Fine ceramics (advanced ceramics, advanced technical ceramics) — Test method for determination of phenol oxidative decomposition performance of semiconducting photocatalytic materials by quantitative analysis of total organic carbon (TOC)

This document provides a testing method for testing phenol oxidative decomposition performance of semiconducting photocatalytic materials or made of a material adsorbed with photocatalyst to its surface for the purpose of purifying water polluting substances in water making use of photocatalytic performance as test piece. The test piece can be planar, spherical, flake or block shape. A test piece that can elute hydrocarbon or the like by immersion into water or phenol aqueous solution or by light irradiation, a semiconducting photocatalytic material that cannot maintain its shape or a powdery semiconducting photocatalytic material are excluded from the scope of application, since they cannot be evaluated.

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Status
Published
Publication Date
05-Sep-2019
Technical Committee
Current Stage
6060 - International Standard published
Start Date
06-Sep-2019
Completion Date
06-Sep-2019
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ISO 22601:2019 - Fine ceramics (advanced ceramics, advanced technical ceramics) -- Test method for determination of phenol oxidative decomposition performance of semiconducting photocatalytic materials by quantitative analysis of total organic carbon (TOC)
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INTERNATIONAL ISO
STANDARD 22601
First edition
2019-09
Fine ceramics (advanced ceramics,
advanced technical ceramics) — Test
method for determination of phenol
oxidative decomposition performance
of semiconducting photocatalytic
materials by quantitative analysis of
total organic carbon (TOC)
Reference number
ISO 22601:2019(E)
ISO 2019
---------------------- Page: 1 ----------------------
ISO 22601:2019(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2019

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

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Published in Switzerland
ii © ISO 2019 – All rights reserved
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ISO 22601:2019(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

Introduction ..................................................................................................................................................................................................................................v

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ...................................................................................................................................................................................... 1

3 Terms and definitions ..................................................................................................................................................................................... 1

4 Symbols .......................................................................................................................................................................................................................... 2

5 Principle ........................................................................................................................................................................................................................ 2

6 Materials ....................................................................................................................................................................................................................... 3

6.1 Chemicals and implements .......................................................................................................................................................... 3

6.1.1 Reagent ...................................................................... ............................................................................................................... 3

6.1.2 Purified water ..................................................................................................................................................................... 3

6.1.3 Purified air ............................................................................................................................................................................ 3

6.1.4 Purified water saturated with dissolved oxygen .................................................................................. 3

7 Test device and instrument ....................................................................................................................................................................... 3

7.1 Test vessel ................................................................................................................................................................................................... 3

7.2 Reserve container ................................................................................................................................................................................. 3

7.3 UV irradiation light source ........................................................................................................................................................... 4

7.4 UV radiometer ......................................................................................................................................................................................... 4

7.5 UV light intensity ................................................................................................................................................................................... 4

7.6 pH meter ....................................................................................................................................................................................................... 4

7.7 TOC measuring device ...................................................................................................................................................................... 4

8 Arrangement of test method .................................................................................................................................................................... 4

8.1 Measuring device setup ................................................................................................................................................................... 4

8.2 Test solution feeding device ........................................................................................................................................................ 4

8.3 Instruments for air flow .................................................................................................................................................................. 5

9 Test material ............................................................................................................................................................................................................. 5

9.1 Test piece ..................................................................................................................................................................................................... 5

9.2 Pre-treatment of the test piece ................................................................................................................................................. 5

10 Procedure of the measurement ............................................................................................................................................................ 6

10.1 Test temperature ................................................................................................................................................................................... 6

10.2 Other test condition ............................................................................................................................................................................ 6

10.3 Preparation for test ............................................................................................................................................................................. 6

10.4 Procedure of the measurement ................................................................................................................................................ 6

11 Evaluation of results ......................................................................................................................................................................................... 7

11.1 Evaluation of dark condition ....................................................................................................................................................... 7

11.2 Evaluation of illuminated condition ..................................................................................................................................... 7

11.3 Phenol oxidative decomposition performance ........................................................................................................... 7

11.4 Condition for establishing a successful test ................................................................................................................... 7

12 Test report ................................................................................................................................................................................................................... 8

Annex A (informative) Example of suitable test vessel ..................................................................................................................... 9

Annex B (informative) Example of suitable test vessel ..................................................................................................................10

Annex C (informative) Example of test position of test vessel and suitable measuring device

component ...............................................................................................................................................................................................................11

Annex D (informative) Example of data evaluation ...........................................................................................................................13

Annex E (informative) Results of the interlaboratory test .........................................................................................................15

© ISO 2019 – All rights reserved iii
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ISO 22601:2019(E)
Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards

bodies (ISO member bodies). The work of preparing International Standards is normally carried out

through ISO technical committees. Each member body interested in a subject for which a technical

committee has been established has the right to be represented on that committee. International

organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.

ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of

electrotechnical standardization.

The procedures used to develop this document and those intended for its further maintenance are

described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the

different types of ISO documents should be noted. This document was drafted in accordance with the

editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/directives).

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of

any patent rights identified during the development of the document will be in the Introduction and/or

on the ISO list of patent declarations received (see www .iso .org/patents).

Any trade name used in this document is information given for the convenience of users and does not

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expressions related to conformity assessment, as well as information about ISO's adherence to the

World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see www .iso

.org/iso/foreword .html.
This document was prepared by Technical Committee ISO/TC 206, Fine ceramics.

Any feedback or questions on this document should be directed to the user’s national standards body. A

complete listing of these bodies can be found at www .iso .org/members .html.
iv © ISO 2019 – All rights reserved
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ISO 22601:2019(E)
Introduction

Since photocatalysts have a wide range of functions such as purification of air or water, antibacterial

effect and self-cleaning, many application products that make use of said functions are developed.

Photocatalyst-applied products for water purification are expected to exert oxidative decomposing

performance against organic compounds composed of hydrocarbon, which is a water polluting

substance. In line with this, there is a necessity for developing a testing method for measuring the

oxidative decomposition against water polluting substances. This document stipulates a test method

for measuring the performance of a semiconducting photocatalytic material irradiated with UV

light in water for the oxidative decomposition of hydrocarbon such as phenol and the byproducts as

intermediate produced by the photocatalysis, by the TOC method.

An examples of data evaluation is given in Annex D while the results of the interlaboratory tests are

given in Annex E.
© ISO 2019 – All rights reserved v
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INTERNATIONAL STANDARD ISO 22601:2019(E)
Fine ceramics (advanced ceramics, advanced technical
ceramics) — Test method for determination of phenol
oxidative decomposition performance of semiconducting
photocatalytic materials by quantitative analysis of total
organic carbon (TOC)
1 Scope

This document provides a testing method for testing phenol oxidative decomposition performance

of semiconducting photocatalytic materials or made of a material adsorbed with photocatalyst to its

surface for the purpose of purifying water polluting substances in water making use of photocatalytic

performance as test piece. The test piece can be planar, spherical, flake or block shape. A test piece

that can elute hydrocarbon or the like by immersion into water or phenol aqueous solution or by light

irradiation, a semiconducting photocatalytic material that cannot maintain its shape or a powdery

semiconducting photocatalytic material are excluded from the scope of application, since they cannot

be evaluated.
2 Normative references

The following documents are referred to in the text in such a way that some or all of their content

constitutes requirements of this document. For dated references, only the edition cited applies. For

undated references, the latest edition of the referenced document (including any amendments) applies.

ISO 8425, Water quality—Guidelines for the determination of total organic carbon (TOC) and dissolved

organic carbon (DOC)
ISO 10523, Water quality — Determination of pH

ISO 10677, Fine ceramics (advanced ceramics, advanced technical ceramics) — Ultraviolet light source for

testing semiconducting photocatalytic materials

ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories

ISO 19722, Fine ceramics (advances ceramics, advanced technical ceramics) — Test method for

determination of photocatalytic activity on semiconducting photocatalytic materials by dissolved oxygen

consumption

ISO 20507, Fine ceramics (advanced ceramics, advanced technical ceramics) — Vocabulary

ISO 22197-1, Fine ceramics (advanced ceramics, advanced technical ceramics) — Test method for air-

purification performance of semiconducting photocatalytic materials — Part 1: Removal of nitric oxide

ISO 80000-1, Quantities and units — Part 1: General principles
3 Terms and definitions

For the purposes of this document, the terms and definitions given in ISO 19722 and ISO 20507 and the

following apply.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https: //www .iso .org/obp
© ISO 2019 – All rights reserved 1
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ISO 22601:2019(E)
— IEC Electropedia: available at http: //www .electropedia .org/
3.1
test piece

planar, spherical, flake or block shaped semiconducting photocatalyst materials for water purification

prescribed in ISO 20507 using semiconducting photocatalyst
3.2
illuminated condition
test condition under which a test is conducted with light source lit
3.3
dark condition

measuring condition under which no light source is lit and no light is incoming from outside

Note 1 to entry: The purpose of this condition is for comparing the result with that conducted under the

illuminated condition.
4 Symbols
Symbol Designation Unit
C concentration of hydrocarbon mg/l
ΔTOC phenol concentration adsorbed to the test piece in the dark mg/l
C phenol concentration measured from the test solution as the initial mg/l
concentration in the dark condition
C phenol concentration measured from the test solution after 6 hours mg/l
in the dark condition
ΔTOC phenol concentration adsorbed to the test piece and decomposed mg/l
by photocatalysis
C phenol concentration measured from the test solution as the initial mg/l
concentration under the illuminated condition
C concentration of residual phenol and byproduct measured from mg/l
the test solution after 6 hours under an illuminated condition
ΔTOC decomposed phenol concentration as hydrocarbon on the test piece mg/l
by the photocatalysis
V volume of test solution ml
λ wavelength nm
I ultraviolet (UV) light irradiation intensity mW/cm
5 Principle

Organic compound in waste water is oxidatively decomposed to CO and water by the photocatalysis,

so called as photocatalytic mineralization. Under the photocatalytic mineralization, many kinds of

byproducts are usually produced and the production mechanism including the changes of a molecular

structure and the concentration of byproducts are depending on the characteristics of photocatalyst,

such as the surface structure, crystal phase and the photocatalytic activity. Accordingly, estimation

of photocatalytic activity by the decrement of initial concentration of organic compounds means

mainly changing the original structure of the organic compound. Preferable estimation method of the

2 © ISO 2019 – All rights reserved
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ISO 22601:2019(E)

photocatalytic activity for waste water treatment should oxidatively decompose organic compound to

CO and water as photocatalytic mineralization. On the basis of the conception, total organic carbon

analysis as measurement of the photocatalytic mineralization is most suitable method because no the

byproducts production as reaction mechanism should be taken into account.
6 Materials
6.1 Chemicals and implements
6.1.1 Reagent
Reagent is phenol and the assay is > 99 wt%.
6.1.2 Purified water

Water used for the preparation of all solutions shall be distilled or deionised water.

6.1.3 Purified air

Air prepared by removing dusts and volatile organic compounds from atmospheric air using a filter or

the like, or synthetic air filled in a high-pressure container as provided in ISO 22197-1.

6.1.4 Purified water saturated with dissolved oxygen

Purified water prepared in accordance with the preparation procedure provided for in ISO 19722 by

saturating water with dissolved oxygen at ±1 °C of water temperature during the test.

7 Test device and instrument
7.1 Test vessel

Use a silica glass for the window glass plate for this test. The test vessel and O-ring used in this test shall

be near-UV irradiation resistant and chemical resistant against phenol. For example, preferred material

for an O-ring is fluorocarbon polymer, and preferred material for other parts is polytetrafluoroethylene.

The test vessel shall be inclined to avoid fogging the inner side of window glass by test solution because

the fogged window glass induces extinction. Therefore, the test vessel shall be structured to maintain

the test piece immersed under the test solution even when the test vessel is inclined as shown in

Annex A. Moreover, a weir shall be provided so as to avoid the test piece from falling off or swept away

by the circulation of the test solution. The height of the weir shall have a clearance of 5 mm + 0 mm,

−1 mm from the window plate.

The size of window glass shall be larger than the size of the place for folding the test piece

7.2 Reserve container

Provide a reserve container for maintaining the condition of the test solution to be supp

...

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