CN108842159B - Preparation method and application of cadmium sulfide nanowire and carbon nanotube composite flexible electrode with high hydrogen production activity - Google Patents

Abstract

The invention discloses a preparation method of a cadmium sulfide nanowire and carbon nanotube composite flexible electrode with high hydrogen production activity, which comprises the following steps: a, dissolving cadmium salt in an organic solvent at room temperature, adding CNT with the mole percentage of 0-5%, uniformly mixing, adding a certain amount of amino acid, uniformly stirring, transferring into a microwave reaction kettle, and reacting for 0.5-2 hours at the temperature of 150-; after cooling to room temperature, washing with water and ethanol, centrifuging, and drying to obtain a sample A; b: preparing a sample A into an aqueous solution, dripping a proper amount of aqueous solution on a clean flexible substrate, performing suction filtration through a vacuum pump, and loading a catalyst on the surface of the flexible substrate; after drying, the mixture is placed into a muffle furnace for roasting at the temperature of 150-350 ℃, so that the interaction between the catalyst and the substrate is enhanced.

Description

Preparation method and application of cadmium sulfide nanowire and carbon nanotube composite flexible electrode with high hydrogen production activity

Technical Field

The invention relates to a preparation method of a cadmium sulfide nanowire and carbon nanotube composite flexible electrode with high hydrogen production activity and application of the electrode.

Background

Environmental and energy issues are one of the major challenges currently facing the world. Hydrogen is widely considered as a clean energy carrier in the future in many applications, such as environmental vehicles, home heating, and power plants. The photocatalytic hydrolysis hydrogen production is a most promising way for realizing hydrogen economic benefits because the photocatalytic hydrolysis hydrogen production utilizes inexhaustible solar energy in nature as an energy source. The photocatalysis technology has the advantages of mild reaction conditions, low energy consumption, less secondary pollution and the like, and has very important application prospects in the aspects of environment and energy. However, in the process of producing hydrogen by photocatalysis of a common photocatalyst, photo-generated electron-hole pairs are easy to recombine in the process of transferring the photo-generated electron-hole pairs to the surface in the catalyst, and reverse reaction of producing hydrogen by photocatalysis is easy to occur, so that the total efficiency of converting light energy into hydrogen energy is low. Most of the commonly used catalysts in the prior art are powder systems, and have the defects of difficult recovery and fixation and difficult practical application.

Disclosure of Invention

The invention aims to solve the technical problems that photocatalytic hydrogen production electron holes are easy to compound and the hydrogen production efficiency is low in the prior art, and provides a preparation method of a cadmium sulfide nanowire and carbon nanotube composite flexible electrode with high hydrogen production activity.

The technical problem to be solved can be implemented by the following technical scheme.

A preparation method of a cadmium sulfide nanowire and carbon nanotube composite flexible electrode with high hydrogen production activity comprises the following steps:

a, dissolving cadmium salt in an organic solvent at room temperature to prepare a solution (preferably 0.025M) with the concentration of 0.01-0.1M, adding CNT with the molar percentage of 0-5%, uniformly mixing, adding a certain amount of amino acid with the molar ratio of 1: 1-3: 1 to the added cadmium salt, uniformly stirring, transferring the mixture into a microwave reaction kettle for 0.5-2 hours at the reaction temperature of 150-300 ℃; after cooling to room temperature, washing with water and ethanol, centrifuging, and drying to obtain a sample A;

b, preparing a sample A into L aqueous solution with the concentration of 1-5 mg/m (preferably 2mg/m L), dripping a proper amount of aqueous solution on a clean flexible substrate, performing suction filtration through a vacuum pump, and loading the synthesized cadmium sulfide nanowire and carbon nanotube composite material on the surface of the flexible substrate;

wherein the organic solvent is ethylenediamine or triethanolamine, preferably ethylenediamine;

the amino acid is cysteine.

As a further improvement of the technical scheme, the cadmium salt is selected from one of cadmium sulfate, cadmium nitrate and cadmium acetate, and cadmium nitrate is preferred.

As a further improvement of the present invention, the molar percentage of the CNTs is 1%, 1.5%, 2%, 3%, 4% or 5%, preferably 1.5%.

Further, the flexible substrate is a stainless steel mesh, copper foam, nickel foam, or titanium sheet, preferably a stainless steel mesh.

In addition, in step A, the molar ratio of amino acid to added cadmium salt is 1:1, or 2:1, or 3: 1.

The invention also aims to provide an application of the composite flexible electrode obtained by the preparation method.

The method comprises the following steps:

1) mounting the prepared flexible electrode on the anode of an electrochemical double-cell, wherein the cathode adopts a platinum sheet, and the reference electrode is silver chloride;

2) respectively adding 30-60ml (preferably 50 ml) of sodium sulfate solution and 5-20ml (preferably 20 ml) of methanol at two sides of the double pool;

3) introducing nitrogen into the double tanks to drive off air, and then sealing;

4) irradiating anode with xenon lamp source with wavelength of 420nm or more for 1H, measuring gas in 0.2-0.8m L (preferably 0.5 ml) with gas sampler via sealed silicon rubber plug, and detecting H with gas chromatograph₂The amount of (c).

The cadmium sulfide nanowire and CNT flexible electrode provided by the invention is used for synthesizing a composite material of the cadmium sulfide nanowire and the CNT in situ by a microwave method, has good crystallinity and provides more transmission channels for rapid conduction of photo-generated electrons. The catalyst is loaded on a stainless steel substrate, forms a three-dimensional net structure with a stainless steel net, has more electron transmission channels, is manufactured into a flexible electrode for photoelectrocatalysis hydrogen production, has higher photoelectrocatalysis hydrogen production activity, and has the highest hydrogen production amount of the catalyst per unit time and unit mass in the current searched literature. Greatly improves the hydrogen production activity and has great application prospect.

The product prepared by the invention is subjected to structural characterization by adopting the following means of carrying out structural analysis on a sample by adopting X-ray diffraction measured on a Rigaku D2000 model X-ray diffractometer in Japan, and analyzing the morphological structure of the sample by adopting a scanning electron microscope photo obtained by a HITACHI S4800 model scanning electron microscope in Japan and a transmission electron microscope photo obtained by a high-resolution transmission electron microscope in JEM 2010 model Japan JEO L.

Compared with the prior art, the invention has the following advantages and outstanding effects: the chemical reagents used in the invention are all common reagents, and are cheap and easy to obtain.

Drawings

The following detailed description of embodiments of the invention refers to the accompanying drawings.

FIG. 1 is a scanning electron microscope image of the CdS and CNT composite material; from the figure, it can be seen that the cadmium sulfide nanowires synthesized in situ by the microwave method have very uniform morphological characteristics.

FIG. 2 is a transmission electron microscope image of the CdS and CNT composite material; the transmission electron microscope image shows that the synthesized cadmium sulfide nano-wire and the carbon nano-tube are mutually interwoven and closely contacted.

FIG. 3 is an XRD pattern of the resulting highly hydrogen producing active material; the abscissa is angle, and the ordinate is intensity, and the XRD spectrum shows that the cadmium sulfide nanowire and carbon nanotube composite material synthesized in situ by the microwave method has good crystallinity.

Detailed Description

The invention will now be described in greater detail, clearly and completely, with reference to specific examples, which are given by way of illustration only and are not intended to limit the scope of the invention.

In the specific embodiment of the invention, the uniform cadmium sulfide and CNT composite material with the shape of a nanowire structure is obtained by optimizing the reaction temperature, the reaction time, the microwave power, the CNT content, the ethylenediamine content and the cysteine content, and the composite material has good crystallinity, and the photocatalytic hydrogen production test also proves that the composite material has good activity. The reaction temperature, the reaction time and the microwave power mainly influence the growth process of the cadmium sulfide crystal, and the contents of CNT, ethylenediamine and cysteine mainly influence the appearance and hydrogen production activity of the cadmium sulfide. The specific embodiment content is as follows:

example 1

Dissolving 0.3g of cadmium sulfate or cadmium nitrate in 40ml of ethylenediamine or triethanolamine, directly performing ultrasonic treatment and stirring in a microwave reaction kettle, adding 0.5g of glycine or cysteine, and continuously performing ultrasonic treatment and stirring until the cadmium sulfate or the cadmium nitrate is dissolved. Carrying out microwave reaction for 60min at 150 deg.C and 1200W. After the reaction was finished and cooled to room temperature, the reaction mixture was washed with water and ethanol by centrifugation and dried in vacuum.

Example 2

Dissolving 0.3g of cadmium sulfate or cadmium nitrate in 40ml of ethylenediamine or triethanolamine, directly performing ultrasonic treatment and stirring in a microwave reaction kettle, adding 0.5g of glycine or cysteine, and continuously performing ultrasonic treatment and stirring until the cadmium sulfate or the cadmium nitrate is dissolved. Carrying out microwave reaction for 60min at 180 deg.C and 1200W. After the reaction was finished and cooled to room temperature, the reaction mixture was washed with water and ethanol by centrifugation and dried in vacuum.

Example 3

Dissolving 0.3g of cadmium sulfate or cadmium nitrate in 40ml of ethylenediamine or triethanolamine, directly performing ultrasonic treatment and stirring in a microwave reaction kettle, adding 0.5g of glycine or cysteine, and continuously performing ultrasonic treatment and stirring until the cadmium sulfate or the cadmium nitrate is dissolved. Carrying out microwave reaction for 60min at 200 deg.C and 1200W. After the reaction was finished and cooled to room temperature, the reaction mixture was washed with water and ethanol by centrifugation and dried in vacuum.

Example 4

Dissolving 0.3g of cadmium sulfate or cadmium nitrate in 40ml of ethylenediamine or triethanolamine, directly performing ultrasonic treatment and stirring in a microwave reaction kettle, adding 0.5g of glycine or cysteine, and continuously performing ultrasonic treatment and stirring until the cadmium sulfate or the cadmium nitrate is dissolved. Carrying out microwave reaction for 60min at 220 deg.C and 1200W. After the reaction was finished and cooled to room temperature, the reaction mixture was washed with water and ethanol by centrifugation and dried in vacuum.

Example 5

Dissolving 0.3g of cadmium sulfate or cadmium nitrate in 40ml of ethylenediamine or triethanolamine, directly performing ultrasonic treatment and stirring in a microwave reaction kettle, adding 0.5g of glycine or cysteine, and continuously performing ultrasonic treatment and stirring until the cadmium sulfate or the cadmium nitrate is dissolved. Carrying out microwave reaction for 70min at 220 deg.C and 1200W. After the reaction was finished and cooled to room temperature, the reaction mixture was washed with water and ethanol by centrifugation and dried in vacuum.

Example 6

Dissolving 0.3g of cadmium sulfate or cadmium nitrate in 40ml of ethylenediamine or triethanolamine, directly performing ultrasonic treatment and stirring in a microwave reaction kettle, adding 0.5g of glycine or cysteine, and continuously performing ultrasonic treatment and stirring until the cadmium sulfate or the cadmium nitrate is dissolved. Carrying out microwave reaction for 80min at 220 deg.C and 1200W. After the reaction was finished and cooled to room temperature, the reaction mixture was washed with water and ethanol by centrifugation and dried in vacuum.

Example 7

Dissolving 0.3g of cadmium sulfate or cadmium nitrate in 40ml of ethylenediamine or triethanolamine, directly performing ultrasonic treatment and stirring in a microwave reaction kettle, adding 0.5g of glycine or cysteine, and continuously performing ultrasonic treatment and stirring until the cadmium sulfate or the cadmium nitrate is dissolved. Carrying out microwave reaction for 90min at 220 deg.C and 1200W. After the reaction was finished and cooled to room temperature, the reaction mixture was washed with water and ethanol by centrifugation and dried in vacuum.

Example 8

Dissolving 0.013g CNT and 0.3g cadmium sulfate or cadmium nitrate in 40ml ethylene diamine or triethanolamine, directly performing ultrasonic treatment and stirring in a microwave reaction kettle, adding 0.5g glycine or cysteine, and continuing ultrasonic treatment and stirring until the solution is dissolved. Carrying out microwave reaction for 60min at 150 deg.C and 1200W. After the reaction was finished and cooled to room temperature, the reaction mixture was washed with water and ethanol by centrifugation and dried in vacuum.

Example 9

Dissolving 0.026g CNT and 0.3g cadmium sulfate or cadmium nitrate in 40ml ethylene diamine or triethanolamine, directly performing ultrasonic treatment and stirring in a microwave reaction kettle, adding 0.5g glycine or cysteine, and continuing ultrasonic treatment and stirring until dissolving. Carrying out microwave reaction for 60min at 150 deg.C and 1200W. After the reaction was finished and cooled to room temperature, the reaction mixture was washed with water and ethanol by centrifugation and dried in vacuum.

Example 10

Dissolving 0.039g CNT and 0.3g cadmium sulfate or cadmium nitrate in 40ml ethylene diamine or triethanolamine, directly performing ultrasonic treatment and stirring in a microwave reaction kettle, adding 0.5g glycine or cysteine, and continuing ultrasonic treatment and stirring until the components are dissolved. Carrying out microwave reaction for 60min at 150 deg.C and 1200W. After the reaction was finished and cooled to room temperature, the reaction mixture was washed with water and ethanol by centrifugation and dried in vacuum.

Example 11

Dissolving 0.3g of cadmium sulfate or cadmium nitrate in 50ml of ethylenediamine or triethanolamine, directly performing ultrasonic treatment and stirring in a microwave reaction kettle, adding 0.5g of glycine or cysteine, and continuously performing ultrasonic treatment and stirring until the cadmium sulfate or the cadmium nitrate is dissolved. Carrying out microwave reaction for 60min at 150 deg.C and 1200W. After the reaction was finished and cooled to room temperature, the reaction mixture was washed with water and ethanol by centrifugation and dried in vacuum.

Example 12

Dissolving 0.3g of cadmium sulfate or cadmium nitrate in 60ml of ethylenediamine or triethanolamine, directly performing ultrasonic treatment and stirring in a microwave reaction kettle, adding 0.5g of glycine or cysteine, and continuously performing ultrasonic treatment and stirring until the cadmium sulfate or the cadmium nitrate is dissolved. Carrying out microwave reaction for 60min at 150 deg.C and 1200W. After the reaction was finished and cooled to room temperature, the reaction mixture was washed with water and ethanol by centrifugation and dried in vacuum.

Example 13

Dissolving 0.3g of cadmium sulfate or cadmium nitrate in 70ml of ethylenediamine or triethanolamine, directly performing ultrasonic treatment and stirring in a microwave reaction kettle, adding 0.5g of glycine or cysteine, and continuously performing ultrasonic treatment and stirring until the cadmium sulfate or the cadmium nitrate is dissolved. Carrying out microwave reaction for 60min at 150 deg.C and 1200W. After the reaction was finished and cooled to room temperature, the reaction mixture was washed with water and ethanol by centrifugation and dried in vacuum.

Example 14

Dissolving 0.3g of cadmium sulfate or cadmium nitrate in 80ml of ethylenediamine or triethanolamine, directly performing ultrasonic treatment and stirring in a microwave reaction kettle, adding 0.5g of glycine or cysteine, and continuously performing ultrasonic treatment and stirring until the cadmium sulfate or the cadmium nitrate is dissolved. Carrying out microwave reaction for 60min at 150 deg.C and 1200W. After the reaction was finished and cooled to room temperature, the reaction mixture was washed with water and ethanol by centrifugation and dried in vacuum.

Example 15

Dissolving 0.3g of cadmium sulfate or cadmium nitrate in 40ml of ethylenediamine or triethanolamine, directly performing ultrasonic treatment and stirring in a microwave reaction kettle, adding 0.6g of glycine or cysteine, and continuously performing ultrasonic treatment and stirring until the cadmium sulfate or the cadmium nitrate is dissolved. Carrying out microwave reaction for 60min at 150 deg.C and 1200W. After the reaction was finished and cooled to room temperature, the reaction mixture was washed with water and ethanol by centrifugation and dried in vacuum.

Example 16

Dissolving 0.3g of cadmium sulfate or cadmium nitrate in 40ml of ethylenediamine or triethanolamine, directly performing ultrasonic treatment and stirring in a microwave reaction kettle, adding 0.7g of glycine or cysteine, and continuously performing ultrasonic treatment and stirring until the cadmium sulfate or the cadmium nitrate is dissolved. Carrying out microwave reaction for 60min at 150 deg.C and 1200W. After the reaction was finished and cooled to room temperature, the reaction mixture was washed with water and ethanol by centrifugation and dried in vacuum.

Example 17

Dissolving 0.3g of cadmium sulfate or cadmium nitrate in 40ml of ethylenediamine or triethanolamine, directly performing ultrasonic treatment and stirring in a microwave reaction kettle, adding 0.8g of glycine or cysteine, and continuously performing ultrasonic treatment and stirring until the cadmium sulfate or the cadmium nitrate is dissolved. Carrying out microwave reaction for 60min at 150 deg.C and 1200W. After the reaction was finished and cooled to room temperature, the reaction mixture was washed with water and ethanol by centrifugation and dried in vacuum.

Example 18

Dissolving 0.3g of cadmium sulfate or cadmium nitrate in 40ml of ethylenediamine or triethanolamine, directly performing ultrasonic treatment and stirring in a microwave reaction kettle, adding 0.9g of glycine or cysteine, and continuously performing ultrasonic treatment and stirring until the cadmium sulfate or the cadmium nitrate is dissolved. Carrying out microwave reaction for 60min at 150 deg.C and 1200W. After the reaction was finished and cooled to room temperature, the reaction mixture was washed with water and ethanol by centrifugation and dried in vacuum.

Example 19

Dissolving 0.3g of cadmium sulfate or cadmium nitrate in 40ml of ethylenediamine or triethanolamine, directly performing ultrasonic treatment and stirring in a microwave reaction kettle, adding 1.0g of glycine or cysteine, and continuously performing ultrasonic treatment and stirring until the cadmium sulfate or the cadmium nitrate is dissolved. Carrying out microwave reaction for 60min at 150 deg.C and 1200W. After the reaction was finished and cooled to room temperature, the reaction mixture was washed with water and ethanol by centrifugation and dried in vacuum.

Example 20

Dissolving 0.3g of cadmium sulfate or cadmium nitrate in 40ml of ethylenediamine or triethanolamine, directly performing ultrasonic treatment and stirring in a microwave reaction kettle, adding 0.5g of glycine or cysteine, and continuously performing ultrasonic treatment and stirring until the cadmium sulfate or the cadmium nitrate is dissolved. Carrying out microwave reaction for 60min at 150 deg.C and 1000W. After the reaction was finished and cooled to room temperature, the reaction mixture was washed with water and ethanol by centrifugation and dried in vacuum.

Example 21

Dissolving 0.3g of cadmium sulfate or cadmium nitrate in 40ml of ethylenediamine or triethanolamine, directly performing ultrasonic treatment and stirring in a microwave reaction kettle, adding 0.5g of glycine or cysteine, and continuously performing ultrasonic treatment and stirring until the cadmium sulfate or the cadmium nitrate is dissolved. Carrying out microwave reaction for 60min at 150 deg.C and microwave power of 1400W. After the reaction was finished and cooled to room temperature, the reaction mixture was washed with water and ethanol by centrifugation and dried in vacuum.

Example 22

Dissolving 0.3g of cadmium sulfate or cadmium nitrate in 40ml of ethylenediamine or triethanolamine, directly performing ultrasonic treatment and stirring in a microwave reaction kettle, adding 0.5g of glycine or cysteine, and continuously performing ultrasonic treatment and stirring until the cadmium sulfate or the cadmium nitrate is dissolved. Carrying out microwave reaction for 60min at 150 deg.C and 1600W. After the reaction was finished and cooled to room temperature, the reaction mixture was washed with water and ethanol by centrifugation and dried in vacuum.

Example 23

Dissolving 0.3g of cadmium sulfate or cadmium nitrate in 40ml of ethylenediamine or triethanolamine, directly performing ultrasonic treatment and stirring in a microwave reaction kettle, adding 0.5g of glycine or cysteine, and continuously performing ultrasonic treatment and stirring until the cadmium sulfate or the cadmium nitrate is dissolved. Carrying out microwave reaction for 60min at 150 deg.C and 1800W. After the reaction was finished and cooled to room temperature, the reaction mixture was washed with water and ethanol by centrifugation and dried in vacuum.

The invention discloses a preparation method and application of a cadmium sulfide nanowire/carbon nanotube composite flexible electrode with high hydrogen production activity. The composite material of cadmium sulfide (CdS) nanowires and Carbon Nano Tubes (CNTs) is synthesized in situ by a microwave method, and is loaded on a stainless steel substrate by a suction filtration method, and a three-dimensional net structure is constructed between two materials with one-dimensional structures and a stainless steel net, so that the interaction between the materials is enhanced, more transmission channels are provided for the conduction of photo-generated electrons, the electron conduction efficiency is improved, and the higher photoelectrocatalytic hydrogen production activity is obtained. The flexible electrode of the cadmium sulfide and CNT composite material prepared by the invention has high hydrogen production activity and good flexibility, and has wide application prospects in the aspects of hydrogen production, energy storage, pollutant degradation, batteries and the like.

The obtained flexible electrode is used for producing hydrogen through photoelectrocatalysis, electrons are guided to the cathode by using external bias voltage, the recombination of the electrons and holes is effectively inhibited, and the hydrogen production activity is greatly improved.

Claims (8)

1. A preparation method of a cadmium sulfide nanowire and carbon nanotube composite flexible electrode with high hydrogen production activity is characterized by comprising the following steps:

a, dissolving cadmium salt in an organic solvent at room temperature to prepare a solution with the concentration of 0.01-0.1M, adding CNT with the mole percentage of 0-5%, uniformly mixing, adding a certain amount of amino acid with the mole ratio of 1: 1-3: 1, uniformly stirring, transferring into a microwave reaction kettle for 0.5-2 hours at the reaction temperature of 150-; after cooling to room temperature, washing with water and ethanol, centrifuging, and drying to obtain a sample A;

b, preparing a sample A into L aqueous solution with the concentration of 1-5 mg/m, dripping a proper amount of aqueous solution on a clean flexible substrate, loading the synthesized cadmium sulfide nanowire and carbon nanotube composite material on the surface of the flexible substrate through vacuum filtration, drying, and roasting in a muffle furnace at the temperature of 150-350 ℃;

the organic solvent is one of ethylenediamine and triethanolamine;

the amino acid is cysteine.

2. The method for preparing the cadmium sulfide nanowire and carbon nanotube composite flexible electrode with high hydrogen production activity as recited in claim 1, wherein the cadmium salt is selected from one of cadmium sulfate, cadmium nitrate and cadmium acetate.

3. The method for preparing the cadmium sulfide nanowire and carbon nanotube composite flexible electrode with high hydrogen production activity as claimed in claim 1, wherein the molar percentage of the CNT is 1%, 1.5%, 2%, 3%, 4% or 5%.

4. The method for preparing the cadmium sulfide nanowire and carbon nanotube composite flexible electrode with high hydrogen production activity as claimed in claim 1, wherein the flexible substrate is a stainless steel mesh, copper foam, nickel foam, copper mesh or titanium sheet.

5. The method for preparing the cadmium sulfide nanowire and carbon nanotube composite flexible electrode with high hydrogen production activity as recited in claim 1, wherein in the step A, cadmium salt is dissolved in an organic solvent at room temperature to prepare a solution with a concentration of 0.025M, and in the step B, a sample A is prepared into an aqueous solution with a concentration of 2mg/M L.

6. The preparation method of the cadmium sulfide nanowire and carbon nanotube composite flexible electrode with high hydrogen production activity as claimed in claim 1, wherein in the step A, the molar ratio of the amino acid to the added cadmium salt is 1:1 or 2:1 or 3: 1.

7. The application of the composite flexible electrode prepared by the preparation method of any one of claims 1 to 6 in a photoelectrocatalysis hydrogen production activity experiment comprises the following steps:

1) mounting the prepared flexible electrode on the anode of an electrochemical double-cell, wherein the cathode adopts a platinum sheet, and the reference electrode is silver chloride;

2) respectively adding 30-60ml of sodium sulfate solution and 5-20ml of methanol into two sides of the double pool;

3) introducing nitrogen into the double tanks to drive off air, and then sealing;

4) irradiating anode with xenon lamp source with wavelength of 420nm or more for 1H, measuring gas in 0.2-0.8m L reactor with gas sampler via sealed silicon rubber plug, and detecting H with gas chromatograph₂The amount of (c).

8. Use according to claim 7, characterized in that it comprises the following steps:

1) mounting the prepared flexible electrode on the anode of an electrochemical double-cell, wherein the cathode adopts a platinum sheet, and the reference electrode is silver chloride;

2) respectively adding 50ml of sodium sulfate solution and 20ml of methanol into two sides of the double pool;

3) introducing nitrogen into the double tanks to drive off air, and then sealing;

4) irradiating anode with 420nm xenon lamp for 1H, measuring gas in 0.5m L reactor with gas sampler via sealed silicon rubber plug, and detecting H with gas chromatograph₂The amount of (c).

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