing this gas into a high frequency inductively coupled plasma emission spectrometer or atomic absorption spectrometer suitable for detecting hydride gas. ing.

[0003]

When the sample is converted into a hydride gas and analyzed in this way, the sensitivity can be improved, but on the other hand, when the sample and hydrochloric acid or sodium borohydride are not sufficiently mixed, the analysis accuracy is improved. There was a problem of causing a decrease. The present invention has been made in view of such problems, and an object thereof is to provide a novel trace amount capable of reliably mixing a sample with hydrochloric acid and sodium borohydride and analyzing with high sensitivity and accuracy. It is to provide an analyzer.

[0004]

In order to solve such a problem, according to the present invention, an outer tube having both ends sealed and provided with a carrier gas supply port, an exhaust port at one end, and an exhaust port at the other end. An inner tube penetrating the outer tube having a sample inlet is coaxially arranged, and a part of the inner tube is made of a gas permeable material to form a hydride gas generating means, and the outlet is filled with gas. And a hydride gas detection means connected via a liquid separation means.

[0005]

The sample injected with hydrochloric acid or sodium borohydride from the sample injection port is bubbled by the carrier gas invading from the gas permeable material in the process of moving through the inner tube to efficiently generate the hydride gas. This gas is separated by the gas-liquid separation means and then flows into the hydride gas detection means to measure its concentration.

[0006]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The details of the present invention will be described below with reference to the illustrated embodiments. FIG. 1 shows an embodiment of the present invention, in which reference numeral 1 is an outer tube made of a material having gas-tightness, for example, quartz, and having a carrier gas inlet 1a, which penetrates the outer tube. The inner tube 2 is coaxially connected so that the area covered by the outer tube 1 blocks the passage of liquid such as porous fluororesin or porous polyethylene resin and selectively permeates only gas. A gas permeable region 2a made of a material to be formed is formed. Material supply ports 2b, 2c, 2d for injecting hydrochloric acid, sodium borohydride, and metal are provided at one end of the inner tube 2, and a discharge port 2e is provided at the other end. A gas-liquid separation means 3 for selectively separating the hydride gas from the liquid is connected.

The gas-liquid separating means 3 comprises a tube made of a material such as a porous fluororesin or a porous polyethylene resin which blocks the passage of a liquid and selectively permeates only a gas. For example, a material is used in which the outside is surrounded by a non-gas permeable material such as quartz and the gas separated by the tube can be collected.

Reference numeral 4 is a hydrogenated gas detection means connected to the gas outlet of the gas-liquid separation means 3 for detecting hydrogenated gas such as a high frequency inductively coupled plasma emission spectrometer or atomic absorption spectrometer. A suitable one is used. Reference numeral 3a in the figure indicates a liquid discharge port of the gas-liquid separating means 3.

In this embodiment, when the carrier gas is supplied from the carrier gas inlet 1a, the carrier gas flows from the gas permeable region 2a into the inner pipe. When the sample to be analyzed, sodium borohydride, and hydrochloric acid are supplied from the supply ports 2b, 2c, and 2d in this state, these move in the inner tube 2 and undergo bubbling by the carrier gas flowing in from the gas permeation region 2a. Stir efficiently and uniformly.

During this stirring process, NaBH ₄ + 3H ₂ O + Hcl H ₃ BO ₄ + Nacl + 8
By the reaction of H MX MY + H ₂ O (where M represents a metal), hydride gas such as arsenic, selenium, antimony, bismuth, tellurium, tin, mercury and germanium contained in the sample is generated. These hydride gases are dissolved in hydrochloric acid, move to the inner tube 2, flow into the gas-liquid separation means 3, separated from the hydrochloric acid, flow into the hydride gas detection means 4, and their concentrations are measured.

On the other hand, a liquid or solid component such as hydrochloric acid that has released the hydride gas is discharged out of the system through the liquid discharge port 3a.

[0012]

As described above, according to the present invention, the outer tube having both ends sealed and the carrier gas supply port, the discharge port at one end, and the sample injection port at the other end are provided. While arranging the inner tube that penetrates the outer tube coaxially,
Since a part of the inner tube is composed of a gas permeable material, a hydride gas generating means and a hydride gas detecting means connected to an outlet through a gas-liquid separating means, a sample, hydrochloric acid and hydrogenation can be obtained. By bubbling sodium borohydride in the reaction process, a trace amount of metal contained in the sample can be surely converted into a hydride gas and can be analyzed with high sensitivity.

[Brief description of drawings]

FIG. 1 is a sectional view of an apparatus showing an embodiment of the present invention.

[Explanation of symbols]

 1 Outer Tube 2 Inner Tube 2a Gas Permeation Region 2b, 2c, 2d Supply Port 2e Discharge Port 4 Gas-Liquid Separation Means 5 Hydride Gas Detection Means

Claims (1)

[Claims] 1. An outer pipe having both ends sealed and provided with a carrier gas supply port and an inner pipe having a discharge port at one end and a sample injection port at the other end and penetrating the outer pipe are coaxial. And a hydride gas detection means connected to the discharge port through a gas-liquid separation means, the hydride gas generation means having a part of the inner tube made of a gas-permeable material. Trace metal analyzer.