EN 62554-2011 en Sample preparation for measurement of mercury level in fluorescent lamps《荧光灯中含汞量测量用样品制备》.pdf

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1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationSample preparation for measurement of mercury level in fluorescent lampsBS EN 62554:2011National forewordThis British Standard is the UK implementation of EN 62554:2011. It is id

2、entical to IEC 62554:2011.The UK participation in its preparation was entrusted by Technical CommitteeCPL/34, Lamps and Related Equipment, to Subcommittee CPL/34/1, Electriclamps.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does no

3、t purport to include all the necessary provisions of acontract. Users are responsible for its correct application. BSI 2011ISBN 978 0 580 68008 3ICS 29.140.30Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of the

4、 StandardsPolicy and Strategy Committee on 30 November 2011.Amendments issued since publicationAmd. No. Date Text affectedBRITISH STANDARDBS EN 62554:2011EUROPEAN STANDARD EN 62554 NORME EUROPENNE EUROPISCHE NORM October 2011 CENELEC European Committee for Electrotechnical Standardization Comit Euro

5、pen de Normalisation Electrotechnique Europisches Komitee fr Elektrotechnische Normung Management Centre: Avenue Marnix 17, B - 1000 Brussels 2011 CENELEC - All rights of exploitation in any form and by any means reserved worldwide for CENELEC members. Ref. No. EN 62554:2011 E ICS 29.140.30 English

6、version Sample preparation for measurement of mercury level in fluorescent lamps (IEC 62554:2011) Prparation des chantillons en vue de la mesure du niveau de mercure dans les lampes fluorescentes (CEI 62554:2011) Vorbereitung des Prfmusters zur Messung des Quecksilbergehalts in Leuchtstofflampen (IE

7、C 62554:2011) This European Standard was approved by CENELEC on 2011-09-23. CENELEC 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 bi

8、bliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CENELEC member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the

9、responsibility of a CENELEC member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CENELEC members are the national electrotechnical committees of Austria, Belgium, Bulgaria, Croatia, Cyprus, the Czech Republic, Denmark, Estonia,

10、Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, the Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. BS EN 62554:2011EN 62554:2011 - 2 - Foreword The text of document 34A/1

11、484/FDIS, future edition 1 of IEC 62554, prepared by SC 34A, “Lamps“, of IEC TC 34, “Lamps and related equipment“ was submitted to the IEC-CENELEC parallel vote and approved by CENELEC as EN 62554:2011. The following dates are fixed: latest date by which the document has to be implemented at nationa

12、l level by publication of an identical national standard or by endorsement (dop) 2012-06-23 latest date by which the national standards conflicting with the document have to be withdrawn (dow) 2014-09-23 Attention is drawn to the possibility that some of the elements of this document may be the subj

13、ect of patent rights. CENELEC and/or CEN shall not be held responsible for identifying any or all such patent rights. Endorsement notice The text of the International Standard IEC 62554:2011 was approved by CENELEC as a European Standard without any modification. BS EN 62554:2011- 3 - EN 62554:2011

14、Annex ZA (normative) Normative references to international publications with their corresponding European publications The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest e

15、dition of the referenced document (including any amendments) applies. NOTE When an international publication has been modified by common modifications, indicated by (mod), the relevant EN/HD applies. Publication Year Title EN/HD Year ISO/IEC 17025 2005 General requirements for the competence of test

16、ing and calibration laboratories EN ISO/IEC 17025 2005 IEC 62321 2008 Electrotechnical products - Determination of levels of six regulated substances (lead, mercury, cadmium, hexavalent chromium, polybrominated biphenyls, polybrominated diphenyl ethers) EN 62321 2009 ISO 3696 1987 Water for analytic

17、al laboratory use - Specification and test methods EN ISO 3696 1995 BS EN 62554:2011 2 62554 IEC:2011 CONTENTS INTRODUCTION . 5 1 Scope . 6 2 Normative references . 6 3 Terms and definitions . 6 4 General 7 5 Procedure for collecting mercury from a fluorescent lamp . 7 5.1 General . 7 5.2 Reagents .

18、 7 5.3 Chemical lab ware . 8 5.4 Sample preparation . 8 5.4.1 Cold spotting methods . 8 5.4.2 Sample preparation of fluorescent lamps by non-cold-spot (sectioning) methods 10 5.4.3 Sample preparation of fluorescent lamps by non-cold-spot (crushing) methods 11 5.4.4 Nitric acid rinse method for linea

19、r fluorescent lamps 12 5.4.5 Direct mercury measurement . 12 5.4.6 Sample preparation of other fluorescent lamps 13 5.5 Sample digestion . 13 5.5.1 Ambient conditions 13 5.5.2 Glass samples (in 250 ml, 500 ml, 1 000 ml or 2 000 ml container) 13 5.5.3 Metal samples (in 125 ml container) 13 5.6 Filter

20、ing . 14 6 Measurement . 14 6.1 Blank test 14 6.2 Data reporting . 14 6.3 Analysis 14 Annex A (informative) Electrothermal vaporization atomic absorption spectrometry (EVAAS) method . 15 Annex B (informative) Information on the cold spotting method . 18 Figure A.1 Configuration of the electrothermal

21、 vaporization atomic absorption spectrometry testing apparatus . 15 Figure A.2 An example of the electrothermal vaporization atomic absorption spectrometer test apparatus layout . 16 Figure B.1 Example of glass cell arrangement . 19 Figure B.2 Example of cooling device arrangement 20 BS EN 62554:201

22、162554 IEC:2011 5 INTRODUCTION The International Electrotechnical Commission (IEC) draws attention to the fact that it is claimed that compliance with this document may involve the use of a patent concerning Cold spotting given in 5.4.1. IEC takes no position concerning the evidence, validity and sc

23、ope of this patent right. The holder of this patent right has assured the IEC that he/she is willing to negotiate licences free of charge with applicants throughout the world. In this respect, the statement of the holder of this patent right is registered with IEC. Information may be obtained from:

24、General Electric Company Appliance Park AP35-1002, Louisville, KY, 40225-0001, US Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights other than those identified above. IEC shall not be held responsible for identifying any or all such

25、patent rights. ISO (www.iso.org/patents) and IEC (http:/patents.iec.ch) maintain on-line data bases of patents relevant to their standards. Users are encouraged to consult the data bases for the most up to date information concerning patents. According to IEC SMB 136/7 decision, the technical commit

26、tee decided to remove designation of a reference method. BS EN 62554:2011 6 62554 IEC:2011 SAMPLE PREPARATION FOR MEASUREMENT OF MERCURY LEVEL IN FLUORESCENT LAMPS 1 Scope This International Standard specifies sample preparation methods for determining mercury levels in new tubular fluorescent lamps

27、 (including single capped, double capped, self-ballasted and CCFL for backlighting) containing 0,1 mg mercury or more. The intended resolution of the methods described in this standard is of the order of 5 %. Mercury level measurement of spent lamps is excluded, as during lamp operation, mercury gra

28、dually diffuses into the glass wall and reacts with the glass materials. The test method of this standard does not recover mercury that is diffused into or reacted with or otherwise incorporated irreversibly with the glass wall of discharge tubes. This standard does not contain information on measur

29、ement. Measurement is specified in IEC 62321. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any a

30、mendments) applies. ISO/IEC 17025:2005, General requirements for the competence of testing and calibration laboratories IEC 62321:2008, Electrotechnical products Determination of levels of six regulated substances (lead, mercury, cadmium, hexavalent chromium, polybrominated biphenyls, polybrominated

31、 diphenyl ethers) ISO 3696:1987, Water for analytical laboratory use Specification and test methods 3 Terms and definitions For the purposes of the present document, the following terms and definitions apply. 3.1 new lamp a lamp that has not been energized since manufacture 3.2 cold cathode fluoresc

32、ent lamp (CCFL) for backlighting small diameter fluorescent lamp having cold cathode in the lamp, in which most of light is emitted by the excitation of phosphors coated in discharge tube and used as backlight in LCD 3.3 external electrode fluorescent lamp (EEFL) for backlighting small diameter fluo

33、rescent lamp having cold cathode attached outside the lamp, in which most of light is emitted by the excitation of phosphors coated in discharge tube and used as backlighting in LCD EEFL is a subtype in CCFL lamp group. BS EN 62554:201162554 IEC:2011 7 4 General Mercury in fluorescent lamps exists i

34、n the following states: a) vapour in a lamp; b) liquid metal; c) compound; d) alloy. There is a wide variety of mercury dosing solutions including appearance and placement of mercury dispensing devices and also composition and structure of those devices. Although some of the lamps are dosed with ama

35、lgam or solid mercury alloy, there are also many fluorescent lamps dosed with liquid mercury. Amalgam dosed lamps often have device(s) that act as an auxiliary amalgam. Form and location of these devices vary widely as well. The introduction of a cold spot (see Annex B) minimizes the loss of mercury

36、 in the vapour state when the discharge tube is opened. With the lamp operating, the cold spot will condense all the mercury in the discharge, allowing superior control for mercury recovery. The procedure in Clause 5 below includes a method to collect liquid mercury, mercury compounds and alloys and

37、 amalgams. The total amount of mercury is determined by measuring the amount of liquid mercury, mercury compounds and alloys and amalgam. The amount of mercury is calculated from the measured mercury concentration, the volume of the filtered solution and the dilution factor. 5 Procedure for collecti

38、ng mercury from a fluorescent lamp 5.1 General For test arrangement and ambient conditions, relevant parts of ISO/IEC 17025:2005 shall be followed. WARNING Persons using this International Standard should be familiar with normal laboratory practice. This standard does not purport to address all of t

39、he safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices, to avoid pollution of the environment and to ensure compliance with any national regulatory conditions. 5.2 Reagents The following reagents shall be used: w

40、ater: Grade 1, as specified in ISO 3696; the mass fraction of mercury in the following reagents shall be below 1 109; potassium permanganate 5 % aqueous solution (m/v); nitric acid, concentrated 65 %; hydrochloric acid, concentrated 37 %; hydrofluoric acid, concentrated 40 %. BS EN 62554:2011 8 6255

41、4 IEC:2011 5.3 Chemical lab ware Chemical lab ware shall be verified to be mercury non-absorbing. Chemical lab ware shall be as follows: disposable vacuum filter pack with medium retention filter; disposable wide mouth screw-capped plastic bottles: 125 ml, 250 ml, 500 ml, 1 000 ml, 2 000 ml; disposa

42、ble wide mouth sturdy plastic bag nominal 500 ml, 1 000 ml; beaker 50 ml, 100 ml, 125 ml, 250 ml, 500 ml; volumetric flasks: 50 ml, 100 ml, 250 ml, 500 ml; micropipettes; dispensers; bench coat: sheet of plastic lined laboratory bench paper. NOTE The plastic bag may be clear polyethylene or similar

43、chemical and acid resistant material nominally 0,01 mm or thicker. The 1 000 ml bag would be approximately 200 mm 300 mm. Sometimes known as a “blender or stomacher bag” they are available from biological laboratory suppliers. Bag size may be adjusted to suit availability and lamp size being tested.

44、 5.4 Sample preparation Sample preparation process shall be a continuous operation without excessive hold time. 5.4.1 Cold spotting methods 5.4.1.1 General Cold spotting is a method for condensing free mercury in a localized position (see Annex B). The mercury localization occurs while the low-press

45、ure discharge lamp is “ON” under normal operating conditions while a small area (the cold spot) of the discharge tube is maintained at a low temperature. During the cold spotting process, no heavy end blackening should be observed. When the free mercury is fully condensed, the light output of the la

46、mp will drop significantly and the discharge colour will typically turn pink. The process of free mercury localization (cold-spotting) is then completed. NOTE Mercury collection with cold spot below 0 C and operating with the normal control gear of the lamp may take several days. 5.4.1.2 Sample prep

47、aration of self-ballasted and single capped compact fluorescent multi limbed lamps with cold-spotting Discharge tube cutting operations shall be carried out above the wide mouth screw capped plastic bottle to minimize the risk of material loss. Sample containers shall be as follows. Use 250 ml wide

48、mouth screw-capped plastic bottle for cold spot section as first container. Use 125 ml wide mouth screw-capped plastic bottle for end portions of discharge tube as second container. Use 500 ml or 1 000 ml wide mouth screw-capped plastic bottle for glass parts of discharge tube, depending on which on

49、e fits better to the discharge tube dimensions under test as third container. BS EN 62554:201162554 IEC:2011 9 The sample preparation shall be executed according to the process steps listed below. a) Separate discharge tube from its outer bulb, if any. b) Clean the discharge tube with chemical wipe. c) Mark discharge tube in a non-destructive manner for first sectioning. Mark 3 cm on both sides of the cold spot. d) Collect the free mercury with cold spotting see 5.4.1