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1、| | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BRITISH STANDARD BS 8855-2:2000 ICS 13.080
2、.10 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Soil analysis Part 2: Method for determination of coal tar-derived phenolic compounds Licensed Copy: London South Bank University, London South Bank University, Fri Dec 08 00:59:01 GMT+00:00 2006, Uncontrolled Copy, (c) BSI T
3、his British Standard, having been prepared under the direction of the Health and Environment Sector Committee, was published under the authority of the Standards Committee and comes into effect on 15 April 2000 BSI 04-2000 The following BSI references relate to the work on this standard: Committee r
4、eference EH/4/3 Draft for comment 99/561879 DC ISBN 0 580 33130 X BS 8855-2:2000 Amendments issued since publication Amd. No.DateComments Committees responsible for this British Standard The preparation of this British Standard was entrusted by Technical Committee EH/4, Soil quality, to Subcommittee
5、 EH/4/3, Chemical methods, upon which the following bodies were represented: Association of Consulting Scientists B G Technology British Ceramic Research Ltd. British Society of Soil Science Environment Agency Laboratory of the Government Chemist Ministry of Agriculture, Fisheries and Food Society o
6、f Chemical Industry Soil Survey and Land Research Centre Water Research Centre Water UK Licensed Copy: London South Bank University, London South Bank University, Fri Dec 08 00:59:01 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 8855-2:2000 BSI 04-2000i Contents Page Committees responsibleInside fro
7、nt cover Forewordii 1Scope1 2Normative references1 3Principle1 4Safety precautions1 5Reagents1 6Apparatus1 7Preparation of reagents and standards2 8Preparation of laboratory sample2 9Procedure2 10Calculations3 Annex A (informative) Performance characteristics4 Bibliography5 Table 1 Analyte concentra
8、tion ranges giving linear detector response2 Table 2 Indicative retention times of phenolic compounds3 Table A.1 Repeatability4 Table A.2 Reproducibility4 Licensed Copy: London South Bank University, London South Bank University, Fri Dec 08 00:59:01 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ii BSI
9、04-2000 BS 8855-2:2000 Foreword This British Standard has been prepared by Subcommittee EH/4/3. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does
10、 not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, pages 1 to 5 and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued. Licensed Copy: London
11、South Bank University, London South Bank University, Fri Dec 08 00:59:01 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BSI 04-20001 BS 8855-2:2000 1) For information on suitable equipment contact BSI Information Centre, British Standards House, 389 Chiswick High Road, London W4 4AL. 1 Scope This Britis
12、h Standard describes a method for determining the concentration of coal tar-derived phenols, namely catechol, resorcinol, phenol, cresols (ortho-, meta-, para-), xylenols (2,3; 2,4; 2,5; 2,6; 3,4 and 3,5); 2-isopropylphenol, 1-naphthol and 2,3,5 trimethylphenol. It is applicable to all types of soil
13、 containing concentrations of phenols in the approximate range 0.02 mg/kg to 10 mg/kg soil. Some performance characteristics of the method are summarized in annex A. The method is not applicable to the determination of halogenated phenols. The range can be extended by suitable dilution of the extrac
14、ts as required. 2 Normative references The following normative documents contain provisions which, through reference in this text, constitute provisions of this part of this British Standard. For dated references, subsequent amendments to, or revisions of, any of these publications do not apply. For
15、 undated references, the latest edition of the publication referred to applies. BS 7755-3.1, Soil quality Part 3: Chemical methods Section 3.1: Determination of dry matter and water content on a mass basis by a gravimetric method. BS 7755-3.5, Soil quality Part 3: Chemical methods Section 3.5: Pretr
16、eatment of samples for physico-chemical analyses. BS EN ISO 3696, Water for analytical laboratory use Specification and test methods. 3 Principle A sample of as-received soil is extracted with a 60:40 v/v methanol:water mixture. Reversed phase high-performance liquid chromatography (HPLC) with direc
17、t aqueous injection of the sample, and electrochemical detection, is used to determine the phenolic compound content. 4 Safety precautions Phenols are both toxic and corrosive and require handling with care. Methanol is toxic and sodium hydroxide is corrosive. Latex or nitrile gloves and eye protect
18、ion should be worn at all times. Spills should immediately be wiped up with adsorbent tissue and placed in sealed containers used for the disposal of toxic chemicals. Samples should be treated as toxic and harmful. 5 Reagents 5.1 Citric acid, (HPLC grade for electrochemical detection). 5.2 Sodium ac
19、etate, (HPLC grade for electrochemical detection). 5.3 Sodium hydroxide, (HPLC grade for electrochemical detection). 5.4 Methanol, (HPLC grade for electrochemical detection). 5.5 De-ionized or distilled water, of at least Grade 1 as defined in BS EN ISO 3696. 5.6 Helium, (chromatography grade). 5.7
20、Phenol, (analytical grade). 5.8 o-, m-, p-cresols, (analytical grade). 5.9 3,4; 3,5; 2,5; 2,3; 2,4; 2,6 xylenols, (analytical grade). 5.10 2-iso-propylphenol, (analytical grade). 5.11 Catechol, (analytical grade). 5.12 Resorcinol, (analytical grade). 5.13 2,3,5-trimethylphenol, (analytical grade). 5
21、.14 1-naphthol, (analytical grade). 6 Apparatus 6.1 An HPLC system1), capable of delivering an isocratic mobile phase at a rate of 1.0 ml/min, and fitted with an electrochemical detector (see 9.2 for set-up details). (Multiple pumping systems may be used if desired.) 6.2 A 5mm octadecyl silica (ODS)
22、, 25 cm 3 4.5 mm internal diameter column (or equivalent)1), fitted with a matching guard column. 6.3 An injection system1), either manual or automatic capable of injecting up to 100 ml of sample. 6.4 Glass syringe, for example 5 ml capacity is suitable. 6.5 Syringe filters, nylon, 0.45 mm nominal p
23、ore size. 6.6 Glass fibre filters, 0.45 mm nominal pore size. 6.7 Balance, capable of weighing to an accuracy of not less than0.000 1 g. Licensed Copy: London South Bank University, London South Bank University, Fri Dec 08 00:59:01 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 2 BSI 04-2000 BS 8855-2:2
24、000 2) As phenols in soil biodegrade, it is common practice for the sample containers to be filled on site to preserve the phenols. Laboratories pre-weigh bottles containing reagent and re-weigh on receipt in the laboratory. 7 Preparation of reagents and standards 7.1 Stock solutions 7.1.1 Solvent P
25、repare a 60:40 methanol:water mixture by adding 150 ml1.0 ml of methanol (5.4) to 100 ml1.0 ml of distilled or de-ionized water (5.5). 7.1.2 Stock solutions of phenolic compounds Weigh accurately 80 mg of each of the phenolic compounds (5.7 to 5.14) and quantitatively transfer into the same, or sepa
26、rate 100 ml volumetric flasks, dissolving them in methanol:water (7.1.1), to give individual or mixed stock solutions. The concentration of each component is nominally 800 mg/l. Divide the stock solution(s) into 5 ml bottles with tight caps and store at 218 8C. 7.2 Standard solutions for calibration
27、 Prepare standard solutions for calibration from the stock solutions prepared in accordance with 7.1.2. For the range 0.3 mg/l to 3.2 mg/l, dilute 0.1, 0.2, 0.3, 0.5, 0.7 and 1.0 ml (2 % of the respective volume) of the stock solution in 250 ml volumetric flasks with methanol:water (7.1.1) to provid
28、e calibration standards containing, respectively, 0.3, 0.6, 0.9, 1.5, 2.1 and 3.2 mg/l (2 % of the respective mass) phenol. The linear range may be extended above 3.2 mg/l if required. Appropriate detector settings are shown in Table 1. For the range 16 mg/l to 800 mg/l prepare an intermediate worki
29、ng standard solution by diluting 2.5 ml0.05 ml of the stock solution (7.1.2) to 100 ml in a volumetric flask with methanol:water (7.1.1). Further dilute, 0.2, 0.7, 1.0, 3.0, 5.0 and 10.0 ml (2 % of the respective volume) in 250 ml volumetric flasks with methanol:water (7.1.1) to provide calibration
30、standards, containing respectively 16, 56, 80, 240, 400 and 800 mg/l (2 % of the respective mass) phenol. 7.3 Blank determinations Use de-ionized or distilled water (5.5) for blank determinations. 7.4 Preparation of the mobile phase Dissolve 12.2 g0.1 g of citric acid (5.1), 4.4 g0.1 g of sodium ace
31、tate (5.2) and 3.9 g0.1 g of sodium hydroxide (5.3) in 1 000 ml5 ml of water (5.5) and mix the solution with methanol in the ratio 40:60. Filter through a 0.45 mm glass-fibre filter (6.6) and de-gas with helium (5.6) for 30 min before use. Ensure that the mobile phase is at ambient temperature befor
32、e use (the heats of mixing and dissolution will raise its temperature). 8 Preparation of laboratory sample If a bulk sample has been submitted to the laboratory, prepare a laboratory sample using an appropriate procedure, for example that given in BS 7755-3.5. Place 150 ml5.0 ml of methanol:water (7
33、.1.1) in a screw-topped glass bottle, weigh it and record the mass in grams (M1). Weigh out between 50 g and 100 g of the bulk sample and add it to the bottle. Reweigh the bottle and record the mass in grams (M2). Calculate the mass of the laboratory sample (Ms) in grams from the following equation2
34、): Ms= M22 M1 Store the sample in the dark at 4 8C and only remove it from this environment immediately prior to analysis. Before analysis, place the bottle onto a flask shaker for 30 min5 min to extract the phenolic compounds from the sample. 9 Procedure 9.1 Sample for analysis Using a clean glass
35、syringe (6.4) withdraw an amount of the methanol:water extract appropriate to the size of the autosampler vial, from the bottle containing the laboratory sample. Filter through a 0.45 mm nylon syringe filter (6.5) into an auto-sample vial. Use polytetrafluoroethylene (PTFE)-faced septa as phenols ad
36、sorb onto silicone rubber causing low analytical results. 9.2 Detector Set the potential on the electrochemical detector to +750 mV, that on the pre-treatment cell to +250 mV and that on the guard cell to +800 mV. Different detector amplifier ranges shall be used depending on the analyte concentrati
37、on expected. Analyte concentration ranges over which detector response is expected to be linear, expressed as a function of detector amplifier setting, are given in Table 1. Table 1 Analyte concentration ranges giving linear detector response Detector amplifier setting Limits of analyte concentratio
38、n range mA Lower mg/l Upper mg/l 150.2 2100.4 5202.0 10404.0 20808.0 5020020.0 Licensed Copy: London South Bank University, London South Bank University, Fri Dec 08 00:59:01 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BSI 04-20003 BS 8855-2:2000 The amplifier range appropriate to the expected analyte
39、 concentration shall be selected. 9.3 Chromatograph set-up Set the total flow rate to 1 ml/min. Use solutions of the individual phenols (e.g. 3.2 mg/l as prepared in 7.2) to determine the actual retention times of the analytes. Set the total flow rate to 1 ml/min. Adjust the chromatographic conditio
40、ns to provide an optimal separation. Inject 100 ml of calibration standards, blanks and samples using either an auto-sampler or manual injection system (6.3). Users of manual injection systems shall ensure that identical volumes are injected. 10 Calculations Areas of the chromatographic peaks are us
41、ed for quantification. Plot a calibration graph of concentration against peak area and convert sample peak areas into concentration by reading off the graph, or use the appropriate regression line to convert peak areas into concentrations. Calculate the mass of phenolic compounds, P, in the soil sam
42、ple, in milligrams per kilogram using the following equation: P = P1 V Ms where P1is the concentration of phenolic compounds in the methanol:water extract, in milligrams per litre (mg/l); Vis the volume of extract, in litres (l) (volume of methanol:water used in clause 8); Msis the mass of the labor
43、atory soil sample, in kilograms (kg). If the dry matter content of the soil has also been determined according to BS 7755-3.1, then phenolic concentration may also be adjusted to a dry mass basis. Indicative retention times are given in Table 2. Table 2 Indicative retention times of phenolic compoun
44、ds CompoundRetention time min Ratio of retention time to that of phenol Resorcinol3.70.63 Catechol4.30.73 Phenol6.01.0 m-cresol9.01.5 p-cresol9.01.51 o-cresol9.11.52 3,4 xylenol13.42.24 2,6 xylenol13.82.3 3,5 xylenol14.22.38 2,3 xylenol14.32.4 2,5 xylenol14.92.49 2,4 xylenol15.32.57 1-naphthol19.53.
45、27 2-isopropylphenol24.34.07 2,3,5-trimethylphenol24.64.12 Licensed Copy: London South Bank University, London South Bank University, Fri Dec 08 00:59:01 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 8855-2:2000 4 BSI 04-2000 Annex A (informative) Performance characteristics Inter-laboratory trials
46、were organized to test the method given in this British Standard. In these trials the concentrations of phenol, groups of phenolic compounds and the sum of the phenolic compounds determined was measured by a number of laboratories on a number of soils. The soils were obtained from sites formerly use
47、d for the manufacture of gas from coal and therefore contained significant quantities of phenolic compounds. The repeatability (r) and the reproducibility (R) of the results of these analyses are given in Tables A.1 and A.2, respectively. These values have been calculated based on the method in BS I
48、SO 5725-2:1994. Table A.1 Repeatability Phenolic compoundNumber of replicatesMean concentration mg/kg Standard deviation (sr) mg/kg Repeatability limit (r) mg/kg Phenol111.20.060.17 Cresols111.50.10.28 Xylenols111.60.150.42 Total115.50.551.5 NOTERepeatability limit, r = 2.8sr. Table A.2 Reproducibil
49、ity Phenolic compoundNumber of laboratories Mean concentration mg/kg Standard deviation (SR) mg/kg Reproducibility limit (R) mg/kg Total1820.82.26.2 Total2029848135 Total2116.72.77.7 Total276.51.85 Phenol161411748 Phenol2091.43.8 Cresols147.30.61.6 Xylenols163.20.51.4 NOTE 1Reproducibility limit R = 2.8SR. NOTE 2Total phenols in this table is related to the sum of the phenols analysed, and is not necessarily a measure of the total phenols in the sample. NOTE 3Performance data are quoted for the summed cresols and xylenols, rather than the
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