ISO/DIS 20579-1

DRAFT INTERNATIONAL STANDARD
ISO/DIS 20579-1
ISO/TC 201/SC 2 Secretariat: ANSI
Voting begins on: Voting terminates on:
2017-08-01 2017-10-23
Surface chemical analysis — Guidelines to sample
handling, preparation and mounting —
Part 1:
Guidelines to handling of specimens prior to analysis
Titre manque —
Partie 1: Titre manque
ICS: 71.040.40
THIS DOCUMENT IS A DRAFT CIRCULATED
FOR COMMENT AND APPROVAL. IT IS
THEREFORE SUBJECT TO CHANGE AND MAY
NOT BE REFERRED TO AS AN INTERNATIONAL
STANDARD UNTIL PUBLISHED AS SUCH.
IN ADDITION TO THEIR EVALUATION AS
BEING ACCEPTABLE FOR INDUSTRIAL,
This document is circulated as received from the committee secretariat.
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STANDARDS MAY ON OCCASION HAVE TO
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WHICH REFERENCE MAY BE MADE IN
Reference number
NATIONAL REGULATIONS.
ISO/DIS 20579-1:2017(E)
RECIPIENTS OF THIS DRAFT ARE INVITED
TO SUBMIT, WITH THEIR COMMENTS,
NOTIFICATION OF ANY RELEVANT PATENT
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PROVIDE SUPPORTING DOCUMENTATION. ISO 2017
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ISO/DIS 20579-1:2017(E)
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© ISO 2017, Published in Switzerland

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

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

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

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

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

4 Symbols and abbreviated terms ........................................................................................................................................................... 1

5 Explanation of Structure of this Standard .................................................................................................................................. 1

6 General Requirements and Classes of Specimen ................................................................................................................ 2

7 Specimen Influences ......................................................................................................................................................................................... 4

7.1 Specimen Information needed by analyst ....................................................................................................................... 4

7.2 History ............................................................................................................................................................................................................ 4

7.3 Handling of samples with respect to other analytical techniques .............................................................. 4

7.4 Identification of specimens .......................................................................................................................................................... 5

7.5 Precautions ................................................................................................................................................................................................ 5

8 Sources of Specimen Contamination in Handling .............................................................................................................. 5

9 Specimen Storage and Transfer ............................................................................................................................................................ 6

9.1 Storage ........................................................................................................................................................................................................... 6

9.1.1 Time ............................................................................................................................................................................................ 6

9.1.2 Containers.............................................................................................................................................................................. 6

9.1.3 Temperature and Humidity .................................................................................................................................... 7

9.2 Descriptive List of Containers .................................................................................................................................................... 7

10 Information on Specimen History ...................................................................................................................................................... 8

11 Education of Specimen Owner on Appropriate Specimen Handling Procedures .............................8

Bibliography ................................................................................................................................................................................................................................ 9

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This International Standard is intended to assist analysts and those seeking surface chemical analysis

in the handling, storage, mounting and treatment of specimens. This is a multipart document, with the

first two parts being general requirements for sample handling and storage in ISO 20579-1: Part 1,

and mounting and treatment of samples in ISO 20579-2: Part 2. The ensuing parts combine any new

requirements of sample handling/storage and/or sample mounting/preparation for new materials

classes. Part 3 focuses on biomaterials and Part 4 focuses on reporting needs for nano-objects. Each

part of this international standard can be used independently of the other parts although, the general

procedures described in Parts 1 and 2 are applicable to a wide range of materials and are not reproduced

Although primarily prepared for the surface-analysis techniques of Auger electron spectroscopy (AES),

X-ray photoelectron spectroscopy (XPS) and secondary ion mass spectrometry (SIMS), the methods

described in this International Standard will also be applicable to many other surface-sensitive

analytical techniques such as ion-scattering spectrometry, scanning probe microscopy, low-energy

electron diffraction and electron energy-loss spectroscopy, where specimen handling can influence

surface-sensitive measurements. AES, XPS and SIMS are sensitive to surface layers that are typically

a few nanometers in thickness. Such thin layers may be subject to severe perturbations caused by

specimen handling or surface treatments that may be necessary prior to introduction into the analytical

chamber. Proper handling and preparation of specimens is particularly critical for dependable analysis.

Improper handling of specimens can result in alteration of the surface composition and unreliable data.

This part of the standard is intended for the specimen owner or the purchaser of surface analytical

services and for the surface analyst. The optimum handling procedures are dependent on the particular

specimen and the needed information, and this document provides illustrative examples for each

specimen type that a specimen owner and surface analyst will typically encounter. It is recommended

that the specimen supplier consult the surface analyst as soon as possible with regard to specimen

history, the specific problem to be solved or information needed, and any particular specimen

Parts of this ISO Standard are based on ASTM/Standard E 1829, Standard Guide for Handling Samples

This part can be used independently of part 2, which gives guidance to the analyst for specimen

This International Standard gives guidance on the handling of and the containers for specimens

submitted for surface chemical analysis. It is intended for the user of surface analysis services as an aid

in understanding the special sample handling requirements of surface chemical analysis techniques,

particularly: Auger electron spectroscopy (AES), Secondary ion mass spectrometry (SIMS), and X-ray

photoelectron spectroscopy (XPS or ESCA). The protocols presented may also be applicable for other

analytical techniques, such as TXRF, that are sensitive to surface composition. In particular instances,

The following documents, in whole or in part, are normatively referenced in this document and are

indispensable for its application. For dated references, only the edition cited applies. For undated

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

For the purposes of this document, the terms and definitions given in ISO 18115 apply.

Section 6 discusses additional considerations, such as specimen history and previous analyses of

the specimen, that affect the composition of the surface. Documentation of these influences should

accompany the carefully handled and packaged specimen when submitted for analysis. Section

7 provides specific recommendations on specimen handling procedures necessary to minimize

contamination of the specimen surface. Moreover, Section 7 gives a series of alternative specimen

handling procedures based on maintaining increasing degrees of specimen cleanliness during handling

and transfer of the specimen to storage containers. Section 8 describes different specimen containers

that may be used in different conditions. Section 8 also discusses specimen storage with respect to

time, humidity, and temperature. Sections 9 and 10 emphasize that specimen handling has an effect

on the information derived from surface analytical measurements, and that specimen owners as well

as analysts will benefit from improved analyses when prescribed specimen handling protocols are

6.1 The degree of cleanliness required by surface-sensitive analytical techniques is much greater than

6.2 Specimens shall never be in contact with the bare hand. Contact of the surface area to be analysed

with handling tools or other equipment shall be eliminated or minimized whenever possible.

6.3 Specimens shall be transported to the analyst in a container that does not come into direct contact

6.4 In many cases, the analysis will be performed on the “as received” specimen; surface contamination

or atmospheric adsorbates are not then usually removed because they are the item of interest. Care shall

be taken in the handling of these specimens to ensure that nothing, apart from air or clean inert gases,

comes in contact with the surface to be investigated. In particular, avoid contacting the specimen surface

with solvents or cleaning solutions, gases such as compressed air or solvent vapours, metals, tissue or

other wrapping materials, tape, cloth, tools, packing materials, or the walls of containers. In cases where

these precautions are not feasible due to the size of the specimen, some alternative specimen handling

6.5 In some cases, it may be necessary to take a representative sample from the specimen. Selection of

a smaller sample from a larger specimen should be done after considering the information being sought

because inhomogeneities are often present. It is recommended that this choice be made in consultation

with an experienced analyst. Specific care should be taken to avoid contaminating the surface of interest

6.6 Special caution shall be exercised with specimens containing potential toxins or other hazardous

materials. Whenever possible, chemical hazard data sheets should be supplied with the specimen.

6.7 The severity of the requirement for careful handling varies dramatically with the condition of the

surface, the depth from the surface of the information being sought, and the detection level required

for the material being analyzed. The following list arranges specimens by their decreasing sensitivity to

b) Specimens with hydrocarbons, molecular films, or biomaterials on the surface that are the object of

d) Specimens that have been exposed to the atmosphere and that are to be analyzed “as received.”

f) Specimens with a contamination layer (or other topmost layer) that is of no interest and that will

be removed just prior to insertion in the analytical chamber (e.g., treatment by solutions, abrasion,

g) Specimens with a contamination layer (or other topmost layer) that is of no interest and that will be

h) Thin films that will be delaminated by the analyst prior to insertion into the analysis chamber.

i) Specimens that will be fractured or freshly prepared outside the analysis chamber, including

j) Uniform thin films that are to be removed by ion etching or scraping in the analysis chamber to

6.81 Surface chemical analysis can be performed on a wide range of specimens and can be used to

obtain very different types of information about surfaces or interfaces. The degree of care that shall be

taken depends upon the type of analysis that is required and the nature of the problem. The information

being sought usually falls into three general categories: (A) information requiring integrity of the