1、BRITISH STANDARD BS ISO 10540-3:2002 Animal and vegetable fats and oils Determination of phosphorus content Part 3: Method using inductively coupled plasma (ICP) optical emission spectroscopy ICS 67.200.10 BS ISO 10540-3:2002 This British Standard was published under the authority of the Standards P
2、olicy and Strategy Committee on 29 January 2003 BSI 29 January 2003 ISBN 0 580 41151 6 National foreword This British Standard reproduces verbatim ISO 10540-3:2002 and implements it as the UK national standard. The UK participation in its preparation was entrusted to Technical Committee AW/307, Oil
3、seeds animal and vegetable fats and oils, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international publications referred to in this document may be found in
4、 the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purport to include all the necessary provisions of a contract. Users are responsib
5、le for its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the U
6、K interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the ISO title page, pages ii and iii, a blank page, pages 1 to 8, an inside back cover and a back cover. The BSI
7、 copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date Comments Reference number ISO 10540-3:2002(E)INTERNATIONAL STANDARD ISO 10540-3 First edition 2002-12-01 Animal and vegetable fats and oils Determination of phosp
8、horus content Part 3: Method using inductively coupled plasma (ICP) optical emission spectroscopy Corps gras dorigines animale et vgtale Dtermination de la teneur en phosphore Partie 3: Mthode par spectromtrie dmission optique avec plasma induit par haute frquence BSISO105403:2002IS-04501 O3:(2002E)
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13、uotfo yr ttseuqer ehe.r ISO cirypothg fofice saCe tsopale 65 eneG 1121-HC 02 av leT. 4 + 10 947 22 1 11 xaF0 947 22 14 + 9 74 E-mial coirypthgis.o gro We bwww.is.o groii BSISO105403:2002 iiiForeword ISO (the International Organization for Standardization) is a worldwide federation of national standa
14、rds 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 has the right to be represented on that committee. International organ
15、izations, 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. International Standards are drafted in accordance with the rules given i
16、n the ISO/IEC Directives, Part 2. The main task of technical committees 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 %
17、 of the member bodies casting a vote. 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. ISO 10540-3 was prepared by Technical Committee ISO/TC 34, Food
18、 products, Subcommittee SC 11, Animal and vegetable fats and oils. ISO 10540 consists of the following parts, under the general title Animal and vegetable fats and oils Determination of phosphorus content: Part 1: Colorimetric method Part 2: Method using graphite furnace atomic absorption spectromet
19、ry Part 3: Method using inductively coupled plasma (ICP) optical emission spectroscopy BSISO105403:2002INTENRATIONAL TSANDADR IS-04501 O3:(2002E)1Animal and vegetable fats and oils Determination of phosphorus content Part 3: Method using inductively coupled plasma (ICP) optical emission spectroscopy
20、 1 Scope This part of ISO 10540 specifies a method for the quantification of phosphorus in oil, which is limited to oils with low phosphorus content, without any turbidity or visible sediment. Depending on the dilution solvent used, most types of vegetable oils can be analysed (crude, degummed, refi
21、ned, bleached, deodorized and hardened oils) and nearly all types of lecithins and phosphatides. This method is only suitable when phosphorus is present in a solubilized form. When it is present as fine particles, such as bleaching earth, ICP-OES analysis results in poor recovery as a result of nebu
22、lization and atomization problems. The only suitable non-ashing direct method for these samples is graphite furnace atomic absorption spectrometry. ISO 10540-1 is the reference (colorimetric) method for the determination of the phosphorus content in fats and oils. 2 Normative references The followin
23、g 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 661, Animal and vegetable fats and oils Preparation of te
24、st sample 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 phosphorus content dissolved phosphorus measured according to the method specified in this part of ISO 10540 NOTE It is measured in milligrams per kilogram. 4 Principle Solvent-diluted
25、 vegetable oils are analysed for phosphorus by direct aspiration. Liquid samples are nebulized and carried into the excitation source by a flowing gas. Atoms are quantified by measuring the specific emission lines produced by atoms decaying from high energy levels. BSISO105403:20022 5 Reagents Use o
26、nly reagents of recognized analytical grade, unless otherwise specified. 5.1 Butanol. 5.2 Kerosene. 5.3 Xylene. 5.4 Standard element, present in solution as an organic soluble material 1) . 5.5 Base oil (Base 20 or Base 75 Oil) 1) , used to check the blank oil used and for the dilution of the standa
27、rd solutions as needed. 6 Apparatus Usual laboratory equipment and, in particular, the following. 6.1 Inductively coupled plasma optical emission spectrometer. 6.2 Analytical balance, capable of weighing to the nearest 0,001 g and displaying 0,000 1 g. 6.3 Oven, capable of maintaining a temperature
28、of 60 C 2 C. 6.4 Tilt table mixer. 6.4 Volumetric flasks, of 100 ml capacity. 7 Sampling It is important that the laboratory receive a sample that is truly representative and has not been damaged or changed during transport and storage. Sampling is not part of the method in this International Standa
29、rd. A recommended sampling method is given in ISO 5555. 8 Preparation of test sample Prepare the test samples in accordance with ISO 661, except that the samples should not be clarified. If the sample is not clear when liquid, this method should not be used. 1) SPEX, 203 Norcross Ave., Metuchen, NJ
30、08840 (908/549-7144) and Base 20 Oil or Base 75 Oil and Constan brand standards available from Accu-Standard, 25 Science Park, New Haven, CT 06511 (800-442-5290) are examples of suitable products available commercially. This information is given for the convenience of users of this part of ISO 10540
31、 and does not constitute an endorsement by ISO of these products. BSISO105403:2002 39 Procedure 9.1 General 9.1.1 Dilute all samples, standards and blanks 1:1 (by mass) with 1-butanol (or kerosene/xylene) to reduce the viscosity of the oil for better nebulization. Some samples are more soluble in 1-
32、butanol than others. NOTE 1 1-Butanol is preferred because it has better moisture tolerance and allows a higher flow rate with higher pressure than kerosene without extinguishing the torch. The increased moisture tolerance permits the analysis of crude oils and lecithins without phase separation. Th
33、e higher flow rate provides for improved detection limits. 9.1.2 Melt solid samples at approximately 10 C above their melting point and mix prior to dilution. Keep the diluted sample warm and monitor throughout the analysis to ensure that it remains in solution. The maximum temperature for the analy
34、sis of hardened fats is 60 C. 9.1.3 Precise operating conditions will vary from instrument to instrument. Operate your instrument according to the manufacturers directions and specifications. Conditions used for identical instruments from the same manufacturer will vary depending on the type of nebu
35、lizer and pumping system used. If kerosene or xylene is used, all instrumental operating conditions, such as pump flow rate, will change from those set for 1-butanol. Therefore, the analysis shall be standardized and all analyses run with all standards, blank and samples dissolved in the same solven
36、t. NOTE 2 Some of the conditions used in the collaborative study are given in Annex B. 9.1.4 Ignite the instrument and allow it to warm up. It is profiled on an internal Hg lamp. Phosphorus may be detected at the major emission lines of 178,2 nm, 213,6 nm or 214,9 nm. Limits of detection are approxi
37、mately 0,5 mg/kg. 9.1.5 Standardize the instrument as described (9.3) and scan all the samples in triplicate. NOTE 3 Calibration drift has been noted. It may result from carbon build-up on the injector tip. 9.2 Preparation of standards 9.2.1 Blank Typically, refined and bleached soya bean, or anothe
38、r oil that has been shown to be free of trace elements, is used. Blank oil is diluted 1:1 as described in 9.1.1. Base 20 or Base 75 oil (5.5) is used as an absolute reference blank to determine that the blank oil is free of trace elements. 9.2.2 Phosphorus standard solution The phosphorus standard i
39、s prepared from commercially available single-element organic-based standard. Weigh accurately the standard and add enough blank oil to total 50,00 g. Add 50,00 g of solvent (1-butanol, kerosene or xylene) to achieve a 1:1 dilution. Although one standard concentration will work, up to four standards
40、 will provide a better calibration for linearity and accuracy. Levels should include 2,5 mg/kg, 5,0 mg/kg and 10,0 mg/kg standards depending on the range of values expected. If an internal standard is used, it may be weighed as part of the elements or incorporated as part of the dilution solvent to
41、yield 10 mg/kg to match that amount added to the sample. BSISO105403:20024 9.3 Standardization Run the blank oil standard and diluted Base 20 or Base 75 oils at the specified wavelength for phosphorus. Run the phosphorus standard solutions (9.2.3) at the phosphorus wavelength chosen. Scan blanks, sa
42、mples and standards in triplicate for phosphorus and average them. Run standards and the blank every 10 samples or less and restandardize the instrument as needed. For accuracy use a narrow range of standardisation (0 mg/kg to 25 mg/kg of phosphorus). Although the linearity is somewhat greater, test
43、 samples should be diluted to keep the phosphorus content within the range of standardization. 9.4 Preparation of test samples Weigh 2,5 g ( 0,02 g) of sample into an autosampler tube and dilute with 2,5 g of 1-butanol (kerosene or xylene) delivered from an automatic pipette. Cap the tube and invert
44、 40 to 50 times on a mixing table. Dilute 0,2 g of lecithins (up to 100 % acetone-insoluble) to 5,0 g with blank soybean oil and then to 10 g with 1-butanol. Mix the samples on a tilt table mixer for 1 h and then dilute 1:10 with 1:1 blank oil/1-butanol to give a total dilution of 1:500. 10 Calculat
45、ion Computation is a feature of most instrument programs. Area counts from known standards are inserted into a linear regression formula. From this relationship, concentrations may be determined from the area counts of the samples. It is important to include the correct dilution factor. 11 Precision
46、 11.1 Interlaboratory test Details of interlaboratory tests on the precision of the method are summarized in Annex A. The values derived from these interlaboratory tests may not be applicable to concentration ranges and matrices other than those given. 11.2 Repeatability The absolute difference betw
47、een two independent single test results, obtained with the same method on identical test material in the same laboratory by the same operator using the same equipment within a short interval of time, will in not more than 5 % of cases be greater than the repeatability limit (r) as shown in Annex A.
48、11.3 Reproducibility The absolute difference between two single test results, obtained with the same method on identical test material in different laboratories with different operators using different equipment, will in not more than 5 % of cases be greater than the reproducibility limit (R) as sho
49、wn in Annex A. BSISO105403:2002 512 Test report The test report shall specify: all information necessary for the complete identification of the sample; the sampling method used, if known; the test method used, with reference to this part of ISO 10540; all operating details not specified in this part of ISO 10540, or regarded as optional, together with details of any incidents which may have influenced the test result(s); the test result
