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1、A Reference number ISO 5667-15:1999(E) INTERNATIONAL STANDARD ISO 5667-15 First edition 1999-08-01 Water quality Sampling Part 15: Guidance on preservation and handling of sludge and sediment samples Qualit de leau chantillonnage Partie 15: Guide gnral pour la prservation et le traitement des chanti
2、llons de boues et de sdiments Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 09:27:09 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 5667-15:1999(E) ISO 1999 All r
3、ights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from the publisher. International Organization for Standardization Case pos
4、tale 56 CH-1211 Genve 20 Switzerland Internetisoiso.ch Printed in Switzerland ii Contents 1 Scope1 2 Normative reference1 3 Sample storage, preservation and handling.1 3.1 General considerations1 3.2 Chemical examination1 3.3 Physical examination .2 3.4 Biological examination.2 3.5 Feasible precauti
5、ons2 3.6 Sample handling.3 3.7 Sample preservation.3 3.8 Sample storage.3 4 Sample record and quality assurance.4 Bibliography7 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 09:27:09 MDTNo repr
6、oduction or networking permitted without license from IHS -,-,- ISOISO 5667-15:1999(E) iii 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 o
7、ut 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 c
8、ollaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3. Draft International Standards adopted by the technical committees
9、 are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. International Standard ISO 5667-15 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 6, Sampling (general met
10、hods). ISO 5667 consists of the following parts, under the general title Water quality Sampling: Part 1: Guidance on the design of sampling programmes Part 2: Guidance on sampling techniques Part 3: Guidance on the preservation and handling of samples Part 4: Guidance on sampling from lakes Part 5:
11、Guidance on sampling of drinking water Part 6: Guidance on sampling of rivers and streams Part 7: Guidance on sampling of water and steam in boiler plants Part 8: Guidance on sampling of wet deposition Part 9: Guidance on sampling from marine waters Part 10: Guidance on sampling of waste waters Part
12、 11: Guidance on sampling of groundwaters Part 12: Guidance on sampling of bottom sediments Part 13: Guidance on sampling of water, wastewater and related sludges Part 14: Guidance on quality assurance of environmental water sampling and handling Part 15: Guidance on preservation and handling of slu
13、dge and sediment samples Part 16: Guidance on biotesting of samples Part 17: Guidance on sampling of suspended sediments Part 18: Guidance on sampling of groundwater on potentially contaminated sites Copyright International Organization for Standardization Provided by IHS under license with ISO Lice
14、nsee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 09:27:09 MDTNo reproduction or networking permitted without license from IHS -,-,- Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 09:27:09 MD
15、TNo reproduction or networking permitted without license from IHS -,-,- INTERNATIONAL STANDARD ISOISO 5667-15:1999(E) 1 Water quality Sampling Part 15: Guidance on preservation and handling of sludge and sediment samples 1 Scope This part of ISO 5667 provides guidance on the procedures for preservat
16、ion and handling of sewage and waterworks sludges, suspended matter, and saltwater and freshwater sediments for subsequent analysis. 2 Normative reference The following normative document contains provisions which, through reference in this text, constitute provisions of this part of ISO 5667. For d
17、ated references, subsequent amendments to, or revisions of, any of these publications do not apply. However, parties to agreements based on this part of ISO 5667 are encouraged to investigate the possibility of applying the most recent edition of the normative documents indicated below. For undated
18、references, the latest edition of the normative document referred to applies. Members of ISO and IEC maintain registers of currently valid International Standards. ISO 5667-3 :1994, Water quality Sampling Part 3: Guidance on the preservation and handling of samples. 3 Sample preservation and handlin
19、g 3.1 General considerations Storage begins when the samples are taken. All storage methods will affect the sample to some extent, and the choice of preservation technique depends mainly on the objective of the sample collection. It is important that the effects that preservation and storage techniq
20、ues can have on sample quality and the results of analysis are understood. Sludge and sediment samples are subject to chemical, physical and biological changes as soon as they are collected. If guidance is required on the type of sampling technique to be used, guidance is given in ISO 5667-12 and IS
21、O 5667-13. Sample handling, preservation and storage shall be designed to minimize any changes in composition of the sample by retarding chemical and/or biological activity and by avoiding contamination. Specific preservation techniques are often necessary for a representative evaluation of the slud
22、ges and sediments, and a variety of chemical, physical and biological investigations can be performed on the collected samples. No single preservation method is applicable to all constituents. The objective of the sampling programme and the nature of the analytical method will determine the handling
23、 operation or preservation technique. 3.2 Chemical examination In this type of investigation, the nature and amounts of the substances which have become absorbed or adsorbed by the sludges and sediments can be determined. Partition of chemicals between solid phase and water phase is influenced by se
24、veral factors, such as particle size, amount of organic matter, pH, redox potential or salinity. The study of such attributes may be a sampling objective and therefore the preservation needs of the analytical methods to be employed should be taken into account (see Table 1). The guidance given in th
25、is part of ISO 5667 is relevant Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 09:27:09 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 5667-15:1999(E) ISO 2 to the
26、 determination of components in the sum of the separate phases of a sludge or sediment, unless otherwise indicated. Preservation of samples by fast-freezing can cause mobilization of contaminants by cellular disruption, whereas not stabilizing samples can permit continued microbial transformation of
27、 critical pollutants. In addition to biodegradation of organics, volatilization is a principal mechanism of loss of volatile compounds during sample handling. Anoxic samples require appropriate preservation techniques such as oxygen exclusion during sample handling. Where refrigeration is not availa
28、ble at the time of collection of liquid sludge samples, particularly in countries with high ambient temperatures, preservation of the samples for sulfide determination can be achieved by raising the pH to greater than 10,5. Analysis should still be carried out as soon as possible after collection. D
29、rying, freezing, and freeze-drying of anoxic samples alter the binding sites of for example heavy metals, making more differentiated investigation of binding forms virtually impossible. 3.3 Physical examination In this type of examination, the structure, texture and, for sediments, the layer formati
30、on, are determined. Sediment fabric changes are obvious if rapid drainage of pore water occurs. The importance of sludge or sediment integrity to the investigation objectives should be evaluated, as it can influence the preservation and handling techniques. In general, any disturbance of the samples
31、 should be minimized. Where sample integrity is important, agitation- and vibration-free conditions should be maintained during transport; fast-freezing of the sludges and sediments may be appropriate. 3.4 Biological examination Biological studies include toxicological, ecotoxicological and ecologic
32、al examinations. The same factors mentioned in relation to chemical investigations could alter bioavailability and toxicity of compounds. Chemicals might bio- degrade, volatilize, oxidize or photolyze during storage. Therefore, careful consideration should be given to these processes and the storage
33、 conditions needed to avoid such alterations. However, the assessment of sludge contamination by laboratory bioassay testing requires different preservation techniques in comparison to ecological or microbial investigation. An ecological investigation generally involves classifying the species and n
34、umbers of flora and/or fauna present on and in fixed sludges or sediments. On the other hand, microbial activity may also be of interest to characterize samples and can only be determined without fixation. Microbial activity may be responsible for changes in the nitrate-nitrite-ammonia content, for
35、decreases in biochemical oxygen demand, or for reducing sulfate to sulfide. To minimize any changes due to microbial activity, samples should be kept as cool as possible, without freezing, until analysis. For bacteriological examination, sterile glass containers shall be used. Containers should be a
36、ble to withstand a sterilization temperature of 175 C for 1 h and should not produce or release at this temperature any chemicals that would influence biological activity. It may be possible to use disposable commercial plastics containers, subject to verification of the absence of interference with
37、 the analysis. Manipulation of the samples is often necessary, and the optimal methods depend on the study objectives. 3.5 Feasible precautions 3.5.1 Safety precautions It is essential for proper health and safety precautions to be observed at all times when sampling potentially hazardous sludges or
38、 sediments. Human exposure to pathogenic organisms or pollutants should be avoided by using respirators, safety glasses and appropriate protective gloves. Primary digestion of sludge produces methane, which presents a risk of fire and explosion if a source of ignition is present. Containers should b
39、e wrapped with waterproof adhesive tape to minimize the fragmentation of the containers if an explosion occurs. Care should be taken when sampling, transporting and utilizing the sludge, to prevent a build-up of gas pressure in the sample container. Manual release of pressure during and after transp
40、ort may be necessary if prolonged storage is required. 3.5.2 Other precautions See ISO 5667-3 for precautions to be taken in the preparation, filling and use of appropriate containers. Sample containers should be made from materials appropriate for conserving the natural properties of both the sampl
41、e and the expected spectrum of contaminants. Careful consideration should also be given to their suitability for cleaning/decontamination or disposal. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2
42、007 09:27:09 MDTNo reproduction or networking permitted without license from IHS -,-,- ISOISO 5667-15:1999(E) 3 Container labels should withstand soaking, drying and freezing without detaching or becoming illegible. The labelling system should be waterproof to allow use in the field. 3.6 Sample hand
43、ling Sample handling is specific for each determination to be conducted. Manipulation of samples is often required to yield consistent material for toxicity testing and laboratory experiments. Homogenization by mixing, sieving, dilution for concentration-effect determinations, and addition of chemic
44、al preservatives all complicate interpretations of in situ comparisons. All information regarding sample manipulation, handling and storage should therefore be included in a sampling report. Generally, samples should completely fill the storage container, leaving no air space. However, note that the
45、 final method of analysis may determine or influence the void space in the container. If the sample is to be frozen, enough air space should be allowed for expansion to take place. Sufficient sample volume should be collected to allow: separate sub-samples to be preserved for each type of analysis o
46、r examination to be undertaken; repeat analysis in the event of error checking or the routine quality control requirements of duplicate analysis (see clause 4); and the preparation of time-dependent composites; for example a daily aliquot of sewage works sludge (preserved as appropriate) may be reta
47、ined to produce a composite for monthly analysis. 3.7 Sample preservation Because the first few hours after sampling are the most critical for changes to occur in the sample, preservation steps should be taken where possible immediately upon sample collection. No recommendations can be given for a u
48、niversal preservation or storage technique. A technique for one group of analyses may interfere with other analyses. To overcome this problem, a sufficient sample volume should be taken to allow specific preservation or storage techniques for each specific investigation. Refrigeration at 2 C to 5 C is the recommended basic preservation method. Freezing or addition of chemicals is recommended for determining organic constituents. Samples for particle analyses or biological examinations should be preserved at 2 C to 5 C , never frozen or dried. All means of p