1、BSI Standards PublicationBS EN 16602-70-05:2014Space product assurance Detection of organiccontamination surfaces byinfrared spectroscopyBS EN 16602-70-05:2014 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN16602-70-05:2014.The UK participation in its preparatio
2、n was entrusted to TechnicalCommittee ACE/68, Space systems and operations.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapp
3、lication. The British Standards Institution 2014. Published by BSI StandardsLimited 2014ISBN 978 0 580 84419 5ICS 49.140Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Committe
4、e on 31 October 2014.Amendments issued since publicationDate Text affectedBS EN 16602-70-05:2014EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16602-70-05 October 2014 ICS 49.140 English version Space product assurance - Detection of organic contamination surfaces by infrared spectroscopy Assu
5、rance produit des projets spatiaux - Dtection des surfaces de contamination organique par spectroscopie infrarouge Raumfahrtproduktsicherung - Detektion von organischen Kontaminationen auf Oberflchen mit InfrarotspektroskopieThis European Standard was approved by CEN on 20 March 2014. CEN and CENELE
6、C members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on app
7、lication to the CEN-CENELEC Management Centre or to any CEN and CENELEC member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN and CENELEC member into its own language and notif
8、ied to the CEN-CENELEC Management Centre has the same status as the official versions. CEN and CENELEC members are the national standards bodies and national electrotechnical committees of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republi
9、c of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels
10、 2014 CEN/CENELEC All rights of exploitation in any form and by any means reserved worldwide for CEN national Members and for CENELEC Members. Ref. No. EN 16602-70-05:2014 EBS EN 16602-70-05:2014EN 16602-70-05:2014 (E) 2 Table of contents Foreword 5 1 Scope . 7 2 Normative references . 8 3 Terms, de
11、finitions and abbreviated terms 9 3.1 Terms defined in other standards . 9 3.2 Terms specific to the present standard . 9 3.3 Abbreviated terms. 11 4 Principles 13 5 Requirements 14 5.1 Preparatory activities 14 5.1.1 Hazard, health and safety precautions 14 5.1.2 Facilities 14 5.1.3 Materials . 15
12、5.1.4 Handling 15 5.1.5 Equipment . 15 5.1.6 Miscellaneous items 16 5.2 Procedure for sampling and analysis 17 5.2.1 Summary 17 5.2.2 Direct method 17 5.2.3 Indirect method . 17 5.3 Reporting of calibration and test data 21 5.4 Quality assurance . 21 5.4.1 Data 21 5.4.2 Nonconformance . 21 5.4.3 Cal
13、ibration . 21 5.4.4 Traceability . 25 5.4.5 Training . 25 5.5 Audit of measurement equipment . 26 5.5.1 General . 26 BS EN 16602-70-05:2014EN 16602-70-05:2014 (E) 3 5.5.2 Audit of the system (acceptance) 26 5.5.3 Annual regular review (maintenance) of the system 27 5.5.4 Special review . 27 Annex A
14、(normative) Calibration and test results DRD . 28 Annex B (informative) Selection criteria for equipment and accessories for performing the infrared analysis of organic contamination 30 Annex C (informative) Calibration of infrared equipment 35 Annex D (informative) Interpretation of infrared spectr
15、a . 40 Annex E (informative) The use of molecular witness plates for contamination control . 44 Annex F (informative) Collecting molecular contamination from surfaces by wiping and rinsing . 49 Annex G (informative) Contact test . 54 Annex H (informative) Immersion test . 56 Figures Figure 5-1: Samp
16、ling and analysis procedure flow chart . 20 Figure C-1 : Example for a calibration curve . 38 Figure C-2 : Measurement of peak heights . 39 Figure D-1 : Characteristic spectrum of bis (2-ethylhexyl) phthalate . 41 Figure D-2 : Characteristic spectrum of a long chain aliphatic hydrocarbon 41 Figure D
17、-3 : Characteristic spectrum of poly (dimethylsiloxane) . 41 Figure D-4 : Characteristic spectrum of poly (methylphenylsiloxane) 41 Figure E-1 : Witness plate holder and witness plate used for organic contamination control 44 Figure E-2 : Example of a witness plate information sheet . 48 Figure F-1
18、: Example of a sample information form 53 Tables Table 5-1: Standard materials used for the IR analysis. 22 Table B-1 : Important properties of common window materials used for infrared spectroscopy 33 Table B-2 : Examples of compound references and suppliers 34 Table C-1 : Volumes to be applied fro
19、m stock solutions and respective target amounts . 38 Table C-2 : Example results of the direct calibration method 39 BS EN 16602-70-05:2014EN 16602-70-05:2014 (E) 4 Table D-1 : Assignment of infrared absorption bands for the four main groups of contaminants 42 BS EN 16602-70-05:2014EN 16602-70-05:20
20、14 (E) 5 Foreword This document (EN 16602-70-05:2014) has been prepared by Technical Committee CEN/CLC/TC 5 “Space”, the secretariat of which is held by DIN. This standard (EN 16602-70-05:2014) originates from ECSS-Q-ST-70-05C. This European Standard shall be given the status of a national standard,
21、 either by publication of an identical text or by endorsement, at the latest by April 2015, and conflicting national standards shall be withdrawn at the latest by April 2015 Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/
22、or CENELEC shall not be held responsible for identifying any or all such patent rights. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association. This document has been developed to cover specifically space systems and has theref
23、ore precedence over any EN covering the same scope but with a wider domain of applicability (e.g. : aerospace). According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria
24、, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey
25、 and the United Kingdom. BS EN 16602-70-05:2014EN 16602-70-05:2014 (E) 6 Introduction One or more of the following organic substances can contaminate spacecraft materials and hardware, as well as vacuum chambers: Volatile condensable products of materials out-gassing under vacuum. Volatile condensab
26、le products of off-gassing materials. Back-streaming products from pumping systems. Handling residues (e.g. human grease). Residues of cleaning agents. Non-filtered external pollution. Creep of certain substances (e.g. silicones). There are several methods for identifying organic species, such as ma
27、ss spectrometry, gas chromatography and infrared spectroscopy, or a combination of these methods. Infrared spectroscopy, which is the most widely used, is a simple, versatile and rapid technique providing high resolution qualitative and quantitative analyses. The technique is therefore baseline for
28、the present Standard. BS EN 16602-70-05:2014EN 16602-70-05:2014 (E) 7 1 Scope This Standard defines test requirements for detecting organic contamination on surfaces using direct and indirect methods with the aid of infrared spectroscopy. The Standard applies to controlling and detecting organic con
29、tamination on all manned and unmanned spacecraft, launchers, payloads, experiments, terrestrial vacuum test facilities, and cleanrooms. The following test methods are covered: Direct sampling of contaminants Indirect sampling of contaminants by washing and wiping Several informative annexes are incl
30、uded to give guidelines to the following subjects: Qualitative and quantitative interpretation of spectral data Calibration of infrared equipment Training of operators Use of molecular witness plates Collecting molecular contamination Contact test to measure the contamination transfer of materials I
31、mmersion test to measure the extractable contamination potential of materials Selection criteria for test equipment This standard may be tailored for the specific characteristics and constraints of space project in conformance with ECSS-S-ST-00. BS EN 16602-70-05:2014EN 16602-70-05:2014 (E) 8 2 Norm
32、ative references The following normative documents contain provisions which, through reference in this text, constitute provisions of this ECSS Standard. For dated references, subsequent amendments to, or revision of any of these publications do not apply. However, parties to agreements based on thi
33、s ECSS Standard are encouraged to investigate the possibility of applying the more recent editions of the normative documents indicated below. For undated references, the latest edition of the publication referred to applies. EN reference Reference in text Title EN 16601-00-01 ECSS-S-ST-00-01 ECSS s
34、ystem Glossary of terms EN 16602-10 ECSS-Q-ST-10 Space product assurance Product assurance management EN 16602-10-09 ECSS-Q-ST-10-09 Space product assurance Nonconformance control system EN 16602-20 ECSS-Q-ST-20 Space product assurance Quality assurance EN 16602-70-01 ECSS-Q-ST-70-01 Space product a
35、ssurance Cleanliness and contamination control BS EN 16602-70-05:2014EN 16602-70-05:2014 (E) 9 3 Terms, definitions and abbreviated terms 3.1 Terms defined in other standards For the purpose of this Standard, the terms and definitions from ECSS-S-ST-00-01 and ECSS-Q-ST-70-01 apply, in particular for
36、: controlled area 3.2 Terms specific to the present standard 3.2.1 absorbance, A logarithm to the base 10 of the reciprocal of the transmittance ASTM-E-131 NOTE The term absorbance is also widely used for the negative log of the ratio of the final to the incident intensities of processes other than
37、transmission, such as attenuated total reflection and diffuse reflection. 3.2.2 absorption transfer of infrared energy to the molecules present within the pathway of the radiation 3.2.3 absorptivity absorbance divided by the product of the concentration of the substance and the sample path length NO
38、TE 1 Absorptivity = A/(l C), where A is the absorbance, C is the concentration of the substance and l is the sample path length. The unit normally used are cm for l, and kg m-3for C. NOTE 2 The equivalent IUPAC term is “specific absorption coefficient”. adapted from ASTM-E-131 BS EN 16602-70-05:2014
39、EN 16602-70-05:2014 (E) 10 3.2.4 attenuated total reflection reflection that occurs when an absorbing coupling mechanism acts in the process of total internal reflection to make the reflectance less than unity ASTM-E-131 3.2.5 diffuse reflection reflection in which the flux is scattered in many dire
40、ctions by diffusion at or below the surfaces ASTM-E-131 3.2.6 Fourier transformation mathematical process used to convert an amplitude-time spectrum to an amplitude-frequency spectrum or vice versa ASTM-E-131 3.2.7 infrared spectroscopy spectroscopy in the infrared region of the electromagnetic spec
41、trum, i.e. with wavelength range from approximately 0,78 m to 1 000 m (wave number range 12 820 cm-1to 10 cm-1) adapted from ASTM-E-131 3.2.8 molar absorptivity, product of the absorptivity and the molecular weight of the substance NOTE The equivalent IUPAC term is “molar absorption coefficient”. ad
42、apted from ASTM-E-131 3.2.9 radiant power, P amount of energy transmitted in the form of electromagnetic radiation per unit time NOTE 1 Unit for radiant power is Watts. NOTE 2 Radiant power should not be confused with intensity (I), which is the radiant energy emitted within a time period per unit s
43、olid angle (measured in Watts per steradian). 3.2.10 reflectance, R ratio of the radiant power reflected by the sample to the radiant power incident on the sample ASTM-E-131 BS EN 16602-70-05:2014EN 16602-70-05:2014 (E) 11 3.2.11 specific area diameter of the infrared beam at the window location NOT
44、E It is expressed as the ratio of the beam diameter over the area. For example, 7 mm/0,38 cm2, 10 mm/0,79 cm2 or 12 mm/1,13 cm2. 3.2.12 transmittance, T ratio of the radiant power transmitted by the sample to the radiant power incident on the sample ASTM-E-131 3.2.13 wave number, number of waves per
45、 unit length NOTE 1 The unit for wave number is cm-1. In terms of this unit, the wave number is the reciprocal of the wavelength, ( where is expressed in cm). NOTE 2 The wave number is normally used as the X-axis unit of an IR spectrum. adapted from ASTM-E-131 3.3 Abbreviated terms For the purpose o
46、f this Standard, the abbreviated terms from ECSS-S-ST-00-01 and the following apply: Abbreviation Meaning ASTM American Society for Testing and Materials ATR attenuated total reflection AU absorbance unit DOP dioctylphthalate, synonym bis (2-ethylhexyl) phthalate DRIFT diffuse reflection infrared Fo
47、urier transform DTGS deuterated triglycine sulphate IR detector ESD electrostatic discharge FTIR Fourier transform infrared (spectrometry) IES Institute of Environmental Sciences IPA isopropyl alcohol IR Infrared IUPAC International Union of Pure and Applied Chemistry ISO International Organization
48、for Standardization MCT mercury cadmium telluride IR detector NVR non-volatile residue BS EN 16602-70-05:2014EN 16602-70-05:2014 (E) 12 PTFE Polytetrafluoroethylene QCM quartz crystal microbalance RI refractive index S/N signal to noise ratio UV Ultraviolet VCM volatile condensable material BS EN 16
49、602-70-05:2014EN 16602-70-05:2014 (E) 13 4 Principles Infrared qualitative analysis is carried out by functional group identification, or by comparison of the IR absorption spectra of unknown materials with those of known reference materials, or both. It is therefore possible to determine structural information about the molecules of contaminants. In some cases, the source of the contamination can be detected. Infrared quantitative analysis of levels of contaminants is based on the Lambert-Beers (henceforth
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