1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS ISO 11349:2010Water quality Determinationof low-volatility lipophilicsubstances GravimetricmethodBS ISO 11349:2010 BRITISH STANDARDNational forewordThis British Standard is th
2、e UK implementation of ISO 11349:2010.The UK participation in its preparation was entrusted to TechnicalCommittee EH/3/2, Physical chemical and biochemical methods.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to in
3、clude all the necessaryprovisions of a contract. Users are responsible for its correctapplication. BSI 2010ISBN 978 0 580 65937 9ICS 13.060.50Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy
4、 and Strategy Committee on 31 December 2010.Amendments issued since publicationDate Text affectedBS ISO 11349:2010Reference numberISO 11349:2010(E)ISO 2010INTERNATIONAL STANDARD ISO11349First edition2010-09-15Water quality Determination of low-volatility lipophilic substances Gravimetric method Qual
5、it de leau Dosage des substances lipophiles peu volatiles Mthode gravimtrique BS ISO 11349:2010ISO 11349:2010(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces wh
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10、.org Published in Switzerland ii ISO 2010 All rights reservedBS ISO 11349:2010ISO 11349:2010(E) ISO 2010 All rights reserved iiiForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing Internat
11、ional Standards is normally carried out 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 I
12、SO, also take part in the work. ISO collaborates 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 2. The main task of technical c
13、ommittees is to prepare International Standards. Draft International Standards adopted by the technical committees 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. Attention is drawn to th
14、e 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. ISO 11349 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 2, Physical, chemical and biochemica
15、l methods. BS ISO 11349:2010BS ISO 11349:2010INTERNATIONAL STANDARD ISO 11349:2010(E) ISO 2010 All rights reserved 1Water quality Determination of low-volatility lipophilic substances Gravimetric method WARNING Persons using this International Standard should be familiar with normal laboratory pract
16、ice. This International Standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions. IMPORTANT It is absolu
17、tely essential that tests conducted according to this International Standard be carried out by suitably trained staff. 1 Scope This International Standard defines a method for the determination of lipophilic substances of low volatility in water using gravimetry. The method is applicable to all kind
18、s of water and allows the determination of low-volatility lipophilic substances which are suspended, emulsified, or dissolved, in concentrations of about 10 mg/l to 500 mg/l. Above this value, the test portion is diluted appropriately. The method is not applicable to water with a separate oil layer.
19、 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 amendments) applies. ISO 3696, Water for analy
20、tical laboratory use Specification and test methods 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 low-volatility lipophilic substances sum of substances extractable by non-polar hydrocarbons, determined gravimetrically after drying at 80 C
21、NOTE Substances covered by this definition are unpolar or weakly polar, with a boiling point above 250 C, and include mainly animal oils, vegetable oils, fats, greases, mineral oils, waxes, and non-ionic surfactants. 4 Principle A test portion of water is extracted with an extracting agent. The extr
22、acting agent is evaporated. The mass of low-volatility lipophilic substances is determined by gravimetry. BS ISO 11349:2010ISO 11349:2010(E) 2 ISO 2010 All rights reserved5 Interferences The formation of stable emulsions caused by surface active substances may lead to the inclusion of extracting age
23、nts in the emulsion and thus to losses. 6 Reagents All reagents shall be suitable for the purpose of this method and shall not significantly influence the blank (see 9.1). 6.1 Water, as specified in ISO 3696, grade 3, distilled water or deionized water. 6.2 Extracting agent. Hydrocarbon or technical
24、 mixture of hydrocarbons, boiling range 36 C to 69 C (e.g. petroleum ether 40 C to 60 C, n-hexane). 6.3 Sodium sulfate, Na2SO4, anhydrous, coarse grained. 6.4 Magnesium sulfate heptahydrate, MgSO47H2O, coarse grained. 6.5 Mineral acid, e.g. sulfuric acid, c(H2SO4) = 2 mol/l ( = 1,12 g/ml). 6.6 Veget
25、able oil, as test substance for the determination of the recovery. NOTE Olive oil has proved to be most suitable. Sunflower oil can be suitable as well. 6.7 Acetone, C3H6O. 7 Apparatus Clean all glass apparatus according to normal cleaning procedures and check the purity by blank determination. If n
26、ecessary, rinse the apparatus with extracting agent (6.2). Usual laboratory equipment and in particular the following. 7.1 Sampling vessel, glass, with glass stopper or polytetrafluoroethene-lined screw cap, e.g. 1 000 ml. 7.2 Homogenization device, e.g. Ultraturrax1). 7.3 Extracting vessel, 1 000 m
27、l. 7.4 Shaking device or magnetic stirrer. 7.5 Separating funnel, e.g. 500 ml. NOTE For phase separation another suitable device can also be used, e.g. a micro-separator. 7.6 Erlenmeyer flask or round-bottomed flask, 250 ml. 7.7 Glass filter funnel with hydrophobic filter. 7.8 Measuring cylinders, g
28、lass, capacities 100 ml, 250 ml, and 500 ml, ISO 47881. 1) Ultraturraxis an example of a suitable product available commercially. This information is given for the convenience of users of this International Standard and does not constitute an endorsement by ISO of this product. BS ISO 11349:2010ISO
29、11349:2010(E) ISO 2010 All rights reserved 37.9 Suitable concentration device, e.g. Rotavapor2). 7.10 Drying oven. 7.11 Desiccator, with a diameter of, for example, 100 mm, 200 mm or 300 mm. 7.12 Balance, capable of being read to at least 0,1 mg. 8 Sampling and sample conservation Fill the sampling
30、vessel (7.1) to about 80 % by volume with the sample and close tight. If analysis is not carried out the same day, add mineral acid (6.5) to adjust the pH to u2. Store at about 4 C and analyse within 7 d. 9 Procedure 9.1 Blank determination Carry out blank determinations regularly including all reag
31、ents and apparatus, in the same way as described for the samples, but replacing the test portion by 500 ml of water (6.1). The blank shall not exceed 3 mg/l. 9.2 Recovery check Prior to determination of the low-volatility lipophilic substances, check the method by extraction of a test substance as f
32、ollows. Transfer 500 ml of water (6.1) to the extracting vessel (7.3) and add about 100 mg of vegetable oil (6.6), precisely weighed and prediluted with about 1 ml of acetone (6.7), and continue the procedure according to this method. The recovery shall be between 90 % and 105 %. 9.3 Extraction Acid
33、ify the water sample to a pH of u2 with mineral acid (6.5), if this step has not already been carried out according to Clause 8. After intensive homogenization (7.2), a test portion of volume, V, between 100 ml and 500 ml is transferred to an extracting vessel (7.3). If necessary, dilute this test p
34、ortion with water (6.1) up to a final volume of approximately 500 ml. Add 50 ml of extracting agent (6.2). Shake several times by hand, allow for pressure adjustment by carefully opening the extracting vessel under a hood. Stopper the vessel and shake intensively for 15 min or intensively stir using
35、 a magnetic stirrer (7.4). Make sure that the stirring cone reaches the bottom of the vessel. For phase separation, allow to stand for 20 min in a separating funnel (7.5), then remove the aqueous phase. Any emulsion formed may be broken by adding in portions up to 20 g of magnesium sulfate heptahydr
36、ate (6.4) and/or sodium sulfate (6.3). Shake after each addition of salt and allow for overpressure release. Wait for phase separation and add any remaining emulsion to the water phase. 2) Rotavapor is an example of a suitable product available commercially. This information is given for the conveni
37、ence of users of this International Standard and does not constitute an endorsement by ISO of this product.BS ISO 11349:2010ISO 11349:2010(E) 4 ISO 2010 All rights reservedRepeat the extraction step with a further 50 ml of extracting agent (6.2) and combine the organic phases. The volume of the reco
38、vered organic phases shall be at least 75 % of the volume of the added extracting agents. If not, repeat the determination with a test portion of smaller volume or with a larger volume of extracting agent. Dry the organic phase with 10 g of sodium sulfate (6.3). Filter the extract using a hydrophobi
39、c filter (7.7) into a flask (7.6) whose mass, m1, has previously been recorded. Rinse the vessel, filter, and sodium sulfate two or three times with about 10 ml of extracting agent (6.2) and add the rinsings to the extract. 9.4 Concentration step Concentrate the extract to about 2 ml using the conce
40、ntration device (7.9). Carefully strip the remaining extracting agent either by blowing nitrogen over it in an exhaust hood or by further treatment in the concentration device. Continue the drying step in an oven (7.10) for 15 min at (80 3) C. Allow the flask and its contents to cool in a desiccator
41、 (7.11) and weigh. Record the mass as m2. Ensure that no crystalline sodium sulfate is visible in the flask. If the weighed mass is above 250 mg, repeat the analysis procedure from 9.3 onwards with a smaller test portion, diluted as appropriate. 10 Calculation Calculate the mass concentration of low
42、-volatility lipophilic substances according to Equation (1): 21mmV= (1) where is the mass concentration, in milligrams per litre, of low-volatility lipophilic substances; m2is the mass, in milligrams, of the flask with contents (9.4); m1is the mass, in milligrams, of the empty flask (9.3); V is the
43、volume, in litres, of the test portion (9.3). 11 Expression of results Report the mass concentration, in milligrams per litre, of low-volatility lipophilic substances to two significant figures. EXAMPLE Low-volatility lipophilic substances: 15 mg/l. BS ISO 11349:2010ISO 11349:2010(E) ISO 2010 All ri
44、ghts reserved 512 Test report The test report shall contain at least the following information: a) the test method used, together with a reference to this International Standard (ISO 11349:2010); b) all the information required for the complete identification of the sample; c) details of sampling, s
45、ample transportation, and sample preparation; d) details of any sample pretreatment; e) test result, according to Clause 11; f) all operation details not specified in this International Standard, or regarded as optional, together with details of any incident that may have influenced the result(s). B
46、S ISO 11349:2010ISO 11349:2010(E) 6 ISO 2010 All rights reservedAnnex A (informative) Precision data The results from an interlaboratory trial, carried out in Germany in spring 2007 are given in Table A.1. Table A.1 Precision data calculated in accordance with ISO 5725-22Sample 1 2 Matrix Parameter
47、Industrial waste water I Industrial waste water II No. laboratories after elimination of outliers, p 16 13 No. results after elimination of outliers, n 34 28 Percentage of outliers, nOP, % 5,6 12,5 Total mean of all analytical results (after elimination of outliers), , mg/l 14,3 200,4 Reproducibilit
48、y standard deviation, sR, mg/l 4,88 19,93 Coefficient of variation of reproducibility, CV,R, % 34,2 9,9 Repeatability standard deviation, sr, mg/l 2,03 10,62 Coefficient of variation of repeatability, CV,r, % 14,2 5,3 BS ISO 11349:2010ISO 11349:2010(E) ISO 2010 All rights reserved 7Bibliography 1 IS
49、O 4788, Laboratory glassware Graduated measuring cylinders 2 ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method BS ISO 11349:2010ISO 11349:2010(E) ICS 13.060.50 Price based on 7 pages ISO 2010 All rights reserved This page deliberately left blankBSI is the independent national body responsible for preparing British Standardsand other standards-r
