1、BSI Standards Publication PD ISO/TR 18105:2014 Soil quality Detection of water soluble chromium(VI) using a ready-to-use test-kit methodPD ISO/TR 18105:2014 PUBLISHED DOCUMENT National foreword This Published Document is the UK implementation of ISO/TR 18105:2014. The UK participation in its prepara
2、tion was entrusted to Technical Committee EH/4, Soil quality. A list of organizations represented on this committee can be obtained on request to its secretary. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application.
3、 The British Standards Institution 2014. Published by BSI Standards Limited 2014 ISBN 978 0 580 79525 1 ICS 13.080.10 Compliance with a British Standard cannot confer immunity from legal obligations. This Published Document was published under the authority of the Standards Policy and Strategy Commi
4、ttee on 30 September 2014. Amendments issued since publication Date Text affectedPD ISO/TR 18105:2014 ISO 2014 Soil quality Detection of water soluble chromium(VI) using a ready- to-use test-kit method Qualit du sol Dtection du chrome(VI) soluble dans leau en utilisant un kit dessai prt lemploi TECH
5、NICAL REPORT ISO/TR 18105 First edition 2014-05-15 Reference number ISO/TR 18105:2014(E)PD ISO/TR 18105:2014ISO/TR 18105:2014(E)ii ISO 2014 All rights reserved COPYRIGHT PROTECTED DOCUMENT ISO 2014 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or util
6、ized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below or ISOs member body in the country of the requester. ISO copyrig
7、ht office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in SwitzerlandPD ISO/TR 18105:2014ISO/TR 18105:2014(E) ISO 2014 All rights reserved iii Contents Page Foreword iv Introduction v 1 Scope . 1 2 References . 1 3 T
8、 erms and definitions . 1 4 Principle 1 5 Reagents 2 6 Interferences 2 7 Apparatus . 2 8 Procedure. 2 8.1 Calibration 2 8.2 Sample detection . 2 8.3 Measurement 2 9 Quality assurance (QA) and quality control (QC) . 3 10 Test report . 3 Annex A (informative) Extraction of Cr(VI) from soil CRMs . 4 An
9、nex B (informative) Comparison of Cr(VI) results obtained with commercially available test-kits . 7 Annex C (informative) Simulation of mapping distributions of Cr(VI) contaminating potential land . 8 Bibliography .14PD ISO/TR 18105:2014ISO/TR 18105:2014(E) Foreword ISO (the International Organizati
10、on 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 ha
11、s 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
12、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 edi
13、torial 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 ri
14、ghts 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 constitute an endorsement. For an e
15、xplanation on the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary information. The committee responsible for this
16、 document is ISO/TC 190, Soil quality, Subcommittee SC 3, Chemical methods and soil characteristics.iv ISO 2014 All rights reservedPD ISO/TR 18105:2014ISO/TR 18105:2014(E) Introduction A test-kit method uses reagents stored in plastic or glass vials prepared for colorimetric detection of specific co
17、mpounds soluble with water. There is a lot of varieties of test-kits developed mainly for the compounds in water samples based on well-known reactions with commonly-used and chemically stable reagents indicating constant magnitudes of intensities of the signals from target compounds. The common reac
18、tions employed for the test-kit usually give colour, by which the user can recognize the concentration level of the compound without absorption spectrophotometers even in the situation when such instruments are not available. Thus, the test-kit determination of the compound in water samples can be u
19、sed to screen specific compounds in soil samples, if they are easily dissolved into water. The reaction applied depends on the target compounds. For chromium(VI), a reaction is used, where 1,5-diphenylcarbazide is used, its isomer or derivatives. When other chemicals or derivatives are used, the per
20、formance is intended to be similar to that obtained with the original reagents. The test-kit consisting of the reagents has to be identified by confirming the spectrum including intensities at a specific wavelength. The spectrum shape should be similar to each other between those from test-kits and
21、bulk reagents commonly used for absorptiometry in laboratories. The intensities and varieties of interferences to the test-kit method should be within those taking place to absorptiometry test methods with bulk reagents. The quality or purity of the reagents packed in test-kits should keep constant
22、with a deviation around that for the bulk reagents for absorptiometry. The detection limit and working curves available with test-kits should be confirmed in prior of the use. When screening contaminated sites for Cr(VI) by test-kit detection, Cr(VI) is extracted from soil into water. The recovery o
23、f extracted Cr(VI) would be slightly lower than that when extracting with alkali solution; however, the repeatability of test-kit detection for Cr(VI) is high enough to apply the detection manner to contaminated sites as a screening method. Basically, laboratory analysis provides with precise concen
24、tration values but takes longer time and higher costs than those of test-kit detection. Furthermore, under the conditions that survey time and the total costs are restricted, test-kit detection is more useful and practical as it can cover more inspection spots, resulting in precise information on th
25、e pollution at investigation sites, compared with a conventional manner applying samples to laboratory analysis that costs and limits the numbers of samples to be analysed due to a lean budget for financial reasons. The two investigation manners, or the conventional methods and the screening work, h
26、ave their specific advantages and characters. Then, it is quite natural to choose one of the two options. In short, one gives precise concentration values at selected spots within a limited number but calling for high costs while the other provides concentration levels at spots with no limits in num
27、ber but showing good cost performance. This Technical Report describes the procedure to screen soil for Cr(VI) using a method with test-kits developed for water samples. ISO 2014 All rights reserved vPD ISO/TR 18105:2014PD ISO/TR 18105:2014Soil quality Detection of water soluble chromium(VI) using a
28、 ready-to-use test-kit method 1 Scope This Technical Report describes the procedure to screen soil samples to detect Cr(VI) using test-kits based on water extraction of Cr(VI) in soil. The test-kit approach in this method is designed to quickly screen soil samples using calibration to indicate the c
29、oncentration level. A batch test at a liquid to solid ratio of 10 l/kg, designated by ISO/TS 21268-2, has been used in Japan for over 30 years to evaluate the risk of Cr(VI) contamination in soil. The Cr(VI) detection by a ready-to-use test-kit method follows ISO/TS 21268-2. This screening technique
30、 is applicable in laboratories but can also be applied for site screening in the field. The standard system detection covers the range mg/kg to % for Cr(VI). This method is expected as a screening technique because of the significant colour change given by 1,5-diphenylcarbazide in the existence of C
31、r(VI). The method may be especially useful in quickly detecting Cr(VI) where a site is assumed to have no Cr(VI) contamination. As with other screening techniques, it is advisable to confirm a certain percentage of both positive and negative test results in another technique, especially when the det
32、ected level is near or above a regulatory action limit or when the presence of background or interfering materials is suspected. Basically, laboratory analysis requires longer time and higher costs than those of test-kit detection. If the same survey time and the costs are allowed with test-kit scre
33、ening work and conventional investigation methods including laboratory analysis, the former way can work on more inspection spots than the latter. However, test-kit detection should carefully be adopted for site investigation because the recovery of Cr(VI) from soil into water dependent on soil matr
34、ices changes the performance of test-kit detection. 2 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 amend
35、ments) applies. ISO 11074, Soil quality Vocabulary 3 T erms a nd definiti ons For the purposes of this document, the terms and definitions given in ISO 11074 and the following apply. 3.1 ready-to-use method analytical method that is ready-made for use, and may be employed in the field Note 1 to entr
36、y: A more familiar name is “field method”. SOURCE: ISO 17381:2003, 3.2, modified definition shortened 4 Principle Chromium(VI) in solution reacts with 1,5-diphenylcarbazide to form a red-violet complex of chromium-1,5, diphenylcarbazone resulting in colour changes of the solution due to the formatio
37、n. Spectrometry and colour charts are applied to determine the complex. The test determines Cr(VI) TECHNICAL REPORT ISO/TR 18105:2014(E) ISO 2014 All rights reserved 1PD ISO/TR 18105:2014ISO/TR 18105:2014(E) present in the soil extract as chromate or dichromate ions. The test-kit method to detect th
38、e Cr(VI) in soil consists of three basic steps: extraction, filtration and detection. 5 Reagents 5.1 Water, de-ionized, as an extraction solvent to extract Cr(VI) from soil samples. 5.2 Test-kit reagent, i.e. 1,5-diphenylcarbazide. 6 Interferences Arsenic, cobalt, iron(II), iron(III), tin, vanadium,
39、 lead and phenol may give colour changes by reacting with 1,5-diphenylcarbazide. Reducing agents like iron(II) and ascorbic acid effect to reduce Cr(VI) to Cr(III). Thus, they also interfere with a chromium(VI)/1,5-diphenylcarbazone reaction. 7 Apparatus 7.1 Spectrometer, hand-held or portable photo
40、meter working at a wavelength of 540 nm. 7.2 Colour chart, with colour bars indicating a value on a reference concentration. 7.3 Spoon, non-metal to take soil samples. 7.4 Sample tube and vial, e.g. plastic or glass tube for the extraction operation by shaking and a transparent glass vial for the te
41、st-kit observation. 8 Procedure 8.1 Calibration When using a photometer for photometric observation of Cr(VI) in the sample solution, prepare a calibration curve using blank and working standards. The working standards should be prepared by spiking an appropriate amount of Cr(VI) solution into de-io
42、nized water. When using a colour chart for the detection of Cr(VI), the calibration process is not necessary. 8.2 Sample detection Weigh out 1 g of a soil sample and put into 10 ml of water. Shake the mixture for 1 min and then filtrate using a 0,45 m pored membrane filter. Dilute 1 ml of the filtra
43、te with water to give at least 10 ml, when the colour of the sample is out of the range of the colour chart supplied by the manufacturer due to too high concentration of Cr(VI) in the filtrate. 8.3 Measurement Introduce a certain volume of the diluted sample (7.2) into the test-kit apparatus. Measur
44、e the absorbance of the solution at a wavelength of 540 nm using a suitable cell with a 10 mm optical path length or observe the colour comparing with the colour chart.2 ISO 2014 All rights reservedPD ISO/TR 18105:2014ISO/TR 18105:2014(E) 9 Quality assurance (QA) and quality control (QC) A program o
45、f field QA/QC should include a minimum of periodic soil blanks, equipment blanks, soil spikes and duplicates. Other procedures should be implemented depending on the specific requirements of each site. To ensure accurate quantification and repeatable results, it is recommended that a recalibration b
46、e run at a certain interval or at least daily. The analytical results contain uncertainty arising from numerous sources, heterogeneity of soil sample, difficulty in using matrix matched reference samples, etc. The expanded uncertainty of measurement can be estimated from the uncertainty budget with
47、standard uncertainties. See ISO/IEC Guide 98 for the guidance on the estimation of expanded uncertainty. 10 Test report The test report (see ISO 12404) should contain at least the following information: a) a reference to this Technical Report; b) complete identification of samples; c) the results of
48、 the determination; d) any details not mentioned in this Technical Report or which are optional, as well as any factor which may have affected the results. ISO 2014 All rights reserved 3PD ISO/TR 18105:2014ISO/TR 18105:2014(E) Annex A (informative) Extraction of Cr(VI) from soil CRMs A preliminary e
49、valuation of test-kit detection performance with certified reference materials (CRMs) showed that test-kits effectively work as a screening method. Figure A.1 and Figure A.2 show the relative concentrations of Cr(VI) in sandy loam and clay CRMs when Cr(VI) was extracted with alkaline solution as designated by ISO 15192 and EPA 3060 as well as with water as designated in this Technical Report. The Cr(VI) recovery when applying the test-kits to the detection of Cr(VI) in the CRMs was high for the sandy loam CRM, even when the Cr(VI) extr
